JPH0717772A - Production of material with gradient function - Google Patents
Production of material with gradient functionInfo
- Publication number
- JPH0717772A JPH0717772A JP5165502A JP16550293A JPH0717772A JP H0717772 A JPH0717772 A JP H0717772A JP 5165502 A JP5165502 A JP 5165502A JP 16550293 A JP16550293 A JP 16550293A JP H0717772 A JPH0717772 A JP H0717772A
- Authority
- JP
- Japan
- Prior art keywords
- film
- layer
- paste
- filler
- gradient
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、傾斜機能材料を任意の
傾斜度合いで効率よく製造する方法に関するものであ
る。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for efficiently manufacturing a functionally gradient material with an arbitrary degree of gradient.
【０００２】[0002]
【従来の技術】傾斜機能材料は、有人宇宙往還機（以
下、スペースプレーンと称す）を利用して宇宙と地上と
の間で人や物資の輸送を行うに際して、スペースプレー
ンが厳しい環境条件下に置かれた場合でもスペースプレ
ーンがその内部に収納した人や物の安全を確保できる超
耐熱材料を探し求める段階で生まれた。2. Description of the Related Art Functionally graded materials are used for transporting humans and materials between space and the ground using manned space vehicles (hereinafter referred to as space planes) under severe environmental conditions. It was born at the stage of searching for a super heat resistant material that can secure the safety of people and things stored inside the space plane even when placed.
【０００３】これらの超耐熱材料に対する要求は過酷で
ある。たとえば、スペースプレーンを宇宙と地上間を往
還させる場合、機体外表面温度は１８００℃近くに達す
るため、機体内部を−２５３℃の液体窒素などの冷媒で
冷却しなければならない。この場合、機体材料の厚さ方
向には大きな温度差とそれによる熱応力が発生する。The demands on these super-heat-resistant materials are severe. For example, when the space plane is moved back and forth between space and the ground, the outer surface temperature of the fuselage reaches nearly 1800 ° C., so the inside of the fuselage must be cooled with a coolant such as liquid nitrogen at −253 ° C. In this case, a large temperature difference and a thermal stress due to the temperature difference occur in the thickness direction of the airframe material.
【０００４】そこで、スペースプレーンの外装材はこの
ような著しい外面と裏面との温度差と熱応力に耐えうる
超耐熱材料で構成されることが必要であり、その１つと
して傾斜機能材料の発想が生まれた。Therefore, it is necessary that the exterior material of the space plane is made of a super heat-resistant material that can withstand such a remarkable temperature difference between the outer surface and the back surface and a thermal stress. One of them is the idea of a functionally graded material. Was born.
【０００５】代表的な傾斜機能材料の製造方法として
は、蒸着法、粒子法、溶射法、燃焼合成法など
が挙げられる。Typical methods for producing a functionally graded material include vapor deposition, particle method, thermal spraying method and combustion synthesis method.
【０００６】の蒸着法は、基材上に化学蒸着法を行う
に際し、蒸着部に供給する２種の原料ガスの流量比を蒸
着時間とともに連続的に変化させ、基材面上に傾斜構造
層を形成する方法である。In the vapor deposition method of (1), when the chemical vapor deposition method is performed on the substrate, the flow rate ratio of the two source gases supplied to the vapor deposition section is continuously changed with the vapor deposition time, and the inclined structure layer is formed on the substrate surface. Is a method of forming.
【０００７】の粒子法は、２種の粒径の異なるミクロ
ン単位の微粒子の混合物の組成比を変えながら容器に詰
め、焼結させるものや、組成比を変えた２種の粒径の異
なる微粒子の混合物と有機バインダー樹脂とよりなる薄
膜（以下、グリーンシートと称す）を作成し、それを積
層して焼結することにより、粒径分布に傾斜構造を与え
たものがある。The particle method of (2) is one in which a mixture of two kinds of microparticles having different particle sizes is packed in a container while changing the composition ratio and sintered, or two kinds of particles having different composition ratios having different particle sizes. There is a thin film (hereinafter referred to as a green sheet) made of a mixture of the above and an organic binder resin, which is laminated and sintered to give a gradient structure to the particle size distribution.
