CN106281159A - 一种led封装用导电胶的制备方法 - Google Patents
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Abstract
本发明公开了一种LED封装用导电胶的制备方法,属于导电胶制备技术领域。本发明以聚丙烯腈纤维炭化制得导电导热性强的碳纤维材料,经沉积反应在其表面包覆一层纳米银粒子,再用紫胶虫生长产生的天然树脂虫胶和微生物对覆银碳纤维进行表面改性,增加其表面树脂颗粒,增强了导电填料与树脂间的结合力以及相容性,再与环氧树脂复配制得导电胶,覆银碳纤维的加入还增强了导电胶的剪切强度及机械性能,有效解决了常见导电胶由于导电填料和树脂基胶体基料间的相容性差,导致产品导热系数低、体积电阻率高、粘结强度差以及剪切强度小的问题,具有广阔的应用前景。
Description
技术领域
本发明涉及一种LED封装用导电胶的制备方法,属于导电胶制备技术领域。
背景技术
发光二极管(LED)是一种能够发光的半导体器件,具有节能环保等许多优势。随着LED不断朝高功率、高亮度的方向发展,LED器件对封装材料提出了更高的要求。导电银胶是一种能同时提供导电性能和粘接性能的功能材料,由于其具有优良的导电性、导热性和剪切强度,因而被广泛用作LED的封装材料。导电胶是一种固化或干燥后具有一定导电性能的胶黏剂,它通常以基体树脂和导电填料即导电粒子为主要组成成分,通过基体树脂的粘接作用把导电粒子结合在一起,形成导电通路,实现被粘材料的导电连接。导电胶作为一种多组分复合型功能材料,主要由基体树脂、固化剂、促进剂、稀释剂、导电填料及其他各种添加剂组成。常用的基体树脂类型主要有酚醛型、环氧型、丙烯酸酯型、聚酰亚胺型及热塑性烯烃型树脂等。由于导电胶的基体树脂是一种胶黏剂,可以选择适宜的固化温度进行粘接,同时,由于电子元件的小型化、微型化及印刷电路板的高密度化和高度集成化的迅速发展,而导电胶可以制成浆料,实现很高的线分辨率。可以用于对温度敏感的材料或无法焊接的材料的组装、芯片在柔性基板上的贴装等;能避免焊接高温使材料变形、元器件的热损坏;使用导电胶传递应力均匀,可避免铆接的应力集中及电磁讯号的损失、泄露等。但目前导电胶普遍存在导热系数偏低、体积电阻率偏高、粘接强度不够、储存运输性能较差等缺点,且存在剪切强度小、接触电阻不稳定和抗冲击性能差等问题。
发明内容
本发明所要解决的技术问题:针对目前导电胶由于导电填料和树脂基胶体基料间的相容性差,导致产品导热系数低、体积电阻率高、粘结强度差以及剪切强度小的弊端,提供了一种以聚丙烯腈纤维炭化制得导电导热性强的碳纤维材料,经沉积反应在其表面包覆一层纳米银粒子,再用紫胶虫生长产生的天然树脂虫胶和微生物对覆银碳纤维进行表面改性,增加其表面树脂颗粒,增强了导电填料与树脂间的结合力以及相容性,再与环氧树脂复配制得导电胶,覆银碳纤维的加入还增强了导电胶的剪切强度及机械性能,有效解决了常见导电胶由于导电填料和树脂基胶体基料间的相容性差,导致产品导热系数低、体积电阻率高、粘结强度差以及剪切强度小的问题,具有广阔的应用前景。
为解决上述技术问题,本发明采用如下所述的技术方案是:
(1)称取200~300g聚丙烯腈纤维放入炭化炉,向炉中通入氩气直至置换出炉中所有空气,加热升温至2000~2200℃,保温炭化2~3h后,出料,得到碳纤维材料;
(2)量取100~200mL质量浓度为10%硝酸银溶液,加入到装有400~600mL乙二醇的烧杯中,再向烧杯中加入15~20g上述得到的碳纤维材料,搅拌均匀后用浓度为1mol/L氢氧化钠溶液调节pH至8.0~8.5,得混合液;
