TWI552825B - A solder paste composition, a solder paste and a soldering flux - Google Patents
A solder paste composition, a solder paste and a soldering flux Download PDFInfo
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Description
本發明係關於一種焊膏組合物、一種焊膏及一種助焊劑。The present invention relates to a solder paste composition, a solder paste and a flux.
焊膏係由合金焊粉及糊狀助焊劑均質混合的一種膏狀焊接材料。目前最常使用的合金焊粉包含Sn-Ag系、Sn-Pb系、Sn-Sb系、Sn-Cu系、Sn-Bi系及Sn-Ag-Cu系合金等。而助焊劑通常包含或由一樹脂、一觸變劑、一活化劑、一溶劑以及選擇性地由其他添加劑所組成。助焊劑是淨化金屬表面、改善濕潤性、防止焊接材料氧化、保證焊膏品質及/或所述材料之優良工藝的一種關鍵材料。此外,助焊劑對於焊膏之儲存穩定性具有重要影響。The solder paste is a paste solder material which is homogeneously mixed by alloy solder powder and paste flux. The alloy solder powder most commonly used at present includes Sn-Ag-based, Sn-Pb-based, Sn-Sb-based, Sn-Cu-based, Sn-Bi-based, and Sn-Ag-Cu-based alloys. The flux typically comprises or consists of a resin, a thixotropic agent, an activator, a solvent, and optionally other additives. Flux is a key material for purifying metal surfaces, improving wettability, preventing oxidation of solder materials, ensuring solder paste quality, and/or superior processes for such materials. In addition, the flux has an important influence on the storage stability of the solder paste.
正常情況下,焊膏於儲存期間會隨時間推移而硬化或凝固。通常用硬化或凝固的速度衡量焊膏之儲存穩定性。焊膏具有一高儲存穩定性,通常較慢硬化或凝固;反之,焊膏具有一低儲存穩定性,其表現出較快硬化或凝固之特性。Under normal circumstances, the solder paste hardens or solidifies over time during storage. The storage stability of the solder paste is usually measured by the speed of hardening or solidification. Solder pastes have a high storage stability and generally harden or solidify slowly; conversely, solder pastes have a low storage stability, which exhibits faster hardening or solidification characteristics.
現存焊膏中,有機酸類、有機胺類小分子或含鹵素化合物係作為活化劑。該活化劑可於焊膏儲存期間與合金焊粉交互作用,因此影響其流變性及其他性能。請注意,上述活化劑會嚴重地降低焊膏之儲存穩定性。In the existing solder paste, an organic acid, an organic amine small molecule or a halogen-containing compound is used as an activator. The activator interacts with the alloy solder powder during solder paste storage, thus affecting its rheology and other properties. Please note that the above activators can seriously reduce the storage stability of the solder paste.
不論先前技術之狀況,本發明係預期提供一種助焊劑、一種焊膏組合物及一種焊膏,以克服存在於焊膏中之活化劑於焊膏儲存期間與合金焊粉交互作用,因此降低焊膏儲存穩定性之技術問題。Regardless of the state of the art, the present invention contemplates providing a flux, a solder paste composition, and a solder paste to overcome the interaction of the activator present in the solder paste with the alloy solder powder during solder paste storage, thereby reducing soldering Technical problems with paste storage stability.
本發明之焊膏具優良焊接性能之同時,亦具有一高度儲存穩定性。The solder paste of the present invention has excellent soldering properties and also has a high storage stability.
本發明之焊膏可藉由添加一長鏈硫醇及/或一有機螯合劑至助焊劑中,而顯著提高其儲存穩定性。The solder paste of the present invention can significantly improve its storage stability by adding a long chain thiol and/or an organic chelating agent to the flux.
因此,本發明係關於一種助焊劑,其包含或由一樹脂、一觸變劑、一活化劑、一溶劑以及一長鏈硫醇及/或一有機螯合劑所組成。Accordingly, the present invention is directed to a flux comprising or consisting of a resin, a thixotropic agent, an activator, a solvent, and a long chain thiol and/or an organic chelating agent.
該術辭「樹脂」、「觸變劑」、「活化劑」、「溶劑」、「長鏈硫醇」或「有機螯合劑」意指一種或超過一種之所述成份可存在於本發明之助焊劑中。The terms "resin", "thixotropy", "activator", "solvent", "long-chain thiol" or "organic chelating agent" mean that one or more than one of the ingredients may be present in the present invention. In the flux.
