CN1405287A - 非易燃性水系切削液组合物以及非易燃性水系切削液 - Google Patents
非易燃性水系切削液组合物以及非易燃性水系切削液 Download PDFInfo
- Publication number
- CN1405287A CN1405287A CN02131852A CN02131852A CN1405287A CN 1405287 A CN1405287 A CN 1405287A CN 02131852 A CN02131852 A CN 02131852A CN 02131852 A CN02131852 A CN 02131852A CN 1405287 A CN1405287 A CN 1405287A
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- CN
- China
- Prior art keywords
- cutting fluid
- salt
- series
- acid
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
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- 239000000203 mixture Substances 0.000 title claims abstract description 35
- 239000003082 abrasive agent Substances 0.000 claims abstract description 51
- 150000003839 salts Chemical class 0.000 claims abstract description 49
- 238000005520 cutting process Methods 0.000 claims abstract description 36
- 239000002253 acid Substances 0.000 claims abstract description 33
- 239000000463 material Substances 0.000 claims abstract description 16
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- -1 alkali metal salt Chemical class 0.000 claims description 36
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- 239000002131 composite material Substances 0.000 claims description 19
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 18
- 229910052783 alkali metal Inorganic materials 0.000 claims description 15
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
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Abstract
本发明提供一种磨料分散性良好、用于硬脆材料的加工时也没有易燃性问题、容易用水洗涤、在油系设备中使用也可以发挥防锈性的非易燃性水系切削液组合物。还提供一种非易燃性水系切削液组合物,其中,除含有重均分子量1,000-200,000的聚羧酸系高分子化合物及/或其盐以外,根据防锈性的需要,还含有羧酸及/或其盐。
Description
技术领域
本发明涉及非易燃性水系切削液组合物以及非易燃性水系切削液,更详细地说,涉及半导体晶体材料单晶硅以及多晶硅、石英、水晶、陶瓷等适于晶锭切割加工的水系切削液和往其中配合磨料所形成的浆状非易燃水性系切削液,此外,还涉及在油系设备中使用的非易燃性水系切削液组合物以及非易燃性水系切削液。
背景技术
此前,在硅锭等硬脆材料切割用切削液中,作为磨料分散剂,主要采用的是以矿物油作为主成分的非水系切削液。该非水系切削液,是把碳化硅等磨料以1∶1(重量比)分散在切削油中而形成的浆料,把该浆料连续供给切削加工面。为了洗涤切下来的晶片,可以采用三氯乙烷和二氯甲烷等氯系有机溶剂以及高浓度非离子性表面活性剂作洗涤液。
然而,由于矿物油是易燃性危险物,必需有防爆设备,储藏量也受到限制,在环境保护和制造管理方面存在问题。另外,采用矿物油切割的晶片,用于洗涤的上述氯系有机溶剂的洗涤剂,由于有致癌性,在安全卫生方面存在问题。另外,它是大气污染和臭氧层破坏的主要原因,近年来禁止使用。作为其代用品而采用非离子性表面活性剂,但是,采用该非离子性表面活性剂进行洗涤,因其洗涤力低而必需采用大型洗涤设备,另外,由于必须以高浓度使用,废水处理和废弃处理也产生问题。
另一方面,已提出不以矿物油作为主成分,并且在切割工序后可用水洗涤的,以聚氧亚烷基二醇及其衍生物等的水溶性醚类作为主成分的二元醇型的水可溶系列的水溶性切削液(参照特开平3-181598号公报以及特开平11-198016号公报)。
因此,二元醇型水溶性切削液,为使发火点消失而必须配合水,但是,当水量少时,产生易燃性问题,而当水量配合多时,磨料的分散性变差等,制造管理方面产生问题。另外,二元醇型水溶性切削液,即使用水易于洗涤,但洗涤水的废水负荷高,废液处理也存在问题。另外,往采用矿物油系切削液的原有设备中导入水溶性切削液时,由于生锈,所以,必需对设备进行改良以及引入专用设备等的投资。
