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1.
This study represents one of the first attempts to deposit multicomponent (more than three components) thin films by magnetron sputtering of multiphase composite targets (three phases or even more). Films of Ti-Si-C-N were synthesized through dc magnetron sputtering of xTiC+yTi3SiC2+zA composite targets (A was TiSi2, SiC, or a mixture of these phases) in an argon atmosphere or in a gaseous mixture of argon and nitrogen. The as-deposited films were characterized using Auger electron spectroscopy, X-ray diffraction, transmission electron microscopy using selected area electron diffraction and high-resolution techniques, and microhardness. It was shown that the substrate temperature and the nitrogen concentration in the reactive gas had a strong influence on the structure and the composition of the as-deposited films. The films deposited from the Si-poor targets were either polycrystalline or contained a mixture of nanocrystalline and amorphous phases. An amorphous phase formed as individual grains rather than as intergrain amorphous layers. All films deposited from the Si-rich target were amorphous in nature. Particular attention has been paid to the atomic structure of grains and grain boundaries in the crystalline films. Polycrystalline grains contained a high density of dislocations and exhibited a curved appearance of the lattice fringes that is probably due to the presence of the long-range stress fields. The measurements of the lattice parameters using the selected area electron diffraction pattern (SA EDP) method indicated, with a high probability, that the polycrystalline grains consist of clusters of atoms with varying compositions. The grain boundaries in the nanocrystalline Ti-Si-C-N films had both ordered and disordered regions, although some regions close to the interface exhibited neither a fully crystalline nor a homogeneously amorphous structure. The atomic structure of an interface was shown to depend on the orientation relationship between adjacent grains. The atomic planes were perfectly matched when the two grains were oriented close to the [110] fcc1//[110] fcc2 zone axis. However, the interface dislocations were frequently observed at or near the grain boundary when [110] fcc1//[001] fcc2. The contribution of compressive stress as determined by an increase in the fcc lattice parameter is also discussed.  相似文献   

2.
The binary Cu-Nb system is rather interesting, because Cu and Nb are virtually immiscible in the solid state, exhibit a relatively strong clustering (phase separating) tendency in the liquid state, and therefore can only be alloyed in a highly metastable form, for example, by vapor quenching techniques such as sputtering. In this article, metastable amorphous Cu-Nb alloy thin films with nominal compositions of Cu-45 at. pct Nb have been deposited by magnetron cosputtering. The amorphous phase in these thin films exhibits nanoscale phase separation in the as-deposited condition. The early stages of devitrification of this amorphous phase have been investigated using three-dimensional atom probe tomography coupled with transmission electron microscopy. The results indicate that devitrification of this phase-separated amorphous phase is initiated by the formation of nanoscale fcc Cu-rich grains uniformly distributed in the amorphous matrix. These nanoscale fcc Cu-rich grains are often faulted and appear to retain some Nb supersaturation. The role of the nanoscale phase separation in the as-deposited amorphous film on the subsequent devitrification is discussed in the context of free energy–composition plots for this system. This article is based on a presentation given in the symposium entitled “Materials Behavior: Far from Equilibrium” as part of the Golden Jubilee Celebration of Bhabha Atomic Research Centre, which occurred December 15–16, 2006 in Mumbai, India.
Rajarshi Banerjee (Associate Professor)Email:
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3.
The precipitation, dissolution, and reprecipitation processes of Al2Cu (θ phase) in Al-2 wt pct Cu thin films were studied. The films were characterized in the as-deposited condition, after annealing at 425 °C for 35 minutes, and after rapid thermal annealing (RTA) at 345 °C, 405 °C, and 472 °C. In the as-deposited samples, the precipitates had a fine even distribution throughout the thin film both at aluminum grain boundaries and within the aluminum grains. Annealing below the solvus temperature caused the grain boundary precipitates to grow and precipitates within the center of aluminum grains to diminish. Annealing above 425 °C caused the θ-phase precipitates to dissolve. Upon cooldown, the θ phase nucleated at aluminum grain boundaries and triple points in the form of plates.In situ heating and cooling experiments documented this process in real time. Analytical microscopy revealed that there is a depletion of copper at the aluminum grain boundaries in regions free of precipitates. The θ-phase precipitates nucleated and grew at the grain boundariesvia a collector plate mechanism and drew copper from the areas adjacent to the aluminum grain boundaries. This paper is based on a presentation made in the symposium “Interface Science and Engineering” presented during the 1988 World Materials Congress and the TMS Fall Meeting, Chicago, IL, September 26–29, 1988, under the auspices of the ASM-MSD Surfaces and Interfaces Committee and the TMS Electronic Device Materials Committee.  相似文献   

