CVD of Silicon Nitride Plate from HsiCl3-NH3-H2 Mixtures

1991 ◽  
Vol 250 ◽  
Author(s):  
J. W. Lennartz ◽  
M. B. Dowell
Keyword(s):  
Silicon Nitride ◽  
Line Broadening ◽  
Multiple Correlation ◽  
Deposition Rates ◽  
Reaction Proceeds ◽  
Designed Experiment ◽  
Transport Control ◽  
Crystallite Sizes ◽  
Thickness Variations ◽  
Optimized Conditions

AbstractPreferred conditions for deposition of thick α-Si3 N4 plate from HSiCl3 -NH3-H2 on the vertical surfaces of a lowpressure, hot-wall CVD reactor were identified by means of a designed experiment. The design included the range of temperatures 1300°C-1500°C, pressures 0.5–2.0 Torr, and residence times 0.01–1.0 sec. The vertical deposition surfaces received a viscous, laminar flow of well mixed, thermally equilibrated reactants. Plates 0.05–0.5 mm thick were produced on multiple vertical substrates 350 cm2 in area at deposition rates 5–70 μm/hr. Plates 0.5–4.0 mm thick were produced on horizontal substrates at deposition rates of 60–120 μm/hr. When NH3 flows in stoichiometric excess, deposition rates on vertical surfaces increase approximately linearly with the flow rate of HSiCl3 but depend little on temperature, as would be expected if the reaction proceeds under mass transport control with product depletion. Multiple correlation analyses show that thickness variations in the deposit are reduced by increasing the temperature and decreasing the gas residence time. CVD silicon nitride plate produced under the optimized conditions exhibits theoretical density and is free of pores and cracks. It exhibits a columnar morphology in which the <222> and <101> crystallographic directions are oriented preferentially normal to a surface, which consists of well-defined trigonal facets 10–50 μm across. Crystallite sizes determined by Xray line broadening range from 0.06–1.0 μm. This CVD plate is gray and contains approximately 0.5 w/o C and 0.5 w/o 0 as principal impurities.

X-ray diffraction characterization of the microstructure of close-packed hexagonal nanomaterials

2008 ◽  
Vol 23 (3) ◽  
pp. 213-223 ◽  
Author(s):  
Zhao-hui Pu ◽  
Chuan-zheng Yang ◽  
Pei Qin ◽  
Yu-wan Lou ◽  
Li-fang Cheng
Keyword(s):  
Stacking Faults ◽  
Triple Line ◽  
Stacking Fault ◽  
Line Broadening ◽  
X Ray Diffraction ◽  
Nano Zno ◽  
X Ray ◽  
Crystallite Sizes ◽  
Small Crystallite ◽  
Charge Discharge

A general least-squares technique for X-ray diffraction line broadening analysis has been developed. The technique can be used to determine single, double, and triple line broadening effects caused by small particle sizes, microstrain, stacking faults, or all three presented in a closed-packed hexagonal nanomaterial. The technique was applied to characterize the microstructure of β-Ni(OH)2, a negative electrode material in nickel-metal hydride (NiMH) batteries. Double line broadening effects caused by both small crystallite sizes and stacking faults in β-Ni(OH)2 were detected and analyzed. Triple line broadening effects caused simultaneously by small crystallite sizes, microstrain, and stacking faults were detected in β-Ni(OH)2 after activation and charge-discharge cycle tests. The triple line broadening effects were found to be selective and most pronounced for diffraction lines with h−k=3n±1. The broadening effects were larger when l=even, but smaller when l=odd. The shape and the average size of the crystallites, microstrain, and stacking fault probability in β-Ni(OH)2 changed dramatically after activation and charge-discharge cycles. The method was also applied to characterize and investigate the microstructure of nano ZnO materials. Results indicate that no selective broadening appears in the XRD patterns of the nano ZnO materials. The average crystallite sizes were different slightly, and the stacking fault probabilities differed significantly with different dopants.

The LPCVD of Silicon Nitride Films from Alkylazidosilanes

1990 ◽  
Vol 204 ◽  
Author(s):  
David A. Roberts ◽  
Arthur K. Hochberg ◽  
David L. O'Meara ◽  
Felicia Rusnak ◽  
Herman Hockenhull
Keyword(s):  
Thin Films ◽  
Silicon Nitride ◽  
Film Properties ◽  
Deposition Rates ◽  
Extreme Caution ◽  
Silicon Nitride Films ◽  
Sensitive Film

ABSTRACTThe series of azidosilanes, SiEtn(N3)4-n where n = 1,2,3 and Si(t-butyl)(N3)3 were evaluated for the LPCVD of silicon nitride thin films. Both SiEt(N3)3 and Si(t-butyl)(N3)3 gave deposition rates of approximately 100 Å/min at temperatures of 450–500°C but films appear to be porous and air sensitive. Film properties improved as deposition temperatures were increased to 600°C. The polyazides must be handled with extreme caution. An unexplained detonation of one sample of SiEt(N3)3 occurred during the course of this study.

