JP2014094318A - Method of producing ceramic honeycomb filter and ceramic honeycomb filter - Google Patents

Method of producing ceramic honeycomb filter and ceramic honeycomb filter Download PDF

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JP2014094318A
JP2014094318A JP2011041034A JP2011041034A JP2014094318A JP 2014094318 A JP2014094318 A JP 2014094318A JP 2011041034 A JP2011041034 A JP 2011041034A JP 2011041034 A JP2011041034 A JP 2011041034A JP 2014094318 A JP2014094318 A JP 2014094318A
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cell
honeycomb filter
ceramic honeycomb
cells
side end
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Tomohisa Ogata
智寿 小方
Toshitaka Ishizawa
俊崇 石澤
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Proterial Ltd
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Hitachi Metals Ltd
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Priority to PCT/JP2012/054428 priority patent/WO2012117942A1/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B11/00—Apparatus or processes for treating or working the shaped or preshaped articles
    • B28B11/003—Apparatus or processes for treating or working the shaped or preshaped articles the shaping of preshaped articles, e.g. by bending
    • B28B11/006—Making hollow articles or partly closed articles
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
    • G01M3/00—Investigating fluid-tightness of structures
    • G01M3/02—Investigating fluid-tightness of structures by using fluid or vacuum
    • G01M3/04—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point
    • G01M3/20—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point using special tracer materials, e.g. dye, fluorescent material, radioactive material
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
    • F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
    • F01N2450/00—Methods or apparatus for fitting, inserting or repairing different elements
    • F01N2450/28—Methods or apparatus for fitting, inserting or repairing different elements by using adhesive material, e.g. cement
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
    • F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
    • F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
    • F01N3/02—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust
    • F01N3/021—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters
    • F01N3/022—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters characterised by specially adapted filtering structure, e.g. honeycomb, mesh or fibrous
    • F01N3/0222—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters characterised by specially adapted filtering structure, e.g. honeycomb, mesh or fibrous the structure being monolithic, e.g. honeycombs

Abstract

PROBLEM TO BE SOLVED: To provide a ceramic honeycomb filter, its production method and method of inspecting a ceramic honeycomb filter which allow inspecting defects of division walls of a ceramic honeycomb filter, do not discard rejected products and secure stable supporting of a catalyst, without increase of the number of steps.SOLUTION: A method of producing a ceramic honeycomb filter comprises opening-sealing, in a checker form, outflow side end parts for the fluid with an opening-sealing material among cells divided and formed with division walls and allowing a fluid to pass through and opening-sealing inflow side end parts for the fluid in remaining cells. The opening-sealing material contains an unbaked ceramic material. In the method of producing a ceramic honeycomb filter, a gas containing fine particles is caused to pass through cells from the inflow side of the ceramic honeycomb filter; presence and absence of cells allowing a predetermined or more amount of the fine particles to flow out from the outflow side and having defects of division walls is inspected; and the opening-sealing material is then baked.

Description

本発明は、セラミックハニカムフィルタの製造方法、および、セラミックハニカムフィルタに関するものである。   The present invention relates to a method for manufacturing a ceramic honeycomb filter and a ceramic honeycomb filter.

図1に示すように、ディーゼルエンジンの排気ガス中の粒子状物質（Particulate Matters、以下「ＰＭ」という）を捕集するセラミックハニカムフィルタ10は、多孔質の隔壁1で区画形成される流体を流通するセル2a、2bを備え、セルの端面が交互に目封止され、流体の流入側端部aが開口されかつ流体の流出側端部bが目封止材3bで目封止されたセル2aと、流体の流入側端部aが目封止材3aで目封止されかつ流体の流出側端部bが開口されたセル2bとが交互に配設されてなる構造を有している。セラミックハニカムフィルタの流入側端部aが開口されたセル2aに流入した排気ガスは、多孔質の隔壁1を通過する際に、排気ガス中のＰＭが捕集される。この時、隔壁にキレやワレ等の欠陥4が生じていると、排気ガス中のＰＭは隔壁に捕集されずに、隣接するセルの流出側端部より流出してしまうため、捕集率低下の原因となる。そのため、隔壁にキレやワレが生じていないか検査する必要がある。   As shown in FIG. 1, a ceramic honeycomb filter 10 that collects particulate matter (Particulate Matters, hereinafter referred to as “PM”) in the exhaust gas of a diesel engine circulates fluid formed by a porous partition wall 1. Cell 2a, 2b to be closed, the end faces of the cells are alternately plugged, the fluid inflow end a is open, and the fluid outflow end b is plugged with a plugging material 3b. 2a and cells 2b in which the fluid inflow side end a is plugged with the plugging material 3a and the fluid outflow side end b is opened are alternately arranged. . When the exhaust gas flowing into the cell 2a in which the inflow side end a of the ceramic honeycomb filter is opened passes through the porous partition wall 1, PM in the exhaust gas is collected. At this time, if defects 4 such as cracks and cracks occur in the partition walls, PM in the exhaust gas flows out from the outflow side end of the adjacent cells without being collected in the partition walls. Causes a drop. Therefore, it is necessary to inspect whether the partition wall is cracked or cracked.

特許文献１には、セラミックハニカムフィルタの一方の端面から軸線方向に粒子を流し、他方の端面に密着させた通気性のあるスクリーンに捕集された粒子の像により隔壁内部および目封止の欠陥を検査する方法が記載されている。   In Patent Document 1, defects inside the partition walls and plugging defects are caused by an image of particles collected on an air-permeable screen in which particles flow in the axial direction from one end face of the ceramic honeycomb filter and are in close contact with the other end face. A method for inspecting is described.

特許文献２には、欠陥を検出するための粒子を所定の粒径範囲をもった定量化用粒子としてセル内に導入し、貫通欠陥を通過して反対側の端面から排出される定量化用粒子の個数及び粒径を、当該粒子を排出している欠陥の有るセル毎に計測し、計測された定量化用粒子の個数及び粒径から欠陥の大きさを定量化するセラミックハニカムフィルタの欠陥検査方法の記載がある。   Patent Document 2 discloses that a particle for detecting a defect is introduced into a cell as a quantifying particle having a predetermined particle size range, passes through a penetration defect, and is discharged from the opposite end surface. Defects in ceramic honeycomb filters that measure the number of particles and the particle size for each defective cell that discharges the particles, and quantify the size of the defect from the measured number and particle size of quantification particles There is a description of the inspection method.

特許文献３には、微粒子を発生させ、その微粒子をセラミックハニカムフィルタの一方の側から当該セラミックハニカムフィルタ内へ導入するとともに、指向性の強い光を発生させ、その光をセラミックハニカムフィルタの他の側を通過させ、更に、前記セラミックハニカムフィルタの他の側で空気の振動を発生させ、その空気の振動によって前記セラミックハニカムフィルタの他の側から排出される微粒子を移動させながら、その微粒子に光を照射して微粒子を可視化するセラミックハニカムフィルタの検査方法が記載されている。   In Patent Document 3, fine particles are generated, the fine particles are introduced into the ceramic honeycomb filter from one side of the ceramic honeycomb filter, light having strong directivity is generated, and the light is transmitted to other ceramic honeycomb filters. The air is generated on the other side of the ceramic honeycomb filter, and the particles discharged from the other side of the ceramic honeycomb filter are moved by the vibration of the air. A method for inspecting a ceramic honeycomb filter in which fine particles are visualized by irradiating is described.

