CN102628009B - Scavenging solution and purging method - Google Patents
Scavenging solution and purging method Download PDFInfo
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- CN102628009B CN102628009B CN201210019335.9A CN201210019335A CN102628009B CN 102628009 B CN102628009 B CN 102628009B CN 201210019335 A CN201210019335 A CN 201210019335A CN 102628009 B CN102628009 B CN 102628009B
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- Prior art keywords
- scavenging solution
- ammonium
- tetramethyl
- cerium oxide
- composition
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- 230000002000 scavenging effect Effects 0.000 title claims abstract description 135
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000010926 purge Methods 0.000 title claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 64
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 50
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 50
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims abstract description 29
- 150000003863 ammonium salts Chemical class 0.000 claims abstract description 26
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 24
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims abstract description 22
- 235000011130 ammonium sulphate Nutrition 0.000 claims abstract description 22
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 12
- KJFVITRRNTVAPC-UHFFFAOYSA-L tetramethylazanium;sulfate Chemical compound C[N+](C)(C)C.C[N+](C)(C)C.[O-]S([O-])(=O)=O KJFVITRRNTVAPC-UHFFFAOYSA-L 0.000 claims abstract description 12
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims abstract description 10
- -1 cerium ion Chemical class 0.000 claims abstract description 10
- KUCWUAFNGCMZDB-UHFFFAOYSA-N 2-amino-3-nitrophenol Chemical compound NC1=C(O)C=CC=C1[N+]([O-])=O KUCWUAFNGCMZDB-UHFFFAOYSA-N 0.000 claims abstract description 8
- OKIZCWYLBDKLSU-UHFFFAOYSA-M N,N,N-Trimethylmethanaminium chloride Chemical compound [Cl-].C[N+](C)(C)C OKIZCWYLBDKLSU-UHFFFAOYSA-M 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims description 72
- 239000000758 substrate Substances 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000013543 active substance Substances 0.000 claims description 14
- 239000004065 semiconductor Substances 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 239000011521 glass Substances 0.000 claims description 5
- 239000010453 quartz Substances 0.000 claims description 5
- 239000003960 organic solvent Substances 0.000 claims description 3
- 239000003002 pH adjusting agent Substances 0.000 claims description 3
- 239000003352 sequestering agent Substances 0.000 claims description 3
- 239000000919 ceramic Substances 0.000 claims description 2
- 239000000243 solution Substances 0.000 description 115
- 238000004140 cleaning Methods 0.000 description 35
- 230000000052 comparative effect Effects 0.000 description 25
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 18
- 230000000694 effects Effects 0.000 description 15
- 238000002156 mixing Methods 0.000 description 15
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 14
- 230000002829 reductive effect Effects 0.000 description 14
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 13
- 229910052710 silicon Inorganic materials 0.000 description 13
- 239000010703 silicon Substances 0.000 description 13
- 239000007788 liquid Substances 0.000 description 11
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 description 10
- 238000000227 grinding Methods 0.000 description 10
- 239000007864 aqueous solution Substances 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 7
- 239000012528 membrane Substances 0.000 description 6
- 239000007769 metal material Substances 0.000 description 6
- 238000012544 monitoring process Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 239000002002 slurry Substances 0.000 description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 5
- 239000004411 aluminium Substances 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 5
- 239000010936 titanium Substances 0.000 description 5
- 229910052719 titanium Inorganic materials 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 4
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 239000007858 starting material Substances 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 229910021642 ultra pure water Inorganic materials 0.000 description 3
- 239000012498 ultrapure water Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- MNWFXJYAOYHMED-UHFFFAOYSA-N heptanoic acid Chemical compound CCCCCCC(O)=O MNWFXJYAOYHMED-UHFFFAOYSA-N 0.000 description 2
- 229960002050 hydrofluoric acid Drugs 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 2
- 229920005591 polysilicon Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 2
- 241000282326 Felis catus Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 229920013701 VORANOL™ Polymers 0.000 description 1
- 150000007933 aliphatic carboxylic acids Chemical class 0.000 description 1
- 150000005215 alkyl ethers Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 239000005388 borosilicate glass Substances 0.000 description 1
- 150000007516 brønsted-lowry acids Chemical class 0.000 description 1
- 150000007528 brønsted-lowry bases Chemical class 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 230000000875 corresponding effect Effects 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 125000003187 heptyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000003973 irrigation Methods 0.000 description 1
- 230000002262 irrigation Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000005360 phosphosilicate glass Substances 0.000 description 1
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000005368 silicate glass Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- DGCPSAFMAXHHDM-UHFFFAOYSA-N sulfuric acid;hydrofluoride Chemical compound F.OS(O)(=O)=O DGCPSAFMAXHHDM-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/046—Salts
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
-
- C11D2111/18—
-
- C11D2111/22—
Abstract
The present invention relates to a kind of scavenging solution and purging method.The object of this invention is to provide cleaned material surface attachment being had to cerium oxide, this cerium oxide can be dissolved with the form of cerium ion and clean the scavenging solution of removing and use the purging method of this scavenging solution.A kind of scavenging solution, it is characterized in that, the cerium oxide of this scavenging solution removing cleaned material remained on surface, this scavenging solution contains (1) hydrogen fluoride and (2) ammonium salt, and described ammonium salt is selected from least a kind in ammonium chloride, ammonium nitrate, ammonium sulfate, tetramethyl ammonium chloride, tetramethyl-ammonium nitrate and tetramethyl-ammonium sulfate.
