CN101228000B - 水溶性预焊剂及其应用 - Google Patents
水溶性预焊剂及其应用 Download PDFInfo
- Publication number
- CN101228000B CN101228000B CN2006800183913A CN200680018391A CN101228000B CN 101228000 B CN101228000 B CN 101228000B CN 2006800183913 A CN2006800183913 A CN 2006800183913A CN 200680018391 A CN200680018391 A CN 200680018391A CN 101228000 B CN101228000 B CN 101228000B
- Authority
- CN
- China
- Prior art keywords
- water
- ethyoxyl
- methyl ethoxy
- acetate
- soluble preflux
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- -1 imidazole compound Chemical class 0.000 claims abstract description 77
- 238000000034 method Methods 0.000 claims abstract description 31
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims abstract description 12
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 12
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 6
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 5
- 150000004693 imidazolium salts Chemical class 0.000 claims description 31
- 238000003466 welding Methods 0.000 claims description 23
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- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 description 3
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- 235000007586 terpenes Nutrition 0.000 description 3
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- KWMXBFIAGYXCCC-UHFFFAOYSA-N 3-(2-methoxyethoxy)propanoic acid Chemical compound COCCOCCC(O)=O KWMXBFIAGYXCCC-UHFFFAOYSA-N 0.000 description 2
- JRXXEXVXTFEBIY-UHFFFAOYSA-N 3-ethoxypropanoic acid Chemical compound CCOCCC(O)=O JRXXEXVXTFEBIY-UHFFFAOYSA-N 0.000 description 2
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- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 description 1
- 229910000165 zinc phosphate Inorganic materials 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
- ZPEJZWGMHAKWNL-UHFFFAOYSA-L zinc;oxalate Chemical compound [Zn+2].[O-]C(=O)C([O-])=O ZPEJZWGMHAKWNL-UHFFFAOYSA-L 0.000 description 1
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Abstract
