PS/金属核壳结构复合微球的制备及其在各向异性导电胶膜上的应用
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摘要
各向异性导电胶膜(Anisotropic Conductive Film, ACF)是一种绿色环保的新型电子封装材料。与传统的锡铅焊料相比,具有封装工艺简单、可进行窄间距互连、低封装温度、环保等优点。ACF是由微米级导电粒子与可控快速固化的树脂胶粘剂共混成膜后得到的复合材料,因其在X、Y方向绝缘,只在Z方向导电,从而呈现各向异性。导电粒子是ACF材料的核心部分,用来实现互连凸点间的电导通；树脂粘合剂除了具有粘接、耐热及绝缘功能外,其主要作用是固定互连凸点的相对位置,并提供压力以维持凸点与导电粒子间的接触面积。
聚合物／金属导电复合微球是以微米级单分散聚合物微球为核,以金属为壳的核壳式复合材料。它可以兼具聚合物微球的真圆度、粒径均一、弹性、轻质等性质和金属的导电性能,因而成为目前ACF导电粒子的主流结构。本文将分别采用分散聚合法和化学镀法制备微米级单分散聚苯乙烯(PS)微球和PS/金属导电复合微球,分析了材料的形成机理及形貌等方面的影响因素,并对导电复合微球的导电性能进行了表征。以改性环氧树脂(EP)为基体,以咪唑类或阳离子型化合物为固化剂,开发新型EP基ACF胶粘剂体系,使其可在中高温条件下快速固化,并具有稳定的室温储存性及优良的粘结强度,以解决目前商用ACF产品在运输、储存等方面存在的问题。
采用分散聚合法制备了尺寸可控的微米级单分散PS微球。研究了加料方式、聚合时间、单体浓度、分散剂浓度、引发剂浓度及种类、分散介质以及聚合温度等因素对PS微球形貌及单分散性的影响。实验结果表明,聚合反应的成核期最为敏感,也是制备单分散PS微球的关键。一步加料法制备的PS微球的形貌及单分散性更好；单体浓度、溶剂极性及聚合温度对PS微球粒径的影响较为明显,分散剂浓度及引发剂浓度则次之,但对PS微球的单分散性影响较大。通过改变聚合条件,可以制备直径为1-3μm的单分散PS微球。
镍(Ni)具有优异的导电性、耐腐蚀性、成本低等特点,以其作为导电壳层,采用化学镀法在单分散PS微球表面施镀制备了PS/Ni导电复合微球。讨论了PS微球活性中心的修饰、化学镀实施方式、镀液中还原剂及络合剂浓度、PS微球装载量等因素对复合微球的分散性、镀层包覆情况及导电性能的影响。另外,在化学镀Ni过程中,微量的稀土元素镧(La)的引入有效地提高了PS/Ni复合微球的镀层致密程度,同时降低了复合微球的密度。当镀液中La203的浓度分别为0mM和0.15mM时,PS微球表面的Ni基合金颗粒的平均尺寸由300nm减小为70nm,复合微球的密度则由4.068g cm-3降低至1.515g cm-3,使其更符合ACF导电粒子的要求。
铜(Cu)具有优异的导电、导热、低成本、低电子迁移率等优点,采用化学镀法对单分散的PS微球表面进行金属化,制备PS/Cu导电复合微球。采用线性扫描伏安法测试化学镀过程中的局部阴阳极极化曲线,以协助分析镀液pH值、还原剂浓度、络合体系等因素对PS/Cu复合微球形貌、镀层包覆情况及分散性的影响。改变PS微球的装载量可以有效地调节复合微球的密度、壳层厚度及导电性能。另外,在镀液中加入稳定剂2,2-联吡啶后,PS微球表面出现了数颗立方体状的Cu颗粒；而加入La203后,则有效地改善了复合微球的表面形貌。
银(Ag)具有很好的导电性、柔韧性及延展性,采用改进的化学镀法在PS微球表面进行银的包覆。在PS微球的镀前处理时,以10nm左右的铂(Pt)溶胶代替PdCl2完成活化,使PS微球表面的活性中心尺寸由70nm减小至10nm,有利于均匀镀层的形成。分析了化学镀Ag过程中温度、时间、PS微球装载量等因素对复合微球形貌、镀层厚度、分散性及导电性的影响。另外,在镀液中添加PVP可有效地改善复合微球镀层的微结构,使Ag镀层更加均匀致密。
将双酚A型环氧树脂(DGEBA)与二聚酸改性DGEBA复合,作为胶粘剂的基体,以2-甲基咪唑(2MZ)或阳离子型六氟锑酸盐(PPH)为固化剂,制备了新型的用于ACF的胶粘剂。分别研究了2MZ/EP和PPH/EP体系的固化行为、室温储存性及固化物的热稳定性。实验结果显示,PPH/EP体系在25-30℃下可放置60天左右,但其固化物的T。仅为100℃。为了提高该体系固化物的热稳定性,将双酚A甲醛环氧树脂复合到胶粘剂基体中,制备了PPH/MEP胶粘剂。测试结果显示,该体系固化物的T。可提高到120℃,而且该体系具有更好的室温储存性能。
