钼合金磁控溅射镀镍薄膜工艺及后续热处理

目的优化钼表面直流磁控溅射镀镍薄膜的工艺,提出后续热处理方法。方法设计正交实验,探究溅射功率、溅射气压、负偏压和沉积时间对镍薄膜沉积速率和附着力的影响,从而优化工艺参数。利用扫描电镜和平整度仪对最佳工艺参数下制备的薄膜的组织结构进行表征,并研究后续热处理对薄膜附着力的影响。结果工艺参数对镀镍薄膜沉积速率影响的主次顺序为:功率溅射气压负偏压;对薄膜附着力的影响主次顺序为:负偏压沉积时间功率溅射气压。随溅射功率增大,沉积速率增大,薄膜附着力先增后减;随溅射气压增大,沉积速率和薄膜附着力均先增后减。负偏压增大对沉积速率影响较小,但有利于提高薄膜附着力。随沉积时间延长,薄膜附着力降低。在氢气气氛下进行850℃×1 h的后续热处理,能够促进扩散层的形成,明显提高镍薄膜的附着力。结论最佳镀镍工艺参数为:溅射功率1.8 k W,溅射气压0.3 Pa,负偏压450 V,沉积时间10 min。在该条件下制备的镍薄膜厚度达到1.15μm左右,与基体结合紧密,表面平整、连续、致密。后续增加热处理工序是提高镍薄膜附着力的有效方法。     

Fe-Ga薄膜的微结构与磁性能研究

采用磁控溅射方法,以Si(1OO)为衬底在40~80 W功率下制备了Fe_(83)Ga_(17)薄膜,通过XRD、SEM、室温磁滞回线以及MFM的测量研究了不同溅射功率制备的Fe-Ga薄膜的结构、形貌、磁性能和磁畴。XRD结果表明室温下薄膜样品是bcc(11O)晶体结构。SEM观察结果表明薄膜颗粒尺寸在40~70 nm且随着功率增大,薄膜颗粒的尺寸变大,薄膜厚度增加。室温磁滞回线的测量结果表明一定范围内随着功率增大,样品的矫顽力H_c总体呈上升趋势,饱和磁化强度M_s的变化规律并不明显,剩余磁化强度M和矩形比Mr/Ms呈缓慢下降的趋势。磁畴的观察结果表明样品的磁畴为迷宫畴结构,且随着功率增大,磁畴的尺寸增大。     

Nd-Fe-B薄膜的磁控溅射法制备与组织结构

对直流磁控溅射法制备Nd-Fe-B薄膜工艺进行了研究.在不同的溅射功率、溅射气压、溅射时间等条件下制备薄膜,并对薄膜进行了AFM、XRD分析.结果表明,Nd-Fe-B薄膜的沉积速率、表面形貌及相结构与溅射功率、溅射气压、溅射时间密切相关.薄膜的沉积速率随磁控溅射功率的增加而增加,薄膜表面晶粒尺寸和表面粗糙度随溅射功率增加而增大.沉积速率随溅射气压的升高先增大后减小.低功率溅射时,薄膜中出现α-Fe、Nd2Fe14B相相对较少,随溅射功率增加,α-Fe相消失,Nd2Fe14B相增多.综合考虑各种因素,最佳溅射功率为100～130 W.     

磁控溅射制备Ru-B薄膜的研究

采用射频磁控溅射技术制备了Ru-B薄膜,利用掠入射X射线衍射(GIXRD)、高分辨透射电子显微镜(HRTEM)、原子力显微镜(AFM)等分析技术对薄膜的相结构、沉积速率以及表面形貌进行了研究分析。结果表明：在室温下制备的 Ru-B 薄膜均为非晶态。薄膜的沉积速率不随溅射时间变化,但随溅射功率的增加而增大。薄膜表面光滑致密质量良好,随着溅射时间的延长,薄膜表面晶粒大小和粗糙度增大。溅射功率影响着基片表面粒子的形核长大和迁移扩散速率,进而影响薄膜的表面形貌。     

磁控溅射制备Fe-Ga薄膜研究

研究了磁控溅射工艺中溅射功率对制备Fe-Ga薄膜的影响,对薄膜进行了热处理以及硬度测试.结果发现,在50～100W,薄膜厚度随溅射功率的增大而增加,并且在100W时所得的薄膜厚度和致密性最佳.热处理后发现薄膜变得更致密、更均匀.在一定功率范围内,薄膜的硬度也随溅射功率的增加而增加.     