本发明的目的之一是提供一种水溶性预焊剂,其包含低挥发性增溶剂,具有使咪唑化合物溶解于水的优良性能,并且能够使咪唑化合物产生优良的成膜性能,并提供一种对金属导电部件表面的处理方法,该方法包括使所述表面与上述水溶性预焊剂进行接触。另一目的是提供一种印刷线路板,其中金属导电部件的所述表面已经与上述水溶性预焊剂进行接触;和一种焊接方法,其包含将金属导电部件的所述表面与上述水溶性预焊剂进行接触和随后对表面进行焊接。一种水溶性预焊剂,包含咪唑化合物和含4-16个碳原子的羧酸化合物,该羧酸化合物由如下通式1表示:[通式1]其中R1表示含1-4个碳原子的直链或支链烷基,R2表示氢原子或甲基,m表示0-3的整数,n表示1或2。
Description
技术领域
本发明涉及一种水溶性预焊剂,其用于焊接构成电子部件和类似物的印刷线路板电路部分的金属导电部件的表面。
背景技术
近年来,具有增强密度的表面贴装技术已被广泛采用。这种表面贴装技术可分为双侧表面贴装技术,该技术使用焊膏将芯片类部件进行连接,和混合贴装技术,该技术使用焊膏的芯片类部件的表面贴装技术与离散部件通孔贴装技术的组合。在每种贴装方法中,对印刷线路板进行两道或更多道焊接步骤,因而要将其置于导致苛刻受热历史的高温之下。
结果,通过加热构成印刷线路板电路部件的金属导电部件的铜、铜合金或银金属表面,加速了氧化膜的形成,从而导电部件的表面不能保持优良的可焊性能。
为了保护印刷线路板的金属导电部件免受空气氧化,使用表面处理剂在导电部件表面形成化学层的处理被广泛进行。然而,甚至在金属导电部件经受多个周期的受热历程之后,通过使化学层免于劣化(degenerating)(即被降解)以保护金属导电部件,这对保持优良可焊性是必要的。
由于咪唑化合物具有优良的成膜性能,如这类表面处理剂,已经提出包含各种咪唑化合物的水溶性预焊剂。例如,专利文献1-4公开了的2-烷基咪唑化合物如2-十一烷基咪唑、2-芳基咪唑化合物如2-苯基咪唑和2-苯基-4-甲基咪唑、2-烷基苯并咪唑化合物如2-壬基苯并咪唑,和2-芳烷基苯并咪唑化合物如2-(4-氯苯基甲基)苯并咪唑。
附带提及,由于咪唑化合物通常难溶于水,所以必须使用形成其水溶性盐的有机酸或无机酸作为增溶剂使其溶解于水中。
近年来,甲酸或乙酸作为增溶剂已经被广泛使用,二者都具有优良的使咪唑化合物溶解于水的性能,并能促使咪唑化合物具有优良的成膜性能。然而,由于这些酸化合物高度挥发并具有刺激性气味,将会引起由于水溶性预焊剂中的酸浓度降低,咪唑化合物可能沉淀和酸化合物可能造成工作环境恶化的问题。
锡-铅合金共熔焊料在前述焊接中已被广泛采用。然而近年来,由于含在焊料合金中包含的铅对人体产生副作用已倍受关注,因此期望使用无铅焊料。
由此,各种的无铅焊料正被研究。例如,已经提出这样的无铅焊料,其中将金属如银、锌、铋、铟,锑或铜加到基础金属锡中,并且其部分产品投入实际使用中。
常规使用的锡-铅合金共熔焊料在金属导电部件的金属如铜、铜合金或银表面上具有优良的可湿性,因此可牢固地粘附在金属上,导致高可靠性。
相反,无铅焊料不如常规使用的锡-铅焊料在金属表面的可湿性能好,因此由于孔隙和其它粘结缺陷表现为较差的可焊接性能和低粘结强度。
因此,当使用无铅焊料时,必须选择一种具有更高可焊接性能的焊料合金和适用于无铅焊料的助熔剂。所使用的用于避免金属导电部件的金属如铜、铜合金或银的表面上氧化的水溶性预焊剂,也需要具有改善无铅焊料的可湿性和可焊接性的功能。
此外,大多数无铅焊料熔点较高,并且焊接温度比常规使用的锡-铅共熔焊料的焊接温度高约20-约50℃。因此,期望水溶性预焊剂具有可形成优良耐热性化学层的特性。
专利文献1:JP-B-46-17046
专利文献2:JP-A-4-206681
专利文献3:JP-A-5-25407
专利文献4:JP-A-5-186888
发明描述
本发明要解决的问题
鉴于前述情况,得到本发明。本发明的目标是提供一种含有低挥发性增溶剂的水溶性预焊剂,其具有使咪唑化合物溶解于水中的优良性能,并使咪唑化合物产生优良的成膜性能,还提供一种对金属导电部件表面处理方法,其包含将所述表面与上述水溶性预焊剂进行接触。
另一目标是提供一种印刷线路板,其中金属导电部件的所述表面已经与上述水溶性预焊剂相接触,和一种焊接方法,该方法包括使金属导电部件的所述表面与上述水溶性预焊剂接触以及随后焊接所述表面。
解决问题的方法
为了解决前述问题,本发明的发明人进行了广泛而深入的研究。结果发现了由下面通式1表示的含4-16个碳原子的羧酸化合物,具有优良的使咪唑化合物溶解于水的性能和使咪唑化合物具有优良的成膜性,因此本发明得以完成。
[式1]
(其中R1表示含1-4个碳原子的直链或支链烷基,R2表示氢原子或甲基,m表示0-3的整数,n表示1或2。)
即,第一项发明涉及一种水溶性预焊剂,其包含咪唑化合物和上述通式1表示的含4-16个碳原子的羧酸化合物。
第二项发明涉及所述水溶性预焊剂,其包含比例为0.01-10wt.%的咪唑化合物,和比例为0.1-50wt.%的上述羧酸化合物。
第三项发明涉及一种金属导电部件的表面处理方法,其包括使金属导电部件的所述表面与第一项或第二项发明的水溶性预焊剂接触。
第四项发明涉及一种印刷线路板,其中金属导电部件的所述表面已经与第一项或第二项发明的水溶性预焊剂接触。
第五项发明涉及一种焊接方法,其包括使金属导电部件的所述表面与第一项或第二项发明的水溶性预焊剂接触和随后进行焊接。
发明效果
