JP2002206421A - Holding-seal material for catalytic converter, ceramic fiber, and method of manufacturing the ceramic fiber - Google Patents
Holding-seal material for catalytic converter, ceramic fiber, and method of manufacturing the ceramic fiberInfo
- Publication number
- JP2002206421A JP2002206421A JP2001003889A JP2001003889A JP2002206421A JP 2002206421 A JP2002206421 A JP 2002206421A JP 2001003889 A JP2001003889 A JP 2001003889A JP 2001003889 A JP2001003889 A JP 2001003889A JP 2002206421 A JP2002206421 A JP 2002206421A
- Authority
- JP
- Japan
- Prior art keywords
- fiber
- ceramic fiber
- catalytic converter
- silica
- sealing material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000835 fiber Substances 0.000 title claims abstract description 170
- 239000000919 ceramic Substances 0.000 title claims abstract description 48
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 39
- 239000000463 material Substances 0.000 title claims abstract description 27
- 238000004519 manufacturing process Methods 0.000 title claims description 18
- 239000003054 catalyst Substances 0.000 claims abstract description 39
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 71
- 239000002245 particle Substances 0.000 claims description 66
- 239000003566 sealing material Substances 0.000 claims description 47
- 239000000377 silicon dioxide Substances 0.000 claims description 46
- 229910044991 metal oxide Inorganic materials 0.000 claims description 34
- 150000004706 metal oxides Chemical class 0.000 claims description 34
- 239000000725 suspension Substances 0.000 claims description 29
- 229910052751 metal Inorganic materials 0.000 claims description 24
- 239000002184 metal Substances 0.000 claims description 24
- 239000010954 inorganic particle Substances 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 18
- 238000010304 firing Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 12
- 229910010272 inorganic material Inorganic materials 0.000 claims description 11
- 239000011147 inorganic material Substances 0.000 claims description 11
- 239000002243 precursor Substances 0.000 claims description 11
- 229920003169 water-soluble polymer Polymers 0.000 claims description 9
- 239000000470 constituent Substances 0.000 claims description 6
- 230000006866 deterioration Effects 0.000 abstract description 4
- 230000001788 irregular Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 20
- 238000009987 spinning Methods 0.000 description 19
- 239000007789 gas Substances 0.000 description 12
- 239000007864 aqueous solution Substances 0.000 description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 210000004027 cell Anatomy 0.000 description 7
- 229910052878 cordierite Inorganic materials 0.000 description 7
- 230000007423 decrease Effects 0.000 description 7
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 7
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 7
- 239000000446 fuel Substances 0.000 description 7
- 229910052863 mullite Inorganic materials 0.000 description 7
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 description 5
- 238000005470 impregnation Methods 0.000 description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 description 5
- 239000011550 stock solution Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000004804 winding Methods 0.000 description 4
- 238000009924 canning Methods 0.000 description 3
- 230000002542 deteriorative effect Effects 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 238000006073 displacement reaction Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- 238000004080 punching Methods 0.000 description 3
- 238000003746 solid phase reaction Methods 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- 239000002518 antifoaming agent Substances 0.000 description 2
- KBPLFHHGFOOTCA-UHFFFAOYSA-N caprylic alcohol Natural products CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000013011 mating Effects 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 229920000620 organic polymer Polymers 0.000 description 2
- 230000002093 peripheral effect Effects 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000002407 reforming Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 101000650817 Homo sapiens Semaphorin-4D Proteins 0.000 description 1
- 101000777301 Homo sapiens Uteroglobin Proteins 0.000 description 1
- 229920000459 Nitrile rubber Polymers 0.000 description 1
- 102100027744 Semaphorin-4D Human genes 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 102100031083 Uteroglobin Human genes 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 229920000800 acrylic rubber Polymers 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000009530 blood pressure measurement Methods 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- 235000012255 calcium oxide Nutrition 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Inorganic Fibers (AREA)
- Nonwoven Fabrics (AREA)
- Exhaust Gas After Treatment (AREA)
- Exhaust Gas Treatment By Means Of Catalyst (AREA)
- Catalysts (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、触媒コンバータ用
保持シール材、セラミック繊維及びセラミック繊維の製
造方法に関するものである。The present invention relates to a holding sealing material for a catalytic converter, a ceramic fiber, and a method for producing a ceramic fiber.
【０００２】[0002]
【従来の技術】従来、車両用、特に自動車の動力源とし
て、ガソリンや軽油を燃料とする内燃機関が百年以上に
わたり用いられてきた。しかしながら、排気ガスが健康
や環境に害を与えることが次第に問題となってきてい
る。それゆえ、最近では排気ガス中に含まれているＣ
Ｏ、ＮＯｘ、ＨＣ等を除去する排気ガス浄化用触媒コン
バータや、ＰＭ等を除去するＤＰＦが各種提案されるに
至っている。通常の排気ガス浄化用触媒コンバータは、
触媒担持体と、前記触媒担持体の外周を覆う金属製シェ
ルと、両者間のギャップに配置される保持シール材とを
備えている。触媒担持体としてはハニカム状に成形した
コージェライト担体が用いられており、それには白金等
の触媒が担持されている。2. Description of the Related Art Conventionally, an internal combustion engine using gasoline or light oil as fuel has been used as a power source for vehicles, particularly automobiles, for more than 100 years. However, it is becoming increasingly problematic that exhaust gases harm health and the environment. Therefore, recently, C contained in exhaust gas
Various exhaust gas purifying catalytic converters for removing O, NOx, HC and the like, and various types of DPFs for removing PM and the like have been proposed. A typical catalytic converter for exhaust gas purification is
The fuel cell system includes a catalyst carrier, a metal shell that covers the outer periphery of the catalyst carrier, and a holding sealing material disposed in a gap between the two. As the catalyst carrier, a cordierite carrier formed in a honeycomb shape is used, on which a catalyst such as platinum is supported.
【０００３】また最近では、石油を動力源としない次期
のクリーンな動力源の研究が進められており、そのうち
特に有望なものとして例えば燃料電池がある。燃料電池
とは、水素と酸素とが反応して水ができる際に得られる
電気を、動力源として用いるものである。酸素は空気中
からじかに取り出される反面、水素についてはメタノー
ル、ガソリン等を改質して用いている。この場合、メタ
ノール等の改質は触媒反応によって行われる。そして、
このような燃料電池にも、触媒担持体と、触媒担持体の
外周を覆う金属製シェルと、両者間のギャップに配置さ
れる保持シール材とを備える燃料電池用触媒コンバータ
が用いられている。触媒担持体としてはハニカム状に成
形したコージェライト担体が用いられており、それには
銅系の触媒が担持されている。In recent years, research on the next clean power source not using oil as a power source has been advanced, and among them, a fuel cell, for example, is particularly promising. A fuel cell uses electricity obtained when water reacts with hydrogen to produce water as a power source. Oxygen is directly extracted from the air, while hydrogen is obtained by reforming methanol, gasoline, and the like. In this case, the reforming of methanol or the like is performed by a catalytic reaction. And
Such a fuel cell also uses a fuel cell catalytic converter including a catalyst carrier, a metal shell that covers the outer periphery of the catalyst carrier, and a holding sealing material disposed in a gap between the two. A cordierite carrier formed in a honeycomb shape is used as the catalyst carrier, and a copper-based catalyst is supported on the cordierite carrier.
【０００４】上記の触媒コンバータを製造する方法をこ
こで簡単に説明しておく。まず、熔融法等によりセラミ
ック繊維を紡糸した後、そのセラミック繊維をマット状
に集合させてなる材料を作製する。この材料を金型で打
ち抜くことによって、帯状の保持シール材を作製する。
次に、この保持シール材を触媒担持体の外周面に巻き付
けた後、金属製シェル内に前記触媒担持体を収容する。
その結果、所望の触媒コンバータが完成する。このよう
な収容状態において保持シール材は厚さ方向に圧縮され
るため、保持シール材にはその圧縮力に抗する反発力
（面圧）が生じる。そして、この反発力が作用すること
により、触媒担持体が金属製シェル内に保持されるよう
になっている。[0004] A method of manufacturing the above catalytic converter will now be briefly described. First, a ceramic fiber is spun by a melting method or the like, and then a material is formed by gathering the ceramic fibers into a mat. A band-shaped holding sealing material is produced by punching out this material with a mold.
Next, after winding the holding sealing material around the outer peripheral surface of the catalyst carrier, the catalyst carrier is accommodated in a metal shell.
As a result, a desired catalytic converter is completed. Since the holding sealing material is compressed in the thickness direction in such a housed state, a repulsive force (surface pressure) against the compressive force is generated in the holding sealing material. When the repulsive force acts, the catalyst carrier is held in the metal shell.
【０００５】[0005]
【発明が解決しようとする課題】しかしながら、上記従
来の保持シール材は使用時に振動や排気ガス等の高温に
晒されることから、時間が経つにつれて次第に面圧が低
下し、比較的早期のうちに触媒担持体の保持性やシール
性が悪くなるという欠点があった。However, since the conventional holding sealing material is exposed to high temperatures such as vibration and exhaust gas during use, the surface pressure gradually decreases with time, and the holding sealing material is relatively early. There was a drawback that the retention and sealing properties of the catalyst carrier deteriorated.
【０００６】本発明は上記の課題に鑑みてなされたもの
であり、その目的は、面圧の経時劣化が起こりにくい触
媒コンバータ用保持シール材を提供することにある。ま
た、本発明の別の目的は、上記の優れた触媒コンバータ
用保持シール材の構成材料として好適なセラミック繊維
及びその製造方法を提供することにある。SUMMARY OF THE INVENTION The present invention has been made in view of the above problems, and an object of the present invention is to provide a holding seal material for a catalytic converter in which the surface pressure hardly deteriorates with time. Another object of the present invention is to provide a ceramic fiber suitable as a constituent material of the above excellent sealing material for a catalytic converter, and a method for producing the same.
