CN102503472A - SiC (silicon carbide)-toughened corundum prefabricated part by means of in-situ formation and preparation method for same - Google Patents
SiC (silicon carbide)-toughened corundum prefabricated part by means of in-situ formation and preparation method for same Download PDFInfo
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- CN102503472A CN102503472A CN2011103296140A CN201110329614A CN102503472A CN 102503472 A CN102503472 A CN 102503472A CN 2011103296140 A CN2011103296140 A CN 2011103296140A CN 201110329614 A CN201110329614 A CN 201110329614A CN 102503472 A CN102503472 A CN 102503472A
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Abstract
The invention discloses an SiC (silicon carbide)-toughened corundum prefabricated part by means of in-situ formation and a preparation method for the same. The method includes the steps of utilizing corundum, simple substance silicon, aluminum oxide micro powder and a bonding agent as basic raw materials, adding a dispersing agent, uniformly and drily mixing the raw materials with the dispersing agent by a stirrer, uniformly stirring the uniformly mixed materials with water and injecting the stirred liquor into a die to form a prefabricated part; carrying out stripping and natural curing prior to baking the prefabricated part in a heating-up furnace; and finally, placing the baked prefabricated part into a high-temperature kiln for firing in a buried carbon reducing atmosphere and at the high temperature ranging from 1450 DEG C to 1550 DEG C, and cooling the fired prefabricated part to the room temperature so that the prefabricated part is prepared. Compared with a traditional corundum prefabricated part, the corundum prefabricated part has the advantages that heat-state breaking strength is remarkably improved, and heat shock stability is also improved to some extent.
Description
Technical field
The present invention relates to a kind of refractory materials, particularly relate to a kind of through toughness reinforcing corundum matter prefab of original position generation SiC and preparation method thereof.
Background technology
At present, refractory materials is main with oxide material and carbon composite mainly on material.Be that the main common fragility of refractory materials is bigger with the oxide compound, be difficult to satisfy simultaneously the requirement of HS and good thermal shock resistance; The carbon composite refractory is in oxide-based refractory materials, to introduce carbonaceous component such as graphite, improves the brittle purpose of oxide-based refractory materials thereby reach.But shortcoming such as this type of material exists that oxidation-resistance is poor, thermal conductivity is too high and use range is limited.On this basis, in oxide system, introduce SiC, Si
3N
4, non-oxidized substance phase such as Sialon way become a new research focus of fire resisting material field.
Numerous researchs show that oxide compound-non-oxidized substance matrix material has higher high temperature strength and antioxidant property, and good heat-shock resistance, erosion-resisting characteristics are expected to become the high-quality high-performance refractory material of new generation that the hot industry key position uses.
Corundum matter prefab adopts the prefabricated shaping of mould material method usually.Common corundum matter prefab hot strength is not high, fragility is bigger, influences its result of use.Therefore, exploration can better the corundum preform product, and quality product is realized controlled, is a kind of approach of effective assurance user stably manufactured, also is the present urgent problem of refractories industry.
Three, summary of the invention:
The technical problem that the present invention will solve: provide a kind of and generate toughness reinforcing corundum matter prefab of SiC and preparation method thereof through original position, the hot modulus of rupture of this corundum matter prefab and high volume stability all are superior to common corundum matter prefab.
In order to address the above problem, the technical scheme that the present invention adopts is:
It is a kind of that raw material is formed and is represented with weight percentage through the toughness reinforcing corundum matter prefab of original position generation SiC, corundum 80～90%, and elemental silicon 1～10%, alumina powder 1 ~ 8%, wedding agent 5～10% adds the dispersion agent that accounts for above-mentioned raw materials gross weight 0.1 ~ 0.5%; Said wedding agent is the mixture of hydrated aluminum oxide and aluminous cement, and both weight ratios are 1:0.5～4.