由于本发明中的水溶性预焊剂含有作为咪唑化合物增溶剂的低挥发性羧酸化合物,因此可稳定保持水溶性预焊剂中增溶剂的浓度,并且不产生难闻的气味。此外,与使用甲酸或乙酸作增溶剂的情况相比,可使咪唑化合物具有优良的成膜性能。
根据本发明的表面处理方法,可在金属导电部件表面形成化学层,并因此避免金属导电部件表面的氧化。
当使用本发明的印刷线路板时,金属导电部件与电子部件之间的粘接可通过焊接安全地实现。
根据本发明的焊接方法,可防止金属导电部件表面的氧化,并因此得到优良的可焊接性。
本发明的最佳实施方式
下文将详细解释本发明。
适合实施本发明的咪唑化合物无特别限制。其实施例包括烷基咪唑化合物、芳基咪唑化合物、芳烷基咪唑化合物、烷基苯并咪唑化合物、芳基苯并咪唑化合物和芳烷基苯并咪唑化合物。
对于上述烷基咪唑化合物,可以提及1-癸基咪唑、2-甲基咪唑、2-十一烷基咪唑、2-十七烷基咪唑、2-乙基-4-甲基咪唑、2-十一烷基-4-甲基咪唑、4-甲基咪唑、4-辛基咪唑、2-环己基咪唑,等。
对于上述芳基咪唑化合物,可以提及1-苯基咪唑、2-苯基咪唑、2-甲苯基咪唑、2-(4-氯苯基)咪唑、2-苯基-4-甲基咪唑、2-苯基-1-苯甲基咪唑、2-苯基-4-苯甲基咪唑、2,4-连苯基咪唑、2,4-联苯基-5-甲基咪唑、2-苯基-4-(3,4-二氯苯基)咪唑、2-苯基-4-(2,4-二氯苯基)-5-甲基咪唑、2-(2,4-二氯苯基)-4-苯基-5-甲基咪唑、4-苯基咪唑、2-壬基-4-苯基咪唑、4-苯基-5-癸基咪唑、2-苯基-4-甲基-5-苯甲基咪唑、2-(1-萘基)咪唑、2-(2-萘基)-4-(4-氯苯基)-5-甲基咪唑、2-苯基-4-(2-萘基)咪唑、2,4,5-三苯基咪唑、2-(2,4-二氯苯基)-4,5-联苯基咪唑、2-(1-萘基)-4,5-联苯基咪唑、2-(4-吡啶基)-4,5-联苯基咪唑,等。
对于上述芳烷基咪唑化合物,可以提及1-苯甲基咪唑、1-(4-氯苯基)甲基-2-甲基咪唑、2-苯甲基咪唑、2-苯甲基-4-甲基咪唑、2-(2-苯乙基)咪唑、2-(5-苯基戊基)咪唑、2-甲基-4,5-联苄基咪唑、1-(2,4-二氯苯基)甲基-2-苯甲基咪唑、2-(1-萘基)甲基-4-甲基咪唑,等。
对于上述烷基苯并咪唑化合物,可以提及1-十二烷基-2-甲基苯并咪唑、2-丙基苯并咪唑、2-戊基苯并咪唑、2-辛基苯并咪唑、2-壬基苯并咪唑、2-十七烷基苯并咪唑、2-己基-5-甲基苯并咪唑、2-戊基-5,6-二氯苯并咪唑、2-(1-乙基戊基)苯并咪唑、2-(2,4,4-三甲基戊基)苯并咪唑、2-环己基苯并咪唑、2-(5-环己基戊基)苯并咪唑、2-苯氧基甲基苯并咪唑、2-(2-氨基乙基)苯并咪唑、2,2’-乙烯基二苯并咪唑、2-(巯甲基)苯并咪唑、2-戊基巯基苯并咪唑,等。
对于上述芳苯基咪唑化合物,可以提及1-苯基苯并咪唑、2-苯基苯并咪唑、2-(4-氯苯基)苯并咪唑、1-苯甲基-2-苯基苯并咪唑、2-o-甲苯基-5,6-二甲基苯并咪唑、2-(1-萘基)-5-氯苯并咪唑、5-苯基苯并咪唑、2-(2-吡啶基)苯并咪唑,等。
对于上述芳烷基苯并咪唑化合物,可以提及1-苯甲基苯并咪唑、2-苯甲基苯并咪唑、2-(4-氯苯基)甲基苯并咪唑、2-(4-溴代苯基)甲基苯并咪唑、2-(2,4-二氯苯基)甲基苯并咪唑、2-(3,4-二氯苯基)甲基苯并咪唑、2-p-甲苯基甲基-5,6-二氯苯并咪唑、1-烯丙基-2-(4-氯苯基)甲基苯并咪唑、2-(2-苯基乙基)苯并咪唑、2-(3-苯基丙基)-5-甲基苯并咪唑、2-(1-萘基)甲基苯并咪唑、2-(2-苯基乙烯基)苯并咪唑、2-(苯甲基巯基)苯并咪唑、2-(2-苯甲基巯基乙基)苯并咪唑,等。
这些咪唑化合物可以0.01-10wt.%,优选0.1-5wt.%的比例存在于水溶性预焊剂中。当所含的咪唑化合物比例小于0.01wt.%,在金属表面形成的化学层会变薄并因此不能充分避免金属表面的氧化。当所含的咪唑化合物比例大于10wt.%,则难以控制为得到适合焊接条件的期望层厚度的表面处理。
在实施本发明中,当通过对咪唑化合物进行增溶(转化成为一种水溶液)制备水溶性预焊剂时,上述通式1所示的具有4-16个碳原子的羧酸化合物被用作增溶剂。
根据本发明人的发现,通过使用具有如下化学结构的羧酸化合物,可使增溶咪唑化合物的性能得以增强,该化学结构中通过亚烷基醚链(-CH2CH(R2)-O-)将烷氧基(R1-O-)与羧甲基(-CH2COOH)或羧乙基(-C2H4COOH)连接,因此m优选为1-3。
此外,具有3个碳原子的羧酸化合物为甲氧基乙酸,但是这种物质据报道难于在生物体内进行代谢并具有导致睾丸萎缩或畸形的后果,因而使其商业用途不优选。
上述通式1所示具有4-16个碳原子的羧酸化合物中,下述通式2所示具有4-16个碳原子的羧酸化合物,即其中n为1的情况,可以按“Yukagaku,Vol.32,P.118(1983)”中描述的方法合成。即式3所示的反应图示,过量的乙醇化合物与预定摩尔数的金属钠反应,然后以0.5摩尔当量金属钠的量加入一氯代乙酸,接着加热以使反应进行。反应结束后,过量的乙醇化合物通过减压蒸馏去除、加入足量的浓盐酸进行中和并通过醚等进行萃取。然后,萃取剂例如醚被减压浓缩,以及所得的浓缩物在减压下进行蒸馏,由此可获得羧酸化合物。
