Growth, Characterization, and Applications of Doped-YAG

Single-crystal Fibers

Chia-Yao Lo

Dr. Sheng-Lung Huang

Nd:YAG
Cr:YAG ASE

2004 12 30


(Nd:YAG)
0.0284
80 mW
28.9% Nd:YAG

(Cr4+:YAG)
Cr4+:YAG

fused silica
29 m 0.1 dB/cm
7 Cr4+

25 m 2.36
mW 265 nm

1.47 m 16 dB

i
 Abstract
Pulling bulk crystal into fiber is suitable for laser, amplified spontaneous
emission (ASE), and optical amplifier applications in optical communications because
of its structural similarity to silica fiber. Moreover, fiber configuration can confine
pump light in a small cross-sectional area with a high energy density for a long
distance. Among crystal fiber growth techniques, the laser-heated pedestal growth
method (LHPG) was adopted. It is crucible free and can therefore produce high-purity,
low-defect-density single crystals. However, interface loss of the crystal fiber is one
of the main causes of optical loss. In order to reduce the optical loss, a proper method
to clad the fiber is important for high device performance.

For laser application, high-efficient Nd:YAG lasers were demonstrated using

gradient-index crystal fibers. We used controlled profile of the active ion resulted in
index difference of 0.0284 between the center and the edge of the fiber to confine the
laser beam in the center region and thus reduced the interface loss. A laser output
power of 80 mW was achieved with a slope efficiency of 28.9%, which, to our
knowledge, is the highest ever achieved for diode-laser-pumped Nd:YAG fiber laser.

For ASE and optical amplifier applications, Cr4+:YAG crystal fiber was studied
due to its fluorescent spectrum just covering the low loss window of silica optical
fiber. To reduce the fiber diameter and propagation loss, a novel cladding technique,
codrawing LHPG (CDLHPG), was developed. Although fused-silica-clad fiber can be
made with a 29-m-diameter core and a propagation loss of less than 0.1 dB/cm,
which is a factor of 7 smaller than that of an unclad fiber, it has almost no Cr4+
fluorescence in the core area due to the entering of SiO2 in YAG. With proper
controlled growth parameters of the CDLHPG method, a double-clad fiber with a core
diameter of 25 m was successfully grown. Up to 2.36 mW of ASE with a bandwidth
of 265 nm was demonstrated. After splicing the double-clad fiber with conventional
single mode fiber, we successfully demonstrated the first transition metal-doped fiber
amplifier in the optical fiber communication band. Up to 16-dB of gross gain at 1.47
m was achieved.

ii
 Table of Contents
i
Abstract ii
Table of Contents . iii
List of Tables. v
List of Figures... vi

Chapter 1 Introduction ... 1

Chapter 2 Laser-heated pedestal growth system .. 6

2.1 Single crystal fiber growth ... 6
2.2 LHPG apparatus ... 9
2.3 Fabrication process of single-crystal fiber ... 11

Chapter 3 Nd3+:YAG crystal fibers .... 15

3.1 Properties of Nd3+:YAG crystal 15
3.2 Characterization of Nd:YAG crystal fiber 18
3.2.1 X-ray diffraction analysis ... 18
3.2.2 Composition analysis ..... 19
3.2.3 Refraction index measurement 21
3.3 Nd:YAG crystal fiber laser ... 25
3.3.1 Fabrication of Nd:YAG fiber laser ...... 25
3.3.2 Characterization of Nd:YAG fiber laser ... 28

Chapter 4 Simulation of Cr4+:YAG crystal fiber devices 32

4.1 Properties of Cr4+:YAG crystal . 32
4.2 Rate equation analysis .. 37
4.3 Simulation of ASE light source 39
4.4 Simulation of laser ... 41

Chapter 5 Characterization of Cr4+:YAG crystal fibers .. 49

5.1 Single crystal fiber ... 49
5.1.1 X-ray diffraction analysis ... 49
5.1.2 Composition analysis ..... 50
5.1.3 Oxidation state analysis ...... 53
5.2 Single-clad crystal fiber ... 59
5.2.1 Growth of single-clad crystal fiber .. 59
5.2.2 Composition analysis ..... 61

iii
 5.2.2.1 Electron probe microanalysis ... 61
5.2.2.2 Cr ion fluorescence measurements .... 62
5.3 Double-clad crystal fiber .. 63
5.3.1 Growth of double-clad crystal fiber . 63
5.3.2 Composition analysis ..... 64
5.3.2.1 Electron probe microanalysis ... 64
5.3.2.2 Cr ion fluorescence and refraction index measurements .... 65
5.3.3 Microstructure analysis using high-resolution TEM . 67
5.3.3.1 Microstructure of core 67
5.3.3.2 Microstructure of inner cladding .. 70
5.3.3.3 Comparison between inner cladding and outer cladding .... 73
5.3.3.4 Comparison of inner cladding with different growth speeds ... 74
5.4 Propagation loss measurement . 77

Chapter 6 Applications of Cr4+:YAG crystal fibers . 80

6.1 ASE light source ... 80
6.1.1 Single crystal fiber ..... 80
6.1.2 Single-clad crystal fiber .. 82
6.1.3 Double-clad crystal fiber .... 84
6.2 Double-clad crystal fiber amplifier .. 88
6.2.1 Fusion of a double-clad fiber with a single-mode fiber . 88
6.2.2 Characterization of double-clad fiber amplifier .... 91

Chapter 7 Conclusions and future work ... 96

7.1 Conclusions .. 96
7.2 Future work .. 98

References . 100
Biography .. 109
Publication List.. 110

iv
 List of Tables
Table 3.1 Structural information and atomic position data of YAG.. 16
Table 3.2 Physical and optical properties of Nd:YAG....... 16
Table 3.3 YAG branching ratio of emission from 4F3/2.. 18
Table 3.4 SiC grit size (Europe). 25
Table 3.5 The mechanical preparation of Nd:YAG crystal fiber laser samples. 25
Table 4.1 Optical properties of Cr4+:YAG.. 34
Table 4.2 Comparison of lattice mismatch between dopant ions and host ions. 35
Table 4.3 Characteristics of Cr:YAG and Cr,Ca:YAG crystal fibers..... 35
Table 4.4 Parameters used for ASE power simulation... 41
Table 4.5 Simulation parameters used in Fig 4.8... 44
4+
Table 4.6 Simulation parameters of Cr :YAG fiber laser..... 45
Table 5.1 Average doping concentrations of Cr4+:YAG raw materials.. 50
Table 5.2 Average doping concentrations of Cr4+:YAG crystal fibers... 51
Table 5.3 Physical properties of borosilicate and fused-silica glasses... 60
Table 5.4 The average sizes and the relative densities of nanoscale particles... 76
Table 6.1 ASE power generated from different core diameters. 86
Table 6.2 Parameters of simulated ASE power.. 86
Table 6.3 Comparison of parameters of absorption, emission and excited-
state absorption cross section..... 87
Table 6.4 The parameters for insertion loss calculation..... 91

v
 List of Figures
Fig. 1.1 Evolution of gain ranges of rare earth-doped fiber amplifiers.
PDFA, TDFA, and EDFA denote praseodymium, thulium, and
erbium-doped fiber amplifiers, respectively. The scripts, -F, -T, and
-S, denote fluoride, tellurite, and silica-based fiber amplifiers,
respectively. 3
Fig. 1.2 Cladding techniques for crystal fibers.... 4
Fig. 2.1 Solidification in capillary tube... 6
Fig. 2.2 Edge-defined film-fed growth 7
Fig. 2.3 Schematic drawing of the -CZ technique. 7
Fig. 2.4 Schematic diagram of the -PD growth apparatus. 8
Fig. 2.5 Laser-heated pedestal growth method.... 9
Fig. 2.6 LHPG system..... 10
Fig. 2.7 Growth chamber..... 10
Fig. 2.8 Mated three-piece design for the diamond-turned copper reflaxicon
element... 11
Fig. 2.9 Illustration of single-crystal growth via the LHPG method... 11
Fig. 2.10 Laser power, P, as a function of source rod diameter. The insets
shows a photograph of YAG molten zone.. 12
Fig. 2.11 Al2O3-Y2O3 phase diagram.... 13
Fig. 2.12 Photograph of a Cr4+:YAG single-crystal fiber with a 70-m
diameter grown by the LHPG method... 13
Fig. 2.13 (a) Photograph of a polished end of a YAG crystal fiber. (b)
Drawing of the YAG atomic structure viewed from <111> direction 14
Fig. 3.1 Crystal structure of YAG. Aluminum atoms occupy tetrahedral and
octahedral polyhedral in YAG. Yttrium atoms are surrounded by
eight oxygen atoms......... 15
Fig. 3.2 Absorption spectrum of Nd:YAG at 300K. 17
Fig. 3.3 Energy level diagram of Nd:YAG.. 17
Fig. 3.4 Calculated diffraction pattern of YAG pattern... 18
Fig. 3.5 X-ray diffraction patterns of (a) the raw material, (b) the 250-m
diameter crystal fiber. The lower parts are the enlargement of main
peaks of upper parts... 19
Fig. 3.6 (a) Schematic diagram of the Nd3+ doping distribution in source
rod and crystal fiber, (b) photograph of line scanning marks on the
cross section of crystal fiber... 20
Fig. 3.7 Doping profiles of Nd:YAG crystal fibers for different growth
rates. The fibers diameters are all 220 m..... 21
Fig. 3.8 Doping profiles of Nd:YAG crystal fibers with multiple regrowth... 21
Fig. 3.9 Configuration of an optical low-coherence reflectometer.. 22
Fig. 3.10 Experimental setup of refraction index measurement of gradient-
index crystal fiber... 23

vi
Fig. 3.11 (a) Collection of reflections by a lens with a numerical aperture of
0.11. The peaks marked with numbers represent the multiple
round-trip reflections from the end face of a 250-m crystal fiber.
(b) Simulated numerical aperture of light of the reflected beam
after multiple round-trips. The length of the crystal fiber is 7.72
mm...... 24
Fig. 3.12 The cross sectional images of a crystal fiber after (a) 1/4 m
diamond polishing, and (b) 1/4 m alumina polishing.. 26
Fig. 3.13 Surface profiles of the crystal fiber after (a) 1/4 m diamond
polishing, and (b) 1/4 m alumina polishing. The outer diameter of
the Pyrex glass capillary is 7 mm... 27
Fig. 3.14 The reflectance of the coatings on the front and end facets of the
crystal fiber laser.... 28
Fig. 3.15 Configuration of the Nd:YAG fiber laser... 29
Fig. 3.16 Slope efficiency vs the output transmittance for pumping sources
of fiber-pigtailed and bare LDs. The symbols are experimental data
and the lines are fitted.... 29
Fig. 3.17 CW output power of the gradient-index Nd:YAG crystal fiber laser
as a function of the absorbed pump power for different output
couplers...... 30
Fig. 3.18 Experimental setup of near-field beam patterns of the fiber laser
measurement....... 31
Fig. 3.19 Near-field beam patterns of the fiber laser in vertical and horizontal
directions. Note: the pulsed behaviors are artifacts of the CCD
array used. Only the envelopes represent the near-field beam
patterns....... 31
Fig. 4.1 Energy level diagram of the Cr4+:YAG crystal... 32
Fig. 4.2 Room temperature absorption spectrum of Cr4+:YAG... 33
Fig. 4.3 Room temperature emission spectrum of Cr4+:YAG.. 33
Fig. 4.4 Configuration of the Cr4+ ion in Cr4+:YAG lattice. It is surrounded
by four oxygen ions in tetrahedral arrangement..... 34
Fig. 4.5 (a) Percentage of Cr4+ to total Cr as a function of Ca/Cr, (b) Cr4+
lifetime as a function of Cr4+ concentration....... 36
Fig. 4.6 Simplified energy level diagram of Cr4+:YAG....... 37
The simulated ASE power as a function of pump power for
Fig. 4.7
different core diameters of the Cr:YAG crystal fiber. 40
Fig. 4.8 The corresponding (a) gains and (b) needed fiber lengths in Fig 4.7. 40
Fig. 4.9 The dependence of the population density and cavity laser intensity
with time. 43
Fig. 4.10 Threshold pump power as a function of propagation loss for
different small signal absorption coefficients. 45
Fig. 4.11 Laser output power as a function of propagation loss.... 46
Fig. 4.12 Laser output power as a function of transmittance of the output
face. 46

vii
Fig. 4.13 Laser output power as a function of fiber core diameter at a
propagation loss of 0.02 dB/cm.. 47
Fig. 4.14 Laser output power as a function of crystal boundary temperature... 47
Fig. 5.1 X-ray diffraction patterns of (a) the raw material and (b) the
400-m diameter fiber.... 49
Fig. 5.2 Doping profiles of (a) Cr2O3 and (b) CaO with multiple regrowths.. 51
Fig. 5.3 Average Cr2O3 concentration of fibers with multiple regrowths... 52
Fig. 5.4 Doping profiles of fibers with different growth speeds..... 52
Fig. 5.5 Schematic drawing of the scanning optical microscope........ 53
Fig. 5.6 (a) fluorescence image and (b) spectrum of Cr3+ ions........ 54
Fig. 5.7 (a) fluorescence image and (b) spectrum of Cr4+ ions........ 55
Fig. 5.8 Cr3+ fluorescence image with different fiber diameters..... 55
Fig. 5.9 Cr3+ fluorescence intensity and Cr2O3 concentration measured by
SOM and EPMA, respectively....... 56
Fig. 5.10 Cr2O3 concentration with different fiber diameters measured by
SOM....... 57
Fig. 5.11 Cr4+ fluorescence intensity with different fiber diameters..... 57
Fig. 5.12 Comparison of Cr4+, Cr2O3, and CaO concentrations in (a) 920 m
diameter and (b) 66 m diameter crystal fibers..... 58
Fig. 5.13 The functional dependence between normalized Cr4+ and Ca2+
concentrations..... 59
Fig. 5.14 (a) Schematic of codrawing laser-heated pedestal growth method,
and photographs of the polished end of (b) a 29-m-core diameter
fused-silica-clad Cr:YAG fiber, (c) a 100-m-core diameter
borosilicate-clad Cr:YAG fiber.......... 61
Fig. 5.15 Distribution of major compositions by line scanning the
cross-section of (a) fused-silica-clad Cr:YAG fiber, and (b)
borosilicate-clad Cr:YAG fiber. The regions between the two
vertical lines designate the core areas........ 62
Fig. 5.16 Cr4+ fluorescence of fused silica and borosilicate-clad Cr:YAG
fibers....... 63
Fig. 5.17 Left: Schematic diagram of the molten zone during growth, right:
photograph of the side view of the grown double-clad Cr4+:YAG
fiber........ 64
Fig. 5.18 Distribution of major compositions by line scanning the
cross-section of the double-clad Cr4+:YAG crystal fiber. The region
between the two vertical lines designates the core area. The inset
shows the photograph of the polished end with a 25-m-diameter
core......... 65
Fig. 5.19 Line scans of Cr fluorescence intensity of a double-clad Cr4+:YAG
crystal fiber......... 66
Fig. 5.20 Line scan of refraction index of a double-clad Cr4+:YAG crystal
fiber.... 66
Fig. 5.21 (a) TEM image of the core ( 4000), and (b) an enlargement of the

viii
 rectangular area in (a)..... 68
Fig. 5.22 Atomic image of the core. The inset shows an atomic drawing of
YAG structure viewed from <111>-direction..... 69
Fig. 5.23 The SAD pattern of the core...... 70
Fig. 5.24 (a) A cross-sectional image of double-clad fiber and the areas taken
for dark-field images were marked with rectangular blocks (A and
B); (b) the dark-field image of region A; (c) the dark-field image of
B......... 71
Fig. 5.25 (a) HRTEM image of region A, and (b) an enlargement of the
rectangular area in (a)............. 72
Fig. 5.26 HRTEM image of region B............ 73
Fig. 5.27 HRTEM images showing (a) the interface between the inner and
outer cladding. (b) The high magnification of the interface in the
rectangle............. 73
Fig. 5.28 Electron diffraction patterns in (a) outer cladding and (b) inner
74
cladding..........
Fig. 5.29 TEM images show the interface between the outer and inner
cladding for the growth speeds of (a) 3.75 mm/min and (b) 30
mm/min, respectively............. 75
Fig. 5.30 HRTEM images show the distribution of crystalline structure in the
inner cladding for the different growth speeds of (a) 3.75 mm/min,
and (b) 30 mm/min............. 76
Fig. 5.31 Experimental setup of the propagation loss measurement..... 77
Fig. 5.32 (a) Absorption coefficient and (b) propagation loss of borosilicate-
clad fiber as a function of incident power...... 78
Fig. 5.33 Attenuation coefficient of fused-silica-clad fiber as a function of
incident power........ 79
Fig. 5.34 (a) Absorption coefficient and (b) propagation loss of double-clad
fiber........ 79
Fig. 6.1 Experimental setup of ASE power of Cr4+:YAG crystal fiber
measurements..... 80
Fig. 6.2 ASE output power of Cr4+:YAG crystal fiber. Inset shows the end
face of the polished crystal fiber.... 81
Fig. 6.3 Calculated ASE power and upper level population density along
the length of the Cr4+:YAG crystal fiber.... 81
Fig. 6.4 Experimental setup for the ASE power measurement of
borosilicate-clad Cr4+:YAG crystal fiber.... 82
Fig. 6.5 ASE output power of the borosilicate-clad Cr4+:YAG crystal fiber.
Inset shows the end face of the polished crystal fiber.... 82
Fig. 6.6 Fluorescence spectra of borosilicate-clad Cr4+:YAG crystal fiber
and Cr4+:YAG crystal fiber without cladding..... 83
Fig. 6.7 Calculated ASE power and upper level population density along
the length of borosilicate-clad Cr4+:YAG crystal fiber... 83
Fig. 6.8 ASE output power of the double-clad Cr4+:YAG crystal fiber. Inset
shows the end face of the polished crystal fiber. 84

ix
Fig. 6.9 ASE (a) fluorescence spectrum, and (b) power stability of the
double-clad Cr4+:YAG crystal fiber.... 85
Fig. 6.10 Calculated ASE power and upper level population density along
the length of double-clad Cr4+:YAG crystal fiber.. 85
Fig. 6.11 Calculated ASE power as a function of pump power for different
small signal absorption coefficients... 87
Fig. 6.12 Calculated ASE power as a function of pump power for two types
of parameters...... 88
Fig. 6.13 Experimental setup of single-mode fiber/double-clad fiber splice 89
Fig. 6.14 Images of before and after fusions at two transverse directions on
Ericsson FSU 995 FA screen...... 89
Fig. 6.15 Return loss at a fusion splice (face 1) and the end face of a double-
clad fiber (face 2). The inset shows the experimental setup.. 90
Fig. 6.16 The enlargement of Fig. 6.15 at (a) peak1 and (b) peak2.. 90
Fig. 6.17 Experimental setup of insertion loss measurement 91
Fig. 6.18 Experimental setup of optical gain measurement.. 92
(a) The gross gains at a wavelength of 1.52 m, (b) Cr4+-doped
Fig. 6.19 fiber amplifier output spectra measured by an optical spectrum 93
analyzer with 0.06-nm resolution...
Fig. 6.20 The gross gains as a function of the signal wavelength for different
input signal powers at pump power of 1.16 W...... 94
Fig. 6.21 Comparison of the gain and ASE profiles... 94
Fig. 6.22 Calculated minimum noise figure of Cr:YAG fiber amplifier. The
inset shows the Cr4+ fluorescence spectrum and absorption
coefficient of Cr4+:YAG crystal fiber. 95
Fig. 7.1 A schematic diagram of a compact RGB lasers. 98

x
 Chapter 1 Introduction

Single-crystal fiber devices have great potential for use in optical fiber
communication modules/systems due to their structural similarity to silica fibers [1.1].
Moreover, a fiber can confine pump light in a small cross-sectional area with a high
intensity over a long distance. Its use in laser applications is very cost-effective in
terms of material consumption, which is typically one-thousandth that of bulk
material. In addition, heat dissipation in the gain medium can be significantly
alleviated because highly heat-conductive material can be applied to the
circumference of the crystal fiber. The laser-heated pedestal growth (LHPG) method
is now a well-established technique for the growth of single-crystal fibers [1.2]. It is
crucible free and can therefore produce high-purity, low-defect-density single crystals.
Besides, the ability to quickly grow single crystal of oxide compound makes it
possible to easily survey potential new hosts and dopings for laser gain medium,
optical amplifier, and nonlinear optical material.

Y3Al5O12 (YAG) has many properties that are desirable in a laser host material. It
is stable, hard, optically isotropic, and has good thermal conductivity, which permits
laser operation at high average power levels. Neodymium-doped yttrium aluminum
garnet (Nd:YAG) is a well-known laser gain medium with high gain and good thermal
and mechanical properties. Nd:YAG lasers were widely used in scientific, medical,
industrial, and military applications. Diode-laser-pumped solid-state laser has the
merits of diode laser, such as compact and high efficiency, as well as the merits of
solid-state laser, such as high mode quality, long fluorescence lifetime, and ease of
maintenance. Four milliwatts of threshold power was achieved in a Nd:YAG crystal
fiber laser using a diode laser as the pumping source [1.3]. However, the slope
efficiency was only 9.5 % and the output power was around 10 mW, which is much
less than that of the bulk Nd:YAG laser. Interface loss at the circumference between
crystal fiber and air is one of the dominant factors that reduce the efficiency of crystal
fiber lasers. It was pointed out that the doping concentration could have a graded
distribution [1.4-1.5]. Due to different crystal pulling conditions, the doping profile of

1
the active ions can be altered appreciably, which will change the index profile and
affect the laser performance in terms of cavity design, gain saturation, etc. Therefore,
it is important to obtain the index profile for laser design. Low-coherence
reflectometry was employed to characterize the index profile. We used a
gradient-index Nd:YAG crystal fiber laser where the laser beam is confined in the
central region of the core, thus reducs the interface loss and increases the slope
efficiency of crystal fiber lasers. A record-high slope efficiency of 28.9% was
achieved [1.6].