Al in the said corundum
2O
3Content>=95%, said corundum are brown corundum, white fused alumina or alundum; Comprise the corundum 15～25% of 5mm＜granularity≤8mm, the corundum 10～20% of 3mm＜granularity≤5mm, the corundum 10～20% of 1mm＜granularity≤3mm, corundum 15～25%, 180 order corundum 5～15% and the 320 order corundum 1～10% of 0.1mm＜granularity≤1mm in said 80～90% the corundum.
Si content >=98% in the said elemental silicon; Said elemental silicon is any in granularity 150 orders and the 200 order elemental silicons, or two kinds mixture; Ratio during two kinds of mixing of said 150 orders and 200 order elemental silicons is 1:0.5～3.
Al in the said alumina powder
2O
3Content>=98%; The meso-position radius D50 of said alumina powder is 1 ~ 6 μ m.
Said dispersion agent is mineral-type dispersion agent or organic type of dispersion agent.
Said mineral-type dispersion agent is tripoly phosphate sodium STPP or Sodium hexametaphosphate 99, or is carbonate, phosphoric acid salt or the oxyhydroxide of calcium, magnesium, barium.
Said organic type of dispersion agent is fatty acid, aliphatic amide type or ester class dispersion agent.
The preparation method of said corundum matter prefab may further comprise the steps:
A, form according to raw material and to take by weighing raw material, adopt that stirrer is dried to be mixed evenly, obtain doing and mix material;
B, in do mixing material, add the water that accounts for siccative gross weight 5 ± 2%, stir, inject mould then, on shaking table or by vibrating head vibratory compaction, obtain prefab after the moulding;
C, with prefab in mould in 25 ℃ of following maintenances of room temperature 1 day, the demoulding again in 25 ℃ of following natural curings of room temperature 1 day, is put into roasting kiln with prefab then and is toasted, 100～150 ℃ of storing temperatures, storing time 24～72 hours after the demoulding;
D, the prefab after will toasting are put into saggar; Prefab top cladding thickness is higher than the coke layer of the coke granule formation of 150mm, then saggar integral body is put into the high temperature shuttle kiln, burns till at 1450～1550 ℃ of following high temperature; Under top temperature, be incubated 24～60 hours; Stop kiln afterwards, be cooled to room temperature, promptly obtain to generate the toughness reinforcing corundum matter preform product of SiC through original position.
Said coke granule is less than 2mm.
Positive beneficial effect of the present invention:
1, product of the present invention is introduced elemental silicon on the basis of original corundum matter prefab, and burns till burying under the charcoal reducing atmosphere, and reaction in can take place the Si in the introducing system, generates the SiC wild phase.Because there is mass transferring in gas phase mechanism in this reaction, the original position SiC wild phase that is generated is fibrous more, and in goods matrix and pore, can tend to disperse distribution, good uniformity.This original position SiC wild phase can significantly improve the hot modulus of rupture of corundum matter prefab.
2, to have solved common corundum matter prefab hot strength not high for product of the present invention, and the knotty problem of stress rupture takes place in the use easily.Product of the present invention has preferable performance, and especially hot modulus of rupture is higher.See table 1 for details.
[0018Table 1 performance of products of the present invention detects data
Embodiment
Following examples have been merely and have further specified the present invention, do not limit content of the present invention.
Embodiment 1:A kind of through toughness reinforcing corundum matter prefab of original position generation SiC and preparation method thereof
A, raw material are formed: represent white fused alumina 87%, elemental silicon 3%, wedding agent 4%, alumina powder 6% with weight percent; Add the mineral-type pentasodium triphosphate of dispersing agent or the Sodium hexametaphosphate 99 that account for above-mentioned raw materials gross weight 0.3%.