[式2]
(其中R1表示具有1-4个碳原子的直链或支链烷基,R2表示氢原子或甲基,m表示0-3的整数。)
[式3]
(其中R1表示具有1-4个碳原子的直链或支链烷基,R2表示氢原子或甲基,m表示0-3的整数。)
在上面式2中m为0情况下的羧酸化合物是乙氧基乙酸、丙氧基乙酸、异丙氧基乙酸、丁氧基乙酸、异丁氧基乙酸、仲-丁氧基乙酸、或叔-丁氧基乙酸。
类似地,m为1、R2为氢原子的情况下的羧酸化合物为2-(2-甲氧基乙氧基)乙酸、2-(2-乙氧基乙氧基)乙酸、2-(2-丙氧基乙氧基)乙酸、2-(2-异丙氧基乙氧基)乙酸、2-(2-丁氧基乙氧基)乙酸、2-(2-异丁氧基乙氧基)乙酸、2-(2-仲-丁氧基乙氧基)乙酸、或2-(2-叔-丁氧基乙氧基)乙酸。
类似地,m为2、R2为氢原子的情况下的羧酸化合物为2-[2-(2-甲氧基乙氧基)乙氧基]乙酸、2-[2-(2-乙氧基乙氧基)乙氧基]乙酸、2-[2-(2-丙氧基乙氧基)乙氧基]乙酸、2-[2-(2-异丙氧基乙氧基)乙氧基]乙酸、2-[2-(2-丁氧基乙氧基)乙氧基]乙酸、2-[2-(2-异丁氧基乙氧基)乙氧基]乙酸、2-[2-(2-仲-丁氧基乙氧基)乙氧基]乙酸或2-[2-(2-叔-丁氧基乙氧基)乙氧基]乙酸。
类似地,m为3、R2为氢原子的情况下的羧酸化合物为2-{2-[2-(2-甲氧基乙氧基)乙氧基]乙氧基}乙酸、2-{2-[2-(2-乙氧基乙氧基)乙氧基]乙氧基}乙酸、2-{2-[2-(2-丙氧基乙氧基)乙氧基]乙氧基}乙酸、2-{2-[2-(2-异丙氧基乙氧基)乙氧基]乙氧基}乙酸、2-{2-[2-(2-丁氧基乙氧基)乙氧基]乙氧基}乙酸、2-{2-[2-(2-异丁氧基乙氧基)乙氧基]乙氧基}乙酸、2-{2-[2-(2-仲-丁氧基乙氧基)乙氧基]乙氧基}乙酸或2-{2-[2-(2-叔-丁氧基乙氧基)乙氧基]乙氧基}乙酸。
类似地,m为1、R2为甲基的情况下的羧酸化合物为2-(2-甲氧基-1-甲基乙氧基)乙酸、2-(2-乙氧基-1-甲基乙氧基)乙酸、2-(2-丙氧基-1-甲基乙氧基)乙酸、2-(2-异丙氧基-1-甲基乙氧基)乙酸、2-(2-丁氧基-1-甲基乙氧基)乙酸、2-(2-异丁氧基-1-甲基乙氧基)乙酸、2-(2-仲-丁氧基-1-甲基乙氧基)乙酸、或2-(2-叔-丁氧基-1-甲基乙氧基)乙酸。
类似地,m为2、R2为甲基的情况下的羧酸化合物为2-[2-(2-甲氧基-1-甲基乙氧基)-1-甲基乙氧基]乙酸、2-[2-(2-乙氧基-1-甲基乙氧基)-1-甲基乙氧基]乙酸、2-[2-(2-丙氧基-1-甲基乙氧基)-1-甲基乙氧基]乙酸、2-[2-(2-异丙氧基-1-甲基乙氧基)-1-甲基乙氧基]乙酸、2-[2-(2-丁氧基-1-甲基乙氧基)-1-甲基乙氧基]乙酸、2-[2-(2-异丁氧基-1-甲基乙氧基)-1-甲基乙氧基]乙酸、2-[2-(2-仲-丁氧基-1-甲基乙氧基)-1-甲基乙氧基]乙酸或2-[2-(2-叔-丁氧基-1-甲基乙氧基)-1-甲基乙氧基]乙酸。
类似地,m为3、R2为甲基的情况下的羧酸化合物为2-{2-[2-(2-甲氧基-1-甲基乙氧基)-1-甲基乙氧基]-1-甲基乙氧基}乙酸、2-{2-[2-(2-乙氧基-1-甲基乙氧基)-1-甲基乙氧基]-1-甲基乙氧基}乙酸、2-{2-[2-(2-丙氧基-1-甲基乙氧基)-1-甲基乙氧基]-1-甲基乙氧基}乙酸、2-{2-[2-(2-异丙氧基-1-甲基乙氧基)-1-甲基乙氧基]-1-甲基乙氧基}乙酸、2-{2-[2-(2-丁氧基-1-甲基乙氧基)-1-甲基乙氧基]-1-甲基乙氧基}乙酸、2-{2-[2-(2-异丁氧基-1-甲基乙氧基)-1-甲基乙氧基]-1-甲基乙氧基}乙酸、2-{2-[2-(2-仲-丁氧基-1-甲基乙氧基)-1-甲基乙氧基]-1-甲基乙氧基}乙酸或2-{2-[2-(2-叔-丁氧基-1-甲基乙氧基)-1-甲基乙氧基]-1-甲基乙氧基}乙酸。
上面通式1所表示含4-16个碳原子的羧酸化合物中,下面的通式4所示的具有4-16个碳原子的羧酸化合物,即n为2的情况,可按“J.Am.Chem.Soc.,Vol.70,p.1333(1948)”所描述的使用氰基乙醚化合物作为起始原料的方法来合成。
氰基乙醚化合物可根据“British Patent No.544421”和“U.S.PatentNo.2280792”中描述的方法合成。
即式5中所示的反应图示中,在碱催化剂如乙醇钠存在下,使乙醇化合物与丙烯腈反应,中和之后,反应产物进行减压蒸馏以合成氰基乙醚化合物。氰基乙醚化合物在强酸如盐酸水溶液中被加热以发生反应,反应混合物被浓缩,通过过滤去除沉淀的铵盐如氯化铵,然后滤液进行减压蒸馏,由此获得羧酸化合物。
[式4]
[式5]
(其中R1表示含1-4个碳原子的直链或支链烷基,R2表示氢原子或甲基,m表示0-3的整数。)
在上式4中m为0情况下的的羧酸化合物是3-乙氧基丙酸、3-丙氧基丙酸、3-异丙氧基丙酸、3-丁氧基丙酸、3-异丁氧基丙酸、3-仲-丁氧基丙酸、或3-叔-丁氧基丙酸。