本發明中,所述之長鏈硫醇係至少具一-SH官能基之化合物,其碳鏈長度大於或等於7個碳原子,其中該碳原子較佳者為彼此互相地共價性鍵結。一具體實施例中,長鏈硫醇係由一或多種具通式R(CH2)nSH之化合物所構成之群組選出,其中R為甲基(methyl)、羧基(carboxyl)、羥基(hydroxyl)、甲醯基(formyl)或醯胺基(amido),n為7至21,較佳為12至18;更佳者,所述之長鏈硫醇係由己硫醇(hexanethiol)、辛硫醇(octanethiol)、癸硫醇(decanethiol)、十二硫醇(dodecanethiol)、十八硫醇(octadecanethiol)及/或其等之混合物所選出。本發明之助焊劑中亦可使用不同長鏈硫醇之混合物。In the present invention, the long-chain thiol is a compound having at least one -SH functional group having a carbon chain length of greater than or equal to 7 carbon atoms, wherein the carbon atoms are preferably covalently bonded to each other. . In a specific embodiment, the long chain thiol is selected from the group consisting of one or more compounds of the formula R(CH 2 ) n SH wherein R is methyl, carboxyl, or hydroxyl ( Hydroxyl), formyl or amido, n is 7 to 21, preferably 12 to 18; more preferably, the long chain thiol is hexanethiol, octyl A mixture of octanethiol, decanethiol, dodecanethiol, octadecanethiol, and/or the like is selected. Mixtures of different long chain thiols can also be used in the flux of the present invention.
本發明中,所述之有機螯合劑較佳為選自鄰-二氮雜菲類(o-naphthisodiazine)螯合劑。更佳者,該有機螯合劑係選自1,10-鄰-二氮雜菲(1-10-o-naphthisodiazine)、2,9-二甲基-4,7-二苯基-1,10-啡囉啉(2,9-dimethyl-4,7-diphenyl-1,10-phenanthroline)、4,7-二甲基-1,10-鄰-二氮雜菲(4,7-dimethyl-1,10-o-naphthisodiazine)、4,7-二苯基-1,10-鄰-二氮雜菲(4,7-diphenyl-1,10-o-naphthisodiazine)及/或其等之混合物。In the present invention, the organic chelating agent is preferably selected from the group consisting of o- naphthisodiazine chelating agents. More preferably those, the organic chelating agent is selected from 1,10 - phenanthroline (1-10- o -naphthisodiazine), 2,9- dimethyl-4,7-diphenyl-1,10 -2,9-dimethyl-4,7-diphenyl-1,10-phenanthroline, 4,7-dimethyl-1,10- o -phenanthroline (4,7-dimethyl-1) , 10- o -naphthisodiazine), 4,7- diphenyl-1,10 - phenanthroline (4,7-diphenyl-1,10- o -naphthisodiazine ) and / or mixtures of the like.
本發明中,所述長鏈硫醇及/或有機螯合劑之含量係為可於合金焊粉顆粒表面形成一單分子保護膜之適當含量,其不影響焊膏之其他性能表現。較佳者,長鏈硫醇及/或有機螯合劑以助焊劑總量為基礎,其存在含量為0.2wt%至10wt%,更佳者為0.5wt%至5wt%。當用量低於0.2wt%,合金焊粉顆粒表面單分子保護膜之形成會不完整;當用量高於10wt%,長鏈硫醇及/或有機螯合劑會負面地影響焊膏之其他性能,諸如焊接性能或印刷性能等。 In the present invention, the content of the long-chain thiol and/or organic chelating agent is an appropriate content for forming a single-molecular protective film on the surface of the alloy solder powder particles, which does not affect other performances of the solder paste. Preferably, the long chain thiol and/or organic chelating agent is present in an amount of from 0.2% by weight to 10% by weight, more preferably from 0.5% by weight to 5% by weight, based on the total of the flux. When the amount is less than 0.2% by weight, the formation of the monomolecular protective film on the surface of the alloy solder powder particles may be incomplete; when the amount is more than 10% by weight, the long-chain mercaptan and/or the organic chelating agent may adversely affect other properties of the solder paste. Such as welding performance or printing performance.