4.
Electron microscopy has been used to study the structure of Ni-P electrodeposited thin films with 7, 12, 20 and 22 at. pct P. For the crystalline as-deposited films with 7 and 12 at. pct P (low P films), the crystal structure is fcc and the grains are a supersaturated solid solution of P in Ni. Grain size decreases with increasing P content; the present findings agree with previous ones. For “amorphous” as-deposited films with 20 and 22 at. pet P (high P content films) the amorphous phase is not completely homogeneous and there are regions in which small microcrystals exist. Electron beam heating a low P con-tent film causes the crystalline array of supersaturated Ni grains to decompose to an equilibrium mixture of Ni and Ni3P; both types of grains are randomly oriented. Electron beam heating a high P content film causes the amorphous regions to undergo several complex transformations. The first reaction to occur is: Amorphous (Ni-P) -NixPy + Ni (random) where NixPy is a newly discovered phase with a variable composition. Further beam heating causes a second transformation to equilibrium phases: NixPy + Ni → Ni3P + Ni (random). The microstructure resulting from the above transformations depends on variations in composition of the as-deposited specimens, rates of heating and temperature gradients. The mode of phase transformation in microcrystalline regions and amorphous regions is distinctly different. Crystallization in amorphous regions occurs by a nucleation and growth of NixPy, and Ni; a crystallization front is seen to advance into the amorphous re-gion. Crystallization in microcrystalline regions occurs by nucleation and growth of the Ni3P phase and grain coarsening of the Ni phase. No distinct crystallization front is ob-served.  相似文献   

5.
A method is described for the transmission and scanning electron microscope study of the relationship between the microstructure and the fracture properties of two quenched and tempered, electron beam melted, modified SAE 4620 steels consisting of tempered low carbon martensite. Among all the microstructure constituents considered, the constituentR (randomly oriented, “tempered low carbon martensite, TLCM”) achieved the highest probability for dimple fracture. The thick TLCM laths (designated as the microstructure constituent II) exhibited higher probability of dimple plus quasi-dimple mode of fracture than the thin laths (I). It is concluded that the steel EB1035 derived the high toughness from a) the high concentration of the “high toughness” microstructure constituentsR and II, b) “non-embrittled” prior austenite grain boundaries with 50 pct probability for smooth plus quasi-smooth mode and 50 pct dimple plus quasi-dimple mode of intergranular fracture. In contrast, besides having low content ofR and II, the steel EB1014 displayed “completely embrittled” prior austenite grain boundaries with 100 pct probability for smooth plus quasi-smooth intergranular fracture. The conclusions derived from the microconstituentsR, II and I seemed to reflect the “embrittling” effect of decreased spacings between the pseudo twin related laths and between the lath boundary cementite films, and the “toughening” effect of the randomly oriented laths. Auger spectra obtained from the fracture surface before and after sputtering is analyzed to determine the presence of grain boundary sulfur segregation.  相似文献   

6.
The composition of thin films of superconducting Sr-Bi-Ca-Cu-Pb ceramic, deposited by magnetron sputtering from targets prepared from oxide powders of the corresponding elements, was investigated. It was found that the film composition differs from that of the target. Microprobe analysis of target and films can be used to determine the correct target composition for the deposition of a superconducting film.Materials Science Institute, Ukrainian Academy of Sciences, Kiev. Translated from Poroshkovaya Metallurgiya, Nos. 5–6, pp. 27–30, May–June, 1996. Original article submitted May 25, 1994.  相似文献   

