JP2012006820A - Ceramic joined body and method for producing the same - Google Patents
Ceramic joined body and method for producing the same Download PDFInfo
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Abstract
Description
本発明は、セラミックスの接合方法およびその製造方法に係り、特に半導体製造装置用部材などに好適なセラミックス接合体およびその製造方法に関する発明である。 The present invention relates to a ceramic bonding method and a manufacturing method thereof, and more particularly to a ceramic bonded body suitable for a member for a semiconductor manufacturing apparatus and the manufacturing method thereof.
セラミックスは、金属やプラスチックなどと比較して耐熱性や耐蝕性、耐摩耗性が高く、高温、腐食環境などの過酷な条件下でも使用できる材料である。中でも、炭化ケイ素セラミックスは、高剛性、高熱伝導性、低熱膨張性などの優れた特性を有することから、高温構造部材や半導体製造装置用部材として利用されている。
このように、セラミックスは過酷な環境下で使用可能な有用な材料であるが、複雑な形状、あるいは大型部材を一体成型で作製することは難しく、比較的小さなセラミックス成形体やセラミックス焼結体を接合させることで複雑な形状や大型部材を作製することが求められている。
Ceramics have higher heat resistance, corrosion resistance, and wear resistance than metals and plastics, and can be used even under severe conditions such as high temperatures and corrosive environments. Among these, silicon carbide ceramics have excellent properties such as high rigidity, high thermal conductivity, and low thermal expansibility, and thus are used as high-temperature structural members and semiconductor manufacturing apparatus members.
In this way, ceramics are useful materials that can be used in harsh environments, but it is difficult to produce complex shapes or large-sized members by integral molding. It is required to produce a complicated shape or a large member by bonding.
従来、SiCセラミックス焼結体がカーボンを介して拡散接合されたセラミックス複合部材が知られている。また、有機物を介してセラミックス部材の接合面同士を互いに接触させて有機物の分解温度以上で、且つ非酸化雰囲気中で加熱するセラミックス複合部材の製造方法が知られている。(例えば、特許文献1参照)
炭素の拡散を利用した上記接合方法の場合、接合層厚みを全体で均一且つ所望の厚さに制御することが困難であるという問題があった。
Conventionally, a ceramic composite member in which a SiC ceramic sintered body is diffusion bonded via carbon is known. In addition, there is known a method for manufacturing a ceramic composite member in which bonding surfaces of ceramic members are brought into contact with each other through an organic substance and heated in a non-oxidizing atmosphere at a temperature higher than the decomposition temperature of the organic substance. (For example, see Patent Document 1)
In the case of the above-described bonding method using carbon diffusion, there is a problem that it is difficult to control the bonding layer thickness to a uniform and desired thickness as a whole.
また、従来、炭化ケイ素基反応焼結体からなる複数の部品ユニットを、炭化ケイ素結晶粒と炭化ケイ素結晶粒の隙間にネットワーク状に連続して存在するシリコン相とから構成される接合層を介して接合してなる炭化ケイ素基接合部材が知られている。この炭化ケイ素基接合部材は、複数の部品ユニットに対応する成形体を有機系接着剤で接着した予備接合体を不活性ガス雰囲気中にて1400℃以上の温度に加熱し、加熱状態を維持した成形体および接合層に溶融したシリコンを含浸して作製されるものである。(例えば、特許文献2参照。)
しかし、この場合は接合工程で溶融したシリコンを含有させるために外部からケイ素を添加する必要があり、接合手法が煩雑であること、及び、外部から添加したケイ素を接合層全体に一様に含有させ、接合層全体を均質にすることが困難であるという問題があった。
In addition, conventionally, a plurality of component units made of silicon carbide-based reaction sintered bodies are connected to each other through a bonding layer composed of silicon carbide crystal grains and silicon phases continuously existing in a network form in the gaps between the silicon carbide crystal grains. Silicon carbide-based joining members obtained by joining are known. This silicon carbide-based joining member was heated to a temperature of 1400 ° C. or higher in an inert gas atmosphere by maintaining a pre-joined body in which molded bodies corresponding to a plurality of component units were bonded with an organic adhesive, and the heated state was maintained. It is produced by impregnating a molded body and a bonding layer with molten silicon. (For example, see Patent Document 2.)
However, in this case, it is necessary to add silicon from the outside in order to contain silicon melted in the joining process, the joining method is complicated, and silicon added from the outside is uniformly contained in the entire joining layer. There is a problem that it is difficult to make the entire bonding layer uniform.
本発明は、上記問題を解決するためになされたもので、外部から金属ケイ素を添加することなく、被接合体から浸透してくる程度の微量な金属ケイ素のみにより接合層を形成するという簡単な接合手法によって得られ、高強度に接合されたセラミックス接合体、およびその製造方法を提供することを目的としている。 The present invention has been made in order to solve the above-described problem. A joining layer is formed only by a small amount of metallic silicon that penetrates from the joined body without adding metallic silicon from the outside. It is an object of the present invention to provide a ceramic joined body obtained by a joining technique and joined with high strength, and a method for producing the same.
上記課題を解決するために本発明の一実施形態は、金属ケイ素を含むセラミックス焼結体からなる第1の被接合体と、セラミックス焼結体からなる第2の被接合体と、が接合層を介して接合され、接合層は金属ケイ素を主成分とすることを特徴とするセラミックス接合体である。本発明のセラミックス接合体によれば、簡単な接合手法によって得られ、高強度に接合されたセラミックス接合体を提供することが可能となる。
尚、「金属ケイ素を含むセラミックス焼結体」とは、セラミックス焼結体を構成する金属ケイ素とセラミックスとが混合物である、いわゆるコンポジット状態であることをさす。金属ケイ素元素を含む化合物で構成されるセラミックス焼結体ではない。
In order to solve the above-described problem, an embodiment of the present invention includes a first bonded body made of a ceramic sintered body containing metal silicon and a second bonded body made of a ceramic sintered body. The bonding layer is a ceramic bonded body characterized in that metal silicon is the main component. According to the ceramic joined body of the present invention, it is possible to provide a ceramic joined body obtained by a simple joining technique and joined with high strength.
The “ceramic sintered body containing metal silicon” means a so-called composite state in which the metal silicon and the ceramic constituting the ceramic sintered body are a mixture. It is not a ceramic sintered body composed of a compound containing a metal silicon element.