以粒径为3μm的PS/Ag复合微球作为导电粒子,以PPH/MEP体系作为树脂胶粘剂,制备了导电性能和粘接性能优异的ACF材料。根据电极间接触电阻理论分析,压力、导电粒子的尺寸、电极间导电粒子的数目等对连接件接触电阻都具有很大的影响。实验结果表明,提高导电微球含量、绑定压力、绑定温度及延长绑定时间对ACF的导电性能都具有积极作用,但ACF的粘接性能主要由树脂胶粘剂的固化程度所决定。在进行间距为500μm的FOG连接时,ACF的导电粒子临界含量为35wt.%左右,当导电粒子含量为20wt.%左右时,ACF可同时具有较好的导电性能和粘接性能。ACF进行FOG互连时的最佳的绑定工艺参数为：绑定压力0.3MPa,绑定温度170℃,绑定时间15s。
As the requirements for interconnection and joining materials in microelectronics packaging applications have moved toward ultra-fine-pitch bonding and environmental friendliness, anisotropic conductive films (ACFs) have attracted considerable attention as an alternative to tin/lead (Sn/Pb) solders. ACFs not only allow products to be thinner, smaller and lighter, but also offer good electrical performance and stability. ACFs mainly consist of polymeric binder matrices and micrometre-scale conductive fillers. Only with applied heat and pressure during bonding process, the electric connections will be established in the Z-direction by a relatively low loading of conductive fillers. The cured polymer adhesive holds the two components together and provides pressure to maintain the interconnection area between bumps/pads and conductive fillers.
Polymer/metal conductive microspheres are a kind of composite materials with a core/shell structure. Owing to the combination of round-shape, monodispersion, elasticity and lightweight of polymer microspheres and the excellent conductivity of metal, polymer/metal composite microspheres have been widely added into insulating adhesive matrix to prepare ACFs. Monodispersed polystyrene (PS)/metal composite microspheres were prepared by dispersion polymerization of styrene followed by electroless plating. The influences on the formation mechanism and morphology of composite microspheres were investigated, and their electrical properties were also characterized. To improve the storage stability of adhesives at ambient, modified epoxy (EP) and cationic hexafluoroantimonate were used as matrix and latent curing agent, respectively, to develop a new epoxy based adhesive. Such adhesives displayed an excellent storage stability at ambient, good adhesive strength and fast curing speed at relatively low temperature.
