JP2019152534A - Preparation method of observation sample of collection filter section and evaluation method of collection state of particulate material in collection filter - Google Patents

Preparation method of observation sample of collection filter section and evaluation method of collection state of particulate material in collection filter Download PDF

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JP2019152534A
JP2019152534A JP2018037813A JP2018037813A JP2019152534A JP 2019152534 A JP2019152534 A JP 2019152534A JP 2018037813 A JP2018037813 A JP 2018037813A JP 2018037813 A JP2018037813 A JP 2018037813A JP 2019152534 A JP2019152534 A JP 2019152534A
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collection filter
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JP6934436B2 (en
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内田　雅之
Masayuki Uchida
雅之 内田
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NGK Insulators Ltd
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Abstract

To provide a preparation method of an observation sample of a collection filter section, which can precisely evaluate a collection state of a particulate material in a collection filter.SOLUTION: A preparation method of an observation sample of a collection filter section for evaluating a collection state of a particulate material includes: a step of forming cutouts on at least two facing surfaces at a position of forming a section of a collection filter; and a step of breaking the cutouts by applying stress to them while supporting the collection filter.SELECTED DRAWING: None

Description

本発明は、捕集フィルタ断面観察試料の作製方法、及び捕集フィルタにおける粒子状物質の捕集状態を評価する方法に関する。   The present invention relates to a method for preparing a collection filter cross-section observation sample and a method for evaluating the collection state of particulate matter in the collection filter.

内燃機関などから排出される排気ガス中の粒子状物質は、人体、環境などへの影響が大きいため、大気への放出を防止する必要性が高まっている。特に、ディーゼルエンジン及びガソリン直噴エンジンから排出されるＰＭ（パティキュレートマター）は、上記影響が甚大であり、ＰＭの規制は、世界的に強化されている。このような背景に伴い、粒子状物質を捕集する捕集フィルタにおいて、粒子状物質がどのように捕集されているのかを評価することが必要となっている。そこで、カッターナイフなどを用いて捕集フィルタを切断加工し、その断面を顕微鏡観察することにより、粒子状物質の捕集状態を評価していた。   Since the particulate matter in the exhaust gas discharged from an internal combustion engine or the like has a great influence on the human body, the environment, etc., there is an increasing need to prevent release to the atmosphere. In particular, PM (particulate matter) discharged from diesel engines and gasoline direct injection engines has the above-mentioned influence, and PM regulations are being strengthened worldwide. With such a background, it is necessary to evaluate how the particulate matter is collected in the collection filter that collects the particulate matter. Therefore, the collection state of the particulate matter has been evaluated by cutting the collection filter using a cutter knife or the like and observing the cross section under a microscope.

しかしながら、カッターナイフなどを用いて捕集フィルタを切断加工した場合、切断粉が断面に付着し易い。切断粉は、顕微鏡観察した際に粒子状物質との区別がつき難いため、粒子状物質の捕集状態を正確に評価できないという問題があった。特に、炭化珪素などから形成された捕集フィルタを評価する場合に、この問題が顕著である。   However, when the collection filter is cut using a cutter knife or the like, the cut powder easily adheres to the cross section. Since the cut powder is difficult to distinguish from the particulate matter when observed under a microscope, there is a problem in that the collection state of the particulate matter cannot be accurately evaluated. In particular, this problem is significant when evaluating a collection filter formed of silicon carbide or the like.

本発明は、上記のような問題を解決するためになされたものであり、捕集フィルタにおける粒子状物質の捕集状態を正確に評価することが可能な捕集フィルタ断面観察試料の作製方法を提供することを目的とする。また、本発明は、捕集フィルタにおける粒子状物質の捕集状態を正確に評価する方法を提供することを目的とする。   The present invention has been made to solve the above-described problems, and provides a method for producing a collection filter cross-sectional observation sample capable of accurately evaluating the collection state of particulate matter in the collection filter. The purpose is to provide. Another object of the present invention is to provide a method for accurately evaluating the collection state of particulate matter in a collection filter.