【０００８】の溶射法としては、プラズマ溶射法があ
り、１個のプラズマガンから発生するプラズマジェット
中に供給する２種の溶射剤の組成比を制御しながら投入
し、基材面に傾斜構造を形成するものや、２台のプラズ
マガンを用いて２種の溶射剤の供給量をそれぞれ独立に
制御して基材面上に傾斜構造を形成するものがある。As a thermal spraying method of 1, there is a plasma thermal spraying method, in which two types of thermal spraying agents supplied into a plasma jet generated from one plasma gun are injected while controlling the composition ratio, and an inclined structure is formed on a substrate surface. And one in which two plasma guns are used to independently control the supply amounts of two types of thermal spraying agents to form an inclined structure on the surface of the base material.
【０００９】の燃焼合成法としては、自己発熱反応法
（ＳＨＳ法）により２種の原料粉末の混合物を、その混
合比を変えながら積層し、その圧粉体を燃焼容器に封入
して静水圧下で着火合成するものがある。As the combustion synthesis method of (1), a mixture of two kinds of raw material powders is laminated by a self-heating reaction method (SHS method) while changing a mixing ratio thereof, and the green compact is enclosed in a combustion container and hydrostatic pressure is applied. There is one that is ignited and synthesized below.
【００１０】[0010]
【発明が解決しようとする課題】上記傾斜機能材料の製
造方法において、の蒸着法は傾斜機能材の形成に真空
系が必要であるため大形部材の製造が困難である。ま
た、厚膜の傾斜機能材料を製造するためには多大の時間
が必要である。In the above-mentioned method of manufacturing a functionally gradient material, the vapor deposition method is difficult to manufacture a large member because a vacuum system is required to form the functionally gradient material. Further, it takes a lot of time to manufacture a thick film functionally gradient material.
【００１１】の溶射法は、金属表面へセラミクスを溶
射する方法として利用されており、なかでもプラズマ溶
射法は比較的複雑な形状の大形部材でも厚膜の傾斜機能
層の形成が可能であるという特徴を有している。しかし
ながら、この溶射法で製造された傾斜機能膜は多数の気
孔が内在するため、機械的強度が低いなど物性上問題が
ある。また、その製造には大型の設備が必要でありコス
トが高くなるという問題がある。The thermal spraying method (1) is used as a method for thermal spraying ceramics onto a metal surface. Among them, the plasma thermal spraying method can form a thick functionally gradient layer even on a large member having a relatively complicated shape. It has the characteristics of However, since the functionally gradient film produced by this thermal spraying method has a large number of pores therein, it has problems in physical properties such as low mechanical strength. In addition, there is a problem that a large-scale facility is required for the production thereof and the cost becomes high.
【００１２】の粒子法の中でも、グリーンシートを積
層、焼結する方法は大形部材の製造に有効である。しか
しながら、このグリーンシートは、ドクターブレード法
により作られているため、厚さが数十ミクロン程度のも
のしか得られておらず、これより薄いグリーンシートを
作るには、技術的な困難が伴う。Among the particle methods, the method of stacking and sintering the green sheets is effective for manufacturing a large member. However, since this green sheet is produced by the doctor blade method, only a thickness of about several tens of microns has been obtained, and it is technically difficult to produce a green sheet thinner than this.
【００１３】の燃焼合成法のうちの自己発熱反応法
（ＳＨＳ法）は、基本的には固体粉末を原料として用い
るため、原料粉末の混合組成を変化させながら積層して
傾斜機能材形成用単体を作る技術が必要である。最近こ
の単体を自動的に作れる装置が開発され、大形の傾斜機
能材料を製造することが可能になったが、実用化にする
には生産性の面で未だ問題がある。In the self-heating reaction method (SHS method) of the combustion synthesis method of (1), since solid powder is basically used as a raw material, the powder is laminated by changing the mixed composition of the raw material powder to form a functionally gradient material alone. Technology is needed. Recently, a device that can automatically produce this simple substance has been developed, and it has become possible to manufacture a large-scale functionally graded material, but there is still a problem in terms of productivity for practical use.
【００１４】本発明は、このような状況に鑑み任意の傾
斜度合いで効率よく傾斜機能材料を製造する方法を提供
することを目的とするものである。In view of such a situation, the present invention has an object to provide a method for efficiently producing a functionally graded material with an arbitrary degree of inclination.
