WO2010134184A1 - 微細加工処理剤、及び微細加工処理方法 - Google Patents
微細加工処理剤、及び微細加工処理方法 Download PDFInfo
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- WO2010134184A1 WO2010134184A1 PCT/JP2009/059370 JP2009059370W WO2010134184A1 WO 2010134184 A1 WO2010134184 A1 WO 2010134184A1 JP 2009059370 W JP2009059370 W JP 2009059370W WO 2010134184 A1 WO2010134184 A1 WO 2010134184A1
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- Prior art keywords
- processing agent
- fine processing
- film
- weight
- oxide film
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- 238000003672 processing method Methods 0.000 title claims abstract description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 75
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 72
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 69
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 69
- 229920003169 water-soluble polymer Polymers 0.000 claims abstract description 40
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 37
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims abstract description 21
- WPKYZIPODULRBM-UHFFFAOYSA-N azane;prop-2-enoic acid Chemical compound N.OC(=O)C=C WPKYZIPODULRBM-UHFFFAOYSA-N 0.000 claims abstract description 9
- AGBXYHCHUYARJY-UHFFFAOYSA-N 2-phenylethenesulfonic acid Chemical compound OS(=O)(=O)C=CC1=CC=CC=C1 AGBXYHCHUYARJY-UHFFFAOYSA-N 0.000 claims abstract description 7
- -1 ester styrenesulfonate Chemical class 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 4
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 4
- XDIJWRHVEDUFGP-UHFFFAOYSA-N azanium;2-phenylethenesulfonate Chemical compound [NH4+].[O-]S(=O)(=O)C=CC1=CC=CC=C1 XDIJWRHVEDUFGP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 71
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 12
- 229920002401 polyacrylamide Polymers 0.000 claims description 12
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 10
- 239000004094 surface-active agent Substances 0.000 claims description 10
- 239000005368 silicate glass Substances 0.000 claims description 8
- 239000002202 Polyethylene glycol Substances 0.000 claims description 6
- 150000007522 mineralic acids Chemical class 0.000 claims description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims description 6
- 229920001577 copolymer Polymers 0.000 claims description 4
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 3
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical group C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 claims description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 150000007933 aliphatic carboxylic acids Chemical class 0.000 claims description 2
- 125000001931 aliphatic group Chemical group 0.000 claims description 2
- 150000005215 alkyl ethers Chemical class 0.000 claims description 2
- 125000005037 alkyl phenyl group Chemical group 0.000 claims description 2
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical class OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 2
- 239000000194 fatty acid Substances 0.000 claims description 2
- 229930195729 fatty acid Natural products 0.000 claims description 2
- 229910052731 fluorine Inorganic materials 0.000 claims description 2
- 239000011737 fluorine Substances 0.000 claims description 2
- 150000007524 organic acids Chemical class 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- 239000012190 activator Substances 0.000 claims 1
- ZZUFCTLCJUWOSV-UHFFFAOYSA-N furosemide Chemical compound C1=C(Cl)C(S(=O)(=O)N)=CC(C(O)=O)=C1NCC1=CC=CO1 ZZUFCTLCJUWOSV-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 18
- 235000012239 silicon dioxide Nutrition 0.000 abstract 2
- 239000000377 silicon dioxide Substances 0.000 abstract 2
- 125000005396 acrylic acid ester group Chemical group 0.000 abstract 1
- 239000010408 film Substances 0.000 description 178
- 238000005530 etching Methods 0.000 description 81
- 239000000243 solution Substances 0.000 description 28
- 230000000052 comparative effect Effects 0.000 description 17
- 239000004065 semiconductor Substances 0.000 description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 14
- 239000003990 capacitor Substances 0.000 description 13
- 230000000694 effects Effects 0.000 description 12
- 238000004519 manufacturing process Methods 0.000 description 11
- 229910021642 ultra pure water Inorganic materials 0.000 description 9
- 239000012498 ultrapure water Substances 0.000 description 9
- 239000011259 mixed solution Substances 0.000 description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 238000001039 wet etching Methods 0.000 description 6
- 241000862969 Stella Species 0.000 description 5
- 239000000654 additive Substances 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- 230000007423 decrease Effects 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 230000008020 evaporation Effects 0.000 description 4
- 230000010354 integration Effects 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 3
- 239000005380 borophosphosilicate glass Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000005459 micromachining Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000007334 copolymerization reaction Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000003112 inhibitor Substances 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 229920000058 polyacrylate Polymers 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000001629 suppression Effects 0.000 description 2
- 239000012756 surface treatment agent Substances 0.000 description 2
- 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 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- BTBJBAZGXNKLQC-UHFFFAOYSA-N ammonium lauryl sulfate Chemical compound [NH4+].CCCCCCCCCCCCOS([O-])(=O)=O BTBJBAZGXNKLQC-UHFFFAOYSA-N 0.000 description 1
- 229940063953 ammonium lauryl sulfate Drugs 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000000909 electrodialysis Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000003014 ion exchange membrane Substances 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 239000012788 optical film Substances 0.000 description 1
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 229910001936 tantalum oxide Inorganic materials 0.000 description 1
Classifications
-
- 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 potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table 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
-
- 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 potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table 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
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3105—After-treatment
- H01L21/311—Etching the insulating layers by chemical or physical means
- H01L21/31105—Etching inorganic layers
- H01L21/31111—Etching inorganic layers by chemical means
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K13/00—Etching, surface-brightening or pickling compositions
- C09K13/04—Etching, surface-brightening or pickling compositions containing an inorganic acid
- C09K13/08—Etching, surface-brightening or pickling compositions containing an inorganic acid containing a fluorine compound
Definitions
- the present invention relates to a fine processing agent used for fine processing, cleaning processing, and the like, and a fine processing method using the same in the manufacture of a semiconductor device, a liquid crystal display device, a micro electro mechanical systems (MEMS) device, and the like.