一具體實施例中,助焊劑係包含至少一本發明長鏈硫醇及至少一本發明有機螯合劑所組成之混合物。 In one embodiment, the flux comprises a mixture of at least one long chain thiol of the invention and at least one organic chelating agent of the invention.
本發明中,樹脂係選自松香樹脂(rosin resins)、酸修飾之松香樹脂(acid modified rosin resins)、氫化松香樹脂(hydrogenated rosin resins)、歧化松香樹脂(disproportionated rosin resins)及/或聚合松香樹脂(polymerized rosin resins),及/或其等之混合物。樹脂含量可為該領域中之常規用量。較佳者,該樹脂以助焊劑總量為基礎,其存在含量為10wt%至60wt%,及更佳者,其含量為30wt%至55wt%。 In the present invention, the resin is selected from the group consisting of rosin resins, acid modified rosin resins, hydrogenated rosin resins, disproportionated rosin resins, and/or polymeric rosin resins. (polymerized rosin resins), and/or mixtures thereof. The resin content can be a conventional amount in the art. Preferably, the resin is present in an amount of from 10% by weight to 60% by weight based on the total amount of the flux, and more preferably in an amount of from 30% by weight to 55% by weight.
此外,本發明之助焊劑包含至少一觸變劑。該觸變劑係選自聚醯胺類(polyamides)、氫化蓖麻油類(hydrogenated castor oils)及/或醯胺修飾之氫化蓖麻油類(amide modified hydrogenated castor oils),及/或其等之混合物。觸變劑含量可為該領域中之常規用量。較佳者,該觸變劑以助焊劑總量為基礎,其存在含量為1wt%至10wt%。 Furthermore, the flux of the present invention comprises at least one thixotropic agent. The thixotropic agent is selected from the group consisting of polyamides, hydrogenated castor oils and/or amide modified hydrogenated castor oils, and/or mixtures thereof . The thixotropic agent level can be a conventional amount in the art. Preferably, the thixotropic agent is present in an amount of from 1% by weight to 10% by weight based on the total amount of the flux.
本發明助焊劑之另一成份為至少一活化劑。該活化劑係選自含鹵素化合物、有機酸類化合物及/或有機胺類化合物,及/或其等之混合物。活化劑含量可為該領域中之常規用量。較佳者,該活化劑以助焊劑總量為基礎,其存在含量為0.5wt%至30wt%。 Another component of the flux of the present invention is at least one activator. The activator is selected from the group consisting of halogen-containing compounds, organic acid compounds, and/or organic amine compounds, and/or mixtures thereof. The activator content can be a conventional amount in the art. Preferably, the activator is present in an amount of from 0.5% by weight to 30% by weight based on the total amount of the flux.
本發明助焊劑之另一成份為至少一溶劑。一具體實施例中,該溶劑為二醇單醚類(diol monoether)及/或二醇雙醚類(diol diether)溶劑,諸如二乙二醇單己醚(diethylene glycol monohexyl ether)及/或聚乙二醇雙丁醚(polyethylene glycol dibutyl ether)等。溶劑含量可為該領域中之常規用量。較佳者,該溶劑以助焊劑總量為基礎,其存在含量為10 wt%至60 wt%。Another component of the flux of the present invention is at least one solvent. In one embodiment, the solvent is a diol monoether and/or a diol diether solvent, such as diethylene glycol monohexyl ether and/or poly Polyethylene glycol dibutyl ether or the like. The solvent content can be a conventional amount in the art. Preferably, the solvent is present in an amount of from 10% to 60% by weight based on the total amount of the flux.
本發明之助焊劑亦包含其他常規添加劑,諸如增塑劑及/或抗氧化劑等。The flux of the present invention also contains other conventional additives such as plasticizers and/or antioxidants.
本發明之助焊劑可為所有成份混合之一組成形式,亦可為多容器包裝或套裝形式,其中每一成份裝於分別之容器或數個成份組裝於一或多個容器中。The flux of the present invention may be in the form of a mixture of all components, or may be in the form of a multi-container package or kit, wherein each component is contained in a separate container or a plurality of components assembled in one or more containers.
本發明中,所述之助焊劑可由該領域中常規方法製備而得,例如藉由加熱及混合每一成份。In the present invention, the flux can be prepared by conventional methods in the art, for example, by heating and mixing each component.