磁控溅射技术制备二氧化钛薄膜研究进展

磁控溅射技术具有溅射速率高、膜基结合力好、易实现工业化生产等技术优势,在二氧化钛薄膜制备方面具有显著优势,但磁控溅射参数对二氧化钛薄膜结构和性能的影响显著,如何通过控制和优化磁控溅射参数,获得高性能二氧化钛薄膜已成为目前的研究热点。概述了不同晶型二氧化钛的结构特点、物理性质和磁控溅射制备二氧化钛薄膜的工作原理,指出成膜过程中的溅射功率、溅射气压、溅射时间、沉积温度和氧分压等是影响薄膜结构和性能的主要因素,并详细阐述了上述五种工艺参数对二氧化钛薄膜沉积速率、膜层厚度、表面粗糙度、相组成和光催化性能等的影响规律和作用机制。此外,还对其他影响薄膜结构和性能的关键因素及影响规律进行了介绍,包括退火温度对膜层组织转变影响的规律,金属元素掺杂和非金属元素掺杂对膜层形貌和性能的影响,以及不同溅射靶材特点及其对成膜过程的影响。最后提出未来磁控溅射技术制备二氧化钛薄膜的研究难点,并对二氧化钛薄膜的下一步研究方向进行了展望。     

直流磁控溅射法在玻璃基片上制备TiN薄膜

采用直流反应磁控溅射法在玻璃片上制备了TiN薄膜,研究不同制备工艺条件与薄膜性能之间的关系。用紫外-可见光分光光度计测试了不同沉积时间和N2流量条件下TiN薄膜透光率;用X射线衍射仪分析了不同N2流量和溅射功率条件下TiN薄膜结构;用扫描电镜(SEM)观察了TiN薄膜的表面腐蚀形貌,用恒电位仪对TiN薄膜的耐腐蚀性进行了分析。结果表明:当沉积时间为2min,N2流量为15mL/min时,在可见光区有较高的透光率,在近红外区的透光率很低;当N2流量为15mL/min,溅射功率为4kW时,TiN薄膜的结晶最致密;当溅射功率为4kW时,TiN薄膜具有较好的耐腐蚀性。     

Mo电极上磁控反应溅射AlN薄膜

采用射频反应磁控溅射法在Mo电极上沉积了AlN薄膜.研究了溅射气压、靶基距、溅射功率、衬底温度及N_2含量等不同工艺条件对AlN薄膜择优取向生长的影响.用XRD分析了薄膜的择优取向,用原子力显微镜、高分辨场发射扫描电镜表征了薄膜的形貌.实验结果表明,靶基距和溅射气压的减小,衬底温度及溅射功率的升高有利于AlN(002)晶面的择优取向生长.氮氩比对AlN薄膜择优取向生长影响较小,N_2≥50%(体积分数)时均可制得高c轴择优取向的AlN薄膜.经优化工艺参数制备的AlN柱状晶薄膜适用于体声波谐振滤波器的制备.     

磁控溅射制备Mo薄膜的优化工艺和组织及性能研究

基于正交试验设计,采用射频磁控溅射技术在不同工艺条件下制备了一系列纯金属Mo薄膜。以薄膜的纳米硬度和结合强度为评价指标,考察分析了溅射靶功率、基片温度、氩气流量和真空度4个工艺参数对溅射Mo薄膜综合力学性能和组织结构的影响规律及机理。结果表明,所制备的多种Mo薄膜均为立方多晶结构,并在(110)和(220)晶面择优生长。薄膜由细小的"树枝"状颗粒随机堆叠而成,表面呈压应力状态。综合考虑薄膜的沉积质量和沉积效率,提出磁控溅射制备Mo薄膜的较佳工艺参数为Mo靶功率100 W,沉积温度120℃,氩气流量90 cm3/min,真空度0.2 Pa。采用优化工艺制备的Mo薄膜具有良好的结晶状态和均匀致密的组织结构,纳米硬度为7.269 GPa,结合强度高达33.8 N。     

