CN107057284A - 一种改性碳化硅导电封装材料的制备方法 - Google Patents
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- 235000010777 Arachis hypogaea Nutrition 0.000 claims description 4
- 235000018262 Arachis monticola Nutrition 0.000 claims description 4
- 239000004844 aliphatic epoxy resin Substances 0.000 claims description 4
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- 238000006243 chemical reaction Methods 0.000 claims description 4
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- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
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Abstract
本发明公开了一种改性碳化硅导电封装材料的制备方法,本发明在封装材料中添加的改性碳化硅复杂形状,且具有热导率高、膨胀系数低、比刚度大、密度小等特点,使得封装材料在固化后的内应力变化值范围较小,机械性能和耐冲击性能优良,产品导电性能优良,且具有良好的分散性、相容性和耐热性。
Description
技术领域
本发明涉及电子器件制造领域,具体涉及一种改性碳化硅导电封装材料的制备方法。
背景技术
由于电子封装材料对电子器件的可靠性和使用寿命有重要的影响,近年来电子封装材料的研究受到了越来越多的关注。电子封装材料是用于承载电子元器件及其相互联线,起机械支撑、密封环境保护、信号专递等作用的基体材料。因此,电子封装材料必须具备高透过率、高耐热性、低黄变率和优良的机械性能。
当封装材料与电子产品组成的封装体系在温度骤变时,封装材料与电子产品的元件间会产生热应力,封装体系产生裂纹而开裂,导致嵌入元件的损坏。虽然添加填料可以在一定程度上减少封装材料的固化收缩、防止开裂、减小固化时的放热,但是填料在脂肪族环氧树脂中的分散性较差,会使封装材料的起始粘度增大,降低工艺性,而且防止开裂的效果不好,制得的封装材料还是容易开裂。
传统的电子封装材料已很难满足现代电子封装的要求。以碳化硅颗粒增强铝基复合材料和硅颗粒增强铝基复合材料为代表的铝基复合材料具有高导热、低膨胀等优点,是目前应用较为广泛的一类电子封装材料,但因铝基体熔点较低,其耐温性能较差而不能很好地满足第 三代半导体器件的封装。纯铜具有比纯铝更高的热导率,理论上碳化硅颗粒增强 铜基复合材料具有更高的热导率、更低的热膨胀系数、更好的耐温性能和更优异的焊接性能等优点,在电子封装领域具有很大的应用潜力。
发明内容
本发明提供一种改性碳化硅导电封装材料的制备方法,本发明在封装材料中添加的改性碳化硅复杂形状,且具有热导率高、膨胀系数低、比刚度大、密度小等特点,使得封装材料在固化后的内应力变化值范围较小,机械性能和耐冲击性能优良,产品导电性能优良,且具有良好的分散性、相容性和耐热性。
为了实现上述目的,本发明提供了一种改性碳化硅导电封装材料的制备方法,该方法包括如下步骤:
(1)制备改性碳化硅
称取200-300重量份花生壳,用去离子水洗涤3-5次,置于115-120℃干燥箱中干燥至恒重后,加入500-530℃真空管式炉中,在氮气氛围下碳化2-3h,冷却至室温,取出,将其与3-5重量份钛酸酯类偶联剂,1-2重量份氟化钾混合均匀,置入真空管式炉中,炉内抽至真空度为5-10Pa后,以150-200mL/min通入氩气,并以15℃/min升温至1150-1300℃,再以5℃/min升温至1500-1550℃,保持温度反应4-6h后,自然冷却至室温,通入空气,在750-800℃下灼烧3-5h,冷却至室温,得碳化硅晶须;
称取60-80重量份上述碳化硅晶须,加入150-200重量份丙酮中,并用300W超声波超声除油20-30min,过滤,将滤渣浸泡在质量分数为25%氢氟酸溶液中8-10h,过滤,用去离子水洗涤滤渣至洗涤液pH呈中性,转入115-120℃真空干燥箱中干燥至恒重,得到改性碳化硅;
(2)按照如下重量份配料:
上述改性碳化硅 10-15份
乙烯基含氢硅树脂 3-5份
氟硅酸钠 3-6份
甲基纳迪克酸酐 1-1.5份
脂肪族环氧树脂 18-20份
钛酸酯类偶联剂 0.5-1份
含氢硅油交联剂 1-3份;
