Contents List and Abstracts from the Journal of the Adhesion Society of Japan

FTIR reflection spectroscopy was used to characterize thin films of a cyanurate prepolymer on evaporated aluminium and on silicon single crystal wafers. Both substrates are covered by their native oxides. The optical function of the prepolymer is derived from ATR measurements. The measured thin film reflectance spectra have to be interpreted in comparison with the corresponding bulk spectra obtained by simulation. All samples re-produce the bulk composition. The cyanate groups of the prepolymer are not involved in specific intermolecular interactions or in preferential orientation. This is also found for the triazine rings on Si. On Al, however, a considerable excess of triazine rings are oriented parallel to the interface. The vibration frequencies of the triazine groupings that are perpendicular to the Al substrate show a red shift to some 2–8 c^?1. This special interaction effect does not occur on Si. Both the preferential orientation and the specific inter-molecular interaction act at least 100 nm into the prepolymer layer.     

Studies on the Interphase of a Model Adhesive Joint

Ultra-thin films of a dicyanate bisphenol A prepolymer on aluminium or silicon substrates are studied as a model for an adhesive interphase. AFM shows structural details of the films with a lateral resolution from some 10 nm up to a few microns. Substrates have to be very flat in order to obtain continuous prepolymer layers. So the aluminium roughness of a few nanometers results in a discontinuous prepolymer distribution below about 10 nm thickness while the films remain intact down to 2 nm on the smoother silicon. XPS and IR spectroscopy show that the as-prepared layers do not undergo serious chemical changes or pronounced adhesive interactions. The native silicon surface is totally inert. The cyanate group is not involved at all. The native aluminium surface induces changes both in energy and orientation of the triazine rings, however. This may be considered as an indirect hint on some adhesive interaction of the cyanurate prepolymer with the aluminium substrate but the experimental facts do not explain the adhesion mechanism in detail yet.     

Raman Spectroscopy of Nanocrystalline Ceria and Zirconia Thin Films

The results of Raman-scattering studies of nanocrystalline CeO₂ and ZrO₂:16% Y (YSZ) thin films are presented. The relationship between the lattice disorder and the form of the Raman spectra is discussed and correlated with the microstructure. It is shown that the Raman line shape results from phonon confinement and spatial correlation effects and yields information about the material nonstoichiometry level.     

Comparison of Ion Irradiation Effects in Silicon-Based Preceramic Thin Films

Thin films of polymers (polysiloxanes, polycarbosilanes, and polysilazanes) and alkoxide-derived siloxane gels, precursors for SiC, SiCN, SiOC, and SiOBC ceramics, were irradiated with increasing fluences of C or Au ions to study the kinetics of their conversion into ceramics. Ion beam analyses showed that the main effect of irradiation on the composition of the films is the selective release of H₂ by radiolysis. During subsequent high-temperature annealing of films converted as much as possible by irradiation, CO _x , CH _x , or silane molecules do not evolve, contrary to what is observed during the pyrolysis of unirradiated precursor films. According to Raman analyses, a large proportion of the carbon atoms segregate into clusters after irradiation and in films converted by direct pyrolysis (or combined treatments). However, carbon particles formed during irradiation are more diamond-like, affording films with 2—3 times higher hardness, as shown by nanoindentation tests. In both types of ceramics (SiC or SiOC), the optimal properties (hardness, thermal stability, and photoluminescence) associated with C segregation are obtained for a C/Si ratio of the order of 1. Boron addition is detrimental to hardening of SiOC glasses, in contrast to nitrogen.     

Infrared Reflection Spectroscopy and Effective Medium Modeling of As-Anodized and Oxidized Porous Silicon Carbide

We present a study of the infrared reflectance of porous silicon carbide (PSC) formed by the electrochemical dissolution of silicon carbide substrates of both 6H and 4H polytypes. The reflectance from n-PSC, both as-anodized and passivated, is reported for the first time. The passivation of PSC has been accomplished using a short thermal oxidation. Fourier transform infrared (FTIR) reflectance spectroscopy is employed ex situ after different stages of the thermal oxidation process. The characteristics of the reststrahlen band normally observed in bulk SiC are altered by anodization; further changes in the reflectance spectra occur following oxidation for different periods of time. An effective medium theory model that includes air, SiC and SiO₂ as component materials is shown to characterize the observed changes in the reflectance spectra after different stages of PSC oxidation.     