发明概述
本发明着眼于这些原有的问题,提供一种通过采用特定的聚羧酸系高分子化合物,即使配合大量水的组合物,其磨料分散性也良好,在用于硬脆材料的切割加工时也不产生易燃性问题,并且,易于用水洗涤,废水处理性良好的非易燃性水系切削液组合物以及非易燃性水系切削液。又使用特定的羧酸和/或其盐,可使用油系设备并发挥防锈性而提供非易燃性水系切削液组合物及非易燃性切削液。
即,本发明的非易燃性水系切削液组合物,其特征是,含有重均分子量1000~200000的聚羧酸系高分子化合物及/或其盐5~45重量%。
可以认为聚羧酸系高分子化合物吸附在磨料粒子上,由于保护胶体的效果而发挥稳定的分散效果。另外,可以认为由于聚羧酸系高分子化合物的盐具有离子性,产生静电排斥力,得到更优良的分散性。
该聚羧酸系高分子化合物的分子量及配合量低于1000时,在粒子表面不能形成均匀的保护胶体层,粒子间的排斥力变弱,分散性和再分散性变差。另外,当分子量大于200,000时,呈现凝聚作用,使再分散性下降。
上述聚羧酸系高分子化合物及/或其盐,优选选自由丙烯酸、马来酸及甲基丙烯酸中的1种或2种或以上单体制成的聚合物、该聚合物的碱金属盐、该聚合物的鎓盐以及它们的1种或2种或以上的混合物中。
另外,上述聚羧酸系高分子化合物及/或其盐,用通式(1)表示的聚合物是优选的。
这里,在通式(1)中,R是氢原子或甲基,M1、M2及M3为氢原子、碱金属原子或鎓中的任何一种,既可以相同也可以相异。n为1以上的整数,m为0以上的整数。
本发明的非易燃性水系切削液组合物还可以含有选自水溶性溶剂、润滑剂、粘性调节剂、非铁金属用防腐蚀剂及消泡剂中的至少1种添加助剂。其中,作为上述添加助剂优选含有1种或2种以上选自聚氧亚烷基二醇及其衍生物的水溶性溶剂。
此外,本发明的非易燃性水系切削液组合物,也可以含有上述羧酸及/或其盐0.05~5重量%。羧酸及其盐用于提高防锈性的功能。
在该通式(2)中,k为6~12的整数。
本发明的非易燃性水系切削液,其特征是含有上述非易燃性水系切削液组合物和磨料。
上述磨料的粒径最好是0.5~50μm。另外,上述非易燃性水系切削液组合物和磨料优选是以重量比1∶0.5~1∶1.5的比例进行分散的切削液。
这种本发明的非易燃性水系切削液用于线状锯或带状锯是合适的,而且特别适用于由硬脆材料的锭的切割。作为上述硬脆材料,可以举出硅、石英及水晶。
本发明的非易燃性水系切削液组合物因为含有聚羧酸系高分子化合物及/或其盐、羧酸及/或其盐,所以,即使配合很多水的组合物其磨料的分散性也好,在用于硬脆材料的切割加工时也不产生易燃性问题。另外,本发明的非易燃性水系切削液组合物具有高的防锈性,所以,即使用于油系设备也不生锈。此外,易于用水洗涤。
另外,本发明的油系设备用的非易燃性水系切削液,因为在上述组合物中配合磨料,所以,可连续供给线状锯、带状锯等切削装置,可进行加工精度高的晶片的切割。
作为本发明所用的聚羧酸系高分子化合物,可以使用丙烯酸、马来酸或甲基丙烯酸的均聚物或共聚物、或者它们和乙烯、丙烯、苯乙烯、甲基丙烯酸酯、马来酸单酯、马来酸二酯、醋酸乙烯等的共聚物。另外,上述聚羧酸系高分子化合物的碱金属盐及/或其鎓盐也可以使用。作为盐的种类,可以举出钠、钾、锂等金属离子盐、铵、单乙醇胺、二乙醇胺、三乙醇胺、甲胺、二甲胺、三甲胺、乙胺、二乙胺、三乙胺、甲基乙醇胺、二甲基乙醇胺、甲基二乙醇胺、乙基乙醇胺、二乙基乙醇胺、乙基二乙醇胺等的鎓离子盐。这些盐中,优选的是钠、钾、铵、单乙醇胺以及二乙醇胺的盐。
上述聚羧酸系高分子化合物中,特别合适使用的是上述化2的通式(1)表示的丙烯酸的均聚物及/或丙烯酸和马来酸的共聚物的碱金属盐及/或鎓盐。
聚羧酸盐系高分子化合物及/或其盐的重均分子量优选的是1,000~200,000,但是,5,000~20,000的处理极容易,制成水溶液时可以得到合适的粘度。分子量低于1,000时,磨料的分散能力低,要求高于50重量%的配合量,从而增大废水负荷。分子量大于200,000时,为了得到合适的粘度,必须降低配合量,此外,磨料的分散性降低。
聚羧酸系高分子化合物及/或其盐的配合量的下限在5重量%以上,优选20重量%以上,而上限在45重量%下,优选40重量以下。当配合量低于5重量%时,得不到充分的磨料分散性,而当高于45重量%时,切削液的粘度上升,磨料的混合变得困难,也不可能连续供给切削装置。
本发明的非易燃性水系切削液组合物,为了实现防锈性,可以配合羧酸及/或其盐。作为本发明中所用的羧酸,可以举出丙酸、丁酸、戊酸、己酸、庚酸、辛酸、壬酸、癸酸、十一碳酸、十二碳酸、十四碳酸、十七碳酸、十八碳酸、油酸等脂肪族单羧酸、安息香酸、邻甲基安息香酸(间甲苯甲酸)、间甲基安息香酸、对甲基安息香酸、邻乙基安息香酸、间乙基安息香酸、对乙基安息香酸、邻丙基安息香酸、间丙基安息香酸、对丙基安息香酸、对叔丁基安息香酸、萘甲酸等芳香族单羧酸、乙二酸、丙二酸、丁二酸、戊二酸、己二酸、庚二酸、辛二酸、壬二酸、癸二酸、十一碳二酸、十二碳二酸、十三碳二酸、十四碳二酸、十五碳二酸、十六碳二酸等脂肪族二羧酸、酞酸、异酞酸、对酞酸等芳香族二羧酸。另外,还可以使用这些酸的碱金属盐及鎓盐。作为这些盐的种类,可以举出钠、钾、锂等的金属离子盐、铵、单乙醇胺、二乙醇胺、三乙醇胺、甲胺、二甲胺、三甲胺、乙胺、二乙胺、三乙胺、甲基乙醇胺、二甲基乙醇胺、甲基二乙醇胺、乙基乙醇胺、二乙基乙醇胺、乙基二乙醇胺等的鎓离子盐。这些盐中,钠、钾、铵、单乙醇胺以及二乙醇胺的盐是优选的。
