WO2004105115A1 - シリコン窒化膜を形成するcvd方法 - Google Patents
シリコン窒化膜を形成するcvd方法 Download PDFInfo
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- WO2004105115A1 WO2004105115A1 PCT/JP2004/007311 JP2004007311W WO2004105115A1 WO 2004105115 A1 WO2004105115 A1 WO 2004105115A1 JP 2004007311 W JP2004007311 W JP 2004007311W WO 2004105115 A1 WO2004105115 A1 WO 2004105115A1
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- WIPO (PCT)
- Prior art keywords
- period
- gas
- silicon nitride
- nitride film
- forming
- Prior art date
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- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 99
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 99
- 238000000034 method Methods 0.000 title claims abstract description 87
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910000077 silane Inorganic materials 0.000 claims abstract description 28
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 21
- 239000000758 substrate Substances 0.000 claims abstract description 20
- 239000007789 gas Substances 0.000 claims description 247
- 238000012545 processing Methods 0.000 claims description 46
- 229930195733 hydrocarbon Natural products 0.000 claims description 33
- 150000002430 hydrocarbons Chemical class 0.000 claims description 33
- 239000004215 Carbon black (E152) Substances 0.000 claims description 32
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 12
- 229910052710 silicon Inorganic materials 0.000 claims description 12
- 239000010703 silicon Substances 0.000 claims description 12
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 6
- 239000005977 Ethylene Substances 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 5
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 4
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims description 3
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 2
- 239000001273 butane Substances 0.000 claims description 2
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 2
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 claims description 2
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 2
- 239000001294 propane Substances 0.000 claims description 2
- GOLAKLHPPDDLST-HZJYTTRNSA-N (9z,12z)-octadeca-9,12-dien-1-amine Chemical compound CCCCC\C=C/C\C=C/CCCCCCCCN GOLAKLHPPDDLST-HZJYTTRNSA-N 0.000 claims 1
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 claims 1
- PZPGRFITIJYNEJ-UHFFFAOYSA-N disilane Chemical compound [SiH3][SiH3] PZPGRFITIJYNEJ-UHFFFAOYSA-N 0.000 claims 1
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 claims 1
- HIAZFYQNGXRLTF-UHFFFAOYSA-N tributylsilane Chemical compound CCCC[SiH](CCCC)CCCC HIAZFYQNGXRLTF-UHFFFAOYSA-N 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 50
- 229910000069 nitrogen hydride Inorganic materials 0.000 abstract 1
- 239000010408 film Substances 0.000 description 148
- 238000005530 etching Methods 0.000 description 73
- LXEXBJXDGVGRAR-UHFFFAOYSA-N trichloro(trichlorosilyl)silane Chemical compound Cl[Si](Cl)(Cl)[Si](Cl)(Cl)Cl LXEXBJXDGVGRAR-UHFFFAOYSA-N 0.000 description 38
- 230000000052 comparative effect Effects 0.000 description 29
- 238000000151 deposition Methods 0.000 description 27
- 230000008021 deposition Effects 0.000 description 26
- 238000002474 experimental method Methods 0.000 description 23
- 238000002407 reforming Methods 0.000 description 22
- 235000012431 wafers Nutrition 0.000 description 17
- 230000004048 modification Effects 0.000 description 16
- 238000012986 modification Methods 0.000 description 16
- 238000004140 cleaning Methods 0.000 description 10
- 239000004065 semiconductor Substances 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 238000002230 thermal chemical vapour deposition Methods 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 238000007796 conventional method Methods 0.000 description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 125000004432 carbon atom Chemical group C* 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000005121 nitriding Methods 0.000 description 4
- 239000010453 quartz Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- 125000004429 atom Chemical group 0.000 description 3
- 239000000356 contaminant Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 150000004767 nitrides Chemical class 0.000 description 3
- 238000010926 purge Methods 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910018540 Si C Inorganic materials 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 102000007469 Actins Human genes 0.000 description 1
- 108010085238 Actins Proteins 0.000 description 1
- 102000004856 Lectins Human genes 0.000 description 1
- 108090001090 Lectins Proteins 0.000 description 1
- 229910014299 N-Si Inorganic materials 0.000 description 1
- 229920006153 PA4T Polymers 0.000 description 1
- 241001454667 Perga Species 0.000 description 1
- -1 Phospho Silicate Chemical class 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 241000705989 Tetrax Species 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000002523 lectin Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011553 magnetic fluid Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- VYIRVGYSUZPNLF-UHFFFAOYSA-N n-(tert-butylamino)silyl-2-methylpropan-2-amine Chemical compound CC(C)(C)N[SiH2]NC(C)(C)C VYIRVGYSUZPNLF-UHFFFAOYSA-N 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000003685 thermal hair damage Effects 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
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/0262—Reduction or decomposition of gaseous compounds, e.g. CVD
-
- 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
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
- H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
- H01L21/02271—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/34—Nitrides
- C23C16/345—Silicon nitride
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
-
- 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
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
- H01L21/02123—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon
- H01L21/0217—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon the material being a silicon nitride not containing oxygen, e.g. SixNy or SixByNz
-
- 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
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/02205—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition
- H01L21/02208—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si
- H01L21/02211—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si the compound being a silane, e.g. disilane, methylsilane or chlorosilane
-
- 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
- H01L21/31—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
- H01L21/314—Inorganic layers
- H01L21/318—Inorganic layers composed of nitrides
- H01L21/3185—Inorganic layers composed of nitrides of siliconnitrides
Definitions
- the present invention relates to a CVD method and apparatus for forming a silicon nitride film on a substrate to be processed.
