衬底温度对FeCrCoNiMn高熵合金氮化物薄膜组织结构和电性能的影响

采用射频反应磁控溅射法在Si(100)衬底上制备出纳米晶高熵合金FeCrCoNiMn氮化物薄膜,结合场发射扫描电子显微镜(FESEM)、电子显微探针(EPMA)、X射线光电子能谱分析仪(XPS)、原子力显微镜(AFM)及四点探针(FPP)研究了衬底温度(40、300、500℃)对沉积薄膜的表面形貌、化学组成、微观结构和导电性能的影响。结果表明,衬底温度对高熵合金FeCrCoNiMn-N薄膜的形貌、组织结构和导电性能有显著影响。随衬底温度的升高,薄膜的表面粗糙度和颗粒/晶粒尺寸增大;与氮反应沉积后,含氮高熵合金薄膜中形成了Mn3N2、MnN、Cr2N和CrN金属氮化物,而Fe、Ni和Co元素则以Fe-Ni-Co合金相形式存在。不含氮合金薄膜其电阻率高达131.78mΩ·cm,加入氮沉积后,随衬底温度的增加,含氮薄膜的电阻率逐渐减小(6.14~0.43mΩ·cm),含氮合金薄膜的电阻率明显小于合金靶材的沉积膜,衬底温度500℃时薄膜的电阻率达到最小值0.43mΩ·cm。     

氧化铱薄膜的制备及其导电机理研究

采用脉冲激光沉积技术在Si(100)衬底上制备了高导电的IrO2薄膜,重点研究了退火前后其电学性能和微观结构的变化规律。采用X射线衍射(XRD)、原子力显微镜(AFM)、光电子能谱(XPS)和四探针法对退火前后IrO2薄膜的结构和电性能进行了表征,并利用霍尔效应研究了IrO2薄膜的导电机理。结果表明:IrO2薄膜在空气中退火后,导电性能得到提高,其中在750℃退火的电阻率达到最小值37μΩ.cm。在25～500℃范围内,IrO2薄膜的高温电阻率随着温度的升高呈线性关系逐渐增大,呈现出类似金属的导电特征。在250～400℃沉积的IrO2薄膜载流子的类型为p型;沉积温度较高(500℃)或在更高温度退火处理后,IrO2薄膜载流子的类型为n型,其导电机理以电子导电为主。     

Ru非磁性中间层的制备及其结构研究

以不同晶面的Si片作为基底,室温下,采用射频磁控溅射的方法制备得到Ru非磁性薄膜.利用X射线衍射仪(XRD)、扫描电子显微镜(SEM)和原子力显微镜(AFM)分析薄膜的结构和形貌.研究不同基底材料对Ru中间层结构和形貌的影响.结果表明:以单晶Si(100)、Si(110)、Si(111)片作为基底制备的Ru薄膜均呈(002)晶面的择优取向生长;Ru-Si(100)、Ru-Si(110)和Ru-Si(111)薄膜表面均由细小的圆形晶粒组成.Si(111)面上生长的Ru薄膜表面颗粒尺寸最小,表面粗糙度最大,有利于磁记录层磁学性能的提高.     

磁致伸合金薄膜的开发

利用反应溅射法制备Sm-Fe超磁致伸缩薄膜；直流磁控溅射蒸镀法制备Fe2.45-Sm合金压缩超磁致伸缩膜；在铜基片两面蒸镀Fe-Pd（拉伸）与Fe-Sm（压缩）磁致伸缩膜的复合材料。[编者按]     

溶胶凝胶法制备SiO2包覆Fe85Si9.6Al5.4软磁复合粉末

采用溶胶凝胶法,通过控制正硅酸乙酯(TEOS)和3-氨丙基三乙氧基硅烷(APTES)偶联剂的加入量,在Fe85Si9.6Al5.4粉末表面包覆SiO2绝缘层。采用X射线衍射(XRD)、傅氏变换红外光谱(FTIR)、X射线光电子能谱(XPS)、扫描电镜(SEM)和磁力显微镜(MFM)对粉末的微观结构及成分进行表征,采用振动样品磁强计(VSM)测试粉末的磁性能。结果表明:利用硅烷偶联剂对Fe85Si9.6Al5.4粉末表面改性后再加入TEOS,能在Fe85Si9.6Al5.4粉末表面包覆一层约1~2μm厚的絮状非晶SiO2;随着TEOS和APTES添加量的增多,SiO2包覆层的厚度也随之增加,饱和磁化强度Ms在0.86~0.90 T之间变化,Hci基本不变;当添加6 mLTEOS、1 mLAPTES时,得到的包覆粉末包覆效果及性能最佳,饱和磁化强度Ms达到0.90 T,矫顽力Hci为1 114A/m。     

