CN110105895B - 用于硅晶片切割工艺的uv光致可剥离胶带的制备方法 - Google Patents

用于硅晶片切割工艺的uv光致可剥离胶带的制备方法 Download PDF

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CN110105895B
CN110105895B CN201910368387.9A CN201910368387A CN110105895B CN 110105895 B CN110105895 B CN 110105895B CN 201910368387 A CN201910368387 A CN 201910368387A CN 110105895 B CN110105895 B CN 110105895B
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刘少杰
郝盼盼
赵婷
刘浩
王晓英
杨文玲
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Hebei University of Science and Technology
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Abstract

本发明涉及一种用于硅晶片切割工艺的UV光致可剥离胶带的制备方法，其包括如下步骤：（1）双官能团聚氨酯预聚物的制备；（2）丙烯酸酯共聚物基胶的制备；（3）UV光致可剥离胶的制备；（4）UV光致可剥离胶带的制备。通过本发明的方法制备的UV光致可剥离胶带具有网络密集、剥离性能好且无残胶优点。

Description

用于硅晶片切割工艺的UV光致可剥离胶带的制备方法
技术领域
本发明属于胶粘剂技术领域，具体涉及一种用于硅晶片切割工艺的UV光致可剥离胶带制备方法。
背景技术
在大规模集成电路的制造和半导体器件的制造加工过程中，必不可少的基础材料是半导体芯片，半导体芯片是以单晶硅片加工而成的。单晶硅片简称晶圆，在对晶圆材料进行切割、磨削加工时，需要用一种特殊的压敏胶带进行粘结固定。加工完毕后，需要把加工好的晶圆切片从固定胶上能不费力地的完全剥离下来，不影响晶圆材料本身，这就要求这种特殊的压敏胶能通过某种方式瞬间失去粘性。通过紫外光照的方式使压敏胶失去粘性的胶粘剂即为UV致可剥离胶。
制备UV致可剥离胶粘剂的关键成分是一种含聚氨酯结构单元的预聚物。其分子结构和分子量决定了粘合剂的韧性、固化收缩率和粘合性能等基本性能。目前应用于UV致可剥离胶的聚氨酯预聚物是多官能团（官能团数不小于3）的聚氨酯丙烯酸酯，这种多官能团光敏树脂不仅结构复杂，且制备过程繁琐，反应不易控制，制备成本较高。而由此多官能团光敏树脂与基胶线性分子等制备而成的可剥离胶带固化后是一种半互穿网状结构。由于这种网络结构的交联度不够高，所以在紫外光照射后容易有残胶等情况。
发明内容
本发明的目的是提供一种网络密集、剥离性能好且无残胶的UV光致可剥离胶带的制备方法。
本发明采用如下技术方案：
1）利用聚乙二醇和二异氰酸酯合成了一种双官能团聚氨酯预聚物，其化学反应式如下：
Figure DEST_PATH_IMAGE001
。