特别适用的羧酸是以化4的通式(2)表示的脂肪族二羧酸的碱金属盐及铵盐,以及链烷醇胺盐的中和物,具体的可以举出辛二酸、壬二酸、癸二酸、十一碳二酸、十二碳二酸、十三碳二酸、十四碳二酸等的钠盐、二乙醇胺盐等。这些化合物的发泡性低,不必使用消泡剂的添加助剂。
羧酸及/或其盐的配合量的下限是0.05重量%以上,优选的是0.2重量%以上,而上限在5重量%以下,优选的是2重量%以下。当配合量低于0.05重量%时,不能得到充分的防锈性,而当高于5重量%时,分散性下降,磨料的混合变得困难,同时,也不可能连续往切削装置供给。
往非易燃性水系切削液中配合时的水含量,在不配合羧酸及/或其盐时,为55~95重量%,当低于55重量%时,不能均匀溶解聚羧酸盐型高分子化合物,是不理想的。另外,通过水含量在55~95重量%的范围内进行配合,即使切割后的被切割物(晶片等)洗涤时,仅用水就可能除去本发明的浆状非易燃性水系切削液。
在配合羧酸及/或其盐时,在易燃性水系切削液中配合时的水量,在50重量%以上,当低于50重量%时,聚羧酸盐型高分子化合物不能均匀溶解,是不理想的。另外,通过配合水量50重量%以上,即使切割后的被切割物(晶片等)洗涤时,仅用水就可能除去本发明的非易燃性水系切割液,洗涤变得容易。另外,在配合羧酸及/或其盐的切削液,最好采用中和盐,使切削液调节至pH7~9,在pH4以下的酸性区域,已经确认铁系材料会生锈,而在pH10以上的碱性区域,附着在手上,造成手粗糙等。
在本发明的非易燃性水系切削液中,根据需要还可以配合各种添加助剂。作为这样的添加助剂,可以举出水溶性溶剂、润滑剂、粘性调节剂、非铁金属用防腐蚀剂、消泡剂等。作为水溶性溶剂的例子,可以举出乙二醇、二甘醇、三甘醇、丙二醇、二丙二醇、三丙二醇、己二醇,丙三醇、聚乙二醇、聚丙二醇、聚乙二醇-聚丙二醇共聚物、己二醇、1,3-丙二醇、1,4-丁二醇、1,6-己二醇、季戊四醇、山梨醇、乙二醇单甲醚、乙二醇单乙醚、乙二醇单丁醚、二甘醇单甲醚、二甘醇单乙醚、三甘醇单丁醚、三甘醇单甲醚、三甘醇单乙醚、三甘醇单丁醚、丙二醇单甲醚、二丙二醇单甲醚、三丙二醇单甲醚以及它们的混合物。另外,作为润滑剂,例如.可以举出非离子表面活性剂、阴离子表面活性剂、脂肪酸、脂肪酸缩聚物等。作为粘性调节剂,例如,可以举出膨润土、水溶性硅溶胶、聚乙烯吡咯烷酮、羧甲基纤维素等。作为非铁金属用防腐蚀剂,例如,可以举出苯并三唑系化合物等,作为消泡剂,例如,可以举出硅氧烷系、乙炔二醇系、聚乙二醇系的化合物以及醇类等。特别合适的添加助剂,可以举出作为水溶性溶剂的乙二醇、二甘醇、丙二醇等聚氧亚烷基二醇系溶剂,这些化合物对防止磨料的沉降有效。
在本发明的非易燃性水系切削液中分散的磨料未作特别限定,可以举出碳化硅、氧化铝、氧化锆、二氧化硅、二氧化铯、金刚石等。磨料的平均粒径优选的是0.5~50μm,更优选的是5~30μm。当磨料的平均粒径大于50μm时,磨料的沉降速度加快,难以分散。另外,磨料的平均粒径小于0.5μm时,切削液的切削能力下降,是不理想的。对非易燃性水系切削液1,磨料的配合比例的下限在0.5(重量比)以上,优选的是0.8以上。另外,磨料的配合比例的上限在1.5(重量比)以下,优选的是1.2以下。磨料的配合比例低于0.5时,浆中的磨料量过少,切割加工需要时间长。另外,磨料的配合比例大于1.5时,磨料的分散性差,本发明的浆状切削液也堆以连续供给切削装置,是不理想的。
本发明的非易燃性水系切削液可用于硬脆性材料的切割,对该硬脆材料未作特别限定,但是,特别适用于单晶硅、多晶硅、石英、水晶、玻璃、钾-砷、陶瓷等硬脆材料,更优选的是适用于单晶硅锭或石英(水晶)锭。本发明的非易燃性水系切削液只要是采用游离磨料进行硬脆材料的切削装置的任何一种类型均可以使用,但是,作为优选的切削装置,例如,可以举出线型锯、条型锯等。
本发明的优选实施方案
其次,根据实施例及比较例进行说明,但是,本发明不受这些实施例的限定。实施例1~14及比较例1~7
对在不配合羧酸及/或其盐的场合,切削液组合物以及切削液的实施例和比较例加以说明。
表1及表2记载的各种成分以所记载的比例加以配合,得到切削液组合物。往得到的切削液组合物中添加磨料,制造切削液,各切削液的分散性、再分散性、粘度变化、切割加工精度、洗涤性以及废水处理性按下法进行测量,其结果示于表3及表4。
表1
切削液组合物 | 实施例 | ||||||||||||||
1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | 11 | 12 | 13 | 14 | ||
聚羧酸盐型高分子化合物 | 平均分子量5000的丙烯酸均聚物 | 20 | |||||||||||||
平均分子量8000的丙烯酸-马来酸共聚物 | 15 | ||||||||||||||
平均分子量4000的丙烯酸钠均聚物 | 35 | ||||||||||||||
平均分子量16万的丙烯酸铵均聚物 | 30 | ||||||||||||||
平均分子量1万的丙烯酸钠均聚物 | 32 | ||||||||||||||
平均分子量1万的丙烯酸铵均聚物 | 35 | ||||||||||||||
平均分子量14万的丙烯酸钠均聚物 | 30 | ||||||||||||||
平均分子量15万的丙烯酸均聚物的二乙醇胺盐 | 25 | ||||||||||||||
平均分子量5000的丙烯酸钾均聚物 | 40 | ||||||||||||||
平均分子量2万的丙烯酸钠-马来酸钠共聚物 | 35 | ||||||||||||||
平均分子量5万的丙烯酸钠-甲基丙烯酸钠共聚物 | 35 | ||||||||||||||
平均分子量10万的马来酸钠-甲基丙烯酸钠共聚物 | 35 | ||||||||||||||
平均分子量7000的苯乙烯-马来酸钠共聚物 | 45 | ||||||||||||||
