薄膜溅射沉积过程中的原子喷丸效应

原子喷丸效应是薄膜溅射沉积过程中的普遍现象，是指反弹工作气体原子和溅射原子构成的荷能粒子流对生长膜面的轰击作用，这些荷能粒子在向基片运输的过程中受到工作气体原子的散射。原子喷丸效应与靶材和工作气体的原子质量比以及工作气体压强密切相关。     

高频辅助溅射沉积及氩气压对Co/Cu磁性多层膜结构和性能的影响

磁控溅射制备薄膜时，工作气体氩气的压强是一个非常重要的参量，氩气压的高低直接影响薄膜的结构形态，这在制备超薄多层膜过程中显得更为重要。利用高频辅助溅射沉积，可使工作气体的压强降低1个数量级，从实验和理论上给予了阐述。最后从巨磁电阻振荡效应方面，对所制备的磁性多层膜的界面状况进行了分析。     

第十九讲 真空溅射镀膜

正用高能粒子(通常是由电场加速的正离子)轰击固体表面,固体表面的原子、分子与入射的高能粒子交换动能后从固体表面飞溅出来的现象称为溅射。溅射出来的原子(或原子团)具有—定的能量,它们可以重新沉积凝聚在固体基片表面上形成薄膜,称为溅射镀膜。通常是利用气体放电产生气体电离,其正离子在电场作用下高速轰击阴极靶材,击出阴极靶材的原子或分子,飞向被镀基片表面沉积成薄膜。     

磁控溅射薄膜生长全过程的计算机模拟研究

本文通过建立多尺度模型,结合模拟了磁控溅射中溅射原子的产生、溅射原子的碰撞传输、以及最终成膜的全过程,研究了基板温度、溅射速率、磁场分布和靶材-基板间距对薄膜生长过程与薄膜性能的影响.模拟结果显示,提高基板温度或降低溅射速率都会增加初期生长阶段薄膜的相对密度;磁场对靶的利用率有显著的影响,而对薄膜最终形貌的影响不大;增大靶材-基板间距会降低薄膜的粗糙度.     

气体流量比对反应溅射Si3N4薄膜的影响

利用射频磁控反应溅射法，以高纯Si为靶材，高纯N2气为反应气体，在Si衬底上制备出了Si3N4薄膜，研究了气体流量比对薄膜质量的影响。结果表明，薄膜的沉积速率主要与气体的流量比有关，随着气体流量比的增加，沉积速率下降，靶面的溅射由金属模式过渡到氮化物模式；薄膜中N／Si的原子比增加；红外吸收谱的Si—N键的振动峰向标准峰逼近。     

溅射条件对FeSiB薄膜磁性及巨磁阻抗效应的影响

采用射频磁控溅射法,在不同溅射条件下制备了FeSiB薄膜。研究了溅射条件对薄膜应力、磁滞回线及巨磁阻抗效应的影响。结果表明:随着溅射氩气压强的增加,薄膜内应力从压应力变为张应力,磁滞回线的形状随溅射条件的不同也发生改变。对磁各向异性的变化作了分析和讨论,而面内横向单轴磁各向异性的重要性在巨磁阻抗效应的实验中充分得到了体现。     

溅射条件下对FeSiB薄膜磁性及巨磁阻抗效应的影响

采用射频磁控溅射法,在不同溅射条件下制备了ＦｅＳｉＢ薄膜。研究了溅射条件下对薄膜应力、磁滞回线及磁阻抗效应的影响。结果表明：随着溅射氩气压强的增加,薄膜内应力从压应力变为张应力,磁滞回线的形状随溅射条件下的不同也发生改变。对磁各向异性的变化作了分析和讨论,而面内横向单轴磁各向异性的重要性在磁阻抗效应的实验中充分得到了体现。     

铜铟镓硒薄膜的真空制备工艺及靶材研究现状

阐述了两种真空法制备铜铟镓硒(CIGS)薄膜的工艺原理和工艺过程,比较和分析了两工艺的优缺点;介绍了溅射靶材的熔融铸造法和粉末冶金法,列举了靶材制备中所需的温度、压强、保温时间等参数。最后分析认为,用均匀细小的黄铜矿相CIGS粉末压制烧结成四元靶材,经溅射成膜后退火处理,可制备出优异的CIGS薄膜,具有更广阔的应用前景。     

