Optical Ceramics Using FT-IR Characterization

Title: Optical Ceramics

Reporter: Jerick Jabien & Bendaud Batabor
Aims of Report:
 To explain the Properties of Optical Ceramics
 To show optical ceramic application.
 To understand the thought and theory behind optical ceramic materials.

Summary of Characterization of Tb3Al5O12 Transparent ceramics

I. Characterization Outline
Phase identification of the powder was identified by X-ray diffraction. The
compositions of the powders were investigated by a Fourier transform infrared
spectroscopy (FTIR). Thermo-gravimetry analysis and differential thermal analysis (TG-
DTA) of the precursor were performed on a TG-DTA analyzer in flowing air atmosphere with
a heating rate of 10 C/min. Specific surface area analysis was performed using a micromeritics
with N2 as the absorption gas at 77 K. Morphologies of the powders were observed with a field
emission scanning electron microscopy. The in-line transmittance of mirror-polished ceramics
(1.5 mm thick) was measured by a UV-VIS-NIR spectrophotometer. Microstructures of the
thermal-etched surfaces of as-sintered ceramics (thermally etched at 1400 C for 3 h) were
observed by a field emission scanning electron microscopy. Grain sizes of the sintered samples
were measured by the linear intercept method and the average grain size was calculated by
multiplying the average linear intercept distance by 1.56. The Verdet constant was measured
with an instrument consisting of a He-Ne laser, an electromagnet and two polarizers. The
measurement was carried out at room temperature.

II. Description of Characterization Technique

FTIR spectroscopy is an established technique for quality control when evaluating
industrially manufactured material, and can often serve as the first step in the material analysis
process. A change in the characteristic pattern of absorption bands clearly indicates a change
in the composition of the material or the presence of contamination. If problems with the
product are identified by visual inspection, the origin is typically determined by FTIR
microanalysis. This technique is useful for analyzing the chemical composition of smaller
particles, typically 10 -50 microns, as well as larger areas on the surface [2].
III. Equipment used in characterization Technique

Most of the instruments are made in Japan.

 FTIR, Bruker VERTEX 70 spectrophotometer, Ettlingen, Germany

 XRD, Model D/max2200 PC, Rigaku, Japan
 Thermo plus EVO II, Rigaku, Japan
 Micromeritics (Model ASAP 2010, Norcross, USA)
 FESEM, SU8220, Hitachi, Japan
 UV-VIS-NIR spectrophotometer (Model Cary-5000, Varian, USA)
 FESEM, S-4800, Hitachi, Japan
 HeeNe laser

IV. Result Summary

Figure below shows the XRD patterns of the as-synthesized precursor and the
powder calcined at 800 C-1200 C for 4 h. XRD analysis shows that the as-
synthesized precursor is amorphous[1].

Figure 1.1 XRD patterns of the as-synthesized precursor and the powders calcined at
different temperatures for 4 h[1].
 Fig. 1.2. FTIR spectra of the precursor and the powders calcined at different
temperatures for 4 h[1].

Figure 1.3. FESEM micrographs of the precursor and the powders calcined at different
temperatures for 4 h: (a) precursor; (b) 800 oC; (c) 900 oC; (d) 1000 oC [1].
Figure 1.4. FESEM micrographs of the precursor and the powders calcined at different
temperatures for 4 h at (e) 1100 oC; and (f) 1200 oC [1].

Figure 1.5. FESEM micrographs of the thermally etched surfaces of TAG ceramics sintered at
(a) 1450 oC, (b) 1500 oC, (c) 1550 oC, (d) 1600 oC for 2h [1].
Figure 1.6. FESEM micrographs of the thermally etched surfaces of TAG ceramics sintered at
(e) 1650 oC and (f) 1700 oC for 2 h [1].

Figure 1.7. In-line transmittance curves of the TAG ceramics (a) sintered at 1650e1700 oC for 2-
20 h and (b) pre-sintered at 1700 oC for 20 h with HIP post-treated at 1700 oC for 3h [1].
V. Application of Tb3Al5O12 Transparent ceramics
Faradays isolators are used in advanced optical applications and high-average-power
laser system and one important component of it is magneto-optical materials that can be
made by synthesizing Tb3Al5O12 Transparent ceramics [1]. TAG was prepared and measured
its optical transparency, verdet constant and thermal conductivity. To reach excellent
magneto-optical property of TAG single crystals, the solution might be the TAG transparent
ceramics [8]. Faradays isolator is a type of optical isolator, can transmit light in specified
direction while blocking light in opposite direction [9]. Faraday isolators and circulators used
widely in laser technology.

VI. Common Parts of the FTIR

FTIR spectrometer consists of the following,
 Source
 Interferometer
 Sample compartment
 Detector
 Amplifier
 A/D convertor
 Computer

Figure 2. Block diagram of an FTIR spectrometer [3].

