CN107805550B - 一种可用于去毛刺的去胶剂、其制备方法和应用 - Google Patents
一种可用于去毛刺的去胶剂、其制备方法和应用 Download PDFInfo
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- CN107805550B CN107805550B CN201710548066.8A CN201710548066A CN107805550B CN 107805550 B CN107805550 B CN 107805550B CN 201710548066 A CN201710548066 A CN 201710548066A CN 107805550 B CN107805550 B CN 107805550B
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- 235000011852 gelatine desserts Nutrition 0.000 description 1
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- GNOIPBMMFNIUFM-UHFFFAOYSA-N hexamethylphosphoric triamide Chemical compound CN(C)P(=O)(N(C)C)N(C)C GNOIPBMMFNIUFM-UHFFFAOYSA-N 0.000 description 1
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- ZUVVLBGWTRIOFH-UHFFFAOYSA-N methyl 4-methyl-2-[(4-methylphenyl)sulfonylamino]pentanoate Chemical compound COC(=O)C(CC(C)C)NS(=O)(=O)C1=CC=C(C)C=C1 ZUVVLBGWTRIOFH-UHFFFAOYSA-N 0.000 description 1
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- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
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- 235000018102 proteins Nutrition 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
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- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 1
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
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- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
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- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/14—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aliphatic hydrocarbons or mono-alcohols
- C11D1/146—Sulfuric acid esters
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/008—Polymeric surface-active agents
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/22—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aromatic compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/34—Derivatives of acids of phosphorus
- C11D1/345—Phosphates or phosphites
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
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Abstract
本发明公开了一种可用于去毛刺的去胶剂、其制备方法和应用。本发明的去胶剂的制备方法,其包括下列步骤:其包括下列步骤:将下述去胶剂的原料混合,即可;所述的原料包括下列质量分数的组分:20%‑70%的溶剂、10%‑50%有机胺、0.01%‑50%还原剂、0.01%‑5%无机碱、0.01%‑10%表面活性剂和水,各组分质量分数之和为100%;所述去胶剂的pH值为7.5‑13.5。本发明的制备方法制得的去胶剂寿命长,可在3个月内循环重复使用;可单独去除tape胶或溢料,或者同时去除tape胶和溢料,并减少后续电镀工艺的锡毛刺的产生;对塑封体和基材无损伤。
Description
技术领域
本发明涉及一种可用于去毛刺的去胶剂、其制备方法和应用。
背景技术
半导体在封装的过程中,塑封体和引脚上会残留各种胶状物质,如tape胶(胶带的胶膜,或称为胶带胶膜,成分一般为硅烷类树脂)或溢料(又称毛刺或飞边,成分一般为环氧塑封料)等,需要清除。否则会导致封装工艺中的框架变形、漏镀、镀层缺陷而影响产品的可靠性,造成产品断路、虚焊等问题,影响管脚的电气导通性能,严重的会导致返工及芯片功能失效甚至报废,这带来了封装工艺的繁杂及成本的上升。因此,去tape胶(detape)和去溢料(deflash或debur)是半导体集成电路封装后处理的重要工艺步骤,尤其是“倒装QFN”(FCQFN)的封装工艺中需要用到。
目前去tape胶(detape)或去溢料(deflash或debur)的方法有高压水喷射去胶、高压水喷砂去胶、激光去胶、化学药水去胶及电化学方法去胶等。其中高压水喷射去胶、高压水喷砂去胶、激光去胶和电化学方法去胶,成本较高且方法剧烈,化学药水去胶由于其低成本及条件温和,逐渐成为主流方法。
化学药水去胶也存在效果不佳的问题,如药水寿命短、药水去除力不够、药水对塑封体和基材有损伤、药水无法一步法去除tape胶和溢料(即只能够单独去除tape或溢料,而不能同时去除tape胶和溢料)等问题。
