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CN1085382C - Electrodeposition of low temperature, high conductivity, powder materials for electrically conductive paste formulations - Google Patents

Electrodeposition of low temperature, high conductivity, powder materials for electrically conductive paste formulations Download PDF

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CN1085382C
CN1085382C CN98108096A CN98108096A CN1085382C CN 1085382 C CN1085382 C CN 1085382C CN 98108096 A CN98108096 A CN 98108096A CN 98108096 A CN98108096 A CN 98108096A CN 1085382 C CN1085382 C CN 1085382C
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electrically conductive
dendritic crystal
conductive paste
dendritic
coating
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CN1202405A (en
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S·K·康
S·普鲁索塔曼
R·S·莱
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
    • C09J9/02—Electrically-conducting adhesives
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J201/00—Adhesives based on unspecified macromolecular compounds
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K3/00—Apparatus or processes for manufacturing printed circuits
    • H05K3/30—Assembling printed circuits with electric components, e.g. with resistor
    • H05K3/32—Assembling printed circuits with electric components, e.g. with resistor electrically connecting electric components or wires to printed circuits
    • H05K3/34—Assembling printed circuits with electric components, e.g. with resistor electrically connecting electric components or wires to printed circuits by soldering
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
    • C09J2203/326—Applications of adhesives in processes or use of adhesives in the form of films or foils for bonding electronic components such as wafers, chips or semiconductors
    • H10W72/073—

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  • Microelectronics & Electronic Packaging (AREA)
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Abstract

一种用于导电焊膏制造的新电解沉积粉末材料，其几种结构形式如下：包括Sn(内涂层)/Cu(枝状晶体)/Sn(阻挡层)/In(外涂层)的电解沉积粉末；包括Sn(内涂层)/Cu(枝状晶体)/Bi-Sn(外涂层)的电解沉积粉末。把这种电解沉积粉末材料用于制造聚合物焊膏。这有助于减少处理过程步骤及化学材料，并减小成本及印刷电路板带来的对环境的影响。这种焊膏可用于将诸如芯片和芯片承载带的电子元件安装在例如显示玻璃屏和印刷线路板的芯片底座的基片上。

A new electrodeposited powder material for the manufacture of conductive solder paste, its several structural forms are as follows: Including Sn(inner coating)/Cu(dendrite)/Sn(barrier layer)/In(outer coating) Electrolytic deposition powder; Electrolytic deposition powder comprising Sn (inner coating layer)/Cu (dendrite)/Bi—Sn (outer coating layer). This electrodeposited powder material is used to make polymer solder pastes. This helps reduce processing steps and chemical materials, and reduces the cost and environmental impact of printed circuit boards. Such solder pastes are useful for mounting electronic components such as chips and chip carrier tapes on substrates such as display glass panels and chip mounts of printed wiring boards.

Description

导电焊膏材料连接结构和制造导电焊膏枝状晶体材料的方法Conductive solder paste material connection structure and method for manufacturing conductive solder paste dendrite material

本发明涉及在导电部件之间形成导电连接的导电焊膏材料，及生产此导电焊膏材料的方法。此外，本发明致力环境安全材料和工艺过程，它可替代含铅焊接技术。The present invention relates to an electrically conductive solder paste material for forming an electrically conductive connection between electrically conductive components, and to a method of producing the electrically conductive solder paste material. Additionally, the present invention addresses environmentally safe materials and processes that can replace leaded soldering techniques.

用于电子设备的大多数电导体由金属制成，如铜、铝、金、银、铅/锡(焊料)、钼或其他金属。使用铅/锡合金的焊接技术，如倒装片连接(或C4)、球栅阵列(BGA)中的焊球连接、IC封装组件连接到印刷电路板(PCB)等，在各种电子封装中起着关键作用。电子封装中产生的焊接点在电气互连及机械/物理连接中具有重要作用。当任一功能失效，则认为焊接点出现故障，它经常威协到整个电子系统停机。Most electrical conductors used in electronic devices are made of metals such as copper, aluminum, gold, silver, lead/tin (solder), molybdenum or other metals. Soldering techniques using lead/tin alloys, such as flip chip connection (or C4), solder ball connection in ball grid array (BGA), IC package component connection to printed circuit board (PCB), etc., in various electronic packages plays a key role. Solder joints created in electronic packaging play an important role in electrical interconnection and mechanical/physical connection. When any function fails, the solder joint is considered to have failed, which often threatens to shut down the entire electronic system.

当微电子封装被组装于印刷电路板时，最广泛使用的是铅/锡合金中具有最低熔点(183℃)的铅/锡易熔焊料，63％Sn-37％Pb。在这些应用中，批量生产中采用两种焊接技术：金属化孔(PTH)和表面安装技术(SMT)焊接。两种技术之间的基本区别在于在PCB设计和其互连机制上的不同。When microelectronic packages are assembled on printed circuit boards, the most widely used lead/tin eutectic solder, 63%Sn-37%Pb, has the lowest melting point (183°C) among the lead/tin alloys. In these applications, two soldering techniques are used in mass production: metallized hole (PTH) and surface mount technology (SMT) soldering. The basic difference between the two technologies lies in the difference in PCB design and its interconnection mechanism.

在SMT焊接中，微电子封装直接附于PCB的表面。SMT的主要优点为高封装密度，它通过消除PCB中的大多数PTH，及利用PCB的两面安装元件而实现。此外，SMT封装比传统的PTH封装具有更细的引线行距和更小封装尺寸。因而，SMT在减小电子封装的尺寸而由此减小整个系统的积体中起了很大作用。In SMT soldering, the microelectronic package is attached directly to the surface of the PCB. The main advantage of SMT is high packaging density, which is achieved by eliminating most of the PTH in the PCB and utilizing both sides of the PCB to mount components. In addition, SMT packages have finer lead spacing and smaller package sizes than traditional PTH packages. Thus, SMT plays a large role in reducing the size of electronic packages and thereby reducing the overall system bulk.