Al in the said white fused alumina
2O
3Content>=98%; 87% white fused alumina comprises the white fused alumina 20% of 5mm＜granularity≤8mm, the white fused alumina 12% of 3mm＜granularity≤5mm, the white fused alumina 16% of 1mm＜granularity≤3mm, white fused alumina 18%, 180 order white fused aluminas 12% and the 320 order white fused aluminas 9% of 0.1mm＜granularity≤1mm; Si content>=98% in the elemental silicon, granularity are 150 orders;
B, take by weighing various raw materials, be mixed evenly, obtain doing and mix material with stirrer is dried;
C, in do mixing material, add the water that accounts for siccative gross weight 5 ± 2%, stir, inject mould then, on shaking table or by vibrating head vibratory compaction, obtain prefab after the moulding;
D, with the prefab that obtains in mould in 25 ℃ of following maintenances of room temperature 1 day, the demoulding then again in 25 ℃ of following natural curings of room temperature 1 day, is put into roasting kiln with the prefab after the natural curing and is toasted after the demoulding, storing temperature is 110 ℃, storing time is 24 hours;
E, the prefab after will baking are put into saggar, and the prefab top is coated with thickness and is higher than the coke layer that the coke granule of 150mm forms, and the granularity of coke granule is less than 2mm; Afterwards saggar integral body is put into the high temperature shuttle kiln, burn till at 1550 ℃ of following high temperature, insulation is 30 hours under this temperature; Stop kiln; Be cooled to room temperature, kiln discharge is rechecked and vanning, promptly obtains to generate the toughness reinforcing corundum matter preform product of SiC through original position.
Embodiment 2: basic identical with embodiment 1, difference is:
Step a: raw material white fused alumina 81%, elemental silicon 9%, wedding agent 4% and alumina powder 6% add the mineral-type dispersion agent lime carbonate or the trimagnesium phosphate that account for above-mentioned raw materials gross weight 0.4%;
Al in the white fused alumina
2O
3Content>=98%; 81% white fused alumina comprises: the white fused alumina 13% of the white fused alumina 18% of 5mm＜granularity≤8mm, the white fused alumina 17% of 3mm＜granularity≤5mm, 1mm＜granularity≤3mm, the white fused alumina of 0.1mm＜granularity≤1mm 20%, 180 order white fused aluminas 8% and 320 order white fused aluminas 5%; Si content>=98% in the said elemental silicon, granularity are 200 orders;
Steps d: the prefab after the natural curing is put into roasting kiln toast, storing temperature is 100 ℃, and storing time is 36 hours;
Step e: the prefab after will baking is put into saggar, and the prefab top is coated with the coke layer that thickness is higher than the coke granule formation of 150mm, and the granularity of coke granule is less than 2mm; Afterwards saggar integral body is put into the high temperature shuttle kiln, burn till at 1450 ℃ of following high temperature, insulation is 36 hours under this temperature; Stop kiln; Be cooled to room temperature, kiln discharge is rechecked and vanning, promptly obtains to generate the toughness reinforcing corundum matter preform product of SiC through original position.
Embodiment 3: basic identical with embodiment 1, difference is:
Step a: raw material palm fibre corundum 90%, elemental silicon 4%, wedding agent 3% and alumina powder 3% add the organic type of dispersion agent that accounts for above-mentioned raw materials gross weight 0.3%; Said organic type of dispersion agent is the fatty acid dispersion agent.
Al in the said brown corundum
2O
3Content>=95%; 90% brown corundum comprises: the brown corundum 20% of the brown corundum 25% of 5mm＜granularity≤8mm, the brown corundum 20% of 3mm＜granularity≤5mm, 1mm＜granularity≤3mm, the brown corundum 15% of 0.1mm＜granularity≤1mm, 180 orders palm fibre corundum 5% and 320 orders palm fibre corundum 5%;
Si content >=98% in the said elemental silicon, granularity are the mixture of 150 orders and 200 order elemental silicons, and the blending ratio of the two is 1:1;
Steps d: the prefab after the natural curing is put into roasting kiln toast, storing temperature is 120 ℃, and storing time is 24 hours;
Step e: the prefab after will baking is put into saggar, and the prefab top is coated with the coke layer that thickness is higher than the coke granule formation of 150mm, and the granularity of coke granule is less than 2mm; Afterwards saggar integral body is put into the high temperature shuttle kiln, burn till at 1500 ℃ of following high temperature, insulation is 40 hours under this temperature; Stop kiln; Be cooled to room temperature, kiln discharge is rechecked and vanning, promptly obtains to generate the toughness reinforcing corundum matter preform product of SiC through original position.
