CN101182210A - Method of synthesizing AlN-SiC composite material while controlling content of carbon and nitrogen - Google Patents
Method of synthesizing AlN-SiC composite material while controlling content of carbon and nitrogen Download PDFInfo
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- CN101182210A CN101182210A CNA2007101772381A CN200710177238A CN101182210A CN 101182210 A CN101182210 A CN 101182210A CN A2007101772381 A CNA2007101772381 A CN A2007101772381A CN 200710177238 A CN200710177238 A CN 200710177238A CN 101182210 A CN101182210 A CN 101182210A
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Abstract
A method of controlling the contents of carbon and nitrogen for synthesizing an AlN-SiC composite material belongs to the technical field of nonmetal mineral deep processing. The preparation technology is using sillimanite as the raw material to synthesize the AlN-SiC composite material by the carbothermal reduction and nitridation process. The technical process is collecting the sillimanite mine, making the sillimanite into fine powder to be sieved through a sieve of 0.074 micron, and binder is added for moulding, drying and firing. The invention utilizes the nonmetal mine of sillimanite which is produced in large quantity and wide used throughout our country as the raw material to prepare for the AlN-SiC composite material with high intensity and heat conduction, which has important application value, and the proportion of the component of AlN-SiC generated after the sintering reaction reaches 70 percent to 90 percent. The preparation technical technology of carbothermal reduction and nitridation process which is adopted by the invention is simple for operating, has low cost and is applicable to the industrialized large production.
Description
Technical field
The invention belongs to non-metallic minerals deep process technology field, particularly proposed a kind of method of controlling carbon, the synthetic AlN-SiC matrix material of nitrogen content.
Background technology
Sillimanite is a kind of high aluminum mineral raw material of natural good anhydrous aluminium silicate, and molecular formula is Al
2O
3SiO
2, Chemical Composition Al
2O
362.93%, SiO 37.07%. rhombic system, crystal are long column shape, needle-like, hair-like, fiber sheet.Because of the foreign matter content difference, color is white, sallow, color such as pink, vitreous luster, Huang Shi hardness 6.5～7.5, proportion 3.23～3.25,1850 ℃ of fusing points. sillimanite irreversibly is converted into mullite through high-temperature calcination, volumetric expansion after the silicon-dioxide calcination that dissociates simultaneously, also no longer to shrink after the cooling. its invert point is 1550～1650 ℃, cubical expansivity 5%～8% all transforms inside and outside the crystal simultaneously, and speed is fast.Current, sillimanite is used as common refractory raw material, and it is less to come from its impurity level.
But, after doctor Lee of Univ Utah USA has invented carbothermal reduction-nitridation (CRN) method,, also established scientific basic for the deep processing of nonmetalliferous ore for traditional nonmetal oxide oxynitride transition (Sialon) provides new method.Oxynitride is the advanced material of inorganic non-metallic structure mineral material, as aluminium nitride, silicon carbide all is the advanced ceramics material of excellent property, but, their development and application have been limited to a certain extent as traditional monophase materials its inherent shortcoming and limitation.In recent years, people find that the two has similarity on atomic size, molecular weight, density and crystalline structure in research AlN-SiC system.The two can form complete solid solution under certain condition, and similar structure and high-temperature behavior mean the compound performance that is expected to improve material of the two.
Aluminium nitride, silicon carbide and simple substance carbon all are under the jurisdiction of highly heat-conductive material, and for example aluminium nitride can be done baseplate material.Current, be object with the sillimanite ore deposit, by accurate carbon, nitrogen content control, the method for preparing the AlN-SiC material does not also have patent report, and therefore, the present invention is a kind of new technology in the preparation method of AlN-SiC material (small portion of residual carbon).
Summary of the invention
The purpose of this invention is to provide a kind of method of controlling carbon, the synthetic AlN-SiC matrix material of nitrogen content, prepare high strength, high heat conduction new texture material.
