Introduction to

X-ray Diffraction
Basic principles and techniques
of X-ray powder diffraction

1
 Outline
A.M.10:00~11:45
Part I: Basis of X-ray diffraction
1. Properties of X-rays
2. Crystal Lattice, Lattice plane and Plane indices
3. X-ray Diffraction Measurement

Part II: Experimental

1. Crystallographic Information from XRD
2. Instrumentation
A.M.13:15~16:00
how to measure using XRD instrument
(SmartLab system)

2
 Part I.
Basis of X-ray Diffraction
Part I. Basis of X-ray Diffraction

1. Properties of X-rays

4
 What are X-rays?
 X-rays are a form of the electromagnetic radiation with
wavelength of 0.01 to 100 Å.

Ultraviolet rays
Far ultraviolet

infrared rays

infrared rays

Short waves

Long waves
Microwaves
Visible rays

Ultra short
X-rays

X-rays
Hard

Soft

waves
γ rays

Near
rays

Far
10-2 1 102 104 106 108 1010 1012 (Å)

10-3 10-1 101 103 105 107 109 1011 (nm)

X-rays were discovered in 1895 by

Wilhelm Conrad Röntgen.

5
 Generation of X-rays
 X-rays are generated when electrons, accelerated by
high-voltage electric field, strike the anode target.
High Vacuum
filament X-ray target (Cu)

electron
‐ +
High voltage
 Most of energy of the electrons is lost as heat. Only a
small percentage of energy is converted to X-rays.
Efficiency of X-ray generation ε = 1.1×10-9ZV （Cu 0.1％）
Z： Atomic number of target element V： accelerating voltage(V)

6
 Wavelength distribution of X-rays
 Characteristic X-rays and continuous X-rays
Example of wavelength distribution Characteristic X-rays
of X-rays generated by Mo target • Characteristic X-rays have
specific wavelengths inherent to
the element of the target.
Intensity (a.u.)

X-ray diffraction

Continuous X-rays
• Continuous X-rays have
continuous wavelength
distribution
• Total intensity is strong
X-ray fluorescence
Wavelength (Å) X-ray imaging

7
 Generation of characteristic X-rays
Characteristic X-rays are emitted from the element when
its outer-shell electrons make transitions between the
atomic energy levels.
M shell Kb (20～30) 8
L shell MⅡor Ⅲ 7
Kb
LⅡ：Ka2 (50) Ka
K shell 6

Intensity
La 5

Nucleus 4

Ka 3
LⅢ：Ka1 (100) 2
Mo

L shell electron Eka1= Ek - EL3 1

Scheme of an atom K shell electron00.3 0.5 0.7 0.9

of target material Wavelength (Å)
Excitation state 8
8
 Properties of characteristic X-rays
 Wavelengths of characteristic X-rays are inherent to the
element of the target.
 Characteristic X-rays need more than excitation voltage
 The excitation voltage depends on the element of the target and
the electron shell (K, L, M and so on.)
 Intensity ratios of Kα1 : Kα2 : Kβ = 10 : 5 : 2
 Ka radiation (a couple of Ka1 and Ka2) or Kα1 radiation is usually
employed in laboratory X-ray diffraction experiments.
Target Wavelength(Å) Excitation
Element Atomic No. Kα 1 Kα 2 Kβ Voltage
Cr 24 2.294 2.26 2.085 6.0 kV
Fe 26 1.94 1.936 1.757 7.1 kV
Co 27 1.793 1.789 1.621 7.7 kV
Cu 29 1.544 1.541 1.392 8.9 kV
Mo 42 0.714 0.709 0.632 20.0 kV
9
 Interaction of X-rays with matter
When X-rays pass through any form of matter, they are
partly absorbed and partly transmitted.
Scattered X-rays
（Compton scattering・ Thomson scattering）

Fluorescent X-rays
(True absorption)
X-ray I0 I
tube
Incident X-rays Transmitted X-rays

Electron
(Total absorption)
Heat
10
Absorption & Absorption Coefficient
When X-rays pass through a material with thickness of
x cm, the intensity of the X-rays decreases from I0 to I.