An evaluation of methods of diffraction-line broadening analysis applied to ball-milled molybdenum

2004 ◽  
Vol 37 (2) ◽  
pp. 300-311 ◽  
Author(s):  
I. Lucks ◽  
P. Lamparter ◽  
E. J. Mittemeijer
Keyword(s):  
Line Profile ◽  
Strain Field ◽  
Fourier Coefficients ◽  
Field Method ◽  
Diffraction Line ◽  
Line Profile Analysis ◽  
Cauchy Type ◽  
Line Broadening ◽  
Integral Breadth ◽  
Crystallite Sizes

A comparison has been carried out of different methods of X-ray diffraction-line profile analysis for the determination of crystallite sizes and microstrains, namely the integral breadth method and three methods based on Fourier analysis of diffraction lines, namely the Warren–Averbach method, an `alternative method' and a profile synthesis strain field method. The analyses have been applied to Mo powder ball milled in two types of mills: an attritor and a planetary mill. Using the Williamson–Hall integral breadth method, the line broadening at moderate deformation is attributed solely to microstrain,i.e.practically no size broadening is detected. The three methods based on the Fourier coefficients of diffraction lines yield comparable values for crystallite sizes and microstrains. With the profile synthesis strain field method, if a size effect is included, it is possible to fit the experimental Fourier coefficients over the entire range of the relevant scale of correlation distances. The line profile shape due to microstrains, as derived with the strain field method, exhibits a systematic dependence on the integral breadth. With increasing breadth, the shape changes from a Cauchy type to a Gaussian type, suggesting a change of the dislocation arrangement with increasing plastic deformation of molybdenum powders.

Evolution of crystalline zirconia structure in heat-treated ceria stabilized zirconia gels

1991 ◽  
Vol 6 (12) ◽  
pp. 2688-2693 ◽  
Author(s):  
V.S. Nagarajan ◽  
K.J. Rao
Keyword(s):  
Heat Treatment ◽  
Temperature Region ◽  
Diffusion Barriers ◽  
Line Broadening ◽  
Stabilized Zirconia ◽  
Major Phase ◽  
X Ray ◽  
Stable Regime ◽  
Heat Treated ◽  
Crystallite Sizes

Transformation characteristics of CeO2 stabilized ZrO2 gels have been studied during heating in the temperature region 1273–1473 K. The nature of the major phase present changes drastically in this temperature region. The crystallite sizes of tetragonal and monoclinic ZrO2 crystallites have been calculated by x-ray line broadening. The change in the nature of the major phase observed during heat treatment seems to be related to the presence of a barrier for transformation from a metastable to a stable regime, which in turn appears to be related to the diffusion barriers of Ce4+ in ZrO2.

Silicon Nitride Deposited at Very Low Silane Pressures Using Electron Cyclotron Resonance Plasmas

1992 ◽  
Vol 284 ◽  
Author(s):  
J. R. Flemish ◽  
R. Pfeffer ◽  
W. Buchwald ◽  
K. A. Jones
Keyword(s):  
Refractive Index ◽  
Silicon Nitride ◽  
Microwave Power ◽  
Material Properties ◽  
Cyclotron Resonance ◽  
Total Pressure ◽  
Electron Cyclotron Resonance ◽  
High Quality ◽  
Deposition Rates ◽  
Hydrogen Incorporation

ABSTRACTWe report on the material properties of SiNx:H films deposited using a 2% SiH4/N2 mixture with additional N2 in an ECR reactor. Deposition rates, refractive index, and stoichiometry have been characterized using ellipsometry, Rutherford backscattering spectroscopy, and infrared spectroscopy. Reactor conditions of 2m Torr total pressure, 650W microwave power, and substrate temperature of 250°C result in high quality, stoichiometric silicon nitride. With a SiH4/N2 ratio = 0.003, hydrogen incorporation is approximately 1.5% and the refractive index is nr =2.0. Lower microwave power and a higher SiH4/N2 ratio result in slightly N-rich films which is attributable to increased H-incorporation. Higher total pressure results in significantly enhanced deposition rates, but with greatly increased H and O content.

Silicon Nitride from Microwave Plasma: Fabrication and Characterization

1986 ◽  
Vol 68 ◽  
Author(s):  
Yves Tessier ◽  
J. E. Klemberg-Sapieha ◽  
S. Poulin-Dandurand ◽  
M. R. Wertheimer
Keyword(s):  
Refractive Index ◽  
Silicon Nitride ◽  
Etch Rate ◽  
Microwave Plasma ◽  
Audio Frequency ◽  
Elastic Recoil ◽  
Deposition Rates ◽  
Elastic Recoil Detection ◽  
Fabrication And Characterization ◽  
Substrate Temperatures

AbstractPlasma silicon nitride (P-SiN) films were prepared from SiH4/NH3 mixtures in a large volume microwave plasma (LMP) apparatus, at substrate temperatures T2 ranging from ambient to 250°C.Under otherwise nominally identical fabrication conditions, deposition rates were 10 to 25 times greater than those reported by others for radio- or audio-frequency plasmas.Based on film compositions, determined by elastic recoil detection (ERD), and measurements of such properties as density, refractive index, etch rate in dilute HF, and moisture permeation coefficient, our best P-SiN films (produced at T2 ≥ 200°C) are very similar to those reported in the literature.