- SiO 2 , PSG (Phospho Silicate ⁇ iass) ⁇ P (formed by plasma CVD) – S SiO, P (formed by plasma CVD) one S i n, SOG (S in O n G lass), S i 3 n 4 ( Shi Li co down nitride film) or the like is used.
- silicon nitride films are often used because they have relatively better insulation properties than silicon oxide films and can function well as etching stopper films. There is a tendency.
- SiH4 monosilane
- DCS dichloromethane
- Si silicon source gas
- H 2 C 12 hexacyclodisilane
- HD Si 2 C 16
- BBAS bis-tert-butylamino silane
- the silicon nitride film is deposited by thermal CVD
- the silicon nitride film is deposited at a high temperature of about 760 ° C.
- the temperature may be lowered to about 600 ° C, and deposition may be performed by thermal CVD.
- a film and an insulating film as described above are laminated on each other, and a multilayer structure is formed while performing pattern etching.
- contaminants are such organic substances and c 1 ⁇ ⁇ I cycle the surface of the field ⁇ the insulating film that form another thin film ⁇ on this after forming the insulating film is adhered
- a cleaning process is performed to remove this contaminant.
- the surface of the insulating film is etched by immersing the semiconductor wafer in a cleaning solution of dilute hydrofluoric acid.o As a result, the surface of the insulating film is removed very thinly to remove contaminants. Remove.
- the etching rate at the time of cleaning the insulating film becomes considerably small. Therefore, the insulating film is not excessively removed at the time of cleaning, and the cleaning process can be performed with good controllability of the film thickness.
- the insulating film is formed by CVD at a low temperature of, for example, about 600 ° C., the etching rate at the time of cleaning the insulating film is considerably large. As a result, the insulating film may be excessively removed during talling, resulting in poor control of the film thickness during the quenching process.
- the silicon nitride film may be used as an etching stop film, and the o field ⁇ and the etching rate of the silicon nitride film need to be sufficiently small. There is. However, conventional methods cannot respond to this 5%.
- a first aspect of the present invention is a CVD method for forming a silicon nitride film.
- a silane-based gas and an ammonia gas are supplied into the processing chamber, and the silicon nitride film is formed on the substrate by cVD.
- the step of forming the silicon nitride film includes the steps of: supplying a HU silane-based gas into the processing chamber; and supplying the silane-based gas to the processing chamber. The second period in which to stop and the period are alternately provided.
- a second aspect of the present invention is a CVD method for forming a silicon nitride film, While treating the substrate containing the substrate, the silane-based gas, ammonia gas, and hydrocarbon gas were fed into the processing chamber while the substrate was being stored. Silicon nitride film on substrate
- Forming a silicon nitride film wherein the step of forming the silicon nitride film comprises: a first period of supplying the silane-based gas into the processing chamber; And a second period in which the supply of gas is stopped is alternately provided.
- the first period can have a length equal to or less than the second period.
- the first period of fu B is set within the range of 15 to 60 seconds
- the second period is
- the step of forming the silicon nitride film includes supplying the ammonia gas into the processing chamber.
- a third period in which the PR is performed and a fourth period in which the supply of the ammonia gas is stopped can be alternately provided.
- the step of forming the silicon nitride film alternates between a third period for supplying the ammonia gas and a fourth period for stopping the supply of the ammonia gas.
