JPS6236088A - Method of forming ceramic coating layer - Google Patents
Method of forming ceramic coating layerInfo
- Publication number
- JPS6236088A JPS6236088A JP60173840A JP17384085A JPS6236088A JP S6236088 A JPS6236088 A JP S6236088A JP 60173840 A JP60173840 A JP 60173840A JP 17384085 A JP17384085 A JP 17384085A JP S6236088 A JPS6236088 A JP S6236088A
- Authority
- JP
- Japan
- Prior art keywords
- ceramic
- coating layer
- thermal expansion
- shaped
- reinforcing layer
- 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
- 238000000034 method Methods 0.000 title claims description 22
- 239000011247 coating layer Substances 0.000 title claims description 10
- 238000005524 ceramic coating Methods 0.000 title claims description 9
- 239000000919 ceramic Substances 0.000 claims description 55
- 239000002002 slurry Substances 0.000 claims description 22
- 239000000454 talc Substances 0.000 claims description 18
- 229910052623 talc Inorganic materials 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 17
- 229910052878 cordierite Inorganic materials 0.000 claims description 9
- 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 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 238000005245 sintering Methods 0.000 claims 1
- 239000010410 layer Substances 0.000 description 25
- 230000003014 reinforcing effect Effects 0.000 description 23
- 239000006260 foam Substances 0.000 description 18
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 14
- 239000000203 mixture Substances 0.000 description 8
- 230000002093 peripheral effect Effects 0.000 description 6
- 229920005862 polyol Polymers 0.000 description 6
- 150000003077 polyols Chemical class 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000001125 extrusion Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000012948 isocyanate Substances 0.000 description 4
- 150000002513 isocyanates Chemical class 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Chemical compound C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 description 2
- 239000004721 Polyphenylene oxide Substances 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005187 foaming Methods 0.000 description 2
- 239000004088 foaming agent Substances 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920000609 methyl cellulose Polymers 0.000 description 2
- 239000001923 methylcellulose Substances 0.000 description 2
- 235000010981 methylcellulose Nutrition 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000006082 mold release agent Substances 0.000 description 2
- 229920000570 polyether Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 239000004604 Blowing Agent Substances 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 229920005830 Polyurethane Foam Polymers 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000004323 axial length Effects 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 239000007809 chemical reaction catalyst Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000004872 foam stabilizing agent Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- -1 organic acid salts Chemical class 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 229920005906 polyester polyol Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000011496 polyurethane foam Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical group CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 1
- CYRMSUTZVYGINF-UHFFFAOYSA-N trichlorofluoromethane Chemical compound FC(Cl)(Cl)Cl CYRMSUTZVYGINF-UHFFFAOYSA-N 0.000 description 1
- 229940029284 trichlorofluoromethane Drugs 0.000 description 1
Landscapes
- Devices For Post-Treatments, Processing, Supply, Discharge, And Other Processes (AREA)
- Catalysts (AREA)
Abstract
(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、例えば内燃機関より排出される排ガス中に浮
遊するカーボン微粒子を捕集する捕集担体あるいは排ガ
ス浄化用触媒担体等として有効に用いられるセラミック
構造体のセラミック被覆層の形成方法に関する。[Detailed Description of the Invention] [Field of Industrial Application] The present invention can be effectively used, for example, as a collection carrier for collecting carbon fine particles suspended in exhaust gas discharged from an internal combustion engine, or as a catalyst carrier for exhaust gas purification. The present invention relates to a method for forming a ceramic coating layer of a ceramic structure.
従来例えばディーゼルエンジンより排出される排ガス中
のカーボン微粒子捕集用フィルタとしては、三次元網目
状のセラミック骨格を有する多孔質セラミックフィルタ
が有効に用いられている。BACKGROUND ART Porous ceramic filters having a three-dimensional mesh ceramic skeleton have been effectively used as filters for collecting carbon particulates in exhaust gas emitted from, for example, diesel engines.
