CN1482095A - Method for preparing bauxite substrate MgAION - Google Patents
Method for preparing bauxite substrate MgAION Download PDFInfo
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- CN1482095A CN1482095A CNA031261485A CN03126148A CN1482095A CN 1482095 A CN1482095 A CN 1482095A CN A031261485 A CNA031261485 A CN A031261485A CN 03126148 A CN03126148 A CN 03126148A CN 1482095 A CN1482095 A CN 1482095A
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- mgalon
- preparation
- alumina base
- magnesium oxide
- described alumina
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Abstract
The present invention provides the preparation process of alumina-base MgAlON and features that high-aluminum alumina mixed with proper amount of metal aluminum powder and small amount of MgO is formed and fast nitrided, reduced and synthesized in a low temperature alumiothermic course to form alumina-base MgAlON with high nitrogen content and fine crystal size. The material of the present invention has high nitrogen content, fine crystal size, high mechanical performance and fireproof performance, excellent slag resistance and low cost, and may be used widely in high quality refractory material and ceramic product for metallurgy, chemical industry and ceramic industry.
Description
Affiliated field:
The present invention relates to the preparation method of a kind of pottery or used for refractory material raw material, be specifically related to a kind of by the preparation method of alumine through the synthetic MgAlON of aluminothermy reduction-nitridation.
Background technology:
MgAlON is a kind of novel stupalith, have excellent in chemical and mechanical property, thereby still in refractory materials, all be widely used at high-performance ceramics, particularly at fire resisting material field, the MgAlON composite refractory has good slag resistance, anti-molten steel performance of flushing, smelts the requirement of high quality ultra-clean steel thereby can satisfy, and can avoid the pollution that causes because of use, be expected to replace carbon containing refractory and be used to smelt Clean Steel; In addition, because the good resistance to fouling of MgAlON matrix material is expected to be widely used at nonferrous metallurgy and chemical industry.
Preparation MgAlON mainly adopts three kinds of processing methodes at present:
1, by AlN, Al
2O
3And MgO is synthetic.This method is a solid-solid reaction mechanism, synthesis temperature height and long reaction time, and the ultra-fine artificial-synthetic material of therefore many employings is easy to control, but the cost height, energy consumption is big.
2, by Al
2O
3And MgO (MgAl
2O
4) and C synthetic.The mechanism of the synthetic MgAlON of carbothermal reduction-nitridation method is reduction-nitrogenize-solid solution mechanism, though the price of raw material is lower than first method, the preparation process processing condition require high, and difficulty is bigger.
3, by Al, Al
2O
3And MgO preparation.This method is by the direct nitrogenize of metal and the synthetic MgAlON of solid solution reaction further takes place.The less employing of this method because technical difficulty is high.
More than three kinds of methods all to adopt aluminum oxide be the synthetic MgAlON of main raw material, cost is higher.In order to reduce cost, it is that main raw material is prepared the material that principal crystalline phase is MgAlON that the natural mineral raw alumine of the cheapness of adopting is also arranged, 99100292.X patent application as the Sun Jialin proposition, its preparation is to adopt carbon reduction nitrogenize synthesis technique, its feature mainly is that raw material is embedded in the carbonaceous material, in sintering process, finally form MgAlON by carbon reduction and with the nitrogen reaction, sintering temperature is 1550-1650 ℃, soaking time is 72-110h, and N content is 1.5-5.8% in institute's synthetic raw material.
Summary of the invention:
The object of the present invention is to provide that a kind of directly to utilize alumine to pass through the Al thermal reduction nitridation sintered, in lesser temps, the preparation method of the synthetic alumina base MgAlON that crystal grain is tiny, nitrogen content is high in the short period.
Technical scheme of the present invention is:
A. the metallic aluminium of 50-80% alumine, 20-40%, the magnesium oxide of 2-10% are mixed, add the wedding agent of raw material total amount 5-10%, continue to be mixed to evenly mechanical pressing or extrusion molding;
B. forming blocks material among a is put into nitriding furnace, carry out nitridation sinteredly under flowing nitrogen atmosphere, nitridation sintered temperature is 1400-1550 ℃, soaking time 4-12 hour;
When c. furnace temperature being reduced to 700 ℃-room temperature, stop logical nitrogen, promptly make alumina base MgAlON.