During the last decade, the maximum capacity of an optical fiber transmission
line more than doubled every year to match the fast-growing communication need.
The technology break through in dry fiber fabrication opens the possibility for fiber
bandwidth all the way from 1.3 m to 1.6 m. The fast-increasing demand for
communication capacity results in the emergence of wavelength division multiplexing
(WDM) technology, enabling tens of channels with different wavelengths to be
transmitted simultaneously on an optical fiber. However, the number of channels in
WDM system depends on the gain bandwidth of optical amplifiers. There are many
types of fiber amplifiers, which can be used to produce optical gains suitable for use
at different communication bands. Figure 1.1 shows the evolution of gain ranges of
rare earth-doped fiber amplifiers since the invention of fiber amplifier in 1987. The
standard amplifier is the well-known silica-based erbium-doped fiber amplifier
(EDFA), which provides gain in the C-band (1530-1565 nm) [1.7-1.8] and L-band
(1570-1605 nm) [1.9] even in the S-band (1450-1520 nm) [1.10]. The other types of
EDFAs are fluoride- [1.11] and tellurite- [1.12] based EDFAs. Thulium-doped fiber
amplifiers can give gain in the S-band. The thulium ions can be doped in fluoride
[1.13-1.14], tellurite [1.15] or silica glass [1.16]. Praseodymium-doped fiber
amplifiers can be operated in the O-band [1.17]. Fiber Raman amplifier (FRA) can
offer gain at broad spectral region as a suitable fiber and a pump are used. Using
silica-based FRA, the O- [1.18], E- [1.19], S- to L- [1.20-1.21] and U-bands [1.22]
have been reported. Tellurite-based FRA was also demonstrated in a WDM system
[1.23].

2
 O E S C L U
2005
TDFA-T
EDFA-S
TDFA-S
2000 TDFA-F

EDFA-T
Year

1995
TDFA-F
PDFA-F
EDFA-F EDFA-S
1990
EDFA-S

1985
1.2 1.3 1.4 1.5 1.6 1.7
Wavelength (m)
Fig. 1.1. Evolution of gain ranges of rare earth-doped fiber amplifiers. PDFA, TDFA, and
EDFA denote praseodymium, thulium, and erbium-doped fiber amplifiers, respectively. The
scripts, -F, -T, and -S, denote fluoride, tellurite, and silica-based fiber amplifiers, respectively.

Of all the methods mentioned above, the gain bandwidth cannot fully cover the
whole 1.3 to 1.6 m with a single fiber amplifier. It is well known that transition
metal doped materials have broadband emission, among them Cr4+ ions [1.24-1.26]
Ni2+ ions [1.27], and V3+ ions [1.28] have shown broadband 1.3-1.6 m emission. By
far, Cr4+ ions are inefficient when incorporate into a glass host, due to the difficulty to
control the local environment. By the addition of a charge-compensating codopant of
Ca2+ in Cr:YAG crystal, it has been shown that the percentage of Cr4+ to total Cr
doping can go up to 6.5% [1.29], which substantially increases the Cr4+ fluorescence
intensity. Besides, the 0.9~1.2 m optical pumping absorption range for Cr4+:YAG
covers available 910~980-nm broad-stripe diode laser with generous wavelength
tolerance, which leads to a compact, cost-effective package. The crystalline host
offers higher thermal conductivity and hence a higher power handling capability than
glass fibers. Such a fiber is, therefore, eminently suitable for super-wideband fiber
amplifier since the required pump power is expected to be higher. This wideband light
source can be used in WDM-component testing, slicing wideband spectrum to obtain
multi-channel light sources using filters, or optical coherence tomography.

3
 Cladding the fiber reduces both scattering loss and the number of propagating
modes. There are many techniques to fabricate crystal fiber cladding, such as
indiffusion [1.30], high-energy ion implantation [1.31] or outdiffusion of controlled
amounts of dopants [1.6,1.32], outside deposition of a cladding layer by electron
beam [1.33], ion-sputtering [1.34] or dip coated in a suspension [1.35-1.36], or
extrusion of a thin index-matched glass coating [1.34]. The cladding techniques for
crystal fibers are schematically illustrated in Fig. 1.2.

In-diffusion Out-diffusion Extrusion method

Nd3+ profile
Glass melt
MgO:LiNbO3

MgO layer Nd3+:YAG

Dip coating E-gun deposition

Glass particle
Nd3+:YAG Cr4+:YAG

SiO2

Fig. 1.2. Cladding techniques for crystal fibers.

The indiffusion and deposition techniques take a long process time due to slow
diffusion and deposition rates. The outdiffusion techniques appear to be rather limited
due to the concentration distributions caused by different ions will have different
refractive indices. The ion implantation could damage the single crystal structure. The
extrusion method needs special care to avoid air bubbles. We have developed a
co-drawing technique and demonstrated a super-wideband amplifier spontaneous
emission (ASE) with a 3-dB bandwidth of 240 nm generated by the single-clad
Cr4+:YAG crystal fiber. Up to 16-dB of gross gain at 1.47 m has also been achieved
by the double-clad Cr4+:YAG crystal fiber. In this co-drawing method, the core was
prepared by the LHPG technique, while the claddings were made from borosilicate or
fused silica capillaries.

4
 This dissertation contains five main chapters. Chapter 2 describes the methods of
growing single-crystal fiber from the melt. Chapter 3 discusses the characterization of
device fabrication, and laser characteristics of Nd:YAG crystal fiber. Chapter 4
describes the properties of Cr4+:YAG crystal and simulates the ASE and laser
performance of Cr4+:YAG crystal fibers. Chapter 5 is mainly on the characterization
of single crystal and glass-clad Cr4+:YAG crystal fibers. Chapter 6 discusses ASE and
optical gain performance of Cr4+:YAG crystal fibers.

5
 Chapter 2 Laser-heated pedestal growth system

It is important that fibers be produced in specific length, diameter and

orientations in order to be useful for optical applications. For this reason, vapor and
solution growth methods are generally not suitable. Several melt growth methods can
satisfy these requirements relatively easily. The most versatile of which is the
laser-heated pedestal growth method. This approach has the advantages of eliminating
any possibility of crucible contamination, and large temperature gradients are readily
achievable permitting rapid growth.

2.1 Single crystal fiber growth

( i ) Solidification in capillary tubes [2.1-2.3]
A glass capillary tube is filled with molten source material by feeding
downwards under gravity, or upwards by capillary attraction. Nucleation of the melt
followed by controlled cooling led to single-crystal growth inside the glass tube as
shown in Fig. 2.1. If the index of refraction of the glass is chosen appropriately, the
glass can serve as an effective optical cladding. This method is suitable for
low-melting point organic crystal. Voids lying between the crystal and the glass wall
were seen to be the major physical defect within the fibers. Besides, thermal
expansion matching and chemical compatibility are critical requirements in this
technique.

Single-crystal fiber

Glass capillary
Molten source

Fig. 2.1. Solidification in capillary tube

( ii ) Edge-defined film-fed growth (EFG) [2.4-2.5]

A capillary tube is dipped in a large crucible. Once dipped in the crucible, the
capillary is filled with molten source material because normal capillarity. The molten

6
source material quickly spread over the top face of the capillary tube, which becomes
the die. When seeded, this film on the die can be grown into a crystal with the same
diameter as the die. The technique is illustrated schematically in Fig. 2.2. The die
edge defines the diameter. The film is continually replenished by the melt, and the
melt can be restocked without affecting the growth zone. Particularly for high melting
point crystals the choice of appropriate die material is crucial to minimize
contamination of melt and provide proper wetting conditions for stable growth.

Single-crystal fiber

Die

Molten source

Fig. 2.2. Edge-defined film-fed growth

( iii ) -CZ [2.6-2.8]

A melt of crystal which wets the surface of a tiny heater in place of a melt in a
crucible as shown in Fig. 2.3. The melt covering the heated surface is small in volume
as well as in thickness, which makes it effective in suppressing the thermal convection
in the melt. A seed crystal contacting the melt is positioned at the top of a micro
protuberance made on the top surface of the heater, and growth of a single-crystal
fiber is carried out by moving the seed crystal upwards without a rotation.

Seed crystal

Single-crystal fiber
Microprotuberance

Platinum heater Source melt

Fig. 2.3. Schematic drawing of the -CZ technique

7
( iv ) -PD [2.9-2.10]
Figure 2.4 shows the growth apparatus of the -PD method. It consists of a
crucible directly heated resistively, a post-growth heater made from Pt wire, an
annealing furnace, and a crystal lowering mechanism. The crystal was melted within
the crucible and allowed to pass through the micro nozzle. The single-crystal fiber
was formed by attaching the seed crystal to the tip of the micro nozzle and slowly
pulling it downward with a constant velocity. The configuration of the micro nozzle
and post-growth heater makes it easy to control the liquid-solid interface temperature
and the crystal diameter.

Pt crucible
Main heater

Molten crystal Micro nozzle

Single-crystal fiber

Post-growth heater

Seed crystal

Fig. 2.4. Schematic diagram of the -PD growth apparatus

( v ) LHPG method [1.1-1.2,1.4]

The laser-heated pedestal growth (LHPG) or miniaturized float-zone (mZF)
method involves melting one end of a source material, and then dipping a seed crystal
into the free end of the melt as shown in Fig. 2.5. A single-crystal fiber is grown by
pulling it from the melt. Contamination problems arising from crucibles and furnace
components are virtually eliminated in this technique. In addition widerange
temperature control allowing to prepare crystal fibers of various materials. Therefore
the laser power serves as a clean and effective source of heat.

8
 Seed crystal Pull
Single-crystal fiber
CO2 laser

Molten zone

Source material
Feed

Fig. 2.5. Laser-heated pedestal growth method

Of all the methods mentioned above, the LHPG offers the greatest flexibility and
has the potential to produce the purest single-crystal fiber. Besides, very high
temperatures can be achieved rapidly, sample size is small and material costs are
therefore low. The shape of the molten zone, macroscopic crystal defects, and the
interface shape can be observed directly during growth. Therefore, we have
constructed such a fiber-pulling system for growing different single-crystal fibers.

2.2 LHPG apparatus

A schematic of our LHPG system is shown in Fig. 2.6. The heat source is a
100-W polarized CO2 laser at a wavelength of 10.6 m. The laser power can be
adjusted with a variable zinc selenide (ZnSe) Polarizer-Analyzer-Attenuators (-VI
Inc.). The CO2 laser system has a collinear He-Ne reference beam (visible) to indicate
where the CO2 beam (invisible) will travel. After passing through a ZnSe
beam-expansion telescope, the CO2 beam enters the growth chamber. The telescope
expands the CO2 beam size to three centimeter in diameter. The whole system is
controlled by a HP VEE program. Within the growth chamber an optical focusing
system is designed to bring the output of the CO2 laser to an axially, azimuthally
symmetric focus on the molten zone as shown in Fig. 2.7. An incident Gaussian beam
from the CO2 laser is converted to an annulus of half-Gaussian cross-section by the
two-cone reflaxicon element. The reflaxicon was fabricated by diamond-turning
technology. Figure 2.8 shows that the mated three-piece design for the
diamond-turned copper reflaxicon element. The inner cone was mounted on the center

9
of the ZnSe window with 4 diameter. This design can obtain a uniform and complete
donut-shape beam. After the 45 degree planar mirror, the parabolidal mirror focuses
the beam on the top end of the source rod. The oxygen-free copper paraboloidal
mirror with a 25 mm focus length was also fabricated by the diamond-turning
technology. The use of a parabolic rather than a spherical annulus eliminates spherical
aberration. The focal spot size is about 25 m. This tight focus is important for the
stable growth of small diameter fibers. All mirrors have gold coating on the copper
optical surfaces for reflectivity enhancement and copper substrate protection. The
pulling and feeding mechanisms are outside the chamber, and consist of
computer-controlled linear stage driven by stepping motor with gearbox to reduce
vibration. The maximum pulling length is 20 cm. The pulling speeds are in the range
of 0.375 to 37.5 mm/min.

Mirror 1
100-W CO2 laser

Power detector

Growth
chamber
Mirror 2 Power Beam splitter
attenuator ZnSe telescope
PC
Fig. 2.6. LHPG system

Paraboloidal mirror

CO2 laser beam

Planar mirror

inner cone
Reflaxicon
outer cone

Fig. 2.7. Growth chamber

10
 Side view End view
Piece 1

ZnSe window

Piece 3

Piece 2

Fig. 2.8. Mated three-piece design for the diamond-turned copper reflaxicon element.

2.3 Fabrication process of single-crystal fiber

Source material can be prepared in the forms of either round or square
cross-section rods from a single crystal, polycrystalline, and sintered or pressured
powder material. The crystal growth process is shown in Fig. 2.9. A seed rod is used
to determine the crystallographic orientation of the fiber to be grown. The growth
starts from using a tightly focused CO2 laser to heat and melt the top end of the source
rod, and then the seed rod is dipped into the molten zone. Finally, a single-crystal
fiber is grown by pulling the seed rod and feeding the source rod upward
simultaneously at a constant growth ratio.

Push
Oriented seed
Growing crystal
Pull
CO2 laser

Molten zone

Source rod

Feed

Fig. 2.9. Illustration of single-crystal growth via the LHPG method.

The fiber-to-source rod diameter ratio can be controlled by setting the pull/feed
speed ratio. At steady state, the volume of molten zone is constant due to conservation

11
of mass. The volume of crystal added to the fiber must equal the volume of the source
rod melted per unit time. Therefore, the ratio of fiber diameter to source rod diameter
is given by

Df vs
= (2.1)
Ds vf

where Df and Ds are diameters of the fiber and source rod, respectively. vf and vs are
speeds of pull and feed, respectively. Figure 2.10 shows the laser power necessary to
form a stable molten zone in YAG. The growth power is proportional to the source rod
diameter up to the power of 1.88. The inset shows the molten zone of YAG. The
solid-liquid growth interface is evident as the slightly darker bowl-shaped region at
the top of the molten zone. The curvature of this isothermal surface reflects the radial
temperature gradients. Typically, the axial temperature gradients are very steep at the
growth interface (~103 C/cm) and this permits faster growth rates (~ a few mm/min)
compared with bulk crystal growth process (~ 0.5 mm/hour). Since YAG is a
congruent material that maintains its composition right up to the melting point, YAG
single crystal fiber is easy to grow by the LHPG method without adding a solvent.
Figure 2.11 shows the phase diagram of the system Al2O3-Y2O3. According to the
phase diagram, YAG is formed by melting with Y2O3 and Al2O3 in the ratio 3:5 and
solidification under 1970 C.

20

16
CO2 laser power (W)

12

8
PDs1.88
4

0
0.2 0.4 0.6 0.8 1
Fiber diameter, Ds (mm)

Fig. 2.10. Laser power, P, as a function of source rod diameter. The inset shows a photograph
of YAG molten zone.

12
 2400

2200
Temperature ( ) Liquid

2000 YAG
YAM Liquid+Y2O3

YAP
Liquid Liquid
1800 +Al2O3 +YAG

Al2O3+YAG Y2O3+YAM
1600

Al2O3 20 40 60 80 Y2O3
Y2O3 ( mol% )

Fig. 2.11. Al2O3-Y2O3 phase diagram

We have grown YAG single-crystal fibers with diameters of 23 to 920 m up to a

length of 20 cm. Figure 2.12 shows a photograph of a 70-m-diameter fiber of
Cr4+:YAG grown at 10 mm/min, the diameter variation is about 1.1% over a 1 cm
length of the fiber.

70 m

100 X

Fig. 2.12. Photograph of a Cr4+:YAG single-crystal fiber with a 70-m diameter grown by the
LHPG method.

Figure 2.13 (a) is a photograph of the polished end of a YAG fiber grown along

13
<111> direction. It shows that the boundary of YAG cross-section is not quite a circle.
One side is almost round, and the other side is hexagonal shape. This shape can be
explained by the 6-fold symmetry of the fiber cross-section, as expected from a
<111>-cut cubic crystal. Figure 2.13 (b) is a drawing of the YAG atomic structure
where hexagonal structure can clearly be seen.

50 m

Y - purple, Al - blue, O - red

(a) (b)

Fig. 2.13. (a) Photograph of a polished end of a YAG crystal fiber. (b) Drawing of the YAG
atomic structure viewed from <111> direction.

14
 Chapter 3 Nd3+:YAG crystal fibers

Crystal fibers have been shown to be compact and cost-effective as solid-state

laser hosts and nonlinear frequencies conversion media. However, interface loss is
one of the dominant factors that reduce the efficiency of crystal fiber lasers. In this
chapter, we use a controlled profile of the active ion distribution to confine the laser
beam in the center region of the core, and thus reduce the interface loss to obtain
highly efficient Nd:YAG crystal fiber laser.

3.1 Properties of Nd3+:YAG crystal

YAG (Y3Al5O12) is a very hard, isotropic crystal and has a good thermal
conductivity, which permits laser operation at high average power levels. It is the
commercially available crystalline laser host for Nd3+, offering low threshold and high
gain. In Nd:YAG, trivalent neodymium substitutes for trivalent yttrium, so charge
compensation is not required. Commercially available Nd:YAG laser crystals are
grown by the Czochralski method. YAG belongs to the garnet family and crystallizes
10
in the cubic space group Ia-3d ( Oh ). The lattice constant is 12.01 , eight formula
units build the unit cell. The 24 Y atoms of the unit cell are surrounded by a
dodecahedron of O atoms, while 16 ( 40% ) of the Al atoms are surrounded by oxygen
octahedrons and 24 ( 60% ) of the Al atoms are surrounded by oxygen tetrahedrons as
show in Fig. 3.1.

Al

O Y

Al

Fig. 3.1. Crystal structure of YAG. Aluminum atoms occupy tetrahedral and octahedral
polyhedral in YAG. Yttrium atoms are surrounded by eight oxygen atoms.

15
 Table 3.1 lists YAG structural information and atomic location parameters. In
Nd:YAG about 1% of Y3+ is substituted by Nd3+. The radii of the two rare earth ions
differ by about 7.8% [3.2]. Therefore, high doping levels tend to shorten the
fluorescent lifetime, broaden the linewidth, and cause strain in the crystal, resulting in
poor optical quality. Some of the important physical properties are listed in Table 3.2.

Table 3.1. Structural information and atomic position data of YAG [3.1]
Atom Valence Cation Atomic position
coordination x y z
Al +3 6 0.0 0.0 0.0
Al +3 4 0.375 0.0 0.25
Y +3 8 0.125 0.0 0.25
O -2 - -0.02985 0.05056 0.14878
Lattice a=b=c=12.008
parameters ===90
Cation-O Al-O 1.937
bond length Al-O 1.761
Y-O 2.303
Y-O 2.432
Space group Ia-3d (garnet)

Table 3.2. Physical and optical properties of Nd:YAG

Chemical formula Nd3+:Y3Al5O12
Nd atomic% 1.0
3
Nd atoms/cm 1.38 1020
Melting point 1970
Hardness (Mohr) 8.5
Density 4.56 g/cm3
Index of refraction 1.82 (at 1 m)
Width of pump bands 1 nm (at 807.5 nm)
Absorption coefficient 10 cm-1 (at 807.5 nm)
Emission linewidth 4.5 (at 1064 nm)
Stimulated emission cross section 2.8 10-19 cm2 (4F3/2 4I11/2)
Fluorescence lifetime 230 s
Thermal conductivity 0.14 W cm-1 K-1 (at 300 K)
Thermal diffusivity 0.046 cm2 s-1 (at 300 K)
Thermal expansion coefficient 7.5 10-6 K-1 (at 300 K)

16
 The absorption spectrum of Nd:YAG in the range of 0.3 to 0.9 m is given in Fig.
3.2. It shows that Nd:YAG has four main absorption bands which are 0.59 m, 0.75
m, 0.81 m and 0.89 m. Of the main pump band shown, the 0.81 m and 0.89 m
bands can obtain higher quantum efficiency.
Optical density

(m)
Fig. 3.2. Absorption spectrum of Nd:YAG at 300K [3.3].

4
F5/2
4
F3/2

1319 nm

4
I15/2
808 nm pump
1064 nm
4
I13/2
946 nm
4
I11/2
4
-1 I9/2
~ 900 cm ground state manifold

Fig. 3.3. Energy level diagram of Nd:YAG.

Figure 3.3 shows a simplified energy level diagram of Nd:YAG. The main lasing
wavelengths are 1064 nm, 946 nm and 1319 nm. The branching ratio of emission
from 4F3/2 is listed in Table 3.3. It shows that almost all the ions transferred from the
ground level to the upper laser level, 4F3/2, and 60% of the ions at the upper laser level
cause fluorescence output at the 4I11/2 manifold.

17
Table 3.3. YAG branching ratio of emission from 4F3/2 [3.4]
Branching ratio of Frequency-double
Emission line Electron transition emission wavelength

1.064 m 4
F3/2 4I11/2 60% 532 nm

0.946 m 4
F3/2 4I9/2 25% 473 nm

1.319 m 4
F3/2 4I13/2 14% 659.5 nm

1.84 m 4
F3/2 4I15/2 < 1% 920 nm

3.2 Characterization of Nd:YAG crystal fiber

3.2.1 X-ray diffraction analysis

Figure 3.4 shows the calculated diffraction pattern of powdered YAG using the
software, Crystallographica. The Cu K1 radiation with a wavelength of 1.54 was
selected as the X-ray source light. The calculated result shows that YAG powder has a
strongest line at (420) plane with a distance of planes spacing of 2.68 .

