CN1566021A - Manufacturing method of black zirconia ceramics - Google Patents
Manufacturing method of black zirconia ceramics Download PDFInfo
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- CN1566021A CN1566021A CN 03129087 CN03129087A CN1566021A CN 1566021 A CN1566021 A CN 1566021A CN 03129087 CN03129087 CN 03129087 CN 03129087 A CN03129087 A CN 03129087A CN 1566021 A CN1566021 A CN 1566021A
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- zirconia ceramics
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Abstract
The invention discloses a manufacturing method of black zirconia ceramics which comprises, processing zirconium oxide ceramic powder into work piece blank, subjecting the obtained zirconium oxide to de-waxing, degreasing or low-temperature biscuit firing treatment with no protective atmosphere, then subjecting the pretreated zirconium oxide plain blank work piece to high-sintering under vacuum condition, or filling argon, hydrogen into the evacuated furnace, and conducting high-sintering in protective atmosphere.
Description
Technical field:
The present invention relates to the technical field of ceramic post sintering, specifically a kind of manufacture method of black zirconia ceramics.
Background technology:
Existing black zirconia ceramics is to adopt the base sintering that the interpolation metal oxide is made in Zirconium oxide powder to form, and its shortcoming has: the first, and operation is long, and the production cycle is longer, wants the many operations that add pigment together before the base.Second, the quality control complexity, the addition of pigment and the fluctuation of sintering temperature to sintering after the color reaction sensitivity of goods, the interpolation operation of pigment since bad and introducing unavoidable impurities of compounding effect can cause goods behind the sintering fall phenomenons such as slag, cracking and colour fluctuation, the 3rd, sintered products poor performance, add pigment in a after tested employing powder, hot injection moulding base then, the workpiece that forms of sintering again, density has only 5.3g/cm behind the sintering
3, because too crisp hardness test can not be successful, the workpiece of this technology is from 1.5m
2Height be free to drop down on the cement flooring just broken.
Summary of the invention:
The object of the present invention is to provide a kind of manufacture method of black zirconia ceramics, this method need not added the black finished product that any pigment just can sinter the color even unanimity into before base.
To achieve these goals; technical scheme of the present invention is: a kind of manufacture method of black zirconia ceramics; mainly comprise the zirconia ceramics powder; it is characterized in that: the zirconia ceramics powder is processed into the workpiece base; the white zirconium white workpiece base that is shaped is dewaxed; degreasing or carry out the biscuiting of low temperature unprotect atmosphere and handle; again pretreated zirconium white biscuit workpiece is carried out high temperature sintering under the condition of vacuum; or in the stove that has vacuumized applying argon gas; hydrogen; under shielding gas, carry out high temperature sintering; the boat of putting workpiece during sintering will use graphite material or at graphite boat upper berth one deck graphite paper, put graphite cake or lid layer graphite paper on the workpiece of putting.
The present invention is fairly simple compared with the prior art operation, processing ease, be easy to control, need before base, not add the black goods that any pigment just can sinter uniformity, colour stable into, because operation is short, the chance of contaminating impurity also reduces relatively, moreover, adopted higher temperature sintering, the density and hardness of finished product is also higher, and toughness and impact resistance also improve a lot.
Embodiment:
The invention will be further described below in conjunction with embodiment.
The present invention mainly comprises: mainly comprise the zirconia ceramics powder; it is characterized in that: the zirconia ceramics powder is processed into the workpiece base; the white zirconium white workpiece base that is shaped is dewaxed; degreasing or carry out the biscuiting of low temperature unprotect atmosphere and handle; again pretreated zirconium white biscuit workpiece is carried out high temperature sintering under the condition of vacuum; or in the stove that has vacuumized applying argon gas; hydrogen; under shielding gas, carry out high temperature sintering; the boat of putting workpiece during sintering will use graphite material or at graphite boat upper berth one deck graphite paper; put graphite cake or lid layer graphite paper on the workpiece of putting; temperature during high temperature sintering remains between 1550 ℃ to 1650 ℃; time remained on more than 1 hour; vacuum tightness in the sintering process remains on below the 30pa, the zirconia ceramics powder is processed into the workpiece base can adopts compacting; injection moulding; injection molding method.
