CN100390330C - Method for preparing flake alpha Al2O3 monocrystal grains at low temperature - Google Patents
Method for preparing flake alpha Al2O3 monocrystal grains at low temperature Download PDFInfo
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- CN100390330C CN100390330C CNB2006101163603A CN200610116360A CN100390330C CN 100390330 C CN100390330 C CN 100390330C CN B2006101163603 A CNB2006101163603 A CN B2006101163603A CN 200610116360 A CN200610116360 A CN 200610116360A CN 100390330 C CN100390330 C CN 100390330C
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- fused salt
- salt
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- single crystal
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 238000000034 method Methods 0.000 title claims abstract description 22
- 229910052593 corundum Inorganic materials 0.000 title 1
- 229910001845 yogo sapphire Inorganic materials 0.000 title 1
- 150000003839 salts Chemical class 0.000 claims abstract description 44
- 239000013078 crystal Substances 0.000 claims abstract description 38
- 239000000843 powder Substances 0.000 claims abstract description 23
- 239000002245 particle Substances 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 10
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 20
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 18
- 238000001354 calcination Methods 0.000 claims description 14
- 239000011780 sodium chloride Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- 238000000498 ball milling Methods 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims description 2
- 241001274216 Naso Species 0.000 claims 1
- 239000000919 ceramic Substances 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000005245 sintering Methods 0.000 abstract description 3
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 abstract description 2
- 229910021502 aluminium hydroxide Inorganic materials 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 238000013329 compounding Methods 0.000 abstract 2
- 238000001816 cooling Methods 0.000 abstract 1
- 229910001679 gibbsite Inorganic materials 0.000 abstract 1
- 239000001103 potassium chloride Substances 0.000 description 8
- 235000011164 potassium chloride Nutrition 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 7
- 238000005303 weighing Methods 0.000 description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- RNUBFUJXCFSMQP-UHFFFAOYSA-N borol-2-one Chemical compound O=C1B=CC=C1 RNUBFUJXCFSMQP-UHFFFAOYSA-N 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to a method to make flake single crystal alumina particle in low temperature. It adopts molten salt growth method, uses sintered Al(OH)3 powder or non crystalline state alumina generated from gama-A1203 as raw material, adding crystal seed alpha-A1203 powder 5-20wt%, using melt salt as compounding medium, and the dosage is 1:1-4:1 of salt material, sintering for 2-9 hours at 660-1300 degree centigrade, cooling and gaining the flake single crystal alumina particle. The invention has the advantages of low compounding temperature, simple technology, high efficiency, cheap raw material and no environment pollution. The particle has high reaction activity and could be added into raw material as crystal seed to make ceramic that has high tenacity.
Description
Technical field
The present invention relates to a kind of low temperature and prepare sheet α-Al
2O
3The method of single crystal grain belongs to ceramic material Al
2O
3The fabricating technology field.
Background technology
Al
2O
3Pottery has good mechanical property and electrical property, is widely used a kind of ceramic material.The fracture toughness property of traditional alumina-ceramic is relatively low, only is 3MPam usually
1/2About.Therefore, how to improve Al
2O
3The fracture toughness of ceramic material is material scholar expectation always and makes great efforts target.Nearest studies show that, under the effect of liquid-phase sintering auxiliary agent, and α-Al
2O
3The platy-monocrystal particle can anisotropic growth be tabular, long column shape pattern, so that the fracture toughness of aluminium oxide ceramics is greatly improved.By α-Al
2O
3Effective control of the size of platy-monocrystal particle, quantity and orientation can realize effective control of aluminium oxide ceramics microstructure and mechanical property.
At present, α-Al
2O
3The platy-monocrystal particle mainly synthesizes by the hot method of alcohol and molten-salt growth method.The hot method of alcohol has high preparation cost.Molten-salt growth method Borolon platy-monocrystal be with aluminum sulfate as initial feed, take sodium sulphate or potassium sulfate as fused salt, synthesize the α-Al of large-size
2O
3There is following shortcoming in this method: at first aluminum sulfate obtains can discharging the toxic gases such as sulfur dioxide and sulfur trioxide in the process of aluminium oxide in decomposition, causes environmental pollution; Secondly, the fusing point of sulfate is higher, and is just higher in the energy consumption of high-temperature calcination; In addition, because the synthetic α-Al that obtains of this method
2O
3The platy-monocrystal particle often has large-size (20 μ m), as these big α-Al
2O
3The bridging action that platelet causes is so that pottery is difficult to densified sintering product.