7.
采用低压等离子喷涂成形技术制备了片状及回转体钼靶材,研究了钼靶材孔隙率、氧含量、微观结构、显微硬度及拉伸强度等性能,开展了片状钼靶材的磁控溅射镀膜研究。研究结果表明:低压等离子喷涂成形钼靶材为典型的定向凝固柱状晶层片结构,层片界面结合紧密,孔隙率约1.1%、氧质量分数为0.18%,显微硬度为HV0.025 361.8,抗拉强度达到373.2 MPa,各项指标均明显优于大气等离子喷涂成形钼制品。低压等离子喷涂成形片状钼靶材可磁控溅射沉积出平整、致密、连续的钼薄膜,镀膜厚度约700 nm,X射线衍射谱线表明钼薄膜为体心立方结构,沿(110)方向择优生长。磁控溅射离子的均匀轰击导致钼靶材表面快速溅射及均匀减薄,溅射表面及截面较为平整光滑,溅射凹坑均为纳米级。  相似文献   

8.
Laser-assisted sputter deposition has been used to deposit thin metallic films onto ceramic substrates. This process allows the building of a film of arbitrary thickness by sequential deposition of 5- to 150-nm-thick layers alternating with laser melting. Highly adherent films of copper on sapphire and on quartz were obtained. Pulsed-laser treatment also enhances the adhesion of nickel films to sapphire substrates. This critical step in the process is the laser irradiation following each of the initial depositions. In these early stages, an interfacial reaction between film and substrate takes place during laser irradiations. An interfacial compound forms whose nature has been studied by transmission electron microscopy. The morphological features of the film, as well as the amount of film removed during these first irradiations, were analyzed as a function of laser energy density by scanning electron microscopy and by energy dispersive X-ray spectroscopy. The results were correlated with computer simulations of the thermal response of the two-media system to laser heating. The role of the interfacial thermal conductivity during laser processing is analyzed. The state of the substrate,e.g., annealed or as-polished, influences the morphology of the irradiated film. This effect is related to an enhancement of interfacial thermal conductivity. This invited paper is based on a presentation made in the symposium “Structure and Properties of Fine and Ultrafine Particles, Surfaces and Interfaces” presented as part of the 1989 Fall Meeting of TMS, October 1–5, 1989, in Indianapolis, IN, under the auspices of the Structures Committee of ASM/MSD.  相似文献   

9.
采用磁控共溅射方法分别制备了含有W和Mo两种不同成分的铜系薄膜,用EDX、XRD、SEM和纳米压痕仪对薄膜成份、结构、形貌和显微硬度进行了分析。结果表明,制备出的Cu—W和Cu-Mo薄膜均呈晶态结构,Cu-W和Cu—Mo形成了均匀的固溶体;经650℃热处理1h后,Cu—W和Cu—Mo薄膜中晶粒长大,有富w和富Mo相从基体Cu相中弥散析出;Cu-W薄膜的显微硬度随W成分的增加先增加后降低;Cu—Mo薄膜的显微硬度随Mo成分的增加而持续升高,薄膜退火态的显微硬度低于沉积态。分析认为,以上结果的产生均因添加W、Mo所引起的晶粒细化效应和薄膜的热稳定性较差所致。  相似文献   

10.
In order to develop a highly sensitive material for nondestructive testing (NDT), (Tb0.3Dy0.7)Fe1.95 thin films were deposited on FeCo substrates at room temperature by magnetron sputtering and annealed. The magnetostrictive properties and the detection efficiency of the composite films were investigated. Results demonstrate that the detection efficiency roughly shows regular consistency with the magnetostrictive strain of the TbDyFe films. Heat treatment has a great effect on the crystalline state and the magnetostrictive strain of the composite materials. The as-deposited (Tb0.3Dy0.7)Fe1.95 films are amorphous, and the saturation magnetostriction (λs) is only 90 ppm. However, the nanostructured crystalline REFe2 is partially separated out in amorphous matrix after annealing at 600 °C for 1 h, and the λs increases to 265 ppm. Simultaneously, the detection efficiency of the composite materials is obviously improved compared to that of the as-deposited films. The detection signal of traditional FeCo strip is 0.4 V at the excitation power of 1.0 P and frequency of 128 kHz and that of the strip increases significantly by depositing one layer of (Tb0.3Dy0.7)Fe1.95 film. The detection signal of the composite material annealed at 600 °C is the best, even reaching saturation value of 2.5 V (1.0 P, 128 kHz). The results may provide us with a method for preparing new materials for NDT.  相似文献   