【０００７】[0007]
【課題を解決するための手段】そこで、上記課題を解決
すべく本願発明者らが鋭意研究を行ったところ、繊維集
合体を圧縮するような外部荷重を長時間加えた場合、繊
維集合体を構成する単繊維同士に滑り・ズレが生じ、そ
れが繊維集合体の面圧の低下を引き起こすという知見を
得た。そこで、本願発明者らは、単繊維同士の滑り・ズ
レという問題を何らかの手段により解消すれば好結果が
得られるであろうとの予測のもとに、繊維外表面の構造
に着目した。そして、かかる部位の構造を改良すべくさ
らに鋭意研究を行い、最終的に本願発明を想到するに至
ったのである。In order to solve the above-mentioned problems, the present inventors have conducted intensive studies. As a result, when an external load such as compressing the fiber assembly is applied for a long time, the fiber assembly is It has been found that slips and deviations occur between the constituent single fibers, which causes a decrease in the surface pressure of the fiber assembly. Therefore, the inventors of the present application paid attention to the structure of the outer surface of the fiber based on the expectation that a good result would be obtained if the problem of slip and displacement between the single fibers was solved by some means. Further, further studies were carried out to improve the structure of such a part, and finally the present invention was conceived.
【０００８】即ち、本発明の請求項１に記載の発明で
は、マット状に集合したセラミック繊維を構成要素と
し、触媒担持体とその触媒担持体の外周を覆う金属製シ
ェルとのギャップに配置される保持シール材であって、
前記セラミック繊維の外表面に無機質からなる凹凸構造
を有することを特徴とする触媒コンバータ用保持シール
材をその要旨とする。That is, according to the first aspect of the present invention, the ceramic fibers which are gathered in a mat shape are used as constituent elements, and are arranged in the gap between the catalyst carrier and the metal shell covering the outer periphery of the catalyst carrier. Holding sealing material,
A gist of the present invention is a holding sealing material for a catalytic converter, which has an uneven structure made of an inorganic material on the outer surface of the ceramic fiber.
【０００９】請求項２に記載の発明は、請求項１におい
て、前記無機質からなる凹凸構造は、前記セラミック繊
維の外表面に付着した金属酸化物粒子からなるとした。
請求項３に記載の発明は、請求項２において、前記金属
酸化物粒子の平均粒径は、５０ｎｍ〜１０００ｎｍであ
るとした。According to a second aspect of the present invention, in the first aspect, the uneven structure made of inorganic material is made of metal oxide particles attached to an outer surface of the ceramic fiber.
According to a third aspect of the present invention, in the second aspect, the metal oxide particles have an average particle size of 50 nm to 1000 nm.
【００１０】請求項４に記載の発明は、請求項２または
３において、前記金属酸化物粒子は、前記セラミック繊
維を構成する物質からなるとした。請求項５に記載の発
明は、請求項２または３において、前記セラミック繊維
はアルミナ−シリカ系繊維であり、前記金属酸化物粒子
はシリカ粒子であるとした。[0010] According to a fourth aspect of the present invention, in the second or third aspect, the metal oxide particles are made of a material constituting the ceramic fibers. According to a fifth aspect of the present invention, in the second or third aspect, the ceramic fibers are alumina-silica-based fibers, and the metal oxide particles are silica particles.
【００１１】請求項６に記載の発明では、繊維集合体を
構成するセラミック繊維であって、その外表面に無機質
からなる凹凸構造を有することを特徴とするセラミック
繊維をその要旨とする。According to a sixth aspect of the invention, there is provided a ceramic fiber constituting a fiber assembly, wherein the ceramic fiber has an uneven structure made of an inorganic material on its outer surface.
【００１２】請求項７に記載の発明は、請求項６に記載
のセラミック繊維を製造する方法であって、焼結状態に
あるセラミック繊維または少なくとも不溶化状態にある
前駆体繊維の外表面に無機粒子懸濁溶液を付着させた状
態で加熱することにより、前記懸濁溶液中に含まれる前
記無機粒子を前記外表面に固定することを特徴とするセ
ラミック繊維の製造方法をその要旨とする。According to a seventh aspect of the present invention, there is provided a method for producing a ceramic fiber according to the sixth aspect, wherein inorganic particles are formed on the outer surface of the sintered ceramic fiber or at least the insolubilized precursor fiber. The gist of the present invention is a method for producing a ceramic fiber, wherein the inorganic particles contained in the suspension solution are fixed to the outer surface by heating the suspension solution while the suspension solution is adhered.
【００１３】請求項８に記載の発明は、請求項７におい
て、前記無機粒子懸濁溶液は、水溶性高分子を含む金属
酸化物粒子懸濁溶液であるとした。請求項９に記載の発
明は、請求項７において、焼結状態にあるアルミナ−シ
リカ系繊維の外表面に、平均粒径５０ｎｍ〜１０００ｎ
ｍのシリカ粒子及び水溶性高分子を含む懸濁溶液を付着
させ、この状態で加熱乾燥を行った後、さらに１２００
℃以上の温度で焼成することにより、前記懸濁溶液中に
含まれる前記シリカ粒子を前記外表面に固定することと
した。According to an eighth aspect of the present invention, in the seventh aspect, the inorganic particle suspension is a metal oxide particle suspension containing a water-soluble polymer. According to a ninth aspect of the present invention, in the seventh aspect, the average particle diameter is 50 nm to 1000 n on the outer surface of the alumina-silica fiber in a sintered state.
m of silica particles and a suspension solution containing a water-soluble polymer were adhered and heated and dried in this state.
By baking at a temperature of not less than ° C., the silica particles contained in the suspension solution are fixed on the outer surface.
【００１４】以下、本発明の「作用」について説明す
る。請求項１，６に記載の発明によると、外表面に凹凸
構造を有するセラミック繊維であると、外表面が滑面状
であるものに比べて確実に摩擦係数が増大するため、繊
維同士の引っ掛かりによって滑り・ズレが生じにくくな
る。従って、繊維集合体を圧縮するような外部荷重を長
時間加えた場合であっても、面圧の低下を引き起こしに
くくなる。また、無機質からなる凹凸構造は耐熱性にも
優れている。ゆえに、例えば保持シール材の使用温度に
凹凸構造が晒されたとしても、それが焼失等するような
ことはない。The "action" of the present invention will be described below. According to the first and sixth aspects of the present invention, when the ceramic fibers have an uneven structure on the outer surface, the friction coefficient surely increases as compared with the case where the outer surface has a smooth surface. As a result, slip and displacement are less likely to occur. Therefore, even when an external load such as compressing the fiber aggregate is applied for a long time, a decrease in the surface pressure hardly occurs. Further, the uneven structure made of an inorganic material has excellent heat resistance. Therefore, even if, for example, the uneven structure is exposed to the use temperature of the holding sealing material, it does not burn out.
【００１５】請求項２に記載の発明によると、金属酸化
物粒子がセラミック繊維と強固に結合することにより、
セラミック繊維の外表面に好適な凹凸形状が保持され
る。また、セラミック繊維の外表面の一部を除去するこ
と等により凹凸構造を形成したものとは異なり、繊維自
体の物理的性質の悪化を招くことがない。よって、繊維
の折れや変形等が生じにくくなり、面圧の低下も引き起
こしにくなる。According to the second aspect of the present invention, the metal oxide particles are firmly bonded to the ceramic fibers,
A suitable uneven shape is retained on the outer surface of the ceramic fiber. Further, unlike a structure in which a concavo-convex structure is formed by removing a part of the outer surface of the ceramic fiber, the physical properties of the fiber itself are not deteriorated. Therefore, the fiber is less likely to be bent or deformed, and the surface pressure is not easily reduced.
【００１６】請求項３に記載の発明によると、金属酸化
物粒子の平均粒径を上記好適範囲内に設定したことによ
り、製造の困難化を伴うことなく確実に繊維の摩擦係数
を増大させることができる。According to the third aspect of the present invention, by setting the average particle diameter of the metal oxide particles within the above-mentioned preferred range, the friction coefficient of the fiber can be reliably increased without making the production difficult. Can be.
【００１７】前記平均粒径が５０ｎｍ未満の粒子の場
合、得られる凹凸がそもそも小さいことから、繊維の摩
擦係数を増大させるためには多くの粒子を付着させる必
要性が生じ、保持シール材を製造しにくくなるおそれが
ある。逆に、前記平均粒径が１０００ｎｍを超える粒子
の場合、得られる凹凸が比較的大きいことから、繊維の
摩擦係数を増大させるためには好都合である。その反
面、粒子を付着させることが困難になり、やはり保持シ
ール材を製造しにくくなるおそれがある。In the case of particles having an average particle diameter of less than 50 nm, the resulting irregularities are originally small, so that it is necessary to attach a large number of particles in order to increase the friction coefficient of the fiber. It may be difficult to do so. Conversely, in the case of particles having an average particle diameter of more than 1000 nm, since the obtained irregularities are relatively large, it is advantageous to increase the friction coefficient of the fiber. On the other hand, it becomes difficult to attach the particles, and there is a possibility that the production of the holding sealing material also becomes difficult.
【００１８】請求項４に記載の発明によると、金属酸化
物粒子はセラミック繊維を構成している物質からなるた
め、繊維との親和性が高く、繊維との接合強度が高くな
る。ゆえに、金属酸化物粒子が繊維の外表面から脱落し
にくくなり、面圧の経時劣化を確実に防止することがで
きる。According to the fourth aspect of the present invention, since the metal oxide particles are made of the material constituting the ceramic fiber, the affinity for the fiber is high, and the bonding strength with the fiber is high. Therefore, the metal oxide particles are less likely to fall off the outer surface of the fiber, and the surface pressure can be reliably prevented from deteriorating with time.