特許文献４には、微粒子を含む気体を加圧してハニカム構造体の一方の面側からセル内へ微粒子の導入をする微粒子導入手段と、その導入される気体の流量を調節する微粒子含有気体流量調節手段と、ハニカム構造体における他の面の近傍を平行に通過するように指向性の強い光を照射する光照射手段と、その光照射手段から出射された光と、ハニカム構造体の他の面との間に、そのハニカム構造体の他の面を覆うように配設される整流板と、ハニカム構造体の一方の面側から他の面側へ向けた方向に、ハニカム構造体の外周に沿って気体を流す気流形成手段とを具備するハニカム構造体の欠陥検査装置の記載がある。   Patent Document 4 discloses a fine particle introducing means for introducing fine particles into a cell from one side of a honeycomb structure by pressurizing a gas containing fine particles, and a fine particle-containing gas flow rate for adjusting the flow rate of the introduced gas. Adjusting means, light irradiating means for irradiating light with strong directivity so as to pass in the vicinity of other surfaces of the honeycomb structure in parallel, light emitted from the light irradiating means, A rectifying plate disposed so as to cover the other surface of the honeycomb structure, and the outer periphery of the honeycomb structure in a direction from one surface side to the other surface side of the honeycomb structure. There is a description of a defect inspection apparatus for a honeycomb structure having an airflow forming means for flowing a gas along the line.

特公平０５-６５８号公報Japanese Patent Publication No. 05-658 特開２００９−８５６７３号公報JP 2009-85673 A 特開２００９−１１５６５５号公報JP 2009-115655 A 特開２００９−２５８０９０号公報JP 2009-258090 A

しかしながら、特許文献１、特許文献２、特許文献３、特許文献４に記載の発明では、いずれも、検査後のセラミックハニカムフィルタには、検査に使用した微粒子が残留している。このままでは、排気ガス中のＮＯｘを酸化させる酸化触媒等の触媒を担持させた場合、この微粒子が不純物となり、安定して触媒を担持することができないという問題のため、検査後に微粒子を除去する工程を増やす必要があり、工数増加の問題があった。さらに、検査でセラミックハニカムフィルタの隔壁の欠陥を検出して、所定の判定基準に従って合否の判定をした後は、不合格となった製品は廃却していた。   However, in the inventions described in Patent Document 1, Patent Document 2, Patent Document 3, and Patent Document 4, all of the fine particles used for the inspection remain in the ceramic honeycomb filter after the inspection. In this state, when a catalyst such as an oxidation catalyst that oxidizes NOx in the exhaust gas is supported, the fine particles become impurities, and the catalyst cannot be stably supported. There was a problem of increasing man-hours. Further, after detecting defects in the partition walls of the ceramic honeycomb filter by inspection and determining pass / fail according to a predetermined criterion, rejected products have been discarded.

したがって、本発明の課題は、工数を増加することがなく、さらに、セラミックハニカムフィルタの隔壁の欠陥を検査して、不合格となった製品を廃却せず、安定して触媒を担持することができるセラミックハニカムフィルタとその製造方法を得ることにある。   Therefore, the object of the present invention is to increase the number of man-hours, further to inspect defects in the partition walls of the ceramic honeycomb filter, and to stably carry the catalyst without discarding the rejected product. It is to obtain a ceramic honeycomb filter that can be manufactured and a manufacturing method thereof.

本発明のセラミックハニカムフィルタの製造方法は、隔壁で区画形成される流体を流通するセルのうち、流体の流出側端部を市松状に目封止材により目封止し、残余のセルにおいて流体の流入側端部を目封止材により目封止するセラミックハニカムフィルタの製造方法であって、
前記目封止材は、未焼成のセラミック材料を含み、
前記セラミックハニカムフィルタの流入側から微粒子を含む気体をセルへ流通させ、流出側から所定量以上の微粒子が流出する隔壁に欠陥部を有するセルの有無を検査し、
その後、目封止材を焼成することを特徴とする。 In the method for manufacturing a ceramic honeycomb filter of the present invention, among the cells through which the fluid partitioned by the partition wall flows, the fluid outflow side end is plugged in a checkered pattern with a plugging material, and the remaining cells A method for manufacturing a ceramic honeycomb filter in which an inflow side end portion of a ceramic plug is plugged with a plugging material,
The plugging material includes an unfired ceramic material,
A gas containing fine particles is circulated from the inflow side of the ceramic honeycomb filter to the cell, and the presence or absence of the cell having a defect portion in the partition wall from which a predetermined amount or more of the fine particles flows out from the outflow side is inspected.
Thereafter, the plugging material is fired.

本発明のセラミックハニカムフィルタの製造方法において、前記検査で、流出側から所定量以上の微粒子が流出する隔壁に欠陥部を有するセルを特定し、
(a)前記特定したセルの流出側端部を未焼成のセラミック材料を含む目封止材で目封止し、
もしくは、
(b)前記特定したセルに隣接するセルの流入側端部を未焼成のセラミック材料を含む目封止材で目封止し、
その後、目封止材を焼成することことが好ましい。 In the method for manufacturing a ceramic honeycomb filter of the present invention, in the inspection, a cell having a defective portion is specified in a partition wall from which a predetermined amount or more of the fine particles flows out from the outflow side,
(a) plugging the outflow side end of the identified cell with a plugging material containing an unfired ceramic material;
Or
(b) plugging the inflow side end of the cell adjacent to the identified cell with a plugging material containing an unfired ceramic material;
Thereafter, the plugging material is preferably fired.

本発明のセラミックハニカムフィルタの製造方法において、前記特定したセルの流出側端部を目封止したセルの数、もしくは、前記特定したセルに隣接するセルの流入側端部を目封止したセルの数が、全セル数の1％以下であることが好ましい。   In the method for manufacturing a ceramic honeycomb filter of the present invention, the number of cells plugged at the outflow side end of the specified cell, or the cell plugged at the inflow side end of a cell adjacent to the specified cell Is preferably 1% or less of the total number of cells.

本発明のセラミックハニカムフィルタの製造方法において、前記セルへ流通させる気体が室温以上の温度であることが好ましい。   In the method for manufacturing a ceramic honeycomb filter of the present invention, it is preferable that a gas to be circulated into the cell is a temperature of room temperature or higher.

