In Situ FT-IR Studies of Oxide and Oxynitride Sol-Gel-Derived Thin Films

1984 ◽  
Vol 32 ◽  
Author(s):  
David M. Haaland ◽  
C. Jeffrey Brinker

ABSTRACTA high-temperature infrared cell was developed to study the gel-to-glass conversion of sol-gel-derived thin films. FT-IR spectra of matched thin-film borosilicate sol-gel samples were taken as the samples were heated at 100°C intervals to 700°C in either air or ammonia. The gels were converted to oxide and oxynitride glasses, respectively, by these heat treatments. The gel-to-glass conversion could be followed and compared for these two treatments by monitoring changes in the vibrational bands present in the spectra. Comparisons between the infrared spectra of NH3-treated and air-treated films heated above 500°C reveal the appearance of new B-N bonds at the expense of B-O-Si bonds for the NH3-fired films. These spectra also exhibit changes which may indicate the formation of Si-N bonds. Thus, ammonolysis reactions can result in thin-film oxynitride glass formation at relatively low temperatures.

2011 ◽  
Vol 117-119 ◽  
pp. 840-844
Author(s):  
Xu Yong Wu ◽  
De Yin Zhang ◽  
Kun Li

The novel lithium enriched lithium tantalate (LiTaO3) targets were papered by employing the sol-gel process and the high temperature sintered process. The sol of LiTaO3 was firstly prepared through reacting lithium ethoxide with tantalum ethoxide. The LiTaO3 powder was fabricated by presintered LiTaO3 dry gel 4 hour, at 800°C. The 11cm13cm1cm lithium enriched LiTaO3 target samples were prepared by sintered the pressed LiTaO3 powder billet 4 hour in the 850°C muffle furnace. The density of the 5% overdose lithium enriched LiTaO3 target is measured 5.96g/cm3. The XRD measured results show that the ion beam enhanced deposited (IBED) thin film samples using the prepared 5% overdose lithium enriched LiTaO3 target have the polycrystal structure of LiTaO3, but there has remanent Ta2O5 existed in the IBED thin film samples. The main reason for the remanent Ta2O5 growth was due to the stoichiometric proportion mismatch between Li and Ta in the IBED thin film samples during the high temperature annealed process, which caused the lithium oxide evaporation loss from the IBED thin film samples and made the proportion of Ta2O5 increase. After multipule repeated target prepared experiments, the 8.76% overdose lithium enriched LiTaO3 target is suitable for fabricating the 550°C annealed IBED LiTaO3 thin film. After the repeated process experiments, the suitable deposited process parameters of the IBED-C600M instrument for the 8.76% overdose lithium enriched LiTaO3 target were obtained. The SEM micrographs of the 550°C annealed IBED LiTaO3 thin films prepared by the 8.76% overdose lithium enriched LiTaO3 target reveal the prepared thin films are uniform, smooth and crack-free on the surface, and the perfect adhesion between the thin film and the substrate. The successfully fabricated LiTaO3 thin film samples verify the prepared processes of novel LiTaO3 sputtering target are effective.


2011 ◽  
Vol 1312 ◽  
Author(s):  
Rafaella T. Paschoalin ◽  
Clarice Steffens ◽  
Alexandra Manzoli ◽  
Mhbuti R. Hlophe ◽  
Paulo S. P. Herrmann

ABSTRACTThe effect of pH was investigated on the morphological and spectroscopic properties of PANI thin films on PET. PANI/PET strips were prepared by a pattern-printing technique and coated with a thin film of polyaniline in situ emeraldine oxidation state, doped with HCl (PANI-HCl), obtained by in situ polymerization. AFM, UV-VIS-NIR and FTIR/ATR spectroscopic results showed that pH has a great influence on the polymer layer morphology of the coating layers, while the intensity of vibrational bands decreases with rising pH, increase due to changes in the H-bonded structure in the polymer chain.