Embodiment 4: basic identical with embodiment 1, difference is:
Step a: alundum 80% in the raw material, elemental silicon 10%, and wedding agent 6% and alumina powder 4% add the organic type of dispersion agent that accounts for above-mentioned raw materials gross weight 0.2%; Said organic type of dispersion agent is aliphatic amide type or ester class dispersion agent.
Al in the said alundum
2O
3Content>=99%; 80% alundum comprises: the alundum 10% of the alundum 15% of 5mm＜granularity≤8mm, the alundum 15% of 3mm＜granularity≤5mm, 1mm＜granularity≤3mm, the alundum of 0.1mm＜granularity≤1mm 25%, 180 order alundums 5% and 320 order alundums 10%;
Si content >=98% in the said elemental silicon, granularity are the mixture of 150 orders and 200 order elemental silicons, and the blending ratio of the two is 1:3;
Steps d: the prefab after the natural curing is put into roasting kiln toast, storing temperature is 100 ℃, and storing time is 36 hours;
Step e: the prefab after will baking is put into saggar, and the prefab top is coated with the coke layer that thickness is higher than the coke granule formation of 150mm, and the granularity of coke granule is less than 2mm; Afterwards saggar integral body is put into the high temperature shuttle kiln, burn till at 1480 ℃ of following high temperature, insulation is 36 hours under this temperature; Stop kiln; Be cooled to room temperature, kiln discharge is rechecked and vanning, promptly obtains to generate the toughness reinforcing corundum matter preform product of SiC through original position.
Claims (9)
1. one kind is passed through the toughness reinforcing corundum matter prefab of original position generation SiC; It is characterized in that said corundum matter prefab raw material consists of: represent corundum 80～90% with weight percentage; Elemental silicon 1～10%; Alumina powder 1 ~ 8%, wedding agent 5～10% adds the dispersion agent that accounts for above-mentioned raw materials gross weight 0.1 ~ 0.5%; Said wedding agent is the mixture of hydrated aluminum oxide and aluminous cement, and both weight ratios are 1:0.5～4.
2. corundum matter prefab according to claim 1 is characterized in that: Al in the said corundum
2O
3Content>=95%, said corundum are brown corundum, white fused alumina or alundum; Comprise the corundum 15～25% of 5mm＜granularity≤8mm, the corundum 10～20% of 3mm＜granularity≤5mm, the corundum 10～20% of 1mm＜granularity≤3mm, corundum 15～25%, 180 order corundum 5～15% and the 320 order corundum 1～10% of 0.1mm＜granularity≤1mm in said 80～90% the corundum.
3. corundum matter prefab according to claim 1 is characterized in that: Si content >=98% in the said elemental silicon; Said elemental silicon is any in granularity 150 orders and the 200 order elemental silicons, or two kinds mixture; Ratio during two kinds of mixing of said 150 orders and 200 order elemental silicons is 1:0.5～3.
4. corundum matter prefab according to claim 1 is characterized in that: Al in the said alumina powder
2O
3Content>=98%; The meso-position radius D50 of said alumina powder is 1 ~ 6 μ m.
5. corundum matter prefab according to claim 1 is characterized in that: said dispersion agent is mineral-type dispersion agent or organic type of dispersion agent.
6. corundum matter prefab according to claim 5 is characterized in that: said mineral-type dispersion agent is tripoly phosphate sodium STPP or Sodium hexametaphosphate 99, or is carbonate, phosphoric acid salt or the oxyhydroxide of calcium, magnesium, barium.
7. corundum matter prefab according to claim 5 is characterized in that: said organic type of dispersion agent is fatty acid, aliphatic amide type or ester class dispersion agent.
