基于XRD的镀锌钝化膜残余应力试验研究

利用XRD技术测试了镀锌钝化膜结合界面的残余应力，同时通过电解抛光法检测了其厚度方向残余应力的分布规律，分析了残余应力对镀锌钝化膜结合强度的影响. 试验结果表明，镀锌钝化膜的残余应力均表现为压应力，并随着基体表面残余应力的增大而减小；钝化膜在2—10μm厚度方向的残应力为-274.5—-428.3MPa，其应力为梯度分布；镀锌钝化膜与基体的界面结合强度与其残余应力成反比，减小薄膜残余应力，有利于提高镀锌钝化膜与基体的结合强度. 关键词： X射线衍射法(XRD) 镀锌钝化膜 结合强度 残余应力     

Effect of temperature on residual stress and mechanical properties of Ti films prepared by both ion implantation and ion beam assisted deposition

Ti films with a thickness of 1.6 μm (group A) and 4.6 μm (group B) were prepared on surface of silicon crystal by metal vapor vacuum arc (MEVVA) ion implantation combined with ion beam assisted deposition (IBAD). Different anneal temperatures ranging from 100 to 500 °C were used to investigate effect of temperature on residual stress and mechanical properties of the Ti films. X-ray diffraction (XRD) was used to measure residual stress of the Ti films. The morphology, depth profile, roughness, nanohardness, and modulus of the Ti films were measured by scanning electron microscopy (SEM), scanning Auger nanoprobe (SAN), atomic force microscopy (AFM), and nanoindentation, respectively. The experimental results suggest that residual stress was sensitive to film thickness and anneal temperature. The critical temperatures of the sample groups A and B that residual stress changed from compressive to tensile were 404 and 428 °C, respectively. The mean surface roughness and grain size of the annealed Ti films increased with increasing anneal temperature. The values of nanohardness and modulus of the Ti films reached their maximum values near the surface, then, reached corresponding values with increasing depth of the indentation. The mechanism of stress relaxation of the Ti films is discussed in terms of re-crystallization and difference of coefficient of thermal expansion between Ti film and Si substrate.     

Low temperature ITO thin film deposition on PES substrate using pulse magnetron sputtering

Experiments were conducted using pulse magnetron sputtering (PMS) to deposit transparent conducting indium tin oxide (ITO) thin film onto flexible polyethersulfone (PES) plastic substrates. The thin film microstructure, optoelectronic and residual stress were analyzed using the modulating PMS power, work pressure, pulse frequency, duty cycle and cycle time process parameters. The residual stress of the thin film was determined by scanning electron microscopy (SEM) combined with the Sony equation. The experimental results show that PMS has a lower process temperature, higher deposition rate and lower resistivity compared with the radio frequency process at the same output power. The duty cycle increase produces the optimum optoelectronic characteristics. When the pressure, power, duty cycle and sputter time are increased, the thin film stress will also increase, causing flexural distortion in the PES plastic substrate. When the deposition thickness reaches 1.5 μm, ITO thin film will appear with a distinct split. Under 5 mtorr work pressure, 60 W power, 33 μs duty time and 2 μs pulse reverse time at duty cycle 95%, thin film with an optimized electrical 3.0 × 10⁻⁴ Ω-cm, RMS surface roughness of 0.85 nm and visible region optical transmittance will be achieved with acquisition of over 85%.     

p型多晶硅薄膜应变因子与掺杂浓度关系理论研究

多晶硅薄膜具有良好的压阻特性,晶粒结构和掺杂浓度决定其压阻特性.一般通过调节掺杂浓度改变压阻参数,但现有的多晶硅薄膜压阻系数与掺杂浓度的理论关系和适用范围不够全面.为了完善多晶硅薄膜压阻理论,基于多晶硅纳米薄膜隧道压阻模型,以及硅价带和空穴电导质量随应力改变的机理,提出了一种p型多晶硅薄膜压阻系数算法.该算法分别求取了晶粒中性区和复合晶界区的压阻系数π_(11),π_(12)和π_(44)的理论公式,据此可以计算任意择优晶向排列多晶硅的纵向和横向压阻系数.根据材料的结构特性,求取了p型多晶硅纳米薄膜和普通多晶硅薄膜应变因子,绘制了应变因子与掺杂浓度的关系曲线,与测试结果比较,具有较好的一致性.因此,该算法全面和准确,对多晶硅薄膜的压阻特性的改进和应用具有重要意义.     

红外双波段激光滤光膜的研制

为了满足红外军用仪器的特殊要求,根据薄膜理论进行了红外双波段滤光膜的膜系设计;采用电子束真空镀膜的方法,通过对工艺参数的调整,在多光谱ZnS基底上镀制了1 064nm高反、3～5μm高透的红外双波段滤光膜.利用低能离子轰击,使膜层与基底间的应力明显减小;使用BGS 6341薄膜应力测试仪,采用渐变梯度法,测得其压应力由...     

