CN105272177A - Preparation method of aluminum oxide sintered body - Google Patents
Preparation method of aluminum oxide sintered body Download PDFInfo
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- CN105272177A CN105272177A CN201510757855.3A CN201510757855A CN105272177A CN 105272177 A CN105272177 A CN 105272177A CN 201510757855 A CN201510757855 A CN 201510757855A CN 105272177 A CN105272177 A CN 105272177A
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- aluminum oxide
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Abstract
The invention relates to a preparation method of an aluminum oxide sintered body. The preparation method includes the steps that aluminum oxide powder, deionized water and binder rho-aluminum oxide are evenly mixed and stirred and placed in a bag, stand still for 12-15 h in a sealed mode, and are placed in a die in a filled mode and subjected to pressure maintaining for 60-150 s at the pressure of 50-80 MPa, preformed cakes are subjected to vacuum sealed packaging and then placed on an isostatic cool pressing machine for isostatic cool pressing, finally, the cakes obtained after isostatic cool pressing are placed in a microwave sintering furnace for vacuum sintering, and then the aluminum oxide sintered body is obtained. The density of the sintered body is larger than 3.75 g/cm<3>, and the purity of the sintered body is larger than 5 N. According to the method, the purity of powder can be effectively controlled, cost is low, industrial production is easy, and high practical application value is achieved.
Description
Technical field
The present invention relates to the preparation method of alumina sintered body, particularly the preparation method of a kind of high-compactness, high-purity alumina sintered body.
Background technology
Sapphire crystal possesses excellent optics, machinery, chemistry and electrical property, is widely used in the fields such as military infrared equipment, guided missile, submarine, satellite spatial technology, detection and high power strong laser, microelectronics, photoelectron, semi-conductor, optical communication, information displaying (especially blue, White-light LED illumination industry provides window material).High purity aluminium oxide sintered compact is the starting material of sapphire crystallization, compared to directly using high purity alumina powder to carry out sapphire crystallization, adopt high purity aluminium oxide sintered compact can increase substantially the tamped density of long brilliant stove as raw material, density is higher, its tamped density is larger, reduces costs.
Preparing the conventional method of the method for high purity aluminium oxide sintered compact is at present the dry-pressing formed and constant-pressure and high-temperature sintering of punching block.Chinese patent literature CN104250017A discloses a kind of shaping method of LED sapphire single-crystal high purity aluminium oxide, the method is in order to obtain the high aluminum oxide cake of purity, do not add any binding agent directly dry-pressing formed, the method purity is high, technique is simple, but only to use dry-pressing formed, density is very low, can not ensure high-compactness; Chinese patent literature CN102581929A discloses a kind of preparation method of high purity aluminium oxide biscuit, adopts isostatic cool pressing method shaping, and then with constant-pressure and high-temperature sintering, although ensure that aluminum oxide biscuit density, aluminum oxide purity is very low.So for the problems of the prior art, the preparation technology that exploitation can reach the alumina sintered body that density is high and purity is high is very necessary.
Summary of the invention
In view of the deficiency of current technology, the object of the invention is to, by the optimization to forming technology and sintering process, provide a kind of preparation method of alumina sintered body, make the alumina sintered body prepared have high-compactness, highly purified advantage simultaneously.
Technical scheme
The preparation method of alumina sintered body of the present invention is: by aluminum oxide powder, deionized water and binding agent ρ-aluminum oxide mixing and stirring, then after putting into sack sealing and standing 12 ~ 15h, insert again in mould, with 50 ~ 80MPa pressurize, 60 ~ 150s on briquetting press, isostatic cool pressing on cold isostatic press is put into by after preformed cake block vacuum sealed package, finally the cake block obtained after isostatic cool pressing is put into microwave agglomerating furnace vacuum sintering, to obtain final product.
Described binding agent ρ-aluminum oxide is vacuum hydro-extraction preparation, and its content is higher than 70%, and purity is greater than 5N.
The churning time of described mix and blend is 5 ~ 8h, and rotating speed is 20 ~ 50r/min.The stirring rake top layer spraying PTFE of mix and blend, teeter column's liner is polythene material, and its advantage does not contact with other metallic impurity in whipping process, can ensure the purity of material.
