CN102674818B - Method for preparing aluminum oxide ceramics through infiltrating body - Google Patents
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Abstract
The invention relates to a method for preparing aluminum oxide ceramics through infiltrating a body. The method comprises the following steps of: forming alpha-aluminum oxide powder to prepare a ceramic body; presintering the ceramic body; naturally cooling the presintered ceramic body; then immersing in an inhibitor solution and infiltrating; removing water on the surface of the infiltrated body and drying; putting the dried ceramic body in a furnace and sintering to obtain the semitransparent aluminum oxide ceramics.
Description
Technical field
The invention belongs to ceramics processing field, particularly relate to a kind of by the method for infiltration body preparation alumina-ceramic.
Background technology
Alumina-ceramic refers to take aluminum oxide as base material and utilizes ceramic process preparation to have the pottery of certain light transmission.Alumina-ceramic not only has the characteristics such as high temperature resistant, corrosion-resistant, the high insulation of pottery own, high strength, also possess and have the incomparable advantage of the optical property of glass and many other materials institute as low in specific conductivity etc., so alumina-ceramic is gradually at extraordinary instrument manufacturing, lighting engineering, wireless electron technology, the fields such as optics and high-temperature technology obtain increasingly extensive application.
The degree of birefringence of alpha-alumina crystals differs little, and the maximum feature of alumina-ceramic is the transparency and the good perviousness to visible ray and infrared light, and also to have electrical isolation good for alumina-ceramic in addition, the advantage that thermal conductivity is high.Therefore alumina-ceramic is at high-strength gas discharge lamp tube, and high-temperature infrared is surveyed also more and more wider with the application in the fields such as window.
In process of production, high temperature can cause increasing rapidly of alpha-alumina crystals to alumina-ceramic, and this result can cause the inner gas of pottery to have little time to discharge and be closed in the interior bubble that forms of pottery, and affects the translucent effect of alumina-ceramic.For the generation of bubble in inhibited oxidation aluminium pottery, need to introduce the rapid growth that auxiliary agent carrys out inhibited oxidation aluminium grain, allow the gas in pottery overflow if having time.Now conventional inhibitor master be contain have Mg, Zr, La, the isoionic oxide compound of Ca.It is exactly that inhibitor is sneaked into solid form with the form of oxide compound that the traditional technology method of introducing inhibitor mainly contains ball milling hybrid system, chemical method now mainly contains co-precipitation or sol-gel method mixes inhibitor, or direct use has been impregnated with the aluminum oxide powder of inhibitor etc.
The processing method complex process that these are traditional, do time in advance long and need to add the organic materialss such as colloid or granulation liquid when premix, binder removal or degreasing again after moulding, but can not guarantee the thorough of binder removal or degreasing, this is the main gas source of bubble in alumina-ceramic.In traditional technology, the usage quantity of granulation liquid or colloid is between the 5%-10% of alumina weight, although these granulation liquids or colloid can carry out reusing of 5 left and right, but this class material has certain pollution to production environment, because colloid or granulation liquid in base substrate can not thoroughly be removed, part colloid or granulation liquid residual when carrying out high temperature sintering also have part Formed shadow to ring the transmittance of alumina-ceramic except generating carbonic acid gas or water vapor simultaneously.
Present method is when aluminum oxide blank forming, not use any colloid or granulation liquid, and is placed in inhibitor deionized water solution to realize the introducing of inhibitor in molding blank pre-burning.The method has been saved colloid in traditional technology or use and binder removal or the degreasing process of granulation liquid, has reduced cost and has reduced production process.
Summary of the invention
The object of the invention is by this technique and production method, no longer need the use of colloid also not need binder removal operation, and when introducing inhibitor, got rid of the use of nitrate radical or chlorion, when reducing environmental pollution, reduce production costs.