类似地,m为1、R2为氢原子的情况下,羧酸化合物为3-(2-甲氧基乙氧基)丙酸、3-(2-乙氧基乙氧基)丙酸、3-(2-丙氧基乙氧基)丙酸、3-(2-异丙氧基乙氧基)丙酸、3-(2-丁氧基乙氧基)丙酸、3-(2-异丁氧基乙氧基)丙酸、3-(2-仲-丁氧基乙氧基)丙酸、或3-(2-叔-丁氧基乙氧基)丙酸。
类似地,m为2,R2为氢原子的情况下的羧酸化合物为3-[2-(2-甲氧基乙氧基)乙氧基]丙酸、3-[2-(2-乙氧基乙氧基)乙氧基]丙酸、3-[2-(2-丙氧基乙氧基)乙氧基]丙酸、3-[2-(2-异丙氧基乙氧基)乙氧基]丙酸、3-[2-(2-丁氧基乙氧基)乙氧基]丙酸、3-[2-(2-异丁氧基乙氧基)乙氧基]丙酸、3-[2-(2-仲-丁氧基乙氧基)乙氧基]丙酸或3-[2-(2-叔-丁氧基乙氧基)乙氧基]丙酸。
类似地,m为3,R2为氢原子的情况下的羧酸化合物为3-{2-[2-(2-甲氧基乙氧基)乙氧基]乙氧基}丙酸、3-{2-[2-(2-乙氧基乙氧基)乙氧基]乙氧基}丙酸、3-{2-[2-(2-丙氧基乙氧基)乙氧基]乙氧基}丙酸、3-{2-[2-(2-异丙氧基乙氧基)乙氧基]乙氧基}丙酸、3-{2-[2-(2-丁氧基乙氧基)乙氧基]乙氧基}丙酸、3-{2-[2-(2-异丁氧基乙氧基)乙氧基]乙氧基}丙酸、3-{2-[2-(2-仲-丁氧基乙氧基)乙氧基]乙氧基}丙酸或3-{2-[2-(2-叔-丁氧基乙氧基)乙氧基]乙氧基}丙酸。
类似地,m为1,R2为甲基的情况下的羧酸化合物为3-(2-甲氧基-1-甲基乙氧基)丙酸、3-(2-乙氧基-1-甲基乙氧基)丙酸、3-(2-丙氧基-1-甲基乙氧基)丙酸、3-(2-异丙氧基-1-甲基乙氧基)丙酸、3-(2-丁氧基-1-甲基乙氧基)丙酸、3-(2-异丁氧基-1-甲基乙氧基)丙酸、3-(2-仲-丁氧基-1-甲基乙氧基)丙酸、或3-(2-叔-丁氧基-1-甲基乙氧基)丙酸。
类似地,m为2,R2为甲基的情况下的羧酸化合物为3-[2-(2-甲氧基-1-甲基乙氧基)-1-甲基乙氧基]丙酸、3-[2-(2-乙氧基-1-甲基乙氧基)-1-甲基乙氧基]丙酸、3-[2-(2-丙氧基-1-甲基乙氧基)-1-甲基乙氧基]丙酸、3-[2-(2-异丙氧基-1-甲基乙氧基)-1-甲基乙氧基]丙酸、3-[2-(2-丁氧基-1-甲基乙氧基)-1-甲基乙氧基]丙酸、3-[2-(2-异丁氧基-1-甲基乙氧基)-1-甲基乙氧基]丙酸、3-[2-(2-仲-丁氧基-1-甲基乙氧基)-1-甲基乙氧基]丙酸或3-[2-(2-叔-丁氧基-1-甲基乙氧基)-1-甲基乙氧基]丙酸。
类似地,m为3,R2为甲基的情况下的羧酸化合物为3-{2-[2-(2-甲氧基-1-甲基乙氧基)-1-甲基乙氧基]-1-甲基乙氧基}丙酸、3-{2-[2-(2-乙氧基-1-甲基乙氧基)-1-甲基乙氧基]-1-甲基乙氧基}丙酸、3-{2-[2-(2-丙氧基-1-甲基乙氧基)-1-甲基乙氧基]-1-甲基乙氧基}丙酸、3-{2-[2-(2-异丙氧基-1-甲基乙氧基)-1-甲基乙氧基]-1-甲基乙氧基}丙酸、3-{2-[2-(2-丁氧基-1-甲基乙氧基)-1-甲基乙氧基]-1-甲基乙氧基}丙酸、3-{2-[2-(2-异丁氧基-1-甲基乙氧基)-1-甲基乙氧基]-1-甲基乙氧基}丙酸、3-{2-[2-(2-仲-丁氧基-1-甲基乙氧基)-1-甲基乙氧基]-1-甲基乙氧基}丙酸或3-{2-[2-(2-叔-丁氧基-1-甲基乙氧基)-1-甲基乙氧基]-1-甲基乙氧基}丙酸。
这些羧酸化合物可以0.1-50wt.%、优选1-30wt.%的比例存在于水溶性预焊剂中。当所含的羧酸化合物比例小于0.1wt.%,咪唑化合物无法充分被增溶。当所含的羧酸化合物比例大于50wt.%,羧酸的助剂成本增加,因此这种情况不可取。
在实施本发明过程中,公知的有机酸、无机酸或有机溶剂可与羧酸化合物组合用作增溶剂。
可用的有机酸的典型实例包括甲酸、乙酸、丙酸、丁酸、乙醛酸、丙酮酸、乙酰乙酸、乙酰丙酸、庚酸、辛酸、癸酸、月桂酸、乙醇酸、甘油酸、乳酸、丙烯酸、苯甲酸、对硝基苯甲酸、对甲基苯磺酸、水杨酸、苦味酸、草酸、琥珀酸、马来酸、富马酸、酒石酸和己二酸;无机酸的实例包括盐酸、磷酸、硫酸和硝酸。
还有作为有机溶剂,可提及低碳醇例如,甲醇、乙醇和异丙醇;或丙酮、N,N-二甲基甲酰胺、乙二醇等,可与水任意混合。
对于本发明中的水溶性预焊剂而言,可加入铜化合物以加速金属导电部件表面化学层的形成速率,可加入锌化合物以进一步增强所形成化学层的耐热性。
上述铜化合物的典型实例包括,乙酸铜、氯化亚铜、氯化铜、溴化亚铜、溴化铜、碘化铜、氢氧化铜、磷酸铜、硫酸铜和硝酸铜,等;锌化合物典型实例包括氧化锌、甲酸锌、乙酸锌、草酸锌、乳酸锌、柠檬酸锌、硫酸锌、硝酸锌、磷酸锌,等。金属化合物中任一种可按0.01wt.%-10wt.%,优选0.02wt.%-5wt.%的比例加入水溶性预焊剂中。
在使用这些铜化合物或锌化合物的情况下,优选通过将具有缓冲作用的物质如氨,或胺如单乙醇胺、二乙醇胺或三乙醇胺加到水溶性预焊剂中从而稳定水溶性预焊剂的pH值。
