WO2004035209A1 - 水分発生用反応炉の白金コーティング触媒層の形成方法 - Google Patents
水分発生用反応炉の白金コーティング触媒層の形成方法 Download PDFInfo
- Publication number
- WO2004035209A1 WO2004035209A1 PCT/JP2003/013146 JP0313146W WO2004035209A1 WO 2004035209 A1 WO2004035209 A1 WO 2004035209A1 JP 0313146 W JP0313146 W JP 0313146W WO 2004035209 A1 WO2004035209 A1 WO 2004035209A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- platinum
- moisture
- catalyst layer
- aluminum
- generating
- Prior art date
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J12/00—Chemical processes in general for reacting gaseous media with gaseous media; Apparatus specially adapted therefor
- B01J12/007—Chemical processes in general for reacting gaseous media with gaseous media; Apparatus specially adapted therefor in the presence of catalytically active bodies, e.g. porous plates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/42—Platinum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0215—Coating
- B01J37/0225—Coating of metal substrates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0215—Coating
- B01J37/0225—Coating of metal substrates
- B01J37/0226—Oxidation of the substrate, e.g. anodisation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B5/00—Water
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/02—Boron or aluminium; Oxides or hydroxides thereof
- B01J21/04—Alumina
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
Definitions
- the present invention relates to an improvement in a method of manufacturing a reactor for generating moisture used mainly in a semiconductor manufacturing apparatus or a chemical product manufacturing apparatus, and includes a platinum-coated catalyst provided on an inner wall surface of a reaction space inside the reactor.
- the present invention relates to a method for forming a barrier film constituting a layer.
- a furnace body having a reaction space P is formed by assembling and welding the furnace body members 22 and 23 to face each other, and a raw material gas inlet is formed in the furnace body. 24, moisture gas outlet 25, inlet-side reflector 26, outlet-side reflector 27, etc., and a platinum-coated catalyst layer 28 on the inner wall surface of the furnace body 23 on the side facing the raw material gas inlet 24. Is formed.
- the platinum-coated catalyst layer 28 is formed on the entire inner surface of the furnace body member 23 on the water gas outlet 25 side made of SUS 316 L. After forming a TiN barrier film 28a, a platinum film 28b is formed thereon.
- the thickness of the barrier coating 28a is most preferably about 0.1 / im to 5 m.
- the barrier coating 28a made of TiN having a thickness of about 5; It is formed by the plating method.
- the thickness of the platinum film 28b is suitably about 0.1 / zm to 3 ⁇ , and in the figure, a platinum film 28b having a thickness of about 3 // m is formed by vacuum evaporation. It has been done.
- the method of forming the coating 28a may be a PVD method such as an ion sputtering method or a vacuum evaporation method, or an ion vapor deposition method (CV). D method), hot press method, thermal spray method, etc. can also be used.
- a PVD method such as an ion sputtering method or a vacuum evaporation method, or an ion vapor deposition method (CV). D method), hot press method, thermal spray method, etc.
- a method of forming the platinum film 28b in addition to the above-described vacuum deposition method, an ion plating method, a ion sputtering method, a chemical vapor deposition method, a hot press method, or the like can be used.
- 8a is a conductive material such as TiN, a plating method is also possible.
- the barrier film 28a is provided to prevent the reaction rate of the platinum film 28b from decreasing due to a change with time.
- Ni and Fe diffuse from the base metal into the platinum film 28b, and this diffuses on the surface of the platinum film 28b in an oxidizing atmosphere. Oxidation causes the platinum film 28b to lose its catalytic activity.
- the barrier film 28a is formed on the surface of the stainless steel (base), thereby preventing Fe and Ni from migrating from the base metal into the platinum film 28b.
- the barrier film 28a a material which does not contain a 1 ⁇ 1 ⁇ 6 component and which does not generate an oxide in the platinum coating film is optimal, and T i A 1 N, T i C, T i addition to the CN and a 1 2 0 3, C r 2 0 3, S i 0 2, C r oxides or nitrides, such as N well, the T i N like the barrier one film 2 8 It has been confirmed that it can be used as a.
- hydrogen and oxygen supplied to the inside of the reactor main body through raw material gas inlet 24 are diffused by a diffusion member including inlet-side reflector 26 and outlet-side reflector 27 and the like. It is diffused and comes into contact with the platinum-coated catalyst layer 28. Oxygen and hydrogen that have come into contact with the platinum-coated catalyst layer 28 are enhanced in reactivity by the catalytic action of platinum, and are in a so-called radicalized state.
- the radicalized hydrogen and oxygen react instantaneously at a temperature lower than the ignition temperature of the hydrogen-mixed gas (approximately 300 ° C to 400 ° C) without burning high temperatures. Generates moisture.
- the generated moisture (moisture gas) is led out from the moisture gas outlet 25 and supplied to a semiconductor manufacturing chamber or the like (not shown).