Monodispersed PS microspheres were prepared by dispersion polymerization with controlled diameters. The effects of polymerization time, monomer concentration, dispersing agent concentration, initiator concentration, initiator type, dispersion medium and polymerization temperature on the monodispersion and morphology of PS microspheres were investigated. The results revealed that the sensitive nucleation period played the most important role on the preparation of monodispersed PS microspheres. Better monodispersion and morphology of PS microspheres can be obtained by one-step procedure. The influences of monomer concentration, dispersion medium and polymerization temperature on the diameters of PS were stronger than that of dispersing agent concentration and initiator concentration. However, they determined the monodispersion of PS to a large extent. In a word, monodispersed PS microspheres with diameters of1～3μm can be obtained by dispersion polymerization with controlled polymerization conditions.
Nickel (Ni) has good conductivity, corrosion resistance and low cost. PS/Ni conductive composite microspheres with Ni coating on PS microspheres were prepared by electroless plating technology. The effects of decoration with active centers on PS microspheres surface, the condition of electroless plating, reductant concentration, complexant concentration and the loading of PS on the dispersion, Ni coating state and the electrical properties of PS/Ni composites were discussed. Furthermore, to improve the surface roughness, subsidiary fracture of the plated layer and high density, lanthanum (La) was added into electroless Ni plating bath. With the La content ranging from0to50mg L-1, the average grain size of the Ni based alloy coating reduced from300nm to70nin, the average shell thickness of the composites reduced from240nm to95nm, and the density of the composites decreased gradually from4.068g cm-3to1.515g cm-3
Copper (Cu) has high electrical, thermal conductivity, moderate hardness, low cost and low electromigration. The formation of Cu shell on PS surface was obtained by electroless plating technology. The effects of pH of plating solution, reductant concentration, mode of feeding reductant and complexing system on morphology. Cu coating state and dispersion of PS/Cu composites were investigated with the assistant of linear sweep voltammetry (LSV) method. Tailoring of density, shell thickness and conductivity can be achieved by varying the loading of PS microspheres in plating bath. In addition, the existence of2,2-dipyridyl or La2O3as a stabilizer had a different influence on the deposition rate of Cu by electrochemical measurements, and thus led to a various morphology of PS/Cu composites. A more compact copper shell on PS surface can be obtained in the presence of La2O3
Silver (Ag) has excellent conductivity, flexibility and malleability'. A modified electroless silver-plating process was developed for the preparation of monodispersed PS/Ag composite microspheres. PS surfaces were decorated with colloidal platinum of approximately10nm in size, much smaller than that of clusters fabricated by a conventional activation method, which contains Sn and Pd species of70nm. The effects of temperature, time of plating and loading of PS in plating bath on morphology. Ag coating state, dispersion and conductivity of PS/Ag composites were investigated. The results showed that a dense, stable and uniform Ag nanoshell was formed on the surface of PS microspheres with the assistant of poly (vinylpyrrolidone).
A new epoxy based adhesive was prepared by using composite resin of diglycidylether of bisphenol A (DGEBA) and dimmer acid modified DGEBA as matrix and2-methylimidazole or N-phenethylpyrazinium hexafluoroantimonate (PPH) as curing agent. The curing behavior, storage stability at ambient of adhesive and thermostability of cured products were studied. The results showed that the pot life of PPH/EP adhesive exceeded to60days at25～30℃, but the glass transition temperature (Tg) of its cured product was only100℃. To improve the thermostability of cured products, bisphenol A novalac epoxy was added into the adhesive matrix to prepare PPH/MEP system. The results showed that Tg of cured PPH/MEP product increased to120℃, and PPH/MEP system maintained an excellent storage stability at ambient.
ACFs with good conductivity and peel strength were prepared, which electrically connect ITO glass and flex print circuit (FPC) with conducting patterns of500μm in pitch. PS/Ag composite microspheres with diameter of3μm and PPH/MEP system were used as conductive fillers and adhesive resin, respectively. According to the theoretical analysis, contact resistance can be strongly influenced by applied pressure, filler size and number of filler between electrodes. The experimental results showed that increasing the filler content, bonding pressure, temperature and time played positive role on the conductivity of ACF. However, the adhesive property of ACF largely depended on the curing degree of resin. The critical content of conductive fillers was35wt.%in the flex on glass (FOG) process using ACF. When the filler content was20wt.%, ACF possessed good conductivity and peel strength at the same time. The optimal bonding pressure, temperature and time for reliability of interconnection using ACF were0.3MPa,170℃and15s, respectively.
