JPH1133322A - Manufacture of ceramic filter - Google Patents
Manufacture of ceramic filterInfo
- Publication number
- JPH1133322A JPH1133322A JP19703197A JP19703197A JPH1133322A JP H1133322 A JPH1133322 A JP H1133322A JP 19703197 A JP19703197 A JP 19703197A JP 19703197 A JP19703197 A JP 19703197A JP H1133322 A JPH1133322 A JP H1133322A
- Authority
- JP
- Japan
- Prior art keywords
- ceramic
- porous support
- thin film
- ceramics
- temperature
- 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
- 239000000919 ceramic Substances 0.000 title claims abstract description 60
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 45
- 239000010409 thin film Substances 0.000 claims abstract description 33
- 239000002002 slurry Substances 0.000 claims abstract description 23
- 238000005245 sintering Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000011148 porous material Substances 0.000 claims description 21
- 238000001354 calcination Methods 0.000 claims description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 11
- 238000010304 firing Methods 0.000 claims description 8
- 239000011164 primary particle Substances 0.000 claims description 7
- 239000011163 secondary particle Substances 0.000 claims description 5
- 239000010408 film Substances 0.000 abstract description 17
- 230000001747 exhibiting effect Effects 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract 1
- 230000009545 invasion Effects 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 17
- 230000007547 defect Effects 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 229920000609 methyl cellulose Polymers 0.000 description 2
- 239000001923 methylcellulose Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 230000000153 supplemental effect Effects 0.000 description 2
- 239000002562 thickening agent Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 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 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 238000007569 slipcasting Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
Landscapes
- Filtering Materials (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】この発明は、特に半導体製造
装置、例えばエッチング、拡散などにおいて気体中のパ
ーティクル除去などに好適に使用されるセラミックスフ
イルターに関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a ceramics filter suitably used for removing particles in a gas in a semiconductor manufacturing apparatus, for example, etching, diffusion and the like.
【０００２】[0002]
【従来の技術】セラミックスフイルターの製造方法とし
ては、１０〜２０μｍの気孔径をもつ多孔質支持体の表
面に、支持体気孔径よりも小さい粒子のアルミナ原料で
薄膜を形成し、その後これを焼成する方法が従来から知
られている。しかしながら、スリップキャスティング法
などで多孔質支持体表面にセラミックス粒子をコーティ
ングする場合に、多孔質支持体に形成されている気孔径
が、この表面に付着するセラミックス粒子径よりも大き
いと、その粒子が多孔質支持体の気孔中に容易に侵入し
てしまい、多孔質支持体表面に薄膜を形成することが困
難であった。2. Description of the Related Art As a method of manufacturing a ceramics filter, a thin film is formed on the surface of a porous support having a pore diameter of 10 to 20 μm using an alumina raw material having particles smaller than the pore diameter of the support, and then fired. Conventionally, there is a known method. However, when the surface of the porous support is coated with ceramic particles by a slip casting method or the like, if the pore diameter formed on the porous support is larger than the diameter of the ceramic particles adhering to the surface, the particles may be damaged. It easily penetrated into the pores of the porous support, and it was difficult to form a thin film on the surface of the porous support.
【０００３】そこで、薄膜を構成する粒子が、多孔質支
持体に形成された気孔の中に侵入するのを防ぐために、
多孔質支持体の気孔中に予め可燃性物質を含浸させるか
又は多孔質支持体にこれを塗布した後薄膜を形成し、そ
の後この多孔質支持体を焼成することが提案されている
（特開平１−２７４８１５号）。[0003] In order to prevent the particles constituting the thin film from entering the pores formed in the porous support,
It has been proposed to impregnate the pores of the porous support with a flammable substance in advance, or to coat the porous support with a flammable substance, form a thin film, and then calcine the porous support (Japanese Patent Laid-Open No. Hei 10 (1999)). 1-274815).
【０００４】しかしながら、この方法では多孔質支持体
表面に形成する薄膜の粒子が微細なために、乾燥、焼結
などの収縮時に薄膜にクラックなどが発生する欠陥が生
じやすかった。また、多孔質支持体に充填した可燃物質
が焼失した際に生じた空隙にも薄膜を構成していた微細
な粒子が移動しやすく、これによっても薄膜にクラック
を生じて膜欠陥の発生を助長していた。However, in this method, since the particles of the thin film formed on the surface of the porous support are fine, defects such as cracks are liable to be generated in the thin film during shrinkage such as drying and sintering. In addition, the fine particles that constitute the thin film easily move into the voids created when the combustible material filled in the porous support is burned out, which also causes cracks in the thin film and promotes the occurrence of film defects. Was.
