离子束增强沉积TiN薄膜的研究

利用多功能离子束增强沉积设备，采用三种不同工艺方法制备ＴｉＮ薄膜，并对制备的ＴｉＮ薄膜进行了ＡＥＳ，ＸＰＳ，ＸＲＤ，ＲＢＳ和ＴＥＭ等分析。结果表明：所制备的薄膜都有很好均匀性，ＴｉＮ薄膜处在压应力状态；在溅射沉积的同时，在０－２０ｋｅＶ范围内，Ｎ＾＋和Ａｒ＾＋离子的轰击使得ＴｉＮ薄膜的生长呈现不同择优取向；随着Ｎ＾＋离子轰击能量的增加，制备的ＴｉＮ薄膜的晶粒增大。     

SiC埋层结构与C^＋注入剂量关系

采用ＭｅｔａｌＶａｐｏｒＶａｃｕｕｍＡｒｃ（ＭＥＶＶＡ）离子源的离子束合成法，往Ｓｉ衬底注入剂量为３．０×１０＾１７～１．６×１０＾１８ｃｍ＾－２的Ｃ＾＋制成ＳｉＣ埋层，Ｃ＾＋离子束的引出能量为５０ｋｅＶ，光电子能谱和红外吸收谱表明ＳｉＣ埋层的结构特征明显地依赖于剂量，采用ＭＥＶＶＡ离子源可以平均衬底温度低于４００℃时得到含有立方结构的ＳｉＣ埋层。     

高取向锐钛矿TiO2薄膜的MOCVD法制备与表征

采用热壁低压ＭＯＣＶＤ方法，以Ｔｉ（ＯＣ４Ｈ９）４为源在ＳｉＯ２／Ｓｉ衬底上制备出高取向锐钛矿ＴｉＯ２薄膜。用Ｘ射线衍射技术研究了沉积温度和衬底对薄膜的结构和相组成的影响规律，采用ＸＰＳ和ＳＥＭ分别研究了薄膜的组成和形貌，结果表明，当沉积温度为５００＾０Ｃ和６００＾０Ｃ时，薄膜为锐钛矿结构，３００＾０Ｃ和４００＾０Ｃ地，薄膜以无定形结构为主，薄膜的组成为ＴｉＯ２，衬底影响薄膜的相组成，不同沉积温度     

喷涂距离和喷涂功率对羟基磷灰石涂层的影响

本文以Ｔｉ－６Ａｌ－４Ｖ合金为基体材料,采用等离子喷涂方法,在不同喷涂距离和喷涂功率下制备羟基磷灰石（ＨＡ）涂层,研究喷涂距离和喷涂功率这两个重要的喷涂参数对涂层结构和组成的影响．使用扫描电子显微镜（ＳＥＭ）观察了羟基磷灰石涂层的形貌．涂层的相组成由Ｘ射线衍射谱仪（ＸＲＤ）分析而得．并使用Ｘ射线荧光谱仪（ＸＲＦ）测定了涂层的Ｃａ／Ｐ摩尔比．研究结果表明,喷涂距离对羟基磷灰石涂层的形貌、相组成以及Ｃａ／Ｐ摩尔比有着明显的影响．随着喷涂距离的增大,羟基磷灰石粉末的熔化状态得到改善,涂层的显微结构较为致密．然而,喷涂距离的增大使得涂层的非晶化更加严重,涂层中非晶相含量增大．在实验范围内,喷涂功率对涂层结构和相组成的影响不明显．Ｃａ／Ｐ比测定显示,等离子喷涂羟基磷灰石涂层均为缺磷涂层,Ｃａ／Ｐ比随喷涂距离的增大而降低,随喷涂功率的增大而增大．     

用PECVD技术淀积PbTiO3薄膜

采用ＰＥＣＶＤ技术，以Ｐｂ（Ｃ２Ｈ５）、ＨｉＣｌ４和Ｏ２为反应源，在１７０℃温度下沉积了ＰｂＴｉＯ３功能薄膜，分别对薄膜进行了Ｘ射线荧光光谱、Ｘ光电子能谱、Ｘ射线衍射光谱和扫描电镜的化学组成及形貌等分析。     