Residual stress of physical vapor-deposited polycrystalline multilayers

An extended one-dimensional stress model for the deposition of multilayer films is built based on the existing stress model by considering the influence of deposition conditions. Both thermal stress and intrinsic stress are considered to constitute the final residual stress in the model. The deposition process conditions such as deposition temperature, oxygen pressure, and film growth rate are correlated to the full stress model to analyze the final residual stress distribution, and thus the deformation of the deposited multilayer system under different process conditions. Also, the model is numerically realized with in-house built code. A deposition of Ag-Cu multilayer system is simulated with the as-built extended stress model, and the final residual stresses under different deposition conditions are discussed with part of the results compared with experiment from other literature.     

Birefringence measurements of MnPc thin film by polarization microscopy

We have studied optical properties of near-infrared (NIR) spectra and birefringence of the manganese phthalocyanine (MnPc) thin films. The morphology of the MnPc thin film grown on KCl (0 0 1) substrates was observed by using an atomic force microscope. The NIR spectral range of 1.0-1.7 μm was studied in this study, because that of 1.3-1.5 μm is known as an optical communication wavelength. The birefringence was measured with changing the growth condition of a deposition rate and a substrate temperature. The birefringence of the film was most affected by the deposition rate.     

Micro-patterning of NdFeB and SmCo magnet films for integration into micro-electro-mechanical-systems

The integration of high-performance RE-TM (NdFeB and SmCo) hard magnetic films into micro-electro-mechanical-systems (MEMS) requires their patterning at the micron scale. In this paper we report on the applicability of standard micro-fabrication steps (film deposition onto topographically patterned substrates, wet etching and planarization) to the patterning of 5-8 μm thick RE-TM films. While NdFeB comprehensively fills micron-scaled trenches in patterned substrates, SmCo deposits are characterized by poor filling of the trench corners, which poses a problem for further processing by planarization. The magnetic hysteresis loops of both the NdFeB and SmCo patterned films are comparable to those of non-patterned films prepared under the same deposition/annealing conditions. A micron-scaled multipole magnetic field pattern is directly produced by the unidirectional magnetization of the patterned films. NdFeB and SmCo show similar behavior when wet etched in an amorphous state: etch rates of approximately 1.25 μm/min and vertical side walls which may be attributed to a large lateral over-etch of typically 20 μm. Chemical-mechanical-planarization (CMP) produced material removal rates of 0.5-3 μm/min for amorphous NdFeB. Ar ion etching of such films followed by the deposition of a Ta layer prior to film crystallization prevented degradation in magnetic properties compared to non-patterned films.     

发光薄膜沉积技术中薄膜晶体管的优化设计

为了能制备高均匀性、大尺寸高清RGB-OLED显示终端,发展了一种全新的、无掩膜低成本的彩色薄膜沉积技术——薄膜晶体管导向的薄膜沉积技术,并研究了薄膜晶体管的宽长比及栅压对电聚合发光薄膜性能的影响,寻找最佳的制备条件。实验中采用像素尺寸大小为200μm×200μm的AMOLED基板,通过TFT来控制发光薄膜在ITO像素上的电化学聚合过程。首先对不同宽长比的TFT性能进行表征,再对不同宽长比的TFT在不同栅压条件下制备的电化学聚合薄膜进行表征和分析。实验结果表明,在同一宽长比的TFT控制下,施加栅压越大,制备的薄膜越厚,发光效果越好;在不同宽长比的TFT控制下,宽长比越大,聚合薄膜越厚,发光效果越好。在较大栅压下,选择宽长比为50μm/10μm的TFT最为适宜。研究结果为电化学聚合技术在AMOLED显示中的应用奠定了良好基础。     

Research on the optical properties of collodion film

This paper centers on the deposition process and optical properties of collodion film. Collodion film was prepared on the double side polished silicon and k9 optical glass using the sol–gel method. The studying results have showed four characteristics of collodion film. First of all, the thickness of collodion film decreases with increasing the revolution speed. Secondly, the refractive index of collodion film changes from 1.529306 to 1.500128, which accords with the normal dispersion. Thirdly, the transmittance of collodion film is higher in the visible wavelength range 380–760 nm and its average transmittance is 91.9%. At last, the absorption property is very well in the infrared region. The infrared absorption coefficient is greater than 0.69/μm in range of 3–5 μm, and it is up to 1.433528/μm in 8–14 μm because of its many strong infrared absorption peaks. In addition, the absorption characteristics have been analyzed in detail.     