本発明者らは、捕集フィルタの断面形成位置の少なくとも対向する２つの表面に切り込み部を形成した後、捕集フィルタを支持しながら切り込み部に応力を加えて破断させることにより、上記の問題を解決することが可能な捕集フィルタ断面観察試料が得られることを見出し、本発明を完成するに至った。   The present inventors have formed the above-mentioned problem by forming a cut portion on at least two opposing surfaces of the cross-section formation position of the collection filter, and then applying stress to the cut portion while supporting the collection filter to cause breakage. As a result, it was found that a sample for observing a collection filter cross-section that can solve the above problem was obtained, and the present invention was completed.

すなわち、本発明は、粒子状物質の捕集状態を評価するための捕集フィルタ断面観察試料の作製方法であって、捕集フィルタの断面形成位置の少なくとも対向する２つの表面に切り込み部を形成する工程と、前記捕集フィルタを支持しながら前記切り込み部に応力を加えて破断させる工程とを含む、捕集フィルタ断面観察試料の作製方法である。   That is, the present invention is a method for preparing a collection filter cross-section observation sample for evaluating the collection state of particulate matter, and forming cut portions on at least two opposing surfaces of the cross-section formation position of the collection filter And a step of applying a stress to the cut portion and breaking the support while supporting the collection filter.

また、本発明は、捕集フィルタにおける粒子状物質の捕集状態を評価する方法であって、前記作製方法によって得られた前記捕集フィルタ断面観察試料の断面を光学顕微鏡で観察する方法である。   Further, the present invention is a method for evaluating the collection state of the particulate matter in the collection filter, and is a method for observing a cross section of the collection filter cross section observation sample obtained by the production method with an optical microscope. .

本発明によれば、捕集フィルタにおける粒子状物質の捕集状態を正確に評価することが可能な捕集フィルタ断面観察試料の作製方法を提供することができる。また、本発明によれば、捕集フィルタにおける粒子状物質の捕集状態を正確に評価する方法を提供することができる。   ADVANTAGE OF THE INVENTION According to this invention, the preparation method of the collection filter cross-section observation sample which can evaluate correctly the collection state of the particulate matter in a collection filter can be provided. Moreover, according to this invention, the method of evaluating correctly the collection state of the particulate matter in a collection filter can be provided.

捕集フィルタの斜視図である。It is a perspective view of a collection filter. 捕集フィルタの断面形成位置の対向する２つの表面に切り込み部を形成した状態を示す捕集フィルタの側面図である。It is a side view of the collection filter which shows the state which formed the cut | notch part in two surfaces where the cross-section formation position of a collection filter opposes. 捕集フィルタの断面形成位置の表面全体に切り込み部を形成した状態を示す捕集フィルタの側面図である。It is a side view of a collection filter which shows the state where the cut part was formed in the whole surface of the section formation position of a collection filter. テープを用いて捕集フィルタを支持した状態を示す捕集フィルタの側面図である。It is a side view of the collection filter which shows the state which supported the collection filter using the tape. 捕集フィルタの切り込み部に３点曲げによって応力を加える状態を示す図である。It is a figure which shows the state which applies stress to the cut | notch part of a collection filter by 3 point | piece bending. 捕集フィルタの切り込み部に４点曲げによって応力を加える状態を示す図である。It is a figure which shows the state which applies stress to the cut | notch part of a collection filter by 4-point bending. 実施例１の捕集フィルタ断面観察試料の光学顕微鏡写真である。2 is an optical micrograph of a collection filter cross-section observation sample of Example 1. FIG. 比較例１の捕集フィルタ断面観察試料の光学顕微鏡写真である。4 is an optical micrograph of a collection filter cross-section observation sample of Comparative Example 1.

