Interplay of microstructural features in Cr1−xAlxN and Cr1−x−yAlxSiyN nanocomposite coatings deposited by cathodic arc evaporation

The interplay between the deposition geometry, the chemical and phase composition, the crystallite size, the lattice strain and the direction and the degree of the preferred orientation of crystallites was investigated in the Cr_1−xAl_xN and Cr_1−x−yAl_xSi_yN nanocrystalline coatings and nanocomposites, which were deposited in cathodic arc evaporation process at different positions of substrates in the deposition apparatus. The different positions of the substrates affected primarily the distance between the samples and the cathodes and consequently the chemical and phase composition of the coatings, the crystallite size, the lattice strain and the preferred orientation of crystallites. In the Cr_1−xAl_xN coatings, the dominating cubic crystallites were preferentially oriented with their 〈111〉 direction perpendicular to the sample surface; this out-of-plane preferred orientation of crystallites was accompanied by a strong in-plane texture. In the Cr_1−x−yAl_xSi_yN coatings, a strong inclination of the {111} texture from the normal direction and a decay of the in-plane preferred orientation were observed in cubic crystallites with increasing silicon (and aluminium) contents.     

Effect of β grain growth on variant selection and texture memory effect during α → β → α phase transformation in Ti-6 Al-4 V

In the present study, the texture evolution and the role of β grain growth on variant selection during β → α phase transformation have been investigated in Ti-6 Al-4 V with and without 0.4 wt.% yttrium addition. The aim of adding yttrium was to control β grain growth above the β transus by pinning grain boundaries with yttria. Both materials were first thermomechanically processed to generate similar starting microstructures and crystallographic textures. Subsequently, both materials were solution-heat-treated above the β transus followed by slow cooling to promote growth of the α lath structure from grain boundary α. Additional interrupted slow cooling experiments were carried out to identify the α lamellae that nucleate first from β grain boundaries. Detailed electron backscatter diffraction analysis was carried out and it was found that the β heat treatment did not generate new texture components although the intensities of the individual components changed dramatically depending on the alloy/β grain size. Variant selection was assessed by comparing measured α texture components with predicted α texture components based on the high-temperature β texture assuming equal variant selection. It was found that with increasing β grain size variant selection intensified favouring the {φ1, Φ, φ2} {90°, 30°, 0°} texture component. Interrupted cooling experiments revealed that α nucleates first on β grain boundaries that are formed by two β grains having a common (1 1 0) normal and that these α lamellae display almost exclusively a {φ1, Φ, φ2} {90°, 30°, 0°} orientation. Consequently, the dominance of this variant with increasing β grain size can be related to the relative free growth of this particular α texture component into an “empty” β grain.     

Thickness Dependent Physical Properties of Thermally Evaporated Nanocrystalline CdSe Thin Films

This paper presents a study on thickness dependent physical properties of cadmium selenide thin films. The films of thickness 445, 631 and 810 nm were deposited employing thermal evaporation technique on glass and ITO-coated glass substrates followed by thermal annealing in air atmosphere at 200 °C. These films were subjected to X-ray diffractometer, UV–Vis spectrophotometer, scanning electron microscopy(SEM) and electrometer for structural, optical,surface morphological and electrical analysis respectively. The structural analysis reveals that the films are nanocrystalline in nature with cubic phase and preferred orientation(111). The crystallographic parameters such as lattice constant, interplanar spacing, grain size, internal strain, dislocation density, number of crystallites per unit area and texture coefficient are calculated and discussed. The optical band gap is found in the range 1.75–1.92 e V and observed to increase with thickness.The SEM study shows that the annealed films are uniform, fully covered and well defined. The electrical analysis shows that the conductivity is varied with film thickness and found within the order of semiconductor behavior.     