本発明の好ましい態様によれば、第2の被接合体が金属ケイ素を含むセラミックス焼結体からなる。また、第1の被接合体および第2の被接合体とが同一のセラミックス焼結体であることも好ましい。 According to the preferable aspect of this invention, a 2nd to-be-joined body consists of a ceramic sintered compact containing metal silicon. Moreover, it is also preferable that the first bonded body and the second bonded body are the same ceramic sintered body.
また本発明の他の実施形態によれば、セラミックス接合体の製造方法であって、接合面を有し、金属ケイ素を含むセラミックス焼結体からなる第1の被接合体を準備する工程と、接合面を有し、セラミックス焼結体からなる第2の被接合体を準備する工程と、第1の被接合体の接合面と第2の被接合体の接合面との間に熱可塑性樹脂薄膜を配置して第1の被接合体と第2の被接合体とを重ね合わせる工程と、前記熱可塑性樹脂薄膜を介して重ね合わされた第1の被接合体と第2の被接合体とを、接合面同士が押圧された状態を維持しつつ、不活性雰囲気下において所定温度で熱処理する工程と、を具備してなることを特徴とする。本発明のセラミックス接合体の製造方法によれば、熱可塑性樹脂薄膜の厚さによって初期の接合層厚さを制御することができるため、塗布ムラのような厚さのばらつきを生じることなく、均一且つ所望の接合層厚さに制御することが可能となる。 According to another embodiment of the present invention, there is provided a method for manufacturing a ceramic joined body, the step of preparing a first joined body made of a ceramic sintered body having a joint surface and containing metallic silicon, A thermoplastic resin between the step of preparing a second bonded body having a bonded surface and made of a ceramic sintered body, and the bonded surface of the first bonded body and the bonded surface of the second bonded body A step of disposing a thin film and superimposing the first and second objects to be joined; and a first and second object to be joined that are superposed via the thermoplastic resin thin film; And a step of heat-treating at a predetermined temperature in an inert atmosphere while maintaining a state where the bonding surfaces are pressed with each other. According to the method for manufacturing a ceramic joined body of the present invention, since the initial joining layer thickness can be controlled by the thickness of the thermoplastic resin thin film, it is uniform without causing thickness variation such as coating unevenness. And it becomes possible to control to desired joining layer thickness.
本発明の好ましい態様によれば、前記所定温度は、前記第1の被接合体に含まれた状態における金属ケイ素の融点よりも高く、且つ、前記第1の被接合体に含まれた状態における金属ケイ素の蒸発温度よりも低い温度である。
かかる温度であれば、熱処理中において第1の被接合体に含まれた金属ケイ素が適当な粘度を有する液体となるため、炭化した熱可塑性樹脂薄膜への金属ケイ素の移動が促進され、接合面全体に渡る接合層の形成を短時間で行うことができる。
According to a preferred aspect of the present invention, the predetermined temperature is higher than the melting point of metal silicon in the state included in the first bonded body and in the state included in the first bonded body. The temperature is lower than the evaporation temperature of metallic silicon.
If it is such temperature, since the metal silicon contained in the first bonded body during the heat treatment becomes a liquid having an appropriate viscosity, the movement of the metal silicon to the carbonized thermoplastic resin thin film is promoted, and the bonding surface The entire bonding layer can be formed in a short time.
金属ケイ素の融点や蒸発温度は、一般に、金属ケイ素の状態によって異なる。即ち、セラミックス焼結体に含まれた状態における金属ケイ素の融点は、単体の結晶である状態における融点よりも一般に低くなる。また、セラミックス焼結体の種類によっても異なるものとなる。
このため、被接合体であるセラミックス焼結体の種類、及び金属ケイ素の含浸状態に応じて、適切な熱処理温度を予め実験により測定しておき、当該温度にて熱処理を行うことで、接合層を短時間で形成させることができる。
In general, the melting point and evaporation temperature of metallic silicon vary depending on the state of metallic silicon. That is, the melting point of metallic silicon in the state contained in the ceramic sintered body is generally lower than the melting point in the state of being a single crystal. In addition, it varies depending on the type of ceramic sintered body.
For this reason, according to the kind of ceramic sintered body to be joined and the impregnation state of metal silicon, an appropriate heat treatment temperature is measured in advance by experiment, and the heat treatment is performed at the temperature, whereby the joining layer is obtained. Can be formed in a short time.
本発明の好ましい態様によれば、前記熱可塑性樹脂薄膜がセロファンからなる薄膜である。セロファンは熱処理によりち密質な炭素素材となることから、外部から金属ケイ素を添加することなく、被接合体から浸透してくる程度の微量な金属ケイ素のみにより接合層を形成することができる。 According to a preferred aspect of the present invention, the thermoplastic resin thin film is a thin film made of cellophane. Since cellophane becomes a dense carbon material by heat treatment, it is possible to form a bonding layer with only a small amount of metal silicon that penetrates from the object to be bonded without adding metal silicon from the outside.
本発明によれば、簡単な接合手法によって得られる高強度に接合されたセラミックス接合体、およびその製造方法を提供することが可能になる。 ADVANTAGE OF THE INVENTION According to this invention, it becomes possible to provide the ceramic joined body joined by high intensity | strength obtained by a simple joining method, and its manufacturing method.
以下に本発明のセラミックス接合体およびその製造方法について詳細に説明する。
本発明のセラミックス接合体は、金属ケイ素を含むセラミックス焼結体からなる第1の被接合体と、セラミックス焼結体からなる第2の被接合体と、が接合層を介して接合され、接合層は金属ケイ素を主成分とすることを特徴とするセラミックス接合体である。また、本発明のセラミックス接合体の製造方法は、接合面を有し、金属ケイ素を含むセラミックス焼結体からなる第1の被接合体を準備する工程と、接合面を有し、セラミックス焼結体からなる第2の被接合体を準備する工程と、第1の被接合体の接合面と第2の被接合体の接合面との間に熱可塑性樹脂薄膜を配置して第1の被接合体と第2の被接合体とを重ね合わせる工程と、熱可塑性樹脂薄膜を介して重ね合わされた第1の被接合体と第2の被接合体とを、接合面同士が押圧された状態を維持しつつ、不活性雰囲気下において所定温度で熱処理する工程と、を具備してなるセラミックス接合体の製造方法である。
The ceramic joined body of the present invention and the manufacturing method thereof will be described in detail below.
