CN115974085A - 一种表面改性的硅微粉及其制备方法 - Google Patents
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- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 46
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 42
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- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 claims description 2
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/28—Compounds of silicon
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- C09C3/043—Drying, calcination
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Abstract
本发明提供一种表面改性的硅微粉及其制备方法,属于电子封装材料领域,其制备方法是以纯度大于99.7%的天然石英砂作为原料,依次经熔融、破碎、粉磨和级配后,再通过表面改性对所述级配硅微粉表面进行改性,本发明在现有技术的基础上,通过微粉级配调节,同时通过表面改性处理,提高硅微粉在树脂熔体中的分散性,提高树脂熔体流动性。
Description
技术领域
本发明涉及电子封装材料领域,具体涉及一种表面改性的硅微粉及其制备方法。
背景技术
球形硅微粉是指颗粒个体呈球形,主要成分为二氧化硅的无定形石英粉体材料,为白色粉末,因纯度高、颗粒细、介电性能优异、热膨胀系数低、热导率高等优越性能而具有广阔的发展前景;球形硅微粉主要用于应用于大规模集成电路封装中覆铜板以及环氧塑封料填料,在航空、航天、涂料、催化剂、医药、特种陶瓷及日用化妆品等高新技术领域也有应用。
目前95%以上的电子元件及集成电路的封装是采用环氧树脂复合材料,其中所使用的基体树脂主要是邻甲酚醛环氧树脂,所使用的填料主要是硅微粉,含量占比达70-90%。随着集成电路向超大规模、高密度、大功率、高精度、多功能方向的发展及电子封装技术的快速发展,环氧模塑料(EMC)的发展方向正在朝着高纯度、高可靠性、高导热、耐高温焊、高耐湿性、高粘接强度及低应力、低膨胀、低吸水、低粘度、低环境污染、易加工等方向发展。要制备这样一种高性能的EMC,关键技术是提高硅微粉填充量,但硅微粉含量和表面结构形态对环氧模塑料的流动性影响很大,对集成电路封装效果影响也很大,加大硅微粉的填充量后带来的主要缺点是EMC的流动性大大下降,不利于封装成型工艺。
发明内容
针对上述问题,本发明提供一种表面改性的硅微粉及其制备方法。
本发明的目的采用以下技术方案来实现:
一种表面改性的硅微粉制备方法,包括以下步骤:
(1)选取纯度大于99.7%的天然石英砂作为原料,先水洗除去表面的灰尘和杂质,再在酸溶液浸泡过夜,然后再以去离子水洗涤至中性,干燥备用;
(2)将步骤(1)制得的石英砂转入高温炉进行熔融处理,待温度降至室温后,得到高纯的石英熔结体,将所述石英熔结体转入球磨机,加入球磨介质进行球磨,球磨后经分级机分级,分别得到中位粒径为13-15μm的第一硅微粉和中位粒径为8-10μm的第二硅微粉,待用;
(3)将所述第二硅微粉加入到气流磨机中进行气流粉碎,粉碎后并在分级区分离得到中位粒径为2.5-3.5μm的第三硅微粉;
(4)将所述第一硅微粉和第三硅微粉按重量比为(6-7):2的比例混合,得到级配微粉;
