CN112592771A - 一种半导体清洗剂及其制备方法 - Google Patents
一种半导体清洗剂及其制备方法 Download PDFInfo
- Publication number
- CN112592771A CN112592771A CN202011473109.9A CN202011473109A CN112592771A CN 112592771 A CN112592771 A CN 112592771A CN 202011473109 A CN202011473109 A CN 202011473109A CN 112592771 A CN112592771 A CN 112592771A
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- CN
- China
- Prior art keywords
- cleaning agent
- semiconductor cleaning
- parts
- mixed solution
- organic solvent
- 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.)
- Pending
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- 239000012459 cleaning agent Substances 0.000 title claims abstract description 60
- 239000004065 semiconductor Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000002736 nonionic surfactant Substances 0.000 claims abstract description 20
- 239000003945 anionic surfactant Substances 0.000 claims abstract description 19
- 239000003960 organic solvent Substances 0.000 claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims description 37
- 239000011259 mixed solution Substances 0.000 claims description 36
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 25
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 239000008367 deionised water Substances 0.000 claims description 23
- 229910021641 deionized water Inorganic materials 0.000 claims description 23
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 239000008139 complexing agent Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 7
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims description 7
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 7
- DZCAZXAJPZCSCU-UHFFFAOYSA-K sodium nitrilotriacetate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CC([O-])=O DZCAZXAJPZCSCU-UHFFFAOYSA-K 0.000 claims description 7
- 239000004094 surface-active agent Substances 0.000 claims description 7
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 5
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 4
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 4
- 150000001298 alcohols Chemical class 0.000 claims description 3
- 150000001408 amides Chemical class 0.000 claims description 3