本發明亦關於一種焊膏組合物,其包含本發明之助焊劑及至少一合金焊粉。該合金焊粉係選自無鉛合金焊粉或含鉛合金焊粉。該術辭「無鉛合金焊粉」係指合金焊粉大致上不包含鉛,其意指該鉛含量以合金焊粉總量為基礎,少於5 wt%,較佳為少於1 wt%,更佳為少於0.01 wt%。The invention also relates to a solder paste composition comprising the flux of the invention and at least one alloy solder powder. The alloy solder powder is selected from a lead-free alloy solder powder or a lead-containing alloy solder powder. The term "lead-free alloy solder powder" means that the alloy solder powder does not substantially contain lead, which means that the lead content is less than 5 wt%, preferably less than 1 wt%, based on the total amount of the alloy solder powder. More preferably less than 0.01 wt%.
較佳者,助焊劑與合金焊粉之體積比為0.8:1至1.2:1。無鉛焊粉較佳為選自Sn-Ag-Cu系、Sn-Ag系、Sn-Cu系、Sn-Zn系及/或Sn-Bi系合金。含鉛焊粉較佳為Sn-Pb系合金。該合金焊粉較佳為一球形粉末形式,其中所述球形粉末之平均顆粒大小較佳為1μm至45μm。Preferably, the volume ratio of the flux to the alloy solder powder is from 0.8:1 to 1.2:1. The lead-free solder powder is preferably selected from the group consisting of Sn-Ag-Cu, Sn-Ag, Sn-Cu, Sn-Zn, and/or Sn-Bi alloys. The lead-containing solder powder is preferably a Sn-Pb-based alloy. The alloy solder powder is preferably in the form of a spherical powder, wherein the spherical powder preferably has an average particle size of from 1 μm to 45 μm.
本發明中,該術辭「平均顆粒大小」係指累積體積分佈曲線(cumulative volume distribution curve)之D50值,其中50%顆粒體積直徑小於所述之值。本發明之平均顆粒大小或D50值係經由雷射繞射測定法(laser diffractometry)測定,其較佳為使用來自Malvern儀器有限公司之Malvern Mastersizer 2000測定。於此技術中,溶於懸浮液或乳化液中之顆粒大小係基於Fraunhofer或Mie理論之應用,利用一雷射光束之繞射加以測定。於本發明中,係利用Mie理論或修正之Mie理論測量非球形顆粒,及該平均顆粒大小或D50值係利用散射測量,其角度相對於入射雷射光束由0.02度至135度。In the present invention, the term "average particle size" refers to a D 50 value of a cumulative volume distribution curve in which 50% of the particle volume diameter is smaller than the stated value. The average particle size or a D 50 value of the present invention by a laser diffraction-based assay (laser diffractometry) was measured, which is preferably measured using a Malvern 2000 from Malvern Instruments Limited Mastersizer. In this technique, the particle size dissolved in the suspension or emulsion is determined by diffraction of a laser beam based on the application of the Fraunhofer or Mie theory. In the present invention, the system using the Mie theory or Mie theory amended measure non-spherical particles, the average particle size and D 50 values based or scattering measurements using, its angle relative to the incident laser beam of 0.02 to 135 degrees.
本發明中,所述焊膏組合物係以多容器包裝或套裝形式,其中每一成份裝於分別之容器或數個成份組裝於一或多個容器中。一具體實施例中,該焊膏組合物包含至少二容器。將長鏈硫醇及/或有機螯合劑作為第一部份,而合金焊粉作為第二部份,二部份較佳為不存放於相同容器中,以避免任何物理性或化學性接觸。例如,所述焊膏組合物為二容器包裝形式,其中一容器內含助焊劑及另一容器內含合金焊粉。於另一具體實施例中,所述焊膏組合物為三容器包裝形式,其中一容器內含長鏈硫醇及/或有機螯合劑,另一容器內含本發明助焊劑之其他成份,及第三容器內含合金焊粉。In the present invention, the solder paste composition is in the form of a multi-container package or kit in which each component is contained in a separate container or a plurality of components assembled in one or more containers. In a specific embodiment, the solder paste composition comprises at least two containers. The long chain mercaptan and/or organic chelating agent is used as the first part, and the alloy solder powder is used as the second part. The two parts are preferably not stored in the same container to avoid any physical or chemical contact. For example, the solder paste composition is in the form of a two-container package in which one container contains a flux and the other container contains an alloy solder powder. In another embodiment, the solder paste composition is in the form of a three-container package, wherein one container contains a long-chain thiol and/or an organic chelating agent, and the other container contains other components of the flux of the present invention, and The third container contains alloy solder powder.