在SMT焊接中，焊膏通过丝网印刷而涂于PCB上。焊膏包括细焊料粉、焊剂，和有机溶剂。在回流过程中，焊料粒子被熔化，焊剂被活化，溶料材料被蒸发，而同时熔化的焊料凝结而最后固化。相反，在波动焊接过程中，PCB首先涂覆焊剂且元件被安装在上面。然后被移至熔化的焊料波中。In SMT soldering, solder paste is applied to the PCB by screen printing. Solder paste includes fine solder powder, flux, and organic solvents. During the reflow process, the solder particles are melted, the flux is activated, and the molten material is evaporated while the molten solder condenses and finally solidifies. In contrast, during wave soldering, the PCB is first coated with flux and the components are mounted on it. It is then moved into a wave of molten solder.

焊接过程通常通过使焊接点经过清洗步骤以去除残留焊剂而完成。出于环境考虑，消除了氯氟烃(CFC)和其他有害清洗剂，而代之以水溶或免清洗焊剂。The soldering process is usually done by subjecting the solder joints to a cleaning step to remove residual flux. Due to environmental concerns, chlorofluorocarbons (CFCs) and other hazardous cleaning agents are eliminated and replaced with water-soluble or no-clean fluxes.

微电子设备中的新发展要求电子封装和印刷电路板之间很小行距的连接(在几百微米行距的数量级)。目前用于SMT的焊膏由于如焊桥或焊球的焊接缺陷，而无法处理此非常精细行距的互连。使用Pb-Sn易熔焊料的另一技术局限为其大约为215℃的高回流温度。此温度已经高于在大多数聚合印刷电路板材料中使用的环氧树脂的玻璃化转变温度。在此回流温度下的热操作在焊接后于印刷电路板中产生显著的热应变，特别是在垂直于PCB表面的方向，在这个方向没有进行结构强化。因而，在组装PCB中的残余热应变将降低电子系统的可靠性。New developments in microelectronics require very small pitch connections (on the order of hundreds of microns pitch) between electronic packages and printed circuit boards. Current solder pastes for SMT cannot handle this very fine pitch interconnection due to soldering defects such as solder bridges or solder balls. Another technique using Pb-Sn eutectic solder is limited by its high reflow temperature of about 215°C. This temperature is already higher than the glass transition temperature of the epoxy resins used in most polymeric printed circuit board materials. Thermal operation at this reflow temperature produces significant thermal strain in the printed circuit board after soldering, especially in the direction perpendicular to the PCB surface, where no structural strengthening is performed. Thus, residual thermal strain in the assembled PCB will reduce the reliability of the electronic system.

关于使用含铅焊料的一个更严重的问题为环境问题，在其他工业中通过从汽油和涂料中清除铅，我们已经经历了这种趋势和影响。A more serious issue with regard to the use of leaded solders is an environmental issue, and we have experienced this trend and impact in other industries through the removal of lead from gasoline and paint.

在电子工业中，关于替代含铅焊料的可能性，目前人们研究两组不同的材料：无铅焊料合金和导电焊膏(ECP)。本发明讨论导电焊膏的发展及应用。导电焊膏(或粘结剂)由加载于聚合材料基体中的金属填料粒子制成。填充银粒子的环氧树脂为概要显示于图1的导电焊膏6的最常见的实例。通常为片状的银粒子2由渗透机制提供电传导，而环氧树脂基体4提供元件8和基片10之间的粘接胶合。很久以来，此种填充银的环氧树脂材料已用于电子应用场合、作为芯片焊接材料，这里更多地利用了其导热而非导电特性。然而，这种材料尚未被要求高导电及细小行距连接的应用所接受；填充银的环氧树脂材料有几个限制，如低导电率，热暴露时接触电阻增大，低焊点强度，银迁移，难于重新加工等等。由于这种填充银的环氧树脂材料在所有方向均导电，在导电性上它被归为“各向同性”。有另一类电导粘结剂(或膜)，它仅在一个方向提供导电性。此类材料即为所谓的“各向异性”导电粘结剂12或膜，如图2中概要显示的。各向异性导电粘结剂12或膜仅在它被压于两导电衬垫22和24之间时导电。此过程要求常温和常压。各向异性导电膜的主要应用为液晶显示面板与其电子印刷电路板的连接。导电粒子14通常是可变形的，如焊球，或镀镍或金的塑料球。粘结材料16大多为热固树脂。In the electronics industry, two different groups of materials are currently being investigated for potential replacements for lead-containing solders: lead-free solder alloys and conductive solder pastes (ECP). This invention discusses the development and application of conductive solder paste. Conductive solder pastes (or binders) are made of metal filler particles loaded in a polymeric material matrix. Epoxy filled with silver particles is the most common example of a conductive solder paste 6 schematically shown in FIG. 1 . Silver particles 2 , generally in the form of flakes, provide electrical conduction by an infiltration mechanism, while epoxy resin matrix 4 provides the adhesive bond between component 8 and substrate 10 . This silver-filled epoxy material has long been used in electronics applications as a die-bonding material, where its thermal rather than electrical properties are used more. However, this material has not been accepted for applications that require high electrical conductivity and fine line spacing connections; silver-filled epoxy materials have several limitations, such as low electrical conductivity, increased contact resistance when exposed to heat, low solder joint strength, silver migration, difficult to rework, etc. Since this silver-filled epoxy material conducts electricity in all directions, it is classified as "isotropic" in terms of conductivity. There is another class of electrically conductive adhesives (or films) that provide conductivity in only one direction. Such materials are so-called "anisotropic" conductive adhesives 12 or films, as schematically shown in FIG. 2 . Anisotropic conductive adhesive 12 or film conducts electricity only when it is pressed between two conductive pads 22 and 24 . This process requires normal temperature and pressure. The main application of anisotropic conductive film is the connection of liquid crystal display panel and its electronic printed circuit board. Conductive particles 14 are usually deformable, such as solder balls, or nickel or gold plated plastic balls. The adhesive material 16 is mostly a thermosetting resin.