11.
During the last 2 decades, research on high-temperature, oxidation-resistant coating systems for refractory metals has focused on a variety of silicides (e.g., Mo and Ta silicides), due to their excellent resistance to oxidation. However, commercialization efforts have been thwarted in large measure due to the diffusion of silicon from the coating to the substrate, resulting not only in the depletion of silicon from the coating, but also the formation of less oxidation-resistant subsilicides. Consequently, the development of a high-temperature, diffusion barrier layer for silicon has assumed considerable importance. Furthermore, introduction of carbon in the system, e.g., during the synthesis of MoSi2-SiC composite thin films on molybdenum substrates, results in the diffusion of both silicon and carbon into the substrate, necessitating the development of a barrier layer for both elements. This article examines the possibility of using a novel approach—that of reactive radio frequency (RF) sputtering—for synthesizing a diffusion barrier (based on the Mo-Si-C-N quaternary system) for both silicon and carbon. It is shown that reactive rf magnetron sputtering of a composite target (MoSi2 + 1.96 moles SiC) in an argon-nitrogen atmosphere results in the formation of an amorphous layer, of an as-yet undetermined stoichiometry, preventing the diffusion of both silicon and carbon into the molybdenum substrate. This layer is thermally and chemically stable up to at least 1260 °C. Submission of a patent application has been made.  相似文献   

12.
The feasibility of solidifying uniformly aligned composites from alloys of hypermonotectic composition was investigated through the use of organic analogues and a directional solidification temperature gradient stage. Previously demonstrated macrostructurally detrimental effects due to coalescence and/or preferential wetting (or lack of) by the excess LII phase have been taken advantage of by the inclusion of constrained fibers aligned parallel to the growth direction. Upon passing through the miscibility gap,L II droplets are shown to attach and grow along the fibers prior to the monotectic reaction, resulting in a uniform composite. The results of different fiber materials in combination with “wetting” and “nonwetting” miscibility gap systems are presented and discussed in reference to processing in a microgravity environment.  相似文献   

13.
采用磁控溅射设备和经过不同温度热处理的Mo靶材,以相同的溅射工艺参数,在Si基片上制备了Mo金属薄膜,研究了靶材的热处理温度对Mo薄膜组织和性能的影响。研究结果发现,所制备Mo薄膜均呈现(110)晶面择优取向,而靶材热处理温度的升高能够提高(110)晶面的择优取向程度。所有薄膜均为T型低温抑制生长。比较结果表明:经1 200℃热处理的Mo靶材溅射率最高(18.5 nm/min),且其溅射膜具有较小的方阻值和较好的厚度均匀性,综合性能最优。  相似文献   

14.
During the last 2 decades, research on high-temperature, oxidation-resistant coating systems for refractory metals has focused on a variety of silicides (e.g., Mo and Ta silicides), due to their excellent resistance to oxidation. However, commercialization efforts have been thwarted in large measure due to the diffusion of silicon from the coating to the substrate, resulting not only in the depletion of silicon from the coating, but also the formation of less oxidation-resistant subsilicides. Consequently, the development of a high-temperature, diffusion barrier layer for silicon has assumed considerable importance. Furthermore, introduction of carbon in the system, e.g., during the synthesis of MoSi2−SiC composite thin films on molybdenum substrates, results in the diffusion of both silicon and carbon into the substrate, necessitating the development of a barrier layer for both elements. This article examines the possibility of using a novel approach—that of reactive radio frequency (RF) sputtering—for synthesizing a diffusion barrier (based on the Mo−Si−C−N quaternary system) for both silicon and carbon. It is shown that reactive rf magnetron sputtering of a composite target (MoSi2 +1.96 moles SiC) in an argon-nitrogen atmosphere results in the formation of an amorphous layer, of an as-yet undetermined stoichiometry, preventing the diffusion of both silicon and carbon into the molybdenum substrate. This layer is thermally and chemically stable up to at least 1260 °C. Submission of a patent application has been made. S. GOVINDARAJAN, formerly Graduate Student, Department of Metallurgical and Materials Engineering, Colorado School of Mines  相似文献   