以下、本発明の捕集フィルタ断面観察試料の作製方法、及び捕集フィルタにおける粒子状物質の捕集状態を評価する方法の好適な実施の形態について、具体的に説明するが、本発明はこれらに限定されて解釈されるべきものではなく、本発明の要旨を逸脱しない限りにおいて、当業者の知識に基づいて、種々の変更、改良などを行うことができる。各実施形態に開示されている複数の構成要素は、適宜な組み合わせにより、種々の発明を形成できる。例えば、実施形態に示される全構成要素からいくつかの構成要素を削除してもよいし、異なる実施形態の構成要素を適宜組み合わせてもよい。   Hereinafter, preferred embodiments of the method for producing a sample for observing a cross section of a collection filter according to the present invention and a method for evaluating the collection state of particulate matter in the collection filter will be described in detail. The present invention should not be construed as being limited thereto, and various changes and improvements can be made based on the knowledge of those skilled in the art without departing from the gist of the present invention. A plurality of constituent elements disclosed in each embodiment can form various inventions by an appropriate combination. For example, some constituent elements may be deleted from all the constituent elements shown in the embodiments, or constituent elements of different embodiments may be appropriately combined.

（捕集フィルタ断面観察試料の作製方法）
本実施形態の捕集フィルタ断面観察試料の作製方法は、捕集フィルタの断面形成位置の少なくとも対向する２つの表面に切り込み部を形成する工程と、捕集フィルタを支持しながら切り込み部に応力を加えて破断させる工程とを含む。 (Production method of sample for collecting filter cross section)
The method for producing the collection filter cross-section observation sample of the present embodiment includes a step of forming cut portions on at least two opposing surfaces of the cross-section formation position of the collection filter, and applying stress to the cut portions while supporting the collection filter And a step of breaking.

本実施形態の捕集フィルタ断面観察試料の作製方法に用いられる捕集フィルタとしては、特に限定されず、ＤＰＦ（ディーゼルパティキュレートフィルタ）、ＧＰＦ（ガソリンパティキュレートフィルタ）などであることができる。捕集フィルタは、捕集フィルタ断面観察試料の作製を容易にする観点から、適切なサイズ及び形状に予め切断加工しておくことが好ましい。捕集フィルタのサイズ及び形状は、特に限定されないが、例えば、軸方向長さが４０〜１５０ｍｍ、軸方向に直交する断面の一辺が１０〜２０ｍｍである四角柱状とすればよい。   It does not specifically limit as a collection filter used for the preparation method of the collection filter cross-section observation sample of this embodiment, DPF (diesel particulate filter), GPF (gasoline particulate filter) etc. can be used. From the viewpoint of facilitating preparation of the collection filter cross-section observation sample, the collection filter is preferably cut into an appropriate size and shape in advance. The size and shape of the collection filter are not particularly limited. For example, the collection filter may have a rectangular column shape having an axial length of 40 to 150 mm and a side of the cross section orthogonal to the axial direction of 10 to 20 mm.

図１は、本実施形態の捕集フィルタ断面観察試料の作製方法に用いられる捕集フィルタの一例を示す斜視図である。図１において、捕集フィルタ１は、第１端面２から第２端面３まで貫通して流体の流路を形成する複数のセル４を区画形成する隔壁５を有するハニカム構造体である。   FIG. 1 is a perspective view showing an example of a collection filter used in the method for producing a collection filter cross-section observation sample of this embodiment. In FIG. 1, the collection filter 1 is a honeycomb structure having partition walls 5 that partition and form a plurality of cells 4 that penetrate from the first end face 2 to the second end face 3 and form fluid flow paths.

捕集フィルタ１を構成する材料としては、特に限定されないが、セラミックスから形成されていることが好ましい。セラミックスの例としては、炭化珪素、珪素−炭化珪素系複合材料、窒化珪素、コージェライト、ムライト、アルミナ、スピネル、コージェライト−炭化珪素系複合材料、リチウムアルミニウムシリケート、チタン酸アルミニウムなどが挙げられる。これらの中でも、炭化珪素又は珪素−炭化珪素系複合材料から形成される捕集フィルタ１は、カッターナイフなどを用いて切断加工した場合に切断粉と粒子状物質との区別がつき難いため、本実施形態の捕集フィルタ断面観察試料の作製に用いるのに適している。なお、「珪素−炭化珪素系複合材料」とは、炭化珪素を骨材とし、珪素を結合材として形成された複合材料である。ここで、本明細書において「主成分」とは、全成分に占める割合が５０質量％を超える成分を意味する。   Although it does not specifically limit as a material which comprises the collection filter 1, It is preferable that it is formed from ceramics. Examples of ceramics include silicon carbide, silicon-silicon carbide based composite material, silicon nitride, cordierite, mullite, alumina, spinel, cordierite-silicon carbide based composite material, lithium aluminum silicate, aluminum titanate and the like. Among these, the collection filter 1 formed from silicon carbide or a silicon-silicon carbide based composite material is difficult to distinguish between cutting powder and particulate matter when cut using a cutter knife or the like. It is suitable for use in the preparation of the collection filter cross-section observation sample of the embodiment. The “silicon-silicon carbide based composite material” is a composite material formed using silicon carbide as an aggregate and silicon as a binder. Here, the “main component” in the present specification means a component that accounts for 50% by mass of all components.

