JPS6163568A - Zirconia porous sintered body and its manufacturing method - Google Patents
Zirconia porous sintered body and its manufacturing methodInfo
- Publication number
- JPS6163568A JPS6163568A JP59089039A JP8903984A JPS6163568A JP S6163568 A JPS6163568 A JP S6163568A JP 59089039 A JP59089039 A JP 59089039A JP 8903984 A JP8903984 A JP 8903984A JP S6163568 A JPS6163568 A JP S6163568A
- Authority
- JP
- Japan
- Prior art keywords
- sintered body
- porous
- zirconia
- oxidizing atmosphere
- cao
- 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
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims description 31
- 238000004519 manufacturing process Methods 0.000 title claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 13
- 239000011148 porous material Substances 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 6
- 238000010304 firing Methods 0.000 claims description 4
- 229910052747 lanthanoid Inorganic materials 0.000 claims description 4
- 150000002602 lanthanoids Chemical class 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 239000000470 constituent Substances 0.000 claims description 3
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical group [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 claims description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims 2
- 229910001928 zirconium oxide Inorganic materials 0.000 claims 2
- 239000010987 cubic zirconia Substances 0.000 claims 1
- 239000000919 ceramic Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 239000003381 stabilizer Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000007809 chemical reaction catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000004053 dental implant Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910002077 partially stabilized zirconia Inorganic materials 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
Landscapes
- Porous Artificial Stone Or Porous Ceramic Products (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.
Description
【発明の詳細な説明】
（イ）技術分野
この発明は微細均一な空孔を含む多孔質のジルコニア焼
結体およびその製造方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION (a) Technical Field The present invention relates to a porous zirconia sintered body containing fine and uniform pores and a method for producing the same.
（ロ）従来技術とその問題点
セラミックス材料は、その耐熱性、耐摩耗性、耐薬品性
などにすぐれた特性を用いて種々の用途に用いられてい
る。(b) Prior art and its problems Ceramic materials are used for various purposes due to their excellent properties such as heat resistance, abrasion resistance, and chemical resistance.
一般には十分に緻密な焼結体として用いることが多いが
、多孔質体としたセラミックスはフィルター、反応触媒
担体をはじめ、ヒートパイプなどの用途開発が進められ
ている。Generally, ceramics are often used as sufficiently dense sintered bodies, but porous ceramics are being developed for use in filters, reaction catalyst carriers, heat pipes, and other applications.
しかしながら、最も一般的なこれらセラミックス多孔質
体が骨材粒子とガラス、粘土などの結合材を混合焼結し
て得られるため、細孔形状が不均一となりやすく、焼結
体強度が低いといった問題点を持ち、ざらに結合材の耐
熱性、純度などにも欠点が多かった。However, since these most common ceramic porous bodies are obtained by mixing and sintering aggregate particles and binders such as glass and clay, the pore shapes tend to be uneven and the strength of the sintered body is low. However, there were also many drawbacks such as the heat resistance and purity of the bonding material.
（ハ）発明の構成
この発明は、骨材のような耐熱性、耐薬品性などに劣る
低純度の物質を使用せず、これらの性質にすぐれたジル
コニア焼結体で１０μ以下の微細で均一な空孔かうなる
多孔質ジルコニア焼結体を提供せんとするものである。(C) Structure of the Invention This invention does not use low-purity substances such as aggregates that have poor heat resistance and chemical resistance, but uses zirconia sintered bodies with excellent properties such as fine and uniform particles of 10μ or less. The present invention aims to provide a porous zirconia sintered body having large pores.
即ち、この発明のジルコニア焼結体は公知の安定化剤を
含むジルコニア組成物であるが、１０μ以下程度の細孔
からなる多孔質高強度ジルコニア焼結体であって、その
主たる構成相が正方晶および／または立方晶であること
を特徴とするものである。That is, the zirconia sintered body of the present invention is a zirconia composition containing a known stabilizer, and is a porous high-strength zirconia sintered body consisting of pores of about 10 μm or less, and its main constituent phase is square. It is characterized by being crystal and/or cubic crystal.
