CN108865542A - 一种去蜡液及其制备方法与应用 - Google Patents
一种去蜡液及其制备方法与应用 Download PDFInfo
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- LWZFANDGMFTDAV-BURFUSLBSA-N [(2r)-2-[(2r,3r,4s)-3,4-dihydroxyoxolan-2-yl]-2-hydroxyethyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O LWZFANDGMFTDAV-BURFUSLBSA-N 0.000 claims description 4
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- 239000002253 acid Substances 0.000 description 1
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- LPEBYPDZMWMCLZ-CVBJKYQLSA-L zinc;(z)-octadec-9-enoate Chemical compound [Zn+2].CCCCCCCC\C=C/CCCCCCCC([O-])=O.CCCCCCCC\C=C/CCCCCCCC([O-])=O LPEBYPDZMWMCLZ-CVBJKYQLSA-L 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D10/00—Compositions of detergents, not provided for by one single preceding group
- C11D10/04—Compositions of detergents, not provided for by one single preceding group based on mixtures of surface-active non-soap compounds and soap
- C11D10/042—Compositions of detergents, not provided for by one single preceding group based on mixtures of surface-active non-soap compounds and soap based on anionic surface-active compounds and soap
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D10/00—Compositions of detergents, not provided for by one single preceding group
- C11D10/04—Compositions of detergents, not provided for by one single preceding group based on mixtures of surface-active non-soap compounds and soap
- C11D10/045—Compositions of detergents, not provided for by one single preceding group based on mixtures of surface-active non-soap compounds and soap based on non-ionic surface-active compounds and soap
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/14—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aliphatic hydrocarbons or mono-alcohols
- C11D1/146—Sulfuric acid esters