𝐼 = 𝐼0 exp(−𝜇𝑥) Beer-Lambert formula

−𝜇𝑥 = ln(𝐼 𝐼0 )

𝐼0 𝐼
x cm

𝜇: linear absorption coefficient (cm-1) 𝜇 =𝜇 𝜌×𝜌

𝜇 𝜌: mass absorption coefficient (cm2 /g )
𝜌: density(g/cm3)
11
 Absorption Curve (Absorption edge)
 Absorption rate of X-rays varies with wavelength

Pt absorption curve
Absorption coefficient (cm2 / g)

LI absorption edge
LII absorption edge
200

100
LIII absorption edge
K absorption edge

0.5 1.0
Wavelength (Å)
The wavelength is an appropriate for
excitation energy of K electron shell
12
 Mass Absorption Coefficient
 Mass absorption coefficients (cm2/g) are largely different
between the Kα and Kβ radiations. The Kβ filter utilizes
this difference for monochromatization.
Mo Cu Co Cr
Kβ Kα Kβ Kα Kβ Kα Kβ Kα
Ti 16.8 23.4 152 200 227 291 444 590
V 18.7 26 166 219 250 325 479 74.7
Cr 21.5 29.9 185 247 293 408 67 86.8
Mn 23.8 33.1 207 270 306 393 75.3 97.5
Fe 27.1 37.6 232 302 342 57.2 86.9 113
Co 29.6 41 248 321 48.1 63.2 96 124
Ni 34 46.9 279 48.8 56 73.5 112 144
Cu 35.7 49.1 39.2 51.8 59.4 78 118 153
(International Tables for X-ray Crystallography C)
13
 Generation of Fluorescent X-rays
Photoelectric effect Fluorescent X-rays are generated
when the energy of an X-ray photon is absorbed by kicking out
a K-shell electron and one of outer orbital electrons falls down
into the vacancy of the K-shell.  True absorption of X-rays
Fluorescent X-rays
(Characteristic X-rays of Fe)

X-ray photon
Photoelectron
K-shell
Fe
Nucleus
L-shell

Scheme in the case of iron

atom in the sample
14
Part I. Basis of X-ray Diffraction

2. Crystal Lattice, Lattice Plane

and Plane Indices

15
 Crystal and Structural Unit
 Crystal is characterized with the periodic arrangement of
atoms, ions or molecules in the three-dimension.
 Basic unit of this repetition is called “unit cell”.
 Eight corners of the unit cell are called “lattice points”.

Lattice point

Lattice

Unit cell
Unit cell

16
 Crystal Lattice
 The periodic arrangement of lattice points in space is
called “crystal lattice”, “space lattice” or merely “lattice”.
 The crystal lattice has several types.
Lattice point

Primitive lattice(P) Face-centered Base-centered Body-centered

lattice(F) lattice(A,B,C) lattice(I)

Non-primitive lattice
17
 Lattice Constants
 Size and shape of the unit cell (or lattice) can be defined
with three axis lengths, a, b, c, and three angles, a, b, g,
between them, in general.
 These parameters are called “lattice constants”, “lattice
parameters” or “unit-cell parameters”.
c

The axis lengths range from

a few to a few ten Å.
b Lattice constants can be
a determined by X-ray
b diffraction technique.
g
a
18
 Seven Crystal Systems
 According to the relationship among the lattice
constants, the crystal lattice can be classified into seven
crystal systems.
Crystal system Axial setting Relationship in unit-cell parameters

Triclinic system 𝑎 ≠ 𝑏 ≠ 𝑐, 𝛼 ≠ 𝛽 ≠ 𝛾 ≠ 90°

1st setting 𝑎 ≠ 𝑏 ≠ 𝑐, 𝛼 = 𝛽 = 90, 𝛾 ≠ 90°
Monoclinic system
2nd setting 𝑎 ≠ 𝑏 ≠ 𝑐, 𝛼 = 𝛾 = 90°, 𝛽 ≠ 90°
Orthorhombic system 𝑎 ≠ 𝑏 ≠ 𝑐, 𝛼 = 𝛽 = 𝛾 = 90°

