CN105121614A - 固定研磨粒线锯用水溶性切削液、使用其的铸锭的切削方法及由其所得的电子材料用基板 - Google Patents

固定研磨粒线锯用水溶性切削液、使用其的铸锭的切削方法及由其所得的电子材料用基板 Download PDF

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CN105121614A
CN105121614A CN201480020233.6A CN201480020233A CN105121614A CN 105121614 A CN105121614 A CN 105121614A CN 201480020233 A CN201480020233 A CN 201480020233A CN 105121614 A CN105121614 A CN 105121614A
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abrasive grain
scroll saw
soluble metalworking
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CN105121614B (zh
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铃木清史
高梨慎也
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Palace Chemical Co Ltd
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Abstract

本发明提供一种起泡少、切削性能高的固定研磨粒线锯用水溶性切削液、使用其的铸锭的切削方法及由其所得的电子材料用基板。一种固定研磨粒线锯用水溶性切削液，其含有化学式(1)表示的(a)2,4,7,9-四甲基-5-癸炔-4,7-二醇的伸烷基加成物。又，一种铸锭的切削方法及由上述切削方法所得的电子材料用基板，上述铸锭的切削方法，是使用上述固定研磨粒线锯用水溶性切削液，通过固定研磨粒线锯切削铸锭而获得作为电子材料基板的晶圆。

