CN114106934B - 一种蓝宝石晶圆清洗剂及其制备方法 - Google Patents
一种蓝宝石晶圆清洗剂及其制备方法 Download PDFInfo
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- CN114106934B CN114106934B CN202111449111.7A CN202111449111A CN114106934B CN 114106934 B CN114106934 B CN 114106934B CN 202111449111 A CN202111449111 A CN 202111449111A CN 114106934 B CN114106934 B CN 114106934B
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- cleaning agent
- cleaning
- sapphire wafer
- wafer cleaning
- organic
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- 239000012459 cleaning agent Substances 0.000 title claims abstract description 32
- 229910052594 sapphire Inorganic materials 0.000 title claims abstract description 32
- 239000010980 sapphire Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000003945 anionic surfactant Substances 0.000 claims abstract description 16
- -1 phosphodiester amino acid Chemical class 0.000 claims description 14
- 239000004094 surface-active agent Substances 0.000 claims description 8
- 239000012498 ultrapure water Substances 0.000 claims description 8
- 239000002738 chelating agent Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- 150000007529 inorganic bases Chemical class 0.000 claims description 6
- 150000007530 organic bases Chemical class 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000012752 auxiliary agent Substances 0.000 claims description 5
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 4
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
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- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
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- HXKKHQJGJAFBHI-UHFFFAOYSA-N 1-aminopropan-2-ol Chemical compound CC(O)CN HXKKHQJGJAFBHI-UHFFFAOYSA-N 0.000 claims description 2
- 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 2
- SBASXUCJHJRPEV-UHFFFAOYSA-N 2-(2-methoxyethoxy)ethanol Chemical compound COCCOCCO SBASXUCJHJRPEV-UHFFFAOYSA-N 0.000 claims description 2
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- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims description 2
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 claims description 2
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 2
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims description 2
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 2
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- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 2
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- 229940075557 diethylene glycol monoethyl ether Drugs 0.000 claims description 2
- LVTYICIALWPMFW-UHFFFAOYSA-N diisopropanolamine Chemical compound CC(O)CNCC(C)O LVTYICIALWPMFW-UHFFFAOYSA-N 0.000 claims description 2
- 229940043276 diisopropanolamine Drugs 0.000 claims description 2
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 2
- 229940102253 isopropanolamine Drugs 0.000 claims description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 239000000176 sodium gluconate Substances 0.000 claims description 2
