CN102686713B - 固定研磨粒线锯用水溶性切割液、使用其的铸锭切割方法、其回收方法及切割所得的晶圆 - Google Patents
固定研磨粒线锯用水溶性切割液、使用其的铸锭切割方法、其回收方法及切割所得的晶圆 Download PDFInfo
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Abstract
本发明提供了一种切割性能高，可抑制因硅与水反应而产生氢气的固定研磨粒线锯用水溶性切割液、使用其的铸锭切割方法、其回收方法及切割所得的晶圆。该固定研磨粒线锯用水溶性切割液的特征在于：含有(a)式(1)所示的聚醚、(b)二醇(glycol)及分子量为100～300的低分子量二醇醚的至少1种、以及(c)水，(a)与(b)之比为1∶99～50∶50，(c)的含量为5～50重量％；C4H9O(EO)m(AO)nR1 (1)，其中，R1表示氢原子或碳数为1～8的烷基或烯基，EO表示氧伸乙基(oxyethylene group)，AO表示碳数为3～4的氧伸烷基(oxyalkylene group)，m及n分别表示1～20的加成摩尔数。
Description
技术领域
本发明是关于一种用于使用固定研磨粒线锯来切割硅铸锭的固定研磨粒线锯用水溶性切割液、使用其的铸锭切割方法、其回收方法及切割所得的晶圆。
背景技术
先前以来，硅铸锭的切割是使用利用游离研磨粒的带锯或线锯的切割。使用游离研磨粒的带锯或线锯的切割具有以下问题：经切割的晶圆上附着有浆料，后续步骤中的清洗负担较高，此外，难以从硅铸锭的切割使用液中分离出游离研磨粒、油污、切割液，而回收性较差。
对于这些问题，业界开发出一种使用电沉积或树脂黏结剂(resin bond)将研磨粒固定于在线的固定线锯，其具有简化清洗步骤及可从硅铸锭的切割使用液中分离出切割液与油污，而提高回收性的优点。业界提出水或如专利文献1及2的水溶性切割液作为使用该固定线锯切割硅时所使用的切割液。
[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，在使用这些水溶性切割液切割硅的情形时，存在硅与水反应而产生氢气的缺点，并且由于硅与水反应所产生的氢气，而引起发泡或硅凝聚，而使切割液的黏度上升，无法获得目标的切割性能。又存在由于硅与水反应所产生的氢气与切割液本身的发泡性，而其后使用离心分离机的回收性较差的问题。
因此，本发明提供了一种切割性能较高，可抑制因硅与水反应而产生氢气的固定研磨粒线锯用水溶性切割液、使用其的铸锭切割方法、其回收方法及切割所得的晶圆。
为解决上述的问题，本发明的众发明人反复潜心研究，结果发现，通过使用以特定比例含有(a)由特定通式所构成的聚醚、(b)二醇(glycol)及分子量为100～300的低分子量二醇醚的至少一种、以及(c)水的水溶性切割液，即便在用于固定研磨粒线锯的情形时，切割性能也高，并且可抑制因硅与水反应而产生氢气。即，本发明是一种固定研磨粒线锯用水溶性切割液，其特征在于：含有(a)式(1)所示的聚醚、(b)二醇(glycol)及分子量为100～300的低分子量二醇醚的至少一种、以及(c)水，(a)与(b)之比为1∶99～50∶50，(c)的含量为5～50重量％。
C4H9O(EO)m(AO)nR1 (1)
其中，R1表示氢原子或碳数为1～8的烷基或烯基，EO表示氧伸乙基(oxyethylene group)，AO表示碳数为3～4的氧伸烷基(oxyalkylene group)，m及n分别表示1～20的加成摩尔数。
此外，本发明是一种铸锭切割方法、固定研磨粒线锯用水溶性切割液的回收方法、及使用上述铸锭切割方法切割所得的晶圆，上述铸锭切割方法的特征在于：使用上述固定研磨粒线锯用水溶性切割液，通过固定研磨粒线锯来切割硅铸锭；上述固定研磨粒线锯用水溶性切割液的回收方法的特征在于：通过该铸锭切割方法进行铸锭的切割后，使用离心分离机从硅中分离出固定研磨粒线锯用水溶性切割液。
如上所述，根据本发明，可提供一种切割性能较高，并且可抑制因硅与水反应而产生氢气的固定研磨粒线锯用水溶性切割液、使用其的铸锭切割方法、其回收方法及切割所得的晶圆。
