CN1253126A - Low-temp liquid-phase sintered zirconium oxide ceramics with higher toughness - Google Patents

Low-temp liquid-phase sintered zirconium oxide ceramics with higher toughness Download PDF

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CN1253126A
CN1253126A CN 99124033 CN99124033A CN1253126A CN 1253126 A CN1253126 A CN 1253126A CN 99124033 CN99124033 CN 99124033 CN 99124033 A CN99124033 A CN 99124033A CN 1253126 A CN1253126 A CN 1253126A
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CN1081176C (en
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秦海霞
黄校先
张玉峰
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Shanghai Institute of Ceramics of CAS
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Shanghai Institute of Ceramics of CAS
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Abstract

A low-temp. liquid-phase sintered zirconium oxide toughened ceramics features that the CeO2, Y2O3, or CeO2 + Y2O3 is used as stabilizer, the glass phase in MgO-Al2O3-SiO2 system is used as principal component of sintering assistant, and it is sintered at 1220-1450 deg.C. The compact sintered body has high strength (700-930 MPa), toughness (6-12 MPm1/2) and hardness (Hv) (8-11.5GPa). Its advantages are wide range of raw material's granularity from ultrafine to microns, lower sintering temp., wide range of sintering temp. and high mechanical property similar to that of solid-phase sintered same material.

