CN101921648B - 水性切削液和浆 - Google Patents
水性切削液和浆 Download PDFInfo
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- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
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Abstract
本发明涉及水性切削液和浆,含有0.01~20wt%改性有机硅的水性切削液与磨料结合形成水性切削浆,其具有磨料的分散稳定性、粘度稳定性、以及较高的加工精度的优点。
Description
技术领域
本发明涉及一种在加工件的切削中起辅助作用的水性切削液和浆,加工件包括用于半导体、太阳能电池和其他工业领域的硅晶、石英、水晶、化合物半导体、磁性合金等的锭材。尤其是,涉及一种含有水性切削液和磨料的水性切削浆,其具有磨料分散稳定性、粘度稳定性以及与现有技术相比具有更高的加工精度的优点。
背景技术
一种已知的切削坚硬和脆性材料的锭材的方法是使用线锯或切断轮。在使用线锯的切削方法中,为了达到在切削工具和加工件之间进行润滑,去除摩擦热,并清除碎屑的目的,切削液通常在切削操作过程中加入。切削液包括含有矿物油和添加剂的油基切削液,含有聚乙二醇或聚丙二醇作为主要组分的二醇基切削液,以及表面活性剂水溶液形式的水性切削液。然而这些切削液有缺点。油基切削液在切削点的冷却效果差。如果加工件或工具被油基切削液污染,需要有机溶剂清洗液,从环境角度考虑是不希望的。二醇基切削液和水性切削液在切削操作中的粘度稳定性以及磨料的分散稳定性方面差。
为了解决这些问题,JP 2000-327838A提出了一种基于多元醇或衍生物的切削液,在其中加入斑脱土、纤维素和云母,从而有利于磨料的分散性。JP2006-278773A公开了一种水性切削液,其含有二醇和/或水密性醚和zeta-电位至少为0mV的颗粒,典型的是氧化铝。JP 2007-031502A公开了一种含有二醇、二醇醚和水的水性切削液。
在工业中,半导体硅晶片从硅锭切削而来,其直径已经从200mm增加到300mm,以及甚至到450mm。太阳能电池以及类似领域中所用的硅晶片变得越来越薄。需要一种能够满足直径和厚度变化需要的水性切削液。需要具有一种比现有技术加工精度更高的水性切削液。
引用列表
专利文献1:JP 2000-327838A(US 2003100455)
专利文献2:JP 2006-278773A
专利文献3:JP 2007-031502A(EP1752521,CN1903968)
发明内容
本发明的一个目的是提供一种水性切削液和浆,其具有磨料的分散稳定性、粘度稳定性以及与现有技术相比具有更高的加工精度的优点。
发明人已经发现通过向水性切削液中加入0.01~20重量%的改性有机硅(A)可以解决这个突出难题。
一方面,本发明提供一种含有(A)0.01~20重量%的改性有机硅的水性切削液。
改性有机硅通常选自聚醚、氨基、羧基、以及环氧基改性的有机硅。
在这种情况下,改性有机硅优选由下述平均组成式(1)表示,
R1 pR2 qR3 rSiO(4-p-q-r)/2 (1)
其中,R1为-(CR4 2)nX,R4为氢原子,具有1~20个碳原子且无脂肪族不饱和键的、取代或未取代的单价烃基,或羟基,n为1~20的整数,X为选自由氨基、羧基和环氧基构成的组中的官能团,R2为具有1~20个碳原子且无脂肪族不饱和键的、取代或未取代的单价烃基,R3为具有如下通式的有机基团:-CfH2fO(CgH2gO)hR5,R5为氢原子,无脂肪族不饱和键的、取代或未取代的单价烃基,或乙酰基,f为2~12的正数,g为2~4的正数,h为1~200的正数,且p,q和r为满足0≤p<2.5,0.01≤q<2.5,0≤r<2.5且0.05<p+q+r≤3.0的数。
切削液可进一步含有(B)1~20重量%的水,和(C)60~98.99重量%的亲水性多元醇和/或其衍生物。亲水性多元醇或其衍生物(C)优选在20℃具有至少为5重量%的水中溶解度,和具有达到0.01mmHg的蒸汽压。
另一方面,本发明提供了一种含有100重量份如上定义的水性切削液和50~200重量份磨料的水性切削浆。
本发明的有益效果
含有0.01~20wt%改性有机硅的水性切削液具有磨料的分散稳定性、浆形态时的粘度稳定性以及与现有技术相比具有更高的加工精度的优点。
具体实施方式
本发明的水性切削液被定义为含有0.01~20重量%改性有机硅(A)。适合的改性有机硅包括聚醚改性有机硅、氨基改性有机硅、羧基改性有机硅和环氧基改性有机硅。尤其是优选聚醚和氨基改性有机硅。含有改性有机硅对于显著降低水性切削液的动态接触角是有效的,导致了切削性能的显著提高。
在这种情况下,改性有机硅(A)优选由下述平均组成式(1)表示,
