CN102603277A - Preparation method for cordierite - Google Patents
Preparation method for cordierite Download PDFInfo
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- CN102603277A CN102603277A CN2011100213818A CN201110021381A CN102603277A CN 102603277 A CN102603277 A CN 102603277A CN 2011100213818 A CN2011100213818 A CN 2011100213818A CN 201110021381 A CN201110021381 A CN 201110021381A CN 102603277 A CN102603277 A CN 102603277A
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Abstract
The invention provides a preparation method for cordierite, which comprises the following steps of: 1) evenly mixing ceramic powder containing magnesium oxide, alumina and quartz with sintering aid, adding polyvinyl alcohol aqueous solution, and carrying out isostatic compaction after the polyvinyl alcohol aqueous solution is evenly dispersed to obtain a cordierite prefabricating product; and 2) carrying out microwave sintering to the cordierite prefabricating product obtained in step (1) to obtain the cordierite, wherein the microwave sintering temperature is 1100-1200 DEG C. With the preparation method provided by the invention, a cordierite product with high density can be obtained, and the preparation method has the advantages of simplified technology and low cost and is suitable for large-scale industrial production.
Description
Technical field
The invention belongs to field of ceramic material preparation, relate in particular to a kind of preparation method of trichroite.
Background technology
Trichroite (2MgO-2Al
2O
3-5SiO
2) have extremely low thermal expansivity and higher thermotolerance, therefore can be used as the heat shock resistance material; In addition, trichroite also has extremely low dielectric loss characteristics.Therefore cordierite ceramic can be widely used in thermal shock resistance and the strict various fields of thermal expansion, and for example ceramic kiln furniture, vehicle exhaust are handled technical fields such as catalyst carrier, ceramic interchanger, electron device.
At present the technology of preparation trichroite adopts the high temperature solid state reaction synthesis method mostly, and this method has that production technique is simple, the production efficiency advantages of higher, but synthesis temperature is too high in this method, causes energy expenditure big, and production cost is higher.Also adopt ultra-high voltage moulding or hot isostatic pressing to prepare trichroite densification ceramic product in the prior art, but the density of the cordierite ceramic product that these two kinds of methods obtain is lower.In addition, the ultra-high voltage moulding can only obtain the square product of solid shape, and Application Areas is narrower; And the hot isostatic pressing method is primarily aimed at the very high cordierite ceramic material of sintering temperature, so this method is high to the heatproof characteristic and the complicated shape requirement of sheath material, and cost is higher, is inappropriate for industrial application.
Summary of the invention
The invention solves that the trichroite density that exists in the prior art is low, complicated process of preparation, cost technical problems of high.
The invention provides a kind of preparation method of trichroite, may further comprise the steps:
1) will contain Natural manganese dioxide, aluminum oxide, quartzy ceramic powder and sintering aid mixes, and adds the aqueous solution of Z 150PH, the isostatic pressing afterwards that is uniformly dispersed obtains the trichroite prefabrication;
2) the trichroite prefabrication to step (1) carries out microwave sintering, obtains trichroite; The temperature of microwave sintering is 1100-1200 ℃.
Among the preparation method of trichroite provided by the invention, obtain the trichroite prefabrication, can make the trichroite prefabrication have definite shape, can guarantee that again the pore of trichroite prefabrication minimizes through isostatic pressing; Then the trichroite prefabrication is carried out microwave sintering; And controlled microwave agglomerating temperature is 1100-1200 ℃; Thereby accurately controlling the trichroite prefabrication is heated evenly; Whole and the partial temperature of trichroite prefabrication is unified, so trichroite prefabrication internal stress in the microwave sintering process is little, can not produce sintering warpage under the prerequisite of assurance cordierite ceramic product high-compactness; In addition, microwave sintering can be accelerated the closed pore process of trichroite prefabrication than ordinary sinter quick heating, thereby obtains the higher trichroite of density.Preparing method provided by the invention can obtain the trichroite goods of high-compactness, work simplification, and cost is lower, is suitable for large-scale commercial prodn.
Embodiment
The invention provides a kind of preparation method of trichroite, may further comprise the steps:
1) will contain Natural manganese dioxide, aluminum oxide, quartzy ceramic powder and sintering aid mixes, and adds the aqueous solution of Z 150PH, the isostatic pressing afterwards that is uniformly dispersed obtains the trichroite prefabrication;
2) the trichroite prefabrication to step (1) carries out microwave sintering, obtains trichroite; The temperature of microwave sintering is 1100-1200 ℃.