In the ceramic joined body of the present invention, a first joined body made of a ceramic sintered body containing metal silicon and a second joined body made of a ceramic sintered body are joined via a joining layer, and joined. The layer is a ceramic joined body characterized by containing metal silicon as a main component. In addition, the method for manufacturing a ceramic joined body of the present invention includes a step of preparing a first joined body having a joint surface and made of a ceramic sintered body containing metal silicon, and a ceramic sintered body having a joint surface. A second to-be-joined body comprising a body, and a thermoplastic resin thin film disposed between the joining surface of the first to-be-joined body and the joining surface of the second to-be-joined body. The state in which the bonding surfaces are pressed between the step of superimposing the bonded body and the second bonded body, and the first bonded body and the second bonded body stacked via the thermoplastic resin thin film. And a step of heat-treating at a predetermined temperature under an inert atmosphere while maintaining the above.
(被接合体)
セラミックス接合体を構成する被接合体のうち第1の被接合体には、金属ケイ素を含有させることができる種々のセラミックスを用いることが可能である。中でも、金属ケイ素を含有する炭化ケイ素セラミックス、金属ケイ素を含有する炭化ホウ素セラミックス、金属ケイ素を含有し炭化ケイ素および炭化ホウ素を含むセラミックス複合体などがあげられる。第2の被接合体には、前記した第1の被接合体に用いることができるセラミックスのほかに、金属ケイ素を含有しない種々のセラミックスも用いることが可能である。
接合体を介して接合される2つの被接合体は、少なくとも一方が金属シリコンを含有するセラミックスであればいいが、2つの被接合体の双方が金属シリコンを含有するセラミックスである場合は、それぞれの被接合体と接合層との密着性が高くなるのでより好ましい。
(Substrate to be joined)
Among the objects to be bonded constituting the ceramic bonded body, various ceramics that can contain metallic silicon can be used for the first bonded object. Among these, silicon carbide ceramics containing metal silicon, boron carbide ceramics containing metal silicon, ceramic composites containing metal silicon and containing silicon carbide and boron carbide, and the like can be given. In addition to the ceramics that can be used for the first bonded body, various ceramics that do not contain metallic silicon can be used for the second bonded body.
The two objects to be bonded to each other through the bonded body may be ceramics containing at least one of metal silicon, but when both of the two objects to be bonded are ceramics containing metal silicon, This is more preferable because the adhesion between the object to be bonded and the bonding layer is increased.
(接合層)
接合層は、第1の被接合体と第2の被接合体との間に介在し両者を接合する層である。熱処理工程において、第1の被接合体と第2の被接合体との間に介在していた熱可塑性樹脂薄膜が炭化した後、そこへいずれかの被接合体から金属ケイ素が浸透し炭素と反応することで、金属ケイ素を含有する炭化ケイ素の層となる。
(Bonding layer)
The bonding layer is a layer that is interposed between the first bonded body and the second bonded body and bonds the both. In the heat treatment step, after the thermoplastic resin thin film interposed between the first bonded body and the second bonded body is carbonized, metal silicon penetrates from any of the bonded bodies into the carbon. By reacting, it becomes a layer of silicon carbide containing metallic silicon.
(熱可塑性樹脂薄膜)
熱可塑性樹脂薄膜としては、炭素を含む種々の樹脂を用いることが可能である。特に、加熱後に収縮し、ち密質な連続した炭素となるものが好ましく、フェノール樹脂、ポリイミド樹脂、ポリアセタール樹脂、ポリカーボネート樹脂、ポリスルホン樹脂、ポリフッ化ビニルデン樹脂、エポキシ系樹脂、ポリエステル系樹脂、ポリブチルアクリレート樹脂、酢酸ビニル樹脂、ポリ塩化ビニル樹脂などの熱可塑性樹脂薄膜があげられる。また、接合層の厚みを調整しやすいという点で薄膜状に成形しやすいものが好ましく、例えば、セロファン樹脂やポリイミド樹脂を好適に用いることができる。
また、熱可塑性樹脂薄膜は熱処理後に1〜200μmに熱収縮するものが接合強度を高くする点で好ましく、1〜50μmに収縮するものがさらに好ましい。
(Thermoplastic resin thin film)
As the thermoplastic resin thin film, various resins containing carbon can be used. In particular, those that shrink after heating and become dense continuous carbon are preferred, such as phenol resin, polyimide resin, polyacetal resin, polycarbonate resin, polysulfone resin, polyvinylidene fluoride resin, epoxy resin, polyester resin, polybutyl acrylate. Examples thereof include thermoplastic resin thin films such as resins, vinyl acetate resins, and polyvinyl chloride resins. Moreover, the thing which is easy to shape | mold into a thin film form from the point that it is easy to adjust the thickness of a joining layer is preferable, for example, a cellophane resin and a polyimide resin can be used suitably.
The thermoplastic resin thin film is preferably heat-shrinkable to 1 to 200 μm after heat treatment from the viewpoint of increasing the bonding strength, and more preferably 1 to 50 μm.
(接合面)
接合時、突き合わせる面の形状に制限はなく、平面突き合わせ、嵌め合わせなどの方法が可能である。熱可塑性樹脂薄膜を介する接合であることから平面突き合わせが簡便で好ましい。
(Joint surface)
At the time of joining, the shape of the surfaces to be abutted is not limited, and methods such as plane abutment and fitting are possible. Since it is joining via a thermoplastic resin thin film, plane matching is simple and preferable.
(接合面粗度)
接合面の面粗度に関しては制限がないが、熱可塑性樹脂薄膜の熱収縮によって隙間ができない程度が好ましく、Ra=3μm以下が好ましく、より好ましくはRa=0.5μm以下が良い。
(Roughness of joint surface)
Although there is no restriction | limiting regarding the surface roughness of a joint surface, The grade which cannot make a clearance gap by the thermal contraction of a thermoplastic resin thin film is preferable, Ra = 3 micrometer or less is preferable, More preferably, Ra = 0.5 micrometer or less is good.