在我们最近的发明(YO893-0292)中，公开了一种导电焊膏(ECP)材料，它包括：镀有一薄层低熔点的、诸如Sn、In、Bi、Sb和其合金的非铅金属的铜粉，混合以对环境安全的焊剂，并分散于热塑或热固聚合物基体。含有镀Sn64的Cu粉62的ECP微观结构以其剖视图形式示于图3中。In our recent invention (YO893-0292), an electrically conductive solder paste (ECP) material is disclosed which comprises: a thin layer of non-lead metals such as Sn, In, Bi, Sb and their alloys plated with a thin layer copper powder, mixed with an environmentally safe flux, and dispersed in a thermoplastic or thermoset polymer matrix. The ECP microstructure containing Sn64-plated Cu powder 62 is shown in FIG. 3 in its cross-sectional view.

由镀Sn的Cu粉和聚酰亚胺-硅氧烷树脂制成的ECP对于诸如C4和与陶瓷基片的焊球连接(SBC)的高温焊点是很好的选择。然而，对聚合印刷电路板应用场合，此ECP就不够了，因为诸如250℃的回流温度比例如FR-4的聚合树脂的玻璃化转变温度高得多。对此目的的一个选择为与聚酰亚胺-硅氧烷组成的镀铟Cu粉。镀铟Cu焊膏的回流温度预计在180℃左右，它甚至低于Pb/Sn的215℃的回流温度。ECPs made of Sn-plated Cu powder and polyimide-siloxane resin are good choices for high-temperature solder joints such as C4 and solder ball connections (SBC) to ceramic substrates. However, for polymeric printed circuit board applications, this ECP is not sufficient because reflow temperatures such as 250°C are much higher than the glass transition temperature of polymeric resins such as FR-4. One option for this purpose is indium-coated Cu powder composed of polyimide-siloxane. The reflow temperature of indium-plated Cu solder paste is expected to be around 180°C, which is even lower than the 215°C reflow temperature of Pb/Sn.

在我们最近的发明(YO994-280，YO994-281)中，公开了用于高导电焊膏应用场合的枝状晶体粉末材料的结构和制造方法，如图4所示。铜枝状晶体结构44淀积于空基片40上，随后是在铜枝状晶体结构顶部电解沉积另一种低熔点金属42(In、Sn、Zn、Bi和Sb及其合金)。然后从基片上收集枝状晶体粉末，并与热塑或热固聚合树脂混合形成导电焊膏。In our recent inventions (YO994-280, YO994-281), the structure and manufacturing method of dendritic powder materials for highly conductive solder paste applications are disclosed, as shown in Figure 4. A copper dendrite structure 44 is deposited on the empty substrate 40, followed by electrolytic deposition of another low melting point metal 42 (In, Sn, Zn, Bi and Sb and their alloys) on top of the copper dendrite structure. The dendrite powder is then collected from the substrate and mixed with a thermoplastic or thermosetting polymeric resin to form a conductive solder paste.

在现有技术中，于美国专利No.5,062,896(Huang et.al.)中公开了一种焊料/聚合物复合焊膏材料，包括如Bi-Sn、Pb-Sn、Bi-Sn-Pb合金的可熔焊料粉状填充料的主要成份，一小部分如聚酰亚胺-硅氧烷的热塑聚合物，和一小部分焊剂。获得了无氧、部分聚合(coalesced)焊料合金连接，它是用聚合物加强的并可在低回流温度下重新加工，或在有聚合物溶剂的情况下更是如此。In the prior art, a solder/polymer composite solder paste material including Bi-Sn, Pb-Sn, Bi-Sn-Pb alloys is disclosed in U.S. Patent No. 5,062,896 (Huang et.al.) The main component of fusible solder powder filler, a small part of thermoplastic polymers such as polyimide-siloxane, and a small part of flux. Oxygen-free, partially coalesced solder alloy connections are obtained that are reinforced with polymers and can be reworked at low reflow temperatures, or more so in the presence of polymer solvents.

在类似的先有技术美国专利No.5,286,417(Mahmoud et.al.)中，公开了一种可熔导电粘结剂，它包括如Sn-Au和Bi-Au的金属合金填充料，及具有超过金属填充料合金的熔化温度的玻璃化转变温度的热塑聚合物。聚合物中导电材料的加载按重量计在15％至20％的范围内。In similar prior art U.S. Patent No. 5,286,417 (Mahmoud et.al.), a fusible conductive adhesive is disclosed, which includes metal alloy fillers such as Sn-Au and Bi-Au, and has more than The melting temperature of the metal filler alloy is the glass transition temperature of the thermoplastic polymer. The loading of conductive material in the polymer ranges from 15% to 20% by weight.