- 150000007942 carboxylates Chemical class 0.000 claims description 3
- 150000002576 ketones Chemical class 0.000 claims description 3
- 239000004471 Glycine Substances 0.000 claims description 2
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 2
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 2
- 150000002334 glycols Chemical class 0.000 claims description 2
- 229920000570 polyether Polymers 0.000 claims description 2
- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 239000001509 sodium citrate Substances 0.000 claims description 2
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 2
- 235000011006 sodium potassium tartrate Nutrition 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 229940074439 potassium sodium tartrate Drugs 0.000 claims 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 36
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- 239000010703 silicon Substances 0.000 abstract description 32
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- 235000012431 wafers Nutrition 0.000 description 30
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- 239000007788 liquid Substances 0.000 description 21
- SVTBMSDMJJWYQN-UHFFFAOYSA-N 2-methylpentane-2,4-diol Chemical compound CC(O)CC(C)(C)O SVTBMSDMJJWYQN-UHFFFAOYSA-N 0.000 description 18
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- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 description 11
- -1 alkyl diphenyl ether Chemical compound 0.000 description 8
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- 229940048842 sodium xylenesulfonate Drugs 0.000 description 7
- QUCDWLYKDRVKMI-UHFFFAOYSA-M sodium;3,4-dimethylbenzenesulfonate Chemical compound [Na+].CC1=CC=C(S([O-])(=O)=O)C=C1C QUCDWLYKDRVKMI-UHFFFAOYSA-M 0.000 description 7
- BTMZHHCFEOXAAN-UHFFFAOYSA-N 2-[bis(2-hydroxyethyl)amino]ethanol;2-dodecylbenzenesulfonic acid Chemical compound OCCN(CCO)CCO.CCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O BTMZHHCFEOXAAN-UHFFFAOYSA-N 0.000 description 6
- MWKFXSUHUHTGQN-UHFFFAOYSA-N decan-1-ol Chemical compound CCCCCCCCCCO MWKFXSUHUHTGQN-UHFFFAOYSA-N 0.000 description 6