このフィルタは振動等の外力に対して強度が小さく、破
損を避ける方法として実開昭５４−９６７４８号公報に
開示されているように、三次元網目状の多孔質セラミッ
ク構造体の外周面に補強層を設けたものが知られている
。このような従来のセラミック構造体は、外周面に形成
された補強層と、内部の三次元網目構造セラミックとの
熱膨張係数がほぼ等しいために、熱衝撃に対して補強層
と内部の多孔質セラミックの温度分布に起因して補強層
にクランクが発生したり、補強層が剥離するという欠点
があった。This filter has low strength against external forces such as vibrations, and as a method to avoid damage, as disclosed in Japanese Utility Model Application Publication No. 54-96748, the outer peripheral surface of the three-dimensional mesh porous ceramic structure is reinforced. One with layers is known. In such conventional ceramic structures, the reinforcing layer formed on the outer peripheral surface and the internal three-dimensional network structure ceramic have approximately the same coefficient of thermal expansion. There were drawbacks such as cracks occurring in the reinforcing layer and peeling of the reinforcing layer due to the temperature distribution of the ceramic.
これに対して実開昭５４−９６７４８号公報にはこのよ
うな温度分布が発生しても補強層にクランクや剥離が発
生しないように補強層の熱膨張係数を内部の多孔質セラ
ミックよりも小さくしたものが開示されている。On the other hand, in Japanese Utility Model Application Publication No. 54-96748, the coefficient of thermal expansion of the reinforcing layer is made smaller than that of the porous ceramic inside so that the reinforcing layer does not crack or peel even if such a temperature distribution occurs. What has been done is disclosed.
しかしながら上記公報には、補強層の熱膨張係数を制御
する具体的方法は記載されておらず、また本発明者らの
実験研究の結果からは、例えばコーディエライト質セラ
ミックの組成を変化させて、このセラミックスラリ−を
塗布等の手段によって付着させ燃焼することによって補
強層を形成する方法は、熱膨張係数の制御がそれほど容
易ではなく、操作も簡便とはいえないという問題があっ
た。However, the above publication does not describe a specific method for controlling the thermal expansion coefficient of the reinforcing layer, and the results of the inventors' experimental research suggest that, for example, by changing the composition of the cordierite ceramic. However, the method of forming a reinforcing layer by depositing this ceramic slurry by means such as coating and burning it has problems in that it is not so easy to control the coefficient of thermal expansion and the operation cannot be said to be simple.
そこで本発明は、上記問題点を解消するために板状もし
くは針状のタルク粒子を含むコーディエライト質セラミ
ックスラリ−を、所定の間隙を有するスリット部から流
出させることにより、前記セラミック粒子を流出方向に
配向させる工程と、この流出したセラミックスラリ−を
コーディエライト質多孔性セラミックス構造体に被覆す
る工程と、
このセラミック構造体を加熱焼結させることにより、前
記被覆層の熱膨張係数を前記多孔性セラミックの熱膨張
係数よりも小さくさせる工程とよりなるセラミック被覆
層の形成方法を採用するものである。Therefore, in order to solve the above-mentioned problems, the present invention allows a cordierite ceramic slurry containing plate-shaped or needle-shaped talc particles to flow out through a slit portion having a predetermined gap, thereby allowing the ceramic particles to flow out. A step of orienting the ceramic slurry in the direction of This method employs a method of forming a ceramic coating layer that includes a step of making the coefficient of thermal expansion smaller than that of the porous ceramic.
上記方法によれば、一定の間隙から押し出されるセラミ
ックスラリ−中の、板状または針状のセラミック粒子が
押し出し方向に配向させられるとともに、セラミック構
造体の外周面に補強層を形成することができる。According to the above method, the plate-shaped or needle-shaped ceramic particles in the ceramic slurry extruded from a certain gap can be oriented in the extrusion direction, and a reinforcing layer can be formed on the outer peripheral surface of the ceramic structure. .
従って本発明の方法によれば、板状もしくは針状のセラ
ミック粒子のセラミックスラリ−に対する配合割合と、
セラミックスラリ−の流出する間隙を調整することによ
り非常に容易に、所望の熱膨張係数、を有する補強層を
形成することができるというすぐれた効果がある。Therefore, according to the method of the present invention, the mixing ratio of plate-shaped or needle-shaped ceramic particles to the ceramic slurry,
An excellent effect is that a reinforcing layer having a desired coefficient of thermal expansion can be formed very easily by adjusting the gap through which the ceramic slurry flows out.
