JPH03237059A - Superplastic deformable zirconium oxide ceramics having high strength - Google Patents
Superplastic deformable zirconium oxide ceramics having high strengthInfo
- Publication number
- JPH03237059A JPH03237059A JP2031960A JP3196090A JPH03237059A JP H03237059 A JPH03237059 A JP H03237059A JP 2031960 A JP2031960 A JP 2031960A JP 3196090 A JP3196090 A JP 3196090A JP H03237059 A JPH03237059 A JP H03237059A
- Authority
- JP
- Japan
- Prior art keywords
- zirconium oxide
- ceramics
- stabilized
- high strength
- superplastic
- 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
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 title claims abstract description 8
- 229910001928 zirconium oxide Inorganic materials 0.000 title claims abstract description 8
- 239000011224 oxide ceramic Substances 0.000 title claims abstract 4
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [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 abstract description 16
- 150000001875 compounds Chemical class 0.000 claims abstract description 11
- 239000002245 particle Substances 0.000 claims description 9
- 239000011230 binding agent Substances 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 abstract description 20
- 229910044991 metal oxide Inorganic materials 0.000 abstract description 7
- 150000004706 metal oxides Chemical class 0.000 abstract description 7
- 239000005368 silicate glass Substances 0.000 abstract description 6
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 3
- -1 Y2O3 and MgO Chemical class 0.000 abstract description 2
- 230000000087 stabilizing effect Effects 0.000 abstract description 2
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 abstract description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract 2
- 229910052710 silicon Inorganic materials 0.000 abstract 2
- 239000010703 silicon Substances 0.000 abstract 2
- 238000000034 method Methods 0.000 abstract 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 11
- 239000013078 crystal Substances 0.000 description 9
- 239000000843 powder Substances 0.000 description 9
- 238000012360 testing method Methods 0.000 description 6
- 238000005245 sintering Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 2
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野）
この発明は、高強度を有し、かつ超塑性変形が可能な酸
化ジルコニウム（以下Ｚ ｒ ０２で示す）系セラミッ
クスに関するものである。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to zirconium oxide (hereinafter referred to as Z r 02) ceramics that have high strength and are capable of superplastic deformation.
従来、例えば自動車エンジンなどの内燃機関の構造部材
の製造に超塑性変形性Ｚ ｒ Ｏ２セラミツクスを用い
る試みがなされている。Previously, attempts have been made to use superplastically deformable Z r O2 ceramics in the manufacture of structural members for internal combustion engines, such as automobile engines.
また、上記超塑性変形性Ｚ ｒ Ｏ２セラミツクスか、
例えば特開昭６２−９１．４８０号公報に記載される通
り、平均粒径： ０．０５〜３μｍを有する部分安定化
ＺｒＯ２、すなわちＹ２Ｏ３，ＭｇＯ，ＣａＯあるいは
Ｃｅ Ｏ２などの安定化金属酸化物を含有させることに
より正方晶と立法晶か共存した組織としたＺ ｒ Ｏ２
で構成されていることも知られている。Moreover, the above-mentioned superplastic deformable Z r O2 ceramics,
For example, as described in JP-A No. 62-91.480, partially stabilized ZrO2 having an average particle size of 0.05 to 3 μm, that is, a stabilized metal oxide such as Y2O3, MgO, CaO or CeO2, is used. By including Z r O2, a structure in which tetragonal crystal and cubic crystal coexist was created.
It is also known that it consists of
一方、近年の各種機関の高性能化および高速化、さらに
省力化に伴ない、構造部材の軽量化（小型化および薄肉
化）が強く望まれ、かつその形状が複雑化する傾向にあ
るが、上記の従来超塑性変形性Ｚ ｒ Ｏ２セラミツク
スは、十分な強度を具備するものでないために、これら
の要求および傾向に満足な対応ができないのが現状であ
る。On the other hand, as the performance and speed of various engines have increased in recent years, as well as labor savings, there has been a strong desire for structural members to be lighter (smaller and thinner), and their shapes are becoming more complex. The conventional superplastically deformable Z r O2 ceramics described above do not have sufficient strength, and therefore cannot satisfactorily meet these demands and trends.