R1 pR2 qR3 rSiO(4-g-q-r)/2 (1)
其中,R1为-(CR4 2)nX,R4为氢原子,具有1~20个碳原子且无脂肪族不饱和键的、取代或未取代的单价烃基,或羟基,n为1~20的整数,X为选自由氨基、羧基和环氧基构成的组中的官能团,R2为具有1~20个碳原子且无脂肪族不饱和键的、取代或未取代的单价烃基,R3为具有如下通式的有机基团:-CfH2fO(CgH2gO)hR5,R5为氢原子,无脂肪族不饱和键的、取代或未取代的单价烃基,或乙酰基,f为2~12的正数,g为2~4的正数,h为1~200的正数,且p,q和r为满足0≤p<2.5,0.01≤q<2.5,0≤r<2.5且0.05<p+q+r≤3.0的数。
R2的例子包括烷基例如甲基、乙基、丙基、丁基、戊基、己基、庚基、辛基、壬基和癸基,环烷基例如环戊基和环己基,氟化烷基例如三氟丙基和十七氟代癸基,其中甲基是优选的。
R5为氢原子、单价烃基或乙酰基。R5的例子包括氢原子、甲基、乙基、丙基、丁基和乙酰基。
在上述式-CfH2fO(CgH2gO)hR5中,f为2~12的正数,优选从2~6,更优选为3,g为2~4的正数,优选为2和3,更优选为2或2和3相结合,以及h为1~200的正数,优选为1~100,更优选为1~50。
在上述式(1)中,n为1~20的整数,优选1~10,更优选1~5。
R4的例子包括氢原子、甲基和羟基,其中氢原子是优选的。
基于水性切削液,改性有机硅的含量为0.01~20重量%,优选0.1~10重量%,且更优选0.1~5重量%。低于0.01wt%导致加工精度的降低,而高于20wt%导致不溶物的形成。
在一个优选的实施方案中,切削液还含有(B)1~20重量%的水,和(C)60~98.99重量%的亲水性多元醇和/或其衍生物。在一个更优选的实施方案中,切削液进一步含有(B)10~20重量%的水,和(C)80~95重量%的亲水性多元醇和/或其衍生物。低于1wt%的水会导致诸如加工精度降低这样的问题,而加入多于20wt%的水会导致水性切削液具有诸如低的粘度稳定性这样的问题。低于60wt%的亲水性多元醇和/或其衍生物会导致磨料分散性降低,而多于98.99wt%会导致加工精度降低。
亲水性多元醇及其衍生物(C)的例子包括乙二醇、二甘醇、三甘醇、二丙二醇、三丙二醇,和聚乙二醇。在聚乙二醇中,具有平均分子量为200~1000的聚乙二醇为优选的。例如,使用聚乙二醇200和400。优选地亲水性多元醇或其衍生物(C)在20℃时具有至少为5重量%的水中溶解度,和具有达到0.01mmHg的蒸汽压。
如果在20℃的水中溶解度低于5重量%,会引发在晶片清洗中必须用有机溶剂的问题。蒸汽压高于0.01mmHg会增加切削操作中起火的危险。
本发明另一个实施方案是含有100重量份水性切削液组分(A)~(C)和50~200重量份磨料的水性切削浆。适宜的磨料包括碳化硅、氧化铝和金刚石。碳化硅和金刚石是更适宜的。含有小于50pbw磨料的浆可能效果较差从而切削硅锭花费较长的时间。大于200pbw的磨料可能会影响分散。
添加剂例如消泡剂、水溶性聚合物、云母、疏水性二氧化硅和羧酸可加入该水性切削液和浆中,只要它们的性能不被削弱。
通常,多线锯具有在一定间隔刻有凹槽的两个导向轮。金属线被缠绕在导向轮的凹槽内并在一定张力下保持平行。
当切削一个待加工的样品时,所述浆供给金属线并造成切削线的双向或单向高速运转。上面放有待加工样品的工作台从上方位置向下行进到金属线,由此样品被同时切削为大量的具有相同形状的产品。
可选择的是,随着样品上升的工艺代替样品下降工艺,带有样品的工作台可以向上运动。
在多线锯切削中,一连串的提供含有磨料的浆给金属线以及使用粘附有浆的金属线切削待加工样品的步骤是重要的操作。
实施例
实施例和比较例如下通过举例的方式但并非限制。所有的份以及%都是以重量计。
实施例1
标记为M-1的流体通过混合13%的去离子水,18%的PEG200,和68%的二甘醇制备,并向其中加入1%的用分子式R2 2.21R3 0.27SiO0.76表示的聚醚改性的有机硅,其中R2为甲基且R3为-C3H6O(C2H4O)7.6H。该流体和碳化硅(SiC)磨料(ShinanoE1ectric Refining Co.,Ltd.,GP#1000,平均粒径11μm)混合并搅拌直到获得用于切削硅锭的水性浆。
通过测量刚刚制成以后以及静置24小时后的平均粒径来测量该水性切削浆的动态接触角并评价磨料的分散稳定性。结果如表3所示。还通过在如下条件下切削硅锭来评价浆的粘度稳定性和加工精度,结果也示于表3中。
切削条件
切削工具:多线锯
金属线直径:0.14mm
磨料:碳化硅(Shinano Electric Refining Co.,Ltd.,GP#1000,平均粒径11μm)
硅锭:多晶硅,尺寸125mm2,长90mm
切削间隔:0.40mm
切削速率:0.3mm/min
金属线运行速度:600m/min
评价
动态接触角