以下本発明を図に示す実施例に基づいて詳細に説明する
。第２図（ａ）、 （ｂ）は本発明のセラミック被覆層
形成方法によって補強層を形成させた円筒形セラミック
フィルタ１の外形を説明する正面図および軸線方向断面
図である。フィルタ１の内部２は、第３図の拡大模式図
に示すように三次元綱目状のコーディエライト組成セラ
ミック骨格３により多数の連通孔４を形成する多孔質セ
ラミックよりなる。外周部にはコーディエライト組成の
うちタルク５が板状の粒子形状で粒径（平面方向の最も
寸法の大きい部分の長さをいう）１０μ以上のものを含
み、この板状タルク粒子５が周方向に配向させて形成さ
れた補強層６が厚さ１．５Ｎで被覆されている。The present invention will be explained in detail below based on embodiments shown in the drawings. FIGS. 2(a) and 2(b) are a front view and an axial cross-sectional view illustrating the outer shape of a cylindrical ceramic filter 1 in which a reinforcing layer is formed by the ceramic coating layer forming method of the present invention. The interior 2 of the filter 1 is made of porous ceramic in which a large number of communicating pores 4 are formed by a three-dimensional mesh-like cordierite composition ceramic skeleton 3, as shown in the enlarged schematic diagram of FIG. In the outer peripheral part, talc 5 of the cordierite composition has a plate-like particle shape and a particle size (meaning the length of the largest part in the plane direction) of 10 μ or more, and this plate-shaped talc particle 5 A reinforcing layer 6 formed and oriented in the circumferential direction is coated with a thickness of 1.5N.
次にこのセラミックフィルタ１の製造方法について説明
する。一般に三次元網目状構造を有するセラミックフィ
ルタを得るには、同様な三次元網目構造を有するポリウ
レタンフォームなどの有機発泡体を骨材として使用し、
この骨材の表面にセラミック材料を固着し、これを焼成
すると母材たる有機化合物が燃焼飛散し、周囲のセラミ
ック材が母材と同様の構造となることを利用する。Next, a method for manufacturing this ceramic filter 1 will be explained. Generally, to obtain a ceramic filter having a three-dimensional network structure, an organic foam such as polyurethane foam having a similar three-dimensional network structure is used as an aggregate.
A ceramic material is fixed to the surface of this aggregate, and when it is fired, the organic compound that is the base material is burned and scattered, and the surrounding ceramic material takes advantage of the fact that it has the same structure as the base material.
すなわちウレタンフオームの成形は、セラミックフィル
タ１と同一の外形形状のキャビティを有する金型のキャ
ビティ内面に予めワックス系離型剤を、成形型の離型剤
の融点以上に加熱しておき、スプレーまたはハケ塗りに
よって塗布する。次に成形型を３０〜５０℃に調整して
おき、成形型容器内に有機イソシアネート、ポリオール
、整泡剤、発泡剤および触媒を混合したウレタンフオー
ム原料混合液を攪拌混合しながら注入する。ここで、前
記有機イソシアネートとし°ζは、トリレンジイソシア
ネート、またはジフェニルメタンジイソシアネートまた
は両者の混合物、前記ポリオールとしては、ポリエーテ
ルポリオールおよび、またはポリエステル系ポリオール
とからなる重合体ポリオール、またはこれとポリエーテ
ルポリオールとの混合物、前記発泡剤としては、水また
は、ノ＼ロゲン置換脂肪族炭化水素系発泡剤（トリクロ
ロモノフロロメタンなどのフロンｇ）、または両者の混
合物、前記整泡剤としては、アルコール変性シリコーン
整泡剤、前記触媒としては、樹脂化反応を促進する触媒
としてアルコールとイソシアネートとの反応触媒として
有効に用いられる３級アミンおよびその有機酸塩類、発
泡反応を促進する触媒としては、水とイソシアネートと
の反応触媒として有効にもちいられるモルホリン、エタ
ノールアミン等を用いた。ウレタンフオーム原料混合液
をキャビティ内で発泡させた後１００℃〜１２０℃で２
０〜６０分間加熱硬化させる。In other words, the urethane foam is molded by heating a wax-based mold release agent on the inner surface of the cavity of a mold having the same external shape as the ceramic filter 1 above the melting point of the mold release agent, and then spraying or Apply by brushing. Next, the temperature of the mold is adjusted to 30 to 50° C., and a urethane foam raw material mixture containing an organic isocyanate, a polyol, a foam stabilizer, a blowing agent, and a catalyst is poured into the mold container while stirring and mixing. Here, the organic isocyanate is tolylene diisocyanate, diphenylmethane diisocyanate, or a mixture of both, and the polyol is a polymer polyol consisting of a polyether polyol and/or a polyester polyol, or a polymer polyol consisting of this and a polyether polyol. The foaming agent is water or a nitrogen-substituted aliphatic hydrocarbon foaming agent (fluorocarbons such as trichloromonofluoromethane), or a mixture of the two, and the foam stabilizer is alcohol-modified silicone. Foam stabilizers, the catalysts include tertiary amines and organic acid salts thereof, which are effectively used as catalysts for the reaction between alcohol and isocyanate, and catalysts for promoting the foaming reaction, such as water and isocyanates. Morpholine, ethanolamine, etc., which can be effectively used as reaction catalysts, were used. After foaming the urethane foam raw material mixture in the cavity, it is heated at 100℃ to 120℃ for 2 hours.