そこで、本発明者等は、上述のような観点から、高強度
を有し、かつ塑性変形性にもすぐれたセラミックスを開
発すべく、特にＺ ｒ ０２セラミツクスに着目し研究
を行なった結果、原料粉末として、Ｙ ＯＭｇＯ，Ｃ
ａｂ、あるいはＣｅ Ｏ２な２３″
どの安定化金属酸化物を１〜１６ＩＩＩＯρ％の範囲内
の所定の割合で含有させて結晶形を正方晶とすると共に
、いずれも平均粒径で０．１即以下に微細化した安定化
正方晶Ｚ ｒ Ｏ２粉末および酸化けい素（以下Ｓ Ｉ
Ｏ２で示す）県北合物粉末、望ましくはけい酸塩ガラ
ス粉末を用い、これら両粉末を所定の割合に配合し、通
常の条件で、混合し、圧粉体に成形し、焼結すると、焼
結時に安定化正方晶Ｚ ｒ Ｏ２中に含有する安定化金
属酸化物がＳｉＯ基化合物中に拡散し、かつＳ ｔ ０
２基化合物は安定化正方晶Ｚ ｒ ０２に対するぬれ性
にもすぐれているので、すぐれた焼結性を示し、さらに
ＳｉＯ県北合物には安定化正方晶Ｚ ｒ Ｏ２の粒成長
を抑制し、かつこれによって単斜晶への変態を抑制する
作用があるので、前記安定化正方晶Ｚ ｒ Ｏ２の焼結
前後および焼結時の結晶構造か一貫して正方晶を維持す
る、すなわち安定化正方晶Ｚ ｒ Ｏ２を微細な粒径に
維持することによって焼結時の変態発生がなくなること
と含まって、この結果製造された、安定化正方晶Ｚ ｒ
Ｏ２からなる分散相と、５ｌＯ２基化合物からなる結
合相とで構成されたＺ ｒ Ｏ２系セラミツクスは、き
イつめて高い強度をもつようになり、さらに結合相を構
成するＳ ｉＯ２基化合物は著しくすぐれた塑性変形性
を有するので、分散相を構成する安定化正方晶Ｚｒ○２
が微細であることと含まって、超塑性変形が可能である
という研究結果を得たのである。Therefore, from the above-mentioned viewpoint, the present inventors conducted research focusing on Zr02 ceramics in order to develop ceramics with high strength and excellent plastic deformability. As a powder, Y OMgO,C
ab, or CeO2, etc., in a predetermined proportion within the range of 1 to 16IIIOρ% to make the crystal form tetragonal, and the average particle size of both is 0.1 or less. Stabilized tetragonal ZrO2 powder and silicon oxide (hereinafter referred to as S I
Using Kenhoku compound powder (denoted as O2), preferably silicate glass powder, blending these powders in a predetermined ratio, mixing under normal conditions, molding into a green compact, and sintering. During sintering, the stabilized metal oxide contained in the stabilized tetragonal Z r O2 diffuses into the SiO-based compound, and S t 0
Since the two-base compound has excellent wettability to the stabilized tetragonal Z r 02, it exhibits excellent sinterability, and furthermore, it suppresses the grain growth of the stabilized tetragonal Z r 02 in the SiO Kenhokuai compound. , and this has the effect of suppressing the transformation to monoclinic, so that the crystal structure of the stabilized tetragonal Z r O2 before and during sintering consistently maintains the tetragonal structure, that is, stabilized The resulting stabilized tetragonal Z r
ZrO2-based ceramics, which are composed of a dispersed phase consisting of O2 and a binder phase consisting of a 5lO2-based compound, have become tightly packed and have high strength. Because it has excellent plastic deformability, the stabilized tetragonal Zr○2 that constitutes the dispersed phase
The research results showed that superplastic deformation is possible, including the fact that the particles are minute.
この発明は、上記研究結果にもとづいてなされたもので
あって、
平均粒径：０．５μｍ以下の安定化正方晶Ｚ ｒ Ｏ２
からなる分散相を主体とし、残りの結合相が０．５〜７
重量％の５Ｉ０２基化合物で構成された高強度を有する
超塑性女形性Ｚ ｒ Ｏ２系セラミツクスに特徴を有す
るものである。This invention was made based on the above research results, and includes stabilized tetragonal Z r O2 with an average particle size of 0.5 μm or less.