Description
Technical field
The present invention relates to the cleaned material for being attached with cerium oxide, by the scavenging solution of this cerium oxide cleaning removing, and the purging method of this scavenging solution can be used.
Background technology
For the purpose of the high-performance realizing large-scale integrated circuit (ULSI), just in the miniaturization of advancing circuit design.Fine to nano level very fine circuit structure in order to be formed, not yet in a lot of manufacturing process, become necessary by the new manufacture be suitable for so far.
Particularly, as the most important operation forming microtexture on a semiconductor substrate, have employ optical means exposure, developing procedure.In order to make this microtexture, same uniform focusing is closely related with the flatness of substrate surface on the surface of the semiconductor substrate.That is, when the flatness of substrate surface is poor, occur the part of focusing and the part not having focusing on the surface of the substrate, do not having the part of focusing can not form desired microtexture, the decline of productivity becomes greatly.In addition, along with the development of miniaturization, the allowable range relevant to flatness diminishes, and improves further the smooth requirement of substrate surface.
In addition, except smooth requirement, also has the requirement of the shortening activity time for the purpose of enhancing productivity.Therefore, the technology also making the high speed of operation become possible except the working accuracy of microfabrication is needed.Because of so technical background, as the technology guaranteeing flatness, generally carry out cmp (CMP).In CMP operation, limit supply abrasive (slurry) lateral dominance grinding pad grinding (leveling) semiconductor substrate surface containing granular grinding abrasive particle.
In above-mentioned CMP operation, widely use silica slurry as abrasive, also use ceria sizing agent, identical with the situation of silica slurry, need the matting for removing the residue remaining in substrate surface.As the clean-out system used in matting, such as, propose following clean-out system.
In patent documentation 1, propose the cleaning liquid containing acid, reductive agent and these 3 kinds of compositions of fluorion.
In patent documentation 2, propose the scavenging solution be made up of hydrofluoric acid and sulfuric acid or nitric acid or phosphoric acid.
But, although scavenging solution in the past can remove the residue of cerium oxide, owing to taking acid as principal constituent, so there is the problem that easily the various metallic substance of corrosion is such.Such as, if the metallic membrane on semiconductor substrate dissolves due to corrosion, then the thickness of metallic membrane reduces and the sheet resistance value of metallic membrane becomes large.Thus, the resistance value of the distribution on unicircuit becomes large and the electric power that increases consumption, therefore not preferred.
Patent documentation 1: Japanese Unexamined Patent Publication 2004-59419 publication
Patent documentation 2: Japanese Unexamined Patent Publication 2000-140778 publication
Summary of the invention
The object of this invention is to provide the cleaned material that effects on surface is attached with cerium oxide, this cerium oxide can be dissolved and cleaning removing with the form of cerium ion, and be difficult to corrode the scavenging solution of various metallic substance and use its purging method.
The present inventor etc. in order to solve above-mentioned problem in the past, to scavenging solution and use its purging method to be studied.Consequently, find, by the scavenging solution used containing hydrogen fluoride and specific ammonium salt, the cerium oxide of cleaned material remained on surface to be cleaned removing effectively, thus complete the present invention.
That is, the present invention relates to a kind of scavenging solution, it is characterized in that, the removing of this scavenging solution residues in the cerium oxide on cleaned material surface, and this scavenging solution contains:
(1) hydrogen fluoride, and
(2) ammonium salt, this ammonium salt is selected from least a kind in ammonium chloride, ammonium nitrate, ammonium sulfate, tetramethyl ammonium chloride, tetramethyl-ammonium nitrate and tetramethyl-ammonium sulfate.
By containing hydrogen fluoride in scavenging solution, cerium oxide can be dissolved with the form of cerium ion, but the cerium ion dissolved is attached to the surface of cleaned material again again with the form of impurity, result is difficult to removing cerium composition.The present inventor etc. find by making specific ammonium salt be contained in together with hydrogen fluoride in scavenging solution, can make the cerium ion of dissolving with dissolved state stabilization in scavenging solution, thus effectively can remove from cleaned material surface.In addition, scavenging solution of the present invention is sour for main component with sulfuric acid, nitric acid or phosphoric acid etc. unlike scavenging solution in the past, so can suppress the corrosion of various metallic substance.Should illustrate, so-called cerium ion refers to Ce
3+, Ce
4+, their hydrate or their complex ion.
Hydrofluoric concentration in scavenging solution is preferably 0.001 ~ 5 % by weight.When hydrofluoric concentration is less than 0.001 % by weight, the trend that the solubility property that there is cerium oxide reduces.On the other hand, during more than 5 % by weight, there is the roughness that cleaned material is subject to etch or burn into or flattens by grinding smooth cleaned material surface and become large trend.In addition, after clean, when being undertaken innoxious by the hydrogen fluoride become in the scavenging solution of draining, the expense required for it and time increase.