CN102864458A中公开了一种环保型弱酸性去毛刺软化液,其组分和百分比为:二甲基乙酰胺30-50%、二甲基亚砜30%-50%、糠醛0.5%-1%、OP-10表面活性剂0.5-1%、其余为水。该软化液存在寿命短的缺陷,寿命在一周左右(见[0022]段),且该软化液仅是用于去毛刺(溢料)。
CN102808190A中公开了一种环保型弱碱性低温去毛刺软化液,其各组分和质量百分比为:四氢呋喃10-35%、丙二醇10%-35%、烷基酚聚氧乙醚烯1-5%、乙醇胺5-20%、N-甲基二乙醇胺1-10%、其余为水。该软化液仅是用于去毛刺(溢料)。
CN1935939A中公开了一种集成电路封装后处理用去毛刺溶液,采用下列配方:乙二醇苯醚35%、二乙二醇二丁醚20%、己内酰胺15%、甘油10%和异氟尔酮20%。该去毛刺溶液仅是用于去毛刺(溢料)。
CN103128892A中公开了一种去溢料的溶液,包含质量百分数为10-60%的1,3-二甲基-2-咪唑烷酮、10-30%的乙醇胺、10-60%的六甲基磷酰三胺、0-10%的去离子水。该去溢料的溶液仅是用于去溢料。
CN102270587B中公开了一种塑封晶体管溢料软化液,包含酰胺化合物、烷基醚、NH4F、碱性调整剂、水。该软化液仅是用于去毛刺(溢料)。
因此,本领域迫切需要开发一种集成电路封装后处理用去tape胶和/或去溢料的方法,来解决这些问题。
发明内容
本发明所要解决的技术问题是为了克服现有技术中半导体在封装的过程中,引脚上残留的各种胶状物质如tape胶或溢料等,在使用化学药水去胶方法去除时,存在的化学药水寿命短、去除力不够、对塑封体和基材有损伤、药水无法一步法去除tape胶和溢料等缺陷,而提供了一种可用于去毛刺的去胶剂、其制备方法和应用。本发明的制备方法制得的去胶剂寿命长,可在3个月内循环重复使用;可单独去除tape胶或溢料,或者同时去除tape胶和溢料,并减少后续电镀工艺的毛刺的产生;对塑封体和基材无损伤。
本发明主要是通过以下技术手段解决上述技术问题的。
本发明提供了一种去胶剂,其由下述原料制得,所述的原料包括下列质量分数的组分:20%-70%的溶剂、10%-50%有机胺、0.01%-50%还原剂、0.01%-5%无机碱、0.01%-10%表面活性剂和水,各组分质量分数之和为100%;所述去胶剂的pH值为7.5-13.5。
所述的溶剂的质量分数优选35%-55%,更优选40%-50%。所述的有机胺的质量分数优选15%-45%,更优选20%-40%。所述的还原剂的质量分数优选0.1%-10%,更优选0.15%-5%。所述的无机碱的质量分数优选0.1%-4%,更优选0.15%-0.35%。所述的表面活性剂的质量分数优选0.1%-5%,更优选0.15%-3%。所述去胶剂的pH值优选8-12,更优选9-11。
所述的溶剂可为本领域常规的溶剂,优选醇类溶剂、酮类溶剂、醚类溶剂、亚砜类溶剂、砜类溶剂、酰胺类溶剂和酯类溶剂中的一种或多种。
其中,所述的醇类溶剂优选甘油、甲醇、乙醇、异丙醇、乙二醇、三缩三乙二醇、正丁醇、异丁醇和苯甲醇中的一种或多种。
其中,所述的酮类溶剂优选丙酮、咪唑烷酮、吡咯烷酮、咪唑啉酮和异氟尔酮中的一种或多种。所述的咪唑烷酮优选2-咪唑烷酮、1,3-二甲基-2-咪唑烷酮和1,3-二乙基-2-咪唑烷酮中的一种或多种。所述的吡咯烷酮优选N-甲基吡咯烷酮、N-乙基吡咯烷酮、N-环己基吡咯烷酮、2-吡咯烷酮和N-羟乙基吡咯烷酮中的一种或多种。所述的咪唑啉酮优选1,3-二甲基-2-咪唑啉酮。
其中,所述的亚砜类溶剂优选二甲基亚砜、二乙基亚砜和甲乙基亚砜中的一种或多种。