热处理温度对Fe-Ni合金薄膜微结构及磁性的影响

采用直流电沉积法在硫酸盐-氯化物镀液中制备了Fe-44wt%Ni纳米晶合金薄膜.通过原子力显微镜(AFM)、X射线衍射(XRD)、透射电子显微镜(TEM)以及开路磁测量装置,对Fe-44wt%Ni合金薄膜镀态和退火态样品的微结构和磁性能进行测量.结果表明:退火温度升高能够降低薄膜内应力,使薄膜结晶均匀,但对薄膜晶粒尺寸和磁性能影响很大.Fe-44wt%Ni合金薄膜是由γ-(Fe,Ni)相和α-(Fe,Ni)相构成.在250℃真空退火处理1h后Fe-44wt%Ni合金薄膜的晶粒尺寸在20～30 nm之间,且具有良好的软磁性能,饱和磁感应强度BS为1.06T,矫顽力HC为40A/m.     

蒸镀法制备ZnS光学薄膜研究

采用真空蒸镀法在Si(111)基板上制备了ZnS光学薄膜,并系统研究了蒸发温度、沉积时间、基板距蒸发源的位置等因素对所制备薄膜物相及显微结构的影响.用X-射线衍射(XRD)、原子力显微镜(AFM)对制备的薄膜进行了表征.结果表明:制备薄膜的物相主要以β-znS闪锌矿(Sphalerite)为主,并有少量的α-ZnS纤锌矿(Wurtzite),薄膜具有(111)结晶取向的生长特征.当沉积温度为1200℃时,所制备薄膜的结晶性能较好,随沉积时间延长,薄膜的结晶性能降低.     

专利名称：在扫描探针显微镜悬臂及其针尖上沉积薄膜的方法

一种利用荷能团簇在扫描探针显微镜悬臂及其针尖上沉积薄膜的方法，包括下列步骤：溅射室的溅射靶架放置溅射靶材；在沉积室的靶架上粘贴扫描探针显微镜（AFM）的悬臂，并确保针尖向外；使靶架和待沉积薄膜的AFM悬臂处于一铜屏蔽室中；用两套真空系统同时分别对溅射室和沉积室抽真空；在溅射室中充入惰性气体Ar，使溅室真空度达8～20Pa，     

以Cu-Ti复合渗镀为先导的Si3N4陶瓷/金属钎焊连接

提出一种陶瓷表面多元离子复合渗镀合金化方法,采用该方法对Si3N4陶瓷表面进行Cu-Ti复合渗镀,然后在复合渗镀真空设备中进行渗镀Cu-Ti的Si3N4陶瓷与金属的钎焊.对Si3N4陶瓷表面的Cu-Ti渗镀合金层进行了EDS、XRD、SEM、OM测试分析和声发射划痕试验.结果表明,渗镀层中含有Cu、Ti、Fe、Si及Al元素,Cu、Ti分布比较均匀,渗镀合金层由Cu、CuTi2、TiSi2组成;声发射划痕试验结果表明,在100 N的最大载荷下,渗镀合金层与陶瓷基体未发生剥离和崩落现象.在100倍的光学显微镜及5000倍的电子显微镜下,钎焊接头中陶瓷/金属界面接合良好,无明显的宏观和微观缺陷.可在较低的真空度下实现陶瓷/金属钎焊,为陶瓷/金属钎焊连接提供了一个新方法.     

空心微球表面化学镀Ni薄膜的工艺研究

比较空心微球表面化学镀Ni薄膜的工艺.分别以Sn-Pd胶体溶液和[Ag(NH3)2]+溶液作为活化剂,将空心微球表面进行活化,再采用化学镀的方法分别在其上淀积金属Ni薄膜.使用扫描电子显微镜(SEM)、能量色散光谱(EDS)和X-射线衍射光谱(XRD)对两种工艺所镀Ni薄膜的表面微观结构和组分进行表征.结果表明:用Sn-Pd胶体溶液活化后的空心微球表面淀积了均匀、致密的金属Ni薄膜,该薄膜是由大小约100 nm的颗粒组成;而以[Ag(NH3)2]+溶液活化后的空心微球表面淀积的金属Ni薄膜,是由大小约1 μm的颗粒组成.并分析了这两种镀层形成的机理.     