In an embodiment of the present invention, with cubic phase PSZ granulation material (specific surface 30m
2/ g) be pressed into (pressure 1.2t/cm
2) ceramic ring of external diameter 33mm * internal diameter 25mm * thick 2.5mm, then ceramic ring underlay graphite paper, loam cake graphite paper are put into the vacuum oven high temperature sintering, the sintering process furnace pressure is not higher than 20pa, temperature control divides five steps in the stove: the first step, with 600 minutes, rise to 1350 ℃ by room temperature, second step, kept 120 minutes at 1350 ℃, in the 3rd step,, temperature is risen to 1610 ℃ by 1350 ℃ with 40 minutes, the 4th step, kept 150 minutes at 1610 ℃, in the 5th step, lower the temperature with stove, after the cooling, take out the intact finished product of sintering.
In another embodiment of the present invention, with specific surface 8m
2/ g, 15m
2/ g, 30m
2The mutually partially stabilized zirconia powder in three kinds of four directions of/g mixed by weight 47.5: 47.5: 5, prepare injection forming feeding (88wt% zirconia powder+12wt% wax-based binder) then, again with feeding injection forming (the material temperature 150 degree/mould temperature 40 degree/injection pressure 50kg/cm that prepare
2), next (process is divided into two steps, the first step with the workpiece of injection forming dewaxing degreasing, from room temperature to 350 ℃, the time spent is 15 hours, second step, from 350 ℃ to 800 ℃, time spent is 5 hours), will be through the workpiece underlay graphite paper after the dewaxing skimming treatment, the loam cake graphite paper is put into the vacuum oven sintering, is the vacuum state below the 20pa in the stove when the temperature below 1000 ℃, when 1000 ℃ of temperature, charge into argon gas to 650pa in stove, temperature control is divided into five steps in the stove: the first step, with 600 minutes, rise to 1350 ℃ by room temperature, second step kept 120 minutes at 1350 ℃, the 3rd step, with 40 minutes, temperature is risen to 1580 ℃ by 1350 ℃, in the 4th step, kept 150 minutes at 1580 ℃, the 5th step, with the stove cooling, after the cooling, take out the intact finished product of sintering.
The every index contrast of finished product of the present invention and prior art finished product is as follows:
| Manufacturing process | Density g/cm3 | Hardness HRA | Fracture toughness property Mpam 1/2 | Shock-resistant degree | |
| Prior art | Add pigment in the powder; hot injection moulding, unprotect atmosphere direct sintering | 5.30～5.33 | Because pressure head is broken once pressing, can't test | ??＜2 | 1.5m highly be free to drop down on the concrete floor just broken |
| The technology of the present invention | Embodiment one | 5.93～5.98 | ?80～83 | ????＞3 | 4 meters highly be free to drop down to can be not broken on the concrete floor |
| Embodiment two | 6.08～6.15 | ?87～91 | ????＞3 | 4 meters highly be free to drop down to can be not broken on the concrete floor |
Can find out obviously that from above every index contrast table every index of the finished product that use the technology of the present invention burns out is better than the finished product that utilizes the prior art sintering to come out.
Claims (4)
1; a kind of manufacture method of black zirconia ceramics; mainly comprise the zirconia ceramics powder; it is characterized in that: the zirconia ceramics powder is processed into the workpiece base; the white zirconium white workpiece base that is shaped is dewaxed; degreasing or carry out the biscuiting of low temperature unprotect atmosphere and handle; again pretreated zirconium white biscuit workpiece is carried out high temperature sintering under the condition of vacuum; or in the stove that has vacuumized applying argon gas; hydrogen; under shielding gas, carry out high temperature sintering; the boat of putting workpiece during sintering will use graphite material or at graphite boat upper berth one deck graphite paper, put graphite cake or lid layer graphite paper on the workpiece of putting.
2, the manufacture method of a kind of black zirconia ceramics according to claim 1 is characterized in that: the temperature during high temperature sintering remains between 1550 ℃ to 1650 ℃, and the time remained on more than 1 hour.
3, the manufacture method of a kind of black zirconia ceramics according to claim 1 is characterized in that: the vacuum tightness in the sintering process remains on below the 30pa.