The present invention utilizes sillimanite to be raw material, adopts high temperature reduction nitrogenize technology, and the aluminum oxide silicon oxide in-situ reducing in the sillimanite is become the AlN-SiC matrix material, makes it to become high strength, high heat conduction new texture material.Processing step is:
(1) collection and powder process: employed sillimanite ore comes from the Gongyi, Henan.The sillimanite ore that collects is made fine powder through grinding, and cross 0.074 μ m sieve; The composition of described sillimanite ore is: SiO
2Account for 50～54%, Al
2O
3Account for 40～46%, all the other are for containing sodium, iron, calcium, titanyl compound;
(2) oven dry: put into baking oven and dry, bake out temperature is: 70～80 ℃;
(3) mix: sillimanite powder and powdered graphite (wherein, the quality of Graphite Powder 99 is 18～25%) mixing back adding polyvinyl alcohol are made binding agent, mix, the add-on of binding agent is 3～5%;
(4) moulding: mixed raw materials is pressed into base substrate;
(5) drying: base substrate was placed 70～90 ℃ of baking ovens dry 8～10 hours, become dry body;
(6) burn till: dry body is buried carbon put into nitriding furnace, the control nitrogen flow is 0.1～0.25L/min, carries out the carbothermal reduction-nitridation sintering, 1550～1580 ℃ of sintering temperatures, soaking time 4～5 hours;
(7) cooling: when temperature drops to 200～400 ℃, cut off furnace power, close source nitrogen, naturally cool to room temperature, obtain the AlN-SiC matrix material.Take out sample, test.
The invention has the advantages that:
(1) found a kind of novel raw mineral materials that is used to prepare the AlN-SiC material.Raw materials cost is cheap and mineral resources abundant, and the AlN-SiC component proportions of burning till the generation of reaction back can reach 70%-90%, and very high using value is arranged.
(2) the carbothermal reduction-nitridation method preparing technique process that is adopted in the invention is simple to operate, and cost is low, is fit to following industrialized production.
Description of drawings
Fig. 1 is the XRD figure that the present invention prepares the burnt product of AlN-SiC material.
Embodiment
Below introduce the specific embodiment of the present invention by description to embodiment
Embodiment 1:
The sillimanite ore that collects is worn into fine powder, cross 0.074 μ m sieve, measure its concrete moiety ratio.To put into 80 ℃ of dryings of thermostatic drying chamber in calculating the compression moulding behind the sillimanite powder of weighing and the 20% Graphite Powder 99 thorough mixing as a result of gained ratio, use graphite landfill goods afterwards, put into electric furnace, feed N
2As protection gas and reactant gases, feeding speed is 0.1L/min.Temperature is risen to 1550 ℃, be incubated 4 hours, reaction finishes the back powered-down, naturally cools to room temperature.AlN-SiC component proportions in the burnt product that obtains as can be known by XRD analysis can reach 72%.
Embodiment 2:
The sillimanite ore that collects is worn into fine powder, cross 0.074 μ m sieve, measure its concrete moiety ratio.With calculating the compression moulding behind the sillimanite powder of weighing and the 25% Graphite Powder 99 thorough mixing as a result of gained ratio, put into 80 ℃ of dryings of thermostatic drying chamber, use graphite landfill goods afterwards, put into electric furnace, feed N
2As protection gas and reactant gases, feeding speed is 0.2L/min.Temperature is risen to 1580 ℃, be incubated 4 hours, reaction finishes the back powered-down, naturally cools to room temperature.AlN-SiC component proportions in the burnt product that obtains as can be known by XRD analysis can reach 88%.
Claims (3)
1. method of controlling the synthetic AlN-SiC matrix material of carbon, nitrogen content is characterized in that processing step is:
(1) collection and powder process: the sillimanite ore that collects is made fine powder through grinding, and cross O.074 μ m sieve;
(2) oven dry: put into baking oven and dry, bake out temperature is: 70～80 ℃;
(3) mix: the sillimanite powder is mixed with powdered graphite, and wherein, the quality of Graphite Powder 99 is 18～25%, mixes back adding polyvinyl alcohol and makes binding agent, and the add-on of binding agent is 3～5%;
(4) moulding: step (3) mixed raw materials is pressed into base substrate;
(5) drying: base substrate was placed 70～90 ℃ of baking ovens dry 8～10 hours, become dry body;
(6) burn till: dry body is buried carbon put into nitriding furnace, the control nitrogen flow is 0.1～0.25L/min, carries out the carbothermal reduction-nitridation sintering, 1550～1580 ℃ of sintering temperatures, soaking time 4～5 hours;
(7) cooling: when temperature drops to 200～400 ℃, cut off furnace power, close source nitrogen, naturally cool to room temperature, obtain the AlN-SiC matrix material.