The concentration of the above-mentioned ammonium salt in scavenging solution is preferably 0.1 ~ 20 % by weight.When the concentration of above-mentioned ammonium salt is less than 0.1 % by weight, there is the cerium ion dissolved and to be difficult in scavenging solution with dissolved state stabilization, be difficult to the trend from cleaned material surface cleaning removing cerium composition.On the other hand, during more than 20 % by weight, the solubility property that there is cerium oxide reduces, or is difficult to owing to producing precipitate the proterties being maintained as solution, and becomes the trend of the reason bad when cleaning.
Above-mentioned scavenging solution is preferably containing tensio-active agent.By containing tensio-active agent in scavenging solution, the surface tension of scavenging solution can be made to reduce, make to improve cleaned material wettability of the surface.Thus, by cleaning removing uniform in effect in the broad range on cleaned material surface, the raising of productivity can therefore be realized.
In addition, the invention provides a kind of purging method, it is characterized in that, by making scavenging solution remove with the cleaned material surface contact and being dissolved with the form of cerium ion by cerium oxide being attached with cerium oxide,
Use the scavenging solution containing (1) hydrogen fluoride and (2) ammonium salt as described scavenging solution,
This ammonium salt is selected from least a kind in ammonium chloride, ammonium nitrate, ammonium sulfate, tetramethyl ammonium chloride, tetramethyl-ammonium nitrate and tetramethyl-ammonium sulfate.
In above-mentioned purging method, the hydrofluoric concentration in scavenging solution is preferably 0.001 ~ 5 % by weight, and the concentration of above-mentioned ammonium salt is 0.1 ~ 20 % by weight.Its reason is described above.
In addition, in above-mentioned purging method, scavenging solution is preferably containing tensio-active agent.Its reason is described above.
In addition, above-mentioned purging method can be used well when cleaned material is semiconductor substrate, glass substrate, ceramic substrate, quartz base plate or quartz wafer.
According to the present invention, have and effectively can clean the cerium oxide of removing at the remained on surface of the cleaned material using abrasive containing cerium oxide to grind, and have and be difficult to corrode the such advantage of various metallic substance.Therefore, such as, in the manufacturing process of semiconductor device, effectively can clean the residue of removing cerium oxide from the semiconductor substrate after grinding, the productivity of semiconductor device can be made to improve.In addition, due to metallic substance on semiconductor substrate can be suppressed and form the corrosion of metallic substance of semiconductor device, so the performance of semiconductor device can be made to improve.
Embodiment
Below the embodiment of scavenging solution of the present invention is described.
Scavenging solution of the present invention contains (1) hydrogen fluoride and (2) ammonium salt, this ammonium salt is selected from least a kind in ammonium chloride, ammonium nitrate, ammonium sulfate, tetramethyl ammonium chloride, tetramethyl-ammonium nitrate and tetramethyl-ammonium sulfate, can use well when cleaning removing and remaining in and use the abrasive (slurry) containing cerium oxide to carry out the cerium oxide on the cleaned material surface of grinding as grinding abrasive particle.Particularly can use well when cleaning removing and remaining in and utilize ceria slurry to carry out the cerium oxide on the cleaned material surface of cmp (CMP).
Hydrofluoric concentration in scavenging solution is preferably 0.001 ~ 5 % by weight, is more preferably 0.001 ~ 2 weight.By reducing hydrogen fluoride concentration, effectively can remove cerium oxide, etch, the corrosion of the material on cleaned material surface can be suppressed simultaneously.
The concentration of the above-mentioned ammonium salt in scavenging solution is preferably 0.1 ~ 20 % by weight, is more preferably 0.1 ~ 10 % by weight, and more preferably 0.1 ~ 5 % by weight.By reducing ammonium salt concentration, can be implemented in the resources conservation of liquid preparatory stage, cost savings.Specifically, prepare the concentrated scavenging solution stoste of constituent concentration, dilute with water etc. before this stoste will be carried out clean shortly, and can be made into the scavenging solution of above-mentioned concentration.Thus, relate to and manufacture scavenging solution or be filled into resource relevant in container for conveying or cost, be filled in the substantially reduction of resource that the scavenging solution in container for conveying is correlated with or cost with carrying, and then, relate to the raising of production efficiency.
As the composition than that described above of scavenging solution of the present invention, preferably based on water, but also can containing composition than water.Such as, tensio-active agent, sequestrant, pH adjusting agent and organic solvent etc. can be enumerated.But, when using them, need to consider to the tolerance of the organic composition of washing unit, discarded time cost and use time danger etc.
Scavenging solution of the present invention is preferably containing tensio-active agent.Tensio-active agent is not particularly limited, such as, can enumerate the nonionic system tensio-active agents such as the negatively charged ion such as aliphatic carboxylic acid or its salt system tensio-active agent, polyethylene glycol alkyl ether, the positively charged ion system tensio-active agents etc. such as fatty amine or its salt.
