CN1298846A - Buffer sinter method for high-hardness, high-strength and high-toughness zirconium oxide ceramics - Google Patents
Buffer sinter method for high-hardness, high-strength and high-toughness zirconium oxide ceramics Download PDFInfo
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- CN1298846A CN1298846A CN 01100463 CN01100463A CN1298846A CN 1298846 A CN1298846 A CN 1298846A CN 01100463 CN01100463 CN 01100463 CN 01100463 A CN01100463 A CN 01100463A CN 1298846 A CN1298846 A CN 1298846A
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Abstract
The present invention relates to a sintering method of zirconium oxide ceramic material for making gauge block. Said method uses box type furnace buffer sintering method including the procedures of drying, degumming, sintering and cooling. Because of raising sintering temperature and heat treatment temperature, it can obtain t+m double phase texture of metastable non equilibrium t phase and equilibrium m phase at room temperature, this double phase texture can obtain veryhigh toughness due to multiphase toughening action of phase change toughening, micro-crack toughening and residual stress toughening. The present invention improves and enhances the mechanical and thermal performances of zirconium oxide ceramics under room temperature to meet the performance requirements of making gauge block.
Description
The present invention relates to the sintering method of zirconia ceramics material.
Existing high temperature resistant, wear-resistant, the corrosion resistant characteristics of zirconia ceramics have high-strength, high-ductility good characteristic again, belong to the engineering structure pottery.Until now, it is an intensity and a highest kind of fracture toughness property under the room temperature in the structural ceramics family, and the gauge block zirconia ceramics material has used its this outstanding advantage just.The industrial preparation of zirconia ceramics material adopts the method for traditional tunnel kiln stoking always: the gauge block blank is at normal temperatures through more than 10 hours, reach 1100 ℃ temperature, afterwards, through 10 hours, sintering temperature rises to 1400 ℃ again, again through 10 hours, makes sintering temperature reach 1700 ℃, through more than 3 hours, be cooled to normal temperature at last.The material that above-mentioned sintering method is produced exists the defective on the following performance: (1) void content height; (2) density is low; (3) hardness is low; (4) intensity is low; (5) the crystalline phase tissue development is unsound.
The object of the present invention is to provide and a kind ofly can improve machinery and thermal property under the zirconia ceramics room temperature, reach the zirconia ceramics material buffer sinter method of the hard high tenacity of the high-strength height of mechanical property.
The technical process and the control condition of buffer sinter method for high-hardness, high-strength and high-toughness zirconium oxide ceramics of the present invention are as follows:
(1) material that sinters into 80% mullite and 20% corundum mixing is made a basket that is complementary with box-type furnace, as fire-resistant chassis; Add 5.2% yttrium oxide and an amount of polyvinyl alcohol glue in the hyperfine micro mist of zirconium white, add-on is advisable product void content＜3%; Gauge block blank with the compression moulding of 200T press, put into fire-resistant chassis, intensive piling up in order, stack thickness is decided on gauge block size and weight, and the thin plate that is fired into zirconium white is gone up on fire-resistant chassis all around, capping oxidation zirconium thin plate again above the chassis;
(2) the gauge block blank evenly is warming up to 100 ℃ by normal temperature through 100min, and keeps constant temperature 90min, carries out drying;
(3) with the temperature rise rate of 1 ℃/min, process 150min makes temperature rise to 250 ℃, and constant temperature 30min, carries out the degumming technology of gauge block blank;
(4) under the condition of filling oxygen, with the temperature rise rate of 1 ℃/min,, make temperature rise to 885 ℃-915 ℃ through 650min, carry out sintering;
(5) pass through the even intensification of 170min again, make temperature reach 1085 ℃-1115 ℃, carry out sintering again;
(6) again with the temperature rise rate of 1 ℃/min,, make sintering temperature rise to 1585 ℃-1615 ℃ through 500min, and constant temperature 30min;
(7) utilize the nature cooling,, and keep constant temperature 60min, finish cooling for the first time to 1085 ℃-1185 ℃;
(8) utilize naturally cooling,, and keep constant temperature 30min, naturally cool to normal temperature once more, finish the secondary cooling to 785 ℃-815 ℃.