【０００５】[0005]
【発明が解決しようとする課題】この発明は、セラミッ
クス一次粒子を後に行われる焼成処理の温度よりも低い
温度で予め仮焼して、これを粉砕、分級したセラミック
ス二次粒子を用いることによって、多孔質支持体表面に
膜を形成する際に膜を構成するセラミックス粒子が多孔
質支持体中に侵入せずまたクラックなどの発生も少く
し、これによって優れたフイルター性能を発揮するセラ
ミックスフイルターを得ようとするものである。SUMMARY OF THE INVENTION The present invention provides a ceramic primary particle which is preliminarily calcined at a temperature lower than the temperature of a firing treatment to be performed later, and is crushed and classified. When forming a film on the surface of the porous support, the ceramic particles constituting the film do not enter the porous support and the occurrence of cracks is reduced, thereby obtaining a ceramics filter exhibiting excellent filter performance. It is to try.
【０００６】[0006]
【課題を解決するための手段】この発明は、多孔質支持
体の表面に薄膜層を形成したセラミックスフイルターの
製造方法であって、セラミックス多孔質支持体の表面
に、セラミックス一次粒子を後工程の焼成処理の温度よ
りも低い温度で予め仮焼しこれを粉砕、分級したセラミ
ックス二次粒子を含有するスラリーを付着して薄膜を形
成し、その後これを前記セラミックスの焼結温度で焼成
することを特徴とするセラミックスフイルターの製造方
法（請求項１）、スラリーに含有されるセラミックス一
次粒子の平均粒径が０．５〜２μｍであることを特徴と
する請求項１記載のセラミックスフイルターの製造方法
（請求項２）、セラミックス多孔質支持体の気孔径が５
〜２０μｍであり、かつ上記粉砕、分級したセラミック
ス二次粒子の粒径が５〜３０μｍであることを特徴とす
る請求項１記載のセラミックスフイルターの製造方法
（請求項３）、セラミックスがアルミナであることを特
徴とする請求項１〜３のいずれかに記載のセラミックス
フイルターの製造方法（請求項４）及び仮焼温度が１１
００〜１４００℃で、かつ焼結温度が１４００〜１６０
０℃であることを特徴とする請求項１〜４のいずれかに
記載のセラミックスフイルターの製造方法（請求項５）
である。SUMMARY OF THE INVENTION The present invention relates to a method for producing a ceramics filter in which a thin film layer is formed on the surface of a porous support. Preliminarily calcined at a temperature lower than the temperature of the baking treatment, pulverized, pulverized, attached a slurry containing the classified ceramic secondary particles to form a thin film, and then bake it at the sintering temperature of the ceramics. The method for producing a ceramic filter according to claim 1, wherein the average particle size of the ceramic primary particles contained in the slurry is 0.5 to 2 µm. Claim 2), wherein the pore size of the ceramic porous support is 5
2. The method for producing a ceramic filter according to claim 1, wherein the ceramic secondary particles have a particle size of 5 to 30 μm, and the ceramic is alumina. The method for producing a ceramics filter according to any one of claims 1 to 3, wherein the calcination temperature is 11%.
00 to 1400 ° C and a sintering temperature of 1400 to 160
The method for producing a ceramics filter according to any one of claims 1 to 4, wherein the temperature is 0 ° C (Claim 5).
It is.
【０００７】[0007]
【発明の実施の形態】この発明のセラミックスフイルタ
ーの製造方法は、従来のセラミックスフイルターの製造
方法と同じように、多孔質支持体の表面に微細な多孔質
薄膜を形成するものである。BEST MODE FOR CARRYING OUT THE INVENTION The method for producing a ceramics filter according to the present invention forms a fine porous thin film on the surface of a porous support in the same manner as the conventional method for producing a ceramics filter.