250
420
200
X-ray intensity (a.u.)

150

100

400 640
50 321 422 521 532 642
444

0
20 30 40 50 60 70 80
2 theta (deg.)
Fig. 3.4. Calculated diffraction pattern of YAG pattern.

The single-crystal quality of <111>-oriented Nd:YAG crystal fiber grown by the

LHPG method was measured by Siemens D5000 diffractometer with a copper target.

18
 Figure 3.5 (a) and (b) are the X-ray diffraction patterns of a raw material rod cut in
<111> crystal orientation grown by the Czochralski (CZ) method and a 250-m
diameter crystal fiber. The full width half maximum (FWHM) values of the main peak
are 0.080 and 0.050 for the raw material and 250-m diameter crystal fiber,
respectively. This result shows that the grown crystal fiber has better crystal quality
than the original bulk crystal rod.

10 10

X-ray intensity ( cps x 10000 )

X-ray intensity ( cps x 1000 )

8 8 422
321
6 6
enlargement, see below enlargement, see below
4 4

2 2

0 0
20 30 40 50 60 70 80 20 30 40 50 60 70 80
2 theta (deg.) 2 theta (deg.)

10 10
X-ray intensity ( cps x 10000 )
X-ray intensity ( cps x 1000 )

8 8
K1
K1
6 6

4 K2 4
K2
2 2

0 0
27.5 27.6 27.7 27.8 27.9 28.0 36.3 36.4 36.5 36.6 36.7 36.8
2 theta (deg.) 2 theta (deg.)

(a) (b)

Fig. 3.5. X-ray diffraction patterns of (a) the raw material, (b) the 250-m diameter crystal
fiber. The lower parts are the enlargement of main peaks of upper parts.

3.2.2 Composition analysis

In order to know the Nd3+ doping distribution in source rod and crystal fiber as
shown in Fig. 3.6 (a), electron probe microanalysis (EPMA) was used to measure the

19
doping profile across the fiber cross section using JEOL JXA-8900R. Samples grown
under different conditions were measured. Figure 3.6 (b) shows the typical line
scanning marks on the cross section of fiber by electron beam.

Nd3+ profile Crystal fiber

Molten zone

YAG

Nd3+ Source rod

100 50 0
Percent diameter (%)

(a) (b)

Fig. 3.6. (a) Schematic diagram of the Nd3+ doping distribution in source rod and crystal fiber,
(b) photograph of line scanning marks on the cross section of crystal fiber.

With a 6:1 pull/push speed ratio for the first growth, 220-m-diameter crystal
fibers were obtained for different growth speed as shown in Fig. 3.7. After growth, the
average Nd3+ doping was reduced because of evaporation at the circumference and
low segregation coefficient from the melt to the growing crystal [3.5,3.6]. The
average doping concentration is about 0.7 atm.% at the growth speed of 0.25 mm/min.
When increasing the growth speed, the average doping concentration and
concentration gradient are raised. This trend stops when the speed reaches 1.25
mm/min. Therefore higher growth rate has higher average doping concentration
compared to lower growth rate. To obtain the maximum concentration gradient, the
growth rate should be properly selected. As shown in Fig. 3.8, after successive
re-growth to reduce the fiber diameter, the doping distribution became quite uniform
again with a lower average doping concentration. The initial source rod is uniformly
doped with an average doping concentration of 1.14 atm.%.

20
 2.6
2.4 0.25 mm/min
2.2 0.5 mm/min
0.75 mm/min
Nd concentration (at.%)
2.0 1.25 mm/min
1.8 1.5 mm/min

1.6
1.4
1.2
1.0
0.8
0.6
0 20 40 60 80 100
Percent diameter (%)
Fig. 3.7. Doping profiles of Nd:YAG crystal fibers for different growth rates. The fibers
diameters are all 220 m.

1.8
500 m
1.6 250 m
Nd concentration (at.%)

85 m
1.4 36 m

1.2

1.0

0.8

0.6
0 20 40 60 80 100
Percent diameter (%)
Fig. 3.8. Doping profiles of Nd:YAG crystal fibers with multiple regrowth.

3.2.3 Refraction index measurement

To estimate the difference in the refraction index between the center and
circumference of the crystal fiber, we assume that the index gradient is proportional to

21
the doping gradient [3.7]. In other words, the crystal fiber is assumed to serve as a
gradient-index lens for the probe light. Consider the transverse doping profile, C(r),
and index profile, n(r), in the following forms,

A 2
C (r ) = C o (1 r ), (3.1)
2
A
n(r ) = no (1 a r 2 ) , (3.2)
2

where Co and no are the doping concentration and refraction index at the fiber center,
respectively. The constant A was determined by the EPMA measurement to be 37.74
mm-2. The constant a is the quantity to be determined. An optical low-coherence
reflectometer (OLCR) was employed to estimate the index gradient [3.8]. A simple
description of OLCR can be given by referring to Fig. 3.9. A cw low-coherence
source with a coherence length on the order of 10 m is divided into the test and
reference arms. When the optical delay for light reflected from the reference arm
matches the delay for light reflected from the device under test (DUT), optical
interference takes place at the photodiode. This interference signal only occurs if the
optical distance to the reference mirror is within a coherence length compare to the
optical distance to the DUT. By scanning the position of the reference mirror and
recording the magnitude of interference signals, a plot of reflectance versus distance
can be obtained for the DUT.

CW
low-coherence
light source Test arm
3dB Rdut
PDUT
X
Photodiode
Reference
PRef arm Movable
Id
mirror

Fig. 3.9. Configuration of an optical low-coherence reflectometer.

Figure 3.10 shows the experimental setup of refraction index measurement of

gradient-index crystal fiber. Due to the gradient index, the probe beam divergent angle

22
varies while propagating inside the crystal fiber. The probe beam bounces back and
forth inside the fiber, and only the reflection with small divergent angle can be
collected by the OLCR. A lens with a small numerical aperture (NA=0.11) was used
to collect the reflections from the crystal fiber, followed by another lens to focus the
light back into the reflectometer.

OLCR Testing light source

Intensity
70 nm Crystal fiber

1330 nm
Glass

Lens Front face End face

Fig. 3.10. Experimental setup of refraction index measurement of gradient-index crystal fiber.

As shown in Fig. 3.11 (a), reflections of the 1st, 2nd, 9th, 10th, and 11th passes from
the end face were collected. The 10th reflection had a local maximum reflection,
indicating that the multipass reflected light is effectively collected by the
reflectometer. Note that the relative intensity of the reflected light, IR, can be
estimated as
4N 2
n 1 NA
I R o lens , (3.3)
n + 1 NA
o light

n
NAlight sin ( out ) sin cos ( 2 NL a A ) sin 1 ( o a A ) , (3.4)
2

where N is the number of round trips of light before it leaves the crystal fiber; NAlens
and NAlight are the numerical apertures of the collecting lens and the reflected light,
respectively and out is the divergence angle of the outgoing beam from the fiber after
N round trips of propagation. L and are the length and diameter of the crystal fiber.
Figure 3.11 (b) shows the simulation results. It can be seen that the numerical aperture
of the probe light has a minimum value after 10 round trips of propagation. The

23
constant a=0.053 was used in the simulation. The gradient-index crystal fiber can
therefore be obtained to have 1.738 pitch, which is equivalent to a 0.0284 index
difference between the center and edge of the crystal fiber.

0
Front face

1
Interference amp. (dB)

-20

-40
10
2
-60 9 11

-80
150 200 250 300 350
Position (mm)
(a)
Numerical aperature of the probe light

0.4
0.3
0.2
0.1
0.0
0 1 2 3 4 5 6 7 8 9 10 11 12 13
-0.1
-0.2
-0.3
-0.4
Numner of round trips
(b)

Fig. 3.11. (a) Collection of reflections by a lens with a numerical aperture of 0.11. The
peaks marked with numbers represent the multiple round-trip reflections from the end face of
a 250-m crystal fiber. (b) Simulated numerical aperture of light of the reflected beam after
multiple round-trips. The length of the crystal fiber is 7.72 mm.

24
3.3 Nd:YAG crystal fiber laser

3.3.1 Fabrication of Nd:YAG fiber laser

After growth, the fibers were mounted in a low-melting-point glass capillary for
further grinding and polishing. Then, the fibers were ground with silicon carbide (SiC)
paper from #600 (grit size 27 m) to #2000 (grit size 11 m) under rotation speed of
300 rpm. Table 3.4 lists the number of SiC papers and its corresponding grit sizes.
Each grinding step usually takes 1-3 minutes or longer until the scratches on the end
face are in the same direction. Then the fibers continued to be polished with diamond
polishing cloths, 6 m, 3 m, 1 m, and 1/4 m in turn for about 6-10 minutes to get
good flatness. In order to obtain the optimal optical quality, alumina polishing is
employed in the final preparation steps and it takes about 20 minutes. Table 3.5
summarizes the mechanical preparation and its corresponding preparation time for
fiber laser samples.

Table 3.4 SiC grit size (Europe)

Number 120 600 800 1200 2000
Grit size (m) 106 27 21.8 15.2 11

Table 3.5 The mechanical preparation of Nd:YAG crystal fiber laser samples
Grinding processes
# of SiC paper Preparation time (min)
# 600 1
# 800 1
# 1200 1
# 2000 3
Polishing processes
Types of Grit size of diamond The amount of lubricant Preparation time
polishing cloths abrasives (drop/min) (min)
MD-Pan 6 m 6 6
MD-Pan 3 m 6 6
MD-Dur 1 m 6 8
MD-Nap 1/4 m 6 10
SP-Policel 2 1/4 m, alumina paste 6 20

25
 Figure 3.12 shows the cross sectional images of fiber after 1/4 m diamond and
alumina polishing. It can be seen that the YAG boundary is a hexagon due to the fiber
was grown from the <111>-oriented seed YAG.

(a) (b)

Fig. 3.12. The cross sectional images of a crystal fiber after (a) 1/4 m diamond polishing,
and (b) 1/4 m alumina polishing.

An step profiler was used to measure the surface profiles of fiber cross section
as shown in Fig. 3.13. It can be seen that the relief and edge rounding taken place on
the surface of the fiber. This is because material from different phases is removed at
different rates, due to varying hardness of the individual phases. Since the hardness of
YAG is much higher than that of Pyrex glass, it is not easy to have a flat polished
surface. As shown in Fig. 3.13 (a), the YAG has a lower surface than the Pyrix glass
after 1/4 m diamond polishing. However, when the fiber was polished by 1/4 m
alumina paste, we can obtain a flat surface as shown in Fig. 3.13 (b). It shows the
flatness across the 200-m YAG fiber is within 0.06 m, which is equivalent to a
radius of curvature of 83 mm. In addition, the surface roughness of fiber measured by
atomic force microscope (AFM) is about 14 nm within a length of 75 m.

26
 Nd:YAG

Pyrex glass
1.8 m

(a)

Pyrex glass

0.06 m
Nd:YAG

(b)

Fig. 3.13. Surface profiles of the crystal fiber after (a) 1/4 m diamond polishing, and (b) 1/4
m alumina polishing. The outer diameter of the Pyrex glass capillary is 7 mm.

Finally, high-reflection coatings were deposited directly onto the two faces of the
crystal fiber as the laser mirror using an electron-beam evaporator. To avoid coating
damage, the high electric field inside the coating layers was designed to be away from
the SiO2/TiO2 layer interface and high-dielectric-constant material (i.e., TiO2). Film
thickness of approximately 3998 nm for input face and 2690 nm for output face
o
were deposited by electron-beam evaporation at a substrate temperature of 300 C in a
Leybold APS1104 plant. The TiO2 and SiO2 films were deposited in an oxygen

27
atmosphere with gas flows of 30 and 10 standard c.c. per minute (sccm) and pressures
of 2.510-4 and 210-4 mbar. The evaporation rates of TiO2 and SiO2 were 0.17 nm/s
and 0.4 nm/s, respectively. In the first trial, a reflectance of 97.6% at the output face
of the gain medium was used for the lasing wavelength of 1064 nm. The reflectance
of the input surface was greater than 99% at 1064 nm and less than 0.1% at the pump
wavelength of 808 nm. The measured reflectance of the coatings on test glass plates is
shown in Fig. 3.14.

100

80
Reflectance (%)

60 Output face Input face

40

20

0
700 800 900 1000 1100 1200
Wavelength (nm)
Fig. 3.14. The reflectance of the coatings on the front and end facets of the crystal fiber laser.

3.3.2 Characterization of Nd:YAG fiber laser

Both fiber-pigtailed and bare LDs were used to pump the Nd:YAG crystal fiber.
A TE-cooled 1.2 W laser diode at 808 nm was focused with 0.23-pitch GRIN lenses
to control the pump beam size to enable mode matching. Using the cut-back method,
the absorption and transmission loss of the pump beam in the crystal fiber was
determined to be about 40 to 50%, depending on the pump power and pump laser
wavelength. The measured absorption coefficient was larger than in a typical 1.1 at.%
Nd:YAG crystal. As mentioned above, the Nd:YAG crystal fibers used in this work
had a high Nd3+ doping concentration in the central region of the core, which resulted
in enhanced pump absorption. A thinned silicon wafer was placed at the output of the
crystal fiber to block out the pump beam. A lens with a focal length of 2.54 cm was

28
used to collimate the 1064 nm laser output. Figure 3.15 shows the configuration of the
Nd:YAG fiber laser. To optimize the laser output and to estimate the intracavity loss,
coatings with transmittances of 4 and 16% were also applied to the output facets.
Figure 3.16 shows the measured slope efficiency and computer fitted curves for both
bare LD and fiber-pigtailed LD as the pump sources. The following simple slope
efficiency equation was used to fit the data:

T
= coup , (3.5)
L ln (1 T )

where is the slope efficiency, coup is a coupling constant, L is the round-trip

distributed loss, and T is the transmittance of the output coupler.

Nd:YAG crystal fiber

Pyrex f=2.54 cm

0.23-pitch
808-nm LD Grin lens
Silicon Power meter
Input Output filter
face face

Fig. 3.15. Configuration of the Nd:YAG fiber laser.

35

30 Pig-tailed LD
Slope efficiency (%)

25

20

15

10
Bare LD
5

0
0 5 10 15 20
Output transmittance (%)
Fig. 3.16. Slope efficiency vs the output transmittance for pumping sources of fiber-pigtailed
and bare LDs. The symbols are experimental data and the lines are fitted.

29
 Using Eq. (3.5), it can be estimated that mode matching for the fiber-pigtailed
LD is 37.5% better than that for the bare LD as the pump source. The intracavity
round-trip distributed loss was also inferred to be 15% (0.7 dB/cm). Figure 3.17
shows the fiber laser output power for different output couplers pumped by the
fiber-pigtailed LD. As much as 80 mW of output power was achieved with a slope
efficiency of 28.9% when using the 16% output transmittance. This slope efficiency,
to our knowledge, is the highest ever achieved for diode-laser pumped Nd:YAG
crystal fiber lasers. It was obtained with a 200-m-diameter 5-mm-long crystal fiber.
It should be noted that the absorbed pump power in Fig. 3.17 included the distributed
loss in the crystal fiber. If we remove the distributed loss, the slope efficiency could
be nearly doubled for the laser with 16% output transmittance.

90
80
T = 16%
70
Output power (mW)

60
50
40
30 T = 4%

20
T = 2.4%
10
0
0 100 200 300 400 500
Absorbed pump power (mW)

Fig. 3.17. CW output power of the gradient-index Nd:YAG crystal fiber laser as a function of
the absorbed pump power for different output couplers.

To measure the near-field pattern of the crystal fiber laser, an image relay was
employed as shown in Fig. 3.18. The laser output transverse mode was focused with a
lens of focal length 2.54 cm and then the image was recorded with a 1-D CCD array.
Figure 3.19 shows the near-field patterns in the transverse directions. It shows the

30
FWHM transverse mode in horizontal and vertical directions are 270 and 274 m,
respectively. The estimated M2 was 1.19.

f=2.54 cm Attenuator
Crystal fiber

1-D CCD
808-nm LD Grin lens
Filter

31 mm 106 mm

Fig. 3.18. Experimental setup of near-field beam patterns of the fiber laser measurement.

Horizontal direction Vertical direction

10 10
FWHM=270 m FWHM=274 m
8 8
Intensity (a.u.)

Intensity (a.u.)

6 6

4 4

2 2

0 0
0 300 600 900 1200 1500 0 300 600 900 1200 1500
Position (m) Position (m)

Fig. 3.19. Near-field beam patterns of the fiber laser in vertical and horizontal directions. Note:
the pulsed behaviors are artifacts of the CCD array used. Only the envelopes represent the
near-field beam patterns.

In conclusion, high-quality gradient index crystal fibers were successfully grown

by the LHPG technique. Doping profiles were measured for various growth
conditions by using EPMA. With proper control of the growth condition, the doping
concentration can be enhanced at the center of the 250-m-diameter fiber by 40%
above that in the raw material. This resulted in an index difference of 0.0284 between
the center and the edge of the crystal fiber. A laser output power of 80 mW was
achieved with a slope efficiency of 28.9%.

31
 Chapter 4 Simulation of Cr4+:YAG crystal fiber devices

The near-infrared fluorescence spectra of Cr+4 doped YAG covers a wide range
from 1200 to 1600 nm. Such wide-band characteristics offer unprecedented
one-for-all convenience, flexibility, and simplicity to multi-band component
manufactures in the telecommunications. Using a fiber configuration was suitable for
this broadband light source because of its structural similarity to silica fiber. Moreover,
the fiber configuration can confine pump light in a small cross-sectional area with a
high energy density for a long distance. To investigate the performance of crystal fiber
devices, the numerical simulation was applied to study the power performance of
amplified spontaneous emission (ASE) and crystal fiber laser. The simulation result
indicates that small core diameter and lower propagation loss are important for higher
ASE and laser efficiency.

4.1 Properties of Cr4+:YAG crystal

Cr4+ doped YAG has a strong coupling between the vibrational energy states of
the host crystal and the electronic energy states of the active ion, resulting in broad
absorption and emission linewidths. The energy level diagram of the Cr4+:YAG
crystal is schematically shown in Fig. 4.1.

Td D2d
3
3 E
T1
ESA
~1m 3
A2
3
3 E
T2 ESA
~1.4 m
3
B2
Pump ~1.4 m
~1m
3
A2 3
B1

Fig. 4.1. Energy level diagram of the Cr4+:YAG crystal [4.1].

The absorption band from 0.9 to 1.1 m corresponds to the 3A2 3T2 transition.
There exist excited-state absorptions (ESA) at the pump and the fluorescence

32
emission wavelengths arising from the transitions between the lower 3T2 state and the
higher 3T1 state. The fluorescence emission in the 1.4-m region occurs as the result
of the transition from the 3T2 state back to the 3A2 state. The room temperature
absorption spectrum in Fig. 4.2 shows three broad bands at 1 m, 0.64 m and 0.48
m. The 0.48-m absorption band may be due to Cr4+ in octahedral sites, a
charge-transfer or a color center. The 0.64 m and 1 m bands are primarily ascribes
to 3A2 3
T1 and 3A2 3
T2 transitions, respectively. Figure 4.3 shows the
near-infrared (NIR) fluorescence spectrum of Cr4+:YAG. The fluorescence band peaks
at 1.37 m and covers a wide range from1.1 to 1.7 m. Some of the important optical
properties are listed in Table 4.1.

10
Absorption coefficient (cm-1)

0
300 600 900 1200
Wavelength (nm)

Fig. 4.2. Room temperature absorption spectrum of Cr4+:YAG [4.2].

Intensity (a.u.)

1000 1200 1400 1600 1800

Wavelength (nm)

Fig. 4.3. Room temperature emission spectrum of Cr4+:YAG [4.2].

33
 Table 4.1. Optical properties of Cr4+:YAG
Tunable rage 1.34~1.58 m
Absorption cross section 1.1210-18 cm2
Emission cross section 4.6 10-20 cm2
ESA cross section 0.96 10-20 cm2
Absorption coefficient 0.5~4.5 cm-1 (at 1064 nm)
Absorption bandwidth 0.9~1.1 m
Spontaneous fluorescence lifetime 4.5 s (at 300K)

The NIR spectrum is attributed to transitions between the 3A2 and 3T2 states of
Cr4+ ions in the tetrahedral site of YAG as shown in Fig. 4.4 [4.3]. Since most Cr ions
enter in YAG tend to become octahedrally coordinated Cr3+, in order to incorporate
the Cr in the quadrivalent state, divalent ions are codoped as the charge compensator
to change Cr3+ ions to Cr4+. In 1997, Markgraf, et al. examined several divalent ions
includes Ca2+, Mg2+, Co2+, Cu2+, Fe2+, Mn2+, Zn2+ and Sr2+. But Be2+ and Pb2+ were
rejected as potential co-dopants for safety concerns [4.4]. They found the only
successful co-dopants were Ca2+ and Mg2+ that produce a large amount of Cr4+ for
NIR emission. In general, Ca2+ ions were used to be dopants in YAG based on size
consideration. Table 4.2 summaries the lattice mismatch between dopant ions and host
ions. For Ca2+ replacing Y3+, the lattice mismatch is +8.7% while Mg2+ replacing Y3+
is -11.1%.

Cr4+

O Y

Cr3+

Fig. 4.4. Configuration of the Cr4+ ion in Cr4+:YAG lattice. It is surrounded by four oxygen
ions in tetrahedral arrangement.