(3)向上述混合液中加入50~60mL质量浓度为10%羧甲基壳聚糖溶液,再将混合液移入微波振荡仪中,在55~65℃下以200~300W功率振荡反应30~40min后,转入布氏漏斗,用去离子水抽滤洗涤10~15min,得滤渣,干燥后研磨并过200目筛,即得覆银碳纤维导电填料;
(4)取一根长为25~30cm、胸径为10~20cm的山合欢树杆,放入陶瓷罐中,并向罐中放入400~500g紫胶虫幼虫,再将上述制得的覆银碳纤维导电填料装入陶瓷罐,让紫胶虫自然生长产胶并对覆银碳纤维导电填料改性处理3~4个月,改性结束后,人工取出树干和紫胶虫,将陶瓷罐底部沉淀用无水乙醇冲洗20~30min后,放入烘箱中,在40~50℃下干燥1~2h,得改性导电填料;
(5)量取400~500mL环氧树脂溶于800~900mL乙二醇丁醚中,搅拌均匀得胶体基液,将胶体基液装入烧杯中,先分别加入100~150g上述改性导电填料和5~10g乙烯基三胺,搅拌5~8min后,再分别加入100~150g上述改性导电填料和12~15mL氨丙基三乙氧基硅烷,继续搅拌10~20min,得到预胶料;
(6)将上述预胶料装入胶体磨中,以2900~3000r/min转速研磨20~30min后,转入密炼机,在120~130℃下密炼15~20min后,出料装罐,即得LED封装用导电胶。
本发明制得的LED封装用导电胶体积电阻率为5.32×10-5~5.34×10-5Ω·cm,热传导率为10.41~11.25W/m·K,热膨胀系数为80~96μm/m·℃,断裂伸长率为136~142%,剪切强度为19.5~20.6MPa。
本发明与其他方法相比,有益技术效果是:
(1)本发明制备步骤简单,制得的导电填料与树脂基胶体基料间相容性好;
(2)所得产品导热系数高、体积电阻率低,粘结强度好,剪切强度大。
具体实施方式
首先称取200~300g聚丙烯腈纤维放入炭化炉,向炉中通入氩气直至置换出炉中所有空气,加热升温至2000~2200℃,保温炭化2~3h后,出料,得到碳纤维材料;量取100~200mL质量浓度为10%硝酸银溶液,加入到装有400~600mL乙二醇的烧杯中,再向烧杯中加入15~20g上述得到的碳纤维材料,搅拌均匀后用浓度为1mol/L氢氧化钠溶液调节pH至8.0~8.5,得混合液;然后向上述混合液中加入50~60mL质量浓度为10%羧甲基壳聚糖溶液,再将混合液移入微波振荡仪中,在55~65℃下以200~300W功率振荡反应30~40min后,转入布氏漏斗,用去离子水抽滤洗涤10~15min,得滤渣,干燥后研磨并过200目筛,即得覆银碳纤维导电填料;取一根长为25~30cm、胸径为10~20cm的山合欢树杆,放入陶瓷罐中,并向罐中放入400~500g紫胶虫幼虫,再将上述制得的覆银碳纤维导电填料装入陶瓷罐,让紫胶虫自然生长产胶并对覆银碳纤维导电填料改性处理3~4个月,改性结束后,人工取出树干和紫胶虫,将陶瓷罐底部沉淀用无水乙醇冲洗20~30min后,放入烘箱中,在40~50℃下干燥1~2h,得改性导电填料;再量取400~500mL环氧树脂溶于800~900mL乙二醇丁醚中,搅拌均匀得胶体基液,将胶体基液装入烧杯中,先分别加入100~150g上述改性导电填料和5~10g乙烯基三胺,搅拌5~8min后,再分别加入100~150g上述改性导电填料和12~15mL氨丙基三乙氧基硅烷,继续搅拌10~20min,得到预胶料;最后将上述预胶料装入胶体磨中,以2900~3000r/min转速研磨20~30min后,转入密炼机,在120~130℃下密炼15~20min后,出料装罐,即得LED封装用导电胶。
实例1