The pressure of described isostatic cool pressing is 150 ~ 300MPa, and the time is 100 ~ 300s.
The sack that the sack of described sealing and standing and isostatic cool pressing vacuumize is polyethylene plastic bag, can effectively prevent introduced contaminants contaminated samples, ensures purity.The advantage of isostatic cool pressing be improve shaping after cake block density, reduce the quantity of pore in cake block, be conducive to sintering densification.
The vacuum tightness of described vacuum sintering is 1 ~ 2Pa.
Described vacuum sintering was divided into for four stages: the first stage is warming up to 300 ~ 350 DEG C with the speed of 8 ~ 10 DEG C/min; Subordinate phase is warming up to 1000 ~ 1400 DEG C with the speed of 13 ~ 15 DEG C/min; Phase III is at this temperature 1 ~ 3h; Finally lower the temperature with stove.Its microwave sintering inner lining of furnace and corundum crucible are high-purity 99% alumina material.The advantage of vacuum sintering is a gaseous volatilization being conducive in pore, is conducive to the density improving sintered compact; Two are beneficial to the impurity volatilization in sintered compact, improve the purity of sintered compact.
The purity of the finally prepd alumina sintered body of the present invention is greater than 99.999%, density is greater than 3.75g/cm
3.The microscopic appearance of its last sintered compact section as shown in Figure 2.
Advantage of the present invention: (1) whole process can not contact any metallic impurity, can be good at controlling purity, ensures that purity is at more than 5N.(2) cold isostatic compaction and vacuum microwave sinter, and can obtain the sintered compact that density is very high.(3) under vacuum condition, can sintering temperature be reduced, reduce cost, be easy to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of alumina sintered body of the present invention;
Fig. 2 is the microscopic appearance figure of alumina sintering body section of the present invention.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described further.
As shown in Figure 1, 2, Fig. 1 is the process flow sheet of alumina sintered body of the present invention, and Fig. 2 is the microscopic appearance figure of the alumina sintering body section that the present invention obtains.
Embodiment 1
By aluminum oxide powder, deionized water and binding agent ρ-aluminum oxide, mix and blend 5h (rotating speed 50r/min), put into pouch seal and leave standstill 12h, insert in mould, with 50MPa pressurize 100s on briquetting press, put into after preformed cake block vacuum sealed package on cold isostatic press with 200MPa pressurize 300s, cake block after isostatic cool pressing is put into microwave agglomerating furnace vacuum sintering, and (vacuum tightness is 1 ~ 2Pa, and vacuum sintering was divided into for four stages: the first stage is warming up to 300 DEG C with the speed of 8 ~ 10 DEG C/min; Subordinate phase is warming up to 1200 DEG C with the speed of 13 ~ 15 DEG C/min; Phase III is at this temperature 3h; Finally lower the temperature with stove.), obtaining density is 3.75g/cm
3, purity 5N alumina sintered body (purity test report in table 1).
Embodiment 2
By aluminum oxide powder, deionized water and binding agent ρ-aluminum oxide, mix and blend 7h (rotating speed 50r/min), put into pouch seal and leave standstill 12h, insert in mould, with 70MPa pressurize 100s on briquetting press, put into after preformed cake block vacuum sealed package on cold isostatic press with 250MPa pressurize 300s, cake block after isostatic cool pressing is put into microwave agglomerating furnace vacuum sintering, and (vacuum tightness is 1 ~ 2Pa, and vacuum sintering was divided into for four stages: the first stage is warming up to 320 DEG C with the speed of 8 ~ 10 DEG C/min; Subordinate phase is warming up to 1300 DEG C with the speed of 13 ~ 15 DEG C/min; Phase III is at this temperature 3h; Finally lower the temperature with stove.), obtaining density is 3.81g/cm
3, purity 5N alumina sintered body.
