CN106753734A - 一种硅片切割液 - Google Patents

一种硅片切割液 Download PDF

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CN106753734A
CN106753734A CN201710050872.2A CN201710050872A CN106753734A CN 106753734 A CN106753734 A CN 106753734A CN 201710050872 A CN201710050872 A CN 201710050872A CN 106753734 A CN106753734 A CN 106753734A
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silicon chip
integer
cutting fluid
cutting
chip cutting
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CN106753734B (zh
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陈同军
牛树怀
赵琦琦
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Zhejiang ChuanHua functional new material Co.,Ltd.
Transfar Zhilian Co Ltd
Hangzhou Transfar Fine Chemicals Co Ltd
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Mass Of Ltd By Share Ltd
HANGZHOU TRANSFER FINE CHEMICAL Co Ltd
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Abstract

本发明公开了一种硅片切割液。目前的低粘度切割液，其润滑性、分散性不好，在硅切片过程中摩擦热量大，砂浆粘度波动大，造成切割的不稳定，还不能应用于负载较大的切割设备。本发明的切割液包括如下质量百分比的各组分：具有PO‑EO‑PO结构的嵌段聚醚30‑60％，分散剂10‑20％，润湿剂4.0‑10％，抗氧化剂1.0‑3.0％，防腐剂0.05‑2.0％，消泡剂0.05‑2.0％，余量为去离子水。本发明通过提高切割液的分散、润滑能力，实现了大功率切片机使用低粘度液进行硅片切割的可能性，即能应用于负载较大的切割设备。