基于硅靶和碳化硅靶的碳化硅薄膜磁控溅射工艺对比

目的 通过基于碳化硅陶瓷靶的直接溅射和基于硅靶与甲烷的反应溅射,在Si(100)基底上沉积碳化硅薄膜,对比两种工艺制备碳化硅薄膜的异同.方法 采用直接磁控溅射与反应磁控溅射工艺制备碳化硅薄膜,通过白光干涉仪、轮廓仪、X光电子能谱仪(XPS)分析薄膜粗糙度、厚度、沉积速率、组分,通过X射线衍射仪和扫描电子显微镜分析薄膜的物相结构和形貌.结果 基于硅靶和甲烷的反应溅射工艺,甲烷流量百分比为20％～70％时,沉积速率从11.3 nm/min升高到36.5 nm/min.甲烷流量百分比为20％～60％时,表面粗糙度Rq值变化不大;甲烷流量百分比为70％时,Rq值有增大的趋势.对于甲烷反应溅射工艺,硅碳元素比例可调,但甲烷气体不易控制.基于碳化硅陶瓷靶工艺,随沉积时间(即膜层沉积厚度)的增加,表面粗糙度Rq变化不大,硅碳原子比接近1:1.两种工艺制备的薄膜均为晶态,且为8H-SiC.结论 比较两种工艺,相同靶功率下,硅靶反应溅射的沉积速率明显快于碳化硅陶瓷靶.硅靶反应溅射的元素比例可调,但甲烷气体不易控制;碳化硅陶瓷靶的沉积过程稳定,硅碳原子比接近1:1.     

Influence of Oblique Sputtering on Stripe Magnetic Domain Structure and Magnetic Anisotropy of CoFeB Thin FilmsEI北大核心CSCD

Magnetic anisotropy is one of the most important fundamental properties of magnetic thin film. The strength of magnetic anisotropy determines the ferromagnetic resonance frequency of magnetic films in the high-frequency applications. Because of the directionality of conventional static magnetic anisotropy in magnetic film, the high-frequency device usually shows an obvious directionality. When the microwave magnetic fi eld deviates from the perpendicular direction of magnetic anisotropy, the devices cannot reveal their best performance. The magnetic film with a stripe magnetic domain structure displays an in-plane rotatable magnetic anisotropy, which can be an important strategy to solve the problem of magnetic fi eld orientation dependent performance in high-frequency device. Therefore, the magnetic domain, the magnetic anisotropy, and the high-frequency behaviors for magnetic fi lms with a stripe magnetic domain structure have received extensive attention. Previously, most of the studies focused on the stripe magnetic domain structure of polycrystalline thin films. However, less attention was paid on amorphous magnetic thin films. Since the amorphous magnetic films have no long-range ordered crystal structure, no magnetocrystalline anisotropy, no grain boundary defects resistance hindering the domain wall displacement, they usually show excellent soft magnetic properties and have been widely applied in high-frequency devices. CoFeB alloy is one of the most important amorphous magnetic materials and has been extensively applied in various spintronic devices. In this work, amorphous CoFeB magnetic thin films were prepared by using a method of oblique sputtering technique at room temperature. The influences of oblique sputtering on the stripe magnetic domain structure, the in-plane static magnetic anisotropy, the in-plane rotational magnetic anisotropy, and the perpendicular magnetic anisotropy of the amorphous CoFeB films were studied by scanning probe microscope, vibrating sample magnetometer, ferromagnetic resonance. It is found that the method of oblique sputtering could effectively reduce the critical thickness for the appearance of stripe magnetic domain in amorphous CoFeB films. For a non-oblique sputtered CoFeB film, the critical thickness for the appearance of the stripe magnetic domain is above 240 nm. In contrast, after been subjected to the oblique sputtering, the critical thickness becomes below 240 nm. The different magnetic characterizations indicate that for the growth of CoFeB films with stripe magnetic domain structure, the oblique sputtering could not only enhance the strength of in-plane static magnetic anisotropy, but also improve the in-plane rotational magnetic anisotropy and the perpendicular magnetic anisotropy. All of the magnetic anisotropies are increased with the angle of oblique sputtering. The observation results of XRD and TEM prove that the prepared CoFeB thin films tend to amorphous structure. The characterization of SEM observation indicates that although the amorphous CoFeB films do not possess long-range ordered crystalline structure, they still could form a kind of columnar structure. The slanted columnar structure of CoFeB films could significantly increase the perpendicular magnetic anisotropy, thus lead to the appearance of stripe magnetic domain structure.     