- the moisture regeneration reactor with the structure shown in Fig. 3 is safe without burning at high temperatures. Excellent practical utility that can react O 2 and H 2 with a reaction rate close to 100%, and can continuously obtain the required amount of ultra-high-purity moisture gas. Is played.
- a barrier coating 28a having a thickness of 1 to 5 / m is formed by ion plating, ion sputtering, vacuum evaporation, or the like.
- ion plating ion sputtering
- vacuum evaporation vacuum evaporation
- the barrier film 2 having a uniform thickness is formed on the inner wall surface of the furnace body member 23. Forming 8a becomes more difficult.
- the formation of the barrier film 28a requires considerable cost, and as a result, there is a problem that it is difficult to reduce the manufacturing cost of the reactor for generating moisture.
- the present invention has the above-mentioned problems in the conventional reactor for generating moisture, namely: (a) it is difficult to form a barrier film having a uniform thickness and no pinholes on the inner wall surface of the reaction space; (Mouth) It is difficult to reduce the cost of forming a non-coated film, and (C) The adhesion of the barrier film to the base material is slightly weak!
- a 1 by selective oxidation properties of a stainless steel alloy, a 1 containing stainless steel predetermined hydrogen and moisture ratio (H 2 / H 2 O) in an inert gas for a predetermined time, by heating at a predetermined temperature, a 1 allows that you very inexpensively manufacture the barrier one coating consisting of a layer mainly composed of a 1 2 0 3 layer and a l 2 ⁇ 3 substantially close to 1 0 0% on the outer surface of the containing stainless steel and To provide a method for forming a platinum-coated catalyst layer in a reaction chamber for generating moisture To offer.
- the invention of claim 1 is to form a water generating reactor having a platinum coating catalyst layer on the inner wall surface of the reaction space, and to contact oxygen and hydrogen supplied into the reaction space with the platinum coating catalyst layer.
- the moisture generating reactor is made of an aluminum-containing alloy. formed, to form a barrier one coating consisting mainly of aluminum oxide (Al 2 0 3) is subjected to selective oxidation treatment Arumiyuumu the inner wall surface of the water generating reactor, then platinum skin at the top of the barrier one film
- the basic configuration of the present invention is to form a platinum-coated catalyst layer by laminating and fixing films.
- the invention of claim 2 is the invention of claim 1, wherein the aluminum-containing alloy is aluminum-containing stainless steel.
- the invention according to claim 3 is the invention according to claim 1, wherein the aluminum-selective oxidation treatment of the aluminum-containing alloy is performed by adjusting the hydrogen-to-water ratio (H 2 / H 2 O) and the heating temperature of the treatment atmosphere to 10 4 / The heating was performed for 1 to 10 9 / ⁇ and 300 to 1500 ° C for a predetermined time.
- H 2 / H 2 O hydrogen-to-water ratio
- the platinum-coated catalyst layer is formed only on the inner wall surface of the furnace main body member on the moisture gas outlet side of the moisture generating reaction furnace.
- the invention of claim 6 is the invention according to claim 2, wherein the aluminum-containing alloy is obtained by adding 17.7 wt% of Cr, 25.5 wt% of Ni, 0.01 wt% of Mo, and 0.1 wt% of Mn. 0.1 wt% or less, input 1 is 3 to 41 1:%, C is 0.01 wt% or less, S is 0.01 wt% or less, P force is 0.01 wt% or less, and the balance is Fe.
- This is an austenitic aluminum-containing alloy.
- the invention according to claim 7 is the invention according to claim 3, wherein the heat treatment is performed at a temperature of 800 ° C for 3 hours in an atmosphere of argon gas containing 10 VOL% of hydrogen and 10 ppm of water. It is what was made.
- Figure 1 is a graph showing the relationship between Arumiyuumu containing stainless in temperature oxidation of the main component of the alloy and atmosphere (H 2 / H 2 O) ( Ellingham diagram).
- Figure 2 is a constitutional diagram of A 1 2 0 3 film formed by applying the A 1 selective oxidation treatment on the surface of the aluminum-containing stainless (FR31).
- FIG. 3 is a schematic cross-sectional view of a conventional moisture regeneration reactor (Japanese Patent Application Laid-Open No. 2000-169109).
- P is a reaction space
- 22 is a furnace body member
- 23 is a furnace body member
- 24 is a raw material gas inlet
- 25 is a moisture gas outlet
- 26 is an inlet-side reflector
- 27 is an outlet-side reflector
- 28 is a platinum-coated catalyst.
- Layer, 28a is a barrier film
- 28b is a platinum film
- 29 is a filter.
- a 1 in Ni, Fe, Cr, and A 1 is selectively oxidized by selecting the H 2 / H 2 O ratio and the temperature within an appropriate range, A 1 is oxidized by the following formula.