平均分子量3万的丙烯酸丁酯-甲基丙烯酸钠共聚物 | 45 | ||||||||||||||
平均分子量900的丙烯酸钠均聚物 | |||||||||||||||
平均分子量25万的丙烯酸钠均聚物 | |||||||||||||||
聚乙烯醇(平均分子量400) | |||||||||||||||
水 | 80 | 85 | 65 | 70 | 68 | 65 | 70 | 75 | 60 | 65 | 65 | 65 | 55 | 55 | |
膨润土 | |||||||||||||||
从市场购得的矿物油切削液(バレス化学(株)制,商品名:PS-LW-1) |
表2
磨料的分散性和再分散性
切削液组合物 | 比较例 | |||||||
1 | 2 | 3 | 4 | 5 | 6 | 7 | ||
聚羧酸盐型高分子化合物 | 平均分子量5000的丙烯酸均聚物 | |||||||
平均分子量8000的丙烯酸-马来酸共聚物 | ||||||||
平均分子量4000的丙烯酸钠均聚物 | 0.1 | |||||||
平均分子量16万的丙烯酸铵均聚物 | ||||||||
平均分子量1万的丙烯酸钠均聚物 | 4 | 50 | ||||||
平均分子量1万的丙烯酸铵均聚物 | ||||||||
平均分子量14万的丙烯酸钠均聚物 | ||||||||
平均分子量15万的丙烯酸均聚物的二乙醇胺盐 | ||||||||
平均分子量5000的丙烯酸钾均聚物 | ||||||||
平均分子量2万的丙烯酸钠-马来酸钠共聚物 | ||||||||
平均分子量5万的丙烯酸钠-甲基丙烯酸钠共聚物 | ||||||||
平均分子量10万的马来酸钠-甲基丙烯酸钠共聚物 | ||||||||
平均分子量7000的苯乙烯-马来酸钠共聚物 | ||||||||
平均分子量3万的丙烯酸丁酯-甲基丙烯酸钠共聚物 | ||||||||
平均分子量900的丙烯酸钠均聚物 | 40 | |||||||
平均分子量25万的丙烯酸钠均聚物 | 20 | |||||||
聚乙烯醇(平均分子量400) | 91 | 40 | ||||||
水 | 96 | 50 | 60 | 80 | 8 | 19 | ||
膨润土 | 1 | |||||||
乙二醇 | 40 | |||||||
合成的锂蒙脱石 | 0.9 | |||||||
从市场购得的矿物油系切削油(バレス化学(株)制,商品名:PS-LW-1) | 100 |
表1和表2中列出的切削剂组合物500g和碳化硅磨料(GP#800,(株)フジミインコ一ポレ一テツド制)500g,放入1000ml的聚合器内,于室温(25℃),采用高分散机(特殊机工业(株)制),以转速3,000rpm搅拌3分钟,得到均匀的浆状非易燃性水系切削液。
把该水系切削液100ml放入100ml的奈斯勒管(直径24mm,高200mm)中,静置后,分别在1小时、6小时、24小时以及48小时,进行下层磨料的容量测定和沉降状态的观察。可以判断下层容量大的,其上部分离水量少,磨料的分散性优良。
关于磨料的再分散性,是在静置48小时后,把放入浆中的奈斯勒管水平倾斜,从磨料层的流动性按下列标准进行判断。
◎…整个磨料层平稳地流动
○…整个磨料层缓慢地流动
△只在磨料层上部流动
×…磨料层几乎不流动
如同表3和表4所示,各实施例的非易燃性水系切削液,可以发挥与矿物油系切削液(比较例7)相当的稳定分散效果。这就表明在各实施例的非易燃性水系切削液中配合的聚羧酸系高分子化合物吸附在磨料粒子上,形成保护胶体。另外,可以认为,这是由于聚羧酸系高分子化合物的碱金属盐以及鎓盐具有离子性,可以发挥静电排斥力所致,从而得到更优良的分散性。聚羧酸系高分子化合物在一定的分子量以下的场合或配合量低的场合,在粒子表面上不能形成均匀的保护胶体层,粒子间排斥力变弱,从而分散性及再分散性下降。另外,在分子量超过20万的场合,呈现凝聚作用,再分散性下降。粘度变化
表1和表2中列出的切削剂组合物500g和碳化硅磨料(GP#800,(株)フジミインユ一ポレ一テツド制)500g,放入1000ml的聚合器内,于室温(25℃),采用高分散机(特殊机工业(株)制),以旋转速度3,000rpm搅拌3分钟,得到均匀的浆状非易燃性水系切削液。对该水系切削液于25℃用BM型粘度计测定粘度。然后,用高混合器(分散器-叶片)以10,000rpm搅拌1小时,调温至25C后测定粘度。以搅拌前后的粘度变化率=(以10,000rpm搅拌1小时后的粘度)/(搅拌前的粘度)求出,研究剪切力的影响。粘度变化率愈接近1,在切割锭时,粘度变化少,可以得到稳定的加工性。
如表3及表4所示,在采用各实施例的非易燃性水系切削液的场合,与比较例的切削液相比,粘度变化少,具有与矿物油系的切削液(比较例7)同等以上的粘度稳定性。切割加工精度
把表1及表2中列出的切削液组合物和碳化硅磨料(GP#800,(株)フジミインコ一ポレ一テツド制)以1∶1(重量比)进行搅拌混合,得到均匀的浆状非易燃性水系切削液。用该切削液,用线径180μm的线型锯切削装置,进行6英寸的单晶硅锭的切割加工,评价被切割的晶片的加工精度。
加工精度,系测定晶片的翘度(WARP,中央部位和外周部位合计5个点的高度差的最大值),求出10块样品的平均值,按下列标准判定切割加工精度。
◎…0μm~10μm
○…101μm~20μm
△…20μm~30μm
×…30μm以上。
如表3及表4所示,采用各实施例的非易燃性水系切削液的场合,与比较例的切削液相比,切割的加工精度高,可以发挥与矿物油系的切削液(比较例7)同等以上的切割加工精度。洗涤性
