Thermoanalytical methods in the study of inorganic thin films

Thermoanalytical (TA) methods are relatively seldom applied for assessing the physical and chemical proeprties of thin films, but they can be used in studies of composition, phase transitions and film—substrate interactions. In the present paper the possibilities of TA methods in thin film studies are reviewed. The thermoanalytical methods considered are the classical TG and DTA/DSC methods but some complementary methods will also be briefly mentioned. The main emphasis is given to true thin films. Details of sample preparation are also given. An important application of TA methods is characterization of precursors for the CVD growth of thin films, and this is also discussed.     

The application of dielectric analysis to drying latex films

Measurements of real and imaginary capacitance (C andC) have been made during the drying of a film-forming latex. In one experiment dielectric measurements at frequencies between 1 Hz and 100 kHz were made simultaneously with gravimetric measurements on a microbalance. It was found that both the rate of water evaporation and the a.c. conductance decrease sharply at high polymer volume fraction. These results are discussed qualitatively in terms of a model for the film-forming process. In another experimentC andC were recorded at 10 Hz along with automatic measurements of the build-up of the scratch resistance of the film. It was found that the mechanical response to film-formation appears significantly earlier than the dielectric response. This is also discussed qualitatively in terms of the model.The authors would like to thank Dr. I. Abrahams, Dr. S. Bell, and Dr. M. Reading for useful discussions regarding this work and M. Bahra for his help with the TFA measurements.     

Surfactant in the gaseous phase II. Influence on stability of foams and thin liquid films

The influence of the vapors ofn-amyl orn-decyl alcohol on the stability of single thin liquid films, single bubbles, and foam columns was determined. It was found that the presence of surfactant vapors lowered the stability of foams and single foam films. The mechanism of the destabilizing action of the surfactant vapors on wet, dynamic foams under dynamic conditions is discussed. It is shown that the destabilizing action of the surfactant vapors is a further indication that surface elasticity forces are the main factor determining stability of wet, dynamic foams.     

Silica-supported PtSn alloy doped with Ga, In or, Tl: Characterization and catalytic behaviour in n-hexane dehydrogenation

Silica-supported trimetallic catalysts containing Pt, Sn and a group 13 metal (PtSnM, M=Ga, In, Tl) were prepared by consecutive impregnation steps from cis-[PtCl₂(PPh₃)₂] and chloride precursors. X-ray diffraction (XRD), transmission electron microscopy (TEM), selected-area electron diffraction (ED) and energy dispersive X-ray analysis (EDX) showed large platelet-like particles of PtSn_1−xM_x phases. PtSnGa catalyst with a Pt/(Sn+Ga) molar ratio of 1.72 showed a bimodal particle distribution and a Pt phase was identified. Differences in surface structures were also revealed by the performance of catalysts in the dehydrogenation of n-hexane. For PtSnIn and PtSnTl (Pt/(Sn+M) molar ratio of about 1) the dehydrogenation was favoured. In contrast, PtSnGa catalyst yielded hydrogenolysis products. Photoelectron spectra showed the Pt 4f_7/2 level at a binding energy of 70.0–71.8 eV in all cases. Moreover, the FT-IR spectra of chemisorbed CO on the PtSnGa showed a slight shift in the ν(CO) toward higher values with respect to the monometallic catalyst, pointing to an electronic effect in accordance with photoelectron spectroscopy.     

Room temperature oxidation of lead-indium alloy films

The kinetics of growth of thin (14 to 40Å) oxide layers on lead-indium alloys was investigated ellipsometrically, using: 3000Å thick films at 23°C; and oxygen exposures at 760 torr for times ranging from five minutes to five days. Assuming that the oxide layer is comprised of a two-phase mixture of PbO and In₂O₃ having a negligible extinction coefficient made it possible to estimate the oxide composition from the ellipsometrically-obtained oxide refractive index. Under these oxidizing conditions, the volume fraction of PbO in the oxide mixture decreases from a value of unity for pure lead to zero for alloys containing more than 30 at. percent In, in agreement with the Auger Electron Spectroscopy results of Chou and coworkers. The oxidation rate equals a exp (X₁/X), where α and X₁ will be seen to vary complexly with alloy composition. A theoretical explanation of these results is also presented.     