(5)将所述级配微粉加热至90-120℃,按质量比例加入1-4%的表面改性溶液,保温并充分搅拌混合0.5-2h,撤去热源后继续搅拌至冷却,制得所述表面改性的硅微粉。
优选的,所述天然石英砂的选取粒度在0.1-3mm。
优选的,步骤(2)所述熔融处理的熔融温度为1850℃,熔融时间12-14h。
优选的,所述球磨介质为重量比1:(2-3):(1.5-2)的直径分别为3cm、4cm和5cm的氧化铝磨球,球磨时间25-35min。
优选的,按重量份数计,所述表面改性溶液包括如下的组分组成:硅烷偶联剂12-25份,聚醚改性聚硅氧烷5-9份,聚二甲基硅氧烷6-12份,弱极性溶剂10-15份,去离子水1-3份。
优选的,所述硅烷偶联剂为甲基三乙氧基硅烷、乙烯基三乙氧基硅烷、3-氨丙基三乙氧基硅烷、γ-(2,3-环氧丙氧)丙基三甲氧基硅烷、N-(β-氨乙基)-γ-氨丙基三甲氧基硅烷或N-(β-氨乙基)-γ-氨丙基三乙氧基硅烷。
优选的,所述弱极性溶剂为甲苯、二甲苯、汽油或石油醚。
优选的,步骤(4)所述级配微粉还包括以下处理步骤:
S1、称取3-氨丙基三乙氧基硅烷并溶解在无水乙醇中,得到浓度在1-3wt.%的溶液,加入1%体积的去离子水,混合搅拌均匀后加入所述级配微粉,低速搅拌反应过夜,滤出并以无水乙醇洗涤,干燥备用;
S2、将S1制得的级配微粉分散在甲苯或二甲苯中,加入3-溴-2-溴甲基丙酸,经通氮脱气后加入五甲基二乙烯三胺,再次通氮脱气,然后在室温下搅拌反应8-12h,反应完成后滤出洗涤并分散在二甲基甲酰胺中,加入叠氮化钠,升温至90-110℃并保温搅拌反应24-30h,反应完成后冷却至室温,滤出洗涤并再次分散在二甲基甲酰胺中,在冰水浴下条件下,加入丙炔酸,再加入4-二甲氨基吡啶作催化剂,待搅拌混合至体系温度稳定,边搅拌边搅拌滴加N,N-二异丙基碳二亚胺,滴加完成后将反应体系继续在冰水浴下搅拌反应8-12h,反应完成后恢复至室温,加入氨基化笼形倍半硅氧烷,继续搅拌反应1-3h后滤出,洗涤干燥后制得第一改性级配微粉;
其中,所述级配微粉与所述3-溴-2-溴甲基丙酸、所述五甲基二乙烯三胺的质量比例为100:(3-5):(2.6-3.2);所述级配微粉与所述叠氮化钠、所述丙炔酸、所述4-二甲氨基吡啶、所述N,N-二异丙基碳二亚胺、所述氨基化笼形倍半硅氧烷的质量比例为100:(2.6-3.6):(1-1.2):(0.1-0.14):(2.3-2.5):(8-12);
S3、将所述第一改性级配微粉转入高温炉中进行高温热处理,待冷却至室温后制得第二改性级配微粉;所述高温热处理的处理温度在800-1200℃,处理时间1-6h。
优选的,所述第二改性级配微粉还包括以下处理步骤:
S1、称取偶联剂并溶解在溶剂中,加入丙二酸并混合搅拌均匀,静置过夜后加入氨水溶液,搅拌反应5-6h后继续静置1-2天;超声分散后制得分散溶液;
其中,所述偶联剂为甲基三甲氧基硅烷或甲基三乙氧基硅烷,所述溶剂为甲醇或乙醇;所述溶剂与所述偶联剂的摩尔比例为(30-35):1,所述偶联剂与所述丙二酸、所述氨水的摩尔比例为1:(0.01-0.02):(0.8-1);
S2、将所述第二改性级配微粉加入到所述分散溶液中,搅拌混合1-2min后滤出,在60-80℃下干燥,平铺并转入真空干燥箱,覆盖聚二甲基硅氧烷薄膜,在氮气气氛下,升温至180-200℃并保温1-3h,制得第三改性级配微粉。
本发明的另一目的在于提供一种表面改性的硅微粉,所述表面改性的硅微粉由前述制备方法制备得到。
本发明的有益效果为:
现有技术多是在天然石英微粉的基础上结合球磨方法提高硅微粉球形度,进而提高其流动性以降低高硅微粉掺量对树脂熔体流动性的影响,本发明在上述现有技术的基础上,通过粒径分级,得到具有窄粒径分布的硅微粉,再通过大粒径(13-15μm)和小粒径(2.5-3.5μm)的特定比例级配,使得硅微粉颗粒间的接触主要发生在大颗粒间,小颗粒则主要填充在大颗粒间隙,以此提高硅微粉间的流动性,同时,还通过表面改性处理进一步提高硅微粉在树脂熔体中的分散性,进而提高树脂熔体流动性,简化封装工艺;具体的,本发明以硅烷偶联剂为表面活化剂、以聚醚改性聚硅氧烷为分散剂、以聚二甲基硅氧烷为润滑剂对硅微粉表面进行改性处理以进一步提高硅微粉的表面惰性。
进一步的,在硅微粉球形度方面,由于原料经研磨得到的外形多为无规则的菱形角状,因而球形度普遍不高,对树脂熔体的流动性提高效果有限,本发明进一步通过表面二氧化硅沉积以提高硅微粉的球形度,具体的,本发明通过3-溴-2-溴甲基丙酸在活化处理的硅微粉表面引入多溴基团,经叠氮化转化后再与丙炔酸反应引入羧基,最后再通过酰胺化在硅微粉表面接枝高刚高硅的笼形倍半硅氧烷,经过高温稳定化处理后进一步提高微粉的球形度。
为更进一步提高表面改性效果,本发明还在高温稳定化处理硅微粉的基础上,在硅微粉表面浸渍一层二氧化硅凝胶层,经热处理后转化为气凝胶层,再在气相沉积条件下表面修饰聚二甲基硅氧烷,可提高表面改性溶液在微球表面的持液含量,提高表面润滑性能。
具体实施方式
结合以下实施例对本发明作进一步描述。
实施例1
一种表面改性的硅微粉制备方法,包括以下步骤:
(1)选取纯度大于99.7%的天然石英砂作为原料,所述天然石英砂的选取粒度在0.1-3mm,先水洗除去表面的灰尘和杂质,再在酸溶液浸泡过夜,然后再以去离子水洗涤至中性,干燥备用;
(2)将步骤(1)制得的石英砂转入高温炉进行熔融处理,熔融温度为1850℃,熔融时间12-14h,待温度降至室温后,得到高纯的石英熔结体,将所述石英熔结体转入球磨机,加入球磨介质进行球磨,所述球磨介质为重量比1:2.5:1.5的直径分别为3cm、4cm和5cm的氧化铝磨球,球磨时间30min,球磨后经分级机分级,分别得到中位粒径为13-15μm的第一硅微粉和中位粒径为8-10μm的第二硅微粉,待用;
(3)将所述第二硅微粉加入到气流磨机中进行气流粉碎,粉碎后并在分级区分离得到中位粒径为2.5-3.5μm的第三硅微粉;
(4)将所述第一硅微粉和第三硅微粉按重量比为3.25:1的比例混合,得到级配微粉;
(5)将所述级配微粉加热至100℃,按质量比例加入2%的表面改性溶液,保温并充分搅拌混合1.5h,撤去热源后继续搅拌至冷却,制得所述表面改性的硅微粉;
按重量份数计,所述表面改性溶液包括如下的组分组成:乙烯基三乙氧基硅烷15份,聚醚改性聚硅氧烷7份,聚二甲基硅氧烷9份,甲苯12份,去离子水1.5份。
实施例2
一种表面改性的硅微粉制备方法,包括以下步骤:
(1)选取纯度大于99.7%的天然石英砂作为原料,所述天然石英砂的选取粒度在0.1-3mm,先水洗除去表面的灰尘和杂质,再在酸溶液浸泡过夜,然后再以去离子水洗涤至中性,干燥备用;
(2)将步骤(1)制得的石英砂转入高温炉进行熔融处理,熔融温度为1850℃,熔融时间12-14h,待温度降至室温后,得到高纯的石英熔结体,将所述石英熔结体转入球磨机,加入球磨介质进行球磨,所述球磨介质为重量比1:2.5:1.5的直径分别为3cm、4cm和5cm的氧化铝磨球,球磨时间30min,球磨后经分级机分级,分别得到中位粒径为13-15μm的第一硅微粉和中位粒径为8-10μm的第二硅微粉,待用;
(3)将所述第二硅微粉加入到气流磨机中进行气流粉碎,粉碎后并在分级区分离得到中位粒径为2.5-3.5μm的第三硅微粉;
(4-1)将所述第一硅微粉和第三硅微粉按重量比为3.25:1的比例混合,得到级配微粉;
(4-2)称取3-氨丙基三乙氧基硅烷并溶解在无水乙醇中,得到浓度在1.5wt.%的溶液,加入1%体积的去离子水,混合搅拌均匀后加入所述级配微粉,低速搅拌反应过夜,滤出并以无水乙醇洗涤,干燥备用;