(炭化処理工程)
第1の被接合体の接合面と第2の被接合体の接合面との間に熱可塑性樹脂薄膜を配置して第1の被接合体と第2の被接合体とを重ね合わせる工程と、熱可塑性樹脂薄膜を介して重ね合わされた第1の被接合体と第2の被接合体とを、接合面同士が押圧された状態を維持しつつ、不活性雰囲気下において所定温度で熱処理する工程と、の間に、接合加熱時に接合層となる熱可塑性樹脂薄膜を炭化する工程を有することが好ましい。熱可塑性樹脂薄膜を炭化する工程における熱処理の温度は、400〜900℃の範囲において、用いる熱可塑性樹脂薄膜に応じて適宜選定できる。保持時間は熱可塑性樹脂薄膜の種類、大きさに応じて適宜選定することができる。
(Carbonization process)
Disposing a thermoplastic resin thin film between the bonding surface of the first bonded body and the bonding surface of the second bonded body and superimposing the first bonded body and the second bonded body; Then, the first and second objects to be joined that are superposed via the thermoplastic resin thin film are heat-treated at a predetermined temperature in an inert atmosphere while maintaining the state where the joining surfaces are pressed with each other. It is preferable to have a step of carbonizing the thermoplastic resin thin film that becomes the bonding layer during bonding heating. The temperature of the heat treatment in the step of carbonizing the thermoplastic resin thin film can be appropriately selected in the range of 400 to 900 ° C. according to the thermoplastic resin thin film to be used. The holding time can be appropriately selected according to the type and size of the thermoplastic resin thin film.
(接合処理工程)
接合処理に要する温度は、第1の被接合体に含まれた状態における金属ケイ素の融点よりも高く、且つ、前記第1の被接合体に含まれた状態における金属ケイ素の蒸発温度よりも低い温度範囲で適宜選定できる。本発明の被接合体は接合処理の際にすでに金属ケイ素を含有する被接合体であり、被接合体の金属ケイ素の移動により金属ケイ素を主成分とする接合層を形成する。本実施形態においては、第1の非接合体に含まれる金属ケイ素は1100℃以上の温度で融解することが分かっており、且つ、1700℃を超えると金属ケイ素の蒸発が無視できなくなる。このため、熱処理の温度としては1200〜1500℃が好ましく、金属ケイ素単体の状態における融点(1412℃)よりも低い温度で熱処理できる1300〜1400℃がさらに好ましい。
接合処理工程においては、熱処理の行う際の圧力を0.1〜200MPaの範囲で適宜選定できる。少なくとも熱可塑性樹脂薄膜の収縮変形により被接合体が剥離しない程度の圧力が必要であり、被接合体同士を重ね合わせた成形体全体を加圧しても良いし、接合面が押圧されるようにジグでクランプして熱処理を行ってもよい。
接合処理工程は適宜の不活性雰囲気下で行われればよく、真空、アルゴン雰囲気もしくは窒素雰囲気などが挙げられる。好ましくはアルゴン雰囲気である。なお、アルゴンと窒素の混合ガスでも接合可能である。
(Joining process)
The temperature required for the bonding process is higher than the melting point of metallic silicon in the state included in the first bonded body and lower than the evaporation temperature of metallic silicon in the state included in the first bonded body. It can be selected appropriately within the temperature range. The to-be-joined body of this invention is a to-be-joined body which already contains metallic silicon in the joining process, and forms the joining layer which has metallic silicon as a main component by the movement of the metallic silicon of a to-be-joined body. In the present embodiment, it is known that the metal silicon contained in the first non-bonded body melts at a temperature of 1100 ° C. or higher, and the evaporation of the metal silicon cannot be ignored when the temperature exceeds 1700 ° C. For this reason, the temperature of the heat treatment is preferably 1200 to 1500 ° C., more preferably 1300 to 1400 ° C. at which the heat treatment can be performed at a temperature lower than the melting point (1412 ° C.) in the state of metal silicon alone.
In the joining treatment step, the pressure during the heat treatment can be appropriately selected within the range of 0.1 to 200 MPa. At least a pressure that does not cause the object to be peeled off due to shrinkage deformation of the thermoplastic resin thin film is required, and the entire molded body in which the objects to be joined are overlapped may be pressed, or the joint surface may be pressed. Heat treatment may be performed by clamping with a jig.
The bonding process may be performed under an appropriate inert atmosphere, and examples thereof include a vacuum, an argon atmosphere, and a nitrogen atmosphere. An argon atmosphere is preferred. Note that bonding is possible even with a mixed gas of argon and nitrogen.
(実施例1)
第1の被接合体および第2の被接合体として金属ケイ素および炭化硼素および炭化ケイ素を含有するセラミックス焼成体を準備した。熱可塑性樹脂薄膜として、厚み35μmのセロファンを準備した。
金属ケイ素および炭化硼素および炭化ケイ素を含有するセラミックス焼成体は以下の方法により作製した。
平均粒径が0.6μmの炭化ケイ素粉末30重量部と平均粒径が25μmの炭化硼素粉末70重量部、平均粒径が55nmのカーボンブラック粉末10重量部を炭化ケイ素粉末、炭化硼素粉末、カーボンブラック粉末に対して0.1〜1重量部の分散剤を添加した純水中に入れ分散させ、アンモニア水等でpHを8〜9.5に調整して500CP未満の低粘度のスラリーを作製した。このスラリーをポットミル等で数時間混合した後バインダーを炭化ケイ素粉末、炭化硼素粉末、カーボン粉末に対して1〜2重量部添加し混合、その後脱泡し石膏板の上に内径80mmのアクリルパイプを置きスラリーを鋳込み、厚み10mm程度の成形体を作製した。成形体は自然乾燥、100〜150℃の乾燥の後、1×10−4〜1×10−3torrの減圧下において温度600℃で2h保持し脱脂を行い、温度1700℃で1h保持することで仮焼を行う。仮焼を行った後、温度1500℃に加熱し30min保持し、成形体中に溶融したシリコンを含浸させることにより反応焼結体を製造した。
得られた金属ケイ素および炭化硼素および炭化ケイ素を含有するセラミックス焼成体を20mm角、厚み6mmに切り出し、接合面がRa=0.2μmとなるように研削加工し、2つの被接合体を作製した。
2つの被接合体の接合面に厚み35μmのセロハンを挟み込み、炭素ジグで固定し、20x40x6mmの形状とした。
固定した試料を炭素炉で1気圧のアルゴン雰囲気中1400℃で熱処理を行った。1400℃まで昇温(昇温速度は300度/1時間とした)する途中では600℃で1時間保持し、セロファンを炭化させた。
接合層を含むセラミックス複合体の電子顕微鏡写真を図1に示す。被接合体1同士が金属ケイ素を主成分とする接合層2を介して接合され、被接合体1が炭化硼素部3および炭化ケイ素部4からなるセラミックス接合体であることが観察された。得られた接合体の接合層厚みは約16μmであった。
加熱後の試料を3x4x40mmのテストピースに加工し、3点曲げ(JISR1601)を行った結果、接合体は接合面で破断し、130MPaの強度を得た。
Example 1
Ceramic fired bodies containing metal silicon, boron carbide, and silicon carbide were prepared as the first and second bonded bodies. Cellophane having a thickness of 35 μm was prepared as a thermoplastic resin thin film.
