CN103304223A - Preparation method of high-purity aluminum oxide ceramic - Google Patents
Preparation method of high-purity aluminum oxide ceramic Download PDFInfo
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- CN103304223A CN103304223A CN2013102322946A CN201310232294A CN103304223A CN 103304223 A CN103304223 A CN 103304223A CN 2013102322946 A CN2013102322946 A CN 2013102322946A CN 201310232294 A CN201310232294 A CN 201310232294A CN 103304223 A CN103304223 A CN 103304223A
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Abstract
The invention discloses a preparation method of a high-purity aluminum oxide ceramic. According to the preparation method, a nano Al2O3 coating formed on the surfaces of aluminum oxide particles is used as a sintering aid to ensure that a small amount of the sintering aid can be uniformly dispersed in a main phase, so that uniform adding of a small dose of the sintering aid is realized. The preparation method not only ensures the purity and performance of the high-purity aluminum oxide ceramic and meets process requirements for preparation of the aluminum oxide ceramic, but also effectively solves the problem that when the particle size difference of main phase powder and the sintering aid is large, particles of a nano auxiliary agent are gathered in a main phase powder particle gap; and moreover, partial over-firing is avoided, so that the uniformity of sintering of the main phase powder particles and the sintering assisting effect of the sintering aid are effectively improved.
Description
Technical field
The present invention relates to technical field of ceramic material, relate in particular to a kind of preparation method of high-purity alumina ceramic.
Background technology
Alumina-ceramic is a kind of with aluminum oxide (AL
2O
3) be the material of main body, have good conductivity, physical strength and high thermal resistance, be the base mateiral of making high strength, wear-resistant, high temperature resistant contour performance ceramic component, be widely used in fields such as machinery, communication, semi-conductor, medicine, food, oil, chemical industry, space flight and aviation.
The fusing point of aluminum oxide is higher, and its sintering temperature is also corresponding higher, and the sintering of especially big particle diameter alumina particle is all the more so, thereby can cause higher energy consumption, the very high preparation cost of generation.For reducing the sintering temperature of aluminum oxide, in its preparation sintering process, need usually to add sintering aid, with the sintering temperature of obvious reduction high-melting-point alumina-ceramic, realize reducing the purpose of preparation cost.The mechanism of action of ceramic post sintering auxiliary agent generally includes following three kinds:
(1) sintering aid itself can form liquid phase under lower temperature, by the mass transfer speed of liquid phase promotion high-melting-point pottery, for example kaolin, B
2O
3, albite, potassium felspar sand etc. be as the sintering of sintering aid for alumina-ceramic.
(2) sintering aid forms eutectic by solid state reaction and sinter, thereby reduction sintering temperature, diffusion and sintering velocity are increased, and for example magnesium oxide can form the Magnesium Silicate q-agent liquid phase with the silicon-dioxide fusion of silicon nitride surface under 1500 ℃ high temperature, forms Mg with silicon nitride simultaneously
2SiO
4And MgSi
3N
2, Mg
2SiO
4And MgSi
3N
2Form eutectic with silicon nitride more than 1600 ℃, can reduce sintering temperature, and promoting the sintering of silicon nitride.
(3) with nano-powder as sintering aid, the character of utilizing the nano-powder fusing point to reduce makes nano-powder have higher sintering activity under lower temperature, promotes the sintering of principal phase with this.
Above which kind of mechanism of action no matter, sintering aid generally can be stayed the combining site of principal phase particle, i.e. crystal boundary place, these materials can cause tangible influence to the character of aluminum oxide.For example, kaolinic interpolation can make the sintering temperature of alumina-ceramic film support (particle diameter of used aluminum oxide is 20～40 μ m) reduce by 50～100 ℃, but kaolin is acid-alkali-corrosive-resisting not, use the 1wt%NaOH solution corrosion after 24 hours, although mass loss has only 0.9%, the intensity of supporter has reduced by 35%.In addition, the sintering aid that contains potassium, sodium adds in the aluminum oxide, can obviously reduce the dielectric coefficient of aluminum oxide, makes it easier to be breakdown.And for the principal phase powder of big particle diameter, the nano-powder sintering aid is easy to reunite in the space of big particle diameter principal phase powder granule, can't play the effect that helps sintering.And, in some particular application, needing high-purity alumina ceramic goods (foreign matter content is lower than 1% or even 0.5%), the use of above-mentioned sintering aid can bring adverse influence to purity and the performance of goods undoubtedly.