立方A^4＋M^5＋2O7型化合物与新型负热膨胀材料

概述了立方Ａ＾４＋Ｍ＾５＋２Ｏ７型化合物的结构特点，讨论了ＡＶ２－ｘＰｘＯ７型（Ａ＝Ｚｒ或Ｈｆ；ｘ＝０．１～１．２）及其部分取代的Ａ＾４＋１－ｙＢ＾４＋ｙＶ２－ｘＰｘＯ７型（Ｂ＝Ｔｉ，Ｃｅ，Ｔｈ，Ｕ，Ｍｏ，Ｐｔ，Ｐｂ，Ｓｎ，Ｇｅ或Ｓｉ；ｙ＝０．１～０．４）和Ａ＾４＋１－ｙＣ＾１＋ｙＤ＾３＋ｙＶ２－ｘＰｘＯ７型（Ｃ为碱金属元素，Ｄ为稀土金属元素）材料的负热膨胀性能。     

氧离子束辅助激光制备具有组构的YBCO薄膜

应用氧离子束辅助准分子脉冲激光沉积薄膜技术,先在ＮｉＣｒ合金（Ｈａｓｔｅｌｌｏｙ ｃ－２７５）基底上在室温下淀积具有平面织构的钇稳锆（ＹＳＺ） 缓冲层薄膜,再在 ＹＳＺ／ＮｉＣｒ基底上在 ７５０℃下制备具有平面织构和高临界电流密度的 ＹＢａ２Ｃｕ３Ｏ７－Ｘ（ＹＢＣＯ）薄膜、 ＹＳＺ和 ＹＢＣＯ薄膜都为 ｃ－轴取向和平面织构的, ＹＳＺ（２０２）和 ＹＢＣＯ（１０３）的 Ｘ射线扫描衍射峰的全宽半峰值分别为 １８＇和 １１＇．ＹＢＣＯ薄膜的临界温度和临界电流密度分别为 ９０Ｋ（Ｒ＝０）和 ７．９ｘ１０５Ａ／ｃｍ２（７７Ｋ,零磁场）．     

WO3/Si纳米晶薄膜的脉冲准分子激光沉积及结构分析

采用脉冲准分子激光大面积扫描沉积技术,在Ｓｉ（１１１）单晶衬底上沉积了 ＷＯ_ｘ薄膜．采用Ｘ射线衍射（ＸＲＤ）、喇曼光谱（ＲＳ）、付里叶红外光谱（ＦＴ－ＩＲ）及透射电镜扫描附件（ＳＴＥＭ）对不同条件下沉积的样品进行了结构分析．结果表明,氧分压和沉积温度是决定薄膜结构和成份的主要参数．在沉积温度３００℃以上及２０Ｐａ氧压下得到了三斜相纳米晶ＷＯ_３薄膜．     

Pb（Zr0.52Ti0.48）O3铁电薄膜的脉冲准分子激光沉积和快速…

用ＡｒＦ脉冲准分子激光在ＳＯＩ和Ｐｔ／ＳＯＩ衬底上沉积了Ｐｂ（Ｚｒ，Ｔｉ）Ｏ３铁电薄膜，并用快速退火进行热处理。Ｘ射线衍射，卢瑟辐背散射等分析表明：所结晶的薄膜是以（１００）和（１１０）为主要取向的多晶膜，且结晶情况与热处理温度和时间密切ＰＺＴ薄膜呈现铁电性，其剩余极化Ｐｒ＝１５μｃ／ｃｍ＾２，矫顽电场Ｅｃ＝５０ｋＶ／ｃｍ；并且具有较高的介电常数和较高的电阻率。     

新型渗透汽化透水膜的研制（II）：膜的结构和性能

确定聚合物共混的相容性最常用的方法是通过测定共混物的玻璃化转变温度（Ｔｇ），本文利用ＤＳＣ－７（Ｅｐｓｏｎ）测定了不同共混比的ＰＶＡ，ＣＳ共混物的玻璃化转变温度，结果表明ＰＶＡ，ＣＳ之间有良好的相容性。本文利用扫描电子显微镜（ＳＥＭ），红外光谱（ＩＲ）和Ｘ－射线衍射（ＸＲＤ）等现代分析仪器，对研制的多元酸交联的ＰＶＡ－ＣＳ／ＰＳＦ膜结构进行了观察测试，探讨了膜结构与性之间的关系。     

Electrophoretic deposition of carbon nanotubes–hydroxyapatite nanocomposites on titanium substrate

Carbon nanotubes–hydroxyapatite (CNTs–HA) composites were synthesized, using an in situ chemical method and characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). HA particles were uniformly absorbed on the CNTs, with strong interfacial bonding. The CNTs–HA composites behaved like single composites when deposited on a titanium substrate by electrophoretic deposition (EPD). EPD was carried out at 10, 20 and 40 V, for 0.5 to 8 min at each voltage. Coating efficiency and weight increased with increasing deposition time, while the slope of the curves decreased, indicating a decrease in deposition rate. The CNTs–HA coating morphology was analyzed with scanning electron microscopy (SEM). The results revealed that decreasing the voltage used for deposition coatings could reduce cracking frequency. Potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) studies showed that the deposition coatings protected the titanium substrate from corroding in simulated body fluid (SBF). In addition, in vitro cellular responses to the CNTs–HA coatings were assessed to investigate the proliferation and morphology of osteoblast cell line.     

