CN109503171A - A kind of silicon nitride combined silicon carbide brick and preparation method thereof - Google Patents
A kind of silicon nitride combined silicon carbide brick and preparation method thereof Download PDFInfo
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- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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Abstract
The invention discloses a kind of silicon nitride combined silicon carbide brick, the component including following parts by weight: 70 ~ 80 parts of silicon carbide, 15 ~ 20 parts of carbide fine powder, 2 ~ 8 parts of metallic silicon, 1 ~ 5 part of Suzhou soil, 1 ~ 3 part of calcium lignosulfonate.Meanwhile the invention also discloses the preparation methods of above-mentioned silicon nitride combined silicon carbide brick.Inventive formulation design science, each component cooperation rationally, merging for each heating time section silicon carbide and other raw materials are improved by the way that the silicon carbide of different shape is added.
Description
Technical field
The invention belongs to fire resisting material fields, and in particular to a kind of silicon nitride combined silicon carbide brick and preparation method thereof.
Background technique
Currently, the aluminium smelter enterprise of China's electrolytic aluminium is completed production capacity and surpasses 45,000,000 tons, has run production capacity up to surpassing 38,000,000
Ton.For the electrolysis temperature of large-scale aluminium electrolysis pre-baking tank between 950~970 DEG C, every 1 ton of aluminium of production consumes about 50kg ice crystal, fluorine
Change the electrolyte such as aluminium, magnesium fluoride, due to heat effect, chemical action, mechanical erosion effect, the infiltration of electro ultrafiltration, sodium and electrolyte
The reaction of fused salt caused by effect etc. chemically reacts, and the cathode carbon pieces in aluminium cell use after a certain period of time can be damaged, general to transport
4~7 Nian Houxu of row carries out large repairs, and the solids such as mainly waste cathode carbon block, waste refractory materials, useless thermal insulation material for removing are useless
Gurry, it is generally the case that 10,000 tons of electrolytic aluminiums of every production will generate about 100 tons of useless carbon materials (predominantly waste cathode carbon), about 80
Ton waste refractory materials and a certain number of thermal insulation materials.Wherein, refractory material is main in addition to part alumina firebrick, fire clay
The refractory material wanted is exactly silicon nitride-silicon carbide composite fireproof brick.
Silicon nitride combined silicon carbide brick refers to that with SiC and Si be raw material, the refractory product of via nitride firing.The product is 20
The later period sixties in century first appears, its main feature is that with Si3N4For bonding agent.Si3N4It is present in needle-shaped or fibrous crystal
It is a kind of important novel refractory between SiC crystal grain.General silicon carbide-containing 70%~75%, silicon nitride 18%~25%.Have
Good resistance to corrosion, 1400 DEG C of flexural strengths are up to 50~55MPa, apparent porosity 15%, and thermal expansion coefficient (4.5~5.0) ×
10-2℃.There are more disadvantages for silicon nitride combined silicon carbide brick at present, and the cost of silicon nitride first is very high, and a large amount of uses will improve
Production cost needs to be added additive in addition, most importantly the conjugation of silicon nitride and silicon carbide is not high to make the two more
It is combined together well, traditional bonding agent is unable to satisfy high heat-proof requirement.
Summary of the invention
Goal of the invention: in view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of silicon nitride combined silicon carbide
Brick.
Another object of the present invention is to provide the preparation methods of above-mentioned silicon nitride combined silicon carbide brick.
Technical solution: in order to achieve the above object of the invention, what the present invention was specifically performed by: a kind of silicon nitride bonded silicon
Silicon carbide brick, the component including following parts by weight: 70 ~ 80 parts of silicon carbide, 15 ~ 20 parts of carbide fine powder, 2 ~ 8 parts of gold
Belong to silicon, 1 ~ 5 part of Suzhou soil, 1 ~ 3 part of calcium lignosulfonate.
Wherein, the carbide fine powder fineness is not more than 100 μm.
The method for preparing silicon nitride combined silicon carbide brick, comprising: measure each raw material by formula, by silicon carbide, silicon carbide is thin
Powder, it is spare that metallic silicon forms mixed powder after mixing；By Suzhou soil, calcium lignosulfonate is mixed, and the water of gross mass 3wt% is added,
Mixing, then mixing is added in the mixed powder of mixing, press-molding is vibrated, 350 DEG C sufficiently dry, and pressurize and burn under nitrogen atmosphere
At.
Wherein, pressurization firing includes that the semi-finished product after drying are imported kiln to heat up under the nitrogen atmosphere, is controlled
Heating-up time 14 ~ 18 hours, temperature rose to 600 DEG C；Continue to heat up and vacuumize, controls the time 1 ~ 2 hour, temperature rises to 700
℃；Continue to heat up and rush nitrogen control kiln inner pressure not less than 1.5 atmospheric pressure, controls the time 8 ~ 10 hours, temperature rises to
1000℃；Continue to heat up, control the time 8 ~ 10 hours, temperature rises to 1350 DEG C；It is carried out 2 ~ 4 hours when temperature reaches 1350 DEG C
Heat preservation.
