退火温度对溅射Al膜微结构及应力的影响

用直流溅射法在Si基片上制备了 2 5 0nm厚的Al膜 ,并在不同退火温度下进行退火处理 ,用X射线衍射和光学干涉相位移法对薄膜的微结构及应力随退火温度的变化进行了研究。结构分析表明 :退火后的Al膜均呈多晶状态 ,晶体结构仍为面心立方 ;随着退火温度由 2 0℃升高到 4 0 0℃ ,薄膜的平均晶粒尺寸由 2 2 8nm增加到 2 5 1nm ;薄膜晶格常数在不同退火温度下均比标准值 4 0 4 96 A稍小。应力分析表明 :随退火温度的升高 ,Al膜应力减小 ,30 0℃时平均应力减小为 2 730× 10 8Pa且分布均匀 ;在 4 0 0℃时选区范围内应力差仅为 3 82 8× 10 8Pa。     

退火温度对硅基溅射银膜微结构和应力的影响

用直流溅射法在硅(111)基底上制备银膜，膜厚为380nm。用BGS6341型电子薄膜应力分布测试仪对膜应力随退火温度的变化进行了研究，结果表明：膜应力随着退火温度的升高而增大，在400℃退火温度下膜应力变化明显。用MXP18AHF型X射线衍射仪测量了膜的衍射谱，对膜微结构随退火温度的变化进行了讨论。制备的Ag膜仍为面心立方结构，呈多晶状态，平均晶粒尺寸为23．63nm，薄膜晶格常数(0．40805nm)比标准样品晶格常数(0．40862nm)稍小。     

ZnS薄膜的制备及性能研究

用射频溅射法在Si基片和石英基片上分别制备了490nm厚的ZnS薄膜,并在不同温度下进行退火处理.微结构分析表明:退火后的ZnS薄膜均呈多晶状态,晶体结构为立方闪锌矿结构的β-ZnS;随着退火温度的升高,薄膜的平均晶粒尺寸逐渐增大,由20℃的10.91nm增大到500℃的15.59nm,晶格常数在不同退火温度下均比标准值0.5414nm稍小.应力分析表明:退火后的ZnS薄膜应力减小,400℃时分布较均匀,平均应力为1.481×108Pa,应力差为1.939×108Pa.且400℃前为张应力,400℃以后转变为压应力.光学分析表明,随着退火温度的升高,ZnS薄膜的透过率增强,吸光度减弱.     

热处理温度对FeCoSiB薄膜及FeCoSiB/Cu/FeCoSiB三明治膜应力阻抗效应的影响

采用DC磁控溅射法在玻璃基片上制备了FeCoSiB薄膜和FeCoSiB/Cu/FeCoSiB 三明治膜,并进行磁场退火热处理以消除残余应力和形成磁织构,提高薄膜的应力阻抗效应。薄膜的磁性能采用振动样品磁强计(VSM)进行测试,采用HP4275A 型阻抗分析仪在200kHz~10MHz频率范围内测试薄膜的应力阻抗效应。结果表明,磁场退火热处理可形成感生磁各向异性,改善薄膜的软磁性能、提高薄膜的应力阻抗效应。在温度低于300℃时,随着退火温度的增加,薄膜的应力阻抗效应增大;当退火温度超过300℃时,薄膜的应力阻抗效应随退火温度增加而降低。与Fe CoSiB单层膜相比, FeCoSiB/Cu/FeCoSiB 三明治膜应力阻抗效应较大。10MHz测试频率下,在基片末端位移为450μm时,经300℃热处理的三明治膜达到了8.3%,而单层膜仅有1.86%。当测试频率较高为10和4MHz时,薄膜的应力阻抗效应变化不大,当测试频率下降到低于1MHz时,薄膜的应力阻抗效应显著降低。     

电子束退火制备二硼化镁超导薄膜的可行性研究

提出了电子束退火制备MgB2超导薄膜新工艺。在对电子束退火制备MgB2超导薄膜可行性进行理论研究的基础上,使用EBW-6型电子束热处理设备,在真空度5.0×10-3Pa、加速电压40 kV、束流2mA、束斑14.2mm、退火时间1.5 s的条件下对[B(10 nm)/Mg(15 nm)]4/SiC夹层结构前驱膜进行了退火实验,得到了零电阻温度为30.3K、转变宽度ΔTc为0.4K、临界电流密度(5 K、0 T)为5.0×106A/cm2、表面平整的MgB2超导薄膜。证明了电子束退火制备MgB2薄膜是切实可行的。该工艺可以推广到大面积MgB2超导薄膜和MgB2线带材的制备。     