34
Table 4.2 Comparison of lattice mismatch between dopant ions and host ions
Host ion Y3+ (D) Al3+ (T) Al3+ (O)
dopant 1.159 0.53 0.675
Nd3+(O) 1.249 +7.8%
Cr3+(O) 0.755 +11.9%
Cr4+(T) 0.55 +3.8%
Cr4+(O) 0.69 +2.2%
Ca2+(O) 1.14 +68.9%
Ca2+(D) 1.26 +8.7%
Mg2+(T) 0.71 +34.0%
Mg2+(O) 0.86 +27.4%
Mg2+(D) 1.03 -11.1%
Yb3+(D) 1.125 -2.9%
Where O, T, and D denote ions in octahedral sites, tetrahedral sites, and dodecahedral
sites, respectively.

Table 4.3 Characteristics of Cr:YAG and Cr,Ca:YAG crystal fibers [4.5]

Cr conc. Ca2+ conc. Growth Color NIR emission
(mol %) (mol %) atmosphere
0.05 N2 colorless not detected
0.05 Air
0.05 O2
0.2 N2 light green
0.2 Air
0.2 O2
0.05 0.05 N2 light brown strong
0.05 0.05 Air
0.05 0.05 O2
0.2 0.2 N2 brown
0.2 0.2 Air
0.2 0.2 O2
1.0 1.0 N2 almost black

35
 Table 4.3 presents the growth conditions and colors of Cr:YAG and Cr,Ca:YAG
single crystal fibers grown by LHPG method. It can be seen that the Cr:YAG crystals
are colorless without Ca2+ doping. When increasing the concentrations of Cr, the
Cr:YAG crystals become light green because of the Cr3+ in octahedral sites. In both
cases, NIR emission was not detected. The Cr,Ca:YAG crystal becomes brown, even
black with strong NIR detection as Cr and Ca2+ are co-doped in YAG. So we can
conclude that doping with Ca2+ ions into Cr:YAG for charge compensation is
necessary to get tetravalent Cr.

Figure 4.5 (a) shows the effect of Ca2+ on the concentration of Cr4+. The
percentage of Cr4+ increases when increasing the Ca/Cr. It saturates when the ration of
Ca/Cr goes up to about 6. This result could be explained that the lattice of YAG is
seriously distorted by higher calcium and reducing the effect of charge compensation.
After annealing in oxygen to improve optical quality of crystal, Cr4+ percentage can
increase about 30% - 50%, and the maximum ratio of Cr4+ to total Cr is about 6.5%.
The room temperature lifetime at 1400 nm as a function of Cr4+ concentration is
shown in Fig. 4.5 (b). The lifetime is about 3.6 s and almost keeps constant up to a
concentration of about 21017 cm-3.

7 7 3.8
Lifetime at 1400 nm (s)

6 6
3.6
after annealing (%)
Cr4+ / total Cr (%)

5 5
Cr4+ / total Cr

4 4 3.4
3 3 3.2
2 2
3.0
1 1
0 0 2.8
0 10 20 30 40 0.1 1 10 10
4+ 17 -3
Ca / Cr Cr concentration (10 cm )

(a) (b)

Fig. 4.5. (a) Percentage of Cr4+ to total Cr as a function of Ca/Cr, (b) Cr4+ lifetime as a
function of Cr4+ concentration [4.6].

36
4.2 Rate equation analysis
In order to investigate the ASE power and laser performance of Cr4+:YAG crystal
fiber, the rate equation analysis was used. We consider the energy levels of the
Cr4+:YAG as shown in Fig. 4.6 [4.7-4.8].

N3 3
A2(3T1)

esa
3
T2 N2 3
B2(3T2)

e , f
a
N1 3
B1(3A2)
3
A2 Ng

Fig. 4.6. Simplified energy level diagram of Cr4+:YAG.

In this model, the ground state (3A2) Cr4+ ions were excited by a pump light to
the 3T2 state. Immediately the electrons nonradiatively decay to the meta-stable state
(3B2(3T2)). Besides the stimulated and spontaneous emission from (3B2(3T2)) to the
lower energy level (3B1(3A2)), the population density N2 may also reduces due to the
excited-state absorption to a higher energy level (3A2(3T1)). The non-radiative decay
rate for population densities in the energy levels 3T2, 3B1(3A2) and 3A2(3T1) are very
fast, so they are ignored in the rate equations. The excited-state absorption at pump
wavelength was also neglected in this model. Therefore, the rate equation for the N2(z)
population density at position z can be described as follows,

dN 2 (z ) a p I p (z )
= N g (z )
dt hc (4.1)
I (z ) esa s I s (z ) 1
N 2 (z ) e s s + + ,
hc hc f

N T = N g (z ) + N 2 ( z ) , (4.2)
where Ng(z) is the population density of the ground state (3A2), a is the absorption
cross section at pumping wavelength p, e is the stimulated emission cross section at

37
spontaneous emission center wavelength s, esa is the excited-state absorption cross
section at s, Ip(z) is the pump intensity, Is(z) is the spontaneous emission intensity, f
is the fluorescence lifetime, h is the Plancks constant, and c is the velocity of light.
And the total ion density NT is the summation of the Ng(z) and N2(z). The fluorescence
lifetime, f, is assumed to be linearly proportional to crystal temperature as shown
below,

f (T ) = f 0 aT (4.3)

where fo is the lifetime measured at 0 C and the thermal lifetime coefficient, a,

shows the sensitivity of f to change in the YAG temperature. The linear
approximation to the temperature dependence of the fluorescence lifetime will also be
used later to access the role of lifetime thermal loading in Cr4+:YAG fiber laser. To
simplify Eq. (4.1), the following parameters are defined,
hc
I sa = (4.4)
a p f ,

hc
I se = (4.5)
e s f ,

esa
fL = (4.6)
e ,
where Isa and Ise are the absorption and emission saturation intensities, respectively. fL
is the normalized excited-state absorption strength. Then Eq. (4.1) can be rewritten as
follows,

dN 2 (z ) I p (z ) I p (z ) I (z ) 1
= N T N 2 (z ) + (1 + f L ) s + (4.7)
dt I sa f I sa f I se f f

Therefore, the steady-state of population density N2(z) as a function of position z

along the fiber, is given by

I p (z )
I sa
N 2 (z ) = N T (4.8)
I (z ) I p (z )
1 + (1 + f L ) s +
I se I sa

38
4.3 Simulation of ASE light source
Assuming that the light intensities are uniformly distributed in the fiber cross
section, the propagation equations of the pump and spontaneous emission intensities
can be expressed as follows:

( )
I p (z ) = I p 0 e
a + pl z
(4.9)

I s (z ) = I s0 e
g z
(4.10)

where Ip0 and Is0 are the initial pump and spontaneous emission intensities, respectively.
a ( aNg) and pl are the absorption coefficient and propagation loss coefficient of
the crystal fiber, respectively. g [ (e-esa)N2-pl ] is the gain coefficient of the
crystal fiber. Therefore, the differential equations of the pump and spontaneous
emission intensities can be expressed as follows,

dI p (z )
= [ a N g ( z ) + pl ] I p ( z ) , (4.11)
dz

dI s (z )
= [(1 f L ) e N 2 ( z ) pl ] I s ( z ) . (4.12)
dz

Since the local spontaneous emission also stimulates the emission of the
meta-stable state Cr4+ ions, the total ASE power at position z was the summation of
the ASE power and the local spontaneous emission power [4.9]. The propagation
equations for the forward and backward ASE power can be obtained as follows,
+
dPASE (z ) = N ( z ) [(1 f )] P + ( z ) + P 0 N ( z ) P + ( z ) , (4.13)
e 2 L ASE ASE 2 e ASE pl
dz

dPASE (z ) = N ( z ) [(1 f )] P ( z ) P 0 N ( z ) + P ( z )
e 2 L ASE ASE 2 e ASE pl , (4.14)
dz

where PASE(z) is the ASE power at position z, the positive and negative signs represent
0
forward and backward directions respectively, PASE (=Mh ) is the local spontaneous
emission power. is the spontaneous emission center frequency, M is the mode
number of the propagating ASE, and is the 3 dB bandwidth of the Cr4+:YAG
spectrum. Based on the theoretical model described above, we can use Eqs. (4.8),

39
 (4.11), (4.13), and (4.14) to simulate the distributions of the population density N2(z),
the absorbed pump power, and the generated ASE power along the crystal fiber.
Figure 4.7 shows the simulated ASE power with different core diameters. The
simulation result indicates that it is crucial to have a small core for higher ASE
efficiency and power. The ASE power could be in excess of 20 dBm for a
10-m-diameter core at a pump power of 1.25 W. The corresponding optical gains
and needed fiber lengths are shown in Fig. 4.8. It can be clearly seen that small core
has higher optical gain as shown in Fig. 4.8 (a) due to higher pump intensity but the
needed fiber length would be longer. The simulation parameters are listed in Table.
4.4.
30

25
Core = 10 m
ASE power (dBm)

20
Core = 20 m
15

10
Core = 30 m
5

0
0.5 1.0 1.5 2.0 2.5 3.0 3.5
Absorbed pump power (W)
Fig. 4.7. The simulated ASE power as a function of pump power for different core diameters
of the Cr:YAG crystal fiber.

55 0.5
50 Core = 10 m
0.4 Core = 10 m
Fiber length (m)

45
Gain (dB)

Core = 20 m
0.3 Core = 20 m
40
0.2
35 Core = 30 m
Core = 30 m
30 0.1

25 0.0
0.5 1.0 1.5 2.0 2.5 3.0 3.5 0.5 1.0 1.5 2.0 2.5 3.0 3.5
Absorbed pump power (W) Absorbed pump power (W)

(a) (b)
Fig. 4.8. The corresponding (a) gains and (b) needed fiber lengths in Fig 4.7.

40
Table 4.4 Parameters used for ASE power simulation.
Parameters Cr4+:YAG crystal fiber Unit
Fiber core diameter 10 20 30 m
Pump wavelength, p 1064 nm
-1
Small signal absorption coefficient, 70 m
-1
Propagation loss coefficient, pl 2.3 m
2
Absorption cross section, a 2.210-22 m
Total ion density (NT= / a)
-3
3.181023 m
Temperature 25 Deg.
-6
Lifetime, f 4.310 Sec
Emission bandwidth, 265 nm
Normalized excited-state absorption strength, fL 0.19 -
2
Emission cross section, e 710-23 m
Refraction index 1.82 -
Numerical aperture 0.789 -
Number of modes, M 15 22 29 -

4.4 Simulation of laser

The simulation of Cr4+:YAG fiber laser is based on a lump model with a
four-level laser system to construct the rate equations for population density, N2(t),
and cavity laser intensity IL(t). In addition, the excited-state absorption at lasing
wavelength, L, and thermal loading effect are also taken into account [4.7]. The
energy level diagram for simulation model is shown in Fig 4.6. The equation of
population density, N2(t), is the same as that in Eq. (4.1) except the parameters of s
and Is were replaced by L and IL. To determine the pump-induced temperature
distribution inside the crystal, let us consider a cylindrically symmetric gain rod of
radius r0. By neglecting longitudinal heat conduction and by assuming a constant
cylindrical heat load radial width h, the axial (r = 0) temperature distribution T0 can
be estimated from [4.10],

ln 2 h Pp r0
T0 = Tb + 1 + 2 ln (4.15)
4 h

41
where Tb is the crystal boundary temperature, Pp is the pump power, and is the
thermal conductivity of the gain medium. h is the heating fraction, which gives the
fraction of the absorbed pump energy that is converted to heat inside the crystal.

The cavity laser intensity correlates closely with the population density N2(t) and
photon lifetime tc. It can be expressed as follows [4.11]:

dI L (t )
= I L (t ) K g N 2 (t)Vg 1 (4.16)
dt tc

2 [n g Lg + ( Lc Lg ) ]
tc = (4.17)
c {1 [ R1 R2 exp ( 2 pl Lg )]}

c e Lg
Kg (4.18)
n g V g Lc

where Vg is the mode volume in the gain medium. ng is the refraction index of the gain
medium. Lg and Lc are the gain medium and cavity lengths, respectively. c is the
velocity of light. R1 and R2 are the reflectances of input face and output face,
respectively. Kg is the coupling coefficient of the gain medium. Then the time domain
of Eqs. (4.1) and (4.16) after t can be expressed as follows:

a p I p ( 0)
N 2 ( t ) = N 2 ( 0 ) + t [N T N 2 (0)]
hc (4.19)
I (0) esa L I L (0) 1
N 2 ( 0) e L L + +
hc hc f (Tb )

1
I L ( t ) = I L (0) + t I L (0) K g N 2 (0)Vg - . (4.20)
tc

Therefore, Eqs. (4.19) and (4.20) can, in general, be expressed as

a p I ip1
N 2i = N 2i 1 + t [ N T N 2i 1 ]
hc
(4.21)
i 1
e LIL i 1
esa L I L 1
N 2i 1 + +
hc hc f (Tb )
42
 1
I Li = I Li 1 + t I Li 1 K g N 2i 1Vg - (4.22)
tc

where N2i, ILi , and Ipi are defined as follows,

N 2i = N 2 (i t ), I Li = I L (i t ), I ip = I ip (i t ).

In addition, mode matching between the pump and cavity mode is assumed, i.e.
rp=ro=r, where rp and ro are the pump and radiative light radii, respectively. Based on
the theoretical model described above, we can use the Eqs. (4.21) and (4.22) by giving
0 0
the initial values of N2 = 1and IL = 1 and using a finite difference time domain
method (FDTD) to calculate the distributions of the population density N2(t) and the
cavity laser intensity IL(t) as shown in Fig. 4.9. Then we can use the following
equation to calculate the laser output power, Pout,

Toc
Pout = I Li r 2 (4.23)
1 Toc

where Toc is the transmittance of the output face. The simulation parameters used in
this case are listed in Table 4.5.

5.6 0.40
Population density (#/m x 10 )
22

0.35

Cavity intensity (GW/m )

2
5.5
N2 0.30
3

5.4
0.25
5.3 0.20
0.15
5.2
0.10
5.1 IL 0.05
5.0 0.00
0 5 10 15 20 25 30
Time (s)

Fig. 4.9. The dependence of the population density and cavity laser intensity with
time.

43
Table 4.5 Simulation parameters used in Fig 4.8.
Parameters of population density
a Absorption cross section 2.2 x 10-22 m2
e Stimulated emission cross section 7 x 10-23 m2
esa Excited-state absorption cross section 1.3 x 10-23 m2
P Pump wavelength 1.064 x 10-6 m
L Lasing wavelength 1.45 x 10-6 m
h Plancks constant 6.626 x 10-34 J-m
c Velocity of light 3.0 x 108 m
f Fluorescence lifetime 4.5 x 10-6 s
Small signal absorption coefficient 15 m-1
NT Total population inversion density (= /a) 6.8 x 1022 #/m3
Parameters of photon intensity
Kg Coupling constant 1.154 x 10-14
Vg Mode volume 1
tc Photon lifetime 1.72 x 10-9 s
Lg Cr4+:YAG crystal length 2 cm
Lc Cavity length 2 cm
pl Propagation loss coefficient 0.16 dB/cm
R1 Reflectance of input face 0.998
R2 Reflectance of output face 0.995
n Refraction index of Cr4+:YAG 1.82
Thermal parameters of Cr4+:YAG crystal
f0 Fluorescence lifetime at 0 oC 5.35 x 10-6 s
a Thermal lifetime coefficient 4.16 x 10-8 s/oC
T0 Axial temperature (r = 0) 20.56 oC
Tb Crystal boundary temperature 20 oC
h Heating fraction 0.931
k Thermal conductivity 12 W/m-K
h Cylindrical heat load of radial width 3 x 10-5 m
r0 Gain rod of radius 1.625 x 10-4 m

44
 In order to investigate the performance of Cr4+:YAG fiber laser, we change
different simulation parameters to know their influences on laser output power. The
main simulation parameters are listed in Table 4.6.

Table 4.6 Simulation parameters of Cr4+:YAG fiber laser.

Parameters Pin (W) (1/cm) pl (dB/cm) Lg (cm) h (m) Tb ()
Value 2 0.15 0.02 4 15 20
Pin is the pump power.

Figure 4.10 shows the calculated threshold pump power as a function of

propagation loss for different small signal absorption coefficients. It can be seen that
the threshold pump power increase exponentially when the propagation loss increases.
In addition, at higher small signal absorption coefficient the fiber laser can lase even
though the propagation loss is higher. For example, under the condition of pump
power of 6 W there are lasing if the propagation losses are less than 0.034 dB/cm,
0.156 dB/cm and 0.434 dB/cm at small signal absorption coefficients are 0.15 cm-1,
0.56 cm-1 and 1.25 cm-1, respectively. Figure 4.11 shows the calculated laser output
power versus the propagation loss. The calculated result indicates that the laser output
power increase exponentially when the propagation loss decreases. Therefore,
reducing the propagation loss can effectively improve the laser output power.

16 -1
= 0.15 cm
Threshold pump power (W)

14 -1
= 0.56 cm
12 -1
= 1.25 cm
10
8
6
4
2
0 Lg = 3 cm

0.0 0.1 0.2 0.3 0.4 0.5

Propagation loss (dB/cm)
Fig. 4.10. Threshold pump power as a function of propagation loss for different small signal
absorption coefficients.

45
 1.2
-1
= 0.15 cm
1.0

Output power (W)

-1
= 0.56 cm

0.8

0.6

0.4

0.2

0.0
0.00 0.03 0.06 0.09 0.12 0.15
Propagation loss (dB/cm)
Fig. 4.11. Laser output power as a function of propagation loss.

Figure 4.12 shows the calculated laser output power as a function of transmittance
of the output face. At a propagation loss of 0.02 dB/cm, the optimum transmittance of
output facet and laser output power are 1.4% and 93 mW, respectively. For the
propagation loss of 0.03 dB/cm, the optimum transmittance and laser output power
are 0.6% and 13.7 mW, respectively. According to the simulation if the propagation
loss is smaller, the transmittance of the output face can be set a higher value to obtain
a higher laser output power as compared with a larger propagation loss sample.
Therefore, proper selecting the transmittance of the output face can obtain the
maximum laser output power.

100

80
Output power (mW)

Pmax = 93.0 mW @ Toc = 1.4%

60

40
Pmax = 13.7 mW @ Toc =0.6%

20
= 0.02 dB/cm
= 0.03 dB/cm
0
0.0 0.5 1.0 1.5 2.0 2.5 3.0
Transmittance of the output face, Toc (%)

Fig. 4.12. Laser output power as a function of transmittance of the output face.

46
 Figure 4.13 shows the calculated laser output power versus the fiber core diameter.
It shows that large fiber core diameter cannot obtain the laser output power because of
smaller pump intensity. Therefore, the laser output power can grow significantly with
reducing the fiber core diameter. Figure 4.14 shows the calculated laser output power
as a function of crystal boundary temperature. It shows that the laser output power
decrease with crystal boundary temperature increase.

80
70
Output power (mW)

60
50
40
30
20
10
0
0 20 40 60 80 100
Crystal fiber core diameter (m)
Fig. 4.13. Laser output power as a function of fiber core diameter at a propagation loss of 0.02
dB/cm.
64
= 12 W/m-K
62 = 1.38 W/m-K
Output power (mW)

60

58

56

54

52

50
0 10 20 30 40 50 60
o
Crystal boundary temperature ( C)

Fig. 4.14. Laser output power as a function of crystal boundary temperature.

In conclusion, the dominating parameters for the performance of Cr4+:YAG fiber

laser are small signal absorption coefficient and propagation loss. The crystal

47
boundary temperature can also appreciatively influence the magnitude of laser output
power. The laser output power could be in excess of 0.5 W at a pump power of 2 W if
the propagation loss and small signal absorption coefficient are 0.02 dB/cm and 0.56
cm-1, respectively.

48
 Chapter 5 Characterization of Cr4+:YAG crystal fibers

As described in Chapter 4, crystal fiber with the small core diameter and lower
propagation loss are important for higher ASE and laser efficiency. Since interface
loss of the crystal fiber is one of main causes of the optical loss, besides fiber
diameter below 30 m is not easy to grow. Therefore, we develop a new cladding
technique to reduce the propagation loss and fiber diameter.

5.1 Single crystal fiber

5.1.1 X-ray diffraction analysis

The quality of Cr4+:YAG crystal fiber grown by the LHPG method was measured
by a Siemens D5000 diffractometer. Figure 5.1 shows the X-ray diffraction patterns of
the raw material grown by the Czochralski (CZ) method and the 400-m diameter
crystal fiber grown under 0.5 mm/min. The higher peak is caused by K1 line of
copper. The lower peak is caused by K2 line of copper. The FWHM values of the
main peaks are 0.0680 and 0.0580 for the raw material and 400-m diameter crystal
fiber, respectively. This result shows that the grown crystal fiber has better crystal
quality than the original bulk crystal rod.

35 35
X-ray intensity (cps x 1000)
X-ray intensity (cps x 1000)

K1 K1
30 FWHM=0.0680 30 FWHM=0.0580
25 25
20 20 K2
K2
15 15
10 Slit:0.2 mm 10 Slit:0.2 mm
5 Step:0.020 5 Step:0.020
0 0
42.0 42.2 42.4 42.6 42.8 43.0 27.2 27.4 27.6 27.8 28.0 28.2
2 theta (deg.) 2 theta (deg.)

(a) (b)

Fig. 5.1. X-ray diffraction patterns of (a) the raw material and (b) the 400-m diameter fiber.

49
5.1.2 Composition analysis
Since doping concentration will influence the device performance, EPMA was
used to measure the doping profile across the fiber cross section using JEOL
JXA-8900R. To know the doping concentration of the crystal fibers compare with the
raw materials we measure the doping concentration of raw materials firstly. Table 5.1
shows the measured doping profiles of raw materials with different absorption
coefficients.