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- 229940005574 sodium gluconate Drugs 0.000 claims description 2
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 2
- 239000000600 sorbitol Substances 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 abstract description 50
- 238000000034 method Methods 0.000 abstract description 14
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- 238000000227 grinding Methods 0.000 abstract description 9
- 239000003344 environmental pollutant Substances 0.000 abstract description 7
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- 235000012431 wafers Nutrition 0.000 description 32
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- 230000000052 comparative effect Effects 0.000 description 9
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 7
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- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 6
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- 230000015572 biosynthetic process Effects 0.000 description 6
- QWXYZCJEXYQNEI-OSZHWHEXSA-N intermediate I Chemical compound COC(=O)[C@@]1(C=O)[C@H]2CC=[N+](C\C2=C\C)CCc2c1[nH]c1ccccc21 QWXYZCJEXYQNEI-OSZHWHEXSA-N 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- 238000003786 synthesis reaction Methods 0.000 description 6
- COLNVLDHVKWLRT-QMMMGPOBSA-N L-phenylalanine Chemical compound OC(=O)[C@@H](N)CC1=CC=CC=C1 COLNVLDHVKWLRT-QMMMGPOBSA-N 0.000 description 5
- COLNVLDHVKWLRT-UHFFFAOYSA-N phenylalanine Natural products OC(=O)C(N)CC1=CC=CC=C1 COLNVLDHVKWLRT-UHFFFAOYSA-N 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- IAZDPXIOMUYVGZ-WFGJKAKNSA-N Dimethyl sulfoxide Chemical compound [2H]C([2H])([2H])S(=O)C([2H])([2H])[2H] IAZDPXIOMUYVGZ-WFGJKAKNSA-N 0.000 description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 239000003814 drug Substances 0.000 description 4
- 239000006210 lotion Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 description 4
- XUJLWPFSUCHPQL-UHFFFAOYSA-N 11-methyldodecan-1-ol Chemical compound CC(C)CCCCCCCCCCO XUJLWPFSUCHPQL-UHFFFAOYSA-N 0.000 description 3
- 229940051841 polyoxyethylene ether Drugs 0.000 description 3
- 229920000056 polyoxyethylene ether Polymers 0.000 description 3
- SAHTYPIPYPIKPB-QRPNPIFTSA-N (2s)-2-amino-3-phenylpropanoic acid;sodium Chemical compound [Na].OC(=O)[C@@H](N)CC1=CC=CC=C1 SAHTYPIPYPIKPB-QRPNPIFTSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
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- 230000009286 beneficial effect Effects 0.000 description 2
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- 238000005516 engineering process Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000009775 high-speed stirring Methods 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
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- 125000000539 amino acid group Chemical group 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
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- 239000003599 detergent Substances 0.000 description 1