The main component is a dispersed phase consisting of 0.5 to 7
It is characterized by superplastic feminoid Z r O2 ceramics having high strength and composed of 5I02 group compounds in the weight percent.
なお、この発明のセラミックスにおいて、分散相を構成
する安定化正方晶Ｚ ｒ ０２の平均粒径を０．５坤以
下にしたのは、その平均粒径が０．５ｕｒｒｌを越える
と塑性変形性に低下傾向が現われるようになって高度の
超塑性変形を確保することができないばかりでなく、強
度も低下するようになるという理由によるものであり、
また結合相を構成する５ＩＯ２基化合物の含有量を０．
５〜７重量％と限定したのは、その含有量が０．５重塁
％未満では、所望の高強度を確保することができないと
共に、さらに−段の塑性変形性の向上も見られず、一方
その含有量か７重量％を越えると、焼結時における安定
化正方晶Ｚ ｒ Ｏ２中の安定化金属酸化物のＳ ｉＯ
２基化合物中への拡散が過度に進行し、この結果前記Ｚ
ｒ Ｏ２中の前記安定化金属酸化物の含有量が少なく
なりすぎ、結晶形が不安定となり、セラミックス強度低
下の原因となる変態を起し易くなるという理由にもとづ
くものである。In addition, in the ceramics of this invention, the average grain size of the stabilized tetragonal Z r 02 constituting the dispersed phase is set to 0.5 urr or less because plastic deformability occurs when the average grain size exceeds 0.5 urrl. This is because not only is it not possible to secure a high degree of superplastic deformation due to a decreasing tendency, but also the strength begins to decrease.
In addition, the content of the 5IO2 group compound constituting the bonded phase was set to 0.
The reason why it is limited to 5 to 7% by weight is that if the content is less than 0.5% by weight, the desired high strength cannot be ensured, and furthermore, no improvement in the plastic deformability of the second stage can be observed. On the other hand, if the content exceeds 7% by weight, the stabilized metal oxide SiO in the stabilized tetragonal ZrO2 during sintering
Diffusion into the two-base compound progresses excessively, and as a result, the Z
This is based on the reason that if the content of the stabilizing metal oxide in rO2 becomes too small, the crystal form becomes unstable and transformation, which causes a decrease in the strength of the ceramic, is likely to occur.
つぎに、この発明のセラミックスを実施例により具体的
に説明する。Next, the ceramics of the present invention will be specifically explained using examples.
原料粉末として、第１表に示される平均粒径、安定化金
属酸化物含有量、および結晶形の４種のＺ ｒ Ｏ２粉
末、並びに同じく第１表に示される平均粒径および成分
組成をもった４種のけい酸塩ガラス粉末を用意し、これ
ら原料粉末を同じく第１表に示される配合割合に配合し
、ボールミル中で７２時時間式混合し、乾燥した後、１
ｔｏｎ／ｃｄの圧力で圧粉体にプレス成形し、ついてこ
の圧粉体を、大気中、温度：１３００°Ｃに２時間保持
の条件で焼結することにより、４ｍｍＸ４ｍｍＸ１００
ｍｍの寸法をもった抗折力（強度）測定用および７ｍ
ｍＸ７ｍｍＸ７ｍｍの寸法をもった塑性変形性測定用の
本発明セラミックス１〜７および比較セラミックス１〜
４をそれぞれ製造した。As raw material powders, four types of Z r O2 powders with the average particle size, stabilized metal oxide content, and crystal form shown in Table 1 were used, as well as the average particle size and component composition also shown in Table 1. Four types of silicate glass powders were prepared, these raw material powders were blended in the proportions shown in Table 1, mixed for 72 hours in a ball mill, dried, and then
By press-forming into a compact with a pressure of ton/cd, and then sintering this compact in the atmosphere at a temperature of 1300°C for 2 hours, a 4mm x 4mm x 100mm
For transverse rupture force (strength) measurement with dimensions of mm and 7 m
Ceramics 1 to 7 of the present invention and comparative ceramics 1 to 7 for measuring plastic deformability with dimensions of mX7mmX7mm
4 were produced respectively.