Embodiment 3
By aluminum oxide powder, deionized water and binding agent ρ-aluminum oxide, mix and blend 8h (rotating speed 50r/min), put into pouch seal and leave standstill 12h, insert in mould, with 80MPa pressurize 100s on briquetting press, put into after preformed cake block vacuum sealed package on cold isostatic press with 300MPa pressurize 300s, cake block after isostatic cool pressing is put into microwave agglomerating furnace vacuum sintering, and (vacuum tightness is 1 ~ 2Pa, and vacuum sintering was divided into for four stages: the first stage is warming up to 350 DEG C with the speed of 8 ~ 10 DEG C/min; Subordinate phase is warming up to 1400 DEG C with the speed of 13 ~ 15 DEG C/min; Phase III is at this temperature 3h; Finally lower the temperature with stove.), obtain density 3.85g/cm
3, purity 5N alumina sintered body.
The elemental composition table of the alumina sintered body that table 1 embodiment 1 is obtained
Claims (5)
1. the preparation method of an alumina sintered body, it is characterized in that, by aluminum oxide powder, deionized water and binding agent ρ-aluminum oxide mixing and stirring, then after putting into sack sealing and standing 12 ~ 15h, insert again in mould, with 50 ~ 80MPa pressurize, 60 ~ 150s on briquetting press, put into isostatic cool pressing on cold isostatic press by after preformed cake block vacuum sealed package, finally the cake block obtained after isostatic cool pressing is put into microwave agglomerating furnace vacuum sintering, to obtain final product;
The content of described binding agent ρ-aluminum oxide is higher than 70%, and purity is greater than 5N.
2. the preparation method of alumina sintered body according to claim 1, is characterized in that, the churning time of described mix and blend is 5 ~ 8h, and rotating speed is 20 ~ 50r/min.
3. the preparation method of alumina sintered body according to claim 1, is characterized in that, the pressure of described isostatic cool pressing is 150 ~ 300MPa, and the time is 100 ~ 300s.
4. the preparation method of alumina sintered body according to claim 1, is characterized in that, the vacuum tightness of described vacuum sintering is 1 ~ 2Pa.
5. the preparation method of the alumina sintered body according to any one of Claims 1-4, is characterized in that, described vacuum sintering was divided into for four stages: the first stage is warming up to 300 ~ 350 DEG C with the speed of 8 ~ 10 DEG C/min; Subordinate phase is warming up to 1000 ~ 1400 DEG C with the speed of 13 ~ 15 DEG C/min; Phase III is at this temperature 1 ~ 3h; Finally lower the temperature with stove.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105834424A (en) * | 2016-05-17 | 2016-08-10 | 昆明理工大学 | Method for agglomerating ferromanganese alloy powder through microwave sintering |
| CN106587940A (en) * | 2016-12-02 | 2017-04-26 | 有研亿金新材料有限公司 | High-purity compact magnesium oxide target material and preparation method thereof |
| CN107619264A (en) * | 2017-10-16 | 2018-01-23 | 深圳市商德先进陶瓷股份有限公司 | Aluminium oxide ceramic substrate and its preparation method and application |
| CN108117380A (en) * | 2017-12-14 | 2018-06-05 | 上海卡贝尼精密陶瓷有限公司 | A kind of forming and sintering method of overlength aluminium oxide ceramics pole |
| CN110802052A (en) * | 2019-10-14 | 2020-02-18 | 江苏吉星新材料有限公司 | Method for removing boron carbide on rough surface of sapphire substrate |
| CN112174177A (en) * | 2020-10-13 | 2021-01-05 | 中国铝业股份有限公司 | Hydraulic alumina and preparation method thereof |
| CN113146804A (en) * | 2021-04-20 | 2021-07-23 | 江苏泰州麦迪医疗科技有限公司 | Ceramic femoral stem prosthesis manufacturing method and forming tool |
| CN113511885A (en) * | 2021-08-03 | 2021-10-19 | 苏州楚翰真空科技有限公司 | Method and system for sintering ceramic material |