Preparation in accordance with the present invention; Earlier ceramic powder and sintering aid are mixed; The aqueous solution that the adds Z 150PH then preparation ceramic size that is uniformly dispersed; Obtain the trichroite prefabrication through isostatic pressing, can make the trichroite prefabrication have definite shape, can guarantee that again the pore of trichroite prefabrication minimizes; Pass through microwave sintering at last; And controlled microwave agglomerating temperature is 1100-1200 ℃, is heated evenly thereby accurately control the trichroite prefabrication, and its whole and partial temperature is unified; Therefore trichroite prefabrication internal stress in the microwave sintering process is little, can not produce sintering warpage.
In addition, the common high temperature sintering of available technology adopting, sintering time is longer, causes green compact amount of localized heat in sintering process to be assembled, and influences the sintering densification process, thereby is difficult to prepare the higher and consistence better products of density.And among the present invention the trichroite prefabrication being adopted microwave sintering, quick heating can be accelerated the closed pore process of trichroite prefabrication, thereby obtains the higher trichroite of density.
Among the present invention, will contain the method that Natural manganese dioxide, aluminum oxide, quartzy ceramic powder and sintering aid mix and to adopt variety of way of the prior art, and for example can directly stir and make its mixing ceramic powder, sintering aid.Under the preferable case, can ceramic powder and sintering aid be dispersed in the organic solvent, drying makes the organic solvent volatilization.Concrete steps comprise: in ceramic powder and sintering aid, add organic solvent, stir, heat drying makes the organic solvent volatilization then, promptly obtains the ceramic powder and the sintering aid that mix.
More preferably under the situation, be benchmark with the ceramic powder of 100 weight parts, the consumption of organic solvent is the 130-160 weight part.Said organic solvent can adopt and well known to a person skilled in the art various low boiling point solvents, for example is selected from least a in acetone, ethanol, the ETHYLE ACETATE.
Among the present invention, ceramic powder is used to prepare trichroite (2MgO-2Al
2O
3-5SiO
2), therefore can form the consumption of confirming various powder in the ceramic powder according to the theory of trichroite.Under the preferable case, be benchmark with the total mass of ceramic powder, magnesian content is 33-35wt%, and the content of aluminum oxide is 13-14wt%, and quartzy content is 52-53wt%.
As those skilled in the art's common practise, therefore the sintering temperature of trichroite and its second-order transition temperature is approaching, firing range is narrower is difficult to densified sintering product under the situation that does not have sintering aid to exist.Therefore, among the preparation method of trichroite provided by the invention, also need add sintering aid.Ceramic powder with 100 weight parts is a benchmark, and the consumption of sintering aid is 0.5-0.6wt%.Among the present invention, the sintering aid that is adopted is conventionally known to one of skill in the art, for example is selected from quicklime (CaO), titanium oxide (TiO
2), chromic oxide (Cr
2O
3) at least a.
According to the method for the invention, behind the ceramic powder and sintering aid that obtains mixing, add the aqueous solution of Z 150PH (PVA) in this mixed system, the preparation ceramic size is uniformly dispersed.Z 150PH improves the sticking power between each powder in the mixed system as sticker, helps follow-up isostatic pressing on the one hand, prevents that on the other hand the trichroite prefabrication deforms in the sintering process.Z 150PH is sheet, cotton-shaped or pulverulent solids; For improving the dispersiveness of ceramic size; Therefore earlier Z 150PH is mixed with polyvinyl alcohol solution, and Z 150PH is insoluble to common organic solvent, water-soluble; Therefore the solvent of polyvinyl alcohol solution adopts water, the i.e. aqueous solution of Z 150PH among the present invention.
The consumption of water is too much unsuitable in the aqueous solution of said Z 150PH, and under the preferable case, the content of Z 150PH is 5-7wt%, prevents to prolong follow-up sintering time, causes the product distortion.The consumption of Z 150PH can not be very little, otherwise between each powder sticking power a little less than; The consumption of Z 150PH also is difficult for too much, otherwise the use temperature of trichroite, thermal expansivity and dielectric properties all can receive influence in various degree.More preferably under the situation, be benchmark with the ceramic powder of 100 weight parts, the consumption of the aqueous solution of Z 150PH is the 4-6 weight part.
Ceramic size is placed isostatic tooling, carry out isostatic pressing, obtain the trichroite prefabrication.The method of said isostatic pressing is conventionally known to one of skill in the art, for example can carry out through isostatic pressing machine.Among the present invention, said isostatic pressing directly at room temperature gets final product, and need not to carry out hot isostatic pressing, therefore heatproof characteristic and shape of product is not had particular requirement.Under the preferable case, the forming pressure position 300-500MPa of isostatic pressing.