本発明のセラミックハニカムフィルタは、隔壁で区画形成される流体を流通するセルを備え、流体の流入側端部が開口されかつ流体の流出側端部が目封止されたセルと、流体の流入側端部が目封止されかつ流体の流出側端部が開口されたセルとが交互に配設されてなるセラミックハニカムフィルタにおいて、
前記セラミックハニカムフィルタの流入側から微粒子を含む気体をセルへ流通させ、流出側から所定量以上の微粒子が流出する隔壁に欠陥部を有するセルを特定し、
(a)前記特定したセルの流出側端部を目封止したこと、
もしくは、
(b)前記特定したセルに隣接するセルの流入側端部を目封止したことを特徴とする。 The ceramic honeycomb filter of the present invention includes a cell that circulates a fluid defined by partition walls, a cell in which an end portion on the inflow side of the fluid is opened and an end portion on the outflow side of the fluid is plugged, and the inflow of fluid In the ceramic honeycomb filter in which the side end portions are plugged and the cells having the fluid outflow side end portions opened alternately are arranged,
A gas containing fine particles is circulated from the inflow side of the ceramic honeycomb filter to the cells, and a cell having a defect portion is specified in a partition wall from which a predetermined amount or more of the fine particles flows out from the outflow side,
(a) plugging the outflow side end of the identified cell;
Or
(b) The inflow side end of a cell adjacent to the specified cell is plugged.

本発明のセラミックハニカムフィルタにおいて、前記特定したセルの流出側端部を目封止したセルの数、もしくは、前記特定したセルに隣接するセルの流入側端部を目封止したセルの数が、全セル数の1％以下であることが好ましい。   In the ceramic honeycomb filter of the present invention, the number of cells plugged at the outflow side end of the specified cell, or the number of cells plugged at the inflow side end of a cell adjacent to the specified cell is The total number of cells is preferably 1% or less.

次に、本発明の作用効果について説明する。
本発明のセラミックハニカムフィルタの製造方法は、隔壁で区画形成される流体を流通するセルのうち、流体の流出側端部を市松状に目封止材により目封止し、残余のセルにおいて流体の流入側端部を目封止材により目封止するセラミックハニカムフィルタの製造方法であって、
前記目封止材は、未焼成のセラミック材料を含み、
前記セラミックハニカムフィルタの流入側から微粒子を含む気体をセルへ流通させ、流出側から所定量以上の微粒子が流出する隔壁に欠陥部を有するセルの有無を検査し、
その後、目封止材を焼成することで、次の作用効果を有する。 Next, the function and effect of the present invention will be described.
In the method for manufacturing a ceramic honeycomb filter of the present invention, among the cells through which the fluid partitioned by the partition wall flows, the fluid outflow side end is plugged in a checkered pattern with a plugging material, and the remaining cells A method for manufacturing a ceramic honeycomb filter in which an inflow side end portion of a ceramic plug is plugged with a plugging material,
The plugging material includes an unfired ceramic material,
A gas containing fine particles is circulated from the inflow side of the ceramic honeycomb filter to the cell, and the presence or absence of the cell having a defect portion in the partition wall from which a predetermined amount or more of the fine particles flows out from the outflow side is inspected.
Thereafter, firing the plugging material has the following effects.

すなわち、目封止材が、未焼成のセラミック材料を含み、セラミックハニカムフィルタの流入側から微粒子を含む気体をセルへ流通させ、流出側から所定量以上の微粒子が流出する隔壁に欠陥部を有するセルの有無を検査し、その後、焼成することで、隔壁に残留している、セラミックハニカムフィルタの流入側から流通させた微粒子が、燃焼して隔壁から除去される。そのため、微粒子を除去する工程を増加させる必要がなく、目封止材の焼成と同時に行うことができるので、工数が増加するという問題が無くなるのである。そして、検査で用いた微粒子が除去されるので、触媒担持の際に、安定して触媒を担持することができる。   That is, the plugging material contains an unfired ceramic material, a gas containing fine particles is circulated from the inflow side of the ceramic honeycomb filter to the cell, and the partition wall from which a predetermined amount or more of fine particles flows out from the outflow side has a defect portion. By inspecting for the presence or absence of cells and then firing, the fine particles remaining on the partition walls and circulated from the inflow side of the ceramic honeycomb filter are burned and removed from the partition walls. Therefore, it is not necessary to increase the number of steps for removing the fine particles, and the process can be performed simultaneously with the firing of the plugging material, thereby eliminating the problem of increasing the number of steps. Since the fine particles used in the inspection are removed, the catalyst can be stably supported when the catalyst is supported.

ここで、流出側から所定量以上の微粒子が流出する隔壁に欠陥部を有するセルは、その有無を次のようにして確認する。すなわち、セラミックハニカムフィルタの流入側からセルへ流通させる気体に含まれる微粒子に、直径3nm〜500nmのカーボン粒子を使用する。そして、カーボン粒子はセルに付着しセルが黒く着色されるので、カーボン粒子が流出するセルの流出端部付近の４つの隔壁がカーボン粒子の付着により黒くなる。そして、カーボン粒子を含む気体の流入を止めたあとでも、簡単に目視で微粒子が流出するセルを確認し、特定することができるのである。キレやワレ等の欠陥のない隔壁でも流入初期では、流出側セルからカーボン粒子が漏れる場合もあるが、キレやワレ等の欠陥のあるセルに比べて極微量であり、流入が進むにつれて流出量が減っていくので流出端近傍の隔壁が目視で判別できるほど黒く着色されないためキレやワレ等の欠陥のあるセルが特定できる。尚、微粒子を含む気体に市販のスモークボールを用いて発生させた煙を使用することもできる。スモークボールで発生させた色の付いた煙が、微粒子が流出するセルの流出端から流出するので目視にて特定が可能である。そのセルをマーキングしておくことで、スモークボールを用いて発生させた煙の流入を止めたあとでも、微粒子が流出するセルを特定することができる。   Here, the presence or absence of a cell having a defect in the partition wall where a predetermined amount or more of the fine particles flows out from the outflow side is confirmed as follows. That is, carbon particles having a diameter of 3 nm to 500 nm are used as fine particles contained in the gas flowing from the inflow side of the ceramic honeycomb filter to the cell. Since the carbon particles adhere to the cells and the cells are colored black, the four partition walls in the vicinity of the outflow end of the cells from which the carbon particles flow out become black due to the adhesion of the carbon particles. And even after stopping the inflow of the gas containing carbon particles, the cell from which the fine particles flow out can be easily confirmed and identified visually. Even in bulkheads without defects such as cracks and cracks, carbon particles may leak from the outflow side cells at the beginning of inflow, but the amount is extremely small compared to cells with defects such as cracks and cracks, and the amount of outflow as the inflow progresses. Since the partition wall in the vicinity of the outflow end is not colored so black that it can be visually discerned, cells having defects such as cracks and cracks can be identified. In addition, the smoke generated using a commercially available smoke ball can also be used for the gas containing fine particles. Since the colored smoke generated by the smoke ball flows out from the outflow end of the cell through which the fine particles flow out, it can be identified visually. By marking the cell, it is possible to identify the cell from which the fine particles flow out even after stopping the inflow of smoke generated using the smoke ball.

本発明のセラミックハニカムフィルタの製造方法において、前記検査で、所定量以上の流出側から微粒子が流出する隔壁に欠陥部を有するセルを特定し、
(a)前記特定したセルの流出側端部を未焼成のセラミック材料を含む目封止材で目封止し、
もしくは、
(b)前記特定したセルに隣接するセルの流入側端部を未焼成のセラミック材料を含む目封止材で目封止し、
その後、目封止材を焼成することで次の作用効果を有する。 In the method for manufacturing a ceramic honeycomb filter of the present invention, in the inspection, a cell having a defective portion is specified in a partition wall from which fine particles flow out from an outflow side of a predetermined amount or more,
(a) plugging the outflow side end of the identified cell with a plugging material containing an unfired ceramic material;
Or
(b) plugging the inflow side end of the cell adjacent to the identified cell with a plugging material containing an unfired ceramic material;
Thereafter, firing the plugging material has the following effects.