この発明で焼結体中の細孔の大きさは破面を２次元的に
観察して得られる２次元的な空孔の大ぎさを示す。なお
、安定化剤としては、ＣａＯいＭｇＯ１Ｙ２０３、ラン
タニド系希土類元素の酸化物等が使用され、ジルコニア
が立方晶に安定化するに必要な母の １／３以上２倍以
下が必要である（例えばＹ２Ｏ３で２．５モル、ＣａＯ
で３モル以上等）。これは安定剤の添加によって焼結体
の構成相が主として正方晶および／または立方晶からな
り、過度の単斜晶含有物に発生するクラックを阻止でき
ることだけでなく、空孔の発生に効果的なためである。In this invention, the size of the pores in the sintered body indicates the two-dimensional size of the pores obtained by two-dimensionally observing the fracture surface. In addition, as a stabilizer, CaO, MgO1Y203, lanthanide-based rare earth element oxides, etc. are used, and the amount is required to be 1/3 or more and 2 times or less of the base required for stabilizing zirconia into a cubic crystal (for example, 2.5 mol of Y2O3, CaO
3 moles or more). This is because the constituent phases of the sintered body are mainly tetragonal and/or cubic by adding a stabilizer, which not only prevents cracks that occur due to excessive monoclinic crystal content, but also effectively prevents the generation of pores. This is for a reason.
空孔率に関しては、５乃至４０％が好ましく、これは５
％以下では空孔の存在する意味がなく、また４０％以上
とするには還元雰囲気中焼成、酸化性雰囲気中加熱を多
数回繰返す必要があり、また焼結体強度が小さくなりす
ぎることから実用的でない。Regarding the porosity, 5 to 40% is preferable;
% or less, there is no point in the presence of pores, and to increase the porosity to 40% or more, it is necessary to repeat firing in a reducing atmosphere and heating in an oxidizing atmosphere many times, and the strength of the sintered body becomes too low, making it impractical. Not on point.
この発明の多孔質ジルコニア焼結体は−０、ＣａＯ、Ｙ
２Ｏ３およびランタニド系元素の酸化物から選ばれた１
種以上の酸化物葎たは容易に酸化物に転換可能な化合物
をｚｒ Ｏｔ粉末に添加し、通常の方法で成型したのち
、非酸化性雰囲気にて焼成する。The porous zirconia sintered body of this invention is -0, CaO, Y
1 selected from oxides of 2O3 and lanthanide elements
One or more oxide seeds or compounds easily convertible to oxides are added to the ZR Ot powder, shaped in a conventional manner, and then fired in a non-oxidizing atmosphere.
非酸化性雰囲気としては真空、窒素ガス、アルゴンガス
、水素ガス雰囲気などが挙げられる。Examples of the non-oxidizing atmosphere include vacuum, nitrogen gas, argon gas, and hydrogen gas atmosphere.
焼成条件としては１３００℃以上を必要とするが、１７
００℃以上の焼成はＺｒ Ｏｐの粒成長が著しく好まし
くない。Firing conditions require a temperature of 1300°C or higher, but 17
Firing at a temperature of 00° C. or higher is unfavorable as grain growth of Zr Op is significant.
しかして得られた焼結体は、さらに熱間静水圧プレスを
行なう、あるいはカーボンダイを用いてホットプレス焼
結を行なうなどの方法も効果が大きい。The thus obtained sintered body can be further effectively subjected to hot isostatic pressing or hot press sintering using a carbon die.
なお、いったん酸化性雰囲気で焼結後、還元性雰囲気で
加熱する方法でもよい。Note that a method may also be used in which the material is sintered in an oxidizing atmosphere and then heated in a reducing atmosphere.
このような焼結法によって黒色１１１畜焼結体を得、引
きつづいて酸化性雰囲気中で１ｏｏｏ℃以上１７００℃
以下に加熱し、酸化させることで黒色焼結体は白色に変
化するとともに空孔が生成する。A black 111 sintered body was obtained by such a sintering method, and then heated at 100°C or higher to 1700°C in an oxidizing atmosphere.