- a fifth period in which the hydrocarbon gas is supplied into the processing chamber and a sixth period in which the supply of the hydrocarbon gas is stopped can be alternately provided.
- the step of forming the silicon nitride film is performed by first using at least one of the silane-based gas and the hydrocarbon gas. It is desirable to supply.
- FIG. 1 is a sectional view showing a CVD apparatus according to an embodiment of the present invention.
- FIGS. 2A, 2B, and 2C are timing charts showing gas supply patterns according to the first and second embodiments of the present invention and a conventional technique, respectively.
- FIG. 3A is a graph showing the dependency of the etching rate of the silicon nitride film on the gas supply pattern according to the first and second embodiments.
- FIG. 3B is a graph showing the dependency of the etching rate of the silicon nitride film on the NH 3 gas flow rate according to the first embodiment.
- 4A and 4B are timing charts showing a gas supply pattern according to the third embodiment of the present invention and its modification.
- FIG. 5 is a timing chart showing a gas supply pattern according to a fourth embodiment of the present invention.
- FIG. 6A is a graph showing the dependence of the etching rate of a silicon nitride film on the length of a deposition period according to the fourth embodiment.
- FIG. 6B is a graph showing the dependency of the etching rate of the silicon nitride film on the length of the modification period according to the fourth embodiment.
- FIGS. 7A, 7B, 7C, and 7D are timing charts showing gas supply patterns according to fifth, sixth, seventh, and eighth embodiments of the present invention, respectively.
- FIG. 8 is a graph showing the dependence of the etching rate of the silicon nitride film on the gas supply pattern according to the fifth to eighth embodiments.
- FIG. 9 shows a series of process pressures for the fifth embodiment.
- a graph showing the dependency of the etch rate of the con-nitride film.
- FIG. 10 is a graph showing the dependency of the silicon nitride film etching rate on the intermittent period pressure in the fifth embodiment.
- FIG. 11 is a graph showing the relationship between the gas supply pattern and the in-plane uniformity of the silicon nitride film thickness in the fifth to eighth embodiments.
- the present inventors have studied the etching rate when etching a silicon nitride film.
- the intermittent supply of a silicon-based gas which is a silicon source gas of the silicon nitride film, enables the etching gray during cleaning. And found that it is possible to reduce the amount of heat.
- the present invention relates to
- FIG. 1 is a plan view showing a CVD apparatus according to an embodiment of the present invention.
- This CVD apparatus 2 is composed of a first gas substantially composed of a silane-based gas (silicon source gas) and a first gas substantially composed of a chemical gas. And a third gas substantially consisting of a hydrocarbon gas are supplied simultaneously to form a silicon nitride film.
- a hydrocarbon gas is supplied into the film. Contains carbon component.
- the CVD apparatus 2 has a cylindrical inner cylinder 4 made of quartz, and an outer cylinder 6 made of quartz concentrically arranged outside the inner cylinder 4 with a predetermined gap 10 therebetween.
- the treatment room 8 has a double pipe structure.
- the outside of the processing chamber 8 is covered with a heating cover 16 provided with a heating means 12 such as a heating heater and a heat insulating material 14.
- the heating means 12 is disposed on the entire inner surface of the heat insulating material 14.
- the inner diameter of the inner cylinder 4 of the processing chamber 8 is about 240 mm and the height is about 130 mm, and the volume of the processing chamber 8 is about 110 mm. It is about the title.
- the lower end of the processing chamber 8 is supported by a cylindrical manifold 18 made of, for example, stainless steel.
- the lower end of the inner cylinder 4 is supported by a ring-shaped support plate 18A protruding inward from the inner wall of the main holder 18.
- a quartz wafer port 20 on which semiconductor wafers W to be processed are mounted in multiple stages is loaded Z unloaded into the processing chamber 8 from the downward force of the manifold 18.
- about 100 to 150 wafers each having a diameter of 200 mm can be supported on the evaporator 20 in multiple stages at a substantially equal pitch.
- the size and the number of wafers W are not limited to those described above. It can also be applied to O mm wafers.
- the wafer boat 20 is placed on a rotating tape 24 via a heat insulating tube 22 made of quartz.
- the rotary table 24 is supported on a rotary shaft 28 that penetrates a lid 26 that opens and closes the lower end opening of the manifold 18.
- a magnetic fluid seal 30 is interposed in the penetrating portion of the rotating shaft 28, and the rotating shaft 28 is rotatably supported in a hermetically sealed state.
