CN1727308A - Method for preparing beta-'Sailong' ceramic powder - Google Patents
Method for preparing beta-'Sailong' ceramic powder Download PDFInfo
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- CN1727308A CN1727308A CN 200410053282 CN200410053282A CN1727308A CN 1727308 A CN1727308 A CN 1727308A CN 200410053282 CN200410053282 CN 200410053282 CN 200410053282 A CN200410053282 A CN 200410053282A CN 1727308 A CN1727308 A CN 1727308A
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- ceramic powder
- sialon
- aluminum
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- 239000000843 powder Substances 0.000 title claims abstract description 15
- 239000000919 ceramic Substances 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 title description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 20
- 229910052751 metal Inorganic materials 0.000 claims abstract description 10
- 239000002184 metal Substances 0.000 claims abstract description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 15
- 239000002994 raw material Substances 0.000 claims description 14
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 6
- 239000000376 reactant Substances 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 239000002210 silicon-based material Substances 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000203 mixture Substances 0.000 abstract description 5
- 238000002156 mixing Methods 0.000 abstract description 3
- 239000011449 brick Substances 0.000 description 4
- 239000003245 coal Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000004134 energy conservation Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002440 industrial waste Substances 0.000 description 2
- 238000005121 nitriding Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 239000011819 refractory material Substances 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910020968 MoSi2 Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 208000012839 conversion disease Diseases 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000010433 feldspar Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000006188 syrup Substances 0.000 description 1
- 235000020357 syrup Nutrition 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
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- Ceramic Products (AREA)
Abstract
A refractory beta-sialon ceramic powder is prepared from aluminium oxide (45-65 Wt%), metallic si material (35-45) and metallic Al material (0-15) through proportional mixing, loading the mixture in reactor, filling high-purity high-pressure N2, using metal wire to ignit the mixture, reaction and ball grinding. Its advantages are high output rate and performance.
Description
(I) technical field
The invention relates to the field of refractory materials, in particular to a preparation method of β -sialon ceramic powder.
(II) background of the invention
Sialon is a compound composed of silicon, aluminum, oxygen and nitrogen, and is called "silica aluminum Oxynitcle" in English, called Sialon for short. Having the chemical formula Si6-zAlzOzN8-z(z is more than 0 and less than or equal to 4.2), wherein z is the number of N atoms replaced by O atoms β -Sialon belongs to a hexagonal system, the thermal shock resistant breaking strength is excellent, and the performance comes from a low thermal expansion coefficient and is 2-3 multiplied by 10-6k-1. Oxidation of sialon material to form SiO on the surface2Or mullite, and has excellent oxidation resistance. The sialon material has excellent mechanical performance and thermal shock resistance at high temperature, small expansion coefficient, high chemical stability, high corrosion resistance, high molten metal resistance and high antioxidant capacity, and is ideal material for refractory material, sealing ring, bearing and valve body.
Chinese patent CN 02146408 discloses a method for preparing BetaeSailon, which adopts coal gangue, coal powder and nitrogen as raw materials, and the synthesis process comprises the steps of pre-mixing the raw material fine powder according to the required proportion, adding a binding agent for mixing, pressing and molding, drying, sintering and synthesizing under the reducing and nitriding atmosphere, cooling and discharging, wherein the raw material fine powder is finely ground to less than 0.08mm, the binding agent adopts syrup, the atmosphere is nitrogen, the sintering and synthesizing temperature is 1400 ℃, keeping the temperature for 8 hours, and then burning to 1600 ℃, keeping the temperature for 2 hours[x]Si[12-(m+n)]Al[m+n]OnN[16-n]The values of x, M and n in the formula are used as main parameters for designing Sialon ceramic (when M is Nd, Sm, Gd, Dy, Y and Yb, x is more than 0.33 and less than 0.67, M is 3x, M is 2n, when M is Ca, x is more than 0.4 and less than 1.4, and M is 2n is 2x), the raw materials are ball-milled and dried, then synthesized by high-temperature self-propagating process and processed to obtain single-phase α -Sialon powder material, which has very good sintering property, and can be used at 1600-1800 deg.C without any impurityPressed and sintered, the density reaches 3.07g/cm3A hardness of 15.53GPa and a toughness of 4.72 MPa-m[1/2]And has a composition much higher than Al2O3And ZrO2Ceramics and erosion resistance superior to SiC ceramics. The two methods have the disadvantages of mixed raw material components, high preparation cost and more reactant impurities.
Self-propagating high-temperature synthesis technology (SHS) is a novel industrial technology that utilizes chemical reactions to continue reactions to synthesize new materials. To date, many new materials such as TiC, TiN, MoSi2、Si3N4AlN has been available for continuous, large-scale production using the SHS process. The SHS method has the advantages that: (1) the time is saved, and the energy is fully utilized; (2) the equipment and the process are simple; (3) the product purity is high (certain impurities are volatilized because the SHS can generate high temperature), and the reaction conversion rate is close to 100%; (4) high yield (because the reaction speed is fast).
Disclosure of the invention
The invention aims to provide a method for preparing β -sialon ceramic powder by using an SHS method, which has the characteristics of energy conservation, simple production process, high productivity, low cost and low harmful impurities.
The preparation method of β -sialon ceramic powder is characterized in that raw materials at least comprise 45-65% by weight of aluminum oxide material with the aluminum oxide content of more than 97%, 35-45% by weight of metal silicon material with the silicon content of more than 97% and 0-15% by weight of metal aluminum material with the aluminum content of more than 95%, then the fully mixed reaction materials are put into a reactor, 20-60MPa of nitrogen with the purity of more than 99.9% is filled, the reaction materials are ignited by metal wires for reaction, and after the reaction is finished, the reactants are ball-milled to obtain β -sialon ceramic powder, wherein the particle size of the powder is less than 0.045 mm.