聚合物／金属导电复合微球是以微米级单分散聚合物微球为核,以金属为壳的核壳式复合材料。它可以兼具聚合物微球的真圆度、粒径均一、弹性、轻质等性质和金属的导电性能,因而成为目前ACF导电粒子的主流结构。本文将分别采用分散聚合法和化学镀法制备微米级单分散聚苯乙烯(PS)微球和PS/金属导电复合微球,分析了材料的形成机理及形貌等方面的影响因素,并对导电复合微球的导电性能进行了表征。以改性环氧树脂(EP)为基体,以咪唑类或阳离子型化合物为固化剂,开发新型EP基ACF胶粘剂体系,使其可在中高温条件下快速固化,并具有稳定的室温储存性及优良的粘结强度,以解决目前商用ACF产品在运输、储存等方面存在的问题。
采用分散聚合法制备了尺寸可控的微米级单分散PS微球。研究了加料方式、聚合时间、单体浓度、分散剂浓度、引发剂浓度及种类、分散介质以及聚合温度等因素对PS微球形貌及单分散性的影响。实验结果表明,聚合反应的成核期最为敏感,也是制备单分散PS微球的关键。一步加料法制备的PS微球的形貌及单分散性更好；单体浓度、溶剂极性及聚合温度对PS微球粒径的影响较为明显,分散剂浓度及引发剂浓度则次之,但对PS微球的单分散性影响较大。通过改变聚合条件,可以制备直径为1-3μm的单分散PS微球。
镍(Ni)具有优异的导电性、耐腐蚀性、成本低等特点,以其作为导电壳层,采用化学镀法在单分散PS微球表面施镀制备了PS/Ni导电复合微球。讨论了PS微球活性中心的修饰、化学镀实施方式、镀液中还原剂及络合剂浓度、PS微球装载量等因素对复合微球的分散性、镀层包覆情况及导电性能的影响。另外,在化学镀Ni过程中,微量的稀土元素镧(La)的引入有效地提高了PS/Ni复合微球的镀层致密程度,同时降低了复合微球的密度。当镀液中La203的浓度分别为0mM和0.15mM时,PS微球表面的Ni基合金颗粒的平均尺寸由300nm减小为70nm,复合微球的密度则由4.068g cm-3降低至1.515g cm-3,使其更符合ACF导电粒子的要求。
铜(Cu)具有优异的导电、导热、低成本、低电子迁移率等优点,采用化学镀法对单分散的PS微球表面进行金属化,制备PS/Cu导电复合微球。采用线性扫描伏安法测试化学镀过程中的局部阴阳极极化曲线,以协助分析镀液pH值、还原剂浓度、络合体系等因素对PS/Cu复合微球形貌、镀层包覆情况及分散性的影响。改变PS微球的装载量可以有效地调节复合微球的密度、壳层厚度及导电性能。另外,在镀液中加入稳定剂2,2-联吡啶后,PS微球表面出现了数颗立方体状的Cu颗粒；而加入La203后,则有效地改善了复合微球的表面形貌。
银(Ag)具有很好的导电性、柔韧性及延展性,采用改进的化学镀法在PS微球表面进行银的包覆。在PS微球的镀前处理时,以10nm左右的铂(Pt)溶胶代替PdCl2完成活化,使PS微球表面的活性中心尺寸由70nm减小至10nm,有利于均匀镀层的形成。分析了化学镀Ag过程中温度、时间、PS微球装载量等因素对复合微球形貌、镀层厚度、分散性及导电性的影响。另外,在镀液中添加PVP可有效地改善复合微球镀层的微结构,使Ag镀层更加均匀致密。
将双酚A型环氧树脂(DGEBA)与二聚酸改性DGEBA复合,作为胶粘剂的基体,以2-甲基咪唑(2MZ)或阳离子型六氟锑酸盐(PPH)为固化剂,制备了新型的用于ACF的胶粘剂。分别研究了2MZ/EP和PPH/EP体系的固化行为、室温储存性及固化物的热稳定性。实验结果显示,PPH/EP体系在25-30℃下可放置60天左右,但其固化物的T。仅为100℃。为了提高该体系固化物的热稳定性,将双酚A甲醛环氧树脂复合到胶粘剂基体中,制备了PPH/MEP胶粘剂。测试结果显示,该体系固化物的T。可提高到120℃,而且该体系具有更好的室温储存性能。
以粒径为3μm的PS/Ag复合微球作为导电粒子,以PPH/MEP体系作为树脂胶粘剂,制备了导电性能和粘接性能优异的ACF材料。根据电极间接触电阻理论分析,压力、导电粒子的尺寸、电极间导电粒子的数目等对连接件接触电阻都具有很大的影响。实验结果表明,提高导电微球含量、绑定压力、绑定温度及延长绑定时间对ACF的导电性能都具有积极作用,但ACF的粘接性能主要由树脂胶粘剂的固化程度所决定。在进行间距为500μm的FOG连接时,ACF的导电粒子临界含量为35wt.%左右,当导电粒子含量为20wt.%左右时,ACF可同时具有较好的导电性能和粘接性能。ACF进行FOG互连时的最佳的绑定工艺参数为：绑定压力0.3MPa,绑定温度170℃,绑定时间15s。
As the requirements for interconnection and joining materials in microelectronics packaging applications have moved toward ultra-fine-pitch bonding and environmental friendliness, anisotropic conductive films (ACFs) have attracted considerable attention as an alternative to tin/lead (Sn/Pb) solders. ACFs not only allow products to be thinner, smaller and lighter, but also offer good electrical performance and stability. ACFs mainly consist of polymeric binder matrices and micrometre-scale