捕集フィルタ１の形状としては、特に限定されないが、四角柱状、六角柱状、八角柱状などの多角柱状、円柱状又は楕円柱状である。   The shape of the collection filter 1 is not particularly limited, but is a polygonal column shape such as a quadrangular column shape, a hexagonal column shape, or an octagonal column shape, a cylindrical shape, or an elliptical column shape.

本実施形態の捕集フィルタ断面観察試料の作製方法では、まず、捕集フィルタ１の断面形成位置６の少なくとも対向する２つの表面に切り込み部を形成する。
ここで、本明細書において「断面形成位置６」とは、断面を形成すべき位置のことを意味する。
捕集フィルタ１の断面形成位置６は、特に限定されず、観察者によって適宜選択されることができる。典型的には、捕集フィルタ１の断面形成位置６は、ハニカム構造体の軸方向に直交する方向にある。この場合、捕集フィルタ１の断面は、ハニカム構造体の軸方向に直交する方向に形成される。 In the method for producing the collection filter cross-section observation sample of the present embodiment, first, cut portions are formed on at least two opposing surfaces of the cross-section formation position 6 of the collection filter 1.
Here, “cross-section forming position 6” in this specification means a position where a cross-section is to be formed.
The cross-section formation position 6 of the collection filter 1 is not particularly limited, and can be appropriately selected by an observer. Typically, the cross-section formation position 6 of the collection filter 1 is in a direction orthogonal to the axial direction of the honeycomb structure. In this case, the cross section of the collection filter 1 is formed in a direction orthogonal to the axial direction of the honeycomb structure.

図２は、捕集フィルタ１の断面形成位置６の対向する２つの表面（上面及び下面）に切り込み部７を形成した状態を示す捕集フィルタの側面図である。対向する２つの表面に切り込み部７を形成することにより、これらの切り込み部７が、応力によって破断させる際の起点及び終点となるため、平坦な断面が形成され易くなる。平坦な断面は、顕微鏡観察の際にピントを合わせ易くすることができるため、断面観察が容易になる。
図３は、捕集フィルタ１の断面形成位置６の表面全体に切り込み部７を形成した状態を示す捕集フィルタ１の側面図である。表面全体に切り込み部７を形成することにより、平坦な断面がより一層形成され易くなるため、上記の効果を安定して得ることができる。 FIG. 2 is a side view of the collection filter showing a state in which cut portions 7 are formed on two opposing surfaces (upper surface and lower surface) of the cross-section formation position 6 of the collection filter 1. By forming the cut portions 7 on the two opposing surfaces, the cut portions 7 serve as starting points and end points when being broken by stress, so that a flat cross section is easily formed. A flat cross-section can be focused easily during microscopic observation, so that cross-section observation is facilitated.
FIG. 3 is a side view of the collection filter 1 showing a state in which the cut portion 7 is formed on the entire surface of the cross-section formation position 6 of the collection filter 1. By forming the cut portion 7 on the entire surface, a flat cross section is more easily formed, and thus the above effect can be stably obtained.

切り込み部７を形成する方法としては、特に限定されず、当該技術分野において公知の方法を用いることができる。例えば、カッターナイフ、レーザーなどの切り込み手段を用いて切り込み部７を形成することができる。   The method for forming the cut portion 7 is not particularly limited, and methods known in the technical field can be used. For example, the cut portion 7 can be formed using a cutting means such as a cutter knife or a laser.