Summary of the invention
The object of the present invention is to provide a kind of low temperature to prepare the processing method of tabular alumina single crystal particle.
A kind of method for preparing the tabular alumina single crystal grain of the present invention is characterized in that it is raw material that employing contains the aluminium original material, adds a small amount of crystal seed, and adds fused salt as synthetic medium, behind 660～1300 ℃ of temperature lower calcinations, obtains sheet α-Al
2O
3Single crystal grain; Technical process and the step of this method are as follows:
(a) with commercially available Al (OH)
3Powder or γ-Al
2O
3Powder is raw material, at first 550～650 ℃ of lower calcinings 2 hours, obtains the amorphous state aluminium oxide; Adding then particle diameter is crystal seed α-Al of 0.02～0.5 μ m
2O
3Powder, it adds amount is Al (OH)
3With α-Al
2O
35～20% of both gross weights were carried out ball milling 2～3 hours then;
(b) add fused salt, fused salt is the mixture of any or two kinds among NaCl, the KCl; Perhaps fused salt is K
2SO
4, Na
2SO
4In the mixture of any or two kinds; For calculating benchmark, promptly both weight ratios of salt material are 1: 1～4: 1 to the add-on of fused salt by original powder; And then carried out ball milling 2～3 hours, the mixture that mixes is dried, sieved;
(c) the above-mentioned mixture that mixes is positioned in the alumina crucible, sealing is calcined in temperature is 660～1300 ℃ cabinet-type electric furnace, and the time is 2～8 hours; Calcining back synthetic product cools to room temperature with the furnace;
(d) synthetic product is removed residual fused salt with repeatedly rinsing of distilled water, namely gets tabular alumina α-Al
2O
3Single crystal grain.
The present invention adopts that widely used aluminium hydroxide is primary raw material in the industry, and adopting sodium chloride and potassium chloride mixture is synthetic medium, and the method by plus seed reaches decrease powder synthesis temperature; Synthetic α-the Al that obtains
2O
3Flaky crystalline grain has littler size; α-Al that the inventive method is made
2O
3Flaky crystalline grain joins in the aluminium oxide ceramics, can obviously improve fracture toughness and other physical and mechanical properties of aluminium oxide ceramics.
Embodiment
After now specific embodiments of the invention being described in.
Embodiment 1
Adopt Al (OH)
3Powder is initiation material, and its purity is 99.99%, 550 ℃ of lower calcinings 2 hours, obtains the amorphous state aluminium oxide; Taking by weighing these amorphous state alumina powder 17 grams and average grain diameter is crystal seed α-Al of 0.2 μ m
2O
3Powder 3 grams are put into the polytetrafluoroethylene (PTFE) ball grinder that zirconia ball is housed with both, carry out ball milling 3 hours, adding then fused salt, is the fused salt mixt that 2: 1 ratio adds 20 gram NaCl and 20 gram KCl in salt material ratio, subsequently ball milling 3 hours again, make to mix, dry then, sieve.
Above-mentioned oven dry, the compound that mixes are put into alumina crucible, and after the sealing, 200 ℃/h speed is warming up to 700 ℃, calcines 4 hours, cools to room temperature subsequently with the furnace, synthetic product.
With the rinsing 10 times in distilled water of above-mentioned synthetic product, remove residual fused salt, obtain at last the tabular alumina single crystal grain.
Embodiment 2
The preparation process of present embodiment and the foregoing description 1 is identical.Different is: (1) α-Al
2O
3The average grain diameter of crystal seed is 0.4 μ m; (2) calcining heat is 1100 ℃, calcines 2 hours.Make the tabular alumina single crystal particle at last.