【００１９】請求項５に記載の発明によると、非晶質成
分の少ないアルミナ−シリカ系繊維を用いているため、
繊維自体の耐熱性が向上し、高温での面圧の経時劣化を
少なくすることができる。また、シリカ粒子はアルミナ
−シリカ系繊維に対する親和性が極めて高いため、繊維
との接合部分のさらなる高強度化を図ることができる。According to the fifth aspect of the present invention, since the alumina-silica fiber containing less amorphous component is used,
The heat resistance of the fiber itself is improved, and deterioration with time of the surface pressure at high temperatures can be reduced. In addition, since the silica particles have extremely high affinity for the alumina-silica-based fiber, it is possible to further increase the strength of the joint portion with the fiber.
【００２０】請求項７に記載の発明によると、焼結状態
にあるセラミック繊維または少なくとも不溶化状態にあ
る前駆体繊維を用いているため、付着処理の際に繊維が
無機粒子懸濁液に溶けてしまうことはなく、繊維形状の
悪化が回避される。また、無機粒子は懸濁溶液において
均一に分散されている。このため、この溶液を用いれば
無機粒子を均一にかつ確実に付着させることができ、繊
維の外表面に好適な凹凸構造を付与することができる。According to the seventh aspect of the present invention, since the ceramic fibers in the sintered state or the precursor fibers in the insolubilized state are used, the fibers are dissolved in the inorganic particle suspension during the adhesion treatment. It does not happen and deterioration of the fiber shape is avoided. Further, the inorganic particles are uniformly dispersed in the suspension solution. For this reason, if this solution is used, the inorganic particles can be uniformly and reliably adhered, and a suitable uneven structure can be provided on the outer surface of the fiber.
【００２１】請求項８に記載の発明によると、金属酸化
物粒子を付着させる際に水溶性高分子がバインダとして
働くため、繊維の外表面に粒子を確実に付着させること
ができる。なお、この水溶性高分子は加熱焼成時に焼失
するので、完成したセラミック繊維には殆ど残らない。According to the eighth aspect of the present invention, since the water-soluble polymer acts as a binder when attaching the metal oxide particles, the particles can be securely attached to the outer surface of the fiber. Since the water-soluble polymer is burned off during heating and firing, it hardly remains in the finished ceramic fiber.
【００２２】[0022]
【発明の実施の形態】以下、本発明を具体化した一実施
形態の自動車排気ガス浄化装置用触媒コンバータを図１
〜図６に基づき詳細に説明する。FIG. 1 shows a catalytic converter for an automobile exhaust gas purifying apparatus according to an embodiment of the present invention.
This will be described in detail with reference to FIG.
【００２３】図３に示される本実施形態の触媒コンバー
タ１は、自動車の車体において、エンジンの排気管の途
中に設けられる。エンジンから触媒コンバータ１までの
距離は比較的短いため、触媒コンバータ１には約７００
℃〜９００℃の高温の排気ガスが供給されるようになっ
ている。エンジンがリーンバーンエンジンである場合に
は、触媒コンバータ１には約９００℃〜１０００℃とい
う、さらに高温の排気ガスが供給されるようになってい
る。The catalytic converter 1 according to the present embodiment shown in FIG. 3 is provided in the body of an automobile in the middle of an exhaust pipe of an engine. Since the distance from the engine to the catalytic converter 1 is relatively short, about 700
Exhaust gas at a high temperature of from 900C to 900C is supplied. When the engine is a lean burn engine, the catalytic converter 1 is supplied with a still higher exhaust gas of about 900 ° C. to 1000 ° C.
【００２４】図３に示されるように、本実施形態の触媒
コンバータ１は、基本的に、触媒担持体２と、触媒担持
体２の外周を覆う金属製シェル３と、両者２，３間のギ
ャップに配置される保持シール材４とによって構成され
ている。As shown in FIG. 3, the catalytic converter 1 of this embodiment basically includes a catalyst carrier 2, a metal shell 3 covering the outer periphery of the catalyst carrier 2, And a holding sealing material 4 arranged in the gap.
【００２５】前記触媒担持体２は、コージェライト等に
代表されるセラミック材料を用いて作製されている。こ
の触媒担持体２は断面円形状をした柱状部材となってい
る。また、触媒担持体２は、軸線方向に沿って延びる多
数のセル５を有するハニカム構造体であることが好まし
い。セル壁には排気ガス成分を浄化しうる白金やロジウ
ム等の貴金属系触媒が担持されている。なお、触媒担持
体２として、上記のコージェライト担体のほかにも、例
えば炭化珪素、窒化珪素等のハニカム多孔質焼結体等を
用いてもよい。The catalyst carrier 2 is made of a ceramic material such as cordierite. The catalyst carrier 2 is a columnar member having a circular cross section. Further, the catalyst carrier 2 is preferably a honeycomb structure having a large number of cells 5 extending along the axial direction. A noble metal catalyst such as platinum or rhodium that can purify exhaust gas components is supported on the cell walls. In addition, as the catalyst carrier 2, besides the above cordierite carrier, for example, a honeycomb porous sintered body of silicon carbide, silicon nitride or the like may be used.
【００２６】前記金属製シェル３としては、例えば組み
付けに際して圧入方式を採用する場合には、断面Ｏ字状
の金属製円筒部材が用いられる。なお、円筒部材を形成
するための金属材料としては、耐熱性や耐衝撃性に優れ
た金属（例えばステンレス等のような鋼材等）が選択さ
れることがよい。圧入方式に代えていわゆるキャニング
方式を採用する場合には、前記断面Ｏ字状の金属製円筒
部材を軸線方向に沿って複数片に分割したもの（即ちク
ラムシェル）が用いられる。As the metal shell 3, for example, when a press-fitting method is employed for assembling, a metal cylindrical member having an O-shaped cross section is used. In addition, as a metal material for forming the cylindrical member, a metal having excellent heat resistance and impact resistance (for example, a steel material such as stainless steel) is preferably selected. When a so-called canning method is adopted instead of the press-fitting method, a metal cylindrical member having an O-shaped cross section divided into a plurality of pieces along the axial direction (ie, a clam shell) is used.
【００２７】そのほか、組み付けに際して巻き締め方式
を採用する場合には、例えば断面Ｃ字状ないしＵ字状の
金属製円筒部材、言い換えるといわば軸線方向に沿って
延びるスリット（開口部）を１箇所にのみ有する金属製
円筒部材が用いられる。この場合、触媒担持体２の組み
付けに際し、触媒担持体２に保持シール材４を固定した
ものを金属製シェル３内に収め、その状態で金属製シェ
ル３を巻き締めた後に開口端が接合（溶接、接着、ボル
ト締め等）される。溶接、接着、ボルト締め等といった
接合作業は、キャニング方式を採用したときにも同様に
行われる。In addition, when the winding method is adopted for assembling, for example, a metal cylindrical member having a C-shaped or U-shaped cross section, in other words, a slit (opening) extending along the axial direction is provided at one place. Only a metal cylindrical member having only one is used. In this case, when assembling the catalyst carrier 2, the one in which the holding sealing material 4 is fixed to the catalyst carrier 2 is put in a metal shell 3, and the metal shell 3 is wound and tightened at the open end in this state ( Welding, bonding, bolting, etc.). Joining operations such as welding, bonding, and bolting are performed similarly when the canning method is adopted.
【００２８】図１に示されるように、この保持シール材
４は長尺状のマット状物であって、その一端には凹状合
わせ部１１が設けられ、他端には凸状合わせ部１２が設
けられている。図２に示されるように、触媒担持体２へ
の巻き付け時には、凸状合わせ部１２が凹状合わせ部１
１にちょうど係合するようになっている。As shown in FIG. 1, the holding sealing material 4 is a long mat-like material, and has a concave mating portion 11 at one end and a convex mating portion 12 at the other end. Is provided. As shown in FIG. 2, at the time of winding around the catalyst carrier 2, the convex fitting portion 12 is
1 just engages.
【００２９】本実施形態の保持シール材４は、マット状
に集合したセラミック繊維（即ち繊維集合体）を主要な
要素として構成されたものである。前記セラミック繊維
として、本実施形態ではアルミナ−シリカ系繊維６が用
いられている。この場合、ムライト結晶含有量が０重量
％以上かつ１０重量％以下のアルミナ−シリカ系繊維６
を用いることがより好ましい。このような化学組成であ
ると、非晶質成分が少なくなることから耐熱性に優れた
ものとなり、かつ圧縮荷重印加時の反発力が高いものと
なるからである。従って、ギャップに配置された状態で
高温に遭遇したときであっても、発生する面圧の低下が
比較的起こりにくくなる。The holding sealing material 4 of the present embodiment is composed mainly of ceramic fibers (that is, fiber aggregates) gathered in a mat shape. In the present embodiment, alumina-silica fibers 6 are used as the ceramic fibers. In this case, the alumina-silica fiber 6 having a mullite crystal content of 0% by weight or more and 10% by weight or less is used.
It is more preferable to use This is because such a chemical composition results in excellent heat resistance due to a reduced amount of amorphous components, and a high repulsive force when a compressive load is applied. Therefore, even when a high temperature is encountered in a state where it is arranged in the gap, a decrease in the generated surface pressure is relatively unlikely to occur.
【００３０】アルミナ−シリカ系繊維６の化学組成は、
アルミナ６８重量％〜８３重量％かつシリカ３２重量％
〜１７重量％であることがよく、具体的にはＡｌ2Ｏ3：
ＳｉＯ2＝７２：２８であることがなおよい。The chemical composition of the alumina-silica fiber 6 is as follows:
68% to 83% by weight of alumina and 32% by weight of silica
To 17% by weight, specifically Al 2 O 3 :
More preferably, SiO 2 = 72: 28.
