CN102173756A - Preparation method of high-purity aluminum oxide sintered body for growing sapphire crystal - Google Patents
Preparation method of high-purity aluminum oxide sintered body for growing sapphire crystal Download PDFInfo
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- CN102173756A CN102173756A CN2011100316617A CN201110031661A CN102173756A CN 102173756 A CN102173756 A CN 102173756A CN 2011100316617 A CN2011100316617 A CN 2011100316617A CN 201110031661 A CN201110031661 A CN 201110031661A CN 102173756 A CN102173756 A CN 102173756A
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Abstract
The invention relates to a preparation method of a high-purity aluminum oxide sintered body for growing a sapphire crystal, which is characterized in that the degree of purification of the production shop must be above Grade 10000. The preparation method comprises the following steps: adding 5N-purity aluminum oxide powder, 5N-purity rho-aluminum oxide, deionized water and steel-core polyurethane balls into a polyurethane ball milling tank, carrying out ball milling and mixing for 5 hours, pouring into a polyethylene plastic bag, sealing, standing for 12 hours, passing through a 60-mesh screen, filling into an aluminum oxide ceramic die, pressing under a pressure intensity of 50Mpa to obtain a blank, putting the blank into a microwave sintering oven, heating to 1850 DEG C within 0.5 hour, keeping the temperature of 1850 DEG C for 0.5 hour, and cooling in the oven to obtain the 5N-purity aluminum oxide sintered body. The sapphire crystal grown by using the aluminum oxide sintered body obtained by using the preparation method provided by the invention is colorless and transparent, has fewer defects, and can be used for preparing LED-substrate sapphire crystal wafers.
Description
Technical field
The present invention relates to the preparation method of alumina-ceramic, particularly a kind of preparation method who is used for the high purity aluminium oxide sintered compact of growing sapphire crystal.
Background technology
The remarkable quality of sapphire performance is controlled easily, is processed into the super-smooth surface of no unrelieved stress and damage easily, becomes preferred material in some substrates application, is able to widespread use in following four industries: 1. blue-ray LED base material (BLED ' s); 2. infrared eye; 3. gallium arsenide wafer (GaAs); 4. microwave integrated circuit material.Sapphire also can be applicable to optics, and especially can use in ultraviolet and infrared band in fields such as aerospace, analytical instrument, medical science, has exceeded the spectral range that the traditional optical material can be suitable for.More need sapphire crystal in high temperature and the severe environment.
The main method of growing sapphire crystal is a kyropoulos, and the high quality sapphire of 70-80% is all produced with kyropoulos in the world at present.Its principle is that alumina raw material is placed on heat fused in the crucible, again the seeding growing crystal.The purity of alumina sintered body is vital in this process.
Utilizing the aluminum oxide of exsiccated ammonium alum production to prepare by flame method used in the sapphire 100 years, its biggest advantage is the powder active height, fusing easily in flame, but the gem crystal defective that grows is too many, foreign matter content is high, optical field can't be used for, more substrate material can not be used as.Afterwards, this aluminum oxide is prepared transparent aluminum oxide polycrystal particle with flame method and obtained success as the raw material of kyropoulos growing sapphire.There are a lot of problems in but this raw material, mainly be following several aspect: (1) exsiccated ammonium alum thermal decomposition method can produce huge environmental pollution, 1000 gram exsiccated ammonium alums can only obtain the aluminum oxide of 100 grams, particularly when the sapphire demand reached very big quantity, its environmental cost was intolerable; (2) can't obtain the aluminum oxide powder (5N) of ultra-high purity; (3) tamped density of the alumina particle that obtains in crucible has only 70%, and single stove production efficiency is low; (4) the particulate preparation needs a large amount of hydrogen and oxygen, preparation cost height.
The high purity aluminium oxide powder that passes through the preparation of metallic aluminium choline hydrolysis method of the invention beginning of this century because its quality and cost advantage have obtained dominant position in the high purity aluminium oxide field rapidly, is particularly demonstrating its huge advantage especially aspect the sapphire crystal raw material.By careful control preparation technology, can obtain the alumina powder of 5N ultra-high purity, with this alumina powder compacting sintering, can obtain the sintered compact of the theoretical density of 85-90%.Yet this method but can not obtain the alumina sintered body of 5N purity, and reason is due to the pollution in its manufacturing processed.At first, because this alumina particle is big, poor activity, processability is bad, and needing to add binding agent could better realize; Secondly, die wear pollutes in the pressing process, and aluminum oxide belongs to the material of 9 grades of Mohs' hardness, and very serious to the wearing and tearing of mould, this wearing and tearing can cause very serious pollution; The 3rd, the volatilization of heating element and refractory materials also can be to its pollution that causes in the sintering process.