其中,所述的砜类溶剂优选甲基砜、乙基砜和环丁砜中的一种或多种。
其中,所述的醚类溶剂优选四氢呋喃、乙二醇单烷基醚、二乙二醇单烷基醚、丙二醇单烷基醚、二丙二醇单烷基醚和三丙二醇单烷基醚中的一种或多种。所述的乙二醇单烷基醚优选乙二醇单甲醚、乙二醇单乙醚、乙二醇苯醚和乙二醇单丁醚中的一种或多。所述的二乙二醇单烷基醚优选二乙二醇单甲醚、二乙二醇单乙醚和二乙二醇单丁醚中的一种或多种。所述的丙二醇单烷基醚优选丙二醇单甲醚、丙二醇单乙醚和丙二醇单丁醚中的一种或多种。所述的二丙二醇单烷基醚优选二丙二醇单甲醚、二丙二醇单乙醚和二丙二醇单丁醚中的一种或多种。所述的三丙二醇单烷基醚优选三丙二醇单甲醚。
其中,所述的酰胺较佳的为二甲基甲酰胺和/或二甲基乙酰胺。
其中,所述的酯类溶剂优选乙酸乙酯、乳酸乙酯和二乙酸乙二醇酯中的一种或多种。
所述的有机胺可为本领域常规的有机胺,优选醇胺、有机多胺、含羧基的有机胺和季铵碱类有机胺中的一种或多种。所述的醇胺优选乙醇胺、二乙醇胺、三乙醇胺、异丙醇胺、N,N-二甲基乙醇胺和N-甲基二乙醇胺中的一种或多种。所述的有机多胺优选二乙烯三胺、五甲基二乙烯三胺和多乙烯多胺中的一中或多种。所述的含羧基的有机胺优选2-氨基乙酸、2-氨基苯甲酸、亚氨基二乙酸,氨三乙酸和乙二胺四乙酸中的一种或多种。所述的季铵碱类有机胺优选四甲基氢氧化铵、四乙基氢氧化铵、三甲基苄基氢氧化铵、四乙基氢氧化铵和三乙基苄基氢氧化铵中的一种或多种。
所述的还原剂可为本领域常规的还原剂,优选硼氢化类还原剂(例如硼氢化钠和/或硼氢化钾)、处于低化合物价时的氧化物(例如双氧水)、处于低化合物价时的盐(例如亚硫酸钠、次磷酸钠、硫酸亚铁和氯化亚铁中的一种或多种)、羟基胺、羟胺衍生物(如硫酸羟胺和/或盐酸羟胺)、联氨、水合肼、肼类衍生物(如甲磺酰肼和/或对甲苯磺酸肼)、醛类还原剂(如甲醛、乙醛、葡萄糖和糠醛中的一种或多种)和羧酸类还原剂(如草酸、柠檬酸和维生素C中的一种或多种)中的一种或多种。
所述的无机碱可为本领域常规的无机碱,优选碳酸盐类无机碱(例如碳酸钠和/或碳酸钾)、碳酸氢盐类无机碱(例如碳酸氢钠)、氢氧化盐类无机碱(例如氢氧化钠、氢氧化钾、氢氧化钡和氢氧化钙中的一种或多种)和氨水中的一种或多种。
所述表面活性剂可为本领域常规的表面活性剂,优选阴离子表面活性剂和/或非离子表面活性剂。所述的阴离子表面活性剂优选全氟烷基磺酸钾、仲烷基磺酸钠、十二烷基苯磺酸(LAS)、脂肪醇醚硫酸钠(AES)、乙氧基化脂肪酸甲酯磺酸钠(FMES)、醇醚羧酸盐(AEC)、醇醚磷酸盐、异辛醇硫酸钠、MOA-3PK、MOA-5PK、苯酚聚氧乙烯醚硫酸钠和烷基磺酸盐中的一种或多种。所述的非离子表面活性剂优选聚乙二醇、渗透剂JFC、聚乙二醇醚、OP-10、羟基聚醚、聚乙烯醇(PVA)、聚乙烯吡咯烷酮、聚氧乙烯(POE)、聚硅氧烷(PSOA)、氟代聚乙烯醇、氟代聚乙烯吡咯烷酮、氟代聚氧乙烯、氟代聚硅氧烷、脂肪醇聚氧乙烯醚、多元醇酯、烷基酚聚氧乙烯醚中的一种或多种。
所述的去胶剂的pH值可根据去胶剂中各组分和含量的实际情况调节。例如可使用有机酸、无机酸、无机碱、强碱弱酸盐和缓冲溶液中的一种或多种。当去胶剂的pH值至过低,可使用无机碱和/或强碱弱酸盐调节;当去胶剂的pH值过高时,可使用有机酸和/或无机酸进行调节;另外,若避免去胶剂的pH值发生剧烈波动,可使用本领域常规的缓冲溶液进行调节。