(4-3)将(4-2)制得的级配微粉分散在甲苯或二甲苯中,加入3-溴-2-溴甲基丙酸,经通氮脱气后加入五甲基二乙烯三胺,再次通氮脱气,然后在室温下搅拌反应8-12h,反应完成后滤出洗涤并分散在二甲基甲酰胺中,加入叠氮化钠,升温至90-110℃并保温搅拌反应24-30h,反应完成后冷却至室温,滤出洗涤并再次分散在二甲基甲酰胺中,在冰水浴下条件下,加入丙炔酸,再加入4-二甲氨基吡啶作催化剂,待搅拌混合至体系温度稳定,边搅拌边搅拌滴加N,N-二异丙基碳二亚胺,滴加完成后将反应体系继续在冰水浴下搅拌反应8-12h,反应完成后恢复至室温,加入氨基化笼形倍半硅氧烷,继续搅拌反应1-3h后滤出,洗涤干燥后制得第一改性级配微粉;
其中,所述级配微粉与所述3-溴-2-溴甲基丙酸、所述五甲基二乙烯三胺的质量比例为100:3.8:2.9;所述级配微粉与所述叠氮化钠、所述丙炔酸、所述4-二甲氨基吡啶、所述N,N-二异丙基碳二亚胺、所述氨基化笼形倍半硅氧烷的质量比例为100:3.2:1.1:0.12:2.3:10.7;
(4-4)将所述第一改性级配微粉转入高温炉中进行高温热处理,待冷却至室温后制得第二改性级配微粉;所述高温热处理的处理温度在1000℃,处理时间4h;
(5)将所述第二改性级配微粉加热至100℃,按质量比例加入2%的表面改性溶液,保温并充分搅拌混合1.5h,撤去热源后继续搅拌至冷却,制得所述表面改性的硅微粉;
按重量份数计,所述表面改性溶液包括如下的组分组成:乙烯基三乙氧基硅烷15份,聚醚改性聚硅氧烷7份,聚二甲基硅氧烷9份,甲苯12份,去离子水1.5份。
实施例3
一种表面改性的硅微粉制备方法,同实施例2,区别在于,所述第二改性级配微粉还包括以下处理步骤:
S1、称取甲基三乙氧基硅烷并溶解在无水乙醇中,加入丙二酸并混合搅拌均匀,静置过夜后加入氨水溶液,搅拌反应5-6h后继续静置1-2天;超声分散后制得分散溶液;
其中,所述溶剂与所述偶联剂的摩尔比例为32:1,所述偶联剂与所述丙二酸、所述氨水的摩尔比例为1:0.01:0.82;
S2、将所述第二改性级配微粉加入到所述分散溶液中,搅拌混合1-2min后滤出,在60-80℃下干燥,平铺并转入真空干燥箱,覆盖聚二甲基硅氧烷薄膜,在氮气气氛下,升温至180-200℃并保温1-3h。
对比例1
同实施例1,所述级配微粉由所述第一硅微粉和第三硅微粉按重量比为2:1的比例混合得到。
对比例2
实施例1步骤(4)所述级配微粉。
以在相同的配方体系中采用对比例与实施例1-3和对比例1-2所述硅微粉进行底部填充胶性能测试,测试结果如下:
最后应当说明的是,以上实施例仅用以说明本发明的技术方案,而非对本发明保护范围的限制,尽管参照较佳实施例对本发明作了详细地说明,本领域的普通技术人员应当理解,可以对本发明的技术方案进行修改或者等同替换,而不脱离本发明技术方案的实质和范围。
Claims (10)
1.一种表面改性的硅微粉制备方法,其特征在于,包括以下步骤:
(1)选取纯度大于99.7%的天然石英砂作为原料,先水洗除去表面的灰尘和杂质,再在酸溶液浸泡过夜,然后再以去离子水洗涤至中性,干燥备用;
(2)将步骤(1)制得的石英砂转入高温炉进行熔融处理,待温度降至室温后,得到高纯的石英熔结体,将所述石英熔结体转入球磨机,加入球磨介质进行球磨,球磨后经分级机分级,分别得到中位粒径为13-15μm的第一硅微粉和中位粒径为8-10μm的第二硅微粉,待用;
(3)将所述第二硅微粉加入到气流磨机中进行气流粉碎,粉碎后并在分级区分离得到中位粒径为2.5-3.5μm的第三硅微粉;
(4)将所述第一硅微粉和第三硅微粉按重量比为(6-7):2的比例混合,得到级配微粉;