Heat and cure for 0 to 60 minutes.
次に、このウレタンフオーム成形体にセラミックスラリ
−を含浸させた後、ポリウレタンを焼成し多孔質セラミ
ックフィルタを得る方法について詳述する。含浸に使用
されるセラミックスラリ−の原料は、焼成によりコーデ
ィエライト組成となる酸化マグネシウム（ＭｇＯ）、ア
ルミナ（Ａ ｊ！ ｚＯｌ）、ケイ酸（ＳｉＯ□）を含
む混合粉末、あるいは上記混合粉末を加熱しコーディエ
ライト系セラミックにし、これを粉末化した合成コーデ
ィエライト粉末、あるいは両者の混合物にメチルセルロ
ース、ポリビニルアルコール等のバインダ、および水を
加えたものである。前記ウレタンフオームの通気孔に存
在する薄膜を公知の爆発処理、ＮａＯＨ処理、オゾン処
理等によって除いた後、ウレタンフオームをこのスラリ
ーに含浸した後、エアガンや遠心分離装置を用いて余分
なスラリーを除去し、１００〜１５０℃の乾燥炉の中で
２〜３時間乾燥する。以上の含浸から乾燥までの毘作を
２〜３回繰り返し、必要量のセラミックスラリ−をウレ
タンフオーム発泡体骨格表面に付着させる。Next, a method for obtaining a porous ceramic filter by impregnating the urethane foam molded body with a ceramic slurry and then firing the polyurethane will be described in detail. The raw material for the ceramic slurry used for impregnation is a mixed powder containing magnesium oxide (MgO), alumina (Aj! Synthetic cordierite powder is prepared by heating to produce cordierite ceramic and pulverizing it, or a mixture of the two is prepared by adding a binder such as methyl cellulose or polyvinyl alcohol, and water. After removing the thin film present in the vents of the urethane foam by known explosion treatment, NaOH treatment, ozone treatment, etc., the urethane foam is impregnated into this slurry, and then excess slurry is removed using an air gun or centrifugal separator. and dry for 2 to 3 hours in a drying oven at 100 to 150°C. The above process from impregnation to drying is repeated two or three times to deposit the required amount of ceramic slurry on the surface of the urethane foam skeleton.
