CN116496851A - 一种半导体芯片清洗剂及其制备方法 - Google Patents
一种半导体芯片清洗剂及其制备方法 Download PDFInfo
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 7
- 150000002191 fatty alcohols Chemical class 0.000 claims description 7
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- BVIXLMYIFZGRBH-UHFFFAOYSA-M sodium;2-chloroethanesulfonate Chemical compound [Na+].[O-]S(=O)(=O)CCCl BVIXLMYIFZGRBH-UHFFFAOYSA-M 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 4
- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- 239000000176 sodium gluconate Substances 0.000 claims description 3
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- 235000012207 sodium gluconate Nutrition 0.000 claims description 3
- JOLVYUIAMRUBRK-UHFFFAOYSA-N 11',12',14',15'-Tetradehydro(Z,Z-)-3-(8-Pentadecenyl)phenol Natural products OC1=CC=CC(CCCCCCCC=CCC=CCC=C)=C1 JOLVYUIAMRUBRK-UHFFFAOYSA-N 0.000 claims description 2
- YLKVIMNNMLKUGJ-UHFFFAOYSA-N 3-Delta8-pentadecenylphenol Natural products CCCCCCC=CCCCCCCCC1=CC=CC(O)=C1 YLKVIMNNMLKUGJ-UHFFFAOYSA-N 0.000 claims description 2
- JOLVYUIAMRUBRK-UTOQUPLUSA-N Cardanol Chemical compound OC1=CC=CC(CCCCCCC\C=C/C\C=C/CC=C)=C1 JOLVYUIAMRUBRK-UTOQUPLUSA-N 0.000 claims description 2
- FAYVLNWNMNHXGA-UHFFFAOYSA-N Cardanoldiene Natural products CCCC=CCC=CCCCCCCCC1=CC=CC(O)=C1 FAYVLNWNMNHXGA-UHFFFAOYSA-N 0.000 claims description 2
- PTFIPECGHSYQNR-UHFFFAOYSA-N cardanol Natural products CCCCCCCCCCCCCCCC1=CC=CC(O)=C1 PTFIPECGHSYQNR-UHFFFAOYSA-N 0.000 claims description 2
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 abstract description 3
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- 230000000052 comparative effect Effects 0.000 description 10
- 229910052782 aluminium Inorganic materials 0.000 description 5
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- 239000012466 permeate Substances 0.000 description 1
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- ONJQDTZCDSESIW-UHFFFAOYSA-N polidocanol Chemical compound CCCCCCCCCCCCOCCOCCOCCOCCOCCOCCOCCOCCOCCO ONJQDTZCDSESIW-UHFFFAOYSA-N 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
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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
- C11D1/66—Non-ionic compounds
- C11D1/83—Mixtures of non-ionic with anionic compounds
- C11D1/831—Mixtures of non-ionic with anionic compounds of sulfonates with ethers of polyoxyalkylenes without phosphates