本發明亦關於一種焊膏,其係為本發明焊膏組合物之所有成份之一混合物。The invention also relates to a solder paste which is a mixture of all of the components of the solder paste composition of the present invention.
本發明之焊膏中,合金焊粉之整個顆粒表面較佳為覆蓋一層單分子膜。該單分子膜係由一或多種長鏈硫醇及/或有機螯合劑自我聚集組裝而成。In the solder paste of the present invention, the entire particle surface of the alloy solder powder is preferably covered with a monomolecular film. The monomolecular film is self-assembled and assembled from one or more long chain thiols and/or organic chelating agents.
本發明之焊膏亦包含常規添加劑,諸如增塑劑及/或抗氧化劑等。The solder paste of the present invention also contains conventional additives such as plasticizers and/or antioxidants and the like.
本發明之焊膏可經由混合本發明之助焊劑及合金焊粉製備而得。The solder paste of the present invention can be prepared by mixing the flux of the present invention and an alloy solder powder.
所述之焊膏儲存溫度較佳為0℃至5℃,以使於長時間儲存中具有一高儲存穩定性。The solder paste storage temperature is preferably from 0 ° C to 5 ° C to provide a high storage stability during long-term storage.
本發明之實施例顯示當於30℃儲存4天之條件下,本發明之焊膏較佳為具有一黏度變化少於±6%。相對地,傳統焊膏於相較之儲存條件下,黏度增加84.1%。其指出本發明之焊膏具有一優異儲存穩定性。The examples of the present invention show that the solder paste of the present invention preferably has a viscosity change of less than ± 6% when stored at 30 ° C for 4 days. In contrast, the traditional solder paste has an 84.1% increase in viscosity compared to storage conditions. It is pointed out that the solder paste of the present invention has an excellent storage stability.
本發明焊膏之儲存穩定性顯著增加,具有較佳儲存性及優良焊接性能。相較於現存之焊膏,本發明之焊膏可以簡單製備步驟製備而得。The storage stability of the solder paste of the invention is remarkably increased, and has better storage properties and excellent soldering properties. Compared with the existing solder paste, the solder paste of the present invention can be prepared by a simple preparation step.
除非特別說明,本發明所使用之所有材料及試劑皆為市面上可購得。All materials and reagents used in the present invention are commercially available unless otherwise stated.
助焊劑之製備:Preparation of flux:
將本發明之溶劑、樹脂、活化劑及觸變劑依比例地加入一不銹鋼反應釜中。將混合物於100℃至150℃下攪拌,直至所有成份皆完全溶解。其後將混合物快速冷卻,補充添加部份揮發之溶劑,並以密封方式儲存備用。The solvent, resin, activator and thixotropic agent of the present invention are added to a stainless steel reaction vessel in proportion. The mixture was stirred at 100 ° C to 150 ° C until all ingredients were completely dissolved. Thereafter, the mixture is rapidly cooled, and a portion of the volatilized solvent is added and stored in a sealed manner.
將11.5 wt%之助焊劑及88.5 wt%之合金焊粉置於雙行星攪拌器(double planetary stirrer)中,於室溫下非均質地(heterogeneously)攪拌,並分裝於500公克錫膏罐。11.5 wt% flux and 88.5 wt% alloy solder powder were placed in a double planetary stirrer, heterogeneously stirred at room temperature, and dispensed in a 500 gram solder paste jar.
此實施例中,使用88.5 wt%之合金焊粉Sn-3.0Ag-0.5Cu,及11.5 wt%之助焊劑,該助焊劑含長鏈硫醇及/或有機螯合劑。In this embodiment, 88.5 wt% of the alloy solder powder Sn-3.0Ag-0.5Cu, and 11.5 wt% of the flux were used, and the flux contained a long-chain thiol and/or an organic chelating agent.