- the present invention relates to a fine processing agent used for fine processing of a laminated film in which at least a silicon oxide film and a silicon nitride film are laminated, and a fine processing method using the same.
- One of the most important processes in the manufacturing process of semiconductor devices is to pattern and etch a silicon oxide film, silicon nitride film, polysilicon film, metal film, etc. formed on the wafer surface into a desired shape. It is.
- wet etching which is a kind of etching technique, a fine processing agent capable of selectively etching only a film to be etched is required.
- examples of the silicon oxide film to be etched include buffered hydrofluoric acid and hydrofluoric acid.
- the buffered hydrofluoric acid or hydrofluoric acid is used as a microfabrication processing agent for the laminated film in which the silicon oxide film and the silicon nitride film are laminated, the silicon nitride film is also etched at the same time. As a result, it becomes difficult to pattern into a desired shape.
- the fine processing agent As a fine processing agent capable of solving such problems and selectively etching only the silicon oxide film, for example, a hydrofluoric acid added with an anionic surfactant such as ammonium lauryl sulfate. (See Patent Document 1 below).
- the fine processing agent has a very high foaming property, which makes it unsuitable as a fine processing agent used in a semiconductor element manufacturing process.
- a DRAM Dynamic Random Access Memory
- the DRAM cell is composed of one transistor and one capacitor. This DRAM has been highly integrated about four times over the past three years. High integration of DRAM is mainly due to high integration of capacitors. Therefore, in order to secure a capacitance value necessary for stable storage operation while reducing the area occupied by the capacitor, the capacitor area is increased, the capacitor insulating film is thinned, and a high dielectric constant film is introduced.
- the capacitor insulating film As the capacitor insulating film, a silicon oxide film is used, and until now, its thinning has been studied. However, the thinning of the silicon oxide film as the capacitor insulating film has reached the limit with 1Mbit DRAM. Therefore, a silicon nitride film is used as an insulating film in a 4M bit DRAM. Furthermore, application of a tantalum oxide film has been started as higher integration progresses.
- the capacitor structure of a 64 Mbit generation DRAM is a cylinder type.
- the silicon oxide film thus formed is removed by wet etching to form a capacitor after forming the cylinder-type capacitor lower electrode, the following problems occur when a conventional etching solution is used.
- Patent Document 2 discloses a technique for forming a support film made of a silicon nitride film between capacitor lower electrodes.
- Patent Document 3 listed below discloses a technique for forming a silicon nitride film as an insulating film in order to improve the insulation characteristics with respect to the bit line. A technique for forming a film as an etching stop film in an etching process of a silicon oxide film is disclosed.
- the present invention has been made in view of the above-described problems, and an object of the present invention is to selectively finely process a silicon oxide film when finely processing a laminated film in which at least a silicon oxide film and a silicon nitride film are laminated.
- An object of the present invention is to provide a fine processing agent that can be used, and a fine processing method using the same.
- the microfabrication processing agent to which a predetermined water-soluble polymer is added can selectively microfabricate only the silicon oxide film with respect to the laminated film in which the silicon oxide film and the silicon nitride film are laminated. As a result, the present invention has been completed.
- the fine processing agent according to the present invention provides at least one of (a) 0.01 to 15% by weight of hydrogen fluoride, or 0.1 to 40% by weight of ammonium fluoride in order to solve the above problems. Any one, (b) water, (c) 0.001 to 10% by weight of acrylic acid, ammonium acrylate, acrylic ester, acrylamide, styrene sulfonic acid, ammonium styrene sulfonate, and styrene sulfonic acid ester And at least one water-soluble polymer selected from the group consisting of:
- the fine processing agent of the present invention can reduce the etching effect on the silicon nitride film without impairing the etching effect on the silicon oxide film by containing the water-soluble polymer.