次にこのセラミックスラリ−を付着させたウレタンフオ
ームを第１図に示す装置で補強層６を形成させた。すな
わち平均粒径１０μの板状タルク５を約３０ｗｔ％、お
よび粉末状カオリン、水酸化アルミニウムを焼成してな
る合成コーディエライト１００部、水３０〜４０分、有
機バインダ３〜５部、界面活性剤０．１〜２部からなる
粘土１０万〜１００万ｃｐｓ程度の高粘土スラリー７を
タンク８に充填し、タンク８の上部をおおう蓋９に接続
された配管１０より１０ｋｇ／ｃＪの空気圧力で加圧し
、タンク８の下部に設けられたスリット８ａよりセラミ
ックスラリ−を押し出した。このスリット８ａは第４図
のその拡大断面図に示すように先端先細り形状となって
おり、その先端部の間隙ｄは１．５ｆｉである。なおこ
のタンク８は紙面垂直方向にセラミックフィルタの軸方
向長さとほぼ同じ長さを有しており、スリット８ａも同
様である。従って押し出されるセラミックスラリ−は厚
さ１．５ ｍのシート状である。この押し出しの際に第
４図に示すようにセラミックラリ−中に含まれる板状タ
ルク５は、先端先細り形状のスリット８ａの先端部に近
づくに従って押し出し方向に平行となるよう配向させら
れ、押し出されたあとはその大部分が配向し、第５図に
セラミックフィルタｌの補強Ｊｉ６の拡大断面図を示す
ように、タルク粒子５は周方向に配向形成されている０
次にこのシート状セラミックスラリ−は、このスリット
８ａの下方に回転可能に設けられたセラミックスラリ−
を付着させたウレタンフオームの外周部にこれを回転さ
せながら巻付被覆した。Next, a reinforcing layer 6 was formed on the urethane foam to which this ceramic slurry was adhered using the apparatus shown in FIG. That is, about 30 wt % of plate-shaped talc 5 with an average particle size of 10 μm, powdered kaolin, 100 parts of synthetic cordierite obtained by firing aluminum hydroxide, 30 to 40 minutes of water, 3 to 5 parts of an organic binder, and surface activity. A tank 8 is filled with a high clay slurry 7 of about 100,000 to 1,000,000 cps consisting of 0.1 to 2 parts of clay, and an air pressure of 10 kg/cJ is supplied from a pipe 10 connected to a lid 9 covering the top of the tank 8. The ceramic slurry was pressed out through the slit 8a provided at the bottom of the tank 8. The slit 8a has a tapered tip as shown in the enlarged sectional view of FIG. 4, and the gap d at the tip is 1.5 fi. Note that this tank 8 has approximately the same length in the direction perpendicular to the plane of the paper as the axial length of the ceramic filter, and the slit 8a also has the same length. Therefore, the extruded ceramic slurry is in the form of a sheet with a thickness of 1.5 m. During this extrusion, as shown in FIG. 4, the plate-shaped talc 5 contained in the ceramic rally is oriented parallel to the extrusion direction as it approaches the tip of the slit 8a, which has a tapered tip, and is extruded. After that, most of the talc particles 5 are oriented in the circumferential direction, and as shown in FIG.
Next, this sheet-like ceramic slurry is transferred to a ceramic slurry rotatably provided below this slit 8a.
This was wrapped and coated around the outer periphery of the urethane foam to which it had been attached while rotating.
次にこのフオームを１００〜１５０℃で１〜３時間乾燥
させた後、炉内に入れ１３５０〜１４１０℃の温度で１
〜３時間焼成することにより可燃性のウレタンフオーム
を消失させることによってセラミックフィルタｌが製作
できた。ちなみに、焼成後の補強層２の熱膨張係数は１
．８ Ｘ １０−ｈ／”Ｃ１内部の多孔質セラミックの
それは２． ＯＸ １０−６／’Ｃであった。Next, this foam is dried at 100-150°C for 1-3 hours, then placed in a furnace and heated at 1350-1410°C for 1 to 3 hours.
A ceramic filter 1 could be manufactured by burning for ~3 hours to eliminate the flammable urethane foam. By the way, the thermal expansion coefficient of the reinforcing layer 2 after firing is 1.
．． That of the porous ceramic inside 8 x 10-h/'C1 was 2.OX 10-6/'C.
第６図は押し出しスリット８ａの間隔を変化させた時の
板状タルクの配向割合と、熱膨張係数の変化の様子を測
定した結果を説明する特性図で、スリットの間隔が小さ
いほど配向性は高く熱膨張係数は小さくなる。板状タル
クはその結晶格子のａ、ｂ、ｃ軸方向に関してＣ軸方向
の熱膨張係数が小さいことが知られており、上記のよう
な方法により板状タルクを補強層の面方向に積層するよ
うに配向させるとこのＣ軸方向の低熱膨張係数の影響が
補強層の面方向の熱膨張係数を低下させる方向に表れる
。FIG. 6 is a characteristic diagram illustrating the results of measuring the orientation ratio of plate-like talc and the change in thermal expansion coefficient when the interval between extrusion slits 8a is changed; the smaller the interval between the slits, the better the orientation. The higher the thermal expansion coefficient, the lower the coefficient of thermal expansion. It is known that plate-shaped talc has a small coefficient of thermal expansion in the C-axis direction with respect to the a, b, and c-axis directions of its crystal lattice, and plate-shaped talc is laminated in the plane direction of the reinforcing layer by the method described above. When the reinforcing layer is oriented in this manner, the effect of the low coefficient of thermal expansion in the C-axis direction appears in a direction that lowers the coefficient of thermal expansion in the plane direction of the reinforcing layer.
