CN109075052B - Composition, composition container, and method for producing composition - Google Patents
Composition, composition container, and method for producing composition Download PDFInfo
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- CN109075052B CN109075052B CN201780025662.6A CN201780025662A CN109075052B CN 109075052 B CN109075052 B CN 109075052B CN 201780025662 A CN201780025662 A CN 201780025662A CN 109075052 B CN109075052 B CN 109075052B
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- hydrogen peroxide
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- metal
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- 239000000203 mixture Substances 0.000 title claims abstract description 305
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 55
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 287
- 239000004065 semiconductor Substances 0.000 claims abstract description 82
- 239000000758 substrate Substances 0.000 claims abstract description 58
- 239000002253 acid Substances 0.000 claims abstract description 57
- 238000003860 storage Methods 0.000 claims abstract description 41
- 229910052751 metal Inorganic materials 0.000 claims description 145
- 239000002184 metal Substances 0.000 claims description 145
- 239000007788 liquid Substances 0.000 claims description 82
- -1 anthraquinone compounds Chemical class 0.000 claims description 79
- 239000002245 particle Substances 0.000 claims description 79
- 238000000746 purification Methods 0.000 claims description 72
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 claims description 48
- 238000011282 treatment Methods 0.000 claims description 46
- 239000000463 material Substances 0.000 claims description 38
- 239000002994 raw material Substances 0.000 claims description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- 229910052759 nickel Inorganic materials 0.000 claims description 30
- 229910052782 aluminium Inorganic materials 0.000 claims description 27
- 239000002904 solvent Substances 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 15
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 15
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 14
- 230000001590 oxidative effect Effects 0.000 claims description 12
- 230000015572 biosynthetic process Effects 0.000 claims description 11
- 239000003054 catalyst Substances 0.000 claims description 11
- 238000003786 synthesis reaction Methods 0.000 claims description 10
- 229920001577 copolymer Polymers 0.000 claims description 9
- 229910052755 nonmetal Inorganic materials 0.000 claims description 9
- 229920001903 high density polyethylene Polymers 0.000 claims description 8
- 239000004700 high-density polyethylene Substances 0.000 claims description 8
- 230000002194 synthesizing effect Effects 0.000 claims description 8
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 6
- 238000000605 extraction Methods 0.000 claims description 5
- HSKPJQYAHCKJQC-UHFFFAOYSA-N 1-ethylanthracene-9,10-dione Chemical group O=C1C2=CC=CC=C2C(=O)C2=C1C=CC=C2CC HSKPJQYAHCKJQC-UHFFFAOYSA-N 0.000 claims description 4
- 150000003013 phosphoric acid derivatives Chemical class 0.000 claims description 3
- RKMPHYRYSONWOL-UHFFFAOYSA-N 1-ethyl-1,2,3,4-tetrahydroanthracene-9,10-dione Chemical group O=C1C2=CC=CC=C2C(=O)C2=C1C(CC)CCC2 RKMPHYRYSONWOL-UHFFFAOYSA-N 0.000 claims description 2
- LZNGSHFBWBKBFH-UHFFFAOYSA-N 1-pentyl-1,2,3,4-tetrahydroanthracene-9,10-dione Chemical compound O=C1C2=CC=CC=C2C(=O)C2=C1C(CCCCC)CCC2 LZNGSHFBWBKBFH-UHFFFAOYSA-N 0.000 claims description 2
- INPHIYULSHLAHR-UHFFFAOYSA-N 1-pentylanthracene-9,10-dione Chemical compound O=C1C2=CC=CC=C2C(=O)C2=C1C=CC=C2CCCCC INPHIYULSHLAHR-UHFFFAOYSA-N 0.000 claims description 2
- 230000007547 defect Effects 0.000 abstract description 65
- 238000000034 method Methods 0.000 description 96
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 83
- 125000004429 atom Chemical group 0.000 description 78
- 239000012535 impurity Substances 0.000 description 55
- 238000004140 cleaning Methods 0.000 description 49
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 46
- 238000001914 filtration Methods 0.000 description 45
- 229910021645 metal ion Inorganic materials 0.000 description 40
- 239000011148 porous material Substances 0.000 description 31
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 27
- 238000005259 measurement Methods 0.000 description 26
- 230000000694 effects Effects 0.000 description 25
- 150000002500 ions Chemical class 0.000 description 25
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- 230000008569 process Effects 0.000 description 21
- 239000002923 metal particle Substances 0.000 description 20
- 238000001179 sorption measurement Methods 0.000 description 19
- 239000004677 Nylon Substances 0.000 description 17
- 239000004743 Polypropylene Substances 0.000 description 17
- 238000004821 distillation Methods 0.000 description 17
- 239000007769 metal material Substances 0.000 description 17
- 229920001778 nylon Polymers 0.000 description 17
- 229920001155 polypropylene Polymers 0.000 description 17
- 150000004056 anthraquinones Chemical class 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 16
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 15
- 239000000126 substance Substances 0.000 description 15
- 238000011156 evaluation Methods 0.000 description 14
- 150000002739 metals Chemical class 0.000 description 14
- 238000002360 preparation method Methods 0.000 description 14
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 13
- 238000004458 analytical method Methods 0.000 description 13
- 239000011651 chromium Substances 0.000 description 13
- QOSATHPSBFQAML-UHFFFAOYSA-N hydrogen peroxide;hydrate Chemical compound O.OO QOSATHPSBFQAML-UHFFFAOYSA-N 0.000 description 13
- 239000000243 solution Substances 0.000 description 13
- 239000004698 Polyethylene Substances 0.000 description 11
- 239000012530 fluid Substances 0.000 description 11
- 239000012528 membrane Substances 0.000 description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- 150000007513 acids Chemical class 0.000 description 10
- 238000000354 decomposition reaction Methods 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 239000004813 Perfluoroalkoxy alkane Substances 0.000 description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 9
- 229920011301 perfluoro alkoxyl alkane Polymers 0.000 description 9
- 229910052710 silicon Inorganic materials 0.000 description 9
- 239000010703 silicon Substances 0.000 description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 8
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 8
- 239000004642 Polyimide Substances 0.000 description 8
- 239000003729 cation exchange resin Substances 0.000 description 8
- 239000011737 fluorine Substances 0.000 description 8
- 229910052731 fluorine Inorganic materials 0.000 description 8
- 238000002156 mixing Methods 0.000 description 8
- 229920001721 polyimide Polymers 0.000 description 8
- 239000004962 Polyamide-imide Substances 0.000 description 7
- 239000011362 coarse particle Substances 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 7
- 229920002312 polyamide-imide Polymers 0.000 description 7
- 229920000573 polyethylene Polymers 0.000 description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 6
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 230000002378 acidificating effect Effects 0.000 description 6
- 125000000217 alkyl group Chemical group 0.000 description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 description 6
- 235000010354 butylated hydroxytoluene Nutrition 0.000 description 6
- 229910052804 chromium Inorganic materials 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 238000012544 monitoring process Methods 0.000 description 6
- 229910000623 nickel–chromium alloy Inorganic materials 0.000 description 6
- 239000003960 organic solvent Substances 0.000 description 6
- 238000012545 processing Methods 0.000 description 6
- SJEBAWHUJDUKQK-UHFFFAOYSA-N 2-ethylanthraquinone Chemical compound C1=CC=C2C(=O)C3=CC(CC)=CC=C3C(=O)C2=C1 SJEBAWHUJDUKQK-UHFFFAOYSA-N 0.000 description 5
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 5
- QPCDCPDFJACHGM-UHFFFAOYSA-N N,N-bis{2-[bis(carboxymethyl)amino]ethyl}glycine Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(=O)O)CCN(CC(O)=O)CC(O)=O QPCDCPDFJACHGM-UHFFFAOYSA-N 0.000 description 5
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 5
- 239000003463 adsorbent Substances 0.000 description 5
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 5
- 238000005530 etching Methods 0.000 description 5
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- 229920003303 ion-exchange polymer Polymers 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- FWFGVMYFCODZRD-UHFFFAOYSA-N oxidanium;hydrogen sulfate Chemical compound O.OS(O)(=O)=O FWFGVMYFCODZRD-UHFFFAOYSA-N 0.000 description 5
- 229960003330 pentetic acid Drugs 0.000 description 5
- 229910052814 silicon oxide Inorganic materials 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- AFINAILKDBCXMX-PBHICJAKSA-N (2s,3r)-2-amino-3-hydroxy-n-(4-octylphenyl)butanamide Chemical compound CCCCCCCCC1=CC=C(NC(=O)[C@@H](N)[C@@H](C)O)C=C1 AFINAILKDBCXMX-PBHICJAKSA-N 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000002738 chelating agent Substances 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- DKAGJZJALZXOOV-UHFFFAOYSA-N hydrate;hydrochloride Chemical compound O.Cl DKAGJZJALZXOOV-UHFFFAOYSA-N 0.000 description 4
- 238000004949 mass spectrometry Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 125000001424 substituent group Chemical group 0.000 description 4
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 description 4
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 4
- 229910021642 ultra pure water Inorganic materials 0.000 description 4
- 239000012498 ultrapure water Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
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- 239000003957 anion exchange resin Substances 0.000 description 3
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- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 3
- 238000001471 micro-filtration Methods 0.000 description 3
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- 229920002223 polystyrene Polymers 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 3
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- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 3
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- AACILMLPSLEQMF-UHFFFAOYSA-N 2,2-dichloroethenyl 2-ethylsulfinylethyl methyl phosphate Chemical compound CCS(=O)CCOP(=O)(OC)OC=C(Cl)Cl AACILMLPSLEQMF-UHFFFAOYSA-N 0.000 description 2
- URDCARMUOSMFFI-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(2-hydroxyethyl)amino]acetic acid Chemical compound OCCN(CC(O)=O)CCN(CC(O)=O)CC(O)=O URDCARMUOSMFFI-UHFFFAOYSA-N 0.000 description 2
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- XNCSCQSQSGDGES-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]propyl-(carboxymethyl)amino]acetic acid Chemical compound OC(=O)CN(CC(O)=O)C(C)CN(CC(O)=O)CC(O)=O XNCSCQSQSGDGES-UHFFFAOYSA-N 0.000 description 1
- SJBOEHIKNDEHHO-UHFFFAOYSA-N 2-[2-aminoethyl(carboxymethyl)amino]acetic acid Chemical compound NCCN(CC(O)=O)CC(O)=O SJBOEHIKNDEHHO-UHFFFAOYSA-N 0.000 description 1
- ZIMXAFGAUMQPMG-UHFFFAOYSA-N 2-[4-[bis(carboxymethyl)amino]butyl-(carboxymethyl)amino]acetic acid Chemical compound OC(=O)CN(CC(O)=O)CCCCN(CC(O)=O)CC(O)=O ZIMXAFGAUMQPMG-UHFFFAOYSA-N 0.000 description 1
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- 125000006290 2-hydroxybenzyl group Chemical group [H]OC1=C(C([H])=C([H])C([H])=C1[H])C([H])([H])* 0.000 description 1
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- HNNQYHFROJDYHQ-UHFFFAOYSA-N 3-(4-ethylcyclohexyl)propanoic acid 3-(3-ethylcyclopentyl)propanoic acid Chemical compound CCC1CCC(CCC(O)=O)C1.CCC1CCC(CCC(O)=O)CC1 HNNQYHFROJDYHQ-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention provides a composition which can be used for manufacturing a semiconductor device and contains hydrogen peroxide, has excellent storage stability and has little influence on defects of a semiconductor substrate. Another object of the present invention is to provide a method for producing a composition containing the hydrogen peroxide and a composition container storing the composition. The composition of the present invention contains hydrogen peroxide, an acid and an Fe component, wherein the content of the Fe component is 10 ‑5～102 in terms of mass ratio to the content of the acid.
Description
Technical Field
The present invention relates to a hydrogen peroxide-containing composition, a method for producing the same, and a composition container.
Background
The manufacturing process of the semiconductor device includes various processes such as a cleaning process, a photolithography process, an etching process, an ion implantation process, and a delamination process of a semiconductor silicon wafer. Here, after each step is completed or before the next step, a step of treating unnecessary organic and inorganic substances with a treatment liquid is generally included.
As the treatment liquid, a treatment liquid containing hydrogen peroxide may be used.
Hydrogen peroxide is generally synthesized by the so-called anthraquinone method using an anthraquinone compound as a raw material (for example, refer to patent document 1).
It is required to use a high-purity processing liquid in a process for manufacturing a semiconductor device. The term "high purity" as used herein means that the concentration of each metal component or particle (particle) contained as an impurity is low.
When an impurity (for example, a metal ion or a metal particle) of a metal component is mixed into the processing liquid, a phenomenon called migration in which a metal diffuses into the target material is caused during the processing. Migration impedes transmission of an electrical signal, and causes defects such as short circuits. In addition, there are cases where the metal impurities are coarse particles of the metal itself as nuclei and remain as residues on the semiconductor substrate after the treatment. The residue may cause defects in addition to deterioration of the photolithography performance, and adversely affect formation of a fine resist pattern or a semiconductor element.
Technical literature of the prior art
Patent literature
Patent document 1: japanese patent laid-open publication No. 2014-108903
Disclosure of Invention
Technical problem to be solved by the invention
The present inventors have studied the applicability of the anthraquinone process to manufacture semiconductor devices using hydrogen peroxide water produced by the anthraquinone process as described in patent document 1, and have found that there is room for improvement in the storage stability of hydrogen peroxide water. As a cause of this low storage stability, it is considered that hydrogen peroxide is decomposed as a result of a catalytic reaction in an acidic region of an Fe component mixed in from a solvent or from a raw material, etc., thereby carrying out hydroxyl radical (so-called fenton reaction) on hydrogen peroxide.