By heating and oxidizing the black sintered body, the black sintered body changes to white and pores are generated.
処１１ｊｌの空孔率は焼結体の空孔率および酸素空孔温
度の増加に従って増加する。The porosity of the sintered body 11jl increases as the porosity of the sintered body and the oxygen pore temperature increase.
また、非酸化性雰囲気中加熱と、酸化性雰囲気中加熱を
繰返すことによって空孔率を増大させることが可能であ
り、保持温度、保持時間の変化によって空孔率、空孔の
大きさを所望の値にコントロールできるのである。In addition, it is possible to increase the porosity by repeating heating in a non-oxidizing atmosphere and heating in an oxidizing atmosphere, and the desired porosity and pore size can be achieved by changing the holding temperature and holding time. It is possible to control the value of
この発明によるジルコニア質多孔性焼結体は良好なイオ
ン導電性とすぐれた強度および均一な組織、組成をもつ
すぐれた材料であり、多孔質セラミックスとして極めて
特異な機能をもつものであり、固体電解質、歯科用イン
ブラント材料などに実用性の極めて高い材料ということ
ができる。The zirconia porous sintered body according to the present invention is an excellent material with good ionic conductivity, excellent strength, and a uniform structure and composition, and has extremely unique functions as a porous ceramic. It can be said that it is an extremely practical material for dental implant materials.
以下実施例により詳細に説明する。This will be explained in detail below using examples.
実施例１
３モルのＹ２Ｏ３を含むＺｒ ０２粉末を１５００℃、
１時間２００に９ Ｊの条件でホットプレス焼結として
１００×１００Ｘ １０ｍｍの大きさの黒色を呈する
部分安定化ジルコニア焼結体を得た。ホットプレスはカ
ーボン製のダイを用いて真空雰囲気で行なった。Example 1 Zr02 powder containing 3 mol of Y2O3 was heated at 1500°C.
A partially stabilized zirconia sintered body having a size of 100 x 100 x 10 mm and exhibiting a black color was obtained by hot press sintering under the conditions of 9 J at 200 J for 1 hour. Hot pressing was performed in a vacuum atmosphere using a carbon die.
得られた焼結体は９５％以上が正方晶ＺｒＯ□からなり
、！Ｉ！度は６．０８であった。More than 95% of the obtained sintered body consists of tetragonal ZrO□,! I! The degree was 6.08.
ホットプレス焼結体は大気炉で１４００℃×５時間加熱
し、酸化させ、白色化した。The hot-pressed sintered body was heated in an atmospheric furnace at 1400° C. for 5 hours to oxidize and turn white.
得られた白色焼結体は、２〜０．２μの均一な空孔が均
一に分散した多孔体ととなり、音度は５．７５ （空
孔率６％）であった。また曲げ強度は１２０ｋｑ ４７
に達し、緻密質焼結体に遜色のない強度を示した。The obtained white sintered body was a porous body in which uniform pores of 2 to 0.2 μm were uniformly dispersed, and the acousticity was 5.75 (porosity: 6%). Also, the bending strength is 120kq 47
It reached a strength comparable to that of a dense sintered body.
実施例２
実施例１で１ｑた多孔質体をカーボン粉末に埋込み、真
空中で１５００″ＣＸ４時間加熱したのち、さらに大気
中で１４００℃×５時間加熱した。Example 2 1 q of the porous body prepared in Example 1 was embedded in carbon powder, heated in vacuum at 1500° C. for 4 hours, and then further heated at 1400° C. for 5 hours in the air.
得られた白色焼結体の密度は５．４５に低下し、空孔率
は１０％となった。The density of the obtained white sintered body was reduced to 5.45, and the porosity was 10%.
本焼結体は曲げ強度が１１０ｋｑ４とほとんど低下せず
、多孔質焼結体としては特異な強度を得た。The bending strength of this sintered body was 110 kq4, which was hardly decreased, and the strength was unique for a porous sintered body.