溅射SmCo基永磁薄膜的结构和磁性能研究

以Sm(Co0.62Fe0.25Cu0.1Zr0.03)7.5合金为靶材,采用磁控溅射工艺在单晶Si基片上沉积了SmCo基永磁薄膜。研究了溅射工艺参数对薄膜的晶体结构、微观结构和磁性能的影响。结果表明:溅射气压和溅射功率的改变引起了永磁相变,这主要依赖于溅射工艺条件对薄膜Sm含量的影响。高的溅射压强和溅射功率都会引起薄膜晶粒的粗大化和薄膜表面的粗糙化。薄膜的晶体结构和微观结构随溅射参数的变化决定了薄膜的面内磁学行为。当溅射压强为0.3 Pa和溅射功率为5.1 W/cm2时,制备的退火态SmCo基薄膜为TbCu7单相晶体结构,其面内永磁性能良好。     

非晶FeSiB薄膜中的巨磁阻抗效应

采用射频溅射法在三组不同溅射条件下制备了FeSiB薄膜。测量了溅射薄膜的磁滞回线 ,并利用HP 41 94A阻抗分析仪 ,在 1～ 40MHz频率范围内研究了样品的巨磁阻抗效应。结果表明 :溅射条件对薄膜磁性能和巨磁阻抗效应影响很大 ,其中氩气压强为 6 65Pa ,磁场感生横向单轴磁各向异性的薄膜具有较好的软磁性能和较大的阻抗变化比值。一定温度下退火能够消除部分应力 ,阻抗变化的灵敏度能提高一倍。另外 ,对巨磁阻抗效应与测量磁场和薄膜易轴的相对位置取向之间的关系也作了讨论     

Effect of Ar gas pressure on growth, structure, and mechanical properties of sputtered Ti, Al, TiAl, and Ti3Al films

Single layers of Ti, Al, TiAl and Ti₃Al were sputter deposited on to 2″ oxidized Si 111 wafers and 7059 Corning Glass to study the effect of film thickness, temperature, and sputtering gas pressure on the mechanical and physical properties. In the present investigation, sputtering gas pressure was varied from 2 mT to 10 mT. The film thickness was varied from 1000 Å to 2 μm. The as-deposited Ti, Al and Ti₃Al films are well crystallized over the entire thickness range. Ti and Ti₃Al films show preferred orientation in the 0002 direction. On the other hand, Al films are random polycrystalline. TiAl films are nearly amorphous for all the thicknesses under consideration. TiAl films show formation of Ti (Al) solid solution phase with increasing Ar pressure. All the materials under consideration, show average film stress to be independent of thickness for thicker films. The nature of the stress (compressive or tensile) depends upon working gas pressure, sputtering power and the target material used. A definite trend is observed in the film stress as a function of Ar gas pressure. Both power and gas pressure influence the energetic bombardment of ions/atoms which in turn influence the average film stress. The nature of the intrinsic stress is explained by the atomic peening model. The Young's modulus of thin films is calculated by using the slope of the stress-temperature plots. The E values seem to change with deposition conditions, however, there is no obvious trend between the sputtering gas pressure and the Young's modulus of these thin films.     

Internal stresses in sputtered chromium

This investigation delineates the effects of deposition rate, working pressure and nature of the working gas on the internal stresses found in wafers of chromium sputtered onto glass using a magnetron-type post-cathode sputtering apparatus. Attention is focused on the thickness range between 0.1 and 0.3 μm, where the measured force per unit width accumulates linearly with film thickness and where the effects of substrate heating are small. High compressive stresses develop when sputtering proceeds at low working pressures and moderate deposition rates. Raising both the deposition rate and the working pressure reduces the magnitude of film compression. The most pronounced effect is that of an increase in pressure, which causes first a complete reversal of stress from high compression to high tension and then a more gradual decrease towards zero. This behavior is the same for sputtering in argon or krypton. Analysis of the chromium films reveals no entrapped gas or structural changes to account for the onset of compression at reduced working pressures. The behavior closely resembles stress changes reported in the literature for bias sputtering as a function of substrate voltage. It is proposed that film compression in both cases results from peening of the depositing film by accelerated ions or neutral atoms.     