Description

Low-temp liquid-phase sintered zirconium oxide ceramics with higher toughness
The present invention is the toughened zirconia ceramics material of low-temp liquid-phase sintering, belongs to the oxide ceramic material field.
R.C.Garvie in 1975 has found that the partially stabilized zirconia ceramics material of CaO is in breaking-down process, its cubic phase (t) changes the martensitic transformation of monocline phase (m) into, can make material obtain higher intensity and fracture toughness property, start the research field of toughened zirconia ceramics.
Discovering subsequently: use Y 2O 3, CeO 2Deng as stablizer, be more suitable in the toughened zirconia ceramics material.With Y 2O 3, CeO 2Or Y 2O 3+ CeO 2Be stablizer, the superfine powder for preparing with wet chemical methods such as co-precipitation is a raw material, and the cubic phase polycrystal zirconia ceramics of preparation (being called for short TZP) has good mechanical property.Particularly with Y 2O 3For the normal temperature bending strength value of the cubic phase polycrystal zirconia ceramics of stablizer (being called for short Y-TZP) very high; With CeO 2For the toughness and the aging performance of the cubic phase polycrystal zirconia ceramics of stablizer (being called for short Ce-TZP) fine; With Y 2O 3+ CeO 2Be stablizer, the toughened zirconia ceramics comprehensive mechanical performance can be improved.These materials are just obtaining in fields such as communication, machinery, weaving, the energy, sports equipment to use.
But all be to obtain fine and close toughened zirconia ceramics material by 1500-1650 ℃ of high temperature solid-phase sintering at present both at home and abroad, concrete sintering temperature is relevant with the kind and the content of stablizer.This is for the widespread use and the suitability for industrialized production of material, and its subject matter is:
1. employing high temperature solid-phase sintering, the grain size of material are difficult to control;
2. owing to the temperature height of solid state sintering, to the requirement height of equipment, energy consumption is big;
3. solid state sintering need adopt the powder (the powder primary particle size is 30-40nm, aggregate particle size<0.5 μ m) of wet chemical method preparations such as co-precipitation.This powder price height, and powder characteristic is difficult to stablize when producing in enormous quantities.
The present invention is the production technique that adopts general stupalith, comprises pre-treatment, batch mixing, the moulding of raw material, steps such as sintering and performance test, and specific implementation method is:
(1) raw material: superfine powder, commercial oxidation zirconium powder body or the mixed powder of the two that can adopt prepared by co-precipitation.The primary particle size of the powder of prepared by co-precipitation is 30-40nm; The particle diameter of commercial oxidation zirconium powder body is 0.8-2.5 μ m; The blending ratio of the two is 10: 90-90: 10 (weight ratios);
(2) stablizer: comprise CeO 2, Y 2O 3Or the mixing (CeO of the two 2+ Y 2O 3); The add-on of simplification compound is CeO 210-16mol%, Y 2O 31.8-4.0mol%, the two blended ratio is 1: 16~1: 1 (mol ratio), add-on is 3-12mol%;
(3) sintering aid: select MgO-Al for use 2O 3-SiO 2The glass of system is major ingredient, and add-on is 0.2~10wt%;
(4) batch mixing: above-mentioned raw materials, stablizer and sintering aid are adopted dried mixing or wet mixing in required ratio, sieve;
(5) moulding: adopt dry-pressing, etc. isostatic pressing process again after static pressure or the dry-pressing, be pressed into required shape, also available wet moulding;
(6) sintering: normal pressure does not have pressure in 1220-1450 ℃ of temperature range under air atmosphere) sintering;
(7) performance test: carry out bending strength, fracture toughness property and measurement of hardness with the method that stupalith is commonly used, performance is listed in table 1.
The different zirconium white raw materials of table 1 are in the mechanical property of the toughened zirconia ceramics material of differing temps liquid phase sintering
Figure A9912403300051
Fig. 1 is MgO-Al 2O 3-SiO 2The glassy phase of system is the sintering aid of major ingredient, at the photo of sprawling of zirconium surface, shows that it has good wettability to zirconia material, and is favourable to zirconic sintering.
Further illustrate substantive distinguishing features of the present invention and marked improvement below by specific embodiment, it must be emphasized that the present invention is confined to these embodiment absolutely not.
Embodiment 1 utilizes the Zirconium powder of prepared by co-precipitation, and its primary particle size is 30nm, adopts CeO 2And Y 2O 3Mixed stabilizer, both ratios are 1: 10 (mol ratio), and the add-on of sintering aid is 3wt%, and is dry-pressing formed then, and 1350 ℃ of air atmospheres are normal pressure-sintered, and the mechanical property of prepared material is listed in shown in the table 1.
The two mixes the Zirconium powder of embodiment 2 prepared by co-precipitation and commercial oxidation zirconium powder body, and the ratio of mixing is 30: 70 (weight ratio), adopts Y 2O 3Be stablizer, add-on is 3mol%, and the addition of sintering aid is 4wt%, behind the cold isostatic compaction under 1250 ℃ of conditions sintering, all the other conditions such as embodiment 1, prepared material property is as shown in table 1.
Embodiment 3 adopts commercial oxidation zirconium powder body, and its particle diameter is 1.0 μ m, uses CeO 2Be stablizer, add-on is 12mol%, and the add-on of sintering aid is 5wt%, sintering under 1250 ℃ of conditions behind first dry-pressing and then the cold isostatic compaction, and prepared material property is as shown in table 1.

Claims (2)

1. the toughened zirconia ceramics material of a low-temp liquid-phase sintering comprises that stablizer is selected, sintering aid is selected, and it is characterized in that:
1) raw material: the superfine zirconia powder of prepared by co-precipitation, commercial oxidation zirconium powder body or the two are by 10: 90-90: 10 (weight ratios) are mixed;
2) stabilizer type: Y 2O 3, CeO 2Or Y 2O 3+ CeO 2Y 2O 3Add-on is 1.8-4mol%; CeO 2Be 10-16mol%; Both mix add-on is 3-12mol%, and its ratio is 1: 16-1: 1;
3) sintering aid: MgO-Al 2O 3-SiO 2The glassy phase of system is a major ingredient, and add-on is 0.2-10wt%;
4) sintering temperature: 1220-1450 ℃.
2. the toughened zirconia ceramics material of low-temp liquid-phase sintering according to claim 1, the Zirconium powder primary particle size that it is characterized in that prepared by co-precipitation is 30-40nm, the particle diameter of commercial oxidation zirconium powder body is 0.8-2.5 μ m.
CN99124033A 1999-11-19 1999-11-19 Low-temp liquid-phase sintered zirconium oxide ceramics with higher toughness Expired - Fee Related CN1081176C (en)