conductive fillers. Only with applied heat and pressure during bonding process, the electric connections will be established in the Z-direction by a relatively low loading of conductive fillers. The cured polymer adhesive holds the two components together and provides pressure to maintain the interconnection area between bumps/pads and conductive fillers.
Polymer/metal conductive microspheres are a kind of composite materials with a core/shell structure. Owing to the combination of round-shape, monodispersion, elasticity and lightweight of polymer microspheres and the excellent conductivity of metal, polymer/metal composite microspheres have been widely added into insulating adhesive matrix to prepare ACFs. Monodispersed polystyrene (PS)/metal composite microspheres were prepared by dispersion polymerization of styrene followed by electroless plating. The influences on the formation mechanism and morphology of composite microspheres were investigated, and their electrical properties were also characterized. To improve the storage stability of adhesives at ambient, modified epoxy (EP) and cationic hexafluoroantimonate were used as matrix and latent curing agent, respectively, to develop a new epoxy based adhesive. Such adhesives displayed an excellent storage stability at ambient, good adhesive strength and fast curing speed at relatively low temperature.
Monodispersed PS microspheres were prepared by dispersion polymerization with controlled diameters. The effects of polymerization time, monomer concentration, dispersing agent concentration, initiator concentration, initiator type, dispersion medium and polymerization temperature on the monodispersion and morphology of PS microspheres were investigated. The results revealed that the sensitive nucleation period played the most important role on the preparation of monodispersed PS microspheres. Better monodispersion and morphology of PS microspheres can be obtained by one-step procedure. The influences of monomer concentration, dispersion medium and polymerization temperature on the diameters of PS were stronger than that of dispersing agent concentration and initiator concentration. However, they determined the monodispersion of PS to a large extent. In a word, monodispersed PS microspheres with diameters of1～3μm can be obtained by dispersion polymerization with controlled polymerization conditions.