Description

一种硅片切割液
技术领域
本发明涉及切割液，特别是一种用于晶体硅多线切割的硅片切割液。
背景技术
近年来，中国太阳能光伏行业的发展经历了过山车式的疯狂发展模式，从高回报的暴利时代到产能过剩引起的倒闭潮，再到国家政策的扶持、补贴，目前光伏行业已基本回归理性，但依然要依靠补贴盈利，随着十三五规划的出台，光伏补贴将从2016年下半年开始逐年取消，这需要光伏企业或转型升级提高效率，或精益生产降低成本，才能在激烈的市场环境中生存。目前，硅片切割行业中单晶硅片的生产基本采用金刚线切割方式，成本已大大降低。而多晶硅由于材料本身和下游制绒工艺的制约，仍然需要采用砂浆切割方式，如何降低生产成本成为多晶硅片生产企业亟待解决的问题。
目前，多晶硅线切割工艺为了提高切割效率多使用结构钢线，结构钢线的使用能够增强钢线的携砂能力，提高切割效率；但在切割过程中相应的会遇到一些问题：比如切割力的增大对硅片表面的损伤也会增大，切割力的增大使切割瞬间产生的热量偏大，破坏切割液分子结构，减少了切割液的使用次数。另外，随着切割速率的提高，硅粉生成的速度加快，如果硅粉不能被切割液及时的润湿分散，会引起砂浆的残留，造成脏污片甚至是涨片现象。结构钢线的使用完全降低了切割设备对切割液粘度上的要求，因为之前的钢线表面光滑，需要切割液的粘性来增加其带砂能力，而结构钢线表面粗糙，已大大增加了其表面的带砂能力，对切割液的粘度要求相应也会降低。这样会给切片企业带来一大好处，就是砂浆粘度的降低会大大降低切割设备的工作负载，达到节能降耗的目的。而粘度的降低会对切割液的润滑和分散性相应地提出了更高的要求，较好的润滑性对降低硅片表面损伤、特别是表面热应力缺陷具有重要作用。分散稳定性则对及时持续地分散切割过程产生的硅粉、防止产生微粉残留至关重要。
国内多晶切割设备仍以MB261，HCTB5，PV-800等机型为主，多使用以PEG为主要成分的切割液，此种切割液旋转粘度相对较高，一般在40-50mpa.s之间。切割后砂浆粘度较大，设备系统能耗较高，随着切割液回收次数的增加，PEG分子容易发生断链，其分散性和润滑性都会受到较大影响，易造成砂浆沉积、硅片表面粗糙等现象。此外，国内市场存在少量日本的安永机型，使用进口或国产化的低粘度切割液，但其润滑性、分散性不好，在硅切片过程中摩擦热量大，砂浆粘度波动大，造成切割的不稳定，还不能应用于负载较大的切割设备。
发明内容
为了解决现有线切割过程的高能耗及在切割工艺中存在的硅片表面损伤、砂浆沉积和热应力等问题，本发明提供一种低粘度、高润滑性能和高分散性能的切割液，将其用于晶体硅多线切割，能明显降低能耗，以提高硅片良品率，保持切割过程的稳定性。
本发明采用的技术方案为：一种用于晶体硅多线切割的切割液，其包括如下质量百分比的各组分：
本发明使用具有PO-EO-PO结构的嵌段聚醚作为润滑剂，一方面其表面张力较低，易于在碳化硅颗粒和切割线表面形成保护膜；另一方面，相邻分子两端的PO链段易于相互缠绕，分子间形成类似“手拉手”的效应，增大了保护膜的强度，进而增强了缓冲摩擦、减少磨损的作用。
另外，切片厂家为降低生产成本，切割后的砂浆通过简单的固液分离可以继续使用，但由于切割瞬间温度很高，不可避免地会氧化破坏切割液的分子链结构，使一些长链分子发生断裂，随着切割液的回收次数不断增加，体系内遭到破坏的分子链逐渐累积增多，进而会影响到切割液的分散、润滑等性能。因此切割液中添加抗氧化剂及防腐剂可以延长切割液的使用寿命。
进一步地，所述嵌段聚醚的结构式为：
R(PO)m(EO)n(PO)qH，
其中，R为OH或烷氧基，m为1～100的整数，n为1～100的整数，q为1～100的整数。
更进一步地，所述的烷氧基为C1-C10烷氧基。
最进一步地，所述的烷氧基为甲氧基、乙氧基或丙氧基。
更进一步地，所述m和q的总和为10～70的整数，n为20～80的整数。
进一步地，所述的分散剂是具有梳型结构的分散剂。
更进一步地，所述的分散剂是由TPEG或/和APEG聚醚单体与丙烯酸、甲基丙烯酸、丙烯酸酯、甲基丙烯酸酯、丙烯酸酰胺、甲基丙烯酸酰胺聚合而成，结构式如下：
结构式一(包含APEG聚醚单体)
结构式二(包含TPEG聚醚单体)
结构式三(包含TPEG和APEG聚醚单体)
式中，R1，R2，R3，R4为-H或-CH3；R5为-CH3或-CH2CH3；n为1-200的整数；a,b,c,d各为1-100的整数。
本发明使用具有梳型结构的分散剂，其分散机理为：羧酸根离子吸附于碳化硅表面，使碳化硅颗粒间由于表面带有同种电荷相互排斥而稳定，另一方面长链聚醚链段在碳化硅表面向外伸展起到空间位阻效应，进而使碳化硅、硅粉达到较好的分散效果，不会沉积残留在硅片表面。此外，分散剂分子中的酯基、酰胺基通过水解会源源不断地提供羧酸根离子，保证了整个分散体系的长效稳定。
更进一步地，所述的分散剂结构式中，n为5-100的整数；a,b,c,d各为1-50的整数。
最进一步地，所述的分散剂结构式中，n为10-50的整数；a,b,c,d各为5-30的整数。