Thermally-treated Pt-coated silicon AFM tips for wear resistance in ferroelectric data storage

In ferroelectric data storage, a conductive atomic force microscopy (AFM) probe with a noble metal coating is placed in contact with a lead zirconate titanate (PZT) film. The understanding and improvement of probe tip wear, particularly at high velocities, is needed for high data rate recording. A commercial Pt-coated silicon AFM probe was thermally treated in order to form platinum silicide at the near-surface. Nanoindentation, nanoscratch and wear experiments were performed to evaluate the mechanical properties and wear performance at high velocities. The thermally treated tip exhibited lower wear than the untreated tip. The tip wear mechanism is adhesive and abrasive wear with some evidence of impact wear. The enhancement in mechanical properties and wear resistance in the thermally treated film is attributed to silicide formation in the near-surface. Auger electron spectroscopy and electrical resistivity measurements confirm the formation of platinum silicide. This study advances the understanding of thin film nanoscale surface interactions.     

蘸水笔刻蚀技术(DPN)影响因素分析

蘸水笔技术(Dip-Pen)是近年来发展起来的一种新的扫描探针刻蚀加工技术,有着广泛的应用前景.该技术是直接把弯曲形水层作为媒介来转移"墨汁"分子,在样品表面形成纳米结构.尖端曲率半径、针尖在基底表面滞留时间、针尖扫描速度、空气湿度、表面粗糙度等均会影响纳米结构的线宽.针尖在基底表面滞留时间与圆半径的平方成一次函数关系,线宽随着尖端半径的增大而变宽,扫描速度与线宽成反比关系.通过控制湿度可以控制"墨水"分子的转移速度,从而影响纳米结构的线宽.线宽随着样品表面粗糙度增加而变宽.     

Preparation of Fe/Cr doped SiO2 thin film on 304 stainless steel substrate originated from corrosion

Abstract

A Fe/Cr doped SiO₂ thin film which can improve the anticorrosion characteristic of materials was prepared on SUS304 stainless steel substrates by a modified hydrothermal method that constitutes a two part preparation process. The corrosion of stainless steel and the dissolution of silica from Na–Ca glass are simultaneously stimulated by an aqueous lithium bromide solution, and then a Fe/Cr doped SiO₂ thin film is coated onto the substrate. The Fe/Cr doped SiO₂ film was characterised by scanning electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy and electron probe X-ray microanalyser. The results showed that the corrosion products and the silica are combined to form a Fe/Cr doped SiO₂ thin film. Furthermore, a chemical bond is formed between the silicon coating and the metal that improves the compactness and the adhesive property of the film. The anticorrosion characteristics of the film were measured by the methods of weight loss and electrochemical potentiodynamic polarisation, indicating that the Fe/Cr doped SiO₂ thin film can improve the anticorrosion performance of stainless steels effectively.     

磁控溅射法制备硅钼薄膜及其性能表征

用射频磁控溅射法在硅基底上成功制备出具有低电阻率的单一四方相二硅化钼薄膜，并通过X射线衍射仪、原子力显微镜及四探针电阻测试仪对退火前后的薄膜样品进行了结构和电学性能分析。结果表明：薄膜的电学特性强烈依赖于薄膜的微结构和相组成。沉积态薄膜主要为非晶结构。经高温退火后，薄膜的晶态结构发生显著的变化，晶化效果明显提高，薄膜方阻大幅降低。     

Si和316L基片上TiN薄膜微观结构和应力的对比分析

目的 比较Si和316L基片上Ti N薄膜的微观结构和应力,分析基片材料和基片初始曲率对薄膜应力的影响。方法 采用电弧离子镀技术在Si基片和316L基片上制备了Ti N薄膜,实测了薄膜应力,通过XRD、SEM、TEM等方法对薄膜的微观结构进行了分析。运用有限元分析技术,以结构力学为原理,分别对不同初始曲率的Si基片和316L基片上的薄膜应力测试进行了计算和校正应用。结果 相同工艺条件下,316L基片上Ti N薄膜的应力比Si基片上的大。Ti N薄膜应力随偏压的增大而增大。薄膜生长至近表面都形成了柱状晶结构,316L基片与Ti N薄膜的膜基界面处出现较多的半共格生长结构,而Si基片的膜基界面结合以纳米晶混合为主。基片的初始曲率半径会导致薄膜应力测试产生误差,初始半径越小,引起的误差越大。结论 偏压作用下,316L基片上薄膜会产生更大的压应力。316L与Ti N薄膜的膜基界面结合更好,有利于其承受更高的薄膜应力。316L基片的初始曲率半径显著小于Si基片,由此引起的薄膜应力测试误差较大,有必要对316L基片上的薄膜应力测试结果进行校正。     