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003104162A1 (en) * 2002-04-27 2003-12-18 Emerson Electric (China) Holdings Co., Ltd. A shape memory ceramic and a producing method thereof
CN100436372C (en) * 2003-02-28 2008-11-26 住友化学工业株式会社 Zirconium oxide ayglutinating body and producing method thereof
CN101928141A (en) * 2010-08-27 2010-12-29 湖南博深实业有限公司 Liquid phase sintering additive for tetragonal polycrystalline zirconia ceramic material and preparation and application thereof
CN101284904B (en) * 2008-06-06 2011-04-13 王加国 Highly effective, energy-conserving and steam-free type ethoxylation reactor
CN102887706A (en) * 2012-09-17 2013-01-23 上海大学 Cerium stabilized cubic zirconia ceramic material and preparation method thereof
CN101970377B (en) * 2007-11-27 2013-11-06 康宁股份有限公司 Fine porosity low-microcracked ceramic honeycombs and methods thereof
US8853112B2 (en) 2005-03-01 2014-10-07 Saint-Gobain Centre De Recherches Et D'etudes Europeen Sintered bead based on zirconia and on cerium oxide
CN108137414A (en) * 2015-07-30 2018-06-08 法商圣高拜欧洲实验及研究中心 Sintered products based on aluminium oxide and based on zirconium oxide
CN114538921A (en) * 2022-03-18 2022-05-27 中钢集团洛阳耐火材料研究院有限公司 Glass-combined large-size zirconia compact sintered product
CN115286373A (en) * 2022-07-01 2022-11-04 河北新玻尔瓷业有限公司 Waterproof and moistureproof ceramic tile and production process thereof

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4923830A (en) * 1989-09-18 1990-05-08 Swiss Aluminum Ltd. Ceramic bodies formed from partially stabilized zirconia
CN1089249A (en) * 1993-11-15 1994-07-13 天津大学 High-temperature aging resisting and high tenacity PSZ pottery

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003104162A1 (en) * 2002-04-27 2003-12-18 Emerson Electric (China) Holdings Co., Ltd. A shape memory ceramic and a producing method thereof
CN100436372C (en) * 2003-02-28 2008-11-26 住友化学工业株式会社 Zirconium oxide ayglutinating body and producing method thereof
US8853112B2 (en) 2005-03-01 2014-10-07 Saint-Gobain Centre De Recherches Et D'etudes Europeen Sintered bead based on zirconia and on cerium oxide
CN101970377B (en) * 2007-11-27 2013-11-06 康宁股份有限公司 Fine porosity low-microcracked ceramic honeycombs and methods thereof
CN101284904B (en) * 2008-06-06 2011-04-13 王加国 Highly effective, energy-conserving and steam-free type ethoxylation reactor
CN101928141A (en) * 2010-08-27 2010-12-29 湖南博深实业有限公司 Liquid phase sintering additive for tetragonal polycrystalline zirconia ceramic material and preparation and application thereof
CN101928141B (en) * 2010-08-27 2013-02-06 湖南博深实业有限公司 Liquid phase sintering additive for tetragonal polycrystalline zirconia ceramic material and preparation and application thereof
CN102887706A (en) * 2012-09-17 2013-01-23 上海大学 Cerium stabilized cubic zirconia ceramic material and preparation method thereof
CN108137414A (en) * 2015-07-30 2018-06-08 法商圣高拜欧洲实验及研究中心 Sintered products based on aluminium oxide and based on zirconium oxide
CN114538921A (en) * 2022-03-18 2022-05-27 中钢集团洛阳耐火材料研究院有限公司 Glass-combined large-size zirconia compact sintered product
CN114538921B (en) * 2022-03-18 2022-11-29 中钢集团洛阳耐火材料研究院有限公司 Glass-combined large-size zirconia compact sintered product
CN115286373A (en) * 2022-07-01 2022-11-04 河北新玻尔瓷业有限公司 Waterproof and moistureproof ceramic tile and production process thereof

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