【００１５】[0015]
【課題を解決するための手段】本発明の要旨とするとこ
ろは、傾斜機能を発現させる少なくとも２種以上のフィ
ラーの混合比率が異なる粒子混合物と、有機バインダー
樹脂とよりなる２種以上のバインダー組成物をスクリー
ン印刷法にて作成したフィルム状物を複数枚積層するに
際し、積層したフィルム状物中の粒子比率が積層物の一
面から他面に向かって順次変化するように積層したもの
を特徴とする傾斜機能材料の製造方法にある。DISCLOSURE OF THE INVENTION The gist of the present invention is to provide at least two binder compositions comprising an organic binder resin and a particle mixture in which at least two fillers exhibiting a gradient function are mixed at different mixing ratios. When laminating a plurality of film-like materials prepared by screen printing, the particles are laminated so that the particle ratio in the laminated film-like materials sequentially changes from one surface to the other surface of the laminated material. There is a method of manufacturing a functionally graded material.
【００１６】本発明を実施するに際して用いるフィラー
の粒径としては、１０μｍ以下のものが好ましい。粒径
が１０μｍを越えるフィラーを用いては、スクリーン印
刷法にて膜厚３０μ以下の膜厚の形成が難しく、また、
その積層体を焼結して得られる焼結体中の空孔率が高く
なり、機械的強度などの物性の低下をまねき好ましくな
い。The particle size of the filler used for carrying out the present invention is preferably 10 μm or less. If a filler having a particle size of more than 10 μm is used, it is difficult to form a film having a film thickness of 30 μ or less by a screen printing method.
The porosity in the sintered body obtained by sintering the laminated body becomes high, which leads to deterioration of physical properties such as mechanical strength, which is not preferable.
【００１７】本発明に用いられるフィラーとしては、Ｓ
ｉＯ2、Ａｌ2Ｏ3、ＭｇＯ、ＺｒＯ2、ムライト（３Ａｌ
2Ｏ3・２ＳｉＯ2）、ジルコン（ＺｒＯ2・ＳｉＯ2）、
スピネル（ＭｇＯ・Ａｌ2Ｏ3）、ＳｉＣ、ＴｉＮ、Ｔｉ
Ｃ、Ｓｉ3Ｎ4、Ｎｉ、Ａｌ、Ｃｕ、Ｗ、ステンレス鋼な
どが挙げられる。The filler used in the present invention is S
iO 2 , Al 2 O 3 , MgO, ZrO 2 , mullite (3Al
2 O 3 · 2SiO 2 ), zircon (ZrO 2 · SiO 2 ),
Spinel (MgO ・ Al 2 O 3 ), SiC, TiN, Ti
C, Si 3 N 4, Ni , Al, Cu, W, and the like of stainless steel.
【００１８】有機バインダー樹脂としては、焼成性に優
れた樹脂でフィラーを均一に混合分散できるものであれ
ば、特に限定されるものではない。有機バインダー樹脂
の具体例としては、例えばセルロース系樹脂、ビニルア
ルコール系樹脂及びメタクリル系樹脂等が上げられる
が、この中で焼成性の点でメタクリル系樹脂が好まし
い。The organic binder resin is not particularly limited as long as it is a resin having excellent baking properties and can uniformly mix and disperse the filler. Specific examples of the organic binder resin include cellulose-based resins, vinyl alcohol-based resins, and methacrylic-based resins. Among them, methacrylic-based resins are preferable from the viewpoint of baking property.
【００１９】有機バインダー樹脂とフィラーとからなる
ペースト状物をスクリーン印刷でフィルム状物にする場
合、ペースト状物を有機溶剤にて希釈し、スクリーン印
刷したのち有機溶剤を乾燥除去する方法を用いるのが望
ましい。有機バインダー樹脂量としては、ペースト状物
中に含まれるフィラーに対して重量比で５０％以下であ
ることが望ましい。When a paste-like material composed of an organic binder resin and a filler is formed into a film-like material by screen printing, a method of diluting the paste-like material with an organic solvent, screen-printing and then removing the organic solvent by drying is used. Is desirable. The amount of the organic binder resin is preferably 50% or less in weight ratio with respect to the filler contained in the pasty material.
【００２０】有機バインダー樹脂量が５０％を越えて大
きなペースト状物を用いて作ったフィルム状物の積層体
を焼結したものは、焼結体中の空孔率が高くなり、機械
的強度などの物性の低下をまねき好ましくない。When a laminate of a film-like material made of a large paste-like material having an organic binder resin content of more than 50% is sintered, the porosity in the sintered body is high and the mechanical strength is high. It is not preferable because it causes deterioration of physical properties such as.