Prior art is not also reported the preparation method of the alumina sintered body that ultra-high purity, super-high density are arranged at present.
Summary of the invention
In view of above-mentioned the deficiencies in the prior art, the objective of the invention is to by improvement starting material preparation, blank forming and sintering process, a kind of preparation method who is used for the high purity aluminium oxide sintered compact of growing sapphire crystal is provided, sapphire crystal water white transparency, the defective of using this method to grow are few, can be used to prepare the sapphire wafer that is used for the LED substrate.
The object of the present invention is achieved like this: a kind of preparation method who is used for the high purity aluminium oxide sintered compact of growing sapphire crystal, and it is characterized in that: envrionment conditions is: production plant purifies to be needed more than 10000 grades; Raw material adopts the aluminum oxide powder of 5N purity; Binding agent adopts ρ type aluminum oxide; Compacting tool set is the above alumina-ceramic of 99.99% purity; Sintering oven is a microwave agglomerating furnace; Preparation process is: add the aluminum oxide powder of 5N purity, ρ type aluminum oxide, deionized water and the steel core urethane ball of 5N purity in the urethane ball grinder, ball milling mixed 5 hours, pouring out back sealing in polyethylene plastic bag placed 12 hours, cross 60 eye mesh screens, insert in the alumina-ceramic mould and suppress with 50MPa pressure, the blank that obtains, blank is put into microwave agglomerating furnace, 0.5 hour be warmed up to 1850 ℃, kept 0.5 hour at 1850 ℃, with stove cooling, the alumina sintered body of the 5N purity that obtains.
Purpose of the present invention can also realize like this: described envrionment conditions is: production plant purifies to be needed more than 1000 grades.
Described compacting tool set is alumina-ceramic of inlaying in the above integral sintered alumina-ceramic of 99.99% purity, the metal die or the aluminum oxide coating layer that sprays on metal die.
The part by weight of the ρ type aluminum oxide of the aluminum oxide powder of 5N purity, 5N purity, deionized water and steel core urethane ball is:
3 kilograms of the aluminum oxide powders of 5N purity
ρ type aluminum oxide 30 grams of 5N purity
Deionized water 60 grams
5 kilograms in steel core urethane ball.
Of the present invention have following advantage and an obvious improvement: the alumina sintered body that utilizes preparation method of the present invention to acquire, cooperate ICP-MS to detect ceramic surface and inner purity respectively with laser ablation, find not that with alumina powder jointed the comparing of employed 5N impurity has considerable change.20 kilograms of alumina sintered body pieces are put into the kyropoulos crystal growing furnace, the filling ratio of crucible can reach 90%, the sapphire crystal water white transparency that obtains, visual inspection is without any being mingled with or defective such as micro-bubble, and detecting its dislocation desity is 512 every square centimeter.Experiment showed, that sapphire crystal water white transparency, defective that the alumina sintered body that utilizes preparation method of the present invention to acquire grows are few, can be used to prepare the sapphire wafer that is used for the LED substrate.
Laser ablation is to utilize the method for the concentrated characteristics of pulsed laser energy with the collected specimens of the local flash evapn gasification of sample, not needing to be characterized in the liquid dissolution process of general icp analysis, to have avoided the analytical results instability that causes because of sample contamination sample.
Embodiment
The alumina sintered body of preparation 5N purity, the cleanliness factor of production environment is very important, particularly in China, airborne suspended particulate is very many, slow in indoor air flows speed, sedimentation will take place in little bigger a little particle, the purity of powder had an immense impact on, and be the material that impossible can produce 5N purity so there is not the workshop for the treatment of plant.In the workshop of 10000 grades of cleanliness factors, settled particle can take place seldom, can reach substantially and produce this purity product environment requirement.Certainly, if impurity is had further requirement, can bring up to 1000 grades even 100 grades with purifying rank.
The aluminium oxide granule granularity of hydrolysis method preparation is approximately the 20-30 micron, by pulverizing the leeway of improving its moulding and sintering activity is very limited, and any pulverizing all can more or less bring impurity into, and this is that the alumina-ceramic of preparation 5N purity is abstained from very much.So had better not carry out pulverization process again to 5N is alumina powder jointed.
