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

This paper discusses a new method of evaluating thin film adhesion both qualitatively and quantitatively via a combination of peeling and image processing techniques. The adhesion of thin film on the entire substrate can be quickly evaluated and quantified to a continuous response variable which is superior to a discrete response variable as described in the ASTM D3359-78 publication. Feasibility of this technique has been demonstrated through a gauge capability study which resulted in 2.7% P/T (precision to tolerance) ratio at six sigma standard deviation for a tolerance of 100. Experimental results using the proposed method to evaluate the process/property relationship of aluminum films as deposited onto various dielectric substrates such as polyimide, silicon dioxide, and silicon nitride have been obtained and have been shown to agree with conventional stud pull test results. The estimated cycle time to evaluate thin film adhesion is five minutes per 4-inch size wafer once the sample is prepared. This short process cycle time and proven reliability show that there is merit in implementing this technique both in the laboratory for process development and in the factory for statistical process control of products.     

Relative Adhesion Measurement for Thin Film Microelectronics Structures

There is a difference between technologically-important adhesion or practical adhesion, and fundamental or basic adhesion. What is important in the understanding of fundamental adhesion may be of insignificant interest to technology. A manufacturer is interested in how to improve the reliability of the structure being built should an interface problem exist, rather than knowing the precise value of the fundamental adhesion. It is not possible to measure fundamental adhesion for technologically-important structures due to the inability to account for all energy dissipating processes during the test. Adhesion measurements are plagued with the mode of interface loading issue: the resemblance of test interface loading to that of the actual manufactured part. What technology needs is a simple adhesion test method that is practical for product development, giving reliable information about the interface integrity. The present paper compares the value of two adhesion tests for microelectronics applications and emphasizes the importance of locus of failure analyses. A realignment of structure reliability modeling is suggested by the usage of effective fundamental adhesion instead of the standard undeterminable fundamental adhesion.     

Relative Adhesion Measurement for Thin Film Microelectronics Structures

There is a difference between technologically-important adhesion or practical adhesion, and fundamental or basic adhesion. What is important in the understanding of fundamental adhesion may be of insignificant interest to technology. A manufacturer is interested in how to improve the reliability of the structure being built should an interface problem exist, rather than knowing the precise value of the fundamental adhesion. It is not possible to measure fundamental adhesion for technologically-important structures due to the inability to account for all energy dissipating processes during the test. Adhesion measurements are plagued with the mode of interface loading issue: the resemblance of test interface loading to that of the actual manufactured part. What technology needs is a simple adhesion test method that is practical for product development, giving reliable information about the interface integrity. The present paper compares the value of two adhesion tests for microelectronics applications and emphasizes the importance of locus of failure analyses. A realignment of structure reliability modeling is suggested by the usage of effective fundamental adhesion instead of the standard undeterminable fundamental adhesion.     

Application of the Island Blister Test for Thin Film Adhesion Measurement

The island blister test has recently been proposed as an adhesion test which allows the peel of thin, well-adhered films without exceeding the tensile strength of the film. The island blister test site is a modification of the standard blister test site, consisting of a suspended membrane of film with an “island” of substrate at the film center. The membrane support and island are secured to a rigid plate and the film is pressurized, peeling the film inward off the island. A model for this inward or “annular” peel indicates that even for systems of good adhesion, peel can be initiated at low enough pressures to prevent film failure by making the center island sufficiently small relative to the size of the film.

We have fabricated island blister test sites using micromachining techniques and have used them to measure the debond energy of polymer films on various substrates. The peel data obtained from these island sites match well to the behavior predicted by a simple fracture mechanics analysis. This paper reports the fabrication of the island test sites, the experimental verification of the test, and the results of application of the test to polyimide films on metallic and polymeric substrates.     

Application of the Island Blister Test for Thin Film Adhesion Measurement

The island blister test has recently been proposed as an adhesion test which allows the peel of thin, well-adhered films without exceeding the tensile strength of the film. The island blister test site is a modification of the standard blister test site, consisting of a suspended membrane of film with an “island” of substrate at the film center. The membrane support and island are secured to a rigid plate and the film is pressurized, peeling the film inward off the island. A model for this inward or “annular” peel indicates that even for systems of good adhesion, peel can be initiated at low enough pressures to prevent film failure by making the center island sufficiently small relative to the size of the film.