なお、比較セラミックス１〜４は、いずれも結合相を構
成するけい酸塩ガラスを含ＨＬないもの、あるいはこれ
を含有してもその含有量がこの発明の範囲から高い方に
外れたものである。In addition, Comparative Ceramics 1 to 4 all do not contain HL of silicate glass constituting the binder phase, or even if they do contain it, the content is higher than the range of the present invention. .
ついで、この結果得られた各種のセラミックスについて
、分散相を構成するＺ ｒ Ｏ２の結晶形および平均粒
径、並びに結合相を構成するけい酸塩ガラスの含有量を
測定した。Next, for the various ceramics obtained as a result, the crystal form and average particle size of Z r O2 constituting the dispersed phase and the content of silicate glass constituting the binder phase were measured.
また、抗折力は、インストロン型試験機を用い、これに
上記の４ ｍｍ Ｘ ４ ｍｍ Ｘ １００ｍｍ＋の寸
法をもった試料片を立設し、これの上下方向から１１０
０℃の温度に加熱した状態で０．５ｍｍ／ｍｉｎの速さ
で圧ｆして、４０ＩＩＩ１１の長さまで塑性変形し、こ
の塑性変形後の試料片から３ｍｍＸ４ｍｍＸ４０ｍｍの
寸法をもった試験片を切り出し、これを用いて測定した
。The transverse rupture strength was measured by using an Instron type testing machine, setting up the sample piece with the above dimensions of 4 mm x 4 mm x 100 mm+, and measuring 110 mm from the top and bottom of the sample piece.
Pressure f at a speed of 0.5 mm/min in a state heated to a temperature of 0 ° C. to plastically deform it to a length of 40III11, cut out a test piece with dimensions of 3 mm x 4 mm x 40 mm from this sample piece after plastic deformation, This was used for measurement.
さらに、塑性変形性試験は、同じくインストロン型試験
機を用い、上記の７ｍｍＸ７ｍｍＸ７ｍ＋ｎの司法をも
った試験片を１２００℃に加熱した状態で、０．１ｍｒ
＠／＋ｎｉｎの速さで圧下し、これに割れが発生した時
点の厚さ：ｔを測定することにより行ない、Ｔ／１ｘ１
ｏｏ （％）を求め（Ｔは試験前の厚さ（７ｍｍ）を
示す）、塑性変形性を評価した。これらの結果を第２表
に示した。Furthermore, the plastic deformability test was conducted using the same Instron type testing machine, with the above 7mm x 7mm x 7m+n test piece heated to 1200°C, and heated to 0.1 mr.
This is done by rolling down at a speed of @/+nin and measuring the thickness: t at the point where cracks occur, T/1x1
oo (%) was determined (T indicates the thickness (7 mm) before the test), and the plastic deformability was evaluated. These results are shown in Table 2.
第１表および第２表に示される結果から、本発明セラミ
ックス１〜７は、いずれも結合相を構成するけい酸塩ガ
ラスを全く含有しない比較セラミックス１，２に比して
高強度を有し、かつ−段と塑性変形性にもすぐれ、超塑
性変形が可能であることを示しており、一方比較セラミ
ックス３４に見られるように、結合相の含有量がこの発
明の範囲から高い方に外れると、分散相を構成するＺ
ｒ Ｏ２中の安定化金属酸化物の結合相への拡散移動が
過度に進み、この結果Ｚ ｒ Ｏ２の結晶形が不安定と
なって正方晶と単斜晶の混在した状態となり、強度か低
下するようになることか明らかである。From the results shown in Tables 1 and 2, ceramics 1 to 7 of the present invention all have higher strength than comparative ceramics 1 and 2, which do not contain any silicate glass constituting the binder phase. , and also have excellent plastic deformability, indicating that superplastic deformation is possible.On the other hand, as seen in Comparative Ceramic 34, the content of the binder phase is higher than the range of the present invention. and Z constituting the dispersed phase
The diffusion movement of the stabilized metal oxide in rO2 to the binder phase progresses excessively, and as a result, the crystal form of ZrO2 becomes unstable, resulting in a mixed state of tetragonal and monoclinic crystals, resulting in a decrease in strength. It is clear that this will become the case.