4, the manufacture method of a kind of black zirconia ceramics according to claim 1 is characterized in that: the zirconia ceramics powder is processed into the workpiece base can adopts compacting, injection moulding, injection molding method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03129087 CN1566021A (en) | 2003-06-16 | 2003-06-16 | Manufacturing method of black zirconia ceramics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03129087 CN1566021A (en) | 2003-06-16 | 2003-06-16 | Manufacturing method of black zirconia ceramics |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1566021A true CN1566021A (en) | 2005-01-19 |
Family
ID=34469215
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|---|---|---|---|
| CN 03129087 Pending CN1566021A (en) | 2003-06-16 | 2003-06-16 | Manufacturing method of black zirconia ceramics |
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| CN (1) | CN1566021A (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101704671B (en) * | 2009-11-27 | 2012-02-08 | 清华大学 | Method for preparing black zirconia ceramics at low temperature |
| CN102659401A (en) * | 2012-04-24 | 2012-09-12 | 邓湘凌 | Manufacturing method for gray zirconia ceramics |
| CN103833355A (en) * | 2014-01-02 | 2014-06-04 | 佛山市东方智柏纳米材料科技有限公司 | Preparation method for black ZrAlYOC ceramic gland die with novel structure |
| CN104003714A (en) * | 2014-01-26 | 2014-08-27 | 湖北国瓷科技有限公司 | Method for preparing cellphone parts in various colors with zirconia ceramics |
| CN104837309A (en) * | 2015-04-16 | 2015-08-12 | 北京赛乐米克材料科技有限公司 | Black ceramic part for use in electronic equipment and manufacturing method therefor |
| CN105198413A (en) * | 2015-10-26 | 2015-12-30 | 沈兴钟 | Manufacturing method of ceramic mosaic |
| CN108863353A (en) * | 2018-06-28 | 2018-11-23 | 东莞信柏结构陶瓷股份有限公司 | black ceramic material and preparation method thereof |
| CN110143816A (en) * | 2019-05-08 | 2019-08-20 | 武汉理工大学 | A kind of Colored zirconia ceramics and preparation method thereof |
| CN110615685A (en) * | 2019-10-09 | 2019-12-27 | 景德镇陶瓷大学 | Black ceramic and preparation method thereof |
| US10737983B2 (en) | 2016-08-31 | 2020-08-11 | Shandong Sinocera Functional Material Co., Ltd. | Black zirconia sintered body and preparation method therefor and use thereof |
-
2003
- 2003-06-16 CN CN 03129087 patent/CN1566021A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101704671B (en) * | 2009-11-27 | 2012-02-08 | 清华大学 | Method for preparing black zirconia ceramics at low temperature |
| CN102659401A (en) * | 2012-04-24 | 2012-09-12 | 邓湘凌 | Manufacturing method for gray zirconia ceramics |
| CN103833355A (en) * | 2014-01-02 | 2014-06-04 | 佛山市东方智柏纳米材料科技有限公司 | Preparation method for black ZrAlYOC ceramic gland die with novel structure |
| CN104003714A (en) * | 2014-01-26 | 2014-08-27 | 湖北国瓷科技有限公司 | Method for preparing cellphone parts in various colors with zirconia ceramics |
| CN104003714B (en) * | 2014-01-26 | 2016-04-27 | 湖北国瓷科技有限公司 | The method of multiple color mobile phone part prepared by a kind of zirconia ceramics |
| CN104837309A (en) * | 2015-04-16 | 2015-08-12 | 北京赛乐米克材料科技有限公司 | Black ceramic part for use in electronic equipment and manufacturing method therefor |
| CN105198413A (en) * | 2015-10-26 | 2015-12-30 | 沈兴钟 | Manufacturing method of ceramic mosaic |
| US10737983B2 (en) | 2016-08-31 | 2020-08-11 | Shandong Sinocera Functional Material Co., Ltd. | Black zirconia sintered body and preparation method therefor and use thereof |
| CN108863353A (en) * | 2018-06-28 | 2018-11-23 | 东莞信柏结构陶瓷股份有限公司 | black ceramic material and preparation method thereof |
| CN110143816A (en) * | 2019-05-08 | 2019-08-20 | 武汉理工大学 | A kind of Colored zirconia ceramics and preparation method thereof |
| CN110615685A (en) * | 2019-10-09 | 2019-12-27 | 景德镇陶瓷大学 | Black ceramic and preparation method thereof |
| CN110615685B (en) * | 2019-10-09 | 2022-03-15 | 景德镇陶瓷大学 | Black ceramic and preparation method thereof |
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