JP2869895B2 - Fabrication method of functionally graded material - Google Patents
Fabrication method of functionally graded materialInfo
- Publication number
- JP2869895B2 JP2869895B2 JP2073807A JP7380790A JP2869895B2 JP 2869895 B2 JP2869895 B2 JP 2869895B2 JP 2073807 A JP2073807 A JP 2073807A JP 7380790 A JP7380790 A JP 7380790A JP 2869895 B2 JP2869895 B2 JP 2869895B2
- Authority
- JP
- Japan
- Prior art keywords
- functionally graded
- materials
- graded material
- composition gradient
- present
- 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.)
- Expired - Lifetime
Links
- 239000000463 material Substances 0.000 title claims description 26
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 238000000034 method Methods 0.000 title description 6
- 238000009826 distribution Methods 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 239000006104 solid solution Substances 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 5
- 239000011268 mixed slurry Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 description 16
- 239000002002 slurry Substances 0.000 description 7
- 238000010586 diagram Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 4
- 238000009694 cold isostatic pressing Methods 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Powder Metallurgy (AREA)
- Compositions Of Oxide Ceramics (AREA)
Description
【発明の詳細な説明】 〈産業上の利用分野〉 この発明は傾斜機能材料の作製方法に関するものであ
る。DETAILED DESCRIPTION OF THE INVENTION <Industrial Application Field> The present invention relates to a method for producing a functionally graded material.
〈従来の技術〉 傾斜機能材料は、一般には耐熱用途の構造材料として
の応用が考えられている複合材料であって、宇宙船、核
融合炉等に利用が計画されている。<Conventional Technology> Functionally graded materials are composite materials that are generally considered to be applied as structural materials for heat-resistant applications, and are planned to be used in spacecraft, fusion reactors, and the like.
このような傾斜機能材料の作製方法としては、従来ド
クターブレード法によるものが知られている。As a method for producing such a functionally gradient material, a method using a doctor blade method has been conventionally known.
この方法にて材料Ａと材料Ｂの２種類の原料を用いて
傾斜機能材料を得る場合には、 下記第１表に示すように材料ＡとＢの混合比が僅か
づつ異なる種類の混合粉末を用意する。When a functionally graded material is obtained by using this method using two types of raw materials, material A and material B, as shown in Table 1 below, mixed powder of a type in which the mixing ratio of materials A and B is slightly different is used. prepare.
それぞれのグリーンシートを作製する。 Make each green sheet.
第８図（ａ）、（ｂ）のように望みとする組成傾斜
に近くなるようにで得たグリーンシートを積層し圧着
する（第７図）。As shown in FIGS. 8 (a) and 8 (b), green sheets obtained so as to approach the desired composition gradient are laminated and pressed (FIG. 7).
焼成を行なう。 Perform baking.
の工程が行なわれている。Is performed.
〈発明が解決しようとする課題〉 上記した従来技術では材料ＡとＢが固溶しあう場合に
は、焼成時に生じる熱拡散を利用することによって第８
図（ａ）のような成形体の段階状の組成傾斜を第９図
（ａ）乃至（ｃ）に示すような連続的に変化する滑らか
な組成傾斜にすることが可能である。<Problems to be Solved by the Invention> In the above-described conventional technology, when the materials A and B are in solid solution with each other, the eighth problem is solved by utilizing the thermal diffusion generated during firing.
The stepwise composition gradient of the molded article as shown in FIG. 9A can be changed to a continuously changing smooth composition gradient as shown in FIGS. 9A to 9C.
しかしながら、材料ＡとＢが固溶しあわず混晶を作る
ような場合には、熱拡散が生じないため、焼成後も第８
図（ａ）のような段階状の組成原料が残ってしまい、第
８図（ｂ）のような連続的に変化する組成傾斜を得るこ
とはできない。However, when the materials A and B do not form a solid solution and form a mixed crystal, thermal diffusion does not occur, so that the material A and B do not dissolve even after firing.
As shown in FIG. 8A, a stepwise composition raw material remains, and a continuously changing composition gradient as shown in FIG. 8B cannot be obtained.
〈課題を解決するための手段〉 この発明は上記に鑑みて、固溶し合わない複数の材料
を用いても組成（混合比）が連続的に傾斜している傾斜
機能材料を得るべく検討の結果、この発明に至ったもの
である。<Means for Solving the Problems> In view of the above, the present invention has been studied in order to obtain a functionally graded material whose composition (mixing ratio) is continuously inclined even when a plurality of materials that do not form a solid solution are used. As a result, the present invention has been achieved.
即ち、この発明は相互に固溶しない、かつ、粒度分布
の異なる複数以上の原料を用いて混合スラリーを得、該
混合スラリーを遠心分離または沈降分離して溶媒を除去
した後の泥濘を成形することを特徴とする傾斜機能材料
の作製方法を提供するものである。That is, the present invention obtains a mixed slurry by using a plurality of raw materials that do not form a solid solution with each other and have different particle size distributions, and forms mud after removing the solvent by centrifuging or sedimenting the mixed slurry. Another object of the present invention is to provide a method for producing a functionally gradient material characterized by the above.