A ceramic fired body containing metallic silicon, boron carbide and silicon carbide was produced by the following method.
30 parts by weight of silicon carbide powder having an average particle diameter of 0.6 μm, 70 parts by weight of boron carbide powder having an average particle diameter of 25 μm, and 10 parts by weight of carbon black powder having an average particle diameter of 55 nm are obtained by silicon carbide powder, boron carbide powder, carbon Disperse in pure water with 0.1 to 1 part by weight of dispersant added to black powder, adjust pH to 8 to 9.5 with aqueous ammonia, etc. to produce low viscosity slurry of less than 500 CP did. After mixing this slurry with a pot mill or the like for several hours, add 1 to 2 parts by weight of binder to silicon carbide powder, boron carbide powder, or carbon powder, mix and defoam, and then place an acrylic pipe with an inner diameter of 80 mm on the gypsum plate. The placed slurry was cast to produce a molded body having a thickness of about 10 mm. The molded body is naturally dried, dried at 100 to 150 ° C., degreased by holding at a temperature of 600 ° C. for 2 hours under a reduced pressure of 1 × 10 −4 to 1 × 10 −3 torr, and held at a temperature of 1700 ° C. for 1 hour. Perform calcination. After calcination, the reaction sintered body was manufactured by heating to a temperature of 1500 ° C. and holding for 30 minutes, and impregnating molten silicon into the molded body.
The obtained ceramic fired body containing metal silicon, boron carbide and silicon carbide was cut into a 20 mm square and a thickness of 6 mm, and ground so that the joint surface was Ra = 0.2 μm, and two joined bodies were produced. .
Cellophane having a thickness of 35 μm was sandwiched between the joining surfaces of the two objects to be joined, and fixed with a carbon jig to form a shape of 20 × 40 × 6 mm.
The fixed sample was heat-treated at 1400 ° C. in an argon atmosphere of 1 atm in a carbon furnace. While the temperature was raised to 1400 ° C. (temperature raising rate was 300 ° C./1 hour), the temperature was maintained at 600 ° C. for 1 hour to carbonize the cellophane.
An electron micrograph of the ceramic composite including the bonding layer is shown in FIG. It was observed that the objects to be bonded 1 were bonded to each other via a bonding layer 2 containing metal silicon as a main component, and the objects to be bonded 1 were ceramic bonded bodies composed of a boron carbide portion 3 and a silicon carbide portion 4. The joined layer thickness of the obtained joined body was about 16 μm.
The heated sample was processed into a 3 × 4 × 40 mm test piece and subjected to three-point bending (JIS R1601). As a result, the joined body was broken at the joining surface, and a strength of 130 MPa was obtained.
(実施例2)
第1の被接合体および第2の被接合体として金属ケイ素および炭化硼素および炭化ケイ素を含有するセラミックス焼成体を準備した。熱可塑性樹脂薄膜として、厚み35μmのセロファンを準備した。
金属ケイ素および炭化硼素および炭化ケイ素を含有するセラミックス焼成体は実施例1と同様の方法により作製し、接合用試料も同様の形状を準備した。
2つの被接合体の接合面に厚み35μmのセロハンを挟み込み、炭素ジグで固定し、20x40x6mmの形状とした。
固定した試料を炭素炉で1気圧のアルゴン雰囲気中1300℃で熱処理を行った。1300℃まで昇温(昇温速度は300度/1時間とした)する途中では600℃で1時間保持し、セロファンを炭化させた。
(Example 2)
Ceramic fired bodies containing metal silicon, boron carbide, and silicon carbide were prepared as the first and second bonded bodies. Cellophane having a thickness of 35 μm was prepared as a thermoplastic resin thin film.
A fired ceramic body containing metal silicon, boron carbide and silicon carbide was produced by the same method as in Example 1, and a joining sample was prepared in the same shape.
Cellophane having a thickness of 35 μm was sandwiched between the joining surfaces of the two objects to be joined, and fixed with a carbon jig to form a shape of 20 × 40 × 6 mm.
The fixed sample was heat-treated at 1300 ° C. in an argon atmosphere of 1 atm in a carbon furnace. While the temperature was raised to 1300 ° C. (temperature raising rate was 300 ° C./1 hour), the temperature was maintained at 600 ° C. for 1 hour to carbonize the cellophane.
(実施例3)
第1の被接合体および第2の被接合体として金属ケイ素および炭化硼素および炭化ケイ素を含有するセラミックス焼成体を準備した。熱可塑性樹脂薄膜として、厚み35μmのセロファンを準備した。
金属ケイ素および炭化硼素および炭化ケイ素を含有するセラミックス焼成体は実施例1と同様の方法により作製し、接合用試料も同様の形状を準備した。
2つの被接合体の接合面に厚み35μmのセロハンを挟み込み、炭素ジグで固定し、20x40x6mmの形状とした。
固定した試料を炭素炉で1気圧のアルゴン雰囲気中1500℃で熱処理を行った。1500℃まで昇温(昇温速度は300度/1時間とした)する途中では600℃で1時間保持し、セロファンを炭化させた。
(Example 3)
Ceramic fired bodies containing metal silicon, boron carbide, and silicon carbide were prepared as the first and second bonded bodies. Cellophane having a thickness of 35 μm was prepared as a thermoplastic resin thin film.
A fired ceramic body containing metal silicon, boron carbide and silicon carbide was produced by the same method as in Example 1, and a joining sample was prepared in the same shape.
Cellophane having a thickness of 35 μm was sandwiched between the joining surfaces of the two objects to be joined, and fixed with a carbon jig to form a shape of 20 × 40 × 6 mm.
The fixed sample was heat-treated at 1500 ° C. in an argon atmosphere of 1 atm in a carbon furnace. While the temperature was raised to 1500 ° C. (temperature raising rate was 300 ° C./1 hour), the temperature was maintained at 600 ° C. for 1 hour to carbonize the cellophane.
(実施例4)
第1の被接合体および第2の被接合体として金属ケイ素および炭化硼素および炭化ケイ素を含有するセラミックス焼成体を準備した。熱可塑性樹脂薄膜として、厚み35μmのセロファンを準備した。
金属ケイ素および炭化硼素および炭化ケイ素を含有するセラミックス焼成体は実施例1と同様の方法により作製し、接合用試料も同様の形状を準備した。
2つの被接合体の接合面に厚み35μmのセロハンを挟み込み、炭素ジグで固定し、20x40x6mmの形状とした。
固定した試料を炭素炉で1気圧のアルゴン雰囲気中1600℃で熱処理を行った。1600℃まで昇温(昇温速度は300度/1時間とした)する途中では600℃で1時間保持し、セロファンを炭化させた。
Example 4
Ceramic fired bodies containing metal silicon, boron carbide, and silicon carbide were prepared as the first and second bonded bodies. Cellophane having a thickness of 35 μm was prepared as a thermoplastic resin thin film.