Table 5.1 Average doping concentrations of Cr4+:YAG raw materials.

Raw material Ave. Cr2O3 Ave. CaO
Absorption coefficient, concentration
dimension of concentration
Cr4+:YAG (mm3) at 1064 nm (cm )
-1
(wt.%) (wt.%)
2 2 30 4.5 0.226 0.018
2 2 30 2.5 0.172 0.005
2 2 30 0.5 0.141 0.005
0.5 0.5 30 > 4.5 0.237 0.038
0.3 0.3 30 > 4.5 0.269 0.036

Figure 5.2 shows the doping profiles with multiple regrowths. Starting from a
2-mm raw material ( = 4.5cm-1) with 3 mm/min, multiple regrowths were performed.
We can see that the doping profiles of raw material are uniform. After the first growth,
the doping profiles of fiber with diameter of 0.92 mm show gradients in concentration.
The doping concentration of Chromium at the fiber center is lower than that of at the
edge. On the contrary, the doping concentration of Calcium becomes higher near the
center portion. This phenomenon is attributed to the signs of the segregation
coefficients. After multiple regrowths to reduce the fiber diameter, the doping profiles
become uniform again. The average doping concentration of fibers with multiple
regrowths were listed in Table 5.2. It shows only a slight decrease in the average CaO
concentration was observed, typically less than 10%, but the average Cr2O3
concentration was decrease quickly with reducing the fiber diameter. From the
measurement of about 30 samples with different growth conditions, an empirical
formula was derived for the average Cr2O3 concentration of the crystal fiber after
growth,

50
 CCr2O3 = 0.68C 0 (v / r ) D 1 / 3 , when v/r <1.7
1/ 2
(5.1)

where C0 is the average Cr2O3 concentration of the raw material. v and r are the
growth speed and pull/push speed ratio, respectively. D is the diameter of source rod.
Therefore, crystal fiber with higher growth speed and lower pull/push speed ratio will
have higher chromium concentration due to the chromium ions have less diffusion
time from the source rod to the fiber. Besides, crystal fiber grown with a larger
diameter of the source rod will have higher chromium concentration due to the
chromium ions have longer diffusion time from the molten zone center to the
circumference and then evaporating to the air.

0.06
0.25
2 mm
CaO concentration (wt.%) 0.05
Cr2O3 concentration (wt.%)

0.92 mm
0.20 0.53 mm
2 mm 0.04 0.32 mm
0.92 mm 0.12 mm
0.15 0.53 mm
0.32 mm 0.03
0.12 mm
0.10
0.02

0.05 0.01

0.00 0.00
0 10 20 30 40 50 60 70 80 90 100 0 10 20 30 40 50 60 70 80 90 100
Percent diameter (%) Percent diameter (%)

(a) (b)

Fig. 5.2. Doping profiles of (a) Cr2O3 and (b) CaO with multiple regrowths.

Table 5.2 Average doping concentrations of Cr4+:YAG crystal fibers.

Cross section of Cr4+:YAG Ave. Cr2O3 Ave. CaO
crystal fiber concentration (wt.%) concentration (wt.%)
= 0.92 mm 0.121 0.019
= 0.53 mm 0.086 0.019
= 0.32 mm 0.062 0.016
= 0.12 mm 0.015 0.016

Figure 5.3 shows the fitting result using Eq. (5.1). It has good match to
experiment data. In addition, the doping profiles of fibers with different growth

51
speeds in first growth were shown in Fig. 5.4. It shows that lower growth speed
results in flatter distribution compared to higher growth speed. Here the fiber
diameters are all 0.92 mm.

0.15
Cr2O3 ave. concentration (wt.%)

measurement
0.12 empirical fitting

0.09

0.06

0.03

0.00
1.0 0.8 0.6 0.4 0.2 0.0
Fiber diameter (mm)

Fig. 5.3. Average Cr2O3 concentration of fibers with multiple regrowths.

0.20
0.18 Cr2O3 3mm/min
Cr2O3 2mm/min
0.16 Cr2O3 1mm/min
Concentration (wt.%)

0.14 CaO 3mm/min

0.12 CaO 2mm/min
CaO 1mm/min
0.10
0.08
0.06
0.04
0.02
0.00
0 10 20 30 40 50 60 70 80 90 100
Percent diameter (%)

Fig. 5.4. Doping profiles of fibers with different growth speeds.

52
5.1.3 Oxidation state analysis
Although using EPMA can measure the concentration of Cr and Ca, it cannot
distinguish the oxidation states of ions. We utilized the different spectral
characteristics of 3+ and 4+ oxidation states of Cr ions to employ a scanning optical
microscope (SOM) for distinguishing between Cr3+ and Cr4+ ions. To measure the Cr3+
and Cr4+ fluorescence intensity profiles across the fiber cross section, a confocal
microscope with a 532-nm frequency double Nd:YVO4 laser and 1064-nm Nd:YVO4
laser were used as the light sources to pump the Cr3+ and Cr4+ ions, respectively. The
experimental setup is shown in Fig. 5.5.

Eyepieces
Objective
Si PD Lens 10x/0.25 Dichroic 2
3+
(For Cr ) Nd:YVO4 laser
(1064 nm)
Prism

Pinhole Band pass filter

600-800 nm Dichroic 1 Frequency doubled
Nd:YVO4 laser
Band pass filter (532 nm)
Fiber coupled 1200-1600 nm
spectrometer
Objective
10x/0.25
Objective
Pinhole 40x/0.65

Lens
Sample
Optical spectrum 2D-stepping motor
analyzer
InGaAs PD
(For Cr4+)
Fig. 5.5. Schematic drawing of the scanning optical microscope.

For the Cr3+ fluorescence measurement, the dichroic beam splitters 1 and 2 were
designed to reflect the excitation laser (532 nm) and pass through the Cr3+
fluorescence (600-800 nm). A band pass filter with a transparent window from 600 to
800 nm was set for increasing the signal-to-noise ratio. A Silicon photodiode (DET
210, Thorlabs) and a fiber coupled spectrometer (USB2000, Ocean Optics) were used
for measuring Cr3+ fluorescence intensity and spectrum. For the Cr4+ fluorescence

53
measurement, another dichroic beam splitter 1 was designed to reflect the excitation
laser (1064 nm) and pass through the Cr4+ fluorescence (1200-1700 nm). The dichroic
beam splitter 2 was the same one as the Cr3+ fluorescence measurement. It was
designed to reflect the Cr4+ fluorescence (1200-1700 nm) and pass through the Cr3+
fluorescence. After the dichroic beam splitter 2, a long pass filter was set for passing
through the wavelength longer than 1300 nm to distinguish the Cr4+ fluorescence
against the excitation laser and noise. An InGaAs photodiode (G8370-05, Hamamatsu)
and an optical spectrum analyzer (86142A, HP) were used for measuring Cr4+
fluorescence intensity and spectrum.

The Cr3+ fluorescence image and spectrum are shown in Fig. 5.6. The Cr3+
fluorescence spectrum range is from 650 to 780 nm and four major peaks were found
at 678 nm, 690 nm, 707 nm and 723 nm. The Cr3+ fluorescence image reflects the
concentration distribution of Cr3+ ion in the crystal fiber. The stress striation of Cr3+
fluorescence was observed in the center of Cr:YAG crystal fiber. This stress striation
is formed by three {211} facet planes [5.1-5.2]. The Cr4+ fluorescence image and
spectrum are shown in Fig. 5.7. The Cr4+ fluorescence spectrum shows the broadband
emission from 1.2 to 1.6 m. The central wavelength was found at 1.38 m. The Cr4+
fluorescence image also showed the same stress striation in the center of Cr:YAG
crystal fiber as that of Cr3+ fluorescence image.

4000
707 nm

3000
Intensity (a.u.)

690 nm

678 nm
2000
723 nm

1000

0
600 650 700 750 800 850
0.92 mm Wavelength (nm)
(a) (b)

Fig. 5.6. (a) fluorescence image and (b) spectrum of Cr3+ ions.

54
 1500

1200

Intensity (a.u.)
900

600

300

0
1100 1200 1300 1400 1500 1600 1700
0.92 mm Wavelength (nm)

(a) (b)

Fig. 5.7. (a) fluorescence image and (b) spectrum of Cr4+ ions.

It has been shown that Nd:YAG crystal fibers with diameters of 2 mm show the
presence of the typical three-fold strain birefringence patterns near the center of the
crystals but no significant birefringence patterns were found in fibers with diameters
of 170 m [1.1]. To find the strain pattern distribution with different fiber diameter,
diameters of 920, 530, 460, 317, 307, 300, 120 and 66 m were tested as shown in Fig.
5.8. Beyond 460 m the three-fold strain birefringence patterns were clearly seen,
while no significant birefringence patterns found below 460 m.

Max

920 m 530 m 460 m 317 m

Min
307 m 300 m 120 m 66 m

Fig. 5.8. Cr3+ fluorescence image with different fiber diameters.

55
 A comparison between SOM and EPMA measurements is shown in Fig. 5.9. The
EPMA curve shows the total concentration of Cr ions, but the Cr3+ fluorescence only
reflects the concentration of Cr3+ ions. The two curves are in good agreement because
most of the Cr ions are Cr3+ ions. It is apparent that the signal-to-noise ratio of SOM
is much higher than that of the EPMA measurement. The Cr3+ measurement
sensitivity of SOM was determined to be 1.61017 cm-3, which is equal to 4.410-4
wt.% with a 0.1-sec/pixel measurement time. However, the Cr2O3 sensitivity of
EPMA measurement was determined to be 0.01 wt.% with a 240-sec-per-spot
measurement time. The SOM measurement exhibits much superior sensitivity and
faster acquisition speed.

100 0.14
Cr fluorescent intensity (a.u.)

3+
90

Cr2O3 concentration (wt.%)

Cr fluorescence
EPMA data 0.12
80
70 0.10
60
0.08
50
40 0.06
3+

30
0.04
0 10 20 30 40 50 60 70 80 90 100
Percent diameter (%)
Fig. 5.9. Cr3+ fluorescence intensity and Cr2O3 concentration measured by SOM and EPMA,
respectively.

Figure 5.10 shows the Cr3+ concentration across the fiber cross sections with
different fiber diameters measured by SOM. Figure 5.11 shows the distribution of
Cr4+ fluorescence intensity across the fiber cross sections with different fiber
diameters. It shows that the distribution of Cr4+ fluorescence intensity is getting
concentrated at the fiber center when the core diameter is less than 300 m. To
explain this phenomenon, the distributions of Cr4+, Cr2O3, and CaO are shown in Fig.
5.12. In the 920 m diameter sample, the distribution of Cr4+ ions is flatter than that

56
of total Cr concentration. The reason is that the concentration of Cr4+ ions depends on
both the concentration of Cr and Ca ions. Although the total concentration of Cr ions
at fiber center is lower than that at the edge, Ca ions tend to accumulate near the fiber
center, which results in the flatter distribution of Cr4+ ions. In the 66 m diameter
sample, the total distribution of Cr is quite flat while Ca ions gather near the fiber
center. Therefore, the concentration of Cr4+ ions peaks at the fiber center.
.
0.20
0.18 920 m
Cr concentration (wt.%)

0.16 530 m
0.14 300 m
66 m
0.12
0.10
0.08
0.06
0.04
3+

0.02
0.00
0 10 20 30 40 50 60 70 80 90 100
Percent diameter (%)

Fig. 5.10. Cr2O3 concentration with different fiber diameters measured by SOM.

0.8
Cr fluorescence intensity (a.u.)

920 m
0.7
530 m
0.6 300 m
66 m
0.5
0.4
0.3
0.2
0.1
4+

0.0
0 10 20 30 40 50 60 70 80 90 100
Percent diameter (%)
Fig. 5.11. Cr4+ fluorescence intensity with different fiber diameters.

57
 0.0012 0.20
4+
Cr

EPMA measurement (wt.%)

Cr concentration (wt.%)
0.0010 EPMA: Cr2O3
EPMA: CaO 0.15
0.0008

0.0006 0.10

0.0004
0.05
4+

0.0002

0.0000 0.00
0 10 20 30 40 50 60 70 80 90 100
Percent diameter (%)

(a)

0.0012 0.04
4+
Cr

EPMA measurement (wt.%)

Cr concentration (wt.%)

0.0010 EPMA: Cr2O3

EPMA: CaO 0.03
0.0008

0.0006 0.02

0.0004
0.01
4+

0.0002

0.0000 0.00
0 10 20 30 40 50 60 70 80 90 100
Percent diameter (%)

(b)

Fig. 5.12. Comparison of Cr4+, Cr2O3, and CaO concentrations in (a) 920 m diameter and (b)
66 m diameter crystal fibers.

To find out the relation between Cr4+, Cr, and Ca2+, the distribution of Cr4+
fluorescence intensity and concentrations of Cr2O3 and CaO by EPMA measurement

58
were used. Compared with A. Sugimotos work [4.6], the Cr4+ measurement
sensitivity was determined to be 7.51015 cm-3, which is equal to 2.110-5 wt.% with a
0.1-sec/pixel measurement time. The dependence of Cr4+ to Ca/Cr ratio can clearly be
seen in Fig. 5.13. There is no Cr4+ in a YAG host without charge compensator. In
addition, only less than 1% of the Ca2+ becomes active in charge compensation. The
low compensation efficiency may be explained by large lattice mismatch (i.e. +8.7%)
with Ca2+ ions incorporated into the dodecahedrally coordinated Y3+ sites. The large
lattice mismatch is also accompanied by the production of oxygen vacancies, which
result in the de-activation of Ca2+ charge compensation.

1.2

1.0
Cr / total Cr (%)

0.8

0.6

0.4
4+

0.2

0.0
0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6
2+
Ca / total Cr

Fig. 5.13. The functional dependence between normalized Cr4+ and Ca2+ concentrations.

5.2 Single-clad crystal fiber

5.2.1 Growth of single-clad crystal fiber

In order to reduce the propagation loss of crystal fibers, borosilicate and
fused-silica capillary tubes were used to form the cladding for enhancing the
light-guiding properties. Table 5.3 lists some physical properties of the borosilicate
and fused-silica glasses.

59
Table 5.3 Physical properties of borosilicate and fused-silica glasses [5.3-5.5].
Borosilicate Fused-silica Unit
SiO2, 99.9 %
Na2O, 0.03 %
SiO2, 80.6 %
Al2O3, 0.02 %
B2O3, 13.0 %
TiO2, 0.01 %
Compositions Na2O, 4.0 % wt.%
K2O, 0.01 %
Al2O3, 2.3 %
CaO, 0.01 %
K2O, 0.1 %
Cr2O3, 0.01 %
....
Refractive index 1.474 1.459 -
o
Softening point 821 1600 C
o
Annealing point 560 1075 C
Thermal expansion
3.25x10-6 0.55x 10-6 m/m-oC
coefficient
Thermal conductivity 1.1 1.38 W/m-K
Density 2.23 2.20 g/cm3
Hardness (Knoop) 418 500 -

Figure 5.14 (a) shows the new fiber cladding method. The source rods were
0.5-mol.%-doped Cr4+:YAG with <111> crystal orientation and 2 mm 2 mm cross
section. After several diameter-reduction steps on the LHPG system, cores with
diameters of less than 100 m were obtained. Then the <111>-oriented core was
inserted into fused-silica and borosilicate capillary tube to be used as the source
material. The same LHPG system used for preparing the core was again used to draw
the Cr:YAG-filled capillary tube. Figure 5.14 (b) and (c) show the polished surfaces
of glass-clad fibers. The sample shown in Fig. 5.14 (b) was prepared from a source
rod with a 66-m Cr:YAG core and fused-silica capillary with 76- and 320-m inner
and outer diameters, respectively. A smooth interface between the core and the
fused-silica can be seen clearly. The core and cladding diameters are 29 m and 64
m, respectively. Our expected core diameter was actually 13.2 m; the reason that
the core became 29 m will be explained later. It can also be seen that the core
boundary is a circle instead of a hexagon, which is usually seen in a <111>-oriented
crystal fiber grown by the LHPG method without a silica capillary tube. Therefore,
strong interaction took place between the core and the cladding during growth. The

60
 sample shown in Fig. 5.14 (c) was prepared from a source rod with a 100-m Cr:YAG
core and a borosilicate capillary with 120 and 260 m inner and outer diameters,
respectively. Figure 5.14 (c) shows that the core boundary is hexagonal. The core and
cladding diameters are 100 m and 250 m, respectively.

64 m 250 m
CO2 laser

29 m 100 m
Cr4+:YAG crystal fiber
Glass tube

(a) (b) (c)

Fig. 5.14. (a) Schematic of codrawing laser-heated pedestal growth method, and photographs
of the polished end of (b) a 29-m-core diameter fused-silica-clad Cr:YAG fiber, (c) a
100-m-core diameter borosilicate-clad Cr:YAG fiber.

5.2.2 Composition analysis

5.2.2.1 Electron probe microanalysis

To determine the composition between the core and cladding, an electron-probe
microanalyzer, JEOL JXA-8900R, was used. Figure 5.15 shows the line scan of
composition of the sample shown in Fig. 5.14. Figure 5.15 (a) shows that the
composition of cladding in Fig. 5.14 (b) is almost SiO2 (> 99.9 wt.%), but the core
area is composed of mixtures of SiO2 and YAG. The average SiO2 concentration in the
core area is ~ 64.9 wt.%. This explains why the core diameter is 29 m when the
speed ratio of pull/push is 25:1. By use of the lever rule, the core radius with
interdiffusion, rw, can be estimated as follows:

61
 rw w/d f + (1 w )/d Y
=
rwo (1 w)/dY , (5.2)

( )
where rwo = Rs / is the core radius without interdiffusion and w and (1-w) are the
average weight percent of SiO2 and YAG, respectively, in the core area. The densities
of fused-silica, df, and YAG, dY, are 2.20 and 4.56 g/cm3, respectively. Rs is radius of
the source rod of Cr4+:YAG crystal. is the pull/push speed ratio. The estimated core
diameter from Eq. (5.2) is 29.02 m, which is in excellent agreement with the
measured result. Figure 5.15 (b) shows the line scan of composition of the sample
shown in Fig. 5.14 (c). It shows that the composition of core area in Fig. 5.14 (c) is
pure YAG. Even in the core edge the composition of SiO2 was less than 0.03 wt.%.

100 SiO2 100 SiO2

Y2O3 Y2O3
Concentration (wt.%)

Concentration (wt.%)

80 Al2O3 80 Al2O3

60 60

40 40

20 20

0 0
0 10 20 30 40 50 60 70 80 90 100 0 10 20 30 40 50 60 70 80 90 100
Percent diameter (%) Percent diameter (%)
(a) (b)

Fig. 5.15. Distribution of major compositions by line scanning the cross-section of (a)
fused-silica-clad Cr:YAG fiber, and (b) borosilicate-clad Cr:YAG fiber. The regions between
the two vertical lines designate the core areas.

5.2.2.2 Cr ion fluorescence measurements

To measure the Cr4+ fluorescence of glass-clad fibers, the SOM system was used
again. Figure 5.16 shows the measured result of line scanning the cross section of the
glass-clad fibers. The borosilicate-clad fiber shows a strong fluorescence in the core
area, while the fused-silica-clad fiber has almost no fluorescence in the core area.
Though the detailed mechanism for the disappearance of the fluorescence in YAG and
SiO2 mixtures is still to be elucidated, the entering of SiO2 into the YAG matrix tends

62
to change the Cr ion oxidation from quadrivalent state to trivalent state is consistent
with the fact that Cr-doped silica fibers have much lower long wavelength emission
efficiency compared to that of Cr-doped YAG.

0.6
Cr fluorescence intensity (a.u.)

Fused-silica-clad
Borosilicate-clad
0.5

0.4

0.3

0.2

0.1
4+

0.0
0 10 20 30 40 50 60 70 80 90 100
Percent diameter (%)

Fig. 5.16. Cr4+ fluorescence of fused silica and borosilicate-clad Cr:YAG fibers.

5.3 Double-clad crystal fiber

5.3.1 Growth of double-clad crystal fiber

Although borosilicate-clad fiber can produce a strong Cr4+ fluorescence in the
core area, it is very difficult to fabricate the core with less 30-m diameter using
LHPG technique. Fused-silica-clad fiber can obtain core diameter below 30 m, but it
has almost no Cr4+ fluorescence in the core area due to the entering of SiO2 in YAG.
With properly controlled growth parameters of CDLHPG method, we successfully
grew a double-clad fiber, where the <111>-oriented crystal fiber with diameter of 68
m was inserted into a fused silica capillary tube with 76- and 320-m inner and
outer diameters, respectively. A crateriform molten zone for downward growth is
shown schematically in the left part of Fig. 5.17. The side view of the grown fiber
with a three-layer structure is shown in the right part of Fig. 5.17. The core diameter
can be controlled by adjusting the CO2 laser power or growth speed.

63
 Cr4+:YAG crystal fiber
Fused silica tube

Molten zone

Core
Inner cladding
Outer cladding

Fig. 5.17. Left: Schematic diagram of the molten zone during growth, right: photograph of the
side view of the grown double-clad Cr4+:YAG fiber.