On the other hand, it is known that the Fenton reaction is suppressed when a metal adsorbent such as an acid is used and the Fe component is used as a metal adsorbent (for example, a chelate complex in the case where the acid has a multi-tooth (polydentate) structure). The present inventors have found that when the Fe component is too small relative to the acid, the hydrogen peroxide water may not satisfy the high purity required for use in the manufacture of semiconductor devices. That is, it has been recognized that when the semiconductor substrate is cleaned with the hydrogen peroxide water, the number of particles (also referred to as "defect number") adhering to the semiconductor substrate increases, and the method cannot be applied to the semiconductor device manufacturing process. In particular, the problem is more remarkable with the high integration and miniaturization (for example, 30nm node or less) of the semiconductor device. In recent years, the production of semiconductor devices having a node of 10nm or less has also been studied, and this problem has become more remarkable.
The invention provides a composition which can be used in the manufacture of semiconductor devices and contains hydrogen peroxide, and has excellent storage stability and little influence on the defects of semiconductor substrates.
The present invention also provides a method for producing a composition containing the hydrogen peroxide and a composition container storing the composition.
Means for solving the technical problems
As a result of intensive studies to achieve the above object, the present inventors have found that the above object can be achieved by a composition containing hydrogen peroxide in which the Fe component and an acid as a metal adsorbent are controlled at a specific ratio, and have completed the present invention.
That is, it has been found that the above object can be achieved by the following structure.
(1) A composition comprising hydrogen peroxide, an acid and an Fe component,
The content of the Fe component was 10 -5～102 in terms of mass ratio to the content of the acid.
(2) The composition according to (1), which further comprises an anthraquinone compound.
(3) The composition according to (1) or (2), wherein the content of the anthraquinone compound is 0.01 ppb by mass to 1000 ppb by mass relative to the total mass of the composition.
(4) The composition according to any one of (1) to (3), wherein the content of the acid is 0.01 ppb by mass to 1000 ppb by mass relative to the total mass of the composition.
(5) The composition according to any one of (1) to (4), wherein the total content of the Fe component is 0.1 ppt to 1 ppb by mass relative to the total mass of the composition.
(6) The composition according to any one of (1) to (5), wherein the content of Fe particles contained in the Fe component is 0.01 to 0.1 ppb by mass of ppt based on the total mass of the composition.
(7) The composition according to any one of (1) to (6), which further contains at least 1 or more metal components containing a specific atom selected from the group consisting of Ni, pt, pd, cr, ti and Al,
The content of the metal component is 0.01 ppt to 10 ppb by mass per the total mass of the composition.
(8) The composition according to any one of (1) to (6), which further contains at least 1 or more metal components containing a specific atom selected from the group consisting of Ni, pt, pd and Al,
The content of the metal component is 0.01 to 1 ppt by mass based on the total mass of the composition.
(9) The composition according to any one of (2) to (8), wherein the anthraquinone compound is at least 1 or more selected from the group consisting of alkylanthraquinone and alkyltetrahydroanthraquinone.
(10) The composition according to (9), wherein the alkylanthraquinone is ethylanthraquinone or pentylanthraquinone and the alkyltetrahydroanthraquinone is ethylanthraquinone or pentylhydroquinone.
(11) The composition according to any one of (1) to (10), wherein the acid is selected from 1 kind of phosphoric acid and a phosphoric acid derivative.
(12) The composition according to any one of (1) to (11), which is used as a treatment liquid for a semiconductor substrate.
(13) A composition container comprising a storage container and the composition according to any one of (1) to (12) contained in the storage container,
The region of the storage container in contact with the composition is formed of a material containing a non-metal as a main component.
(14) The composition container according to (13), wherein the material containing a nonmetal as a main component is 1 selected from the group consisting of high-density polyethylene, tetrafluoroethylene perfluoroalkyl vinyl ether copolymer and polytetrafluoroethylene.
(15) The composition container according to (13) or (14), wherein the contact angle with water of the material containing a nonmetal as a main component is 60 ° to 120 °.
(16) A method for producing the composition according to any one of (1) to (12), comprising:
A raw material purification step of purifying 1 or more of the raw material components selected from the group consisting of a solvent and an anthraquinone compound;
A hydrogen peroxide synthesis step of synthesizing an anthrahydroquinone compound by reducing the anthraquinone compound in the presence of a catalyst, and further oxidizing the anthrahydroquinone compound to synthesize hydrogen peroxide;
a hydrogen peroxide separation step of extracting the hydrogen peroxide obtained by the extraction step to remove the hydrogen peroxide from the reaction system; and
And a hydrogen peroxide composition purification step of further purifying a hydrogen peroxide composition containing hydrogen peroxide separated from the reaction system.
Effects of the invention
According to the present invention, a composition which can be used for manufacturing a semiconductor device and contains hydrogen peroxide and has excellent storage stability and suppressed influence on defects of a semiconductor substrate can be provided.
Further, according to the present invention, a method for producing a composition containing the hydrogen peroxide and a composition container storing the composition can be provided.
Further, according to the present invention, it is possible to provide a processing liquid and a container for containing a composition thereof, which can suppress occurrence of defects and have excellent storage stability, particularly in the formation of a semiconductor device having an ultrafine pattern (for example, a node of 10nm or less) in recent years.
Drawings
FIG. 1 is a schematic view showing one embodiment of a purification apparatus that can be used in the method for producing a composition of the present invention.
FIG. 2 is a schematic view showing another embodiment of a purification apparatus that can be used in the method for producing a composition of the present invention.
Detailed Description
The present invention will be described in detail below.
The following description of the constituent elements is sometimes made based on the representative embodiments of the present invention, but the present invention is not limited to such embodiments.
In the present specification, the numerical range indicated by "to" means a range in which numerical values before and after "to" are included as a lower limit value and an upper limit value.
In the labeling of the groups (atomic groups) in the present specification, the unsubstituted and substituted labels are not described, and include both groups (atomic groups) having no substituent and groups (atomic groups) having a substituent within a range that does not impair the effects of the present invention. For example, "alkyl" means to include not only an alkyl group having no substituent (unsubstituted alkyl group) but also an alkyl group having a substituent (substituted alkyl group). This is synonymous for each compound.
In the present specification, the term "preparation" refers to a case where a specific material is synthesized or blended, and a case where a predetermined article is placed by purchase or the like.
In the present specification, "ppm" means "parts-per-million (10 -6)", "ppb" means "parts-per-trillion (10 -9)", and "ppt" means "parts-per-trillion (10 -12)".
In the present specification, the "semiconductor substrate" is not particularly limited as long as it can be used for manufacturing a semiconductor device, and examples thereof include a silicon substrate (Si substrate), a silicon oxide film substrate (SiO substrate), and a silicon nitride substrate (SiN substrate). The substrate is not limited to a wafer, and may be a substrate structure including a circuit structure formed on a wafer.
[ Composition ]
The composition of the present invention contains hydrogen peroxide, an acid and an Fe component, wherein the content of the Fe component is 10 -5～102 in terms of mass ratio to the content of the acid.
The composition of the present invention has the above-described structure, and therefore, the composition is excellent in storage stability and is less likely to affect defects in a semiconductor substrate in a semiconductor device manufacturing process. That is, the composition of the present invention has a small decomposition rate of hydrogen peroxide after storage over time. Further, for example, when the composition of the present invention is applied to a semiconductor device manufacturing process as a treatment liquid, the adhesion of particles to a semiconductor substrate to be treated is small (in other words, the number of defects is small), and therefore, a decrease in the yield of semiconductor substrates can be suppressed.
The details thereof are not clear, but can be presumed as follows.
The composition of the present invention is preferably a composition which is obtained by removing and purifying trace amounts of organic contaminants, metal contaminants, grease and other impurities contained in a liquid by filtration, ion exchange or the like in a manner suitable for use in a semiconductor device manufacturing process. The composition of the present invention is characterized in that the removal and purification are excessively performed during the preparation, but the impurities are not completely removed, and at least a trace amount of Fe component remains. In addition, it is considered that the Fe component exists to some extent in the raw material component containing the solvent or anthraquinone, and is mixed into the composition by these solvents or raw materials. In the present specification, the Fe component includes Fe atoms in an ionic state and Fe atoms in a nonionic state, and includes, for example, fe ions and forms of metal particles (Fe particles) of Fe. That is, the Fe component is a component (Fe ion, fe particle) derived from Fe atoms representing all of the components contained in the composition, and the content of the Fe component is a component representing the total metal amount (total Fe atomic weight).
In the preparation of the composition of the present invention, the Fe component may be purified to be smaller than the lower limit of the above-mentioned predetermined numerical range, and then the Fe component may be added so as to be in the predetermined numerical range.
The above-mentioned removal and purification of impurities may be carried out by using a solvent or a raw material component used in the synthesis of hydrogen peroxide, or by using a composition containing hydrogen peroxide after the synthesis of hydrogen peroxide.
As described above, in the composition of the present invention, the acid is considered to function as a metal adsorbent. The Fe component decomposes hydrogen peroxide by the Fenton reaction (the higher the pH, the faster the decomposition rate), particularly in the acidic region, but the Fenton reaction can be suppressed by complexing the Fe component with an acid as a metal adsorbent. If the content of the Fe component exceeds 10 2 in terms of the mass ratio relative to the content of the acid, it is difficult to suppress the fenton reaction, and the storage stability of the composition is insufficient. On the other hand, if the content of the Fe component to the content of the acid is less than 10 -5 in terms of mass ratio, colloidal particles are formed in the liquid, which causes an increase in the number of defects adhering to the semiconductor substrate. In the composition, when the content of the Fe component is 10 -5～102 in terms of mass ratio relative to the content of the acid, the composition is excellent in storage stability and less liable to affect defects of the semiconductor substrate when applied to the semiconductor device manufacturing process.
In the composition of the present invention, the total content of the Fe component is preferably 0.1 ppt to 1 ppb by mass relative to the total mass of the composition. The effect of the present invention is further improved by setting the total content of the Fe component contained in the composition to the above range. The reason for this is not clear, but it is assumed that when the total content of the Fe component is in the low concentration range, most of the complex ions are usually dispersed as hydroxide colloids obtained by condensing Fe hydrates unless complex ions having solubility are formed. If the total content of the Fe component is 0.1 mass ppt or more, the effect as a positive colloid is reduced, and it is difficult to adsorb an oxide film having a negative Zeta potential slightly higher than the silicon surface, so that it is difficult to develop a defect influence on the semiconductor substrate.
Further, when the total content of the Fe component was 0.1 mass ppt or more relative to the total mass of the composition, it was also confirmed that the oxidizing power of the composition was excellent. The reason for this is not clear, but it is considered that when the total content of the Fe component is 0.1 mass ppt or more relative to the total mass of the composition, the amount of the hydroxyl radical as a reactive species is present in an appropriate amount in the system. In other words, when the total content of the Fe component is less than 0.1 mass ppt relative to the total mass of the composition, the amount of hydroxyl radicals as reactive species is too small in the system, and there is a tendency that the oxidizing power is reduced.
On the other hand, if the total content of the Fe component is 1 ppb by mass or less relative to the total mass of the composition, the Fe component does not become particles, and defects of the semiconductor substrate do not increase when the composition is applied to a manufacturing process of a semiconductor device.
The content of the acid in the composition of the present invention is preferably 0.01 ppb by mass to 1000 ppb by mass relative to the total mass of the composition. When the content of the acid is less than 0.01 ppb by mass relative to the total mass of the composition, the content of the Fe component in the composition may be relatively excessive. When the content of the acid is 0.01 ppb or more by mass relative to the total mass of the composition, the content of the Fe component is adjusted to an appropriate range, so that the storage stability is more excellent or the Fe component does not become nuclei in the liquid to form particles, and defects in the semiconductor substrate can be suppressed when used in the manufacturing process of the semiconductor device.
On the other hand, when the content of the acid exceeds 1000 ppb by mass relative to the total mass of the composition, the content of the Fe component in the composition may be relatively too small. If the content of the acid is 1000 ppb by mass or less relative to the total mass of the composition, colloidal particles are hardly formed in the liquid, and defects in the semiconductor substrate can be suppressed when the composition is applied to a manufacturing process of a semiconductor device.
Hydrogen peroxide is generally synthesized by the anthraquinone method. In many cases, although a trace amount of impurities derived from the raw material (for example, metal components derived from anthraquinone compounds or catalysts which can be used in the step of synthesizing anthrahydroquinones by reducing anthraquinones and containing atoms selected from the group consisting of Ni, pt, pd and Al) remain in the composition containing hydrogen peroxide synthesized by the anthraquinone method. These impurities are generally preferably removed, but are not completely removed in the present invention, but are preferably at least to the extent that a trace amount remains in the composition.
In the composition of the present invention, the content of the anthraquinone compound is preferably 0.01 to 1000 ppb by mass relative to the total mass of the composition. As long as the content of the anthraquinone compound is 0.01 mass ppb or more relative to the total mass of the composition, there is an effect of improving defective properties. On the other hand, if the content of the anthraquinone compound is 1000 ppb by mass or less relative to the total mass of the composition, the influence of defects on the semiconductor substrate is small when the composition is applied to a process for producing a semiconductor device.
The composition of the present invention may contain a metal component containing an atom (hereinafter, also referred to as "specific atom") selected from the group consisting of Ni, pt, pd, cr, ti and Al.
The content of the metal component is preferably 0.01 ppt to 10 ppb by mass per specific atom relative to the total mass of the composition.
The metal component contains specific atoms in an ionic state and specific atoms in a nonionic state, and includes, for example, specific metal ions and specific metal particles (nonionic metals). That is, when the composition of the present invention contains, for example, only a Pt component, all the components (Pt ions, pt particles) derived from Pt atoms contained in the composition are contained in the Pt component, and the content of the Pt component is a total metal amount (total Pt atomic weight) representing Pt (the total metal amount is as above). The expression "the content of the metal component is 0.01 ppt to 10 ppb by mass per specific atom relative to the total mass of the composition" means that when the composition of the present invention contains 2 types of Pt component and Ni component, for example, the content of the metal component is 0.01 ppt to 10 ppb by mass per specific atom (in other words, any one of the content of Pt component and Ni component) relative to the total mass of the composition.