Microstructure of thin film platinum electrodes on yttrium stabilized zirconia prepared by sputter deposition

(111) oriented thin film Pt electrodes were prepared on single crystals of yttrium-stabilized zirconia (YSZ) by sputter deposition of platinum. The electrodes were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), X-ray diffraction (XRD), energy-dispersive X-ray analysis (EDX), atomic force microscopy (AFM) and by profilometry. SEM images of the as-sputtered platinum film show a compact amorphous Pt film covering uniformly the substrate. Upon annealing at 1123 K, gaps and pores at the interface develop leading to a partial dewetting of the Pt film. Increasing the annealing temperature to 1373 K transforms the polycrystalline Pt film into single crystalline grains exhibiting a (111) orientation towards the substrate.     

Morphological and structural characterisation of osseointegrable Mn2+ and CO32− doped hydroxylapatite thin films

We report a morphological and structural study of osseointegrable hydroxylapatite thin films doped with divalent manganese and carbonate ions. The films were grown by pulsed laser deposition on medical grade Ti substrates at low oxygen pressure (13 Pa). Deposition targets were prepared from powders obtained by precipitation. During deposition, the substrates were kept at constant temperature within the temperature range 350–450 °C and the obtained films were subsequently annealed in hot water vapours at the deposition temperature. The films were characterised by scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), grazing incidence X-ray diffraction (GIXRD), energy dispersive X-ray spectrometry (EDS), and X-ray photoelectron spectroscopy (XPS). Film specimens for cross-section TEM were prepared by focused ion beam (FIB) machining. The inferred Ca/P atomic ratio in films varied between 1.6 and 1.8, depending on experimental conditions. XPS confirmed the presence of chemically bonded Mn²⁺. Cross-section TEM micrographs showed uniform thickness of the coatings, which consisted of amorphous and crystalline domains. Examination of the SEM micrographs revealed an increased smoothness of the surface with increase in substrate deposition temperature. XRD patterns of samples processed at temperatures over 400 °C showed well-crystallized hydroxylapatite, suggesting that deposition and annealing have to be performed at higher substrate temperature if highly crystalline coatings are required.     

Fabrication and characterization of bioactive glass coatings produced by the ion beam sputter deposition technique

Ion beam sputtering and ion beam sputtering/mixing deposition techniques were used to produce thin bioactive glass coatings on titanium substrate. It was found that as-deposited coatings were amorphous. Scanning electron microscopical examination showed that the coatings had a uniform and dense structure and that fabrication parameters affected the surface morphology of the coatings. The surface Ca/P ratio of the coatings, which varied from 5.9 to 8.6 according to semi-quantitative EDX analyses, was correlated with the fabrication condition. Depth profiling of the coatings revealed four distinct zones: the top surface, the thin coating zone, the intermixed zone of coating and substrate, and the substrate. Scratch tests showed that the coatings adhered well to the substrate.     

Synthesis and characterization of nanocrystalline silver coating of fly ash cenosphere particles by electroless process

Electroless nanocrystalline Ag coating of fly ash cenosphere particles utilizing a Sn-Pd catalyst system is demonstrated in this article. The deposition of pure metallic nanocrystalline Ag on the fly ash cenosphere particle surface is confirmed by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), and X-ray diffraction (XRD) analysis. Under the described conditions of electroless coating, average nanocrystalline Ag-coating thickness is observed to be approximately 220 nm, using a focused ion beam technique, which is less than that observed by transmission electron microscopy (TEM) (260-360 nm). TEM observation further reveals that the Ag-coating is made up of 50 nm Ag nanocrystallites, which is comparable with the size of approximately 37 nm obtained from the XRD data. The mechanism of the electroless Ag-coating process is discussed. Ag-coated fly ash particles find applications in manufacturing conducting polymers for electromagnetic interference shielding applications.     