The present invention has following effect:
(1) box-type furnace buffering sintering process is oxygenation after dewatering, coming unstuck, and relies on the air oxygenating more abundant than tunnel furnace stoking method;
(2) box-type furnace buffering sintering process keeps through stricter control temperature rise rate and constant temperature than tunnel furnace stoking method, make that agglomerated material internal temperature field is even, form the complex phase phase-change mechanism, thereby breaking tenacity, fracture toughness property are greatly improved under the room temperature, and its main test parameter is as follows: elastic modulus E/Gpa 288; Hardness H/Gpa14.4; Hs113.9 (HV 〉=1200); Density p/gcm
36.0; Linear expansivity α/10
-6K
-19.2.
The specific embodiment of the invention and process explanation are as follows: one, kiln-loading method: with the material that 80% mullite and 20% corundum mixing sinter into, make a basket that is complementary with box-type furnace, use as fire-resistant chassis.In the hyperfine micro mist of zirconium white, add 5.2% yttrium oxide, add an amount of polyvinyl alcohol glue, make product void content＜3%, gauge block blank with the compression moulding of 200T press, put into fire-resistant chassis, orderly intensive piling up, stack thickness is decided on gauge block size and weight, the thin plate that is fired into zirconium white is gone up on fire-resistant chassis all around, capping oxidation zirconium thin plate again above the chassis.Stove is put on this fire-resistant chassis to get final product.Two, sintering method: moulding gauge block blank does not have in the kiln of packing under the external force effect, is warming up to 100 ℃ by normal temperature through 100 minutes, and constant temperature 90 minutes, makes in the moulding gauge block blank moisture content fully remove and avoid blank distortion and cracking; Temperature rise rate with per minute 1 degree was warming up to 250 ℃ through 150 minutes again, constant temperature 30 minutes, and the binding agent that makes in the parison is partly sloughed, and avoids occurring more pockmark and pore; Fill oxygen afterwards, and, heated up 650 minutes,, supply oxygen, make the abundant oxidation of binding agent and complete drainage water and carbonic acid gas, keep good colour, finish the m-t phase transformation with purity oxygen to 900 ℃ with the temperature rise rate that per minute 1 is spent; With 170 minutes time, temperature is risen to 1100 ℃ continue sintering again, afterwards the temperature rise rate of spending with per minute 1, through 500 minutes to 1600 ℃ sintering temperature, and constant temperature 30 minutes, promote and also keep sintering temperature, make the agglomerated material internal temperature even, form the brilliant structure of t+c complex phase; Through after the above sintering process, to the blank naturally cooling, during to 1100 ℃, constant temperature 60 minutes, short its is separated into t+c duplex structure; Treat after the constant temperature time 60 minutes, when continuing to naturally cool to 800 ℃, kept constant temperature 30 minutes again, make its generation, the t-m phase transformation produces pinning effect, further strengthens breaking tenacity; At last, through naturally cooling, gauge block is come out of the stove.At room temperature obtain non-equilibrium meta t and balance m t+m duplex structure mutually owing to improve to burn temperature with thermal treatment temp, this tissue owing to transformation toughening, tiny crack is toughness reinforcing and the toughness reinforcing multiple complex phase toughening effect of unrelieved stress obtains very high toughness.