〈作用〉 この発明は、特に成形時に従来法のような階段状の組
成傾斜ではなく、連続的な組成傾斜を形成することによ
って問題を解決するものである。<Operation> The present invention solves the problem by forming a continuous composition gradient, not a stepwise composition gradient as in the conventional method, particularly during molding.
この発明で連続的な組成傾斜を有する成形体を得るの
に用いる方法は、材料の粒度分布を利用する方法であ
る。The method used to obtain a molded article having a continuous composition gradient in the present invention is a method utilizing the particle size distribution of the material.
これを具体的に述べると、 （１） 第１図に示すように、材料ＡとＢの粒度分布の
間に適当な差を設ける。Specifically, (1) As shown in FIG. 1, an appropriate difference is provided between the particle size distributions of the materials A and B.
（２） 材料ＡとＢを適当量混合したスラリーを作製す
る。(2) A slurry in which materials A and B are mixed in an appropriate amount is prepared.
（３） 得られたスラリーを沈降分離、遠心分離するこ
とによって、第２図のように粒度分布に従って材料Ａ、
Ｂの混合比が連続的に変化している泥濘を得る。(3) By sedimentation and centrifugation of the obtained slurry, as shown in FIG.
Mud in which the mixing ratio of B continuously changes is obtained.
（４） 脱水、乾燥によって余分の溶媒を除去した後、
残渣の固形分に冷間静水圧成形（Cold Isostatic Pres
s、以下CIPという）、湿式プレス成形などを施すことに
よって成形体を得る。(4) After removing excess solvent by dehydration and drying,
Cold Isostatic Pressing (Cold Isostatic Pres
s, hereinafter referred to as CIP), and wet press molding to obtain a molded body.
ものである。Things.
〈実施例〉 以下、この発明を実施例により詳細に説明する。<Example> Hereinafter, the present invention will be described in detail with reference to examples.
原料として純度99％以上のCaTiO3およびMgTiO3の粉体
を用意した。Powders of CaTiO 3 and MgTiO 3 having a purity of 99% or more were prepared as raw materials.
このCaTiO3およびMgTiO3の粉体の粒度分布は前者を第
３図（ａ）に、後者を第３図（ｂ）に示した。The particle size distribution of the CaTiO 3 and MgTiO 3 powders is shown in FIG. 3 (a) for the former and FIG. 3 (b) for the latter.
500mlのポリポットにCaTiO3 50g、MgTiO3 50g、水200
cc、酢酸ビニル系バインダー3g、PSZ玉石100gを入れ、
約２時間ボールミルで混合してスラリーを得た。CaTiO 3 50g, MgTiO 3 50g, water 200 in a 500ml polypot
Put cc, vinyl acetate binder 3g, PSZ cobblestone 100g,
The mixture was mixed in a ball mill for about 2 hours to obtain a slurry.
次に、第４図に示すような薄いフィルム製の容器２を
内挿した遠心分離機用のサンプル容器１を用意し、その
中に上記で得たスラリー３を流し込んだ後、遠心分離を
行なった。Next, a sample container 1 for a centrifuge in which a container 2 made of a thin film as shown in FIG. 4 is inserted is prepared, and the slurry 3 obtained above is poured into the container, and then centrifuged. Was.
遠心分離操作後、生じた上澄み液を除去し、約１日の
自然乾燥を行なってロッド状の固形物を得た。After the centrifugation operation, the resulting supernatant was removed and air-dried for about 1 day to obtain a rod-shaped solid.
次いで、得られたロッド状固形物をフィルムごと容器
から取出し、フィルムを剥した後、該固形物を3t/cm2の
圧力でCIPすることによって強固で充填密度の高いロッ
ド状成形体を得た。Next, the obtained rod-shaped solid was taken out of the container together with the film, the film was peeled off, and the solid was subjected to CIP at a pressure of 3 t / cm 2 to obtain a rod-shaped molded body having a strong and high packing density. .
この成形体を空気中400℃の条件で加熱して、バイン
ダーを燃焼させた後、空気中1350℃で５時間焼成するこ
とによって第５図（ａ）に示すようなロッド状の焼結体
４を得た。This compact is heated in air at 400 ° C. to burn the binder, and then calcined in air at 1350 ° C. for 5 hours to obtain a rod-shaped sintered body 4 as shown in FIG. I got
この第５図（ａ）のようなロッド状焼結体４から第５
図（ｂ）のような形状の板状試料５をダイヤモンドカッ
ターを用いて切り出し、Ｘ線マイクロアナライザー（XM
A）分析を行なったところ、この焼結体は第６図に示す
ような連続的に変化している組成傾斜を有していること
が認められた。The rod-shaped sintered body 4 shown in FIG.
A plate-shaped sample 5 having a shape as shown in FIG.
A) Analysis showed that the sintered body had a continuously changing composition gradient as shown in FIG.