Be the preparation high-purity alumina ceramic, prior art also has the nano-aluminum hydroxide of use colloidal sol as sintering aid, not introducing other materials with when guaranteeing purity, effectively reduces the sintering temperature of alumina-ceramic.Yet this method only is suitable for the alumina powder jointed of small particle size, because alumina powder jointed just being easy to of small particle size evenly mixed with nano-aluminum hydroxide colloidal sol, promotes the alumina powder jointed sintering of small particle size by the sintering of nano-aluminum hydroxide colloidal sol.α-Al for big particle diameter
2O
3Powder, nano-aluminum hydroxide colloidal sol can be at big particle diameter α-Al
2O
3Assemble in the gap of particle packing, the colloidal sol of these gatherings preferentially sinters large-size particles in sintering process, helps nodulizing and can't play.In addition, this method is not suitable for the preparation of the alumina-ceramic that needs dried preparation or the clean compact dimensions of needs yet.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of preparation method of high-purity alumina ceramic is provided, by the nanometer Al that forms on the alumina particle surface
2O
3Coating is as sintering aid, improving the even sintering of alumina particle, and guarantees purity and the performance of high-purity alumina ceramic, satisfies the process requirements of alumina-ceramic preparation.
Purpose of the present invention is achieved by the following technical programs:
The preparation method of a kind of high-purity alumina ceramic provided by the invention may further comprise the steps:
(1) aluminum isopropylate is dissolved in the solvent and forms aluminum isopropylate solution, the alumina powder jointed volume of the volume 〉=principal phase of solvent wherein, the consumption of aluminum isopropylate is according to its nanometer Al that generates
2O
30.5～the 25wt% that accounts for the principal phase aluminum oxide determines;
(2) with described aluminum isopropylate solution and alumina powder jointed the mixing of principal phase and obtain mixing suspension;
(3) described mixing suspension is placed hydrothermal reaction kettle, under 120～180 ℃ of temperature, handled 6～12 hours; Remove suspension mixed upper solution then, obtain the aluminum oxide powder slurry of bottom;
(4) with after the described aluminum oxide powder slurry drying, calcine under 750～900 ℃ of temperature in retort furnace, it is alumina powder jointed to obtain pre-treatment;
(5) carry out moulding, calcining to described pre-treatment is alumina powder jointed, obtain the high-purity alumina ceramic product.
Further, solvent is dimethylbenzene in the step of the present invention (1), also can be the solvent of other solubilized aluminum isopropylates.The alumina powder jointed median size of principal phase is 0.05～500 μ m in the described step (1), preferred 0.5～50 μ m.
Calcining temperature is 1100～1800 ℃ in the forming methods such as that the present invention is applicable to is dry-pressing formed, extrusion moulding, gel pouring, injection molding, described step (5).
The present invention has following beneficial effect:
1, the present invention makes a small amount of sintering aid evenly to disperse in principal phase by forming the nano oxidized aluminum coating of one deck on the alumina particle surface, utilizes formed nano particle as sintering aid, has realized the even interpolation of low dose of sintering aid.Prepared nano oxidized aluminum coating is evenly distributed in the surface of main body alumina particle, and can not be filled in the oarse-grained gap, solved the problem that the nano assistant powder granule was assembled when particle diameter differed greatly in big particle diameter principal phase powder granule space, effectively avoided the agglomeration of ceramic post sintering auxiliary agent, realize even dispersion, even and while sintering, avoided the problem of local burning.
2, as sintering aid, the interpolation by low dose has just effectively improved and has helped nodulizing with the nano aluminium oxide that forms on alumina particle surface in the present invention; And do not introduce other material, and the aluminum oxide with principal phase behind the sintering becomes integral body, thereby has guaranteed the purity of high-purity alumina ceramic, and the while does not influence the character of the alumina-ceramic behind the sintering.
3, suitability is wide.No matter the present invention is the alumina powder jointed of big particle diameter or alumina powder jointed than small particle size relatively, and nano aluminium oxide can both be evenly distributed in particle surface, no agglomeration; And the present invention is applicable to various forming methods, needing to be particularly useful for the preparation of the alumina-ceramic of dried preparation or the clean compact dimensions of needs.
Description of drawings
The present invention is described in further detail below in conjunction with embodiment and accompanying drawing:
Fig. 1 is the stereoscan photograph of the embodiment of the invention one its section of high-purity alumina ceramic goods;
Fig. 2 is the transmission electron microscope photo of the embodiment of the invention one its section of high-purity alumina ceramic goods;
Fig. 3 is the stereoscan photograph of the embodiment of the invention two its sections of high-purity alumina ceramic goods.