The composition is more excellent in oxidizing power as long as the content of the metal component containing the specific atoms selected from the group consisting of Ni, pt, pd, cr, ti and Al is 0.01 ppb by mass or more per each specific atom relative to the total mass of the composition. On the other hand, if the content of the metal component containing the specific atoms selected from the group consisting of Ni, pt, pd, cr, ti and Al is 1000 ppb by mass or less (preferably 10 ppb by mass or less) per the total mass of the composition, the defect of the semiconductor substrate is less affected when the composition is applied to the manufacturing process of the semiconductor device.
As described above, the composition containing hydrogen peroxide synthesized by the anthraquinone method can contain a large number of metal components derived from a catalyst that can be used in the step of synthesizing anthrahydroquinones by reducing anthraquinones, and containing Ni atoms, pt atoms, pd atoms, and/or Al atoms. In addition, there are many cases where other metal components derived from the raw material components other than the above are mixed. Among these metal components, the above-mentioned effects were confirmed to be obtained by setting the content of the metal component containing an atom selected from the group consisting of Ni, pt, pd, cr, ti and Al, in particular, to the above-mentioned range.
The content of the metal component containing atoms (hereinafter, also referred to as "specific atoms") selected from the group consisting of Ni, pt, pd and Al in the composition of the present invention is preferably 0.01 ppt to 1 ppb by mass relative to the total mass of the composition. The metal component includes specific atoms in an ionic state and specific atoms in a nonionic state, and includes, for example, specific metal ions and specific metal particles (nonionic metals). That is, when the composition of the present invention contains, for example, only a Pt component, all the components (Pt ions, pt particles) derived from Pt atoms contained in the composition are contained in the Pt component, and the content of the Pt component is a total metal amount (total Pt atomic weight) representing Pt (the total metal amount is as above). The composition is more excellent in oxidizing power as long as the content of the metal component containing a specific atom selected from the group consisting of Ni, pt, pd and Al is 0.01 mass ppb or more relative to the total mass of the composition. On the other hand, if the content of the metal component containing a specific atom selected from the group consisting of Ni, pt, pd and Al is 1000 ppb by mass or less (preferably 1 ppb by mass or less) relative to the total mass of the composition, the defect of the semiconductor substrate is less affected when the composition is applied to the manufacturing process of the semiconductor device.
As described above, the composition containing hydrogen peroxide synthesized by the anthraquinone method can contain a large number of metal components derived from a catalyst that can be used in the step of synthesizing anthrahydroquinones by reducing anthraquinones, and containing Ni atoms, pt atoms, pd atoms, and/or Al atoms. The above effect was confirmed by setting the content of the metal component containing atoms selected from the group consisting of Ni, pt, pd and Al to the above range.
The components of the composition of the present invention will be described in more detail below.
< Hydrogen peroxide >, a method for producing the same
The content of hydrogen peroxide in the composition of the present invention is preferably 0.001 to 70% by mass, more preferably 10 to 60% by mass, and even more preferably 15 to 60% by mass.
< Acid >
The compositions of the present invention contain an acid. The "acid" referred to herein does not contain hydrogen peroxide.
The acid is not particularly limited as long as it can adsorb metal ions (examples of adsorption form include ionic bonding and coordinate bonding) existing in the liquid, but is preferably a water-soluble acidic compound.
The water-soluble acidic compound is not particularly limited as long as it has a dissociable functional group that is acidic when dissolved in water, and may be an organic compound or an inorganic compound. The term "water-soluble" as used herein means that 5g or more of the water is dissolved in 100g of water at 25 ℃.
Examples of the water-soluble acidic compound and its salt include acidic compounds such as inorganic acids (e.g., hydrochloric acid, sulfuric acid, phosphoric acid, and nitric acid), carboxylic acid derivatives, sulfonic acid derivatives, and phosphoric acid derivatives. These acidic functional groups may be salt-forming compounds.
Among them, the water-soluble acidic compound is preferably a phosphoric acid derivative or phosphoric acid from the viewpoint of being able to chelate impurities effectively and remove the impurities.
Examples of the phosphoric acid derivative include pyrophosphoric acid and polyphosphoric acid.
Examples of the cations that form the water-soluble acidic compound and the salt include alkali metal, alkaline earth metal, and a quaternary alkyl compound (for example, tetramethylammonium hydroxide (TMAH), tetraethylammonium hydroxide (TEAH), methylpropylammonium hydroxide (TPAH), and tetrabutylammonium hydroxide (TBAH)). The cations forming the above salts may be 1 kind or 2 or more kinds.
As the water-soluble acidic compound, a so-called chelating agent may be used in addition to the above-mentioned water-soluble acidic compound. The chelating agent is not particularly limited, but is preferably a polyamine-based polycarboxylic acid.
The polyamino polycarboxylic acid is a compound having a plurality of amine groups and a plurality of carboxylic acid groups, and examples thereof include mono-or polyalkylenepolyamine polycarboxylic acid, polyaminoalkane polycarboxylic acid, polyaminoalkanol polycarboxylic acid and hydroxyalkyl ether polyamine polycarboxylic acid.
Examples of suitable polyamine polycarboxylic acid chelating agents include butanediamine tetraacetic acid, diethylenetriamine pentaacetic acid (DTPA), ethylenediamine tetraacetic acid, triethylenetetramine hexaacetic acid, 1, 3-diamino-2-hydroxypropane-N, N '-tetraacetic acid, propylenediamine tetraacetic acid, ethylenediamine tetraacetic acid (EDTA), trans-1, 2-diaminocyclohexane tetraacetic acid, ethylenediamine diacetic acid, ethylenediamine dipropionic acid, 1, 6-hexamethylenediamine-N, N' -tetraacetic acid, N-bis (2-hydroxybenzyl) ethylenediamine-N, N-diacetic acid, diaminopropane tetraacetic acid, 1,4,7, 10-tetraazacyclododecane-tetraacetic acid, diaminopropanol tetraacetic acid and (hydroxyethyl) ethylenediamine triacetic acid. Among them, diethylenetriamine pentaacetic acid (DTPA), ethylenediamine tetraacetic acid (EDTA) or trans-1, 2-diaminocyclohexane tetraacetic acid is preferable.
In the composition of the present invention, 2 or more acids may be blended singly or in combination.
As described above, the content of the acid is preferably 0.01 to 1000 ppb by mass relative to the total mass of the composition. From the viewpoint of further improving the effect of the present invention, it is more preferably 0.05 to 800 ppb by mass, still more preferably 0.05 to 500 ppb by mass.
< Fe component >
The composition of the present invention contains an Fe component.
As described above, in the composition of the present invention, the content of the Fe component relative to the content of the acid was 10 -5～102 in terms of mass ratio. From the viewpoint of further improving the effect of the present invention, the content of the Fe component to the content of the acid is preferably 10 -3～10-1 in terms of mass ratio.
Further, as described above, in the composition of the present invention, the content of the Fe component is preferably 0.1 ppt to 1 ppb by mass relative to the total mass of the composition. From the viewpoint of further improving the effect of the present invention, it is more preferably 0.1 to 800 mass ppt, still more preferably 0.1 to 500 mass ppt. The content herein means the total metal content of Fe atoms.
< Water >)
The composition of the present invention may contain water as a solvent.
The water content is not particularly limited, and may be 1 to 99.999% by mass based on the total mass of the composition.
As water, ultrapure water used in the manufacture of semiconductor devices is preferable.
Among them, water in which the ion concentration of metal atoms derived from Fe, co, na, K, ca, cu, mg, mn, li, al, cr, ni and Zn is reduced is more preferable, and water in which the concentration of metal atoms is adjusted to ppt or less (in one form, the metal content is less than 0.001 mass ppt) is more preferable when the composition of the present invention is used for liquid preparation. As the adjustment method, purification using a filtration membrane or an ion exchange membrane or purification by distillation is preferably used. Examples of the adjustment method include the methods described in paragraphs [0074] to [0084] of Japanese patent application laid-open No. 2011-110515 and the methods described in Japanese patent application laid-open No. 2007-254168.
The water used in the embodiment of the present invention is preferably water obtained as described above. When the composition of the present invention is used as a treatment liquid for semiconductor manufacturing, the water is more preferably used not only for the composition of the present invention but also for cleaning of a storage container and for preparing a reagent kit described later, from the viewpoint that the desired effect of the present invention can be obtained remarkably. The water is preferably used in the production process of the composition of the present invention, the measurement of the components of the composition of the present invention, the measurement of the evaluation of the composition of the present invention, and the like.
< Anthraquinone Compounds >)
The composition of the present invention may contain an anthraquinone compound.
Examples of the anthraquinone compound include anthraquinone compounds used in the synthesis of hydrogen peroxide by the anthraquinone method. Specifically, at least 1 or more selected from the group consisting of alkylanthraquinone and alkyltetrahydroanthraquinone is preferable.
The alkyl group contained in the alkylanthraquinone and the alkyltetrahydroanthraquinone is preferably a carbon atom number of 1 to 8, more preferably a carbon atom number of 1 to 5, for example. Among these, ethylanthraquinone or pentynthraquinone is preferable. Further, as the alkyl tetrahydroanthraquinone, ethyl tetrahydroanthraquinone or amyl tetrahydroanthraquinone is preferable.
In the composition of the present invention, the anthraquinone compound may be blended singly or in combination of 2 or more.
When the composition of the present invention contains an anthraquinone compound, the content thereof is preferably 0.01 to 1000 ppb by mass relative to the total mass of the composition, as described above. From the viewpoint of further improving the effect of the present invention, it is more preferably from 0.05 to 800 ppb by mass, and still more preferably from 0.05 to 500 ppb by mass.
< Metal component containing specific atom selected from the group consisting of Ni, pt, pd, cr, ti and Al)
The composition of the present invention may contain at least 1 or more metal components containing a specific atom selected from the group consisting of Ni, pt, pd, cr, ti and Al.
When the composition of the present invention contains a metal component containing a specific atom selected from the group consisting of Ni, pt, pd, cr, ti and Al, as described above, the content of the metal component is preferably 0.01 mass ppt to 10 mass ppb, respectively, per the total mass of the composition, per each specific atom. From the viewpoint of further improving the effect of the present invention, it is more preferably 0.01 to 1 ppb by mass, still more preferably 0.01 to 800 ppt by mass, and particularly preferably 0.01 to 500 ppt by mass.
< Metal component containing specific atom selected from the group consisting of Ni, pt, pd and Al)
The composition of the present invention may contain at least 1 or more metal components containing a specific atom selected from the group consisting of Ni, pt, pd and Al.
When the composition of the present invention contains a metal component containing a specific atom selected from the group consisting of Ni, pt, pd and Al, as described above, the content thereof is preferably 0.01 mass ppt to 1 mass ppb relative to the total mass of the composition. From the viewpoint of further improving the effect of the present invention, it is more preferably 0.01 to 800 mass ppt, still more preferably 0.01 to 500 mass ppt.
The composition of the present invention may contain other additives in addition to the above components within the range where the effects of the present invention are exerted. Examples of the other additives include surfactants, defoamers, pH adjusters, and fluorides.
[ Method for producing composition ]
The method for producing the composition of the present invention comprises:
A raw material purification step (hereinafter also referred to as "step 1") of purifying 1 or more of the raw material components selected from the group consisting of solvents and anthraquinone compounds;
A hydrogen peroxide synthesis step (hereinafter also referred to as "step 2") of synthesizing an anthrahydroquinone compound by reducing the anthraquinone compound in the presence of a catalyst, and further oxidizing the anthrahydroquinone compound to synthesize hydrogen peroxide;
A hydrogen peroxide separation step (hereinafter also referred to as "step 3"), in which the obtained hydrogen peroxide is extracted and taken out of the reaction system; and
A hydrogen peroxide composition purification step (hereinafter also referred to as "step 4") of further purifying a hydrogen peroxide composition containing hydrogen peroxide separated from the reaction system.
Hereinafter, the 1 st to 4 th steps will be described in detail.
(Step 1: raw material purification step)
The method for producing the composition of the present invention is a method for synthesizing hydrogen peroxide by the so-called anthraquinone method using an anthraquinone compound as a raw material.
In step 1,1 or more of the raw material components selected from the group consisting of solvents and anthraquinone compounds are purified beforehand by distillation, ion exchange, filtration, and the like. As the degree of purification, for example, purification to a raw material purity of preferably 99% or more, and purification to a purity of more preferably 99.9% or more is performed. In order to obtain the remarkable effect based on the present invention, it is important to use such a high purity raw material.
The solvent in step 1 means a solvent which is used in the synthesis reaction of hydrogen peroxide and which is used in step 2, and which is water as an extraction solvent for hydrogen peroxide in step 3 or is optionally used before the completion of the purification step of the composition.
The raw material component containing an anthraquinone compound in step 1 is a reduction catalyst containing an anthraquinone compound in addition to the anthraquinone compounds such as alkylanthraquinone and alkyltetrahydroanthraquinone.
The purification method is not particularly limited, and examples thereof include a method of passing through an ion exchange resin, an RO membrane (reverse osmosis membrane (Reverse Osmosis Membrane)) or the like, a method of distillation, filtration described later, and the like. Specifically, for example, a method in which a liquid is passed through a reverse osmosis membrane or the like to perform 1 purification, and then the liquid is passed through a purification apparatus including a cation exchange resin, an anion exchange resin, or a mixed bed ion exchange resin to perform 2 purifications may be mentioned.
The purification treatment may be performed by combining a plurality of the above known purification methods.
Further, the purification treatment may be performed a plurality of times.
(Step 2: hydrogen peroxide Synthesis step)
The present step 2 can be applied to a known method for synthesizing hydrogen peroxide using an anthraquinone compound as a raw material. For example, a method described in Japanese patent application laid-open No. 2014-108903 is mentioned.
(Step 3: hydrogen peroxide separation step)
The present 3 rd step is a step of extracting and taking out the hydrogen peroxide obtained in the 2 nd step, and a known method of extracting hydrogen peroxide can be applied. For example, a method described in Japanese patent application laid-open No. 2014-108903 is mentioned.