助焊劑之特殊配方如下:The special formulation of the flux is as follows:
此實施例中,使用88.5 wt%之合金焊粉Sn-3.0Ag-0.5Cu,及11.5 wt%之助焊劑,該助焊劑含長鏈硫醇及/或有機螯合劑。In this embodiment, 88.5 wt% of the alloy solder powder Sn-3.0Ag-0.5Cu, and 11.5 wt% of the flux were used, and the flux contained a long-chain thiol and/or an organic chelating agent.
助焊劑之特殊配方如下:The special formulation of the flux is as follows:
此實施例中,使用88.5 wt%之合金焊粉Sn-3.0Ag-0.5Cu,及11.5 wt%之助焊劑,該助焊劑含長鏈硫醇及/或有機螯合劑。In this embodiment, 88.5 wt% of the alloy solder powder Sn-3.0Ag-0.5Cu, and 11.5 wt% of the flux were used, and the flux contained a long-chain thiol and/or an organic chelating agent.
助焊劑之特殊配方如下:The special formulation of the flux is as follows:
此實施例中,使用88.5 wt%之合金焊粉Sn-3.0Ag-0.5Cu,及11.5 wt%之助焊劑,該助焊劑不包含長鏈硫醇及/或有機螯合劑。In this example, 88.5 wt% of alloy solder powder Sn-3.0Ag-0.5Cu, and 11.5 wt% flux were used, which flux did not contain long chain mercaptans and/or organic chelating agents.
助焊劑之特殊配方如下:The special formulation of the flux is as follows:
儲存穩定性及濕潤性Storage stability and wettability
測定所有實施例及對比實施例之儲存穩定性及焊接濕潤性。The storage stability and weld wettability of all the examples and comparative examples were measured.
Malcom黏度:Malcom viscosity:
利用Malcom PCU-201黏度計分別測量儲存前及儲存後之黏度。黏度於轉速為10rpm下進行比較,以表現黏度變化。The viscosity before and after storage was measured using a Malcom PCU-201 viscometer. The viscosity was compared at a rotational speed of 10 rpm to show a change in viscosity.
黏度變化%=(儲存後10rpm黏度一儲存前10rpm黏度)/儲存前10rpm黏度% change in viscosity = (10 rpm viscosity after storage - 10 rpm viscosity before storage) / 10 rpm viscosity before storage
當上述實施例之焊膏於30℃下儲存4天後,利用Malcom黏度測量其儲存穩定性。其測試與比較結果如表一所示。When the solder paste of the above example was stored at 30 ° C for 4 days, its storage stability was measured by Malcom viscosity. The test and comparison results are shown in Table 1.
由表一結果可知,本發明之焊膏(實施例1至3)相較於對比實施例1,展現出一較佳儲存穩定性。As can be seen from the results of Table 1, the solder pastes of the present invention (Examples 1 to 3) exhibited a better storage stability than Comparative Example 1.
此即說明長鏈硫醇及/或鄰-二氮雜菲之添加可顯著地提高焊膏之儲存穩定性,其中該焊接濕潤性仍表現良好。This means that the addition of long-chain thiols and/or o -phenanthroline can significantly improve the storage stability of the solder paste, wherein the solder wettability still performs well.
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TW317519B (en) * | 1995-05-24 | 1997-10-11 | Fry Metals Inc | |
JP3273757B2 (en) * | 1998-03-19 | 2002-04-15 | 株式会社東芝 | Solder paste and flux for forming solder joints |
JP3814594B2 (en) * | 2003-08-08 | 2006-08-30 | 株式会社東芝 | Solder and solder paste |
TW201039962A (en) * | 2009-03-30 | 2010-11-16 | Arakawa Chem Ind | Lead-free solder flux composition and lead-free solder composition |
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TW317519B (en) * | 1995-05-24 | 1997-10-11 | Fry Metals Inc | |
JP3273757B2 (en) * | 1998-03-19 | 2002-04-15 | 株式会社東芝 | Solder paste and flux for forming solder joints |
JP3814594B2 (en) * | 2003-08-08 | 2006-08-30 | 株式会社東芝 | Solder and solder paste |
TW201039962A (en) * | 2009-03-30 | 2010-11-16 | Arakawa Chem Ind | Lead-free solder flux composition and lead-free solder composition |
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