具体实施方式
本发明的固定研磨粒线锯用水溶性切割液所使用的(a)聚醚的式(1)中，R1为氢原子或碳数为1～8的烷基或烯基，EO为氧伸乙基，AO为碳数为3或4的氧伸烷基，m及n分别表示1～20的加成摩尔数。又，式(1)所示的聚醚可通过无规聚合而聚合，也可以通过嵌段聚合而聚合。式(1)所示的聚醚的重量平均分子量优选为200～2,000。如此将聚醚限定为式(1)所示的聚伸烷二醇丁醚是因为：若使用甲基或乙基等的醚，则在固定研磨粒线锯中无法获得充分的切割性能。作为此种聚伸烷二醇丁醚，例如有Yukanol 50MB-5(日油公司制造)等。
又，(b)的二醇优选为具有2个OH基，且分子量或重量平均分子量为60～3,500，例如有单乙二醇、二乙二醇、三乙二醇、单丙二醇、二丙二醇、三丙二醇、己二醇及聚乙二醇、聚丙二醇等聚伸烷二醇等。并且，(b)的低分子量二醇醚的分子量为100～300即可，例如有二乙二醇单甲醚、二乙二醇单丁醚及二乙二醇单己醚等。
该(b)是包含(b1)式(2)所示的聚伸烷二醇、与(b2)除(b1)以外的二醇及分子量为100～300的低分子量二醇醚的至少一种，(b1)的含量优选相对于水溶性切割液总体为0.01～5.0重量％。式(2)中，x、y、z分别表示1～20的加成摩尔数。式(2)所示的聚醚的重量平均分子量优选为1,000～3,000。又，使(b1)为0.01～5.0重量％的原因在于，若未达0.01重量％则无法改善发泡问题，回收性会变差，若为5.0重量％以上则切割性能会变差。(b1)的含量更佳为0.1～2.0重量％。
HO(C3H6O)x(C2H4O)y(C3H6O)zH (2)
(x、y、z分别表示1～20的加成摩尔数。)
本发明的固定研磨粒线锯用水溶性切割液可根据需要而添加(d)分散剂。作为所使用的分散剂，有：在烯丙醇、顺丁烯二酸酐的共聚物中接枝聚合聚氧伸烷基单烷基醚的聚羧酸或其盐，在烯丙醇、顺丁烯二酸酐、苯乙烯的共聚物中接枝聚合聚氧伸烷基单烷基醚的聚羧酸或其盐，萘磺酸缩合物或其盐等，通常作为分散剂，可使用市售的相关产品。分散剂的含量优选为0.1～5.0重量％。在0.1～5.0重量％时，切割时切屑的分散性良好，可抑制由于发泡而引起的切割性能及回收性能的下降。(d)分散剂的含量更佳为0.1～1重量％。
在本发明的固定研磨粒线锯用水溶性切割液中，若(a)与(b)之比为1∶99～50∶50，则抑制因硅与水反应而产生氢气的效果较高，不易发生由于氢气的产生而引起的发泡或硅凝聚，可使黏度变化变少。又，对工作机械中所使用的树脂零件的影响也较少，可提高切割性能。(a)与(b)之比更佳为5∶95～30∶70。
在本发明的固定研磨粒线锯用水溶性切割液中，若(c)水为5～50重量％，则不会有切割时的引火性问题，将切割时的发热进行冷却的能力较高，发热所引起的水分蒸发量较少，故可提高切割性能。又，可抑制切割中的晶圆表面的干燥，降低后续步骤的清洗步骤的负担。水分量更佳为5～40重量％。
本发明的固定研磨粒线锯用水溶性切割液根据需要也可以添加防锈剂、防腐剂、香料、染料等。
本发明的固定研磨粒线锯用水溶性切割液在作为半导体元件或太阳电池的材料的硅晶圆的切割时，可使用固定研磨粒线锯作为切割工具，使用多线锯作为切割加工机。
本发明的固定研磨粒线锯用水溶性切割液可在切割后，使用离心分离机将硅与水溶性切割液分离并回收。
使用本发明的铸锭的切割方法切割所得的晶圆与先前的使用固定研磨粒线锯用水溶性切割液切割所得的晶圆相比，可获得表面粗糙度、起伏度良好的晶圆，可用作半导体元件用或太阳电池用晶圆。
[实施例]
以下，对本发明的固定研磨粒线锯用水溶性切割液的实施例进行说明，但本发明并不限于实施例。首先，根据表1至表4的调配量，使用通常的方法将这些混合，借此获得实施例1至实施例12的固定研磨粒线锯用水溶性切割液、及比较例1至比较例10的固定研磨粒线锯用水溶性切割液。
[表1]
*1：(聚乙二醇200、日油公司制造)
*2：(Yukanol 50MB-5、日油公司制造)
*3：(Malialim AKM-0531、日油公司制造)
*4：(Lavelin FAN、第一工业制药公司制造)