进一步地，所述的润湿剂为磺化油、快速渗透剂T、硅醇类非离子表面活性剂、脂肪醇聚氧乙烯醚中的一种或几种的混合物；所述的抗氧化剂为抗坏血酸、二丁基羟基甲苯、茶多酚、吩噻嗪中的一种或几种的混合物。
进一步地，所述的防腐剂为异噻唑啉酮、苯甲酸钠、山梨酸、山梨酸盐、尼泊金酯类中的一种或几种的混合物；所述的消泡剂为有机硅消泡剂、聚醚改性硅油消泡剂、高碳醇消泡剂中的一种或几种的混合物。
本发明通过提高切割液的分散、润滑能力，实现了大功率切片机使用低粘度液进行硅片切割的可能性，即能应用于负载较大的切割设备。
本发明具有的有益效果如下：
1)切割液粘度相对较低，能降低切割设备10％左右的能耗，达到了降本增效的目的；
2)润滑、润湿和冷却作用显著，线痕片、TTV片、热应力片明显减少，提高了良品率；
3)分散性能优秀，能有效解决砂浆沉积现象，有利于硅片的清洗及后续加工；
4)通过提高切割液的分散、润滑能力，实现了大功率切片机使用低粘度液进行硅片切割的可能性，即能应用于负载较大的切割设备；
5)可应用于多晶硅线切割工艺。
具体实施方式
下面结合具体实施方式对本发明作进一步的说明，但本发明并不限于下列实施例。
实施例一
配制1000g切割液，各组分配比如下：嵌段聚醚(R为甲氧基，n＝20，m+q＝10)300g、梳型结构分散剂(R1，R2，R3，R4为-H，R5为-CH3，n＝10,a＝5,b＝5,c＝5,d＝5)200g、JFC-6100g、抗坏血酸20g、异噻唑啉酮20g、有机硅消泡剂10g、去离子水350g。
烧瓶中加入去离子水，室温条件下开动搅拌器，缓慢依次加入上述数量的嵌段聚醚、烯丙基聚氧乙烯醚-丙烯酸聚合物、JFC-6、抗坏血酸、异噻唑啉酮、有机硅消泡剂，继续搅拌40min，得到切割液1号。其性能指标见附表。
实施例二
配制1000g切割液，各组分配比如下：嵌段聚醚(R为乙氧基，n＝50，m+q＝40)600g、梳型结构分散剂(R1，R2，R3，R4为-CH3，R5为-CH2CH3，n＝50,a＝30,b＝30,c＝30,d＝30)100g、磺化油40g、二丁基羟基甲苯1g、苯甲酸钠0.5g、聚醚改性硅油消泡剂0.5g、去离子水258g。
烧瓶中加入去离子水，室温条件下开动搅拌器，缓慢依次加入上述数量的嵌段聚醚、甲基烯丙基聚氧乙烯醚-丙烯酸-甲基丙烯酸酯聚合物、磺化油、二丁基羟基甲苯、苯甲酸钠、聚醚改性硅油消泡剂，继续搅拌40min，得到切割液2号。其性能指标见附表。
实施例三
配制1000g切割液，各组分配比如下：嵌段聚醚(R为丙氧基，n＝80,m+q＝70)500g、梳型结构分散剂(R1，R2为-H，R3，R4为-CH3，R5为-CH3，n＝30,a＝18,b＝18,c＝18,d＝18)150g、快速渗透剂T 70g、茶多酚10g、山梨酸钾10g、高碳醇消泡剂5g、去离子水255g。
烧瓶中加入去离子水，室温条件下开动搅拌器，缓慢依次加入上述数量的嵌段聚醚、烯丙基聚氧乙烯醚-甲基丙烯酸-丙烯酰胺聚合物、快速渗透剂T、茶多酚、山梨酸钾、高碳醇消泡剂，继续搅拌40min，得到切割液3号。其性能指标见附表。
实施例四
配制1000g切割液，各组分配比如下：嵌段聚醚(R为甲氧基，n＝20，m+q＝70)400g、梳型结构分散剂(R1，R2，R3为-CH3，R4为-H，R5为-CH2CH3，n＝10,a＝30,b＝20,c＝30,d＝20)180g、硅醇类非离子表面活性剂50g、吩噻嗪5g、尼泊金酯5g、有机硅消泡剂2g、去离子水358g。
烧瓶中加入去离子水，室温条件下开动搅拌器，缓慢依次加入上述数量的嵌段聚醚、甲基烯丙基聚氧乙烯醚-丙烯酸-丙烯酸酯-甲基丙烯酰胺聚合物、硅醇类非离子表面活性剂、吩噻嗪、尼泊金酯、有机硅消泡剂，继续搅拌40min，得到切割液4号。其性能指标见附表。
实施例五
配制1000g切割液，各组分配比如下：嵌段聚醚(R为丙氧基，n＝80，m+q＝10)350g、梳型结构分散剂(R1，R2，R3为-H，R4为-CH3，R5为-CH3，n＝28,a＝10,b＝19,c＝26,d＝5)180g、硅醇类非离子表面活性剂50g、吩噻嗪5g、尼泊金酯5g、有机硅消泡剂2g、去离子水408g。
烧瓶中加入去离子水，室温条件下开动搅拌器，缓慢依次加入上述数量的嵌段聚醚、甲基烯丙基聚氧乙烯醚-丙烯酸-丙烯酸酯-甲基丙烯酰胺聚合物、硅醇类非离子表面活性剂、吩噻嗪、尼泊金酯、有机硅消泡剂，继续搅拌40min，得到切割液5号。其性能指标见附表。
表1硅片切割液的理化指标
注：摩擦系数通过四球摩擦机测得，以摩擦系数可以表征产品的润滑性能。
表2硅片切割液的分散性
注：分散性是通过测定切割液对碳化硅微粉的悬浮能力来表征的，将切割液与碳化硅微粉按1:1质量比例混合均匀后，于100ml具塞量筒内静置，记录碳化硅微粉在切割液中的沉降高度h。悬浮率＝(100-h)*100％/100。
对于本领域的技术人员而言，阅读上述说明后，各种变化和修正无疑将显而易见。因此，所附的权利要求书应看作是涵盖本发明的真实意图和范围的全部变化和修正。在权利要求书范围内任何和所有等价的范围与内容，都应认为仍属本发明的意图和范围内。