所述的去胶剂的原料组分还可进一步包含氟化物。所述的氟化物可为本领域常规的氟化剂。所述的氟化剂优选氟化氢、氟硅酸、氟硅酸铵、氟硼酸、氟硼酸铵、和、氟化氢与碱形成的盐中的一种或多种。其中,所述的氟化氢与碱形成的盐中所述的碱优选氨水、季胺氢氧化物或醇胺。所述的氟化氢与碱形成的盐优选氟化氢铵(NH4HF2)、四甲基氟化铵(N(CH3)4F)和三羟乙基氟化铵(N(CH2OH)3HF)中的一种或多种。所述的氟化物的质量分数优选0-1%,但不为0;更优选0.1%-0.5%。
所述的去胶剂的原料组分还可进一步包含金属腐蚀抑制剂。所述金属腐蚀抑制剂可为本领域常规的金属腐蚀抑制剂,优选联苯三酚、邻苯二酚、草酸、酒石酸、琥珀酸、马来酸、乙酸、柠檬酸、3-氨基-1,2,4-三氮唑、苯并三氮唑、甘氨酸、丙氨酸、亮氨酸和异亮氨酸中的一种或多种。所述金属腐蚀抑制剂的质量分数优选0-1%,但不为0;更优选0.1%-0.5%。
所述的去胶剂的原料组分还可进一步包含保湿剂。所述保湿剂可为本领域常规的保湿剂,优选甘油、丁二醇、聚乙二醇、丙二醇、已二醇、木糖醇、聚丙二醇、山梨糖醇、乳酸钠、尿素、吡咯烷酮羧酸钠、动物胶、透明质酸、维生素和氨基酸类保湿剂中的一种或多种。所述氨基酸类保湿剂可为植物蛋白、大豆蛋白、动物蛋白和水解蛋白中的一种或多种等。所述保湿剂的质量分数优选0-1%,但不为0;更优选0.1%-0.5%。
所述的去胶剂的原料组分中优选不包含增稠剂。所述增稠剂可为本领域常规的增稠剂,优选硫酸钠、氯化钠、硼砂、CMC、HPMC、甲基纤维素、羟乙基纤维素、海藻酸钠、聚丙烯酸钠、聚丙烯酰胺和聚乙烯醇中的一种或多种。
所述的水优选去离子水、纯水或超纯水。
在本发明一优选实施方式中,所述的去胶剂由下述原料制得,所述的原料由下列质量分数的组分组成:20%-70%的溶剂、10%-50%有机胺、0.01%-50%还原剂、0.01%-5%无机碱、0.01%-10%表面活性剂、水、0-1%的氟化物、0-1%的金属腐蚀抑制剂和0-1%的保湿剂,各组分质量分数之和为100%;所述去胶剂的pH值为7.5-13.5。其中,当所述的原料包含氟化物、金属腐蚀抑制剂和保湿剂中的一种或多种时,所述的氟化物、金属腐蚀抑制剂或保湿剂的质量分数不为0。
本发明还提供了一种所述的去胶剂的制备方法,其包括下列步骤,将所述的原料混合,即可。所述的混合优选将所述的原料组分中的固体组分加入到液体组分中,搅拌均匀,即可。
所述的去胶剂中的原料还可以若干独立组分的套装形式保存。
本发明还提供了一种所述的去胶剂在去除集成电路封装后处理中的tape胶和/或溢料中的应用。
所述的应用优选包括下列步骤:将集成电路封装后处理中的引线框架浸泡在所述的去胶剂中,然后去除去胶剂,干燥,即可。
所述的浸泡的温度可为本领域常规的浸泡温度,优选60-130℃,更优选65-100℃,最优选70-80℃。
所述的浸泡的时间可为本领域常规的时间,优选10-100min,更优选15-90min,最优选30-85min(例如40min、50min或80min)。
所述的去除去胶剂的方法可为本领域常规的方法,优选将浸泡后的引线框架用水冲洗,即可。
在去除去胶剂后,还可包含将浸泡后的塑封体过水刀的操作。所述的过水刀的操作可为本领域常规的操作。
所述的干燥的方法可为本领域常规的方法,优选氮气吹干。
所述的应用中,浸泡在去胶剂中的引线框架可以是单片,也可以是一批(即多片,个数可不作限定,根据实际能够浸泡的个数确定)。
所述的集成电路封装的方法可为本领域常规的集成电路封装的方法,优选采用QFN封装。所述的QFN封装优选倒装QFN(即FCQFN)。
在不违背本领域常识的基础上,上述各优选条件,可任意组合,即得本发明各较佳实例。