快速退火对溅射沉积Al膜微结构及应力的影响

用直流溅射法在聚酰亚胺（PI）基底上制备了300nm厚的Al膜,并进行快速退火（RTA）处理。用X射线衍射、扫描电子显微镜和曲率法对Al薄膜的微结构及应力随退火温度和时间的变化进行了研究。结果表明,采用快速退火可以使其压应力松弛,甚至转变成张应力。     

磁控溅射本底真空度对制备高锰硅的形貌影响

基于当前不同研究者在研究高锰硅过程中选用的本底真空度区间跨度过大的现状,本文以本底真空度为变量,在Si衬底上沉积锰膜,对不同本底真空度下获得的Mn/Si膜同时进行Ar气氛退火处理,退火前后的样品均用SEM对其形貌进行表征,并对结果进行分析,以确定合适的本底真空度参数。结果表明:在10~(-3) Pa本底真空度下,退火前薄膜表面的锰粒子会出现明显团聚现象,当本底真空度提高到10~(-4) Pa量级时,团聚现象得到显著改善。在4×10~(-3)～8×10~(-4) Pa本底真空度下,锰粒子的分布均匀程度较差。而本底真空度达到7×10~(-5) Pa时,薄膜表面会出现碎裂的情况。在溅射用于制备高锰硅的锰膜时,建议本底真空度在5.7×10~(-4)～7×10~(-5) Pa范围内。     

退火气氛与扩散阻挡层对Cu膜表面完整性的影响

用反应磁控溅射和离子束辅助沉积 (IBAD)方法分别在 ( 111)单晶硅基体上沉积了Cu/ZrSiN与Cu/ZrN膜系 ,制得的试样在 80 0℃下分别在真空和N2 、H2 混合气体两种气氛中退火 1h ,结果表明 ,在真空中退火的Cu/ZrSiN膜由于ZrSiN膜裂纹导致Cu膜裂纹的产生 ;ZrSiN和ZrN扩散阻挡层上的Cu膜还有很多由晶界迁移导致的孔洞。在氮氢混合气体中退火时ZrSiN扩散阻挡层上的Cu膜由于具有高的应力而发生断裂 ,ZrN扩散阻挡层上的Cu膜则没有这一现象。在N2 、H2 混合气体中退火时Cu由于还原性气氛抑制了晶界迁移而使Cu膜的孔洞变小、减小     

氧分压对TiO2膜结构与光学性质的影响

报道了用反应溅射法制备TiO2 膜的实验研究 .详细研究了膜的沉积、膜结构及其光学性质 ,随溅射氧分压的变化 .随氧分压由 6× 10 - 2 Pa增加到 9× 10 - 2 Pa时 ,晶体结构由金红石变到锐钛矿 ,氧分压超过 9× 10 - 2 Pa时趋向于无定形结构 .与膜结构密切相关的折射率n随氧分压的增大由 2 .4 4变到 1.96 ,禁带宽度Eg 则由大变小 ,然后再增大的变化 (3.4 1→ 3.2 6→3.4 2 ) .     

Ar压强对硅基Al膜应力和微结构的影响

用直流磁控溅射法在室温Si基片上制备了溅射时间分别为5 min和10 min,氩气压强分别为0.7、3、6 Pa的6种Al膜,用光学相移法和X射线衍射法对Al膜的应力和微结构随着压强的变化进行了研究.应力分析表明:在同一溅射时间,随着氩气压强的减小,Al膜厚度增大,在相同选区范围内,Al膜的应力差变小,应力分布趋于均匀.结构分析表明:制备的Al膜呈多晶状态,晶体结构仍为面心立方,在相同溅射时间下,压强为0.7 Pa的Al膜结晶度最好.随着压强的减小,平均晶粒尺寸和晶格常数增大.     