The present invention is achieved by the following technical solutions:
By the method for infiltration body preparation alumina-ceramic, carry out in accordance with the following steps:
(1), by alpha-alumina powder moulding, prepare ceramic body, described ceramic body adopts Hpdc moulding;
(2), the ceramic body of die cast is carried out to presintering processing, calcined temperature is 900-1250 ℃, and soaking time is 0.5-5 hour;
(3), immerse in inhibitor solution after the ceramic body after preheating is cooled to 50-75 ℃ naturally and infiltrate, the infiltration time is 3-8 hour, and infiltration temperature is 25-60 ℃ of constant temperature infiltration;
(4), by dry after the base substrate removal surface water after infiltration, drying temperature is 30-100 ℃, and be 30-60 hour time of drying;
(5), dried ceramic body is placed in to stove sintering, sintering temperature is 1700-1900 ℃, and soaking time is 2-4 hour, obtains translucent alumina ceramics.
Described alpha-alumina powder purity is 99.9%-99.99%, and particle diameter is no more than 20nm.
Described ceramic body moulding adopts the moulding of powder Hpdc, and described pressure is 350-550MPa.
The described inhibitor aqueous solution is saturated calcium hydroxide aqueous solution.
The invention has the beneficial effects as follows:
The method has been saved for the ammonia that the colloid of blank forming or the use of granulation liquid have also been avoided in sintering process because of colloid or granulation liquid is residual when having the generation of carbon black and having avoided because of organic removal or nitrate radical or chlorion at sintering or the pollution of chlorine.
Embodiment
The invention provides a kind of method of passing through infiltration body preparation alumina-ceramic, below by embodiment, describe the present invention.
The present invention is achieved by the following technical solutions:
By the method for infiltration body preparation alumina-ceramic, carry out in accordance with the following steps:
(1), by alpha-alumina powder moulding, prepare ceramic body, described ceramic body adopts Hpdc moulding; Described alpha-alumina powder purity is 99.9%-99.99%, and particle diameter is no more than 20nm.In alternate manner of the present invention, alpha-alumina powder purity be more than 85% all can, when selecting the low aluminum oxide of purity, other material in it can be silicon-dioxide as required, calcium oxide, magnesium oxide, zinc oxide or rare earth oxide etc. are for improving the material of Alumina Ceramics.
Described ceramic body moulding adopts the moulding of powder Hpdc, and described pressure is 350-550MPa, is preferably 500-550MPa in actual industrial production.
Also can select other molding mode in other embodiments, such as the modes such as high pressure injection moulding also can realize object of the present invention.
(2), the ceramic body of die cast is carried out to presintering processing,, calcined temperature is 900-1250 ℃, soaking time is 0.5-5 hour; Best Times is 2-4 hour, the selection of calcined temperature difference to some extent according to parts to be manufactured, particularly when a ceramic product is while being made from multiple components, for the calcined temperature that is fitted into inner parts, higher than the part temperatures in outside, its temperature difference is generally between 150-200 ℃.
(3), immerse in inhibitor solution after the ceramic body after preheating is cooled to 50-75 ℃ naturally and infiltrate, the infiltration time is 3-8 hour, and infiltration temperature is 25-60 ℃ of constant temperature infiltration; If select, not the alumina powder of purity, while including calcium constituent in powder, can omit this operation.
(4), will after the base substrate removal surface water after infiltration, put into oven drying, drying temperature is 30-100 ℃, and be 30-60 hour time of drying; Also can select other drying mode in the present invention but can not select air seasoning, after the pre-burning of air seasoning, the scrap rate of base substrate in sintering process is higher than 30%, and its principle is not clear.
(5), dried ceramic body is placed in to stove sintering, sintering temperature is 1700-1900 ℃, and soaking time is 2-4 hour, obtains transparent alumina ceramics.
The stove using in preparation process can adopt the different type of furnaces also can select the identical type of furnace in pre-burning and sintering two-step.The type of furnace of now using all can be used the present invention to be not particularly limited, but preferred hydrogen furnace, be mainly that fast and product is that water can be absorbed in refining process from escaping gas in base substrate because the temperature of hydrogen furnace raises, reduce this part gas and with billet surface, react again generation under high-temperature condition.And electric furnaces etc. just do not have this advantage.
The described inhibitor aqueous solution is saturated calcium hydroxide aqueous solution.
The above is only the specific descriptions to technical solution of the present invention, and those skilled in the art can improve according to the technical program certainly, and these improvement should be considered in protection scope of the present invention.