(5)将所述级配微粉加热至90-120℃,按质量比例加入1-4%的表面改性溶液,保温并充分搅拌混合0.5-2h,撤去热源后继续搅拌至冷却,制得所述表面改性的硅微粉。
2.根据权利要求1所述的一种表面改性的硅微粉制备方法,其特征在于,所述天然石英砂的选取粒度在0.1-3mm。
3.根据权利要求1所述的一种表面改性的硅微粉制备方法,其特征在于,步骤(2)所述熔融处理的熔融温度为1850℃,熔融时间12-14h。
4.根据权利要求1所述的一种表面改性的硅微粉制备方法,其特征在于,所述球磨介质为重量比1:(2-3):(1.5-2)的直径分别为3cm、4cm和5cm的氧化铝磨球,球磨时间25-35min。
5.根据权利要求1所述的一种表面改性的硅微粉制备方法,其特征在于,按重量份数计,所述表面改性溶液包括如下的组分组成:硅烷偶联剂12-25份,聚醚改性聚硅氧烷5-9份,聚二甲基硅氧烷6-12份,弱极性溶剂10-15份,去离子水1-3份。
6.根据权利要求5所述的一种表面改性的硅微粉制备方法,其特征在于,所述硅烷偶联剂为甲基三乙氧基硅烷、乙烯基三乙氧基硅烷、3-氨丙基三乙氧基硅烷、γ-(2,3-环氧丙氧)丙基三甲氧基硅烷、N-(β-氨乙基)-γ-氨丙基三甲氧基硅烷或N-(β-氨乙基)-γ-氨丙基三乙氧基硅烷。
7.根据权利要求5所述的一种表面改性的硅微粉制备方法,其特征在于,所述弱极性溶剂为甲苯、二甲苯、汽油或石油醚。
8.根据权利要求1所述的一种表面改性的硅微粉制备方法,其特征在于,步骤(4)所述级配微粉还包括以下处理步骤:
S1、称取3-氨丙基三乙氧基硅烷并溶解在无水乙醇中,得到浓度在1-3wt.%的溶液,加入1%体积的去离子水,混合搅拌均匀后加入所述级配微粉,低速搅拌反应过夜,滤出并以无水乙醇洗涤,干燥备用;
S2、将S1制得的级配微粉分散在甲苯或二甲苯中,加入3-溴-2-溴甲基丙酸,经通氮脱气后加入五甲基二乙烯三胺,再次通氮脱气,然后在室温下搅拌反应8-12h,反应完成后滤出洗涤并分散在二甲基甲酰胺中,加入叠氮化钠,升温至90-110℃并保温搅拌反应24-30h,反应完成后冷却至室温,滤出洗涤并再次分散在二甲基甲酰胺中,在冰水浴下条件下,加入丙炔酸,再加入4-二甲氨基吡啶作催化剂,待搅拌混合至体系温度稳定,边搅拌边搅拌滴加N,N-二异丙基碳二亚胺,滴加完成后将反应体系继续在冰水浴下搅拌反应8-12h,反应完成后恢复至室温,加入氨基化笼形倍半硅氧烷,继续搅拌反应1-3h后滤出,洗涤干燥后制得第一改性级配微粉;
其中,所述级配微粉与所述3-溴-2-溴甲基丙酸、所述五甲基二乙烯三胺的质量比例为100:(3-5):(2.6-3.2);
S3、将所述第一改性级配微粉转入高温炉中进行高温热处理,待冷却至室温后制得第二改性级配微粉;所述高温热处理的处理温度在800-1200℃,处理时间1-6h。
9.根据权利要求8所述的一种表面改性的硅微粉制备方法,其特征在于,所述第二改性级配微粉还包括以下处理步骤:
S1、称取偶联剂并溶解在溶剂中,加入丙二酸并混合搅拌均匀,静置过夜后加入氨水溶液,搅拌反应5-6h后继续静置1-2天;超声分散后制得分散溶液;
其中,所述偶联剂为甲基三甲氧基硅烷或甲基三乙氧基硅烷,所述溶剂为甲醇或乙醇;所述溶剂与所述偶联剂的摩尔比例为(30-35):1,所述偶联剂与所述丙二酸、所述氨水的摩尔比例为1:(0.01-0.02):(0.8-1);
S2、将所述第二改性级配微粉加入到所述分散溶液中,搅拌混合1-2min后滤出,在60-80℃下干燥,平铺并转入真空干燥箱,覆盖聚二甲基硅氧烷薄膜,在氮气气氛下,升温至180-200℃并保温1-3h,制得第三改性级配微粉。
10.根据权利要求1-9之一所述制备方法制备得到的表面改性的硅微粉。
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