为了进一步增强化学层的形成速率和该层的耐热性,可按0.001wt.%-1wt.%,优选0.01wt.%-0.5wt.%的比例将卤素类化合物加入到本发明的水溶性预焊剂中。卤素类化合物的实例包括氟化钠、氟化钾、氟化铵、氯化钠、氯化钾、氯化铵、溴化钠、溴化钾、溴化铵、碘化钠、碘化钾和碘化铵。
至于使用本发明中的水溶性预焊剂处理印刷线路板金属导电部件表面的条件,水溶性预焊剂的液体温度优选10-70℃,接触时间优选1秒-10分钟。接触方法可提及浸渍、喷溅、涂布等方法。
根据本发明所述的方法对表面进行整理之后,也可通过用热塑性树脂在化学层上形成双层结构以进一步增强耐热性。
即,在金属导电层表面形成化学层之后,化学层和热塑性树脂的双层结构可通过将具有优良耐热性的热塑性树脂溶解在溶剂如甲苯、乙酸乙酯或异丙醇中,并利用辊涂机或类似设备将该溶液均匀涂敷在化学层上达到1-30μm的厚度来制成的,所述热塑性树脂可由松香衍生物如松香或松香酯、萜烯树脂衍生物如萜烯树脂或萜烯酚树脂、烃类树脂如芳香烃树脂、脂肪烃树脂或它们的混合物组成。
本发明的焊接方法可适合流体焊接方法,其包括在焊料浴中熔融的液态焊料上移动印刷线路板以焊接电子部件和印刷线路板之间的接点;和回流焊接方法,其包括根据电路图事先在印刷线路板上印有膏状焊料,将电子部件贴装其上,并加热整个印刷线路板以熔化焊料来完成焊接。
根据本发明适合焊接的焊料可提及,不仅包括通常使用的锡-铅合金共熔焊料,也可使用无铅焊料例如Sn-Ag-Cu基、Sn-Ag-Bi基、Sn-Bi基、Sn-Ag-Bi-In基、Sn-Zn基和Zn-Cu基焊料。
实施例
下文将参考实施例和对比例来具体描述该发明,但不应解释为发明受限于这些内容。
顺便提及,实施例和对比例中使用的咪唑化合物、羧酸化合物和评价方法如下:
[咪唑化合物]
2-十一烷基咪唑(商品名:C11Z,Shikoku Chemicals Corporation制造)
2-苯基咪唑(商品名:2PZ,Shikoku Chemicals Corporation制造)
2-苯基-4-甲基咪唑(商品名:2P4MZ,Shikoku ChemicalsCorporation制造)
2-苯基-4-(3,4-二氯苯基)咪唑(根据JP-A-2005-104878中所描述的方法合成)
2-苯基-4-(2-萘基)-5-甲基咪唑(根据对比例1中所述的方法合成)
2-苯基-4-(2-萘基)咪唑(根据对比例2中所述的方法合成)
2-苄基-4-甲基咪唑(Poly Organix制造)
2-壬基苯并咪唑(试剂,SIGMA-ALDRICH制造)
2-(4-氯苯甲基)苯并咪唑(根据Science of Synthesis,12卷,529页(2002年)中所描述的方法合成)
2-(1-萘基)甲苯并咪唑(根据Biochemical Pharmacology,36卷,463页(1987年)所描述的方法合成)
对比例1
(2-苯基-4-(2-萘基)-5-甲基咪唑的合成方法)
苯甲脒盐酸盐和等摩尔量的甲醇钠在四氢呋喃中回流加热1小时。冷却后,在其中滴加等摩尔量的2-溴-2’-丙酰萘的四氢呋喃溶液,以使温度不超过30℃,然后再加入等摩尔量的甲醇钠,随后回流加热1小时。减压蒸馏去除溶剂之后,剩余物用水清洗并且由乙腈进行再结晶以获得灰蓝色晶体。
对比例2
(2-苯基-4-(2-萘基)咪唑的合成方法)
苯甲脒盐酸盐和等摩尔量的甲醇钠在四氢呋喃中回流加热1小时。冷却后,在其中滴加等摩尔量的ω-溴-2-萘乙酮以使温度不超过30℃,然后再加入等摩尔量的甲醇钠,而后回流加热1小时。减压蒸馏去除溶剂之后,剩余物用水清洗并且由乙腈进行再结晶以获得灰蓝色晶体。
(羧酸化合物)
2-乙氧基乙酸(试剂,SIGMA-ALDRICH制造,简称化合物A)
2-(2-甲氧基乙氧基)乙酸(简称化合物B)
2-[2-(2-乙氧基乙氧基)乙氧基]乙酸(简称化合物C)
2-{2-[2-(2-乙氧基乙氧基)乙氧基]乙氧基}乙酸(简称化合物D)
2-(2-甲氧基-1-甲基乙氧基)乙酸(简称化合物E)
2-[2-(2-丙氧基-1-甲基乙氧基)-1-甲基乙氧基]乙酸(简称化合物F)
2-{2-[2-(2-丁氧基-1-甲基乙氧基)-1-甲基乙氧基]-1-甲基乙氧基}乙酸(简称化合物G)
3-乙氧基丙酸(简称化合物H)
3-(2-甲氧基乙氧基)丙酸(简称化合物I)
3-(2-甲氧基-1-甲基乙氧基)丙酸(简称化合物J)
3-[2-(2-甲氧基乙氧基)乙氧基]丙酸(简称化合物K)
3-{2-[2-(2-乙氧基乙氧基)乙氧基]乙氧基}丙酸(简称化合物L)
化合物B到G根据“Yukagaku,32卷,118页(1983年)”描述的方法合成。
化合物H到L根据“J.Am.Chem.Soc.,70卷,1333页(1948年)”和“British Patent No.544421”和/或“U.S.Patent No.2280792”中描述的方法合成。
在这点上,化合物A到L的结构式列于表1中。
[表1]
对比例3
(咪唑化合物增溶性测试)
为用于本发明,将0.20克2-苯基-(3,4-二氯苯基)咪唑溶解于2.0g羧酸化合物中之后,当加入离子交换水时,测量直到溶液变浑浊时所需水量。水量较大时则判断羧酸化合物对咪唑化合物溶解性更加优良。