R.F. reactive sputter deposition of hydrogenated amorphous silicon carbide films

The preparation of hydrogenated amorphous silicon carbide films by r.f. reactive sputtering of a silicon target in Ar-CH₄ gas mixtures with and without an r.f. bias on the substrates was studied. Starting with a pure silicon target and increasing monotonically the CH₄ percentage from 0% to about 10%, films with 1 ⩾ x ⩾ 0 were obtained at decreasing deposition rates. After sputtering for some hours in methane-rich gas mixtures, carbon atoms were incorporated into the silicon target surface, probably as a result of atomic peening, and nearly stoichiometric SiC films were prepared by sputtering of such a target in pure argon. The different mechanisms of film formation, deposition rate, composition, hardness, friction coefficient and stresses in the films as functions of the partial pressure of methane and the value of the r.f. bias were investigated. The IR spectra offilms with different carbon contents were analysed. The greatest hardness was found for nearly stoichiometric SiC films deposited with a bias.     

Some features of magnetron sputtering

In a low pressure sputtering system of the magnetron type for depositing thin solid films, two different discharge modes occur: a positive space-charge-dominated mode and a negative space-charge-dominated mode. The positive space-charge-dominated mode predominates in a weak magnetic field of some few hundred gauss and is widely used for sputtering, although the current density is non-uniform at the cathode surface. The negative space-charge-dominated mode predominates in a strong magnetic field of more than several hundred gauss and is also used for sputtering since the mode shows uniform current distribution at the cathode surface.In the magnetron sputtering system the working pressure is so low that the scattering of sputtered atoms by gas molecules can be neglected. Thus energetic sputtered atoms impinge on the substrates during film growth. This causes some phenomena which are rarely observed in a conventional diode sputtering system, e.g. an abnormal surface texture and an unusual crystalline structure are found in the resultant sputtered films. There is evidence that thin films of compounds normally only formed at high temperature can be synthesized at lower substrate temperatures.     

Stress evolution in magnetron sputtered Ti-Zr-N and Ti-Ta-N films studied by in situ wafer curvature: Role of energetic particles

Stress evolution during reactive magnetron sputtering of binary TiN, ZrN and TaN thin films as well as ternary Ti-Zr-N and Ti-Ta-N solid-solutions was studied using real-time wafer curvature measurements. The energy of the incoming particles (sputtered atoms, backscattered Ar, ions) was tuned by changing either the metal target (M_Ti = 47.9, M_Zr = 91.2 and M_Ta = 180.9 g/mol), the plasma conditions (effect of pressure, substrate bias or magnetron configuration) for a given target or by combining different metal targets during co-sputtering. Experimental results were discussed using the average energy of the incoming species, as calculated using Monte-Carlo simulations (SRIM code). In the early stage of growth, a rapid evolution to compressive stress states is noticed for all films. A reversal towards tensile stress is observed with increasing thickness at low energetic deposition conditions, revealing the presence of stress gradients. The tensile stress is ascribed to the development of a ‘zone T’ columnar growth with intercolumnar voids and rough surface. At higher energetic deposition conditions, the atomic peening mechanism is predominant: the stress remains largely compressive and dense films with more globular microstructure and smooth surface are obtained.     

CoFe合金薄膜的制备及原子力表征

室温下采用射频磁控溅射技术在涤纶纺粘非织造布表面沉积钴铁(CoFe)合金薄膜.通过原子力显微镜(AFM)观察了CoFe合金薄膜在无纺织布表面沉积的微观结构,并较为系统地分析了溅射时间、溅射压强及溅射功率对CoFe合金薄膜微观结构的影响.结果表明,磁控溅射的工艺参数配置对CoFe合金薄膜表面形貌的影响很大,溅射时间的长短、溅射功率的大小对成膜的均匀性有很大影响,在一定的溅射压强(0.5Pa)时合金颗粒将会因团聚而急速增大.     