- a sealing member 32 made of, for example, an O-ring is provided between the periphery of the lid 26 and the lower end of the manifold 18 to maintain the sealing in the processing chamber 8. .
- the rotating shaft 28 is attached to the tip of an arm 36 supported by, for example, a lifting mechanism 34 of a boat elevator.
- Lifting mechanism 34 of a boat elevator.
- the exhaust port 38 is connected to a vacuum exhaust unit 39 provided with a vacuum pump or the like.
- a gas supply section 40 for supplying a predetermined processing gas into the inner cylinder 4 is disposed on the side of the manifold 18.
- the gas supply section 40 includes a silane-based gas supply system 42, a nitriding gas supply system 44, and a hydrogen ash gas supply system 46.
- Each of the gas supply systems 42, 44 ⁇ ⁇ 46 has a linear gas nozzle 48, 552 provided through the side wall of the manifold 18.
- Mass flow control is provided for each gas nozzle 48, 50, 52.
- the gas flow paths 60, 62, and 64 are connected to the flow controllers 54, 56, and 58, respectively, respectively.
- HCD gas power S is used as a silane-based gas (silicon source gas)
- NH 3 gas is used as a nitriding gas
- hydrocarbons! Ethylene (C 2 H 4 ) gas is used as the gas
- the gas supply unit 40 includes a pergas supply system 72 for supplying a purge gas.
- the purge gas supply system 72 is connected to the side of the manifold 18 by a gas flow path 76 through a flow controller 74 such as a mass flow controller, which is a P-controller.
- a flow controller 74 such as a mass flow controller, which is a P-controller.
- an inert gas such as N 2 is used.
- the processing recipe of the CVD process for example, the thickness of the silicon nitride film to be formed, which is previously considered in the storage section 5 s of the PU 5, can be adjusted in accordance with the J thickness.
- the relationship between the processing gas flow and the thickness of the silicon nitride film is preliminarily recorded as control data, and the CPU 5 transmits the stored processing recipe and control data to these stored processing recipes and control data. It is possible to control the gas supply section 40, etc.
- the cVD device loads the wafer and puts it in a good machine state.
- the process temperature in process 8 is maintained at a process temperature of, for example, about 500 ° C.
- a large number of pieces for example, 100 pieces of quenches W, for example, are mounted at room temperature. Is raised into the processing chamber 8 from below, and is then moved into the processing chamber 8 by ⁇ . Then, in the section 26, the nozzle is closed, and the opening of the lower itfB in the section 18 is closed. To seal the inside of the processing chamber 8
- the inside of the processing chamber 8 is evacuated to maintain a predetermined process pressure, and at the same time, the process speed for film formation is raised.
- the nozzles of the gas supply section 40 are controlled while controlling the flow rates of the predetermined silane-based gas, HCD gas, ammonia gas, which is a nitriding gas, and ethylene gas, which is a hydrocarbon gas. Supply, 50, 52 power, etc. At this time, a silicon nitride film is formed using a gas supply pattern according to the embodiment described below.
- FIGS. 2A, 2B, and 2C are timing charts showing gas supply patterns according to the first and second embodiments of the present invention and the prior art, respectively.
- HCD gas which is a silane-based gas
- FIGS. 2A and 2B HCD gas, which is a silane-based gas
- NH 3 gas and C 2 H 4 gas are continuously supplied.
- FIG. 2B while C 2 H 4 gas is supplied continuously, NH 3 gas is supplied intermittently in synchronization with the HCD gas.
- HCD gas and NH 3 gas are During a single simultaneous supply period (deposition period) ⁇ 1, a silicon nitride film containing ash is deposited on the surface of the wafer w. In addition, the silicon nitride film deposited immediately before in the intermittent period (reforming period) ⁇ 2 where the supply of the HCD gas is stopped is performed.
- the deposition period T 1 and the modification period T 2 are alternately repeated, and a silicon-containing silicon nitride film is formed in multiple layers.
- one deposition period T 1 and one modification period T 2 are defined as one cycle, and the number of cycles is determined according to the film thickness to be deposited. .
- the process temperature is constant at 600 ° C.
- the process pressure is the simultaneous supply period ⁇
- the reforming period ⁇ 2 is about 60 seconds, for example.
- a silicon nitride film is formed, for example, C 2 H gas is supplied as a hydrocarbon gas into the processing vessel 8 to form a silicon nitride film on the surface.
- the resulting silicon nitride film contains carbon components.
- the conventional film forming temperature for example, 760 is obtained.