15.
We compare two types of tests for measurement of mechanical properties of thin films and small scale structures: a microtensile test and a thermomechanical fatigue test induced by alternating current at low frequency and high current density. The microtensile test was used as a reference for evaluating the feasibility of using the electrical test for measurement of mechanical properties. Tests were performed on structures cofabricated from thin film Al deposited on Si to ensure comparable mechanical properties. The films had a grain diameter of 220 nm and a thickness of 1.9 μm. The electrical test resulted in an estimated ultimate tensile strength of 250 ± 40 MPa. This value was based on extrapolation of high-cycle fatigue data to one reversal through a modified Basquin equation while accounting for varying mean stress. An ultimate tensile strength of 239 ± 4 MPa was determined from the microtensile test. Differences between these values are explained in terms of the effects of substrate constraint on the strength of the thin film. We conclude that electrical testing methods offer a feasible means for measuring mechanical properties of individual patterned structures. This article is based on a presentation given in the symposium entitled “Deformation and Fracture from Nano to Macro: A Symposium Honoring W.W. Gerberich’s 70th Birthday,” which occurred during the TMS Annual Meeting, March 12–16, 2006 in San Antonio, Texas and was sponsored by the Mechanical Behavior of Materials and Nanomechanical Behavior Committees of TMS.  相似文献   

16.
谢波玮  李弢  古宏伟 《稀有金属》2006,30(3):407-410
用射频磁控溅射法在快速热处理过的Pt/Ti/SiO2/Si(100)基体上制备了Ba0.7sr0.3TiO3薄膜。通过引入溅射因子α,在相同工艺条件(高温大功率溅射)下,对靶材成分进行调整,使薄膜成分无化学计量比偏离。薄膜成相较未调整前有显著改善,低角区的衍射杂峰消失。{100}方向有择优生长,同体材料及sol-gel法制备的BST薄膜有明显不同,研究认为是成分调整后,薄膜成分无偏离所致。  相似文献   

17.
The microstructures and mechanical properties of a family of sputter-deposited Cu1−x Ta x (0<x<0.18) alloys have been investigated. The as-deposited microstructures for all film compositions consisted of a polycrystalline, face-centered-cubic (fcc) Cu matrix, with varying levels of Ta in solid solution, plus a very high density of discrete, 1 to 3 nm, fcc Ta particles. Decreased deposition temperature (−120 °C vs 100 °C) increased the level of Ta in solid solution. After annealing (900 °C for 1 hour) the as-deposited 6 at. pct Ta films, the Cu matrix grains remained submicron and the Ta particles remained fcc with no apparent particle coarsening. Additionally, the fcc Ta particles were found before and after annealing to be oriented identically with the Cu matrix and aligned on {111} and {100} habit planes. Annealing 17 at. pct Ta films at 900 °C for 1 hour resulted in the formation of body-centered-cubic (bcc) Ta particles (>50-nm diameter) in addition to the much smaller fcc Ta particles. Annealing the low and high Ta composition films at 900 °C for as long as 100 hours produced no observed change in either the Cu matrix grain size or the size and distribution of the fcc and bcc Ta particles. Microhardness and nanoindentation mechanical property evaluations of bulk hot-pressed materials indicated that the high strengths of the composites were unchanged, even after annealing for 100 hours at 900 °C.  相似文献   

18.
The transmission electron microscopy (TEM) and X-ray characterization of lattice distortion forms caused by low-energy Ar+ bombardment of grown thin silicon films on a silicon (001) substrate were studied. The isotropic case (of spherical distortions) takes place in epitaxial silicon “as grown” processes. The intensity distribution consists of two maxima—one from the distorted layer and the other from the original unaffected silicon lattice. Significant changes in the 2θ location, peak broadening, and integrated intensity from the (004)* reflections were obtained as functions of aging temperatures. First, aging heat treatment, affects the distribution of distortions obtained from local regions at the “as grown” layer, which changes to a special topography of continued distortions at higher aging temperatures. At aging temperatures above 923 K (650 °C), this extra diffraction peak disappears. The TEM observations reveal the appearance of dislocation lines with dark and bright contrasts around the lines and interdislocation strain contrasts and disorder of Ar atoms in Si matrix regions with coherent interfaces.  相似文献   