すなわち、(a)の場合、図１に示すように、目封止材3a、3bは、未焼成のセラミック材料を含み、前記セラミックハニカムフィルタの流入側aから微粒子を含む気体をセルへ流通させ、流出側bから所定量以上の微粒子が流出する隔壁に欠陥部を有するセル22bを特定し、特定したセル22bの流出側端部bを未焼成のセラミック材料を含む目封止材33bで目封止したことで、隔壁にキレやワレ等の欠陥4を有していても、開口された流入側端部から流入した排気ガス中のＰＭが、隔壁のキレやワレ等の欠陥を通過して隣接するセルにＰＭが流出しても、隣接するセルの流出側端部が目封止されていることから、ＰＭはセラミックハニカムフィルタから流出しない。そのため、捕集率は低下することがなく、隔壁にキレやワレ等の欠陥を有していても、不合格として廃却する必要のないセラミックハニカムフィルタを得ることができる。   That is, in the case of (a), as shown in FIG. 1, the plugging materials 3a and 3b contain an unfired ceramic material, and a gas containing fine particles is circulated from the inflow side a of the ceramic honeycomb filter to the cell. Then, the cell 22b having a defect portion in the partition wall where a predetermined amount or more of the fine particles flow out from the outflow side b is identified, and the outflow side end b of the identified cell 22b is plugged with a plugging material 33b containing an unfired ceramic material. By sealing, PM in the exhaust gas flowing in from the opening end on the inflow side passes through defects such as cracks and cracks even if the partition has defects 4 such as cracks and cracks. Even if PM flows out to the adjacent cells, PM does not flow out of the ceramic honeycomb filter because the outflow side end of the adjacent cell is plugged. Therefore, the collection rate does not decrease, and a ceramic honeycomb filter that does not need to be discarded as a reject can be obtained even if the partition has defects such as cracks and cracks.

そして、特定したセル22bの流出側端部bを未焼成のセラミック材料を含む目封止材33bで目封止し、その後、目封止材を焼成することで、流体の流出側端部と流入側端部を目封止された未焼成のセラミック材料を含む目封止材3a、3bと、特定したセル22bの流出側端部を目封止した未焼成のセラミック材料を含む目封止材33bとを、同時に焼成することができるので、別々に焼成する場合と比べて、工数を低減することができる。そして、隔壁に残留している、セラミックハニカムフィルタの流入側から流通させた微粒子が、燃焼して隔壁から除去されるので、微粒子を除去する工程を増加させる必要がなく、目封止材の焼成と同時に行うことができるので、工数が増加するという問題が無くなるのである。そして、検査で用いた微粒子が除去されるので、触媒担持の際に、安定して触媒を担持することができる。   Then, the outflow side end b of the identified cell 22b is plugged with a plugging material 33b containing an unfired ceramic material, and then the plugging material is fired, so that the outflow side end of the fluid and Plugging material 3a, 3b containing unfired ceramic material plugged at the inflow side end and plugging containing unfired ceramic material plugged at the outflow side end of the identified cell 22b Since the material 33b can be fired at the same time, the number of man-hours can be reduced as compared with the case of firing separately. The fine particles remaining in the partition walls and circulated from the inflow side of the ceramic honeycomb filter are burned and removed from the partition walls, so there is no need to increase the number of steps for removing the fine particles, and the plugging material is fired. Since it can be performed at the same time, the problem of increasing man-hours is eliminated. Since the fine particles used in the inspection are removed, the catalyst can be stably supported when the catalyst is supported.

一方、(b)の場合、図２に示すように、目封止材3a、3bは、未焼成のセラミック材料を含み、前記セラミックハニカムフィルタの流入側aから微粒子を含む気体をセルへ流通させ、流出側bから所定量以上の微粒子が流出する隔壁に欠陥部を有するセル22bを特定し、特定したセル22bに隣接するセル22aの流入側端部aを未焼成のセラミック材料を含む目封止材33aで目封止したことで、隔壁にキレやワレ等の欠陥4を有していても、排気ガス中のＰＭは、流入側端部から隔壁にキレやワレ等の欠陥を有しているセルに流入せず、隔壁にキレやワレ等の欠陥のない、流入側端部が開口されたセルに流入して隔壁で捕集される。そのため、捕集率は低下することがなく、隔壁にキレやワレ等の欠陥を有していても、不合格として廃却する必要のないセラミックハニカムフィルタを得ることができる。   On the other hand, in the case of (b), as shown in FIG. 2, the plugging materials 3a and 3b contain an unfired ceramic material, and a gas containing fine particles is circulated from the inflow side a of the ceramic honeycomb filter to the cell. Then, a cell 22b having a defect in the partition wall from which a predetermined amount or more of the fine particles flow out from the outflow side b is specified, and the inflow side end a of the cell 22a adjacent to the specified cell 22b is plugged with an unfired ceramic material. By plugging with the stopper 33a, PM in the exhaust gas has defects such as cracks and cracks from the inflow side end even if the partition has defects 4 such as cracks and cracks. The flow does not flow into the cell, and the partition wall has no defects such as cracks or cracks, and flows into the cell with the inflow side end opened, and is collected by the partition wall. Therefore, the collection rate does not decrease, and a ceramic honeycomb filter that does not need to be discarded as a reject can be obtained even if the partition has defects such as cracks and cracks.

そして、特定したセル22bに隣接するセル22aの流入側端部aを未焼成のセラミック材料を含む目封止材33aで目封止し、その後、目封止材を焼成することで、流体の流出側端部bと流入側端部aを目封止された未焼成のセラミック材料を含む目封止材3a、3bと、特定したセル22bに隣接するセル22aの流入側端部aを目封止した未焼成のセラミック材料を含む目封止材33aとを、同時に焼成することができるので、別々に焼成する場合と比べて、工数を低減することができる。そして、隔壁に残留している、セラミックハニカムフィルタの流入側から流通させた微粒子が、燃焼して隔壁から除去されるので、微粒子を除去する工程を増加させる必要がなく、目封止材の焼成と同時に行うことができるので、工数が増加するという問題が無くなるのである。そして、検査で用いた微粒子が除去されるので、触媒担持の際に、安定して触媒を担持することができる。   Then, the inflow side end a of the cell 22a adjacent to the identified cell 22b is plugged with a plugging material 33a containing an unfired ceramic material, and then the plugging material is fired, Plugging materials 3a and 3b containing an unfired ceramic material with the outflow side end b and the inflow side end a plugged, and the inflow side end a of the cell 22a adjacent to the identified cell 22b Since the plugged material 33a containing the sealed unfired ceramic material can be fired at the same time, the number of man-hours can be reduced as compared with the case of firing separately. The fine particles remaining in the partition walls and circulated from the inflow side of the ceramic honeycomb filter are burned and removed from the partition walls, so there is no need to increase the number of steps for removing the fine particles, and the plugging material is fired. Since it can be performed at the same time, the problem of increasing man-hours is eliminated. Since the fine particles used in the inspection are removed, the catalyst can be stably supported when the catalyst is supported.