2）将上述双官能团聚氨酯预聚物与丙烯酸酯共聚物基胶、稀释剂和光引发剂按照一定比例混合并均匀涂覆于经处理的PET膜的内侧，制得UV光致可剥离胶带。两官能团聚氨酯预聚物与基胶在UV固化前可预先形成一个网络结构，与UV固化得到的聚合物网络生成互穿网状结构，相比于半互穿网状结构网络更密集，固化收缩率更高，剥离性能更好，不易形成残胶。
所述制备方法具体步骤为：
（1）双官能团聚氨酯预聚物的制备：向四口烧瓶中加入二异氰酸酯、二月桂酸二丁烯，开启搅拌通氮气保护，升温至50℃，用蠕动泵将聚乙二醇、对叔丁邻苯二酚的丙酮溶液滴加到烧瓶中，滴加时间为0.25~0.5 h，滴加完毕后继续反应4~6 h。
（2）丙烯酸酯共聚物基胶的制备：称取一定量的丙烯酸、甲基丙烯酸甲酯、丙烯酸羟乙酯、丙烯酸丁酯、丙烯酸异辛酯于烧杯中均匀混合制得单体溶液；称取一定量过氧化苯甲酰溶于乙醇中制得引发剂溶液；室温下将10~20%的单体溶液加入四口烧瓶中，滴加1~3%引发剂溶液后搅拌0.9~1.1 h，升温至70℃，用蠕动泵滴加剩余单体溶液和引发剂溶液。滴加完毕后，反应2 h，旋蒸，得到无色透明状粘稠液体，即为丙烯酸酯共聚物基胶。
（3）UV光致可剥离胶的制备：取步骤（2）制备的丙烯酸酯共聚物基胶，一定温度下加热一定时间进行预处理。将加热后的基胶与双官能团聚氨酯预聚物、光引发剂1-羟环已基苯酮、稀释剂三羟甲基丙烷三丙烯酸酯按一定比例混合均匀。
（4）UV光致可剥离胶带的制备：将步骤（3）制备的UV光致固化可剥离胶用涂布器均匀涂抹在经处理的PET膜的内侧，随后将样品在温度为23℃、相对湿度为65％条件下静置3天老化，制得UV光致可剥离胶带。
优选的，步骤（1）中，溶液A的加入量为，以得到30g双官能团聚氨酯预聚物计，取对叔丁邻苯二酚0.0382g~0.0394g溶于150ml丙酮中。
优选的，步骤（2）中，引发剂溶液通过如下方法配制：取单体溶液总质量1%的过氧化苯甲酰溶于10ml乙醇中。
优选地，所述步骤（1）中二异氰酸酯为异佛尔酮二异氰酸酯（IPDI）、甲苯二异氰酸酯（TDI）或二苯基甲烷二异氰酸酯（MDI），二异氰酸酯与聚乙二醇的摩尔比分别为1.5~2∶1，A溶液滴加时间为0.25~0.3 h。
优选地，所述步骤（2）中丙烯酸、甲基丙烯酸甲酯、丙烯酸羟乙酯、丙烯酸异辛酯与丙烯酸丁酯的摩尔比为0.15~0.2∶ 0.4~0.5∶0.2~0.3∶4~4.5∶1，剩余单体溶液和引发剂溶液的滴加时间为1.5～2 h。
优选地，所述步骤（3）中丙烯酸酯共聚物基胶预处理方式为，在75~85℃加热20~25分钟，95~115℃加热1分钟。
优选地，所述步骤（3）中基胶：聚氨酯预聚物：稀释剂：光引发剂的质量比为1∶1∶0.025~0.03∶0.3~0.4。
本发明的有益效果在于：本发明利用二异氰酸酯与聚乙二醇合成双官能团聚氨酯预聚物，合成工艺简单，过程易控，成本较低。将其与丙烯酸酯共聚物基胶、稀释剂和光引发剂按照一定比例混合并均匀涂覆于经处理的PET膜的内侧即可制得UV光致可剥离胶带。端基为异氰酸基的聚氨酯预聚物可与含有羟基、羧基的丙烯酸酯共聚物基胶发生交联反应形成网状结构，进而与UV照射后生成的聚合物网络形成互穿网状结构，相比于半互穿网状结构网络更密集，剥离性能更好，且无残胶。
具体实施方式
下面结合本发明的几个具体实施例对本发明作进一步说明，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明技术范围内，可轻易想到变化或替换，都应涵盖在本发明的保护范围之内。
实施例1
