CN110938862A - High-purity monocrystalline corundum powder and preparation method thereof - Google Patents
High-purity monocrystalline corundum powder and preparation method thereof Download PDFInfo
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- CN110938862A CN110938862A CN201911342322.3A CN201911342322A CN110938862A CN 110938862 A CN110938862 A CN 110938862A CN 201911342322 A CN201911342322 A CN 201911342322A CN 110938862 A CN110938862 A CN 110938862A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/10—Single-crystal growth directly from the solid state by solid state reactions or multi-phase diffusion
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/12—Single-crystal growth directly from the solid state by pressure treatment during the growth
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/20—Aluminium oxides
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Abstract
A high-purity monocrystalline corundum powder and a preparation method thereof belong to the technical field of ceramic materials. The preparation method of the high-purity monocrystalline corundum powder comprises the following steps of uniformly mixing powder raw materials according to a certain weight part, wherein the powder raw materials comprise an inorganic oxyhydrogen compound of aluminum, aluminum chloride, aluminum fluoride and aluminum nitrate; and sintering under the conditions of low temperature and high pressure to obtain the monocrystalline corundum powder. The preparation process is simple, and the high-purity monocrystalline corundum powder can be prepared by low-temperature sintering without adding additives containing other metal elements.
Description
Technical Field
The invention relates to a technology in the field of ceramic materials, in particular to high-purity monocrystalline corundum powder and a preparation method thereof.
Background
The single crystal corundum is a better abrasive in corundum series, has the characteristics of good toughness and high hardness, and is commonly used for high-grade grinding materials. At present, the monocrystalline corundum is mostly smelted by alumina and additives in an electric arc furnace. The method needs to be carried out under the high-temperature condition, has high energy consumption and high impurity content, and further needs to be subjected to impurity removal treatment if high-purity monocrystalline corundum needs to be obtained, so that the process is complex.
For example, in the Chinese patent application with publication (publication) No. CN101906663B, alumina powder, anatase titanium dioxide, titanium powder, aluminum fluoride, zirconium dioxide powder and the like are heated to 2000-2600 ℃ and continuously heated for 25-32 hours, the obtained powder needs to be crushed and subjected to impurity removal and other complicated processes, in order to reduce the temperature, for example, in the Chinese patent application with publication (publication) No. CN104499051B, α -alumina powder with the particle size of 1-5 mu m is uniformly mixed with an inhibitor and then is smelted at the temperature of 1500-1700 ℃, and the monocrystalline corundum is obtained by cooling, although the temperature required by the preparation is reduced by adding seeds for slow growth, the temperature is still higher than 1500 ℃.
The present invention has been made to solve the above-mentioned problems occurring in the prior art.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the high-purity monocrystalline corundum powder and the preparation method thereof, the preparation process is simple, and the high-purity monocrystalline corundum powder can be prepared by low-temperature sintering without adding additives containing other metal elements.
The invention relates to a preparation method of high-purity monocrystalline corundum powder, which comprises the following steps of uniformly mixing powder raw materials according to a certain weight part, wherein the powder raw materials comprise an inorganic oxyhydrogen compound of aluminum, aluminum chloride, aluminum fluoride and aluminum nitrate; and sintering under the conditions of low temperature and high pressure to obtain the monocrystalline corundum powder.
Preferably, the weight portion of the inorganic oxyhydrogen element compound of aluminum is 30-70, the weight portion of aluminum chloride is 5-15, the weight portion of aluminum fluoride is 1-5, and the weight portion of aluminum nitrate is 1-5.
Further preferably, the inorganic oxyhydrogen-containing compound of aluminum is at least one of aluminum hydroxide, polyaluminum chloride, boehmite, and pseudoboehmite.
Preferably, the sintering temperature is 1000-.
Preferably, the particle size D50 of each powder raw material is 500nm-100 μm, and the purity is 99% -99.999%.
Preferably, the mixing is stirred in a dry powder mixer for 2-7 h.
The invention relates to high-purity monocrystalline corundum powder which is prepared by the method, the particle size D50 of the prepared powder is 5-275 mu m, the requirement of F46-F150 in the current market is met, and the purity is 99-99.999%. The particle size can be adjusted by changing the proportion of the aluminum inorganic hydroxide compound in the mixed powder and the sintering time.