本发明中,所述QFN封装是指方形扁平无引脚封装(Quad Flat No-leadPackage)。
本发明中,各组分的质量分数是指各组分的质量占所有原料组分总质量的质量百分比。
本发明中,所述的室温是指10-30℃。
本发明所用试剂和原料均市售可得。
本发明的积极进步效果在于:
1、本发明的制备方法制得的去胶剂寿命长,可在3个月内循环重复使用;可单独去除tape胶或溢料,或者同时去除tape胶和溢料,并减少后续电镀工艺的锡毛刺的产生;对塑封体(基材)无损伤。
2、本发明的制备方法制得的去胶剂可实现操作安全、方便、稳定,操作成本低,可适用于单片或批量处理,生产效率高,便于自动化操作,对基体无损害,电性能优良,因此可以广泛地应用于各种集成电路封装后处理中,尤其是QFN封装后处理。
3、本发明的制备方法制得的去胶剂具有非常广阔的市场应用前景,为微电子企业解决了难题,对促进我国微电子行业的发展起了积极的作用,也具有较高的经济效益。
具体实施方式
下面通过实施例的方式进一步说明本发明,但并不因此将本发明限制在所述的实施例范围之中。下列实施例中未注明具体条件的实验方法,按照常规方法和条件,或按照商品说明书选择。
下述各实施例中,去胶剂的制备方法均为将各实施例中去胶剂原料组分中的固体组分加入到液体组分中,搅拌均匀,即可。
下述实例中,未限定具体操作温度的,均是在室温条件下进行。
去胶剂在去除集成电路封装后处理中的tape胶和/或溢料中的应用的具体操作为:将倒装QFN工艺中molding(封装)后的各单片引线框架(6cm*6cm)浸泡在各实施例的去胶剂中,浸泡时间和温度参照下述应用实施例,操作完成后,用纯水冲洗,过水刀、用氮气吹干,即可。用金相显微镜观察去胶效果,然后进一步电镀锡,并用金相显微镜观察电镀效果。
下述实施例1-14中,水是指去离子水。
去胶剂使用寿命是指去胶剂在浸泡槽中从配槽(将新的去胶剂倒入洗干净的浸泡槽中)开始使用到下一次换槽(将浸泡槽中老去胶剂全部排干净,然后洗干净槽,再倒入新去胶剂)的周期,其间由于去胶剂挥发,样条(即引脚框架)携带等原因会导致浸泡槽中去胶剂液位下降,故每天都会进行补加新去胶剂使浸泡槽中的液位保持稳定。因此,使用寿命是单槽去胶剂换槽的周期。
实施例1-6
表1 去胶剂的各原料组分
表2 各原料组分的质量分数和去胶剂pH值
实施例7-14
实施例7-14为在实施例2的基础上,增加下述组分,并相应调整水的用量,使各组分的质量分数之和为100%。表3中,“/”表示该组分无添加。
表3 实施例7-14新添加的各原料组分和质量分数
应用实施例1-15
表4
表5 各符号含义
严重残留 | × | 严重毛刺 | × |
中等残留 | △ | 中等毛刺 | △ |
轻微残留 | ○ | 轻微毛刺 | ○ |
无残留 | ◎ | 无毛刺 | ◎ |
从以上各应用实施例(1-15)可以看出,本发明的去胶剂去tape胶和去溢料较佳,进而使的镀锡效果也较佳。在操作时间较短或添加增稠剂时,会有轻微残留及镀锡毛刺出现,但并不会影响到引线框架产品的使用效果。
以上各应用实施例(1-15)中,在金相显微镜观察时,并没有观察到镀锡前后的引线框架有基质受损的情况。
另外,将以上各应用实施例(1-15)中的单片引线框架的操作变为批量多片操作,并不影响去tape胶、去溢料及后续的镀锡效果。
进一步进行去胶剂寿命实验发现,本发明的上述各实施例中的去胶剂可重复循环使用3个月以上,使用寿命较长。
对比实施例1-6
表6 去胶剂各原料组分
表7 各原料组分质量分数和去胶剂的pH值
应用实施例16-27