【００２１】有機バインダー樹脂５０％以下のペースト
状物を用いてスクリーン印刷法によりフィルム状物を作
り、その積層物を焼結して得た焼結体は空孔率が小さ
く、極めて機能性を発揮しやすい傾斜機能構造体とする
ことができるという大きな特徴を有している。すなわ
ち、フィルム状物中のフィラー含有率を従来法に比べ、
極めて大きくすることができる。A sintered body obtained by forming a film-like material by a screen printing method using a paste-like material having an organic binder resin of 50% or less and sintering the laminate has a small porosity and is extremely functional. It has a great feature that it can be a functionally graded structure that can be easily exhibited. That is, compared with the conventional method the filler content in the film,
It can be quite large.
【００２２】また、本発明を実施するに際しては、フィ
ルム状物積層体を焼結するときに、高圧をかけるホット
プレス法を用いることもできる。この方法を用いること
もできる。この方法を用いることより空孔率の低い焼結
体を得ることができる。In carrying out the present invention, it is also possible to use a hot pressing method in which a high pressure is applied when the film-shaped material laminate is sintered. This method can also be used. By using this method, a sintered body having a low porosity can be obtained.
【００２３】上記方法により得られたフィルム状物を積
層して積層体を形成する際の積層順序は、本発明の目的
を満足させるために必要な重ね方を選べば良い。The laminating order when laminating the film-like materials obtained by the above method to form a laminated body may be selected as a laminating manner necessary for satisfying the object of the present invention.
【００２４】以下、図１に示した傾斜機能材料形成用フ
ィルム積層物を例にして説明をする。２種類のフィラー
をＡ、Ｂとした場合、第１層目は、Ａ／Ｂ＝１０／０
（重量比）からなるフィラーを有機バインダー樹脂に均
一分散させたペースト状物により形成したフィルム状物
である。第２層目は、Ａ／Ｂ＝９／１（重量比）からな
るフィラーを有機バインダー樹脂に均一分散させたペー
スト状物により形成したフィルム状物である。The film laminate for forming a functionally gradient material shown in FIG. 1 will be described below as an example. When the two kinds of fillers are A and B, the first layer is A / B = 10/0
It is a film-like material formed by a paste-like material in which a filler (weight ratio) is uniformly dispersed in an organic binder resin. The second layer is a film-like material formed of a paste-like material in which a filler composed of A / B = 9/1 (weight ratio) is uniformly dispersed in an organic binder resin.
【００２５】以下Ａ／Ｂ＝８／２、７／３、６／４、５
／５、４／６、３／７、２／８、１／９、０／１０（い
ずれも重量比）からなるフィラーを有機バインダー樹脂
に均一分散させたペースト状物により、第３層目、第４
層目、第５層目、第６層目、第７層目、第８層目、第９
層目、第１０層目、第１１層目のフィルム状物を形成し
た順序を示したものである。Hereinafter, A / B = 8/2, 7/3, 6/4, 5
/ 5, 4/6, 3/7, 2/8, 1/9, 0/10 (all are weight ratios) by a paste-like material in which the filler is uniformly dispersed in the organic binder resin, Fourth
The fifth layer, the fifth layer, the sixth layer, the seventh layer, the eighth layer, the ninth layer
It shows the order in which the film-shaped objects of the layer, the tenth layer, and the eleventh layer were formed.
【００２６】また、必要に応じてこれらのフィルム状物
中には、焼結助剤、解こう剤、湿潤剤、可塑剤、保護コ
ロイド剤、静電気防止剤、消泡剤、殺菌剤、キレート及
び隠ペイ剤、界面活性剤などの添加剤を加えても良い。In addition, if necessary, these film materials may include sintering aids, deflocculants, wetting agents, plasticizers, protective colloid agents, antistatic agents, antifoaming agents, bactericides, chelates and Additives such as a hidden pay agent and a surfactant may be added.
【００２７】フィルム膜厚は、スクリーン版及び印刷条
件を変えることにより任意に制御することができる。し
たがって本方法を用いれば、任意の傾斜度合いの傾斜機
能材料を得ることができる。The film thickness can be arbitrarily controlled by changing the screen plate and printing conditions. Therefore, by using this method, a functionally graded material having an arbitrary degree of gradient can be obtained.
【００２８】得られた傾斜機能材料の耐熱衝撃性を調べ
る方法としては、レーザー照射によるものが挙げられ
る。As a method for investigating the thermal shock resistance of the obtained functionally graded material, there is a method by laser irradiation.
【００２９】[0029]
【実施例】以下、本発明を実施例を用いて説明する。実
施例中、部は重量部を示す。EXAMPLES The present invention will be described below with reference to examples. In the examples, “part” means “part by weight”.
