CN116714325B - 一种ic封装用高可靠性无卤覆铜板及其制备方法 - Google Patents
一种ic封装用高可靠性无卤覆铜板及其制备方法 Download PDFInfo
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- CN116714325B CN116714325B CN202310694657.1A CN202310694657A CN116714325B CN 116714325 B CN116714325 B CN 116714325B CN 202310694657 A CN202310694657 A CN 202310694657A CN 116714325 B CN116714325 B CN 116714325B
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- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims abstract description 49
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Abstract
本发明涉及无卤覆铜板领域,公开了一种IC封装用高可靠性无卤覆铜板及其制备方法。本发明中,采用巯基改性的三聚氰胺甲醛树脂溶液做壁材包覆红磷,获得稳定性强的阻燃固化剂;以碳酸乙烯亚乙酯与聚醚胺为原料制备一种增韧固化剂,两种固化剂优化互补,有效缓解因高分子材料与阻燃剂相容性差而导致的力学性能下降的问题;同时,在升温固化后进行光固化,光固化过程中的巯基‑乙烯基反应可以帮助降低自由基聚合过程中的氧阻聚,有效降低固化应力;通过该方法可制得一种阻燃性能好、韧性好的IC封装用高可靠性无卤覆铜板。
Description
技术领域
本发明涉及无卤覆铜板领域,公开了一种IC封装用高可靠性无卤覆铜板及其制备方法。
背景技术
电子技术随时代快速发展,在追求发展迅速的同时也追求安全环保,IC封装是集成电路芯片生产完成后必不可少的工序之一,这一环节对产品的质量影响极大。
在IC封装用覆铜板的制备标准中,耐热性能和阻燃性能为重要性能指标;传统覆铜板采用含卤阻燃剂,但由于卤系阻燃剂在燃烧时会释放有害物质,会对人员安全和环境造成危害,已逐渐被替代。
现有技术常用无机阻燃剂或磷系阻燃剂代替传统的含卤阻燃剂,然而,该类物质与高分子材料相容性差,添加后会造成材料韧性下降,使得现有无卤覆铜板力学性能差,同时,升温固化过程中产生的固化应力也会导致产品力学性能下降;因此,需研究一种阻燃性能好且韧性强的IC封装用高可靠性无卤覆铜板。
发明内容
本发明的目的在于提供一种IC封装用高可靠性无卤覆铜板及其制备方法,以解决上述背景技术中提出的问题。
为了解决上述技术问题,本发明提供如下技术方案:
一种IC封装用高可靠性无卤覆铜板的制备方法:所述IC封装用高可靠性无卤覆铜板的制备过程包括以下步骤:
S1:将基础环氧树脂、光敏性环氧树脂、阻燃固化剂、增韧固化剂、氢氧化铝、咪唑、光引发剂,混合均匀,得到胶液;
S2:将胶液涂覆于玻璃纤维织物,干燥,光固化,得到固化片;
S3:将两张固化片堆叠在一起,放置于两张铜箔之间,热压,得到IC封装用高可靠性无卤覆铜板。
较为优化地,所述胶液包括以下原料:按重量份数计,70~80份基础环氧树脂、20~30份光敏性环氧树脂、25~34份阻燃固化剂、14~20份增韧固化剂、1~5份氢氧化铝、0.5~1份咪唑、0.1~0.5份光引发剂。