Influence of tantalum's crystal phase growth on the microstructural,electrical and mechanical properties of sputter-deposited tantalum thin film layer

High melting point refractory tantalum (Ta) metal is frequently grown into thin film layer for many applications in biomedical implants, microelectronic devices and micro-level mechanical systems. Tantalum growth mechanism is still in debate and the inconsistent crystal phase outcome has puzzled many, though it is certain that the properties of the grown film are highly dependent on the formed crystal phase configuration. The microstructure, surface morphology, crystal orientation and residual stress of the sputter-deposited Ta thin films using direct current (DC) magnetron sputtering technique are studied at 0.4 Pa – 2 Pa of sputtering pressure, 100 W – 250 W of DC sputtering power on bare silicon and silicon dioxide substrate and 10 min – 50 min of sputtering duration. α-phase Ta is preferably grown at high sputtering time (high thickness) and high DC sputtering power (high growth rate). The sputtering pressure affects the thin film's microstructural porosity while the sputtering power controls the crystallisation's quality. Both sputtering pressure and power affect the generated argon plasma in the DC magnetron sputterer where α-phase Ta is preferably formed at high plasma. The presence of 3 μm silicon dioxide underlayer makes no difference compared to bare silicon substrate. Our study reveals that β-phase Ta is grown first irrespective of sputtering conditions and then transformed into α-phase Ta after reaching a certain thickness. The grown major α-phase content promotes small thin film sheet resistivity (58.9 μΩcm – 86.1 μΩcm) and is suspected to be the dominant factor that increases the compressive stress within the thin film layer and reduces the adhesion of Ta layer onto the substrate surface. The study has given a new insight in controlling the conductivity and adhesion level of Ta thin film based on the grown phase layer.     

高功率脉冲磁控溅射制备的TiN薄膜 应力释放及其结合稳定性研究

目的 探究高功率脉冲磁控溅射（HPPMS）制备的氮化钛（TiN）薄膜在自然时效过程中,应力、薄膜/基体结合性能随时间的变化规律。方法 采用高功率脉冲磁控溅射（HPPMS）技术,通过调控基体偏压（-50、-150 V）,制备出具有不同残余压应力（3.18、7.46 GPa）的TiN薄膜,并采用基片曲率法、X射线衍射法、划痕法和超显微硬度计评价了薄膜的应力、薄膜/基体结合性能、硬度随时间的变化规律。结果 在沉积完成后1 h内,-50 V和-150 V基体偏压下制备的TiN薄膜压应力分别在3.12~3.39 GPa和7.40~7.55 GPa范围内波动,薄膜压应力没有发生明显变化;沉积完成后1~7天,平均每天分别下降28.57 MPa和35.71 MPa;7~30天,平均每天分别下降2.08 MPa和2.50 MPa;30~60天内,平均每天分别下降1.67 MPa和7.00 MPa。其压应力连续下降,且均表现出前期下降速率快,后期下降逐渐放缓的趋势。自然放置60天后,应力基本释放完毕,薄膜性质基本保持稳定。同时,薄膜/基体结合性能随时间逐渐变差,薄膜硬度下降。结论 HPPMS制备的TiN薄膜在自然时效过程中,其残余应力会随时间增加,连续下降,进而影响薄膜的力学性能。     

Effect of fabrication parameters on the microstructure,in-plane anisotropy and magnetostriction of Fe-Ga thin films