表1和表2中列出的切削剂组合物500g和碳化硅磨料(GP#800,(株)フジミインコ一ポレ一テツド制)500g,放入1000ml的聚合器内,于室温(25℃),采用高速混合机(分散机-叶片),以旋转速度3,000rpm搅拌3分钟,得到均匀的浆状非易燃性水系切削液。
在硅晶片和石英晶片上涂布上述切削液,于80C干燥1小时后作为切割加工后的模拟检测样品。把该模拟检测样品的晶片用流水(室温25C)洗涤3分钟,按以下标准判断洗涤性。
○…无磨料残渣洗落下来
×…有磨料残留但未洗落下来
如表3及表4所示,采用各实施例的非易燃性水系切削液的场合,在硅晶片以及石英晶片的任何一种情况下,可以得到与采用比较例的切削液的场合同等以上的洗涤性。还有,矿物油系的切削液(比较例7),不能用水洗涤,洗涤性的评价为‘×’,在这种情况下,不能全部除去磨料,而且,与各实施例相比洗涤性显然变差。废水处理性
配制表1及表2中列出的切削液组合物的0.1%水溶液,测定它的化学需氧量(COD)以及生物化学需氧量(BOD),按下列标准判断废水处理性。
○…OD及BOD低于1,000mg/L
×…COD及BOD大于1,000mg/L。
如同表3及表4所示,采用各实施例的非易燃性水系切削液的场合,明显优于比较例的废水处理性。还有,矿物油系的切削液(比较例7)作为工业废弃物处理,废水处理不可能。从处理成本和对环境的影响考虑,可明确知道各实施例的优越性。
表3
表4
实施例15~32以及比较例8~17
切削液组合物 | 磨料的分散性 | 再分散性,48h | 粘度变化 | 切割加工精度 | 洗涤性 | 废水处理性 | |||||
1h | 12h | 24h | 48h | 硅晶片 | 石英晶片 | ○ | |||||
实施例 | 1 | 95 | 79 | 72 | 67 | ○ | 1.2 | ○ | ○ | ○ | ○ |
2 | 96 | 80 | 73 | 67 | ○ | 1.2 | ○ | ○ | ○ | ○ | |
3 | 97 | 82 | 73 | 67 | ◎ | 1.1 | ◎ | ○ | ○ | ○ | |
4 | 97 | 85 | 75 | 69 | ◎ | 1.0 | ◎ | ○ | ○ | ○ | |
5 | 100 | 89 | 75 | 70 | ◎ | 1.0 | ◎ | ○ | ○ | ○ | |
6 | 100 | 89 | 75 | 70 | ◎ | 1.0 | ◎ | ○ | ○ | ○ | |
7 | 99 | 88 | 75 | 70 | ◎ | 1.0 | ◎ | ○ | ○ | ○ | |
8 | 99 | 88 | 75 | 70 | ◎ | 1.0 | ◎ | ○ | ○ | ○ | |
9 | 98 | 87 | 75 | 69 | ◎ | 1.0 | ◎ | ○ | ○ | ○ | |
10 | 99 | 87 | 75 | 70 | ◎ | 1.0 | ◎ | ○ | ○ | ○ | |
11 | 98 | 87 | 75 | 69 | ◎ | 1.0 | ◎ | ○ | ○ | ○ | |
12 | 98 | 86 | 74 | 68 | ◎ | 1.0 | ◎ | ○ | ○ | ○ | |
13 | 97 | 85 | 74 | 68 | ◎ | 1.0 | ◎ | ○ | ○ | ○ | |
14 | 98 | 85 | 74 | 68 | ◎ | 1.0 | ◎ | ○ | ○ | ○ |
切削液组合物 | 磨料的分散性 | 再分散性,48h | 粘度变化 | 切割加工精度 | 洗涤性 | 废水处理性 | |||||
1h | 12h | 24h | 48h | 硅晶片 | 石英晶片 | ||||||
比较例 | 1 | 50 | 50 | 50 | 50 | × | 0.3 | × | ○ | ○ | ○ |
2 | 72 | 65 | 60 | 50 | △ | 5.0 | × | × | × | ○ | |
3 | 50 | 50 | 50 | 50 | × | 0.4 | × | ○ | ○ | ○ | |
4 | 70 | 62 | 58 | 50 | × | 8.5 | × | × | × | ○ | |
5 | 80 | 68 | 59 | 50 | △ | 2.5 | △ | × | × | × | |
6 | 73 | 65 | 60 | 50 | ○ | 1.9 | × | ○ | ○ | × | |
7 | 99 | 88 | 74 | 68 | ○ | 1.3 | ○ | × | × | ×(非水系) |
对配合羧酸及/或其盐时切削液组合物及切削液的实施例和比较例加以说明。
把表5及表6中记载的各种成分按记载的比例加以配合,得到切削液组合物。往得到的切削液组合物中添加磨料,配制切削液,各切削液的分散性、再分散性、粘度变化、切割加工精度、洗涤性以及防锈性、按下法进行研究,其结果示于表7及表8。
表5
切削液组合物 | 实施例 | ||||||||||||||||||
15 | 16 | 17 | 18 | 19 | 20 | 21 | 22 | 23 | 24 | 25 | 26 | 27 | 28 | 29 | 30 | 31 | 32 | ||
聚羧酸系高分子化合物 | 平均分子量5000的丙烯酸均聚物 | 15 | |||||||||||||||||
平均分子量8000的丙烯酸-马来酸共聚物 | 10 | ||||||||||||||||||
平均分子量4000的丙烯酸钠均聚物 | 30 | ||||||||||||||||||
平均分子量16万的丙烯酸铵均聚物 | 25 | ||||||||||||||||||
平均分子量1万的丙烯酸钠均聚物 | 30 | 15 | 45 | 30 | 30 | ||||||||||||||
