CN107311634A - A kind of nitride bonded sandwich setter plate and preparation method thereof - Google Patents
A kind of nitride bonded sandwich setter plate and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of nitride bonded sandwich setter plate and preparation method thereof, belong to technical field of refractory materials, including mullite sealer, silicon nitride combined silicon carbide are intermediate layer；Each layer is made up of following raw material：Mullite protective layer：Coarseness is 0.2 1mm mullite, 200 mesh mullite fine powders, 325 mesh mullites and clay, organic bond；Silicon nitride combined silicon carbide intermediate layer：The carborundum that coarseness is 1 3mm is, 0.5 1mm, 325 mesh carbide fine powders, silicon carbide ultrafine powder, clay and the mesh of metallic silicon power 325, organic bond.The present invention is used as intermediate layer using silicon nitride combined silicon carbide, the high temperature break resistant intensity of silicon nitride combined silicon carbide is high, and the rupture strength not anti-reflection under high temperature was once, and the reaction of magnetic material and load bearing board is avoided in sintering magnetic materials, indirectly improved the service life of load bearing board.
Description
Technical field
The present invention relates to a kind of nitride bonded sandwich setter plate and preparation method thereof, belong to refractory technology neck
Domain.
Background technology
Sandwich setter plate is a kind of a kind of fire resistant bearing board for being widely used in magnetic material industry sintering, is usually with oxygen
Compound silicon carbide is intermediate layer, mullite or the structure that corundum is sealer.The routine of magnetic material burns till temperature
Degree is between 1350 DEG C -1450 DEG C, with nitrogen protection atmosphere, simultaneously because magnetic material contains the metallic elements such as iron, manganese, zinc
Sandwich setter plate easily with oxide combined silicon carbide reacts, and causes the consequences such as magnetic material pollution, electrical property decline.This
Outside, the sandwich setter plate full-size for the oxide combined silicon carbide that producer can produce in batches is no more than both at home and abroad at present
400*400mm, thickness must could meet the sintering of some big specification magnetic materials in more than 15mm.When in use because under high temperature
The low defect of rupture strength, often easily causes load bearing board fracture, causes kiln accident, cause economic loss.Magnetic material is given birth to
Producer is produced in the urgent need to, the high load bearing board of big specification, thickness of thin, load-carrying to fire some super-huge ferrite beads, is also state
The Main way of interior kiln furnitures manufacturer exploitation.
The content of the invention
In view of the shortcomings of the prior art, the first object of the present invention is can to provide a kind of nitride bonded sandwich to hold burning
Plate；The second object of the present invention is to provide a kind of process for preparing nitride bonded sandwich setter plate.
The purpose of the present invention is achieved by the following technical programs：
A kind of nitride bonded sandwich setter plate, including mullite sealer, silicon nitride combined silicon carbide are intermediate layer；
Each layer by following raw material by weight：
Mullite protective layer：Coarseness is 0.2-1mm 40 parts -50 parts of mullite, 200 10 parts -40 parts of mesh mullite fine powders,
325 10 parts -20 parts of mesh mullites and 1 part -5 parts of clay, 0.1 part -1 part of organic bond；
Silicon nitride combined silicon carbide intermediate layer：The carborundum that coarseness is 1-3mm is 20 parts -50 parts, 0.5-1mm is 10 part -40
Part, 325 mesh carbide fine powders be 10 parts -20 parts, silicon carbide ultrafine powder be 1 part -10 parts, 1 part -5 parts of clay and metallic silicon power
325 5 parts -20 parts of mesh, 0.1 part -1 part of organic bond.
Wherein, the organic bond is sodium carboxymethylcellulose（CMC）, 20 parts of concentration yellow starch gum solution.
The clay is the mud of Suzhou one.
A kind of preparation method of nitride bonded sandwich setter plate, comprises the following steps：
（1）It is prepared by raw material
Mullite fabric：Take coarseness be 0.2-1mm 40 parts -50 parts of mullite, 200 10 parts -40 parts of mesh mullite fine powders,
1 part -5 parts of 325 10 parts -20 parts of mesh mullites and clay are poured into edge runner and stirred 10 minutes, add organic bond 0.1
Part -1 part carries out wet stone roller with 1 part -10 parts of water, is then placed in stainless steel bucket old；
The black material of silicon nitride combined silicon carbide：To take 325 mesh carbide fine powders be 10 parts -20 parts, silicon carbide ultrafine powder is 1 part -10 parts,
5 parts -20 parts of 1 part -5 parts of clay and 325 mesh of metallic silicon power are put into Double cone mixer, add zirconium oxide abrasive ball, are carried out thin
Powder is pre-mixed, and incorporation time is 30 minutes.The carborundum for taking coarseness to be 1-3mm again is 20 parts -50 parts, 0.5-1mm be 10 parts -
40 parts are put into stirring 10 minutes in edge runner, add 1 part -10 parts of water, 0.1 part -1 part of organic bond, remix 10 minutes,
The fine powder of premixing is subsequently added, wet stone roller 25 minutes is finally putting into stainless steel bucket old；
（2）Shaping
Add load weighted mullite fabric in a mold and strike off rapidly, then pour into the black material of carborundum and strike off rapidly, and with pressure
Flitch flicking once, makes black material have certain orthostatic, then pours into mullite fabric again and strikes off rapidly, finally starts shooting
It is compressing；
（3）Dry
Sandwich setter plate after forming is put into electric drying chamber, dried to 1 part of moisture content ＜；
（4）Burn till
By on the loading kiln car of dried green compact in order, enter kiln and burnt till, because intermediate layer is silicon nitride combined silicon carbide,
Burning till environment must be sintered in a nitrogen atmosphere, and the kiln burnt till is full-automatic vacuum-pumping formula nitrogen firing furnace, and calcining system is pressed
Carried out according to silicon nitride combined silicon carbide material, maximum temperature is incubated 3-8 hours between 1350 DEG C -1450 DEG C.