另一现有技术、美国专利No.5,136,365(Pennisi et.al.)中，公开了一粘结剂材料，它在环氧树脂基体中含有焊剂和如Sn、Pb、In、Bi、Sb、Ag和其他材料的用于回流焊接的金属粒子。在回流焊接时，所述粘结剂在电子元件和基片之间形成各向异性的导电。Another prior art, U.S. Patent No. 5,136,365 (Pennisi et.al.), discloses a binder material that contains flux and solder such as Sn, Pb, In, Bi, Sb, Ag in an epoxy matrix. and other materials for reflow soldering metal particles. The adhesive forms anisotropic conduction between the electronic component and the substrate during reflow soldering.

另一现有技术、美国专利No.5,213,715(Pennisi et.al.)中，公开了一种方向性导电聚合物，它包含有Ni或Cu粉的金属填充料。金属粉由不同于用作基体树脂的聚合物处理。加压时，涂覆的聚合物被位移，在填充料粒子之间形成电传导。Another prior art, U.S. Patent No. 5,213,715 (Pennisi et.al.), discloses a directional conductive polymer containing a metal filler of Ni or Cu powder. The metal powder is treated with a different polymer than the resin used as the matrix. When pressure is applied, the coated polymer is displaced, creating electrical conduction between the filler particles.

本发明的目的在于提供对环境安全且低成本的导电焊膏材料。An object of the present invention is to provide an environmentally safe and low-cost conductive solder paste material.

本发明的目的在于提供产生比传统的填充银的环氧树脂具有更高导电性的导电焊膏材料。It is an object of the present invention to provide conductive solder paste materials that yield higher conductivity than conventional silver-filled epoxies.

本发明的目的在于提供可在比Pb-Sn易熔焊膏的回流温度更低的温度下处理的导电焊膏材料。It is an object of the present invention to provide a conductive solder paste material which can be processed at a lower temperature than the reflow temperature of Pb-Sn eutectic solder paste.

本发明的目的在于提供比传统的填充银的环氧树脂焊膏更抗腐蚀的导电焊膏材料。It is an object of the present invention to provide conductive solder paste materials that are more corrosion resistant than conventional silver-filled epoxy solder pastes.

在一个特别的实施例中，我们公开了一种包括Sn(内涂层)/Cu(枝状晶体)/Sn(阻挡层)/In(外涂层)的电解沉积的粉末结构。此粉末结构顺序地电解沉积于诸如钛或不锈钢的空基片上，电解沉积材料可很容易地从其上分离。内涂层Sn层对Cu表面提供抗氧化或抗腐蚀的保护，并在它们相接触时控制所述上涂层的成分、以便在粉末粒子间形成金相粘合。Sn阻挡层减缓快速的Cu-In化合物形成，它可防止粒子与粒子间的粘合。In外涂层与Sn内涂层及阻档层一起使得能够在150℃的低温下发生粒子与粒子间的粘合。内涂层、阻挡层和外涂层的厚度约在1微米或更小的范围。Cu枝状晶体的大小在1至50微米长的范围。In a particular embodiment, we disclose an electrodeposited powder structure comprising Sn(inner coat)/Cu(dendrite)/Sn(barrier)/In(outer coat). The powder structure is sequentially electrolytically deposited on an empty substrate, such as titanium or stainless steel, from which the electrodeposited material can be easily separated. The undercoat Sn layer provides protection to the Cu surface against oxidation or corrosion and controls the composition of the overcoat when they are in contact so as to form a metallographic bond between the powder particles. The Sn barrier slows down the rapid Cu-In compound formation, which prevents particle-to-particle adhesion. The In overcoat, together with the Sn undercoat and barrier layer, enables particle-to-particle bonding to occur at low temperatures of 150°C. The thickness of the inner coat, barrier layer and outer coat is in the range of about 1 micron or less. The Cu dendrites range in size from 1 to 50 microns long.

在一个特别的实施例中，我们公开了一种包括Sn(内涂层)/Cu(枝状晶体)/Bi-Sn(外涂层)的电解沉积粉末结构。此结构中Cu和Bi-Sn金属之间不需要有阻挡层。Bi-Sn外涂层是利用商品电镀液以近易熔混合物的形式电解沉积而形成的。收集的电解沉积粉粒的粒径有很大差异。为了获得一致的粒径，要求与微筛分(micro-sieve screening)工艺的同时进行喷射研磨工艺或超声波粒径缩减。最佳粒径分布为5至10微米。In a particular embodiment, we disclose an electrodeposited powder structure comprising Sn (inner coating)/Cu (dendrites)/Bi-Sn (outer coating). There is no need for a barrier layer between Cu and Bi-Sn metal in this structure. The Bi-Sn topcoat is formed by electrolytic deposition in the form of a near-fusible mixture using commercial plating baths. The particle size of the collected electrodeposited powders varies greatly. To achieve a consistent particle size, a jet milling process or ultrasonic particle size reduction is required concurrently with the micro-sieve screening process. The optimum particle size distribution is 5 to 10 microns.

然后，具有一致且最佳粒径的电解沉积粉末与热塑或热固树脂混合形成前述本发明的(YO994-280，YO994-281)的导电焊膏。Then, the electrolytic deposition powder with consistent and optimal particle size is mixed with thermoplastic or thermosetting resin to form the aforementioned conductive solder paste of the present invention (YO994-280, YO994-281).

