Effects of CO2 laser pretreatment conditions on adhesion properties of Cu/Ti films and polyimide substrates

Journal of Materials Science: Materials in Electronics - Polyimide is widely used as an insulating substrate for flexible printed circuit boards. However, the metallic thin films deposited on...     

无机掺杂改性聚酰亚胺薄膜的制备及表征

采用聚酰亚胺为树脂基体,甲基三乙氧基硅烷、异丙醇铝和钛酸四丁酯为无机前驱体,在N,N-二甲基乙酰胺溶液中进行溶胶-凝胶反应,制备聚酰亚胺／SiO2／Al2O3和聚酰亚胺／SiO2／TiO2两种无机掺杂聚酰亚胺薄膜,采用红外光谱仪、热重分析仪、扫描电镜等测试方法对薄膜的化学结构和表面形貌及其热稳定性进行了表征分析．结果表明：在一定的无机组分含量范围内,无机相均匀的分散在有机基体中,但两种杂化薄膜的分散形态及粒径尺寸不同,热性能均较未掺杂的聚酰亚胺薄膜有所提高。     

聚酰亚胺的侧链功能化

侧链功能化的聚酰亚胺是一类特殊的高性能聚合物,可用来制备非线性光学材料,绝缘薄膜,耐高温气液分离膜,射线屏蔽膜,柔性印刷电路板基膜和宇来得及航材料等,用于航天航空。国防军工,电子,电机电器,核动力学各个工业领域。本文就近１０年来国内外对聚酰亚胺侧链功能化的研究现状和应用前景进行了综述。     

聚酰亚胺/LTNO复合膜介电性能及其影响因素

采用溶胶-凝胶法合成出Li和Ti改性的氧化镍(LTNO)粒子,并通过前体溶液共混法首先制备聚酰胺酸/LTNO前体膜,再经亚胺化得到高介电常数聚酰亚胺/LTNO复合膜。研究发现,复合膜的介电性能可以通过调节LTNO的含量以及Li和Ti在LTNO中的比例来进行调控。选用按Li、Ni和Ti的摩尔百分比为0.30∶0.68∶0.02制备的LTNO粒子做填料,当其体积分数为0.4时,复合膜在100 Hz电场中的介电常数可以达到570。     

A novel technique for fabrication of metallic structures on polyimide by selective electroless copper plating using ion implantation

The successful use of palladium ion implantation into polyimide to seed an electroless plated film of copper on the polyimide surface is reported. Polyimide (Hitachi PIX 3400) was implanted with palladium ions to doses of 1.5 × 10¹⁵ − 1.2 × 10¹⁷ ions cm⁻² using a MEVVA ion implanter. The implanted ions acted as sites for nucleation of copper film. A copper film was then deposited on implanted polyimide using a commercial electroless plating solution. The ion energy was kept low enough to facilitate a low critical ‘seed’ threshold dose that was measured to be 3.6× 10¹⁶ Pd ions cm⁻². Test patterns were made using polyimide to study the adaptability of this technique to form thick structures. Plated films were studied with optical microscopy, Rutherford Backscattering Spectrometry (RBS) and Profilometry. The adhesion of films was qualitatively assessed by a ‘scotch tape test’. The film growth (thickness) was observed to be linear with plating time. A higher implantation dose led to greater plating rates. The adhesion was found to improve with increasing dose.     

Properties of polyimide/Al2O3 and Si3N4 deposited thin films

Polyimide (PI) nanocomposites with different proportions of Al₂O₃ were prepared via two-step reaction. Silicon nitride (Si₃N₄) was deposited on PI composite films by a RF magnetron sputtering system and used as a gas barrier to investigate the water vapor transmission rate (WVTR). The thermal stability and mechanical properties of a pure PI film can be improved obviously by adding adequate content of Al₂O₃. At lower sputtering pressure (4 mTorr), the PI/Al₂O₃ hybrid film deposited with Si₃N₄ barrier film exhibits denser structure and lower root mean square (RMS) surface roughness (0.494 nm) as well as performs better in preventing the transmission of water vapor. The lowest WVTR value was obtained from the sample, 4 wt.%Al₂O₃-PI hybrid film deposited with Si₃N₄ barrier film with the thickness of 100 nm, before and after bending test. The interface bonding, Al-N and Al-O-Si, was confirmed with the XPS composition-depth profile.     