首先称取200g聚丙烯腈纤维放入炭化炉,向炉中通入氩气直至置换出炉中所有空气,加热升温至2000℃,保温炭化2h后,出料,得到碳纤维材料;量取100mL质量浓度为10%硝酸银溶液,加入到装有400mL乙二醇的烧杯中,再向烧杯中加入15g上述得到的碳纤维材料,搅拌均匀后用浓度为1mol/L氢氧化钠溶液调节pH至8.0,得混合液;然后向上述混合液中加入50mL质量浓度为10%羧甲基壳聚糖溶液,再将混合液移入微波振荡仪中,在55℃下以200W功率振荡反应30min后,转入布氏漏斗,用去离子水抽滤洗涤10min,得滤渣,干燥后研磨并过200目筛,即得覆银碳纤维导电填料;取一根长为25cm、胸径为10cm的山合欢树杆,放入陶瓷罐中,并向罐中放入400g紫胶虫幼虫,再将上述制得的覆银碳纤维导电填料装入陶瓷罐,让紫胶虫自然生长产胶并对覆银碳纤维导电填料改性处理3个月,改性结束后,人工取出树干和紫胶虫,将陶瓷罐底部沉淀用无水乙醇冲洗20min后,放入烘箱中,在40℃下干燥1h,得改性导电填料;再量取400mL环氧树脂溶于800mL乙二醇丁醚中,搅拌均匀得胶体基液,将胶体基液装入烧杯中,先分别加入100g上述改性导电填料和5g乙烯基三胺,搅拌5min后,再分别加入100g上述改性导电填料和12mL氨丙基三乙氧基硅烷,继续搅拌10min,得到预胶料;最后将上述预胶料装入胶体磨中,以2900r/min转速研磨20min后,转入密炼机,在120℃下密炼15min后,出料装罐,即得LED封装用导电胶。
本发明制备步骤简单,制得的导电填料与树脂基胶体基料间相容性好;所得产品导热系数高、体积电阻率低,粘结强度好,剪切强度大;制得的LED封装用导电胶体积电阻率为5.32×10-5Ω·cm,热传导率为10.41W/m·K,热膨胀系数为80μm/m·℃,断裂伸长率为136%,剪切强度为19.5MPa。
实例2
首先称取250g聚丙烯腈纤维放入炭化炉,向炉中通入氩气直至置换出炉中所有空气,加热升温至2100℃,保温炭化3h后,出料,得到碳纤维材料;量取150mL质量浓度为10%硝酸银溶液,加入到装有500mL乙二醇的烧杯中,再向烧杯中加入18g上述得到的碳纤维材料,搅拌均匀后用浓度为1mol/L氢氧化钠溶液调节pH至8.3,得混合液;然后向上述混合液中加入55mL质量浓度为10%羧甲基壳聚糖溶液,再将混合液移入微波振荡仪中,在60℃下以250W功率振荡反应35min后,转入布氏漏斗,用去离子水抽滤洗涤13min,得滤渣,干燥后研磨并过200目筛,即得覆银碳纤维导电填料;取一根长为28cm、胸径为15cm的山合欢树杆,放入陶瓷罐中,并向罐中放入450g紫胶虫幼虫,再将上述制得的覆银碳纤维导电填料装入陶瓷罐,让紫胶虫自然生长产胶并对覆银碳纤维导电填料改性处理4个月,改性结束后,人工取出树干和紫胶虫,将陶瓷罐底部沉淀用无水乙醇冲洗25min后,放入烘箱中,在45℃下干燥2h,得改性导电填料;再量取450mL环氧树脂溶于850mL乙二醇丁醚中,搅拌均匀得胶体基液,将胶体基液装入烧杯中,先分别加入125g上述改性导电填料和8g乙烯基三胺,搅拌7min后,再分别加入125g上述改性导电填料和13mL氨丙基三乙氧基硅烷,继续搅拌15min,得到预胶料;最后将上述预胶料装入胶体磨中,以2950r/min转速研磨25min后,转入密炼机,在125℃下密炼18min后,出料装罐,即得LED封装用导电胶。
本发明制备步骤简单,制得的导电填料与树脂基胶体基料间相容性好;所得产品导热系数高、体积电阻率低,粘结强度好,剪切强度大;制得的LED封装用导电胶体积电阻率为5.33×10-5Ω·cm,热传导率为10.83W/m·K,热膨胀系数为88μm/m·℃,断裂伸长率为139%,剪切强度为20.1MPa。
实例3