Technical effects
Compared with the prior art, the invention has the following technical effects:
1) the preparation process is simple, the powder raw materials are uniformly mixed and then sintered, the complex process of preparing a calcined precursor by adopting a sol-gel method is avoided, and the high-purity monocrystalline corundum powder can be prepared under the condition of not adding additives containing other metal elements; in addition, compared with a preparation process needing to add an additive containing other metal elements, the calcination temperature is low, and the energy consumption is reduced;
2) the prepared high-purity monocrystalline corundum is in an obvious polyhedral structure, has good dispersibility, high hardness and good wear resistance.
Drawings
FIG. 1 is a scanning electron micrograph of a single crystal corundum in example 1;
FIG. 2 is an XRD pattern of single crystal corundum in example 1;
FIG. 3 is an optical microscope photograph of single crystal corundum in example 3.
Detailed Description
The invention is described in detail below with reference to the drawings and the detailed description.
The embodiment of the invention relates to a preparation method of high-purity monocrystalline corundum powder, which comprises the following steps of taking powder raw materials in parts by weight, stirring and mixing the powder raw materials in a dry powder mixer for 2-7 hours, wherein the powder raw materials comprise 30-70 parts by weight of an inorganic oxyhydrogen compound of aluminum, 5-15 parts by weight of aluminum chloride, 1-5 parts by weight of aluminum fluoride and 1-5 parts by weight of aluminum nitrate; then heating to 1000-1400 ℃ at the speed of 1-10 ℃/min, and sintering for 1-10h under the pressure condition of 0.1-10MPa to obtain the single-crystal corundum powder.
Further preferably, the inorganic oxyhydrogen-containing compound of aluminum is at least one of aluminum hydroxide, polyaluminum chloride, boehmite, and pseudoboehmite.
Preferably, the particle size D50 of each powder raw material is 500nm-100 μm, and the purity is 99% -99.999%.
Example 1
Taking Al (OH) with the particle size D50 of 1 μm3Mixing 30kg of powder, 5kg of aluminum chloride, 2kg of aluminum fluoride and 2kg of aluminum nitrate in a dry powder mixer for 2 hours; then placing the mixture into an alumina crucible, placing the alumina crucible into a high-temperature furnace, heating the mixture to 1300 ℃ at the speed of 5 ℃/min, keeping the pressure in the furnace at 5MPa, and carrying out heat preservation treatment for 6 hours to obtain high-purity monocrystalline corundum powder; the SEM photograph is shown in FIG. 1, which shows a clear polyhedral structure, the XRD pattern is shown in FIG. 2, no diffraction peak of impurities is observed, and the purity is high.
Example 2
Taking Al (OH) with the particle size D50 of 15 mu m3Mixing 40kg of powder, 5kg of aluminum chloride, 3kg of aluminum fluoride and 3kg of aluminum nitrate in a mixer for 3 hours; then placing the mixture into an alumina crucible, placing the alumina crucible into a high-temperature furnace, heating the mixture to 1300 ℃ at the speed of 5 ℃/min, keeping the pressure in the furnace at 5MPa, and carrying out heat preservation treatment for 6 hours to obtain the high-purity monocrystalline corundum powder.
Example 3
30kg of boehmite powder with the particle size D50 of 50 mu m, 5kg of aluminum chloride, 2kg of aluminum fluoride and 2kg of aluminum nitrate are mixed in a mixer for 2 hours; then placing the mixture into an alumina crucible, placing the alumina crucible into a high-temperature furnace, heating the mixture to 1300 ℃ at the speed of 5 ℃/min, keeping the pressure in the furnace at 5MPa, and carrying out heat preservation treatment for 6 hours to obtain high-purity monocrystalline corundum powder; the optical microscopic image thereof is shown in FIG. 3, which demonstrates good dispersibility.
Example 4
60kg of polyaluminium chloride powder with the particle size D50 of 5 mu m, 12kg of aluminium chloride, 3kg of aluminium fluoride and 3kg of aluminium nitrate are mixed in a mixer for 2 hours; then placing the mixture into an alumina crucible, placing the alumina crucible into a high-temperature furnace, heating the mixture to 1100 ℃ at the speed of 5 ℃/min, keeping the pressure in the furnace at 2MPa, and carrying out heat preservation treatment for 4 hours to obtain the high-purity monocrystalline corundum powder.