Optical properties of organo-soluble polyimide thin films and their applications in liquid crystal displays

Three organo-soluble polyimide powders have been synthesized. Their imidization was verified by Fourier transform infrared (FTIR) and thermal gravimetric analysis (TGA) techniques. The amorphous morphology of their thin films were confirmed by X-ray diffraction. Polyimide thin films were prepared by solution casting or spin coating. UV–visible transmission spectra of thin films revealed that they are almost transparent in the range of visible light. With in-plane orientation, revealed by FTIR spectra, negative birefringence (Δn) of thin films were observed, and refractive indices of the thin films along the film plane (n_TE) and normal to the plane (n_TM) were measured by a prism coupler. Because of negative birefringence of the thin films, they can be substituted for the compensation films for twisted nematic liquid crystal displays (TN-LCDs) to extend their viewing angles. In this paper, a 90°C TN-LCD and 120°C TN-LCD were taken as examples to show the compensation effect of thin films of a qualified polyimide.     

低热膨胀系数纳米碳化硅/聚酰亚胺复合薄膜的制备与性能

以原位分散聚合法制备出纳米碳化硅/聚酰亚胺(n-SiC/PI)复合薄膜, 采用SEM、热机械分析仪(TMA)、阻抗分析仪和热重分析(TG)研究了所制备薄膜的表面形貌、热膨胀、介电性能及热稳定性。结果表明: SiC粒子均匀分散在PI基体中, 复合薄膜的热膨胀系数(CTE)随着SiC含量的增加逐渐减小, SiC质量分数为15%时, CTE降低了11%, 且复合膜的热膨胀系数实验值比较接近于Kerner公式的计算值。复合膜的介电常数和介电损耗随着填料含量的变化而变化, 但始终维持在较低的范围内, 并在相当大的频率范围内保持稳定。      

类金刚石薄膜中杂质Fe对其力学性能的影响

描述了利用射频等离子体溅射法采用不同阴极在衬底Ｓｉ片上形成类金刚石薄膜的杂质含量及杂质对厚度和硬度的影响分析与结果,比较了ＤＬＣ膜的力学性能在有无金属杂质情况下的异同,分析和计算了其硬度与硬度与制备参数间的关系,得出利用石墨作电极能制备出质量较好的ＤＬＣ膜,初步探讨在Ｓｉ衬底上沉积高硬度和强附着度类金刚石薄膜的有关工艺条件,并在理论上对这一结果进行了解释。     

离子束技术沉积羟基磷灰石薄膜的结构及溶解性能

分别采用离子束溅射和离子束增强沉积技术,以烧结羟基磷灰石（HA）陶瓷为靶材,在纯钛金属基片表面沉积HA薄膜．X光电子能谱分析表明：薄膜中Ca、P、O元素的化学态与所用HA陶瓷靶材相接近;相比HA靶材,薄膜表面存在CO₃^2-．X射线衍射分析表明：沉积薄膜均为非晶态结构,经650℃退火处理转变为结晶磷灰石．在模拟体液中的溶解实验揭示：薄膜仅与溶液中Ca、P和O存在离子交换;薄膜易降解,浸泡10天,样品经历了降解、再沉积过程;相比离子束溅射沉积膜,离子束增强沉积膜具有加速沉积Ca、P的能力．     

砷化镓衬底CVD金刚石薄膜辐射探测器的研究

在砷化镓（GaAs）衬底上采用微波等离子体化学气相沉积法（MPCVD）制备了金刚石薄膜,并对制备的薄膜进行抛光、表面氧化、退火等处理以提高薄膜质量,再用磁控溅射法在薄膜表面沉积金（Au）铝（Al）电极,制备了简易的CVD金刚石薄膜辐射探测器。采用扫描电子显微镜（SEM）和拉曼光谱（Raman）技术对制得的金刚石薄膜质量进行了分析研究。结果表明,薄膜为[100]晶面取向,表面平整,杂质含量低。采用5.9keV55FeX射线对所制备的探测器进行辐射实验,测出其光电流和暗电流特性,从而对辐射探测器性能进行了表征。     

Structural investigation of silicon films chemically vapour deposited onto amorphous SiO2 substrates

The influence of substrate temperature and the silane-to-nitrogen ratio on the structure of silicon films 0.5–0.6 μm thick deposited onto amorphous SiO₂ substrates was investigated by X-ray diffraction. The investigations were carried out for silicon films deposited at various temperatures in the range 500–750 °C and with various silane-to-nitrogen ratios in the range 3.04 × 10^-4-2.84 × 10^-3 by volume. The silicon films deposited at 500 °C were amorphous while the films deposited at 550 °C were randomly oriented polycrystalline. The films deposited in the temperature range 600–700 °C were polycrystalline with a preferred orientation that changed from 〈110〉 through 〈100〉 to 〈111〉. The structure of the films deposited at 750 °C was randomly oriented polycrystalline. Investigations of the influence of the silane-to-nitrogen ratio on the silicon film structure revealed that the structure of films deposited at a substrate temperature of 500 °C was independent of the silane-to-nitrogen ratio. The structure of the films deposited at 600 °C depended on the silane-to-nitrogen ratio and changed from polycrystalline with a 〈110〉 preferred orientation to randomly oriented polycrystalline when the ratio was increased. The structure of films deposited at 700 °C also depended on the silane-to-nitrogen ratio and changed from randomly oriented polycrystalline to polycrystalline with double preferred orientation (〈100〉 and 〈111〉) when the ratio was increased.     