*5：(Adeka Pluronic 17R4、ADEKA制造)
[表2]
*6：(聚乙二醇2000、日油公司制造)
[表3]
*7：平均分子量为500
[表4]
*7：平均分子量为500
*8：平均分子量为500
*9：平均分子量为500
*10：(Epan 450、第一工业制药制造)
(切割试验)
以下，使用实施例1至实施例12的固定研磨粒线锯用水溶性切割液、及比较例1至比较例10的固定研磨粒线锯用水溶性切割液，进行切割试验，测定切割距离。切割试验是在以下条件下进行：线锯试验机：3032-4(WELL制造)，线：芯线0.12mm、金刚石直径12-25μm(旭金刚石公司(Asahi Diamond Industrial)制造)，线速度：200m/min，加工负荷：30g，加工时间：30分钟，加工工件：20mm×30mm×30mm，试验温度：25℃。将结果示于表5及表6。由表5及表6可知，本实施例的固定研磨粒线锯用水溶性切割液的切割性能良好。
[表5]
| 切割液 | 切割距离(mm) |
| 实施例1 | 12.8 |
| 实施例2 | 13.3 |
| 实施例3 | 13.5 |
| 实施例4 | 14.3 |
| 实施例5 | 13.8 |
| 实施例6 | 11.9 |
| 实施例7 | 13.3 |
| 实施例8 | 12.8 |
| 实施例9 | 13.6 |
| 实施例10 | 13.3 |
| 实施例11 | 13.8 |
| 实施例12 | 14.0 |
[表6]
| 切割液 | 切割距离(mm) |
| 比较例1 | 10.2 |
| 比较例2 | 6.7 |
| 比较例3 | 6.2 |
| 比较例4 | 8.2 |
| 比较例5 | 9.8 |
| 比较例6 | 10.5 |
| 比较例7 | 11.1 |
| 比较例8 | 10.0 |
| 比较例9 | 10.8 |
| 比较例10 | 11.5 |
(黏度及气体产生试验)
继而，假定有使用固定研磨粒线锯切割单晶硅铸锭时混入的活性硅屑，而在实施例1至实施例12的固定研磨粒线锯用水溶性切割液、以及比较例1至比较例3及比较例5至比较例9的固定研磨粒线锯用水溶性切割液中，添加20重量％的硅粉(粒径约为5μm)，使用行星式球磨机进行粗粉碎，使用BL型旋转黏度计(转子No.160rpm)测定其在25℃下的黏度(黏度1)。其后，将其放入可密封的聚乙烯袋(厚度为0.04mm)并进行抽气，确认在50℃下保存24小时后的硅反应气体量，并且测定其在25℃下的黏度(黏度2)。粗粉碎是在以下条件下进行：杯：500ml氧化锆罐，介质：ψ2mm氧化锆珠，试样量：200ml，介质量：200ml，转数：250rpm，时间：30分钟。反应气体量的确认是在以下条件下进行：聚乙烯袋：透明封口袋(日本高科技(股)(Nihon Hitech)制造)，厚度：0.04mm，确认方法：目视(聚乙烯袋的膨胀状况)。将结果示于表7及表8。由表7及表8可知，本发明的固定研磨粒线锯用水溶注切割液是硅与水的反应气体量极少，黏度变化也较小。
[表7]
| 切割液 | 黏度1(mPa·s) | 反应气体量 | 黏度2(mPa·s) |
| 实施例1 | 60.0 | N.D. | 60.0 |
| 实施例2 | 15.0 | N.D. | 15.0 |
| 实施例3 | 40.0 | N.D. | 40.0 |
| 实施例4 | 25.0 | N.D. | 25.0 |
| 实施例5 | 25.0 | N.D. | 25.0 |
| 实施例6 | 20.0 | 产生(小) | 40.0 |
| 实施例7 | 20.0 | N.D. | 20.0 |
| 实施例8 | 45.0 | N.D. | 50.0 |
| 实施例9 | 20.0 | N.D. | 20.0 |
| 实施例10 | 30.0 | N.D. | 40.0 |
| 实施例11 | 25.5 | N.D. | 26.0 |
| 实施例12 | 24.0 | N.D. | 25.0 |
[表8]
| 切割液 | 黏度1(mPa·s) | 反应气体量 | 黏度2(mPa·s) |
| 比较例1 | 50.0 | 产生(大) | 100＜ |