平均分子量1万的丙烯酸铵均聚物 | 30 | ||||||||||||||||||
平均分子量14万的丙烯酸钠均聚物 | 25 | ||||||||||||||||||
平均分子量15万的丙烯酸均聚物的二乙醇胺盐 | 20 | ||||||||||||||||||
平均分子量5000的丙烯酸钾均聚物 | 35 | ||||||||||||||||||
平均分子量2万的丙烯酸钠-马来酸钠共聚物 | 30 | ||||||||||||||||||
平均分子量5万的丙烯酸钠-甲基丙烯酸钠共聚物 | 30 | ||||||||||||||||||
平均分子量10万的马来酸钠-甲基丙烯酸钠共聚物 | 30 | ||||||||||||||||||
平均分子量7000的苯乙烯-马来酸钠共聚物 | 30 | ||||||||||||||||||
平均分子量3万的丙烯酸丁酯-甲基丙烯酸钠共聚物 | 30 | ||||||||||||||||||
平均分子量900的丙烯酸钠均聚物 | |||||||||||||||||||
平均分子量25万的丙烯酸钠均聚物 | |||||||||||||||||||
壬酸 | 1 | ||||||||||||||||||
癸酸的三乙醇胺盐 | 1 | ||||||||||||||||||
对叔丁基安息香酸钠盐 | 0.5 | ||||||||||||||||||
癸二酸二乙醇胺盐 | 1 | 1 | 1 | 1 | 1 | 1 | 1 | 1 | 1 | 1 | 3 | ||||||||
十二碳二酸的钠盐 | 0.5 | 1 | 2 | 0.3 | |||||||||||||||
乙二醇 | 10 | 10 | 10 | 5 | 15 | 25 | 3 | 15 | 15 | ||||||||||
丙二醇 | 10 | 10 | 10 | 5 | 15 | ||||||||||||||
聚乙二醇(平均分子量400) | |||||||||||||||||||
水 | 84 | 89 | 70 | 74 | 60 | 59 | 63 | 69 | 54 | 59 | 64 | 54 | 64 | 54 | 59 | 51 | 55 | 52 | |
膨润土 | |||||||||||||||||||
单乙醇胺 | |||||||||||||||||||
从市场购得的矿物油切削液(バレス化学(株)制,商品名:PS-LW-1) |
表6
磨料的分散性和再分散性
切削液组合物 | 比较例 | ||||||||||
8 | 9 | 10 | 11 | 12 | 13 | 14 | 15 | 16 | 17 | ||
聚羧酸系高分子化合物 | 平均分子量5000的丙烯酸均聚物 | ||||||||||
平均分子量8000的丙烯酸-马来酸共聚物 | |||||||||||
平均分子量4000的丙烯酸钠均聚物 | 0.1 | ||||||||||
平均分子量16万的丙烯酸铵均聚物 | |||||||||||
平均分子量1万的丙烯酸钠均聚物 | 3 | 50 | 30 | 30 | 30 | ||||||
平均分子量1万的丙烯酸铵均聚物 | |||||||||||
平均分子量14万的丙烯酸钠均聚物 | |||||||||||
平均分子量15万的丙烯酸均聚物的二乙醇胺盐 | |||||||||||
平均分子量5000的丙烯酸钾均聚物 | |||||||||||
平均分子量2万的丙烯酸钠-马来酸钠共聚物 | |||||||||||
平均分子量5万的丙烯酸钠-甲基丙烯酸钠共聚物 | |||||||||||
平均分子量10万的马来酸钠-甲基丙烯酸钠共聚物 | |||||||||||
平均分子量7000的苯乙烯-马来酸钠共聚物 | |||||||||||
平均分子量3万的丙烯酸丁酯-甲基丙烯酸钠共聚物 | |||||||||||
平均分子量900的丙烯酸钠均聚物 | 40 | ||||||||||
平均分子量25万的丙烯酸钠均聚物 | 20 | ||||||||||
壬酸 | |||||||||||
癸酸的三乙醇胺盐 | |||||||||||
对叔丁基安息香酸钠盐 | |||||||||||
癸二酸二乙醇胺盐 | 1 | 1 | 5.5 | ||||||||
十二碳二酸的钠盐 | 1 | 1 | 0.02 | 1 | |||||||
乙二醇 | |||||||||||
丙二醇 | 80 | ||||||||||
聚乙二醇(平均分子量400) | 90 | ||||||||||
水 | 96 | 49 | 59 | 79 | 69 | 70 | 64.5 | 8 | 19 | ||
膨润土 | 1 | ||||||||||
单乙醇胺 | 1 | ||||||||||
合成的锂蒙脱石(日本シリカ工业制,粒径0.02μm) | 0.9 | ||||||||||
从市场购得的矿物油切削液(バレス化学(株)制,商品名:PS-LW-1) | 100 |
与上述实施例1~14及比较例1~7的场合同样,对磨料的分散性和再分散性进行研究。
如表7及表8的结果所示,各实施例的非易燃性水系切削液可以发挥与矿物油系切削液(比较例17)相当的稳定分散效果。这表示在各实施例的非易燃性水系切削液中配合的聚羧酸系高分子化合物吸附在磨料粒子上,形成保护胶体。另外,聚羧酸系高分子化合物的碱金属盐以及鎓盐具有离子性,发挥静电排斥力,可以得到更优良的分散性。在聚羧酸系高分子化合物的一定分子量以下的场合以及配合量低的场合,在粒子表面不能形成均匀的保护胶体层,粒子间的排斥力变弱,分散性及再分散性下降。另外,分子量大于20万的场合,呈现凝聚作用,再分散性下降。粘度变化
与上述实施例1~14及比较例1~7的场合同样,对粘度变化进行研究。