Al2O3基陶瓷及玻璃基底制备Ta-N薄膜微结构与电学特性的比较研究

在N2、Ar气氛中,采用反应直流磁控溅射法在Al2O3基陶瓷及玻璃基底上制备了Ta-N薄膜,并对各样品的形貌结构、化学组分及电学特性进行了比较分析研究。结果表明,沉积于Al2O3陶瓷及玻璃基底的Ta-N薄膜分别呈团簇状生长与层状紧密堆积生长;Al2O3陶瓷基底沉积的Ta-N为单相薄膜,而玻璃基底上的Ta-N薄膜,随N2、Ar流量比增加,呈单相向多相共存转变;薄膜表面形貌和微结构与基底材料的原始形貌和微结构紧密相关,这说明基底材料对薄膜的形成有重要的影响;N2、Ar流量比相同时,玻璃基底上沉积的Ta-N薄膜电性能优于Al2O3基陶瓷基底上沉积的Ta-N薄膜。     

基底温度对直流溅射Nb掺杂TiO2薄膜性能的影响

采用陶瓷靶直流磁控溅射,以玻璃为基底制备2.5wt%Nb掺杂TiO2薄膜,控制薄膜厚度在300~350 nm,研究了不同基底温度下所制得薄膜的结构、形貌和光学特性.XRD分析表明,基底温度为150℃、250℃和350℃时,薄膜分别为非晶态、锐钛矿(101)和金红石相(110)结构.基底温度250℃时,锐钛矿相薄膜的晶粒尺寸最大,约为32 nm.薄膜表面形貌的SEM分析显示,薄膜粗糙度和致密度随基底温度升高得到改善.薄膜的平均可见光透过率在基底温度为250℃以内约为70%,随基底温度升高至350℃,平均透过率下降为59%,金红石相的存在不利于可见光透过.Nb掺杂TiO2薄膜的光学带宽在3.68~3.78 eV之间变化.基底温度为250℃时,锐钛矿相薄膜的禁带宽度最大,为3.78 eV.     

Improvement in salt-water durability of Ag thin films deposited by magnetron sputtering using argon and nitrogen mixed gas

Ag thin films were deposited by magnetron sputtering in a mixture of argon and nitrogen. The salt-water durability and reflectance of Ag thin films were investigated as a function of nitrogen gas flow ratio during sputter deposition. The reflectance of as-deposited Ag thin films decreased with increasing nitrogen gas flow ratio; however, the difference in visible-light reflectance between the Ag thin films deposited with and without nitrogen was less than 1%. The reflectance of Ag thin films that were deposited using pure argon significantly decreased after the films were soaked in salt water. In contrast, the salt-water durability of Ag thin films was improved when the nitrogen gas flow ratio was increased. X-ray diffraction and atomic force microscopy analyses revealed that the Ag thin films deposited in sufficient nitrogen exhibited smooth surfaces and small crystallite sizes. Hence, the agglomeration of Ag thin films was suppressed; as a consequence, the reflectance of Ag thin films deposited in nitrogen did not decrease to the same extent, despite being soaked in salt water.     

钠钙玻璃上Mg2Si薄膜的制备及其电学性质

采用磁控溅射技术和退火工艺在钠钙玻璃衬底上制备了Mg_2Si半导体薄膜,研究了Mg膜厚度对Mg_2Si薄膜结构及其电学性质的影响。在钠钙玻璃上分别溅射两组相同厚度(175nm)的P-Si和N-Si膜,然后在其上溅射不同厚度Mg膜(240nm、256nm、272nm、288nm、304nm),低真空退火4h制备一系列Mg_2Si半导体薄膜。通过X射线衍射仪(XRD)、扫描电子显微镜(SEM)、霍尔效应测试仪对Mg_2Si薄膜的晶体结构、表面形貌、电学性质进行表征与分析。结果表明:采用磁控溅射技术在钠钙玻璃衬底上成功制备出以Mg_2Si(220)为主的Mg_2Si薄膜。随着沉积Mg膜厚度的增加,Mg_2Si衍射峰逐渐增强,薄膜表面更连续,电阻率逐渐减小,霍尔迁移率逐渐降低,载流子浓度逐渐增加。此外,Si膜导电类型和Mg膜厚度共同影响Mg_2Si薄膜的导电类型。溅射N-Si膜时,Mg_2Si薄膜的导电类型随着Mg膜厚度的增加由P型转化为N型;溅射P-Si膜时,Mg_2Si薄膜的导电类型为P型。可以控制制备的Mg_2Si半导体薄膜的导电类型,这对Mg_2Si薄膜的器件开发有着重要的指导意义。     