切り込み部７の深さとしては、特に限定されず、捕集フィルタ１の大きさに応じて適宜調整すればよい。典型的には、切り込み部７の深さは、平坦な断面を形成する観点から、切り込み方向の捕集フィルタ１の長さの１／１５以上であることが好ましく、１／１３以上であることが好ましい。また、切り込み部７の深さは、切り込み粉が断面に付着することを防止する観点から、切り込み方向の捕集フィルタ１の長さの１／５以下であることが好ましく、１／８以下であることが好ましい。   The depth of the cut portion 7 is not particularly limited, and may be appropriately adjusted according to the size of the collection filter 1. Typically, from the viewpoint of forming a flat cross section, the depth of the cut portion 7 is preferably 1/15 or more of the length of the collection filter 1 in the cut direction, and 1/13 or more. Is preferred. Further, the depth of the cut portion 7 is preferably 1/5 or less of the length of the collecting filter 1 in the cut direction, and 1/8 or less, from the viewpoint of preventing the cut powder from adhering to the cross section. Preferably there is.

切り込み部７の幅としては、特に限定されないが、平坦な断面を形成する観点から、典型的に０．１ｍｍ〜３ｍｍ、好ましくは０．５ｍｍ〜２ｍｍ、より好ましくは０．５〜１．５ｍｍである。   Although it does not specifically limit as a width | variety of the cut | notch part 7, From a viewpoint of forming a flat cross section, it is typically 0.1 mm-3 mm, Preferably it is 0.5 mm-2 mm, More preferably, it is 0.5-1.5 mm. is there.

次に、切り込み部７が形成された捕集フィルタ１は、捕集フィルタ１を支持しながら切り込み部７に応力を加えることによって破断させる。このようにして断面を形成することにより、カッターナイフなどを用いて切断加工した場合のように切断粉が断面に付着することを抑制することができる。また、捕集フィルタ１を支持しながら破断させているため、破断時の衝撃によって捕集フィルタ１に捕集された粒子状物質が移動することを防止することができる。したがって、捕集フィルタ１における粒子状物質の捕集状態を正確に評価することができる。   Next, the collection filter 1 in which the cut portion 7 is formed is broken by applying stress to the cut portion 7 while supporting the collection filter 1. By forming the cross section in this way, it is possible to prevent the cutting powder from adhering to the cross section as in the case of cutting using a cutter knife or the like. Moreover, since it is made to break while supporting the collection filter 1, it can prevent that the particulate matter collected by the collection filter 1 moves by the impact at the time of a fracture | rupture. Therefore, the collection state of the particulate matter in the collection filter 1 can be accurately evaluated.

捕集フィルタ１を支持する方法としては、特に限定されず、当該技術分野において公知の方法を用いることができる。例えば、捕集フィルタ１は、テープ、弾性部材などの支持手段を用いて支持することができる。
図４は、テープ１０を用いて捕集フィルタ１を支持した状態を示す捕集フィルタ１の側面図である。図４では、断面形成位置６の表面全体を被覆するようにテープ１０が貼着されているが、断面形成位置６の一部のみを被覆するように貼着されていてもよい。
弾性部材を用いて捕集フィルタ１を支持する場合、断面形成位置６の底部に弾性部材を配置すればよい。弾性部材としては、特に限定されないが、例えば、スポンジ製のクッション部材などを用いればよい。 It does not specifically limit as a method to support the collection filter 1, A well-known method can be used in the said technical field. For example, the collection filter 1 can be supported using a support means such as a tape or an elastic member.
FIG. 4 is a side view of the collection filter 1 showing a state in which the collection filter 1 is supported using the tape 10. In FIG. 4, the tape 10 is attached so as to cover the entire surface of the cross-section formation position 6, but may be attached so as to cover only a part of the cross-section formation position 6.
When the collection filter 1 is supported using an elastic member, the elastic member may be disposed at the bottom of the cross-section forming position 6. The elastic member is not particularly limited. For example, a sponge cushion member or the like may be used.