The reaction of silicon and nitrogen in the reactant of the invention is exothermic reaction, the released heat is 723.8KJ/mol, the reaction of aluminum and nitrogen is also exothermic reaction, the released heat is 293.4KJ/m0l, the exothermic reaction generates high temperature, so that the alumina also participates in the reaction to form β -sialon, the main reaction is as follows:
in the formula, Si3Al3O3N5β -sialon with Z-3.
Compared with the synthetic method adopting coal dry stone, natural raw materials or industrial waste, the sialon material prepared by the method has harmful impurities such as K2O、Na2The contents of O, CaO and MgO are extremely low, and the high-temperature-resistant brick can be applied to harsh high-temperature conditions such as bricks for blast furnaces, sliding nozzle bricks, air bricks, iron runner castables, kiln furniture, high-temperature engines and the like. The sialon material prepared by the synthesis method of coal dry stone, natural raw materials or industrial waste has obvious reduction of high-temperature performance, and the oxidized product is a feldspar with low melting point, so that the application field is very limited.
Compared with the preparation method of mechanical pressing forming and high-temperature nitriding sintering, the raw materials of the invention do not need forming, high-temperature heating equipment and fuel, and the reaction raw materials are ignited by metal wires, and the reaction can be sufficiently maintained by the heat released by the self reaction. Therefore, the method has the characteristics of energy conservation, simple production process, high production efficiency, low cost and the like.
(IV) detailed description of the preferred embodiments
The formula of the reaction raw materials is as follows:
alumina with purity greater than 97%: 45 to 65 wt.% (weight percentage)
Metallic silicon material with purity more than 97%: 35 to 45 wt.% (weight percentage)
Metallic aluminum material with purity greater than 95%: 0-15% (weight percentage)
Table 1 lists the ingredients of the five formulation numbers of the reaction raw materials and the composition of the reactant phases (in weight percent);
TABLE 1
The reaction raw materials in the table 1 are fully mixed and then are filled into a reactor, 20-60MPa of nitrogen with the purity of more than 99.9 percent is filled, the reaction materials are ignited by metal wires for reaction, and after the reaction is finished, the reactants are ball-milled, so that the high-performance 3-sialon ceramic powder with the granularity of less than 0.045mm can be obtained.
Claims (1)
1. A preparation method of β -sialon ceramic powder is characterized in that raw materials at least comprise 45-65% by weight of aluminum oxide material with the aluminum oxide content more than 97%, 35-45% by weight of metal silicon material with the silicon content more than 97% and 0-15% by weight of metal aluminum material with the aluminum content more than 95%, the fully mixed reaction materials are put into a reactor, 20-60MPa of nitrogen with the purity more than 99.9% is filled, the reaction materials are ignited by metal wires for reaction, and after the reaction is finished, the reactants are ball-milled to obtain β -sialon ceramic powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100532828A CN1298676C (en) | 2004-07-29 | 2004-07-29 | Method for preparing beta-'Sailong' ceramic powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100532828A CN1298676C (en) | 2004-07-29 | 2004-07-29 | Method for preparing beta-'Sailong' ceramic powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1727308A true CN1727308A (en) | 2006-02-01 |
| CN1298676C CN1298676C (en) | 2007-02-07 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004100532828A Expired - Fee Related CN1298676C (en) | 2004-07-29 | 2004-07-29 | Method for preparing beta-'Sailong' ceramic powder |
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| Country | Link |
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| CN (1) | CN1298676C (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100389233C (en) * | 2006-05-22 | 2008-05-21 | 东北大学 | Beta'-Sialon whisker gas phase reaction preparation method |
| CN106634557A (en) * | 2016-12-08 | 2017-05-10 | 长兴天晟能源科技有限公司 | High-temperature-resisting and oxidation-resisting coating for SiAlON-AlN-TiN-based stainless steel |
| CN106892666A (en) * | 2017-03-17 | 2017-06-27 | 太原理工大学 | A kind of coal gangue combustion synthesizes the method for β SIALON based composite powders |
| CN109704782A (en) * | 2019-01-30 | 2019-05-03 | 中国科学院理化技术研究所 | A kind of Si for photovoltaic production of polysilicon2N2The preparation method of O ceramic powder |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1019939C (en) * | 1991-04-23 | 1993-03-03 | 内蒙古自治区农业科学院 | Seed-breeding technique of No.2 seeds <<Neikuiza>> for extracting sunflower oil |
| CN1102557C (en) * | 2000-04-21 | 2003-03-05 | 清华大学 | Process for preparing Sailong and silicon carbide combined ceramic powder from river sand |
| CN1152843C (en) * | 2002-04-05 | 2004-06-09 | 清华大学 | Prepn of beta-sialon silicon carbide complex phase powder with coal gangue |
-
2004
- 2004-07-29 CN CNB2004100532828A patent/CN1298676C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100389233C (en) * | 2006-05-22 | 2008-05-21 | 东北大学 | Beta'-Sialon whisker gas phase reaction preparation method |
| CN106634557A (en) * | 2016-12-08 | 2017-05-10 | 长兴天晟能源科技有限公司 | High-temperature-resisting and oxidation-resisting coating for SiAlON-AlN-TiN-based stainless steel |
| CN106892666A (en) * | 2017-03-17 | 2017-06-27 | 太原理工大学 | A kind of coal gangue combustion synthesizes the method for β SIALON based composite powders |
| CN109704782A (en) * | 2019-01-30 | 2019-05-03 | 中国科学院理化技术研究所 | A kind of Si for photovoltaic production of polysilicon2N2The preparation method of O ceramic powder |
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| Publication number | Publication date |
|---|---|
| CN1298676C (en) | 2007-02-07 |
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