Claims (10)

1.一种硅片切割液，其包括如下质量百分比的各组分：
2.根据权利要求1所述的硅片切割液，其特征在于：所述嵌段聚醚的结构式为：
R(PO)m(EO)n(PO)qH，
其中，R为OH或烷氧基，m为1～100的整数，n为1～100的整数，q为1～100的整数。
3.根据权利要求2所述的硅片切割液，其特征在于：所述的烷氧基为C1-C10烷氧基。
4.根据权利要求3所述的硅片切割液，其特征在于：所述的烷氧基为甲氧基、乙氧基或丙氧基。
5.根据权利要求2所述的硅片切割液，其特征在于：所述m和q的总和为10～70的整数，n为20～80的整数。
6.根据权利要求1-5任一项所述的硅片切割液，其特征在于：所述的分散剂是具有梳型结构的分散剂。
7.根据权利要求6所述的硅片切割液，其特征在于：所述的分散剂是由TPEG或/和APEG聚醚单体与丙烯酸、甲基丙烯酸、丙烯酸酯、甲基丙烯酸酯、丙烯酸酰胺、甲基丙烯酸酰胺聚合而成，结构式如下：
式中，R1，R2，R3，R4为-H或-CH3；R5为-CH3或-CH2CH3；n为1-200的整数；a,b,c,d各为1-100的整数。
8.根据权利要求7所述的硅片切割液，其特征在于：所述的分散剂结构式中，n为5-100的整数；a,b,c,d各为1-50的整数。
9.根据权利要求8所述的硅片切割液，其特征在于：所述的分散剂结构式中，n为10-50的整数；a,b,c,d各为5-30的整数。
10.根据权利要求1-5任一项所述的硅片切割液，其特征在于：所述的润湿剂为磺化油、快速渗透剂T、硅醇类非离子表面活性剂、脂肪醇聚氧乙烯醚中的一种或几种的混合物；所述的抗氧化剂为抗坏血酸、二丁基羟基甲苯、茶多酚、吩噻嗪中的一种或几种的混合物；所述的防腐剂为异噻唑啉酮、苯甲酸钠、山梨酸、山梨酸盐、尼泊金酯类中的一种或几种的混合物；所述的消泡剂为有机硅消泡剂、聚醚改性硅油消泡剂、高碳醇消泡剂中的一种或几种的混合物。
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