如表7及表8的结果所示,采用各实施例的非易燃性水系切削液的场合,与比较例的切削液相比,粘度变化小,具有矿物油系切削液(比较例17)同等以上的粘度稳定性。切割加工精度
与上述实施例1~14及比较例1~7的场合同样,对切割加工精度进行研究。
如表7及表8的结果所示,采用各实施例的非易燃性水系切削液的场合,与比较例的切削液进行比较,切割加工精度高,发挥矿物油系的切削液(比较例17)同等以上的切割加工精度。洗涤性
与上述实施例1~4及比较例1~7的场合同样,对洗涤性进行研究。
如表7及表8所示,采用各实施例的非易燃性水系切削液的场合,在硅晶片及石英晶片的任何一种场合下,可以得到与采用比较例切削液时同等以上的洗涤性。还有,矿物油系切削液(比较例17)不可能用水洗涤,洗涤性的评价为‘×’在这种情况下不能全部除去磨料,与各实施例相比,洗涤性显然差。防锈性
把表5及表6中列出的切削液往铸铁粉(FC20)上滴2mL,在室温条件下放置,判明3小时、1天、3天的生锈状况,按下列标准进行比较。
◎…未生锈
○…生锈面积小于5%
△…生锈面积5%~25%
×…生锈面积在25%以上。
如表7及表8所示,采用各实施例的非易燃性水系切削液的场合,显示与比较例同等以上的防锈性,显示与矿物油切削液(比较例17)同等或接近的防锈性。
表7
切削液组合物 | 磨料的分散性 | 再分散性48h | 粘度变化 | 切割加工精度 | 洗涤性 | 防锈性 | |||||||
1h | 12h | 24h | 48h | 硅晶片 | 石英晶片 | 3h | 1日 | 3日 | |||||
实施例 | 15 | 90 | 78 | 70 | 65 | ○ | 1.3 | ○ | ○ | ○ | ◎ | ○ | △ |
16 | 90 | 77 | 70 | 65 | ○ | 1.3 | ○ | ○ | ○ | ◎ | ○ | △ | |
17 | 91 | 78 | 71 | 65 | ○ | 1.3 | ○ | ○ | ○ | ◎ | ○ | △ | |
18 | 91 | 78 | 72 | 66 | ○ | 1.3 | ○ | ○ | ○ | ◎ | ◎ | ◎ | |
19 | 100 | 88 | 75 | 69 | ◎ | 1.0 | ◎ | ○ | ○ | ◎ | ◎ | ◎ | |
20 | 100 | 87 | 75 | 68 | ◎ | 1.0 | ◎ | ○ | ○ | ◎ | ◎ | ◎ | |
21 | 98 | 87 | 75 | 68 | ◎ | 1.0 | ◎ | ○ | ○ | ◎ | ◎ | ◎ | |
22 | 98 | 86 | 74 | 68 | ◎ | 1.0 | ◎ | ○ | ○ | ◎ | ◎ | ◎ | |
23 | 98 | 84 | 74 | 68 | ◎ | 1.0 | ◎ | ○ | ○ | ◎ | ◎ | ◎ | |
24 | 97 | 85 | 75 | 68 | ◎ | 1.1 | ◎ | ○ | ○ | ◎ | ◎ | ◎ | |
25 | 97 | 85 | 75 | 68 | ◎ | 1.1 | ◎ | ○ | ○ | ◎ | ◎ | ◎ | |
26 | 97 | 85 | 75 | 68 | ◎ | 1.1 | ◎ | ○ | ○ | ◎ | ◎ | ◎ | |
27 | 93 | 80 | 72 | 67 | ○ | 1.3 | ○ | ○ | ○ | ◎ | ◎ | ◎ | |
28 | 93 | 81 | 73 | 67 | ○ | 1.3 | ○ | ○ | ○ | ◎ | ◎ | ◎ | |
29 | 90 | 78 | 71 | 65 | ○ | 1.3 | ○ | ○ | ○ | ◎ | ○ | △ | |
30 | 91 | 79 | 72 | 66 | ○ | 1.3 | ○ | ○ | ○ | ◎ | ◎ | ○ | |
31 | 93 | 80 | 73 | 67 | ○ | 1.3 | ○ | ○ | ○ | ◎ | ○ | △ | |
32 | 93 | 80 | 72 | 66 | ○ | 1.3 | ○ | ○ | ○ | ◎ | ◎ | ◎ |
表8
切削液组合物 | 磨料的分散性 | 再分散性48h | 粘度变化 | 切割加工精度 | 洗涤性 | 防锈性 | |||||||
1h | 12h | 24h | 48h | 硅晶片 | 石英晶片 | 3h | 1日 | 3日 | |||||
比较例 | 8 | 50 | 50 | 50 | 50 | × | 0.2 | × | ○ | ○ | ◎ | ◎ | ◎ |
9 | 71 | 63 | 58 | 50 | △ | 5.5 | × | × | × | ◎ | ◎ | ◎ | |
10 | 50 | 50 | 50 | 50 | × | 0.4 | × | ○ | ○ | ◎ | ◎ | ◎ | |
11 | 68 | 60 | 55 | 50 | × | 9.2 | × | × | × | ◎ | ◎ | ◎ | |
12 | 80 | 71 | 60 | 52 | × | 5.2 | × | ○ | ○ | △ | × | × | |
13 | 100 | 88 | 75 | 68 | ◎ | 1.0 | △ | × | × | × | × | × | |
14 | 62 | 55 | 50 | 50 | × | 10.8 | × | × | × | ◎ | ◎ | ◎ | |
15 | 80 | 68 | 59 | 50 | △ | 2.5 | △ | × | × | △ | △ | × | |