【００３０】粘度：２５℃、Ｅ型粘度計（東京計器
（株）製）で調整を行った。 耐熱衝撃性：ＹＡＧレーザー照射により、スポット径お
よそ２ｍｍで行った。Viscosity: 25 ° C., adjusted with an E-type viscometer (Tokyo Keiki Co., Ltd.). Thermal shock resistance: A spot diameter of about 2 mm was obtained by irradiation with YAG laser.
【００３１】［実施例１］ 〈第１層目〉イソブチルメタクリレート９９部、メタク
リル酸１部、及びアゾイソブチロニトリル１．３部をブ
チルセロソルブ中にて８０℃、１０時間反応させた。得
られたアクリル樹脂１５部（固形分）に、Ａｌ2Ｏ3１０
０部を分散、混練し、ブチルセロソルブにて粘度を１０
０００ｃｐｓに調整しペースト状物を得た。次いで、得
られたペースト状物をガラス板上に＃２００メッシュの
スクリーン版により膜厚１５μｍにベタ印刷を行い、１
５０℃で４０分間乾燥し、フィルム状物を作成した。[Example 1] <First layer> 99 parts of isobutyl methacrylate, 1 part of methacrylic acid, and 1.3 parts of azoisobutyronitrile were reacted in butyl cellosolve at 80 ° C for 10 hours. 15 parts (solid content) of the obtained acrylic resin was mixed with Al 2 O 3 10
0 part was dispersed and kneaded, and the viscosity was adjusted to 10 with butyl cellosolve.
The paste was obtained by adjusting the pressure to 000 cps. Then, the obtained paste-like material was solid-printed on a glass plate with a # 200 mesh screen plate to a film thickness of 15 μm.
It dried at 50 degreeC for 40 minutes, and created the film-form.
【００３２】〈第２層目〉アクリル樹脂１５部（固形
分）に、Ａｌ2Ｏ3９０部、Ｎｉ１０部を分散、混練する
以外は、第１層目と同様にしてペースト状物を得た。次
いで、得られたペースト状物を第１層目のフィルム状物
上に第１層目と同様にして重ね印刷、乾燥を行い、フィ
ルム状物を作成した。<Second Layer> A paste-like product was obtained in the same manner as in the first layer, except that 90 parts of Al 2 O 3 and 10 parts of Ni were dispersed and kneaded in 15 parts (solid content) of the acrylic resin. . Next, the obtained paste-like material was overprinted and dried on the first-layer film-like material in the same manner as in the first layer to form a film-like material.
【００３３】〈第３層目〉アクリル樹脂１５部（固形
分）に、Ａｌ2Ｏ3８０部、Ｎｉ２０部を分散、混練する
以外は、第１層目と同様にしてペースト状物を得た。次
いで、得られたペースト状物を第２層目のフィルム状物
上に第１層目と同様にして重ね印刷、乾燥を行い、フィ
ルム状物を作成した。<Third Layer> A paste-like material was obtained in the same manner as in the first layer except that 80 parts of Al 2 O 3 and 20 parts of Ni were dispersed and kneaded in 15 parts (solid content) of the acrylic resin. . Then, the obtained paste-like material was overprinted and dried on the second-layer film-like material in the same manner as in the first layer to form a film-like material.
【００３４】〈第４層目〉アクリル樹脂１５部（固形
分）に、Ａｌ2Ｏ3７０部、Ｎｉ３０部を分散、混練する
以外は、第１層目と同様にしてペースト状物を得た。次
いで、得られたペースト状物を第３層目のフィルム状物
上に第１層目と同様にして重ね印刷、乾燥を行い、フィ
ルム状物を作成した。<Fourth layer> A paste-like material was obtained in the same manner as in the first layer except that 15 parts (solid content) of acrylic resin were dispersed and kneaded with 70 parts of Al 2 O 3 and 30 parts of Ni. . Next, the obtained paste-like material was overprinted and dried on the film-like material of the third layer in the same manner as the first layer to form a film-like material.