较为优化地,所述阻燃固化剂的制备方法:(1)将三聚氰胺溶液在1~2h滴加入4-巯基苯甲醛溶液,加入冰乙酸,搅拌1~2h,调节反应液pH至6.5~7.5,除去溶剂,得到三聚氰胺预聚体,将其使用去离子水稀释,得到巯基改性三聚氰胺甲醛树脂溶液;(2)在乳化剂溶液中加入红磷粉末,剪切乳化10~15min,在0.5~1h滴入巯基改性三聚氰胺甲醛树脂溶液,剪切乳化2~5min,将温度升至60~80℃,以600~800r/min的速度搅拌2~3h,得到阻燃固化剂。
较为优化地,所述阻燃固化剂包括以下原料:按重量份数计,乳化剂18~25份、红磷粉末8~12份、巯基改性三聚氰胺甲醛树脂溶液8~20份;其中,所述巯基改性三聚氰胺甲醛树脂溶液包括以下原料:按重量份数计,三聚氰胺20~30份、溶剂350~500份、4-巯基苯甲醛50~70份、冰乙酸0.5~2份、去离子水8~15份。
较为优化地,所述增韧固化剂为聚醚胺,所述光敏性环氧树脂为环氧树脂621A-80,所述基础环氧树脂为环氧树脂6101,所述光引发剂为邻苯甲酰苯甲酸甲酯。
较为优化地,所述增韧固化剂是碳酸乙烯亚乙酯改性聚醚胺。
较为优化地,碳酸乙烯亚乙酯改性聚醚胺工艺为:保持温度为60~70℃,在0.5~1h,将碳酸乙烯亚乙酯滴加到聚醚胺,依次进行保温、抽真空、反应,加入硅烷偶联剂,升温至80~95℃,反应30~40min,降温,得到增韧固化剂。
较为优化地,所述增韧固化剂包括以下原料:按重量份数计,碳酸乙烯亚乙酯6~15份、聚醚胺20~30份、硅烷偶联剂0.5~2份。
较为优化地,所述紫外光照射条件为:波长为365nm,样品处紫外光强为45~55mw/cm2,辐照距离为8~15cm;热压压制的压力为20~40kg/cm2,温度为150~180℃,压制的时间为80~100min;涂覆设备为上胶机,涂覆的车速为17~25m/min,涂胶量为160~200g/m2。
较为优化的,所述玻璃纤维织物厚度为0.3mm。
与现有技术相比,本发明所达到的有益效果是:
(1)用4-巯基苯甲醛改性三聚氰胺,通过醛胺缩合反应得到巯基改性三聚氰胺甲醛树脂,既可做壁材包覆红磷,获得一种阻燃性能好、稳定性强、具有固化效果的阻燃固化剂,又可以与后续工艺制备的增韧固化剂中的乙烯基反应,巯基与乙烯基在紫外光照下发生加成反应,可使固化应力降低,产品韧性提升;
(2)以碳酸乙烯亚乙酯与聚醚胺开环反应制备一种增韧固化剂,该固化剂不仅能进一步改进优化环氧树脂的性能,其中乙烯基还能与上述阻燃固化剂中的巯基反应,两种固化剂优化互补,有效缓解因高分子材料与阻燃剂相容性差导致力学性能下降的问题;
(3)本发明的主要原料按质量份为:70~80份基础环氧树脂、20~30份光敏性环氧树脂、25~34份阻燃固化剂、14~20份增韧固化剂,按3:1的比例混合使用基础环氧树脂与光敏性环氧树脂,按2:1的比例使用阻燃固化剂与增韧固化剂,可以获得一种阻燃性能好、韧性好、IC封装用的高可靠性无卤覆铜板。如果改变原料用量,均会在不同程度上导致产品的阻燃性能或韧性下降,本发明中所述比例可使所得覆铜板综合性能最好;
(4)制备工艺中,先进行升温固化后进行光固化;紫外光照过程,阻燃固化剂中的巯基与增韧固化剂中的乙烯基发生反应,降低自由基聚合过程中的氧阻聚,有效降低产生的固化应力。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