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/22—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aromatic compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/22—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aromatic compounds
- C11D1/24—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aromatic compounds containing ester or ether groups directly attached to the nucleus
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/34—Derivatives of acids of phosphorus
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
- C11D2111/10—Objects to be cleaned
- C11D2111/14—Hard surfaces
- C11D2111/22—Electronic devices, e.g. PCBs or semiconductors
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Abstract
本发明涉及半导体工业用清洗剂领域,尤其涉及一种去蜡液及其制备方法与应用。该去蜡液的配方为:N‑甲基吡咯烷酮15.0kg、氢氧化钾0.1kg、碳酸钾3.4kg、硬脂酸钠3.0kg、十二烷基硫酸钠0.6kg、吐温20 1.5kg、蓖麻油酸锌1.5kg和水74.9kg。该去蜡液去蜡活性高,不会对人体产生显著毒性、能够去除半导体晶片上多余的蜡以及在加工过程中吸附在晶片表面的颗粒物。其制备方法全程自动化,不会引入杂质和污染,能使去蜡液具有较佳的作用效果。将该去蜡液用于去除半导体抛光后多余的蜡,能达到很好的去除效果。
Description
技术领域
本发明涉及半导体工业用清洗剂领域,尤其涉及一种去蜡液及其制备方法与应用。
背景技术
在半导体晶片的制作过程中,为了增加晶片的亮度,通常需要对晶片进行抛光处理,一般是将蜡涂在待抛光的晶片的一面,将其固定使其可转动,然后对另一面抛光,抛光完成后需要除去多余的蜡。
在中国专利201410646025.9中公开了清洁半导体晶片的方法,其除蜡的清洁液中含有微气泡、季铵氢氧化物和表面活性剂。其中含有的季铵氢氧化物除含有较强的腐蚀性外,毒性也较大,会影响机体的生育能力。因此,提供一种去蜡效果好,毒性低的去蜡液配方非常必要。
发明内容
本发明的目的在于提供一种半导体高活性去蜡液,该去蜡液配方合理,去蜡活性高,不会对人体产生显著毒性,能够去除半导体晶片上多余的蜡以及在加工过程中吸附在晶片表面的颗粒物。
本发明的第二目的在于提供上述去蜡液的制备方法,该制备方法全程自动化,不会引入杂质和污染,能使去蜡液具有较佳的作用效果。
本发明的第三目的在于提供上述去蜡液的应用,将其用于去除半导体抛光后多余的蜡,能达到很好的去除效果。
本发明解决其技术问题是采用以下技术方案来实现:
本发明提出一种半导体高活性去蜡液,按重量份计,其包括以下组分:
进一步地,在本发明较佳实施例中,按质量百分数计,其包括以下组分:
进一步地,在本发明较佳实施例中,按质量百分数计,其包括以下组分:
进一步地,在本发明较佳实施例中,所述无机碱选自氢氧化钾、氢氧化钠、碳酸钠和碳酸钾中的至少一种。在一些具体的实施方式中,无机碱选自碳酸钠和碳酸钾中至少一种,可选地,还含有氢氧化钠和氢氧化钾;上述无机碱安全性和稳定性都好,形成的水溶液对人体损害很小。
进一步地,在本发明较佳实施例中,所述阴离子表面活性剂和非离子表面活性剂和的质量比为1:(1.5-3),在一些具体的实施方式中,阴离子表面活性剂和非离子表面活性剂的质量比为1:2.5、1:3、1:1.5和1:2。