图1为对包括作为环氧树脂基体中填充料的银片粒子的导电焊膏的简要说明。此导电焊膏在导电性上为各向同性。(现有技术)Figure 1 is a schematic illustration of a conductive solder paste including silver flake particles as filler in an epoxy matrix. This conductive solder paste is isotropic in conductivity. (current technology)

图2为对当粘结剂膜被压于两接触或粘合焊盘之间时，仅在一个方向导电的导电粘结剂的简要说明。此导电粘结剂(或膜)被归类为各向异性的。(现有技术)Figure 2 is a schematic illustration of a conductive adhesive that conducts electricity in only one direction when the adhesive film is pressed between two contact or bonding pads. This conductive adhesive (or film) is classified as anisotropic. (current technology)

图3为对一种导电粘结剂材料的简要说明，它包括填充于热塑聚合树脂中的球形铜粉。铜粒子镀有诸如锡、铟、铋及其他材料的低熔点无毒金属。Figure 3 is a schematic illustration of a conductive adhesive material comprising spherical copper powder filled in a thermoplastic polymer resin. The copper particles are plated with low melting non-toxic metals such as tin, indium, bismuth and others.

图4为对淀积于空基片的枝状晶体铜粉、随后在枝状晶体粉末上电解沉积一薄层铟金属的简要说明。Figure 4 is a schematic illustration of the deposition of dendritic copper powder on an empty substrate, followed by the electrolytic deposition of a thin layer of indium metal on the dendritic powder.

图5为对淀积于空基片的新电解沉积粉末结构：Sn(内涂层)/Cu(枝状晶体)/Sn(阻挡层)/In(外涂层)的简要说明。Figure 5 is a brief illustration of the new electrodeposited powder structure: Sn(inner coat)/Cu(dendrite)/Sn(barrier)/In(outer coat) deposited on a blank substrate.

图6为对淀积于空基片的新电解沉积粉末结构：Sn(内涂层)/Cu(枝状晶体)/Bi-Sn(外涂层)的简要说明。Figure 6 is a brief illustration of the new electrodeposited powder structure: Sn (inner coat)/Cu (dendrites)/Bi-Sn (outer coat) deposited on an empty substrate.

在上述发明YO994-280和YO994-281中，我们公开了淀积于空基片的枝状晶体铜粉，随后在铜枝状晶体结构顶部电解沉积薄的铟金属。镀铟的铜枝状晶体粉末可很容易地通过刮空基片而收集。所公开的关于铜枝状晶体电解沉积的详细条件为三个阶段的电镀机制：(i)高密度铜的初始电镀，(ii)枝状晶体核形成阶段，和(iii)枝状晶体生长阶段。In the aforementioned inventions YO994-280 and YO994-281 we disclosed dendrite copper powder deposited on a hollow substrate, followed by electrolytic deposition of a thin layer of indium metal on top of the copper dendrite structure. Indium-coated copper dendrite powder can be easily collected by scraping the substrate. The detailed conditions disclosed for the electrowinning of copper dendrites are a three-stage plating mechanism: (i) initial plating of high-density copper, (ii) dendrite nucleation stage, and (iii) dendrite growth stage .

还公开了铟电镀条件和镀液。Indium electroplating conditions and plating solutions are also disclosed.

图5为对淀积于空基片50的新电解沉积粉末结构：Sn(内涂层)52/Cu(枝状晶体)54/Sn(阻挡层)56/In(外涂层)58的简要说明。内涂层Sn52和阻挡层Sn层56利用LeaRonal，Inc公司的Solderon TinConcentrate溶液电解沉积。Sn阻挡层可由诸如Ni、Co、Cr、Fe、Pd及其合金的其他金属和合金替代。Figure 5 is a brief overview of the new electrodeposited powder structure deposited on an empty substrate 50: Sn (inner coating) 52/Cu (dendrites) 54/Sn (barrier layer) 56/In (outer coating) 58 illustrate. The inner coating Sn52 and the barrier layer Sn layer 56 are electrolytically deposited using Solderon TinConcentrate solution of LeaRonal, Inc. The Sn barrier layer can be replaced by other metals and alloys such as Ni, Co, Cr, Fe, Pd and their alloys.

图6为对淀积于空基片60的新电解沉积粉末结构：Sn(内涂层)62/Cu(枝状晶体)64/Bi-Sn(外涂层)66的简要说明。以Bi-Sn合金的形式淀积外涂层Bi-Sn层66，其成分为近易熔物，按重量计60％Bi-40％Sn。Bi-Sn合金层是利用来自LeaRonal，Inc公司的包括SolderonTin Concentrate、Solderon Bi Concentrate、Solderon Acid、SolderonBi Primary和Solderon Bi Secondary的镀液淀积的。Sn/Cu/Bi-Sn粉末材料的典型电解沉积条件如下：FIG. 6 is a schematic illustration of the new electrodeposited powder structure: Sn (inner coat) 62 /Cu (dendrites) 64 /Bi-Sn (outer coat) 66 deposited on an empty substrate 60 . The overcoat Bi-Sn layer 66 is deposited in the form of a Bi-Sn alloy having a near eutectic composition of 60% Bi-40% Sn by weight. Bi-Sn alloy layers were deposited using baths from LeaRonal, Inc. including SolderonTin Concentrate, Solderon Bi Concentrate, Solderon Acid, SolderonBi Primary, and Solderon Bi Secondary. Typical electrodeposition conditions for Sn/Cu/Bi-Sn powder materials are as follows:

(i)Sn(内涂层)：对100平方英寸面积为2A、0.5V、3分钟，(i) Sn (inner coating): 2A, 0.5V, 3 minutes for an area of 100 square inches,

(ii)Cu(枝状晶体)：对100平方英寸面积为20A、2.5V、3分钟，(ii) Cu (Dendrite): 20A, 2.5V, 3 minutes for 100 square inches area,

(iii)Bi-Sn(外涂层)：对100平方英寸面积为14A、2.0V、2分钟。(iii) Bi-Sn (overcoat): 14A, 2.0V, 2 minutes for a 100 square inch area.