【００３１】アルミナが６８重量％未満の場合またはシ
リカが３２重量％を超える場合には、耐熱性の向上及び
圧縮荷重印加時の反発力の向上を十分に達成できなくな
るおそれがある。アルミナが８３重量％を超える場合ま
たはシリカが１７重量％未満の場合についても同様に、
耐熱性の向上及び圧縮荷重印加時の反発力の向上を十分
に達成できなくなるおそれがある。If the amount of alumina is less than 68% by weight or the amount of silica exceeds 32% by weight, it may not be possible to sufficiently improve the heat resistance and the resilience when a compressive load is applied. Similarly, when the alumina is more than 83% by weight or the silica is less than 17% by weight,
There is a possibility that the improvement in heat resistance and the improvement in repulsion force when a compressive load is applied may not be sufficiently achieved.
【００３２】図４にて概略的に示されるように、この保
持シール材４を構成するアルミナ−シリカ系繊維６は、
繊維の外表面６ａに無機質からなる凹凸構造を有してい
る。本実施形態においては、繊維の外表面６ａに金属酸
化物粒子７を付着させることにより凹凸構造が形成され
ている。As schematically shown in FIG. 4, the alumina-silica fibers 6 constituting the holding sealing material 4 are:
The outer surface 6a of the fiber has an uneven structure made of an inorganic material. In the present embodiment, an uneven structure is formed by attaching metal oxide particles 7 to the outer surface 6a of the fiber.
【００３３】前記金属酸化物粒子７の平均粒径は５０ｎ
ｍ〜１０００ｎｍ、特には５０ｎｍ〜５００ｎｍである
ことがよい。前記平均粒径が５０ｎｍ未満の場合、得ら
れる凹凸がそもそも小さい。従って、アルミナ−シリカ
系繊維６の摩擦係数を増大させるためには、多くの金属
酸化物粒子７を付着させる必要性が生じ、保持シール材
４を製造しにくくなるおそれがある。逆に、前記平均粒
径が１０００ｎｍを超える場合、得られる凹凸が比較的
大きいことから、アルミナ−シリカ系繊維６の摩擦係数
を増大させるためには好都合である。その反面、金属酸
化物粒子７を均一に分散した懸濁溶液を作製することが
難しく、金属酸化物粒子７を効率よく付着させることが
困難になるため、やはり保持シール材４を製造しにくく
なるおそれがある。The average particle size of the metal oxide particles 7 is 50 n.
m to 1000 nm, and particularly preferably 50 nm to 500 nm. When the average particle size is less than 50 nm, the obtained irregularities are originally small. Therefore, in order to increase the friction coefficient of the alumina-silica fiber 6, it becomes necessary to attach a large number of metal oxide particles 7, and it may be difficult to manufacture the holding sealing material 4. On the other hand, when the average particle size exceeds 1000 nm, the obtained irregularities are relatively large, which is advantageous for increasing the friction coefficient of the alumina-silica fiber 6. On the other hand, it is difficult to prepare a suspension solution in which the metal oxide particles 7 are uniformly dispersed, and it is difficult to attach the metal oxide particles 7 efficiently. Therefore, it is also difficult to manufacture the holding sealing material 4. There is a risk.
【００３４】この場合、金属酸化物粒子７としては、セ
ラミック繊維を構成している物質からなることが好まし
い。繊維との親和性が高く、接着部分の強度が高くなる
ため、面圧の経時劣化を確実に防止することができるか
らである。このような事情のもと、アルミナ−シリカ系
繊維６を選択した本実施形態では、シリカ粒子（ＳｉＯ
2粒子）を用いている。上記シリカ粒子に代えて、例え
ばアルミナ、ジルコニア、チタニア、イットリア、セリ
ア、カルシア、マグネシア等を用いることも可能であ
る。In this case, it is preferable that the metal oxide particles 7 be made of a material constituting ceramic fibers. This is because the affinity with the fiber is high and the strength of the bonded portion is increased, so that the deterioration with time of the surface pressure can be reliably prevented. Under such circumstances, in this embodiment in which the alumina-silica fiber 6 is selected, the silica particles (SiO 2
2 particles). Instead of the silica particles, for example, alumina, zirconia, titania, yttria, ceria, calcia, magnesia, and the like can be used.
【００３５】アルミナ−シリカ系繊維６の平均繊維径
は、３μｍ〜２５μm程度であることがよく、さらには
１０μｍ〜２０μm程度であることがなおよい。平均繊
維径を小さくしすぎると、呼吸器系に吸い込まれやすく
なるという不都合が生じるからである。アルミナ−シリ
カ系繊維６の平均繊維長は、０．１mm〜１００mm程度で
あることがよく、さらには２mm〜５０mm程度であること
がなおよい。また、アルミナ−シリカ系繊維６の繊維自
体の引っ張り強度は、０．１ＧＰａ以上、特には０．５
ＧＰａ以上であることがよい。アルミナ−シリカ系繊維
６の断面形状は、図４にて示されたもののような真円形
状でもよいほか、異形断面形状（例えば楕円形状、長円
形状、略三角形状等）でも構わない。The average fiber diameter of the alumina-silica fiber 6 is preferably about 3 μm to 25 μm, and more preferably about 10 μm to 20 μm. If the average fiber diameter is too small, there is a disadvantage that the fiber is easily sucked into the respiratory system. The average fiber length of the alumina-silica fiber 6 is preferably about 0.1 mm to 100 mm, and more preferably about 2 mm to 50 mm. The tensile strength of the alumina-silica fiber 6 itself is 0.1 GPa or more, especially 0.5 GPa.
GPa or more is preferable. The cross-sectional shape of the alumina-silica-based fiber 6 may be a perfect circular shape as shown in FIG. 4 or a modified cross-sectional shape (for example, an elliptical shape, an oval shape, a substantially triangular shape, etc.).
【００３６】組み付け前の状態における保持シール材４
の厚さは、触媒担持体２と金属製シェル３とがなすギャ
ップの１．１倍〜４．０倍程度、さらには１．５倍〜
３．０倍程度であることが望ましい。前記厚さが１．１
倍未満であると、高い担持体保持性を得ることができ
ず、触媒担持体２が金属製シェル３に対してズレたりガ
タついたりするおそれがある。勿論、この場合には高い
シール性も得られなくなるため、ギャップ部分からの排
気ガスのリークが起こりやすくなり、高度な低公害性を
実現できなくなってしまう。また、前記厚さが４．０倍
を超えると、特に圧入方式を採用した場合には、触媒担
持体２の金属製シェル３への配置が困難になってしま
う。よって、組み付け性の向上を達成できなくなるおそ
れがある。Holding seal material 4 in state before assembly
Is about 1.1 times to 4.0 times the gap formed between the catalyst carrier 2 and the metal shell 3, and more preferably 1.5 times to
It is desirably about 3.0 times. The thickness is 1.1
If the ratio is less than twice, high support holding property cannot be obtained, and the catalyst support 2 may shift or rattle with respect to the metal shell 3. Of course, in this case, a high sealing property cannot be obtained, so that the leakage of the exhaust gas from the gap portion is likely to occur, and a high low pollution property cannot be realized. On the other hand, when the thickness exceeds 4.0 times, it is difficult to arrange the catalyst carrier 2 on the metal shell 3 particularly when the press-fitting method is adopted. Therefore, there is a possibility that improvement in assemblability cannot be achieved.
【００３７】また、組み付け後における保持シール材４
のＧＢＤ（嵩密度）は、０．１０ｇ／ｃｍ3〜０．３０
ｇ／ｃｍ3、さらには０．１０ｇ／ｃｍ3〜０．２５ｇ／
ｃｍ3となるように設定されることが好ましい。ＧＢＤ
の値が極端に小さいと、十分に高い初期面圧を実現する
ことが困難になる場合がある。一方、ＧＢＤが大きすぎ
ると、材料として使用すべきアルミナ−シリカ系繊維６
の量が増え、コスト高を招きやすくなる。Further, the holding sealing material 4 after the assembling is performed.
Has a GBD (bulk density) of 0.10 g / cm 3 to 0.30.
g / cm 3 , and further 0.10 g / cm 3 to 0.25 g /
It is preferably set to be cm 3 . GBD
Is extremely small, it may be difficult to realize a sufficiently high initial surface pressure. On the other hand, if the GBD is too large, the alumina-silica fiber 6
And the cost is likely to increase.
【００３８】組み付け状態における保持シール材４の初
期面圧は５０ｋＰａ以上、さらには７０ｋＰａ以上であ
ることが好ましい。初期面圧の値が高ければ、面圧の経
時劣化が起こったとしても、触媒担持体２の好適な保持
性を維持することができるからである。The initial surface pressure of the holding sealing material 4 in the assembled state is preferably 50 kPa or more, more preferably 70 kPa or more. This is because if the value of the initial surface pressure is high, even if the surface pressure deteriorates with time, a suitable holding property of the catalyst carrier 2 can be maintained.
【００３９】なお、保持シール材４に対し必要に応じ
て、ニードルパンチ処理や樹脂含浸処理等を施してもよ
い。これらの処理を施すことにより、保持シール材４を
厚さ方向に圧縮して肉薄化することが可能となるからで
ある。The holding sealing material 4 may be subjected to a needle punching process, a resin impregnation process, or the like, if necessary. This is because by performing these processes, the holding sealing material 4 can be compressed in the thickness direction to be reduced in thickness.
【００４０】次に、触媒コンバータ１を製造する手順を
説明する。まず、アルミニウム塩水溶液、シリカゾル及
び有機重合体を混合し、紡糸原液を作製する。言い換え
ると、無機塩法により紡糸原液を作製する。アルミナ源
であるアルミニウム塩水溶液は、紡糸原液に粘性を付与
するための成分でもある。なお、このような水溶液とし
て、塩基性アルミニウム塩の水溶液を選択することがよ
い。シリカ源であるシリカゾルは、繊維に高い強度を付
与するための成分でもある。有機重合体は紡糸原液に曳
糸性を付与するための成分である。Next, a procedure for manufacturing the catalytic converter 1 will be described. First, an aluminum salt aqueous solution, a silica sol, and an organic polymer are mixed to prepare a spinning solution. In other words, a spinning stock solution is prepared by the inorganic salt method. The aqueous solution of an aluminum salt as an alumina source is also a component for imparting viscosity to the spinning dope. It is preferable to select an aqueous solution of a basic aluminum salt as such an aqueous solution. Silica sol, which is a silica source, is also a component for imparting high strength to fibers. The organic polymer is a component for imparting spinnability to the spinning dope.