- the microfabrication processing agent of the present invention when the microfabrication processing agent of the present invention is applied to microfabrication of a laminated film in which a silicon oxide film and a silicon nitride film are laminated, selective microfabrication of the silicon oxide film while suppressing etching of the silicon nitride film Is possible. As a result, the yield in the semiconductor element manufacturing process can be reduced.
- the content of the water-soluble polymer is in the range of 0.001 to 10% by weight.
- the lower limit By setting the lower limit to 0.001% by weight, the effect of adding the water-soluble polymer can be exhibited, and the etching of the silicon nitride film can be suppressed.
- the increase in the metal impurity in a fine processing agent can be suppressed by making an upper limit into 10 weight%.
- an increase in viscosity can also be suppressed, thereby preventing a reduction in the rinse removal performance of the fine processing agent with a rinse agent such as ultrapure water.
- “microfabrication” means including etching of a film to be processed and surface cleaning.
- the “water-soluble polymer” means a polymer that dissolves 1 mass% or more (10 g / L) at room temperature in a mixed solution containing the components (a) and (b).
- the water-soluble polymer is preferably a copolymer of ammonium acrylate and methyl acrylate.
- the water-soluble polymer is polyacrylamide.
- the water-soluble polymer preferably has a weight average molecular weight in the range of 1,000 to 1,000,000.
- the stabilizer that serves as a polymerization inhibitor can be reduced in the production of the water-soluble polymer.
- the water-soluble polymer can be prevented from being contaminated with metal.
- the weight average molecular weight is set to 1 million or less, an increase in the viscosity of the fine processing agent can be suppressed, so that handleability can be improved.
- a rinse agent such as ultrapure water.
- the silicon oxide film preferably has an etch rate at 25 ° C. in the range of 1 to 5000 nm / min. As a result, it is possible to improve the production efficiency by preventing the processing time of the fine processing for the silicon oxide film from being prolonged, and to easily control the film thickness and surface roughness of the silicon oxide film after the micro processing. To do.
- the microfabrication processing method microfabricates a laminated film in which at least a silicon oxide film and a silicon nitride film are laminated, using the micromachining treatment agent described above. It is characterized by that.
- the silicon oxide film and a silicon nitride film are added to the fine processing agent capable of reducing the etching effect on the silicon nitride film without impairing the etching effect on the silicon oxide film by adding the water-soluble polymer. Therefore, the silicon oxide film can be selectively finely processed while suppressing the etching of the silicon nitride film. As a result, the yield in the semiconductor element manufacturing process can be reduced.
- the silicon oxide film is a natural oxide film, a thermal silicon oxide film, a non-doped silicate glass film, a phosphorus-doped silicate glass film, a boron-doped silicate glass film, a phosphorus-doped silicate glass film, a TEOS film, or a fluorine-containing silicon oxide film. It is preferable that
- the silicon nitride film is preferably a silicon nitride film or a silicon oxynitride film.
- the present invention has the following effects by the means described above. That is, according to the present invention, only the silicon oxide film can be selectively finely processed with respect to the laminated film in which at least the silicon oxide film and the silicon nitride film are laminated.
- a semiconductor device a liquid crystal display device, It enables fine processing suitable for manufacturing micromachine devices and the like.
- the fine processing agent according to the present invention includes (a) at least one of hydrogen fluoride and ammonium fluoride, (b) water, and (c) a water-soluble polymer. .
- the content of hydrogen fluoride in the component (a) is preferably in the range of 0.01 to 15% by weight with respect to the total weight of the fine processing agent, and 0.05 to 10% by weight. It is more preferable that it is within the range.
- the content of hydrogen fluoride is less than 0.01% by weight, it is difficult to control the concentration of hydrogen fluoride, and thus there may be a large variation in etch rate with respect to the silicon oxide film.
- the content of hydrogen fluoride exceeds 15% by weight, the etching rate for the silicon oxide film becomes excessively high, and the controllability of etching deteriorates.
- the content of the ammonium fluoride is preferably in the range of 0.1 to 40% by weight and preferably in the range of 5 to 25% by weight with respect to the total weight of the fine processing agent. More preferred. If the content of ammonium fluoride is less than 0.1% by weight, it is difficult to control the concentration of ammonium fluoride, and thus there may be a large variation in etch rate with respect to the silicon oxide film. Moreover, when the content of ammonium fluoride exceeds 40% by weight, it approaches the saturation solubility of ammonium fluoride. Therefore, when the liquid temperature of the fine processing agent decreases, the fine processing agent reaches the saturation solubility, Crystals may be deposited.
- the etching rate with respect to the silicon nitride film can be selectively suppressed, and the etching selectivity (silicon oxide film / silicon nitride film) can be increased. More specifically, for example, the etching rate for the silicon nitride film can be suppressed to 80% or less as compared with the case where the component (a) is not added.
- the component (a) may be hydrogen fluoride or ammonium fluoride alone or a mixture thereof.
- the 3rd component may contain.