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/32—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of salts of sulfonic acids
-
- 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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/2003—Alcohols; Phenols
- C11D3/2006—Monohydric alcohols
- C11D3/201—Monohydric alcohols linear
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- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
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- C11D3/20—Organic compounds containing oxygen
- C11D3/2068—Ethers
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- 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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/2075—Carboxylic acids-salts thereof
- C11D3/2086—Hydroxy carboxylic acids-salts thereof
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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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
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- C11D3/26—Organic compounds containing nitrogen
- C11D3/30—Amines; Substituted amines ; Quaternized amines
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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- 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
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Abstract
本发明公开了一种半导体芯片清洗剂及其制备方法,涉及半导体技术领域,由以下质量百分含量的原料组成:磺酸型含氟表面活性剂3~6%、非离子表面活性剂6~10%、络合剂0.2~1%、乙醇0~3%、二乙二醇单丁醚3~8%,余量为去离子水;其制备是将磺酸型含氟表面活性剂、非离子表面活性剂加入到去离子水中,搅拌,向其中加入乙醇和二乙二醇单丁醚,搅拌,再加入络合剂,搅拌,即得。本发明清洗剂有着卓越的清洗效果,能够有效去除半导体芯片上的锡膏、焊锡膏、助焊剂残留等,清洗后芯片表面残留物少,从而有效改善水性清洗剂对狭缝清洗不到位的现象,避免芯片表面变色,该清洗剂可适用于超声波清洗工艺或喷淋清洗工艺。
Description
技术领域
本发明涉及半导体技术领域,尤其涉及一种半导体芯片清洗剂及其制备方法。
背景技术
随着电子信息产业的高速发展,电子产品向小型化、智能化、多功能、高可靠性方向发展。在集成电路芯片尺寸逐步缩小,集成度不断提高的情况下,电子工业对集成电路封装技术提出了越来越高的要求,因此半导体芯片键合区的质量将直接影响到集成电路器件的可靠性。
半导体芯片是通过在半导体片材上进行浸蚀,布线,制成的能实现某种功能的半导体器件。制造过程中需要在半导体芯片的表面电镀一层铝作为有源区金属层,参加电化学反应,在半导体芯片与框架键合步骤中,通常会采用锡铅焊料焊接,因此在真空回流焊后,芯片表面以及周边会残留大量助焊剂污染物;但残留的助焊剂会导致芯片表面的铝层变色,表面张力降低,如不清洗将会影响到后续金线和铝层的键合失效,以及会降低后续封装过程的可靠性。因此,采用清洗剂去除沾污在上述电镀有铝层的半导体芯片上的杂质是确保产品质量的必要手段。相较于溶剂型清洗剂,水基型清洗剂因有机组分比例较少,VOC和ODP值较低,具备环境友好等优势而被广泛使用。然而,现有的水基型清洗剂的清洗效果一般,对狭缝清洗不到位,芯片表面的铝层变色。
发明内容
基于背景技术存在的技术问题,本发明提出了一种半导体芯片清洗剂及其制备方法,该清洗剂能够有效去除半导体芯片上的锡膏、焊锡膏、助焊剂残留等,清洗后芯片表面残留物少。
本发明提出的一种半导体芯片清洗剂,由以下质量百分含量的原料组成:磺酸型含氟表面活性剂3~6%、非离子表面活性剂6~10%、络合剂0.2~1%、乙醇0~3%、二乙二醇单丁醚3~8%,余量为去离子水。
优选地,所述磺酸型含氟表面活性剂的制备如下:将环己烷和钠加入到反应容器中,在氮气保护下,滴加全氟辛醇,冰浴下反应,然后再向其中滴加2-氯乙基磺酸钠的环己烷溶液,加热,回流反应;反应结束后减压蒸馏回收环己烷,向其中加入热无水乙醇,抽滤,再用无水乙醇洗涤,干燥,即得。