The addition of tensio-active agent is preferably in the scope of 0.001 ~ 0.1 % by weight, is more preferably in the scope of 0.003 ~ 0.05 % by weight.By adding tensio-active agent, chapping of the surface of the cleaned material implementing clean can be suppressed.And then, the wettability to cleaned material can be improved, and realize the homogeneity of the cleaning performance in face.But, when addition is less than 0.001 % by weight, because the surface tension of scavenging solution does not fully reduce, so the raising effect of wettability becomes insufficient sometimes.In addition, when above-mentioned addition is more than 0.1 % by weight, sometimes not only can not obtain its corresponding effect, and defoaming is deteriorated and at cleaned material surface attachment foam, cleaning occurs uneven.
As long as the purity of above-mentioned scavenging solution and degree of cleaning are considered the problem of the pollution of the cleaned material of carrying out clean and manufacturing cost and set.Such as, when using scavenging solution of the present invention in the manufacturing process of unicircuit, the metallic impurity contained in this scavenging solution are preferably below 0.1ppb.
Scavenging solution of the present invention can by carrying out mixing by hydrogen fluoride, above-mentioned ammonium salt and remaining any composition and preparing in any order.Or, also the compound that can synthesize above-mentioned each composition can be mixed as raw material, finally prepare the scavenging solution of mentioned component and concentration.Specifically, scavenging solution of the present invention can be prepared by mixed fluoride hydrogen, sulfuric acid, ammonium and water.That is, undertaken neutralizing by sulfuric acid and ammonium and generate ammonium sulfate.In addition, such as scavenging solution of the present invention can be prepared by mixed fluoride ammonium, sulfuric acid and ammonia.
Form as long as scavenging solution of the present invention becomes above-mentioned in the wash phase being equivalent to operational phase, to the form of preparatory stage without any restriction.Such as, field of employment can be arrived and make through concentrated scavenging solution stoste, carry out diluting and preparing scavenging solution of the present invention before will using shortly.In addition, also can prepare each composition respectively, carry out before will using shortly mixing and preparing scavenging solution of the present invention.
The use temperature of scavenging solution of the present invention is without any restriction.From practicality, preferably use under the normal temperature as useful temperature province.In addition, according to cleaning condition, such as, clean at the temperature of low 10 DEG C than normal temperature, thus suppress the side reaction beyond cleaning, or such as clean under the high temperature of high 80 DEG C than normal temperature, the raising of cleaning performance can also be realized.
Scavenging solution of the present invention may be used for the cleaned material of various material and shape.As cleaned material, such as, can enumerate silicon, glass, pottery.The surfacing that can be suitable for the cleaned material of scavenging solution of the present invention is not particularly limited, such as, can enumerate silicon single crystal, polysilicon, non-crystalline silicon, thermal oxidation silicon film, non-impurity-doped silicate glass film, mix phosphosilicate glass film, glass membrane mixed with borosilicate, mix phosphorus borosilicate glass film, TEOS film, plasma CVD oxide film, silicon nitride film, silicon carbide film, silicon oxide carbide (シ リ コ Application オ キ サ イ De カ mono-バ イ De) film or carbonitride silicon oxide (シ リ コ Application オ キ サ イ De カ mono-バ イ De Na イ ト ラ イ De) film etc.In addition, glass, quartz, crystal, pottery etc. can also be applicable to.They can be formed separately, also two or more can form pattern with certain distribution or be laminated.
Scavenging solution of the present invention also can perform well in utilizing grinding step and the smooth cleaned material that flattens.As the Ginding process on cleaned material surface, be not particularly limited, known various method can be adopted.Ginding process can according to the shape of this cleaned material, suitably select as the grinding precision of target.Specifically, can enumerate such as mechanical stone mill, cmp (CMP) etc., scavenging solution of the present invention is suitable for the cmp (CMP) using ceria slurry.Ceria slurry is the slurry that will be scattered in as the cerium oxide grinding abrasive particle in solution.
As the purging method using scavenging solution of the present invention, various wet-cleaned method can be adopted.Such as, dip treating method cleaned material being immersed in and being filled in the scavenging solution of rinse bath can be enumerated.In addition, by making scavenging solution spray, be sprayed on the single-wafer processing method etc. of the cleaned materials such as the silicon wafer of rotation being carried out clean.In addition, in above-mentioned dip treating method, limit can also be adopted scavenging solution to be applied to the method for carrying out on ultrasonic wave limit.And then what can also be suitable for that limit winding-up scavenging solution lateral dominance brush carries out cleaning scrubs (BrushScrub) method.Should illustrate, cleaning can be carried out repeatedly.Now, in each clean, all can use composition or the different scavenging solution of concentration at every turn.
There is no particular limitation for scavenging period, suitably can set according to the pollution level etc. of the cerium oxide being attached to cleaned material.Usually less than 10 minutes are preferably, more preferably less than 1 minute.When scavenging period was more than 10 minutes, the surface of cleaned material is etched and surfaceness increase sometimes.