应用实施例23-27对应的对比实例8-12分别为CN102864458A中的实施例1中的去毛刺软化液、CN102808190A中的实施例1中的去毛刺软化液、CN1935939A中的实施例的去毛刺溶液、CN103128892A实施例1中的去毛刺溶液和CN102270587A实施例1中的毛刺软化液。
表8
从以上各应用实施例(16-22)可以看出,对比例1-12的去胶剂去tape胶和去溢料较差,进而使的镀锡效果也较差。在金相显微镜观察时,观察到镀锡前后的引线框架有基质有受损的情况。
进一步进行去胶剂寿命实验发现,上述各对比实施例中的去胶剂最长可重复循环使用2个月,对比例7和8甚至只能重复循环使用一个星期,使用寿命短。
Claims (19)
1.一种去胶剂的制备方法,其特征在于,其包括下列步骤:将下述去胶剂的原料混合,即可;所述的原料由下列质量分数的组分组成:35%-55%的溶剂、10%-50%有机胺、0.1%-10%还原剂、0.1%-4%无机碱、0.1%-5%表面活性剂和水,各组分质量分数之和为100%;所述去胶剂的pH值为8-12;
所述的溶剂为醇类溶剂、酮类溶剂、醚类溶剂、亚砜类溶剂和酯类溶剂中的一种或多种;
所述的醇类溶剂为甘油、甲醇、乙醇、异丙醇、乙二醇、三缩三乙二醇、正丁醇、异丁醇和苯甲醇中的一种或多种;
所述的酮类溶剂为丙酮、咪唑烷酮、吡咯烷酮、咪唑啉酮和异氟尔酮中的一种或多种;
所述的亚砜类溶剂为二甲基亚砜、二乙基亚砜和甲乙基亚砜中的一种或多种;
所述的醚类溶剂为四氢呋喃、乙二醇单烷基醚、二乙二醇单烷基醚、丙二醇单烷基醚、二丙二醇单烷基醚和三丙二醇单烷基醚中的一种或多种;
所述的酯类溶剂为乙酸乙酯、乳酸乙酯和二乙酸乙二醇酯中的一种或多种;
所述的有机胺为醇胺、有机多胺和含羧基的有机胺中的一种或多种;
所述的醇胺为乙醇胺、二乙醇胺、三乙醇胺、异丙醇胺、N,N-二甲基乙醇胺和N-甲基二乙醇胺中的一种或多种;
所述的有机多胺为二乙烯三胺和/或五甲基二乙烯三胺;
所述的含羧基的有机胺为2-氨基乙酸、2-氨基苯甲酸、亚氨基二乙酸,氨三乙酸和乙二胺四乙酸中的一种或多种;
所述的还原剂为羟基胺、羟胺衍生物、联氨、水合肼、肼类衍生物和羧酸类还原剂中的一种或多种;
所述的羟胺衍生物为硫酸羟胺和/或盐酸羟胺;
所述的肼类衍生物为甲磺酰肼和/或对甲苯磺酸肼;
所述的羧酸类还原剂为草酸、柠檬酸和维生素C中的一种或多种;
所述的无机碱为碳酸盐类无机碱、碳酸氢盐类无机碱和氢氧化盐类无机碱中的一种或多种;
所述的碳酸盐类无机碱为碳酸钠和/或碳酸钾;
所述的碳酸氢盐类无机碱为碳酸氢钠;
所述的氢氧化盐类无机碱为氢氧化钠、氢氧化钾、氢氧化钡和氢氧化钙中的一种或多种;
所述表面活性剂为阴离子表面活性剂和/或非离子表面活性剂;
所述的阴离子表面活性剂为全氟烷基磺酸钾、仲烷基磺酸钠、十二烷基苯磺酸、脂肪醇醚硫酸钠、乙氧基化脂肪酸甲酯磺酸钠、醇醚羧酸盐、异辛醇硫酸钠、MOA-3PK、MOA-5PK和苯酚聚氧乙烯醚硫酸钠中的一种或多种;
所述的非离子表面活性剂为聚乙烯吡咯烷酮、脂肪醇聚氧乙烯醚和烷基酚聚氧乙烯醚中的一种或多种。
2.如权利要求1所述的去胶剂的制备方法,其特征在于,
所述的有机胺的质量分数为15%-45%。
3.如权利要求2所述的去胶剂的制备方法,其特征在于,
所述的溶剂的质量分数为40%-50%;
和/或,所述的有机胺的质量分数为20%-40%;
和/或,所述的还原剂的质量分数为0.15%-5%;
和/或,所述的无机碱的质量分数为0.15%-0.35%;
和/或,所述的表面活性剂的质量分数为0.15%-3%;