5.3.2 Composition analysis

5.3.2.1 Electron probe microanalysis

In order to know the composition in the double-clad fiber, an EPMA, (JEOL
JXA-8900R), was used. Figure 5.18 shows the distribution of major compositions by
line scanning the clad fiber cross-section. The inset shows the polished end face of the
clad fiber. A double-clad fiber structure can clearly be seen. The core, inner, and outer
cladding diameters are 25 m, 100 m, and 320 m, respectively. The measurement
result shows that the compositions of core and outer cladding are almost YAG and
SiO2, respectively. But the compositions of the inner cladding are mixtures of SiO2
and YAG. Slight increase of the SiO2 concentration near the core is due to the
softening point of fused silica is much lower than the melting point of YAG so that the
in-diffusion of SiO2 is blocked at the inner cladding-core boundary. The average SiO2
concentration in the inner cladding is 39.8 wt.%, which can be used to estimate the
inner cladding diameter when the core diameter is known. Using the lever rule, the
inner cladding radius, ri, can be expressed as follows,

64
 w/d f + (1 w)/d Y
ri =
(1 w)/d Y
(R
2
Y )
rc2 + rc2 , (5.3)

where w and (1-w) are the average weight percent of SiO2 and YAG in the inner
cladding, respectively. The densities of fused silica, df, and YAG, dY, are 2.20 and 4.56
g/cm3, respectively. RY is the Cr4+:YAG source rod radius and rc is the core radius. The
calculated inner cladding diameter using Eq. (5.3) is 100.5 m, which is in excellent
agreement with the measured result.

100
Concentration (wt.%)

core
80
SiO2
60 Y2O3
Al2O3
40

20 inner cladding

0
0 20 40 60 80 100
Percent diameter (%)
Fig. 5.18. Distribution of major compositions by line scanning the cross-section of the
double-clad Cr4+:YAG crystal fiber. The region between the two vertical lines designates the
core area. The inset shows the photograph of the polished end with a 25-m-diameter core.

5.3.2.2 Cr ion fluorescence and refraction index measurements

The Cr fluorescence of double-clad fiber was measured by the SOM system. The
measured result is shown in Fig. 5.19. It shows that the majority of the Cr4+
fluorescence concentrates within the core region and the Cr3+ fluorescence almost
concentrates in the core and inner cladding.

65
 Norm. fluorescence intensity (a.u.)
1.0
3+
Cr
4+
0.8 Cr

0.6

0.4

0.2

0.0
20 30 40 50 60 70 80
Percent diameter (%)
Fig. 5.19. Line scans of Cr fluorescence intensity of a double-clad Cr4+:YAG crystal fiber.

To measure the refraction index of the double-clad fiber, a SOM system with a
635-nm DFB laser (S1FC635, Thorlabs) was used as the light source. A 40 objective
lens with a NA of 0.65 focused the laser beam and achieved 1-m laterally spatial
resolution. The power noise of the single-mode DFB laser is 0.5%, which results in a
sensitivity of n ~ 0.003. The refraction index profile of double-clad fiber is shown in
Fig. 5.20. It shows that the refraction index profile in the inner cladding is from 1.66
to 1.58 corresponding to the SiO2 concentrations from about 30 wt.% to 50 wt.%, and
the refraction index of core and outer cladding are 1.82 and 1.46, respectively.

2.0

1.9
YAG
Refraction index

1.8
YAG YAG
+ +
1.7 SiO2 SiO2

1.6

1.5 SiO2 SiO2

1.4
20 30 40 50 60 70 80
Percent diameter (%)

Fig. 5.20. Line scan of refraction index of a double-clad Cr4+:YAG crystal fiber.

66
5.3.3 Microstructure analysis using high-resolution TEM
The microstructure of double-clad fiber was investigated using an analytical
TEM: a JEOL JEM-3010 electron microscopy equipped with a LaB6 electron gun
operating at 300 kV, which provides a point to point resolution of 0.12 nm.

Before the double-clad fiber was analyzed by TEM, the thickness of fiber needs
to be electron-transparent. The process of TEM specimen preparation was described
as follows. First, the fiber was cut and sectioned by a diamond saw. The thickness of
each section is about 500 m for further thinning. Then the specimen was ground with
silicon carbide paper from #800 to #1200. After grinding, the specimen is polished to
a thickness of less than 10 m. Finally, specimens were ion-milled by Gatan precision
ion polishing system (PIPS). The method described above allows us to achieve the
electron-transparent area on the core region, inner cladding, and the interface between
outer and inner cladding of the fibers.

5.3.3.1 Microstructure of core

Figure 5.21 (a) shows the TEM image of the core with diameter of 31 m. Figure
5.21 (b) shows an enlargement of rectangular area in Fig. 5.21 (a). It shows that the
atomic image at the center part ranked in hexagon, which can be seen in a
<111>-oriented YAG crystal. Beyond the center part of the atomic image, it cannot be
seen the hexagon obviously due to the specimen defocus.

Figure 5.22 shows an enlargement of the center part in Fig. 5.21 (b). The
hexagonal area of the inset designates a unit cell. The inset was drawn by
Crystallography, and it shows YAG structure viewed from <111>-direction. The
lattice constant is about 1.1 nm by calculating the atomic image directly. The value is
close to that in literature, which is 1.201 nm [3.1]. The mismatch of lattice constant
between measurement and literature could be TEM measurement error or stress from
the inner cladding due to thermal expansion coefficient mismatch.

67
 5 m

(a)

Defocus: ~ 155 nm, thickness: 30-40 nm

2 nm

Defocus: ~ 110 nm, thickness: 30-40 nm

(b)
Fig. 5.21. (a) TEM image of the core ( 4000), and (b) an enlargement of the rectangular area
in (a).

68
 :O

:Y

: Al

1 nm

Fig. 5.22. Atomic image of the core. The inset shows an atomic drawing of YAG structure
viewed from <111>-direction.

In addition, we also measured a selected-area diffraction (SAD) pattern of the

core as shown in Fig. 5.23. It shows that the core is a cubic structure and the
diffraction pattern is a (111) plane. The lattice constant, a, can be calculated by the
following equations:

Rd hkl = L , (5.4)

d hkl = a/ h 2 + k 2 + l 2 , (5.5)

69
where R is the distance from the transmitted electron beam to the diffraction spot. dhkl
is spacing between two adjacent (hkl) planes. and L are the electron wavelength and
camera length, respectively. In this case, R is about 4.625 mm, which was measured
from beam center to the I0 diffraction spot on the negative of SAD pattern. is
0.01968 for accelerating voltage of 300 kV, and L is 200 cm. The calculated
result of lattice constant is 1.2 nm, which is very close to that in literature. Therefore,
the core is a YAG structure with a <111>-oriented cross-section.

2
0I
I0
0I

I0
I0
0I

[111] 2

Fig. 5.23. The SAD pattern of the core.

5.3.3.2 Microstructure of inner cladding

The inner cladding of double-clad fiber is an inter-diffusion layer with mixtures
of SiO2 and YAG. The TEM images of the inner cladding for two different regions A
and B in Fig 5.24 (a) were measured. Fig. 5.24 (b) and (c) exhibit the dark-field
images in the inner cladding for the region A and the region B, respectively, which
indicates that toward the core direction, it has better crystallinity due to Fig. 5.24 (c)
has better contrast (depicted as black arrows) compared with Fig. 5.24 (b). The

70
dark-field images also give a good agreement with EPMA measurement in the inner
cladding. Namely, the less amount of SiO2 diffused towards the core direction (EPMA
data), the better crystallinity formed (dark-field TEM images).

~ 20 m

core B
~ 40 m
A

inner cladding

(a)

SiO2+YAG SiO2+YAG
A B

10 nm 10 nm

(b) (c)

Fig. 5.24. (a) A cross-sectional image of double-clad fiber and the areas taken for dark-field
images were marked with rectangular blocks (A and B); (b) the dark-field image of region A;
(c) the dark-field image of B.

71
 The TEM images of regions A and B are shown in Figs. 5.25 and 5.26,
respectively. In Fig. 5.25 (b), a high-resolution micrograph is shown, which reveals
the crystalline nano-structures of around 10-nm thickness and less than 15-nm length
surrounded by SiO2 amorphous matrix. At this crystalline orientation the phase
contrast allows to differentiate lattice planes of ~0.29-nm separation. In addition, the
shapes of crystalline structures far from the core are nearly spheric (see Fig. 5.25 (a)),
and they become irregular with better crystal quality (see Fig. 5.26) towards the core
(YAG) direction. The crystalline nano-structures surrounded by amorphous matrix can
also be found in literatures [5.6-5.18].

Crystalline structures

30 nm

(a)

3 nm

(b)

Fig. 5.25. (a) HRTEM image of region A, and (b) an enlargement of the rectangular area in
(a).

72
 YAG+SiO2

5 nm

Fig. 5.26. HRTEM image of region B.

5.3.3.3 Comparison between inner cladding and outer cladding

The HRTEM images of inner and outer cladding interface are shown in Fig. 5.27.
It can be clearly seen that many dark areas (as marked with white arrows) are in the
inner cladding, and there exists the evidence of crystalline nano-structures in each
dark area.

SiO2
SiO2

SiO2+YAG
0.5 m
10 nm
SiO2+YAG
(a) (b)
Fig. 5.27. HRTEM images showing (a) the interface between the inner and outer cladding. (b)
The high magnification of the interface in the rectangle.

73
 The electron diffraction patterns of inner and outer cladding are shown in Fig.
5.28. The outer cladding is an amorphous structure as shown in Fig. 5.28 (a). The
randomly distributed fine spots shown in Fig. 5.28 (b) indicate the existence of
crystalline structures in the inner cladding, which were formed during the process of
SiO2 (amorphous phase) diffusing into YAG (crystal structure). In addition, it also
consists of diffusing rings, resulting from the numerous amorphous phases
surrounding the nanocrystallites observed by the HRTEM images.

(a) (b)

Fig. 5.28. Electron diffraction patterns in (a) outer cladding and (b) inner cladding.

5.3.3.4 Comparison of inner cladding with different growth speeds

We also investigated the process of crystallization for the nanoscale particles in
the inner cladding with different growth speeds. Figure 5.29 presents the TEM images
with a medium magnification in the interface between the inner and outer claddings
for growth speeds of 3.75 mm/min and 30 mm/min. For 3.75 mm/min, it shows that
the inner cladding is flush with dark areas, which they are the evidence of particles,
and they have a good dispersion, but it has a reverse result for 30 mm/min. The result
indicates that 30 mm/min growth speed is too fast for the mixtures to be crystallized
near the interface between the outer and inner cladding.

74
 Outer cladding Outer cladding

Inner cladding Inner cladding

20 nm 20 nm

(a) (b)

Fig. 5.29. TEM images show the interface between the outer and inner cladding for the
growth speeds of (a) 3.75 mm/min and (b) 30 mm/min, respectively.

The HRTEM images shown in Fig. 5.30 present the distribution of crystalline
particles in the inner cladding for growth speeds of 3.75 and 30 mm/min. It can be
observed that the number of particles with slower growth speed is less than those with
higher growth speed, and for both of them the crystalline structures form in a line
direction. It indicates that crystallization of nanoscale particles from early diffusion
process (SiO2 diffused into YAG), and they arranged in a line direction. As the growth
speed decreasing, more and more nanoscale particles formed; the particles size was
enlarged and the crystallization was improved. Besides, the statistics of the average
sizes and the relative densities of nanoscale particles in the specimens of 3.75 and 30
mm/min were obtained directly from HRTEM images as shown in Table 5.4. Because
of the thickness of the specimens in HRTEM observation were unclear, relative
density is used in stead of absolute density. When the growth speed was increasing
from 3.75 to 30 mm/min, the particles decreased 1.86 times in density, while the
average size decreased about 16.7%.

75
 Crystalline nanoparticles
30 nm

(a)

Crystalline nanoparticles
30 nm

(b)

Fig. 5.30. HRTEM images show the distribution of crystalline structure in the inner cladding
for the different growth speeds of (a) 3.75 mm/min, and (b) 30 mm/min.

Table 5.4 The average sizes and the relative densities of nanoscale particles.
Specimens 3.75 mm/min 30 mm/min

Average sizes 12 nm 10 nm

Relative density 1.86 1

76
5.4 Propagation loss measurement
The wave-guiding characteristics of the glass-clad Cr:YAG fibers were
investigated by a modified cut-back method. It started with focusing a laser beam into
the end face of the glass-clad Cr:YAG fiber, then the through output power at two
out
different fiber lengths were measured. The through output power, P1, can be described
as follows,

P1out = lens coup Pin et l 1 (5.6)

where Pin is the input laser power. lens and coup are the transmittance of the focal
lens and coupling efficiency of the laser into the fiber end face, respectively. t (= +
pl) is the attenuation coefficient. and pl are the absorption coefficient and
propagation loss, respectively. l 1 is the fiber length. Assuming the coupling efficiency
and the Fresnel loss at the two ends of the fiber are unchanged after shortening the
length of the fiber, then the attenuation coefficient can be described as follows,

t =
(
ln P1out P2out ) (5.7)
l 2 l 1
out
where P2 and l 2 are the through output power and the fiber length after shortening
the length of the fiber, respectively. In order to obtain the value of propagation loss we
used at least two different wavelengths of lasers as the test light sources to estimate
the attenuation coefficients. Figure 5.31 shows the experimental setup.

Lens
Mirror 2

Half-wave Glass-clad
plate Detector
Cr:YAG fiber
Ti3+:sapphire
laser
Mirror 1
PBS

Fig. 5.31. Experimental setup of the propagation loss measurement.

A tunable Ti3+:sapphire laser was used as the test light source. The input laser
power was changed by a half-wave plate, followed by a lens to focus it into the end
face of the glass-clad Cr:YAG fiber. For the borosilicate-clad Cr:YAG fiber, the initial

77
 and shortening lengths of the fibers were 53.8 mm and 7 mm, respectively. Figure
5.32 shows the measured absorption coefficient and propagation loss as a function of
incident power. Figure 5.32 (a) shows the absorption coefficients of the fiber at an
incident power of 0.5 W for the incident laser wavelength at 980 nm, 840 nm, and 750
nm were 2.28 dB/cm, 0.98 dB/cm, and 0.64 dB/cm, respectively. The propagation loss
of the fiber was measured to be about 0.6 dB/cm as shown in Fig. 5.32 (b).

2.5 1.0
Absorption coefficient (dB/cm)

Propagation loss (dB/cm)

0.9 750 nm - 840 nm
2.0 980 nm 750 nm - 980 nm
0.8 840 nm - 980 nm
840 nm
1.5 750 nm 0.7
0.6
1.0 0.5
0.5 0.4
0.3
0.0 0.2
0.3 0.4 0.5 0.6 0.7 . 0.3 0.4 0.5 0.6 0.7
Incident power (W) Incident power (W)
(a) (b)

Fig. 5.32. (a) Absorption coefficient and (b) propagation loss of borosilicate-clad fiber as a
function of incident power.

For the fused-silica-clad Cr:YAG fiber, the initial and shortening lengths were
11.2 mm and 4.6 mm, respectively. Figure 5.33 shows the attenuation coefficient of
the fiber. When the incident power increased, the attenuation coefficient reduced due
to the pump absorption saturation. Therefore, the propagation loss of the fiber was
less than 0.1 dB/cm for the incident laser wavelength at 980 nm, which is a factor of 7
smaller than that of an unclad crystal fiber. In addition, we also measured the
propagation loss of double-clad Cr:YAG fiber. The initial and shortening lengths of
the fibers were 40.5 mm and 7.7 mm, respectively. Figure 5.34 shows the measured
absorption coefficient and propagation loss as a function of incident power. Figure
5.34 (a) shows the absorption coefficients of the fiber at an incident power of 100 mW
for the incident laser wavelength at 980 nm, 940 nm, and 900 nm were 2.91 dB/cm,

78
 2.43 dB/cm, and 2.38 dB/cm, respectively. The propagation loss of the fiber was
measured to be about 1.3 dB/cm as shown in Fig. 5.34 (b).

Attenuation coefficient (dB/cm)

0.8
0.7 =750 nm
=980 nm
0.6
0.5
0.4
0.3
0.2
0.1
0.0
0.20 0.25 0.30 0.35 0.40 0.45 0.50
Incident power (W)

Fig. 5.33. Attenuation coefficient of fused-silica-clad fiber as a function of incident power.

3.0 2.0
Absorption coefficient (dB/cm)

Propagation loss (dB/cm)

2.5 1.6

2.0 1.2

1.5 980 nm 0.8 900 nm - 940 nm

940 nm 940 nm - 980 nm
900 nm 900 nm - 980 nm
1.0 0.4
50 100 150 50 100 150
Incident power (mW) Incident power (mW)

(a) (b)

Fig. 5.34. (a) Absorption coefficient and (b) propagation loss of double-clad fiber.

79
 Chapter 6 Applications of Cr4+:YAG crystal fibers

Cr4+:YAG has a wideband spectrum that just covers the low loss window of
optical fiber. Such wideband characteristic is needed as light source or fiber amplifier
for the optical fiber communications. The wideband light source can be used in
WDM-component testing, sliced spectrum multi-channel light sources, or optical
coherence tomography. The wideband Cr4+:YAG fiber amplifier has a great potential
to be used in optical communications to cover all the O, E, S, C, L, and U bands with
a single fiber amplifier.

6.1 ASE light source

6.1.1 Single crystal fiber

To generate ASE from a Cr4+:YAG crystal fiber with a length of 15.7 mm, the
fiber was packaged with PbSn alloy in a copper groove. A 940-nm fiber-coupled laser
diode was used as the pump, followed by a 10 objective lens to focus the pump
beam and the ASE output was collimated by an achromatic lens followed by a
long-wavelength-pass filter to block the pump beam as shown in Fig. 6.1.
940-nm
fiber-coupled laser

Achromatic
Collimating lens
Crystal fiber Power meter
lens

Objective lens
10 PbSn alloy Filter
Fig. 6.1. Experimental setup of ASE power of Cr4+:YAG crystal fiber measurements.

Figure 6.2 shows the measured and simulated ASE power as a function of the
pump power. In the experiment, as much as 172 W of the ASE power was obtained.
The inset shows the polished end of crystal fiber with a diameter of 920 m. In the
simulation, good agreement was achieved between experiment and simulation result.

80
We also simulated the evolution of ASE power and upper level population density
along the crystal fiber at pump power of 7.98 W as shown in Fig. 6.3. It shows the
backward ASE output power at the fiber input facet is more intense than the forward
ASE output power at the fiber output facet, since the beginning section of the fiber,
with a forward pump, has more population inversion than that of the end section.
Besides, the population density decreases quickly and the forward ASE power
increase slowly at the fiber end section due to depletion the pump by fiber absorption.

200
180 Single crystal fiber
160 Core: 920 m
ASE power (W)

140 Pmax: 172 W

120
100
80
60
40 Experiment
20 Simulation
0
0 2 4 6 8 10
Absorbed pump power (W)
Fig. 6.2. ASE output power of Cr4+:YAG crystal fiber. Inset shows the end face of the
polished crystal fiber.

140 3.5
Forward ASE
120 Backward ASE 3.0
ASE power (W)

N2 ( x 10 m )

100 N2 2.5
-3
22

80 2.0
60 1.5
40 1.0
20 0.5
0 0.0
0 2 4 6 8 10 12 14 16
Position along fiber (mm)
Fig. 6.3. Calculated ASE power and upper level population density along the length of the
Cr4+:YAG crystal fiber.

81
6.1.2 Single-clad crystal fiber
The ASE power generated from a borosilicate-clad crystal fiber with a length of
46.6 mm was also measured. The fiber was packaged with PbSn alloy in a copper
groove and clamped to a cooled copper heat sink. A 1064-nm Yb fiber laser was used
as the pump and the ASE output was collimated by an achromatic lens followed by a
long-wavelength-pass filter as shown in Fig. 6.4. Figure 6.5 shows the measured and
simulated ASE power as a function of the absorbed pump power. In the experiment, as
much as 2.45 mW of the ASE power was obtained. The inset shows the polished end
of crystal fiber with core diameter of 100 m. In the simulation, good agreement was
achieved between experiment and simulation results.

Driver
Yb fiber laser

Borosilicate-clad Filter
Cr4+:YAG crystal fiber Detector

Lens PbSn alloy Achromatic lens

Fig. 6.4. Experimental setup for the ASE power measurement of borosilicate-clad Cr4+:YAG
crystal fiber.

3.0
Single-clad fiber
2.5 Core: 100 m
ASE power (mW)

Pmax: 2.45 mW
2.0

1.5

1.0

0.5 Experiment
Simulation
0.0
0 2 4 6 8 10
Absorbed pump power (W)

Fig. 6.5. ASE output power of the borosilicate-clad Cr4+:YAG crystal fiber. Inset shows the
end face of the polished crystal fiber.

82
 Figure 6.6 shows Cr4+ fluorescence spectra with and without the borosilicate
cladding. Only slight differences between the spectra were observed. We also
simulated the evolution of ASE power and upper level population density along the
crystal fiber at pump power of 9.38 W as shown in Fig. 6.7. It shows that the
backward ASE output power at the fiber input facet is close to the forward ASE
output power at the fiber output facet, since the upper level population density along
the crystal fiber decrease slowly, and the pump power was only absorbed about 77%
by the fiber.
1.0
Cr4+:YAG
Cr fluoresence intensity (a.u.)

single crystal
0.8

0.6

0.4

0.2
4+

Borosilicate-clad Cr4+:YAG
0.0
1100 1200 1300 1400 1500 1600
Wavelength (nm)
Fig. 6.6. Fluorescence spectra of borosilicate-clad Cr4+:YAG crystal fiber and Cr4+:YAG
crystal fiber without cladding.

1.6 2.4
Forward ASE
1.4 2.2
Backward ASE
1.2 N2
ASE power (mW)

2.0
N2 ( x 10 m )
-3

1.0
1.8
23

0.8
1.6
0.6
0.4 1.4

0.2 1.2
0.0 1.0
0 10 20 30 40 50
Position along fiber (mm)
Fig. 6.7. Calculated ASE power and upper level population density along the length of
borosilicate-clad Cr4+:YAG crystal fiber.