- the film was formed at a temperature lower than about c, for example, at 600 ° C., it is rarely used during the tangling or etching of the surface of the silicon nitride film.
- the etchant rate for hydrofluoric acid can be reduced.
- the silicon nitride film is prevented from being excessively removed during the cleaning process, and the controllability of the film thickness can be improved.
- the silicon nitride film has a sufficient function as an etch stop film. You will be able to accomplish it.
- the reforming period T2 is provided by intermittently supplying the HCD gas.
- the surface of the silicon nitride film formed immediately before each modification period T 2 is modified in the modification period T 2 to improve the film quality.
- the etching rate of the silicon nitride film can be further suppressed.
- the effect at the atomic level during the reforming process is considered as follows. That is, when a silicon nitride film containing carbon atoms is formed, one atom that cannot be desorbed during deposition in the HCD gas is bonded to the outermost surface of the thin film in an activated state.
- the gas such as the HCD gas when the gas such as the HCD gas is intermittently supplied, the gas consumption can be reduced as compared with the case where all the gases such as the ammonia HCD gas are simultaneously and continuously supplied for a long time. Further, in this case, it is possible to improve the inter-plane and in-plane uniformity of the film thickness.
- the process temperature was 600 ° C.
- the flow rate of NH 3 gas was 600 sccm
- the flow rate of HCD gas was 200 ° C.
- the flow rate of 0 sccm and C 2 H 4 gas was set to 600 sccm.
- the deposition period T1 was 30 seconds
- the modification period T2 was 60 seconds.
- the process pressure during the deposition period T 1 was set at 27 Pa (0.2 T orr), and the process pressure during the reforming period T 2 was set at 53 32 Pa (4 T orr).
- a carbon-containing silicon nitride film was formed under such conditions.
- Comparative Example C 1 of the prior art the process temperature is 6 0 0 ° C, process pressure is 2 7 P a (0. 2 T orr), NH 3 gas flow rate 6 0 0 sccm, the flow rate of the HCD gas was set to 20 sccm.
- the C 2 H 4 gas was not supplied, and the NH 3 gas and the HCD gas were continuously supplied.
- a silicon nitride film containing no carbon was formed under such conditions.
- the films of Examples E11, E21 and Comparative Example C1 formed in this manner were immersed in an etching solution and etched.
- the etching solution was 0.1% HF solution (99.9% is H 2 O), the etching temperature was room temperature, and the etching time was 30 seconds.
- FIG. 3A is a graph showing the comparison between the etching rates of the films obtained in Examples E11 and E21 and Comparative Example C1. As shown in FIG. 3A, in the case of Comparative Example C1, The etching rate was a very large value of 3.41 nm / min. In contrast, Example E according to the first embodiment
- Example E21 In the case of 11, the value was 0.97 nm / min, and in the case of Example E21 according to the second embodiment, the value was 0.60 nm / min. That is, in Examples E11 and E21, the etching rate was considerably suppressed as compared with Comparative Example C1.
- Example E21 was able to suppress the etching rate more than that of Example E11 was as follows. That is, in Example E 21 according to the second embodiment, the supply of the NH 3 gas and the HCD gas is stopped during the reforming period T 2, and only the C 2 H 4 gas is supplied. In this case ⁇
- Example E12 a silicon nitride film was formed by reducing the flow rate of NH 3 gas to 100 sccm, and the etching rate was evaluated.
- the other process and viewing conditions were the same as described for Figure 3A.
- FIG. 3B shows the etching rate of the film obtained in this experiment according to Example E12, which was obtained in Example E11 (NH 3 gas).
- the flow rate of the gas is 600 sccm), which is a graph shown in comparison with the etching rate of the film of Comparative Example C1.
- the etching rate was reduced by reducing the flow rate of NH 3 gas from 600 sccm (Example El) to 100 sccm (Example El2).
- the force decreased to 0.77 nra / min, and 0.75 nm Zmin. For this reason, it was found that reducing the NH 3 gas was effective to some extent, but not as effective as the gas supply pattern of the second embodiment.
- a preferable range of the deposition period T1 is 15 seconds to 60 seconds, and a more preferable range is 15 seconds to 30 seconds. If the deposition period is shorter than T 1 force S 15 seconds, not only will the silicon nitride film not be deposited sufficiently, but it will also take a long time to achieve the target film thickness, resulting in a high throughput. Is not realistic. On the other hand, if the deposition period 1 is longer than 60 seconds, the amount of C 1 element taken into the silicon nitride film increases, and this modification cannot be performed in + minutes.