【００４１】紡糸原液には消泡剤等が添加されていても
よい。なお、アルミニウム塩及びシリカゾルの比率を変
更することにより、アルミナ−シリカ系繊維６の化学組
成をある程度コントロールすることができる。An antifoaming agent or the like may be added to the spinning dope. The chemical composition of the alumina-silica fiber 6 can be controlled to some extent by changing the ratio of the aluminum salt and the silica sol.
【００４２】次いで、得られた紡糸原液を減圧濃縮する
ことにより、紡糸に適した濃度・温度・粘度等に調製し
た紡糸原液とする。ここでは、２０重量％程度であった
紡糸液を濃縮して３０重量％〜４０重量％程度にするこ
とがよい。また、粘度を１０ポアズ〜２０００ポアズに
設定することがよい。Next, the obtained spinning dope is concentrated under reduced pressure to obtain a spinning dope adjusted to a concentration, temperature, viscosity and the like suitable for spinning. Here, the spinning solution, which was about 20% by weight, is preferably concentrated to about 30% to 40% by weight. Further, the viscosity is preferably set to 10 poise to 2000 poise.
【００４３】さらに、調製後の紡糸原液を紡糸装置のノ
ズルから空気中に連続的に噴出するとともに、形成され
た前駆体繊維を延伸しながら巻き取るようにする。この
場合、例えば乾式圧力紡糸法などが採用されることが好
ましい。Further, the prepared spinning dope is continuously jetted from the nozzle of the spinning device into the air, and the formed precursor fiber is wound while being drawn. In this case, for example, a dry pressure spinning method is preferably employed.
【００４４】次に、第１回目の焼成工程を行って前駆体
繊維をセラミック化（結晶化）することにより、前駆体
繊維を硬化させ、アルミナ−シリカ系繊維６を得る。こ
の時点においては、まだ繊維外表面６ａは平滑であるた
め、その摩擦係数も比較的小さい。Next, the first firing step is performed to ceramicize (crystallize) the precursor fiber, whereby the precursor fiber is cured and the alumina-silica fiber 6 is obtained. At this time, since the outer fiber surface 6a is still smooth, its coefficient of friction is relatively small.
【００４５】前記焼成工程においては、得られるアルミ
ナ−シリカ系繊維６におけるムライト結晶含有量が１０
重量％以下となるような焼成条件を設定することが望ま
しい。例えば、焼成工程における焼成温度は１０００℃
〜１３００℃に設定されることがよい。焼成温度が１０
００℃未満であると、前駆体繊維を完全に乾燥・焼結さ
せることができず、優れた耐熱性及び高い圧縮荷重印加
時の反発力を保持シール材４に確実に付与できなくなる
おそれがある。逆に、焼成温度が１３００℃を超える
と、アルミナ−シリカ系繊維６におけるムライト結晶化
が進行しやすくなる。このため、ムライト結晶含有量を
１０重量％以下に抑えることが困難になり、優れた耐熱
性及び高い圧縮荷重印加時の反発力を保持シール材４に
確実に付与できなくなるおそれがある。In the firing step, the mullite crystal content in the obtained alumina-silica fiber 6 is 10%.
It is desirable to set the firing conditions so as to be less than the weight%. For example, the firing temperature in the firing step is 1000 ° C.
It is good to set to ~ 1300 ° C. Firing temperature is 10
If the temperature is lower than 00 ° C., the precursor fibers cannot be completely dried and sintered, and there is a possibility that excellent heat resistance and high repulsion force when a compressive load is applied cannot be reliably applied to the holding sealing material 4. . Conversely, if the firing temperature exceeds 1300 ° C., mullite crystallization in the alumina-silica fiber 6 tends to proceed. For this reason, it is difficult to suppress the mullite crystal content to 10% by weight or less, and there is a possibility that excellent heat resistance and a high repulsive force when a high compressive load is applied cannot be reliably applied to the holding sealing material 4.
【００４６】続いて、上記の各工程を経て得られたアル
ミナ−シリカ系繊維６の長繊維を所定長さにチョップし
てある程度短繊維化する。この後、短繊維を集綿、解繊
及び積層することにより、あるいは、短繊維を水に分散
させて得た繊維分散液を成形型内に流し込んで加圧・乾
燥することにより、マット状の繊維集合体を得る。さら
に、この繊維集合体を所定形状に打ち抜いて保持シール
材４とする。Subsequently, the long fiber of the alumina-silica fiber 6 obtained through each of the above steps is chopped to a predetermined length to shorten the fiber to some extent. Thereafter, by collecting, defibrating and laminating the staple fibers, or by pouring a fiber dispersion obtained by dispersing the staple fibers in water into a molding die and pressing and drying, a mat-like shape is obtained. Obtain a fiber assembly. Further, the fiber assembly is punched into a predetermined shape to form the holding sealing material 4.
【００４７】上記の成形工程の後、凹凸構造形成工程を
行って繊維集合体を構成するアルミナ−シリカ系繊維６
の外表面６ａに凹凸構造を形成する。具体的には以下の
ように行う。After the above-described molding step, an alumina-silica-based fiber 6 constituting a fiber aggregate by performing a concave-convex structure forming step
Is formed on the outer surface 6a. Specifically, this is performed as follows.
【００４８】まず、無機粒子懸濁溶液として、先に列挙
した金属酸化物粒子７のゾルまたは分散水溶液を作製す
る。これにはポリビニルアルコール等のような水溶性高
分子が添加されていることがよい。水溶性高分子がある
と、金属酸化物粒子７を付着させる際にそれが有機バイ
ンダとして働くため、繊維の外表面６ａに金属酸化物粒
子７を確実に付着させることができるからである。ま
た、水溶性高分子は後述の加熱焼成時に焼失するので、
完成したアルミナ−シリカ系繊維６には殆ど残らない。
上記無機粒子懸濁溶液は、例えば、ポリビニルアルコー
ルを１０重量％含む水溶液に、所定分量のシリカゾル水
溶液を加えることによって容易に作製することができ
る。この場合、シリカゾル水溶液の添加量を５重量％〜
２０重量％程度に設定することがよい。First, a sol or an aqueous dispersion of the metal oxide particles 7 listed above is prepared as an inorganic particle suspension. It is preferable that a water-soluble polymer such as polyvinyl alcohol is added to this. This is because the presence of the water-soluble polymer serves as an organic binder when the metal oxide particles 7 are adhered, so that the metal oxide particles 7 can be surely adhered to the outer surface 6a of the fiber. Also, since the water-soluble polymer is burned off during heating and firing described below,
Almost no residue remains in the completed alumina-silica fiber 6.
The above-mentioned inorganic particle suspension solution can be easily prepared, for example, by adding a predetermined amount of a silica sol aqueous solution to an aqueous solution containing 10% by weight of polyvinyl alcohol. In this case, the addition amount of the silica sol aqueous solution is from 5% by weight to
It is preferable to set it to about 20% by weight.
【００４９】次いで、この無機粒子懸濁溶液をアルミナ
−シリカ系繊維６の外表面６ａに付着させることを目的
として含浸を行う。このような含浸に代えて、例えば繊
維集合体を溶液に浸漬して内部に含浸させたり、スプレ
ー噴霧によりミスト状の溶液を繊維集合体内に供給する
等の方法を採ってもよい。なお、含浸法によれば、無機
粒子懸濁溶液を繊維集合体の内部にまで確実にかつ均一
に入り込ませることが可能である。Next, impregnation is performed for the purpose of attaching the inorganic particle suspension solution to the outer surface 6a of the alumina-silica fiber 6. Instead of such impregnation, for example, a method may be adopted in which the fiber aggregate is immersed in a solution to impregnate the interior, or a mist-like solution is supplied into the fiber aggregate by spraying. In addition, according to the impregnation method, the inorganic particle suspension solution can be surely and uniformly penetrated into the fiber aggregate.
【００５０】含浸の後、繊維集合体を加熱して乾燥する
ことが好ましい。加熱乾燥を行うことにより、原料溶液
中の余分な水分がある程度除去されるため、次工程にお
ける焼成を安定的に行うことができるからである。After the impregnation, the fiber assembly is preferably dried by heating. This is because by performing the heating and drying, excess water in the raw material solution is removed to some extent, so that the firing in the next step can be stably performed.
【００５１】次いで、乾燥された繊維集合体を高温下で
再び焼成することにより、アルミナ−シリカ系繊維６と
金属酸化物粒子７との間での固相反応を促し、繊維外表
面６ａに金属酸化物粒子７を強固な結合をもって固定す
る。その結果、繊維外表面６ａに微細な凹凸構造が形成
され、摩擦係数の増大が図られる。なお、繊維外表面６
ａと金属酸化物粒子７との界面には、図４にて概略的に
示されるようにムライト層８が形成されるものと考えら
れる。Next, the dried fiber assembly is fired again at a high temperature to promote a solid-phase reaction between the alumina-silica fiber 6 and the metal oxide particles 7, and the metal outer surface 6a The oxide particles 7 are fixed with strong bonds. As a result, a fine uneven structure is formed on the fiber outer surface 6a, and the friction coefficient is increased. The fiber outer surface 6
It is considered that a mullite layer 8 is formed at the interface between a and the metal oxide particles 7 as schematically shown in FIG.