Characterization of LPCVD of Silicon Nitride in a Rapid Thermal Processor

1989 ◽  
Vol 146 ◽  
Author(s):  
F. Scott Johnson ◽  
Roderick M. Miller ◽  
Mehmet C. Öztüirk ◽  
Jimmie J. Wortman
Keyword(s):  
Chemical Vapor Deposition ◽  
Silicon Nitride ◽  
Vapor Deposition ◽  
Chemical Vapor ◽  
Electrical Characteristics ◽  
Deposition Rates ◽  
Silicon Nitride Films ◽  
Tube Furnaces ◽  
Pressure Chemical

ABSTRACTLow pressure chemical vapor deposition of silicon nitride has been studied using a cold-walled, lamp heated, rapid thermal processor. Films were deposited at low presure using both silane and dichlorosilane, diluted in hydrogen and argon carrier gasses. The dichlorosilane and ammonia reaction was found to be unsuitable for use in the cold-walled system. Rapid thermal chemical vapor depositions using silane and ammonia did not result in “bullseye” non-uniformities reported for low presure depositions in conventional hot-walled tube furnaces. Ammonia to silane ratios of 120:1 were found to result in stoichiometric silicon nitride films. Deposition rates are well suited for dielectricapplications. Electrical characteristics are comparable to those of films deposited using APCVD and LPCVD methods.

Strong Visible Photoluminescence in Silicon Nitride thin Films Deposited at High Rates

1993 ◽  
Vol 325 ◽  
Author(s):  
Sadanand V. Deshpande ◽  
Erdogan Gulari ◽  
Steven W. Brown ◽  
S.C. Rand
Keyword(s):  
Thin Films ◽  
Silicon Nitride ◽  
Amorphous Silicon ◽  
Amorphous Materials ◽  
Visible Region ◽  
Chemical Vapor ◽  
Peak Position ◽  
Deposition Rates ◽  
Nitrogen Alloy ◽  
Hot Filament

AbstractAmorphous silicon nitrogen alloy (a-Si:Nx) thin films have been deposited using a novel hot filament chemical vapor deposition (HFCVD) technique. In this method, a hot tungsten filament is used to decompose ammonia to obtain highly reactive nitrogen precursor species which further react with disilane to form silicon nitride thin films. This allows for very high deposition rates ranging from 600 Å/min to 2500 Å/min at low substrate temperatures. These films deposited at high rates show strong photoluminescence (PL) at room temperature in the visible region when excited with the 457 nm line of Ar+ ion laser. Intrinsic defects introduced into the amorphous silicon nitride matrix due to the rapid deposition rates seem to give rise to the visible PL. The PL intensity is at least 8-10 times stronger than silicon nitride films deposited by conventional plasma enhanced CVD. PL peak position of this broad luminescence was varied in the visible region by changing the film stoichiometry (Si/N ratio). The PL peak energy also scales predictably with the refractive index and optical band gap of the films. These samples showed reversible PL fatigue and also have band edge tail states characteristic of amorphous materials.

Silicon nitride from microwave plasma: fabrication and characterization

1987 ◽  
Vol 65 (8) ◽  
pp. 859-863 ◽  
Author(s):  
Yves Tessier ◽  
J. E. Klemberg-Sapieha ◽  
S. Poulin-Dandurand ◽  
M. R. Wertheimer ◽  
S. Gujrathi
Keyword(s):  
Silicon Nitride ◽  
Etch Rate ◽  
Microwave Plasma ◽  
Ternary Mixtures ◽  
Audio Frequency ◽  
Elastic Recoil ◽  
Deposition Rates ◽  
Elastic Recoil Detection ◽  
Fabrication And Characterization ◽  
Substrate Temperatures

Plasma silicon nitride (P-SiN) films were prepared from SiH4–NH3 mixtures and from ternary mixtures with Ar or N2 in a large-volume microwave plasma apparatus, at substrate temperatures Ts ranging from ambient to 250 °C. Under otherwise nominally identical fabrication conditions, deposition rates were 10 to 25 times greater than those reported by others for radio-or audio-frequency plasmas. Based on film compositions determined by elastic recoil detection, and measurements of such properties as density, refractive index, etch rate in dilute HF, and the moisture permeation coefficient, our best P-SiN films (produced at Ts ≥ 200 °C) were very similar to those reported in the literature.

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