切り込み部７に応力を加える方法としては、特に限定されず、当該技術分野において公知の方法を用いることができる。例えば、応力は、３点曲げ又は４点曲げによって切り込み部７に加えることができる。
ここで、本明細書において「３点曲げ」とは、図５に示すように、捕集フィルタ１の両端を支点１１とし、切り込み部７に１つの力点１２を設けて負荷を印加することを意味する。また、「４点曲げ」とは、図６に示すように、捕集フィルタ１の両端を支点１１とし、切り込み部７を挟むようにして２つの力点１２を設けて負荷を印加することを意味する。 The method for applying stress to the cut portion 7 is not particularly limited, and methods known in the technical field can be used. For example, the stress can be applied to the cut portion 7 by three-point bending or four-point bending.
Here, “three-point bending” in the present specification means that, as shown in FIG. 5, both ends of the collection filter 1 are set as fulcrums 11 and one force point 12 is provided in the cut portion 7 to apply a load. means. In addition, “four-point bending” means that a load is applied by providing two force points 12 with the both ends of the collection filter 1 as fulcrums 11 and the notches 7 interposed therebetween, as shown in FIG. 6.

応力は、市販の万能試験機を用いることによって容易に適用することができる。ここで、本明細書において「万能試験機」とは、引張試験、圧縮試験、曲げ試験などの多様な試験を行うことが可能な試験装置のことを意味する。   The stress can be easily applied by using a commercially available universal testing machine. Here, the “universal testing machine” in this specification means a test apparatus capable of performing various tests such as a tensile test, a compression test, a bending test and the like.

応力は、破断時に停止させることが好ましい。例えば、万能試験機を用いる場合には、破断時に応力の付与が自動停止するように設定すればよい。このようにすることで、捕集フィルタ１に捕集された粒子状物質が破断後に移動することを防止することができる。   The stress is preferably stopped at the time of breakage. For example, when a universal testing machine is used, it may be set so that application of stress automatically stops at the time of fracture. By doing in this way, it can prevent that the particulate matter collected by the collection filter 1 moves after a fracture | rupture.

（捕集フィルタにおける粒子状物質の捕集状態を評価する方法）
本実施形態の捕集フィルタにおける粒子状物質の捕集状態を評価する方法は、上記の作製方法によって得られた捕集フィルタ断面観察試料の断面を光学顕微鏡で観察する。
捕集フィルタ断面観察試料の断面を電子顕微鏡で観察する場合、顕微鏡内を真空にする必要があり、その際に捕集フィルタに捕集された粒子状物質が移動してしまい、粒子状物質の捕集状態を正確に評価できないことがある。
これに対して本実施形態の評価方法では、捕集フィルタ断面観察試料の断面を光学顕微鏡で観察するため、顕微鏡内を真空にする必要がなく、捕集フィルタに捕集された粒子状物質が移動することを防止することができる。そのため、本実施形態の評価方法によれば、捕集フィルタに捕集された粒子状物質の捕集状態を正確に評価することができる。 (Method of evaluating the collection state of particulate matter in the collection filter)
In the method of evaluating the collection state of the particulate matter in the collection filter of the present embodiment, the cross section of the collection filter cross section observation sample obtained by the above production method is observed with an optical microscope.
When observing the cross section of the sample of the collection filter cross section with an electron microscope, the inside of the microscope must be evacuated, and the particulate matter collected by the collection filter will move at this time, and the particulate matter The collection state may not be evaluated accurately.
On the other hand, in the evaluation method of this embodiment, since the cross section of the collection filter cross section observation sample is observed with an optical microscope, there is no need to evacuate the inside of the microscope, and the particulate matter collected by the collection filter is It can be prevented from moving. Therefore, according to the evaluation method of the present embodiment, the collection state of the particulate matter collected by the collection filter can be accurately evaluated.