Its form of high purity aluminium oxide powder of 20-30 micron is just as the fine sand grain, and its inertia is very strong, and each other without any cementability, direct compression moulding is without any feasibility in mould.In order to improve its plasticity, best bet adds binding agent exactly.Common organic binder bond majority in preparation process has all used catalyzer, and binding agent can be brought impurity in preparation process.Though polymer substance at high temperature can be decomposed into volatilizable material and remove, but the impurity of bringing in the preparation adhesive process at high temperature can't decompose volatilization, can stay the ash content of 0.1-0.5%, these grey branches cause fatal infringement to the purity of 5N aluminum oxide.The preparation of aluminium hydroxide of 5N is become ρ type aluminum oxide, and this ρ type aluminum oxide can produce aluminium hydroxide and thin nurse stone colloidal sol after adding moisture, and thin nurse stone colloidal sol can play bonding and solidification.In addition, an amount of nitric acid of adding also can form colloidal sol and play bonding effect in aluminium hydroxide or aluminum oxide, but the nitrogen oxide that decomposites under the high temperature can pollute environment, can corrode sintering oven simultaneously.
In moulding process, mould also can not be ignored the pollution that alumina-ceramic causes.At first, adopt metal die, even the quenching mould steel, its hardness also ratio aluminum oxide particulate hardness is little a lot, alumina particle is very big to the wearing and tearing of mould in pressing process, even sintering can be seen ferric oxide russet on the surface of alumina-ceramic after finishing.Secondly, mould of plastics can't use because bearing big pressing force.In order to overcome this problem, the contriver creatively adopts metal die inside to inlay 5N high purity ceramic chamber lining, and last push-down head adopts the 5N alumina-ceramic, and this design can effectively solve the pollution problem of mould.The mould of whole employing alumina-ceramic also is feasible, but cost can be much higher, and reliability is much lower.The method that adopts plasma spraying is at metal die surface spraying one deck aluminum oxide, also can reach identical effect, but the density of coating has only 80%, and the bonding force with metal is limited simultaneously, easily comes off under long-time repeated stress effect repeatedly.
The volatile matter of refractory materials and heating element also can cause damage to the purity of 5N alumina sintered body in the sintering oven.The application of microwave agglomerating furnace in the stupalith sintering has vicennial history, this sintering oven is once great concern occurring just having caused, because its heating principle is different fully to the understanding of stove with original people, can carry out Fast Sintering to sintered compact, can reach the inaccessiable high temperature of present sintering oven simultaneously; Microwave energy acted directly on ceramic surface and inside simultaneously when this was externally sintered, sintering temperature distributes very evenly, heat-up rate is very fast, the tissue of sintered body that obtains is even, want the agglomerating ceramic heating because of having only in addition, do not have heating element, the temperature of lagging material is also lower on every side, so the ceramic based on very high purity that sintering goes out, density is very big.Along with the maturation of microwave heating technique, manufacturing cost has descended much now, and work reliability is more and more higher, and the size of stove can be done very greatly, and it is fully feasible being used for industrial production.
Embodiment:
The aluminum oxide powder that in 10 liters of urethane ball grinders, adds 3 kilograms of 5N purity, the ρ type aluminum oxide of 30 gram 5N purity, 5 kilograms in deionized water 60 grams and steel core urethane ball, ball milling mixed 5 hours, pouring out back sealing in polyethylene plastic bag placed 12 hours, cross 60 eye mesh screens, insert in the mould of the aluminum oxide lining of inlaying 5N purity and suppress with 50MPa pressure, the blank of the size Φ 200*30mm that obtains, blank is put into microwave agglomerating furnace, 0.5 hour be warmed up to 1850 ℃, kept 0.5 hour at 1850 ℃, with the stove cooling, the alumina sintered body pottery that obtains is of a size of Φ 161*24mm, and density is 3.85g/cm
3, be 96.25% of sapphire theoretical density.Cooperate ICP-MS to detect ceramic surface and inner purity respectively with laser ablation, find not that with alumina powder jointed the comparing of employed 5N purity impurity has considerable change.
20 kilograms of alumina sintered body ceramic blocks are put into the kyropoulos crystal growing furnace, the filling ratio of crucible can reach 90%, the sapphire crystal water white transparency that obtains, visual inspection is without any being mingled with or defective such as micro-bubble, and detecting its dislocation desity is 512 every square centimeter.
Claims (4)
1. preparation method who is used for the high purity aluminium oxide sintered compact of growing sapphire crystal, it is characterized in that: envrionment conditions is: production plant purifies to be needed more than 10000 grades; Raw material adopts the aluminum oxide powder of 5N purity; Binding agent adopts ρ type aluminum oxide; Compacting tool set is the above alumina-ceramic of 99.99% purity; Sintering oven is a microwave agglomerating furnace; Preparation process is: add the aluminum oxide powder of 5N purity, ρ type aluminum oxide, deionized water and the steel core urethane ball of 5N purity in the urethane ball grinder, ball milling mixed 5 hours, pouring out back sealing in polyethylene plastic bag placed 12 hours, cross 60 eye mesh screens, insert in the alumina-ceramic mould and suppress with 50MPa pressure, the blank that obtains, blank is put into microwave agglomerating furnace, 0.5 hour be warmed up to 1850 ℃, kept 0.5 hour at 1850 ℃, with stove cooling, the alumina sintered body of the 5N purity that obtains.