| CN115321990A (en) * | 2022-09-09 | 2022-11-11 | 山东倍辰新材料有限公司 | Preparation process of microwave sintered ceramic slag remover |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1724465A (en) * | 2005-06-03 | 2006-01-25 | 中国科学院上海硅酸盐研究所 | The yttrium aluminum garnet transparent ceramic material and the preparation method of codope |
| US20090142590A1 (en) * | 2007-12-03 | 2009-06-04 | General Electric Company | Composition and method |
| CN102173756A (en) * | 2011-01-30 | 2011-09-07 | 河北恒博精细陶瓷材料有限公司 | Preparation method of high-purity aluminum oxide sintered body for growing sapphire crystal |
| CN102659392A (en) * | 2012-04-24 | 2012-09-12 | 中国铝业股份有限公司 | Preparation method of calcined alumina powder for black ceramics |
| CN104326751A (en) * | 2014-07-01 | 2015-02-04 | 郑州大学 | Microwave sintering method of ZTA ceramic |
-
2015
- 2015-11-09 CN CN201510757855.3A patent/CN105272177B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1724465A (en) * | 2005-06-03 | 2006-01-25 | 中国科学院上海硅酸盐研究所 | The yttrium aluminum garnet transparent ceramic material and the preparation method of codope |
| US20090142590A1 (en) * | 2007-12-03 | 2009-06-04 | General Electric Company | Composition and method |
| CN102173756A (en) * | 2011-01-30 | 2011-09-07 | 河北恒博精细陶瓷材料有限公司 | Preparation method of high-purity aluminum oxide sintered body for growing sapphire crystal |
| CN102659392A (en) * | 2012-04-24 | 2012-09-12 | 中国铝业股份有限公司 | Preparation method of calcined alumina powder for black ceramics |
| CN104326751A (en) * | 2014-07-01 | 2015-02-04 | 郑州大学 | Microwave sintering method of ZTA ceramic |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105834424A (en) * | 2016-05-17 | 2016-08-10 | 昆明理工大学 | Method for agglomerating ferromanganese alloy powder through microwave sintering |
| CN106587940B (en) * | 2016-12-02 | 2020-03-27 | 有研亿金新材料有限公司 | High-purity compact magnesium oxide target material and preparation method thereof |
| CN106587940A (en) * | 2016-12-02 | 2017-04-26 | 有研亿金新材料有限公司 | High-purity compact magnesium oxide target material and preparation method thereof |
| CN107619264A (en) * | 2017-10-16 | 2018-01-23 | 深圳市商德先进陶瓷股份有限公司 | Aluminium oxide ceramic substrate and its preparation method and application |
| CN107619264B (en) * | 2017-10-16 | 2020-04-03 | 深圳市商德先进陶瓷股份有限公司 | Alumina ceramic substrate and preparation method and application thereof |
| CN108117380A (en) * | 2017-12-14 | 2018-06-05 | 上海卡贝尼精密陶瓷有限公司 | A kind of forming and sintering method of overlength aluminium oxide ceramics pole |
| CN110802052A (en) * | 2019-10-14 | 2020-02-18 | 江苏吉星新材料有限公司 | Method for removing boron carbide on rough surface of sapphire substrate |
| CN112174177A (en) * | 2020-10-13 | 2021-01-05 | 中国铝业股份有限公司 | Hydraulic alumina and preparation method thereof |
| CN113146804A (en) * | 2021-04-20 | 2021-07-23 | 江苏泰州麦迪医疗科技有限公司 | Ceramic femoral stem prosthesis manufacturing method and forming tool |
| CN113511885A (en) * | 2021-08-03 | 2021-10-19 | 苏州楚翰真空科技有限公司 | Method and system for sintering ceramic material |
| CN113511885B (en) * | 2021-08-03 | 2023-10-27 | 苏州楚翰真空科技有限公司 | Method and system for sintering ceramic material |
| CN115321990A (en) * | 2022-09-09 | 2022-11-11 | 山东倍辰新材料有限公司 | Preparation process of microwave sintered ceramic slag remover |
| CN115321990B (en) * | 2022-09-09 | 2023-08-29 | 山东倍辰新材料有限公司 | Preparation process of microwave sintering ceramic slag remover |
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| CN105272177B (en) | 2018-01-16 |
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Address after: 210038 No. 5 Xianxin Middle Road, Qixia District, Nanjing City, Jiangsu Province Patentee after: Nanjing Changjiang Industrial Furnace Technology Group Co., Ltd. Address before: 210038 No. 5 Xianxin Middle Road, Qixia District, Nanjing City, Jiangsu Province Patentee before: Nanjing Changjiang Industrial Furnace Technology Co.,Ltd. |