- the third component include surfactants and inorganic acids.
- an organic acid such as formic acid because the effect of selectively suppressing etching on the silicon nitride film is reduced.
- the surfactant is not particularly limited.
- the component (a) is hydrofluoric acid alone, it is selected from the group consisting of polyethylene glycol alkyl ether, polyethylene glycol alkyl phenyl ether, and polyethylene glycol fatty acid ester.
- At least any one nonionic surfactant is preferably exemplified.
- an aliphatic alcohol, aliphatic carboxylic acid, hydrofluoroalkyl alcohol, hydrofluoroalkyl carboxylic acid, hydrofluoroalkyl It may be used in at least any one selected from the group consisting of a salt of a kill carboxylic acid, an aliphatic amine salt, and an aliphatic sulfonic acid, and the form thereof may be solid or liquid.
- the amount of the surfactant added is preferably in the range of 0.001 to 0.1% by weight and in the range of 0.003 to 0.05% by weight with respect to the total weight of the fine processing agent. Is more preferred.
- By adding the surfactant it is possible to suppress the roughness of the surface of the silicon nitride film or semiconductor substrate subjected to the etching process.
- the conventional etching solution tends to remain locally on the surface of the semiconductor substrate on which a fine pattern has been formed due to ultra-high integration, and uniformly etches when the resist interval is about 0.5 ⁇ m or less. It becomes more difficult.
- the fine processing agent of the present invention to which a surfactant is added is used as an etching solution, the wettability to the surface of the semiconductor substrate is improved, and the uniformity of etching in the substrate surface is improved.
- the addition amount is less than 0.001% by weight, the surface tension of the fine processing agent is not sufficiently lowered, and the effect of improving wettability may be insufficient.
- the addition amount exceeds 0.1% by weight, not only the effect corresponding to that can not be obtained, but also the defoaming property deteriorates, the bubbles adhere to the etched surface, the etching unevenness occurs, or the fine gaps are formed. Bubbles may enter and cause etching failure.
- the inorganic acid is not particularly limited, and examples thereof include hydrochloric acid, sulfuric acid, and phosphoric acid.
- the addition amount of the inorganic acid is preferably in the range of 0.01 to 30% by weight, more preferably in the range of 0.05 to 10% by weight, based on the total weight of the fine processing agent. Is preferred. If the addition amount is less than 0.01% by weight, it is difficult to control the concentration of the inorganic acid, which causes a disadvantage that the variation in the etching rate with respect to the silicon oxide film becomes large. On the other hand, when it exceeds 30% by weight, for example, when hydrochloric acid is used, the vapor pressure becomes large, so there is a disadvantage that the chemical composition against evaporation is not stable.
- the water-soluble polymer in the component (c) is at least any selected from the group consisting of acrylic acid, ammonium acrylate, acrylic ester, acrylamide, styrene sulfonic acid, ammonium styrene sulfonate, and styrene sulfonic acid ester. Or one.
- the copolymer of ammonium acrylate and methyl acrylate is the case where the component (a) is composed of hydrogen fluoride alone or when hydrogen fluoride and ammonium fluoride are used in combination.
- the etching suppression effect on the silicon nitride film is high.
- the copolymerization ratio of ammonium acrylate and methyl acrylate is preferably in the range of 9.9: 0.1 to 5: 5. If the copolymerization ratio of methyl acrylate is larger than the above numerical range, there may be a disadvantage that the solubility of the copolymer of ammonium acrylate and methyl acrylate is reduced.
- polyacrylamide has a high etching suppression effect on the silicon nitride film, particularly when the component (a) uses hydrogen fluoride and ammonium fluoride in combination, or when hydrogen fluoride and hydrochloric acid are used in combination.
- the content of the water-soluble polymer in the component (c) is preferably in the range of 0.001 to 10% by weight with respect to the total weight of the fine processing agent, and is 0.1 to 5% by weight. It is more preferable to be within the range of%. If the content is less than 0.001% by weight, the effect of adding the water-soluble polymer is lowered, and the effect of suppressing the etch rate on the silicon nitride film becomes insufficient, such being undesirable. On the other hand, if the content exceeds 10% by weight, the metal impurities in the fine processing agent increase and the viscosity becomes high, so that the rinse removal performance of the fine processing agent with a rinse agent such as ultrapure water is lowered. As a result, it is not suitable as a fine processing agent used in the manufacturing process of a semiconductor device.
- the weight average molecular weight of the water-soluble polymer is preferably in the range of 1,000 to 1,000,000, and more preferably in the range of 1,000 to 10,000. If the weight average molecular weight is less than 1000, the amount of stabilizer used as a polymerization inhibitor is increased. As a result, it may be a cause of metal contamination to the fine processing agent. When the weight average molecular weight exceeds 1,000,000, the viscosity of the fine processing agent increases, and the handleability may deteriorate. Moreover, the rinse removal performance of the fine processing agent with a rinse agent such as ultrapure water may be reduced.