IC封装用高可靠性无卤覆铜板的制备过程包括以下化学品:三聚氰胺CAS:108-78-1;N,N-二甲基甲酰胺(DMF)CAS:68-12-2;4-巯基苯甲醛CAS:91358-96-2;冰乙酸CAS:64-19-7;氢氧化钠CAS:1310-73-2;乳化剂SMA-520(CAS:9011-13-6,武汉海山科技有限公司,含固量25%);红磷CAS:7723-14-0;碳酸乙烯亚乙酯CAS:4427-96-7;聚醚胺D-230(CAS:9046-10-0,上海方野化工有限公司,AHEW:~61g/eq);光敏性环氧树脂(型号:621A-80,有鸣化学有限公司);基础环氧树脂(型号6101,环氧当量:210-244g/eq,南京百慕达生物科技有限公司);邻苯甲酰苯甲酸甲酯CAS:606-28-0;氢氧化铝CAS:21645-51-2;咪唑(CAS:288-32-4,湖北鑫红利化工有限公司);间苯二甲胺(CAS:1477-55-0,特斯科化工有限公司);水性三聚氰胺甲醛树脂(型号:CYMEL385,杭州力帮电子商务有限公司,不挥发物79±2%);
以下份数为质量份;
实施例1:S1:取25份三聚氰胺溶于130份N,N-二甲基甲酰胺,70℃搅拌加热至溶解,在2h滴加入称取60份4-巯基苯甲醛和250份N,N-二甲基甲酰胺的混合液中,加入1份冰乙酸,搅拌1h,随后用NaOH溶液调节反应液pH至7,旋蒸除去N,N-二甲基甲酰胺,加入10份水,得到巯基改性三聚氰胺甲醛树脂溶液;
S2:在20份乳化剂SMA-520中加入10份红磷粉末,用剪切机以10000r/min的速度剪切10min,在0.5h滴入10份巯基改性三聚氰胺甲醛树脂溶液,以10000r/min的速度剪切乳化2min,将温度升至70℃,以600r/min的速度搅拌3h,得到阻燃固化剂;
S3:保持温度为70℃,耗费0.5h将12份碳酸乙烯亚乙酯滴加入25份聚醚胺,保温3h,抽真空,真空度≤-0.08MPa并保持温度70℃,1h后停真空,加入1份KH550,升温至95℃,反应30min,降温至60℃后,得到增韧固化剂;
S4:取75份环氧树脂621A-80、25份环氧树脂6101、32份阻燃固化剂、16份增韧固化剂、2份氢氧化铝、0.5份咪唑、0.1份光引发剂邻苯甲酰苯甲酸甲酯,混合均匀,得到胶液;
S5:保持涂覆的车速为20m/min,涂胶量为180g/m2,将胶液涂覆于玻璃纤维织物,120℃下烘干4h;置于波长为365nm的紫外光下照射2h,样品处紫外光强为50mw/cm2,辐照距离为10cm,得到固化膜;
S6:将两张固化膜堆叠在一起,放置两张铜箔之间,置于真空热压机中热压,热压压制的压力为30kg/cm2,温度为160℃,压制的时间为90min,得到IC封装用高可靠性无卤覆铜板。
实施例2:S1:取25份三聚氰胺溶于130份N,N-二甲基甲酰胺,70℃搅拌加热至溶解,在2h滴加入称取60份4-巯基苯甲醛和250份N,N-二甲基甲酰胺的混合液中,加入1份冰乙酸,搅拌1h,随后用NaOH溶液调节反应液pH至7,旋蒸除去N,N-二甲基甲酰胺,加入10份水,得到巯基改性三聚氰胺甲醛树脂溶液;
S2:在20份乳化剂SMA-520中加入10份红磷粉末,用剪切机以10000r/min的速度剪切10min,在0.5h滴入10份巯基改性三聚氰胺甲醛树脂溶液,以10000r/min的速度剪切乳化2min,将温度升至70℃,以600r/min的速度搅拌3h,得到阻燃固化剂;
S3:保持温度为70℃,耗费0.5h将12份碳酸乙烯亚乙酯滴加进25份聚醚胺,保温3h,抽真空,真空度≤-0.08MPa并保持温度70℃,1h后停真空,加入1份KH550,升温至95℃,反应30min,降温至60℃后,得到增韧固化剂;