Stress and preferred orientation in nitride-based PVD coatings

Nitride-based coatings are nowadays widely studied both from fundamental and technological point of views due to their unique physical and mechanical properties. Among the binary nitrides, TiN is the most stable thermodynamically and has been widely used due to the combination of its covalent and metal-like characteristics. Coatings produced by Physical Vapor Deposition (PVD) techniques generally exhibit a crystallographic texture, which in turn may strongly affect their properties, such as hardness, wear resistance, or diffusion barrier properties in microelectronic devices. Therefore great efforts have been made in recent years to understand the underlying mechanisms governing texture development in nitride thin films. In particular, the issue of stress build-up during PVD growth and its possible interplay with film preferred orientation is essential to address.We present a brief overview of stress and preferred orientation in nitride-based thin films, either in the form of single-, multi-layered or nanocomposite coatings. X-ray Diffraction (XRD) was used in the standard θ-2θ configuration to study the texture development with film thickness, while the sin²ψ method combined with linear elasticity theory was employed to determine the complete strain/stress state. XRD measurements were made in the framework of the crystallite group method, which is of prime importance in thin films exhibiting a mixed texture, as it enables to selectively measure the elastic strain in a given subset of grains. For PVD films grown with energetic particles, the appropriate modeling requires the use of a triaxial stress tensor, including a hydrostatic stress component to take into account the local distortions induced by growth-defects. This approach enables us to determine the ‘stress-free and defect-free lattice parameter’, a₀, solely linked to chemical effect.Illustrations will be given for fiber-textured TiN and ZrN films deposited on Si substrates, epitaxial TiN layers as well as epitaxial TiN sub-layers in TiN/Cu multilayers grown on (001) MgO single crystal substrates. Ternary TiN-based coatings, either in the form of solid solutions or nanocomposites will be also investigated.     

Crystalline texture and magnetic anisotropy of Co-P films prepared by chemical deposition

Chemically deposited Co-P films with a P concentration of 2.5% have been studied by X-ray diffraction (Bragg geometry), electron microscopy, and magnetometry. The films have been found to represent a fine-grained medium in which the orientation of crystallites depends on the film thickness. At a thickness less than 70 nm, the films have a certain crystalline texture with a preferred orientation of the hexagonal axis c of the crystallites perpendicular to the film plane. With increasing film thickness, the character of the texture changes; the c axes of crystallites lie now predominantly in the film plane. At thicknesses exceeding 500 nm, the texture becomes stronger; the c axes are now distributed in the film plane equiprobably. These results can be used when producing magnetic media for longitudinal and transverse magnetic recording.     

热轧W80Cu20合金的织构演变分析

采用XRD织构测试仪在角度为0°~90°时测量W80Cu20合金及经多道次热轧后的不完整极图,应用三维取向分布函数(ODF)研究W-Cu合金热轧板材中织构的演变规律。结果表明:热轧前,W80Cu20合金的取向密度值接近1,织构强度很弱,取向不明显,认为没有织构出现;W80Cu20合金轧制变形后,织构强度增加,表现出明显的轧制织构特征,择优取向明显,织构的取向密度值较大,形成稳定的织构组分:Brass型织构取向{110}<112>、Copper型织构取向{211}<111>和旋转立方织构取向{200}<011>。     

Crystallographic Texture Evolution of ■-Fe_4N and Its Influences on Tribological Property of Nitrided Steel

The crystallographic texture of ■-Fe4 N in compound layer and its influences on the tribological properties of nitrided steel 38 Cr Mo Al are investigated in the study. The preferred orientation of(200)■ is produced by low-temperature nitriding in atmosphere with low nitrogen–hydrogen ratio and increases with the nitriding time. The preferred orientation of(220)■ appears after 72 h cyclic nitriding. The orientation relationships(0001)_ε//(101)_■ and [110]_ε//[111]_■,(111)_■//(0001)_ε and 011_■//[1■10]_g,(200)■//(110)_■ and [011]_■//[111]_■, as well as (1■03)_ε //(220)_■ and [0100]_ε//[1■0]_■ are established by first-principles method. The misfit of interatomic distance(δ), determining the phase transition resistance, is calculated. Accordingly, two reaction pathways during nitriding, ■→■ and ■→ε→■, are assumed, which determines the preferred orientations of ■-Fe_4 N. Results of wear tests demonstrate that the specimen with preferred orientation of(200)■ exhibits lower frictional coefficient and lower wear rate in comparison with the specimen with(220)■ preferred orientation.(111)■ texture usually relates to the lower frictional coefficient but higher wear rate due to the main slip system parallel to the sliding plane. Therefore, the(200)■ preferred orientation has a positive significance in improving the wear properties of steels.     

Cu/X(X=Cr,Nb)纳米多层膜力/电学性能的尺度依赖性

利用纳米压痕实验以及四探针法,系统研究了相同层厚Cu/X(X=Cr,Nb)纳米金属多层膜的力学性能(强/硬度)和电学性能(电阻率)的尺度依赖性.微观分析表明:Cu/X多层膜调制结构清晰,Cu层沿{111}面择优生长,X层沿{110}面择优生长.纳米压入结果表明,Cu/X多层膜的强度依赖于调制周期,并随调制周期的减小而增加.多层膜变形机制在临界调制周期(λ~c≈25 nm)由Cu层内单根位错滑移转变为位错切割界面.多层膜的电阻率不仅与表面/界面以及晶界散射相关,而且在小尺度下受界面条件显著影响.通过修正的FS-MS模型可以量化界面效应对多层膜电阻率的影响.Cu/X纳米多层膜可以通过调控微观结构实现强度-电导率的合理匹配.     