【００３５】〈第５層目〉アクリル樹脂１５部（固形
分）に、Ａｌ2Ｏ3６０部、Ｎｉ４０部を分散、混練する
以外は、第１層目と同様にしてペースト状物を得た。次
いで、得られたペースト状物を第４層目のフィルム状物
上に第１層目と同様にして重ね印刷、乾燥を行い、フィ
ルム状物を作成した。<Fifth Layer> A paste-like material was obtained in the same manner as in the first layer except that 60 parts of Al 2 O 3 and 40 parts of Ni were dispersed and kneaded in 15 parts (solid content) of the acrylic resin. . Then, the obtained paste-like material was overprinted and dried on the film-like material of the fourth layer in the same manner as in the first layer to form a film-like material.
【００３６】〈第６層目〉アクリル樹脂１５部（固形
分）に、Ａｌ2Ｏ3５０部、Ｎｉ５０部を分散、混練する
以外は、第１層目と同様にしてペースト状物を得た。次
いで、得られたペースト状物を第５層目のフィルム状物
上に第１層目と同様にして重ね印刷、乾燥を行い、フィ
ルム状物を作成した。<Sixth Layer> A paste-like material was obtained in the same manner as in the first layer except that 50 parts of Al 2 O 3 and 50 parts of Ni were dispersed and kneaded in 15 parts (solid content) of the acrylic resin. . Next, the obtained paste-like material was overprinted and dried on the film-like material of the fifth layer in the same manner as in the first layer to form a film-like material.
【００３７】〈第７層目〉アクリル樹脂１５部（固形
分）に、Ａｌ2Ｏ3４０部、Ｎｉ６０部を分散、混練する
以外は、第１層目と同様にしてペースト状物を得た。次
いで、得られたペースト状物を第６層目のフィルム状物
上に第１層目と同様にして重ね印刷、乾燥を行い、フィ
ルム状物を作成した。<Seventh Layer> A paste-like material was obtained in the same manner as in the first layer except that 40 parts of Al 2 O 3 and 60 parts of Ni were dispersed and kneaded in 15 parts (solid content) of the acrylic resin. . Next, the obtained paste-like material was overprinted and dried on the sixth-layer film-like material in the same manner as in the first layer to form a film-like material.
【００３８】〈第８層目〉アクリル樹脂１５部（固形
分）に、Ａｌ2Ｏ3３０部、Ｎｉ７０部を分散、混練する
以外は、第１層目と同様にしてペースト状物を得た。次
いで、得られたペースト状物を第７層目のフィルム状物
上に第１層目と同様にして重ね印刷、乾燥を行い、フィ
ルム状物を作成した。<Eighth Layer> A paste-like product was obtained in the same manner as in the first layer, except that 30 parts of Al 2 O 3 and 70 parts of Ni were dispersed and kneaded in 15 parts (solid content) of the acrylic resin. . Next, the obtained paste-like material was overprinted and dried on the film-like material of the seventh layer in the same manner as in the first layer to form a film-like material.
【００３９】〈第９層目〉アクリル樹脂１５部（固形
分）に、Ａｌ2Ｏ3２０部、Ｎｉ８０部を分散、混練する
以外は、第１層目と同様にしてペースト状物を得た。次
いで、得られたペースト状物を第８層目のフィルム状物
上に第１層目と同様にして重ね印刷、乾燥を行い、フィ
ルム状物を作成した。<Ninth Layer> A paste-like product was obtained in the same manner as in the first layer, except that 20 parts of Al 2 O 3 and 80 parts of Ni were dispersed and kneaded in 15 parts (solid content) of the acrylic resin. . Then, the obtained paste-like material was overprinted and dried on the film-like material of the eighth layer in the same manner as in the first layer to form a film-like material.
【００４０】〈第１０層目〉アクリル樹脂１５部（固形
分）に、Ａｌ2Ｏ3１０部、Ｎｉ９０部を分散、混練する
以外は、第１層目と同様にしてペースト状物を得た。次
いで、得られたペースト状物を第９層目のフィルム状物
上に第１層目と同様にして重ね印刷、乾燥を行い、フィ
ルム状物を作成した。<10th layer> A paste-like product was obtained in the same manner as in the 1st layer except that 15 parts (solid content) of acrylic resin were dispersed and kneaded with 10 parts of Al 2 O 3 and 90 parts of Ni. . Next, the obtained paste-like material was overprinted and dried on the film-like material of the ninth layer in the same manner as in the first layer to form a film-like material.