S4:取80份环氧树脂621A-80、20份环氧树脂6101、34份阻燃固化剂、14份增韧固化剂、2份氢氧化铝、0.5份咪唑、0.1份光引发剂邻苯甲酰苯甲酸甲酯,混合均匀,得到胶液;
S5:保持涂覆的车速为20m/min,涂胶量为180g/m2,将胶液涂覆于玻璃纤维织物,120℃下烘干4h;置于波长为365nm的紫外光下照射2h,样品处紫外光强为50mw/cm2,辐照距离为10cm,得到固化膜;
S6:将两张固化膜堆叠在一起,放置两张铜箔之间,置于真空热压机中热压,热压压制的压力为30kg/cm2,温度为160℃,压制的时间为90min,得到IC封装用高可靠性无卤覆铜板。
实施例3:S1:取25份三聚氰胺溶于130份N,N-二甲基甲酰胺,70℃搅拌加热至溶解,在2h滴加入称取60份4-巯基苯甲醛和250份N,N-二甲基甲酰胺的混合液中,加入1份冰乙酸,搅拌1h,随后用NaOH溶液调节反应液pH至7,旋蒸除去N,N-二甲基甲酰胺,加入10份水,得到巯基改性三聚氰胺甲醛树脂溶液;
S2:在20份乳化剂SMA-520中加入10份红磷粉末,用剪切机以10000r/min的速度剪切10min,在0.5h滴入10份巯基改性三聚氰胺甲醛树脂溶液,以10000r/min的速度剪切乳化2min,将温度升至70℃,以600r/min的速度搅拌3h,得到阻燃固化剂;
S3:保持温度为70℃,耗费0.5h将12份碳酸乙烯亚乙酯滴加进25份聚醚胺,保温3h,抽真空,真空度≤-0.08MPa并保持温度70℃,1h后停真空,加入1份KH550,升温至95℃,反应30min,降温至60℃后,得到增韧固化剂;
S4:取70份环氧树脂621A-80、30份环氧树脂6101、25份阻燃固化剂、20份增韧固化剂、2份氢氧化铝、0.5份咪唑、0.1份光引发剂邻苯甲酰苯甲酸甲酯,混合均匀,得到胶液;
S5:保持涂覆的车速为20m/min,涂胶量为180g/m2,将胶液涂覆于玻璃纤维织物,120℃下烘干4h;置于波长为365nm的紫外光下照射2h,样品处紫外光强为50mw/cm2,辐照距离为10cm,得到固化膜;
S6:将两张固化膜堆叠在一起,放置两张铜箔之间,置于真空热压机中热压,热压压制的压力为30kg/cm2,温度为160℃,压制的时间为90min,得到IC封装用高可靠性无卤覆铜板。
对比例1:(不对红磷进行包覆处理,其他方法步骤与实施例1一致)S1:保持温度为70℃,耗费0.5h将12份碳酸乙烯亚乙酯滴加进25份聚醚胺,保温3h,抽真空,真空度≤-0.08MPa并保持温度70℃,1h后停真空,加入1份KH550,升温至95℃,反应30min,降温至60℃后,得到增韧固化剂;
S2:取75份环氧树脂621A-80、25份环氧树脂6101、10份红磷、16份增韧固化剂、2份氢氧化铝、0.5份咪唑、0.1份光引发剂邻苯甲酰苯甲酸甲酯,混合均匀,得到胶液;
S3:保持涂覆的车速为20m/min,涂胶量为180g/m2,将胶液涂覆于玻璃纤维织物,120℃下烘干4h;置于波长为365nm的紫外光下照射2h,样品处紫外光强为50mw/cm2,辐照距离为10cm,得到固化膜;
S4:将两张固化膜堆叠在一起,放置两张铜箔之间,置于真空热压机中热压,热压压制的压力为30kg/cm2,温度为160℃,压制的时间为90min,得到IC封装用高可靠性无卤覆铜板。