Description

固定研磨粒线锯用水溶性切削液、使用其的铸锭的切削方法及由其所得的电子材料用基板
技术领域
本发明涉及一种用以切削硅铸锭的固定研磨粒线锯用水溶性切削液、使用其的铸锭的切削方法及由其所得的电子材料用基板。
背景技术
先前以来，电子材料用基板的晶圆是通过使用有游离研磨粒的利用带锯(バンドソー)或线锯的切削而获得。然而，使用有游离研磨粒的切削存在如下问题：浆料附着于经切削的晶圆，后续步骤中的洗净负荷高，又，不易自使用液将游离研磨粒、沉淀物(スラッジ)、切削液分离，再利用性差。
针对这些问题，开发出利用电镀或树脂黏合剂将研磨粒固定于在线的固定研磨粒线锯，具有简化洗净步骤、或通过将切削液与沉淀物分离而提高再利用性的优点。作为使用此固定研磨粒线锯切削为电子材料用基板的晶圆时所使用的切削液，提出了水或例如专利文献1及2中的水溶性切削液。
专利文献1：日本特开2003-82334号公报
专利文献2：日本特开2009-57423号公报。
发明内容
然而，近年来，为了提高质量方面及切削速度，而使线速度逐步加快，存在如下问题：若使用如专利文献1及2所揭示的水溶性切削液切削成为电子材料用基板的铸锭，则所使用的水溶性切削液会起泡，而无法获得质量良好的晶圆。
因此，本发明提供一种起泡少、切削性能高的固定研磨粒线锯用水溶性切削液、使用其的铸锭的切削方法及由其所得的电子材料用基板。
为了达成以上目的，本发明人等努力进行反复研究，结果发现通过使用含有(a)2,4,7,9-四甲基-5-癸炔-4,7-二醇(2,4,7,9―テトラメチル－5－デシン－4,7－ジオール)的伸烷基(アルキレン)加成物的水溶性切削液，即便在用于固定研磨粒线锯时，亦可进行起泡少、切削性能高的切削，从而完成本发明。即，本发明涉及一种固定研磨粒线锯用水溶性切削液，其特征在于：含有下述化学式(1)表示的(a)2,4,7,9-四甲基-5-癸炔-4,7-二醇的伸烷基加成物。
[化学式1]
化学式(1)
(其中，R表示分别相同或不同的碳数1～4的伸烷基，m1+m2+n1+n2表示伸烷基加成物的总加成摩尔数，为1以上的整数)。
又，本发明涉及一种铸锭的切削方法、及由上述切削方法所得的电子材料用基板，上述铸锭的切削方法的特征在于：使用上述固定研磨粒线锯用水溶性切削液，通过固定研磨粒线锯切削铸锭而获得作为电子材料用基板的晶圆。
如上所述，根据本发明，可提供一种起泡少、切削性能高的固定研磨粒线锯用水溶性切削液、使用其的铸锭的切削方法及由其所得的电子材料用基板。
具体实施方式
本发明的固定研磨粒线锯用水溶性切削液中使用的(a)成分即2,4,7,9-四甲基-5-癸炔-4,7-二醇的伸烷基加成物具有下述化学式(1)表示的结构。
[化学式2]
化学式(1)
(其中，R表示分别相同或不同的碳数1～4的伸烷基，m1+m2+n1+n2表示伸烷基加成物的总加成摩尔数，为1以上的整数)。
于上述化学式(1)中，作为加成于2,4,7,9-四甲基-5-癸炔-4,7-二醇上的环氧烷，只要为碳数1～4的环氧烷即可，具体而言，特别优选为环氧乙烷单体、或环氧乙烷及环氧丙烷两者。
又，所加成的环氧烷是以无规聚合加成，因此若上述化学式(1)的4个伸烷基(-OR-)均为碳数1～4的伸烷基，则可相同或不同，优选为4个伸烷基为乙烯单体、或乙烯及丙烯两者中任一者，特别优选为4个伸烷基均为乙烯。
于上述化学式(1)中，伸烷基加成物的加成摩尔数以总量计为1摩尔以上，优选为1～20摩尔，更优选为4～12摩尔。尤其是，于所加成的伸烷基加成物为环氧乙烷单体时，优选为环氧乙烷4～12摩尔，更优选为4～8摩尔，特别优选为4～6摩尔。又，于所加成的伸烷基加成物为环氧乙烷及环氧丙烷时，优选为环氧乙烷4～8摩尔及环氧丙烷2～4摩尔。
(a)成分可单独使用1种，亦可并用2种以上，作为(a)成分的添加量，相对于水溶性切削液，优选为0.01～5.0重量％，更优选为0.05～2.0重量％。若(a)的添加量未达0.01重量％，则消泡效果小、水溶性切削液的动态表面张力较高，因此存在水溶性切削液难以进入加工部位而使切削质量恶化的倾向，若超过5.0重量％，则存在水溶性切削液难以获得如显示消泡效果的调配平衡的情况。
本发明的固定研磨粒线锯用水溶性切削液，优选为除了上述(a)成分，亦含有下述所示的(b)、(c)及(d)成分。通过含有(b)、(c)及(d)成分，可控制固定研磨粒线与加工物的间的润滑性，提高固定研磨粒线的工具寿命。
于本发明中，(b)成分优选为羧酸、巯基苯并噻唑、苯并噻唑基硫代乙酸(ベンゾチアゾリルチオ酢酸)及苯并噻唑基硫代丙酸(ベンゾチアゾリルチオプロピオン酸)中的至少1种以上。作为羧酸，只要具有1个以上的COOH基即可，例如可列举：辛酸、己酸、月桂酸、油酸、柠檬酸、顺丁烯二酸、反丁烯二酸、己二酸、间苯二甲酸、苹果酸、酒石酸、十二烷二酸及癸二酸等。(b)成分可单独使用1种，亦可并用2种以上。
又，(c)成分优选为胺、氢氧化钠及氢氧化钾中的至少1种以上，更优选为胺。作为胺，可列举：单乙醇胺、二乙醇胺、三乙醇胺、单异丙醇胺、二异丙醇胺、三异丙醇胺、二环己基胺、三羟甲基丙烷聚(氧化丙烯)三胺、N,N-双(2羟基乙基)-N-环己基胺及间二甲苯二胺(メタキシレンジアミン)的伸烷基加成物等。(c)成分可单独使用1种，亦可并用2种以上。
关于(b)成分与(c)成分，若均可溶于水，则可以任意比例含有，优选为(c)成分为将(b)成分中和的量或为此量以上，较理想的是(b)成分与(c)成分的总和为5重量％以下。
又，(d)成分优选为二醇、聚伸烷基二醇(ポリアルキレングリコール)、二醇醚、聚伸烷基二醇醚、甘油及甘油的伸烷基加成物中的至少1种以上。二醇只要具有2个OH基即可，例如可列举：单乙二醇、二乙二醇、三乙二醇、单丙二醇、二丙二醇、三丙二醇及己二醇等，作为聚伸烷基二醇，例如可列举：聚乙二醇、聚丙二醇、聚氧乙烯聚氧丙烯的共聚物及聚氧乙烯聚氧丁烯的共聚物。作为二醇醚，例如可列举：二乙二醇单甲醚、二乙二醇单丁醚及二乙二醇单己醚等。作为聚氧伸烷基二醇醚，例如可列举：聚氧乙烯单甲醚、聚氧丙烯单甲醚及聚氧乙烯聚氧丙烯共聚物的单丁醚。作为甘油的伸烷基加成物，例如可列举：甘油的乙烯加成物、丙烯加成物及乙烯丙烯共聚合加成物。(d)成分可单独使用1种，亦可并用2种以上。(d)成分的含量只要可溶于水即可，优选为70重量％以下。
又，本发明的固定研磨粒线锯用水溶性切削液，亦可视需要添加防锈剂、防腐剂、香料、染料等。
使用本发明的固定研磨粒线锯用水溶性切削液，通过固定研磨粒线锯切削铸锭，由此可获得质量良好的电子材料用基板。
在用于本发明的固定研磨粒线锯中，成为母线的线可为铁制或不锈钢制，亦可为经镀铜者、经镀铂者。作为固着于在线的研磨粒，可使用市售的研磨粒，优选为金刚石、氮化硼。为了将研磨粒固着于在线，优选为利用镍等金属的电镀或使用树脂的树脂附着。
又，作为用于本发明的切削机，只要为市场上贩卖的多线锯加工机，则并无特别限定，优选为固定研磨粒线锯专用多线锯加工机。
又，作为用于本发明的铸锭，只要为用以制造电子材料用基板的铸锭，则并无特别限定，例如优选为使用使硅、蓝宝石、水晶、石英、碳化硅、钽酸锂、氮化镓及砷化镓等结晶成长并高纯度化而成的铸锭。
如上所述，于通过固定研磨粒线锯自铸锭切削作为电子材料铜基板的晶圆时，通过使用本发明的固定研磨粒线锯用水溶性切削液，可使起泡少，又，可提高切削性能。
实施例
继而，对本发明的固定研磨粒线锯用水溶性切削液的实施例进行说明，但本发明并不限定于此。首先，依据表1及表2表示的各成分的调配量，通过常法将这些混合，由此获得实施例1至实施例9的固定研磨粒线锯用水溶性切削液、以及比较例1至比较例4的固定研磨粒线锯用水溶性切削液。
[表1]
[表2]
(起泡试验)
其次，假定切削中的起泡，将50ml的实施例1至实施例9的固定研磨粒线锯用水溶性切削液、及比较例1至比较例4的固定研磨粒线锯用水溶性切削液添加至有栓式100ml量筒中，塞住栓后，剧烈摇晃，确认刚摇晃后的初期起泡量及起泡消失为止的消泡时间。将其结果示于表3。再者，稳定性是在25℃静置1周而判定，○：于1周无分离、沉淀，△：于4日以上且未达1周发生分离、沉淀，×：于未达4日发生分离、沉淀。
[表3]
根据表3可知，比较例2的切削液的稳定性较差，比较例3及4的切削液的起泡较多，消泡时间亦超过60秒。相对于此，可知本发明的固定研磨粒线锯用水溶性切削液的起泡较少，较良好。再者，稳定性较差的比较例2中，已分离的(a)成分会附着于装置、配管内而引起污染，或者因自切削液去除(a)成分而使切削质量恶化，从而难以用作切削液。
(切削试验)
其次，使用实施例1至实施例9的固定研磨粒线锯用水溶性切削液、以及比较例1至比较例4的固定研磨粒线锯用水溶性切削液，于表4的条件进行切削试验，测定经切削的晶圆的剖面曲线的最底部高度(PV)。将结果示于表5。
[表4]
[表5]
根据表5可知，比较例1及2的切削液无法切削铸锭，比较例3及4的切削液的PV值较大，无法形成良好剖面。相对于此，可知本实施例的固定研磨粒线锯用水溶性切削液的PV值较小，切削性能良好。