In addition, in purging method of the present invention, after above-mentioned clean, suitably can also carry out the flushing operation utilizing the irrigations such as ultrapure water as required.Thus, the remained on surface scavenging solution in cleaned material can be prevented.
Embodiment
Below, the preferred embodiments of the present invention are described in detail illustratively.But, unless there is the record of being particularly limited to property to the material, use level etc. described in this embodiment, otherwise be not intended to scope of the present invention to be defined in this, and be illustrative examples.
(making method of scavenging solution)
The scavenging solution of each embodiment or comparative example by shown below raw-material any one suitably coordinate and make.The salt used in an embodiment is the bronsted lowry acids and bases bronsted lowry selecting to form salt from following shown starting material, makes them carry out reacting obtaining.Namely, by (1) 50 % by weight high-purity hydrogen fluoric acid (StellaChemifa Co., Ltd. system), (2) EL level, 36 % by weight hydrochloric acid (Mitsubishi chemical Co., Ltd's system), (3) EL level, 69 % by weight nitric acid (Mitsubishi chemical Co., Ltd's system), (4) EL level, 97 % by weight sulfuric acid (Mitsubishi chemical Co., Ltd's system), (5) EL level, 28 % by weight ammoniacal liquor (Hayashi Pure Chemical Ind Ltd.'s system), (6) Tetramethylammonium hydroxide (trade(brand)name: TokusoSD-25, Tokuyama Co., Ltd. system) in each starting material carry out coordinating with the blending ratio of regulation and make.
In embodiments, when using tensio-active agent, following each shown starting material are suitably coordinated.That is, each starting material in (1) Voranol EP 2001 (nonionogenic tenside), (2) heptyl amice (cats product), (3) enanthic acid (nonionogenic tenside) are added with the concentration of regulation.
(measuring method of the residue Restzustand on cleaned material surface)
For the residue state of the cerium oxide solids on cleaned material surface, TREX610-T (Co., Ltd. Teknos system) is utilized to carry out.That is, measure utilizing before and after the clean of scavenging solution, confirm the cleaning performance utilizing scavenging solution.
(embodiment 1 ~ 13)
As shown in table 1, hydrogen fluoride as composition (a), the ammonium sulfate as composition (b) and the water as composition (c) are carried out mixing and makes scavenging solution, make hydrofluoric concentration be 0.001 ~ 5 % by weight, the concentration of ammonium sulfate is 1 ~ 20 % by weight.
(embodiment 14 ~ 17)
As shown in table 1, using the hydrogen fluoride as composition (a), tetramethyl-ammonium sulfate as composition (b) with carry out mixing as the water of composition (c) and make scavenging solution, make hydrofluoric concentration be 0.01 ~ 0.1 % by weight, the concentration of tetramethyl-ammonium sulfate is 1 ~ 10 % by weight.
(embodiment 18)
As shown in table 1, hydrogen fluoride as composition (a), the ammonium sulfate as composition (b), ammonium chloride and the water as composition (c) are carried out mixing and makes scavenging solution, hydrofluoric concentration is made to be 0.1 % by weight, the concentration of ammonium sulfate is 5 % by weight, and the concentration of ammonium chloride is 5 % by weight.
(comparative example 1)
As shown in table 1, make the aqueous solution that ammonium sulfate concentrations is 20 % by weight.
(comparative example 2)
As shown in table 1, make the aqueous solution that Neutral ammonium fluoride concentration is 20 % by weight.
(comparative example 3)
As shown in table 1, hydrogen fluoride as composition (a), the Neutral ammonium fluoride as composition (b) and the water as composition (c) are carried out mixing and makes scavenging solution, make hydrofluoric concentration be 0.5%, the concentration of Neutral ammonium fluoride is 20 % by weight.
(comparative example 4)
As shown in table 1, making hydrogen fluoride concentration is the aqueous solution of 5%.
Then, be formed on surface
the diameter of TEOS film be the cmp that the silicon substrate of 200mm carries out cerium oxide to be used as abrasive particle, used as cleaned material.In this cleaned material, by the mensuration of residue Restzustand described later, 1 × 10
12atom/cm
2the cerium oxide of left and right is identified as residue composition.
Next, above-mentioned scavenging solution is filled in the cleaning liquid bath that volume is 90L, rinse liquid temperature is adjusted to 25 DEG C, rinse liquid temperature is stablized.Here, make after above-mentioned cleaned material remains on the resinous silicon substrate holding member of PFA, proofing 30 seconds in above-mentioned cleaning liquid bath.After dipping, mentioned from cleaning liquid bath by each silicon substrate holding member, being immersed in pre-prepd volume is in the ultrapure water groove of 90L, is washed off by the scavenging solution being attached to cleaned material surface.Then, cleaned material is carried out drying, again carry out the mensuration of above-mentioned residue Restzustand.Good, the difference of removing performance be using process after cerium component content be reduced to 8.5 × 10 of the Monitoring lower-cut value as Restzustand evaluating apparatus
9atom/cm
2following situation, as good, will not be reduced to 8.5 × 10
9atom/cm
2situation as difference.Cleaning evaluation result based on this is shown in following table 1.