The utility model has the advantages that the present invention compared with traditional technology, has the advantage that
(1) inventive formulation design science, each component cooperation are rationally, each to improve by the silicon carbide that different shape is added
Heating time section silicon carbide is merged with other raw materials；
(2) in preparation process of the present invention key point be nitrogen addition, in system be added nitrogen after, over time greatly
Grained silicon carbide takes the lead in fusing with unclassified stores, and the silicon carbide of small fineness is not fused with unclassified stores as free ingredient,
After temperature is warming up to 1350 DEG C, small fineness silicon carbide enters molten condition, participates in the thawing mixing of other compositions, forms high cause
The brick body of density.
Specific embodiment
Embodiment 1:
70 parts of silicon carbide, 18 parts of carbide fine powder, 5 parts of metallic silicon, 3 parts of Suzhou soil, 1 part of wood are taken in parts by weight
Quality sulfoacid calcium, by silicon carbide, carbide fine powder, it is spare that metallic silicon forms mixed powder after mixing；By Suzhou soil, sulfomethylated lignin
Sour calcium mixing, is added the water of gross mass 3wt%, mixes, then the mixed powder of mixing is added and is mixed, vibration press-molding, and 350
DEG C sufficiently drying, by after drying semi-finished product import kiln heat up, control the heating-up time 14 ~ 18 hours, temperature rises to 600
℃；Continue to heat up and vacuumize, controls the time 1 ~ 2 hour, temperature rises to 700 DEG C；Continue to heat up and rush nitrogen control kiln internal pressure
Power is not less than 1.5 atmospheric pressure, controls the time 8 ~ 10 hours, temperature rises to 1000 DEG C；Continue to heat up, the control time 8 ~ 10 is small
When, temperature rises to 1350 DEG C；Heat preservation in 2 ~ 4 hours is carried out when temperature reaches 1350 DEG C.
Embodiment 2:
Take 80 parts of silicon carbide in parts by weight, 17 parts of carbide fine powder, 2 parts of metallic silicon, 4 parts of Suzhou soil, 3 parts
Calcium lignosulfonate, by silicon carbide, carbide fine powder, it is spare that metallic silicon forms mixed powder after mixing；By Suzhou soil, lignin
Sulfoacid calcium mixes, and the water of gross mass 3wt% is added, and mixes, then mixing is added in the mixed powder of mixing, vibrates press-molding,
Semi-finished product after drying are imported kiln and heated up, controlled the heating-up time 14 ~ 18 hours, temperature rises to by 350 DEG C of sufficiently drying
600℃；Continue to heat up and vacuumize, controls the time 1 ~ 2 hour, temperature rises to 700 DEG C；Continue to heat up and rush in nitrogen control kiln
Pressure is not less than 1.5 atmospheric pressure, controls the time 8 ~ 10 hours, temperature rises to 1000 DEG C；Continue to heat up, the control time 8 ~ 10 is small
When, temperature rises to 1350 DEG C；Heat preservation in 2 ~ 4 hours is carried out when temperature reaches 1350 DEG C.
Embodiment 3:
Take 72 parts of silicon carbide in parts by weight, 15 parts of carbide fine powder, 8 parts of metallic silicon, 2 parts of Suzhou soil, 2 parts
Calcium lignosulfonate, by silicon carbide, carbide fine powder, it is spare that metallic silicon forms mixed powder after mixing；By Suzhou soil, lignin
Sulfoacid calcium mixes, and the water of gross mass 3wt% is added, and mixes, then mixing is added in the mixed powder of mixing, vibrates press-molding,
Semi-finished product after drying are imported kiln and heated up, controlled the heating-up time 14 ~ 18 hours, temperature rises to by 350 DEG C of sufficiently drying
600℃；Continue to heat up and vacuumize, controls the time 1 ~ 2 hour, temperature rises to 700 DEG C；Continue to heat up and rush in nitrogen control kiln
Pressure is not less than 1.5 atmospheric pressure, controls the time 8 ~ 10 hours, temperature rises to 1000 DEG C；Continue to heat up, the control time 8 ~ 10 is small
When, temperature rises to 1350 DEG C；Heat preservation in 2 ~ 4 hours is carried out when temperature reaches 1350 DEG C.