【０００８】ここに用いる多孔質支持体は、従来のもの
をそのまま使用することが出来る。例えば粒度分布が１
０〜３０μｍのアルミナ、シリカ、ムライト、炭化ケイ
素、窒化ケイ素などの粉末に、結合材としてメチルセル
ロース系バインダーを５〜１０重量％混合し、これを押
し出し成形などで所定の厚さ及び長さの円筒体或いは板
状体としたものが用いられる。次に、これを１７００〜
１８５０℃で焼成して気孔径が５〜２０μｍの多孔質支
持体とする。支持体の気孔径が５μｍ未満ではフイルタ
ー全体のガス流量特性が悪くなってしまう。また、気孔
径が２０μｍを超えると気孔が大き過ぎて気孔の中にも
薄膜を構成するスラリーが充填されて薄膜の形成が困難
となる。As the porous support used here, a conventional one can be used as it is. For example, if the particle size distribution is 1
A 5 to 10% by weight of a methylcellulose binder as a binder is mixed with a powder of alumina, silica, mullite, silicon carbide, silicon nitride, etc. of 0 to 30 μm, and the mixture is extruded and molded into a cylinder having a predetermined thickness and length. A body or a plate-like body is used. Next, this is 1700
It is fired at 1850 ° C. to obtain a porous support having a pore size of 5 to 20 μm. If the pore diameter of the support is less than 5 μm, the gas flow characteristics of the entire filter deteriorate. On the other hand, if the pore diameter exceeds 20 μm, the pores are too large and the pores are filled with the slurry constituting the thin film, making it difficult to form a thin film.
【０００９】この発明では、こうした多孔質支持体の表
面に薄膜を形成するが、この薄膜はセラミックス微粉末
を仮焼しこれを粉砕、分級したもののスラリーを支持体
表面に付着させる。In the present invention, a thin film is formed on the surface of such a porous support. This thin film is obtained by calcining ceramic fine powder, pulverizing and classifying the powder, and then attaching a slurry to the surface of the support.
【００１０】薄膜に用いられる出発原料のセラミックス
一次粒子の平均粒径は好ましくは０．５〜２μｍであ
る。この平均粒子径が０．５μｍ未満では粒子が細か過
ぎて薄膜が緻密になり過ぎ、良好なガス流量特性が得ら
れない。また、平均粒子径が２μｍを超えると粒子が大
き過ぎて目的とするパーティクル除去が十分に達成され
ない恐れがある。こうしたセラミックス一次粒子の粉末
は、その後の最終工程で行われる焼成温度よりも低い温
度で仮焼し、粉砕してから所定の粒度分布に分級して用
いる。セラミックス一次粒子粉末の仮焼温度をその後の
工程で行われる焼成温度よりも低い温度で行わないと、
支持体表面に形成される薄膜に気孔を形成するような多
孔質仮焼体、換言すると多孔質二次粒子を造ることがで
きない。なお、仮焼温度と焼成温度の関係は、仮焼温度
が焼成温度より５０〜１００℃程度低ければよい。この
仮焼体は、その後これを粉砕、分級して多孔質支持体の
表面に薄膜を形成するのに適する粒度とする。The average particle size of the ceramic primary particles as a starting material used for the thin film is preferably 0.5 to 2 μm. If the average particle diameter is less than 0.5 μm, the particles are too fine and the thin film becomes too dense, so that good gas flow characteristics cannot be obtained. On the other hand, if the average particle diameter exceeds 2 μm, the particles may be too large and the intended removal of particles may not be sufficiently achieved. The powder of the ceramic primary particles is calcined at a temperature lower than the firing temperature performed in the subsequent final step, pulverized, and then classified into a predetermined particle size distribution for use. If the calcination temperature of the ceramic primary particle powder is not performed at a temperature lower than the firing temperature performed in the subsequent process,
A porous calcined body that forms pores in a thin film formed on the surface of the support, in other words, porous secondary particles cannot be produced. The relationship between the calcination temperature and the calcination temperature may be such that the calcination temperature is about 50 to 100 ° C. lower than the calcination temperature. The calcined body is then pulverized and classified to a particle size suitable for forming a thin film on the surface of the porous support.