Tetragonal system 𝑎 = 𝑏 ≠ 𝑐, 𝛼 = 𝛽 = 𝛾 = 90°

Rhombohedral axes 𝑎 = 𝑏 = 𝑐, 𝛼 = 𝛽 = 𝛾 < 120° ≠ 90°
Trigonal system
Hexagonal axes 𝑎 = 𝑏 ≠ 𝑐, 𝛼 = 𝛽 = 90°, 𝛾 = 120°
Hexagonal system 𝑎 = 𝑏 ≠ 𝑐, 𝛼 = 𝛽 = 90°, 𝛾 = 120°

Cubic system 𝑎 = 𝑏 = 𝑐, 𝛼 = 𝛽 = 𝛾 = 90° 19

 The 14 Bravais Lattices
 The 14 Bravais lattices can be derived by combining 7
crystal systems for the primitive lattice and lattice types.
Triclinic Tetragonal

P
Primitive P I
Primitive Body centered

Monoclinic Trigonal Hexagonal

P C P/R P
Primitive Base centered Primitive/Rhombohedral Primitive

Orthorhombic Cubic

P I F C P I F
Primitive Body centered Face centered Base centered Primitive Body centered Face centered 20
 Why not 7x4 Bravais Lattices?
Example)
Base-centered tetragonal cell has the same array as
that of the simple tetragonal cell with a smaller unit-cell.

Base-centered Primitive
tetragonal cell tetragonal cell

⇒ The crystal lattices are classified into 14 types called

Bravais lattices.
21
 Lattice plane and lattice spacing
 Plane that passes through all lattice points is called
“lattice plane”.
 The distance between the adjacent two lattice planes is
called “lattice spacing” or “d-spacing”.

Lattice spacing

Lattice plane

22
 Miller indices
 The lattice plane can uniquely be defined with three
integers hkl.
 These integers are called “plane indices” or “Miller
indices”, and they are expressed by enclosing them by
parenthesis as (hkl).

c/l
b/k

a/h

23
 Examples of Miller indices
(hkl) : Miller indices
c {111} c c {hkl } : Plane group
1/1 1/∞ 1/∞

b 1/1 b 1/1 b
1/1
1/1 1/1
1/∞
(111) (110) (010)
c c

b b
___
a (111) a (020)
24
Miller indices and observed data
c

25
 Miller indices, lattice spacing and
lattice constant
 The lattice spacing and lattice constant d of a certain plane
is calculated by lattice constants and Miller indices (hkl) by
the following formula.

Cubic

Tetragonal

Orthorhombic

Rhombohedral

Hexagonal

Monoclinic

Triclinic

26
Part I. Basis of X-ray Diffraction

3. X-ray Diffraction Measurement

27
 X-ray Diffraction and Bragg’s Law
 X-ray diffraction occurs when the Bragg’s law holds.
 The angle qB is called the Bragg angle. Bragg’s Law

Characteristic X-ray CuKα 1.5418Å

2d sinqB =l
Wavelength l
CuKα1 1.5406Å d is calculated from
→high resolution 2θ angle.

Intensity
q q

Lattice spacing d
(1~10Å)

2λ Kα1+λ Kα2
λKα =
3 Diffraction angle
28
 Powder X-ray Diffraction Pattern
 The X-rays which enter into the sample are diffracted
along the cones with cone angles of 2qB.
 So-called powder X-ray diffraction (PXRD) pattern is
observed. 2θ
2θ

2q
Incident X-ray I

sample

Debye rings 29
 Measurement with q-2q Scan Mode
 In q-2q scan mode, the incident and diffracted angles are
kept identical against the specimen surface.
 So the crystal planes parallel to the specimen surfaces
are always concerned with X-ray diffraction.