- the present invention utilizes the selective oxidation characteristics of A1 as described above to oxidize only A1 on the inner surfaces of the furnace body members 22 and 23 made of a stainless alloy containing A1. der to form a barrier one film L comprising a furnace body member 22, 23 a 1 2 0 3 layer and a 12 0 3 film i.e. of 1 100% on the inner surface of the a 1 2 O 3 from the layer mainly You.
- Table 1 shows the conventional stainless steel (SUS316L).
- a pretreatment such as cleaning was performed on the inner surface of the furnace body member 23 made of the above-described A1 containing stainless steel, and after cleaning the inner surface, the furnace body was placed in a heat treatment furnace and subjected to heat treatment under the following conditions.
- Figure 2 shows the depth profile (depth direction analysis result) using ES CA. Shows the internal components structure of A 1 2 0 3 Skin film formed on the inner surface of the furnace body member 23 by the A 1 selective oxidation process.
- curve E is the atomic ratio of oxygen O (%)
- F is the number of A 1 atoms (%)
- G is the number of Fe atoms (%)
- H is the number of Ni atoms (%)
- I the C r atoms (° / 0) is indicative of the range of the inner a 1 2 0 3 skin film as is clear from FIG. 2 to about 180nm from the (base metal) (0. 18 ⁇ )
- L is a so-called a 1 Li Tutsi of film, further, the range of about 50nm of (0. 05 ⁇ ) the outermost external surface portion has a full a 1 2 0 3 film.
- the furnace body member 22, 23 is formed by A 1 containing stainless steel, first barrier one coating L for the inner wall surface thereof is subjected to the A 1 selective oxidation mainly of A 1 2 0 3 To form Next, a platinum film 28b is laminated and fixed on the barrier film L on the inner wall surface of the furnace body member 23 on the moisture gas outlet side, and the furnace body member 23 and the furnace body member 22 on the source gas inlet 24 side are connected. Welding the outer peripheral surfaces of the contacting parts in opposition to each other forms a reactor for generating moisture.
- the water generation reaction using the TiN barrier-one film 28a formed by the conventional ion plating method was performed. Compared to the furnace, it has been confirmed that there is no inferior change in the reaction rate over time and the adhesion (mechanical strength) of the platinum-coated catalyst layer 28.
- the furnace body members 22 and 23 are formed using A1 containing stainless steel (austenitic HR31), but any kind of metal may be used if it is an alloy containing A1. It may be.
- the barrier film L is formed on both of the main body members 22 and 23, but the barrier film is formed only on the inner wall surface of the furnace main body member 23 on the moisture gas outlet 25 side.
- the film L may be formed.
- a platinum coating catalyst layer is formed by laminating and fixing a platinum coating on the barrier coating.
- the present invention has excellent practical utility.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
Description
Claims
Priority Applications (7)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AU2003272998A AU2003272998A1 (en) | 2002-10-16 | 2003-10-14 | Method for forming platinum coating catalyst layer in reaction furnace for generating water gas |
IL16427403A IL164274A0 (en) | 2002-10-16 | 2003-10-14 | A process for forming a platinum coating catalyst layer |
KR1020047012636A KR100619154B1 (ko) | 2002-10-16 | 2003-10-14 | 수분발생용 반응로의 백금 코팅 촉매층의 형성방법 |
US10/510,758 US7595087B2 (en) | 2002-10-16 | 2003-10-14 | Process of forming platinum coating catalyst layer in moisture-generating reactor |
CA002480894A CA2480894A1 (en) | 2002-10-16 | 2003-10-14 | Process of forming platinum coating catalyst layer in moisture-generating reactor |
EP03754111A EP1552885A1 (en) | 2002-10-16 | 2003-10-14 | Method for forming platinum coating catalyst layer in reaction furnace for generating water gas |
IL164274A IL164274A (en) | 2002-10-16 | 2004-09-26 | Process for creating a platinum coating in a catalyst layer |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2002301423A JP4119218B2 (ja) | 2002-10-16 | 2002-10-16 | 水分発生用反応炉の白金コーティング触媒層の形成方法 |