Embodiment 3
The preparation process of present embodiment and the foregoing description 1 is identical.Different is: the fused salt that (1) adds is the Na of 1: 1 ratio adding 10 grams in salt material ratio
2SO
4K with 10 grams
2SO
4Fused salt mixt; (2) calcining temperature is 1300 ℃, calcines 2 hours.Make the tabular alumina single crystal particle at last.
Embodiment 4
The preparation process of present embodiment and the foregoing description 1 is identical.Different is: the fused salt that (1) adds is the fused salt mixt that 1: 1 ratio adds the KCl of the NaCl of 10 grams and 10 grams in salt material ratio.Finally make the tabular alumina single crystal particle.
Embodiment 5
The preparation process of present embodiment and the foregoing description 1 is identical.Different is: (1) raw material takes by weighing 16 gram amorphous state alumina powders and 4 gram crystal grain diameters are crystal seed α-Al of 0.2 μ m
2O
3Powder; (2) fused salt that adds is 4: 1 ratio adding 40 gram NaCl and the fused salt mixt of 40 gram KCl in salt material ratio.Finally make the tabular alumina single crystal particle.
Embodiment 6
The preparation process of present embodiment and the foregoing description 1 is identical.Different is: (1) raw material takes by weighing 19 gram amorphous state alumina powders and 1 gram crystal grain diameter is crystal seed α-Al of 0.2 μ m
2O
3Powder; (2) fused salt that adds is 4: 1 ratio adding 40 gram NaCl and the fused salt mixt of 40 gram KCl in salt material ratio; (3) calcining heat is 700 ℃, calcines 8 hours.Finally make the tabular alumina single crystal particle.
Embodiment 7
Adopt γ-Al
2O
3Powder is initiation material, and its purity is 99.99%, 550 ℃ of calcinings 2 hours, obtains the amorphous state aluminium oxide; Take by weighing 17 the gram amorphous state alumina powders and 3 the gram crystal grain diameters be crystal seed α-Al of 0.2 μ m
2O
3Powder; Both are put into the polytetrafluoroethylene (PTFE) spherical tank that zirconia ball is housed, and ball milling 3 hours is 4: 1 ratio adding 40 gram NaCl and the fused salt mixt of 40 gram KCl in salt material ratio then, carries out ball milling 3 hours again, makes to mix, and dries then, sieves.
With above-mentioned oven dry, sieve, the compound that mixes is put into alumina crucible, after the sealing, is warming up to 700 ℃ with 200 ℃/h speed, calcines 4 hours.Cool to synthetic product with the furnace room temperature subsequently.Finally make the tabular alumina single crystal particle.
Embodiment 8
The preparation process of present embodiment and the foregoing description 7 is identical.Different is: (1) takes by weighing 19 grams by γ-Al
2O
3The amorphous state aluminium oxide that obtains after the calcining and 1 gram crystal grain diameter are crystal seed α-Al of 0.05 μ m
2O
3Powder; (2) fused salt that adds is 1: 1 ratio adding 10 gram NaCl and the fused salt mixt of 10 gram KCl in salt material ratio; (3) calcining heat is 1100 ℃, and calcination time is 4 hours.Finally make the tabular alumina single crystal particle.
The aluminum oxide that makes in the foregoing description is observed through field emission scanning electron microscope, and can see its crystal grain is sheet, is evenly distributed, and particle diameter is 2-3 μ m.Through XRD determining, its crystalline phase is single-phase α-Al
2O
3
With this α-Al
2O
3Join in the original powder as crystal seed, adopt common process to prepare aluminium oxide ceramics; Can find that the aluminium oxide ceramics microstructure can add α-Al by changing
2O
3The mode of platelet quantity is regulated and control.By instrument test, find that this ceramic toughness has improved 30% than common alumina-ceramic.