Embodiment
Embodiment one:
The preparation method of a kind of high-purity alumina ceramic of present embodiment, its step is as follows:
(1) gets the 20g aluminum isopropylate and be dissolved in formation aluminum isopropylate solution in the 100ml dimethylbenzene;
(2) getting 100g alumina powder jointed (W40, median size is 40 μ m) mixes with above-mentioned aluminum isopropylate solution stirring and obtains mixing suspension;
(3) above-mentioned mixing suspension is placed hydrothermal reaction kettle, under 150 ℃ of temperature, handled 10 hours; Remove suspension mixed upper solution then, obtain the aluminum oxide powder slurry of bottom;
(4) above-mentioned aluminum oxide powder is starched in baking oven after oven dry under 100 ℃ of temperature, risen to 800 ℃ with the temperature rise rate of 3 ℃/min and calcine in retort furnace, be incubated 2 hours, it is alumina powder jointed to obtain pre-treatment;
(5) in above-mentioned pre-treatment is alumina powder jointed, add 2wt%PVA, dry-pressing formed under 6Mpa pressure, be pressed into 10 * 10 * 400mm rectangle strip; Temperature rise rate with 1 ℃/min rises to 600 ℃, and the temperature rise rate with 2 ℃/min rises to 1650 ℃ then, is incubated 2 hours, obtains high-purity porous alumina ceramic product, can be used as ceramic film support.
As can be seen from Figure 1, nano aluminium oxide covers the surface of big particle diameter alumina particle.As can be seen from Figure 2, the about 10nm of the thickness of nano oxidized aluminum coating.
Embodiment two:
The preparation method of a kind of high-purity alumina ceramic of present embodiment, its step is as follows:
(1) gets the 20g aluminum isopropylate and be dissolved in formation aluminum isopropylate solution in the 100ml dimethylbenzene;
(2) get 90g alumina powder jointed (W40, median size is 40 μ m), 10g alumina powder jointed (W1, median size is 1 μ m) ball milling mixes and obtains the mixed aluminium oxides powder, mix with above-mentioned aluminum isopropylate solution stirring then and obtain mixing suspension;
(3) above-mentioned mixing suspension is placed hydrothermal reaction kettle, under 180 ℃ of temperature, handled 8 hours; Remove suspension mixed upper solution then, obtain the aluminum oxide powder slurry of bottom;
(4) above-mentioned aluminum oxide powder is starched in baking oven after oven dry under 100 ℃ of temperature, risen to 750 ℃ with the temperature rise rate of 3 ℃/min and calcine in retort furnace, be incubated 2 hours, it is alumina powder jointed to obtain pre-treatment;
(5) in above-mentioned pre-treatment is alumina powder jointed, add 2wt%PVA, dry-pressing formed under 6Mpa pressure, be pressed into 10 * 10 * 400mm rectangle strip; Temperature rise rate with 1 ℃/min rises to 600 ℃, and the temperature rise rate with 2 ℃/min rises to 1500 ℃ then, is incubated 2 hours, obtains high-purity porous alumina ceramic product, can be used as ceramic film support.
As can be seen from Figure 3, nano aluminium oxide is evenly distributed in the surface of alumina particle.
Embodiment three:
The preparation method of a kind of high-purity alumina ceramic of present embodiment and embodiment one difference are:
Alumina powder jointed in the step (2) is 120g; In pre-treatment is alumina powder jointed, add methylcellulose gum, tung oil, glycerol, water in the step (5), obtain suitable pug through batch mixing, refining mud, old etc., obtain pipe shape (or cylindric, hyperchannel tubulose) through extrusion moulding; At 1650 ℃ of temperature lower calcinations, be incubated 2 hours then, obtain high purity aluminium oxide rod (pipe).
Embodiment four:
The preparation method of a kind of high-purity alumina ceramic of present embodiment and embodiment one difference are:
In pre-treatment is alumina powder jointed, add polyacrylic acid and water in the step (5), using ammoniacal liquor to adjust the pH of suspension value is 9.5, at powder: the zirconium white mill is situated between: water=condition under with rotating speed 350r/min ball milling mix 12 hour at 1: 1.5: 1, obtain stable suspension, behind flow casting molding, obtain the curtain coating raw cook; At 1550 ℃ of temperature lower calcinations, be incubated 2 hours then, obtain the high purity aluminium oxide sheet.
Claims (5)
1. the preparation method of a high-purity alumina ceramic is characterized in that may further comprise the steps:
(1) aluminum isopropylate is dissolved in the solvent and forms aluminum isopropylate solution, the alumina powder jointed volume of the volume 〉=principal phase of solvent wherein, the consumption of aluminum isopropylate is according to its nanometer Al that generates
2O
30.5～the 25wt% that accounts for the principal phase aluminum oxide determines;
(2) with described aluminum isopropylate solution and alumina powder jointed the mixing of principal phase and obtain mixing suspension;
(3) described mixing suspension is placed hydrothermal reaction kettle, under 120～180 ℃ of temperature, handled 6～12 hours; Remove suspension mixed upper solution then, obtain the aluminum oxide powder slurry of bottom;
(4) with after the described aluminum oxide powder slurry drying, calcine under 750～900 ℃ of temperature in retort furnace, it is alumina powder jointed to obtain pre-treatment;
(5) carry out moulding, calcining to described pre-treatment is alumina powder jointed, obtain the high-purity alumina ceramic product.