The crystallography of stress corrosion cracking in face centered cubic single crystals

The crystallography of transgranular stress corrosion cracking was studied for single crystals of α-brass (tested in 14 N NH₃), copper (tested in 1 M NaNO₂), and 304L austenitic stainless steel (tested in boiling 45 wt% MgCl₂). All fracture surfaces had characteristic flat parallel facets separated by crystallographic and/or fan-shaped steps. In α-brass and copper the facets consisted of {110} planes with the crystallographic steps following {111} planes. In 304L austenitic stainless steel cracking occurred primarily on the {100}, but secondary cracking on {110} was also found. Very smooth crystallographic-like steps were observed, generally following {100} planes. It is concluded that stress corrosion cracking in all systems tested occurred by cleavage. It is suggested that the stress corrosion cracks propagate on the lowest surface energy planes.     

COLD-ROLLING AND RECRYSTALLIZATION OF (110)[110] IRON-SILICON SINGLE CRYSTALS

After70-90% cold-rolling,strong{111}〈110〉and weak {111},〈112〉 cold-rolled tex- tures and perfect{111}〈112〉 recrystallization texture were obtained in Fe-Si single crys- tals.The cold-rolled textures with different orientations possesses different ability for recov- ery because of the difference of dislocation structure and store energy alter cold-rolling.The recovery taking place at{111}〈112〉orientation region was prior to that at{111}〈110〉 orientation region.hese subgrains with{111}〈112〉 orientation became recrvstallization nuclei during their growth at expending the surrounding matrix which was sluggish in recovery process.The development of recrystallization textures may be suggested as a process of “nucleation in-situ-selective growth”.The formation of(111)textures in low carbon steel sheets has been discussed in the light of this suggestion.     

Effect of Axial Magnetic Field on the Microstructure,Hardness and Wear Resistance of TiN Films Deposited by Arc Ion Plating

TiN films were deposited on stainless steel substrates by arc ion plating. The influence of an axial magnetic field was examined with regard to the microstructure, chemical elemental composition, mechanical properties and wear resistance of the films. The results showed that the magnetic field puts much effect on the preferred orientation, chemical composition, hardness and wear resistance of TiN films. The preferred orientation of the TiN films changed from(111) to(220) and finally to the coexistence of(111) and(220) texture with the increase in the applied magnetic field intensity. The concentration of N atoms in the TiN films increases with the magnetic field intensity, and the concentration of Ti atoms shows an opposite trend. At first, the hardness and elastic modulus of the TiN films increase and reach a maximum value at 5 m T and then decrease with the further increase in the magnetic field intensity. The high hardness was related to the N/Ti atomic ratio and to a well-pronounced preferred orientation of the(111) planes in the crystallites of the film parallel to the substrate surface. The wear resistance of the Ti N films was significantly improved with the application of the magnetic field, and the lowest wear rate was obtained at magnetic field intensity of 5 m T. Moreover, the wear resistance of the films was related to the hardness H and the H3/E*2 ratio in the manner that a higher H3/E*2 ratio was conducive to the enhancement of the wear resistance.     

Study on the orientation degree of Pb1 − xLaxTiO3 thin films by the rocking curve technique and its morphological aspects

Thin films of perovskite-type materials such as PbTiO₃, BaTiO₃, (Pb,La)TiO₃, (Pb, La)(Zr,Ti)O₃, KNbO₃, and Pb(Mg,Nb)O₃ have been attracting great interest for applications like non-volatile memories, ultrasonic sensors and optical devices. Thin film should be epitaxially grown or at least highly textured since the properties of this anisotropic material depend on the crystallographic orientation. For optical devices, in particular, an epitaxial thin film without defects are essential to reduce optical propagation losses. Pb_1 − xLa_xTiO₃ (PLT) where x = 0, 13 and 27% thin films were prepared by a chemical method (polymeric precursors method), and deposited by the spin coating technique onto substrates of SrTiO₃ (STO) and LaAlO₃ (LAO). The films were then heat treated at 500 °C in a controlled atmosphere of O₂. The orientation degree of the thin films was obtained from rocking curve technique, by means of X-ray diffraction analysis. A microstructural study revealed that the films were crack-free, homogeneous and have low roughness.     