2. the preparation method who is used for the high purity aluminium oxide sintered compact of growing sapphire crystal according to claim 1, it is characterized in that: described envrionment conditions is: production plant purifies to be needed more than 1000 grades.
3. the preparation method who is used for the high purity aluminium oxide sintered compact of growing sapphire crystal according to claim 1 is characterized in that: described compacting tool set is alumina-ceramic of inlaying in the above integral sintered alumina-ceramic of 99.99% purity, the metal die or the aluminum oxide coating layer that sprays on metal die.
4. according to claim 1, the 2 or 3 described preparation methods that are used for the high purity aluminium oxide sintered compact of growing sapphire crystal, it is characterized in that: the part by weight of the ρ type aluminum oxide of the aluminum oxide powder of 5N purity, 5N purity, deionized water and steel core urethane ball is:
3 kilograms of the aluminum oxide powders of 5N purity
ρ type aluminum oxide 30 grams of 5N purity
Deionized water 60 grams
5 kilograms in steel core urethane ball.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102503104A (en) * | 2011-10-27 | 2012-06-20 | 扬州高能新材料有限公司 | Alpha-aluminum oxide quasi-fusion cake microwave sintering method |
| CN102603273A (en) * | 2012-03-10 | 2012-07-25 | 锦州晶城新能源材料制造有限公司 | Preparation method of high-purity sintered alumina for monocrystal sapphire growth |
| CN103011844A (en) * | 2011-12-27 | 2013-04-03 | 江苏有能光电科技有限公司 | Sintering method of alumina powder raw material for LED sapphire |
| CN105272177A (en) * | 2015-11-09 | 2016-01-27 | 南京长江工业炉科技有限公司 | Preparation method of aluminum oxide sintered body |
| CN105777079A (en) * | 2016-01-28 | 2016-07-20 | 深圳市商德先进陶瓷有限公司 | Plasma etching resistant ceramic body and manufacturing method thereof, and plasma etching device |
| CN108329019A (en) * | 2018-02-28 | 2018-07-27 | 新疆三锐佰德新材料有限公司 | Sapphire high density large scale alumina material and preparation method thereof |
| CN109265174A (en) * | 2018-09-21 | 2019-01-25 | 河南晟道科技有限公司 | Ball mill steel core ceramic grinding ball |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102503104A (en) * | 2011-10-27 | 2012-06-20 | 扬州高能新材料有限公司 | Alpha-aluminum oxide quasi-fusion cake microwave sintering method |
| CN103011844A (en) * | 2011-12-27 | 2013-04-03 | 江苏有能光电科技有限公司 | Sintering method of alumina powder raw material for LED sapphire |
| CN102603273A (en) * | 2012-03-10 | 2012-07-25 | 锦州晶城新能源材料制造有限公司 | Preparation method of high-purity sintered alumina for monocrystal sapphire growth |
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| CN105777079A (en) * | 2016-01-28 | 2016-07-20 | 深圳市商德先进陶瓷有限公司 | Plasma etching resistant ceramic body and manufacturing method thereof, and plasma etching device |
| CN108329019A (en) * | 2018-02-28 | 2018-07-27 | 新疆三锐佰德新材料有限公司 | Sapphire high density large scale alumina material and preparation method thereof |
| CN109265174A (en) * | 2018-09-21 | 2019-01-25 | 河南晟道科技有限公司 | Ball mill steel core ceramic grinding ball |
| CN109265174B (en) * | 2018-09-21 | 2021-03-30 | 河南晟道科技有限公司 | Ceramic grinding ball with steel core for ball mill |
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Denomination of invention: Preparation method of high-purity aluminum oxide sintered body for growing sapphire crystal Effective date of registration: 20140513 Granted publication date: 20130320 Pledgee: China Everbright Bank Handan branch Pledgor: Hebei Hengbo Fine Ceramic Material Co., Ltd. Registration number: 2014990000346 |
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Address after: 057250 Hebei city of Handan Province in Quzhou county Luo Zhuang Industrial Zone Patentee after: Hebei Hengbo new materials Polytron Technologies Inc Address before: 057250 in Quzhou County of Hebei province Luo Zhuang Industrial Zone Patentee before: Hebei Hengbo Fine Ceramic Material Co., Ltd. |