A fired ceramic body containing metal silicon, boron carbide and silicon carbide was produced by the same method as in Example 1, and a joining sample was prepared in the same shape.
Cellophane having a thickness of 35 μm was sandwiched between the joining surfaces of the two objects to be joined, and fixed with a carbon jig to form a shape of 20 × 40 × 6 mm.
The fixed sample was heat-treated at 1600 ° C. in an argon atmosphere of 1 atm in a carbon furnace. While the temperature was raised to 1600 ° C. (temperature raising rate was 300 ° C./1 hour), the temperature was maintained at 600 ° C. for 1 hour to carbonize the cellophane.
(実施例5)
第1の被接合体および第2の被接合体として金属ケイ素および炭化硼素および炭化ケイ素を含有するセラミックス焼成体を準備した。熱可塑性樹脂薄膜として、厚み35μmのセロファンを準備した。
金属ケイ素および炭化硼素および炭化ケイ素を含有するセラミックス焼成体は実施例1と同様の方法により作製し、接合用試料も同様の形状を準備した。
2つの被接合体の接合面に厚み35μmのセロハンを挟み込み、炭素ジグで固定し、20x40x6mmの形状とした。
固定した試料を炭素炉で1気圧の窒素雰囲気中1400℃で熱処理を行った。1400℃まで昇温(昇温速度は300度/1時間とした)する途中では600℃で1時間保持し、セロファンを炭化させた。
(Example 5)
Ceramic fired bodies containing metal silicon, boron carbide, and silicon carbide were prepared as the first and second bonded bodies. Cellophane having a thickness of 35 μm was prepared as a thermoplastic resin thin film.
A fired ceramic body containing metal silicon, boron carbide and silicon carbide was produced by the same method as in Example 1, and a joining sample was prepared in the same shape.
Cellophane having a thickness of 35 μm was sandwiched between the joining surfaces of the two objects to be joined, and fixed with a carbon jig to form a shape of 20 × 40 × 6 mm.
The fixed sample was heat-treated at 1400 ° C. in a nitrogen atmosphere of 1 atm in a carbon furnace. While the temperature was raised to 1400 ° C. (temperature raising rate was 300 ° C./1 hour), the temperature was maintained at 600 ° C. for 1 hour to carbonize the cellophane.
(実施例6)
第1の被接合体および第2の被接合体として金属ケイ素および炭化硼素および炭化ケイ素を含有するセラミックス焼成体を準備した。熱可塑性樹脂薄膜として、厚み35μmのセロファンを準備した。
金属ケイ素および炭化硼素および炭化ケイ素を含有するセラミックス焼成体は実施例1と同様の方法により作製し、接合用試料も同様の形状を準備した。
2つの被接合体の接合面に厚み35μmのセロハンを挟み込み、炭素ジグで固定し、20x40x6mmの形状とした。
固定した試料を炭素炉で真空中1300℃で熱処理を行った。1300℃まで昇温(昇温速度は300度/1時間とした)する途中では600℃で1時間保持し、セロファンを炭化させた。
(Example 6)
Ceramic fired bodies containing metal silicon, boron carbide, and silicon carbide were prepared as the first and second bonded bodies. Cellophane having a thickness of 35 μm was prepared as a thermoplastic resin thin film.
A fired ceramic body containing metal silicon, boron carbide and silicon carbide was produced by the same method as in Example 1, and a joining sample was prepared in the same shape.
Cellophane having a thickness of 35 μm was sandwiched between the joining surfaces of the two objects to be joined, and fixed with a carbon jig to form a shape of 20 × 40 × 6 mm.
The fixed sample was heat-treated at 1300 ° C. in a vacuum in a carbon furnace. While the temperature was raised to 1300 ° C. (temperature raising rate was 300 ° C./1 hour), the temperature was maintained at 600 ° C. for 1 hour to carbonize the cellophane.
(実施例7)
第1の被接合体および第2の被接合体として金属ケイ素および炭化硼素および炭化ケイ素を含有するセラミックス焼成体を準備した。熱可塑性樹脂薄膜として、厚み35μmのセロファンを準備した。
金属ケイ素および炭化硼素および炭化ケイ素を含有するセラミックス焼成体は実施例1と同様の方法により作製し、接合用試料も同様の形状を準備した。
2つの被接合体の接合面に厚み35μmのセロハンを挟み込み、炭素ジグで固定し、20x40x6mmの形状とした。
固定した試料を炭素炉で真空中1400℃で熱処理を行った。1400℃まで昇温(昇温速度は300度/1時間とした)する途中では600℃で1時間保持し、セロファンを炭化させた。
(Example 7)
Ceramic fired bodies containing metal silicon, boron carbide, and silicon carbide were prepared as the first and second bonded bodies. Cellophane having a thickness of 35 μm was prepared as a thermoplastic resin thin film.
A fired ceramic body containing metal silicon, boron carbide and silicon carbide was produced by the same method as in Example 1, and a joining sample was prepared in the same shape.
Cellophane having a thickness of 35 μm was sandwiched between the joining surfaces of the two objects to be joined, and fixed with a carbon jig to form a shape of 20 × 40 × 6 mm.
The fixed sample was heat-treated at 1400 ° C. in a vacuum in a carbon furnace. While the temperature was raised to 1400 ° C. (temperature raising rate was 300 ° C./1 hour), the temperature was maintained at 600 ° C. for 1 hour to carbonize the cellophane.
(実施例8)
第1の被接合体および第2の被接合体として金属ケイ素および炭化硼素および炭化ケイ素を含有するセラミックス焼成体を準備した。熱可塑性樹脂薄膜として、厚み20μmのセロファンを準備した。
金属ケイ素および炭化硼素および炭化ケイ素を含有するセラミックス焼成体は実施例1と同様の方法により作製し、接合用試料も同様の形状を準備した。
2つの被接合体の接合面に厚み20μmのセロハンを挟み込み、炭素ジグで固定し、20x40x6mmの形状とした。
固定した試料を炭素炉で1気圧のアルゴン雰囲気中1300℃で熱処理を行った。1300℃まで昇温(昇温速度は300度/1時間とした)する途中では600℃で1時間保持し、セロファンを炭化させた。
(Example 8)
Ceramic fired bodies containing metal silicon, boron carbide, and silicon carbide were prepared as the first and second bonded bodies. As a thermoplastic resin thin film, cellophane having a thickness of 20 μm was prepared.