透0.45 μm～1.6 μm反8 μm～12 μm宽光谱分色滤光片的制备

光谱分色滤光片对成像光谱技术至关重要,是实现光电仪器体积小、质量轻的一个重要器件.根据金属膜具有高反射率的特点和可以进行诱增透的原理,介绍了透0.45 μm～1.6 μm反8 μm～12 μm光谱分色滤光片的膜料选择和膜系设计,并应用JGP560A2型磁控溅射镀膜机制备出了光谱性能和理化性能较好的宽光谱分色滤光片,其光谱性能达到0.45 μm～1.6 μm波段范围内,平均透过率大于80%;8 μm～12 μm波段范围内,平均反射率大于91%.     

使用SiNx原位淀积方法生长的GaN外延膜中的应力研究

采用低压MOCVD系统，在生长过程中使用SiN_x原位淀积的方法产生纳米掩模，并 在纳米掩模上进行选区生长和侧向外延制备了GaN外延薄膜.使用拉曼光谱和光荧光的手段对 GaN外延膜中的残余应力进行了研究.研究发现，用SiN_x原位淀积出纳米掩模后 ，GaN生长将由二维向三维转变，直到完全合并为止.利用拉曼光谱和光荧光谱分别研究了薄 膜中的残余应力，两者符合得很好；这种方法生长出的GaN薄膜的应力分布较传统的侧向外 延更加均匀；并且从中发现随着生长过程中SiN_x原位淀积时间的增加，生长在 其上的GaN外延膜中的残余应力减小.这是因为，随着SiN_x原位淀积时间的增加 ，SiN_x纳米掩模的覆盖度也增大.因此侧向外延区的比例增大，残余应力随之减 小. 关键词： GaN x原位淀积')" href="#">SiN_x原位淀积 拉曼 光荧光 残余应力     

Catalytic decomposition of trichloroethylene over Pt-/Ni-catalyst under microwave heating

Microwave (MW)-activated catalytic reactor system was studied and the results were compared with that of a conventional system based on the thermal activation method. Trichloroethylene (TCE) was decomposed under various MW-powers supply. Results showed that there is an optimum film thickness that was loaded on supports in MW heating system. The threshold may be within 1-3 μm. Lower temperature cannot activate the catalyst, while higher temperature results in carbon deposition and catalyst deactivation. This means that the dechlorination reaction needs to fix an optimum film MW-power supply in order to avoid the deposition of carbon on the surface of the active phase. MW-activated system is also worth compensating the conventional system in VOCs decomposition reaction.     

The effects of dc bias voltage on the crystal size and crystal quality. of cBN films

For the deposition of cubic boron nitride thin films in Ar–N₂–BF₃–H₂ system by dc jet plasma chemical vapor deposition, the role of dc substrate bias ranging from -70 V to -150 V was investigated. A critical bias voltage was observed for the formation of cBN phase. The cBN content in the film increased with bias voltage and reached a maximum at the bias voltage of -85 V. Increasing the bias voltage further caused a decrease in cBN content and peeling of the films from the substrate. By combining the results of infrared spectroscopy, Raman spectroscopy and X-ray diffraction, the bias voltage was also found to strongly affect the crystal size, crystal quality and residual stress of the deposited films. A bias voltage a little higher than the critical value was demonstrated to be favorable for the deposition of a high-quality cBN film with large crystal size and low residual stress. Received: 13 June 2000 / Accepted: 21 June 2000 / Published online: 23 August 2000     

双离子束溅射中红外SiO2薄膜热稳定性研究

通过双离子束溅射方法在蓝宝石、硅衬底上制备了单层SiO2薄膜,分析了SiO2薄膜残余应力、表面形貌、微观结构以及光学性能(可见-近红外0.4~1.2 μm和中红外3~5 μm波段)在400 ℃~1 000 ℃温度范围内的演化规律.研究结果表明:在400 ℃附近,SiO2薄膜残余应力存在局部极小值;SiO2薄膜光学性能的演化与膜层表面质量、内部残余应力及微观结构变化密切相关;经1 000 ℃高温处理后,蓝宝石窗口表面SiO2薄膜红外透射性能仍能保持很好的稳定性,且膜层表面没有出现显著的气泡、开裂等损伤形貌.该研究结果可为恶劣环境下光学窗口头罩表面薄膜系统的设计提供指导.     