Elaboration and characterization of Fe1-xO thin films sputter deposited from magnetite target

Majority of the authors report elaboration of iron oxide thin films by reactive magnetron sputtering from an iron target with Ar-O₂ gas mixture. Instead of using the reactive sputtering of a metallic target we report here the preparation of Fe_1-xO thin films, directly sputtered from a magnetite target in a pure argon gas flow with a bias power applied. This oxide is generally obtained at very low partial oxygen pressure and high temperature. We showed that bias sputtering which can be controlled very easily can lead to reducing conditions during deposition of oxide thin film on simple glass substrates. The proportion of wustite was directly adjusted by modifying the power of the substrate polarization. Atomic force microscopy was used to observe these nanostructured layers. Mössbauer measurements and electrical properties versus bias polarization and annealing temperature are also reported.     

Structure and electrical properties of ITO thin films deposited at high rate by facing target sputtering

High rate deposition of ITO thin films at a low substrate temperature was attempted by using a facing target sputtering (FTS) system. Deposition rate as high as 53 nm/min was realized on polycarbonate film substrate of 80-μm thickness. When the film was deposited at a deposition rate above 80 nm/min, polycarbonate film substrate was thermally damaged. The film deposited by FTS has much smaller compressive film stress than the film deposited by conventional magnetron sputtering. The film stress was reduced significantly by increasing the sputtering gas pressure and stress-free films can be obtained by adjusting the sputtering gas pressure. This may be mainly caused by the fact that bombardment by high energy negative oxygen ions to substrate surface during deposition can be completely suppressed in the FTS. Film structure and electrical properties changed little with substrate position, and uniform films were obtained by the FTS.     

Microstructural characterizations and hardness evaluation of d.c. reactive magnetron sputtered CrN thin films on stainless steel substrate

Chromium nitride (CrN) thin films were deposited on stainless steel (grade: SA304) substrate by using d.c. reactive magnetron sputtering and the influence of process parameters such as substrate temperature, pressure, and power on their microstructural characteristics were investigated in the present work. The CrN films were characterized with X-ray diffraction (XRD) to reveal the formation of different phases and its texture. The films showed the (111) preferred orientation but its intensity decreased, while intensity of peak (200) increased with increase in working pressure. The mixture of CrN and Cr₂N phases were identified at low working pressure and temperature. The preferred orientations of CrN thin films are strongly influenced by sputtering conditions, thickness, and the induced residual stress in the films as observed in the present work. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) were used to characterize the morphology and surface topography of thin films, respectively. The study shows that the hardness of films strongly depends on the grain size and the film density, which are influenced by combined effect of the working pressure, temperature, and power of the sputtering process.     

The compressive stress transition in Al,V, Zr,Nb and W metal films sputtered at low working pressures

Investigation of internal stresses in thin sputtered films of Al, V, Zr, Nb and W extends the observation of compression at low working pressures that was originally detected with Cr (D. W. Hoffman and J. A. Thornton, Thin Solid Films, 40 (1977) 355–363) and probes the atomic mass dependence of the transition pressure that was subsequently detected with Ti, Ni, Mo and Ta (J. A. Thornton and D. W. Hoffman, J. Vac. Sci. Technol., 14 (1977) 164–168). The observation of compressive stresses at sufficiently low sputtering pressures in all ten of the elements so far examined strongly supports the generality of this phenomenon. The five new metals under study also confirm the overall increase of the transition pressure with atomic mass indicated by the metals examined earlier. However, periodic deviations from the general trend are now evident among the group IVB, VB and VIB elements examined. The electrical conductivity and optical reflectance of the sputtered metal films exhibit abrupt changes in behavior near the transition pressure for compressive stresses. Above the transition pressure the conductivity and reflectance drop off rapidly; below the transition pressure these properties tend to level off at maximum values for the sputtered metal films. The interpretation of these observations in terms of a peening mechanism of energetic particle bombardment is discussed. Data are presented for films up to 0.3 μm thick sputtered onto glass substrates at a nominal deposition rate of 1 nm s^?1 over the pressure range 0.067–4.0 Pa of argon.