〈発明の効果〉 以上述べたように、この発明によって固溶し合わず混
晶を作るような材料を用いた場合でも、連続的な組成傾
斜を持つ傾斜機能材料が得られることがわかった。<Effects of the Invention> As described above, it has been found that a functionally gradient material having a continuous composition gradient can be obtained even when a material that does not form a solid solution and forms a mixed crystal is used according to the present invention.
そして、この発明の方法で得られた傾斜機能材料を耐
熱用途に用いた場合、接合界面が存在しないために理想
的な熱応力の緩和効果が得られるようになった。When the functionally graded material obtained by the method of the present invention is used for heat-resistant applications, an ideal thermal stress relaxation effect can be obtained because there is no bonding interface.
第１図はこの発明で用いる材料Ａ、Ｂの粒度分布を示す
線図、第２図は材料Ａ、Ｂの混合比が連続的に変化して
いることを示す線図、第３図（ａ）及び（ｂ）はこの発
明で用いる材料Ａ、Ｂのそれぞれの粒度分布を示す線
図、第４図はスラリーの遠心分離に用いるサンプル容器
の例と、該容器にスラリーを充填した状態を示す説明
図、第５図（ａ）は実施例にて得られたロッド状焼結体
の説明図、第５図（ｂ）は第５図（ａ）から切り出した
板状試料の説明図、第６図は第５図（ｂ）の試料のXMA
分析後の連続的組成傾斜を示す線図、第７図は従来の傾
斜機能材料製造におけるグリーンシート積層を示す斜視
図、第８図（ａ）は従来の成形体の段階状組成傾斜を示
す線図、第８図（ｂ）は成形体の理想とする組成傾斜を
示す線図、第９図（ａ）乃至（ｃ）は成形体の組成傾斜
の階段状から連続的変化への状態を示す線図である。 １……サンプル容器、２……フィルム製容器 ３……スラリー、４……ロッド状焼結体 ５……板状試料FIG. 1 is a diagram showing the particle size distribution of the materials A and B used in the present invention, FIG. 2 is a diagram showing that the mixing ratio of the materials A and B is continuously changing, and FIG. ) And (b) are diagrams showing the respective particle size distributions of the materials A and B used in the present invention, and FIG. 4 shows an example of a sample container used for centrifugal separation of the slurry and a state where the container is filled with the slurry. FIG. 5 (a) is an explanatory view of a rod-shaped sintered body obtained in the example, FIG. 5 (b) is an explanatory view of a plate-like sample cut from FIG. 5 (a), and FIG. Fig. 6 shows the XMA of the sample of Fig. 5 (b).
FIG. 7 is a diagram showing a continuous composition gradient after the analysis, FIG. 7 is a perspective view showing a conventional green sheet lamination in the production of a functionally graded material, and FIG. 8 (a) is a line showing a stepwise composition gradient of a conventional molded body. FIG. 8 (b) is a diagram showing an ideal composition gradient of the molded body, and FIGS. 9 (a) to 9 (c) show a state where the composition gradient of the molded body is changed from stepwise to continuous change. FIG. DESCRIPTION OF SYMBOLS 1 ... Sample container 2, ... Film container 3 ... Slurry 4, ... Rod-shaped sintered compact 5 ... Plate-shaped sample
───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.6，ＤＢ名) B28B 1/00 - 1/54 C04B 35/00 B22F 3/22 ────────────────────────────────────────────────── ─── Continued on the front page (58) Fields surveyed (Int. Cl. 6 , DB name) B28B 1/00-1/54 C04B 35/00 B22F 3/22
Claims (1)
る複数以上の原料を用いて混合スラリーを得、該混合ス
ラリーを遠心分離または沈降分離して溶媒を除去した後
の泥濘を成形することを特徴とする傾斜機能材料の作製
方法。1. A mixed slurry is obtained by using a plurality of raw materials which do not form a solid solution with each other and have different particle size distributions, and the mixed slurry is centrifuged or settled to form a mud after removing a solvent. A method for producing a functionally graded material, comprising:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2073807A JP2869895B2 (en) | 1990-03-23 | 1990-03-23 | Fabrication method of functionally graded material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2073807A JP2869895B2 (en) | 1990-03-23 | 1990-03-23 | Fabrication method of functionally graded material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03274105A JPH03274105A (en) | 1991-12-05 |
| JP2869895B2 true JP2869895B2 (en) | 1999-03-10 |
Family
ID=13528808
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2073807A Expired - Lifetime JP2869895B2 (en) | 1990-03-23 | 1990-03-23 | Fabrication method of functionally graded material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2869895B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE69330341T2 (en) * | 1992-09-24 | 2001-09-20 | Toto Ltd., Kitakyushu | MATERIAL WITH DEPENDENT GRADIENT AND THEIR PRODUCTION |
| JP4161051B2 (en) * | 2003-06-16 | 2008-10-08 | 独立行政法人産業技術総合研究所 | Method for manufacturing gradient material |
| CN114515829B (en) * | 2021-12-28 | 2024-03-05 | 西安理工大学 | Preparation method of layered gradient W-Cu composite material |
-
1990
- 1990-03-23 JP JP2073807A patent/JP2869895B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH03274105A (en) | 1991-12-05 |
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