| 比较例2 | 15.0 | 产生(大) | 100＜ |
| 比较例3 | 3.5 | 产生(大) | 20.0 |
| 比较例5 | 21.0 | 产生(大) | 100＜ |
| 比较例6 | 9.5 | 产生(大) | 100＜ |
| 比较例7 | 30.0 | 产生(大) | 60.0 |
| 比较例8 | 60.0 | 发生(大) | 100＜ |
| 比较例9 | 60.0 | 产生(大) | 100＜ |
(清洗试验)
继而，假定有使用固定研磨粒线锯切割单晶硅铸锭时混入的活性硅屑，而在实施例1至实施例12的水溶性切割液、以及比较例3及比较例6的水溶性切割液中添加20重量％的硅粉(粒径约为5μm)，令使用行星式球磨机在与上述(黏度及气体产生试验)粗粉碎相同的条件下进行粗粉碎的液体，附着于3英时硅晶圆的所有面上，一直垂直地维持晶圆，并在室温下静置24小时。其后，用流水清洗，确认清洗性。将结果示于表9。由表9可知，本发明的固定研磨粒线锯用水溶性切割液在后续步骤中的清洗良好。
[表9]
| 切割液 | 清洗性 |
| 实施例1 | ○ |
| 实施例2 | ○ |
| 实施例3 | ○ |
| 实施例4 | ○ |
| 实施例5 | ○ |
| 实施例6 | ○ |
| 实施例7 | ○ |
| 实施例8 | ○ |
| 实施例9 | ○ |
| 实施例10 | ○ |
| 实施例11 | ○ |
| 实施例12 | ○ |
| 比较例3 | × |
| 比较例6 | × |
<评价方法>
○：可全部清洗
△：有部分清洗不均
×：所有面清洗不良
(发泡试验)
继而，假定在切割中发泡或回收中发泡，而将实施例1至12的固定研磨粒线锯用水溶性切割液，以及比较例1、比较例2、及比较例6的固定研磨粒线锯用水溶性切割液在有塞式100量筒中加入至50，在塞紧后激烈震荡。确认其后的发泡量及直至能看见液表面为止的消泡时间。将结果示于表10。由表10可知，本发明的水溶性切割液的发泡较少而良好。
[表10]
| 切割液 | 发泡量(·) | 消泡时间 |
| 实施例1 | 2 | 10秒 |
| 实施例2 | 3 | 20秒 |
| 实施例3 | 0 | 0 |
| 实施例4 | 0 | 0 |
| 实施例5 | 0 | 0 |
| 实施例6 | 4 | 55秒 |
| 实施例7 | 4 | 40秒 |
| 实施例8 | 3 | 20秒 |
| 实施例9 | 4 | 10秒 |
| 实施例10 | 4 | 20秒 |
| 实施例11 | 6 | 20秒 |
| 实施例12 | 1 | 10秒 |
| 比较例1 | 15 | 1分钟以上 |
| 比较例2 | 15 | 1分钟以上 |
| 比较例6 | 10 | 1分钟以上 |
Claims (5)
1.一种固定研磨粒线锯用水溶性切割液，其特征在于：含有（a）式（1）所示的聚醚、（b）分子量或重量平均分子量为60～3,500的二醇及分子量为100～300的低分子量二醇醚的至少一种、以及（c）水；
（a）与（b）的重量比为1：99～50：50，（c）的含量为5～50重量%；
C4H9O（EO）m（AO）nR1 （1）
其中，R1表示氢原子或碳数为1～8的烷基或烯基，EO表示氧伸乙基（oxyethylene group），AO表示碳数为3～4的氧伸烷基（oxyalkylene group），m及n分别表示1～20的加成摩尔数。
2.根据权利要求1所述的固定研磨粒线锯用水溶性切割液，其中，该（b）包含：（b1）式（2）所示的聚伸烷二醇、与（b2）除（b1）以外的分子量或重量平均分子量为60～3,500的二醇及分子量为100～300的低分子量二醇醚的至少一种；（b1）的含量相对于水溶性切割液总体为0.01～5.0重量%；
HO（C3H6O）x（C2H4O）y（C3H6O）zH （2）
其中，x、y、z分别表示1～20的加成摩尔数。
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割液，其进一步含有0.1～5.0重量%的（d）分散剂。
4.一种铸锭切割方法，其特征在于：