（1）双官能团聚氨酯预聚物的制备：向四口烧瓶中加入异佛尔酮二异氰酸酯16.670g、二月桂酸二丁烯0.00767g，开启搅拌通氮气保护，升温至50℃，用蠕动泵将聚乙二醇10g、对叔丁邻苯二酚0.0382g和150mL的丙酮溶液滴加到烧瓶中，滴加时间为15min，滴加完毕后继续反应6 h，得到双官能团异氰酸基封端的聚氨酯预聚物。
（2））丙烯酸酯共聚物基胶的制备：分别称取0.680g丙烯酸、1.748g甲基丙烯酸甲酯、1.045g丙烯酸羟乙酯、4.001g丙烯酸丁酯、16.001g丙烯酸异辛酯于烧杯中均匀混合制得单体溶液；称取单体溶液总质量1%的过氧化苯甲酰溶乙醇中制得引发剂溶液；将15%的单体溶液加入四口烧瓶中，滴加1.5%引发剂溶液后搅拌1 h，升温至70℃，用蠕动泵滴加剩余单体溶液和引发剂溶液。滴加完毕后，反应2 h，旋蒸，得到无色透明状粘稠液体，即为丙烯酸酯共聚物基胶。测得压敏胶的收率为93%，剥离强度为6.208N/25mm。
（3）UV光致可剥离胶的制备：取2 g步骤（2）制备的丙烯酸酯共聚物基胶，在100℃烘箱中烘1分钟进行预处理。将加热后的基胶与双官能团聚氨酯预聚物、光引发剂1-羟环已基苯酮、稀释剂三羟甲基丙烷三丙烯酸酯按质量比为1∶1∶0.025∶0.4比例混合均匀。
（4）UV光致可剥离胶带的制备：将步骤（3）制备的UV光致固化可剥离胶用涂布器均匀涂抹在经电晕处理的长40cm，宽为2.5cm的PET膜内侧，随后将样品在温度为23℃、相对湿度为65％条件下静置3天老化，制得UV光致可剥离胶带PSA-1。经紫外光照射后可剥离，无残胶。测得光照前PSA-1胶带180°剥离强度为8.789N/25mm，光照后剥离强度为0.495N/25mm。
实施例2
（1）双官能团聚氨酯预聚物的制备：向四口烧瓶中加入异佛尔酮二异氰酸酯16.774g、二月桂酸二丁烯0.00766g，开启搅拌通氮气保护，升温至50℃，用蠕动泵将聚乙二醇10.07g、对叔丁邻苯二酚0.0394g和150mL的丙酮溶液滴加到烧瓶中，滴加时间为15min，滴加完毕后继续反应6 h，得到双官能团异氰酸基封端的聚氨酯预聚物。
（2）丙烯酸酯共聚物基胶的制备：分别称取0.685g丙烯酸、1.757g甲基丙烯酸甲酯、1.054g丙烯酸羟乙酯、4.019g丙烯酸丁酯、16.017g丙烯酸异辛酯于烧杯中均匀混合制得单体溶液；称取单体溶液总质量1%的过氧化苯甲酰溶乙醇中制得引发剂溶液；将15%的单体溶液加入四口烧瓶中，滴加1.5%引发剂溶液后搅拌1 h，升温至70℃，用蠕动泵滴加剩余单体溶液和引发剂溶液。滴加完毕后，反应2 h，旋蒸，得到无色透明状粘稠液体，即为丙烯酸酯共聚物基胶。测得压敏胶的收率为94%，剥离强度为5.988N/25mm。
（3）UV光致可剥离胶的制备：取2 g步骤（2）制备的丙烯酸酯共聚物基胶，在100℃烘箱中烘1分钟进行预处理。将加热后的基胶与双官能团聚氨酯预聚物、光引发剂1-羟环已基苯酮、稀释剂三羟甲基丙烷三丙烯酸酯按质量比为1∶1∶0.025∶0.4比例混合均匀。
（4）UV光致可剥离胶带的制备：将步骤（3）制备的UV光致固化可剥离胶用涂布器均匀涂抹在经电晕处理的长40cm，宽为2.5cm的PET膜内侧，随后将样品在温度为23℃、相对湿度为65％条件下静置3天老化，制得UV光致可剥离胶带PSA-2。经紫外光照射后可剥离，无残胶。测得光照前PSA-1胶带180°剥离强度为10.298N/25mm，光照后剥离强度为0.499N/25mm。