Smart Biopolymer-Based Nanocomposite Materials Containing pH-Sensing Colorimetric Indicators for Food Freshness Monitoring

Nanocomposite biopolymer materials containing colorimetric pH-responsive indicators were prepared from gelatin and chitosan nanofibers. Plant-based extracts from barberry and saffron, which both contained anthocyanins, were used as pH indicators. Incorporation of the anthocyanins into the biopolymer films increased their mechanical, water-barrier, and light-screening properties. Infrared spectroscopy and scanning electron microscopy analysis indicated that a uniform biopolymer matrix was formed, with the anthocyanins distributed evenly throughout them. The anthocyanins in the composite films changed color in response to alterations in pH or ammonia gas levels, which was used to monitor changes in the freshness of packaged fish during storage. The anthocyanins also exhibited antioxidant and antimicrobial activity, which meant that they could also be used to slow down the degradation of the fish. Thus, natural anthocyanins could be used as both freshness indicators and preservatives in biopolymer-based nanocomposite packaging materials. These novel materials may therefore be useful alternatives to synthetic plastics for some food packaging applications, thereby improving the environmental friendliness and sustainability of the food supply.     

Al掺杂ZnO薄膜原子力显微图像的多重分形研究

用原子力显微镜观察溶胶-凝胶法制备Al掺杂znO薄膜的表面形貌,运用多重分形理论研究Al掺杂ZnO薄膜的原子力显微图像,多重分形谱可以很好地定量表征薄膜的表面形貌.结果显示:Al掺杂量为0.5 at.%的ZnO薄膜经550℃退火处理后,rms粗糙度为1.817,Al掺杂量为1.0 at.%的ZnO薄膜经600℃退火处理后,rms粗糙度增大到4.625,相应的分形谱宽△α从0.019增大到0.287,分形参数△f由-0.075变为0.124.     

负色散镜的设计、制备及在掺钛蓝宝石激光谐振腔内的使用

根据钛宝石激光器的要求设计了性能优良的两种负色散镜(NDM1和NDM2)。NDM1同时引入啁啾效应和G-T效应产生大的群延迟色散量以减少光在负色散镜上的反射次数。NDM2仅引入G-T效应产生较小的群延迟色散以补偿腔内自相位调制带来的部分啁啾。选用离子束溅射法制备了这两种负色散镜。用分光光度计测试了它们的透射率。结果表明,所制备的负色散镜的性能与设计性能非常接近。使用这两种负色散镜进行掺钛蓝宝石激光谐振腔内色散补偿实现了飞秒脉冲锁模,获得了15 fs的超短脉冲。     

电流卡钳传输阻抗的线性补偿

为了扩展电流卡钳的频率测试范围,根据其等效电路模型,分析并测试了传输阻抗特性,发现了传输阻抗在频率范围内的非线性现象,进而提出了基于放大器的线性补偿方法.通过测试结果表明,在1-50kHz的被测信号情况下,匹配了放大器的电流探头的传输阻抗的波动范围≤±1dB.因而,利用这一补偿方法,可以给单片机信号采集转换成被测电流值带来方便.     

Nb4Si含量对激光熔覆Ti-Fe合金涂层组织和性能的影响

采用激光熔覆技术,在TA15钛合金表面制备了具有不同Nb4Si添加量的Ti-Fe合金涂层。采用X射线衍射仪(XRD)、扫描电镜(SEM)、显微硬度计、纳米压痕仪和摩擦磨损试验机,系统研究了Nb4Si含量对合金涂层组织和性能的影响规律。研究结果表明,不同Nb4Si含量的Ti-Fe合金涂层皆主要是由β-TiNb树枝初晶和β-TiNb+TiFe共晶组织所构成。但有所不同的是,随着Nb4Si添加量的增加,涂层中共晶组织的数量呈现出先增后减的变化趋势,即在Nb4Si添加量为2.0%(粒子数分数,下同)时,共晶组织的数量为最多,且在Nb4Si的添加量超过0.5%时,涂层中开始有少量的β-(TiNb)5Si3相形成。由于受共晶组织增强作用的影响,在Nb4Si添加量为2.0%时,合金涂层的硬度、减磨性和耐磨性能为最高,而弹性模量为最低。