[table 1]
As can be known from the results of Table 1, when using the scavenging solution of the present embodiment 1 ~ 18,8.5 × 10 are reduced at the cerium composition on cleaned material surface
9atom/cm
2below, to the cleaning removing excellent effect of cerium oxide.
On the other hand, during the scavenging solution of known comparative example 1 ~ 4, cerium composition is not reduced to below the Monitoring lower-cut value of evaluating apparatus, low to the cleaning removing effect of cerium oxide.
(embodiment 19 ~ 31)
As shown in table 2, change the composition of scavenging solution and concentration, in addition, carry out same with above-described embodiment 1 and made each scavenging solution.And then, utilize each scavenging solution to carry out clean etc. equally with above-described embodiment 1.The results are shown in following table 2.
(comparative example 5)
As shown in table 2, change the composition of scavenging solution and concentration, in addition, carry out same with above-described embodiment 1 and make each scavenging solution.And then, utilize each scavenging solution to carry out clean etc. equally with above-described embodiment 1.The results are shown in following table 2.
[table 2]
As can be known from the results of Table 2, when using the scavenging solution of the present embodiment 19 ~ 31,8.5 × 10 are reduced at the cerium composition on cleaned material surface
9atom/cm
2below, to the cleaning removing excellent effect of cerium oxide.
On the other hand, during the scavenging solution of known comparative example 5, cerium composition is not reduced to below the Monitoring lower-cut value of evaluating apparatus, low to the cleaning removing effect of cerium oxide.
(embodiment 32 ~ 44)
As shown in table 3, change the composition of scavenging solution and concentration, in addition, carry out same with above-described embodiment 1 and make each scavenging solution.And then, utilize each scavenging solution to carry out clean etc. equally with above-described embodiment 1.The results are shown in following table 3.
(comparative example 6)
As shown in table 3, change the composition of scavenging solution and concentration, in addition, carry out same with above-described embodiment 1 and make each scavenging solution.And then, utilize each scavenging solution to carry out clean etc. equally with above-described embodiment 1.The results are shown in following table 3.
[table 3]
As can be known from the results of Table 3, when using the scavenging solution of the present embodiment 32 ~ 44,8.5 × 10 are reduced at the cerium composition on cleaned material surface
9atom/cm
2below, to the cleaning removing excellent effect of cerium oxide.
On the other hand, during the scavenging solution of known comparative example 6, cerium composition is not reduced to below the Monitoring lower-cut value of evaluating apparatus, low to the cleaning removing effect of cerium oxide.
(embodiment 45 ~ 47)
As shown in table 4, using the hydrogen fluoride as composition (a), the ammonium sulfate as composition (b), make scavenging solution as the water of composition (c) and then nonionic, cationic or anionic surfactant's mixing, such that hydrofluoric concentration is 0.1 % by weight, the concentration of ammonium sulfate is 10 % by weight.Then, equally with above-described embodiment 1 clean utilizing each scavenging solution is carried out.The results are shown in following table 4.
[table 4]
As can be known from the results of Table 4, when using the scavenging solution of the present embodiment 45 ~ 47,8.5 × 10 are reduced at the cerium composition on cleaned material surface
9atom/cm
2below, to the cleaning removing excellent effect of cerium oxide.
(embodiment 48 ~ 59)
As shown in table 5, using the hydrogen fluoride as composition (a), the ammonium sulfate as composition (b), ammonium chloride, ammonium nitrate or tetramethyl-ammonium sulfate and carry out mixing as the water of composition (c) and make scavenging solution, make the concentration of composition (a) be 0.1 ~ 5 % by weight, the concentration of composition (b) is 5 % by weight.
(comparative example 7)
As shown in table 5, make the aqueous solution that ammonium sulfate concentrations is 5 % by weight.
(comparative example 8)
As shown in table 5, make the aqueous solution that Neutral ammonium fluoride concentration is 20 % by weight.
(comparative example 9)
As shown in table 5, hydrogen fluoride as composition (a), the Neutral ammonium fluoride as composition (b) and the water as composition (c) are carried out mixing and makes scavenging solution, make hydrofluoric concentration be 0.5%, the concentration of Neutral ammonium fluoride is 20 % by weight.
(comparative example 10)
As shown in table 5, making hydrogen fluoride concentration is the aqueous solution of 5%.
Then, be formed on surface
the diameter of non-impurity-doped polysilicon film is the cmp that the silicon substrate of 200mm carries out cerium oxide to be used as abrasive particle, used as cleaned material.In this cleaned material, by the mensuration of residue Restzustand described later, 1 × 10
12atom/cm
2the cerium oxide of left and right is identified as residue composition.
Next, equally with above-described embodiment 1 clean etc. utilizing each scavenging solution is carried out.The results are shown in following table 5.
[table 5]
As can be known from the results of Table 5, when using the scavenging solution of the present embodiment 48 ~ 59,8.5 × 10 are reduced at the cerium composition on cleaned material surface
9atom/cm
2below, to the cleaning removing excellent effect of cerium oxide.