【００１１】粉砕はポットミルなどで行い、分級は水簸
などの常法によって行われる。粉砕、分級したセラミッ
クス粉末の粒径は５〜３０μｍが好ましい。この粒径が
５μｍ未満では、この粒子が多孔質支持体の気孔に侵入
してフイルターとしてのガス流量特性が低下する。また
これが３０μｍを超えると気孔が大きくなり膜厚が厚く
なる恐れがある。薄膜が厚くなるとパーティクルの補足
特性は向上するがガスの流量特性は低下する。一方、粒
子径が小さくて膜厚が薄くなると薄膜の耐圧特性が低下
して亀裂などの欠陥を生じるおそれがある。粉砕、分級
したセラミックス粉末の粒径を５〜３０μｍとすること
によって膜厚の厚さを所定の厚さとしてパーティクルの
補足特性を確保しつつ薄膜の耐圧特性を維持することが
可能である。The pulverization is performed by a pot mill or the like, and the classification is performed by a conventional method such as elutriation. The particle size of the pulverized and classified ceramic powder is preferably 5 to 30 μm. If the particle size is less than 5 μm, the particles enter the pores of the porous support and the gas flow characteristics as a filter deteriorate. If it exceeds 30 μm, the pores may become large and the film thickness may be increased. As the thin film becomes thicker, the supplemental characteristics of the particles improve, but the flow characteristics of the gas decrease. On the other hand, if the particle diameter is small and the film thickness is small, the pressure resistance of the thin film may be reduced, and defects such as cracks may be generated. By setting the particle size of the pulverized and classified ceramic powder to 5 to 30 μm, it is possible to maintain the pressure resistance of the thin film while securing the supplemental characteristics of the particles by setting the thickness to a predetermined thickness.
【００１２】粉砕、分級したセラミックス粉末には増粘
剤、分散剤を添加し撹拌、混合する。撹拌、混合は例え
ばスターラーで２０〜４０時間行い、その後減圧、脱泡
してスラリーの調整を終了する。次に、これを多孔質支
持体の表面に塗布するが、その前に多孔質支持体に予め
水を含浸させる。これによって多孔質支持体中に存在す
る気泡で膜欠陥が生じることを防ぐことが出来る。ま
た、支持体気孔径より小さい仮焼粉粒子がスラリー中に
存在する場合は、それらが支持体中に急激に侵入するの
を抑えることが出来る。A thickener and a dispersant are added to the pulverized and classified ceramic powder, followed by stirring and mixing. Stirring and mixing are performed, for example, with a stirrer for 20 to 40 hours, and then pressure reduction and defoaming are performed to complete the preparation of the slurry. Next, this is applied to the surface of the porous support, but before that, the porous support is previously impregnated with water. As a result, it is possible to prevent the occurrence of a membrane defect due to bubbles existing in the porous support. Further, when calcined powder particles smaller than the pore diameter of the support are present in the slurry, it is possible to suppress the rapid intrusion of the particles into the support.
【００１３】多孔質支持体の表面に上記のスラリーを付
着して多孔質支持体の表面に薄膜を形成する方法は、例
えば図１に示す通りにして行うが、この外にも塗布して
もよくまたこれらに限定されるものではない。図１の
（Ａ）において１は多孔質の支持体で、図示した事例の
ものは筒体である。この支持体１はスラリー溜め２とチ
ューブ３で連結されている。スラリー溜め２とチューブ
３の連結部には二方向コック４が設けられている。チュ
ーブ３の端部と支持体１の結合部には栓５を用いて連結
されて気密が保たれている。また、支持体１の他端は目
盛管６と栓７を用いて連結されている。多孔質支持体１
を上記のようにセットして、スラリー溜め２に上記のよ
うに調整したスラリー８を入れて二方向コック４を開き
（Ｂ）、スラリー８をチューブ３を通って多孔質支持体
１の中へ、さらにその先端に目盛管６へと通過させる。
この状態にしてスラリー溜め２を上下してスラリーが目
盛管６の所定の位置に達したところでスラリー溜め２の
下方の二方向コック４を閉じる（Ｃ）。この状態に保持
しておくとスラリーは多孔質支持体１の内面に加圧され
て水分が多孔質支持体１の外面に滲出する一方で、スラ
リーの粒子が多孔質支持体１の内側に付着してここに薄
膜が形成される。その後、多孔質支持体１の上下の栓を
外して多孔質支持体１を静かに取り外し、この多孔質支
持体を７０〜８０℃で１〜３時間乾燥して仮焼しさらに
焼結する。ここに用いる多孔質支持体及びセラミックス
粉末は、アルミナ、シリカ、ジルコニア粉などが用いら
れるが、フッ素ガスなどに対する耐蝕性などからアルミ
ナが好適である。A method of forming the thin film on the surface of the porous support by attaching the slurry to the surface of the porous support is performed, for example, as shown in FIG. It is not limited to these well. In FIG. 1A, reference numeral 1 denotes a porous support, and the illustrated case is a cylindrical body. The support 1 is connected to a slurry reservoir 2 and a tube 3. A two-way cock 4 is provided at the connection between the slurry reservoir 2 and the tube 3. The end of the tube 3 and the connecting portion of the support 1 are connected with a plug 5 to maintain airtightness. The other end of the support 1 is connected to the scale tube 6 using a plug 7. Porous support 1
Is set as described above, the slurry 8 adjusted as described above is put into the slurry reservoir 2, the two-way cock 4 is opened (B), and the slurry 8 is passed through the tube 3 into the porous support 1. Then, the tip is passed through the scale tube 6.