Example 5
64kg of polyaluminium chloride powder with the particle size D50 of 5 mu m, 10kg of aluminium chloride, 2.5kg of aluminium fluoride and 2.5kg of aluminium nitrate are mixed in a mixer for 3 hours; then placing the mixture into an alumina crucible, placing the alumina crucible into a high-temperature furnace, heating the mixture to 1100 ℃ at the speed of 5 ℃/min, keeping the pressure in the furnace at 8MPa, and carrying out heat preservation treatment for 6 hours to obtain the high-purity monocrystalline corundum powder.
It is to be emphasized that: the above embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and all simple modifications, equivalent changes and modifications made to the above embodiments according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.
Claims (7)
1. A preparation method of high-purity monocrystalline corundum powder is characterized in that powder raw materials are taken and uniformly mixed according to a certain weight part, wherein the powder raw materials comprise an inorganic oxyhydrogen compound of aluminum, aluminum chloride, aluminum fluoride and aluminum nitrate; and sintering under the conditions of low temperature and high pressure to obtain the monocrystalline corundum powder.
2. The method for preparing high-purity monocrystalline corundum powder according to claim 1, wherein the aluminum inorganic hydroxide compound is 30-70 parts by weight, the aluminum chloride is 5-15 parts by weight, the aluminum fluoride is 1-5 parts by weight, and the aluminum nitrate is 1-5 parts by weight.
3. The method for preparing a high-purity single-crystal corundum powder according to claim 1, wherein the inorganic oxyhydrogen-containing compound of aluminum is at least one of aluminum hydroxide, polyaluminum chloride, boehmite and pseudo-boehmite.
4. The method for preparing high-purity monocrystalline corundum powder according to claim 1, wherein the sintering temperature is 1000-1400 ℃, the heating rate is 1-10 ℃/min, the sintering pressure is 0.1-10MPa, and the sintering time is 1-10 h.
5. The method for preparing high-purity monocrystalline corundum powder according to claim 1, characterized in that the particle diameters D50 of the powder raw materials are respectively 500nm-100 μm, and the purities are respectively 99% -99.999%.
6. The method for preparing a high-purity single-crystal corundum powder according to claim 1, wherein the mixing is carried out by stirring and mixing for 2 to 7 hours in a dry powder mixer.
7. A high-purity monocrystalline corundum powder, characterized in that the powder is prepared by the method of any one of claims 1 to 5, the particle diameter D50 of the prepared powder is 5-275 μm, and the purity is 99-99.999%.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1050366A (en) * | 1989-09-21 | 1991-04-03 | 阿托化学公司 | Big xln of the Alpha-alumina of wafer form and method for making thereof |
| CN1062560A (en) * | 1991-11-22 | 1992-07-08 | 武汉工业大学 | The method of preparing boule monocrystal abrasive at low temp |
| CN101935877A (en) * | 2010-09-03 | 2011-01-05 | 昆明理工大学 | Method for synthesizing mullite whiskers by normal pressure sintering |
| CN107074574A (en) * | 2015-09-30 | 2017-08-18 | 日本碍子株式会社 | The preparation method of plate-like aluminum oxide powder |
| CN110139833A (en) * | 2016-12-22 | 2019-08-16 | Dic株式会社 | The manufacturing method of alpha aluminium oxide particle and the manufacturing method of resin combination |
-
2019
- 2019-12-23 CN CN201911342322.3A patent/CN110938862A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1050366A (en) * | 1989-09-21 | 1991-04-03 | 阿托化学公司 | Big xln of the Alpha-alumina of wafer form and method for making thereof |
| CN1062560A (en) * | 1991-11-22 | 1992-07-08 | 武汉工业大学 | The method of preparing boule monocrystal abrasive at low temp |
| CN101935877A (en) * | 2010-09-03 | 2011-01-05 | 昆明理工大学 | Method for synthesizing mullite whiskers by normal pressure sintering |
| CN107074574A (en) * | 2015-09-30 | 2017-08-18 | 日本碍子株式会社 | The preparation method of plate-like aluminum oxide powder |
| CN110139833A (en) * | 2016-12-22 | 2019-08-16 | Dic株式会社 | The manufacturing method of alpha aluminium oxide particle and the manufacturing method of resin combination |
Non-Patent Citations (1)
| Title |
|---|
| 李懋强等: "《热学陶瓷 性能测试工艺》", 30 June 2013, 中国建材工业出版社 * |
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Application publication date: 20200331 |