On the other hand, during the scavenging solution of known comparative example 7 ~ 10, cerium composition is not reduced to below the Monitoring lower-cut value of evaluating apparatus, low to the cleaning removing effect of cerium oxide.
(embodiment 60 ~ 71)
As shown in table 6, using the hydrogen fluoride as composition (a), the ammonium sulfate as composition (b), ammonium chloride, ammonium nitrate or tetramethyl-ammonium sulfate and carry out mixing as the water of composition (c) and make scavenging solution, make the concentration of composition (a) be 0.1 ~ 5 % by weight, the concentration of composition (b) is 5 % by weight.
(comparative example 11)
As shown in table 6, make the aqueous solution that ammonium sulfate concentrations is 5 % by weight.
(comparative example 12)
As shown in table 6, make the aqueous solution that Neutral ammonium fluoride concentration is 20 % by weight.
(comparative example 13)
As shown in table 6, hydrogen fluoride as composition (a), the Neutral ammonium fluoride as composition (b) and the water as composition (c) are carried out mixing and makes scavenging solution, make hydrofluoric concentration be 0.5%, the concentration of Neutral ammonium fluoride is 20 % by weight.
(comparative example 14)
As shown in table 6, making hydrogen fluoride concentration is the aqueous solution of 5%.
Then, 1000 are formed with on surface
the diameter of silicon nitride film is the cmp that the silicon substrate of 200mm carries out cerium oxide to be used as abrasive particle, used as cleaned material.In this cleaned material, by the mensuration of residue Restzustand described later, 1 × 10
12atom/cm
2the cerium oxide of left and right is identified as residue composition.
Next, equally with above-described embodiment 1 clean etc. utilizing each scavenging solution is carried out.The results are shown in following table 6.
[table 6]
As can be known from the results of Table 6, when using the scavenging solution of the present embodiment 60 ~ 71,8.5 × 10 are reduced at the cerium composition on cleaned material surface
9atom/cm
2below, to the cleaning removing excellent effect of cerium oxide.
On the other hand, during the scavenging solution of known comparative example 11 ~ 14, cerium composition is not reduced to below the Monitoring lower-cut value of evaluating apparatus, low to the cleaning removing effect of cerium oxide.
(embodiment 72 ~ 74)
As shown in table 7, hydrogen fluoride as composition (a), the ammonium sulfate as composition (b) and the water as composition (c) are carried out mixing and makes scavenging solution, make hydrofluoric concentration be 0.01 ~ 0.5 % by weight, the concentration of ammonium sulfate is 10 % by weight.
(comparative example 15 ~ 17)
As shown in table 7, hydrogen fluoride as composition (a), the sulfuric acid as composition (b) and the water as composition (c) are carried out mixing and makes scavenging solution, make hydrofluoric concentration be 0.01 ~ 0.5 % by weight, the concentration of sulfuric acid is 10 % by weight.
(comparative example 18)
As shown in table 7, using the hydrogen fluoride as composition (a), the sulfuric acid as composition (b) is with xitix and carry out mixing as the water of composition (c) and make scavenging solution, hydrofluoric concentration is made to be 0.01 % by weight, the concentration of sulfuric acid is 10 % by weight, and the concentration of xitix is 0.1 % by weight.
Then, prepare respectively to be formed on surface
titanium film and
the diameter of aluminium film is the silicon substrate of 200mm, it can be used as cleaned material to use.
Next, above-mentioned scavenging solution is filled in the cleaning liquid bath that volume is 90L, rinse liquid temperature is adjusted to 25 DEG C, rinse liquid temperature is stablized., make after above-mentioned cleaned material remains on the resinous silicon substrate holding member of PFA here, impregnated in the specified time of the silicon substrate with titanium film and aluminium film shown in table 7 in above-mentioned scavenging solution.After proofing, mentioned from cleaning liquid bath by each silicon substrate holding member, proofing is in the ultrapure water groove of 90L at pre-prepd volume, is washed off by the scavenging solution being attached to cleaned material surface.Then, make cleaned material dry, utilize 4 sonde-type surface resistivity testers (development of republicanism reason, K705-RS) to measure sheet resistance value.Its measurement result is shown in following table 7.
[table 7]
As shown in Table 7, when using the scavenging solution of embodiment 72 ~ 74, the rising of the titanium film on cleaned material surface and the sheet resistance value of aluminium film becomes and is less than comparative example 15 ~ 17, little on the impact of titanium film and aluminium film.It can thus be appreciated that scavenging solution of the present invention not only can clean removing cerium oxide, and compared with the scavenging solution of comparative example, the increase of the resistance value of metallic membrane more can be suppressed.
On the other hand, the increase of the titanium film of the scavenging solution of known comparative example 18 and the sheet resistance value of aluminium film is large, namely allows to cleaning removing cerium oxide, also can increase the resistance value of metallic membrane.
Claims (7)
1. a scavenging solution, is characterized in that, the removing of this scavenging solution residues in the cerium oxide on cleaned material surface, and this scavenging solution is made up of (1) hydrogen fluoride, (2) ammonium salt and (3) water,
This ammonium salt is selected from least a kind in ammonium chloride, ammonium nitrate, ammonium sulfate, tetramethyl ammonium chloride, tetramethyl-ammonium nitrate and tetramethyl-ammonium sulfate.