A fired ceramic body containing metal silicon, boron carbide and silicon carbide was produced by the same method as in Example 1, and a joining sample was prepared in the same shape.
A cellophane having a thickness of 20 μm was sandwiched between the joining surfaces of the two objects to be joined, and fixed with a carbon jig to form a shape of 20 × 40 × 6 mm.
The fixed sample was heat-treated at 1300 ° C. in an argon atmosphere of 1 atm in a carbon furnace. While the temperature was raised to 1300 ° C. (temperature raising rate was 300 ° C./1 hour), the temperature was maintained at 600 ° C. for 1 hour to carbonize the cellophane.
(実施例9)
第1の被接合体および第2の被接合体として金属ケイ素および炭化硼素および炭化ケイ素を含有するセラミックス焼成体を準備した。熱可塑性樹脂薄膜として、厚み20μmのセロファンを準備した。
金属ケイ素および炭化硼素および炭化ケイ素を含有するセラミックス焼成体は実施例1と同様の方法により作製し、接合用試料も同様の形状を準備した。
2つの被接合体の接合面に厚み20μmのセロハンを挟み込み、炭素ジグで固定し、20x40x6mmの形状とした。
固定した試料を炭素炉で1気圧のアルゴン雰囲気中1400℃で熱処理を行った。1400℃まで昇温(昇温速度は300度/1時間とした)する途中では600℃で1時間保持し、セロファンを炭化させた。
Example 9
Ceramic fired bodies containing metal silicon, boron carbide, and silicon carbide were prepared as the first and second bonded bodies. As a thermoplastic resin thin film, cellophane having a thickness of 20 μm was prepared.
A fired ceramic body containing metal silicon, boron carbide and silicon carbide was produced by the same method as in Example 1, and a joining sample was prepared in the same shape.
A cellophane having a thickness of 20 μm was sandwiched between the joining surfaces of the two objects to be joined, and fixed with a carbon jig to form a shape of 20 × 40 × 6 mm.
The fixed sample was heat-treated at 1400 ° C. in an argon atmosphere of 1 atm in a carbon furnace. While the temperature was raised to 1400 ° C. (temperature raising rate was 300 ° C./1 hour), the temperature was maintained at 600 ° C. for 1 hour to carbonize the cellophane.
(実施例10)
第1の被接合体および第2の被接合体として金属ケイ素および炭化硼素および炭化ケイ素を含有するセラミックス焼成体を準備した。熱可塑性樹脂薄膜として、厚み20μmのセロファンを準備した。
金属ケイ素および炭化硼素および炭化ケイ素を含有するセラミックス焼成体は実施例1と同様の方法により作製し、接合用試料も同様の形状を準備した。
2つの被接合体の接合面に厚み20μmのセロハンを挟み込み、炭素ジグで固定し、20x40x6mmの形状とした。
固定した試料を炭素炉で1気圧のアルゴン雰囲気中1500℃で熱処理を行った。1500℃まで昇温(昇温速度は300度/1時間とした)する途中では600℃で1時間保持し、セロファンを炭化させた。
(Example 10)
Ceramic fired bodies containing metal silicon, boron carbide, and silicon carbide were prepared as the first and second bonded bodies. As a thermoplastic resin thin film, cellophane having a thickness of 20 μm was prepared.
A fired ceramic body containing metal silicon, boron carbide and silicon carbide was produced by the same method as in Example 1, and a joining sample was prepared in the same shape.
A cellophane having a thickness of 20 μm was sandwiched between the joining surfaces of the two objects to be joined, and fixed with a carbon jig to form a shape of 20 × 40 × 6 mm.
The fixed sample was heat-treated at 1500 ° C. in an argon atmosphere of 1 atm in a carbon furnace. While the temperature was raised to 1500 ° C. (temperature raising rate was 300 ° C./1 hour), the temperature was maintained at 600 ° C. for 1 hour to carbonize the cellophane.
(実施例11)
第1の被接合体および第2の被接合体として金属ケイ素および炭化硼素および炭化ケイ素を含有するセラミックス焼成体を準備した。熱可塑性樹脂薄膜として、厚み20μmのセロファンを準備した。
金属ケイ素および炭化硼素および炭化ケイ素を含有するセラミックス焼成体は実施例1と同様の方法により作製し、接合用試料も同様の形状を準備した。
2つの被接合体の接合面に厚み20μmのセロハンを挟み込み、炭素ジグで固定し、20x40x6mmの形状とした。
固定した試料を炭素炉で1気圧のアルゴン雰囲気中1600℃で熱処理を行った。1600℃まで昇温(昇温速度は300度/1時間とした)する途中では600℃で1時間保持し、セロファンを炭化させた。
(Example 11)
Ceramic fired bodies containing metal silicon, boron carbide, and silicon carbide were prepared as the first and second bonded bodies. As a thermoplastic resin thin film, cellophane having a thickness of 20 μm was prepared.
A fired ceramic body containing metal silicon, boron carbide and silicon carbide was produced by the same method as in Example 1, and a joining sample was prepared in the same shape.
A cellophane having a thickness of 20 μm was sandwiched between the joining surfaces of the two objects to be joined, and fixed with a carbon jig to form a shape of 20 × 40 × 6 mm.
The fixed sample was heat-treated at 1600 ° C. in an argon atmosphere of 1 atm in a carbon furnace. While the temperature was raised to 1600 ° C. (temperature raising rate was 300 ° C./1 hour), the temperature was maintained at 600 ° C. for 1 hour to carbonize the cellophane.
(実施例12)
第1の被接合体および第2の被接合体として金属ケイ素および炭化硼素および炭化ケイ素を含有するセラミックス焼成体を準備した。熱可塑性樹脂薄膜として、厚み20μmのセロファンを準備した。
金属ケイ素および炭化硼素および炭化ケイ素を含有するセラミックス焼成体は実施例1と同様の方法により作製し、接合用試料も同様の形状を準備した。
2つの被接合体の接合面に厚み20μmのセロハンを挟み込み、炭素ジグで固定し、20x40x6mmの形状とした。
固定した試料を炭素炉で1気圧の窒素雰囲気中1500℃で熱処理を行った。1500℃まで昇温(昇温速度は300度/1時間とした)する途中では600℃で1時間保持し、セロファンを炭化させた。
(Example 12)
Ceramic fired bodies containing metal silicon, boron carbide, and silicon carbide were prepared as the first and second bonded bodies. As a thermoplastic resin thin film, cellophane having a thickness of 20 μm was prepared.