【００５２】焼成時の温度は１２００℃以上であること
がよく、好ましくは１２００℃〜１４００℃程度である
ことがよい。このときの温度が低すぎると、固相反応を
十分に促すことができず、結合強度が不十分になって、
金属酸化物粒子７が脱落しやすくなるおそれがあるから
である。一方、このときの温度を必要以上に高くして
も、固相反応の顕著な促進にはつながらず、かえってエ
ネルギーの無駄になり不経済的になるからである。The temperature at the time of firing is preferably 1200 ° C. or more, and more preferably, about 1200 ° C. to 1400 ° C. If the temperature at this time is too low, the solid phase reaction cannot be sufficiently promoted, and the bonding strength becomes insufficient,
This is because the metal oxide particles 7 may easily fall off. On the other hand, if the temperature at this time is increased more than necessary, it does not lead to remarkable promotion of the solid-phase reaction, but rather wastes energy and becomes uneconomical.
【００５３】この後、必要に応じて保持シール材４に対
する有機バインダの含浸を行った後、さらに保持シール
材４を厚さ方向に圧縮成形してもよい。この場合の有機
バインダとしては、アクリルゴムやニトリルゴム等のよ
うなラテックス等のほか、ポリビニルアルコール、アク
リル樹脂等が挙げられる。After that, if necessary, the holding seal material 4 may be impregnated with an organic binder, and then the holding seal material 4 may be compression-molded in the thickness direction. In this case, examples of the organic binder include latex such as acrylic rubber and nitrile rubber, as well as polyvinyl alcohol and acrylic resin.
【００５４】そして、前記繊維集合体を所定形状に打ち
抜いて得た保持シール材４を、触媒担持体２の外周面に
巻き付けて有機テープ１３を固定する。その後、圧入、
キャニングまたは巻き締めを行えば、所望の触媒コンバ
ータ１が完成する。Then, the holding sealing material 4 obtained by punching the fiber assembly into a predetermined shape is wound around the outer peripheral surface of the catalyst carrier 2, and the organic tape 13 is fixed. Then press-fit,
When canning or winding is performed, a desired catalytic converter 1 is completed.
【００５５】以下、上記実施形態をより具体化した実施
例及びその比較例について説明する。Hereinafter, examples and comparative examples of the above embodiment will be described.
【００５６】[0056]
【実施例及び比較例】（実施例１）実施例１では、以下
のようにして保持シール材４の面圧評価用サンプルを作
製した。EXAMPLES and COMPARATIVE EXAMPLES (Example 1) In Example 1, a sample for evaluating the surface pressure of the holding sealing material 4 was manufactured as follows.
【００５７】まず、塩基性塩化アルミニウム水溶液（２
３．５重量％）、シリカゾル（２０重量％、シリカ粒径
１５μｍ）、ポリビニルアルコール（１０重量％）及び
消泡剤（ｎ−オクタノール）を混合し、紡糸原液を作製
した。次いで、得られた紡糸原液をエバポレータを用い
て５０℃で減圧濃縮し、濃度３８重量％、粘度１０００
ポアズの紡糸原液に調製した。First, a basic aluminum chloride aqueous solution (2
3.5 wt%), silica sol (20 wt%, silica particle size 15 μm), polyvinyl alcohol (10 wt%) and an antifoaming agent (n-octanol) were mixed to prepare a spinning stock solution. Next, the obtained spinning stock solution was concentrated under reduced pressure at 50 ° C. using an evaporator to obtain a concentration of 38% by weight and a viscosity of 1000%.
It was prepared into Poise spinning stock solution.
【００５８】調製後の紡糸原液を紡糸装置のノズルから
空気中に連続的に噴出するとともに、形成された前駆体
繊維を延伸しながら巻き取った。さらに、空気雰囲気に
保持された電気炉内で、上記前駆体繊維に対する２５０
℃かつ３０分間の加熱（前処理）を行った後、同じく電
気炉内で１２５０℃かつ１０分間の焼成を行った。The prepared spinning dope was continuously jetted from the nozzle of the spinning device into the air, and the formed precursor fiber was wound while being drawn. Further, in an electric furnace maintained in an air atmosphere, 250
After heating at 30 ° C. for 30 minutes (pretreatment), firing was also performed at 1250 ° C. for 10 minutes in an electric furnace.
【００５９】その結果、ムライト結晶含有量が約８重量
％、アルミナ／シリカの重量比が７２：２８、平均繊維
径が９μｍの真円状アルミナ−シリカ系繊維６を得た。
続いて、アルミナ−シリカ系繊維６の長繊維を５ｍｍ長
にチョップして短繊維化した。その後、この短繊維（約
１．０ｇ）を水に分散させ、得られた繊維分散液を成形
型枠内に流し込んで加圧・乾燥することにより、縦横２
５ｍｍ角のマット状繊維集合体を得た。As a result, a perfect circular alumina-silica fiber 6 having a mullite crystal content of about 8% by weight, an alumina / silica weight ratio of 72:28, and an average fiber diameter of 9 μm was obtained.
Subsequently, the long fiber of the alumina-silica fiber 6 was chopped to a length of 5 mm to be shortened. Thereafter, the short fibers (approximately 1.0 g) are dispersed in water, and the obtained fiber dispersion is poured into a molding frame, and is pressurized and dried.
A 5 mm square mat-shaped fiber aggregate was obtained.
【００６０】そして、ポリビニルアルコールを１．０重
量％含む水溶液に、シリカを４０重量％含むシリカゾル
水溶液（シリカ粒子の平均粒径：１５０ｎｍ）を添加し
て、無機粒子懸濁溶液を作製した。そして、この懸濁溶
液に繊維集合体を１秒〜６０秒程度含浸した後、繊維集
合体を１００℃で１０分以上加熱乾燥した。さらに、乾
燥された繊維集合体を１２３０℃で１０分焼成し、前記
短繊維の繊維外表面６ａに多数の金属酸化物粒子７から
なる微細な凹凸構造を形成した。図６のＳＥＭ写真は、
凹凸構造を有する本実施例のアルミナ−シリカ系繊維６
を示すものである。Then, an aqueous silica sol solution containing 40% by weight of silica (average particle diameter of silica particles: 150 nm) was added to an aqueous solution containing 1.0% by weight of polyvinyl alcohol to prepare a suspension of inorganic particles. Then, the suspension was impregnated with the fiber assembly for about 1 to 60 seconds, and then the fiber assembly was dried by heating at 100 ° C. for 10 minutes or more. Further, the dried fiber assembly was fired at 1230 ° C. for 10 minutes to form a fine uneven structure composed of a large number of metal oxide particles 7 on the fiber outer surface 6a of the short fiber. The SEM photograph of FIG.
Alumina-silica fiber 6 of the present embodiment having an uneven structure 6
It shows.
【００６１】この繊維集合体を面圧評価用サンプルとし
て用い、そのサンプルをオートグラフの圧縮治具内に収
容した。そして、同サンプルに対して厚さ方向から押圧
力を加えて３ｍｍ厚にしたときの、１，１０，１００時
間後の面圧（ＭＰａ）を測定した。その結果を図５のグ
ラフに示す。 （実施例２〜７）実施例２，３，４では、シリカ粒子の
平均粒径をそれぞれ５０ｎｍ，３００ｎｍ，４５０ｎｍ
に設定した。実施例５では、シリカ粒子に代えて平均粒
径３００ｎｍのアルミナ粒子（Ａｌ2Ｏ3粒子）を含む無
機粒子懸濁溶液を作製し、これを用いて凹凸構造形成工
程を行った。実施例６では、シリカ粒子に代えて平均粒
径３００ｎｍのジルコニア粒子（ＺｒＯ2粒子）を含む
無機粒子懸濁溶液を作製し、これを用いて凹凸構造形成
工程を行った。実施例７では、シリカ粒子に代えて平均
粒径３００ｎｍのチタニア粒子（ＴｉＯ2粒子）を含む
無機粒子懸濁溶液を作製し、これを用いて凹凸構造形成
工程を行った。 （比較例）比較例では、凹凸構造形成工程を実施しない
ことを除き、基本的には実施例１に準じて面圧評価用サ
ンプルを作製した。そして、オートグラフを用いて実施
例１と同じく面圧測定試験を行った。その結果を図５の
グラフに示す。 （試験結果）図５のグラフによると、初期面圧値につい
ては、実施例１のほうが比較例に比べて高かった。しか
も、１００時間経過後における面圧の低下度合いは、実
施例１のほうが比較例に比べて明らかに小さかった。具
体的なデータは省略するが、実施例２〜７について同様
の試験を行ったところ、明らかに実施例１に近い好結果
を得ることができた。This fiber assembly was used as a sample for evaluating surface pressure, and the sample was accommodated in a compression jig of an autograph. Then, when a pressing force was applied to the sample from the thickness direction to make the sample 3 mm thick, the surface pressure (MPa) after 1, 10, and 100 hours was measured. The results are shown in the graph of FIG. (Examples 2 to 7) In Examples 2, 3, and 4, the average particle diameter of the silica particles was 50 nm, 300 nm, and 450 nm, respectively.
Set to. In Example 5, an inorganic particle suspension containing alumina particles (Al 2 O 3 particles) having an average particle diameter of 300 nm was prepared in place of the silica particles, and the concave-convex structure forming step was performed using this. In Example 6, an inorganic particle suspension containing zirconia particles (ZrO 2 particles) having an average particle diameter of 300 nm was prepared in place of the silica particles, and the concave-convex structure forming step was performed using the solution. In Example 7, an inorganic particle suspension containing titania particles (TiO 2 particles) having an average particle diameter of 300 nm was prepared in place of the silica particles, and this was used to perform an uneven structure forming step. (Comparative Example) In Comparative Example, a sample for evaluating surface pressure was prepared basically according to Example 1, except that the step of forming an uneven structure was not performed. Then, the same surface pressure measurement test as in Example 1 was performed using an autograph. The results are shown in the graph of FIG. (Test Results) According to the graph of FIG. 5, the initial surface pressure value of Example 1 was higher than that of Comparative Example. Moreover, the degree of decrease in the surface pressure after 100 hours had elapsed was clearly smaller in Example 1 than in Comparative Example. Although specific data is omitted, similar tests were performed for Examples 2 to 7, and a good result close to that of Example 1 was clearly obtained.