首先称取300g聚丙烯腈纤维放入炭化炉,向炉中通入氩气直至置换出炉中所有空气,加热升温至2200℃,保温炭化3h后,出料,得到碳纤维材料;量取200mL质量浓度为10%硝酸银溶液,加入到装有600mL乙二醇的烧杯中,再向烧杯中加入20g上述得到的碳纤维材料,搅拌均匀后用浓度为1mol/L氢氧化钠溶液调节pH至8.5,得混合液;然后向上述混合液中加入60mL质量浓度为10%羧甲基壳聚糖溶液,再将混合液移入微波振荡仪中,在65℃下以300W功率振荡反应40min后,转入布氏漏斗,用去离子水抽滤洗涤15min,得滤渣,干燥后研磨并过200目筛,即得覆银碳纤维导电填料;取一根长为30cm、胸径为20cm的山合欢树杆,放入陶瓷罐中,并向罐中放入500g紫胶虫幼虫,再将上述制得的覆银碳纤维导电填料装入陶瓷罐,让紫胶虫自然生长产胶并对覆银碳纤维导电填料改性处理4个月,改性结束后,人工取出树干和紫胶虫,将陶瓷罐底部沉淀用无水乙醇冲洗30min后,放入烘箱中,在50℃下干燥2h,得改性导电填料;再量取500mL环氧树脂溶于900mL乙二醇丁醚中,搅拌均匀得胶体基液,将胶体基液装入烧杯中,先分别加入150g上述改性导电填料和10g乙烯基三胺,搅拌8min后,再分别加入150g上述改性导电填料和15mL氨丙基三乙氧基硅烷,继续搅拌20min,得到预胶料;最后将上述预胶料装入胶体磨中,以3000r/min转速研磨30min后,转入密炼机,在130℃下密炼20min后,出料装罐,即得LED封装用导电胶。
本发明制备步骤简单,制得的导电填料与树脂基胶体基料间相容性好;所得产品导热系数高、体积电阻率低,粘结强度好,剪切强度大;制得的LED封装用导电胶体积电阻率为5.34×10-5Ω·cm,热传导率为11.25W/m·K,热膨胀系数为96μm/m·℃,断裂伸长率为142%,剪切强度为20.6MPa。
Claims (1)
1.一种LED封装用导电胶的制备方法,其特征在于具体制备步骤为:
(1)称取200~300g聚丙烯腈纤维放入炭化炉,向炉中通入氩气直至置换出炉中所有空气,加热升温至2000~2200℃,保温炭化2~3h后,出料,得到碳纤维材料;
(2)量取100~200mL质量浓度为10%硝酸银溶液,加入到装有400~600mL乙二醇的烧杯中,再向烧杯中加入15~20g上述得到的碳纤维材料,搅拌均匀后用浓度为1mol/L氢氧化钠溶液调节pH至8.0~8.5,得混合液;
(3)向上述混合液中加入50~60mL质量浓度为10%羧甲基壳聚糖溶液,再将混合液移入微波振荡仪中,在55~65℃下以200~300W功率振荡反应30~40min后,转入布氏漏斗,用去离子水抽滤洗涤10~15min,得滤渣,干燥后研磨并过200目筛,即得覆银碳纤维导电填料;
(4)取一根长为25~30cm、胸径为10~20cm的山合欢树杆,放入陶瓷罐中,并向罐中放入400~500g紫胶虫幼虫,再将上述制得的覆银碳纤维导电填料装入陶瓷罐,让紫胶虫自然生长产胶并对覆银碳纤维导电填料改性处理3~4个月,改性结束后,人工取出树干和紫胶虫,将陶瓷罐底部沉淀用无水乙醇冲洗20~30min后,放入烘箱中,在40~50℃下干燥1~2h,得改性导电填料;
(5)量取400~500mL环氧树脂溶于800~900mL乙二醇丁醚中,搅拌均匀得胶体基液,将胶体基液装入烧杯中,先分别加入100~150g上述改性导电填料和5~10g乙烯基三胺,搅拌5~8min后,再分别加入100~150g上述改性导电填料和12~15mL氨丙基三乙氧基硅烷,继续搅拌10~20min,得到预胶料;
(6)将上述预胶料装入胶体磨中,以2900~3000r/min转速研磨20~30min后,转入密炼机,在120~130℃下密炼15~20min后,出料装罐,即得LED封装用导电胶。
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