第７図は板状タルク５の平均粒径を変化させたときの配
向割合をスリット８ａの間隔０．５鰭、ｌ。FIG. 7 shows the orientation ratio when the average grain size of the plate-shaped talc 5 is changed at a spacing of 0.5 fins and 1 between the slits 8a.
５Ｎの二水準で測定した結果を示すもので、１０μ以下
では配向の割合は小さく、粒・径が大きくなるに従って
配向め割合は大きくなるが、１００μを超えると補強層
表面がガサガサとなり機械的強度も低下するので好まし
くない。This shows the results measured at two levels of 5N. Below 10μ, the orientation ratio is small, and as the grain size increases, the orientation ratio increases, but when it exceeds 100μ, the surface of the reinforcing layer becomes rough and the mechanical strength deteriorates. This is not preferable as it also lowers the amount of water.
第８図は押し出し圧力を変化させたときの配向の割合の
変化を板状タルク５の平均粒径１０μ、スリット８ａの
間隔１．５龍で測定した結果を示すもので、押し出し圧
力が大きいほど配向の割合は大きくなるが、３ｋｇ／−
でも８０％以上の配向割合とすることが可能であった。Figure 8 shows the results of measuring the change in the orientation ratio when the extrusion pressure is changed, with the average grain size of the plate-shaped talc 5 being 10 μm and the spacing between the slits 8a being 1.5 mm. Although the orientation ratio increases, 3 kg/-
However, it was possible to achieve an orientation ratio of 80% or more.
以上のように配向の割合を変化させることにより熱膨張
係数の異なる補強層６を形成したセラミックフィルタ１
の熱衝撃試験をあらかじめ所定の温度に加熱保持した加
熱炉中にフィルタ１を入れることによって調べた。従来
の板状タルク５を含まず熱膨張係数が２．ＯＸ １０−
’／’Ｃで、内部の多孔質セラミックと同じものでは炉
内温度６００〜６５０℃でクラックを発生するのに対し
、本発明の方法により熱膨張係数を１．８ Ｘ １０−
”／’Ｃ以下にしたものでは８００〜８５０℃までクラ
ンクが発生せず熱衝撃に強いことが示された。そして、
補強層の熱膨張係数は１．９〜１．５ Ｘ １０−ｂ／
’Ｃ１すなわち内部の多孔質セラミックの熱膨張係数よ
り０．１〜０．５ Ｘ １０−’／’Ｃ小さい範囲で本
発明の耐熱衝撃特性の向上が確認された。Ceramic filter 1 in which reinforcing layers 6 having different coefficients of thermal expansion are formed by changing the orientation ratio as described above.
A thermal shock test was conducted by placing the filter 1 in a heating furnace that had been heated and maintained at a predetermined temperature in advance. It does not include the conventional plate-shaped talc 5 and has a thermal expansion coefficient of 2. OX 10-
'/'C, if the porous ceramic is the same as the internal one, cracks will occur at the furnace temperature of 600 to 650°C, but the method of the present invention reduces the thermal expansion coefficient to 1.8 x 10-
It was shown that when the temperature was lower than '/'C, cranking did not occur up to 800-850℃, making it resistant to thermal shock.
The thermal expansion coefficient of the reinforcing layer is 1.9 to 1.5 x 10-b/
It was confirmed that the thermal shock resistance of the present invention was improved within a range of 0.1 to 0.5 x 10-'/'C smaller than the thermal expansion coefficient of 'C1, that is, the internal porous ceramic.