83
6.1.3 Double-clad crystal fiber
A 1064-nm Yb fiber laser was also used to pump a double-clad crystal fiber with
a length of 81.4 mm. The experimental setup is the same as the Fig. 6.4 except the
focal lens was replace by a 40 objective lens with a NA of 0.65. Figure 6.8 shows
the measured and simulated ASE powers as a function of the absorbed pump power.
In the experiment, as much as 2.36 mW of the ASE power was obtained. The inset
shows the polished end of crystal fiber with core diameter of 25 m. In the simulation,
good agreement was achieved between experiment and simulation result.

3.0
Double-clad fiber
2.5 Core: 25 m
ASE power (mW)

Pmax: 2.36 mW
2.0

1.5

1.0

0.5 Experiment
Simulation
0.0
0 1 2 3 4 5
Absorbed pump power (W)

Fig. 6.8. ASE output power of the double-clad Cr4+:YAG crystal fiber. Inset shows the end
face of the polished crystal fiber.

Figure 6.9 (a) shows the measured Cr4+ fluorescence spectrum and the 3-dB
bandwidth is 265 nm. The ASE power fluctuation is 0.4% within one hour as shown
in Fig. 6.9 (b). The calculated evolution of ASE power and upper level population
density along the crystal fiber at pump power of 4.41 W is shown in Fig. 6.10. It
shows that the backward ASE along the fiber grows up almost linearly while the
forward ASE begins to decrease at the end section. The reason for the forward ASE
drop may result from the propagation loss is larger than the ASE gain at the end
section.

84
Cr fluorescence intensity (a.u.)
500 58.4
58.3
400 Stability: 0.4%

ASE power (a.u.)

58.2
300 58.1
200 58.0
57.9
100
57.8
4+

0 57.7
1100 1200 1300 1400 1500 1600 1700 30 40 50 60 70 80 90
Wavelength (nm) Time (minutes)
(a) (b)

Fig. 6.9. ASE (a) fluorescence spectrum, and (b) power stability of the double-clad Cr4+:YAG
crystal fiber.

2.0 3.5

3.0
1.5
ASE power (mW)

N2 ( x 10 m )
2.5

-3
23
1.0 2.0

1.5
0.5 Forward ASE
Backward ASE 1.0
N2
0.0 0.5
0 10 20 30 40 50 60 70 80
Position along fiber (mm)
Fig. 6.10. Calculated ASE power and upper level population density along the length of
double-clad Cr4+:YAG crystal fiber.

We had measured the ASE power generated from single-crystal fiber,

borosilicate-clad crystal fiber, and double-clad crystal fiber with core diameters of
920 m, 100 m, and 25 m, respectively. The corresponding ASE power was
summarized in Table 6.1. Compared with the ASE power generated from different
core diameters, the magnitude of ASE intensity increases a factor of four orders from
core diameter of 920 m to 25 m. In addition, the parameters of simulated ASE
power for different core diameters were listed in Table 6.2. Therefore, our best-fit

85
 parameters for absorption, emission, and excited-state absorption cross section are
2210-19, 710-19, and 1.310-19 cm2, respectively. These values are compared with
other reported results and are shown in Table 6.3. According to the literature our
crystal fiber has large emission cross section compared with the average value in
literature while the absorption cross section is slight lower than the average value in
literature. Besides, the excited-state absorption cross section of our crystal fiber is also
lower than that in literature.

Table 6.1 ASE power generated from different core diameters.

Core diameter ASE power ASE intensity
(m) (mW) (W/m2)
Single-crystal fiber 920 0.172 2.59102
Borosilicate-clad crystal fiber 100 2.45 3.12105
Double-clad crystal fiber 25 2.36 4.81106

Table 6.2 Parameters of simulated ASE power.

Parameters Single-crystal fiber Single-clad fiber Double-clad fiber Unit
Pump wavelength, p 940 1064 1064 nm
Fiber length 15.77 46.6 81.4 mm
Core diameter 920 100 27 m
-1
Small signal absorption coefficient, 216 55 72 m
-1
Propagation loss, pl 13.8 13.8 32 m
2
Absorption cross section, a 2210-23 2210-23 2210-23 m
-3
Total ion density (NT= / a) 9.8181023 2.501023 3.2731023 m
Temperature 25 18 25 Deg.
Lifetime, f 4.3110-6 4.610-6 4.3110-6 Sec.
Emission bandwidth, 265 265 265 nm
fL 0.19 0.19 0.19 -
-23 -23 -23 2
Emission cross section, e 710 710 810 m
Refraction index (core, inner-clad) 1.82, 1 1.82, 1.474 1.82, 1.64 -
Numerical 1.52066 1.06758 0.78918 -
Allowed mode numbers 1.51107 88198.45 1927.835 -
Mode number, M 325.72 76.03 48.6 -

86
Table 6.3 Comparison of parameters of absorption, emission and excited-state
absorption cross section.
Reference a ( 10-19 cm2 ) e ( 10-19 cm2 ) esa ( 10-19 cm2 )
[6.1]1990 50 8 5
[6.2]1992 3.6
[6.3]1992 57 8
[6.4]1993 30 2
[6.5]1994 57 3.5
[6.6]1995 8.7 2.2
[6.7]1995 3.3
[6.8]1997 25 3
[4.8]1999 14 1.2
[6.9]1999 31 3.4 1.8
[6.10]2001 11.2 0.46 0.096
[6.11]2003 8 0.95
Mean 26.9 3.73 2.18
This work 22 7 1.3

With the parameters extracted from the ASE power of double-clad fiber
experiments, a simulation was performed to estimate the ASE for Cr4+:YAG with
higher small signal absorption coefficient. The simulation result is shown in Fig. 6.11.
It indicates that the calculated ASE power could be excess of 20 mW for a small
signal absorption coefficient of 4.5 cm-1 with a fiber length of 4 cm at an absorbed
pump power of 2.6 W.

25
= 2 cm , L=5 cm
-1

= 2.8 cm , L=5 cm
-1
20
ASE power (mW)

= 4.5 cm , L=4 cm
-1

15

10

0
0.0 0.5 1.0 1.5 2.0 2.5 3.0
Absorbed pump power (W)

Fig. 6.11. Calculated ASE power as a function of pump power for different small signal
absorption coefficients.

87
 If we want to obtain 100 mW of ASE power, the propagation loss should be
improved significantly. Figure 6.12 shows the calculated ASE power versus absorbed
pump power for two types of parameters. It indicates that the calculated ASE power
could be excess of 100 mW for a small signal absorption coefficient of 1.5 cm-1 with a
fiber length of 15 cm at an absorbed pump power of 2.4 W.

160
=4.5 cm , pl= 0.5 dB/cm, L=5 cm
-1
140
=1.5 cm , pl= 0.1 dB/cm, L=15 cm
-1

120
ASE power (mW)

100
80
60
40
20
0
0.0 0.5 1.0 1.5 2.0 2.5 3.0
Absorbed pump power (W)

Fig. 6.12. Calculated ASE power as a function of pump power for two types of parameters.

6.2 Double-clad crystal fiber amplifier

6.2.1 Fusion of a double-clad fiber with a single-mode fiber

In order to make the fiber amplifier experiment conveniently, a double-clad fiber
was spliced to a single-mode fiber (SMF) using Ericsson FSU 995 FA fusion splicer.
Then the double-clad fiber can connect to WDM coupler, tunable laser diode (LD) or
Yb fiber laser through single-mode fiber connectors. The experimental setup of
splicing double-clad fiber with a SMF is shown in Fig. 6.13. Since the diameter of the
double-clad fiber was larger than the SMF, auto mode of the splicer cannot be used to
find the core of double-clad fiber. A signal light with a wavelength of 1600 nm was
delivered into the SMF, and a detector measured the signal light from the other side of
double-clad fiber. Through moving the SMF, we can obtain the maximum of signal
power to align the SMF and the double-clad fiber. Then the splicing procedure was

88
 ran. Figure 6.14 shows the images of fusion on splicer screen. Because the splicer
cannot see the core of the double-clad fiber, the splice loss cannot be estimated after
fusion. To know the splice loss, an OLCR was used to measure the return loss
between the SMF and the double-clad fiber. The measured result is shown in Fig. 6.15
and the inset is the experimental setup.

Electrode
Double-clad fiber
SMF

=1600
nm Monitor area Detector

0 pixels 235 pixels 510 pixels

Fig. 6.13. Experimental setup of single-mode fiber/double-clad fiber splice.

Before fusion After fusion

SMF
Double-clad fiber
X-direction

Double-clad fiber
SMF
Y-direction

Fig. 6.14. Images of before and after fusions at two transverse directions on Ericsson FSU
995 FA screen.

89
 -30
1 Return loss=10log10(Reflectance)
OLCR
Return loss (dB) -40

-50
Double-clad fiber 2

-60 SMF
face 1 face 2

-70

-80
240 260 280 300 320 340 360 380
Distance (mm)
Fig. 6.15. Return loss at a fusion splice (face 1) and the end face of a double-clad fiber (face
2). The inset shows the experimental setup.

The measured return loss at face 1 is -35.7 dB as shown in Fig. 6.16 (a) however
the theoretical return loss at face 1 resulted in index difference is -19.17 dB
(Reflectance=1.21%). The measured return loss was lower than expected, which may
be caused by index gradient at the interface. Figure 6.16 (b) shows the return loss of
fiber-air interface (face 2). We can clearly see that the width of peak2 is wider than
the peak1 due to multimode dispersion in the double-clad fiber.

-30 -50
1 2
-40
-60
Return loss (dB)
Return loss (dB)

-50
-60 -70
-70
-80
-80
-90 -90
253.0 253.2 253.4 253.6 253.8 254.0 362 363 364 365 366 367
Distance (mm) Distance (mm)
(a) (b)

Fig. 6.16. The enlargement of Fig. 6.15 at (a) peak1 and (b) peak2.

90
 In addition, we also measured the insertion loss, IL, from SMF to double-clad
fiber after fusion. The experimental setup is shown in Fig. 6.17. A 980-nm laser was
sent into one side of the SMF, and a detector measured the laser power from the other
side. The laser input power, Pin, and output power, Pout, should follows

[ ]
Pout = (1 IL ) e
( )+ pl L
T Pin , (6.1)

where (), pl and L are the absorption coefficient, propagation loss and length of
double-clad fiber, respectively. T is the transmittance of double-clad fiber to the air.
is the coupling efficiency for the laser is coupled into the detector. Table 6.4 lists the
parameters for insertion loss calculation and the calculated insertion loss using Eq. 6.1
is 62.2% (-4.23 dB). In addition, we also measure the insertion loss tested by a signal
wavelength of 1600 nm. The insertion loss at the signal wavelength is -3.1 dB.
Therefore, less than half of light can enter the double-clad fiber when it transmitted
from SMF to double-clad fiber. To achieve lower insertion loss, the splicing procedure
should be optimized to reduce the splicing loss or the double-clad fiber should be
spliced to a thermally expanded core (TEC) fiber with a matched core.

Double-clad fiber
SMF
Pin Pout

Detector

Insertion loss Absorption and propagation loss

Fig. 6.17. Experimental setup of insertion loss measurement.

Table 6.4 The parameters for insertion loss calculation.

Pout Pin PL L T
0.0216 mW 19.73 mW 0.6 cm-1 0.345 cm-1 6.09 cm 91.54% 100%

6.2.2 Characterization of double-clad fiber amplifier

A 1064-nm Yb fiber laser was used as a pump source to test the optical gain of a
6-cm-long double-clad fiber at a wavelength of 1520 nm and the experimental setup is

91
shown in Fig. 6.18. The pump beam was combined with the signal beam through a
C-band WDM coupler. The output of the WDM coupler was spliced to the clad fiber
using an Ericsson FSU 995 FA fusion splicer. The output light from the clad fiber was
measured by a detector and an optical spectrum analyzer (HP 86142A).

Driver
Yb-fiber laser

Pump in FL=10 mm Detector

Collimator Splice

SMF Double-clad
1060/1550 Cr4+:YAG fiber Filter
WDM coupler

Tunable Laser Signal in

(1510~1640nm)

Fig. 6.18. Experimental setup of optical gain measurement.

Values of optical gain were determined by comparing the ratio of signal power
obtained with and without Yb fiber pumping. Account was taken of the contribution
from the ASE power. Therefore, the gain was defined as the following equation
[6.12-6.13]:

Ppump on Ppump on
signal on signal off

Gross gain (dB) = 10 log signal on (6.2)
Ppump off

Figure 6.19 (a) shows the measured result of gross gain, which shows that the
in
input signal saturation power, Psat , for the fiber is about -19.6 dBm at 1-W pump
power estimated by the following equation:

G0
Gross gain = (6.3)
1 + P in Psat
in

where G0 and Pin are the gain constant and the input signal power, respectively. When
the input signal power is -20 dBm, a gross gain of 10.0 dB was obtained at a pump
power of 0.83 W. Figure 6.19 (b) shows the signal spectra with and without pump
power. No spurious modes were observed in the vicinity of the signal.

92
 12
Input signal power = -20 dBm
10

Gross gain (dB)

8
-16 dBm
6
-13 dBm
4
-10 dBm

2 -6 dBm

0
0.0 0.2 0.4 0.6 0.8 1.0
Pump power (W)
(a)

1400
output signal w/o pump
1200 output signal w/ pump
Spectra density (a.u.)

1000
Gain = 10.0 dB
800
600
400
200
0
1519.8 1519.9 1520.0 1520.1
Wavelength (nm)
(b)

Fig. 6.19. (a) The gross gains at a wavelength of 1.52 m, (b) Cr4+-doped fiber amplifier
output spectra measured by an optical spectrum analyzer with 0.06-nm resolution.

Besides, the gross gains for different signal wavelengths were also measured as
shown in Fig. 6.20. At input signal wavelength and power were 1470 nm and -30 dBm,
a gross gain of 16 dB was obtained at a pump power of 1.16 W. Figure 6.21 shows a
comparison of the gain and ASE profile. From Figure 6.21 the bandwidth of
double-clad fiber amplifier could be estimated to be about 270 nm.

93
 16
-30 dBm
14 -20 dBm
12 -10 dBm
Gross gain (dB)
10
8
6
4
2
0
1470 1500 1530 1560 1590 1620 1650
Signal wavelength (nm)

Fig. 6.20. The gross gains as a function of the signal wavelength for different input signal
powers at pump power of 1.16 W.

20 30

ASE spectrum density (a.u.)

28
16
26
Gross gain (dB)

12 24

8 22
Gross gain
20
ASE spectrum
4
Input signal power = -30 dBm 18
0 16
1200 1300 1400 1500 1600
Wavelength (nm)

Fig. 6.21. Comparison of the gain and ASE profiles.

The noise of amplifier is also another important parameter, and it can be

quantified through its noise figure. The noise figure, NF, is defined as the ratio of the
signal to noise ratio (SNR) at the input of the amplifier to that at the output of the
amplifier:

94
 (SNR )in
NF (6.4)
(SNR )out
The noise figure will always be greater than one, due to the fact that the amplifier
adds noise during the amplification process. It has been shown that for an ideal
amplifier the quantum limit of the noise figure is 3 dB [6.14]. For high gain amplifier,
the noise figure always greater than 3 dB, and the minimum amplifier noise figure can
be given by [6.15]:

NF min ( p , s ) =
2
( ) a (s ) (6.5)
1 e p
a ( p ) e (s )
where p and s are the pump and the signal wavelength, respectively. e and a are
the emission and absorption cross sections, respectively. Assuming the emission and
absorption cross sections are proportional to Cr4+ fluorescence spectrum and
absorption coefficient of the Cr4+:YAG crystal fiber, the calculated result using Eq.
(6.5) is shown in Fig. 6.22. It shows the minimum noise figure is close to 3 dB at
signal wavelength from 1240 nm to 1610 nm when the pump wavelength is 1064 nm.
The inset shows the Cr4+ fluorescence spectrum and absorption coefficient of the
Cr4+:YAG crystal fiber.

5.5
3.0 12
Cr fluorescence spectrum (a.u.)

Absorption coefficient (cm )

-1

5.0 2.5 10
Min. noise figure (dB)

2.0 8

4.5 1.5 6

1.0 4
4.0 0.5 2
4+

0.0 0
600 800 1000 1200 1400 1600 1800
3.5 Wavelength (nm)

3.0
1100 1200 1300 1400 1500 1600 1700
Wavelength (nm)
Fig. 6.22. Calculated minimum noise figure of Cr:YAG fiber amplifier. The inset shows the
Cr4+ fluorescence spectrum and absorption coefficient of Cr4+:YAG crystal fiber.

95
 Chapter 7 Conclusions and future work

7.1 Conclusions
High-quality gradient-index Nd3+:YAG crystal fibers were successfully grown by
the LHPG technique. EPMA was adopted to measure the doping profile across the
fiber cross-section. Samples with different growth condition were measured. The
doping profile is basically affected by the ion diffusion, segregation at the solid/melt
interface, and the evaporation at the circumference. With proper control of the growth
condition, the doping concentration can be enhanced at the center of the
250-m-diameter fiber by 40% above that in the raw material. An OLCR was
employed to probe the index gradient and the measured result shows an index
difference of 0.0284 between the center and the edge of the crystal fiber. Using the
gradient-index fiber as a laser gain medium, the laser beam is confined in the central
region of the core, thus reduces the interface loss. A laser output power of 80 mW was
achieved with a slope efficiency of 28.9%, which, to our knowledge, is the highest
ever achieved for diode-laser-pumped Nd:YAG crystal fiber laser. The estimated M2
of laser beam was 1.19. Loss analysis indicates that the intracavity round-trip
distributed loss is about 15%. If the distributed loss can be eliminated, the slope
efficiency could be nearly doubled for the fiber laser.

Rate equation analysis was used to investigate the ASE power and laser
performance of the Cr4+:YAG gain media. The simulation result of ASE power
performance indicates that it is crucial to have a small core for higher ASE efficiency
and power. Because smaller core has higher pump power density, the ASE power can
significantly increase along the fiber with higher population density of upper level.
The ASE power could be in excess of 20 dBm for a 10-m-diameter core at a pump
power of 1.25 W. The simulation result of laser performance indicates that increasing
the small signal absorption coefficient, reducing the propagation loss and fiber core
diameter, the laser output power and slope efficiency can be significantly improved.

For an unclad crystal fiber the propagation loss increases with decreased fiber

96
diameter. This dependence, expected from a surface scattering mechanism, goes
approximately as a-1.5 (a=core radius) [7.1]. In addition, the LHPG technique is not
easy to grow small fiber diameter (<30 m). Therefore, we developed a new cladding
technique, CDLHPG, to reduce the propagation loss and core diameter. For
single-clad fiber, the borosilicate-clad fiber can produce a strong Cr4+ fluorescence in
the core area; however, the core diameter is very difficult to grow below 30 m.
Fused-silica-clad fiber with 29-m-core diameter was fabricated. The propagation
loss was less than 0.1 dB/cm, which is a factor of 7 smaller than that of an unclad
fiber, but it has almost no Cr4+ fluorescence in the core area due to the entering of
SiO2 in YAG. With proper controlled growth parameters of CDLHPG method to
prevent SiO2 from diffusing into the core center, we successfully grew a double-clad
fiber. The core, inner, and outer cladding diameters were 25 m, 100 m, and 320 m,
respectively. EPMA measured result showed that the compositions of core and outer
cladding were almost YAG and SiO2, respectively. But the compositions of the inner
cladding were mixtures of SiO2 and YAG. The average SiO2 concentration in the inner
cladding was 39.8 wt.%. HRTEM was adopted to measure the microstructure of
double-clad fiber. A SAD pattern of the core revealed that the core was a cubic
structure and the diffraction pattern was in (111) plane. The calculated lattice constant
was 1.2 nm, which is very close to that in the literature. Therefore, the core is a YAG
structure with a <111>-oriented cross-section. According to the HRTEM micrograph,
the crystalline nanostructures in the inner cladding were approximately 10 nm in
thickness and less than 15 nm in length, which were surrounded by a SiO2 amorphous
matrix. At this crystalline orientation the phase contrast allows to differentiate lattice
planes of ~0.29-nm separation. The diffraction pattern of outer cladding has a ring
pattern, which indicated that the outer cladding was an amorphous structure.

We had measured the ASE power generated from different core diameters, the
ASE intensity increases by four orders of magnitudes from core diameters of 920 m
to 25 m. In addition, the simulated parameters extracted from the ASE experiments
for different core diameters showed that our best-fit parameters for absorption,
emission, and excited-state absorption cross section were 2210-19, 710-19, and

97
1.310-19 cm2, respectively. According to the literature our crystal fiber has better
emission efficiency compared with the average value of emission cross section in
literature, while the absorption efficiency is slight lower than that in literature.
Besides, the excited-state absorption cross section of our crystal fiber was also lower.
In optical gain measurement of DCF, we had successfully demonstrated the first
transition metal-doped fiber amplifier in the optical fiber communication band. The
return loss and insertion loss at the single mode fiber and DCF were estimated to be
-35.7 dB and -3.1 dB, respectively. The coupling loss between the DCF and standard
SMF could be reduced if adiabatic tapering on the core diameter of SMF to match that
of the DCF and/or gradient index change between SMF and DCF are developed.
When the input signal wavelength and power are 1470 nm and -30 dBm, respectively,
a gross gain of 16 dB is obtained at a pump power of 1.16 W. From a comparison of
gross gains and ASE spectrum, the bandwidth of double-clad fiber amplifier could be
estimated to be about 270 nm. This wideband chromium-doped fiber amplifier has
great potential to be employed in the whole 1.31.6-m range.