Claims (2)
1. a method for preparing the tabular alumina single crystal grain is characterized in that it is raw material that employing contains the aluminium original material, adds a small amount of crystal seed, and adds fused salt as synthetic medium, behind 660～1300 ℃ of temperature lower calcinations, obtains sheet α-Al
2O
3Single crystal grain; Technical process and the step of this method are as follows:
(a) with commercially available Al (OH)
3Powder or γ-Al
2O
3Powder is raw material, at first 550～650 ℃ of lower calcinings 2 hours, obtains the amorphous state aluminium oxide; Adding then particle diameter is crystal seed α-Al of 0.02～0.5 μ m
2O
3Powder, it adds amount is Al (OH)
3With α-Al
2O
35～20% of both gross weights were carried out ball milling 2～3 hours then;
(b) add fused salt, fused salt is the mixture of any or two kinds among NaCl, the KCl; Perhaps fused salt is K
2SO
4, Na
2SO
4In the mixture of any or two kinds; For calculating benchmark, promptly both weight ratios of salt material are 1: 1～4: 1 to the add-on of fused salt by original powder; And then carried out ball milling 2～3 hours, the mixture that mixes is dried, sieved;
(c) the above-mentioned mixture that mixes is positioned in the alumina crucible, sealing is calcined in temperature is 660～1300 ℃ cabinet-type electric furnace, and the time is 2～8 hours; Calcining back synthetic product cools to room temperature with the furnace;
(d) synthetic product is removed residual fused salt with repeatedly rinsing of distilled water, namely gets tabular alumina α-Al
2O
3Single crystal grain.
2. a kind of method for preparing the tabular alumina single crystal particle as claimed in claim 1 is characterized in that the fused salt that adds is the fused salt mixt that NaCl and KCl salt are formed, and both weight proportions are 1: 1; Perhaps the fused salt of Jia Ruing is NaSO
4And K
2SO
4The fused salt mixt that salt is formed, both weight proportions 1: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101163603A CN100390330C (en) | 2006-09-21 | 2006-09-21 | Method for preparing flake alpha Al2O3 monocrystal grains at low temperature |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101163603A CN100390330C (en) | 2006-09-21 | 2006-09-21 | Method for preparing flake alpha Al2O3 monocrystal grains at low temperature |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1936114A CN1936114A (en) | 2007-03-28 |
| CN100390330C true CN100390330C (en) | 2008-05-28 |
Family
ID=37953837
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006101163603A Active CN100390330C (en) | 2006-09-21 | 2006-09-21 | Method for preparing flake alpha Al2O3 monocrystal grains at low temperature |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102009993A (en) * | 2010-12-15 | 2011-04-13 | 中国铝业股份有限公司 | Method for preparing submicron aluminium oxide by two-stage roasting method |
| CN103058240A (en) * | 2013-01-15 | 2013-04-24 | 雅安百图高新材料有限公司 | Method for preparing spherical alpha-phase alumina |
| CN103359764B (en) * | 2013-07-09 | 2015-07-08 | 东华大学 | Preparation method of sheet-shaped alpha-aluminium oxide |
| CN104986786B (en) * | 2015-07-31 | 2018-02-27 | 华南理工大学 | A kind of controllable sheet α Al of particle size2O3Powder and preparation method thereof |
| CN107829132A (en) * | 2017-10-10 | 2018-03-23 | 上海应用技术大学 | A kind of method for preparing alumina single crystal |
| CN108560052B (en) * | 2018-04-26 | 2020-05-01 | 闽江学院 | Preparation method and application of monocrystal hexagonal alumina |
| CN113173590B (en) * | 2021-05-01 | 2022-05-24 | 百色学院 | Method for preparing flaky alumina based on liquid metal |
| CN113233488B (en) * | 2021-05-08 | 2023-03-21 | 中铝山东有限公司 | Preparation method of alpha-alumina with narrow primary grain size distribution |
| CN115849877A (en) * | 2022-06-13 | 2023-03-28 | 池州学院 | Preparation method for gamma alumina crystal transformation |
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Effective date of registration: 20201030 Address after: 454174 Zhongzhou aluminum factory, Qixian town, Xiuwu County, Jiaozuo City, Henan Province Patentee after: Chalco Zhongzhou Aluminium Industry Co.,Ltd. Patentee after: Chinalco Zhongzhou new Mstar Technology Ltd. Address before: 100082 No. 62 North Main Street, Beijing, Xizhimen Patentee before: ALUMINUM CORPORATION OF CHINA Ltd. |