Discrete and continuous deformation during nanoindentation of thin films

This paper describes nanoindentation experiments on thin films of polycrystalline Al of known texture and different thicknesses, and of single crystal Al of different crystallographic orientations. Both single-crystalline and polycrystalline films, 400–1000 nm in thickness, are found to exhibit multiple bursts of indenter penetration displacement, h, at approximately constant indentation loads, P. Recent results from the nanoindentation studies of Suresh et al. (Suresh, S., Nieh T.-G. and Choi, B.W., Scripta mater., 1999, 41, 951) along with new microscopy observations of thin films of polycrystalline Cu on Si substrates are also examined in an attempt to extract some general trends on the discrete and continuous deformation processes. The onset of the first displacement burst, which is essentially independent of film thickness, appears to occur when the computed maximum shear stress at the indenter tip approaches the theoretical shear strength of the metal films for all the cases examined. It is reasoned that these displacement bursts are triggered by the nucleation of dislocations in the thin films. A simple model to estimate the size of the prismatic dislocation loops is presented along with observations of deformation using transmission electron microscopy and atomic force microscopy. It is demonstrated that the response of the nanoindented film is composed of purely elastic behavior with intermittent microplasticity. The overall plastic response of the metal films, as determined from nanoindentation, is shown to scale with film thickness, in qualitative agreement with the trends seen in wafer curvature or X-ray diffraction measurements.     

Improvement of soft magnetic properties of CoFeSiB thin film by external magnetic field and Zr addition

Co₄₀Fe₁₇Si₃₂B₁₁ thin film (150 nm) was deposited by using an RF magnetron co-sputtering system on a Si (100) substrate. A self-designed substrate holder, including various hard magnets arranged around the substrates, was utilized so that various external magnetic fields could be applied to the Si substrates during the film deposition. By the effect of this deposition field, the applied field during the sample deposition, the squareness of the CoFeSiB thin film was significantly enhanced. From the angular analysis of the magnetic hysteresis curves from easy (parallel to external magnetic field) to hard (perpendicular to external magnetic field) direction of magnetization, it can be deduced that Co and Fe atoms were magnetically arranged to the easy magnetization axis by an external magnetic field which was induced during deposition. Also, the compositional cluster size of the CoFeSiB thin film was remarkably reduced by Zr addition, causing a decrease in the value of coercivity. These results suggest that apparent magnetic anisotropy was achieved, and the soft magnetic property of the CoFeSiB thin film was remarkably enhanced by the combination of the deposition field and Zr addition.     

Numerical analysis on thickness effect of magnetic thin films on conduction noise absorption in microstrip line

Noise absorbing properties of two kinds of magnetic thin films (one is electrically conductive Co-Zr-O granular thin film and the other is Ni-Zn ferrite thin film with high electrical resistivity) are analyzed by the finite element method (FEM) with various film thicknesses. For the Ni-Zn ferrite film with high electrical resistivity (～2 × 10 ² Ωm), a low reflection parameter (S₁₁) value is predicted, and the value does not significantly change with increased film thickness up to 10 μm. However, the transmission parameter (S₂₁) is reduced with increased film thickness due to increased power absorption by magnetic loss. For the Co-Zr-O thin films with low electrical resistivity (～1.6 × 10^?5 Ωm), however, reflection signal is increased with increased film thickness due to diminished sheet resistance of the thin film. Transmission loss is not very sensitive to the thickness of the conductive film. Large power absorption is, therefore, predicted for conductive film of smaller thickness. It is concluded that film thickness is an important control parameter for the achievement of a highly absorptive thin film with increased electrical conductivity.     

On the use of atomic force microscopy for structural mapping of metallic-glass thin films

In this article, we discuss the recent use of the high-resolution dynamic atomic force microscopy (DAFM) in mapping the nano-scale dynamical structural heterogeneity in thin film metallic-glasses (TFMGs). Our focus is laid on the major factors which can influence the structural contrast in the DAFM images, such as tip radius, free-amplitude, set-point amplitude and surface roughness. Finally, through a comparative study of different TFMGs and single-crystal silicon, we demonstrate that the DAFM technique is effective in distinguishing different nanostructures through their energy dissipation spectra.     

定向沉积法对Nd2Fe14B薄膜形态和磁性能的影响

采用直流励磁性溅射法制备Nd2Fe14B稀土磁薄膜。通过对衬底预热，在溅射过程中持续动态加热并保湿10min，实现定向沉积。主要考虑了该方法对薄膜磁性能的影响。结果表明薄膜取向度良好，有明显柱状生长迹象。薄膜矫顽力大磊提高，H1/HII比值改善。在预热湿度200℃逐渐加热到500℃并保湿10min时，薄膜磁性能最佳。