Preparation of b-Axis-Oriented MFI Zeolite Thin Films Using Slow Dissolution of Source Material

A novel in situ hydrothermal method involving the slow dissolution of silicate glasses as a source material was used to successfully prepare b -axis-oriented high-silica zeolite ZSM-5 (MFI) thin films.     

自洁净玻璃纳米TiO2薄膜制备的研究进展

自洁净玻璃是采用特有的镀膜工艺在玻璃表面上制备纳米TiO2薄膜的新型环保智能产品,具有广泛的用途,其中纳米TiO2薄膜的制备是关键。综述了自洁净玻璃表面纳米TiO2薄膜的制备方法,包括基片的清洗方法、溶胶的制备方法及薄膜的涂覆方法。     

基片上镀TiO2薄膜光催化降解有机磷农药

以基片上镀ＴiO2薄膜为光催化剂降解有机磷农药. 结果表明,基片为铜丝比基片为钛网和硅片时光催化降解率高;随光照时间延长,光降解率增大;当溶液pH值为2时,光降解率最高;对于钛网,当退火温度为450℃时光催化降解率最大;用HNO3调节溶液pH值比用H2SO4和HCl调节光降解率高;膜使用次数越多,光催化活性越小;硫杆磷酸酯类农药比磷酸酯类农药更容易发生光催化降解;农药浓度越稀,越容易进行光催化降解. 当用铜丝作为基底物、光照时间为60 min 时,光催化降解率可高于80%.     

衬底取向对 Al 掺杂3C-SiC 薄膜微结构的影响

采用低压化学气相沉积(LPCVD)法分别在 Si(100)和 Si(111)衬底上制备了 Al 掺杂的3C-SiC 薄膜。采用 X 射线衍射、扫描电子显微镜、Raman 光谱对所制备薄膜的微结构、形貌以及内部应力的演变进行分析。结果表明：在 Si(100)衬底上制备的 Al 掺杂 SiC 薄膜具有较好的结晶质量,而且结晶质量受 Al 掺杂浓度的影响比较大。Al 掺杂 SiC 薄膜的生长模式为二维层状生长模式。Si(100)衬底上所制备的 Al 掺杂 SiC 薄膜表面为层状的四边形结构,而 Si(111)衬底上的 Al 掺杂 SiC 薄膜表面为层状的截角三角形结构。Si(100)衬底上的薄膜厚度略大于 Si(111)衬底上的。由于 Al 离子的掺入和薄膜厚度的增加,Si(100)衬底上所制备的 Al 掺杂 SiC 薄膜内部的应力得到很好的释放。Si(111)衬底上的 Al 掺杂 SiC 薄膜内部的应力则由张应力模式转为压应力模式,而且纵光学声子(LO)、横光学声子(TO)特征峰分离变大,出现这种现象的原因可能与 Al3+替代 Si4+使 SiC离子性增强和生长模式的转变有关。     

衬底温度对Al2O3(0001)表面外延6H-SiC薄膜的影响

采用固源分子束外延技术,以α-Al2O3(0001)为衬底,在不同衬底温度下制备了6H-SiC薄膜.利用反射式高能电子衍射,原子力显微镜、X射线衍射对生长样品的结构和结晶质量进行了表征.结果表明:在衬底温度为1100℃时生长的薄膜质量较好,在较低温度(1000℃)和较高温度(1200℃)条件下生长的薄膜质量较差.同时发...     

TiO2/SiO2复合薄膜的形成历程与超亲水性关系

考察了溶胶-凝胶法制备TiO2／SiO2复合薄膜过程中,正硅酸乙酯(TEOS)的水解时间与膜的超亲水性的关系,通过XRD分析了SiO2添加量对TiO2锐钛矿晶型的影响,并研究复合薄膜的表面处理对其亲水性的影响。实验发现,当无因次反应时间为0．4时,复合薄膜的亲水性最好;SiO2的引入能够抑制金红石晶型的生长,最佳含量在10～20％。     

Sol–Gel Fabrication of Epitaxial and Oriented TiO2 Thin Films

Thin films of titania have been prepared by spin coating on fused silica, Si(100), and rutile(110), starting with a sol–gel process. The alkoxide solution was chelated with diisopropanolamine, and the resulting precursor solution was hydrolyzed prior to coating. Oriented rutile films were obtained on fused silica and Si(100), while epitaxially oriented film was formed on rutile (110). X-ray diffraction results indicated that the as-deposited films transformed to rutile via anatase with increasing temperature. The phase transformation temperature was found to be dependent on the substrate, and it was in general higher on the substrates than that observed for the gel powder. Microstructural studies revealed that these films consisted of finely dispersed grains of 0.05 to 0.15 μm in size.     