- the fine processing agent of the present embodiment can be mixed with additives other than surfactants within a range that does not impede its effect.
- additives other than surfactants include hydrogen peroxide and a chelating agent.
- the water-soluble polymer to be added may be purified by distillation, ion exchange resin, ion exchange membrane, electrodialysis, filtration, etc. Purification may be performed by filtration or the like.
- micromachining method using the micromachining agent according to the present embodiment will be described by taking wet etching as an example.
- the fine processing agent of the present embodiment is employed in various wet etching methods.
- an etching method there are an immersion method, a spray method, and the like, and the microfabrication processing agent of the present invention can be adopted in any method.
- the immersion method is preferable because the composition change of the fine processing agent is small due to evaporation in the etching process.
- the etching temperature is preferably in the range of 5 to 50 ° C., more preferably in the range of 15 to 35 ° C. It is more preferable that the temperature is within a range of 20 to 30 ° C. Within the above range, evaporation of the fine processing agent can be suppressed, and a change in composition can be prevented. In addition, it is difficult to control the etching rate due to evaporation of the fine processing agent at high temperatures, and the disadvantage is that the components in the micro processing agent are likely to crystallize at low temperatures, resulting in a decrease in etch rate and an increase in liquid particles. Can be avoided. Note that since the etch rate varies from film to film depending on the etching temperature, the difference between the etch rate for the silicon oxide film and the etch rate for the silicon nitride film may be affected.
- the etch rate for the silicon oxide film at 25 ° C. is preferably in the range of 1 to 5000 nm / min, and in the range of 15 to 1000 nm / min. Is more preferred. If the etch rate is less than 1 nm / min, it takes time for fine processing such as etching, which may lead to a decrease in production efficiency. On the other hand, if it exceeds 5000 nm / min, the controllability of the film thickness after etching and the roughness of the substrate surface (surface opposite to the surface on which the silicon oxide film etc. are formed) become remarkable, and the yield may decrease. is there.
- Etch rate for silicon oxide film and silicon nitride film The film thickness of the silicon oxide film and the silicon nitride film before and after etching was measured using an optical film thickness measuring device (Nanospec 6100, manufactured by Nanometrics Japan Co., Ltd.), and the change in film thickness due to etching was measured. The above measurement was repeated at three different etching times to calculate the etch rate.
- Example 1 7.0 parts by weight of hydrogen fluoride (manufactured by Stella Chemifa Corporation, high purity grade for semiconductor, concentration 50% by weight) and ammonium fluoride (manufactured by Stella Chemifa Corporation, high purity grade for semiconductor, concentration 40% by weight) )
- a mixed solution of 50.0 parts by weight and 40.5 parts by weight of ultrapure water
- an etching solution fine processing agent of 3.5% by weight of hydrogen fluoride, 20.0% by weight of ammonium fluoride, and 1% by weight of ammonium polyacrylate was prepared.
- Example 2 Example 2 to 10 were the same as Example 1 except that the contents of hydrogen fluoride and ammonium fluoride and the content and type of the water-soluble polymer were changed as shown in Table 1. Thus, an etching solution was prepared. Furthermore, the etching rate obtained with respect to the TEOS film and the silicon nitride film and the selectivity of the etching rate (silicon oxide film / silicon nitride film) were evaluated using the etching solution obtained in each example. The results are shown in Table 2 below.
- Comparative Examples 1 and 2 were the same as in Example 1 except that the contents of hydrogen fluoride and ammonium fluoride were changed as shown in Table 1 and no water-soluble polymer was added. Thus, an etching solution was prepared. Furthermore, using the etching solutions obtained in the respective comparative examples, the etching rate with respect to the TEOS film and the silicon nitride film and the selectivity of the etching rate (silicon oxide film / silicon nitride film) were evaluated. The results are shown in Table 2 below.
- Comparative Examples 3 to 7 In Comparative Examples 3 to 7, the contents of hydrogen fluoride and ammonium fluoride were changed as shown in Table 1, except that the additives shown in Table 1 were used instead of the water-soluble polymer.
- An etching solution was prepared in the same manner as in Example 1. Furthermore, using the etching solutions obtained in the respective comparative examples, the etching rate with respect to the TEOS film and the silicon nitride film and the selectivity of the etching rate (silicon oxide film / silicon nitride film) were evaluated. The results are shown in Table 2 below.
- the additive added to the etching solutions according to Comparative Examples 3 to 7 selectively suppresses the etch rate for the silicon nitride film and selects the etch rate for the silicon oxide film relative to the silicon nitride film.
- the ratio (silicon oxide film / silicon nitride film) could not be increased.
- the etch rate with respect to the silicon nitride film is selectively suppressed, and the etch rate of the silicon oxide film with respect to the silicon nitride film is reduced. It was confirmed that the selectivity (silicon oxide film / silicon nitride film) was increased.