Nickel (Ni) has good conductivity, corrosion resistance and low cost. PS/Ni conductive composite microspheres with Ni coating on PS microspheres were prepared by electroless plating technology. The effects of decoration with active centers on PS microspheres surface, the condition of electroless plating, reductant concentration, complexant concentration and the loading of PS on the dispersion, Ni coating state and the electrical properties of PS/Ni composites were discussed. Furthermore, to improve the surface roughness, subsidiary fracture of the plated layer and high density, lanthanum (La) was added into electroless Ni plating bath. With the La content ranging from0to50mg L-1, the average grain size of the Ni based alloy coating reduced from300nm to70nin, the average shell thickness of the composites reduced from240nm to95nm, and the density of the composites decreased gradually from4.068g cm-3to1.515g cm-3
Copper (Cu) has high electrical, thermal conductivity, moderate hardness, low cost and low electromigration. The formation of Cu shell on PS surface was obtained by electroless plating technology. The effects of pH of plating solution, reductant concentration, mode of feeding reductant and complexing system on morphology. Cu coating state and dispersion of PS/Cu composites were investigated with the assistant of linear sweep voltammetry (LSV) method. Tailoring of density, shell thickness and conductivity can be achieved by varying the loading of PS microspheres in plating bath. In addition, the existence of2,2-dipyridyl or La2O3as a stabilizer had a different influence on the deposition rate of Cu by electrochemical measurements, and thus led to a various morphology of PS/Cu composites. A more compact copper shell on PS surface can be obtained in the presence of La2O3
Silver (Ag) has excellent conductivity, flexibility and malleability'. A modified electroless silver-plating process was developed for the preparation of monodispersed PS/Ag composite microspheres. PS surfaces were decorated with colloidal platinum of approximately10nm in size, much smaller than that of clusters fabricated by a conventional activation method, which contains Sn and Pd species of70nm. The effects of temperature, time of plating and loading of PS in plating bath on morphology. Ag coating state, dispersion and conductivity of PS/Ag composites were investigated. The results showed that a dense, stable and uniform Ag nanoshell was formed on the surface of PS microspheres with the assistant of poly (vinylpyrrolidone).
A new epoxy based adhesive was prepared by using composite resin of diglycidylether of bisphenol A (DGEBA) and dimmer acid modified DGEBA as matrix and2-methylimidazole or N-phenethylpyrazinium hexafluoroantimonate (PPH) as curing agent. The curing behavior, storage stability at ambient of adhesive and thermostability of cured products were studied. The results showed that the pot life of PPH/EP adhesive exceeded to60days at25～30℃, but the glass transition temperature (Tg) of its cured product was only100℃. To improve the thermostability of cured products, bisphenol A novalac epoxy was added into the adhesive matrix to prepare PPH/MEP system. The results showed that Tg of cured PPH/MEP product increased to120℃, and PPH/MEP system maintained an excellent storage stability at ambient.
ACFs with good conductivity and peel strength were prepared, which electrically connect ITO glass and flex print circuit (FPC) with conducting patterns of500μm in pitch. PS/Ag composite microspheres with diameter of3μm and PPH/MEP system were used as conductive fillers and adhesive resin, respectively. According to the theoretical analysis, contact resistance can be strongly influenced by applied pressure, filler size and number of filler between electrodes. The experimental results showed that increasing the filler content, bonding pressure, temperature and time played positive role on the conductivity of ACF. However, the adhesive property of ACF largely depended on the curing degree of resin. The critical content of conductive fillers was35wt.%in the flex on glass (FOG) process using ACF. When the filler content was20wt.%, ACF possessed good conductivity and peel strength at the same time. The optimal bonding pressure, temperature and time for reliability of interconnection using ACF were0.3MPa,170℃and15s, respectively.
引文
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