In addition, in the case of extraction, water is preferably used for extraction of hydrogen peroxide.
The "water" in step 3 is preferably "water" having been reduced in ion concentration derived from metal atoms such as Fe, co, na, K, ca, cu, mg, mn, li, al, cr, ni and Zn through step 1, i.e., the raw material purification step, and more preferably ion-exchanged water or ultrapure water used in the production of semiconductor devices.
(Step 4: purification step of Hydrogen peroxide composition)
The 4 th step is a step of purifying the hydrogen peroxide composition (hydrogen peroxide water) obtained in the 3 rd step.
The purification method is not particularly limited, and examples thereof include a method of passing through an ion exchange resin, a method of distillation under reduced pressure, and the like.
As a method of passing through the ion exchange resin, for example, a method using a mixed bed of an anion exchange resin and a cation exchange resin is exemplified in addition to a method using an acidic cation exchange resin.
The hydrogen peroxide water may be filtered as described below.
The purification treatment may be performed by combining a plurality of the above known purification methods.
Further, the purification treatment may be performed a plurality of times.
< Filtering >
The filter is not particularly limited as long as it is a filter conventionally used for filtration and the like. For example, filters based on fluorine resins such as Polytetrafluoroethylene (PTFE) and tetrafluoroethylene perfluoroalkyl vinyl ether copolymer (PFA), polyamide resins such as nylon, polyolefin resins (including high density and ultra high molecular weight) such as Polyethylene and Polypropylene (PP), and the like are exemplified. Among these materials, a material selected from the group consisting of polyethylene, polypropylene (including high density polypropylene), fluorine resins such as PTFE and PTA, and polyamide resins such as nylon is preferable, and among these, a filter of polypropylene (including high density polypropylene) and nylon is more preferable. By using the filter made of these materials, it is possible to effectively remove foreign matters having high polarity which easily cause defects (residue defects or particle defects) of the semiconductor substrate, and in addition, it is possible to effectively reduce the amount of the specific metal component of the present application.
In one embodiment, the pore diameter of the filter is preferably about 0.001 to 1.0. Mu.m, more preferably about 0.02 to 0.5. Mu.m, and still more preferably about 0.01 to 0.1. Mu.m. By setting the range to this value, it is possible to prevent clogging by filtration and to reliably remove fine foreign substances such as impurities and aggregates contained in the object to be treated (the solution to be filtered, for example, the solvent or the raw material component used in step 1 and the hydrogen peroxide water obtained in step 3).
When filters are used, different filters may also be combined.
When different filters are used in combination, for example, a method of using the 1 st filter and the 2 nd filter can be mentioned. In this case, the filtration in the 1 st filter may be performed 1 time or 2 or more times. Further, the 1 st filter having different pore diameters may be combined in the above range. The pore size can be referred to herein as the nominal value of the filter manufacturer. As commercially available filters, for example, various filters provided by NIHON PALL LT d., toyo Roshi Kaisha, ltd., nihon Entegris k.k. (old Japan Microlis co., ltd.), KITZ MICRO FILTER CORPORATION, or the like can be selected.
As the 2 nd filter, a filter made of the same material as the 1 st filter or the like can be used. In one embodiment, the pore diameter of the 2 nd filter is preferably about 0.01 to 1.0. Mu.m, and more preferably about 0.1 to 0.5. Mu.m. When the content of the component particles (for example, fe particles described later) is within this range, foreign matter mixed in the object to be treated can be removed while the component particles remain.
The filter to be used is preferably treated before filtering the object to be treated. The liquid used in this treatment is not particularly limited, but the metal content is preferably less than 0.001 mass ppt, and the desired effect of the present invention can be clearly obtained if the liquid is a liquid in which other organic solvents are purified and the metal content is in the above-described range, or the composition of the present invention itself, a liquid in which the composition of the present invention is diluted, or a liquid containing a compound added to the composition of the present invention, in addition to the above-described water.
Hereinafter, a purification apparatus which can be preferably used for purifying an object to be treated and which is provided with a filter will be described.
Purification device
FIG. 1 is a schematic diagram showing one embodiment of a purification apparatus. The purification apparatus 100 includes a tank 101, and the tank 101 includes a supply port 102 for supplying an object to be treated. The purification apparatus 100 includes a filter 105, and the tank 101 and the filter 105 are connected by a supply line 109 so that a fluid (an object to be treated) can be transported between the tank 101 and the filter 105. The valve 103 and the pump 104 are disposed in the supply line 109. In fig. 1, the purification apparatus 100 includes a tank 101 and a filter apparatus 105, but the purification apparatus is not limited to this, and may be used for filtering an object to be treated.
In the purification apparatus 100, the fluid supplied from the supply port 102 flows into the filter device 105 via the valve 103 and the pump 104. The fluid discharged from the filter device 105 is stored in the tank 101 through the circulation line 110.
The purification apparatus 100 includes a discharge unit 111 for discharging the object to be treated into the circulation line 110. The discharge unit 111 includes a valve 107 and a container 108, and can store the object to be processed in the container 108 by switching between the valve 106 provided in the circulation line and the valve 107. A switchable line 113 is connected to the valve 107, and the object to be treated after the cycle cleaning can be discharged to the outside of the purification apparatus 100 through the line 113. The object to be processed after the cyclic cleaning may contain particles, metal impurities, and the like, and according to the purification apparatus 100 including the pipe 113 for discharging the object to the outside of the apparatus, the foreign matter which is likely to cause defects in the semiconductor substrate can be effectively removed without contaminating the filling portion of the container 108, and the like.
The purification apparatus 100 further includes a treatment object monitoring unit 112 in the circulation line 110. In fig. 1, the purification apparatus 100 includes the object monitoring unit 112 in the circulation line 110, but the purification apparatus is not limited to this, and may be used for filtering the object. The object monitoring unit 112 may be provided in the supply line 109 or may be provided in the supply line 109 and the circulation line 110. In the purification apparatus 100, the object to be treated monitoring unit 112 is directly provided in the circulation line 110, but the purification apparatus is not limited to this, and may be used for filtering the object to be treated. The object monitoring unit may be provided in a temporary storage tank (different from tank 101) for a fluid (not shown) provided in the pipeline.
Fig. 2 is a schematic diagram showing another embodiment of a purification apparatus that can be used for filtering an object to be treated. The purification apparatus 200 includes the tank 101 and the filter apparatus 105, and further includes a distillation column 201, and the distillation column 201 is connected to a line 202, a line 204, and a line 203 through the tank 101, and is configured so that a fluid can be transferred between the line and the tank 101 through the lines. On the other hand, the purification apparatus that can be used for filtering the object to be treated is not necessarily provided with the filtration apparatus 105 and/or the distillation column 201, but may be provided with a reaction vessel or the like connected to the distillation column 201 via a line 203. In the case where the object to be treated is hydrogen peroxide water, a reaction vessel or the like connected to the distillation column 201 via a line 203 and the distillation column 201 may not be provided.
In the purification apparatus 200, a fluid supplied to the distillation column 201 via a line 203 is distilled in the distillation column 201. The distilled fluid is contained in tank 101 via line 202. The supply line 109 is provided with a valve 103 and a valve 206, and fluid discharged from the tank 101 can be caused to flow into the filter device 105 by switching with a valve 205 provided in the line 204.
In the purification apparatus 200, the fluid discharged from the tank 101 can be again introduced into the distillation column 201. In this case, by switching the valves 103, 206, and 205, the fluid flows from the line 204 into the distillation column 201 via the valve 207 and the line 203.
The material of the liquid receiving portion of the purification apparatus (definition of the liquid receiving portion will be described later) is not particularly limited, and is preferably formed of at least 1 selected from the group consisting of a nonmetallic material and an electropolished metallic material in view of being able to further reduce foreign matter of the object to be treated. In the present specification, the term "liquid receiving portion" means a region having a thickness of 100nm from a surface of a portion (for example, an inner surface of a tank, an inner surface of a pipe, or the like) where there is a possibility of fluid contact.
The nonmetallic material is not particularly limited, but polyolefin resins such as polyethylene resin, polypropylene resin and polyethylene-polypropylene resin, and fluorine-containing resin materials such as perfluorinated resin are preferable, and fluorine-containing resins are preferable from the viewpoint of less elution of metal atoms.
Examples of the fluorine-containing resin include a perfluoro resin and the like, and examples thereof include a tetrafluoroethylene resin (PTF E), a tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer (PFA), a tetrafluoroethylene-hexafluoropropylene copolymer resin (FEP), a tetrafluoroethylene-ethylene copolymer resin (ETFE), a chlorotrifluoroethylene-ethylene copolymer resin (ECTFE), a vinylidene fluoride resin (PVDF), a chlorotrifluoroethylene copolymer resin (PCTFE), and a vinyl fluoride resin (PVF).
Among them, the fluorine-containing resin is preferably a tetrafluoroethylene resin, a tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer, or a tetrafluoroethylene-hexafluoropropylene copolymer resin.
The metal material is not particularly limited, and known materials can be used.
The metal material may be, for example, a metal material in which the total content of chromium and nickel exceeds 25 mass% based on the total mass of the metal material, and is preferably 30 mass% or more. The upper limit of the total content of chromium and nickel in the metal material is not particularly limited, but is generally preferably 90 mass% or less.
Examples of the metal material include stainless steel and nickel-chromium alloy.
The stainless steel is not particularly limited, and known stainless steel can be used. Among these, an alloy containing 8 mass% or more of nickel is preferable, and an austenitic stainless steel containing 8 mass% or more of nickel is more preferable. Examples of austenitic stainless Steel include SUS (Steel Use STAINLES S)) 304 (Ni content 8 mass%, cr content 18 mass%), SUS304L (Ni content 9 mass%, cr content 18 mass%), SUS316 (Ni content 10 mass%, cr content 16 mass%) and SUS316L (Ni content 12 mass%, cr content 16 mass%).
The nickel-chromium alloy is not particularly limited, and a known nickel-chromium alloy can be used. Among them, a nickel-chromium alloy having a nickel content of 40 to 75 mass% and a chromium content of 1 to 30 mass% is preferable.
Examples of the nickel-chromium alloy include Hastelloy (trade name, the same applies hereinafter), monel (trade name, the same applies hereinafter), and Inconel (trade name, the same applies hereinafter). More specifically, hastelloyC-276 (Ni content 63 mass%, cr content 16 mass%), hastelloy-C (Ni content 60 mass%, cr content 17 mass%), hastelloyC-22 (Ni content 61 mass%, cr content 22 mass%) and the like can be cited.
The nickel-chromium alloy may contain boron, silicon, tungsten, molybdenum, copper, cobalt, and the like, in addition to the above alloy, if necessary.
The method of electropolishing the metal material is not particularly limited, and a known method can be used. For example, the methods described in paragraphs 0011 to 0014 of Japanese patent application laid-open No. 2015-227501, paragraphs 0036 to 0042 of Japanese patent application laid-open No. 2008-264929, and the like can be used.
The metallic material may be presumed to be a metallic material in which the chromium content in the surface passivation layer (passivation layer) is greater than the chromium content in the parent phase by electropolishing. Therefore, it is difficult to flow out the metal impurities containing metal atoms in the object to be treated from the distillation column formed of the metal material electropolished in the liquid receiving section, and therefore, it is presumed that the metal material can give a distilled object to be treated with reduced impurity content.
In addition, the metallic material may also be polished (buffing). The polishing method is not particularly limited, and a known method can be used. The size of the abrasive grains (abrasive grain) used in the polishing process is not particularly limited, but is preferably #400 or less in view of the ease of making the irregularities on the surface of the metal material smaller. In addition, polishing is preferably performed before electropolishing.
In view of further reducing foreign matter in the object to be treated, the liquid receiving portion is preferably formed of electropolished stainless steel. In particular, when the purification apparatus includes a tank, it is more preferable that the purification apparatus is formed of stainless steel in which the liquid receiving portion of the tank is electropolished. The ratio by mass of the Cr content to the Fe content in the liquid receiving portion (hereinafter also referred to as "Cr/Fe") is not particularly limited, but is preferably generally 0.5 to 4, and more preferably exceeds 0.5 and is less than 3.5, and still more preferably 0.7 to 3.0, in view of the fact that metal impurities and/or organic impurities are more difficult to be eluted from the object to be treated. When Cr/Fe exceeds 0.5, elution of metal from the tank can be suppressed, and when Cr/Fe is less than 3.5, peeling of the liquid receiving portion, which is a cause of particles, or the like is less likely to occur.
The method for adjusting the Cr/Fe in the metal material is not particularly limited, and examples thereof include a method for adjusting the Cr atom content in the metal material, a method for electropolishing to make the Cr content in the polished surface passivation layer larger than the Cr content in the mother phase, and the like.
The metallic material may be applied to a coating technique.
Coating techniques can be broadly classified into 3 types, i.e., metal coating (various plating), inorganic coating (various chemical conversion treatments, glass, concrete, ceramics, etc.), and organic coating (rust preventive oil, paint, rubber, plastic, etc.).
The coating technique is preferably a surface treatment with a rust preventive oil, a rust preventive agent, a corrosion inhibitor, a chelating compound, a releasable plastic or a lining agent.
Among them, various carboxylic acids such as chromates, nitrites, silicates, phosphates, oleic acid, dimer acid, and naphthenic acid, corrosion inhibitors such as carboxylic acid metal soaps, sulfonates, amine salts, and esters (glycerin esters and phosphoric esters of higher fatty acids), chelating compounds such as ethylenediamine tetraacetic acid, gluconic acid, nitrilotriacetic acid, hydroxyethyl ethylenediamine triacetic acid, and diethylenetriamine pentaacetic acid, and fluororesin liners are preferable, and phosphate treatment and fluororesin liners are particularly preferable.