In above-mentioned preparation method, said alumine is raw material or light-burned material, and the mass percent of the main component after its calcination is: Al
2O
380-95%, SiO
25-10%, TiO
22-5%; Said metallic aluminium is as reductive agent, and wherein the content of Al is 95-99.9%; The content of MgO is 95-99% in the said magnesium oxide; Magnesium oxide can be used MgAl
2O
4Substitute, wherein MgO+Al
2O
3Content be 95-99%; Said wedding agent is one or more in lignosulfite, polyvinyl alcohol, dextrin, xylogen, carboxymethyl cellulose, the resin.
Compared with prior art, the invention has the advantages that:
1, the present invention is a raw material with the profuse alumine of Chinese reserves, not only can reduce the manufacturing cost of MgAlON widely, and can improve China's relative state that falls behind aspect alumine processing and use at present, improves the added value of raw material.
2, preparation technology of the present invention is simple, and sintering temperature is lower, the time is shorter, need not complicated processing unit and technological process.
3, synthetic product MgAlON crystal grain of the present invention is tiny, and less than 5 μ m, nitrogen content is higher, 〉=6wt%.
Description of drawings:
Accompanying drawing 1 is the XRD analysis figure of the embodiment of the invention 1 products therefrom, has reflected the thing phase composite of product 1.
Accompanying drawing 2 is the XRD analysis figure of the embodiment of the invention 2 products therefroms, has reflected the thing phase composite of product 2.
The invention will be further described below in conjunction with accompanying drawing.
Embodiment:
Embodiment 1
Alumine (composition such as table 1), metallic aluminium, magnesium oxide with Dengfeng City, Henan Province are main raw material.
| ??Component | Al 2O 3 | ?SiO 2 | ?TiO 2 | ?Fe 2O 3 | ?CaO | ?MgO | ?K 2O | ?Na 2O |
| Wt% after the calcination | 87.76 | ?6.72 | ?4.45 | ?0.4 | ?0.11 | ?0.44 | ?0.05 | ?0.07 |
With giving birth to vanadine, metallic aluminium, magnesium oxide respectively by after 65%, 30%, 5% the weight ratio batching, put into ball grinder, dried be mixed even; The taking-up mixed powder is a binding agent with 8% polyvinyl alcohol, and the 70MPa mechanical pressing is dry under 80 ℃ of temperature; Put into atmosphere sintering furnace then, carry out nitridation sinteredly in flowing nitrogen atmosphere, sintering temperature is 1550 ℃, keeps temperature 8 hours; Be cooled to 700 ℃ and close nitrogen, continue to be cooled to room temperature and take out, obtain MgAlON piece material, after broken and fine grinding, can make MgAlON particulate material and powder.
The XRD analysis figure of product as shown in Figure 1 in the present embodiment.Through XRD analysis, the product principal crystalline phase is MgAlON.After testing, nitrogen content 6.01wt%, crystal size is less than 2 μ m.
Embodiment 2
Alumine (composition such as table 1), metallic aluminium, magnesium oxide with Dengfeng City, Henan Province are main raw material.
| Component | Al 2O 3 | ?SiO 2 | ?TiO 2 | Fe 2O 3 | ?CaO | ?MgO | ?K 2O | ?Na 2O |
| Wt% after the calcination | 87.76 | ?6.72 | ?4.45 | ?0.4 | ?0.11 | ?0.44 | ?0.05 | ?0.07 |
To give birth to vanadine, metallic aluminium (as reductive agent), MgAl
2O
4By after 62: 24: 14 the weight ratio batching, put into ball grinder respectively, dried be mixed even; The taking-up mixed powder is a binding agent with 8% polyvinyl alcohol, and the 70MPa mechanical pressing is dry under 80 ℃ of temperature; Put into atmosphere sintering furnace then, carry out nitridation sinteredly in flowing nitrogen atmosphere, sintering temperature is 1550 ℃, keeps temperature 8 hours; Be cooled to 700 ℃ and close nitrogen, continue to be cooled to room temperature and take out, obtain MgAlON piece material, after the broken fine grinding, can make MgAlON particulate material and powder.