上述のように、この発明のセラミックスは、高強度と超
塑性変形性を兼ね備えているので、これを各種構造部材
の製造に適用した場合、軽量化および形状複雑化をはか
ることが可能となるなど工業上有用な特性を有するので
ある。As mentioned above, the ceramics of this invention have both high strength and superplastic deformability, so when applied to the manufacture of various structural members, it is possible to reduce weight and create complex shapes. It has industrially useful properties.
Claims (1)
ルコニウムからなる分散相を主体とし、残りの結合相が
０．５〜７重量％の酸化けい素基化合物からなることを
特徴とする高強度を有する超塑性変形性酸化ジルコニウ
ム系セラミックス。(1) Average particle size: Mainly composed of a dispersed phase consisting of stabilized tetragonal zirconium oxide with an average particle size of 0.5 μm or less, and the remaining binder phase consists of 0.5 to 7% by weight of a silicon oxide-based compound. A superplastically deformable zirconium oxide ceramic with high strength.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2031960A JPH03237059A (en) | 1990-02-13 | 1990-02-13 | Superplastic deformable zirconium oxide ceramics having high strength |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2031960A JPH03237059A (en) | 1990-02-13 | 1990-02-13 | Superplastic deformable zirconium oxide ceramics having high strength |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH03237059A true JPH03237059A (en) | 1991-10-22 |
Family
ID=12345528
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2031960A Pending JPH03237059A (en) | 1990-02-13 | 1990-02-13 | Superplastic deformable zirconium oxide ceramics having high strength |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH03237059A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1995029141A1 (en) * | 1994-04-22 | 1995-11-02 | Shinagawa Refractories Co., Ltd. | Zirconia sinter, process for producing the same, grinding part material, and orthodontic bracket material |
| CN102482162A (en) * | 2009-08-21 | 2012-05-30 | 株式会社则武 | Zirconia sintered body, and mixture, pre-sintered compact and pre-sintered calcined body for sintering zirconia sintered body |
| US8987157B2 (en) | 2010-08-20 | 2015-03-24 | Noritake Co., Limited | Sintered zirconia, and composition for sintering and calcined body therefor |
| CN115894016A (en) * | 2022-12-14 | 2023-04-04 | 圣泉(扬州)新材料科技有限公司 | Preparation method of zirconia ceramic |
-
1990
- 1990-02-13 JP JP2031960A patent/JPH03237059A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1995029141A1 (en) * | 1994-04-22 | 1995-11-02 | Shinagawa Refractories Co., Ltd. | Zirconia sinter, process for producing the same, grinding part material, and orthodontic bracket material |
| US5656564A (en) * | 1994-04-22 | 1997-08-12 | Shinagawa Refractories Co., Ltd. | Zirconia-based sinter, process for producing the same, gringing part material, and bracket material for dental correction |
| CN102482162A (en) * | 2009-08-21 | 2012-05-30 | 株式会社则武 | Zirconia sintered body, and mixture, pre-sintered compact and pre-sintered calcined body for sintering zirconia sintered body |
| EP2468699A1 (en) * | 2009-08-21 | 2012-06-27 | Noritake Co., Limited | Zirconia sintered body, and mixture, pre-sintered compact and pre-sintered calcined body for sintering zirconia sintered body |
| EP2468699A4 (en) * | 2009-08-21 | 2013-06-05 | Noritake Co Ltd | Zirconia sintered body, and mixture, pre-sintered compact and pre-sintered calcined body for sintering zirconia sintered body |
| US8877664B2 (en) | 2009-08-21 | 2014-11-04 | Noritake Co., Limited | Zirconia sintered body, and mixture, pre-sintered compact and pre-sintered calcined body for sintering zirconia sintered body |
| US8987157B2 (en) | 2010-08-20 | 2015-03-24 | Noritake Co., Limited | Sintered zirconia, and composition for sintering and calcined body therefor |
| CN115894016A (en) * | 2022-12-14 | 2023-04-04 | 圣泉(扬州)新材料科技有限公司 | Preparation method of zirconia ceramic |
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