和/或,所述去胶剂的pH值为9-11。
4.如权利要求1所述的去胶剂的制备方法,其特征在于,
当所述的酮类溶剂为咪唑烷酮时,所述的咪唑烷酮为2-咪唑烷酮、1,3-二甲基-2-咪唑烷酮和1,3-二乙基-2-咪唑烷酮中的一种或多种;
和/或,当所述的醚类溶剂为乙二醇单烷基醚时,所述的乙二醇单烷基醚为乙二醇单甲醚、乙二醇单乙醚、乙二醇苯醚和乙二醇单丁醚中的一种或多种。
5.如权利要求1所述的去胶剂的制备方法,其特征在于,当所述的酮类溶剂为吡咯烷酮时,所述的吡咯烷酮为N-甲基吡咯烷酮、N-乙基吡咯烷酮、N-环己基吡咯烷酮、2-吡咯烷酮和N-羟乙基吡咯烷酮中的一种或多种;
和/或,当所述的醚类溶剂为二乙二醇单烷基醚时,所述的二乙二醇单烷基醚为二乙二醇单甲醚、二乙二醇单乙醚和二乙二醇单丁醚中的一种或多种。
6.如权利要求1所述的去胶剂的制备方法,其特征在于,当所述的酮类溶剂为咪唑啉酮时,所述的咪唑啉酮为1,3-二甲基-2-咪唑啉酮;
和/或,当所述的醚类溶剂为丙二醇单烷基醚时,所述的丙二醇单烷基醚为丙二醇单甲醚、丙二醇单乙醚和丙二醇单丁醚中的一种或多种。
7.如权利要求1所述的去胶剂的制备方法,其特征在于,当所述的醚类溶剂为二丙二醇单烷基醚时,所述的二丙二醇单烷基醚为二丙二醇单甲醚、二丙二醇单乙醚和二丙二醇单丁醚中的一种或多种。
8.如权利要求1所述的去胶剂的制备方法,其特征在于,当所述的醚类溶剂为三丙二醇单烷基醚时,所述的三丙二醇单烷基醚为三丙二醇单甲醚。
9.如权利要求1所述的去胶剂的制备方法,其特征在于,所述的去胶剂的原料组分还进一步包含氟化物、金属腐蚀抑制剂和保湿剂中的一种或多种。
10.如权利要求9所述的去胶剂的制备方法,其特征在于,所述的氟化物的质量分数为0-1%,但不为0。
11.如权利要求10所述的去胶剂的制备方法,其特征在于,所述的氟化物的质量分数为0.1%-0.5%。
12.如权利要求9所述的去胶剂的制备方法,其特征在于,所述金属腐蚀抑制剂的质量分数为0-1%,但不为0。
13.如权利要求12所述的去胶剂的制备方法,其特征在于,所述金属腐蚀抑制剂的质量分数为0.1%-0.5%。
14.如权利要求9所述的去胶剂的制备方法,其特征在于,所述保湿剂的质量分数为0-1%,但不为0。
15.如权利要求14所述的去胶剂的制备方法,其特征在于,所述保湿剂的质量分数为0.1%-0.5%。
16.如权利要求9所述的去胶剂的制备方法,其特征在于,
所述的氟化物为氟化氢、氟硅酸、氟硅酸铵、氟硼酸、氟硼酸铵、和、氟化氢与碱形成的盐中的一种或多种;
和/或,所述金属腐蚀抑制剂为联苯三酚、邻苯二酚、草酸、酒石酸、琥珀酸、马来酸、乙酸、柠檬酸、3-氨基-1,2,4-三氮唑、苯并三氮唑、甘氨酸、丙氨酸、亮氨酸和异亮氨酸中的一种或多种;
和/或,所述保湿剂为甘油、丁二醇、聚乙二醇、丙二醇、已二醇、木糖醇、聚丙二醇、山梨糖醇、乳酸钠、尿素、吡咯烷酮羧酸钠、动物胶、透明质酸、维生素和氨基酸类保湿剂中的一种或多种。
17.如权利要求16所述的去胶剂的制备方法,其特征在于,所述的氟化氢与碱形成的盐中所述的碱为氨水、季胺氢氧化物或醇胺。
18.如权利要求16所述的去胶剂的制备方法,其特征在于,所述的氟化氢与碱形成的盐为氟化氢铵、四甲基氟化铵和三羟乙基氟化铵中的一种或多种。
19.如权利要求1所述的去胶剂的制备方法,其特征在于,所述的混合为将所述的原料组分中的固体组分加入到液体组分中,搅拌均匀,即可。
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