- 229940028356 diethylene glycol monobutyl ether Drugs 0.000 description 6
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 6
- JCGNDDUYTRNOFT-UHFFFAOYSA-N oxolane-2,4-dione Chemical compound O=C1COC(=O)C1 JCGNDDUYTRNOFT-UHFFFAOYSA-N 0.000 description 6
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- XFRVVPUIAFSTFO-UHFFFAOYSA-N 1-Tridecanol Chemical compound CCCCCCCCCCCCCO XFRVVPUIAFSTFO-UHFFFAOYSA-N 0.000 description 3
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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 description 3
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- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000011133 lead Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 3
- 239000011863 silicon-based powder Substances 0.000 description 3
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- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- FDIPWBUDOCPIMH-UHFFFAOYSA-N 2-decylphenol Chemical compound CCCCCCCCCCC1=CC=CC=C1O FDIPWBUDOCPIMH-UHFFFAOYSA-N 0.000 description 2
- JWAZRIHNYRIHIV-UHFFFAOYSA-N 2-naphthol Chemical compound C1=CC=CC2=CC(O)=CC=C21 JWAZRIHNYRIHIV-UHFFFAOYSA-N 0.000 description 2
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 2
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 2
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
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- 229910019142 PO4 Inorganic materials 0.000 description 2
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- UCEWJVUQTXFLFM-UHFFFAOYSA-N 1,4-dihexoxy-1,4-dioxobutane-2-sulfonic acid;sodium Chemical compound [Na].[Na].CCCCCCOC(=O)CC(S(O)(=O)=O)C(=O)OCCCCCC UCEWJVUQTXFLFM-UHFFFAOYSA-N 0.000 description 1
- CBCQTCPKFYFJEU-UHFFFAOYSA-N 1,4-dioxo-1,4-dipentoxybutane-2-sulfonic acid Chemical compound CCCCCOC(=O)CC(S(O)(=O)=O)C(=O)OCCCCC CBCQTCPKFYFJEU-UHFFFAOYSA-N 0.000 description 1
- CUVLMZNMSPJDON-UHFFFAOYSA-N 1-(1-butoxypropan-2-yloxy)propan-2-ol Chemical compound CCCCOCC(C)OCC(C)O CUVLMZNMSPJDON-UHFFFAOYSA-N 0.000 description 1
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- 241000721179 Clarias Species 0.000 description 1