- Example 11 20.0 parts by weight of hydrogen fluoride (manufactured by Stella Chemifa Co., Ltd., high-purity grade for semiconductor, concentration 50% by weight) and 27 hydrochloric acid (manufactured by Hayashi Pure Chemical Industries, Ltd., electronic industry grade, concentration 36% by weight) 27 1.0 part by weight of polyacrylamide (concentration 50% by weight, weight average molecular weight 10,000) as a water-soluble polymer was added to a solution obtained by mixing 0.8 part by weight and 51.2 parts by weight of ultrapure water, and stirred. After mixing, the temperature of the mixed solution was adjusted to 25 ° C. and left for 3 hours. As a result, an etching solution (fine processing agent) of 10% by weight of hydrogen fluoride, 10% by weight of hydrochloric acid, and 0.5% by weight of polyacrylamide was prepared.
- etching solution fine processing agent
- Example 12 In Example 12, an etching solution was prepared in the same manner as in Example 11 except that the polyacrylamide content was changed as shown in Table 3. Furthermore, using the etching solution obtained in this example, the etching rate with respect to the BPSG film and the silicon nitride film and the selectivity of the etching rate (silicon oxide film / silicon nitride film) were evaluated. The results are shown in Table 3 below.
- Comparative Example 8 In Comparative Example 8, an etching solution was prepared in the same manner as in Example 12 except that the water-soluble polymer was not added as shown in Table 3. Furthermore, using the etching solution obtained in this comparative example, the etching rate with respect to the BPSG film and the silicon nitride film and the selectivity of the etching rate (silicon oxide film / silicon nitride film) were evaluated. The results are shown in Table 3 below.
- Example 13 25.0 parts by weight of ammonium fluoride (manufactured by Stella Chemifa Co., Ltd., high purity grade for semiconductors, concentration 40% by weight) and hydrochloric acid (manufactured by Hayashi Junyaku Kogyo Co., Ltd., electronics industry grade, concentration 36% by weight) 27
- ammonium fluoride manufactured by Stella Chemifa Co., Ltd., high purity grade for semiconductors, concentration 40% by weight
- hydrochloric acid manufactured by Hayashi Junyaku Kogyo Co., Ltd., electronics industry grade, concentration 36% by weight
- Comparative Example 9 an etching solution was prepared in the same manner as in Example 13 except that the water-soluble polymer was not added as shown in Table 4. Furthermore, using the etching solution obtained in this comparative example, the etch rate with respect to the TEOS film and the silicon nitride film and the selectivity of the etch rate (silicon oxide film / silicon nitride film) were evaluated. The results are shown in Table 4 below.
- Example 14 25.0 parts by weight of ammonium fluoride (manufactured by Stella Chemifa Co., Ltd., high purity grade for semiconductor, concentration 40% by weight) and phosphoric acid (manufactured by Kishida Chemical Co., Ltd., electronics industry grade, concentration 85% by weight)
- ammonium fluoride manufactured by Stella Chemifa Co., Ltd., high purity grade for semiconductor, concentration 40% by weight
- phosphoric acid manufactured by Kishida Chemical Co., Ltd., electronics industry grade, concentration 85% by weight
- Comparative Example 10 Comparative Example 10, as shown in Table 4, an etching solution was prepared in the same manner as in Example 14 except that the water-soluble polymer was not added. Furthermore, using the etching solution obtained in this comparative example, the etch rate with respect to the TEOS film and the silicon nitride film and the selectivity of the etch rate (silicon oxide film / silicon nitride film) were evaluated. The results are shown in Table 4 below.