7.2 Future work

Nd:YAG lasers have three main lasing wavelengths, i.e. 1064 nm, 946 nm, and
1319 nm, which can generate red (659.5 nm), green (532 nm), and blue (473 nm) after
frequency doubling. Periodically-poled LiNbO3 (PPLN) is suitable for frequency
doubling material and can be grown by the LHPG method as well with different
domain periods to meet the quasi-phase matching conditions across the visible
wavelengths [7.2]. Combining the laser diodes, Nd:YAG crystal fiber lasers, and
PPLN crystal fibers, a compact RGB lasers can be achieved as shown in Fig. 7.1.

PPLN crystal fiber

Blue laser

LD array Green laser

Red laser
Nd:YAG crystal fiber

Fig. 7.1. A schematic diagram of a compact RGB lasers.

98
 It is needed for large-screen color projection display systems and can be used in
high-density storage systems.

From the ASE simulation of Cr4+:YAG crystal fiber, increasing the absorption
coefficient, reducing the propagation loss and core diameter are important to obtain
higher ASE efficiency. Due to the out-diffusion and evaporation of Cr2O3 during the
crystal fiber growth, the Cr4+ concentration decreases substantially, and results in
decreased absorption coefficient. To increasing the absorption coefficient we can try
to enhancement of Cr4+ concentration by E-gun deposition of CaO and Cr2O3 on the
circumference of the Cr4+:YAG source rod followed by re-growth. To reduce the
propagation loss, the refraction index difference between core and inner cladding
should be reduced. From the refraction index measurement, the index profile of the
inner cladding is from 1.66 to 1.58, corresponding to the SiO2 concentrations from 30
to 50 wt.%. Therefore, we may find proper growth condition to reduce the SiO2
concentration in the inner cladding and obtain small index difference between core
and inner cladding. To reduce the core diameter, the CO2 power variation should be
small. For DCF, the core diameter variation is about 4% over a 1-cm length of the
fiber when the CO2 power variation was less than 0.25%. Therefore, we may use a
sapphire tube as a heat capacity to stabilize the heat power for better uniformity of the
core diameter. If the core diameter of DCF is close to the core diameter of SMF, the
coupling loss between DCF and SMF will be improved after fusion. Finally, if the
power conversion efficiency of ASE can go up to 10%, DCF will have a great impact
in wideband light source, optical amplifier, and laser applications.

99
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Reflectometry, Applied Physics Letters 73, 3342 (1998).

Chapter 4
[4.1] Y. Chang, Ultrashort Optical Pulse Generation from a Cr4+-doped Yttrium
Aluminium Garnet Tunable Solid-state Laser, Ph. D. Dissertation, Universit de
Montral, Quebec, Canada, (1999).
[4.2] H. Eilers, W. M. Dennis, W. M. Yen, S. Kck, K. Peterman, G. Huber, and W. Jia,
Performance of a Cr:YAG Laser, IEEE Journal of Quantum Electronics 29, 2508
(1993).
[4.3] W. Jia, Near-infrared Luminescence in Cr, Ca-Doped Yttrium Aluminum Garnet,
OSA Proceedings on Advanced Solid-State Lasers 10, 87 (1991).
[4.4] S. A. Markgraf, M. F. Pangborn, and R. Dieckmann, Influence of Different
Divalent Co-dopants on the Cr4+ Content of Cr-doped Y3Al5O12, Journal of Crystal
Growth 180, 81 (1997).
[4.5] B. M. Tissue, W. Jia, L. Lu, and W. M. Yen, Coloration of Chromium-doped
Yttrium Aluminum Garnet Single-crystal Fibers Using a Divalent Codopant,
Journal of Applied Physics 70, 3775 (1991).
[4.6] A. Sugimoto, Y. Nobe, and K. Yamagishi, Crystal Growth and Optical
Characterization of Cr,Ca:Y3Al5O12, Journal of Crystal Growth 140, 349 (1994).

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[4.7] A. Sennaroglu, Analysis and Optimization of Lifetime Thermal Loading in
Continuous-wave Cr4+-doped Solid-state Lasers, Journal of the Optical Society of
America. B 18, 1578 (2001).
[4.8] A. Suda, A. Kadoi, K. Nagasaka, H. Tashiro, and K. Midorikawa, Absorption and
Oscillation Characteristics of a Pulsed Cr4+:YAG Laser Investigated by a
Double-Pulse Pumping Technique, IEEE Journal of Quantum Electronics 35, 1548
(1999).
[4.9] P. C. Becker, N. A. Olsson, and J. R. Simpson, Erbium-Doped Fiber Amplifiers:
Fundamentals and Technology (Academic, San Diego, Calif., 1999).
[4.10] A. Sennaroglu, Continuous Wave Thermal Loading in Saturable Absorbers: Theory
and Experiment, Applied Optics 36, 9528 (1997).
[4.11] C. W. Wang, Y. L. Weng, P. L. Huang, H. Z. Cheng, and S. L. Huang, Passively
Q-switched Quasi-three-level Laser and Its Intracavity Frequency Doubling,
Applied Optics 41, 1075 (2002).

Chapter 5
[5.1] D. Jun, D. Peizhen, and X. Jun, The Growth of Cr4+, Yb3+:Yttrium Aluminum
Garnet (YAG) Crystal and Its Absorption Spectra Properties, Journal of Crystal
Growth 203, 163 (1999).
[5.2] B. Cockayne, Developments in Melt-grown Oxide Crystals, Journal of Crystal
Growth 3, 4, 60 (1968).
[5.3] www.udel.edu/chem/GlassShop/
[5.4] www.hoben.co.uk/industrialcasting/
[5.5] www.sciner.com/Opticsland/
[5.6] Li-ping You, C. L. Heng, S. Y. Ma, Z. C. Ma, W. H. Zong, Zheng-long Wu, and G.
G. Qin, Precipitation and Crystallization of Nanometer Si Clusters in Annealed
Si-rich SiO2 Films, Journal of Crystal Growth 212, 109 (2000).
[5.7] O. Conde, A. G. Rolo, M. J. M. Gomes, C. Ricolleau, and D. J. Barber, HRTEM
and GIXD Studies of CdS Nanocrystals Embedded in Al2O3 Films Produced by
Magnetron RF-sputtering, Journal of Crystal Growth 247, 371 (2003).
[5.8] Y. J. Bai, Z. G. Liu, X. G. Xu, D. L. Cui, X. P. Hao, X. Feng, and Q. L. Wang,
Precipitation of InN Nanocrystals by Solvo-thermal Method, Journal of Crystal
Growth 241, 189 (2002).

105
[5.9] Z. Sun, D. Yuan, X. Duan, X. Wei, H. Sun, C. Luan, Z. Wang, X. Shi, D. Xu, and
M. Lv, Preparation and Characterization of Co2+-doped Y3Al5O12 Nano-crystal
Powders by Sol-gel Technique, Journal of Crystal Growth 260, 171 (2004).
[5.10] F. Yun, B. J. Hinds, S. Hatatani, S. Oda, Q. X. Zhao, and M. Willander, Study of
Structural and Optical Properties of Nanocrystalline Silicon Embedded in SiO2,
Thin Solid Films 375, 137 (2000).
[5.11] W. T. Young, L. K. L. Falk, H. Lemercier, V. Peltier-Baron, Y. Menke, and S.
Hampshire, The Crystallization of the Yttrium-sialon Glass:
Y15.2Si14.7Al18.7O54.1N7.4, Journal of Non-Crystalline Solids 270, 6 (2000).
[5.12] L. Kepinski, D. Hreniak, and W. Strek, Microstructure and Luminescence
Properties of Nanocrystalline Cerium Silicates, Journal of Alloys and Compounds
341, 203 (2002).
[5.13] P. Mutti, G. Ghislotti, S. Bertoni, L. Bonoldi, G. F. Cerofolini, L. Meda, E. Grilli,
and M. Guzzi, Room-temperature Visible Luminescence from Nanocrystals in
Silicon Implanted SiO2 Layers, Applied Physics Letters 66, 851 (1995).
[5.14] M. Aparicio, R. Moreno, and A. Duran, Colloidal Stability and Sintering of
Yttria-silica and Yttria-silica-alumina Aqueous Suspensions, Journal of European
Ceramic Society 19, 1717 (1999).
[5.15] K. Sato, T. Izumi, M. Iwase, Y. Show, H. Morisaki, T. Yaguchi, and T. Kamino,
Nucleation and Growth of Nanocrystalline Silicon Studied by TEM, XPS and
ESR, Applied Surface Science 216, 376 (2003).
[5.16] A. M. Tonejc, I. Djerdj, and A. Tonejc, Evidence from HRTEM Image Processing,
XRD and EDS on Nanocrystalline Iron-doped Titanium Oxide Powders, Materials
Science and Engineering: B 85, 55 (2001).
[5.17] L. Kepinski, and M. Wolcyrz, Nanocrystalline Rare Earth Silicates: Structure and
Properties, Materials Chemistry and Physics 81, 396 (2003).
[5.18] J. Dutkiewicz, L. Stoch, J. Morgiel, G. Kostorz, and P. Stoch, Analytical and
HREM Study of the Early Stages of SiO2-Al2O3-(Mg, Zn)O Glass Crystallisation,
Materials Chemistry and Physics 81, 411 (2003).

Chapter 6
[6.1] N. I. Borodin, V. A. Zhitnyuk, A. G. Okhrimchuk, and A. V. Shestakov, Oscillation
of a Y3Al5O12:Cr4+ Laser in Wavelength Region of 1.34-1.6 m, Bulletin of the

106
 Academy of Sciences of the USSR, Physical series 54, 54 (1990).
[6.2] I. J. Miller, A. J. Alcock, and J. E. Bernard, Experimental Investigation of Cr4+ in
YAG as a Passive Q-switch, OSA Proceedings on Advanced Solid-State Lasers 13,
322 (1992).
[6.3] H. Eilers, K. R. Hoffman, W. M. Dennis, S. M. Jacobsen, and W. M. Yen,
Saturation of 1.064 m Absorption in Cr,Ca:Y3Al5O12 Crystals, Applied Physics
Letters 61, 2958 (1992).
[6.4] K. Spariosu, W. Chen, R. Stultz, M. Birnbaum, and A. V. Shestakov, Dual Q
Switching and Laser Action at 1.06 and 1.44 m in a Nd3+:YAG-Cr4+:YAG
Oscillator at 300 K, Optics Letters 18, 814 (1993).
[6.5] H. Eilers, U. Hmmerich, S. M. Jacobsen, W. M. Yen, K. R. Hoffman, and W. Jia,
Spectroscopy and Dynamics of Cr4+:YAG, Physical Review B 49, 15505 (1994).
[6.6] Y. Shimony, Z. Burshtein, and Y. Kalisky, Cr4+:YAG as Passive Q-switch and
Brewster Plate in a Pulsed Nd:YAG Laser, IEEE Journal of Quantum Electronics
31, 1738 (1995).
[6.7] S. Kck, K. Petermann, U. Pholmann, and G. Huber, Near-infrared Emission of
Cr4+-doped garnets: Lifetimes, Quantum Efficiencies, and Emission Cross Sections,
Physical Review B 51, 17323 (1995).
[6.8] S. Camacho-Lopez, R. P. M. Green, G. J. Crofts, and M. J. Damzen, 4+
Intensity-induced Birefringence in Cr:YAG, Journal of Modern Optics 44, 209
(1997).
[6.9] J. C. Diettrich, I. T. McKinnie, and D. M. Warrington, The Influence of Active Ion
Concentration and Crystal Parameters on Pulsed Cr:YAG Laser Performance,
Optics Communications 167, 133 (1999).
[6.10] A. Sennaroglu, Optimization of Power Performance in Room-temperature
Continuous-wave Cr4+:YAG Lasers, Optics Communications 192, 83 (2001).
[6.11] R. Feldman, Y. Shimony, and Z. Burshtein, Dynamics of Chromium Ion Valence
Transformations in Cr, Ca:YAG Crystals Used as Laser Gain and Passive
Q-switching Media, Optical Materials 24, 333 (2003).
[6.12] G. M. Davis, I. Yokohama, S. Sudo, and K. Kubodera, 1.3-m Nd:YAG Crystal
Fiber Amplifiers, IEEE Photonics Technology Letters 3, 459 (1991).
[6.13] C. J. Koester and E. Snitzer, Amplification in a Fiber Laser, Applied Optics 3,
1182 (1964).

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[6.14] G. P. Agrawal, Fiber-Optic Communication Systems (John Wiley & Sons, Inc., New
York, 1997).
[6.15] A. M. Emara, Y. M. Zakaria, M. H. Aly, A. M. Okaz, and M. S. Abou-EI-Wafa,
Noise Figure and Gain Coefficient of Doped Fiber Amplifiers for Different Host
Materials, Eighteen National Radio Science Conference, 577 (2001).

Chapter 7
[7.1] M. M. Fejer, Single Crystal Fiber: Growth Dynamics and Nonlinear Optical
Interations, Ph. D. Dissertation, Stanford University, Stanford, CA (1986).
[7.2] D. H. Jundt, Lithium Niobate: Single Crystal Fiber Growth and Quasi-
phase-matching, Ph. D. Dissertation, Stanford University, Stanford, CA (1986).

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 Biography

: (Lo, Chia-Yao)

: 65 8 30

: (1991.9~1994.6)

(1994.9~1998.6)

(1998.9~1999.6)

(1999.9~2005.1)

2001 (OPT)

2000 International Photonics Conference

Growth, Characterization, and Applications of Doped-YAG

Single-crystal Fibers

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 Publication List

I. SCI listed paper:

1. C. Y. Lo, K. Y. Huang, J. C. Cheng, C. Y. Chuang, C. C. Lai, S. L. Huang, Y. S. Lin,
and P. S. Yeh, Double-clad Cr4+:YAG Crystal Fiber Amplifier, to appear in Optics
Letters, January (2005).
2. J. C. Chen, C. Y. Lo, K. Y. Huang, F. J. Kao, S. Y. Tu, and S. L. Huang,
Fluorescence Mapping of Oxidation States of Cr Ions in YAG Crystal Fibers, to
appear in Journal of Crystal Growth.
3. C. Y. Lo, K. Y. Huang, J. C. Cheng, S. Y. Tu, and S. L. Huang, Glass-clad
Cr4+:YAG Crystal Fiber for the Generation of Superwideband Amplified Spontaneous
Emission, Optics Letters, 29, 439 (2004).
4. C. Y. Lo, P. L. Huang, T. S. Chou, L. M. Lee, T. Y. Chang, S. L. Huang, L. Lin, and
F. C. Ho, Efficient Nd:Y3Al5O12 Crystal Fiber Laser, Japanese Journal of Applied
Physics 41, L1228 (2002).

II. Invited paper

1. S. L. Huang, C. Y. Lo, K. Y. Huang, J. C. Cheng, P. L. Huang, and L. M. Lee,
Glass-clad Cr4+:YAG Crystal Fiber for the Generation of Super-wideband Amplified
Spontaneous Emission, International Symposium on Advances and Trends in Fiber
Optics and Applications, Chongqing, China (2004).
2. S. L. Huang, C. Y. Lo, L. M. Lee, K. Y. Huang, and J. C. Chen, Crystal Fiber
Devices for Super Wideband Optical Communication, Taiwan-Japan
Optoelectronics Workshop, Tainan, Taiwan (2003).
3. C. Y. Lo, L. M. Lee, S. Y. Tu, K. Y. Huang, Y. C. Cho, and S. L. Huang, Crystal
Fiber Devices for Optical Fiber Communications, Japan-Taiwan Joint Symposium
on Nanophotonics Technology, Osaka, Japan (2002).
4. C. Y. Lo, L. M. Lee, T. S. Chou, C. C. Lin, and S. L. Huang, Crystal Fiber Devices
for Laser and Nonlinear Frequency Conversion, ROC-Lithuania Bilateral
Conference on Optoelectronics and Magnetic Materials, Taipei, Taiwan (2002).

110
III. International conference paper
1. S. L. Huang, C. Y. Lo, K. Y. Huang, J. C. Cheng, C. Y. Chuang, C. C. Lai, Y. S. Lin
and P. S. Yeh, Broadband Cr4+:YAG Crystal Fiber Amplifier, Nonlinear Optics:
Material, Fundamental, and Applications, postdeadline paper ThD3, Hawaii, USA
(2004).
2. C. Y. Lo, K. Y. Huang, J. C. Cheng, C. Y. Chuang, and S. L. Huang,
Super-wideband Amplified Spontaneous Emission Generated by Double-clad
Cr4+:YAG Crystal Fiber, Conference on Lasers and Electro-Optics, paper CTuS7,
San Francisco, California, USA (2004).
3. J. C. Cheng, C. Y. Lo, K. Y. Huang, C. C. Li, P. L. Huang, Y. H. Lin, F. J. Kao, S. L.
Huang, and Y. S. Lin, Mapping of Cr Ions and Refraction Index Profile in Cr:YAG
Crystal Fiber with Double-cladding Structure, Conference on Lasers and
Electro-Optics, paper CTuU7, San Francisco, California, USA (2004).
4. C. Y. Lo, S. Y. Tu, K. Y. Huang, and S. L. Huang, Fused-silica-clad Cr:YAG
Fiber, The 5Th Pacific Rim Conference on Lasers and Electro-Optics, paper
TH4H-(7)-5, Taipei, Taiwan (2003).
5. J. C. Chen, C. Y. Lo, S. L. Huang, and F. J. Kao, The Use of Fluorescence Confocal
Microscopy in Mapping Cr3+ Profile within the YAG Crystal Fiber, The 5Th Pacific
Rim Conference on Lasers and Electro-Optics, paper F2H-(7)-4, Taipei, Taiwan
(2003).
6. C. Y. Lo, K. Y. Huang, S. Y. Tu, and S. L. Huang, 280-nm Amplified Spontaneous
Emission Generated by Cr4+:YAG Crystal Fiber, Conference on Lasers and
Electro-Optics, paper CWA55, Baltimore, Maryland, USA (2003).
7. J. C. Chen, C. Y. Lo, S. L. Huang, and F. J. Kao, Mapping of Cr Ion Profile in
Cr:YAG Crystal Fiber by Confocal Microscopy, Conference on Lasers and
Electro-Optics, paper CWQ2, Baltimore, Maryland, USA (2003).
8. P. L. Huang, Y. J. Lu, J. Y. Yi, C. Y. Lo, and S. L. Huang, High Doping Gradient
Nd:YAG Crystal Fiber, Conference on Lasers and Electro-Optics, paper CWA2,
Baltimore, Maryland, USA (2003).
9. K. Y. Huang, C. Y. Lo, S. Y. Tu, S. L. Huang, and P. S. Yeh, Diode Array Directly
Pumped Cr:YAG Crystal Fiber Broadband Light Source, Advanced Solid-State
Photonics, paper TuB12, Texas, USA (2003).
10. C. Y. Lo, T. S. Chou, P. L. Huang, L. M. Lee, and S. L. Huang, High-efficient
Nd:YAG Crystal Fiber Laser, Conference on Lasers and Electro-Optics, paper
CTuP6, Long Beach, California, USA (2002).

111
11. C. Y. Lo, T. S. Chou, L. M. Lee, P. L. Huang, S. L. Huang, and Y. J. Huo,
Gradient-index Nd:YAG Crystal Fiber Laser, Advanced Solid-State Lasers, paper
MB-19, Quebec City, Canada (2002).
12. C. Y. Lo, L. M. Lee, C. Y. Tai, and S. L. Huang, Growth and Characterization of
Gradient Index Laser Crystal Fibers, International Photonics Conference, paper
Th-T3-P001, Hsinchu, Taiwan (2000).

IV. Domestic conference paper

1. C. Y. Lo, K. Y. Huang, J. C. Cheng, C. N. Tsai, C. C. Lai, S. L. Huang, and Y. S.
Lin, Wideband Chromium-doped Fiber Amplifier, Symposium on Technologies for
High-Capacity Optical Communications, paper FRI-2, Kaohsiung, Taiwan (2004).
2. J. C. Cheng, C. Y. Lo, K. Y. Huang, P. L. Huang, Y. H. Lin, F. J. Kao, and S. L.
Huang, Mapping of Cr Ions Profile in Cr:YAG Crystal Fiber with Double-cladding
Structure, Optics and Photonics Taiwan03, paper FH1-1, Taipei, Taiwan (2003).
3. K. Y. Huang, C. Y. Lo, S. Y. Tu, and S. L. Huang, Super-wideband ASE Light
Source Generated by Cr:YAG Crystal Fiber, Optics and Photonics Taiwan02, paper
TG2-2, Taipei, Taiwan (2002).
4. J. C. Chen, C. Y. Lo, S. L. Huang, and F. J. Kao, Mapping of Cr Ion Profile in
Cr:YAG Crystal Fiber by Confocal Microscopy, Optics and Photonics Taiwan02,
paper FA3-5, Taipei, Taiwan (2002).
5. L. M. Lee, Y. C. Cho, C. J. Lin, C. Y. Lo, and S. L. Huang, The Study and
Fabrication of Periodically-poled Lithium Niobate Crystal Fiber, Optics and
Photonics Taiwan02, paper FF1-5, Taipei, Taiwan (2002).
6. C. Y. Lo, T. S. Chou, P. L. Huang, L. M. Lee, S. L. Huang, L. Lin, C. S. Chang, H.
Y. Lin, and F. C. Ho, Diode Laser Pumped Crystal Fiber Lasers with Gradient-index
Profile, Optics and Photonics Taiwan01, paper TD2-2, Kaohsiung, Taiwan (2001).

112