The XRD analysis figure of product as shown in Figure 2 in the present embodiment.Through XRD analysis, the product principal crystalline phase is MgAlON.After testing, nitrogen content 9.00wt%, crystal size is less than 2 μ m.
Claims (6)
1, the preparation method of alumina base MgAlON is characterized in that:
A. the metallic aluminium of 50-80% alumine, 20-40%, the magnesium oxide of 2-10% are mixed, add the wedding agent of raw material total amount 5-10%, continue to be mixed to evenly mechanical pressing or extrusion molding;
B. forming blocks material among a is put into nitriding furnace, carry out nitridation sinteredly under flowing nitrogen atmosphere, nitridation sintered temperature is 1400-1550 ℃, soaking time 4-12 hour;
When c. furnace temperature being reduced to 700 ℃-room temperature, stop logical nitrogen, promptly make alumina base MgAlON.
2, according to the preparation method of the described alumina base of claim 1 MgAlON, it is characterized in that: alumine is raw material or light-burned material, and the mass percent of the main component after its calcination is: Al
2O
380-95%, SiO
25-10%, TiO
22-5%.
3, according to the preparation method of the described alumina base of claim 1 MgAlON, it is characterized in that: the content of Al is 95-99.9% in the metallic aluminium.
4, according to the preparation method of the described alumina base of claim 1 MgAlON, it is characterized in that: the content of MgO is 95-99% in the magnesium oxide.
5, according to the preparation method of claim 1 and 3 described alumina base MgAlON, it is characterized in that: magnesium oxide can be used MgAl
2O
4Substitute, wherein MgO+Al
2O
3Content be 95%-99%.
6, according to the preparation method of the described alumina base of claim 1 MgAlON, it is characterized in that: said wedding agent is one or more in lignosulfite, polyvinyl alcohol, dextrin, xylogen, carboxymethyl cellulose, the resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03126148 CN1241866C (en) | 2003-05-09 | 2003-05-09 | Method for preparing bauxite substrate MgAION |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03126148 CN1241866C (en) | 2003-05-09 | 2003-05-09 | Method for preparing bauxite substrate MgAION |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1482095A true CN1482095A (en) | 2004-03-17 |
| CN1241866C CN1241866C (en) | 2006-02-15 |
Family
ID=34153047
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03126148 Expired - Fee Related CN1241866C (en) | 2003-05-09 | 2003-05-09 | Method for preparing bauxite substrate MgAION |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100413804C (en) * | 2005-06-14 | 2008-08-27 | 郑州大学 | Sheet-like microcrystalline toughened MgAlON composite corindon material preparation method |
| CN100453451C (en) * | 2006-02-16 | 2009-01-21 | 郑州大学 | MgAlON powder preparation method and its product |
| CN103833391A (en) * | 2014-01-06 | 2014-06-04 | 宜兴市钰玺窑业有限公司 | Silicon nitride-silicon carbide composite brick and preparation method thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102020006167A1 (en) | 2020-10-07 | 2022-04-07 | Technische Universität Bergakademie Freiberg, Körperschaft des öffentlichen Rechts | Coatings and ceramic filters for molten metal filtration |
-
2003
- 2003-05-09 CN CN 03126148 patent/CN1241866C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100413804C (en) * | 2005-06-14 | 2008-08-27 | 郑州大学 | Sheet-like microcrystalline toughened MgAlON composite corindon material preparation method |
| CN100453451C (en) * | 2006-02-16 | 2009-01-21 | 郑州大学 | MgAlON powder preparation method and its product |
| CN103833391A (en) * | 2014-01-06 | 2014-06-04 | 宜兴市钰玺窑业有限公司 | Silicon nitride-silicon carbide composite brick and preparation method thereof |
| CN103833391B (en) * | 2014-01-06 | 2016-03-02 | 宜兴市钰玺窑业有限公司 | A kind of silicon nitride complex phase silicon carbide brick and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN1241866C (en) | 2006-02-15 |
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