16 | 73 | 65 | 60 | 50 | ○ | 1.9 | × | ○ | ○ | × | × | × | |
17 | 99 | 88 | 74 | 68 | ○ | 1.3 | ○ | × | × | ◎ | ◎ | ◎ |
Claims (14)
1.一种非易燃性水系切削液组合物,其中含有重均分子量1,000-200,000的聚羧酸系高分子化合物及/或其盐5-45重量%。
2.权利要求1中所述的非易燃性水系切削液组合物,其中,上述聚羧酸系高分子化合物及/或其盐是选自由丙烯酸、马来酸及甲基丙烯酸中选择的1种或2种或以上单体而制成的聚合物、该聚合物的碱金属盐、该聚合物的鎓盐以及它们中的1种或2种以上的混合物。
4.权利要求1-3中任何一项所述的非易燃性水系切削液组合物,其中还可以含有选自水溶性溶剂、润滑剂、粘性调节剂、非铁金属用防蚀剂以及消泡剂中的至少一种添加助剂。
5.权利要求4中所述的非易燃性水系切削液组合物,其中含有选自聚氧亚烷基二醇及其衍生物中的1种或2种或以上的水溶性溶剂作为上述添加助剂。
6.权利要求1-5中任何一项所述的非易燃性水系切削液组合物,其中还含有羧酸及/或其盐0.05-5重量%。
8.权利要求7中所述的非易燃性水系切削液组合物,其中,所述聚羧酸系高分子化合物及/或其盐系选自具有重均分子量5,000~150,000的丙烯酸均聚物的碱金属盐、丙烯酸均聚物的鎓盐、丙烯酸与马来酸的共聚物的碱金属盐以及丙烯酸和马来酸的共聚物的鎓盐中的,该聚羧酸系高分子化合物及/或其盐的含量为20-40重量%,
所述羧酸及/或其盐系选自以化2的通式(2)表示的脂肪族二羧酸、该脂肪族二羧酸的碱金属盐以及该脂肪族二羧酸的鎓盐中的,该羧酸及/或其盐的含量为0.5-2重量%,
所述添加助剂系选自聚氧亚烷基二醇及其衍生物中的水溶性溶剂,该水溶性溶剂的含量为5-20重量%。
9.一种非易燃性水系切削液,其中含有权利要求1-8中的任何一项所述的非易燃性水系切削液组合物以及磨料。
10.权利要求9中所述的非易燃性水系切削液,其中所述磨料的粒径为0.5-50μm。
11.权利要求9或10中所述的非易燃性水系切削液,把权利要求1-3中的任何一项所述的非易燃性水系切削液组合物和磨料以重量比1∶0.5-1∶1.5的比例分散而制成的。
12.权利要求9-11中任何一项所述的非易燃性水系切削液,可用于线型锯和条型锯。
13.权利要求9-12中任何一项所述的非易燃性水系切削液,可用于硬脆材料的锭的切割。
14.权利要求13中所述的非易燃性水系切削液,其中,所述硬脆材料系选自硅、石英及水晶中。
Applications Claiming Priority (6)
Application Number | Priority Date | Filing Date | Title |
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JP271553/2001 | 2001-09-07 | ||
JP2001271553A JP2003082381A (ja) | 2001-09-07 | 2001-09-07 | 非引火性水系切削液組成物及び非引火性水系切削液 |
JP271539/2001 | 2001-09-07 | ||
JP271539/01 | 2001-09-07 | ||
JP2001271539A JP2003082380A (ja) | 2001-09-07 | 2001-09-07 | 非引火性水系切削液組成物及び非引火性水系切削液 |
JP271553/01 | 2001-09-07 |
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CN1405287A true CN1405287A (zh) | 2003-03-26 |
CN1234827C CN1234827C (zh) | 2006-01-04 |
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US (1) | US6673754B1 (zh) |
EP (1) | EP1291408A1 (zh) |
KR (1) | KR100494296B1 (zh) |
CN (1) | CN1234827C (zh) |
TW (1) | TW575660B (zh) |
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- 2002-09-06 CN CNB021318522A patent/CN1234827C/zh not_active Expired - Fee Related
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- 2002-09-06 US US10/236,899 patent/US6673754B1/en not_active Expired - Fee Related
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EP1291408A1 (en) | 2003-03-12 |
CN1234827C (zh) | 2006-01-04 |
KR20030022066A (ko) | 2003-03-15 |
US6673754B1 (en) | 2004-01-06 |
KR100494296B1 (ko) | 2005-06-10 |
TW575660B (en) | 2004-02-11 |
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