实施例3
（1）双官能团聚氨酯预聚物的制备：向四口烧瓶中加入异佛尔酮二异氰酸酯20.683g、二月桂酸二丁烯0.00766g，开启搅拌通氮气保护，升温至50℃，用蠕动泵将聚乙二醇9.317g、对叔丁邻苯二酚0.0387g和150mL的丙酮溶液滴加到烧瓶中，滴加时间为15分钟，滴加完毕后继续反应6 h，得到双官能团异氰酸基封端的聚氨酯预聚物。
（2）丙烯酸酯共聚物基胶的制备：分别称取0.687g丙烯酸、1.784g甲基丙烯酸甲酯、1.087g丙烯酸羟乙酯、4.020g丙烯酸丁酯、16.031g丙烯酸异辛酯于烧杯中均匀混合制得单体溶液；称取单体溶液总质量1%的过氧化苯甲酰溶乙醇中制得引发剂溶液；将15%的单体溶液加入四口烧瓶中，滴加1.5%引发剂溶液后搅拌1 h，升温至70℃，用蠕动泵滴加剩余单体溶液和引发剂溶液。滴加完毕后，反应2 h，旋蒸，得到无色透明状粘稠液体，即为丙烯酸酯共聚物基胶。测得压敏胶的收率为75%，剥离强度为5.295N/25mm。
（3）UV光致可剥离胶的制备：取2 g步骤（2）制备的丙烯酸酯共聚物基胶，在100℃烘箱中烘1分钟进行预处理。将加热后的基胶与双官能团聚氨酯预聚物、光引发剂1-羟环已基苯酮、稀释剂三羟甲基丙烷三丙烯酸酯按质量比为1∶1∶0.025∶0.4比例混合均匀。
（4）UV光致可剥离胶带的制备：将步骤（3）制备的UV光致固化可剥离胶用涂布器均匀涂抹在经电晕处理的长40cm，宽为2.5cm的PET膜内侧，随后将样品在温度为23℃下、相对湿度为65％条件下静置3天老化，制得UV光致可剥离胶带PSA-3。经紫外光照射后可剥离，无残胶。测得光照前PSA-3胶带180°剥离强度为15.298N/25mm，光照后剥离强度为0.499N/25mm。
对比例
（1）双官能团聚氨酯丙烯酸酯预聚物的制备：向四口烧瓶中加入异佛尔酮二异氰酸酯16.674g、二月桂酸二丁烯0.00769g，开启搅拌通氮气保护，升温至50℃，用蠕动泵将聚乙二醇10.063g、对叔丁邻苯二酚0.0386g和150mL的丙酮溶液滴加到烧瓶中，滴加时间为15分钟，滴加完毕后继续反应4 h。最后加入丙烯酸羟乙酯11.612g，继续反应2h，得到双官能团丙烯酸酯封端的聚氨酯丙烯酸酯预聚物。
（2）丙烯酸酯共聚物基胶的制备：分别称取0.680g丙烯酸、1.786g甲基丙烯酸甲酯、1.060g丙烯酸羟乙酯、4.006g丙烯酸丁酯、16.028g丙烯酸异辛酯于烧杯中均匀混合制得单体溶液；称取单体溶液总质量1%的过氧化苯甲酰溶乙醇中制得引发剂溶液；将15%的单体溶液加入四口烧瓶中，滴加1.5%引发剂溶液后搅拌1 h，升温至70℃，用蠕动泵滴加剩余单体溶液和引发剂溶液。滴加完毕后，反应2 h，旋蒸，得到无色透明状粘稠液体，即为丙烯酸酯共聚物基胶。测得压敏胶的收率为92%，剥离强度为6.157N/25mm。
（3）UV光致可剥离胶的制备：取2 g步骤（2）制备的丙烯酸酯共聚物基胶，在100℃烘箱中烘1分钟进行预处理。将加热后的基胶与双官能团聚氨酯丙烯酸酯预聚物、光引发剂1-羟环已基苯酮、稀释剂三羟甲基丙烷三丙烯酸酯按质量比为1∶1∶0.025∶0.4比例混合均匀。
（4）UV光致可剥离胶带的制备：将步骤（3）制备的UV光致固化可剥离胶用涂布器均匀涂抹在经电晕处理的长40cm，宽为2.5cm的PET膜内侧，随后将样品在温度为23℃下、相对湿度为65％条件下静置3天老化，制得UV光致可剥离胶带PSA-4。经紫外光照射后可剥离，有大量残胶。