Superhydrophobic polytetrafluoroethylene thin films with hierarchical roughness deposited using a single step vapor phase technique

Superhydrophobic polytetrafluoroethylene films with hierarchical surface roughness were deposited using pulse electron deposition technique. We were able to modulate roughness of the deposited films by controlling the beam energy and hence the electron penetration depth. The films deposited at higher beam energy showed contact angle as high as 166°. The scanning electron and atomic force microscope studies revealed clustered growth and two level sub-micron asperities on films deposited at higher energies. Such dual-scale hierarchical roughness and heterogeneities at the water-surface interface was attributed to the observed contact angle and thus its superhydrophobic nature.     

A study of nano-mechanical properties and nano-scratch behavior of boron carbonitride films

Boron carbonitride (BCN) films were deposited by d.c. unbalanced magnetron sputter deposition where a substrate bias ranging from -50 V to -300 V was applied to the sample. X-ray photoelectron spectroscopy and Fourier transform infrared spectroscopy were used to confirm the composition and bonding structure of the BCN films. Surface morphology and roughness were analyzed by atomic force microscopy. The nano-mechanical properties and nano-scratch behavior of the prepared films were determined by a nano-indentation system equipped with continuous stiffness measurement and lateral-force measurement attachments. The results indicate that there is little change in the content of B, C, and N. The films deposited are compounds with hybridized B-C-N bonds and the disordered degree of the structure increases with increasing the substrate bias. The substrate biasing can enhance the nanohardness, elastic modulus, nano-scratch resistance, and cohesion strength of the deposited films. During the nano-scratch test, plastic deformation and ploughing wear appears for the BCN films deposited at lower bias. Elastic deformation becomes the dominant deformation mechanism for the films deposited at higher bias. The coefficient of friction between the deposited BCN films and the diamond tip depends on the loading critical load. The increasing of the substrate bias leads to the improvement of the critical load and the elastic deformation proportion.     

Microstructures of ITO films deposited by d.c. magnetron sputtering with H2O introduction

ITO films were deposited by d.c. magnetron sputtering with/without H₂O introduction. The structural and optoelectrical properties of the films were analyzed in detail. The films deposited with H₂O introduction exhibited an entirely amorphous structure, whereas the as-deposited films deposited without H₂O introduction exhibited a polycrystalline In₂O₃ structure. The amorphous ITO films deposited under the high H₂O partial pressure were confirmed to contain a much higher concentration of hydrogen inside the films by secondary ion mass spectroscopy, which remained after post-annealing at 350 °C. The crystallization temperature of the films subjected to post-annealing was increased to higher than 220 °C. These stable amorphous ITO films had a wet-etching rate in oxalic acid solution two orders of magnitude higher than that of the films deposited without H₂O introduction.     

Atomic force microscopy and X-ray photoelectron spectroscopy evaluation of adhesion and nanostructure of thin Cr films

Chromium (Cr) thin films were deposited on float glass using electron beam (e-beam) physical vapor deposition and radio frequency (RF) magnetron sputtering techniques. Surface morphology of these Cr films was studied using atomic force microscopy (AFM). The e-beam deposited Cr films consisted of isolated surface mounds while in RF sputtered samples, these mounds combined to form larger islands. Lower surface adhesive properties were observed for e-beam deposited films, as determined from AFM force-distance curves, presumably due to the nanostructural differences. Similar amounts of adsorbed atmospheric carbonaceous contaminants and water vapor were detected on samples deposited using both methods with e-beam deposited samples having additional carbide species, as determined by X-ray photoelectron spectroscopy data. The dominant crystallographic plane in both e-beam deposited and RF sputtered Cr thin films was (110) of body-centered cubic Cr metal structure as determined from X-ray diffraction data. Weak (211) reflection was also observed in RF sputtered samples and was attributed to a different thin Cr film condensation and growth mechanism which resulted in nanostructural differences between films deposited using two different methods.