埋点靶中CH薄膜的制备工艺研究

 CH薄膜的制备是埋点靶制备的关键技术之一,本文主要研究了钨丝辅助裂解制备CH薄膜的制备工艺。研究表明蒸发舟温度和衬底温度对沉积速率影响较大,而衬底距离对沉积速率影响较小;红外光谱和质谱分析表明薄膜的主要成分是聚对二甲苯。     

Influence of Co:Cu ratio on properties of Co–Cu films deposited at different conditions

A series of Co–Cu films with different Co:Cu ratio was electrodeposited at different electrolyte pH, deposition potential and film thickness, and their morphology, crystal structure and magnetic properties were investigated. Compositional analysis by energy dispersive x-ray spectroscopy disclosed that the Co and Cu content were 75 and 25 wt%, respectively, at high pH (3.2) level, while for films at low pH (2.5) level the compositions are 61 Co and 39 wt% Cu, and further decrease of Co:Cu ratio occurred as the film thicknesses increased. The surface morphology of the films changed from an initial dendritic stage to expanded dendrites with increasing Cu content by the electrolyte pH. The dendrites became more obvious at 3 μm and the dendritic structures increased with further increase of film thickness as the Co:Cu ratio decreased. Hence, the increase of the Cu content is thought to be the cause of the increase of dentritic structure. Structural characterizations by x-ray diffraction (XRD) showed that all films have face-centered cubic structure. In the XRD patterns, the peak intensity of Co (111) is lower for the films grown at low pH compared to that of high pH, and the (111) peaks of Co and Cu slightly separated at 3 μm and then the intensity of the Cu (111) increased with increasing film thickness from 4 to 5 μm, so that the Co:Cu ratio changed at all deposition parameters. Magnetic measurements displayed that the saturation magnetization decreased and the coercivity increased as the Co:Cu ratio decreased with all deposition parameters. Also, the magnetic easy axis was found to be in the film plane for all films. It was seen that the variations in the properties of the films might be attributed to the change of Co:Cu ratio caused by the deposition parameters.     

Laser controlled melting of pre-treated zirconia surface

Laser treatment of pre-prepared zirconia surface is carried out. The pre-prepared surface, prior to laser treatment, consists of 50 μm carbon film and 7% titanium carbide particles, which are imbedded in the carbon film. The microstructural and morphological changes in the laser treated surface layer are examined using optical and scanning electron microscopes, energy dispersive spectroscopy, and X-ray diffraction. The fracture toughness of the laser treated surface is measured and the residual stress formed at the surface vicinity is determined from the X-ray diffraction technique. It is found that the microhardness of the laser treated surface increased slightly due to the dense layer formed at the surface vicinity. However, the laser treatment process reduces the fracture toughness of the surface due to improved surface hardness and the residual stress formed in the surface vicinity.     

双波段截止分色滤光片研究

为实现45°入射情况下K9基底上双波段截止分色的特性(截止带波长0.5~0.68μm、0.73~0.79μm,通带波长0.83~0.87μm),采用F-P型的带通滤光片膜系结构为初始结构,与常规设计理念相比有效减少了膜层的数量,薄膜的高折材料采用Ti O2,低折材料采用Si O2,以实现双波段截止的目的。膜层的设计层数为23层,总厚度为2.278μm,借助电子束蒸发物理气相沉积法实现了镀制,利用分光光度计对镀制样品的透过率进行评估。测试结果显示,截止区(0.5~0.68μm和0.73~0.79μm)平均截止深度分别达到了12.57%和20.39%,通带0.83~0.87μm波段内的平均透过率达到了91.35%,样品测试曲线与设计相比,"蓝移"将近10 nm。薄膜样品基本实现了设计目标,具有双波段截止、高通带透过率的特性。在环境测试中:薄膜表现出显著的稳定性,膜层间匹配度适宜。该双波段截止分色滤光片能够应用在一些极端的情况下。     

An application of Raman spectroscopy on the measurement of residual stress in porous silicon

The porous silicon film, at micron level, and the bulk silicon substrate is a basic structure in MEMS components. The residual stress, due to the lattice mismatch between the film and the substrate, exists on the interface and may cause cracking and damaging on the component. Micro-Raman spectroscopy is an optical measurement method that was rapidly applied into the fields of chemistry, physics, material science and mechanics. In this paper, the method is introduced and applied to the study of the stress problems in porous silicon as follows. (1) In the electrochemical etching technique for porous silicon preparation, the distribution of the tensile residual stress along the transitional region between etched and un-etched area is experimentally studied and the result reveals the stress is continuous across the region. In the etched region it reaches GPa level, and in the transition region the gradient of the stress is high. (2) In chemical etching preparation of porous silicon, the residual stress rises up seriously in the cracked area, up to 0.92 GPa. With the porosity increasing, the tensile stress on the porous silicon film increases accordingly. The appearance of the porous silicon film surface is also given by metalloscope and atomic force microscope. The structure of the micro-pores is expected to have a close relation with the distribution of the residual stress.