Cu电镀的阳极材料为无氧铜金属，而Sn和Bi-Sn电镀的阳极材料为纯锡金属。The anode material of Cu electroplating is oxygen-free copper metal, while the anode material of Sn and Bi-Sn electroplating is pure tin metal.

收集的电解沉积粉粒的粒径有很大差异。为了获得一致的粒径，要求与微筛分(micro-sieve screening)工艺过程的同时进行喷射研磨工艺过程或超声波粒径缩减。最佳粒径分布为5至10微米。The particle size of the collected electrodeposited powders varies greatly. To achieve a consistent particle size, a jet milling process or ultrasonic particle size reduction is required in parallel with the micro-sieve screening process. The optimum particle size distribution is 5 to 10 microns.

具有一致且最佳粒径的电解沉积粉末储存于“免清洗”焊剂Qualitek#305中，直至用于焊膏制造。如上所述，通过将具有一致且所需粒径的所述填充料弥散在热塑或热固树脂基体中来制造上述发明(YO994-280，YO994-281)的导电焊膏。Electrodeposition powders with consistent and optimal particle size were stored in "no-clean" flux Qualitek #305 until used for solder paste manufacture. As mentioned above, the conductive solder pastes of the above inventions (YO994-280, YO994-281) are manufactured by dispersing said fillers having a uniform and desired particle size in a thermoplastic or thermosetting resin matrix.

为了说明电气和机械性能，通过两个L形铜试样。利用所述低温、无铅导电焊膏制作了接点样品。接连操作在180℃、15分钟、25磅/平方英寸(psi)的条件下进行。由Sn/Cu/Bi-Sn和聚酰亚胺-硅氧烷树脂制成的样品接点与焊点相比显示出良好的电气和机械性能。To illustrate the electrical and mechanical properties, two L-shaped copper coupons were passed. Joint samples were fabricated using the low temperature, lead-free conductive solder paste. Successive runs were performed at 180°C, 15 minutes, 25 pounds per square inch (psi). Sample joints made of Sn/Cu/Bi-Sn and polyimide-siloxane resin showed good electrical and mechanical properties compared to solder joints.

Claims (73)