使用权利要求1至3中任一项所述的固定研磨粒线锯用水溶性切割液，通过固定研磨粒线锯来切割硅铸锭。
5.一种固定研磨粒线锯用水溶性切割液的回收方法，其特征在于：
使用权利要求4所述的铸锭切割方法进行铸锭的切割后，使用离心分离机从硅中分离出固定研磨粒线锯用水溶性切割液。
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| JP2009-258864 | 2009-11-12 | ||
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| PCT/JP2010/069716 WO2011058929A1 (ja) | 2009-11-12 | 2010-11-05 | 固定砥粒ワイヤーソー用水溶性切断液、それを用いたインゴットの切断方法、そのリサイクル方法及び切断によって得られるウェハー |
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| CN201080051078.6A Expired - Fee Related CN102686713B (zh) | 2009-11-12 | 2010-11-05 | 固定研磨粒线锯用水溶性切割液、使用其的铸锭切割方法、其回收方法及切割所得的晶圆 |
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| JP (1) | JP5764067B2 (zh) |
| KR (1) | KR20130001210A (zh) |
| CN (1) | CN102686713B (zh) |
| MY (1) | MY161383A (zh) |
| TW (1) | TWI484029B (zh) |
| WO (1) | WO2011058929A1 (zh) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102952621B (zh) * | 2011-08-19 | 2015-01-21 | 台湾水再生科技股份有限公司 | 硅晶圆切割研磨废弃物的回收处理方法及其设备 |
| WO2013061695A1 (ja) * | 2011-10-24 | 2013-05-02 | パレス化学株式会社 | 固定砥粒ワイヤーソー用水溶性切断液、それを用いた切断方法及びそのリサイクル方法 |
| CN102876441B (zh) * | 2012-09-24 | 2013-10-30 | 广西大学 | 环境友好的钛合金微乳化切削液 |
| JP2015536379A (ja) | 2012-12-06 | 2015-12-21 | ダウ グローバル テクノロジーズ エルエルシー | 水溶性切削流体組成物 |
| KR200481449Y1 (ko) | 2014-07-25 | 2016-10-04 | 삼성중공업 주식회사 | 다기능 루버 |
| CN105235084B (zh) * | 2015-09-30 | 2017-07-18 | 浙江辉弘光电能源有限公司 | 一种硅片切割机用切削液去水装置 |
| CN105273823B (zh) * | 2015-11-27 | 2018-06-08 | 上海应用技术学院 | 一种多线硅片切割水溶性切削液及其制备方法 |
| JP6860266B2 (ja) * | 2017-03-17 | 2021-04-14 | 出光興産株式会社 | 脆性材料加工液 |
| CN111826225A (zh) * | 2019-04-17 | 2020-10-27 | 陕西省石油化工研究设计院 | 一种钐钴永磁加工专用冷却液及其制备方法 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1746281A (zh) * | 2004-09-06 | 2006-03-15 | 大连广汇化学有限公司 | 环保型水基合成切削液 |