Claims (8)
- A kind of buffer sinter method for high-hardness, high-strength and high-toughness zirconium oxide ceramics is characterized in that:(1) material that sinters into 80% mullite and 20% corundum mixing is made a basket that is complementary with box-type furnace, as fire-resistant chassis; Add 5.2% yttrium oxide and an amount of polyvinyl alcohol glue in the hyperfine micro mist of zirconium white, add-on is advisable product void content＜3%; Gauge block blank with the compression moulding of 200T press, put into fire-resistant chassis, intensive piling up in order, stack thickness is decided on gauge block size and weight, and all around go up on fire-resistant chassis, the thin plate that is fired into zirconium white, capping oxidation zirconium thin plate again above the chassis;
- (2) the gauge block blank evenly is warming up to 100 ℃ by normal temperature through 100min, and keeps constant temperature 90min, carries out drying;
- (3) with the temperature rise rate of 1 ℃/min, process 150min makes temperature rise to 250 ℃, and constant temperature 30min, carries out the degumming technology of gauge block blank;
- (4) under the condition of filling oxygen, with the temperature rise rate of 1 ℃/min,, make temperature rise to 885 ℃-915 ℃ through 650min, carry out sintering;
- (5) pass through the even intensification of 170min again, make temperature reach 1085 ℃-1115 ℃, carry out sintering again;
- (6) again with the temperature rise rate of 1 ℃/min,, make to rise to 1585 ℃-1615 ℃ of sintering temperatures through 500min, and constant temperature 30min;
- (7) utilize the nature cooling,, and keep constant temperature 60min, finish cooling for the first time to 1085 ℃-1185 ℃;
- (8) utilize naturally cooling,, and keep constant temperature 30min, naturally cool to normal temperature once more, finish the secondary cooling to 785 ℃-815 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01100463 CN1125001C (en) | 2001-01-15 | 2001-01-15 | Buffer sinter method for high-hardness, high-strength and high-toughness zirconium oxide ceramics |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01100463 CN1125001C (en) | 2001-01-15 | 2001-01-15 | Buffer sinter method for high-hardness, high-strength and high-toughness zirconium oxide ceramics |
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| Publication Number | Publication Date |
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| CN1298846A true CN1298846A (en) | 2001-06-13 |
| CN1125001C CN1125001C (en) | 2003-10-22 |
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| CN 01100463 Expired - Fee Related CN1125001C (en) | 2001-01-15 | 2001-01-15 | Buffer sinter method for high-hardness, high-strength and high-toughness zirconium oxide ceramics |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102557626A (en) * | 2011-12-14 | 2012-07-11 | 北京矿冶研究总院 | Preparation method of honeycomb-structure spherical powder material for rare earth modified zirconia thermal barrier coating |
| WO2015043388A1 (en) * | 2013-09-29 | 2015-04-02 | 福建省佳美集团公司 | Sintering process for ceramic sheets |
| CN105174962A (en) * | 2015-09-11 | 2015-12-23 | 杨洋 | High-strength high-temperature titanium ceramic and preparation method thereof |
| CN106977201A (en) * | 2017-03-30 | 2017-07-25 | 南京云启金锐新材料有限公司 | High-purity high-strength high-ductility zirconia composite ceramics ultra thin plate and preparation method thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101228099B (en) * | 2005-07-27 | 2013-01-16 | 株式会社日本触媒 | Method for producing solid electrolyte sheet and solid electrolyte sheet |
-
2001
- 2001-01-15 CN CN 01100463 patent/CN1125001C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102557626A (en) * | 2011-12-14 | 2012-07-11 | 北京矿冶研究总院 | Preparation method of honeycomb-structure spherical powder material for rare earth modified zirconia thermal barrier coating |
| WO2015043388A1 (en) * | 2013-09-29 | 2015-04-02 | 福建省佳美集团公司 | Sintering process for ceramic sheets |
| US9718736B2 (en) | 2013-09-29 | 2017-08-01 | Fujian Jiamei Group Corporation | Sintering process for ceramic sheets |
| CN105174962A (en) * | 2015-09-11 | 2015-12-23 | 杨洋 | High-strength high-temperature titanium ceramic and preparation method thereof |
| CN106977201A (en) * | 2017-03-30 | 2017-07-25 | 南京云启金锐新材料有限公司 | High-purity high-strength high-ductility zirconia composite ceramics ultra thin plate and preparation method thereof |
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| CN1125001C (en) | 2003-10-22 |
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