In this state, the slurry reservoir 2 is moved up and down, and when the slurry reaches a predetermined position of the scale tube 6, the two-way cock 4 below the slurry reservoir 2 is closed (C). In this state, the slurry is pressurized on the inner surface of the porous support 1 and water oozes to the outer surface of the porous support 1, while the slurry particles adhere to the inside of the porous support 1. Then, a thin film is formed here. Thereafter, the upper and lower plugs of the porous support 1 are removed, and the porous support 1 is gently removed. The porous support 1 is dried at 70 to 80 ° C. for 1 to 3 hours, calcined, and sintered. As the porous support and the ceramic powder used here, alumina, silica, zirconia powder and the like are used, but alumina is preferable because of corrosion resistance to fluorine gas and the like.
【００１４】このときの仮焼温度は１１００〜１４００
℃が好ましい。１１００℃未満では仮焼不十分であり、
次工程の焼成時に薄膜部分の熱収縮が大きく剥離等が生
じ、多孔質支持体表面に多孔質薄膜が形成されず、また
１４００℃を超えると仮焼体が緻密になり過ぎ、所望の
気孔が形成されない。この仮焼体は、その後これを粉
砕、分級して、多孔質支持体の表面に薄膜を形成するの
に適する粒径とする。また、焼結温度は１４００〜１６
００℃とする。焼結温度が１４００℃未満では十分な焼
結が行われず支持体と膜との接合強度が十分でない。ま
た焼結温度が１４００℃を超えると小径の粒子が焼結し
て他の粒子と結合し、その結果、膜の気孔径が大きくな
って好ましくない。The calcination temperature at this time is 1100 to 1400
C is preferred. If the temperature is lower than 1100 ° C, the calcination is insufficient.
During the firing in the next step, the heat shrinkage of the thin film portion is large and peeling occurs, and a porous thin film is not formed on the surface of the porous support. If the temperature exceeds 1400 ° C., the calcined body becomes too dense and desired pores are formed Not formed. The calcined body is then pulverized and classified to have a particle size suitable for forming a thin film on the surface of the porous support. The sintering temperature is 1400-16
Set to 00 ° C. If the sintering temperature is lower than 1400 ° C., sufficient sintering is not performed, and the bonding strength between the support and the film is not sufficient. On the other hand, if the sintering temperature exceeds 1400 ° C., small-diameter particles are sintered and combined with other particles, and as a result, the pore size of the film becomes undesirably large.
【００１５】なお、上記では多孔質支持体及びセラミッ
クス粉末をアルミナとした場合の仮焼温度及び焼結温度
の好ましい範囲について説明したが、同等の理由により
各々をシリカとした場合には仮焼温度は１２００〜１３
００℃、焼結温度は１３００〜１４００℃が好ましく、
また各々がジルコニアの場合にはそれぞれ９００〜１２
００℃、１２００〜１３５０℃とすることが好ましい。
こうして得られたセラミックスフイルターは、これを図
示しない金属ケースなどにセットして最終的な製品とす
る。The preferred ranges of the calcination temperature and the sintering temperature when the porous support and the ceramic powder are made of alumina have been described above. Is 1200 to 13
00 ° C, the sintering temperature is preferably 1300 to 1400 ° C,
When each is zirconia, 900 to 12
The temperature is preferably set to 00 ° C and 1200 to 1350 ° C.
The ceramic filter thus obtained is set in a metal case (not shown) or the like to obtain a final product.
