CN103058240A - Method for preparing spherical alpha-phase alumina - Google Patents
Method for preparing spherical alpha-phase alumina Download PDFInfo
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- CN103058240A CN103058240A CN2013100132078A CN201310013207A CN103058240A CN 103058240 A CN103058240 A CN 103058240A CN 2013100132078 A CN2013100132078 A CN 2013100132078A CN 201310013207 A CN201310013207 A CN 201310013207A CN 103058240 A CN103058240 A CN 103058240A
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Abstract
The invention discloses a method for preparing spherical alpha-phase alumina. The method comprises the following steps of: step 1, heating aluminum-containing powder at 2100-2300 DEG C for spheroidization to obtain spherical alumina powder; and step 2, heating and calcining the spherical alumina powder at 1200-2072 DEG C to obtain spherical alpha-phase alumina. The prepared alpha-phase alumina is spherical, the spheroidization rate is higher than 90%, and the spherical alpha-phase alumina has high fluidity, uniform stress and high filling volume and can be widely applied to the field; besides, breaking is not needed in the preparation process, so that not only is the spheroidization of the alpha-phase alumina guaranteed, but also the preparation steps are decreased; and moreover, the alumina smaller than 40 microns is subjected to secondary heating, so the problem of difficultly preparing the high-content alpha phase from the alumina smaller than 40 microns is solved. Therefore, the preparation method and the preparation process are simple, the preparation time is short, and the spherical alpha-phase alumina with high content can be prepared.
Description
Technical field
The present invention relates to the method that twice high-temperature calcination of a kind of employing prepares spherical alpha-phase aluminum oxide.
Background technology
Alpha-phase aluminum oxide, thermal conductivity is strong, good moldability, crystalline phase is stable, hardness is high, good stability of the dimension, the strengthening and toughening that can be widely used in the products such as various plastics, rubber, pottery, refractory materials, the wear resisting property that particularly improves ceramic compactness, smooth finish, cold and hot fatigability, fracture toughness property, creep-resistant property and macromolecular material product is particularly remarkable.Because alpha-phase aluminum oxide also is the far-infrared emission material of excellent performance, is applied in fiber product and the high-pressure mercury lamp as far infrared transmission and lagging material.In addition, alpha-phase aluminum oxide resistivity is high, has good insulating property, can be applicable in the main accessory and ic substrate of YGA laser crystalline substance.The α-aluminum oxide of existing routine techniques preparation mainly adopts electric-heating technology that other are converted into alpha-phase aluminum oxide such as the γ phase alumina, and this method α phase content is very high, but prepared product is non-sphere.Aspheric aluminum oxide is restricted in application.Simultaneously, the preparation method to the α phase ball-aluminium oxide of the above particle diameter of 40 μ m in the prior art is comparatively ripe, but is difficult to prepare the following alpha-phase aluminum oxide of 40 high μ m of α phase content.
Summary of the invention
The objective of the invention is to overcome the defective of prior art, provide a kind of and prepare spherical alpha-phase aluminum oxide below the 40 high μ m of α phase content by twice heating process.
In order to solve the problems of the technologies described above, the present invention takes following technical scheme:
A kind of preparation method of spherical alpha-phase aluminum oxide may further comprise the steps:
Step 1: will contain the aluminium powder body in 2100-2300 ℃ of lower heating spheroidization, and obtain the ball-aluminium oxide powder;
Step 2: the ball-aluminium oxide powder in 1200-2072 ℃ of lower heating and calcining, is obtained spherical alpha-phase aluminum oxide.Contain in the aluminium powder body spheroidization process each in the step 1 and can transform between mutually, can form the α phase of lower aq, adopt step 2 again to calcine at 1200 ℃ to 2072 ℃, can improve the α phase content.
As the preferred embodiments of the present invention, among the preparation method of above-mentioned spherical alpha-phase aluminum oxide, preferably: the described aluminium powder body that contains is in aluminum oxide, partial dehydration aluminium hydroxide or the aluminium hydroxide one or more.
As the preferred embodiments of the present invention, among the preparation method of above-mentioned spherical alpha-phase aluminum oxide, preferably: described ball-aluminium oxide powder median size is 0.1 μ m to 40 μ m.Because large long in the time 1200 ℃-2072 ℃ of the temperature ranges of step 1 of volume, α is easily formation mutually during greater than 40 μ m for alumina powder jointed particle diameter; 0.1 the ball-aluminium oxide of μ m to 40 μ m is owing to the lifetime of 1200 ℃-2072 ℃ of the little temperature ranges in step 1 of volume is short, α is difficult for forming mutually, therefore the present invention is that the ball-aluminium oxide of 0.1 μ m to 40 μ m carries out the heat treated of step 2 with particle diameter, thereby increases the content of α phase.
As the preferred embodiments of the present invention, among the preparation method of above-mentioned spherical alpha-phase aluminum oxide, preferably: the equipment that adds thermal recovery is the triple tube burner, reaches the Heating temperature that requires in 3 seconds.Powder passes in tube core, through flame by instantaneously heating to high temperature.