A fired ceramic body containing metal silicon, boron carbide and silicon carbide was produced by the same method as in Example 1, and a joining sample was prepared in the same shape.
A cellophane having a thickness of 20 μm was sandwiched between the joining surfaces of the two objects to be joined, and fixed with a carbon jig to form a shape of 20 × 40 × 6 mm.
The fixed sample was heat-treated at 1500 ° C. in a nitrogen atmosphere of 1 atm in a carbon furnace. While the temperature was raised to 1500 ° C. (temperature raising rate was 300 ° C./1 hour), the temperature was maintained at 600 ° C. for 1 hour to carbonize the cellophane.
(実施例13)
第1の被接合体および第2の被接合体として金属ケイ素および炭化硼素および炭化ケイ素を含有するセラミックス焼成体を準備した。熱可塑性樹脂薄膜として、厚み20μmのセロファンを準備した。
金属ケイ素および炭化硼素および炭化ケイ素を含有するセラミックス焼成体は実施例1と同様の方法により作製し、接合用試料も同様の形状を準備した。
2つの被接合体の接合面に厚み20μmのセロハンを挟み込み、炭素ジグで固定し、20x40x6mmの形状とした。
固定した試料を炭素炉で真空中1300℃で熱処理を行った。1300℃まで昇温(昇温速度は300度/1時間とした)する途中では600℃で1時間保持し、セロファンを炭化させた。
(Example 13)
Ceramic fired bodies containing metal silicon, boron carbide, and silicon carbide were prepared as the first and second bonded bodies. As a thermoplastic resin thin film, cellophane having a thickness of 20 μm was prepared.
A fired ceramic body containing metal silicon, boron carbide and silicon carbide was produced by the same method as in Example 1, and a joining sample was prepared in the same shape.
A cellophane having a thickness of 20 μm was sandwiched between the joining surfaces of the two objects to be joined, and fixed with a carbon jig to form a shape of 20 × 40 × 6 mm.
The fixed sample was heat-treated at 1300 ° C. in a vacuum in a carbon furnace. While the temperature was raised to 1300 ° C. (temperature raising rate was 300 ° C./1 hour), the temperature was maintained at 600 ° C. for 1 hour to carbonize the cellophane.
(実施例14)
第1の被接合体および第2の被接合体として金属ケイ素および炭化硼素および炭化ケイ素を含有するセラミックス焼成体を準備した。熱可塑性樹脂薄膜として、厚み20μmのセロファンを準備した。
金属ケイ素および炭化硼素および炭化ケイ素を含有するセラミックス焼成体は実施例1と同様の方法により作製し、接合用試料も同様の形状を準備した。
2つの被接合体の接合面に厚み20μmのセロハンを挟み込み、炭素ジグで固定し、20x40x6mmの形状とした。
固定した試料を炭素炉で真空中1400℃で熱処理を行った。1400℃まで昇温(昇温速度は300度/1時間とした)する途中では600℃で1時間保持し、セロファンを炭化させた。
(Example 14)
Ceramic fired bodies containing metal silicon, boron carbide, and silicon carbide were prepared as the first and second bonded bodies. As a thermoplastic resin thin film, cellophane having a thickness of 20 μm was prepared.
A fired ceramic body containing metal silicon, boron carbide and silicon carbide was produced by the same method as in Example 1, and a joining sample was prepared in the same shape.
A cellophane having a thickness of 20 μm was sandwiched between the joining surfaces of the two objects to be joined, and fixed with a carbon jig to form a shape of 20 × 40 × 6 mm.
The fixed sample was heat-treated at 1400 ° C. in a vacuum in a carbon furnace. While the temperature was raised to 1400 ° C. (temperature raising rate was 300 ° C./1 hour), the temperature was maintained at 600 ° C. for 1 hour to carbonize the cellophane.
以上の実施例において接合した試料は、それぞれ実施例1に記載と同一の方法、すなわち、加熱後の試料を3x4x40mmのテストピースに加工し、3点曲げ(JISR1601)を行い破断することで強度の測定を行った。
その測定結果を表1に示す。
In the above examples, the bonded samples are each of the same method as described in Example 1, that is, the heated sample is processed into a 3 × 4 × 40 mm test piece, subjected to three-point bending (JISR1601) and fractured. Measurements were made.
The measurement results are shown in Table 1.
Claims (8)
金属ケイ素を含むセラミックス焼結体からなる第1の被接合体と、セラミックス焼結体からなる第2の被接合体と、が接合層を介して接合され、
前記接合層は金属ケイ素を主成分とすることを特徴とするセラミックス接合体。 A ceramic joined body,
A first bonded body made of a ceramic sintered body containing metal silicon and a second bonded body made of a ceramic sintered body are bonded via a bonding layer,
The bonded ceramic body according to claim 1, wherein the bonding layer contains metal silicon as a main component.
接合面を有し、金属ケイ素を含むセラミックス焼結体からなる第1の被接合体を準備する工程と、
接合面を有し、セラミックス焼結体からなる第2の被接合体を準備する工程と、
第1の被接合体の接合面と第2の被接合体の接合面との間に熱可塑性樹脂薄膜を配置して第1の被接合体と第2の被接合体とを重ね合わせる工程と、
前記熱可塑性樹脂薄膜を介して重ね合わされた第1の被接合体と第2の被接合体とを、接合面同士が押圧された状態を維持しつつ、不活性雰囲気下において所定温度で熱処理する工程と、を具備してなることを特徴とするセラミックス接合体の製造方法。 A method for producing a ceramic joined body, comprising:
Preparing a first bonded body having a bonding surface and made of a ceramic sintered body containing metallic silicon;
Preparing a second bonded body having a bonding surface and made of a ceramic sintered body;
Disposing a thermoplastic resin thin film between the bonding surface of the first bonded body and the bonding surface of the second bonded body and superimposing the first bonded body and the second bonded body; ,
The first bonded body and the second bonded body that are overlapped with each other through the thermoplastic resin thin film are heat-treated at a predetermined temperature in an inert atmosphere while maintaining a state where the bonded surfaces are pressed to each other. A process for producing a ceramic joined body comprising the steps of:
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