We have fabricated island blister test sites using micromachining techniques and have used them to measure the debond energy of polymer films on various substrates. The peel data obtained from these island sites match well to the behavior predicted by a simple fracture mechanics analysis. This paper reports the fabrication of the island test sites, the experimental verification of the test, and the results of application of the test to polyimide films on metallic and polymeric substrates.     

漆膜附着力及其测试方法

本详细介绍了漆膜附着力测试的3项国家标难，并对各方法进行了比较；简要介绍了2项IS0标准和2项ASTM标准。     

Sol—Gel法制备WO3薄膜的研究

采用络合物ｓｏｌ－ｇｅｌ浸渍提拉法以过钨酸酯的乙醇溶液为先驱制备了ＷＯ３薄膜,研究了有机添加剂草酸对膜结构的影响,并对所得薄膜进行了红外光谱、可见光谱和ＳＥＭ等测试和观察。结果表明该法能制得质量好的ＷＯ３薄膜,在溶液中加入草酸可以有效地控制裂纹扩展。因此在优化工艺条件后将能得到无裂纹的ＷＯ３薄膜。     

Fracture Mechanics of aV-peel Adhesion Test - Transition from a Bending Plate to a Stretching Membrane

A linear elastic solution is proposed for a “V-peel” adhesion test for a thin film adhered to a rigid substrate. The mechanical responses of a stiff plate-like coating under pure bending, a semi-flexible film under mixed bending and stretching, and a flexible membrane-like film under pure stretching are discussed. For delamination to occur, the mechanical energy release rate is shown to be G = χ(Fw₀/2bl) with χ a numerical constant varying from 3/2 for a plate-like disc to 3/4 for a thin flexible membrane.     

The Contact Adhesion of Self-Adhesive Strain Gauges

Thin pieces of flexible polymers may be adhered to rigid substrates merely by pressing the two surfaces into intimate contact. The peel strength of the bond is poor, but the shear strength can be sufficiently high for strain gauge operation. This paper offers an explanation for the adhesion which can account quantitatively for the behaviour of various materials. Frictional phenomena, resulting from a normal force produced by the surface tension of a surface film, can explain why a gauge with a PVC body does not slip. With other polymers, other liquids or electrostatic effects may be of importance. Any surface “fluid” film of sufficiently high viscosity that viscous effects are important will behave as an integral part of the elastomer.     

纳米TiO2薄膜的制备、表征及杀菌性能

利用溶胶-凝胶法制备了TiO<,2>溶胶,以浸渍--提拉法制备瓷砖负载的纳米TiO<,2>薄膜,采用XRD和AFM技术对其进行了表征,通过自然落菌实验和人为接菌实验分别考察了纳米TiO<,2>薄膜的杀菌性能.研究表明:纳米TiO<,2>薄膜中生成的是锐钛矿相纳米二氧化钛,晶粒的粒径为18.98 nm,颗粒粒径比较均匀;...     

Evaluation of the Constrained Blister Test for Measuring Adhesion

The constrained blister test (CBT) was evaluated as a method for measuring adhesion using a model system, electrical tape bonded to polystyrene. Pressure is applied through a circular inlet hole in the substrate, causing the adhesive to “blister” up and peel radially away from the substrate. A glass constraint, placed some distance above the adhesive, limits deformation of the adhesive in the vertical direction and promotes radial peel. By operating at low spacer height (the distance of the constraint above the adhesive) and very low growth rates, the energy spent for deformation of the adhesive and viscoelastic dissipation is minimized. Blister radial growth was linear with time, and growth rate increased linearly with the second power of the energy input. An intrinsic, rate-independent adhesion energy was obtained by extrapolation to zero crack growth rate. The CBT was compared with two peel tests. The dependence of the growth rate on energy input was different, but the extrapolation to zero growth rate gave the same value of the intrinsic adhesion energy.     

Adhesion of polyvinyl alcohol cord,and fabric to special purpose rubbers in the presence of HRH dry-bonding agents

The adhesion of polyvinyl alcohol (PVOH) cord and fabric to different special purpose rubbers has been studied with a view to making use of the textile in various applications such as in gaskets, diaphragms, and other industrial molded goods. Adhesion was measured with both raw and chemically treated cords and fabrics, and in the presence of hydrated silica-resorcinol-hexamethylenetetramine (HRH) dry-bonding agents. The pull adhesion strength of the PVOH cable cord (untreated) to EPDM rubber and polyurethane rubber improved significantly on incorporating HRH dry-bonding agents. However, for chemically treated cords the bond strength improved for EPDM rubber but decreased marginally for polyurethane rubber. The peel adhesion strength of the PVOH fabric (both raw and chemically treated) improved slightly with the introduction of dry-bonding agents for all the rubbers studied except nitrile rubber. The physicomechanical properties and aging characteristics of the rubber vulcanizates in the presence of the dry-bonding agents are reported.     