以下、本発明を実施例によって更に具体的に説明するが、本発明はこれらの実施例によって何ら限定されるものではない。
（実施例１）
炭化珪素から形成された使用済みＤＰＦから、軸方向長さ５０ｍｍ、軸方向に直交する断面が１５ｍｍ×２０ｍｍの長方形である四角柱状のハニカム構造体を切断加工によって得た。
このハニカム構造体の断面形成位置の表面全体にカッターナイフを用いて、幅１ｍｍ×深さ２ｍｍの切り込み部を形成した。次に、切り込み部の全体を被覆するようにテープを貼着した。その後、万能試験機（インストロン社製３３６６デュアルコラム卓上型試験機）を用いて、図６に示すような４点曲げによって応力を切り込み部に加えて破断させることにより、捕集フィルタ断面観察試料を得た。万能試験機は、破断時に応力の付与が自動停止するように設定した。 EXAMPLES Hereinafter, the present invention will be described more specifically with reference to examples, but the present invention is not limited to these examples.
Example 1
From a used DPF formed of silicon carbide, a rectangular columnar honeycomb structure having an axial length of 50 mm and a rectangular shape having a cross section perpendicular to the axial direction of 15 mm × 20 mm was obtained by cutting.
Using a cutter knife, a cut portion having a width of 1 mm and a depth of 2 mm was formed on the entire surface of the cross-section formation position of the honeycomb structure. Next, a tape was attached so as to cover the entire cut portion. Then, using a universal testing machine (Instron 3366 dual column tabletop testing machine), the stress is applied to the cut portion by four-point bending as shown in FIG. Got. The universal testing machine was set so that the application of stress automatically stopped when ruptured.

（比較例１）
カッターナイフを用いた切断加工によってハニカム構造体を切断したこと以外は、実施例１と同様の条件にて捕集フィルタ断面観察試料を得た。 (Comparative Example 1)
A collection filter cross-section observation sample was obtained under the same conditions as in Example 1 except that the honeycomb structure was cut by a cutting process using a cutter knife.

上記の実施例１及び比較例１で得られた捕集フィルタ断面観察試料について、光学顕微鏡（キーエンス社製ＶＨＸ−１０００）を用いて断面の観察を行った。実施例１の捕集フィルタ断面観察試料の光学顕微鏡写真を図７、比較例１の捕集フィルタ断面観察試料の光学顕微鏡写真を図８に示す。なお、図７及び８において、（ａ）は３０倍、（ｂ）は１５０倍の光学顕微鏡写真である。
図７及び８に示すように、比較例１の捕集フィルタ断面観察試料では、多くの切断粉が断面に付着しているため、捕集フィルタと粒子状物質との区別がつき難かったのに対し、実施例１の捕集フィルタ断面観察試料は、切断粉が断面にほとんど付着しておらず、捕集フィルタと粒子状物質との区別が容易であった。 About the collection filter cross-sectional observation sample obtained by said Example 1 and Comparative Example 1, the cross section was observed using the optical microscope (VHX-1000 by Keyence Corporation). FIG. 7 shows an optical micrograph of the collection filter cross-section observation sample of Example 1, and FIG. 8 shows an optical micrograph of the collection filter cross-section observation sample of Comparative Example 1. 7 and 8, (a) is an optical micrograph of 30 times and (b) is 150 times.
As shown in FIGS. 7 and 8, in the collection filter cross-section observation sample of Comparative Example 1, since many cutting powders are attached to the cross section, it was difficult to distinguish the collection filter from the particulate matter. On the other hand, in the collection filter cross-section observation sample of Example 1, the cut powder hardly adhered to the cross section, and it was easy to distinguish the collection filter from the particulate matter.

以上の結果からわかるように、本発明によれば、捕集フィルタにおける粒子状物質の捕集状態を正確に評価することが可能な捕集フィルタ断面観察試料の作製方法を提供することができる。また、本発明によれば、捕集フィルタにおける粒子状物質の捕集状態を正確に評価する方法を提供することができる。   As can be seen from the above results, according to the present invention, it is possible to provide a method for producing a collection filter cross-section observation sample capable of accurately evaluating the collection state of particulate matter in the collection filter. Moreover, according to this invention, the method of evaluating correctly the collection state of the particulate matter in a collection filter can be provided.