ここで、特定したセルに隣接するセルの流入側端部を未焼成のセラミック材料を含む目封止材で目封止する場合、四角形セルの場合、特定したセルに隣接する４つのセルのうち何れかを目封止すれば良いが、欠陥部のある隔壁の位置が確認できないことがあるので、４つのセルを目封止することが好ましい   Here, when the inflow side end of the cell adjacent to the specified cell is plugged with a plugging material containing an unfired ceramic material, among the four cells adjacent to the specified cell in the case of a rectangular cell Any one may be plugged, but it may be impossible to confirm the position of the partition wall having a defective portion, so it is preferable to plug four cells.

また、従来は不合格として廃却していた、隔壁に、開口幅0.1mm以上、長さ0.3mm以上の欠陥部を有するセラミックハニカムフィルタであっても、流出側から所定量以上の微粒子が流出するセル、もしくは、流出側から微粒子が流出するセルに隣接するセルの流入側端部を目封止材で目封止することで、排気ガス中のＰＭはセラミックハニカムフィルタから流出せず、捕集率は低下することがなく、不合格として廃却する必要がないセラミックハニカムフィルタを得ることができるのである。   Even if the ceramic honeycomb filter has a defect part with an opening width of 0.1 mm or more and a length of 0.3 mm or more, which has been discarded as a failure in the past, a predetermined amount or more of fine particles flow out from the outflow side. The PM in the exhaust gas does not flow out of the ceramic honeycomb filter and is trapped by plugging the inflow side end of the cell adjacent to the cell to be discharged or from the outflow side with a plugging material. The collection rate does not decrease, and a ceramic honeycomb filter that does not need to be discarded as a reject can be obtained.

本発明のセラミックハニカムフィルタの製造方法において、前記特定したセルの流出側端部を目封止したセルの数、もしくは、前記特定したセルに隣接するセルの流入側端部を目封止したセルの数が、全セル数の1％以下であることが好ましいのは次の理由による。すなわち、前記特定したセルの流出側端部を目封止したセル22bは、その流入側端部も目封止されている。さらに、前記特定したセルに隣接するセルの流入側端部を目封止したセル22aは、その流出側端部も目封止されている。この場合、セラミックハニカムフィルタとして使用した場合、排気ガスが流通するセルが減少するため、圧力損失が上昇することになるが、全セル数の１％以下であれば、圧力損失の上昇が小さいセラミックハニカムフィルタを得ることができるのである。好ましくは、0.8％以下である。   In the method for manufacturing a ceramic honeycomb filter of the present invention, the number of cells plugged at the outflow side end of the specified cell, or the cell plugged at the inflow side end of a cell adjacent to the specified cell The number of is preferably 1% or less of the total number of cells for the following reason. That is, the inflow side end of the cell 22b in which the outflow side end of the specified cell is plugged is also plugged. Further, in the cell 22a in which the inflow side end of the cell adjacent to the specified cell is plugged, the outflow side end is also plugged. In this case, when used as a ceramic honeycomb filter, the number of cells through which exhaust gas flows decreases, so the pressure loss increases. However, if the number of cells is 1% or less, the increase in pressure loss is small. A honeycomb filter can be obtained. Preferably, it is 0.8% or less.

本発明のセラミックハニカムフィルタの製造方法において、前記セルへ流通させる気体が室温以上の温度であることで、流出側bから微粒子が流出するセル22bを特定する検査を行いながら、目封止材3a、3bの乾燥を行うことができる。そのため、目封止材を形成した後に行う乾燥工程を単独で行うことなく、検査を行いながら乾燥が可能であるので工数を短縮することができる。セルへ流通させる気体の温度は、目封止材の乾燥が行えるよう、50℃以上が好ましく、70℃以上がさらに好ましい。   In the method for manufacturing a ceramic honeycomb filter of the present invention, the plugging material 3a is obtained while performing an inspection for identifying the cells 22b from which the fine particles flow out from the outflow side b because the gas flowing into the cells is at room temperature or higher. 3b can be dried. Therefore, since the drying can be performed while performing the inspection without performing the drying process performed after forming the plugging material, the number of steps can be reduced. The temperature of the gas circulated into the cell is preferably 50 ° C. or higher, and more preferably 70 ° C. or higher so that the plugging material can be dried.

次に、本発明のセラミックハニカムフィルタは、隔壁で区画形成される流体を流通するセルを備え、流体の流入側端部が開口されかつ流体の流出側端部が目封止されたセルと、流体の流入側端部が目封止されかつ流体の流出側端部が開口されたセルとが交互に配設されてなるセラミックハニカムフィルタにおいて、前記セラミックハニカムフィルタの流入側から微粒子を含む気体をセルへ流通させ、流出側から所定量以上の微粒子が流出する隔壁に欠陥部を有するセルを特定し、
(a)前記特定したセルの流出側端部を目封止したこと、
もしくは、
(b)前記特定したセルに隣接するセルの流入側端部を目封止したことで、次の作用効果を有する。 Next, the ceramic honeycomb filter of the present invention includes a cell through which a fluid defined by partition walls is circulated, a cell in which the fluid inflow end is opened and the fluid outflow end is plugged, In a ceramic honeycomb filter in which cells having fluid inflow end portions plugged and fluid outflow end portions opened are alternately arranged, gas containing fine particles is introduced from the inflow side of the ceramic honeycomb filter. Distribute to the cell, identify the cell having a defect in the partition wall where a predetermined amount or more of the fine particles flow out from the outflow side,
(a) plugging the outflow side end of the identified cell;
Or
(b) Since the inflow side end of the cell adjacent to the specified cell is plugged, the following effects are obtained.

すなわち、(a)の場合、図１に示すように、流出側bから所定量以上の微粒子が流出する隔壁に欠陥部を有するセル22bを特定し、特定したセル22bの流出側端部bを目封止材33bで目封止したことで、隔壁にキレやワレ等の欠陥4を有していても、開口された流入側端部から流入した排気ガス中のＰＭが、隔壁のキレやワレ等の欠陥を通過して隣接するセルにＰＭが流出しても、隣接するセルの流出側端部が目封止されていることから、ＰＭはセラミックハニカムフィルタから流出せず、捕集率は低下することがなく、隔壁にキレやワレ等の欠陥を有しているセラミックハニカムフィルタであっても不合格として製品を廃却する必要がなくなる。   That is, in the case of (a), as shown in FIG. 1, the cell 22b having a defective portion is specified in the partition wall from which the predetermined amount or more of the fine particles flows out from the outflow side b, and the outflow side end b of the specified cell 22b is specified. By plugging with the plugging material 33b, even if the partition has defects 4 such as cracks and cracks, the PM in the exhaust gas flowing in from the opened inflow side end portion is damaged by cracks and cracks in the partition. Even if PM flows out to adjacent cells through defects such as cracks, the outflow side end of the adjacent cells is plugged, so PM does not flow out of the ceramic honeycomb filter, and the collection rate Therefore, even if the ceramic honeycomb filter has defects such as cracks and cracks in the partition walls, it is not necessary to dispose of the product as a failure.