使用接触角测量仪(型号CA-D,Kyowa Interface Science Co.,Ltd.),水性浆滴下以后30秒测量液滴在玻璃板上的接触角。
磨料的分散稳定性
使用Cilas公司的激光散射衍射粒度分布分析仪Cilas 1064,测量水性切削液刚刚制备完成后以及静置24小时后的平均粒径。计算粒径的增量。
粒径增量=(24小时后的平均粒径)/(制备完成的平均粒径)
水性切削浆的粘度稳定性
使用Brookfield粘度仪,在硅锭切削操作前后测量水性切削浆的粘度,计算粘度增加百分比。
切削后的加工精度
切削后,检查切削晶片表面的锯痕。
○:没有锯痕
×:有锯痕
还检测晶片的总厚度变化(TTV)以及翘曲度或三维波度。硅锭被切成晶片以后,从每个锭相对的末端和中心切下的三个晶片,共九个晶片做为样品。每个晶片在四个角及其中间测量厚度,共八个点。总共获得72个厚度数据,从此计算出一个标准偏差。
实施例2
除了使用以式R1 0.67R2 2SiO0.67表示的氨基改性的有机硅以外,水性切削液(M-2)如实施例1中制备,其中作为改性有机硅,R1为-(CH2)2NH2且R2为甲基。其按照实施例1被评价。
实施例3
除了使用以式R1 0.33R2 2.33SiO0.67表示的羧基改性的有机硅以外,水性切削液(M-3)如实施例1中制备,其中作为改性有机硅,R1为-(CH2)2COOH且R2为甲基。其按照实施例1被评价。
实施例4
除了使用以式R1 0.67R2 2SiO0.67表示的环氧基改性的有机硅以外,水性切削液(M-4)如实施例1中制备,其中作为改性有机硅,R1为且R2为甲基。其按照实施例1被评价。
实施例5~9和比较实施例1~7
如实施例1,通过混合和搅拌如表1和2中所示的数量的组分制备水性切削液(M-5~M-18)。如实施例1,该流体和SiC磨料(Shinano Eiectric RefiningCo.,Ltd.,GP#1000,平均粒径11μm)混合并搅拌直到获得水性浆。
通过测量刚刚制备完成后以及静置24小时后的平均粒径来测量该水性切削浆的动态接触角并评价磨料的分散稳定性。结果如表3和4所示。还通过在实施例1中相同条件下切削硅锭来评价浆的粘度稳定性和加工精度。结果也示于表3和4中。
表1
表2
Noigen TDS-30:Dai-Ichi Kogyo Seiyaku Co.,Ltd.的商标,RO(CH2CH2)nOH,R=13个碳,n=3
Noigen TDS-80:Dai-Ichi Kogyo Seiyaku Co.,Ltd.的商标,RO(CH2CH2)nOH,R=13个碳,n=8
PEG200:Sanyo Chemical Industries Ltd.的商标,聚乙二醇,平均分子量200
PEG400:Sanyo Chemical Industries Ltd.的商标,聚乙二醇,平均分子量400
表3
表4
Claims (17)
1.水性切削液,含有(A)0.01~20重量%的改性有机硅、(B)1~20重量%的水和(C)60~98.99重量%的亲水性多元醇和/或其衍生物;
其中改性有机硅为由下述平均组成式(1)表示,
R1 pR2 qR3 rSiO(4-p-q-r)/2 (1)
其中,R1为-(CR4 2)nX,R4为氢原子,具有1~20个碳原子且无脂肪族不饱和键的、取代或未取代的单价烃基,或羟基,n为1~20的整数,X为选自氨基、羧基和环氧基中的官能团,R2为具有1~20个碳原子且无脂肪族不饱和键的、取代或未取代的单价烃基,R3为具有通式-CfH2fO(cgH2gO)hR5的有机基团,R5为氢原子,无脂肪族不饱和键的、取代或未取代的单价烃基,或乙酰基,f为2~12的正数,g为2~4的正数,h为1~200的正数,且p,q和r为满足0≤p<2.5,0.01≤q<2.5,0≤r<2.5且0.05<p+q+r≤3.0的数。
2.权利要求1的切削液,其中改性有机硅为聚醚、氨基、羧基、或环氧基改性的有机硅。
3.权利要求1的切削液,其中亲水性多元醇或其衍生物(C)在20℃具有至少为5重量%的水中溶解度,和具有0.01mmHg的蒸汽压。
4.权利要求1的切削液,其中成分(C)选自乙二醇、二甘醇、三甘醇、二丙二醇、三丙二醇、和聚乙二醇。
5.权利要求1的切削液,其中成分(C)是具有200~1000的平均分子量的聚乙二醇。
6.含有100重量份权利要求1的水性切削液和50~200重量份磨料的水性切削浆。
7.权利要求6的水性切削浆,其中磨料选自碳化硅、氧化铝和金刚石。
8.含有100重量份权利要求4的水性切削液和50~200重量份磨料的水性切削浆。
9.权利要求8的水性切削浆,其中磨料选自碳化硅、氧化铝和金刚石。
10.含有100重量份权利要求5的水性切削液和50~200重量份磨料的水性切削浆。
11.权利要求4的水性切削浆,其用于辅助切削选自硅晶、石英、水晶、化合物半导体、和磁性合金的锭材。
12.使用水性切削液切削锭材的方法,其中水性切削液包含:
(A)下述平均组成式(1)表示的0.01~20重量%的改性有机硅,
R1 pR2 qR3 rSiO(4-p-q-r)/2 (1)
其中,R1为-(CR4 2)nX,R4为氢原子,具有1~20个碳原子且无脂肪族不饱和键的、取代或未取代的单价烃基,或羟基,n为1~20的整数,X为选自氨基、羧基和环氧基中的官能团,R2为具有1~20个碳原子且无脂肪族不饱和键的、取代或未取代的单价烃基,R3为具有通式-CfH2fO(cgH2gO)hR5的有机基团,R5为氢原子,无脂肪族不饱和键的、取代或未取代的单价烃基,或乙酰基,f为2~12的正数,g为2~4的正数,h为1~200的正数,且p,q和r为满足0≤p<2.5,0.01≤q<2.5,0≤r<2.5且0.05<p+q+r≤3.0的数;
(B)1~20重量%的水;和
(C)60~98.99重量%的亲水性多元醇和/或其衍生物。
13.权利要求12的方法,其中成分(C)选自乙二醇、二甘醇、三甘醇、二丙二醇、三丙二醇、和聚乙二醇。
14.要得要求12的方法,其中成分(C)是具有200~1000的平均分子量的聚乙二醇。
15.权利要求12的方法,其中多线锯用于切削。
16.权利要求15的方法,其中切削被引导以使多线锯沿双向或单向移动。
17.权利要求12至16中任一项的方法,其中锭材是硅晶、石英、水晶、化合物半导体、和磁性合金。
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- 2010-06-09 WO PCT/JP2010/059752 patent/WO2010143649A1/ja active Application Filing
- 2010-06-09 BR BRPI1011223A patent/BRPI1011223A2/pt not_active IP Right Cessation
- 2010-06-09 US US12/934,749 patent/US8591611B2/en active Active
- 2010-06-09 KR KR1020117021047A patent/KR20120036796A/ko not_active Application Discontinuation
- 2010-06-09 JP JP2011518552A patent/JP5408251B2/ja not_active Expired - Fee Related
- 2010-06-09 EP EP10786180.9A patent/EP2441550B1/en not_active Not-in-force
- 2010-06-09 MY MYPI2011003613 patent/MY152049A/en unknown
- 2010-06-11 CN CN201010246951.9A patent/CN101921648B/zh not_active Expired - Fee Related
- 2010-06-11 TW TW099119118A patent/TW201113357A/zh unknown
- 2010-06-11 KR KR1020100055163A patent/KR20100133907A/ko not_active Application Discontinuation
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JP特开2005-129637A 2005.05.19 |
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TW201113357A (en) | 2011-04-16 |
EP2441550A1 (en) | 2012-04-18 |
EP2441550B1 (en) | 2016-09-07 |
WO2010143649A1 (ja) | 2010-12-16 |
CN101921648A (zh) | 2010-12-22 |
KR20100133907A (ko) | 2010-12-22 |
KR20120036796A (ko) | 2012-04-18 |
JPWO2010143649A1 (ja) | 2012-11-29 |
BRPI1011223A2 (pt) | 2016-03-15 |
US8591611B2 (en) | 2013-11-26 |
JP5408251B2 (ja) | 2014-02-05 |
EP2441550A4 (en) | 2012-11-21 |
US20110113699A1 (en) | 2011-05-19 |
MY152049A (en) | 2014-08-15 |
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