特許出願人 住友電気工業株式会社
代 理 人 弁理士 和 １） 昭手続
補装置（方式）
％式％Patent Applicant Sumitomo Electric Industries Co., Ltd. Agent Patent Attorney Kazu 1) Showa Procedural Auxiliary Device (Method) % Formula %
Claims (5)
コニアであり、１０μ以下の微細均一な大きさの孤立あ
るいは連続した空孔が均一に分散存在していることを特
徴とするジルコニア質多孔焼結体。(1) Zirconia porous sintered material whose main constituent phase is tetragonal and/or cubic zirconia, and in which fine, uniformly sized isolated or continuous pores of 10μ or less are uniformly dispersed. Body.
請求の範囲第１項記載のジルコニア質多孔焼結体。(2) The zirconia porous sintered body according to claim 1, which has a porosity of 5 to 40%.
とを特徴とする特許請求の範囲第１項記載のジルコニア
質多孔焼結体。(3) A porous zirconia sintered body according to claim 1, wherein the dense sintered body is made porous by heat treatment.
ド系元素の酸化物から選ばれた少なくとも１種を含む酸
化ジルコニウム粉末を非酸化性雰囲気中で焼成して黒色
の焼結体としたのち、引続いて該焼結体の酸化性雰囲気
中での加熱を１回以上繰返すことによつて白色化焼結体
を得ることを特徴とするジルコニア質多孔焼結体の製造
方法。(4) After firing zirconium oxide powder containing at least one selected from MgO, CaO, Y_2O_3, or oxides of lanthanide elements in a non-oxidizing atmosphere to form a black sintered body, A method for producing a porous zirconia sintered body, the method comprising obtaining a whitened sintered body by repeating heating the sintered body in an oxidizing atmosphere one or more times.
系元素の酸化物から選ばれた少なくとも１種を含む酸化
ジルコニウム粉末を酸化性雰囲気中で焼成したのち、非
酸化雰囲気中で加熱して、黒色焼結体を得、次いで該焼
結体の酸化性雰囲気中での加熱を１回以上繰返すことに
よつて白色化焼結体を得ることを特徴とするジルコニア
質多孔焼結体の製造方法。(5) Zirconium oxide powder containing at least one selected from MgO, CaO, Y_2O_3 and oxides of lanthanide elements is fired in an oxidizing atmosphere, and then heated in a non-oxidizing atmosphere to form a black sintered body. 1. A method for producing a porous zirconia sintered body, which comprises obtaining a whitened sintered body by repeating heating the sintered body in an oxidizing atmosphere one or more times.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59089039A JPS6163568A (en) | 1984-05-02 | 1984-05-02 | Zirconia porous sintered body and its manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59089039A JPS6163568A (en) | 1984-05-02 | 1984-05-02 | Zirconia porous sintered body and its manufacturing method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6163568A true JPS6163568A (en) | 1986-04-01 |
Family
ID=13959748
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP59089039A Pending JPS6163568A (en) | 1984-05-02 | 1984-05-02 | Zirconia porous sintered body and its manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6163568A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04115469A (en) * | 1990-09-04 | 1992-04-16 | Ngk Insulators Ltd | Solid electrolyte film and solid electrolyte type fuel cell therewith and manufacture thereof |
| JPH04124073A (en) * | 1990-09-12 | 1992-04-24 | Shinagawa Refract Co Ltd | Zirconia-based complex refractory and heat-insulating material |
| US6773825B2 (en) | 1997-03-31 | 2004-08-10 | Porvair Corporation | Porous articles and method for the manufacture thereof |
-
1984
- 1984-05-02 JP JP59089039A patent/JPS6163568A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04115469A (en) * | 1990-09-04 | 1992-04-16 | Ngk Insulators Ltd | Solid electrolyte film and solid electrolyte type fuel cell therewith and manufacture thereof |
| JPH04124073A (en) * | 1990-09-12 | 1992-04-24 | Shinagawa Refract Co Ltd | Zirconia-based complex refractory and heat-insulating material |
| US6773825B2 (en) | 1997-03-31 | 2004-08-10 | Porvair Corporation | Porous articles and method for the manufacture thereof |
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