The invention has the beneficial effects as follows:
1) alpha-phase aluminum oxide of the present invention's preparation is spherical, the nodularization rate is more than 90%, has high workability in Application Areass such as heat conduction films, stress equalizing, high filler loading capacity can be widely used in this area, and need not to carry out fragmentation in the preparation process, both can guarantee the spheroidization of alpha-phase aluminum oxide, reduce again preparation section.
2) the present invention has solved the following difficult problem for preparing the α phase of high-content of ball-aluminium oxide of 40 μ m by the aluminum oxide below the 40 μ m is carried out second-heating.
3) preparation method of the present invention, step are simple, and preparation time is short, can make the spherical alpha-phase aluminum oxide of high-content.
Embodiment
Below in conjunction with specific embodiment of the present invention the present invention is made further explanation and description.
Embodiment 1:
Commercially available α-aluminum oxide is crushed to median size 10 μ m, as raw material, raw material is dropped into the triple tube burner and controls temperature and carry out the melting spheroidization at 2100 ℃ to 2300 ℃, get test sample 1-1.Test sample 1-1 dropped into burner again and control flame temperature and carry out heat treated at 1800 ℃ to 2000 ℃ and get test sample 1-2.Through XRD determining gained sample, calculate the content of each crystallization phases from the intensitometer at each crystalline characteristics peak and list table 1 in.
Embodiment 2:
Commercially available gamma-alumina is crushed to median size 10 μ m, as raw material, raw material is dropped into the triple tube burner and controls temperature and carry out the melting spheroidization at 2100 ℃ to 2300 ℃, get test sample 2-1.Test sample 2-1 is dropped into burner again and control flame temperature and heat-treat to get test sample 2-2 at 1800 ℃ to 2000 ℃.Through XRD determining gained sample, calculate the content of each crystallization phases from the intensitometer at each crystalline characteristics peak and list table 1 in.
Embodiment 3:
Commercially available α-aluminum oxide is crushed to median size 5 μ m, as raw material, raw material is dropped into the triple tube burner and controls temperature and carry out the melting spheroidization at 2100 ℃ to 2300 ℃, get test sample 3-1.Test sample 3-1 is dropped into burner again and control flame temperature and heat-treat to get test sample 3-2 at 1800 ℃ to 2000 ℃.Through XRD determining gained sample, calculate the content of each crystallization phases from the intensitometer at each crystalline characteristics peak and list table 1 in.
Embodiment 4:
Commercially available α-aluminum oxide is crushed to median size 2 μ m, as raw material, raw material is dropped into the triple tube burner and controls temperature and carry out the melting spheroidization at 2100 ℃ to 2300 ℃, get test sample 4-1.Test sample 4-1 is dropped into burner again and control flame temperature and heat-treat to get test sample 4-2 at 1800 ℃ to 2000 ℃.Through XRD determining gained sample, calculate the content of each crystallization phases from the intensitometer at each crystalline characteristics peak and list table 1 in.
Embodiment 5:
Commercially available aluminium hydroxide is crushed to median size 2 μ m, as raw material, raw material is dropped into the triple tube burner and controls temperature and carry out the melting spheroidization at 2100 ℃ to 2300 ℃, get test sample 5-1.Test sample 5-1 is dropped into burner again and control flame temperature and heat-treat to get test sample 5-2 at 1800 ℃ to 2000 ℃.Through XRD determining gained sample, calculate the content of each crystallization phases from the intensitometer at each crystalline characteristics peak and list table 1 in.
The content of the different crystalline phases of aluminum oxide in the sample of table 1 embodiment 1-5
Although invention has been described with reference to explanatory embodiment of the present invention here, above-described embodiment only is the better embodiment of the present invention, embodiments of the present invention are not restricted to the described embodiments, should be appreciated that, those skilled in the art can design a lot of other modification and embodiments, and these are revised and embodiment will drop within the disclosed principle scope and spirit of the application.
Claims (4)
1. the preparation method of a spherical alpha-phase aluminum oxide is characterized in that may further comprise the steps:
Step 1: will contain the aluminium powder body in 2100-2300 ℃ of lower heating spheroidization, and obtain the ball-aluminium oxide powder;
Step 2: the ball-aluminium oxide powder in 1200-2072 ℃ of lower heating and calcining, is obtained spherical alpha-phase aluminum oxide.
2. the preparation method of spherical alpha-phase aluminum oxide according to claim 1 is characterized in that the described aluminium powder body that contains is in aluminum oxide, partial dehydration aluminium hydroxide or the aluminium hydroxide one or more.
3. the preparation method of spherical alpha-phase aluminum oxide according to claim 1, the median size that it is characterized in that described ball-aluminium oxide powder is 0.1 μ m to 40 μ m.