一方、(b)の場合、図２に示すように、流出側bから所定量以上の微粒子が流出する隔壁に欠陥部を有するセル22bを特定し、前記特定したセル22bに隣接するセル22aの流入側端部を目封止材33aで目封止したことで、隔壁にキレやワレ等の欠陥4を有していても、排気ガス中のＰＭは、流入側端部から隔壁にキレやワレ等の欠陥を有しているセルに流入せず、隔壁にキレやワレ等の欠陥のない、流入側端部が開口されたセルに流入して隔壁で捕集される。そのため、ＰＭはセラミックハニカムフィルタから流出せず、捕集率は低下することがなく、隔壁にキレやワレ等の欠陥を有しているセラミックハニカムフィルタであっても不合格として製品を廃却する必要がなくなる。   On the other hand, in the case of (b), as shown in FIG. 2, a cell 22b having a defect in the partition wall from which a predetermined amount or more of particles flows out from the outflow side b is identified, and the cell 22a adjacent to the identified cell 22b is identified. By plugging the inflow side end portion with the plugging material 33a, the PM in the exhaust gas is sharpened from the inflow side end portion to the partition wall even if the partition wall has defects 4 such as cracks and cracks. It does not flow into a cell having defects such as cracks, but flows into a cell having no defects such as cracks or cracks in the partition wall, and is collected by the partition walls. Therefore, PM does not flow out from the ceramic honeycomb filter, the collection rate does not decrease, and even if the ceramic honeycomb filter has defects such as cracks and cracks in the partition walls, the product is discarded as rejected. There is no need.

ここで、特定したセルに隣接するセルの流入側端部を未焼成のセラミック材料を含む目封止材で目封止する場合、四角形セルの場合、特定したセルに隣接する４つのセルのうち何れかを目封止すれば良いが、欠陥部のある隔壁の位置が確認できないことがあるので、４つのセルを目封止することが好ましい   Here, when the inflow side end of the cell adjacent to the specified cell is plugged with a plugging material containing an unfired ceramic material, among the four cells adjacent to the specified cell in the case of a rectangular cell Any one may be plugged, but it may be impossible to confirm the position of the partition wall having a defective portion, so it is preferable to plug four cells.

また、従来は不合格として廃却していた、隔壁に、開口幅0.1mm以上、長さ0.3mm以上の欠陥部を有するセラミックハニカムフィルタであっても、流出側から微粒子が流出するセル、もしくは、流出側から微粒子が流出するセルに隣接するセルの流入側端部を目封止材で目封止することで、排気ガス中のＰＭはセラミックハニカムフィルタから流出せず、捕集率は低下することがなく、不合格として廃却する必要がなくなるのである。   Further, even in the case of a ceramic honeycomb filter having a defect portion having an opening width of 0.1 mm or more and a length of 0.3 mm or more in the partition wall, which has been discarded as a failure in the past, cells in which fine particles flow out from the outflow side, or By plugging the inflow side end of the cell adjacent to the cell from which the fine particles flow out from the outflow side with a plugging material, PM in the exhaust gas does not flow out of the ceramic honeycomb filter, and the collection rate decreases. There is no need to dispose of it as a failure.

本発明のセラミックハニカムフィルタにおいて、前記特定したセルの流出側端部を目封止したセルの数、もしくは、前記特定したセルに隣接するセルの流入側端部を目封止したセルの数が、全セル数の1％以下であることが好ましいのは次の理由による。すなわち、前記特定したセルの流出側端部を目封止したセル22bは、その流入側端部も目封止されている。さらに、前記特定したセルに隣接するセルの流入側端部を目封止したセル22aは、その流出側端部も目封止されている。この場合、セラミックハニカムフィルタとして使用した場合、排気ガスが流通するセルが減少するため、圧力損失が上昇することになるが、全セル数の１％以下であれば、圧力損失の上昇が小さく、セラミックハニカムフィルタとして良好に使用することができるのである。好ましくは、0.8％以下である。   In the ceramic honeycomb filter of the present invention, the number of cells plugged at the outflow side end of the specified cell, or the number of cells plugged at the inflow side end of a cell adjacent to the specified cell is The reason why the total number of cells is preferably 1% or less is as follows. That is, the inflow side end of the cell 22b in which the outflow side end of the specified cell is plugged is also plugged. Further, in the cell 22a in which the inflow side end of the cell adjacent to the specified cell is plugged, the outflow side end is also plugged. In this case, when used as a ceramic honeycomb filter, the number of cells through which exhaust gas flows decreases, so that the pressure loss increases. However, if the total number of cells is 1% or less, the increase in pressure loss is small, It can be used favorably as a ceramic honeycomb filter. Preferably, it is 0.8% or less.

本発明によれば、工数を増加することがなく、さらに、セラミックハニカムフィルタの隔壁の欠陥を検査して、不合格となった製品を廃却せず、安定して触媒を担持することができるセラミックハニカムフィルタとその製造方法を得ることができる。   According to the present invention, the number of man-hours is not increased, and further, the defects of the partition walls of the ceramic honeycomb filter are inspected, and the rejected product is not discarded, and the catalyst can be stably supported. A ceramic honeycomb filter and a manufacturing method thereof can be obtained.

本発明に係るセラミックハニカムフィルタを示した図The figure which showed the ceramic honeycomb filter which concerns on this invention 本発明に係るセラミックハニカムフィルタを示した図The figure which showed the ceramic honeycomb filter which concerns on this invention 本発明に係る検査装置を示した図The figure which showed the inspection apparatus which concerns on this invention

以下、本発明の実施の形態を実施例を基に説明する。
（実施例）
カオリン、タルク、シリカ、アルミナなどの粉末を調整し、質量比で、SiO2：48〜52％、Al2O3：33〜37％、MgO：12〜15％を含むコージェライト生成原料粉末とし、これにバインダーとしてメチルセルロース、ヒドロキシプロピルメチルセルロース、潤滑剤、造孔材として発泡済み樹脂を添加し、乾式で十分混合した後、規定量の水を添加、十分な混練を行って可塑化したセラミック杯土を作製した。次に、このセラミック坏土を押出成形用口金を通過させた後、所定長さに切断し、周縁部と隔壁とが一体に形成されたセラミックハニカム構造を有する成形体とした。次に、セラミックハニカム成形体の周縁部を加工により除去して、セラミックハニカム本体とした。次に、セラミックハニカム成形体を乾燥および焼成し、外径が267mm、全長が305mm、隔壁厚が0.3mm、セルピッチが1.57mmのコージェライト質のセラミックハニカム構造体とした。 Hereinafter, embodiments of the present invention will be described based on examples.
(Example)
Adjust kaolin, talc, silica, a powder such as alumina, in a mass ratio, SiO 2: 48~52%, Al 2 O 3: 33~37%, MgO: a cordierite generation material powder containing 12-15% Then, add methylcellulose, hydroxypropylmethylcellulose as a binder, a foamed resin as a pore former, and mix thoroughly in a dry process, then add a specified amount of water, thoroughly knead and plasticize the ceramic cup Soil was made. Next, the ceramic clay was passed through an extrusion molding die, and then cut into a predetermined length to obtain a molded body having a ceramic honeycomb structure in which a peripheral edge portion and partition walls were integrally formed. Next, the peripheral part of the ceramic honeycomb formed body was removed by processing to obtain a ceramic honeycomb body. Next, the ceramic honeycomb formed body was dried and fired to obtain a cordierite ceramic honeycomb structure having an outer diameter of 267 mm, an overall length of 305 mm, a partition wall thickness of 0.3 mm, and a cell pitch of 1.57 mm.