| CN101240217A (zh) * | 2008-02-29 | 2008-08-13 | 益田润石（北京）化工有限公司 | 微乳型金属切削液组合物 |
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| US6383991B1 (en) * | 1998-04-03 | 2002-05-07 | Kao Corporation | Cutting oil composition |
| JP2002053788A (ja) * | 2000-08-09 | 2002-02-19 | Mitsubishi Pencil Co Ltd | 水性ボールペン用インキ組成物 |
| JP4497767B2 (ja) * | 2001-09-06 | 2010-07-07 | ユシロ化学工業株式会社 | 固定砥粒ワイヤソー用水溶性加工液組成物 |
| WO2005037968A1 (ja) * | 2003-10-16 | 2005-04-28 | Mitsubishi Denki Kabushiki Kaisha | シリコンインゴット切断用スラリー及びそれを用いるシリコンインゴットの切断方法 |
| JP4481898B2 (ja) * | 2005-07-25 | 2010-06-16 | ユシロ化学工業株式会社 | 水性砥粒分散媒組成物 |
| WO2009133612A1 (ja) * | 2008-04-30 | 2009-11-05 | パレス化学株式会社 | 水溶性切断液組成物、水溶性切断液及びその水溶性切断液を用いた切断方法 |
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- 2010-11-05 CN CN201080051078.6A patent/CN102686713B/zh not_active Expired - Fee Related
- 2010-11-05 KR KR1020127016097A patent/KR20130001210A/ko not_active Application Discontinuation
- 2010-11-05 WO PCT/JP2010/069716 patent/WO2011058929A1/ja active Application Filing
- 2010-11-05 MY MYPI2012001959A patent/MY161383A/en unknown
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1746281A (zh) * | 2004-09-06 | 2006-03-15 | 大连广汇化学有限公司 | 环保型水基合成切削液 |
| CN101240217A (zh) * | 2008-02-29 | 2008-08-13 | 益田润石（北京）化工有限公司 | 微乳型金属切削液组合物 |
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| JP特开2007-31502A 2007.02.08 |
Also Published As
| Publication number | Publication date |
|---|---|
| TW201134936A (en) | 2011-10-16 |
| TWI484029B (zh) | 2015-05-11 |
| JPWO2011058929A1 (ja) | 2013-03-28 |
| CN102686713A (zh) | 2012-09-19 |
| JP5764067B2 (ja) | 2015-08-12 |
| MY161383A (en) | 2017-04-14 |
| KR20130001210A (ko) | 2013-01-03 |
| WO2011058929A1 (ja) | 2011-05-19 |
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