优选地,所述钠、全氟辛醇、2-氯乙基磺酸钠的摩尔比为1.5~2:1:1~1.3。
优选地,将环己烷和钠加入到反应容器中,在氮气保护下,滴加全氟辛醇,冰浴下反应1~2h,然后再向其中滴加2-氯乙基磺酸钠的环己烷溶液,加热至70~75℃,回流反应7~10h。
优选地,所述非离子表面活性剂包括失水山梨醇脂肪酸酯聚氧乙烯醚;优选地,还包括腰果酚聚氧乙烯醚、脂肪醇聚氧乙烯醚中的至少一种。
优选地,所述非离子表面活性剂由失水山梨醇脂肪酸酯聚氧乙烯醚和脂肪醇聚氧乙烯醚按照1~3:1的质量比复配组成的。
优选地,所述络合剂是由葡萄糖酸钠和三乙醇胺按照2~4:1的质量比复配组成的。
本发明还提出了上述半导体芯片清洗剂的制备方法,步骤如下:将磺酸型含氟表面活性剂、非离子表面活性剂加入到去离子水中,搅拌,向其中加入乙醇和二乙二醇单丁醚,搅拌,再加入络合剂,搅拌,即得。
有益效果:本发明提出了一种半导体芯片清洗剂,其原料中的磺酸型含氟表面活性剂具有强表面活性,能够减弱助焊剂等有机污染物成分与半导体芯片之间的相互作用,在超声波中易于从芯片中清除且不会二次附着;加入的非离子表面活性剂与磺酸型含氟表面活性剂之间具有良好的协同作用,其协同作用有效增强清洗剂的渗透性,使其容易渗透到半导体芯片间隙中,快速浸润污染物与芯片之间的界面,从而消除助焊剂等残留物;加入的络合剂与表面活性剂相结合,有效去除芯片表面的金属离子。
本发明清洗剂有着卓越的清洗效果,能够有效去除半导体芯片上的锡膏、焊锡膏、助焊剂残留等,清洗后芯片表面残留物少,从而有效改善水性清洗剂对狭缝清洗不到位的现象,避免芯片表面变色,该清洗剂可适用于超声波清洗工艺或喷淋清洗工艺。
具体实施方式
下面,通过具体实施例对本发明的技术方案进行详细说明。
实施例1
磺酸型含氟表面活性剂,其制备如下:
将350mL环己烷和0.18mol的钠加入到反应容器中,在氮气保护下,滴加0.1mol的全氟辛醇,冰浴下反应2h,然后再向其中滴加250mL的0.5mol/L的2-氯乙基磺酸钠的环己烷溶液,加热至70℃,回流反应10h,减压蒸馏回收环己烷,向其中加入热无水乙醇,抽滤,再用无水乙醇洗涤2次,干燥,即得。
实施例2-5和对比例1-2
实施例2-5和对比例1-2公开的半导体芯片清洗剂,其配方如表1所示。
表1实施例2-5和对比例1-2中半导体芯片清洗剂配方组成(wt%)
其制备如下:将磺酸型含氟表面活性剂、失水山梨醇脂肪酸酯聚氧乙烯醚T60、脂肪醇聚氧乙烯醚AEO-9加入到去离子水中,搅拌,向其中加入乙醇和二乙二醇单丁醚,搅拌,再加入葡萄糖酸钠和三乙醇胺,搅拌,即得。
对本发明实施例2-5和对比例1-2中制备的半导体芯片清洗剂的性能进行检测,是将清洗剂和去离子水按照1:10的体积比混合,将半导体芯片放入其中,60℃下超声清洗5min,捞出,用去离子水冲洗干净。采用30×20显微镜进行镜检,每个实施例中清洗3个样品,结果统计见表。
表2半导体芯片清洗剂性能检测结果
从表2中可以看出,相较于对比例1,实施例4中同时采用磺酸型含氟表面活性剂和非离子表面活性剂时对有机污染物有更好的清除效果。对比例4中非离子表面活性剂仅采用失水山梨醇脂肪酸酯聚氧乙烯醚时,其清洗效果与实施例4还有一定的差距,这说明采用失水山梨醇脂肪酸酯聚氧乙烯醚和脂肪醇聚氧乙烯醚复配同磺酸型含氟表面活性剂共同使用时,其清洗效果更佳,且通过对实施例4和对比例2中体系的表面张力检测发现,对比例2中的表面张力降低至17mN/m,而实施例4中则降低至12mN/m,这说明采用失水山梨醇脂肪酸酯聚氧乙烯醚和脂肪醇聚氧乙烯醚复配的非离子表面活性剂,其与磺酸型含氟表面活性剂配合使用时的表面张力更低,渗透性更好,去除污染物效果更佳。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。
Claims (8)
1.一种半导体芯片清洗剂,其特征在于,由以下质量百分含量的原料组成:磺酸型含氟表面活性剂3~6%、非离子表面活性剂6~10%、络合剂0.2~1%、乙醇0~3%、二乙二醇单丁醚3~8%,余量为去离子水。
2.根据权利要求1所述的半导体芯片清洗剂,其特征在于,所述磺酸型含氟表面活性剂的制备如下:将环己烷和钠加入到反应容器中,在氮气保护下,滴加全氟辛醇,冰浴下反应,然后再向其中滴加2-氯乙基磺酸钠的环己烷溶液,加热,回流反应;反应结束后减压蒸馏回收环己烷,向其中加入热无水乙醇,抽滤,再用无水乙醇洗涤,干燥,即得。
3.根据权利要求2所述的半导体芯片清洗剂,其特征在于,所述钠、全氟辛醇、2-氯乙基磺酸钠的摩尔比为1.5~2:1:1~1.3。
4.根据权利要求2所述的半导体芯片清洗剂,其特征在于,将环己烷和钠加入到反应容器中,在氮气保护下,滴加全氟辛醇,冰浴下反应1~2h,然后再向其中滴加2-氯乙基磺酸钠的环己烷溶液,加热至70~75℃,回流反应7~10h。
5.根据权利要求1所述的半导体芯片清洗剂,其特征在于,所述非离子表面活性剂包括失水山梨醇脂肪酸酯聚氧乙烯醚;优选地,还包括腰果酚聚氧乙烯醚、脂肪醇聚氧乙烯醚中的至少一种。
6.根据权利要求5所述的半导体芯片清洗剂,其特征在于,所述非离子表面活性剂由失水山梨醇脂肪酸酯聚氧乙烯醚和脂肪醇聚氧乙烯醚按照1~3:1的质量比复配组成的。
7.根据权利要求1所述的半导体芯片清洗剂,其特征在于,所述络合剂是由葡萄糖酸钠和三乙醇胺按照2~4:1的质量比复配组成的。
8.一种如权利要求1-7任一项所述的半导体芯片清洗剂的制备方法,其特征在于,步骤如下:将磺酸型含氟表面活性剂、非离子表面活性剂加入到去离子水中,搅拌,向其中加入乙醇和二乙二醇单丁醚,搅拌,再加入络合剂,搅拌,即得。
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