- the length of the reforming period T 2 is set to be longer than the length of the deposition period T 1.
- the preferable range of the reforming period T2 is 30 seconds to 180 seconds, and the more preferable range is 30 seconds to 60 seconds. If the reforming period T 2 is shorter than 30 seconds, problems such as insufficient removal of NH 3 , HCD and C 2 H 4 gas, or insufficient reforming treatment may occur. On the other hand, if the reforming period is longer than T2 180 seconds, one cycle The length of the file becomes long and it is not realistic from a throughput perspective.
- the process temperature was examined.
- the preferred range of process temperature is 450 to 60
- the silicon nitride film cannot be formed sufficiently by thermal CVD.
- FIG. 4A and 4B are timing charts showing a gas supply pattern according to the third embodiment of the present invention and its modification.
- NH 3 gas is continuously supplied, and C 2 H 4 gas, which is a hydrocarbon gas, is intermittently supplied in synchronization with intermittent supply of HCD gas.
- C 2 H 4 gas which is hydrogen ash gas, is supplied in the opposite direction to the intermittent supply of HCD gas. Supply intermittently with a cruise. That is, in FIG. 4B, ⁇
- the hydrocarbon gas is C 2
- H 4 (ethylene) is exemplified.
- one or more selected from the group consisting of acetylene, ethylene, methane, ethane, propane, and butane as the hydrocarbon gas Gas can be used.
- ethane as a hydrocarbon gas it is preferable to supply it into the processing vessel 8 after preheating it to about 50 ° to 100 ° C.
- a hydrocarbon gas such as C 2 H 4 gas is supplied to flow the silicon nitride film.
- a carbon component is contained in the nitride film.
- a silicon nitride film is formed by intermittently supplying a silane-based gas without flowing a hydrocarbon gas. In this case, the etching rate can be suppressed.
- FIG. 5 is a timing chart showing a gas supply pattern according to the fourth embodiment of the present invention.
- no hydrocarbon gas is used here, and ammonia gas is continuously supplied, and, for example, HCD gas is intermittently supplied as a silane-based gas.
- the simultaneous supply period of both gases is the deposition period T1
- the intermittent period during which the supply of the HCD gas is stopped and only the NH 3 gas flows is the reforming period T2.
- Such a film forming process can be easily realized by completely shutting off the hydrocarbon gas supply system 46 in the film forming apparatus shown in FIG.
- the silicon nitride film does not contain carbon atoms.
- the thin silicon nitride film deposited during the deposition period T 1 was modified by NH 3 gas immediately after the modification period T 2, and the C 1 element on the outermost surface was changed to the N element. Will be replaced.
- the silicon nitride film finally formed is etched. Chingleates can be suppressed.
- the process temperature was 600 ° C.
- the flow rate of NH 3 gas was 900 sccm
- the flow rate of HCD gas was 3 0 sccm.
- the reforming period T 2 in FIG. 5 is constant at 60 seconds
- the deposition period T 1 is different values in Examples E 41, E 42 and E 43 from 60 seconds and 3 seconds, respectively.
- the process pressure during the deposition period T 1 is 27 Pa (H 2 .2 T rr), and the process pressure during the
- Comparative Example C1 In Comparative Example C1 according to the prior art, the process temperature was 600 ° C., the process pressure was 27 Pa (0.2 Torr), the flow rate of NH 3 gas was 600 sccm, and HCD gas was used. The flow rate was 20 sccm.
- the NH 3 gas and the HCD gas were continuously supplied without supplying the C 2 H 4 gas. That is, the comparative example C1 is the same as the comparative example C1 described with reference to FIG. 3A.
- the films of Examples E41, E42, E43 and Comparative Example C1 formed in this manner were immersed in an etching solution and etched.
- the etching solution is 0.1% HF solution (99.9% is H 2 O), the etching temperature is room temperature, and the etching time is 30 seconds. Was.
- FIG. 6A is a graph showing the comparison between the etching rates of the films obtained in this experiment according to Examples E41, E42, E43, and Comparative Example C1.
- the etching rate was a very large value of 3.41 nmZmin.
- the etching rate was 3.1 nm / min, which was slightly lower than Comparative Example C1 ( A little effect appeared).
- the etching rates were 2.28 nm / min and 1.8 nm / min, respectively. Decreased
- Example E44 In order to examine the dependence of the etching rate of the silicon nitride film on the length of the modification period T 2, an additional experiment was performed using the gas supply pattern according to the fourth embodiment.