2. a scavenging solution, it is characterized in that, the removing of this scavenging solution residues in the cerium oxide on cleaned material surface, the composition that this scavenging solution is selected from tensio-active agent, sequestrant, pH adjusting agent and organic solvent by (1) hydrogen fluoride, (2) ammonium salt, (3) water with (4) is formed
This ammonium salt is selected from least a kind in ammonium chloride, ammonium nitrate, ammonium sulfate, tetramethyl ammonium chloride, tetramethyl-ammonium nitrate and tetramethyl-ammonium sulfate.
3. scavenging solution according to claim 1 and 2, wherein, hydrofluoric concentration is 0.001 ~ 5 % by weight, and the concentration of ammonium salt is 0.1 ~ 20 % by weight.
4. a purging method, is characterized in that, by making scavenging solution remove with the cleaned material surface contact and being dissolved with the form of cerium ion by cerium oxide being attached with cerium oxide,
Use the scavenging solution be made up of (1) hydrogen fluoride, (2) ammonium salt and (3) water as described scavenging solution,
This ammonium salt is selected from least a kind in ammonium chloride, ammonium nitrate, ammonium sulfate, tetramethyl ammonium chloride, tetramethyl-ammonium nitrate and tetramethyl-ammonium sulfate.
5. a purging method, is characterized in that, by making scavenging solution remove with the cleaned material surface contact and being dissolved with the form of cerium ion by cerium oxide being attached with cerium oxide,
Use scavenging solution that the composition being selected from tensio-active agent, sequestrant, pH adjusting agent and organic solvent by (1) hydrogen fluoride, (2) ammonium salt, (3) water and (4) is formed as described scavenging solution,
This ammonium salt is selected from least a kind in ammonium chloride, ammonium nitrate, ammonium sulfate, tetramethyl ammonium chloride, tetramethyl-ammonium nitrate and tetramethyl-ammonium sulfate.
6. the purging method according to claim 4 or 5, wherein, hydrofluoric concentration is 0.001 ~ 5 % by weight, and the concentration of ammonium salt is 0.1 ~ 20 % by weight.
7. the purging method according to claim 4 or 5, wherein, cleaned material is semiconductor substrate, glass substrate, ceramic substrate, quartz base plate or quartz wafer.
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CN102380490B (en) * | 2011-10-20 | 2016-03-09 | 高佳太阳能股份有限公司 | The cleaning method of mono-crystalline silicon side skin |
CN104619806A (en) * | 2012-09-17 | 2015-05-13 | 株式会社Lg化学 | Method for recycling waste abrasive material containing ceria |
KR101932774B1 (en) * | 2013-03-15 | 2018-12-26 | 동우 화인켐 주식회사 | Composition for cleaning flat panel display and cleaning method using the same |
AU2014271674B2 (en) | 2013-05-30 | 2017-02-16 | Toyota Jidosha Kabushiki Kaisha | Error diagnostic device for exhaust purification device |
WO2015089023A1 (en) | 2013-12-11 | 2015-06-18 | Fujifilm Electronic Materials U.S.A., Inc. | Cleaning formulation for removing residues on surfaces |
CN106190616A (en) * | 2016-07-13 | 2016-12-07 | 苏州普锐晶科技有限公司 | The caustic solution of frequency chip |
WO2018168207A1 (en) * | 2017-03-14 | 2018-09-20 | 株式会社フジミインコーポレーテッド | Surface treatment composition and production method therefor, and surface treatment method using same |
CN107164109A (en) * | 2017-03-31 | 2017-09-15 | 吴江创源新材料科技有限公司 | Cleaning fluid and preparation method thereof and cleaning before a kind of sapphire wafer annealing |
KR102475619B1 (en) * | 2017-03-31 | 2022-12-07 | 간또 가가꾸 가부시끼가이샤 | cleaning liquid composition |
CN109731849A (en) * | 2018-11-30 | 2019-05-10 | 东莞市晶博光电有限公司 | A kind of hand-set lid clean method |
CN111376169A (en) * | 2018-12-28 | 2020-07-07 | 安集微电子科技(上海)股份有限公司 | Method for cleaning polished wafer |
JP7107332B2 (en) * | 2020-06-02 | 2022-07-27 | 栗田工業株式会社 | Separation membrane cleaning method |
CN114717295B (en) * | 2022-06-09 | 2022-09-30 | 季华实验室 | Liquid phase chip method hybridization buffer solution, preparation method and liquid phase chip detection method |
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CN101084573A (en) * | 2004-12-20 | 2007-12-05 | 斯泰拉化工公司 | Fine processing treatment agent and fine processing treatment method using same |
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CN101084573A (en) * | 2004-12-20 | 2007-12-05 | 斯泰拉化工公司 | Fine processing treatment agent and fine processing treatment method using same |
WO2010134184A1 (en) * | 2009-05-21 | 2010-11-25 | ステラケミファ株式会社 | Fine-processing agent and fine-processing method |
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