2020 ◽  
Vol 27 (5) ◽  
pp. 1209-1217 ◽  
Author(s):  
Anders Bank Blichfeld ◽  
Kristine Bakken ◽  
Dmitry Chernyshov ◽  
Julia Glaum ◽  
Tor Grande ◽  
...  

Understanding the crystallization process for chemical solution deposition (CSD) processed thin films is key in designing the fabrication strategy for obtaining high-quality devices. Here, an in situ sample environment is presented for studying the crystallization of CSD processed thin films under typical processing parameters using near-grazing-incidence synchrotron X-ray diffraction. Typically, the pyrolysis is performed in a rapid thermal processing (RTP) unit, where high heating rates, high temperatures and atmosphere control are the main control parameters. The presented in situ setup can reach heating rates of 20°C s−1 and sample surface temperatures of 1000°C, comparable with commercial RTP units. Three examples for lead-free ferroelectric thin films are presented to show the potential of the new experimental set-up: high temperature, for crystallization of highly textured Sr0.4Ba0.6Nb2O6 on a SrTiO3 (001) substrate, high heating rate, revealing polycrystalline BaTiO3, and atmosphere control with 25% CO2, for crystallization of BaTiO3. The signal is sufficient to study a single deposited layer (≥10 nm for the crystallized film) which then defines the interface between the substrate and thin film for the following layers. A protocol for processing the data is developed to account for a thermal shift of the entire setup, including the sample, to allow extraction of maximum information from the refinement, e.g. texture. The simplicity of the sample environment allows for the future development of even more advanced measurements during thin-film processing under non-ambient conditions.


2002 ◽  
Vol 748 ◽  
Author(s):  
N. J. Donnelly ◽  
G. Catalan ◽  
C. Morros ◽  
R. M. Bowman ◽  
J. M. Gregg ◽  
...  

ABSTRACTThin film capacitor structures of Pb(Mg1/3Nb2/3)O3 (PMN) - PbTiO3 (PT) were fabricated using pulsed laser deposition (PLD) on MgO{100} substrates using (La1/2,Sr1/2)CoO3 (LSCO) as a lower electrode. Crystallographic and dielectric characterisation confirmed perovskite relaxor-like behaviour. Measurements of the electrostrictive coefficients by in-situ X-ray diffraction, piezo-response atomic force microscopy and three point bending experiments showed both Q11 and Q13 to be comparable to accepted values for single crystals. However, for a given field, the electric field-induced strain in the thin films was much less than that of single crystal. This was clearly intimately linked to poor thin film polarisability. Previous work had shown sol-gel PMN-PT films to have significantly greater permittivities than PLD films, and a TEM investigation was undertaken to see if functional differences could be related to differences in microstructure, and hence if the functional and electromechanical properties of PLD films could be improved by attempting to replicate sol-gel microstructures.


Author(s):  
K. Barmak

Generally, processing of thin films involves several annealing steps in addition to the deposition step. During the annealing steps, diffusion, transformations and reactions take place. In this paper, examples of the use of TEM and AEM for ex situ and in situ studies of reactions and phase transformations in thin films will be presented.The ex situ studies were carried out on Nb/Al multilayer thin films annealed to different stages of reaction. Figure 1 shows a multilayer with dNb = 383 and dAl = 117 nm annealed at 750°C for 4 hours. As can be seen in the micrograph, there are four phases, Nb/Nb3-xAl/Nb2-xAl/NbAl3, present in the film at this stage of the reaction. The composition of each of the four regions marked 1-4 was obtained by EDX analysis. The absolute concentration in each region could not be determined due to the lack of thickness and geometry parameters that were required to make the necessary absorption and fluorescence corrections.