Incident X-ray Detector

θ 2θ

2θ (˚)

30
Reflection and Transmission Modes
 In reflection mode, X-rays reflected on the specimen
surface are measured with a detector.
 In transmission mode, X-rays transmitted through the
specimen are measured.
Detector Detector

2θ 2θ
Specimen Specimen

Reflection mode Transmission mode

31
 Part II.
Experimental
Part II. Experimental

1. Crystallographic Information
from XRD

33
High Quantitativity of XRD Technique
 X-ray diffraction (XRD) technique can elucidate the
three-dimensional structure of crystal.
 It can determine the positions of atoms in the unit-cell at
the accuracy in the order of 10-4 nm.

 Axis length of unit cell is 5.64Å

34
 States of Matters
 Crystalline solid is characterized with periodic
arrangement of atoms

Gas Liquid or amorphous Crystal

35
 States of Matters and XRD Patterns
 X-ray diffraction/scattering patterns clearly elucidate the
states of matters.
1500

1000 Crystal
Intensity (cps)

500 Amorphous or liquid

Gas
0
5 10 15 20 25 30 35 40
2θ (˚)
36
Angular range of XRD Measurement
 XRD pattern is usually measured in a wide 2q -range.
 Small-angle X-ray scattering (SAXS) give different
structural information.
10000

Angular range of XRD measurement (about 2 ˚ < 2θ)

1000
Intensity (cps)

100

10

Angular range of SAXS (2θ = 0.1~10˚)

1
0 5 10 15 20
2θ (˚)
37
 Information from XRD pattern
Peak Position
• Lattice spacing
Qualitative analysis
Lattice constant
• Shift of d value
Residual stress
Analysis for solid solution
Intensity
angle (2θ)
With or without peak
• crystal or amorphous
FWHM
(Full Width Half • Direction of sample and
intensity (orientation)
Maximum) Texture
• Crystallization Fiber structure
• Crystal size Pole figure
• Lattice strain
Intensity ratio of the peak
• Degree of crystallinity
Integral intensity of amorphous
Integral intensity of crystal
• Quantitative analysis
38
 XRF and XRD Analyses
 X-ray fluorescence (XRF) analysis can elucidate which
elements are present in the sample.
 X-ray diffraction (XRD) analysis can distinguish which
compounds are present in the sample.
 Peak positions are a function of lattice constants and
Miller indices.
 Intensities are a function of atoms (elements), their
coordinates and Miller indices.
XRD pattern differs for different crystal structures.

39
XRF & XRD Analyses of Iron Oxides
X-ray Fluorescence analysis X-ray diffraction analysis
100

Fe
(counts)

(counts)
80

FeO

）
強度（count）

強度（count
60
Intensity

Intensity
40

20

0
100
(counts)

(counts)
80

Fe2O3

）
強度（count）

強度（count
60
Intensity

Intensity
40

20

0
100
(counts)

(counts)
80
）
強度（count）

強度（count

Fe3O4
60
Intensity

Intensity

40

20

0
10 20 30 40 50 60 70 80 90
Wavelength (Å)
2q (degree)
2q（deg.）

40
 Polymorphic analysis
 Compounds even with the same chemical composition
can be distinguished.
 Example : Titanium Oxide (TiO2) , White powder

●：Ti
●：O

Rutile Anatase
Paint, Ink Photocaralyst
41
 Polymorphic analysis of TiO2
Fluorescence X-ray analysis X-ray diffraction analysis

Ti O 100 Rutile
Intensity (counts)

Intensity (counts)
80

Rutile 60

40
TiO2
20

0
Anatase 100 Anatase
Intensity (counts)

TiO2

Intensity (counts)
80

60

40

20

0
10 20 30 40 50 60 70 80 90
Wavelength (Å)
2q (degree)

42
 Qualitative Phase Analysis
Search Matching by existing
patterns in the database
30000

20000
PDF card No. 00-005-0628
Intensity (a.u.)

Chemical formula：NaCl (Halite)