【００１６】[0016]
【実施例】粒径１０〜３０μｍのアルミナ粉末に結合材
としてメチルセルロース系バインダーを１０重量％混合
した原料を押出機で押出し、内径１５mm、外径１９mm、
長さ４００mmの円筒体を成形した。その後これを１８５
０℃で焼成して気孔径が２０μｍの多孔質支持体とし
た。EXAMPLE An extruder was used to extrude a raw material obtained by mixing 10% by weight of a methylcellulose-based binder as a binder with alumina powder having a particle size of 10 to 30 μm.
A cylinder having a length of 400 mm was formed. Then 185
By firing at 0 ° C., a porous support having a pore size of 20 μm was obtained.
【００１７】別に、平均粒径が１．５μｍのアルミナ原
料を１３００℃で仮焼した。これをポットミルで粉砕し
水簸分級して粒径２０μｍ以下の粉末とした。このアル
ミナ粉を用いてアルミナ濃度１５重量％のスラリーを得
た。これにさらに増粘剤（ポリエチレングリコール、分
子量20,000、和光純薬工業社製品）を外率で４重量％、
分散剤（ポリアクリル酸アンモニウム塩、アロン−３０
ＳＬ，東亜合成化学社の商品名）を外率で０．０１％加
えてスターラーで２０時間撹拌し、さらにこれを減圧脱
泡した。Separately, an alumina raw material having an average particle size of 1.5 μm was calcined at 1300 ° C. This was pulverized with a pot mill and subjected to elutriation classification to obtain a powder having a particle size of 20 μm or less. Using this alumina powder, a slurry having an alumina concentration of 15% by weight was obtained. In addition, a thickener (polyethylene glycol, molecular weight 20,000, manufactured by Wako Pure Chemical Industries, Ltd.) has an external ratio of 4% by weight,
Dispersant (ammonium polyacrylate, Aron-30
SL, trade name of Toa Gosei Chemical Co., Ltd.) was added at an external rate of 0.01%, and the mixture was stirred with a stirrer for 20 hours, followed by defoaming under reduced pressure.
【００１８】これを図１に示したと同じ方法で前記の多
孔質支持体表面に付着して支持体表面に膜を形成した。
次いで、これを８０℃で２時間乾燥し１５００℃で焼成
しセラミックスフイルターを得た。This was adhered to the porous support surface in the same manner as shown in FIG. 1 to form a film on the support surface.
Next, this was dried at 80 ° C. for 2 hours and fired at 1500 ° C. to obtain a ceramics filter.
【００１９】このフイルターについて元圧５ kgf／ｍ2
でガス流量特性を測定したところ２２〜２６Ｎｌ／min
であった。さらに、バブルポイントを測定したところ、
４０００mmＨ2 Ｏ（エタノール中）であった。その結
果、従来のフイルターとガス流量特性において同等であ
ることが認められた。The original pressure of this filter is 5 kgf / m 2.
22 to 26 Nl / min
Met. Furthermore, when we measured the bubble point,
4000mmH was 2 O (ethanol). As a result, it was recognized that the gas flow characteristics were equivalent to those of the conventional filter.
【００２０】さらに、このフイルターの膜厚をＳＥＭで
測定したところ４０〜５０μｍであった。通常のフイル
ターの膜厚は２０〜３０μｍであるので本発明のフイル
ターでは膜厚が大幅に厚いことが認められた。Further, when the film thickness of this filter was measured by SEM, it was 40 to 50 μm. Since the film thickness of a normal filter is 20 to 30 μm, it was recognized that the film thickness of the filter of the present invention was significantly large.
【００２１】こうしたことは、本願発明のフイルターは
膜厚が従来のフイルターよりも膜厚が大幅に厚いにも拘
らず、ガス流量特性の点においても優れていることを示
すもので、このことは本願発明のフイルターはそれだけ
パーティクルの補足能力が高いことを示す。（発明の効
果）以上のように、この発明によれば多孔質支持体表面
の薄膜を構成するセラミックスに、予めその後に行われ
る焼成処理の温度よりも低い温度で仮焼したセラミック
スを粉砕，分級したセラミックス粉末を用いるので、こ
のセラミックス粉が多孔質支持体の気孔の中に入ること
が防げるとともに、被膜が収縮してクラックが発生する
といったことも生じなくなり、膜欠陥発生の恐れのない
良好なセラミックスフイルターを得ることが出来るよう
になった。This indicates that the filter of the present invention is excellent in gas flow characteristics in spite of the fact that the film thickness is much larger than that of a conventional filter. This shows that the filter of the present invention has a high ability to capture particles. (Effect of the Invention) As described above, according to the present invention, the ceramics constituting the thin film on the surface of the porous support are ground and classified by calcining the ceramics previously calcined at a temperature lower than the temperature of the subsequent firing treatment. Since the ceramic powder is used, it is possible to prevent the ceramic powder from entering the pores of the porous support, to prevent the film from shrinking and to generate cracks, and to prevent the occurrence of film defects. Ceramic filters can now be obtained.