4. the preparation method of spherical alpha-phase aluminum oxide according to claim 1 is characterized in that the described equipment that adds thermal recovery is the triple tube burner.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103482665A (en) * | 2013-10-18 | 2014-01-01 | 长沙华科特种陶瓷材料有限公司 | Preparation method of high-purity spherical alpha-Al2O3 |
| CN111170345A (en) * | 2020-01-15 | 2020-05-19 | 珠海琴晟新材料有限公司 | preparation method of nano α phase aluminum oxide material |
| CN112391659A (en) * | 2019-08-14 | 2021-02-23 | 浙江苏泊尔股份有限公司 | Method for preparing oxide film containing alpha-alumina and vessel |
| CN113184886A (en) * | 2021-04-14 | 2021-07-30 | 雅安百图高新材料股份有限公司 | Preparation method and product of high-thermal-conductivity spherical alumina |
| CN113237789A (en) * | 2021-05-12 | 2021-08-10 | 雅安百图高新材料股份有限公司 | Method for detecting content of organic modifier on surface of alumina powder |
| CN113735149A (en) * | 2021-09-17 | 2021-12-03 | 江苏联瑞新材料股份有限公司 | Preparation method of spherical alumina powder for high-thermal-conductivity underfill |
| CN113816407A (en) * | 2021-09-14 | 2021-12-21 | 江苏联瑞新材料股份有限公司 | Preparation method of low-viscosity high-thermal-conductivity spherical alpha-alumina |
| CN113929122A (en) * | 2021-11-12 | 2022-01-14 | 联瑞新材(连云港)有限公司 | Preparation method of multimodal distribution high heat conduction alpha phase spherical alumina |
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| CN1227189A (en) * | 1998-12-07 | 1999-09-01 | 金玉琢 | Method for producing hollow aluminium oxide ball in DC electric arc ore-smelting furnace |
| CN1936114A (en) * | 2006-09-21 | 2007-03-28 | 上海大学 | Method for preparing flake alpha Al2O3 monocrystal grains at low temperature |
| CN101445259A (en) * | 2008-12-26 | 2009-06-03 | 陕西科技大学 | Method for preparing micro-nano structure alumina particle |
| CN101528604A (en) * | 2006-10-31 | 2009-09-09 | 电气化学工业株式会社 | Alumina powder, process for producing the same, and use thereof |
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2013
- 2013-01-15 CN CN2013100132078A patent/CN103058240A/en active Pending
Patent Citations (4)
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| CN1227189A (en) * | 1998-12-07 | 1999-09-01 | 金玉琢 | Method for producing hollow aluminium oxide ball in DC electric arc ore-smelting furnace |
| CN1936114A (en) * | 2006-09-21 | 2007-03-28 | 上海大学 | Method for preparing flake alpha Al2O3 monocrystal grains at low temperature |
| CN101528604A (en) * | 2006-10-31 | 2009-09-09 | 电气化学工业株式会社 | Alumina powder, process for producing the same, and use thereof |
| CN101445259A (en) * | 2008-12-26 | 2009-06-03 | 陕西科技大学 | Method for preparing micro-nano structure alumina particle |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103482665A (en) * | 2013-10-18 | 2014-01-01 | 长沙华科特种陶瓷材料有限公司 | Preparation method of high-purity spherical alpha-Al2O3 |
| CN112391659A (en) * | 2019-08-14 | 2021-02-23 | 浙江苏泊尔股份有限公司 | Method for preparing oxide film containing alpha-alumina and vessel |
| CN111170345A (en) * | 2020-01-15 | 2020-05-19 | 珠海琴晟新材料有限公司 | preparation method of nano α phase aluminum oxide material |
| CN113184886A (en) * | 2021-04-14 | 2021-07-30 | 雅安百图高新材料股份有限公司 | Preparation method and product of high-thermal-conductivity spherical alumina |
| CN113237789A (en) * | 2021-05-12 | 2021-08-10 | 雅安百图高新材料股份有限公司 | Method for detecting content of organic modifier on surface of alumina powder |
| CN113816407A (en) * | 2021-09-14 | 2021-12-21 | 江苏联瑞新材料股份有限公司 | Preparation method of low-viscosity high-thermal-conductivity spherical alpha-alumina |
| WO2023040599A1 (en) * | 2021-09-14 | 2023-03-23 | 江苏联瑞新材料股份有限公司 | Preparation method for spherical alumina having low viscosity and high thermal conductivity |
| CN113735149A (en) * | 2021-09-17 | 2021-12-03 | 江苏联瑞新材料股份有限公司 | Preparation method of spherical alumina powder for high-thermal-conductivity underfill |
| CN113929122A (en) * | 2021-11-12 | 2022-01-14 | 联瑞新材(连云港)有限公司 | Preparation method of multimodal distribution high heat conduction alpha phase spherical alumina |
| CN113929122B (en) * | 2021-11-12 | 2023-09-05 | 联瑞新材(连云港)有限公司 | Preparation method of multimodal distributed high-heat-conductivity alpha-phase spherical alumina |
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Application publication date: 20130424 |