对比例2:(将增韧固化剂替换为普通固化剂,其他方法步骤与实施例1一致)S1:取25份三聚氰胺溶于130份N,N-二甲基甲酰胺,70℃搅拌加热至溶解,在2h滴加入称取60份4-巯基苯甲醛和250份N,N-二甲基甲酰胺的混合液中,加入1份冰乙酸,搅拌1h,随后用NaOH溶液调节反应液pH至7,旋蒸除去N,N-二甲基甲酰胺,加入10份水,得到巯基改性三聚氰胺甲醛树脂溶液;
S2:在20份乳化剂SMA-520中加入10份红磷粉末,用剪切机以10000r/min的速度剪切10min,在0.5h滴入10份巯基改性三聚氰胺甲醛树脂溶液,以10000r/min的速度剪切乳化2min,将温度升至70℃,以600r/min的速度搅拌3h,得到阻燃固化剂;
S3:取75份环氧树脂621A-80、25份环氧树脂6101、32份阻燃固化剂、16份间苯二甲胺、2份氢氧化铝、0.5份咪唑、0.1份光引发剂邻苯甲酰苯甲酸甲酯,混合均匀,得到胶液;
S5:保持涂覆的车速为20m/min,涂胶量为180g/m2,将胶液涂覆于玻璃纤维织物,120℃下烘干4h;置于波长为365nm的紫外光下照射2h,样品处紫外光强为50mw/cm2,辐照距离为10cm,得到固化膜;
S6:将两张固化膜堆叠在一起,放置两张铜箔之间,置于真空热压机中热压,热压压制的压力为30kg/cm2,温度为160℃,压制的时间为90min,得到IC封装用高可靠性无卤覆铜板。
对比例3:(使用未经巯基改性的三聚氰胺甲醛树脂做壁材包覆红磷,其他方法步骤与实施例1一致)S1:在20份乳化剂SMA-520中加入10份红磷粉末,用剪切机以10000r/min的速度剪切10min,在0.5h滴入10份三聚氰胺甲醛树脂溶液,以10000r/min的速度剪切乳化2min,将温度升至70℃,以600r/min的速度搅拌3h,得到阻燃固化剂;
S2:保持温度为70℃,耗费0.5h将12份碳酸乙烯亚乙酯滴加进25份聚醚胺,保温3h,抽真空,真空度≤-0.08MPa并保持温度70℃,1h后停真空,加入1份KH550,升温至95℃,反应30min,降温至60℃后,得到增韧固化剂;
S3:取75份环氧树脂621A-80、25份环氧树脂6101、32份阻燃固化剂、16份增韧固化剂、2份氢氧化铝、0.5份咪唑、0.1份光引发剂邻苯甲酰苯甲酸甲酯,混合均匀,得到胶液;
S4:保持涂覆的车速为20m/min,涂胶量为180g/m2,将胶液涂覆于玻璃纤维织物,120℃下烘干4h;置于波长为365nm的紫外光下照射2h,样品处紫外光强为50mw/cm2,辐照距离为10cm,得到固化膜;
S5:将两张固化膜堆叠在一起,放置两张铜箔之间,置于真空热压机中热压,热压压制的压力为30kg/cm2,温度为160℃,压制的时间为90min,得到IC封装用高可靠性无卤覆铜板。
对比例4:(调换固化顺序,先进行光固化再进行升温固化,其他步骤与实施例1一致)S1:取25份三聚氰胺溶于130份N,N-二甲基甲酰胺,70℃搅拌加热至溶解,在2h滴加入称取60份4-巯基苯甲醛和250份N,N-二甲基甲酰胺的混合液中,加入1份冰乙酸,搅拌1h,随后用NaOH溶液调节反应液pH至7,旋蒸除去N,N-二甲基甲酰胺,加入10份水,得到巯基改性三聚氰胺甲醛树脂溶液;
S2:在20份乳化剂SMA-520中加入10份红磷粉末,用剪切机以10000r/min的速度剪切10min,在0.5h滴入10份巯基改性三聚氰胺甲醛树脂溶液,以10000r/min的速度剪切乳化2min,将温度升至70℃,以600r/min的速度搅拌3h,得到阻燃固化剂;
S3:保持温度为70℃,耗费0.5h将12份碳酸乙烯亚乙酯滴加进25份聚醚胺,保温3h,抽真空,真空度≤-0.08MPa并保持温度70℃,1h后停真空,加入1份KH550,升温至95℃,反应30min,降温至60℃后,得到增韧固化剂;