进一步地,在本发明较佳实施例中,阴离子表面活性剂选自烷基磺酸盐、烷基二苯醚二磺酸盐、烷基酚聚氧乙烯醚磷酸酯盐、脂肪醇聚氧乙烯醚硫酸盐中一种或多种;优选地,阴离子表面活性剂选自十二烷基硫酸钠、十二烷基苯磺酸钠、十二烷基磷酸钠、十二烷基二苯醚二磺酸钠中的一种或多种。
进一步地,在本发明较佳实施例中,所述非离子表面活性剂为多元醇脂类非离子表面活性剂。具体地,其中多元醇脂类非离子表面活性剂为Span和Tween系列表面活性剂;其中吐温系列可选地为吐温20、吐温40、吐温60、吐温80和吐温85中任意一种;司盘系列可选地为司盘20、司盘40、司盘60和司盘80中任意一种。
本发明的一些具体实施方式中,阴离子表面活性剂和非离子表面活性剂复配的具体实例包括:十二烷基硫酸钠与吐温20、十二烷基苯磺酸酸钠和吐温80、十二烷基磷酸钠和司盘20、十二烷基硫酸钠和司盘80、十二烷基硫酸钠和吐温40、十二烷基磷酸钠和司盘60。
本发明提供的去蜡液呈淡黄色液体,去蜡活性高,对抛光蜡具有很好的去除效果,且不残留蜡颗粒,本发明提供的去蜡液成分稳定安全,不易挥发,不属于易燃品和危险品,通过密闭容器存放在阴凉、避光的环境中能够增加其保质期限。
本发明还提出了上述去蜡液的制备方法,其包括以下步骤:依次称取上述配方量的各原料组分,利用气动隔膜泵传送到反应釜中,经过定时循环搅拌使各原料组分混合均匀,采用精密过滤器过滤后即得,经检验合格后利用精密自动灌装机进行灌装。
其制备流程图为:来料检测→送料→过滤→混合→循环搅拌→精密过滤→检测→灌装→标贴→检验→入库。
本发明还提出了上述去蜡液在去除抛光蜡中的应用。
本发明还提供上述应用的具体操作方法,将上述去蜡液倒入容器中,加入去离子水稀释至浓度10%-20%后使用;然后放入带有抛光蜡的半导体材料,在20℃至40℃下浸泡合适的时间后,取出用去离子水漂洗干净,再用高纯氮气吹干。
本发明较佳实施例提供的去蜡液及其制备方法与应用的有益效果包括:本发明选用N-甲基吡咯烷酮和水作为溶剂体系,加入阴离子表面活性剂和非离子活性剂,并添加无机碱,能够溶解并乳化抛光蜡,去除大多数的抛光蜡,且有大量微小颗粒残留,而添加硬脂酸钠和蓖麻油酸锌后,能够提高去蜡液的活性,能够增强溶液体系对抛光蜡的乳化和去除效果,且对肉眼不易发现的抛光蜡细小颗粒也能完全去除,此外,本发明提供的去蜡液不易挥发不会对人体产生显著毒性。其制备方法全程自动化,不会引入杂质和污染,能使去蜡液具有较佳的作用效果。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚,下面将对本发明实施例中的技术方案进行清楚、完整地描述。实施例中未注明具体条件者,按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者,均为可以通过市售购买获得的常规产品。
以下结合实施例对本发明的特征和性能作进一步的详细描述。
实施例1
本实施例提供的半导体高活性去蜡液,其配方如下:N-甲基吡咯烷酮15.0kg、氢氧化钾0.1kg、碳酸钾3.4kg、硬脂酸钠3.0kg、十二烷基硫酸钠0.6kg、吐温20 1.5kg、蓖麻油酸锌1.5kg和水74.9kg。
本实施例提供的去蜡液的制备方法,包括以下步骤:依次称取上述配方量的各原料组分,利用气动隔膜泵传送到反应釜中,经过定时循环搅拌450s让各种原材料混合反应均匀,采用精密过滤器过滤后即得,经检验合格后利用精密自动灌装机进行灌装。
实施例2
本实施例提供的半导体高活性去蜡液,其配方如下:N-甲基吡咯烷酮12.0kg、碳酸钾1.0kg、硬脂酸钠2.5kg、十二烷基硫酸钠0.8kg、吐温80 2.0kg、蓖麻油酸锌1.0kg和水80.7kg,制备方法同实施例1。
实施例3
本实施例提供的半导体高活性去蜡液,其配方如下:N-甲基吡咯烷酮18.0kg、碳酸钠2.0kg、硬脂酸钠3.5kg、十二烷基磷酸钠0.2kg、司盘20 0.6kg、蓖麻油酸锌2.0kg和水73.7kg,制备方法同实施例1。
实施例4
本实施例提供的半导体高活性去蜡液,其配方如下:N-甲基吡咯烷酮20.0kg、碳酸钠0.9kg、氢氧化钠0.1kg、硬脂酸钠4.0kg、十二烷基苯磺酸钠1.0kg、司盘80 1.5kg、蓖麻油酸锌0.5kg和水72.0kg,制备方法同实施例1。
实施例5
本实施例提供的半导体高活性去蜡液,其配方如下:N-甲基吡咯烷酮10.0kg、碳酸钠6.0kg、硬脂酸钠2.0kg、十二烷基硫酸钠0.2kg、吐温40 0.6kg、蓖麻油酸锌2.5kg和水78.7kg,制备方法同实施例1。