The purification apparatus can further reduce foreign matter in the object to be treated by providing the filter 105. The filter member included in the filter device 105 is not particularly limited, but is preferably at least 1 selected from the group consisting of a filter having a particle removal diameter (particle-ELIMINATING DIAMETER) of 20nm or less and a metal ion adsorption filter, and more preferably a filter having a particle removal diameter of 20nm or less and a metal ion adsorption filter.
Filter with particle removal diameter of 20nm or less
The filter having a particle removal diameter of 20nm or less has a function of effectively removing particles having a diameter of 20nm or more from an object to be treated.
The particle removal diameter of the filter is preferably 1 to 15nm, more preferably 1 to 12nm. When the particle removal diameter is 15nm or less, finer particles can be removed, and when the particle removal diameter is 1nm or more, the filtration efficiency is improved.
Here, the particle removal diameter means the smallest size of particles that can be removed by the filter. For example, when the particle removal diameter of the filter is 20nm, particles having a diameter of 20nm or more can be removed.
Examples of the material of the filter include nylon such as 6-nylon and 6, 6-nylon, polyethylene, polypropylene, polystyrene, polyimide, polyamideimide, and fluororesin. The polyimide and/or polyamideimide may have at least 1 selected from the group consisting of a carboxyl group, a salt-type carboxyl group, and an-NH-bond. With respect to solvent resistance, fluororesin, polyimide and/or polyamideimide are excellent. Further, from the viewpoint of adsorbing metal ions, nylon such as 6-nylon and 6, 6-nylon is preferable.
The filter device 105 may also comprise a plurality of filters as described above. When the filtration device 105 includes a plurality of filters, the other filters are not particularly limited, and filters having a particle removal diameter of 50nm or more (for example, fine filtration membranes for removing particles having a pore diameter of 50nm or more) are preferable. When there are particulates in addition to colloidal impurities, particularly colloidal impurities containing metal atoms such as iron and aluminum, the filter with a particle removal diameter of 20nm or less (for example, a microfiltration membrane for particulate removal with a pore diameter of 50nm or more) is used before the filter with a particle removal diameter of 20nm or less (for example, a microfiltration membrane for particulate removal with a pore diameter of 50nm or more) is used, and filtration of the object to be purified is performed, whereby the filtration efficiency of the filter with a particle removal diameter of 20nm or less (for example, a microfiltration membrane with a pore diameter of 20nm or less) is improved, and the removal performance of the particles is further improved.
Metal ion adsorption filter
The filter device 105 preferably includes a metal ion adsorption filter.
The metal ion adsorption filter is not particularly limited, and a known metal ion adsorption filter can be used.
Among them, as the metal ion adsorption filter, a filter capable of ion exchange is preferable. The metal ion to be adsorbed is not particularly limited, and is preferably at least 1 metal ion selected from the group consisting of Fe ion, ni ion, pt ion, pd ion, cr ion, ti ion, and Al ion, and more preferably all metal ions such as Fe ion, ni ion, pt ion, pd ion, cr ion, ti ion, and Al ion.
From the viewpoint of improving the adsorption performance of metal ions, the metal ion adsorption filter preferably has acid groups on the surface. Examples of the acid group include a sulfo group and a carboxyl group.
Examples of the base material constituting the metal ion adsorption filter include cellulose, diatomaceous earth, nylon, polyethylene, polypropylene, polystyrene, and fluororesin. Nylon is particularly preferred from the viewpoint of the efficiency of adsorbing metal ions.
The metal ion adsorption filter may be made of a material containing polyimide and/or polyamideimide. Examples of the metal ion adsorption filter include polyimide and/or polyamideimide porous membranes described in JP 2016-155121A (JP 2016-155121).
The polyimide and/or polyamideimide porous membrane may contain at least 1 selected from the group consisting of carboxyl groups, salt-type carboxyl groups, and-NH-bonds. The metal ion adsorption filter has more excellent solvent resistance if it contains a fluororesin, polyimide and/or polyamideimide.
Organic impurity adsorption filter
The filtration device 105 may also comprise an organic impurity adsorbing filter.
The organic impurity adsorbing filter is not particularly limited, and a known organic impurity adsorbing filter can be used.
Among them, as the organic impurity adsorbing filter, it is preferable that the organic impurity adsorbing filter has an organic skeleton capable of interacting with the organic impurity on the surface (in other words, the surface is modified by the organic skeleton capable of interacting with the organic impurity) in terms of improving the adsorption performance of the organic impurity. Examples of the organic framework capable of interacting with the organic impurities include chemical structures that react with the organic impurities to trap the organic impurities in the organic impurity adsorbing filter. More specifically, when n-long-chain alkyl alcohol (structural isomer when 1-long-chain alkyl alcohol is used as an organic solvent) is contained as the organic impurity, an alkyl group is exemplified as the organic skeleton. When dibutylhydroxytoluene (BHT) is contained as an organic impurity, a phenyl group is exemplified as the organic skeleton.
Examples of the base material (material) constituting the organic impurity adsorbing filter include cellulose, diatomaceous earth, nylon, polyethylene, polypropylene, polystyrene, and fluororesin, which carry activated carbon.
Further, as the organic impurity adsorbing filter, a filter in which activated carbon is fixed to a nonwoven fabric as described in japanese unexamined patent publication No. 2002-273123 and japanese unexamined patent publication No. 2013-150979 can be used.
As the organic impurity adsorbing filter, not only the chemical adsorption described above (adsorption using an organic impurity adsorbing filter having an organic skeleton capable of interacting with organic impurities on the surface) but also physical adsorption methods can be applied.
For example, when BHT is contained as an organic impurity, the structure of BHT is greater than 10 angstroms (=1 nm). Therefore, by using an organic impurity adsorbing filter having a pore diameter of 1nm, BHT cannot pass through the pores of the filter. That is, BHT is physically captured by the filter, and is therefore removed from the object to be purified. Thus, the removal of organic impurities may be applied not only to chemical interactions but also to physical removal methods. In this case, a filter having a pore size of 3nm or more is used as the "particle removal filter", and a filter having a pore size of less than 3nm is used as the "organic impurity adsorbing filter".
Again, the description is repeated, and different filters may be combined when using the filters. As a method of combining different filters, for example, a method of combining the 1 st filter and the 2 nd filter described above is given. In this case, the filtration in the 1 st filter may be performed only 1 time, or may be performed 2 times or more. When the filtration is performed 2 times or more by combining different filters, the filters may be of the same kind or different kinds, but are preferably of different kinds. Typically, the 1 st filter and the 2 nd filter are different in at least one of the preferable pore sizes and constituent raw materials.
The filter pore size after the 2 nd time is preferably the same as or smaller than the filter pore size of the 1 st time. Further, the 1 st filter having different pore diameters may be combined in the above range. The pore size can be referred to herein as the nominal value of the filter manufacturer. As a commercially available filter, for example, it is possible to select from various filters provided by NIHON PALL ltd., toyo Ro SHI KAISHA, ltd., nihon Entegris k.k. (old Japan Microlis co., ltd.), KITZ MICRO FILTER CORPORATION, or the like. Further, a polyamide "P-nylon filter- (pore size 0.02 μm, critical surface tension 77 mN/m)"; (NIHON PALL LTD. Manufactured), PE clean filter (pore size 0.02 μm) manufactured by high density polyethylene; (NIHON PALL LTD. Times.) "PE clean filter (pore size 0.01 μm)" made of high-density polyethylene; (NIHON PALL LTD. Manufactured).
In view of further reducing foreign matter in the object to be treated, the purification device is preferably preliminarily cleaned with a cleaning liquid. In this method, a cleaning liquid is supplied from a supply port 102 of a tank 101. The amount of the supplied cleaning liquid is not particularly limited, and is preferably an amount sufficient to clean the liquid receiving portion of the tank 101, and the volume of the supplied cleaning liquid is preferably 30% by volume or more with respect to the volume of the tank 101. The valve 103 may be closed or opened when the cleaning liquid is supplied from the supply port 102, but it is preferable to close the valve 103 when the cleaning liquid is supplied from the supply port 102 in terms of easier cleaning of the tank 101.
The cleaning liquid supplied to the tank 101 may be directly supplied to the purification apparatus, or may be supplied to the purification apparatus (for example, through the supply line 109) after the cleaning in the tank 101. The method of cleaning the inside of the tank 101 with the cleaning liquid is not particularly limited, and for example, a method of cleaning the inside of the tank 101 by rotating a stirring blade, not shown, provided in the tank 101 may be mentioned. The time for cleaning the tank with the cleaning liquid is not particularly limited, and may be appropriately selected according to the material of the liquid receiving portion of the tank 101, the possibility of contamination, and the like. Generally, it is preferably about 0.1 seconds to 48 hours. In addition, when only the tank 101 is cleaned, for example, the cleaned cleaning liquid may be discharged from a discharge port, not shown, provided at the bottom of the tank.
The method of cleaning the supply line 109 and the like of the purification apparatus 100 with the cleaning liquid is not particularly limited, and a method of circulating the cleaning liquid in the purification apparatus through the supply line 109 and the circulation line 110 by operating the pump 104 with the valves 103 and 106 opened and the valve 107 closed (hereinafter, also referred to as "circulation cleaning") is preferable. By providing the above configuration, it is possible to transport the cleaning liquid and to effectively disperse and/or more effectively dissolve foreign matters and the like adhering to the liquid receiving portions of the tank 101, the filter 105, the supply line 109 and the like in the cleaning liquid by the cleaning liquid.
In particular, when the purification apparatus is provided with a filtration apparatus, a cyclic washing is preferable as the washing method. An example of cyclic cleaning is described with reference to fig. 1. First, the cleaning liquid supplied from the tank 101 to the purification apparatus via the valve 103 is returned to the tank 101 again (circulated) via the supply line 109 (via the filter apparatus 105, the circulation line 110, and the valve 106). At this time, the cleaning liquid is filtered by the filtering device 105, and particles and the like dissolved and dispersed in the cleaning liquid are removed, so that the cleaning effect can be further improved.
As another mode of the cleaning method, for example, a method may be used in which the pump 104 is operated while the valves 103 and 107 are opened and the valve 106 is closed, the cleaning liquid supplied from the supply port 102 of the tank 101 into the purification apparatus is flowed into the filter apparatus 105 through the valves 103 and 104, and then the cleaning liquid is discharged to the outside of the purification apparatus through the valve 107 without circulating (in this specification, this method is also referred to as "intermittent cleaning"). In this case, the cleaning liquid may be intermittently supplied to the purification apparatus in a predetermined amount, or may be continuously supplied to the purification apparatus as described above.
Filtration in step 4
When filtration is performed in step 4, filtration of the hydrogen peroxide composition is preferably performed by the following method in addition to the above-described method. In step 1, filtration by the following method may be performed.
The filter is not particularly limited as long as it is a filter conventionally used for filtration and the like. Examples thereof include filters based on fluororesins such as Polytetrafluoroethylene (PTFE) and tetrafluoroethylene perfluoroalkyl vinyl ether copolymer (PFA), polyamide-based resins such as nylon, polyolefin resins (including high density and ultra high molecular weight) such as Polyethylene and Polypropylene (PP), and the like. Among these materials, a material selected from the group consisting of polyethylene, polypropylene (including high density polypropylene), a fluororesin such as PTFE and PTA, and a polyamide resin such as nylon is preferable, and among these, a fluororesin filter such as PTFE and PTA is more preferable. By using the filter made of these materials, it is possible to effectively remove foreign matters having high polarity which easily cause defects (residue defects or particle defects) of the semiconductor substrate, and in addition, it is possible to effectively reduce the amount of the specific metal component of the present application.
The critical surface tension of the filter is preferably 70mN/m or more, more preferably 95mN/m or less, and still more preferably 75mN/m or more and 85mN/m or less. In addition, the value of the critical surface tension is the manufacturer's nominal value. By using a filter having a critical surface tension in the above range, it is possible to effectively remove foreign matter having high polarity which is liable to cause defects (residue defects and particle defects) of the semiconductor substrate, and in addition, it is possible to effectively reduce the amount of the specific metal component of the present application.
In one embodiment, the pore diameter of the filter is preferably about 2 to 20nm, more preferably 2 to 15nm. By setting the content to this range, the amount of the specific metal component of the present application can be effectively reduced, while suppressing the clogging due to filtration and reliably removing fine foreign matters such as impurities and aggregates contained in the hydrogen peroxide composition.
When filters are used, different filters may also be combined. In this case, the filtration in the 1 st filter may be performed only 1 time or may be performed 2 times or more. When the filtration is performed 2 times or more by combining different filters, the filter pore size after the 2 nd time is preferably the same as or smaller than the filter pore size of the 1 st time. Further, the 1 st filter having different pore diameters may be combined in the above range. The pore size can be referred to herein as the nominal value of the filter manufacturer. As a commercially available filter, for example, it is possible to select from various filters provided by NIHON PALL ltd., toyo Ro SHI KAISHA, ltd., nihon Entegris k.k. (old Japan Microlis co., ltd.), KITZ MICRO FILTER CORPORATION, or the like. Further, a polyamide "P-nylon filter- (pore size 0.02 μm, critical surface tension 77 mN/m)"; (NIHON PALL LTD. Manufactured), PE clean filter (pore size 0.02 μm) manufactured by high density polyethylene; (NIHON PALL LTD. Times.) "PE clean filter (pore size 0.01 μm)" made of high-density polyethylene; (NIHON PALL LTD. Manufactured).
As the 2 nd filter, a filter made of the same material as the 1 st filter or the like can be used. The pore diameter of the 2 nd filter is preferably about 1 to 10 nm.
In the present invention, the filtration step is preferably performed at room temperature (25 ℃) or lower. More preferably at most 23℃and still more preferably at most 20 ℃. The temperature is preferably 0℃or higher, more preferably 5℃or higher, and still more preferably 10℃or higher.
In the filtration step, the particulate foreign matter and impurities can be removed, and if the temperature is set to the above temperature, the amount of the particulate foreign matter and/or impurities dissolved in the hydrogen peroxide composition is reduced, and thus the particulate foreign matter and impurities can be effectively removed by filtration.