- 229940043237 diethanolamine Drugs 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
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- 229940031098 ethanolamine Drugs 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
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- 229910052751 metal Inorganic materials 0.000 description 1
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- 229910021645 metal ion Inorganic materials 0.000 description 1
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- 238000012986 modification Methods 0.000 description 1
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- 230000003287 optical effect Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
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- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 229960004418 trolamine Drugs 0.000 description 1
- 239000002699 waste material Substances 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
- 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
- C11D1/347—Other P-containing 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
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/044—Hydroxides or bases
-
- 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
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/08—Silicates
-
- 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
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/10—Carbonates ; Bicarbonates
-
- 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
- C11D3/2041—Dihydric alcohols
- C11D3/2044—Dihydric alcohols linear
-
- 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
- C11D3/2065—Polyhydric alcohols
-
- 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
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- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/2068—Ethers
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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
- 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
- C11D3/16—Organic compounds
- C11D3/26—Organic compounds containing nitrogen
- C11D3/30—Amines; Substituted amines ; Quaternized amines
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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
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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
- 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
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- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Emergency Medicine (AREA)
- Inorganic Chemistry (AREA)
- Detergent Compositions (AREA)
- Cleaning Or Drying Semiconductors (AREA)
Abstract
本发明提供了一种蓝宝石晶圆清洗剂及其制备方法,该清洗剂由无机碱、有机碱、螯合剂、有机助剂、阴离子表面活性及高纯水组成。本发明通过特定的阴离子表面活性剂与无机强碱混配,能有效解决现有技术中蓝宝石晶圆制程工艺中线切清洗、研磨后清洗、退火前清洗以及上蜡前清洗洗剂的四合一,有利于提高蓝宝石晶圆的清洗效果,有效减少蓝宝石上污染物的残留数量,在优化客户工艺制程的同时大大降低了客户成本且环保。
Description
技术领域
本发明涉及半导体制造领域,特别是涉及一种用于线切清洗、研磨后清洗、退火前清洗以及上蜡前清洗四段工艺洗剂四合一的蓝宝石晶圆清洗剂及其制备方法。
背景技术