S4:取75份环氧树脂621A-80、25份环氧树脂6101、32份阻燃固化剂、16份增韧固化剂、2份氢氧化铝、0.5份咪唑、0.1份光引发剂邻苯甲酰苯甲酸甲酯,混合均匀,得到胶液;
S5:置于波长为365nm的紫外光下照射2h,样品处紫外光强为50mw/cm2,辐照距离为10cm;保持涂覆的车速为20m/min,涂胶量为180g/m2,将胶液涂覆于玻璃纤维织物,120℃下烘干4h;得到固化膜;
S6:将两张固化膜堆叠在一起,放置两张铜箔之间,置于真空热压机中热压,热压压制的压力为30kg/cm2,温度为160℃,压制的时间为90min,得到IC封装用高可靠性无卤覆铜板。
对比例5(将阻燃固化剂与增韧固化剂的比例改为1:2,其他方法步骤与实施例1一致):S1:取25份三聚氰胺溶于130份N,N-二甲基甲酰胺,70℃搅拌加热至溶解,在2h滴加入称取60份4-巯基苯甲醛和250份N,N-二甲基甲酰胺的混合液中,加入1份冰乙酸,搅拌1h,随后用NaOH溶液调节反应液pH至7,旋蒸除去N,N-二甲基甲酰胺,加入10份水,得到巯基改性三聚氰胺甲醛树脂溶液;
S2:在20份乳化剂SMA-520中加入10份红磷粉末,用剪切机以10000r/min的速度剪切10min,在0.5h滴入10份巯基改性三聚氰胺甲醛树脂溶液,以10000r/min的速度剪切乳化2min,将温度升至70℃,以600r/min的速度搅拌3h,得到阻燃固化剂;
S3:保持温度为70℃,耗费0.5h将12份碳酸乙烯亚乙酯滴加进25份聚醚胺,保温3h,抽真空,真空度≤-0.08MPa并保持温度70℃,1h后停真空,加入1份KH550,升温至95℃,反应30min,降温至60℃后,得到增韧固化剂;
S4:取75份环氧树脂621A-80、25份环氧树脂6101、16份阻燃固化剂、32份增韧固化剂、2份氢氧化铝、0.5份咪唑、0.1份光引发剂邻苯甲酰苯甲酸甲酯,混合均匀,得到胶液;
S5:保持涂覆的车速为20m/min,涂胶量为180g/m2,将胶液涂覆于玻璃纤维织物,120℃下烘干4h;置于波长为365nm的紫外光下照射2h,样品处紫外光强为50mw/cm2,辐照距离为10cm,得到固化膜;
S6:将两张固化膜堆叠在一起,放置两张铜箔之间,置于真空热压机中热压,热压压制的压力为30kg/cm2,温度为160℃,压制的时间为90min,得到IC封装用高可靠性无卤覆铜板。
实验:(1)取尺寸为130mm×6.5mm×3.2mm的样条,照标准ASTMD2863-2008检测其极限氧指数;
(2)力学性能测试:按照GB/T2567—2008标准测试其拉伸强度,拉伸速率10mm/min;
(3)取尺寸为80×10×2.5mm的样条,照标准ASTMD256-2010检测抗冲击性能,所得数据如下表所示:
表1性能测试数据
LOI/% | 拉伸强度(MPa) | 抗冲击强度/(KJ/m2) | |
实施例1 | 33.6 | 68 | 6.43 |
实施例2 | 32.8 | 63 | 6.08 |
实施例3 | 31.1 | 65 | 6.15 |
对比例1 | 30.6 | 56 | 5.12 |
对比例2 | 29.8 | 58 | 5.33 |
对比例3 | 29.1 | 59 | 5.41 |
对比例4 | 32.4 | 62 | 5.98 |
对比例5 | 26.6 | 60 | 6.15 |