【００４１】〈第１１層目〉アクリル樹脂１５部（固形
分）に、Ｎｉ１００部を分散、混練する以外は、第１層
目と同様にしてペースト状物を得た。次いで、得られた
ペースト状物を第１０層目のフィルム状物上に重ね印
刷、乾燥を行い、フィルム状物を作成した。このように
して得られた１１層の積層体を、１４００℃、５時間焼
結することにより傾斜機能材料を得た。<Eleventh Layer> A paste-like material was obtained in the same manner as in the first layer except that 100 parts of Ni was dispersed and kneaded in 15 parts (solid content) of the acrylic resin. Next, the obtained paste-like material was overprinted on the 10th layer film-like material and dried to form a film-like material. The thus obtained 11-layer laminate was sintered at 1400 ° C. for 5 hours to obtain a functionally graded material.
【００４２】得られた傾斜機能材料の耐熱衝撃性を調べ
た結果、パワー密度２．８７ｗ／ｍｍ2 では割れは発生
しなかったが、パワー密度３．８７ｗ／ｍｍ2で割れが
発生した。The result of examining the thermal shock resistance of the resulting FGM, cracks in the power density 2.87w / mm 2 did not occur, cracks occurred in power density 3.87w / mm 2.
【００４３】［実施例２］実施例１と同様にしてスクリ
ーン印刷法により積層体を得た後、１ｔｏｎ／ｃｍ2 の
圧力をかけながら１４００℃、５時間焼結することによ
り傾斜機能材料を得た。Example 2 A laminated body was obtained by the screen printing method in the same manner as in Example 1, and then sintered at 1400 ° C. for 5 hours while applying a pressure of 1 ton / cm 2 , to obtain a functionally graded material. It was
【００４４】得られた傾斜機能材料の耐熱衝撃性を調べ
た結果、パワー密度２．８７ｗ／ｍｍ2 および３．８７
ｗ／ｍｍ2 では割れは発生しなかったが、パワー密度
４．８７ｗ／ｍｍ2 で割れが発生した。As a result of examining the thermal shock resistance of the obtained functionally graded material, the power density was 2.87 w / mm 2 and 3.87.
In w / mm 2 cracking did not occur, cracking occurs in the power density 4.87w / mm 2.
【００４５】［比較例１］イソブチルメタクリレート９
９部、メタクリル酸１部、及びアゾイソブチロニトリル
１．３部をブチルセロソルブ中にて８０℃、１０時間反
応させた。得られたアクリル樹脂１５部（固形分）に、
Ａｌ2Ｏ3１００部を分散、混練し、ブチルセロソルブに
て粘度を１００００ｃｐｓに調整しペースト状物を得
た。[Comparative Example 1] Isobutyl methacrylate 9
9 parts, methacrylic acid 1 part, and azoisobutyronitrile 1.3 parts were made to react in butyl cellosolve at 80 degreeC for 10 hours. To 15 parts (solid content) of the obtained acrylic resin,
100 parts of Al 2 O 3 was dispersed and kneaded, and the viscosity was adjusted to 10,000 cps with butyl cellosolve to obtain a paste.
【００４６】次いで、得られたペースト状物をガラス板
上に＃２００メッシュのスクリーン版により膜厚１５μ
ｍにベタ印刷を行い、１５０℃で４０分間乾燥し、フィ
ルム状物を作成した。同じペースト状物を用いて重ね印
刷、乾燥の操作を１０回繰り返し、厚さ１６５μｍの積
層体を得た。Then, the paste-like material thus obtained was coated on a glass plate with a # 200 mesh screen plate to a film thickness of 15 μm.
m was solid-printed and dried at 150 ° C. for 40 minutes to prepare a film-like material. The same paste-like material was used to repeat the printing and drying operations 10 times to obtain a laminated body having a thickness of 165 μm.
【００４７】得られた積層体を１４００℃、５時間焼結
することにより、Ａｌ2Ｏ3焼結体を得た。得られたＡｌ
2Ｏ3焼結体の熱衝撃性をスポット径およそ２ｍｍで行っ
たところ、パワー密度２．８７ｗ／ｍｍ2 で割れが発生
した。The obtained laminated body was sintered at 1400 ° C. for 5 hours to obtain an Al 2 O 3 sintered body. The obtained Al
When the thermal shock resistance of the 2 O 3 sintered body was performed with a spot diameter of about 2 mm, cracking occurred at a power density of 2.87 w / mm 2 .
【発明の効果】以上詳述したように、本発明の方法は、
超耐熱材料である傾斜機能材料を任意の傾斜度合いで効
率よく製造することができ、その工業的意義は著大であ
る。As described in detail above, the method of the present invention is
It is possible to efficiently produce a functionally graded material that is a super heat resistant material with an arbitrary degree of gradient, and its industrial significance is remarkable.