Spectroscopic measurements of stress relaxation during thermally induced crystallization of amorphous titania films

Amorphous TiO₂ optical films transform irreversibly to a crystalline phase when subjected to temperatures in excess of 573 K. The transformation is accompanied by film densification and a marked change in the intrinsic film stress. Work reported here involves the application of real-time Raman spectroscopy to follow the transformation dynamics and to evaluate transient stresses which evolve during thermally induced crystallization of amorphous sol-gel deposited films. Relative changes in vibrational mode intensities characteristic of the crystalline phase correlate with the degree of crystallinity in the film while mode frequency shifts also acquired in real time are used to estimate the film temperature and the magnitude of internal stress. A contour analysis method is presented whereby knowledge of two vibrational mode frequencies is sufficient to determine these quantities uniquely. Results suggest that both deposition temperature and crystallization temperature affect the intrinsic film stress. Advantages and limitations of this method for the evaluation of stress in dielectric films are discussed.     

Computer simulation of the thermal stability of nickel films on two-layer graphene

The structure and the dynamic and mechanical properties of monolayer nickel films deposited on two-layer graphene are studied in the temperature range 300 < T < 3300 K by the molecular-dynamics method. A part of the Ni atoms remains on the graphene sheet even at T = 3300 K for both one- and two-sided coatings. The radial distribution functions of the upper and lower metal films differ significantly even at T = 300 K. The temperature dependence of the horizontal and vertical components of the self-diffusion coefficient of a one-sided nickel film exhibits a jump above 1800 K. No similar specific feature was observed for a two-sided coating of graphene with this film. The stress components acting in the nickel-film plane disappear with an increase in temperature for a shorter time in the case of one-sided coating.     

Amplitude-dependent internal friction in copper thin films on silicon substrates

Internal friction in copper thin films 0.2–1.5 μm thick on silicon substrates has been measured between 180 and 340 K as a function of strain amplitude. Analysis of the amplitude-dependent internal friction in the copper films shows the relation between the plastic strain of the order of 10⁻⁹ and the effective stress on dislocation motion. The stress–strain curves thus obtained for the copper films tend to shift to a higher stress with decreasing film thickness and also with decreasing temperature, both indicating a suppression of microplastic flow. It is concluded that the microflow stress at a constant level of the plastic strain varies inversely with the film thickness at all temperatures examined. The film thickness effect in the microplastic range can be explained on the basis of a dislocation-bowing model.     

Comparative study on the characteristics of network and continuous Ni films

Ni films were deposited on anodic aluminum oxide (AAO) and SiO₂/Si(100) substrates at 300 K by direct current magnetron sputtering with the oblique target. The film thickness was 80 nm, 160 nm and 260 nm. The films grown on AAO substrates have a network structure while those deposited on SiO₂/Si(100) substrates are continuous. The network film consists of granules and is formed by granule connection. The granule consists of many fine grains. The granule size increases with increasing film thickness. The 80 nm-thick network film has a honeycomb-like structure. The continuous films grow with a columnar structure and the transverse size of columnar grains increases with increasing film thickness. All the network films show a Ni(111) diffraction peak while the 160 nm- and 260 nm-thick continuous films exhibit the Ni(111) and Ni(200) diffraction peaks. The network films have higher coercivity and residual magnetization ratio compared with the continuous films. The coercivity and the residual magnetization ratio increase with increasing film thickness for the network films while they are almost independent of the film thickness for the continuous films. A temperature dependence of the resistance within 5-200 K reveals that the 80 nm-thick network Ni film exhibits markedly a minimal resistance at about 40 K. A logarithmic temperature dependence of the conductance is verified at temperatures below 40 K. The temperature coefficient of resistance is smallest for the 80 nm-thick network film and is largest for the 260 nm-thick continuous film.     

Effects of texture and residual stress on the transition of ferroelectric perovskite thin films with C-axis polarization

Based on the Landau-Devonshire theory, the effects of texture and residual stress on the transition of ferroelectric perovskite thin films with C-axis polarization were studied where the influence of texture dispersion was considered. Using the results, the effect of residual stress on the transition temperature of textured ferroelectric film can be predicted. As an example, the influence rules of residual stress on the PbTiO₃ films with various texture types and degrees were obtained. For (001)-oriented PbTiO₃ film, the compressive stress increases the transition temperature, but tensile stress decreases the transition temperature. And the shift of the transition temperature increases with the texture degree increasing for both compressive stress and tensile stress in (001)-oriented PbTiO₃ films. For (111)-oriented PbTiO₃ film, the effects of stresses for different texture degrees on the transition temperature are different from that for (001)-oriented PbTiO₃ film. At the same residual stress level, the shift of the transition temperature in (001)-oriented PbTiO₃ film is greater than that in (111)-oriented PbTiO₃ film.     