(3)按上述组分按比例混合均匀,加热搅拌至混合均匀,将混合物在真空脱泡机中进行脱泡,脱泡时间为5-7h;
将所述脱泡后的混合物加入到双螺杆挤出机的料斗中,螺杆转速设定为600-800r/min,经过熔融挤出,水冷切粒得到粒料;接着,进行低温加压干燥,用注塑机注塑成型,制备得到改性碳化硅导电封装材料。
具体实施方式
实施例一
称取200重量份花生壳,用去离子水洗涤3次,置于115℃干燥箱中干燥至恒重后,加入500℃真空管式炉中,在氮气氛围下碳化2h,冷却至室温,取出,将其与3重量份钛酸酯类偶联剂,1重量份氟化钾混合均匀,置入真空管式炉中,炉内抽至真空度为5Pa后,以150mL/min通入氩气,并以15℃/min升温至1150℃,再以5℃/min升温至1500℃,保持温度反应4h后,自然冷却至室温,通入空气,在750℃下灼烧3h,冷却至室温,得碳化硅晶须。
称取60重量份上述碳化硅晶须,加入150重量份丙酮中,并用300W超声波超声除油20min,过滤,将滤渣浸泡在质量分数为25%氢氟酸溶液中8h,过滤,用去离子水洗涤滤渣至洗涤液pH呈中性,转入115℃真空干燥箱中干燥至恒重,得到改性碳化硅。
按如下重量份配料:
上述改性碳化硅 10份
乙烯基含氢硅树脂 3份
氟硅酸钠 3份
甲基纳迪克酸酐 1份
脂肪族环氧树脂 18份
钛酸酯类偶联剂 0.5份
含氢硅油交联剂 1份;
按上述组分按比例混合均匀,加热搅拌至混合均匀,将混合物在真空脱泡机中进行脱泡,脱泡时间为5h。
将所述脱泡后的混合物加入到双螺杆挤出机的料斗中,螺杆转速设定为600r/min,经过熔融挤出,水冷切粒得到粒料;接着,进行低温加压干燥,用注塑机注塑成型,制备得到改性碳化硅导电封装材料。
实施例二
称取300重量份花生壳,用去离子水洗涤5次,置于120℃干燥箱中干燥至恒重后,加入530℃真空管式炉中,在氮气氛围下碳化3h,冷却至室温,取出,将其与5重量份钛酸酯类偶联剂,2重量份氟化钾混合均匀,置入真空管式炉中,炉内抽至真空度为10Pa后,以200mL/min通入氩气,并以15℃/min升温至1300℃,再以5℃/min升温至1550℃,保持温度反应6h后,自然冷却至室温,通入空气,在800℃下灼烧5h,冷却至室温,得碳化硅晶须。
称取80重量份上述碳化硅晶须,加入200重量份丙酮中,并用300W超声波超声除油30min,过滤,将滤渣浸泡在质量分数为25%氢氟酸溶液中10h,过滤,用去离子水洗涤滤渣至洗涤液pH呈中性,转入120℃真空干燥箱中干燥至恒重,得到改性碳化硅。
按如下重量份配料:
上述改性碳化硅 15份
乙烯基含氢硅树脂 5份
氟硅酸钠 6份
甲基纳迪克酸酐 1.5份
脂肪族环氧树脂 20份
钛酸酯类偶联剂 1份
含氢硅油交联剂 3份;
按上述组分按比例混合均匀,加热搅拌至混合均匀,将混合物在真空脱泡机中进行脱泡,脱泡时间为7h。
将所述脱泡后的混合物加入到双螺杆挤出机的料斗中,螺杆转速设定为800r/min,经过熔融挤出,水冷切粒得到粒料;接着,进行低温加压干燥,用注塑机注塑成型,制备得到改性碳化硅导电封装材料。
Claims (1)
1.一种改性碳化硅导电封装材料的制备方法,该方法包括如下步骤:
(1)制备改性碳化硅
称取200-300重量份花生壳,用去离子水洗涤3-5次,置于115-120℃干燥箱中干燥至恒重后,加入500-530℃真空管式炉中,在氮气氛围下碳化2-3h,冷却至室温,取出,将其与3-5重量份钛酸酯类偶联剂,1-2重量份氟化钾混合均匀,置入真空管式炉中,炉内抽至真空度为5-10Pa后,以150-200mL/min通入氩气,并以15℃/min升温至1150-1300℃,再以5℃/min升温至1500-1550℃,保持温度反应4-6h后,自然冷却至室温,通入空气,在750-800℃下灼烧3-5h,冷却至室温,得碳化硅晶须;
称取60-80重量份上述碳化硅晶须,加入150-200重量份丙酮中,并用300W超声波超声除油20-30min,过滤,将滤渣浸泡在质量分数为25%氢氟酸溶液中8-10h,过滤,用去离子水洗涤滤渣至洗涤液pH呈中性,转入115-120℃真空干燥箱中干燥至恒重,得到改性碳化硅;
(2)按照如下重量份配料:
上述改性碳化硅 10-15份
乙烯基含氢硅树脂 3-5份
氟硅酸钠 3-6份
甲基纳迪克酸酐 1-1.5份
脂肪族环氧树脂 18-20份
钛酸酯类偶联剂 0.5-1份
含氢硅油交联剂 1-3份;
(3)按上述组分按比例混合均匀,加热搅拌至混合均匀,将混合物在真空脱泡机中进行脱泡,脱泡时间为5-7h;
将所述脱泡后的混合物加入到双螺杆挤出机的料斗中,螺杆转速设定为600-800r/min,经过熔融挤出,水冷切粒得到粒料;接着,进行低温加压干燥,用注塑机注塑成型,制备得到改性碳化硅导电封装材料。
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