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Abstract
Description
即ち、本発明によれば、シリコン酸化膜とシリコン窒化膜が少なくとも積層された積層膜に対し、シリコン酸化膜のみを選択的に微細加工処理することができるので、例えば半導体装置、液晶表示装置、マイクロマシンデバイス等の製造に於いて好適な微細加工を可能にする。
本実施の形態に係る本発明に係る微細加工処理剤は、(a)フッ化水素又はフッ化アンモニウムの少なくとも何れか1種類と、(b)水と、(c)水溶性重合体とを含む。
光学式膜厚測定装置(ナノメトリクスジャパン(株)社製、Nanospec6100)を用いてエッチング前後のシリコン酸化膜、及びシリコン窒化膜の膜厚を測定し、エッチングによる膜厚の変化を測定した。3つの異なるエッチング時間に於いて前記測定を繰り返し実施し、エッチレートを算出した。
後述する各実施例において使用した水溶性重合体、及び各比較例において使用した添加剤は下記表1に示す通りである。
フッ化水素(ステラケミファ(株)製、半導体用高純度グレード、濃度50重量%)7.0重量部と、フッ化アンモニウム(ステラケミファ(株)製、半導体用高純度グレード、濃度40重量%)50.0重量部と、超純水40.5重量部とを混合した溶液に、水溶性重合体としてのポリアクリル酸アンモニウム(濃度40重量%、重量平均分子量6000)2.5重量部を添加し、攪拌混合した後、混合液を25℃に調温し3時間静置した。これにより、フッ化水素3.5重量%、フッ化アンモニウム20.0重量%、ポリアクリル酸アンモニウム1重量%のエッチング液(微細加工処理剤)を調製した。
実施例2~10に於いては、表1に示す通りにフッ化水素及びフッ化アンモニウムの含有量と、水溶性重合体の含有量及び種類を変更したこと以外は、前記実施例1と同様にしてエッチング液を調製した。更に、各実施例で得られたエッチング液を用いて、TEOS膜及びシリコン窒化膜に対するエッチレート、エッチレートの選択比(シリコン酸化膜/シリコン窒化膜)を評価した。結果を下記表2に示す。
比較例1~2に於いては、表1に示す通りにフッ化水素及びフッ化アンモニウムの含有量を変更し、かつ水溶性重合体を添加しなかったこと以外は、前記実施例1と同様にしてエッチング液を調製した。更に、各比較例で得られたエッチング液を用いて、TEOS膜及びシリコン窒化膜に対するエッチレート、エッチレートの選択比(シリコン酸化膜/シリコン窒化膜)を評価した。結果を下記表2に示す。
比較例3~7に於いては、表1に示す通りにフッ化水素及びフッ化アンモニウムの含有量を変更し、水溶性重合体に代えて、表1に示す添加剤を用いたこと以外は、前記実施例1と同様にしてエッチング液を調製した。更に、各比較例で得られたエッチング液を用いて、TEOS膜及びシリコン窒化膜に対するエッチレート、エッチレートの選択比(シリコン酸化膜/シリコン窒化膜)を評価した。結果を下記表2に示す。
フッ化水素(ステラケミファ(株)製、半導体用高純度グレード、濃度50重量%)20.0重量部と、塩酸(林純薬工業(株)製、電子工業グレード、濃度36重量%)27.8重量部と、超純水51.2重量部とを混合した溶液に、水溶性重合体としてのポリアクリルアミド(濃度50重量%、重量平均分子量10000)1.0重量部を添加し、攪拌混合した後、混合液を25℃に調温し3時間静置した。これにより、フッ化水素10重量%、塩酸10重量%、ポリアクリルアミド0.5重量%のエッチング液(微細加工処理剤)を調製した。
実施例12に於いては、表3に示す通りにポリアクリルアミドの含有量を変更したこと以外は、前記実施例11と同様にしてエッチング液を調製した。更に、本実施例で得られたエッチング液を用いて、BPSG膜及びシリコン窒化膜に対するエッチレート、エッチレートの選択比(シリコン酸化膜/シリコン窒化膜)を評価した。結果を下記表3に示す。
比較例8に於いては、表3に示す通りに水溶性重合体を添加しなかったこと以外は、前記実施例12と同様にしてエッチング液を調製した。更に、本比較例で得られたエッチング液を用いて、BPSG膜及びシリコン窒化膜に対するエッチレート、エッチレートの選択比(シリコン酸化膜/シリコン窒化膜)を評価した。結果を下記表3に示す。
フッ化アンモニウム(ステラケミファ(株)製、半導体用高純度グレード、濃度40重量%)25.0重量部と、塩酸(林純薬工業(株)製、電子工業グレード、濃度36重量%)27.8重量部と、超純水45.2重量部とを混合した溶液に、水溶性重合体としてのポリアクリルアミド(濃度50重量%、重量平均分子量10000)2.0重量部を添加し、撹拌混合した後、混合液を25℃に調温し3時間静置した。これにより、フッ化アンモニウム10重量%、塩酸10重量%、ポリアクリルアミド1重量%のエッチング液(微細加工処理剤)を調製した。
比較例9に於いては、表4に示す通りに水溶性重合体を添加しなかったこと以外は、前記実施例13と同様にしてエッチング液を調製した。更に、本比較例で得られたエッチング液を用いて、TEOS膜及びシリコン窒化膜に対するエッチレート、エッチレートの選択比(シリコン酸化膜/シリコン窒化膜)を評価した。結果を下記表4に示す。
フッ化アンモニウム(ステラケミファ(株)製、半導体用高純度グレード、濃度40重量%)25.0重量部と、リン酸(キシダ化学(株)製、電子工業グレード、濃度85重量%)23.5重量部と、超純水49.5重量部とを混合した溶液に、水溶性重合体としてのポリアクリルアミド(濃度50重量%、重量平均分子量10000)2.0重量部を添加し、撹拌混合した後、混合液を25℃に調温し3時間静置した。これにより、フッ化アンモニウム10重量%、リン酸20重量%、ポリアクリルアミド1重量%のエッチング液(微細加工処理剤)を調製した。