玻璃基底表面抗蛋白吸附膜的制备及性能测试

通过分子自组装技术和原子转移自由基聚合方法(ATRP)在玻璃基底表面分别制备了不同的抗蛋白吸附膜,采用接触角测量,光波导模式谱仪和荧光标记蛋白的吸附对膜表面性能进行了测试。结果表明,两种方式形成的3种抗蛋白吸附膜能够阻止绝大部分的蛋白吸附,其中ATRP方式形成的聚乙二醇(PEG)膜表面其抗蛋白吸附性能略优于自组装膜,而磺酸基甜菜碱—异丁烯酸(SBMA)形成的聚合物刷相比于PEG具有更好的抗蛋白吸附能力。     

氧化钒薄膜制备方法专利技术分析

氧化钒由于其独特的光电性能在红外探测器、光电调节器、智能窗、光存储及传感器等应用领域备受关注。对制备氧化钒薄膜采用的专利技术进行了梳理,对日后氧化钒薄膜的制备及性能优化具有很好的指导意义。     

PECVD制备富硅氮化硅薄膜的工艺条件及其性质的研究

采用等离子体增强化学气相沉积法(PECVD)以SiH4和N2为反应气体,分别在射频功率、硅烷稀释度[SiH4/N2]、衬底温度为变量的情况下制备了富硅氮化硅薄膜材料,利用X射线衍射谱(XRD)、傅里叶变换红外谱(FTIR)、紫外-可见光吸收谱(UV-Vis)对薄膜材料进行了表征,并研究了薄膜材料的微结构和晶化状况、光学特性等.实验结果表明,所沉积薄膜都为富硅的非晶氮化硅材料,改变射频功率、硅烷稀释度和衬底温度可以控制氮化硅薄膜中N元素的含量、光学带隙的大小和薄膜的折射率,并制备出最适宜富硅氮化硅薄膜,为进一步退火析出硅量子点奠定了基础.     

工艺参数对TiO2薄膜性能的影响

研究了基本工艺参数（如聚乙二醇的添加量和分子量、热处理制度、薄膜层数）对溶胶凝胶法制备TiO2薄膜性能的影响。结果表明：添加分子量2000的聚乙二醇1．0g（相对于100ml溶胶）,以2℃/min的速度缓慢升温至550℃,保温1h,制得的TiO2 10层薄膜,表现出分解稀醋酸的光催化活性较好。     

铁电薄膜的制备工艺及发展趋势

随着陶瓷材料新技术生产发展的需求,多功能的铁电薄膜材料日益引起科研人员的广泛关注,并成为近年来研究的热点。论述了铁电薄膜的发展过程、种类、性能以及应用,着重介绍了铁电薄膜的制备方法,并指出了铁电薄膜的发展趋势。     

Effect of Precursor Pyrolysis on the Dielectric Properties of Hydrothermally Derived Barium Titanate Thin Films

BaTiO₃ thin films were processed hydrothermally on Ag-coated quartz substrates at 90°C by reacting films of titanium dimethoxy dineodecanoate (TDD) in aqueous solutions of Ba(OH)₂. Two reaction sequences were used: either the TDD was reacted directly in aqueous Ba(OH)₂, or the TDD was first pyrolyzed in air at temperatures ranging from 200° to 500°C before hydrothermal reaction. Depending on the processing conditions, the dielectric constant of the thin films ranged from 5 to 170, the dielectric constant increasing with increasing pyrolysis temperature. Thin film porosimetry data suggest that the improvement in film dielectric performance is related to decreases in thin film residual porosity after hydrothermal reaction.     

溶胶凝胶法制备PbTiO3薄膜的研究

利用ＩＲ、ＤＴＡ、ＴＧ、ＸＲＤ及Ｒａｍａｎ光谱等测试手段,研究了乙酰丙酮改性的Ｐｂ－Ｔｉ系统的溶胶凝胶过程。结果表明通过乙酰丙酮的改性可以得到稳定的溶胶前驱体,由此溶胶制备的薄膜在６００℃即形成完全晶化的钛酸铅薄膜。