实施例6
本实施例提供的半导体高活性去蜡液,其配方如下:N-甲基吡咯烷酮15.0kg、碳酸钾5.0kg、硬脂酸钠2.5kg、十二烷基磷酸钠0.7kg、司盘60 1.4kg、蓖麻油酸锌1.0kg和水74.4kg,制备方法同实施例1。
对比例1
本对比例提供的去蜡液,与实施例1提供的去蜡液的区别在于:将蓖麻油酸锌采用等量的水替代。
对比例2
本对比例提供的去蜡液,与实施例1提供的去蜡液的区别在于:将硬脂酸钠替换成等量的水。
对比例3
本对比例提供的去蜡液,与实施例1提供的去蜡液的区别在于:将硬脂酸钠和蓖麻油酸锌替换成等量的水。
试验例1
为了评价上述实施例1~6和对比例1~3的去蜡液对抛光蜡的去除效果,进行如下实验。将去蜡液倒入容器中,加入去离子水稀释至浓度为15%;然后放入带有抛光蜡的半导体材料,在30℃下浸泡合适10min,取出用去离子水漂洗干净,再用高纯氮气吹干。通过光学显微镜和肉眼观察抛光蜡的去除情况,结果如表1所示。
抛光蜡去除情况的评价基准
◎:肉眼观察抛光蜡去除100%,显微镜观察表面无抛光蜡颗粒残留;
○:肉眼观察抛光蜡去除100%,显微镜观察表面颗粒有颗粒残留物;
△:肉眼观察抛光蜡去除80%;
×:肉眼观察抛光蜡去除小于60%。
为了评价去蜡液因长时间使用而挥发所损失的程度,进行如下实验。
将上述实施例1~6和对比例1~3中制备的去蜡液,在75℃下放置24h,测定去蜡液挥发度,结果如表1所示
挥发度(%)=[(实验开始去蜡液质量)-(24小时后去蜡液质量)/实验开始去蜡液质量]×100
<评价基准>
◎:小于1%
○:1%以上且小于5%
△:5%以上且小于10%
×:10%以上且小于20%
××:20%以上
表1评价结果
从上表的评价结果可知,从挥发度上看,实施例1-6以及对比例1-3提供的去蜡液的挥发情况没有明显差异;从对抛光蜡的去除效果上看,实施例1-6提供的去蜡液配方对抛光蜡能够很好的去除,且没有颗粒残留;而对比例2中的去蜡液配方,肉眼观察不到抛光蜡的存在,但通过显微镜观察,半导体表面存在颗粒物残留,说明在去蜡液中添加蓖麻油酸锌对去蜡液颗粒物的去除具有明显影响;而对比例1和对比3的抛光蜡的去除情况约80%,说明体系中硬脂酸钠能够促进去蜡液的对抛光蜡的乳化和溶解作用。由此可见去蜡液中采用蓖麻油乳酸锌和硬脂酸钠复配对于半导体上的抛光蜡的去除具有协同作用。
以上所描述的实施例是本发明一部分实施例,而不是全部的实施例。本发明的实施例的详细描述并非旨在限制要求保护的本发明的范围,而是仅仅表示本发明的选定实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
Claims (10)
1.一种半导体高活性去蜡液,按重量份计,其包括以下组分:
2.根据权利要求1所述的去蜡液,其特征在于,按质量百分数计,其包括以下组分:
3.根据权利要求1所述的去蜡液,其特征在于,按质量百分数计,其包括以下组分:
4.根据权利要求1-3任一项所述的去蜡液,其特征在于,所述无机碱选自氢氧化钾、氢氧化钠、碳酸钠和碳酸钾中的至少一种。
5.根据权利要求1-3任一项所述的去蜡液,其特征在于,所述阴离子表面活性剂和非离子表面活性剂和的质量比为1:(1.5-3)。
6.根据权利要求1-3任一项所述的去蜡液,其特征在于,所述阴离子表面活性剂选自十二烷基硫酸钠、十二烷基苯磺酸钠、十二烷基磷酸钠和十二烷基二苯醚二磺酸钠中一种或多种。
7.根据权利要求1-3任一项所述的去蜡液,其特征在于,所述非离子表面活性剂选自吐温20、吐温40、吐温60、吐温80、吐温85、司盘20、司盘40、司盘60和司盘80中一种或多种。
8.权利要求书1-7任一项所述半导体高活性去蜡液的制备方法,其包括以下步骤:依次称取上述配方量的各原料组分,利用气动隔膜泵传送到反应釜中,经过定时循环搅拌使各原料组分混合均匀,采用精密过滤器过滤后即得,经检验合格后利用精密自动灌装机进行灌装。
9.权利要求1-7任一项所述半导体高活性去蜡液在去除抛光蜡中的应用。
10.根据权利要求9所述的应用,其特征在于,所述去蜡液可以采用原液或者用去离子水稀释至浓度为10%-20%后使用。
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