【図１】図１は、傾斜機能材料の概念を示すための断面
図である。FIG. 1 is a cross-sectional view showing the concept of a functionally graded material.
─────────────────────────────────────────────────────
─────────────────────────────────────────────────── ───
【手続補正書】[Procedure amendment]
【提出日】平成５年９月３日[Submission date] September 3, 1993
【手続補正１】[Procedure Amendment 1]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】００２２[Name of item to be corrected] 0022
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【００２２】また、本発明を実施するに際しては、フィ
ルム状物積層体を焼結するときに、高圧をかけるホット
プレス法を用いることもできる。この方法を用いること
により、空孔率の低い焼結体を得ることができる。In carrying out the present invention, it is also possible to use a hot pressing method in which a high pressure is applied when the film-shaped material laminate is sintered. By using this method, a sintered body having a low porosity can be obtained.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.6 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ｂ３２Ｂ 27/20 Ｚ 8413−4Ｆ 31/04 7148−4Ｆ Ｃ０８Ｋ 3/22 ＫＡＥ ─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. 6 Identification code Office reference number FI technical display location B32B 27/20 Z 8413-4F 31/04 7148-4F C08K 3/22 KAE
Claims (2)
のフィラーの混合比率が異なるフィラー混合物と、有機
バインダー樹脂とよりなるペースト状物をスクリーン印
刷法により作成した２種以上のフィルムを、そのフィラ
ー混合比率が順次変化するように積層した積層物を焼結
し、傾斜機能構造体を得ることを特徴とする傾斜機能材
料の製造方法。1. A filler comprising two or more kinds of films prepared by a screen printing method from a paste mixture consisting of a filler mixture having different mixing ratios of at least two kinds of fillers exhibiting a gradient function and an organic binder resin. A method of manufacturing a functionally gradient material, comprising: laminating a laminated material so that a mixing ratio is sequentially changed to obtain a functionally gradient structure.
５０％以下であることを特徴とする請求項１記載の傾斜
機能構造体の製造方法。2. The method for producing a functionally gradient structure according to claim 1, wherein the organic binder resin content of the film-like material is 50% or less.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5165502A JPH0717772A (en) | 1993-07-05 | 1993-07-05 | Production of material with gradient function |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5165502A JPH0717772A (en) | 1993-07-05 | 1993-07-05 | Production of material with gradient function |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0717772A true JPH0717772A (en) | 1995-01-20 |
Family
ID=15813614
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5165502A Pending JPH0717772A (en) | 1993-07-05 | 1993-07-05 | Production of material with gradient function |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0717772A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000109370A (en) * | 1998-10-02 | 2000-04-18 | Kikusui Chemical Industries Co Ltd | Production of burning tool with pattern |
| WO2000023523A1 (en) * | 1998-10-22 | 2000-04-27 | Ube Nitto Kasei Co., Ltd. | Organic-inorganic composite graded material, method for preparation thereof and use thereof |
| JP2000246114A (en) * | 1999-02-26 | 2000-09-12 | Orient Chem Ind Ltd | Organic-inorganic hybrid material and its production |
| KR20150009530A (en) * | 2012-03-30 | 2015-01-26 | 쓰리엠 이노베이티브 프로퍼티즈 컴파니 | Protective coating for low index material |
-
1993
- 1993-07-05 JP JP5165502A patent/JPH0717772A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000109370A (en) * | 1998-10-02 | 2000-04-18 | Kikusui Chemical Industries Co Ltd | Production of burning tool with pattern |
| WO2000023523A1 (en) * | 1998-10-22 | 2000-04-27 | Ube Nitto Kasei Co., Ltd. | Organic-inorganic composite graded material, method for preparation thereof and use thereof |
| US6737145B1 (en) | 1998-10-22 | 2004-05-18 | Ube Nitto Kasei Co., Ltd. | Organic-inorganic composite graded material, method for preparation thereof and use thereof |
| JP2000246114A (en) * | 1999-02-26 | 2000-09-12 | Orient Chem Ind Ltd | Organic-inorganic hybrid material and its production |
| KR20150009530A (en) * | 2012-03-30 | 2015-01-26 | 쓰리엠 이노베이티브 프로퍼티즈 컴파니 | Protective coating for low index material |
| JP2015516872A (en) * | 2012-03-30 | 2015-06-18 | スリーエム イノベイティブ プロパティズ カンパニー | Protective coating for low refractive index materials |
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