1999 ◽  
Vol 606 ◽  
Author(s):  
Keishi Nishio ◽  
Jirawat Thongrueng ◽  
Yuichi Watanabe ◽  
Toshio Tsuchiya

AbstructWe succeeded in the preparation of strontium-barium niobate (Sr0.3Ba0.7Nb2O6 : SBN30)that have a tetragonal tungsten bronze type structure thin films on SrTiO3 (100), STO, or La doped SrTiO3 (100), LSTO, single crystal substrates by a spin coating process. LSTO substrate can be used for electrode. A homogeneous coating solution was prepared with Sr and Ba acetates and Nb(OEt)5 as raw materials, and acetic acid and diethylene glycol monomethyl ether as solvents. The coating thin films were sintered at temperature from 700 to 1000°C for 10 min in air. It was confirmed that the thin films on STO substrate sintered above 700°C were in the epitaxial growth because the 16 diffraction spots were observed on the pole figure using (121) reflection. The <130> and <310> direction of the thin film on STO were oriented with the c-axis in parallel to the substrate surface. However, the diffraction spots of thin film on LSTO substrate sintered at 700°C were corresponds to the expected pattern for (110).


2002 ◽  
Vol 725 ◽  
Author(s):  
S.B. Phelan ◽  
B.S. O'Connell ◽  
G. Farrell ◽  
G. Chambers ◽  
H.J. Byrne

AbstractThe current voltage characteristics of C60 thin film sandwich structures fabricated by vacuum deposition on indium tin oxide (ITO) with an aluminium top electrode are presented and discussed. A strongly non-linear behavior and a sharp increase in the device conductivity was observed at relatively low voltages (∼2V), at both room and low temperatures (20K). At room temperature the system is seen to collapse, and in situ Raman measurements indicate a solid state reduction of the fullerene thin film to form a polymeric state. The high conductivity state was seen to be stable at elevated voltages and low temperatures. This state is seen to be reversible with the application of high voltages. At these high voltages the C60 film was seen to sporadically emit white light at randomly localized points analogous to the much documented Electroluminescence in single crystals.


2006 ◽  
Vol 326-328 ◽  
pp. 689-692
Author(s):  
Seung Jae Moon

The thermal conductivity of amorphous silicon (a-Si) thin films is determined by using the non-intrusive, in-situ optical transmission measurement. The thermal conductivity of a-Si is a key parameter in understanding the mechanism of the recrystallization of polysilicon (p-Si) during the laser annealing process to fabricate the thin film transistors with uniform characteristics which are used as switches in the active matrix liquid crystal displays. Since it is well known that the physical properties are dependent on the process parameters of the thin film deposition process, the thermal conductivity should be measured. The temperature dependence of the film complex refractive index is determined by spectroscopic ellipsometry. A nanosecond KrF excimer laser at the wavelength of 248 nm is used to raise the temperature of the thin films without melting of the thin film. In-situ transmission signal is obtained during the heating process. The acquired transmission signal is fitted with predictions obtained by coupling conductive heat transfer with multi-layer thin film optics in the optical transmission measurement.


2006 ◽  
Vol 21 (2) ◽  
pp. 505-511 ◽  
Author(s):  
Lili Hu ◽  
Junlan Wang ◽  
Zijian Li ◽  
Shuang Li ◽  
Yushan Yan

Nanoporous silica zeolite thin films are promising candidates for future generation low-dielectric constant (low-k) materials. During the integration with metal interconnects, residual stresses resulting from the packaging processes may cause the low-k thin films to fracture or delaminate from the substrates. To achieve high-quality low-k zeolite thin films, it is important to carefully evaluate their adhesion performance. In this paper, a previously reported laser spallation technique is modified to investigate the interfacial adhesion of zeolite thin film-Si substrate interfaces fabricated using three different methods: spin-on, seeded growth, and in situ growth. The experimental results reported here show that seeded growth generates films with the highest measured adhesion strength (801 ± 68 MPa), followed by the in situ growth (324 ± 17 MPa), then by the spin-on (111 ± 29 MPa). The influence of the deposition method on film–substrate adhesion is discussed. This is the first time that the interfacial strength of zeolite thin films-Si substrates has been quantitatively evaluated. This paper is of great significance for the future applications of low-k zeolite thin film materials.


Sign in / Sign up

Export Citation Format

Share Document