对向靶溅射TiN薄膜的结构和物性

利用对向靶溅射（ＦＴＳ）沉积出（１１１）择优取向的单相ＴｉＮ膜，膜硬度（ＨＶ）最高可达３８００，择优取向随基板偏压增高，可由（１１１）转向（２００），晶格常数随氮气分压增高而增大，这是氮原子进入四面体间隙引起的。     

NON-EQUILIBRIUM SEGREGATION STRUCTURE OF P IN COLD ROLLED Fe-P ALLOYS AND ITS RELATION WITH TEXTURE VARIATION

The relations between the non-equilibrium segregation process of P and the change of thetexture in Fe-P alloys have been studied by analytical electron microscope and orientationdistribution function.It was shown that P segregated preferentialy on the{110}slip planes,the P segregation structures with repeating cycle a=1.582 nm form at 450℃.<001>//ND direction abated.<111>//ND direction heightened.And{111}<110>has a tendancyto transform into{111}<143>texture in recovering process.{111}<143>direction trans-forms into{111}<112>direction after recrystalizing.A model to describe the effects ofnon-equilibrium segregation structures of P on orientation change was proposed and em-ployed to interpret the experiment results.     

Twin formation during the atomic deposition of copper

Vapor deposited copper films with 〈111〉 growth texture usually contain twin plates stacked normal to the growth direction. However, twins are rarely seen when growth occurs in other principle crystallographic directions. Atomistic modeling indicated that during 〈111〉 growth, adatoms occupied either parent or twin surface lattice sites with almost equal probability, resulting in a high nucleation density of twin domains. During growth on either {110} or {100} surfaces, adatoms were only able to occupy parent lattice sites, and no twin nucleation occurred. A phase field method was used to model the twin domain evolution during 〈111〉 growth as a function of deposition rate and temperature. Simulation results indicated that twin domains evolved by rapid lateral expansion with very little vertical thickening. The lateral expansion was found to be fast compared with the deposition rate, and as a result twin domains usually grew to occupy the entire width of a growth column, in good agreement with experimental observations. The model indicated that the twin structures formed during the 〈111〉 growth of copper are not directly controllable by either the processing temperature or the deposition rate.     

Crystallographic analysis of the martensitic transformation in medium-carbon steel with packet martensite

Based on X-ray diffraction studies of the martensite texture in a single martensite packet, exact orientation relationships between the orientations of martensite crystallites and the original austenite single crystal in medium-carbon steel 37KhN3A have been determined to be as follows: (011)_α||(1; 0.990; 1.009)_γ to an accuracy of \( \pm 0.15^\circ ,{\left[ {01\overline 1 } \right]_\alpha }||{\left[ {1;1.163; - 2.133} \right]_\gamma }\) to an accuracy of ±0.15°. It has been shown that the orientation relationships proved to be almost the same as in the Fe–31% Ni alloy with a twinned martensite with close lattice parameters. Therefore, the conclusion has been drawn that the mechanism of the lattice deformation upon the martensitic transformation is the same in both alloys. It is described as follows. The lattice deformation occurs by shear on the (111) plane in the \({\left[ {11\overline 2 } \right]_{_\gamma }}\) direction and is accompanied by an additional change in the dimensions in the mutually perpendicular directions \({\left[ {11\overline 2 } \right]_{_\gamma }},\left[ {111} \right],\;and{\left[ {1\overline 1 0} \right]_{_\gamma }}\). The invariantlattice deformation is implemented by slip in martensite on the planes of the (112)_α type in the direction \({\left[ {\overline 1 \overline 1 1} \right]_\alpha }\). One of the 24 crystallographically equivalent variants of the transformation mechanism has been considered. Apart from this type of deformation, an additional deformation of martensite is possible that does not change its orientation. It has been shown that the orientation of the martensite crystallite calculated via the phenomenological theory of the martensitic transformations (PTMT) differs by approximately 1° from the experimentally determined orientation. This refers to both the lath and twinned martensite. In the twinned martensite, the invariant plane obtained in the PTMT calculations and the habit plane coincide. In lath martensite of 37KhN3A steel, the invariant plane of the martensite crystal obtained in PTMT calculations deviates by ~25° from the orientation of the surface of the martensite plate (habit plane), which is close to the (111)_γ plane. An explanation of this phenomenon is given.     