对UV致可剥离胶带进行测试，硬度根据GB/T1730-1993测定，180°剥离强度测试方法根据GB/T2792-1981测定，测试结果如下表所示：
Figure 645825DEST_PATH_IMAGE002
。
用双官能团异氰酸基封端的聚氨酯预聚物与基胶、光引发剂、稀释剂按一定比例混合涂抹于PET膜上制备的胶带紫外光固化前剥离强度大于8N/25mm，紫外光固化后剥离强度小于1N/25mm，并且无残胶，符合硅晶片切割工艺要求。对比例PSA-4经UV照射后无法剥离，因此UV照射后剥离强度无法测量。
本发明已通过优选的实施方式进行了详尽的说明。本领域普通技术人员通过阅读本发明说明书而对本发明技术方案采取的任何对此产品进行的等效的变换、修饰与改良，在专利范围或范畴内同类或相近物质的替代与使用，均属于本发明专利保护范围。

Claims (6)

1.一种用于硅晶片切割工艺的UV光致可剥离胶带的制备方法，其特征在于，其包括如下步骤：
（1）二异氰酸酯和二月桂酸二丁烯混合搅拌通氮气保护，升温至50℃，将聚乙二醇和对叔丁邻苯二酚的丙酮溶液滴加到二异氰酸酯和二月桂酸二丁烯的混合液中，滴加时间为0.25~0.5 h，滴加完毕后继续反应4~6 h，制得双官能团聚氨酯预聚物；
（2）将丙烯酸、甲基丙烯酸甲酯、丙烯酸羟乙酯、丙烯酸丁酯和丙烯酸异辛酯混合均匀制得单体溶液；将过氧化苯甲酰溶于乙醇中制得引发剂溶液；取单体溶液质量的10~20%和引发剂溶液质量的1~3%混合后搅拌0.9~1.1 h，升温至70℃，再向混合液中同时滴加剩余的单体溶液和引发剂溶液；滴加完毕后，反应2 h，旋蒸后得到无色透明状粘稠液体，制得丙烯酸酯共聚物基胶；所述丙烯酸、甲基丙烯酸甲酯、丙烯酸羟乙酯、丙烯酸异辛酯与丙烯酸丁酯的摩尔比为0.15~0.2∶ 0.4~0.5∶0.2~0.3∶4~4.5∶1；
（3）取步骤（2）制备的丙烯酸酯共聚物基胶，加热进行预处理；将预处理后的丙烯酸酯共聚物基胶与双官能团聚氨酯预聚物、1-羟环已基苯酮和三羟甲基丙烷三丙烯酸酯混合均匀；制得UV光致可剥离胶；双官能团聚氨酯预聚物、1-羟环已基苯酮和三羟甲基丙烷三丙烯酸酯的质量比为1∶1∶0.025~0.03∶0.3~0.4；
（4）将步骤（3）制备的UV光致可剥离胶用涂布器均匀涂抹在经处理的PET膜的内侧，随后将样品在温度为23℃、相对湿度为65％条件下静置3天老化，制得UV光致可剥离胶带。
2.根据权利要求1所述的制备方法，其特征在于，所述步骤（1）中，二异氰酸酯为异佛尔酮二异氰酸酯、甲苯二异氰酸或二苯基甲烷二异氰酸酯。
3.根据权利要求1所述的制备方法，其特征在于，所述步骤（1）中，所述二异氰酸酯和二月桂酸二丁烯的质量比为16.670∶0.007656。
4.根据权利要求1所述的制备方法，其特征在于，所述二异氰酸酯与聚乙二醇的摩尔比为1.5~2∶1。
5.根据权利要求1所述的制备方法，其特征在于，所述步骤（3）中，丙烯酸酯共聚物基胶预处理方式为，在75~85℃加热20~25分钟，然后在95~115℃加热1分钟。
6.根据权利要求1所述的制备方法，其特征在于，所述步骤（2）中，所述剩余单体溶液和引发剂溶液的滴加时间为1.5～2 h。
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