In particular, when the hydrogen peroxide composition contains a metal component containing a specific atom selected from the group consisting of Ni, pt, pd, cr, ti and Al in an amount exceeding that desired in the present application, filtration is preferably performed at the above-described temperature. The mechanism is not clear, but it is considered that when a metal component containing a specific atom selected from the group consisting of Ni, pt, pd, cr, ti and Al is contained in the hydrogen peroxide composition, most of the metal component exists in a particulate colloidal state. It is considered that, when filtration is performed at the above temperature, a part of the metal component suspended in a colloidal state is aggregated, and therefore, the aggregate is effectively removed by filtration, and is easily adjusted to the desired amount of the present application.
Also, the filter used is preferably treated prior to filtering the hydrogen peroxide composition. The liquid used in this treatment is not particularly limited, but it is preferable that the metal content is less than 0.001 ppt (parts per trillion% by mass), and examples thereof include a liquid in which other organic solvents are purified so that the metal content falls within the above range, a liquid in which the composition of the present invention is itself (a liquid adjusted in advance) or diluted, and a liquid in which the composition of the present invention is further purified so that the metal components, impurities, coarse particles, and the like are further reduced, in addition to the above water. The desired effect of the present invention is remarkably obtained by pretreating the filter with the liquid having a reduced metal content as described above.
The step of purifying the hydrogen peroxide composition in the step 4 is preferably performed by combining the above-described respective purification methods.
The composition of the present invention, which can achieve high purity to the extent that it can be used in the production of semiconductor devices, can be obtained through steps 1 to 4.
In addition, the composition of the present invention is as above. The acid contained in the composition of the present invention may be an acid such as phthalic acid by-produced during the synthesis of hydrogen peroxide by the anthraquinone method, or may be an acid added separately in the step 4 or after the step 4. From the viewpoint of further improving the purity of the composition and the effect of the present invention, it is preferable to add an acid component (preferably phosphoric acid or a phosphoric acid derivative) to the composition in step 4, and it is more preferable to further perform a purification step after adding the acid component.
< Quantitative method >)
Various amounts of the acid component or anthraquinone compound contained in water, the solvent, the raw material component, the composition of the present invention, or the like can be analyzed by ion chromatography.
Various amounts of water, a solvent, a raw material component, or a Fe component or a metal component contained in the composition of the present invention can be analyzed by ICP-MS (inductively coupled plasma mass spectrometry (inductive ly coupled PLASMA MASS spectrometry)) or the like, and Yok ogawa ANALYTICAL SYSTEMS, manufactured by inc. And Agilent 7500cs type, for example, can be used as a measurement device. In the ICP-MS method, the total mass of metal atoms, that is, the total mass of metal ions (ionic metals) and metal particles (nonionic metals) (also referred to as "total metal amount") is quantified.
Further, according to the recently developed SNP-ICP-MS (single nanoparticle-inductively coupled plasma mass spectrometry (Single Nano Particle-Inductively Coupled Plasma-Mass Spectrometr y)), the amount of metal atoms present in a liquid can be measured by dividing the metal ions (ionic metals) and the metal particles (nonionic metals). The metal particles (nonionic metal) herein refer to components that are not dissolved in a solution but exist as solids.
The amount of metal atoms contained in a processing liquid for semiconductor production and the like has been analyzed by ICP-MS method and the like, whereas ionic metals and metal particles (nonionic metals) derived from metal atoms cannot be identified by conventional methods such as ICP-MS method and the like, and therefore, the amount of metal atoms, that is, the total mass of ionic metals and particulate metals (nonionic metals) (hereinafter, also referred to as "total metal amount" and the like) has been quantified.
Metal atoms contained as impurities in a processing liquid for semiconductor manufacturing are one of the main causes of defects in fine patterns and fine semiconductor elements. Therefore, it is considered that the smaller the amount of metal atoms contained in the treatment liquid for semiconductor manufacturing is, the better. However, the present inventors found that the amount of metal atoms contained in the treatment liquid is not necessarily related to the occurrence rate of defects, and that there is a deviation in the occurrence rate of defects.
The present inventors have made intensive studies on the influence of each of an ionic metal derived from a metal atom contained in a treatment liquid for semiconductor production and metal particles (nonionic metal) on defects, which can be identified and quantified by measurement using the SNP-ICP-MS method. As a result, it was found that the amount of metal particles (nonionic metal) greatly affects the occurrence of defects, and that there is a correlation between the amount of metal particles (nonionic metal) and the occurrence of defects. As an apparatus for the SNP-ICP-MS method, for example, agilent Technologies Japan, ltd. Manufactured by Agilent 8800 triple quadrupole ICP-MS (inductively coupled PLASMA MASS electrolyte, option (option) # 200) can be used for measurement by the method described in examples. In addition to the above, perkinElmer co., ltd. NexION S, and AGILENT TEC hnologies Japan, ltd. Agilent 8900 may be mentioned.
In the composition of the present invention, the content of Fe particles (nonionic metal) when measured by SNP-ICP-MS method is preferably 0.01 to 0.1 ppb by mass ppt based on the total mass of the composition, from the viewpoints of improving defect performance and securing stability with time.
When the composition of the present invention contains a metal component containing a specific atom selected from the group consisting of Ni, pt, pd, cr, ti and Al and the metal component contains metal particles (nonionic metal), the content of the metal particles in the composition of the present invention is preferably 0.01 to 100 mass ppt, more preferably 0.01 to 50 mass ppt, and even more preferably 0.01 to 10 mass ppt, per the total mass of the composition, per each specific atom, from the viewpoints of improving defect performance and securing stability over time. That is, when the composition of the present invention contains, for example, only Pt particles, the Pt particles fall within the above-mentioned numerical range. On the other hand, when the composition of the present invention contains Pt particles and Ni particles, for example, the Pt particles and the Ni particles respectively fall within the above numerical ranges. The content of the metal particles is a value measured by the SNP-ICP-MS method.
The treatment, analysis and measurement including preparation of the composition of the present invention, opening and closing and/or cleaning of the container, filling of the composition and the like are preferably performed in a clean room (clean room). Preferably the clean room meets the 14644-1 clean room standard. Preferably, any of ISO (international standard organization) level 1, ISO level 2, ISO level 3, ISO level 4 is satisfied, more preferably, ISO level 1, ISO level 2, and even more preferably, ISO level 1 is satisfied.
< Organic impurity >)
In addition, a gas chromatography-mass spectrometry apparatus (product name "GCMS-2020", manufactured by SHIMADZU CORPORATION) is also used in some cases for measuring the content of organic impurities. In addition, when the organic impurity is a high molecular weight compound, the structure can be identified and the concentration can be quantified from the decomposed product by a method such as Py-QTOF/MS (pyrolyzer quadrupole time-of-flight mass spectrometry), py-IT/MS (pyrolyzer ion trap mass spectrometry), py-Sector/MS (pyrolyzer magnetic field mass spectrometry), py-FTICR/MS (pyrolyzer fourier transform ion trap mass spectrometry), py-Q/MS (pyrolyzer quadrupole mass spectrometry), and Py-IT-TOF/MS (pyrolyzer ion trap time-of-flight mass spectrometry). For example, py-QTOF/MS can use a device such as that manufactured by SHIMADZU CORPORATION.
< Impurity and coarse particle >)
The composition of the present invention preferably contains substantially no coarse particles.
The coarse particles contained in the composition of the present invention are particles such as dust, dirt, organic solid matter, or inorganic solid matter contained as impurities in the raw material, and particles such as dust, dirt, organic solid matter, or inorganic solid matter contained as contaminants in the preparation of the composition correspond to the particles that are not finally dissolved in the composition of the present invention and are present as particles. The amount of coarse particles present in the composition of the present invention can be measured in a liquid phase by a commercially available measuring device in a light scattering type liquid particle measuring system using a laser as a light source.
Kit and concentrate
The composition of the present invention may be used as a kit for adding other raw materials. In this case, as another raw material to be added separately at the time of use, other compounds may be mixed and used according to the use, in addition to water, a solvent such as an organic solvent, and the like. From the viewpoint of remarkably obtaining the effects of the present invention, among the solvents that can be used in this case, if the ranges of the contents of the Fe component or the metal component contained in the solvents are the same as the ranges specified in the above-described composition of the present invention, the desired effects of the present invention can be remarkably obtained even in the kit and the concentrate.
< Usage >
The composition of the present invention can be preferably used in the manufacture of semiconductor devices. The composition of the present invention can be used in any process for producing a semiconductor device, specifically, in a process for producing a semiconductor device including a photolithography process, an etching process, an ion implantation process, a stripping process, and the like, and can be used as a treatment liquid for treating an organic or inorganic substance after each process is completed or before the next process, specifically, can be used preferably as a cleaning liquid, a removing liquid, a stripping liquid, or the like.
When the composition of the present invention is used in the manufacture of a semiconductor device, it is not particularly limited, and for example, it can be preferably used in the case of mixing with hydrochloric acid for the purpose of removing inorganic metal ions on a silicon substrate and removing the metal ions from the silicon substrate by a chemical solution treatment called SC-2 (standard cleaning (STANDARD CLEAN) 2). And, it may be preferably used in the case where ammonia is mixed for the purpose of removing particles on a silicon substrate, and silicon particles are removed from the silicon substrate by a chemical solution treatment called SC-1 (standard cleaning 1). The removal of the resist layer herein also includes removal of a resist film, an etching residue, an anti-reflection film and an ashing residue, wherein the etching residue is a residue generated when etching the resist layer, and the ashing residue is a residue generated when ashing the resist layer.
Furthermore, the composition of the present invention can be preferably used in applications other than semiconductor manufacturing. For example, the composition can be used as a cleaning solution, a stripping solution, or a removing solution for polyimide, a resist for sensor, a resist for lens, or the like.
The present invention can be used for cleaning other than the above, and can be preferably used for cleaning a container, a pipe, a substrate (for example, a wafer, glass, or the like), or the like. And, it is also possible to use a raw material for an organic peroxide or an inorganic peroxide; a raw material of an organic compound; a raw material of an epoxy compound; bleaching of paper, pulp, wood, etc.; a raw material for the fibers; bleaching the fibers; oxidizing agent of metal in the smelting process; raw materials for foods, medicines, etc.; in various applications such as cleaning agents and bactericides for manufacturing facilities and containers.
[ Composition Container ]
The composition container of the present invention comprises a storage container and the composition of the present invention contained in the storage container, wherein a region of the storage container in contact with the composition is formed of a material mainly composed of a non-metal. The main component herein means 80 mass% or more of the region where the predetermined component is in contact.
The form of the storage container is not particularly limited as long as the region in contact with the composition of the present invention is formed of a material mainly composed of a non-metal, and the storage container can be filled in any container for storage, transportation and use. The container is preferably a container having high cleanliness and less elution of impurities in the container for semiconductor applications. Examples of usable containers include "clean bottle" series manufactured by AICELLO CORPORATION, KODAMA PLASTICS co., ltd. The region of the container in contact with the composition of the present invention, for example, the inner wall of the housing portion or the flow path of the composition of the present invention is formed of a material mainly composed of a non-metal, and is preferably formed of a material selected from the group consisting of High Density Polyethylene (HDPE), tetrafluoroethylene perfluoroalkyl vinyl ether copolymer (PFA) and polytetrafluoroethylene (PTF E) from the viewpoint of preventing contamination of the dissolved matter from the container due to excessive affinity associated with the container. Among them, the resin is more preferably formed of a material having a contact angle with water of 60 to 120 ° and a nonmetallic component, and further preferably a fluorine-based resin (perfluoro resin). In particular, the use of a container in which the above-described region in contact with the composition of the present invention is a fluororesin is preferable because the occurrence of such a problem that ethylene or propylene oligomers are eluted can be suppressed as compared with the use of a container in which the region in contact with the composition of the present invention is a polyethylene resin, a polypropylene resin or a polyethylene-polypropylene resin.
Specific examples of the container in which the composition of the present invention is in contact with the fluororesin include, for example, entegris co., ltd. FluoroPurePFA composite barrels. Furthermore, containers described in page 4 and the like of Japanese patent application laid-open No. Hei 3-502677, page 3 and the like of International publication No. 2004/016526, page 9 and page 16 and the like of International publication No. 99/46309, and the like can also be used. These containers are preferably cleaned inside the container prior to filling. The liquid used for the cleaning is not particularly limited, and the metal content is preferably less than 0.001 mass ppt (megaly).
Further, according to the application, for example, the desired effect of the present invention can be remarkably obtained by using a liquid in which the metal content is in the above range by purifying other organic solvents in addition to the above water, a liquid in which the composition of the present invention is itself diluted or a liquid in which the composition of the present invention is further purified to further reduce the metal components, impurities, coarse particles, or the like, for cleaning.
Further, it is preferable to prevent the contamination of foreign matter from the lid by removing foreign matter adhering to the lid by cleaning the lid of various containers with an acid or an organic solvent before cleaning the containers.
The composition of the present invention may be stored in a container such as a gallon bottle or a coated bottle after being manufactured. The gallon bottle may be made of glass material or may be made of other materials.
When the composition of the present invention is stored, the inside of the container may be replaced with an inert gas (nitrogen, argon, or the like) having a purity of 99.99995% by volume or more in order to prevent the change of the components in the composition during storage. In particular, a gas having a small water content is preferable. The temperature is not particularly limited in transportation or storage, and the temperature may be controlled within a range of-20 ℃ to 20 ℃ in order to prevent deterioration.
Examples
Hereinafter, the present invention will be described in more detail with reference to examples. The materials, amounts used, ratios, treatment contents, treatment steps and the like shown in the following examples can be appropriately changed without departing from the gist of the present invention. Accordingly, the scope of the present invention should not be construed as being limited by the examples shown below.
< Purification of raw materials etc. >)
The raw materials and catalysts used in the examples shown below were purified by distillation, ion exchange, filtration, and the like, using a high purity grade having a purity of 99% or more.