绿色薄膜型前处理工艺

介绍了世界著名厂商的绿色前处理工艺与超高泳透力阴极电泳(CED)涂料的应用成果。     

电子束蒸发制备HfO2薄膜的性能研究

用电子束蒸发方法沉积HfO2薄膜,用X射线衍射和透射光谱测定HfO2薄膜的结构特征和光学性能,并测定薄膜的弱吸收和损伤阈值.结果表明:HfO2薄膜在沉积温度为350℃时,达到了较好的结晶程度.在可见光和近红外光区具有很高的透过率;HfO2薄膜的损伤阈值比较高,达到10.5 J/cm2.     

传统磷化转锆系薄膜前处理的前期工艺试验

锆系薄膜或硅烷薄膜前处理在国内主机厂已有部分应用,但多数为新建薄膜线,直接按薄膜工艺规划并使用,而对老线由传统磷化转为锆系薄膜前处理的研究甚少。为研究工厂传统磷化转薄膜前处理的可行性,降低转换带来的风险,本文设计了一系列实验,结合工厂现有电泳漆和车身板材,通过对泳透力、上电电压、停线性能、电泳入槽方式、打磨印遮盖等的研究,验证薄膜前处理与电泳漆以及车身板材的配套性能。通过实验结果评估薄膜前处理的使用对工艺参数、外观质量等方面的影响,为进行传统磷化转薄膜前处理工作打好基础。结果表明:薄膜前处理工艺对停线时间较为敏感,但其他工艺参数波动对其影响不大,并且在泳透力及电泳成膜的表现上也优于传统磷化。     

二氧化钛薄膜的制备及性能研究

二氧化钛具有无毒、光催化性能强,热稳定和化学结构稳定,耐腐蚀性能良好等特点,可作为半导体催化材料和耐腐蚀材料。二氧化钛薄膜可以采用物理的方法和化学的方法制备,薄膜态材料在未来将有着潜在的应用。本文结合近年来二氧化钛薄膜的研究进展,介绍了二氧化钛薄膜的制备方法和应用领域,并对未来二氧化钛薄膜的研究进行了展望。     

A New Method of Fabricating NASICON Thin Film

Nasicon thin films of 15 μm thick on YSZ sub-strates were prepared by means of solid state reaction at 1230℃ for 10 hours,Stuctural characteriza-tion of the films were performed by XRD ,SEM and EDX,A new tyype of CO2 gas sensor with Nasicon thin film as solid electrolyte was developed.     

TiO2光催化薄膜的制备及其性能

在稀硫酸溶液中的阳极氧化钛箔,采用混合增长模型技术控制氧化膜的生长,制备了TiO2光催化薄膜,TiO2薄膜通过苯酚的光催化降解实验检验,具有较高的催化活性及很好的催化稳定性,实验结果表明：阳极氧化法固定TiO2薄膜切实地,不仅解决了TiO2微粒光催化过程催化剂微料与水难分离的问题,而且阳极氧化制膜所需时间短（几秒到几分）、工艺简单,十分有利于工业化制备。     

Testing of adhesion of thin films to substrates

The results of the measurement of the adhesion strength of thin films or coatings to substrates are often influenced by system parameters that may be influenced by preparation of the specimen for testing or by deposition of the film itself. In this paper, the scratch, pull, and peel tests are analyzed in terms of criteria for film/coating removal and for the effects of system parameters such as film hardness and ductility, film thickness, substrate hardness, etc.     

干膜粘贴促进剂ST-10+的研制

本文介绍了一种能提高干膜与线路板铜基粘合力的新型铜面处理剂ST-10 。这种处理剂以双氧水/硫酸为基础,配以特殊的微观结构调整剂,能在铜面形成均匀粗化的微表面,提高了铜面的表面积,从而促进了干膜与铜面的粘合,提高了超细线路产品的制作良品率。