JP2002-301423 | 2002-10-16 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2004035209A1 true WO2004035209A1 (ja) | 2004-04-29 |
Family
ID=32105014
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/JP2003/013146 WO2004035209A1 (ja) | 2002-10-16 | 2003-10-14 | 水分発生用反応炉の白金コーティング触媒層の形成方法 |
Country Status (10)
Country | Link |
---|---|
US (1) | US7595087B2 (ja) |
EP (1) | EP1552885A1 (ja) |
JP (1) | JP4119218B2 (ja) |
KR (1) | KR100619154B1 (ja) |
CN (1) | CN100387342C (ja) |
AU (1) | AU2003272998A1 (ja) |
CA (1) | CA2480894A1 (ja) |
IL (2) | IL164274A0 (ja) |
TW (1) | TWI246940B (ja) |
WO (1) | WO2004035209A1 (ja) |
Families Citing this family (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20090148357A1 (en) * | 2005-03-31 | 2009-06-11 | Masato Kaneeda | Apparatus and catalyst for purifying exhaust gas |
JP5837733B2 (ja) * | 2009-04-24 | 2015-12-24 | 国立大学法人東北大学 | 水分発生用反応炉 |
JP5665408B2 (ja) * | 2010-08-04 | 2015-02-04 | 国立大学法人東北大学 | 水分発生用反応炉 |
RU2468866C1 (ru) * | 2011-09-15 | 2012-12-10 | Владимир Андреевич Шепелин | Способ изготовления катализатора и импрегнированный пористый носитель катализатора для рекомбинации водорода и кислорода |
US10180708B2 (en) | 2016-05-24 | 2019-01-15 | Microsoft Technology Licensing, Llc | Curved circuit board |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0390321A1 (en) * | 1989-03-14 | 1990-10-03 | Corning Incorporated | Porous sintered metal structure with a cured oxide layer |
US5301217A (en) * | 1990-05-11 | 1994-04-05 | Siemens Aktiengesellschaft | Device for the recombination of hydrogen and oxygen and nuclear power plant using the device |
EP1238942A1 (en) * | 2000-06-05 | 2002-09-11 | Fujikin Incorporated | Reactor for moisture generation |
Family Cites Families (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4086085A (en) * | 1976-11-02 | 1978-04-25 | Mcgurty James A | Austenitic iron alloys |
US5069938A (en) * | 1990-06-07 | 1991-12-03 | Applied Materials, Inc. | Method of forming a corrosion-resistant protective coating on aluminum substrate |
CN1166536A (zh) * | 1996-05-27 | 1997-12-03 | 杨清平 | 一种表面覆铝的钢材、铁基工件及其覆铝方法 |
JP3686762B2 (ja) | 1998-12-04 | 2005-08-24 | 株式会社フジキン | 水分発生用反応炉 |
TR200200511T2 (tr) * | 1999-12-21 | 2002-06-21 | Alcoa Inc. | Alüminyum alaşımı gıda ve içecek kapları için kopolimer astar. |
-
2002
- 2002-10-16 JP JP2002301423A patent/JP4119218B2/ja not_active Expired - Fee Related
-
2003
- 2003-10-14 WO PCT/JP2003/013146 patent/WO2004035209A1/ja active IP Right Grant
- 2003-10-14 CN CNB2003801002269A patent/CN100387342C/zh not_active Expired - Fee Related
- 2003-10-14 US US10/510,758 patent/US7595087B2/en not_active Expired - Fee Related
- 2003-10-14 IL IL16427403A patent/IL164274A0/xx active IP Right Grant
- 2003-10-14 KR KR1020047012636A patent/KR100619154B1/ko not_active IP Right Cessation
- 2003-10-14 CA CA002480894A patent/CA2480894A1/en not_active Abandoned
- 2003-10-14 EP EP03754111A patent/EP1552885A1/en not_active Withdrawn
- 2003-10-14 AU AU2003272998A patent/AU2003272998A1/en not_active Abandoned
- 2003-10-15 TW TW092128607A patent/TWI246940B/zh not_active IP Right Cessation
-
2004
- 2004-09-26 IL IL164274A patent/IL164274A/en not_active IP Right Cessation
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0390321A1 (en) * | 1989-03-14 | 1990-10-03 | Corning Incorporated | Porous sintered metal structure with a cured oxide layer |
US5301217A (en) * | 1990-05-11 | 1994-04-05 | Siemens Aktiengesellschaft | Device for the recombination of hydrogen and oxygen and nuclear power plant using the device |
EP1238942A1 (en) * | 2000-06-05 | 2002-09-11 | Fujikin Incorporated | Reactor for moisture generation |
Also Published As
Publication number | Publication date |
---|---|
US7595087B2 (en) | 2009-09-29 |
TWI246940B (en) | 2006-01-11 |
KR20040089635A (ko) | 2004-10-21 |
CN1691980A (zh) | 2005-11-02 |
IL164274A0 (en) | 2005-12-18 |
AU2003272998A1 (en) | 2004-05-04 |
US20050157834A1 (en) | 2005-07-21 |
TW200413094A (en) | 2004-08-01 |
IL164274A (en) | 2008-04-13 |
JP2004136163A (ja) | 2004-05-13 |
CN100387342C (zh) | 2008-05-14 |
EP1552885A1 (en) | 2005-07-13 |
CA2480894A1 (en) | 2004-04-29 |
JP4119218B2 (ja) | 2008-07-16 |
KR100619154B1 (ko) | 2006-08-31 |
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