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- SUAKHGWARZSWIH-UHFFFAOYSA-N N,N‐diethylformamide Chemical compound CCN(CC)C=O SUAKHGWARZSWIH-UHFFFAOYSA-N 0.000 description 1
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- 125000001117 oleyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])/C([H])=C([H])\C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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- AJXVJQAPXVDFBT-UHFFFAOYSA-M sodium;naphthalen-2-olate Chemical compound [Na+].C1=CC=CC2=CC([O-])=CC=C21 AJXVJQAPXVDFBT-UHFFFAOYSA-M 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- 238000003911 water pollution Methods 0.000 description 1
Images
Classifications
-
- 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
-
- 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
- C11D3/0005—Other compounding ingredients characterised by their effect
- C11D3/0026—Low foaming or foam regulating compositions
-
- 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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Abstract
本申请公开了一种半导体清洗剂及其制备方法,属于半导体清洗技术领域。该半导体清洗剂包括非离子表面活性剂、阴离子表面活性剂及有机溶剂,按质量份数计,非离子表面活性剂2‑5份,阴离子表面活性剂9‑12份、有机溶剂3‑6份。通过半导体清洗剂制备方法制备的半导体清洗剂对硅片表面的研磨剂、金属离子等具有极佳的分散性能和容忍度,清洗表面均匀光洁,极好的满足了客户的生产需求,同时降低了对环境的污染。
Description
技术领域
本申请涉及一种半导体清洗剂及其制备方法,属于半导体清洗技术领域。
背景技术
在硅晶体管和集成电路生产中,几乎每道工序都有硅片清洗的问题,硅片的好坏对器件性能有很严重的影响,处理不当,可能使硅片全部报废,做不出合格的产品,或者制造出来的产品性能低劣,稳定性和可靠性很差。
硅材料经过一系列的加工后形成的硅片的表面会形成砂粒、切削磨料、指纹及金属离子,清洗的目的就是为了去除硅片表面颗粒、金属离子以及有机物等污染物,使硅片表面达到无腐蚀氧化、无残留等技术指标。
在现有的硅晶片清洗液中,会选择盐酸、强碱液、或含有磷酸盐类的表面活性剂作为清洗剂,但是盐酸具有腐蚀性,不能去除颗粒物和有机成分,强碱液清洗剂整体去除效果不理想,具有磷酸盐类表面活性剂的清洗剂虽然清洗效果好,但是对环境不友好,易造成水源富营养化、水污染等问题。因此,随着人们环保意识的日益提高,硅晶片清洗剂的无磷化必将成为日后的发展趋势,可以降低企业的污水处理难度,保护环境。
发明内容
为了解决上述问题,提供了一种半导体清洗剂及其制备方法,通过该方法制备的半导体清洗剂对硅片表面的研磨剂、金属离子等具有极佳的分散性能和容忍度,清洗表面均匀光洁,极好的满足了客户的生产需求,同时降低了对环境的污染。
根据本申请的一个方面,提供了一种半导体清洗剂,包括非离子表面活性剂、阴离子表面活性剂及有机溶剂,按质量份数计,所述非离子表面活性剂2-5份,阴离子表面活性剂9-12份、有机溶剂3-6份。
优选地,还包括络合剂和PH调节剂,按质量份数计,络合剂1-8份,PH调节剂将所述清洗剂PH值调节至10-13.5。
优选地,非离子表面活性剂3-4份,阴离子表面活性剂9-11份、有机溶剂4-5.5份,络合剂3-6份。
优选地,所述阴离子表面活性剂选自羧酸盐类、磺酸盐类及硫酸盐类表面活性剂中的一种或多种。
进一步地,羧酸盐类包括DOW D-518聚羧酸盐、辛烯基琥珀酸酐;磺酸盐类包括十二烷基苯磺酸乙醇胺、十二烷基苯磺酸二乙醇胺、十二烷基苯磺酸三乙醇胺、二甲苯磺酸钠、琥珀酸二己酯单磺酸钠、琥珀酸二戊酯单磺酸钠、科莱恩SAS-60仲烷基磺酸钠、DOWC10L烷基二苯醚磺酸盐;硫酸盐类包括异构十醇聚氧乙烯醚硫酸钠、异构十三醇聚氧乙烯醚硫酸钠、萘酚聚氧乙烯醚硫酸钠、辛基酚聚氧乙烯醚硫酸钠、DOW AS-801聚氧乙烯醚硫酸钠。