2. the preparation method of high-purity alumina ceramic according to claim 1 is characterized in that: solvent is dimethylbenzene in the described step (1).
3. the preparation method of high-purity alumina ceramic according to claim 1 is characterized in that: the alumina powder jointed median size of principal phase is 0.05～500 μ m in the described step (1).
4. the preparation method of high-purity alumina ceramic according to claim 1 is characterized in that: the alumina powder jointed median size of principal phase is 0.5～50 μ m in the described step (1).
5. the preparation method of high-purity alumina ceramic according to claim 1 is characterized in that: calcining temperature is 1100～1800 ℃ in the described step (5).
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104193310A (en) * | 2014-08-29 | 2014-12-10 | 潮州三环（集团）股份有限公司 | Ceramic material and preparation method thereof |
| CN104987113A (en) * | 2015-07-24 | 2015-10-21 | 合肥凯士新材料贸易有限公司 | Zirconium silicate whisker modified tabular alumina porous ceramic used in LED lamp heat dissipation, and preparation method thereof |
| CN105036717A (en) * | 2015-07-24 | 2015-11-11 | 合肥凯士新材料贸易有限公司 | Flake alumina porous ceramic used for packaging high-power LED and preparation method thereof |
| CN105461293A (en) * | 2016-01-08 | 2016-04-06 | 梁小利 | Low thermal-conductivity aluminum oxide ceramic and preparation method thereof |
| CN107245323A (en) * | 2017-01-10 | 2017-10-13 | 白鸽磨料磨具有限公司 | Production method of alumina abrasive and products thereof |
| CN107963883A (en) * | 2017-12-14 | 2018-04-27 | 上海卡贝尼精密陶瓷有限公司 | A kind of preparation method of high-purity alumina ceramic powder |
| WO2018095277A1 (en) * | 2016-11-25 | 2018-05-31 | 山东硅元新型材料股份有限公司 | Preparation method of plate-shaped corundum ceramic film support |
| CN108298947A (en) * | 2018-01-10 | 2018-07-20 | 淮阴师范学院 | A kind of purposes of attapulgite ceramic film support, preparation method and boracic sintering aid |
| CN110240492A (en) * | 2018-03-07 | 2019-09-17 | 海加尔(厦门)科技有限公司 | A kind of preparation method of the ceramic separation film supporter of acid and alkali-resistance |
| CN113121209A (en) * | 2021-03-26 | 2021-07-16 | 福建华清电子材料科技有限公司 | Preparation method of 996 aluminum oxide ceramic substrate |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104193310A (en) * | 2014-08-29 | 2014-12-10 | 潮州三环（集团）股份有限公司 | Ceramic material and preparation method thereof |
| CN104987113A (en) * | 2015-07-24 | 2015-10-21 | 合肥凯士新材料贸易有限公司 | Zirconium silicate whisker modified tabular alumina porous ceramic used in LED lamp heat dissipation, and preparation method thereof |
| CN105036717A (en) * | 2015-07-24 | 2015-11-11 | 合肥凯士新材料贸易有限公司 | Flake alumina porous ceramic used for packaging high-power LED and preparation method thereof |
| CN105461293A (en) * | 2016-01-08 | 2016-04-06 | 梁小利 | Low thermal-conductivity aluminum oxide ceramic and preparation method thereof |
| WO2018095277A1 (en) * | 2016-11-25 | 2018-05-31 | 山东硅元新型材料股份有限公司 | Preparation method of plate-shaped corundum ceramic film support |
| CN107245323A (en) * | 2017-01-10 | 2017-10-13 | 白鸽磨料磨具有限公司 | Production method of alumina abrasive and products thereof |
| CN107963883A (en) * | 2017-12-14 | 2018-04-27 | 上海卡贝尼精密陶瓷有限公司 | A kind of preparation method of high-purity alumina ceramic powder |
| CN108298947A (en) * | 2018-01-10 | 2018-07-20 | 淮阴师范学院 | A kind of purposes of attapulgite ceramic film support, preparation method and boracic sintering aid |
| CN108298947B (en) * | 2018-01-10 | 2020-10-30 | 淮阴师范学院 | Attapulgite ceramic membrane support, preparation method and application of boron-containing sintering aid |
| CN110240492A (en) * | 2018-03-07 | 2019-09-17 | 海加尔(厦门)科技有限公司 | A kind of preparation method of the ceramic separation film supporter of acid and alkali-resistance |
| CN113121209A (en) * | 2021-03-26 | 2021-07-16 | 福建华清电子材料科技有限公司 | Preparation method of 996 aluminum oxide ceramic substrate |
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