结论:通过对比表1中数据可知,实施例1制得的覆铜板综合性能优于实施例2和实施例3,说明调整阻燃剂或增韧剂的用量均会导致其他性能下降,本发明给出的比例为最佳比例。
由对比例可知,红磷阻燃剂与高分子化合物相容性差,若不进行包覆,则会对产品韧性产生不利影响,由此可见包覆红磷阻燃剂和增韧剂搭配使用的重要性。同时,当更换增韧固化剂,巯基-乙烯基反应不存在时,所得产品的力学性能下降,由此可知巯基-乙烯基反应可降低固化应力,使成品韧性上升。由对比例4和对比例5可知按顺序进行多步固化的重要性。
综上,数据表明,本发明提供的一种IC封装用高可靠性无卤覆铜板的制备方法可以制得IC封装用可靠性高、阻燃性能好、韧性好的无卤覆铜板。
最后应说明的是:以上所述仅为本发明的优选实例而已,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (3)
1.一种IC封装用高可靠性无卤覆铜板的制备方法,其特征在于:包括以下步骤:
S1:取基础环氧树脂、光敏性环氧树脂、阻燃固化剂、增韧固化剂、氢氧化铝、咪唑、光引发剂,混合均匀,得到胶液;
S2:将胶液涂覆于玻璃纤维织物,干燥,光固化,得到固化片;
S3:将两张固化片堆叠在一起,放置于两张铜箔之间,热压,得到IC封装用高可靠性无卤覆铜板;
所述阻燃固化剂的制备方法:(1)将三聚氰胺溶液在1~2h滴加入4-巯基苯甲醛溶液,加入冰乙酸,搅拌1~2h,调节反应液pH至6.5~7.5,除去溶剂,得到三聚氰胺预聚体,将其使用去离子水稀释,得到巯基改性三聚氰胺甲醛树脂溶液;(2)在乳化剂中加入红磷粉末,剪切乳化10~15min,在0.5~1h滴加巯基改性三聚氰胺甲醛树脂溶液,剪切乳化2~5min,将温度升至60~80℃,以600~800r/min的速度搅拌2~3h,得到阻燃固化剂;
所述增韧固化剂是聚醚胺,所述光敏性环氧树脂为环氧树脂621A-80,所述基础环氧树脂为环氧树脂6101;
所述增韧固化剂是碳酸乙烯亚乙酯改性聚醚胺;
碳酸乙烯亚乙酯改性聚醚胺的工艺为:保持温度为60~70℃,在0.5~1h将碳酸乙烯亚乙酯滴加进聚醚胺,依次进行保温、抽真空、反应,加入硅烷偶联剂,升温至80~95℃,反应30~40min,降温,得到增韧固化剂;
所述胶液包括以下原料:按重量份数计,20~30份基础环氧树脂、70~80份光敏性环氧树脂、25~34份阻燃固化剂、14~20份增韧固化剂、1~5份氢氧化铝、0.5~1份咪唑、0.1~0.5份光引发剂;
所述阻燃固化剂包括以下原料:按重量份数计,乳化剂18~25份、红磷粉末8~12份、巯基改性三聚氰胺甲醛树脂溶液8~20份;其中,所述巯基改性三聚氰胺甲醛树脂溶液包括以下原料:按重量份数计,三聚氰胺20~30份、溶剂350~500份、4-巯基苯甲醛50~70份、冰乙酸0.5~2份、去离子水8~15份;
所述增韧固化剂包括以下原料:按重量份数计,碳酸乙烯亚乙酯6~15份、聚醚胺20~30份、硅烷偶联剂0.5~2份。
2.根据权利要求1所述的一种IC封装用高可靠性无卤覆铜板的制备方法,其特征在于:紫外光照射条件为:波长为365nm,样品处紫外光强为45~55mw/cm2,辐照距离为8~15cm;热压压制的压力为20~40kg/cm2,温度为150~180℃,压制的时间为80~100min;涂覆设备为上胶机,涂覆的车速为17~25m/min,涂胶量为160~200g/m2。
3.根据权利要求1~2中任意一项所述的一种IC封装用高可靠性无卤覆铜板的制备方法得到的IC封装用高可靠性无卤覆铜板。
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