优选地,所述非离子表面活性剂选自脂肪醇聚氧乙烯醚、烷基酚聚氧乙烯醚、聚醚类表面活性剂中的一种或多种。
进一步地,脂肪醇聚氧乙烯醚包括异构十醇聚氧乙烯醚、异构十醇聚氧乙烯聚氧丙烯醚、异构十三醇聚氧乙烯醚、异构十三醇聚氧乙烯聚氧丙烯醚、月桂醇聚氧乙烯醚、月桂醇聚氧乙烯醚聚氧丙烯醚、丁醇聚氧乙烯醚聚氧丙烯醚;
烷基酚聚氧乙烯醚包括癸基酚聚氧乙烯醚、辛基酚聚氧乙烯醚、辛基酚聚氧乙烯聚氧丙烯醚、壬基酚聚氧乙烯聚氧丙烯醚、癸基酚聚氧乙烯聚氧丙烯醚、β-萘酚聚氧乙烯醚、双酚A-聚氧乙烯醚;
非离子表面活性剂还包括DOW EH-9异构醇聚氧乙烯醚、AKZO Ethylan 1005异构醇聚氧乙烯醚、DOW TWN-100X支链仲醇聚氧乙烯醚、DOW L-61 EO/PO共聚物、AKZOEthomeen O/12LC油基聚氧乙烯醚。
优选地,所述有机溶剂选自二醇衍生物、酮类、醇类、酰胺类中的一种或多种;
醇类包括:甲醇、乙醇、2-甲基-2,4戊二醇、1-丙醇、2-丙醇、1-己醇、1-壬醇、乙二醇单乙醚、乙二醇单丁醚、二甘醇单乙醚、二甘醇单乙醚、二甘醇单丁醚、丙二醇单乙醚、丙二醇单乙醚中选择的至少一种化合物,丙二醇单丁醚,二丙二醇单甲醚,二丙二醇单乙醚,二丙二醇单丁醚,二甘醇二甲醚,二丙二醇二甲醚;
酮类包括N-甲基吡咯烷酮、N-乙基吡咯烷酮;
酰胺类包括甲酰胺,一甲基甲酰胺,二甲基甲酰胺,一乙基甲酰胺,二乙基甲酰胺,乙酰胺,一甲基乙酰胺;
所述络合剂选自乙二胺四乙酸二钠、氨三乙酸三钠、酒石酸钾钠、柠檬酸钠、乙醇胺、二乙醇胺、三乙醇胺、甘氨酸中的一种或多种。
根据本申请的另一方面,提供了一种前述的半导体清洗剂的制备方法,包括以下步骤:
S1、第一混合液的制备:称取非离子表面活性剂、阴离子表面活性剂及有机溶剂,向反应釜内加入有机溶剂,向有机溶剂内加入非离子表面活性剂,进行第一次混合搅拌,然后再向反应釜内加入阴离子型表面活性剂,进行第二次混合搅拌,获得第一混合液;
S2、第二混合液的制备:将PH调节剂、络合剂及去离子水进行混合溶解,获得第二混合液;
S3、向第二混合液中加入第一混合液,进行充分搅拌混合,获得所述半导体清洗剂。
半导体清洗剂的PH值为10-13.5。
半导体清洗剂的PH值为11-13。
优选地,在步骤S1中,还包括加入去离子水,在步骤S2中去离子水为步骤S1中去离子水的3-9倍。
本申请的有益效果包括但不限于:
1.根据本申请的半导体清洗剂,具有对硅晶片表面的研磨剂、金属离子等具有极佳的分散性能和容忍度,清洗表面均匀光洁,无任何花斑、砂粒、研磨料、金属离子及指纹等残留,通过滤纸擦拭,无任何硅粉等物质残留,极好的满足了客户的生产需求,同时降低了对环境的污染。
2.根据本申请的半导体清洗剂,其有机溶剂、非离子表面活性剂及阴离子表面活性剂通过合理的配比,使得半导体清洗剂具有优异的分散、渗透和乳化效果,能快速浸入油污与硅晶片,达到快速剥离的效果和油污乳化效果,能很好的乳化硅晶片表面的颗粒物和有机物,不伤底材,并且低泡易降解。
附图说明
此处所说明的附图用来提供对本申请的进一步理解,构成本申请的一部分,本申请的示意性实施例及其说明用于解释本申请,并不构成对本申请的不当限定。在附图中:
图1为本申请实施例1制备的1#清洗剂清洗的硅晶片表面前后对比图;
图2为本申请实施例2制备的2#清洗剂清洗的硅晶片表面前后对比图;
图3为本申请实施例3制备的3#清洗剂清洗的硅晶片表面前后对比图;
具体实施方式
下面结合实施例详述本申请,但本申请并不局限于这些实施例。
如无特别说明,本申请的实施例中的原料和催化剂均通过商业途径购买。
实施例1
S1、配置第一混合液:
其成分和用量如下:
有机溶剂:
二乙二醇丁醚 1.5g
2-甲基-2,4戊二醇 2.5g
非离子表面活性剂:
DOW EH-9异构醇聚氧乙烯醚 2.5g
辛基酚聚氧乙烯聚氧丙烯醚 0.5g
阴离子表面活性剂:
十二烷基苯磺酸乙醇胺 4.5g
琥珀酸二己酯单磺酸钠 2g
二甲苯磺酸钠 3g
配制工艺:往反应釜中加入去离子水100克,缓慢加入二乙二醇丁醚1.5克,搅拌分散溶解;然后缓慢加入2-甲基-2,4戊二醇2.5克,搅拌分散溶解;然后缓慢加入DOW EH-9异构醇聚氧乙烯醚2.5克,充分反应,分散溶解至均匀透明液体;然后缓慢加入辛基酚聚氧乙烯聚氧丙烯醚0.5克,充分反应,分散溶解至均匀透明液体;边搅拌,缓慢加入二甲苯磺酸钠3克,充分反应,至固体完全溶解分散,直至呈现均匀透明液体;边搅拌,缓慢加入十二烷基苯磺酸乙醇胺4.5克,充分反应,分散溶解至均匀透明液体;边搅拌,缓慢加入琥珀酸二己酯单磺酸钠2克,充分反应,分散溶解至均匀透明液体;获得第一混合液1#。
S2、在反应釜中加入600克去离子水,一次加入氢氧化钾4克,氨三乙酸三钠2克,乙二胺四乙酸二钠2.5克,充分搅拌溶解,获得第二混合液1#;
S3、向第二混合液1#缓慢加入上述第一混合液1#,加上去离子水,定容至1升,充分搅拌1小时至分散完全,即获得半导体清洗剂1#。
实施例2