According to the method for the invention, the trichroite prefabrication is carried out microwave sintering, can obtain said trichroite; The temperature of microwave sintering is 1100-1200 ℃.When the trichroite prefabrication is carried out microwave sintering; Heat directly acts on the trichroite prefabrication and is evenly distributed, and is heated evenly thereby accurately control the trichroite prefabrication, and its whole and partial temperature is unified; Make that the internal stress of trichroite prefabrication is little in the sintering process, can not produce sintering warpage.In addition, microwave sintering heats up very fast, accelerates the closed pore process of trichroite prefabrication, thereby effectively shortens sintering time, has reduced the heat local accumulation effect that long-time sintering brings, and obtains the trichroite of high-compactness.Therefore, need not of microwave sintering time of the present invention is long, and under the preferable case, sintering time is 18-25min.More preferably under the situation, the temperature of microwave sintering is 1150 ℃.
Below in conjunction with embodiment the present invention is described further.The raw material that adopts all is commercially available in embodiment and the Comparative Examples.
Embodiment 1
(1) with 33 weight part Natural manganese dioxide, 14 weight part aluminum oxide, 53 weight parts quartz, 0.2 weight part CaO and 0.3 weight part TiO
2Be scattered in after the mixing in the ethanol, electronic stirring 60min makes uniform mixing, and heat drying makes the ethanol volatilization.
(2) the past dried mixed system of step (1) adds the polyvinyl alcohol water solution of the 6wt% of 5 weight parts, stirs to make to mix, and granulation is inserted in the isostatic tooling then, on isostatic pressing machine, carries out moulding and obtains prefabrication, and compacting pressure is 400MPa.
(3) prefabrication with step (2) places microwave oven, and 1100 ℃ of following sintering 20min obtain cordierite products S1.
Embodiment 2
(1) with 13.5 weight part aluminum oxide, 33.5 weight part Natural manganese dioxide, 53 weight parts quartz, 0.2 weight part CaO and 0.3 weight part TiO
2Be scattered in after the mixing in the ethanol, electronic stirring 60min makes uniform mixing, and heat drying makes the ethanol volatilization.
(2) the past dried mixed system of step (1) adds the polyvinyl alcohol water solution of the 6wt% of 5 weight parts, stirs to make to mix, and granulation is inserted in the isostatic tooling then, on isostatic pressing machine, carries out moulding and obtains prefabrication, and compacting pressure is 400MPa.
(3) prefabrication with step (2) places microwave oven, and 1200 ℃ of following sintering 20min obtain cordierite products S2.
Embodiment 3
(1) with 13.5 weight part aluminum oxide, 33.5 weight part Natural manganese dioxide, 53 weight parts quartz, 0.2 weight part CaO and 0.3 weight part TiO
2Be scattered in after the mixing in the ethanol, electronic stirring 60min makes uniform mixing, and heat drying makes the ethanol volatilization.
(2) the past dried mixed system of step (1) adds the polyvinyl alcohol water solution of the 6wt% of 5 weight parts, stirs to make to mix, and granulation is inserted in the isostatic tooling then, on isostatic pressing machine, carries out moulding and obtains prefabrication, and compacting pressure is 500MPa.
(3) prefabrication with step (2) places microwave oven, and 1150 ℃ of following sintering 20min obtain cordierite products S3.
Comparative Examples 1
(1) with 13.5 weight part aluminum oxide, 33.5 weight part Natural manganese dioxide, 53 weight parts quartz, 0.2 weight part CaO and 0.3 weight part TiO
2Be scattered in after the mixing in the ethanol, electronic stirring 60min makes uniform mixing, and heat drying makes the ethanol volatilization.
(2) the past dried mixed system of step (1) adds the polyvinyl alcohol water solution of the 6wt% of 5 weight parts, stirs to make to mix granulation; Pack in the punching block; Dry pressing under the 50Mpa uniaxial pressure is put into then under 1150 ℃ of the High Temperature Furnaces Heating Apparatuss and is carried out sintering, insulation 3h; Obtain cordierite products, be designated as DS1.
Performance test:
(the Cu target, λ=0.15405nm) S1-S3 and DS1 are carried out thing crystal structure analysis mutually writes down the content of trichroite phase in each sample to adopt Japanese D/MAX-PC2200 X x ray diffractometer x of science.
Adopt the density of Archimedes's drainage test S1-S3 and DS1, compare, calculate the density of each sample with theoretical density 2.59.
Test result is as shown in table 1.
Table 1
| Sample | S1 | S2 | S3 | DS1 |
| Trichroite phase purity | 96.2% | 98.5% | 97.3% | 92.7% |
| Density | 2.51 | 2.57 | 2.53 | 2.12 |
| Density | 96.9% | 99.2% | 97.7% | 93% |
Test result by last table 1 can find out that the cordierite ceramic sample S1-S3 that embodiment 1-3 prepares is guaranteeing that its density is also apparently higher than Comparative Examples 1 under the higher prerequisite of purity.
Preparing method provided by the invention combines with microwave sintering process through waiting static pressure premolding, can obtain the trichroite of high purity, high-compactness, work simplification, and cost is lower, is very suitable for industrial production.