FHA涂层的制备及生物活性

采用沉淀法制备了F掺杂HA的FHA(Ca_(10)(PO_4)_6(OH)F)粉末,并通过电泳沉积在钛合金(Ti6Al4V)表面制备了FHA涂层。通过X射线衍射(XRD),扫描电镜(SEM),能谱仪(EDS)研究了基体预处理方式对涂层形貌和结合力的影响,并且研究了涂层的生物活性。结果表明:酸处理后涂层表面有微裂纹存在,酸处理+碱处理后的涂层表面无裂纹并具有更高的结合强度;FHA涂层浸泡后表面形成缺钙类骨磷灰石,成花瓣状生长,长度为几百纳米,具有优良的生物活性。     

Growth and characterization of hydroxyapatite nanorice on TiO2 nanofibers

Hydroxyapatite (HA) coating with nanoparticles like nanorice is fabricated on chemically pretreated titanium (Ti) surface, through an electrochemical deposition approach, for biomaterial applications. The Ti surface was chemically patterned with anatase TiO₂ nanofibers. These nanofibers were prepared by in situ oxidation of Ti foils in a concentrated solution of H₂O₂ and NaOH, followed by proton exchange and calcinations. Afterward, TiO₂ nanofibers on Ti substrate were coated with HA nanoparticles like nanorice. The obtained samples were annealed at high temperature to produce inter diffusion between TiO₂ and HA layers. The resultant layers were characterized by Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), X-ray Photoelectron Spectroscopy (XPS), X-ray Diffraction (XRD), Infrared Spectroscopy (FTIR), corrosion tests in SBF solution, and Electron Probe Micro Analysis (EPMA). It was found that only Ti from the titanium substrate diffuses into the HA coating and a good corrosion resistance in simulated body fluid was obtained.     

Carbon coatings on silica glass optical fibers studied by reflectance Fourier-transform infrared spectroscopy and focused ion beam scanning electron microscopy

Carbon coatings applied on optical fibers via chemical vapor deposition were characterized by a resistance technique, focused ion beam/scanning electron microscopy (FIB/SEM), and reflectance Fourier-transform infrared spectroscopy (FTIR). The resistance technique measures the thickness of carbon film by measuring the resistance over a section of optical fiber, and backing out the film thickness. The FIB/SEM system was used to remove a cross section of the optical fiber and carbon coating and using a scanning transmission electron detector the thickness was measured. The FTIR approach is based on the fact that the wavelength of the light in the mid-infrared region (~ 10 μm) is significantly larger than the typical thickness of the carbon coatings (< 0.1 μm) which makes the coating “semi-transparent” to the infrared light. Carbon coating deposition results in significant transformations of the band profiles of silica in the reflectance spectra that were found to correlate with the carbon coating thickness for films ranging from 0.7 nm to 54.6 nm. The observed transformations of the reflectance spectra were explained within the framework of Fresnel reflection of light from a dual-layer sample. The advantage of this approach is a much higher spatial resolution in comparison with many other known methods and can be performed more quickly than many direct measurement techniques.     

SEM study of defects in PVD hard coatings

Hard coating defects are produced by foreign particle contamination on substrate surface before and during coating, or due to arcing. In this work, CrN, TiAlN and CrN/TiAlN multilayer hard coatings were prepared by thermoionic arc ion plating deposition system BAI 730 (Balzers) and by sputter deposition in CC800 (CemeCon). We investigated the concentration of defects, its size and structure after tool steel substrate surface pretreatment (polishing, ion etching) as well as after deposition by means of atomic force microscopy (AFM) and scanning electron microscopy (SEM).     

Formation of hydroxyapatite coating on titanium at 200°C through pulsed laser deposition followed by hydrothermal treatment

Pulsed laser deposition (PLD) has emerged as an acceptable technique to coat hydroxyapatite on titanium-based permanent implants for the use in orthopedics and dentistry. It requires substrate temperature higher than 400°C to form coatings of good adhesion and crystallinity. As this range of temperatures is likely to affect the bulk mechanical properties of the implant, lowering the substrate temperature during the coating process is crucial for the long-term performance of the implant. In the present study, hydroxyapatite target was ablated using a pulsed Nd:YAG laser (355 nm) onto commercially pure titanium substrates kept at 200°C. The coating thus obtained has been subjected to hydrothermal treatment at 200°C in an alkaline medium. The coatings were analysed using microscratch test, optical profilometry, scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), X-ray diffraction (XRD) and infrared spectroscopy (FTIR). XRD, EDS and FTIR showed that the as-deposited coating contained amorphous calcium phosphate and the hydrothermal treatment converted it into crystalline hydroxyapatite. The micro-morphology was granular, with an average size of 1 micron. In the micro-scratch test, a remarkable increase in adhesion with the substrate was seen as a result of the treatment. The plasma plume during the deposition has been analysed using optical emission spectroscopy, which revealed atomic and ionic species of calcium, phosphorous and oxygen. The outcomes demonstrate the possibility of obtaining adherent and crystalline hydroxyapatite on titanium substrate at 200°C through pulsed laser deposition and subsequent hydrothermal treatment.