1. electrically conductive paste material syndeton comprises:
Many material dendritic crystals;
Described dendritic crystal has core and from the dendritic filament of the outwardly directed branch of described core; And
Described dendritic crystal has at first coating of the first of described dendritic crystal with at second coating of the second portion of described dendritic crystal.
2. the electrically conductive paste material syndeton of claim 1 is characterized in that described racemosus shape crystal is a powder.
3. the electrically conductive paste material syndeton of claim 1 is characterized in that described material comprises Cu.
4. the electrically conductive paste material syndeton of claim 1, it is characterized in that described first coating is selected material from the one group of material that comprises In, Sn, Zn, Bi and Sb, and second coating is selected different materials from the one group of material that comprises In, Sn, Zn, Bi and Sb.
5. the electrically conductive paste material syndeton of claim 3 is characterized in that in the described dendritic crystal that at least some dendritic crystals merge mutually by other dendritic crystals in conductive coating and the described dendritic crystal.
6. the electrically conductive paste material syndeton of claim 1 is characterized in that described racemosus shape crystal embedded polymer thing material.
7. the electrically conductive paste material syndeton of claim 1 is characterized in that described structure is an electrical interconnection arrangement.
8. the electrically conductive paste material syndeton of claim 1 is characterized in that described conductive coating has the fusion temperature lower than described dendritic crystal.
9. the electrically conductive paste material syndeton of claim 1 is characterized in that also comprising first and second surfaces, and described structure is arranged between the two so that interconnection between described first and second surfaces is provided.
10. the electrically conductive paste material syndeton of claim 6 is characterized in that described polymeric material is through supersolidification or bake.
11. the structure that claim 6 electrically conductive paste material connects is characterized in that described polymeric material is to select from one group of material of the biological poly resin that comprises polyimides, siloxanes, polyimides-siloxanes, epoxy resin and made by lignin, cellulose, tung oil and crop oil.
12. the structure that claim 6 electrically conductive paste material connects is characterized in that described polymeric material is solvent-laden thermoplastic adhesive.
13. the structure that claim 6 electrically conductive paste material connects is characterized in that described polymeric material is not solvent-laden thermoplastic adhesive.
14. the structure that claim 9 electrically conductive paste material connects is characterized in that described many dendritic crystals embed in the polymeric material of formation described first and the gluing joint of described second surface.
15. the electrically conductive paste material syndeton of claim 9 it is characterized in that described first surface is the first electronic installation contact position, and described second surface is the second electronic device contact position.
16. the electrically conductive paste material syndeton of claim 15 is characterized in that described first electronic installation is a semiconductor chip and described second electronic device is an enclosed chip.
17. the electrically conductive paste material syndeton of claim 9 is characterized in that one of described first surface and described second surface are solder surface.
18. the electrically conductive paste material syndeton of claim 9 is characterized in that described structure is an electronic installation.
19. the electrically conductive paste material syndeton of claim 9 is characterized in that described structure is a calculation element.
20. an electrically conductive paste material syndeton comprises:
The network that has the interconnection dendritic crystal in space therebetween;
In the described dendritic crystal each has first and second coating of soluble material on the second portion of described dendritic crystal;
The adjacent dendritic crystal that in described each network, is bonded together by described fusible material.
21. the electrically conductive paste material syndeton of claim 20 is characterized in that described space comprises polymeric material.
22. the electrically conductive paste material syndeton of claim 20 is characterized in that described dendritic crystal has core and from the dendritic filament of the outwardly directed branch of described core.
23. the electrically conductive paste material syndeton of claim 1 is characterized in that described dendritic crystal has the aspect ratio of length and width and described length and the ratio of described width.
24. the electrically conductive paste material syndeton of claim 23 is characterized in that described aspect ratio is between about 1 to about 10.
25. the electrically conductive paste material syndeton of claim 23 is characterized in that described aspect ratio is between about 1 to about 5.
26. the electrically conductive paste material syndeton of claim 20 is characterized in that described material conducts electricity.
27. the electrically conductive paste material syndeton of claim 6 is characterized in that described dendritic crystal accounts for about 10% to about 90% of described structure by weight.
28. the electrically conductive paste material syndeton of claim 6 is characterized in that described material selects from the one group of material that comprises polyimides, siloxanes, polyimides-siloxanes, epoxy resin and biological poly resin.
29. the electrically conductive paste material syndeton of claim 9, it is characterized in that described coating form to described first and the metallographic of described second surface bonding.
30. the electrically conductive paste material syndeton of claim 9, it is characterized in that described first and described second surface conduct electricity.
31. the electrically conductive paste material syndeton of claim 1 is characterized in that described coating conducts electricity.
32. the electrically conductive paste material syndeton of claim 6 is characterized in that it also comprises solution, butyric acid and ethylene glycol.
33. the electrically conductive paste material syndeton of claim 6 is characterized in that it also comprises solution and comprises " exempt from clean " solder flux of low residue, halogen catalyst.
34. the electrically conductive paste material syndeton of claim 6 is characterized in that described polymeric material is the solvent-free thermal cured binders.
35. the electrically conductive paste material syndeton of claim 6 is characterized in that described polymeric material is a solubility epoxy resin.
36. the electrically conductive paste material syndeton of claim 35 is characterized in that described solubility epoxy resin selects from the one group of material that comprises ketal and acetal diepoxides.
37. an electrically conductive paste material syndeton comprises:
Many copper dendritic crystals;
Described dendritic crystal has the core of copper and from the filament of the outwardly directed branch of described core; And
Described dendritic crystal has first coating and second coating on described dendritic crystal second portion in described dendritic crystal first, described first coating is Sn, and described second coating has at ground floor tin on the described copper dendritic crystal and the top layer In on described Sn layer.
38. a method of making electrically conductive paste dendritic crystal material may further comprise the steps:
Be provided with and the contacted surface of plating of first plating bath;
The dendritic crystal of from described plating bath, growing on described surface; And
Forming the dendritic crystal that formation second coating applies with formation on first coating and the second portion at described dendritic crystal in the first of described dendritic crystal.
39. the method according to the manufacturing electrically conductive paste dendritic crystal material of claim 38 is characterized in that described first plating bath is an electroplate liquid.
40., it is characterized in that described second plating bath selects from the one group of plating bath that comprises chemical plating fluid, immersion plating plating bath and electroplate liquid according to the method for the manufacturing electrically conductive paste dendritic crystal material of claim 38.
41., it is characterized in that the described surface of plating conducts electricity according to the method for the manufacturing electrically conductive paste dendritic crystal material of claim 38.
42. according to the method for the manufacturing electrically conductive paste dendritic crystal material of claim 38, it is characterized in that it also comprise from the described dendritic crystal of described surface removal and on described conductive coating.
43. the method according to the manufacturing electrically conductive paste dendritic crystal material of claim 38 is characterized in that described dendritic crystal has core and divides outwardly directed branch dendritic filament from central division.
44., it is characterized in that described removal step comprises from described surface to scrape off described dendritic crystal according to the method for the manufacturing electrically conductive paste dendritic crystal material of claim 42.