Figure 3. Ray diagram of FTIR micro spectrometer [7].

Figure 4. Fourier transform infrared spectroscopy Instrumentation [4].

Figure 5. Image of the sample compartment of the Bruker Equinox 55 FT-IR
spectrometer with custom-made gas cell. The top of the MCT detector is visible at the top
left corner. The IR beam path is indicated in red [5].

Figure 6. FT-IR Spectrometer Detectors [6].

VII. Companies/Manufacturers of FTIR

Below are the FTIR spectrometer manufactures/companies [11],

 Bristol Instruments Inc. - Victor, NY
 MOORI Technologies Co.
 Block Engineering
 D&P Instruments
 Interspectrum OU
 JASCO Inc.
 Newport - Oriel Instruments, Unit of MKS Instruments
 Spectrolab Systems Ltd., An Anaspec Group Co.
 Agilent Technologies Inc., Chemical Analysis
 Analytik Ltd.
 Blue Sky Spectroscopy Inc.
 Bruker Optics Inc., Member of the Bruker Corp.
 Consolidated Sciences (CONSCI)
 Delta Photonics
 Idealab Inc.
 International Equipment Trading (IET) Ltd.
 Lasnix
 LR Tech Inc.
 NETZSCH company
 Lumetrics
 MKS Instruments Inc.
 Nireos
 nortus Systronic GmbH
 PerkinElmer Instruments
 Petrolab Co., An AMETEK Co.
 Rebellion Photonics Inc.
 Remspec Corp.
 Gasera Company
 Shimadzu Europa GmbH -
 Shimadzu Scientific Instruments Inc., Sub. of Shimadzu Corp.
 SphereOptics GmbH
 Topnir Systems, Aix-en-Provence, France

One of the Top companies of FTIR is Bruker Optics Inc. under Bruker
Corporation which was founded in the United States and was published in
1974. It followed by the NETZSCH and Gasera companies. NETZSCH
founded at the year 1873 in Germany and Gasera was located in Finland
[12].
VIII. HISTORY OF THE CHARACTERIZATION METHOD
In 1940’s, the commercialization of chemical infrared spectroscopy was still not
large, until the following years. Peter Fellgett an astrophysicist used an interferometer in
1949 to measure the light from celestial bodies and he produced the first Fourier
transform infrared spectrum in the history[10]. After two decades, still researcher have
limitation in using FTIR. Until 1960’s the Fourier transform became available using
microcomputers and the commercialization of FTIR spectrometers began. And later the
Cooley-Tukey algorithm developed which quickly execute the Fourier transform the Fast
Fourier Transform or FFT).
FTIR spectrometers have optical system which can be show below.

Figure 6. The Michelson interferometer [10].

IX. Reference
[1]. J. Dai, Y. Pan, W. Wang, W. Luo, T, Xie, H. Kou, J. Li, Fabrication of Tb3Al5O12
transparent ceramics using co-precipitated nanopowders, Optical Materials 73 (2017) 38-44.
[2]. https://rtilab.com/techniques/ftir-analysis/
[3].https://chem.libretexts.org/Bookshelves/Physical_and_Theoretical_Chemistry_Textbook_
Maps/Supplemental_Modules_(Physical_and_Theoretical_Chemistry)/Spectroscopy/Vibratio
nal_Spectroscopy/Infrared_Spectroscopy/How_an_FTIR_Spectrometer_Operates#:~:text=F
TIR%20Spectrometers,The%20Components%20of%20FTIR%20Spectrometers,interferomet
er%20and%20reaches%20the%20detector.
[4]. http://delloyd.50megs.com/MOBILE/infrared_spectroscopy.html
[5].https://www.researchgate.net/publication/26834284_An_approach_to_the_spectral_simul
ation_of_infrared_hollow_waveguide_gas_sensors/figures?lo=1
[6]. https://www.newport.com/f/detectors-for-oriel-mir8035-ft-spectrometers
[7].https://www.researchgate.net/publication/231338007_Application_of_vibrational_micros
pectroscopy_to_biology_and_medicine/figures?lo=1
[8]. https://www.sciencedirect.com/science/article/abs/pii/S0925346711003302
[9].https://www.rpphotonics.com/faraday_isolators.html#:~:text=A%20Faraday%20isolator
%20is%20a,important%20type%20of%20optical%20isolators.
[10].https://silo.tips/download/ftirinstrumentation#:~:text=In%201949%20astrophysicist%20
Peter%20Fellgett,first%20Fourier%20transform%20infrared%20spectrum.&text=In%20the
%20late%201960s%20when,available%2C%20commercial%20FTIR%20spectrometers%20
appeared.
[11]. https://www.photonics.com/Buyers_Guide/Bristol_Instruments_Inc/ca60875/c1995
[12]. https://www.ventureradar.com/keyword/FTIR