The microstructure,in-plane anisotropy,and magnetic properties of Fe-Ga thin films were investigated by X-ray diffraction analysis,vibrating sample magnetometer,and capacitive cantilever method.The in-plane induced anisotropy is well formed by the applied magnetic field during sputtering,and the anisotropy field Hk decreases with the sputtering power increasing.The coercivity of Fe-Ga thin films decreases with increasing power when the sputtering power is less than 60 W and increases when the power is larger than 60 W.The magnetostriction of the thin films reaches 66 × 10-6 at the sputtering power of 60 W.Excellent Fe-Ga films,which exhibit good field sensitivity,low coercivity and high magnetostriction,have been fabricated at the power of 60 W,and they can be used as the materials of magnetostrictive transducers.     

Technology of metal oxide thin film deposition with interruptions

The idea to obtain metal-oxide films with small grain size is to use a special regime of thin film deposition by r.f. sputtering of pure metal or metal oxide targets. This regime includes the deposition of thin films with one or several interruptions during the deposition process. WO₃ films were r.f. sputtered onto pure and oxidized silicon wafers. Four types of films were prepared, i.e. using continual deposition, one, two and three interrupted depositions with an actual deposition time of 40 min. The interruption time changed from 0.5 min to 5.0 min for the different samples. It was found that the total thickness of WO₃ films decreased with the increase of the number of interruptions and the increase in interruption time. Phase composition and features of surface morphology of the films deposited and annealed in the temperature range from room temperature to 900 °C have been investigated by XRD and AFM, respectively. It is shown that grain size in the metal oxide films decreased essentially with the increase of the number of interruption during the deposition process.     

Influence of carbon sputtering power on structure, corrosion resistance, adhesion strength and wear resistance of platinum/ruthenium/nitrogen doped diamond-like carbon thin films

Platinum/ruthenium/nitrogen doped diamond-like carbon (PtRuN-DLC) thin films were deposited on conductive p-Si substrates using a DC magnetron sputtering deposition system by varying carbon sputtering power. The chemical composition, bonding structure, surface morphology and adhesion strength of the PtRuN-DLC films were investigated using X-ray photoelectron spectroscopy (XPS), micro-Raman spectroscopy, atomic force microscopy (AFM), and micro-scratch test, respectively. The corrosion behavior of the PtRuN-DLC films in a 0.1 M NaCl solution was investigated using potentiodynamic polarization test. The corrosion results indicated that the corrosion resistance of the PtRuN-DLC films increased with increased carbon sputtering power probably due to decreased porosity level in the films with increased growth rate and film thickness. The wear performance of the PtRuN-DLC films was investigated with a ball-on-disc micro-tribometer. It was found that the increased carbon sputtering power significantly improved the wear performance of the films by enhancing the adhesion strength of the films.     

304不锈钢表面直流磁控溅射钛膜的耐蚀性

采用直流磁控溅射的方法在304不锈钢表面上制备金属钛薄膜,溅射5min后,通过扫描电镜(SEM)观察薄膜厚度为15μm。对比研究了304不锈钢镀膜前和镀膜后在FeCl3溶液中的腐蚀速率,通过显微镜观察两者在腐蚀之后的组织形貌,结果表明,通过在表面制备金属膜的方法(镀膜时间至少5min)可以有效提高304不锈钢在氯离子环境下的耐腐蚀性能。     

磁控溅射温度与时间对ZrN薄膜附着力的影响

采用非平衡磁控溅射技术在1Cr18Ni9Ti不锈钢上制备了ZrN薄膜。用SEM、EDS观察并分析了薄膜的表面形貌和成分,用光电轮廓仪测量了膜层厚度。并采用划格法测试不同溅射时间和温度制备的薄膜附着力大小。分析不同溅射时间和温度对薄膜附着力的影响规律。结果表明,通过调节磁控溅射时间和温度可以得到具有一定厚度,成分稳定,结构致密的ZrN薄膜,且溅射时间在1～20 min范围内时间越长薄膜附着力越大,溅射时间超过20 min,附着力趋于稳定;溅射温度在30～90℃范围内温度越高薄膜附着力越大,超过90℃溅射温度继续升高附着力减小。