次に、セラミックハニカム構造体の端面に樹脂製フィルムを貼り付け、このフィルムに対してセルが市松模様になるようレーザ加工で溶融させて貫通孔を開けて、このセラミックハニカム構造体端面をコージェライト質の目封止材スラリーが配置された容器内に浸漬し、目封止部長さ約15ｍｍが得られるように、セラミックハニカム構造体のもう一方の端面から加圧手段により圧力を加えることにより、貫通穴を通じて目封止材スラリーをセルの端部に導入した。そして、フィルムを除去し、目封止されたセラミックハニカムフィルタを得た。この時、目封止の乾燥の有無を表１に示す条件とした。   Next, a resin film is affixed to the end face of the ceramic honeycomb structure, and through holes are formed by melting the cells so that the cells have a checkered pattern, and the end faces of the ceramic honeycomb structure are cordierite. By immersing in a container in which a high quality plugging material slurry is disposed and applying pressure from the other end face of the ceramic honeycomb structure by a pressure means so as to obtain a plugging portion length of about 15 mm, The plugging material slurry was introduced into the end of the cell through the through hole. Then, the film was removed to obtain a plugged ceramic honeycomb filter. At this time, the presence or absence of dry plugging was set as the conditions shown in Table 1.

次いで、得られたセラミックハニカムフィルタを、図３に示す検査装置50にセットして、隔壁の欠陥部の有無を検査する。検査装置50は、筒状の保持治具51、52にセラミックハニカムフィルタ10を保持し、一方の保持治具52からブロアー53で吸引し、他方の保持治具51からすす発生装置54で人工カーボンを投入する。ブロアーは室温の空気を10Nm3/minの流量で、人工カーボンを2g/minで投入する。10分間人工カーボンを投入した後、検査装置からセラミックハニカムフィルタを取り出し、流出側端部に人工カーボンが黒く付着したセルを有するセラミックハニカムフィルタを選定して本実施例１〜６の試料とした。   Next, the obtained ceramic honeycomb filter is set in an inspection apparatus 50 shown in FIG. The inspection device 50 holds the ceramic honeycomb filter 10 in the cylindrical holding jigs 51 and 52, sucks the blower 53 from one holding jig 52, and artificial carbon by the soot generator 54 from the other holding jig 51. . The blower is charged with room temperature air at a flow rate of 10 Nm3 / min and artificial carbon at 2 g / min. After introducing the artificial carbon for 10 minutes, the ceramic honeycomb filter was taken out from the inspection apparatus, and a ceramic honeycomb filter having cells with the artificial carbon adhered to the outflow side end portion was selected and used as samples of Examples 1-6.

そして、流出側端部に人工カーボンが黒く付着したセルを特定し、特定されたセルの流出側端部に目封止材スラリーを導入した。人工カーボンが黒く付着し、目封止材スラリーを導入したセル数の全セル数に対する割合を表１に示す。   And the cell which the artificial carbon adhered to the outflow side edge part was specified, and the plugging material slurry was introduced into the outflow side end part of the specified cell. Table 1 shows the ratio of the number of cells in which the artificial carbon adheres black and the plugging material slurry is introduced to the total number of cells.

次に、再び、検査装置50にセットして、同じ検査を実施し、流出側端部に人工カーボンが黒く付着するセルの有無を確認した。   Next, it was set again in the inspection apparatus 50, and the same inspection was performed, and it was confirmed whether or not there was a cell in which artificial carbon adhered to the outflow side end.

次に、検査済みのセラミックハニカムフィルタを焼成炉に入れ、1400℃で10時間で目封止材の焼成を行った。   Next, the inspected ceramic honeycomb filter was placed in a firing furnace, and the plugging material was fired at 1400 ° C. for 10 hours.

その後、セラミックハニカムフィルタの外周に外周壁を形成し、圧力損失の測定を行った。圧力損失テストスタンドに固定したセラミックハニカムフィルタに、空気を流量10 Nm3/minで送り込み、流入側と流出側との差圧（圧力損失）で表した。圧力損失が0.7 kPa以下の場合を「◎」、0.7を超え1.0 kPa以下の場合を「○」、1.0を超え1.5 kPa以下の場合を「△」、1.5 kPaを越える場合を「×」として初期圧力損失を評価した。 Thereafter, an outer peripheral wall was formed on the outer periphery of the ceramic honeycomb filter, and pressure loss was measured. Air was fed into a ceramic honeycomb filter fixed to a pressure loss test stand at a flow rate of 10 Nm 3 / min, and expressed as a differential pressure (pressure loss) between the inflow side and the outflow side. Initially, “◎” when pressure loss is 0.7 kPa or less, “◯” when 0.7 and 1.0 kPa or less, “△” when 1.0 and 1.5 kPa or less, and “×” when 1.5 kPa or less. Pressure loss was evaluated.

また、触媒を担持させて、触媒が担持可能か確認を行った。   Further, it was confirmed whether or not the catalyst can be supported by loading the catalyst.

（比較例１）
実施例と同様に、コージェライト質のセラミックハニカム構造体を作製し、目封止材スラリーをセルの端部に導入し、フィルムを除去し、80℃の熱風炉で目封止材を乾燥し、目封止されたセラミックハニカムフィルタを得た。
次に、セラミックハニカムフィルタを焼成炉に入れ、1400℃で10時間で目封止材の焼成を行った。
次に、検査装置50にハニカムフィルタをセットして、実施例と同様に、人工カーボンを投入した。
その後、人工カーボンが黒く付着したセルを有するハニカムフィルタは廃却した。
一方、人工カーボンを投入した状態で、人工カーボンが黒く付着したセルの無いハニカムフィルタは、焼成炉で1400℃で10時間の焼成を行って、人工カーボンを燃焼除去した。
尚、人工カーボンを投入した状態で、人工カーボンが黒く付着したセルの無いハニカムフィルタに、触媒を担持することを試みたが、触媒は担持されなかった。 (Comparative Example 1)
As in the example, a cordierite-like ceramic honeycomb structure was produced, the plugging material slurry was introduced into the end of the cell, the film was removed, and the plugging material was dried in a hot air oven at 80 ° C. A plugged ceramic honeycomb filter was obtained.
Next, the ceramic honeycomb filter was placed in a firing furnace, and the plugging material was fired at 1400 ° C. for 10 hours.
Next, a honeycomb filter was set in the inspection apparatus 50, and artificial carbon was introduced as in the example.
Thereafter, the honeycomb filter having cells with artificial carbon adhered in black was discarded.
On the other hand, in the state where the artificial carbon was added, the honeycomb filter without the cells with the artificial carbon attached black was fired at 1400 ° C. for 10 hours in a firing furnace to burn and remove the artificial carbon.
In addition, with the artificial carbon introduced, an attempt was made to support the catalyst on a honeycomb filter without cells to which the artificial carbon adhered black, but the catalyst was not supported.