また本発明のセラミック被覆層の形成方法としては、第
９図に示すようにセラミックスラリ−を付着させたウレ
タンフオームの外周表面をＰＶＡ、メチルセルロース等
で固化させ空孔を充填閉塞させた緻密Ｎ２Ｂを形成した
後、回転可能に固定し、このウレタンフオーム外周表面
とその先端部で１゜５鶴の間隔を保つヘラ１１との間に
板状タルク５を含むセラミックスラリ−を入れ、ウレタ
ンフオームを回転させることにより補強層６を塗布形成
させてもよい。この場合ヘラ１１の先端部はウレタンフ
オーム外周面との間隙が徐々に狭くなるよう形成されて
いるので前述の実施例と同様に板状タルク５の配向を促
し、補強層６の熱膨張係数が小さくなる。As shown in FIG. 9, the method for forming the ceramic coating layer of the present invention is to use dense N2B, which is made by solidifying the outer peripheral surface of urethane foam to which ceramic slurry is attached with PVA, methylcellulose, etc., and filling and closing the pores. After forming, a ceramic slurry containing plate-like talc 5 is placed between a spatula 11 which is rotatably fixed and maintains a spacing of 1°5 between the outer circumferential surface of the urethane foam and its tip, and the urethane foam is rotated. The reinforcing layer 6 may be formed by coating. In this case, since the tip of the spatula 11 is formed so that the gap with the outer peripheral surface of the urethane foam gradually narrows, the orientation of the plate-like talc 5 is promoted as in the previous embodiment, and the coefficient of thermal expansion of the reinforcing layer 6 is increased. becomes smaller.
また本発明の補強層形成用セラミックスラリ−中に含ま
れる配向粒子は板状タルク５のみに限定されるものでは
なく、針状のものでもよい（なおこの場合の粒径とは軸
方向の長さをいうものとする）。Furthermore, the oriented particles contained in the ceramic slurry for forming a reinforcing layer of the present invention are not limited to only the plate-shaped talc 5, but may also be needle-shaped (in this case, the particle size refers to the length in the axial direction). ).
第１図は本発明のセラミック被覆層の形成方法を説明す
る断面模式図、第２図（ａ）、 （ａｌ−＝−は本発明
の方法により製作したセラミックフィルタ１の形状を説
明する正面図および軸線方向断面図、第３′図は三次元
網目状セラミック骨格の形状を説明する模式図、第４図
、第５図は補強層６の構造を示す部分拡大図、第６図、
第７図、第８図は種々の条件における板状タルクの配向
割合の変化を説明する特性図、第９図は本発明の他の実
施例の方法を説明する断面模式図である。
６・・・補強層、７・・・セラミックスラリ−０代理人
弁理士 岡 部 隆
第１図
（、） （ｂ ）第２図
第３図
第４図 第５図
スリマ￥−ｄの幡 ｒｍｍ ）
第６図
寥ｔ 投 （μ）
第７図
０．１ １ １０ １００押し＄しＦ
Ｌ刀 （蓼−Ｌ）
第８図
第９図FIG. 1 is a schematic cross-sectional view illustrating the method of forming a ceramic coating layer of the present invention, and FIG. 2(a) is a front view illustrating the shape of the ceramic filter 1 manufactured by the method of the present invention and an axial sectional view, FIG. 3' is a schematic diagram explaining the shape of the three-dimensional mesh ceramic skeleton, FIGS. 4 and 5 are partially enlarged views showing the structure of the reinforcing layer 6, FIG.
7 and 8 are characteristic diagrams illustrating changes in the orientation ratio of plate-shaped talc under various conditions, and FIG. 9 is a schematic cross-sectional diagram illustrating a method according to another embodiment of the present invention. 6... Reinforcement layer, 7... Ceramic slurry - 0 Representative Patent Attorney Takashi Okabe Figure 1 (,) (b) Figure 2 Figure 3 Figure 4 Figure 5 Slima ￥-d no Hanata rmm ) Figure 6 t Throw (μ) Figure 7 0.1 1 10 100 push $ F
L sword (蓼-L) Figure 8 Figure 9
Claims (3)
ライト質セラミックスラリーを、所定の間隙を有するス
リット部から流出させることにより、前記セラミック粒
子を流出方向に配向させる工程と、 この流出したセラミックスラリーをコーディエライト質
多孔性セラミックス構造体に被覆する工程と、 このセラミック構造体を加熱焼結させることにより、前
記被覆層の熱膨張係数を前記多孔性セラミックの熱膨張
係数よりも小さくさせる工程とよりなるセラミック被覆
層の形成方法。(1) A step of orienting the ceramic particles in the flow direction by flowing a cordierite ceramic slurry containing plate-shaped or needle-shaped talc particles through a slit portion having a predetermined gap; a step of coating a cordierite porous ceramic structure with the slurry; and a step of heating and sintering the ceramic structure to make the coefficient of thermal expansion of the coating layer smaller than the coefficient of thermal expansion of the porous ceramic. A method for forming a ceramic coating layer.