所得到的测试结果列于表2-表4。认为通过亚烷基醚链(-CH2CH(R2)-O-)将烷氧基(R1-O-)与羧甲基(-CH2COOH)或羧乙基(-C2H4COOH)结合在一起的化学结构增强了咪唑化合物溶解性能。
[表2]
羧酸化合物 | 加入水量(ml) |
2-乙氧基乙酸 | 3.3 |
化合物C | 3.6 |
[表3]
羧酸化合物 | 加入水量(ml) |
2-(n-丙氧基)乙酸 | 2.8 |
化合物F | 3.0 |
[表4]
羧酸化合物 | 加入水量(ml) |
2-(n-丁氧基)乙酸 | 1.0 |
化合物G | 2.0 |
(焊料流动性测评)
由120mm(长)×150mm(宽)×1.6mm(厚)的玻璃环氧树脂制成并带有300个内径为0.80mm的铜通孔的印刷线路板作为测试件。该测试件经脱脂,并经受微蚀刻,然后水洗。其后,测试件浸泡在规定液体温度的水溶性预焊剂中保持规定时间,水洗,然后干燥以在铜表面形成厚度为约0.10-0.50μm的化学层。
使用红外线回流装置(商品名:MULTI-PRO-306,Vetronix Co.,Ltd.制造),对表面处理过的测试件在最高温度为240℃下进行三个周期回流-加热,随后使用流体焊接装置进行焊接(传输速度:1.0m/min)。
所采用焊料为锡-铅共熔焊料,其组成为63%锡和37%铅(wt.%)(商品名:H63A,Senju Metal Industry Co.,Ltd.制造),用于焊接的助熔剂为JS-64MSS(Koki Co.,Ltd.制造)。焊接温度为240℃。
上面处理后的测试件表面也可采用无铅焊料以与锡-铅共熔焊料情况相同的方式进行焊接。所采用的焊料为无铅焊料(商品名:H705“ECOSOLCER”,Senju Metal Industry Co.,Ltd.制造),其组成为锡96.5%、银3.0%和铜0.5%(wt.%)。用于焊接的助熔剂为JS-E-09(KokiCo.,Ltd.制造)。回流-加热最高温度为245℃,焊接温度也是245℃。
对于焊接测试件而言,对焊料充满到铜通孔上部区域(upper land)的通孔数量进行计算,并计算其相对于铜通孔(300孔)总量的比例。
焊料在铜表面可湿性能大时,熔融焊料可穿入铜通孔内部,并很容易将焊料填充到通孔的上部区域。即,当其上部区域被焊接的通孔的数量较大时,焊料对铜的润湿性可被认为优良,以及对其焊接性能也被认良好。
(焊料可铺展性测评)
由50mm(长)×50mm(宽)×1.2mm(厚)的玻璃环氧树脂制成的印刷线路板作为测试件。该印刷线路板具有这样的电路布局,其中以1.0mm的间距在宽度方向形成10片宽0.80mm、长20mm铜箔片电路。此测试件脱脂后,经受微蚀刻,然后水洗。其后,测试件被浸泡在规定液体温度的水溶性预焊剂中保持规定时间,水洗,然后干燥以在铜表面形成厚度为约0.10-0.50μm的化学层。
使用红外线回流装置(商品名:MULTI-PRO-306,由VetronixCo.,Ltd.制造),对表面处理过的测试件在最高温度为240℃下进行一个周期的回流-加热。其后使用具有1.2mm孔径和150mm厚度的金属模版,将锡-铅焊膏印在铜电路的中心,并且按上述条件回流-加热以进行焊接。所使用的锡-铅焊膏是由63%锡和37%铅(wt.%)组成的共熔焊料(商品名:OZ-63-330F-40-10,Senju Metal Industry Co.,Ltd.制造)。
如上处理后的测试件表面也可采用无铅焊料以与锡-铅共熔焊料情况相同的方式进行焊接。所采用的无铅焊膏,由锡96.5%、银3.0%和铜0.5%(wt.%)组成(商品名:H705-221BM5-42-11,Senju MetalIndustry Co.,Ltd.制造)。焊膏印刷前后所达到的最高回流-加热温度设定为245℃。
对润湿和铺展在所得到的测试件铜电路表面上的焊料长度(mm)进行测试。
当长度较长时,焊料对铜的润湿性能可认为优良,对其可焊接性被认为良好。
实施例1
作为咪唑化合物的2-十一烷基咪唑、作为增溶剂的乙氧基乙酸、作为金属盐的乙酸铜、和作为卤素化合物的氯化铵溶解于离子交换水中以获得表5所述组分,溶液分别且依次用氨水调整到pH为3.7,由此制成水溶性预焊剂。
然后,将印刷线路板的测试件浸到温度控制在40℃的水溶性预焊剂里。之后,对测试件进行清洗和干燥,测定焊料流动性和焊料可铺展性能。这些测试结果列于表5中。
实施例2到16
每种具有如表5中所述组分的水溶性预焊剂以与实施例1相同方式制备,并且按照表5所述的处理条件对其进行表面处理。然后,进行测评。所得测试结果列于表5中。
对比例1到11
每种具有如表6所述组成的水溶性预焊剂以与实施例1相同方式制备,并且按照表6所述的处理条件对其进行表面处理。然后,进行测评。所得测试结果列于表6中。
根据表5、6中所示的测试结果,认为使用包含化合物A到L中的每一种作为增溶剂的水溶性预焊剂进行表面处理,然后使用共熔焊料或无铅焊料进行焊接的情况下,焊料流动性和焊料可铺展性与使用甲酸或乙酸作为增溶剂的情况相比得到显著改善,而不管咪唑化合物的种类。