19.
Mechanical properties of thin films   总被引:20,自引:0,他引:20  
The mechanical properties of thin films on substrates are described and studied. It is shown that very large stresses may be present in the thin films that comprise integrated circuits and magnetic disks and that these stresses can cause deformation and fracture to occur. It is argued that the approaches that have proven useful in the study of bulk structural materials can be used to understand the mechanical behavior of thin film materials. Understanding the mechanical properties of thin films on substrates requires an understanding of the stresses in thin film structures as well as a knowledge of the mechanisms by which thin films deform. The fundamentals of these processes are reviewed. For a crystalline film on a nondeformable substrate, a key problem involves the movement of dislocations in the film. An analysis of this problem provides insight into both the formation of misfit dislocations in epitaxial thin films and the high strengths of thin metal films on substrates. It is demonstrated that the kinetics of dislocation motion at high temperatures are expecially important to the understanding of the formation of misfit dislocations in heteroepitaxial structures. The experimental study of mechanical properties of thin films requires the development and use of nontraditional mechanical testing techniques. Some of the techniques that have been developed recently are described. The measurement of substrate curvature by laser scanning is shown to be an effective way of measuring the biaxial stresses in thin films and studying the biaxial deformation properties at elevated temperatures. Submicron indentation testing techniques, which make use of the Nanoindenter, are also reviewed. The mechanical properties that can be studied using this instrument are described, including hardness, elastic modulus, and time-dependent deformation properties. Finally, a new testing technique involving the deflection of microbeam samples of thin film materials made by integrated circuit manufacturing methods is described. It is shown that both elastic and plastic properties of thin film materials can be measured using this technique. The Institute of Metals Lecture was established in 1921, at which time the Institute of Metals Division was the only professional division within the American Institute of Mining and Metallurgical Engineers Society. It has been given annually since 1922 by distinguished men from this country and abroad. Beginning in 1973 and thereafter, the person selected to deliver the lecture will be known as the “Institute of Metals Division Lecturer and R.F. Mehl Medalist” for that year. WILLIAM D. NIX, Professor, obtained his B.S. degree in Metallurgical Engineering from San Jose State University, San Jose, CA, and his M.S. and Ph.D. degrees in Metallurgical Engineering and Materials Science, respectively, from Stanford University, Stanford, CA. He joined the faculty at Stanford in 1963 and was appointed Professor in 1972. In 1964, Professor Nix received the Western Electric Fund Award for Excellence in Engineering Instruction and, in 1970, the Bradley Stoughton Teaching Award of ASM. He received the 1979 Champion Herbert Mathewson Award and, in 1988, was the Institute of Metals Lecturer and recipient of the Robert Franklin Mehl Award of TMS-AIME. He was elected Fellow of the American Society for Metals in 1978 and elected Fellow of TMS-AIME in 1988. He also received a Distinguished Alumnus Award from San Jose State University in 1980, and he served as Chairman of the 1985 Gordon Conference on Physical Metallurgy. In 1987, he was elected to the National Academy of Engineering. In 1966, he participated in the Ford Foundation's “Residence in Engineering Practice” program as Assistant to the Director of Technology at the Stellite Division of Union Carbide Corporation. From 1968 to 1970, Professor Nix was Director of Stanford's Center for Materials Research. Professor Nix is engaged in research on the mechanical properties of solids. He is principally concerned with the relation between structure and mechanical properties of materials in both thin film and bulk form. He is coauthor of about 190 publications in these and related fields. Professor Nix teaches courses on dislocation theory and mechanical properties of materials. He is coauthor of “The Principles of Engineering Materials,” published in 1973 by Prentice-Hall, Incorporated, Englewood Cliffs, NJ.  相似文献   

20.
The effect of structure, phase composition and method of preparation on the cavitation resistance of composite eutectic coatings was investigated. It was established that a finely dispersed columnar eutectic structure provided maximum resistance to crack growth. Methods for producing the desired coating structure by the use of concentrated energy sources are proposed. Ukraine National Technical University “KPI.”. Translated from Poroshkovaya Metallurgiya, Nos. 7–8(402), pp. 36–43, July–August, 1998.  相似文献   

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