8. the preparation method of each said corundum matter prefab of claim 1-7 is characterized in that said preparation method may further comprise the steps:
A, form according to raw material and to take by weighing raw material, adopt that stirrer is dried to be mixed evenly, obtain doing and mix material;
B, in do mixing material, add the water that accounts for siccative gross weight 5 ± 2%, stir, inject mould then, on shaking table or by vibrating head vibratory compaction, obtain prefab after the moulding;
C, with prefab in mould in 25 ℃ of following maintenances of room temperature 1 day, the demoulding again in 25 ℃ of following natural curings of room temperature 1 day, is put into roasting kiln with prefab then and is toasted, 100～150 ℃ of storing temperatures, storing time 24～72 hours after the demoulding;
D, the prefab after will toasting are put into saggar; Prefab top cladding thickness is higher than the coke layer of the coke granule formation of 150mm, then saggar integral body is put into the high temperature shuttle kiln, burns till at 1450～1550 ℃ of following high temperature; Under top temperature, be incubated 24～60 hours; Stop kiln afterwards, be cooled to room temperature, promptly obtain to generate the toughness reinforcing corundum matter preform product of SiC through original position.
9. preparation method according to claim 8 is characterized in that: said coke granule is less than 2mm.
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| CN 201110329614 CN102503472B (en) | 2011-10-26 | 2011-10-26 | SiC (silicon carbide)-toughened corundum prefabricated part by means of in-situ formation and preparation method for same |
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| CN 201110329614 CN102503472B (en) | 2011-10-26 | 2011-10-26 | SiC (silicon carbide)-toughened corundum prefabricated part by means of in-situ formation and preparation method for same |
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Cited By (4)
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| CN102701769A (en) * | 2012-07-06 | 2012-10-03 | 山国强 | In-situ SiC toughened flint clay prefabricated part |
| CN103033057A (en) * | 2012-09-24 | 2013-04-10 | 瑞泰科技股份有限公司 | Combustor refractory lining prefabricated building block for cement kiln, production method and application of combustor refractory lining prefabricated building block |
| CN108276017A (en) * | 2018-01-31 | 2018-07-13 | 景德镇陶瓷大学 | It is a kind of to utilize corundum-silicon carbide whisker composite ceramic material and preparation method thereof that natural minerals are raw material |
| CN109516831A (en) * | 2018-12-03 | 2019-03-26 | 浙江昕明环境科技有限公司 | A kind of preparation method of aluminum oxide porous material |
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| CN101445379A (en) * | 2008-12-19 | 2009-06-03 | 周建国 | Dedicated pouring material for cement kiln outlet and jetting coal pipe and preparation method thereof |
| CN102173651A (en) * | 2011-01-27 | 2011-09-07 | 王立珍 | Multifunctional wear-resistant material |
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| CN1683283A (en) * | 2004-04-15 | 2005-10-19 | 宜兴市泰科耐火材料有限公司 | Silicon carbide corundum pouring material |
| CN101024556A (en) * | 2006-10-12 | 2007-08-29 | 洛阳鹏飞耐火材料有限公司 | Metal ceramic wear-resisting composite material and preparing method |
| CN101445379A (en) * | 2008-12-19 | 2009-06-03 | 周建国 | Dedicated pouring material for cement kiln outlet and jetting coal pipe and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102701769A (en) * | 2012-07-06 | 2012-10-03 | 山国强 | In-situ SiC toughened flint clay prefabricated part |
| CN103033057A (en) * | 2012-09-24 | 2013-04-10 | 瑞泰科技股份有限公司 | Combustor refractory lining prefabricated building block for cement kiln, production method and application of combustor refractory lining prefabricated building block |
| CN103033057B (en) * | 2012-09-24 | 2016-01-20 | 瑞泰科技股份有限公司 | A kind of burner refractory lining body for cement kiln is prefabricated builds block and production method and application thereof |
| CN108276017A (en) * | 2018-01-31 | 2018-07-13 | 景德镇陶瓷大学 | It is a kind of to utilize corundum-silicon carbide whisker composite ceramic material and preparation method thereof that natural minerals are raw material |
| CN109516831A (en) * | 2018-12-03 | 2019-03-26 | 浙江昕明环境科技有限公司 | A kind of preparation method of aluminum oxide porous material |
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