１ 捕集フィルタ
２ 第１端面
３ 第２端面
４ セル
５ 隔壁
６ 断面形成位置
７ 切り込み部
１０ テープ
１１ 支点
１２ 力点 DESCRIPTION OF SYMBOLS 1 Collection filter 2 1st end surface 3 2nd end surface 4 Cell 5 Partition 6 Cross-section formation position 7 Cut part 10 Tape 11 Supporting point 12 Power point

Claims (11)

粒子状物質の捕集状態を評価するための捕集フィルタ断面観察試料の作製方法であって、
捕集フィルタの断面形成位置の少なくとも対向する２つの表面に切り込み部を形成する工程と、
前記捕集フィルタを支持しながら前記切り込み部に応力を加えて破断させる工程と
を含む、捕集フィルタ断面観察試料の作製方法。 A method for producing a sample for cross-sectional observation of a collection filter for evaluating the collection state of particulate matter,
Forming a notch in at least two opposing surfaces of the cross-section formation position of the collection filter;
And a step of applying a stress to the cut portion to break the support while supporting the collection filter. 前記捕集フィルタは、前記断面形成位置の少なくとも一部を被覆するように貼着されたテープ、又は前記断面形成位置の底部に配置された弾性部材によって支持される、請求項１に記載の捕集フィルタ断面観察試料の作製方法。   The collection filter according to claim 1, wherein the collection filter is supported by a tape attached so as to cover at least a part of the cross-section formation position, or an elastic member disposed at a bottom of the cross-section formation position. A method for producing a sample for collecting cross-section of a collecting filter. 前記応力が、３点曲げ又は４点曲げによって加えられる、請求項１又は２に記載の捕集フィルタ断面観察試料の作製方法。   The method for producing a collection filter cross-section observation sample according to claim 1 or 2, wherein the stress is applied by three-point bending or four-point bending. 前記切り込み部が、前記捕集フィルタの断面形成位置の表面全体に形成される、請求項１〜３のいずれか一項に記載の捕集フィルタ断面観察試料の作製方法。   The manufacturing method of the collection filter cross-section observation sample as described in any one of Claims 1-3 with which the said notch part is formed in the whole surface of the cross-section formation position of the said collection filter. 前記応力は破断時に停止させる、請求項１〜４のいずれか一項に記載の捕集フィルタ断面観察試料の作製方法。   The method for producing a collection filter cross-section observation sample according to any one of claims 1 to 4, wherein the stress is stopped at the time of fracture. 前記応力が万能試験機によって加えられる、請求項１〜５のいずれか一項に記載の捕集フィルタ断面観察試料の作製方法。   The method for producing a collection filter cross-sectional observation sample according to any one of claims 1 to 5, wherein the stress is applied by a universal testing machine. 前記捕集フィルタが、第１端面から第２端面まで貫通して流体の流路を形成する複数のセルを区画形成する隔壁を有するハニカム構造体である、請求項１〜６のいずれか一項に記載の捕集フィルタ断面観察試料の作製方法。   7. The honeycomb structure according to claim 1, wherein the collection filter is a honeycomb structure having partition walls that partition and form a plurality of cells that penetrate from the first end face to the second end face to form a fluid flow path. The preparation method of the collection filter cross-section observation sample of description. 前記捕集フィルタの断面が、前記ハニカム構造体の軸方向に直交する方向に形成される、請求項７に記載の捕集フィルタ断面観察試料の作製方法。   The method for producing a collection filter cross-section observation sample according to claim 7, wherein a cross section of the collection filter is formed in a direction orthogonal to an axial direction of the honeycomb structure. 前記捕集フィルタがＤＰＦである、請求項１〜８のいずれか一項に記載の捕集フィルタ断面観察試料の作製方法。   The manufacturing method of the collection filter cross-section observation sample as described in any one of Claims 1-8 whose said collection filter is DPF. 前記捕集フィルタが、セラミックスから形成されている、請求項１〜９のいずれか一項に記載の捕集フィルタ断面観察試料の作製方法。   The method for producing a collection filter cross-section observation sample according to any one of claims 1 to 9, wherein the collection filter is formed of ceramics. 捕集フィルタにおける粒子状物質の捕集状態を評価する方法であって、
請求項１〜１０のいずれか一項に記載の作製方法によって得られた前記捕集フィルタ断面観察試料の断面を光学顕微鏡で観察する方法。 A method for evaluating the collection state of particulate matter in a collection filter,
The method of observing the cross section of the said collection filter cross-section observation sample obtained by the preparation method as described in any one of Claims 1-10 with an optical microscope.
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