Morphology and texture evolution of FeCrAlTi-Y2O3 foil fabricated by EBPVD

An electron beam physical vapor deposition method was used to fabricate freestanding Y₂O₃ dispersive strengthened FeCrAlTi foils for high-temperature applications. The vapor incidence mode was found to have great impact on the morphology and crystallographic orientation of the foils. Under symmetric vapor incidence mode, an out-of-plane < 100> fiber texture was formed. While under asymmetric vapor incidence mode, both out-of-plane preference of < 111> direction and several in-plane preferences were developed. As the deposition proceeded, the extent of in-plane orientation increased, and the preferred out-of-plane orientation increasingly deviated from the surface normal. The vapor incidence mode played a role on the growth rate of < 100> direction and < 110> direction, by which the morphology and crystallographic orientation of grains were modified.     

柱状晶对Fe-3%Si电工钢冷轧织构演变规律的影响

Fe-3%Si电工钢铸锭中普遍存在柱状晶,其晶体学及形状各向异性对随后的热轧、冷轧及退火织构产生很大的影响.利用xRD与EBSD技术对长轴分别平行于轧面法向(ND),轧制方向(RD)和横向(TD)的柱状晶冷轧样品的织构及组织进行了研究,并对晶界的特殊作用进行了分析.结果表明,中等压下量下,3种柱状晶样品具有不同程度的{001}织构遗传性,即3种样品均不同程度的摆脱了{111}线织构的形成;柱状晶长轴平行于ND和TD时,{001}取向在冷轧时得到大的保留;柱状晶长轴平行于RD时,得到最强的{111}〈112〉织构;柱状晶长轴平行于TD时,冷轧组织中旋转立方织构及{111}〈110〉织构较强.此外,3种样品的织构均表现出由立方→{001}〈130〉→{113}〈251〉的过渡路径,与等轴多晶样品沿α线和γ线转动的路径不同.不同方向的柱状晶晶界对冷轧变形过程中晶粒转动的作用不同,但因晶粒尺寸大而作用有限,且与初始取向相关.     

Crystallography and structural evolution during reverse transformation in an Fe–17Cr–0.5C tempered martensite

The mechanism and the crystallography of austenite and δ-ferrite formation from tempered martensite at temperatures of 900–1200°C have been studied by means of transmission electron microscopy in an Fe–17Cr–0.55C alloy. It was found that austenite nucleates within ferrite at low angle, high angle and twin-related lath boundaries as well as at high angle equiaxed grain boundaries in contact with M₂₃C₆ grain/lath boundary carbides. The austenite grains are in a cube–cube relationship with the M₂₃C₆ carbide particles and bear the Kurdjumov–Sachs orientation relationship with at least one of the adjacent ferrite grains. They are often in the Kurdjumov–Sachs relationship with both ferrite laths separated by a high angle boundary as far as the laths had formed from the same austenite. The {111}_A close packed plane of γ precipitate is parallel to the {110}_F plane most parallel to the grain boundary. The close packed planes of some austenite grains nucleating at the high angle lath boundaries are parallel to the close packed planes of both ferrite laths. These crystallographic features often result in a single variant of austenite orientation at a grain boundary. After nucleation, the austenite grains grow by the migration of both semicoherent and incoherent interfaces. These results demonstrate that a specific orientation relationship is preferred for the austenite nucleation, but is not necessary for the subsequent growth. The kinetics of austenite growth are controlled by chromium diffusion. The δ-ferrite particles precipitate at high temperatures as a non-equilibrium phase. No rational orientation relationship between δ-ferrite and retained austenite was found. The experimental results are discussed qualitatively in terms of the thermodynamic predictions using the software ThermoCalc, assuming local equilibrium at the moving interfaces.     

Microstructure and Physical–Mechanical Properties of (TiAlSiY)N Nanostructured Coatings Under Different Energy Conditions

Nanostructured multicomponent (TiAlSiY)N coatings were fabricated by the cathodic-arc physical vapor deposition (CA-PVD). In this study, a bias potential applied to the substrate was ??200 and ??500 V, and changes in structure and properties of coatings were investigated. Samples had a single-phase state with a face-centered cubic (FCC) lattice. Small crystallites of about 7.5 nm and texture with [110] axis were observed at ??500 V. However, lower bias potential resulted in the formation of crystallites of about 41.6 nm with [111] preferred orientation. Moreover, coatings were characterized by superhard state and demonstrated low wear, high abrasion and crack resistance. The testing of the polycrystalline cubic boron nitride (PCBN) cutting inserts covered with (TiAlSiY)N revealed an increase in the tool life coefficient during cutting by 1.66 times in comparison with the base tool material. Therefore, (TiAlSiY)N coating is a perspective material for application as a protective layer in cutting tools.