Claims (10)
1. the preparation method of a trichroite may further comprise the steps:
1) will contain Natural manganese dioxide, aluminum oxide, quartzy ceramic powder and sintering aid mixes, and adds the aqueous solution of Z 150PH, the isostatic pressing afterwards that is uniformly dispersed obtains the trichroite prefabrication;
2) the trichroite prefabrication to step (1) carries out microwave sintering, obtains trichroite; The temperature of microwave sintering is 1100-1200 ℃.
2. preparation method according to claim 1 is characterized in that, the method that ceramic powder and sintering aid mix in the step (1) comprises ceramic powder and sintering aid are dispersed in the organic solvent that drying is volatilized organic solvent.
3. preparation method according to claim 2 is characterized in that, is benchmark with the ceramic powder of 100 weight parts, and the consumption of organic solvent is the 130-160 weight part.
4. according to claim 2 or 3 described preparing methods, it is characterized in that organic solvent is selected from least a in acetone, ethanol, the ETHYLE ACETATE.
5. preparation method according to claim 1 is characterized in that, is benchmark with the total mass of ceramic powder, and magnesian content is 33-35wt%, and the content of aluminum oxide is 13-14wt%, and quartzy content is 52-53wt%; Ceramic powder with 100 weight parts is a benchmark, and the consumption of sintering aid is the 0.5-0.6 weight part.
6. according to claim 1 or 5 described preparing methods, it is characterized in that said sintering aid is selected from least a in quicklime, titanium oxide, the chromic oxide.
7. preparation method according to claim 1 is characterized in that, the content of Z 150PH is 5-7wt% in the aqueous solution of Z 150PH.
8. preparation method according to claim 7 is characterized in that, is benchmark with the ceramic powder of 100 weight parts, and the consumption of the aqueous solution of Z 150PH is the 4-6 weight part.
9. preparation method according to claim 1 is characterized in that, the forming pressure position 300-500MPa of isostatic pressing.
10. preparation method according to claim 1 is characterized in that, the temperature of microwave sintering is 1150 ℃, and sintering time is 18-25min.
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| CN201110021381.8A CN102603277B (en) | 2011-01-19 | 2011-01-19 | Preparation method for cordierite |
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|---|---|---|---|
| CN201110021381.8A CN102603277B (en) | 2011-01-19 | 2011-01-19 | Preparation method for cordierite |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105819846A (en) * | 2016-03-13 | 2016-08-03 | 浙江展邦电子科技有限公司 | Cordierite type microwave medium ceramic material and preparation method thereof |
| CN107434410A (en) * | 2017-08-28 | 2017-12-05 | 中国兵器工业第五二研究所烟台分所 | A kind of cordierite ceramic raw powder's production technology |
| CN115849925A (en) * | 2022-12-30 | 2023-03-28 | 江苏材睿科技有限公司 | Preparation method of pressureless sintering refractory material |
| CN116848074A (en) * | 2021-03-05 | 2023-10-03 | Ａｇｃ株式会社 | Cordierite sintered body and method for producing same |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101189199A (en) * | 2005-05-31 | 2008-05-28 | 康宁股份有限公司 | Low CTE cordierite body and methods of manufacturing same |
| CN101381240A (en) * | 2008-10-09 | 2009-03-11 | 武汉理工大学 | Method for preparing dichroite heat proof/refractory materials |
| WO2010141000A1 (en) * | 2009-06-05 | 2010-12-09 | Corning Incorporated | Cordierite-forming batch materials and methods of using the same |
-
2011
- 2011-01-19 CN CN201110021381.8A patent/CN102603277B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101189199A (en) * | 2005-05-31 | 2008-05-28 | 康宁股份有限公司 | Low CTE cordierite body and methods of manufacturing same |
| CN101381240A (en) * | 2008-10-09 | 2009-03-11 | 武汉理工大学 | Method for preparing dichroite heat proof/refractory materials |
| WO2010141000A1 (en) * | 2009-06-05 | 2010-12-09 | Corning Incorporated | Cordierite-forming batch materials and methods of using the same |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105819846A (en) * | 2016-03-13 | 2016-08-03 | 浙江展邦电子科技有限公司 | Cordierite type microwave medium ceramic material and preparation method thereof |
| CN107434410A (en) * | 2017-08-28 | 2017-12-05 | 中国兵器工业第五二研究所烟台分所 | A kind of cordierite ceramic raw powder's production technology |
| CN107434410B (en) * | 2017-08-28 | 2020-08-11 | 中国兵器工业第五二研究所烟台分所 | Preparation method of cordierite ceramic powder |
| CN116848074A (en) * | 2021-03-05 | 2023-10-03 | Ａｇｃ株式会社 | Cordierite sintered body and method for producing same |
| CN115849925A (en) * | 2022-12-30 | 2023-03-28 | 江苏材睿科技有限公司 | Preparation method of pressureless sintering refractory material |
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