45. the method according to the manufacturing electrically conductive paste dendritic crystal material of claim 38 is characterized in that described dendritic crystal is formed by electric conducting material.
46. the method according to the manufacturing electrically conductive paste dendritic crystal material of claim 45 is characterized in that described electric conducting material comprises Cu.
47. according to the method for the manufacturing electrically conductive paste dendritic crystal material of claim 38, it is characterized in that described coating be conduction and form by described dendritic crystal is immersed second plating bath.
48. the method according to the manufacturing electrically conductive paste dendritic crystal material of claim 47 is characterized in that described second plating bath is an electroplate liquid.
49., it is characterized in that described second plating bath selects from the one group of plating bath that comprises chemical plating fluid and immersion plating plating bath according to the method for the manufacturing electrically conductive paste dendritic crystal material of claim 47.
50., it is characterized in that when described surface is exposed to described first plating bath, first voltage is added on described surface described lip-deep dendritic crystal being electroplated according to the method for the manufacturing electrically conductive paste dendritic crystal material of claim 38; And when described dendritic crystal is exposed to described second plating bath, second voltage is added on described dendritic crystal the coat on the described dendritic crystal is electroplated.
51. method according to the manufacturing electrically conductive paste dendritic crystal material of claim 38, it is characterized in that described first coating selects from the one group of material that comprises Sn, Zn, In, Bi and Sb, and the different materials of described second coating for from the one group of material that comprises Sn, Zn, In, Bi and Sb, selecting.
52. the method according to the manufacturing electrically conductive paste dendritic crystal material of claim 42 is characterized in that making a kind of powder by the dendritic crystal of described coating.
53., it is characterized in that also comprising that dendritic crystal with described coating adds in the polymeric material makes soldering paste according to the method for the manufacturing electrically conductive paste dendritic crystal material of claim 52.
54., it is characterized in that also comprising solvent, butyric acid, ethylene glycol and " exempting to clean " solder flux to make soldering paste according to the method for the manufacturing electrically conductive paste dendritic crystal material of claim 53.
55., it is characterized in that described polymeric material selects from one group of material of the bio-based resin that comprises polyimides, siloxanes, polyimides-siloxanes, epoxy resin, made by lignin, cellulose, tung oil and crop oil according to the method for the manufacturing electrically conductive paste dendritic crystal material of claim 53.
56. the method according to the manufacturing electrically conductive paste dendritic crystal material of claim 53 is characterized in that described soldering paste is placed between first and second conductive surfaces.
57. the method according to the manufacturing electrically conductive paste dendritic crystal material of claim 53 it is characterized in that described first conductive surface is the chip contact site, and described second conductive surface is the substrate contact site.
58. the method according to the manufacturing electrically conductive paste dendritic crystal material of claim 56 is characterized in that described first conductive surface is the LCDs contact site, and described second conductive surface is chip bearing belt lead-in wire position.
59. the method according to the manufacturing electrically conductive paste dendritic crystal material of claim 56 is characterized in that described soldering paste is heated to first temperature to melt the coating on the adjacent dendritic crystal.
60. according to the method for the manufacturing electrically conductive paste dendritic crystal material of claim 56, it is characterized in that described soldering paste is heated to is enough to second temperature that described polymer is solidified.
61. a method of making electrically conductive paste dendritic crystal material may further comprise the steps:
The dendritic crystal of growing from the teeth outwards;
In the first of described dendritic crystal, apply described dendritic crystal, and on the second portion of described dendritic crystal, apply described dendritic crystal, to form the dendritic crystal that applies with second coat with first coating; And
Dendritic crystal from the described coating of described surface removal.
62. the method according to the manufacturing electrically conductive paste dendritic crystal material of claim 61 is characterized in that described first coat and described second coat conduct electricity.
63. the method according to the manufacturing electrically conductive paste dendritic crystal material of claim 53 is characterized in that described polymeric material is a solubility epoxy resin.
64., it is characterized in that described solubility epoxy resin selects from the one group of material that comprises ketal and acetal diepoxides according to the method for the manufacturing electrically conductive paste dendritic crystal material of claim 63.
65. the method according to the manufacturing electrically conductive paste dendritic crystal material of claim 64 is characterized in that the dendritic crystal of described coating is scattered between first and second conductive surfaces.
66., it is characterized in that described first coating and described second coating conduct electricity according to the method for the manufacturing electrically conductive paste dendritic crystal material of claim 38.
67. the method according to the manufacturing electrically conductive paste dendritic crystal material of claim 61 is characterized in that also comprising solvent, butyric acid and ethylene glycol.
68., it is characterized in that also comprising solvent and contain " exempting to clean " solder flux of low residue, halogen catalyst according to the method for the manufacturing electrically conductive paste dendritic crystal material of claim 61.
69. the method according to the manufacturing electrically conductive paste dendritic crystal material of claim 61 is characterized in that also comprising that polymeric material is no solution hot setting adhesive.
70. the method according to the manufacturing electrically conductive paste dendritic crystal material of claim 69 is characterized in that described polymeric material is a solubility epoxy resin.
71., it is characterized in that described solubility epoxy resin selects from the one group of material that comprises ketal and acetal diepoxides according to the method for the manufacturing electrically conductive paste dendritic crystal material of claim 70.
72. a method of making electrically conductive paste dendritic crystal material may further comprise the steps:
The contacted surface of plating of first plating bath is set;
Described surface is on-chip Sn;
From described plating bath at the described surface growth Cu dendritic crystal that plates; With
On described dendritic crystal, form coating to form the dendritic crystal that applies;
On the exposed surface of described Cu dendritic crystal, form the Sn layer, and on the Sn layer, form the In layer;
Remove described dendritic crystal from described substrate, described substrate formation has the first of coating Sn and the dendritic crystal Cu particle that Sn goes up the second portion that applies the In layer.
73. a method of making electrically conductive paste dendritic crystal material may further comprise the steps:
Be provided with and the contacted surface of plating of first plating bath;
Described surface is on-chip Sn;
From described plating bath at the described surface growth Cu dendritic crystal that plates;
On described dendritic crystal, form coating to form the dendritic crystal that applies;
On the exposed surface of described Cu dendritic crystal, form the Sn-Bi alloy-layer; And
Remove described dendritic crystal from described substrate, described substrate forms has first that applies Sn and the dendritic crystal Cu particle that applies the second portion of Sn-Bi alloy-layer.
CN98108096A 1997-06-04 1998-05-04 Electrodeposition of low temperature, high conductivity, powder materials for electrically conductive paste formulations Expired - Fee Related CN1085382C (en)

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CN1129339A (en) * 1994-10-20 1996-08-21 国际商业机器公司 Conductive colloid material and its application
JPH08273431A (en) * 1995-03-31 1996-10-18 Internatl Business Mach Corp <Ibm> Dendrite powder material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0528829A (en) * 1991-07-12 1993-02-05 Tokyo Cosmos Electric Co Ltd Conductive paint and method for forming conductive film thereof
JPH065116A (en) * 1992-06-19 1994-01-14 Shin Etsu Polymer Co Ltd Low melting point metal-bonded anisotropic conductive film
CN1129339A (en) * 1994-10-20 1996-08-21 国际商业机器公司 Conductive colloid material and its application
JPH08273431A (en) * 1995-03-31 1996-10-18 Internatl Business Mach Corp <Ibm> Dendrite powder material

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SG76544A1 (en) 2000-11-21
CN1202405A (en) 1998-12-23

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