【図１】この発明で用いる多孔質支持体に薄膜を形成す
る方法の一例を示した説明図。FIG. 1 is an explanatory view showing an example of a method for forming a thin film on a porous support used in the present invention.
１……多孔質支持体、２……スラリー溜め、３……チュ
ーブ、４……二方向向コック、６……目盛管、８……ス
ラリー。1 ... porous support, 2 ... slurry reservoir, 3 ... tube, 4 ... two-way cock, 6 ... scale tube, 8 ... slurry.
Claims (5)
セラミックスフイルターの製造方法であって、セラミッ
クス多孔質支持体の表面に、セラミックス一次粒子を後
工程の焼成処理の温度よりも低い温度で予め仮焼しこれ
を粉砕、分級したセラミックス二次粒子を含有するスラ
リーを付着して薄膜を形成し、その後これを前記セラミ
ックスの焼結温度で焼成することを特徴とするセラミッ
クスフイルターの製造方法。1. A method for producing a ceramics filter comprising a thin film layer formed on a surface of a porous support, wherein the ceramic primary particles are coated on the surface of the ceramic porous support at a temperature lower than the temperature of a subsequent firing treatment. A method for producing a ceramics filter, comprising: applying a slurry containing secondary particles of ceramics, which has been calcined in advance and pulverized and classified, to form a thin film, and thereafter firing the same at the sintering temperature of the ceramics. .
粒子の平均粒径が０．５〜２μｍであることを特徴とす
る請求項１記載のセラミックスフイルターの製造方法。2. The method according to claim 1, wherein the ceramic primary particles contained in the slurry have an average particle size of 0.5 to 2 μm.
〜２０μｍであり、かつ上記粉砕、分級したセラミック
ス二次粒子の粒径が５〜３０μｍであることを特徴とす
る請求項１記載のセラミックスフイルターの製造方法。3. The ceramic porous support having a pore size of 5
2. The method for producing a ceramics filter according to claim 1, wherein the particle size of the pulverized and classified ceramic secondary particles is 5 to 30 [mu] m.
徴とする請求項１〜３のいずれかに記載のセラミックス
フイルターの製造方法。4. The method for producing a ceramics filter according to claim 1, wherein the ceramics is alumina.
つ焼結温度が１４００〜１６００℃であることを特徴と
する請求項１〜４のいずれかに記載のセラミックスフイ
ルターの製造方法。5. The method for producing a ceramic filter according to claim 1, wherein the calcination temperature is 1100 to 1400 ° C. and the sintering temperature is 1400 to 1600 ° C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19703197A JPH1133322A (en) | 1997-07-23 | 1997-07-23 | Manufacture of ceramic filter |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19703197A JPH1133322A (en) | 1997-07-23 | 1997-07-23 | Manufacture of ceramic filter |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH1133322A true JPH1133322A (en) | 1999-02-09 |
Family
ID=16367597
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19703197A Pending JPH1133322A (en) | 1997-07-23 | 1997-07-23 | Manufacture of ceramic filter |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH1133322A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009001970A1 (en) * | 2007-06-27 | 2008-12-31 | Ngk Insulators, Ltd. | Separation membrane complex, and method for production of separation membrane complex |
-
1997
- 1997-07-23 JP JP19703197A patent/JPH1133322A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009001970A1 (en) * | 2007-06-27 | 2008-12-31 | Ngk Insulators, Ltd. | Separation membrane complex, and method for production of separation membrane complex |
| US7971729B2 (en) | 2007-06-27 | 2011-07-05 | Ngk Insulators, Ltd. | Separation membrane complex, and method for manufacturing the separation membrane complex |
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