Embodiment 4:
Take 74 parts of silicon carbide in parts by weight, 16 parts of carbide fine powder, 3 parts of metallic silicon, 5 parts of Suzhou soil, 3 parts
Calcium lignosulfonate, by silicon carbide, carbide fine powder, it is spare that metallic silicon forms mixed powder after mixing；By Suzhou soil, lignin
Sulfoacid calcium mixes, and the water of gross mass 3wt% is added, and mixes, then mixing is added in the mixed powder of mixing, vibrates press-molding,
Semi-finished product after drying are imported kiln and heated up, controlled the heating-up time 14 ~ 18 hours, temperature rises to by 350 DEG C of sufficiently drying
600℃；Continue to heat up and vacuumize, controls the time 1 ~ 2 hour, temperature rises to 700 DEG C；Continue to heat up and rush in nitrogen control kiln
Pressure is not less than 1.5 atmospheric pressure, controls the time 8 ~ 10 hours, temperature rises to 1000 DEG C；Continue to heat up, the control time 8 ~ 10 is small
When, temperature rises to 1350 DEG C；Heat preservation in 2 ~ 4 hours is carried out when temperature reaches 1350 DEG C.
Embodiment 5:
76 parts of silicon carbide, 20 parts of carbide fine powder, 4 parts of metallic silicon, 1 part of Suzhou soil, 1 part of wood are taken in parts by weight
Quality sulfoacid calcium, by silicon carbide, carbide fine powder, it is spare that metallic silicon forms mixed powder after mixing；By Suzhou soil, sulfomethylated lignin
Sour calcium mixing, is added the water of gross mass 3wt%, mixes, then the mixed powder of mixing is added and is mixed, vibration press-molding, and 350
DEG C sufficiently drying, by after drying semi-finished product import kiln heat up, control the heating-up time 14 ~ 18 hours, temperature rises to 600
℃；Continue to heat up and vacuumize, controls the time 1 ~ 2 hour, temperature rises to 700 DEG C；Continue to heat up and rush nitrogen control kiln internal pressure
Power is not less than 1.5 atmospheric pressure, controls the time 8 ~ 10 hours, temperature rises to 1000 DEG C；Continue to heat up, the control time 8 ~ 10 is small
When, temperature rises to 1350 DEG C；Heat preservation in 2 ~ 4 hours is carried out when temperature reaches 1350 DEG C.
Claims (4)
1. a kind of silicon nitride combined silicon carbide brick, which is characterized in that the component including following parts by weight: 70 ~ 80 parts of carbonization
Silicon, 15 ~ 20 parts of carbide fine powder, 2 ~ 8 parts of metallic silicon, 1 ~ 5 part of Suzhou soil, 1 ~ 3 part of calcium lignosulfonate.
2. silicon nitride combined silicon carbide brick according to claim 1, which is characterized in that the carbide fine powder fineness is little
In 100 μm.
3. the method for preparing silicon nitride combined silicon carbide brick described in claim 1 characterized by comprising measured by formula each
Raw material, by silicon carbide, carbide fine powder, it is spare that metallic silicon forms mixed powder after mixing；By Suzhou soil, calcium lignosulfonate is mixed
It is even, the water of gross mass 3wt% is added, mixes, then mixing is added in the mixed powder of mixing, vibrates press-molding, 350 DEG C are sufficiently
It dries, firing of pressurizeing under nitrogen atmosphere.
4. preparing the method for silicon nitride combined silicon carbide brick according to claim 3, which is characterized in that under the nitrogen atmosphere
Pressurization firing includes that the semi-finished product after drying are imported kiln to heat up, and is controlled the heating-up time 14 ~ 18 hours, temperature rises to
600℃；Continue to heat up and vacuumize, controls the time 1 ~ 2 hour, temperature rises to 700 DEG C；Continue to heat up and rush in nitrogen control kiln
Pressure is not less than 1.5 atmospheric pressure, controls the time 8 ~ 10 hours, temperature rises to 1000 DEG C；Continue to heat up, the control time 8 ~ 10 is small
When, temperature rises to 1350 DEG C；Heat preservation in 2 ~ 4 hours is carried out when temperature reaches 1350 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115417674A (en) * | 2022-10-14 | 2022-12-02 | 郴州市拓道新材料科技有限公司 | Wear-resistant silicon nitride/silicon carbide composite ceramic and preparation method and application thereof |
| CN116178026A (en) * | 2022-12-05 | 2023-05-30 | 山西华钠碳能科技有限责任公司 | Sagger for sintering battery material and preparation method and application thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115417674A (en) * | 2022-10-14 | 2022-12-02 | 郴州市拓道新材料科技有限公司 | Wear-resistant silicon nitride/silicon carbide composite ceramic and preparation method and application thereof |
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| CN116178026A (en) * | 2022-12-05 | 2023-05-30 | 山西华钠碳能科技有限责任公司 | Sagger for sintering battery material and preparation method and application thereof |
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Application publication date: 20190322 |