Intensity (a.u.)
10000

20 30 40 50 60 70 80 90
2θ (˚)
0
20 30 40 50 60 70 80 90
2θ (˚) Identify as NaCl
43
 Format of ICDD-PDF Card
Number of card Reliability of card
04-0784 ★
Au dÅ Int h k l dÅ Int h k l
Gold 2.3550 100 111
Chemical formula , name 2.0390 52 200
1.4420 32 220
Rad. CuKa 1 l 1.54056 Filter Ni 1.2300 36 311
Dia. Cutoff Coll 1.1774 12 222
I/I 0 G0C0diffractometer d cor.abs 1.0196 6 400
Ref. Swanson, Tatge Natl. Bur. Stand. (U.S.), 0.9358 23 331
Circ. 539 vI p33 (1953) 0.9120 22 420
Sys. Cubic S.G Fm-3m (225) 0.8235 23 422
a 4.0786 b c A C
a 900786 b g Z4 mp 1061.6-1063.2
Ref. Ibid
ea nw b eg Sign
Lattice spacing
2V Dx 19.302mp Color Relative intensity
Ref.
Sample purified at NBS,Gaithersburg, Maryland, USA and is about
Miller index
99.997% Au. Pattern taken at 26 C

44
 Quantitative analysis by RIR method
The weight ratio can be calculated from the integrated intensity
of the highest peak and RIR(Reference Intensity Ratio) values.
RIR values is estimated by intensity ration between Al2O3 and
substance.

8.0e+003
Substance Integrated RIR values
Intensity(cps・deg) Ri
6.0e+003
TiO2 736 4.99
強度 (cps)

4.0e+003
CaCO3 883 3.22
Al2O3 190 1.05
2.0e+003
Substance Wi (I/R) Quantitative value(%)

TiO2 147 20.9

0.0e+000
Anatase, syn, Ti O2, 01-084-1285

Calcite, syn, Ca ( C O3 ), 01-086-0174 (=被検物質Wi/全Wi)

Corundum, Al2 O3, 01-075-6776 CaCO3 274 47.6
20 40
2θ (deg)
60 80 Al2O3 181 31.5

45
Part II. Experimental

2. Instrumentation

46
 Scheme of X-ray Diffractometer
Cooling system Detector
Cooling water

XG
High voltage cable

High voltage generator

Sample
Control and
X-ray generator Sample Stage operating system
(XG)

Data output
47
 Powder X-ray Diffractometer

X-ray source θ Mechanical section 2θ

Detector

Incident beam
optics Sample
Diffracted
beam optics
X-ray diffractometer for powder analysis
SmartLab

48
 X-ray Generator
Tube sealed-off type Rotating anode X-ray
2-3kW generator, 9-18kW

Cooling water

Be window Target

49
 Goniometer
Monochrometer

Kβ filter
X-ray generator
Detector

Soller slit Receiving Slit

Soller slit
Divergence Slit Goniometer Anti-scatter slit

50
 Types of Goniometer
Horizontal Type Vertical type

Sample horizontal type

(Theta-Theta type)
51
 Typical Systems of Optics
 Para-focusing optics  Parallel beam optics

Focusing circle

X-ray source Receiving slit X-ray source

Divergence slit
Scatter slit Detector
Detector
Multi-layer Parallel slits
mirror
Sample Sample
 Widely used as the standard optic  Intensity and resolution depend on
system for powder XRD the multi-layer mirror and slits
 High intensity and high resolution  Free from systematic errors arising
 Multiple sources of systematic from specimen position
errors
Bragg-Brentano para-focusing geometry 52
Slits System in Para-focusing Optics
 In the case of para focusing optics, slits of tree different
types are used.
DS
To define the irradiated area
Divergence Slit
RS
To define the receiving width
Receiving Slit
SS
Blockig off extra scattering
Anti-Scatter Slit
Type Width Intensity Resolution
DS wide strong (low)
Divergence Slit narrow week （high）
RS wide strong low
Receiving Slit narrow week high
SS wide
Anti-Scatter Slit narrow