S1、配置第一混合液:
其成分和用量如下:
有机溶剂:
二乙二醇丁醚 2.5g
2-甲基-2,4戊二醇 2.5g
非离子表面活性剂:
辛基酚聚氧乙烯醚 2.5g
异构十醇聚氧乙烯醚 1.5g
阴离子表面活性剂:
十二烷基苯磺酸三乙醇胺 4.5g
DOW C10L烷基二苯醚磺酸盐 3.5g
二甲苯磺酸钠 3g
配制工艺:往反应釜中加入去离子水100克,缓慢加入二乙二醇丁醚2.5克,搅拌分散溶解;然后缓慢加入2-甲基-2,4戊二醇2.5克,搅拌分散溶解;然后缓慢加入辛基酚聚氧乙烯醚2.5克,充分反应,分散溶解至均匀透明液体;然后缓慢加入异构十醇聚氧乙烯醚1.5克,充分反应,分散溶解至均匀透明液体;边搅拌,缓慢加入二甲苯磺酸钠3克,充分反应,至固体完全溶解分散,直至呈现均匀透明液体;边搅拌,缓慢加入十二烷基苯磺酸三乙醇胺4.5克,充分反应,分散溶解至均匀透明液体;边搅拌,缓慢加入DOW C10L烷基二苯醚磺酸盐3.5克,充分反应,分散溶解至均匀透明液体,获得第一混合液2#。
S2、在反应釜中加入600克去离子水,一次性加入氢氧化钾4克,氨三乙酸三钠2克,乙二胺四乙酸二钠2.5克,充分搅拌溶解,获得第二混合液2#;
S3、向第二混合液2#缓慢加入上述第一混合液2#,加上去离子水,定容至1升,充分搅拌1小时至分散完全,即获得半导体清洗剂2#。
实施例3
S1、配置第一混合液:
其成分和用量如下:
有机溶剂:
二乙二醇丁醚 2.5g
二丙二醇二甲醚 3g
非离子表面活性剂:
异构十醇聚氧乙烯醚 2.5g
异构十三醇聚氧乙烯醚 1.5g
阴离子表面活性剂:
十二烷基苯磺酸乙醇胺 4.5g
琥珀酸二己酯单磺酸钠 3.5g
科莱恩SAS-60仲烷基磺酸钠 3g
配制工艺:往反应釜中加入去离子水100克,缓慢加入二乙二醇丁醚2.5克,搅拌分散溶解;然后缓慢加入二丙二醇二甲醚3克,搅拌分散溶解;然后缓慢加入异构十醇聚氧乙烯醚2.5克,充分反应,分散溶解至均匀透明液体;然后缓慢加入异构十三醇聚氧乙烯醚1.5克,充分反应,分散溶解至均匀透明液体;边搅拌,缓慢加入科莱恩SAS-60仲烷基磺酸钠3克,充分反应,至固体完全溶解分散,直至呈现均匀透明液体;边搅拌,缓慢加入十二烷基苯磺酸三乙醇胺4.5克,充分反应,分散溶解至均匀透明液体;边搅拌,缓慢加入琥珀酸二己酯单磺酸钠3.5克,充分反应,分散溶解至均匀透明液体,获得第一混合液3#。
S2、在反应釜中加入600克去离子水,搅拌下,一次加入氢氧化钾4克,氨三乙酸三钠2克,乙二胺四乙酸二钠2.5克,充分搅拌溶解,获得第二混合液3#;
S3、向第二混合液3#缓慢加入上述第一混合液3#,加上去离子水,定容至1升,充分搅拌1小时至分散完全,即获得半导体清洗剂3#。
对比例1
S1、配置第一混合液:
其成分和用量如下:
有机溶剂:
二乙二醇丁醚 2.5g
2-甲基-2,4戊二醇 2.5g
非离子表面活性剂:
辛基酚聚氧乙烯聚氧丙烯醚 9.4g
异构十醇聚氧乙烯醚 5.6g
此处需要说明的是,本实施例中的非离子表面活性剂的用量与实施例2中的非离子表面活性剂和阴离子表面活性剂的用量相同。
配制工艺:往反应釜中加入去离子水100克,缓慢加入二乙二醇丁醚2.5克,搅拌分散溶解;然后缓慢加入2-甲基-2,4戊二醇2.5克,搅拌分散溶解;然后缓慢加入辛基酚聚氧乙烯聚氧丙烯醚9.4克,充分反应,分散溶解至均匀透明液体;然后缓慢加入异构十醇聚氧乙烯醚5.6克,充分反应,分散溶解至均匀透明液体,获得对比第一混合液1'#。
S2、在反应釜中加入600克去离子水,搅拌下,一次加入氢氧化钾4克,氨三乙酸三钠2克,乙二胺四乙酸二钠2.5克,充分搅拌溶解,获得第二混合液1'#;
S3、向第二混合液2#缓慢加入上述第一混合液2#,加上去离子水,定容至1升,充分搅拌1小时至分散完全,即获得半导体清洗剂1'#。
对比例2
S1、配置第一混合液:
其成分和用量如下:
有机溶剂:
二乙二醇丁醚 2.5g
2-甲基-2,4戊二醇 2.5g
阴离子表面活性剂:
十二烷基苯磺酸三乙醇胺 6g
DOW C10L烷基二苯醚磺酸盐 5g
二甲苯磺酸钠 4g
此处需要说明的是,本实施例中的阴离子表面活性剂的总用量与实施例2中的非离子表面活性剂和阴离子表面活性剂的用量相同。
配制工艺:往反应釜中加入去离子水100克,缓慢加入二乙二醇丁醚2.5克,搅拌分散溶解;然后缓慢加入2-甲基-2,4戊二醇2.5克,搅拌分散溶解;边搅拌,缓慢加入二甲苯磺酸钠4克,充分反应,至固体完全溶解分散,直至呈现均匀透明液体;边搅拌过程中,缓慢加入十二烷基苯磺酸三乙醇胺6克,充分反应,分散溶解至均匀透明液体;边搅拌,缓慢加入DOW C10L烷基二苯醚磺酸盐5克,充分反应,分散溶解至均匀透明液体,获得对比第一混合液2'#。
S2、在反应釜中加入600克去离子水,搅拌下,一次加入氢氧化钾4克,氨三乙酸三钠2克,乙二胺四乙酸二钠2.5克,充分搅拌溶解,获得第二混合液2'#;
S3、向第二混合液2'#缓慢加入上述第一混合液2'#,加上去离子水,定容至1升,充分搅拌1小时至分散完全,即获得半导体清洗剂2'#。
实施例4