【００６２】そして、前記実施例については、さらに上
記繊維集合体を所定形状に打ち抜いて保持シール材４を
作製した後、これを触媒担持体２に巻き付けて金属製シ
ェル３内に圧入した。触媒担持体２としては、外径１３
０ｍｍφ、長さ１００ｍｍのコージェライトモノリスを
用いた。金属製シェル３としては、肉厚１．５ｍｍかつ
内径１４０ｍｍφであって断面Ｏ字状のＳＵＳ３０４製
円筒部材を用いた。このようにして組み立てられた触媒
コンバータ１を、３リットルのガソリンエンジンに実際
に搭載して連続運転するという試験を行った。その結
果、走行時における異音の発生も触媒担持体２のガタつ
きも認められなかった。Then, in the above-described embodiment, after the above fiber assembly was punched into a predetermined shape to form a holding sealing material 4, this was wound around the catalyst carrier 2 and pressed into the metal shell 3. The catalyst carrier 2 has an outer diameter of 13
A cordierite monolith having a diameter of 0 mm and a length of 100 mm was used. As the metal shell 3, a cylindrical member made of SUS304 having a thickness of 1.5 mm, an inner diameter of 140 mmφ, and an O-shaped cross section was used. A test was conducted in which the catalytic converter 1 thus assembled was actually mounted on a 3-liter gasoline engine and operated continuously. As a result, generation of abnormal noise during running and no rattling of the catalyst carrier 2 were observed.
【００６３】従って、本実施形態によれば以下のような
効果を得ることができる。 （１）本実施形態の保持シール材４では、アルミナ−シ
リカ系繊維６の短繊維の外表面６ａに無機質からなる凹
凸構造が設けられている。従って、外表面６ａが滑面状
であるものに比べて繊維の摩擦係数が大きくなる。ゆえ
に、繊維同士の引っ掛かりによって滑り・ズレが生じに
くくなる。従って、繊維集合体を圧縮するような外部荷
重を長時間加えた場合であっても、面圧の低下を引き起
こしにくくなる。また、無機質からなる凹凸構造は耐熱
性にも優れている。ゆえに、保持シール材４が使用時に
１０００℃程度の高温に晒されたとしても、凹凸構造が
焼失・脱落等するようなことはない。よって、大きな摩
擦係数が確実に維持され、この点からしても面圧の低下
を引き起こしにくい構造となる。Therefore, according to the present embodiment, the following effects can be obtained. (1) In the holding sealing material 4 of the present embodiment, an uneven structure made of an inorganic material is provided on the outer surface 6a of the short fiber of the alumina-silica fiber 6. Therefore, the friction coefficient of the fiber is larger than that of the outer surface 6a having a smooth surface. Therefore, slipping and displacement are less likely to occur due to the catch between the fibers. Therefore, even when an external load such as compressing the fiber aggregate is applied for a long time, a decrease in the surface pressure hardly occurs. Further, the uneven structure made of an inorganic material has excellent heat resistance. Therefore, even when the holding sealing material 4 is exposed to a high temperature of about 1000 ° C. during use, the uneven structure does not burn out or fall off. Therefore, a large friction coefficient is reliably maintained, and from this point, a structure that does not easily cause a decrease in surface pressure is obtained.
【００６４】（２）本実施形態の保持シール材４では、
無機質からなる凹凸構造は、繊維外表面６ａに付着した
金属酸化物粒子７からなる。従って、金属酸化物粒子７
がアルミナ−シリカ系繊維６と強固に結合することによ
り、繊維外表面６ａに好適な凹凸形状が保持される。ま
た、エッチング等により繊維外表面６ａの一部を除去す
ること等により凹凸構造を形成したものとは異なり、繊
維自体の外表面形状が保持されるため、繊維自体の物理
的性質の悪化を招くことがない。よって、アルミナ−シ
リカ系繊維６に折れや変形等が生じにくくなり、面圧の
低下も引き起こしにくなる。(2) In the holding sealing material 4 of the present embodiment,
The uneven structure made of inorganic material is composed of metal oxide particles 7 attached to the outer surface 6a of the fiber. Therefore, the metal oxide particles 7
Is firmly bonded to the alumina-silica fiber 6, whereby a suitable uneven shape is maintained on the fiber outer surface 6a. Also, unlike a structure in which the irregular surface structure is formed by removing a part of the fiber outer surface 6a by etching or the like, the outer surface shape of the fiber itself is maintained, thereby deteriorating the physical properties of the fiber itself. Nothing. Therefore, the alumina-silica fiber 6 is unlikely to be broken or deformed, and the surface pressure is not easily reduced.
【００６５】また、金属酸化物粒子７としてシリカ粒子
を選択した場合、アルミナ−シリカ系繊維６との親和性
が極めて高いことから、両者間に高い接合強度が確保さ
れる。即ち、ムライト相８を介してシリカ粒子が強固に
結合された状態となる結果、シリカ粒子が繊維外表面６
ａから脱落しにくくなり、面圧の経時劣化を確実に防止
することができる。When silica particles are selected as the metal oxide particles 7, since the affinity for the alumina-silica fiber 6 is extremely high, a high bonding strength is secured between them. That is, as a result of the silica particles being firmly bound via the mullite phase 8, the silica particles
a, it is possible to prevent the surface pressure from deteriorating with time.
【００６６】（３）本実施形態の保持シール材４では、
金属酸化物粒子７の平均粒径を上記好適範囲内に設定し
ている。従って、製造の困難化を伴うことなく、確実に
アルミナ−シリカ系繊維６の摩擦係数を増大させること
ができる。(3) In the holding sealing material 4 of the present embodiment,
The average particle size of the metal oxide particles 7 is set within the above preferred range. Therefore, the friction coefficient of the alumina-silica fiber 6 can be surely increased without complicating the production.
【００６７】なお、本発明の実施形態は以下のように変
更してもよい。 ・ 実施形態にて例示したアルミナ−シリカ系繊維６の
代わりに、例えば結晶質アルミナ繊維、シリカ繊維等の
ような他のセラミック繊維を用いて、保持シール材４を
作製してもよい。The embodiment of the present invention may be modified as follows. In place of the alumina-silica fiber 6 exemplified in the embodiment, the holding sealing material 4 may be manufactured using other ceramic fibers such as, for example, crystalline alumina fiber and silica fiber.
【００６８】・ 凹凸構造を形成する無機質は粒子状の
みに限定されることはなく、例えば繊維状であっても構
わない。 ・ 無機質からなる粒子として、金属酸化物粒子の代わ
りに金属単体粒子（具体的には金、白金、銀、パラジウ
ム等の貴金属粒子など）を用いてもよい。The inorganic substance forming the uneven structure is not limited to the particle form, but may be, for example, a fibrous form. As the inorganic particles, metal simple particles (specifically, noble metal particles such as gold, platinum, silver, and palladium) may be used instead of metal oxide particles.
【００６９】・ 前記実施形態では、焼結状態にあるア
ルミナ−シリカ系繊維６の外表面６ａに対し、無機粒子
懸濁溶液を付着させた状態で加熱することを行ってい
た。このような処理を、より早期の段階で、例えば数百
℃程度の仮焼成を行って不溶化した前駆体繊維の状態で
実施してもよい。In the above-described embodiment, heating was performed with the inorganic particle suspension solution attached to the outer surface 6a of the alumina-silica fiber 6 in the sintered state. Such a treatment may be performed at an earlier stage, for example, in a state of precursor fibers insoluble by performing preliminary firing at about several hundred degrees Celsius.
【００７０】・ 触媒担持体２の断面形状は真円状に限
定されることはなく、例えば楕円状または長円状等であ
ってもよい。この場合、金属製シェル３の断面形状も、
それに合わせて楕円状または長円状等に変更してもよ
い。The sectional shape of the catalyst carrier 2 is not limited to a perfect circle, but may be, for example, an ellipse or an ellipse. In this case, the cross-sectional shape of the metal shell 3 is also
The shape may be changed to an elliptical shape, an elliptical shape, or the like accordingly.
【００７１】・ 触媒担持体２としては、実施形態のよ
うなハニカム状に成形したコージェライト担体が用いら
れるほか、例えば炭化珪素、窒化珪素等のハニカム多孔
質焼結体などが用いられてもよい。As the catalyst carrier 2, a cordierite carrier formed in a honeycomb shape as in the embodiment may be used, or a honeycomb porous sintered body such as silicon carbide or silicon nitride may be used. .
【００７２】・ 実施形態では、本発明の保持シール材
４を排気ガス浄化装置用触媒コンバータ１に使用した例
を示した。勿論、本発明の保持シール材４は、排気ガス
浄化装置用触媒コンバータ１以外のもの、例えばディー
ゼルパティキュレートフィルタ（ＤＰＦ）や、燃料電池
改質器用触媒コンバータ等に使用することも許容され
る。In the embodiment, an example is shown in which the holding sealing material 4 of the present invention is used for the catalytic converter 1 for an exhaust gas purifying device. Of course, the holding sealing material 4 of the present invention is also allowed to be used for a material other than the catalytic converter 1 for an exhaust gas purifying device, for example, a diesel particulate filter (DPF), a catalytic converter for a fuel cell reformer, and the like.