The ultrapure water used in the examples was purified by the method described in Japanese patent application laid-open No. 2007-254168, and the atomic content of each of Na, ca and Fe was set to less than 10 mass ppt by measurement by the ordinary ICP-MS method described later.
The compositions of examples and comparative examples (hereinafter also referred to as "hydrogen peroxide compositions") were prepared, filled, stored, and analyzed and measured in clean rooms satisfying the ISO 2 level or less. The container to be used is used after being cleaned in advance with the composition of the present invention. In order to improve the measurement accuracy, in the measurement of the metal component content and the measurement of the water content, the measurement is performed by concentrating the metal component content and the water content to 1 in volume conversion to 100 minutes in the measurement of the detection limit or less in the normal measurement, and the content calculation is performed by converting the metal component content and the water content into the concentration of the composition before concentration.
Example 1
[ Preparation of Hydrogen peroxide composition ]
The hydrogen peroxide composition was prepared by performing the following steps 1 to 4. (step 1: raw material purification step)
In step 1, 2-ethylanthraquinone as a raw material is passed through a cation exchange resin packed in a column, and the process is repeated until the concentration of metal ions contained in the raw material becomes 1 mass ppm. Then, 2-ethylanthraquinone was isolated.
(Step 2: hydrogen peroxide Synthesis step)
To a solution obtained by dissolving 2-ethyl anthraquinone in benzene, a Pt catalyst was added, thereby obtaining a suspension. Next, 2-ethylanthraquinone is hydrogenated in the presence of Pt catalyst by contacting hydrogen with the resulting suspension, thereby producing 2-ethylanthrahydroquinone. In addition, the catalyst was removed by filtering the resulting composition.
Then, 2-ethylanthrahydroquinone is oxidized by bringing oxygen in the air into contact with the obtained composition, thereby producing 2-ethylanthraquinone and hydrogen peroxide.
(Step 3: hydrogen peroxide separation step)
The hydrogen peroxide produced in the step 2 is extracted with water and separated to obtain an aqueous hydrogen peroxide solution (hydrogen peroxide composition).
(Step 4: purification step of Hydrogen peroxide composition)
After the step 3, the aqueous hydrogen peroxide solution was purified by a cation exchange resin. This removes metal components containing atoms such as aluminum, potassium, magnesium, sodium, and the like contained in the aqueous hydrogen peroxide solution. As the cation exchange resin, a strongly acidic cation exchange resin having a sulfonic acid group (-SO 3 H) as an ion exchange group is used. In the conventional process, the concentration of metal ions contained in the aqueous hydrogen peroxide solution is about 1 ppb by mass. Then, the obtained aqueous hydrogen peroxide solution is filtered using a PTFE (polytetrafluoroethylene) filter having an average pore diameter of 0.001 to 0.01 μm or less, and the metal atom concentration is further reduced. Then, phosphoric acid is added to the aqueous hydrogen peroxide solution. The aqueous hydrogen peroxide solution is then contacted with a mixed bed of anion exchange resin and cation exchange resin. Thus, the metal ion concentration in the aqueous hydrogen peroxide solution was confirmed to be ppt.
[ Evaluation ]
Subsequently, the obtained aqueous hydrogen peroxide solution (hydrogen peroxide composition) was subjected to various evaluations shown below.
(Determination of Fe component in composition)
In the ICP-MS analysis (normal ICP-MS analysis is shown, and not SNP-ICP-MS analysis), the concentration of each atom was measured in the same manner as in the SNP-ICP-MS analysis described later except that the analysis software was replaced with that of an ICP-MS analysis device described later.
In addition, the amount of Fe particles in the Fe component is measured by SNP-ICP-MS analysis described later, and the amount of Fe ions can be calculated by subtracting the amount of Fe particles measured by SNP-ICP-MS analysis from the amount of Fe component (total metal amount) measured by ICP-MS analysis.
(SNP-ICP-MS (Single nanoparticle-inductively coupled plasma Mass Spectrometry) measurement)
Determination of Fe particle content
The content of Fe particles was measured using Perkinelmer co., ltd. System "Nexion S".
1) Preparation of standard substance
The standard substance was added by metering ultrapure water into a clean glass vessel so that the concentration of 10000 particles per ml of the metal particles to be measured having a median particle diameter of 50nm was attained, and then the dispersion obtained by treatment with an ultrasonic cleaner for 30 minutes was used as the standard substance for measuring the transport efficiency.
2) Measurement conditions
The measurement object liquid was aspirated at about 0.2mL/min using a coaxial atomizer made of PFA (in addition, "PFA" means a copolymer of tetrafluoroethylene and perfluoroalkyl vinyl ether), a cyclone spray chamber made of quartz, and a torch syringe (To rch Injector) made of quartz having an inner diameter of 1 mm. The oxygen addition was 0.1L/min, the plasma output was 1600W, and the cell cleaning was performed with ammonia gas. Analysis was performed at a time resolution (time resolut ion) of 50 mus.
3) The content of Fe particles was measured using the following analysis software attached to the manufacturer.
Content of Fe particles: syngistix nanometer application module special for SNP-ICP-MS of nanoparticle analysis
4) The content of Fe atoms was measured using the following analysis software (ICP-MS analysis) attached to the manufacturer.
Content of Fe atoms: syngistix was used for ICP-MS software.
(Determination of the Metal Components derived from other specific atoms (Ni, pt, pd, cr, ti and Al) in the composition)
For measurement, agilent 8800 triple quadrupole ICP-MS (option #200 for semiconductor analysis) was used. According to the above measuring apparatus, the ionic metal and the nonionic metal in each measurement sample can be classified and the content of each can be measured. The sum of the content of the ionic metal and the content of the nonionic metal corresponds to the total metal amount.
Measurement conditions
The sample introduction system used a quartz torch and a coaxial PFA (perfluoroalkoxyalkane) atomizer (for self priming) and a platinum interface cone (Platinum interface cone). The measurement parameters of the cold plasma conditions are as follows.
RF (Radio Frequency) output (W): 600
Carrier gas flow (L/min): 0.7
Make-up gas flow (L/min): 1
Sampling depth (mm): 18
(Determination of acids and anthraquinones in the composition)
The acid or anthraquinone compound in the composition was measured by the following method.
The measurement was performed by liquid chromatography (ion exchange chromatography mass spectrometry) using an ion exchange resin in a stationary phase and an aqueous electrolyte solution in a mobile phase (a solution). Ion chromatography mass spectrometry (IC-MS) is a method in which a mass spectrometer is connected as an IC detector. Mass spectrometers use electrospray ionization (electrospray ionization) method (ESI) for ionization and tandem mass spectrometers for mass spectrometry because mass/charge (m/z) separation is performed. Further, the separated molecular ions are split in a Collision cell (collisioncell), and the resultant product ions (reflecting the structure of the molecular ions) are detected.
(Evaluation of storage stability of Hydrogen peroxide composition)
The hydrogen peroxide composition immediately after preparation was titrated by a known method using potassium iodide and sodium thiosulfate, and the hydrogen peroxide amount of the immediately after preparation hydrogen peroxide composition was measured. The hydrogen peroxide composition was left to stand at 25℃for 1 week and then stored, and then the amount of hydrogen peroxide (residual amount) in the hydrogen peroxide composition was determined by the same method as described above.
Next, the decomposition rate was calculated by the following formula, and the storage stability was evaluated.
(Decomposition rate) = [ amount of hydrogen peroxide composition immediately after preparation) - (residual amount of hydrogen peroxide composition after storage with time ]/(amount of hydrogen peroxide composition immediately after preparation) ×100
The evaluation criteria are as follows. In the following criteria, if the evaluation is "D" or more, the storage stability is practically required, and "C" or more is preferable.
"A": the decomposition rate of hydrogen peroxide is less than 5%
"B": the decomposition rate of hydrogen peroxide is more than 5% and less than 10%
"C": the decomposition rate of hydrogen peroxide is more than 10% and less than 20%
"D": the decomposition rate of hydrogen peroxide is more than 20% and less than 30%
"E": the decomposition rate of hydrogen peroxide is above 30%
(Evaluation of oxidizing Activity of Hydrogen peroxide composition)
The oxidation potential (oxidizing power) of the hydrogen peroxide composition was determined electrochemically. The OCP (open circuit potential (Open Cirkit Potential)) at this time was obtained using the hydrogen electrode as a reference electrode.
The evaluation criteria are as follows.
"A": the oxidation force is more than 1.8mV
"B": the oxidation force is 1.6mV or more and less than 1.8mV
"C": oxidizing power of less than 1.6mV
(Defect Performance of Hydrogen peroxide composition (measurement of the number of defects adhering to a semiconductor substrate))
The number of particles having a diameter of 32nm or more (hereinafter, also referred to as "defects") present on the surface of a 300mm diameter silicon oxide film substrate was measured by a surface inspection apparatus (SP-5; manufactured by KLA Tencor). Next, the silicon oxide film substrate was set in a spin-on device, and the obtained hydrogen peroxide composition was sprayed onto the surface of the silicon oxide film substrate at a flow rate of 1.5L/min while rotating the substrate. Then, rinsing treatment is performed and drying is performed. The number of defects existing on the surface of the silicon oxide film substrate was measured again using the above-described apparatus (SP-5) for the obtained sample, and the difference from the initial value was used as the number of defects. The results of evaluating the number of defects obtained based on the following criteria are shown in table 1. In the following criteria, if the evaluation is "C" or more, the defect suppression capability required as a treatment liquid for semiconductor device manufacturing is achieved.
"A": the number of defects is 0 to 50
"B": the number of defects exceeds 50 and is 100 or less
"C": the number of defects exceeds 100 and is less than 500
"D": the number of defects exceeds 500 and is less than 1000
"E": the defect number exceeds 1000
Examples 2 to 23, comparative example 1, comparative example 2 >, and
The hydrogen peroxide compositions of examples 2 to 23, comparative examples 1 and comparative example 2 were prepared by changing the preparation method and the materials of the hydrogen peroxide composition of example 1 so as to obtain the hydrogen peroxide compositions having the compositions shown in table 1 below, and the same evaluation was performed. The results are shown in Table 1.
In Table 1, for example, 10 (-1) represents "10 to the power of-1" (0.1). And, for example, 10≡1 represents "1 th power of 10" (10).
The "acid" in table 1 includes a phthalic acid derivative produced as a decomposition product of anthraquinone in addition to phosphoric acid added in step 4.
The total metal amount is indicated for each metal component in columns (D) and (E) in table 1.
Table 2 shows the composition of the metal components in table 1, specifically, the metal ions (ionic metals) and the metal particles (nonionic metals) are shown separately. In table 2, the metal particles (nonionic metals) are various metal particles measured by "SNP-ICP-MS".
From the results of table 1, it was confirmed that the hydrogen peroxide composition according to the example was excellent in storage stability and less affected by defects of the semiconductor substrate when applied to the manufacturing process of the semiconductor device.
Further, according to the comparison of example 1, examples 9, 10, 11 and comparative example 2, it was confirmed that when the content of the Fe component was 0.1 to 1 ppb by mass (preferably 0.1 to 800 ppt by mass, more preferably 0.1 to 500 ppt by mass) relative to the total mass of the composition, the effect of excellent storage stability and less influence on defects of the semiconductor substrate when applied to the manufacturing process of the semiconductor device could be achieved at an excellent level, and the oxidizing power was also more excellent.
Further, according to comparison of example 1, examples 6, 7, 8 and comparative example 1, it was confirmed that when the content of the acid is 0.01 to 1000 ppb by mass (preferably 0.05 to 800 ppb by mass, more preferably 0.05 to 500 ppb by mass) relative to the total mass of the composition, the effect of excellent storage stability and less influence on defects of the semiconductor substrate when applied to the manufacturing process of the semiconductor device can be achieved at an excellent level.
Further, it was confirmed from the comparison of examples 1 and examples 2 to 5 that when the anthraquinone compound is contained, if the content of the anthraquinone compound is 0.01 to 1000 ppb by mass (preferably 0.05 to 800 ppb by mass, more preferably 0.05 to 500 ppb by mass) relative to the total mass of the composition, the defect influence on the semiconductor substrate is further small when the composition is applied to the manufacturing process of the semiconductor device.
Further, according to comparison of example 1, example 12, and example 13, it was confirmed that when a metal component containing a specific atom selected from the group consisting of Ni, pt, pd, cr, ti and Al is contained, if the content of the metal component is 0.01 to 1 ppb by mass (preferably 0.01 to 800 ppt by mass, more preferably 0.01 to 500 ppt by mass) per each specific atom relative to the total amount of the composition, the defect influence on the semiconductor substrate is further small when the composition is applied to the manufacturing process of the semiconductor device.
Further, according to the results of examples, it was confirmed that when the content of the Fe component relative to the content of the acid was 10 -3～10-1 in terms of mass ratio, the storage stability was excellent, and the influence of defects on the semiconductor substrate was small when applied to the manufacturing process of the semiconductor device, and the oxidizing power was further excellent.
Further, according to the results of examples, it was confirmed that when the metal component containing a specific metal atom selected from the group consisting of Ni atom, pt atom, pd atom, cr atom, ti atom and Al atom contains metal particles, if the content of the metal particles is 0.01 mass ppt to 500 mass ppt (preferably 0.01 mass ppt to 100 mass ppt, more preferably 0.01 mass ppt to 50 mass ppt) each independently with respect to the total amount of the composition, the defect influence on the semiconductor substrate is further small when the composition is applied to the manufacturing process of the semiconductor device.
On the other hand, the hydrogen peroxide composition of the comparative example had a result that the storage stability and the defect influence on the semiconductor substrate could not be simultaneously achieved.
Examples A1 to A3
The hydrogen peroxide composition of example 1 was added to a storage container having a region in contact with the hydrogen peroxide composition as a component in table 3, and after storage at 25 ℃ for 1 month, SNP-ICP-MS was measured and defect performance was evaluated. The SNP-ICP-MS and the defect performance evaluation and measurement method were the same as in example 1. The results are shown in Table 3. The concentration of each metal component shown in columns A1 to A3 of examples A3 in table 3 below represents the concentration after storage. In Table 3, the object to be measured in "SNP-ICP-MS" is Fe particles.