蓝宝石是最常见的一种衬底材料,其组成为氧化铝。但由于蓝宝石在生产过程中往往有一些杂质附着在蓝宝石表面上,所以需要对蓝宝石进行清洗才能得到合格的产品。
在晶圆制造过程中,必须对晶圆基材进行线切、研磨、退火和上蜡等工艺处理。晶圆线切后,其表面残留有大量的氧化铝粉尘。为了得到均匀平整的表面,需以碳化硼为研磨材料对蓝宝石进行双面研磨加工。在研磨过程中,晶圆表面很容易吸附研磨下来的残留物以及研磨液中的金属、颗粒、有机物以及金属离子等污染物,所述污染物颗粒容易在后续工艺制造中造成缺陷(defect);退火清洗是在研磨清洗后的基础上再进行更深程度的精洗,主要是针对表层及损伤层中的粉末、磨料和人体接触所产生的油脂等有机物或无机物。上蜡清洗即在上蜡之前清洗晶圆表面残留的颗粒等污染物。各个工艺段对晶圆进行清洗,有利于清除晶圆表面的污染物颗粒以减少缺陷。其中,对退火清洗及研磨清洗两道清洗段的清洗要求相对较高。由于碳化硼稳定的化学性能,研磨后的清洗非常的困难,碳化硼微粉残留在蓝宝石表面,高温退火后再蓝宝石表面形成油亮斑,导致蓝宝石晶圆需返工甚至报废。目前采用的清洗方式基本是RCA清洗法,该清洗法涉及的工艺复杂,操作步骤多,需消耗大量的酸、碱、氧化剂等化学试剂,对环境污染较严重。
发明内容
本发明的目的针对现有清洗工艺技术的缺陷,提供一种用于晶圆制程工艺中对蓝宝石晶圆进行清洗的水基清洗剂及其制备方法,实现一款洗剂采用不同浓度,即可完成四个不同工艺的清洗功能,具有一次清洗即可达到清洗要求,操作方便,减少切换,优化管路,降低客户成本等特点。
为实现上述目的,本发明采用如下技术方案:
本发明的技术解决方案是:一种蓝宝石晶圆清洗剂,其原料按质量百分比计如下:
余量为高纯水。
所述的无机碱为氢氧化钾、氢氧化钠、碳酸钠、碳酸钾、偏硅酸钠中的一种或多种。所述的有机碱为乙醇胺、二乙醇胺、三乙醇胺、异丙醇胺、二异丙醇胺、三异丙醇胺中的一种或多种。所述的螯合剂为葡萄糖酸钠、乙二胺四乙酸、乙二胺四乙酸二钠、柠檬酸、山梨糖醇中的一种或多种。所述的有机助剂为乙二醇、乙二醇甲醚、乙二醇乙醚、乙二醇丁醚、二乙二醇单甲醚、二乙二醇单乙醚中的一种或多种。所述的高纯水为去离子水,其在25℃时的电导率不低于18MΩ·cm。
蓝宝石晶圆清洗剂的制备方法为:往高纯水中先添加无机碱,有机碱,有机助剂,然后加入阴离子表面活性剂,在500rpm的搅拌速度下使其形成均一体系,再一边搅拌一边加入螯合剂,最终得到均一稳定澄清透明的溶液。
所述的阴离子表面活性剂为磷酸双酯氨基酸阴离子表面活性剂,其结构为:
表面活性剂中的一种,n为1-13内的整数。
所述的磷酸双酯氨基酸阴离子表面活性剂的制备方法,包括如下步骤:
(1)中间体Ⅰ的合成
向装有温度计的100ml三口烧瓶中加入称量好的异构十三醇聚氧乙烯醚,在高速搅拌下,温度控制在30℃以下,分批次加入五氧化二磷,加完五氧化二磷后,逐步升温至70℃,反应8h,即得到中间体Ⅰ,结构如下所示:
(2)中间体Ⅱ的合成
向装有温度计、球形冷凝管,机械搅拌器和氯化氢吸收装置的四口瓶中加入甲苯、中间体Ⅰ和N,N-二甲基甲酰胺,搅拌混合均匀,加热至内温50℃,滴加二氯亚砜,滴加完毕,50℃恒温反应3h,再减压蒸馏即得到中间体Ⅱ,结构如下所示:
(3)磷酸双酯氨基酸阴离子表面活性剂的合成
称取一定量的苯丙氨酸与氢氧化钠固体用适量的丙酮与水混合溶剂溶解,将溶解后的苯丙氨酸钠溶液倒入装有机械搅拌器的四颈烧瓶中,充分搅拌的同时将中间体Ⅱ逐滴滴加进烧瓶,滴加时间0.5h,同时向烧瓶中滴加质量分数为32%的氢氧化钠水溶液,使反应体系保持碱性,控制反应在低温下进行。反应结束后,加入纯盐酸调节体系pH为1,药液经萃取、洗涤、减压蒸馏即可得到磷酸双酯氨基酸阴离子表面活性剂,结构如下所示。
本发明的有益效果为:
(1)本发明所述的磷酸双酯氨基酸表面活性剂,具有较好的耐碱性能。氨基酸基团具有优良的润湿性、抗菌性和可生物降解能力,减少清洗过程中细菌污染及环境污染;磷酸酯具有优良的抗静电性、润湿性、乳化性、平滑性等性能,可以快速均匀的渗透到晶圆表面,去除晶圆表面的污染物,防止污染物回粘,提高晶圆清洗的合格率。
(2)本发明公开的一种蓝宝石衬底清洗剂,克服了现有蓝宝石衬底制程工艺中需要用到多种化学试剂对蓝宝石衬底表面残留的Al2O3粉末、磨料等有机/无机污染物进行去除,且清洗废液难以处理。使用本发明的清洗剂,可以有效降低蓝宝石衬底清洗成本,实现不同工艺洗剂四合一的目的,即一种药液解决4个不同工艺的清洗要求。
附图说明
图1为实施例1的清洗剂组合物晶圆清洗前后效果图,a为晶圆清洗前,b为晶圆清洗后。
图2为对比例1的清洗剂组合物晶圆清洗前后效果图,a为晶圆清洗前,b为晶圆清洗后。
具体实施方式
一种蓝宝石晶圆清洗剂,其原料按质量百分比计如下:
余量为高纯水。
所述的磷酸双酯氨基酸阴离子表面活性剂结构为:
所述的磷酸双酯氨基酸阴离子表面活性剂的制备方法,包括如下步骤:
(1)中间体Ⅰ的合成
向装有温度计的100ml三口烧瓶中加入称量好的异构十三醇聚氧乙烯醚,在高速搅拌下,温度控制在30℃以下,分批次加入五氧化二磷,异构十三醇聚氧乙烯醚和五氧化二磷添加摩尔比为2.2:1,再逐步升温至70℃,反应8h,即得到中间体Ⅰ。
(2)中间体Ⅱ的合成
向装有温度计、球形冷凝管,机械搅拌器和氯化氢吸收装置的四口瓶中加入7.28mol甲苯、1mol中间体Ⅰ和0.05mol N,N-二甲基甲酰胺,搅拌混合均匀,加热至内温50℃,滴加1.1mol二氯亚砜,滴加完毕,50℃恒温反应3h,再减压蒸馏即得到中间体Ⅱ。
(3)磷酸双酯氨基酸阴离子表面活性剂的合成
称取一定量的苯丙氨酸与氢氧化钠固体用适量的丙酮与水混合溶剂溶解,丙酮和水混合体积比为3:2,将溶解后的苯丙氨酸钠溶液倒入装有机械搅拌器的四颈烧瓶中,充分搅拌的同时将中间体Ⅱ逐滴滴加进烧瓶,添加至中间体Ⅱ和苯丙氨酸摩尔比为1:1.4,滴加时间0.5h,同时向烧瓶中滴加质量分数为32%的氢氧化钠水溶液,使反应体系保持碱性,控制反应在低温下反应4h。反应结束后,加入纯盐酸调节体系pH为1,药液经萃取、洗涤、减压蒸馏即可得到磷酸双酯氨基酸阴离子表面活性剂。
所用的磷酸双酯氨基酸阴离子表面活性剂,当n=2时,表征数据如下:
1H NMR(300MHz,DMSO-d6),δ:0.96(t,6H,CH3),1.33(m,4H,CH2),1.29-1.46(m,20H,CH2),3.37(t,4H,CH2-O),3.54(m,16H,CH2-CH2-O),3.37(t,4H,CH2),1.29-1.46(m,12H,CH2),1.3(t,4H,CH2),2.0(d,2H,NH2),3.84(t,1H,CH),3.04(d,2H,CH2),7.08(m,1H,ArH),7.21(m,2H,ArH),7.12(m,2H,ArH)
13CNMR(125MHz,DMSO-d6),δ:14,23.1,32.5,30.0,26.6,31.0,70.2,70.9,30.7,27.3,22.0,22.7,63.0,177,39.7,127.9,140.2,128.4,125.7
HRMS计算值C51H81O9NPNa(M+H)+:521.29,实测值522.29.