附带提及,实施例中制备的水溶性预焊剂无气味而对比例中的水溶性预焊剂有典型的甲酸或乙酸挥发导致的刺激性气味。
虽然对本发明是参考其具体实施例进行了详细描述,但在未脱离本发明目的和范围下可对其进行各种变化和修正这一点,对本领域技术人员是清楚明显的。
本申请是基于申请日为2005年5月24日申请号为2005-150279的日本专利申请和申请日为2005年12月9日申请号为2005-355985的日本专利申请,上述内容在此引入以供参考。
工业应用
由于本发明的水溶性预焊剂包含低挥发性羧酸化合物作为咪唑化合物的增溶剂,可以稳定保持水溶性预焊剂中增溶剂浓度而且没有难闻的气味产生。此外,与甲酸或乙酸作为增溶剂的情况比较,也可使咪唑化合物具有优良的成膜性能。
根据本发明的表面处理方法,在金属导电部件的表面上可形成化学层并因此可避免金属导电部件表面的氧化。
当使用本发明的印刷线路板时,金属导电部件表面和电子部件之间的接合可通过焊接安全进行。
根据本发明的焊接方法,可避免金属导电部件表面的氧化,并因此得到良好的可焊接性能。
Claims (5)
2.根据权利要求1所述的水溶性预焊剂,其包含比例为0.01-10wt.%的咪唑化合物和比例为0.1-50wt.%的羧酸化合物。
3.一种金属导电部件的表面处理方法,其包括将所述金属导电部件表面与根据权利要求1或2所述的水溶性预焊剂进行接触。
4.一种印刷线路板,其中金属导电部件所述表面已与根据权利要求1或2所述的水溶性预焊剂进行了接触。
5.一种焊接方法,其包括使金属导电部件所述表面与根据权利要求1或2所述的水溶性预焊剂进行接触和然后进行焊接。
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JP2005355985A JP4883996B2 (ja) | 2005-05-24 | 2005-12-09 | 水溶性プレフラックス及びその利用 |
JP355985/2005 | 2005-12-09 | ||
PCT/JP2006/310271 WO2006126551A1 (ja) | 2005-05-24 | 2006-05-23 | 水溶性プレフラックス及びその利用 |
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JP5301218B2 (ja) * | 2008-08-25 | 2013-09-25 | 四国化成工業株式会社 | 銅または銅合金の表面処理剤及びその利用 |
US8263177B2 (en) * | 2009-03-27 | 2012-09-11 | Kesheng Feng | Organic polymer coating for protection against creep corrosion |
EP2440024B1 (en) * | 2009-06-01 | 2014-03-12 | Sumitomo Electric Industries, Ltd. | Connection method |
JP5457814B2 (ja) * | 2009-12-17 | 2014-04-02 | コーア株式会社 | 電子部品の実装構造 |
CN102766874A (zh) * | 2012-08-20 | 2012-11-07 | 合肥奥福表面处理科技有限公司 | Osp铜面保护剂 |
EP3075735B1 (en) * | 2013-11-25 | 2020-09-23 | Shikoku Chemicals Corporation | Glycolurils having functional group and use thereof |
CN104470202B (zh) * | 2014-12-31 | 2017-10-24 | 上海创功通讯技术有限公司 | 用于移动终端的印刷电路板及其焊盘表面处理方法 |
US11021430B2 (en) | 2016-04-05 | 2021-06-01 | Moresco Corporation | Oxa acid compound |
CN109843293A (zh) * | 2016-08-26 | 2019-06-04 | 百时美施贵宝公司 | 吲哚胺2,3-双加氧酶的抑制剂及其使用方法 |
JP7053247B2 (ja) * | 2017-12-21 | 2022-04-12 | 東京応化工業株式会社 | 表面処理液、表面処理方法、及びパターン倒れの抑制方法 |
JP6916731B2 (ja) | 2017-12-28 | 2021-08-11 | 東京応化工業株式会社 | 基板の撥水化方法、表面処理剤、及び基板表面を洗浄液により洗浄する際の有機パターン又は無機パターンの倒れを抑制する方法 |
CN114932335B (zh) * | 2022-05-13 | 2024-03-26 | 深圳市荣昌科技有限公司 | 一种大功率led封装用水溶性固晶锡膏及其制备方法 |
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