Claims (7)

1.一种固定研磨粒线锯用水溶性切削液，含有下述化学式(1)表示的(a)2,4,7,9-四甲基-5-癸炔-4,7-二醇的伸烷基加成物，
[化学式1]
其中，R表示分别相同或不同的碳数1～4的伸烷基，m1+m2+n1+n2表示伸烷基加成物的总加成摩尔数，为1以上的整数。
2.根据权利要求1所述的固定研磨粒线锯用水溶性切削液，其中，所述(a)的伸烷基加成物的总加成摩尔数为4～12摩尔。
3.根据权利要求1或2所述的固定研磨粒线锯用水溶性切削液，其中，所述(a)的含量为0.01～5.0重量％。
4.根据权利要求1至3中任一项所述的固定研磨粒线锯用水溶性切削液，其进而含有(b)羧酸、巯基苯并噻唑、苯并噻唑基硫代乙酸及苯并噻唑基硫代丙酸中的至少1种以上，及(c)胺、氢氧化钠及氢氧化钾中的至少1种以上。
5.根据权利要求1至4中任一项所述的固定研磨粒线锯用水溶性切削液，其进而含有(d)二醇、聚伸烷基二醇、二醇醚、聚伸烷基二醇醚、甘油及甘油的伸烷基加成物中的至少1种以上。
6.一种铸锭的切削方法，使用根据权利要求1至5中任一项所述的固定研磨粒线锯用水溶性切削液，通过固定研磨粒线锯切削铸锭而获得电子材料用基板。
7.一种电子材料用基板，是通过根据权利要求6所述的铸锭的切削方法而获得。
CN201480020233.6A 2013-04-05 2014-03-26 固定研磨粒线锯用水溶性切削液、使用其的铸锭的切削方法及由其所得的电子材料用基板 Active CN105121614B (zh)

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