There is almost no influence on the resolution by DS

53
 Divergence Slit and Irradiation Width
Goniometer radius185 mm Goniometer radius285 mm Goniometer radius 300 mm
MultiFlex・UltimaIV Protectus UltimaIV・RINT TTR III SmartLab
40 40 40
---：2˚ ---：2/3˚ ---：2/3˚
35 ---：1˚ 35 ---：1/2˚ 35 ---：1/2˚
---：1/2˚ ---：1/3˚ ---：1/3˚
30 30 ---：1/4˚ 30
---：1/4˚ ---：1/4˚
Irradiation width (mm)

---：1/6˚ ---：1/6˚ ---：1/6˚

照射幅（mm）

照射幅（mm）
25 25 25
Available width of Available width of Available width of
20 20
sample holder (20 mm) sample holder (20 mm)
20 sample holder (20 mm)

15 15 15

10 10 10

5 5 5

0 0 0
0 20 40 60 80 0 20 40 60 80 0 20 40 60 80
2θ (˚) 2θ (˚) 2θ (˚)
1 1
Irradiation width 2A = + ・R sin(β / 2) β : divergence angle
sin(θ + β / 2) sin(θ - β / 2)
54
 Influence of RS Width on Profile
 Narrower receiving slit (RS) width  higher resolution
and decreased intensity

RS-0.15 mm
4000

RS-0.45 mm
Intensity (cps)

RS-0.80 mm
強度 (cps)

3000

2000

1000

0
67.0 67.5 68.0 68.5 69.0
2θ (deg)
2θ(deg)
55
 Soller Slits
 Soller slits have the effect of reducing the axial
divergence of incident and diffracted beams and thus of
suppressing the so-called umbrella effect.

---：0.5deg.
15000
---：2.5deg.
---：5deg.

Intensity（CPS）
---：without Soller Slits
10000 （Gonio radius ：285mm）

5000

0
Standard Soller slits : 5deg.
5 5.5 6 6.5 7
2θ（deg.）
56
Monochromatization of X-ray Beams
 X-rays entering into a detector are consisting of various
wavelength components which sometimes hinder the
data analysis.
 To monochromatize the X-rays only for target wavelength
component is required.
 Some components
 Diffracted X-ray beam consisting of only Kα
component  Needed.
 Kβ component which gives extra diffraction
lines.
 Continuous X-rays  Raising background
height
sample  Fluorescence X-rays from sample  Raising
background height
57
 Methods of Monochromatization
 Physical and electronic methods are usually combined in
monochromatizing X-rays before and after entering into
the detector.
Methods Principles Effects
Absorbing Kb com-
Resultant intensity ratio =
Physical Kb filter ponent by properly
100:1 for Ka:Kb
selected element

Mono- Use of Bragg

Effective monochromatization
chromator reflection

PHA (pulse- Selection of

Eliminating continuous and
Electronic height electronic pulses in
fluorescent X-ray components
analyzer) detector

58
 Kb Filter
 Mass absorption coefficient of an element greatly
changes at an absorption edge.
Kα：Kβ = 5：1 Ni Kα：Kβ = 100：1
Transmitted
Mass absorption coefficient

Kα

Mass absorption coefficient

Cu Kα

μ/ρ = 48.8
Intensity

Intensity
Kα
Kβ
Cu Kβ
μ/ρ = 279
Kβ

1.2 1.4 1.6 1.8 Absorbed 1.2 1.4 1.6 1.8

λ (Å) λ (Å)
59
 Kβ Filters for Various Wavelengths
Wavelength (Å) Filter
Condition : IKβ /IKα = 1/100
Target Wavelength of
Kα 1 Kβ Absorber
absorption edge (Å) Kα 1Transmission
Thickness (mm)
ratio (%)
Cr 2.2896 2.0848 V 2.269 0.011 63
Fe 1.9360 1.7565 Mn 1.896 0.011 62
Co 1.7889 1.6208 Fe 1.743 0.012 61
Cu 1.5405 1.3922 Ni 1.488 0.015 55
Mo 0.7093 0.6323 Zr 0.689 0.081 43