2. in accordance with the method for claim 1, it is characterized in that the composition of described sillimanite ore is: SiO
2Account for 50～54%, Al
2O
3Account for 40～46%, all the other are for containing sodium, iron, calcium, titanyl compound.
3. in accordance with the method for claim 1, it is characterized in that bake out temperature is: 70～80 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007101772381A CN100532327C (en) | 2007-11-13 | 2007-11-13 | Method of synthesizing AlN-SiC composite material while controlling content of carbon and nitrogen |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007101772381A CN100532327C (en) | 2007-11-13 | 2007-11-13 | Method of synthesizing AlN-SiC composite material while controlling content of carbon and nitrogen |
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|---|---|
| CN101182210A true CN101182210A (en) | 2008-05-21 |
| CN100532327C CN100532327C (en) | 2009-08-26 |
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|---|---|---|---|
| CNB2007101772381A Expired - Fee Related CN100532327C (en) | 2007-11-13 | 2007-11-13 | Method of synthesizing AlN-SiC composite material while controlling content of carbon and nitrogen |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102731095A (en) * | 2012-07-17 | 2012-10-17 | 山东宝纳新材料有限公司 | SiC (silicon carbide)-AlN (aluminium nitride) ceramic composite material with high thermal conductivity and preparation method of composite material |
| RU2490232C1 (en) * | 2012-02-17 | 2013-08-20 | Мансур Хузиахметович Зиатдинов | METHOD OF OBTAINING FIRE-PROOF MATERIAL BASED ON SILICON BETA-NITRIDE β-Si3N4 |
| CN103641483A (en) * | 2013-12-16 | 2014-03-19 | 武汉科技大学 | Method for preparing AlN/SiC composite ceramic powder from biomass power plant ash |
| CN109852799A (en) * | 2019-04-11 | 2019-06-07 | 昆明理工大学 | A kind of bauxite prepares metallic aluminium and the method for SiC |
| CN111592342A (en) * | 2020-05-27 | 2020-08-28 | 西北工业大学 | Alumina ceramic powder, alumina ceramic and preparation method thereof |
-
2007
- 2007-11-13 CN CNB2007101772381A patent/CN100532327C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2490232C1 (en) * | 2012-02-17 | 2013-08-20 | Мансур Хузиахметович Зиатдинов | METHOD OF OBTAINING FIRE-PROOF MATERIAL BASED ON SILICON BETA-NITRIDE β-Si3N4 |
| CN102731095A (en) * | 2012-07-17 | 2012-10-17 | 山东宝纳新材料有限公司 | SiC (silicon carbide)-AlN (aluminium nitride) ceramic composite material with high thermal conductivity and preparation method of composite material |
| CN102731095B (en) * | 2012-07-17 | 2013-09-04 | 山东宝纳新材料有限公司 | SiC (silicon carbide)-AlN (aluminium nitride) ceramic composite material with high thermal conductivity and preparation method of composite material |
| CN103641483A (en) * | 2013-12-16 | 2014-03-19 | 武汉科技大学 | Method for preparing AlN/SiC composite ceramic powder from biomass power plant ash |
| CN103641483B (en) * | 2013-12-16 | 2015-06-03 | 武汉科技大学 | Method for preparing AlN/SiC composite ceramic powder from biomass power plant ash |
| CN109852799A (en) * | 2019-04-11 | 2019-06-07 | 昆明理工大学 | A kind of bauxite prepares metallic aluminium and the method for SiC |
| CN111592342A (en) * | 2020-05-27 | 2020-08-28 | 西北工业大学 | Alumina ceramic powder, alumina ceramic and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN100532327C (en) | 2009-08-26 |
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Assignee: Liaoning Fucheng refractories (Group) Co., Ltd. Assignor: University of Science and Technology Beijing Contract record no.: 2012990000469 Denomination of invention: Method of synthesizing AlN-SiC composite material while controlling content of carbon and nitrogen Granted publication date: 20090826 License type: Exclusive License Open date: 20080521 Record date: 20120703 |
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Granted publication date: 20090826 Termination date: 20121113 |