Figure 2014094318
Figure 2014094318

表１より、本発明は、工数を増加することがなく、さらに、セラミックハニカムフィルタの隔壁の欠陥を検査して、不合格となった製品を廃却せず、安定して触媒を担持することができるセラミックハニカムフィルタを得ることができる。一方、比較例では、工数が増加し、不合格となった製品を廃却する必要がある。   From Table 1, the present invention does not increase the man-hours, and further checks the defects of the partition walls of the ceramic honeycomb filter and does not discard the rejected product, and stably supports the catalyst. A ceramic honeycomb filter that can be obtained can be obtained. On the other hand, in the comparative example, the number of man-hours increases and it is necessary to discard the rejected product.

１：隔壁
２ａ：流入側端部が開口されかつ流出側端部が目封止されたセル
２ｂ：流入側端部が目封止されかつ流出側端部が開口されたセル
２２ａ：特定したセル22bに隣接するセル
２２ｂ：流出側から微粒子が流出するセル（特定したセル）
３ａ、３ｂ：目封止材
３３ａ：セル22aの流入側端部を目封止する目封止材
３３ｂ：セル22bの流出側端部を目封止する目封止材
４：欠陥
１０：セラミックハニカムフィルタ
ａ：流体の流入側端部
ｂ：流体の流出側端部

1: partition wall 2a: cell with inflow side end opened and outflow side end plugged 2b: cell with inflow side end plugged and outflow side end opened 22a: specified cell Cell 22b adjacent to 22b: Cell from which fine particles flow out from the outflow side (specified cell)
3a, 3b: plugging material 33a: plugging material 33b plugging the inflow side end of the cell 22a: plugging material plugging the outflow side end of the cell 22b 4: defect 10: ceramic Honeycomb filter a: Fluid inflow side end b: Fluid outflow side end

Claims (6)

隔壁で区画形成される流体を流通するセルのうち、流体の流出側端部を市松状に目封止材により目封止し、残余のセルにおいて流体の流入側端部を目封止材により目封止するセラミックハニカムフィルタの製造方法であって、
前記目封止材は、未焼成のセラミック材料を含み、
前記セラミックハニカムフィルタの流入側から微粒子を含む気体をセルへ流通させ、流出側から所定量以上の微粒子が流出する隔壁に欠陥部を有するセルの有無を検査し、
その後、目封止材を焼成することを特徴とするセラミックハニカムフィルタの製造方法。 Out of the cells flowing through the fluid partitioned by the partition wall, the fluid outflow side end is plugged in a checkered pattern with a plugging material, and the fluid inflow end in the remaining cells is plugged with the plugging material. A method for manufacturing a plugged ceramic honeycomb filter,
The plugging material includes an unfired ceramic material,
A gas containing fine particles is circulated from the inflow side of the ceramic honeycomb filter to the cell, and the presence or absence of the cell having a defect portion in the partition wall from which a predetermined amount or more of the fine particles flows out from the outflow side is inspected.
Thereafter, the plugging material is fired, and a method for manufacturing a ceramic honeycomb filter is provided. 前記検査で、流出側から所定量以上の微粒子が流出する隔壁に欠陥部を有するセルを特定し、
(a)前記特定したセルの流出側端部を未焼成のセラミック材料を含む目封止材で目封止し、
もしくは、
(b)前記特定したセルに隣接するセルの流入側端部を未焼成のセラミック材料を含む目封止材で目封止し、
その後、目封止材を焼成することを特徴とする請求項１に記載のセラミックハニカムフィルタの製造方法。 In the inspection, a cell having a defective portion is identified in the partition wall from which a predetermined amount or more of the fine particles flows out from the outflow side,
(a) plugging the outflow side end of the identified cell with a plugging material containing an unfired ceramic material;
Or
(b) plugging the inflow side end of the cell adjacent to the identified cell with a plugging material containing an unfired ceramic material;
Thereafter, the plugging material is fired, and the method for manufacturing the ceramic honeycomb filter according to claim 1. 前記特定したセルの流出側端部を目封止したセルの数、もしくは、前記特定したセルに隣接するセルの流入側端部を目封止したセルの数が、全セル数の1％以下であることを特徴とする請求項１または請求項２に記載のセラミックハニカムフィルタの製造方法。 The number of cells plugged at the outflow side end of the specified cell or the number of cells plugged at the inflow side end of a cell adjacent to the specified cell is 1% or less of the total number of cells The method for manufacturing a ceramic honeycomb filter according to claim 1 or 2, wherein: 前記セルへ流通させる気体が室温以上の温度であることを特徴とする請求項１乃至請求項３の何れかに記載のセラミックハニカムフィルタの製造方法。 The method for manufacturing a ceramic honeycomb filter according to any one of claims 1 to 3, wherein a gas to be circulated into the cell is a temperature of room temperature or higher. 隔壁で区画形成される流体を流通するセルを備え、流体の流入側端部が開口されかつ流体の流出側端部が目封止されたセルと、流体の流入側端部が目封止されかつ流体の流出側端部が開口されたセルとが交互に配設されてなるセラミックハニカムフィルタにおいて、
前記セラミックハニカムフィルタの流入側から微粒子を含む気体をセルへ流通させ、流出側から所定量以上の微粒子が流出する隔壁に欠陥部を有するセルを特定し、
(a)前記特定したセルの流出側端部を目封止したこと、
もしくは、
(b)前記特定したセルに隣接するセルの流入側端部を目封止したこと、
を特徴とするセラミックハニカムフィルタ。 A cell that circulates the fluid defined by the partition wall, the fluid inflow end portion of the fluid being opened and the fluid outflow end portion being plugged, and the fluid inflow end portion being plugged In addition, in the ceramic honeycomb filter in which the cells having the open ends on the fluid outflow side are alternately arranged,
A gas containing fine particles is circulated from the inflow side of the ceramic honeycomb filter to the cells, and a cell having a defect portion is specified in a partition wall from which a predetermined amount or more of the fine particles flows out from the outflow side,
(a) plugging the outflow side end of the identified cell;
Or
(b) plugging the inflow side end of a cell adjacent to the identified cell;
Ceramic honeycomb filter characterized by. 前記特定したセルの流出側端部を目封止したセルの数、もしくは、前記特定したセルに隣接するセルの流入側端部を目封止したセルの数が、全セル数の1％以下であることを特徴とする請求項５に記載のセラミックハニカムフィルタ。 The number of cells plugged at the outflow side end of the specified cell or the number of cells plugged at the inflow side end of a cell adjacent to the specified cell is 1% or less of the total number of cells The ceramic honeycomb filter according to claim 5, wherein:
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