 Advantage： simple and low cost. It is just to insert a

metal filter in X-ray pass.
 Disadvantage： some components of Kβ, continuous and
fluorescence X-rays are remained unmonochromatized.
60
 Effects of Kβ Filter
 Kβ lines can efficiently be  Filtering is not effective for
removed with a metal filter. some fluorescent X-rays
10000
Sample: α-Quartz (SiO2) Sample: Hematite (Fe2O3)
60000 Kα 5000
4000 8000
Intensity

3000
Intensity (cps)

Intensity (cps)
2000
1000
40000 0
6000
23 24 25 26 27 28
2θ (Å)
Removal of Kβ lines 4000
20000 is not complete for
Kα Kβ strong lines. Fluorescent X-rays from
2000
Iron in the sample
Kβ Kβ Kα Kα
0 0
20 25 30 35 40 30 32 34 36 38 40
2θ (˚) 2θ (˚)

61
 Crystal Monochromator
 X-rays of only Ka component satisfy the Bragg’s law,
and they pass through the monochromator.
 Other components are blocked off.
 Perfect crystals such as Si or Ge are used.

Ka, Kb, continuous 2dsinθm = λKα

and fluorescent X-
rays
λKα
θm
Kα X-rays
Crystal monochromator
/crystal analyzer
62
Effects of Monochromator (Cu case)
 Low background and well  Higher background for the
resolved peaks sample containing Cu.
 Lowered intensities
Hematite (Fe2O3) 10000
10000 Sample : Copper
---：Kβ Filter
40 (By using monochrometer)
Intensity

---：Monochrometer
8000
8000 20

Intensity (cps)
Intensity (cps)

0
38.5 39 39.5 40 6000
6000 2θ (˚)

4000
4000

2000
2000

0
0 40 42 44 46 48 50 52
30 32 34 36 38 40
2θ (˚)
2θ (˚)
63
 X-ray Detectors
 X-ray photons are directly or indirectly converted to
electronic charges, and then finally to electronic signals.
 X-ray photons, converted to electronic pulses, are
counted one by one in photon-counting type detectors.
Type Sensing mechanism Detectors
Electronic charge Semiconductor detectors (1D-Si strip
Photon conversion detector, pixelated 2D-detector)
counting Proportional counter, Position sensitive
Ionization
proportional counter
Charge coupling device (CCD),
Fluorescence
Scintillation counter, Fluorescence plate
Photon
integrating Phosphorescence Imaging plate (IP)
Silver halide photo effect Photo film

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 Zero-dimensional Detector
 Scintillation counter has widely been used for powder
diffractometer. Focusing Circle

 All X-ray photons pass through a receiving slit

are counted. Goniometer
circle
 Angular position of the detector is determined
by the central position of a receiving slit.
 Resolution of the angular position is
determined by the width of receiving slit.

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 One-dimensional Detector
 One-dimensional silicon strip detector (1D-SSD) has, for
example, 256 pairs of strip sensor and electronic circuit
for counting X-ray photons.
 Each strip corresponds to a receiving slit.
 If we scan the diffraction pattern with this 1D-SSD, it is
identical to scan the pattern 256-times with 0D-counter.

2θ
Detected by each strip
--> 1-Dimensional data

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 Some Features of 1D-SSD
 High speed and high intensity  High energy resolution and low
measurement background intensity
Sample : Zeolite Sample : Hematite(Fe2O3)
4000 40000
Measurement Time 1 min. Measurement Time 1 min.
35000
--- : Standard mode
3000 30000 --- : Fluorescence
Reduction mode

Intensity（Counts）
Intensity（Counts）

25000

2000 20000

15000

1000 10000

5000

0 0
5 10 15 20 25 30 35 40 45 50 55 20 30 40 50 60

2θ（deg.） 2θ（deg.）
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Thank you for your attention.

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