- the deposition period T1 was 30 seconds
- the modification period T2 was 180 seconds.
- Other process conditions and etching conditions were the same as those described with reference to FIG. 6A.
- FIG. 6B shows the etching rate of the film obtained in this experiment according to Example E44, which was obtained in Example E44 (deposition period T1 force S30 seconds, modification period T30). 2 is 60 seconds), according to Comparative Example C 1
- the etch rate of Example E42 (reforming period T2 was 60 seconds) was 2.28 nm / min, while Example E44 ( In the modification period T2 force (S180 seconds), the lectin concentration was S2.16 nm Zmin. That is, the reforming period T 2
- the length of the deposition period T1 was set to 30 seconds or less, and the reforming was performed. It has been found that it is preferable to set the length of the period T2 to 60 seconds or more.
- the HCD gas which is a silane-based gas
- ammonia gas which is another gas
- ethylene gas which is a hydrocarbon gas
- all of the ammonia gas, the silane-based gas, and the hydrocarbon gas may be supplied intermittently (in a pulsed manner).
- in one cycle of gas supply at least one of the silane-based gas and the hydrocarbon gas is supplied first.
- FIGS. 7A, 7B, 7C, and 7D are timing charts showing gas supply patterns according to the fifth, sixth, seventh, and eighth embodiments of the present invention, respectively.
- the gas supply timing that is, the supply timing
- the gas supply timing is set to be different from each other. That is, HCD gas is supplied first, then NH 3 gas is supplied, and finally, C 2 H 4 gas is supplied.
- One cycle is continuously performed several times.
- the supply period T3 of one gas (one pulse) is set to, for example, about 1 minute.
- the intermittent period T4 between the adjacent gas supply periods is set to, for example, about 0.5 minute.
- the length of one cycle is about 4.5 minutes.
- the intermittent period is the film reforming period, and the entire period of film formation! :
- the processing chamber is evacuated in the same manner as described in the first to fourth embodiments.
- the intermittent period (reforming period) it is possible to stop the supply of all the above three types of gases and to continue only evacuation. Instead, during the intermittent period (reforming period), supply of all three types of gas is stopped, and the inert gas is changed to N, for example.
- the supply period of ammonia gas and the supply period of C 2 H 4 gas are set to the same timing and supplied in synchronization. That is, HCD gas is supplied first, and then NH 3 gas and C 2 H 4 gas are supplied simultaneously. One cycle is continuously performed plural times.
- the gas supply period T3 for one (one pulse) is set to, for example, about 1 minute.
- the intermittent period T4 is set to, for example, about 0.5 minutes. Therefore, in the case of the sixth embodiment, In this case, the length of one cycle is about 3 minutes.
- the supply period of the HCD gas and the supply period of the C 2 H 4 gas are set at the same timing and supplied in synchronization. That is, first, the HCD gas and the C 2 H 4 gas are supplied simultaneously in synchronization with each other, and then the NH 3 gas is supplied, and one cycle is continuously performed a plurality of times.
- the supply period T3 of one gas (one pulse) is set to, for example, about 1 minute.
- the intermittent period T4 is set to, for example, about 0.5 minute. Therefore, in the case of the seventh embodiment, the length of one cycle is about 3 minutes.
- the supply periods of the three types of gases are set to be different from each other.
- HCD gas is supplied, then C 2 H 4 gas is supplied, and finally, NH 3 gas is supplied.
- One cycle is repeated several times.
- the supply order of the C 2 H 4 gas and the NH 3 gas is opposite to that of the fifth embodiment shown in FIG. 7A.
- the supply period T 3 of one gas (one pulse) is set to, for example, about 1 minute.
- the intermittent period T4 between the adjacent gas supply periods is set to, for example, about 0.5 minute. Therefore, in the case of the eighth embodiment, the length of one cycle is about 4.5 minutes.
- Si-C bond (It is difficult to etch.) It forms Si-C bond. That is, for a substrate to be processed having a silicon surface, a processing gas containing C is first supplied to form a Si—C bond on the silicon surface. Protect.
- the process temperature was 500 ° C.
- the flow rate of NH 3 gas was 600 sccm
- the flow rate of the HCD gas was 20 sccm
- the flow rate of the C 2 H 4 gas was 600 sccm.
- the supply period T3 in Figs. 7A to 7D was 30 seconds
- the intermittent period ⁇ 4 was 60 seconds.
- the number of execution cycles during film formation was set to 50 times.