比較例10に於いては、表4に示す通り、水溶性重合体を添加しなかったこと以外は、前記実施例14と同様にしてエッチング液を調製した。更に、本比較例で得られたエッチング液を用いて、TEOS膜及びシリコン窒化膜に対するエッチレート、エッチレートの選択比(シリコン酸化膜/シリコン窒化膜)を評価した。結果を下記表4に示す。
Claims (16)
- (a)0.01~15重量%のフッ化水素、又は0.1~40重量%のフッ化アンモニウムの少なくとも何れか1種類と、
(b)水と、
(c)0.001~10重量%のアクリル酸、アクリル酸アンモニウム、アクリル酸エステル、アクリルアミド、スチレンスルホン酸、スチレンスルホン酸アンモニウム、及びスチレンスルホン酸エステルからなる群より選択される少なくとも何れか1種の水溶性重合体とを含むことを特徴とする微細加工処理剤。 - 前記水溶性重合体がアクリル酸アンモニウムとアクリル酸メチルの共重合体であることを特徴とする請求の範囲第1項に記載の微細加工処理剤。
- 前記水溶性重合体がポリアクリルアミドであることを特徴とする請求の範囲第1項に記載の微細加工処理剤。
- 前記水溶性重合体の重量平均分子量が1000~100万の範囲内であることを特徴とする請求の範囲第1項に記載の微細加工処理剤。
- シリコン酸化膜に対する25℃でのエッチレートが1~5000nm/分の範囲内であることを特徴とする請求の範囲第1項に記載の微細加工処理剤。
- 前記微細加工処理剤が界面活性剤を含むことを特徴とする請求の範囲第1項に記載の微細加工処理剤。
- 前記界面活性剤の添加量が0.001~0.1重量%であることを特徴とする請求の範囲第1項に記載の微細加工処理剤。
- 前記(a)成分がフッ化水素のみからなり、前記界面活性剤がポリエチレングリコールアルキルエーテル、ポリエチレングリコールアルキルフェニルエーテル、及びポリエチレングリコール脂肪酸エステルからなる群より選択される少なくとも何れか1種の非イオン界面活性剤であることを特徴とする請求の範囲第6項に記載の微細加工処理剤。
- 前記(a)成分がフッ化水素酸及びフッ化アンモニウム、またはフッ化アンモニウムのみからなり、前記界面活性剤が脂肪族アルコール、脂肪族カルボン酸、ハイドロフルオロアルキルアルコール、ハイドロフルオロアクキルカルボン酸、ハイドロフルオロアクキルカルボン酸の塩、脂肪族アミン塩、及び脂肪族スルホン酸からなる群より選択される少なくとも何れか1種であることを特徴とする請求の範囲第6項に記載の微細加工処理剤。
- 前記(a)成分には無機酸が含まれることを特徴とする請求の範囲第1項に記載の微細加工処理剤。
- 前記無機酸の添加量が0.01~30重量%であることを特徴とする請求の範囲第1項に記載の微細加工処理剤。
- 前記(a)成分には有機酸が含まれないことを特徴とする請求の範囲第1項に記載の微細加工処理剤。
- 請求の範囲第1項に記載の微細加工処理剤を用いて、少なくともシリコン酸化膜、及びシリコン窒化膜が積層された積層膜を微細加工することを特徴とする微細加工処理方法。
- 前記シリコン酸化膜は、自然酸化膜、熱シリコン酸化膜、ノンドープシリケートガラス膜、リンドープシリケートガラス膜、ボロンドープシリケートガラス膜、リンボロンドープシリケートガラス膜、TEOS膜、又はフッ素含有シリコン酸化膜の何れかであることを特徴とする請求の範囲第13項に記載の微細加工処理方法。
- 前記シリコン窒化膜は、シリコン窒化膜、又はシリコン酸窒化膜であることを特徴とする請求の範囲第13項に記載の微細加工処理方法。
- 前記微細加工処理剤は、その液温を5~50℃の範囲内で使用することを特徴とする請求の範囲第13項に記載の微細加工処理方法。
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US20130244444A1 (en) * | 2012-03-16 | 2013-09-19 | Fujifilm Corporation | Method of producing a semiconductor substrate product and etching liquid |
CN106587649A (zh) * | 2016-12-31 | 2017-04-26 | 庞绮琪 | Tft玻璃基板薄化工艺预处理剂 |
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Also Published As
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US20120056126A1 (en) | 2012-03-08 |
US8974685B2 (en) | 2015-03-10 |
EP2434536A1 (en) | 2012-03-28 |
EP2434536A4 (en) | 2012-12-19 |
KR20120018335A (ko) | 2012-03-02 |
EP2434536B1 (en) | 2019-03-13 |
SG176129A1 (en) | 2011-12-29 |
CN102428547A (zh) | 2012-04-25 |
CN102428547B (zh) | 2014-12-10 |
KR101560433B1 (ko) | 2015-10-14 |
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