Claims (6)
1. by the method for infiltration body preparation alumina-ceramic, it is characterized in that: carry out in accordance with the following steps:
(1), by alpha-alumina powder moulding, prepare ceramic body, described ceramic body adopts Hpdc moulding; Described pressure is 350-550MPa;
(2), the ceramic body of die cast is carried out to presintering processing, calcined temperature is 900-1250 ℃, and soaking time is 0.5-5 hour; The selection of calcined temperature difference to some extent according to parts to be manufactured, when a ceramic product is while being made from multiple components, for the calcined temperature that is fitted into inner parts, higher than the part temperatures in outside, its temperature difference is generally between 150-200 ℃;
(3), immerse in inhibitor solution after the ceramic body after preheating is cooled to 50-75 ℃ naturally and infiltrate, the infiltration time is 3-8 hour, and infiltration temperature is 25-60 ℃ of constant temperature infiltration;
(4), by dry after the base substrate removal surface water after infiltration, drying temperature is 30-100 ℃, and be 30-60 hour time of drying;
(5), dried ceramic body is placed in to stove sintering, sintering temperature is 1700-1900 ℃, and soaking time is 2-4 hour, obtains translucent alumina ceramics.
2. according to claim 1 by the method for infiltration body preparation alumina-ceramic, it is characterized in that: described alpha-alumina powder purity is 99.9%-99.99%, and particle diameter is no more than 20nm.
3. according to claim 1 by the method for infiltration body preparation alumina-ceramic, it is characterized in that: described pressure is 500-550MPa.
4. according to claim 1 by the method for infiltration body preparation alumina-ceramic, it is characterized in that: the described inhibitor aqueous solution is saturated calcium hydroxide aqueous solution.
5. according to claim 1 by the method for infiltration body preparation alumina-ceramic, it is characterized in that: the described type of furnace is hydrogen furnace.
6. according to claim 1 by the method for infiltration body preparation alumina-ceramic, it is characterized in that: described dry employing oven drying.
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| US9287106B1 (en) | 2014-11-10 | 2016-03-15 | Corning Incorporated | Translucent alumina filaments and tape cast methods for making |
| CN105777205B (en) * | 2016-03-07 | 2018-06-05 | 宁波泰格尔陶瓷有限公司 | Wear resistant corrosion resistant transparent alumina ceramics tube preparation method |
| CN111484319B (en) * | 2020-03-27 | 2022-07-05 | 宁波南海泰格尔陶瓷有限公司 | Preparation method of polycrystalline semitransparent alumina ceramic with directionally arranged crystal grains |
| CN114349485B (en) * | 2022-01-11 | 2023-01-10 | 无锡特科精细陶瓷有限公司 | Preparation method of high-hardness alumina ceramic |
| CN114751726B (en) * | 2022-06-10 | 2022-09-02 | 秦皇岛日福陶瓷有限公司 | Environment-friendly processing technology for ceramics |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1699269A (en) * | 2005-05-17 | 2005-11-23 | 叶荣崧 | Process for making tile with natural jade effect |
| CN102093037A (en) * | 2010-12-03 | 2011-06-15 | 清华大学 | Method for preparing semitransparent alumina ceramic by introducing sintering auxiliary agent through impregnated blank |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1699269A (en) * | 2005-05-17 | 2005-11-23 | 叶荣崧 | Process for making tile with natural jade effect |
| CN102093037A (en) * | 2010-12-03 | 2011-06-15 | 清华大学 | Method for preparing semitransparent alumina ceramic by introducing sintering auxiliary agent through impregnated blank |
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Effective date of registration: 20210722 Address after: 315511 Shangtian Street Industrial Park, Fenghua District, Ningbo City, Zhejiang Province (No. 3 Meishan Road) Patentee after: Ningbo Nanhai tiger Ceramics Co., Ltd Address before: 315511 No.2 Meishan Road, Shangtian Industrial Park, Fenghua City, Ningbo City, Zhejiang Province Patentee before: NINGBO TIGER CERAMICS Co.,Ltd. |
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