In addition, the contact angle with the container was measured by a contact angle meter DM-901 (Kyowa INTERFACE SCIENCE co., ltd.).
In the table, PFA represents a tetrafluoroethylene perfluoroalkyl vinyl ether copolymer, and PTFE represents polytetrafluoroethylene.
TABLE 3
From the results of table 3, it was confirmed that the defect performance was excellent even after long-term storage by storing the hydrogen peroxide composition in a storage container in which the region in contact with the hydrogen peroxide composition was formed of a material mainly composed of a non-metal.
Examples B1 to B7
The hydrogen peroxide compositions of examples B1 to B7, and the hydrogen peroxide compositions of examples B5, B6 and B7, in which only the hydrogen peroxide concentration (mass%) of the hydrogen peroxide composition of example 1 was changed to the hydrogen peroxide concentration (mass%) shown in table 4, were mixed with sulfuric acid water (sulfuric acid concentration (mass%) shown in table 4) at the mixing ratio (mass ratio) shown in table 4, and the resist stripping test was performed under the conditions shown in table 4 below. The resist layer of the test object is shown below.
(Resist stripping test)
Test wafer: a film of PMER P-CA1000PM (positive resist manufactured by TOK) was formed on a silicon wafer, and the stripping ability with respect to the resist was evaluated under the following conditions.
Amount of chemical solution: 200ml.
Wafer size: 3cm by 3cm
The processing method: immersing the wafer in the liquid medicine
Treatment time 1min
In table 4, in examples B1 to B4, sulfuric acid water was heated to 90 ℃ in advance and then mixed with a hydrogen peroxide composition. In examples B5 to B7, sulfuric acid water was heated to 65℃in advance and then mixed with a hydrogen peroxide composition. In any of the examples, the hydrogen peroxide composition and sulfuric acid water were mixed, and then heated to a "treatment temperature", and then used for a resist layer peeling test.
The resist peelability was determined based on the following evaluation criteria.
"A": the resist removal of 100% was shown by visual inspection.
"B": the resist layer removing property of 90% or more and less than 100% is shown by visual observation.
"C": less than 90% resist removal was exhibited under visual inspection.
TABLE 4
| Hydrogen peroxide water | Sulfuric acid water | Mixing ratio | Treatment temperature (. Degree. C.) | Resist stripping ability | |
| Example B1 | 30％ | 98％ | 1:1 | ＞150 | A |
| Example B2 | 30％ | 98％ | 2:1 | ＞150 | A |
| Example B3 | 30％ | 98％ | 3:1 | ＞150 | A |
| Example B4 | 30％ | 98％ | 1:1 | ＞100 | A |
| Example B5 | 15％ | 50％ | 1:1 | 60 | B |
| Example B6 | 10％ | 50％ | 1:1 | 60 | C |
| Example B7 | 3％ | 50％ | 1:1 | 60 | C |
From the results of table 4 above, it was confirmed that the hydrogen peroxide composition of the present invention can be preferably used in SPM treatment.
Examples C1 to C5 and comparative example 3
Hydrogen peroxide water (hydrogen peroxide compositions of examples C1 to C3, and hydrogen peroxide compositions of examples C4 to C5, wherein only the hydrogen peroxide concentration (mass%) of the hydrogen peroxide composition of example 1 was changed to the hydrogen peroxide concentration (mass%) shown in table 5) and ammonia water (ammonia concentration (mass%) shown in table 5) were mixed at the mixing ratio (mass ratio) shown in table 5, and the particle removal test on the Si substrate was performed under the following conditions. The aqueous ammonia used in this example was high-purity aqueous ammonia having a total metal concentration of 10 mass ppt or less. The hydrogen peroxide composition used in comparative example 3 was the hydrogen peroxide composition of comparative example 2 in table 1.
In addition, in any of the examples, the hydrogen peroxide composition and ammonia water were mixed, heated until the temperature became "treatment temperature", and then used in the particle removal treatment.
Particle removal test
Each chemical solution was applied to a TEOS (tetraethyl orthosilicate) substrate, and the number of defects before and after the treatment was counted in a measurement mode of a bright field (brightfield) of UVison (APPLIE D MATERIALS, inc.). In this count, EDAX (elemental analysis) was evaluated for defect classification, and the number of defects containing Si was set as the total particles. The total particle count on the TEOS substrate before measurement was 200.
The particle removability was determined based on the following evaluation criteria.
"A": the total particle number is below 50
"B": the total particle number exceeds 50 to 100
"C": the total particle number exceeds 100 to 200
"D": total particle count exceeding 200
TABLE 5
| Hydrogen peroxide water | Ammonia water | Mixing ratio | Treatment temperature (. Degree. C.) | Particle removability | |
| Example C1 | 30％ | 30％ | 1:1 | 60 | A |
| Example C2 | 30％ | 30％ | 2:1 | 60 | A |
| Example C3 | 30％ | 30％ | 3:1 | 60 | A |
| Example C4 | 10％ | 10％ | 1:1 | 45 | B |
| Example C5 | 3％ | 3％ | 1:1 | 35 | C |
| Comparative example 3 | 30％ | 30％ | 1:1 | 60 | D |
From the results of Table 5, it was confirmed that the hydrogen peroxide composition of the present invention was excellent in particle removability when SC-1 treatment was performed.
Examples D1 to D6 and comparative example 4
Hydrogen peroxide water (hydrogen peroxide compositions of example 1 were used in examples D1 to D6. Hydrogen peroxide compositions of example 1 were used in examples D5 to D6, and only the hydrogen peroxide concentration (mass%) of the hydrogen peroxide composition was changed to the hydrogen peroxide concentration (mass%) shown in table 6), and hydrochloric acid water (hydrochloric acid concentration (mass%) shown in table 6) were mixed at the mixing ratio (mass ratio) shown in table 6, and a metal removal test on a Si substrate was performed under the following conditions.
The hydrochloric acid water used in this example was high-purity hydrochloric acid water having a total metal concentration of 10 mass ppt or less. The hydrogen peroxide composition used in comparative example 4 was the hydrogen peroxide composition of comparative example 2 in table 1.
In addition, in any of the examples, after mixing the hydrogen peroxide composition and the aqueous ammonia, heating was performed until the temperature reached the "treatment temperature", and then the mixture was used as a metal ion removal treatment liquid.
Metal ion removal test
Each chemical solution was applied to a TEOS substrate, and then the number of defects before and after the treatment was counted in a light field measurement mode of UVison (APPLIED MATERIALS, inc.). EDAX (elemental analysis) was evaluated for defect classification in this count, and the number of defects containing metal atoms other than Si was set as the total metal ion composition number. The metal ion composition on the TEOS substrate before measurement was 50.
Regarding the metal ion removability, a determination was made based on the following evaluation criteria.
"A": the metal ion content is below 20
"B": more than 20 to 30 metal ion components
"C": more than 30 to 50 metal ion components
"D": more than 50 metal ion components
TABLE 6
| Hydrogen peroxide water | Hydrochloric acid water | Mixing ratio | Treatment temperature (. Degree. C.) | Metal ion removability | |
| Example D1 | 30％ | 37％ | 1:1 | ＞150 | A |
| Example D2 | 30％ | 37％ | 2:1 | ＞150 | A |
| Example D3 | 30％ | 37％ | 3:1 | ＞150 | A |
| Example D4 | 30％ | 37％ | 1:1 | ＞100 | A |
| Example D5 | 15％ | 10％ | 1:1 | 60 | B |
| Example D6 | 3％ | 3％ | 1:1 | 60 | C |
| Comparative example 4 | 30％ | 30％ | 1:1 | 60 | D |
From the results of Table 6, it was confirmed that the metal ion-removing property was excellent when SC-2 treatment was performed using the hydrogen peroxide composition of the present invention.
Examples E1 to E4
The reference solution (which is a pre-purification solution corresponding to "before treatment" in table 7) was subjected to the filtration test shown in table 7 below, and the total metal concentration of each metal (Fe component, pt component) after filtration and the amount of Fe particles measured by SNP-ICP-MS were confirmed. The reference liquid was prepared by changing the preparation method of the hydrogen peroxide composition of example 1 so as to obtain a hydrogen peroxide composition having a composition "before treatment" shown in table 7 below. In each example, each composition described above represents a composition purified by the filtration step described in table 7. That is, for example, in example E1, the hydrogen peroxide composition before treatment was filtered with nylon (pore size: 5 nm) described in Table 7, and the results showed that the content of the anthraquinone compound (B) was 0.1 ppb by mass, the acid concentration was 0.1 ppb by mass, the Fe component concentration was 31 ppt by mass, and the Pt component concentration was 8 ppt by mass. The results are shown in Table 7.
TABLE 7
From the results of table 7, it was confirmed that the use of a filter made of a fluorine-based resin such as PTFE or PTA effectively reduced the amount of metal components.
Symbol description
100. 200-Manufacturing device, 101-tank, 102-supply port, 103, 106, 107-valve, 104-pump, 105-filter device, 108-vessel, 109-supply line, 110-circulation line, 111-discharge, 112-cleaning liquid monitoring section, 113-line, 201-distillation column, 202, 203, 204-line, 205, 206, 207-valve.
Claims (13)
1. A composition comprising hydrogen peroxide, an acid and an Fe component,
The content of the Fe component relative to the content of the acid is 10 -5～102 in terms of mass ratio,
The acid is 1 selected from phosphoric acid and phosphoric acid derivatives,
The composition also contains anthraquinone compounds,
The content of the anthraquinone compound is 0.01 to 1000 ppb by mass relative to the total mass of the composition.
2. The composition of claim 1, wherein,
The content of the acid is 0.01 to 1000 ppb by mass relative to the total mass of the composition.
3. The composition according to claim 1 or 2, wherein,
The total content of the Fe component is 0.1 to 1 ppt by mass relative to the total mass of the composition.
4. The composition according to claim 1 or 2, wherein,
The content of Fe particles contained in the Fe component is 0.01 to 0.1 ppb by mass relative to the total mass of the composition.
5. The composition according to claim 1 or 2, further comprising at least 1 or more metal component containing a specific atom selected from Ni, pt, pd, cr, ti and Al,
The content of the metal component is 0.01 ppt to 10 ppb by mass relative to the total mass of the composition, per each specific atom.
6. The composition according to claim 1 or 2, further comprising at least 1 or more metal component containing a specific atom selected from Ni, pt, pd and Al,
The content of the metal component is 0.01 to 1 ppt by mass based on the total mass of the composition.
7. The composition of claim 1, wherein,
The anthraquinone compound is at least 1 selected from alkyl anthraquinone and alkyl tetrahydroanthraquinone.
8. The composition of claim 7, wherein,
The alkyl anthraquinone is ethyl anthraquinone or amyl anthraquinone, and the alkyl tetrahydroanthraquinone is ethyl tetrahydroanthraquinone or amyl tetrahydroanthraquinone.
9. The composition according to claim 1 or 2, which is used as a treatment liquid for a semiconductor substrate.
10. A composition container comprising a storage container and the composition according to any one of claims 1 to 9 contained in the storage container,
The region of the storage container in contact with the composition is formed of a material having a nonmetallic component as a main component.
11. The composition container according to claim 10, wherein,
The material with nonmetal as the main component is 1 selected from high-density polyethylene, tetrafluoroethylene perfluoroalkyl vinyl ether copolymer and polytetrafluoroethylene.
12. The composition container according to claim 10 or 11, wherein,
The contact angle of the material with water, which takes the nonmetal as a main component, is 60-120 degrees.
13. A method for producing the composition according to any one of claims 1 to 9, comprising:
A raw material purification step of purifying 1 or more of the raw material components selected from the group consisting of a solvent and an anthraquinone compound;
a hydrogen peroxide synthesis step of synthesizing an anthrahydroquinone compound by reducing the anthraquinone compound in the presence of a catalyst, and further oxidizing the anthrahydroquinone compound to synthesize hydrogen peroxide;
a hydrogen peroxide separation step of extracting the hydrogen peroxide obtained by the extraction step to remove the hydrogen peroxide from the reaction system; and
And a hydrogen peroxide composition purification step of further purifying a hydrogen peroxide composition containing hydrogen peroxide separated from the reaction system.
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| KR20080016808A (en) * | 2005-05-19 | 2008-02-22 | 미츠비시 가스 가가쿠 가부시키가이샤 | Aqueous hydrogen peroxide for sterilization |
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| GB1222734A (en) * | 1968-07-25 | 1971-02-17 | Fmc Corp | Purification and stabilization of hydrogen peroxide |
| JP2629507B2 (en) * | 1991-01-14 | 1997-07-09 | 住友化学工業株式会社 | Purification method of hydrogen peroxide solution |
| FI924124A (en) * | 1991-09-19 | 1993-03-20 | Ube Industries | FOERFARANDE FOER RENING AV VAETEPEROXIDVATTENLOESNING |
| JP2608825B2 (en) * | 1991-09-19 | 1997-05-14 | 宇部興産株式会社 | Purification method of aqueous hydrogen peroxide solution |
| JP2687194B2 (en) * | 1991-11-26 | 1997-12-08 | 宇部興産株式会社 | Purification method of hydrogen peroxide solution |
| JP4232002B2 (en) * | 2003-01-16 | 2009-03-04 | 日本電気株式会社 | Cleaning composition for device substrate, cleaning method and cleaning apparatus using the cleaning composition |
| JP5031334B2 (en) * | 2006-11-17 | 2012-09-19 | 三徳化学工業株式会社 | Method and apparatus for purifying hydrogen peroxide water |
| US20100105595A1 (en) * | 2008-10-29 | 2010-04-29 | Wai Mun Lee | Composition comprising chelating agents containing amidoxime compounds |
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| KR20080016808A (en) * | 2005-05-19 | 2008-02-22 | 미츠비시 가스 가가쿠 가부시키가이샤 | Aqueous hydrogen peroxide for sterilization |
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