セラミック粒子の粒径の５０〜１５０倍であることを特
徴とする特許請求の範囲第１項記載のセラミック被覆層
の形成方法。(2) The method for forming a ceramic coating layer according to claim 1, wherein the gap between the slits is 50 to 150 times the particle size of the plate-shaped or needle-shaped ceramic particles.
ことを特徴とする特許請求の範囲第１項または第２項記
載のセラミック被覆層の形成方法。(3) The method for forming a ceramic coating layer according to claim 1 or 2, wherein the talc particles have a particle size of 10 to 100 microns.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60173840A JPS6236088A (en) | 1985-08-07 | 1985-08-07 | Method of forming ceramic coating layer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60173840A JPS6236088A (en) | 1985-08-07 | 1985-08-07 | Method of forming ceramic coating layer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6236088A true JPS6236088A (en) | 1987-02-17 |
Family
ID=15968131
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP60173840A Pending JPS6236088A (en) | 1985-08-07 | 1985-08-07 | Method of forming ceramic coating layer |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6236088A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1977827A1 (en) * | 2007-03-07 | 2008-10-08 | Ibiden Co., Ltd. | Catalyst carrier |
| WO2008126308A1 (en) * | 2007-03-30 | 2008-10-23 | Ibiden Co., Ltd. | Catalyst carrier |
| JP2008272728A (en) * | 2007-03-30 | 2008-11-13 | Ibiden Co Ltd | Catalyst carrier |
-
1985
- 1985-08-07 JP JP60173840A patent/JPS6236088A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1977827A1 (en) * | 2007-03-07 | 2008-10-08 | Ibiden Co., Ltd. | Catalyst carrier |
| WO2008126308A1 (en) * | 2007-03-30 | 2008-10-23 | Ibiden Co., Ltd. | Catalyst carrier |
| JP2008272728A (en) * | 2007-03-30 | 2008-11-13 | Ibiden Co Ltd | Catalyst carrier |
| US7871958B2 (en) | 2007-03-30 | 2011-01-18 | Ibiden Co., Ltd. | Catalyst carrier |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP2604876B2 (en) | Method for manufacturing ceramic honeycomb structure | |
| US4869944A (en) | Cordierite honeycomb-structural body and a method for producing the same | |
| JP4266103B2 (en) | Method for producing porous ceramic body | |
| EP1679120B1 (en) | Honeycomb structure and method of producing the same | |
| EP2119487B1 (en) | Honeycomb structure and method for manufacturing the same | |
| JPS61293518A (en) | Ceramic structure | |
| US20110151181A1 (en) | Fiber Enhanced Porous Substrate | |
| EP1780187A1 (en) | Honeycomb structure | |
| KR101677486B1 (en) | Ceramic honeycomb structure and process for producing same | |
| US8551579B2 (en) | Method for producing ceramic honeycomb structure | |
| JP4001800B2 (en) | Method for manufacturing honeycomb catalyst carrier | |
| JPS61183182A (en) | Porous ceramic structure | |
| EP1816323B2 (en) | Plugged honeycomb structure | |
| WO2005068396A1 (en) | Honeycomb structure and method for producing the same | |
| JPS6236088A (en) | Method of forming ceramic coating layer | |
| JPH04187578A (en) | Production of sintered compact of porous silicon carbide | |
| JP2651170B2 (en) | Ceramics porous body | |
| JPS62149317A (en) | Porous ceramic structural body and its production | |
| JP2901303B2 (en) | Method for producing porous silicon carbide sintered body | |
| JPH03257081A (en) | Production of porous ceramics | |
| JPS62234519A (en) | Porous ceramic structural body | |
| JPS5842418Y2 (en) | porous ceramic structure | |
| JPS6236082A (en) | Porous ceramic structure | |
| JPS6011281A (en) | Ceramic three dimentional network structure and manufacture | |
| JPS6240166B2 (en) |