使用半导体清洗剂1#-3#、1'#和2'#对工艺研磨后6寸硅晶片进行清洗,清洗过程中半导体清洗剂的温度为65℃,pH值为11-13,超声波振动搅拌,超声振动清洗时间为2-5分钟。
实施例5
性能测试:
1、各半导体清洗剂1#-3#、1'#和2'#对研磨剂的分散能力的测试
根据工艺线生产流程,分别以研磨剂10g/L、25g/L、100g/L溶解于半导体清洗剂1#-3#中,都均匀分散,未出现分层和沉淀现象,体系对研磨剂具有极佳的分散性能和容忍范围;同时将研磨剂100g/L溶解于半导体清洗剂1'#和2'#中,却出现了轻微的分层和浑浊现象。说明半导体清洗剂1'#和2'#对研磨剂的容忍度不如半导体清洗剂1#-3#。
2、金相检测
以下分别使用1#-3#、1'#和2'#对硅晶片进行清洗试验,具体工艺参数参考实施例4,硅晶片上占有大于5倍硅片正常研磨剂含量,按照工艺清洗前后的金相检测1000X倍的效果对比图。
由图1-图3可以看出,清洗之前,硅晶片上覆盖有研磨剂,清洗后,硅晶片表面均匀,研磨剂完全被去除。1#、2#和3#清洗的硅晶片表面更加均匀,色泽灰色一致,表面无任何残留和腐蚀现象。1'#和2'#清洗后亮点相对较多,表面不均匀,且有硅粉残留。
3、滤纸刮擦
采用中性滤纸,分别擦拭1#-3#、1'#和2'#清洗完的硅晶片。结果是:1#-3#清洗完的硅晶片,滤纸表面仍为白色,无任何硅粉及残渣显示。1'#和2'#清洗完的硅晶片,滤纸有硅粉残留在滤纸上,清洗效果相对较差。
4、对金属离子的分散能力
若硅晶片表面残留有金属离子,会影响后续线路板电路问题。半导体清洗剂1#-3#、1'#和2'#,分别对金属离子钙、镁、铜、镍、铁、铅的分散容忍度进行实验。由实验得出,半导体清洗剂1#-3#均对钙离子达到600ppm,对镁离子达到80ppm,对铜离子达到400ppm,对镍离子达到300ppm,对铁离子达到150ppm,对铅离子达到1000ppm,相应的溶液均显示澄清透明的状态;而半导体清洗剂1'#和2'#对钙离子达到600ppm,对镁离子达到80ppm,对铜离子达到400ppm,对镍离子达到300ppm,对铁离子达到150ppm,对铅离子达到1000ppm,相应的溶液均出现轻微浑浊,说明半导体清洗剂1'#和2'#对金属离子容忍度不如半导体清洗剂1#-3#,半导体清洗剂1#-3#对金属离子容忍度相对较高,能够满足硅晶片槽液金属离子的需求。
此处需要说明的是,本申请提供的半导体清洗剂,并不限于清洗硅晶片,也可适用于其它材质的半导体。
以上所述,仅为本申请的实施例而已,本申请的保护范围并不受这些具体实施例的限制,而是由本申请的权利要求书来确定。对于本领域技术人员来说,本申请可以有各种更改和变化。凡在本申请的技术思想和原理之内所作的任何修改、等同替换、改进等,均应包含在本申请的保护范围之内。
Claims (10)
1.一种半导体清洗剂,其特征在于,包括非离子表面活性剂、阴离子表面活性剂及有机溶剂,按质量份数计,所述非离子表面活性剂2-5份,阴离子表面活性剂9-12份、有机溶剂3-6份。
2.根据权利要求1所述的半导体清洗剂,其特征在于,还包括络合剂和PH调节剂,按质量份数计,络合剂1-8份,PH调节剂将所述清洗剂PH值调节至10-13.5。
3.根据权利要求2所述的半导体清洗剂,其特征在于,非离子表面活性剂3-4份,阴离子表面活性剂9-11份、有机溶剂4-5份,络合剂3-6份。
4.根据权利要求1所述的半导体清洗剂,其特征在于,所述阴离子表面活性剂选自羧酸盐类、磺酸盐类及硫酸盐类表面活性剂中的一种或多种。
5.根据权利要求2所述的半导体清洗剂,其特征在于,所述非离子表面活性剂选自脂肪醇聚氧乙烯醚、烷基酚聚氧乙烯醚、聚醚类表面活性剂中的一种或多种。
6.根据权利要求5所述的半导体清洗剂,其特征在于,所述有机溶剂选自二醇衍生物、酮类、醇类、酰胺类中的一种或多种;
所述络合剂选自乙二胺四乙酸二钠、氨三乙酸三钠、酒石酸钾钠、柠檬酸钠、乙醇胺、二乙醇胺、三乙醇胺、甘氨酸等的一种或多种。
7.如权利要求1-6任一所述的半导体清洗剂的制备方法,其特征在于,包括以下步骤:
S1、第一混合液的制备:称取非离子表面活性剂、阴离子表面活性剂及有机溶剂,向反应釜内加入有机溶剂,然后向有机溶剂内加入非离子表面活性剂,进行第一次混合搅拌,然后再向反应釜内加入阴离子型表面活性剂,进行第二次混合搅拌,获得第一混合液;
S2、第二混合液的制备:将PH调节剂、络合剂及去离子水进行混合溶解,获得第二混合液;
S3、向第二混合液中加入第一混合液,进行充分混合,获得所述半导体清洗剂。
8.根据权利要求7所述的半导体清洗剂的制备方法,其特征在于,
半导体清洗剂的PH值为10-13.5。
9.根据权利要求8所述的半导体清洗剂的制备方法,其特征在于,
半导体清洗剂的PH值为11-13。
10.根据权利要求7所述的半导体清洗剂的制备方法,其特征在于,在步骤S1中,还包括加入去离子水,在步骤S2中去离子水为步骤S1中去离子水的3-9倍。
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