【００７３】次に、特許請求の範囲に記載された技術的
思想のほかに、前述した実施形態によって把握される技
術的思想を以下に列挙する。 （１） 請求項１乃至５に記載の触媒コンバータ用保持
シール材を製造する方法であって、セラミック繊維紡糸
原液を材料として前駆体繊維を得る紡糸工程と、前記前
駆体繊維を加熱して焼結させる焼成工程と、得られたセ
ラミック繊維を三次元的に集合させてマット状にする成
形工程と、前記集合体に無機粒子懸濁溶液を含浸させた
うえで加熱する凹凸構造形成工程とを含むことを特徴と
する触媒コンバータ用保持シール材の製造方法。従っ
て、この技術的思想１に記載の発明によれば、上記の優
れた触媒コンバータ用保持シール材を確実に製造するこ
とができる。Next, in addition to the technical ideas described in the claims, technical ideas grasped by the above-described embodiments will be enumerated below. (1) A method for producing the holding sealing material for a catalytic converter according to any one of claims 1 to 5, wherein a spinning step of obtaining a precursor fiber using a ceramic fiber spinning stock solution as a material, and heating and firing the precursor fiber. Sintering step, forming step of forming the mat into a mat by gathering the obtained ceramic fibers three-dimensionally, and forming an uneven structure step of heating after impregnating the aggregate with the inorganic particle suspension solution. A method for producing a holding sealing material for a catalytic converter, comprising: Therefore, according to the invention described in the technical idea 1, the excellent catalytic converter holding seal material can be reliably manufactured.
【００７４】（２） セラミック繊維の外表面に無機粒
子懸濁溶液を付着させた状態で加熱することにより、前
記懸濁溶液中に含まれる前記無機粒子を前記外表面に固
定することを特徴とするセラミック繊維外表面の摩擦係
数増大方法。(2) The method is characterized in that the inorganic particles contained in the suspension are fixed to the outer surface by heating the ceramic fiber with the inorganic particle suspension attached to the outer surface. To increase the coefficient of friction of the outer surface of the ceramic fiber.
【００７５】[0075]
【発明の効果】以上詳述したように、請求項１〜５に記
載の発明によれば、面圧の経時劣化が起こりにくい触媒
コンバータ用保持シール材を提供することができる。As described in detail above, according to the first to fifth aspects of the present invention, it is possible to provide a catalytic converter holding seal material in which the surface pressure hardly deteriorates with time.
【００７６】請求項６に記載の発明によれば、上記の優
れた触媒コンバータ用保持シール材の構成材料として好
適なセラミック繊維を提供することができる。請求項７
〜９に記載の発明によれば、上記の優れた触媒コンバー
タ用保持シール材の構成材料として好適なセラミック繊
維を簡単にかつ確実に得ることができる製造方法を提供
することができる。According to the sixth aspect of the present invention, it is possible to provide a ceramic fiber suitable as a constituent material of the excellent sealing material for a catalytic converter. Claim 7
According to the inventions described in (1) to (9), it is possible to provide a manufacturing method capable of easily and reliably obtaining a ceramic fiber suitable as a constituent material of the above-mentioned excellent holding material for a catalytic converter.
【図１】本発明を具体化した一実施形態の触媒コンバー
タ用保持シール材の斜視図。FIG. 1 is a perspective view of a holding material for a catalytic converter according to an embodiment of the present invention.
【図２】実施形態の触媒コンバータを製造工程を説明す
るための斜視図。FIG. 2 is a perspective view for explaining a manufacturing process of the catalytic converter of the embodiment.
【図３】実施形態の触媒コンバータの部分断面図。FIG. 3 is a partial cross-sectional view of the catalytic converter according to the embodiment.
【図４】実施形態のセラミック繊維の要部拡大断面図。FIG. 4 is an enlarged sectional view of a main part of the ceramic fiber of the embodiment.
【図５】実施例及び比較例についての比較試験の結果を
示すグラフ。FIG. 5 is a graph showing the results of a comparative test for Examples and Comparative Examples.
【図６】保持シール材を構成するセラミック繊維のＳＥ
Ｍ写真。FIG. 6 shows SE of a ceramic fiber constituting a holding sealing material.
M photo.
１…触媒コンバータ、２…触媒担持体、３…金属製シェ
ル、４…触媒コンバータ用保持シール材、６…セラミッ
ク繊維としてのアルミナ−シリカ系繊維、７…凹凸構造
を構成する金属酸化物粒子。DESCRIPTION OF SYMBOLS 1 ... Catalytic converter, 2 ... Catalyst support, 3 ... Metal shell, 4 ... Holding sealing material for catalytic converters, 6 ... Alumina-silica fiber as ceramic fiber, 7 ... Metal oxide particles which form an uneven structure.
フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｄ０１Ｆ 9/08 Ｄ０４Ｈ 1/42 Ｄ ４Ｌ０４７ Ｄ０４Ｈ 1/42 Ｂ０１Ｄ 53/36 Ｃ Ｄ０６Ｍ 11/79 Ｄ０６Ｍ 11/12 Ｆターム(参考） 3G091 AB01 BA09 BA10 BA39 GA06 HA26 HA27 HA28 HA29 4D048 BA03X BA06X BA41X BA42X BB02 BB18 4G069 AA08 AA11 AA12 BA01B BA02B BA03A BA03B BA04B BA05B CA03 DA06 EA01X EA01Y EA03X EA09 EB18X EB18Y FB33 4L031 AA24 AA29 AB34 BA09 BA20 DA00 4L037 AT02 CS19 FA03 PA40 PA41 PA45 PF19 PS02 UA20 4L047 AA04 AB02 BA21 BA24 CA02 CB10 CC16 DA00 Continued on the front page (51) Int.Cl. 7 Identification symbol FI Theme coat II (Reference) D01F 9/08 D04H 1/42 D 4L047 D04H 1/42 B01D 53/36 C D06M 11/79 D06M 11/12 F term ( Reference) 3G091 AB01 BA09 BA10 BA39 GA06 HA26 HA27 HA28 HA29 4D048 BA03X BA06X BA41X BA42X BB02 BB18 4G069 AA08 AA11 AA12 BA01B BA02B BA03A BA03B BA04B BA05B CA03 DA06 EA01X EA01Y EA03A19 EB03 A19A18 EB09 A19A18 EB03 PA41 PA45 PF19 PS02 UA20 4L047 AA04 AB02 BA21 BA24 CA02 CB10 CC16 DA00
Claims (9)
要素とし、触媒担持体とその触媒担持体の外周を覆う金
属製シェルとのギャップに配置される保持シール材であ
って、前記セラミック繊維の外表面に無機質からなる凹
凸構造を有することを特徴とする触媒コンバータ用保持
シール材。1. A holding seal material comprising a ceramic fiber assembled in a mat shape as a constituent element and disposed in a gap between a catalyst carrier and a metal shell covering an outer periphery of the catalyst carrier, wherein the holding seal material comprises A holding sealing material for a catalytic converter, which has an uneven structure made of an inorganic material on an outer surface.
ミック繊維の外表面に付着した金属酸化物粒子からなる
ことを特徴とする請求項１に記載の触媒コンバータ用保
持シール材。2. A holding seal material for a catalytic converter according to claim 1, wherein said uneven structure made of inorganic material is made of metal oxide particles attached to an outer surface of said ceramic fiber.
ｍ〜１０００ｎｍであることを特徴とする請求項２に記
載の触媒コンバータ用保持シール材。3. An average particle diameter of the metal oxide particles is 50 n.
The holding sealing material for a catalytic converter according to claim 2, wherein the thickness is from m to 1000 nm.
維を構成する物質からなることを特徴とする請求項２ま
たは３に記載の触媒コンバータ用保持シール材。4. The holding sealing material for a catalytic converter according to claim 2, wherein the metal oxide particles are made of a material constituting the ceramic fiber.
繊維であり、前記金属酸化物粒子はシリカ粒子であるこ
とを特徴とする請求項２または３に記載の触媒コンバー
タ用保持シール材。5. The holding sealing material for a catalytic converter according to claim 2, wherein said ceramic fibers are alumina-silica fibers, and said metal oxide particles are silica particles.
って、その外表面に無機質からなる凹凸構造を有するこ
とを特徴とするセラミック繊維。6. A ceramic fiber constituting a fiber assembly, wherein the ceramic fiber has an uneven structure made of an inorganic material on its outer surface.
る方法であって、焼結状態にあるセラミック繊維または
少なくとも不溶化状態にある前駆体繊維の外表面に無機
粒子懸濁溶液を付着させた状態で加熱することにより、
前記懸濁溶液中に含まれる前記無機粒子を前記外表面に
固定することを特徴とするセラミック繊維の製造方法。7. A method for producing a ceramic fiber according to claim 6, wherein the inorganic particle suspension is adhered to the outer surface of the ceramic fiber in a sintered state or at least the precursor fiber in an insolubilized state. By heating in the state,
A method for producing a ceramic fiber, comprising fixing the inorganic particles contained in the suspension solution to the outer surface.
含む金属酸化物粒子懸濁溶液であることを特徴とする請
求項７に記載のセラミック繊維の製造方法。8. The method according to claim 7, wherein the inorganic particle suspension is a metal oxide particle suspension containing a water-soluble polymer.
外表面に、平均粒径５０ｎｍ〜１０００ｎｍのシリカ粒
子及び水溶性高分子を含む懸濁溶液を付着させ、この状
態で加熱乾燥を行った後、さらに１２００℃以上の温度
で焼成することにより、前記懸濁溶液中に含まれる前記
シリカ粒子を前記外表面に固定することを特徴とする請
求項７に記載のセラミック繊維の製造方法。9. A suspension containing silica particles having an average particle diameter of 50 nm to 1000 nm and a water-soluble polymer is adhered to the outer surface of the alumina-silica fiber in a sintered state, and heated and dried in this state. 8. The method according to claim 7, wherein the silica particles contained in the suspension solution are fixed to the outer surface by further firing at a temperature of 1200 ° C. or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001003889A JP2002206421A (en) | 2001-01-11 | 2001-01-11 | Holding-seal material for catalytic converter, ceramic fiber, and method of manufacturing the ceramic fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001003889A JP2002206421A (en) | 2001-01-11 | 2001-01-11 | Holding-seal material for catalytic converter, ceramic fiber, and method of manufacturing the ceramic fiber |
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