Effects of thermal treatment on the tribological characteristics of thermoplastic polymer film

Friction tests were carried out using a microtribometer to investigate the effect of thermal treatment on microscale friction and wear between poly(methyl methacrylate) (PMMA) film and a fused silica lens. Two films were examined: one that was baked at 413 K for 2 min and one that was baked at 433 K for 24 h. The friction forces on the PMMA films were measured under atmospheric conditions as the temperature of the films was increased from 300 K to 443 K. The contact area between the films and the lens was also examined. As the temperature increased, the friction force increased for both films. The slope of the friction force with temperature and the contact area varied, depending on the state of the film surface; glassy, rubbery, and viscous flow states. The baking conditions also affected the slope, contact area, and wear generation. For temperatures at which the samples were in a glassy state, wear particles were not generated on the sample baked for 24 h. The results demonstrate that the tribological characteristics can be altered by the thermal treatment of the PMMA film as well as the temperature. When the film contains some residual solvent, the residual solvent in the PMMA film can diffuse to the PMMA surface due to heating and thus decrease the friction force under room-temperature conditions.     

蒸发速率对ZnS薄膜性能的影响

为了研究蒸发速率对ZnS薄膜的折射率、表面形貌和应力等性能的影响,本文采用电子束蒸发技术进行了ZnS薄膜的制备.首先在K9玻璃基片上镀制薄膜,采用分光光度计进行透射率曲线的测试,利用光谱反演法得出薄膜的折射率,采用原子力显微镜表征了样品的表面形貌.最后在聚酰亚胺基底上镀制薄膜,利用Stoney公式计算出薄膜的应力.结果...     

nc-Si:H薄膜的内应力特性研究

测试了采用PECVD生长的氢化纳米硅(nc-Si：H)薄膜的内应力。利用XRD、Raman、AFM、HRTEM研究了nc-Si：H薄膜的微结构，用全场薄膜应力测试仪测量了nc-Si：H薄膜的内应力。结果表明：nc-Si：H薄膜的内应力与薄膜的微结构密切相关，强烈依赖于制备工艺。压应力随掺杂浓度的提高而增加；在一定功率密度范围内掺磷nc-Si：H薄膜的压应力随功率密度增加而减少，并过渡为张应力；在373-523K之间，掺硼nc-si：H薄膜的压应力随衬底温度升高而增加；nc-Si：H薄膜的压应力随氢气对硅烷稀释比的变化而变化。     

磁控溅射沉积制备SnSe薄膜及其热电性能研究

因为晶体结构以及热电性能各向异性,硒化锡(SnSe)沿b轴方向表现出优异的热电性能,受到业内的广泛关注。但关于SnSe薄膜研究的报道较少。本研究利用磁控溅射技术,将SnSe沉积到Si/SiO₂基底得到SnSe薄膜,分析了沉积温度对SnSe薄膜结构和热电性能的影响。结果显示:沉积温度升高,晶粒尺寸相应增加,薄膜的结晶质量也随之提高。在573 K的沉积温度条件下,能获得高结晶质量和良好化学计量比的(111)取向SnSe薄膜,该薄膜具有约为1.25μW/(cm·K²)的最大功率因子(PF)。当沉积温度升高至773 K时,可以得到具有超高迁移率和赛贝克系数的(400)织构SnSe薄膜,该薄膜在573 K的测试温度下,其最大PF为0.5μW/(cm·K²),实现接近于文献报道的相同温度下单晶SnSe沿a轴的PF。本研究的结果证明了高沉积温度对SnSe薄膜微观结构和热电性能调控的重要性,并且为通过设计和调控SnSe基薄膜有序结构来提升其热电性能提供了新的研究思路。     

X-ray analysis of heat-treated titanium nitride films

Titanium nitride films deposited onto steel substrates maintained at 423 K were heat treated in the temperature interval 773–1173 K. Samples were studied by electron probe microanalysis and X-ray diffraction. The high values of the microhardness observed for the as-deposited films decreased after annealing for 3 h at 973 K to nearly bulk values. This decrease is mainly due to the improvement in the microstructure of the films. It is accompanied by strong decreases in strain, stress and the lattice parameter of δ-TiN_x. Growth of the ε-Ti₂N phase at the expense of the δ-TiN_x phase was observed in a film with 34 at .% N when it was annealed for 3 h at 973 K. The lattice parameter and strain in the substrate increased after film deposition, most probably due to a dissolution of nitrogen or titanium atoms in the lattice of -Fe.