为了使本发明所述的内容更加便于理解,下面结合具体实施方式对本发明所述的技术方案做进一步的说明,但是本发明不仅限于此。
按表1配方配制不同组成的清洗剂组合物。
表1不同清洗剂组合物中各组分及其含量
研磨后晶圆的清洗难度最大,所以本次将研磨后的蓝宝石晶圆分别浸泡在实施例1-6和对比例1-5制备的清洗剂组合物中,药液稀释20倍使用,在70±5℃、40KHZ条件下超声20min,取出后用去离子水清洗,吹干,利用光学显微镜和电子显微镜进行观察,以确认晶圆表面的清洗效果。
表2不同清洗剂组合物对研磨后晶圆的清洗效果
结合表1-2可以看出,在设定的温度和时间内,本发明的蓝宝石晶圆清洗剂可以将研磨后的晶圆清洗干净,得到均一稳定的溶液,且其易漂洗,无洗剂残留。
与实施例1相比,对比例1不含有机碱,提高了无机碱的比例,在操作温度下,其体系均一稳定,但晶圆表面有少量碳化硼粉末残留。
与实施例1相比,对比例2不含有机助剂,在操作温度下,可以将碳化硼粉末和氧化铝粉末清洗干净,但有洗剂残留。
与实施例1相比,对比例3不含螯合剂,在操作温度下,其体系均一稳定,可以将碳化硼粉末和洗剂清洗干净,有氧化铝粉末残留。
与实施例1相比,对比例4用LAS代替磷酸双酯氨基酸阴离子表面活性剂,在操作条件下,其体系出现分层现象,有少量碳化硼粉末和氧化铝粉末残留,但无洗剂残留。LAS不耐碱,清洁剂体系的碱性环境会对该表面活性剂造成破坏,导致该表面活性剂无法发挥作用,清洗渗透性差,影响清洗剂的清洗效果。
与实施例1相比,对比例5不含磷酸双酯氨基酸型表面活性剂,在操作温度下,体系均一稳定,但是碳化硼粉末和氧化铝粉末均有残留,清洗不干净。
由上述实施例1和对比例1-5可以说明,有机碱与无机碱具有清洗协同作用,有机助剂具有一定的助漂洗作用,螯合剂具有一定的分散作用,磷酸双酯氨基酸型表面活性剂提高了体系的表面活性,提高了对碳化硼粉末和氧化铝粉末的清洗效果,且具有较好的耐碱性能,各成分缺一不可。
图1为实施例1的清洗剂组合物晶圆清洗前后效果图,a为晶圆清洗前,b为晶圆清洗后,由图可以看出,无碳化硼粉末和氧化铝粉末残留,且无洗剂残留,清洗效果符合要求。
图2为对比例1的清洗剂组合物晶圆清洗前后效果图,a为晶圆清洗前,b为晶圆清洗后,由图可以看出,仍有少量的碳化硼粉末残留,但无洗剂残留。
上述实施例对本发明进行了详细描述,但其只是作为范例,并非因此限制本发明的专利范围。凡是利用本发明说明书对本发明进行的等同任何修改和替代也都在本发明的范畴之中,均包括在本发明的专利保护范围内。
Claims (7)
1.一种蓝宝石晶圆清洗剂,其特征在于,其原料按质量百分比计包括如下:
无机碱 5-30%
有机碱 1-10%
螯合剂 2-10%
有机助剂 1-5%
阴离子表面活性剂 0.1-5%
余量为高纯水;
所述的有机助剂为乙二醇、乙二醇甲醚、乙二醇乙醚、乙二醇丁醚、二乙二醇单甲醚、二乙二醇单乙醚中的一种或多种;
所述的阴离子表面活性剂为磷酸双酯氨基酸表面活性剂,其结构为:
表面活性剂中的一种,n为1-13内的整数。
2.根据权利要求1所述的蓝宝石晶圆清洗剂,其特征在于,所述的无机碱为氢氧化钾、氢氧化钠、碳酸钠、碳酸钾、偏硅酸钠中的一种或多种。
3.根据权利要求1所述的蓝宝石晶圆清洗剂,其特征在于,所述的有机碱为乙醇胺、异丙醇胺中的一种或多种。
4.根据权利要求1所述的蓝宝石晶圆清洗剂,其特征在于,所述的有机碱为二乙醇胺、三乙醇胺、二异丙醇胺、三异丙醇胺中的一种或多种。
5.根据权利要求1所述的蓝宝石晶圆清洗剂,其特征在于,所述的螯合剂为葡萄糖酸钠、乙二胺四乙酸、乙二胺四乙酸二钠、柠檬酸、山梨糖醇中的一种或多种。
6.根据权利要求1所述的蓝宝石晶圆清洗剂,其特征在于,所述的高纯水为去离子水,其在25℃时的电导率不低于18MΩ·cm。
7.根据权利要求1所述的蓝宝石晶圆清洗剂,其特征在于,所述的蓝宝石晶圆清洗剂的制备方法为:往高纯水中先添加无机碱,有机碱、有机助剂,然后加入阴离子表面活性剂,在500rpm的搅拌速度下使其形成均一体系,再一边搅拌一边加入螯合剂,最终得到均一稳定澄清透明的溶液。
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