- the process pressure during supply of each gas, that is, during the supply period ⁇ 3, was set to 0.6 Torr (80 Pa). In the intermittent period T4, the supply of all the gas was stopped, and only the evacuation was performed (0.002 to 0.0004 ⁇ ⁇ ⁇ ⁇ rr base pressure).
- the films of E81 and Comparative Examples C2 and C3 were immersed in an etching solution and etched.
- the etching solution is 0.1% HF solution (99
- the etching temperature is room temperature
- the etching time is
- FIG. 8 shows the results of Examples E51 and E6 obtained by the experiment of (1).
- Examples E51, E61, E71, and E81 are respectively 0.61 nm / m ⁇ n ⁇ 0.76 nvn / in,
- Example E52 An additional experiment was performed using the gas supply pattern according to the fifth embodiment to examine the dependence of the etching rate of the cine-nitride film on the process pressure during gas supply.
- the process pressure at the time of gas supply was set to 1.
- O T rr (133 P a).
- the other process conditions and the jetting conditions were the same as described with reference to FIG.
- FIG. 9 shows the etching rate of the membrane according to Example E52 obtained in this experiment, which was obtained from Example E51 (where the process pressure during gas supply was 0.6 Torr ( 8 0 P a)) Comparative example c
- Example 2 is a graph shown in comparison with the etching rate of the film according to FIG.
- the working plate force of Example E51 (process pressure: 0.6 Torr) was 0.61 nm / min.
- the etching rate of Example E52 (process pressure was 10 Torr) was 0.73 nm / m1n. Therefore, it has been found that the etching rate has little dependence on the process pressure at the time of gas supply, and that the film quality can be sufficiently improved if this pressure is set to 1 Torr or less.
- the intermittent period T 4 the process chamber performing-out vacuum pulling while supplying N 2 gas is inert gas was set to 0.6 Torr.
- Other process conditions and etching conditions were the same as those described with reference to FIG.
- FIG. 10 shows the etching rate of the film according to Example E53 obtained in this experiment, which was obtained by the above-mentioned Example E51 (only the evacuation was performed during the intermittent period T4 (0.002). ⁇ 0.04 Torr (base pressure), which is a graph shown in comparison with the etching rate of the film obtained in Comparative Example C2. 1 etch rate (intermittent period T 4 only for evacuation).
- Example E 53 N 2 supply and evacuation during intermittent period T 4) was 0.
- the film thicknesses of the silicon nitride films according to 1 and Comparative Example C2 were measured at the upper, middle, and lower wafer positions of the wafer boat.
- FIG. 11 shows examples E51 and E obtained by this experiment.
- FIG. 6 is a graph showing the thickness of a silicon nitride film according to 61, E71, E81, and Comparative Example C2.
- TOP “CTR” and “BTM” indicate the wafer position at the top, center, and bottom of the wafer port, respectively.
- CTR the uniformity of the film thickness in the planes of Examples E51, E61, E71, and E81 is smaller than that of Comparative Example C2.
- good results were obtained (the in-plane film thickness difference was small).
- all of Examples E51, E61, E71, and E81 showed a better result than Comparative Example C2.
- the fifth to eighth embodiments were effective even when the etching liquid was changed as described above.
- the supply period ⁇ 3 and the intermittent period 54 in the fifth to eighth embodiments are merely examples, and are not particularly limited to the values used in the description.
- a case where hexachlorodisilane (HCD) is used as a silane-based gas to form a silicon nitride film is exemplified.
- TCS peroxirane
- DSA disilylane
- TSA trisilylane
- BBAS Vista-butylamino-silane
- a vertical batch type device is exemplified as the CVD device.
- the present invention can also be applied to a horizontal batch type CVD apparatus or a single-wafer type CVD apparatus that processes substrates to be processed one by one. Further, with respect to the substrate to be processed, the present invention relates to a glass substrate other than a semiconductor substrate or a glass substrate.
Abstract
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Also Published As
Publication number | Publication date |
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US7462376B2 (en) | 2008-12-09 |
TWI343951B (en) | 2011-06-21 |
KR20060015708A (ko) | 2006-02-20 |
KR20090037984A (ko) | 2009-04-16 |
JP2005012168A (ja) | 2005-01-13 |
JP4403824B2 (ja) | 2010-01-27 |
KR100956468B1 (ko) | 2010-05-07 |
US20060286817A1 (en) | 2006-12-21 |
TW200500485A (en) | 2005-01-01 |
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