The nitride bonded sandwich setter plate of the present invention, intermediate layer employs silicon nitride combined silicon carbide, silicon nitride knot
Close carbofrax material and have that density is big, intensity is high, thermal shock resistance can good, load softening point is high, good heat conductivity the characteristics of.
The combining form that the material tight interweaves enables silicon-carbide particle surface obtain good protection again, and candle is invaded to external
Medium osmosis, which is played, to be delayed and inhibition, improves the chemical stability of silicon nitride combined silicon carbide material.
Silicon nitride combined silicon carbide has good inoxidizability, in high-temperature oxydation, and material surface can generate densification
Silica glass phase, blocking enclose stomata so that prevent internal material be oxidized and cause the strength of materials it is quick under
Drop.Its antioxygenic property is a very important performance indications, if the antioxygenic property of product is poor, product epidermis is being used
In progressively can aoxidize to form silica, the erosion-resisting characteristics of material weakens, and heat conductivility significantly declines, and causes entering for material
One step invades candle.
The invention has the advantages that：
（1）The present invention is using silicon nitride combined silicon carbide as intermediate layer, and the high temperature break resistant intensity of silicon nitride combined silicon carbide is
Rupture strength not anti-reflection under 2-5 times of normal silicon oxides silicon carbide, and high temperature once, the three of the 400*400*10mm being made
Mingzhi's load bearing board doubles the above than thickness for 15mm normal silicon oxides silicon carbide sandwich boards load-carrying, meets significantly
The harsh use requirement of client.
（2）Nitride bonded phase is in the intermediate layer that the present invention is used, in sintering magnetic materials, because its nitrogen atmosphere is protected
Shield, easily forms that match is grand to be combined thing again with the part free silica in mullite fabric, so that superficial layer and intermediate layer are tied
Close performance more preferable, it is to avoid the reaction of magnetic material and load bearing board, indirectly improve the service life of load bearing board.
（3）Intermediate layer in the present invention is due to using nitride bonded phase, and thermal coefficient of expansion is compared to wanting that oxide is combined
It is much smaller, cause that the thermal shock resistance of load bearing board is better, load bearing board does not allow easy fracture in Reusability process, so as to avoid kiln
Stove collapse accident.
（Sintered in 4 present invention using nitrogen atmosphere, because metallic silicon and nitrogen react generation silicon nitride at high temperature, together
When give off heat, the energy resource consumption for burning till the later stage is gradually reduced, compared to oxide combine reduce energy resource consumption, reduce life
Produce cost.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment 1
（1）Mullite fabric：Take 50 parts of the mullite, about 30 parts of 200 mesh mullite fine powder, 325 mesh that coarseness is 0.2-1mm not
The clay for carrying out 15 parts and 5 parts of stone pours into stirring 10 minutes in edge runner, and the water for adding CMC0.5 parts and 5 parts carries out wet stone roller,
It is then placed in stainless steel bucket old；
The black material of silicon nitride combined silicon carbide：To take 325 mesh carbide fine powders be 15 parts, silicon carbide ultrafine powder is 3 parts, 2 parts of clay with
And 10 parts of 325 mesh of metallic silicon power is put into Double cone mixer, zirconium oxide abrasive ball is added, fine powder premixing, incorporation time is carried out
For 30 minutes.Take 20 parts of the carborundum, 0.5-1mm that coarseness is 1-3mm to be 50 parts again and be put into stirring 10 minutes in edge runner, plus
Enter 3 parts of water, 1 part of the yellow starch gum solution of 20 parts of concentration.
Remix 10 minutes, be subsequently added the fine powder of premixing, wet stone roller 25 minutes is finally putting into stainless steel bucket old
It is rotten；
（2）Shaping
By taking 400*400*10mm nitride bonded sandwich setter plates as an example：
Add load weighted mullite fabric in a mold and strike off rapidly, then pour into the black material of carborundum and strike off rapidly, and with pressure
Flitch flicking once, makes black material have certain orthostatic, then pours into mullite fabric again and strikes off rapidly, finally starts shooting
It is compressing.
（3）Dry
Sandwich setter plate after forming is put into electric drying chamber, dried to 1 part of moisture content ＜.
（4）Burn till
Dried green compact are loaded on kiln car in order, in the case where maximum temperature is 1350 DEG C, 5 hours are incubated.
Embodiment 2
Step is substantially the same manner as Example 1, and difference is：
Mullite fabric：40 parts of mullite, about 35 parts of 200 mesh mullite fine powder, 325 mesh for taking coarseness to be 0.2-1mm do not come
The clay that 20 parts and 5 parts of stone.
The black material of silicon nitride combined silicon carbide：To take 325 mesh carbide fine powders be 15 parts, silicon carbide ultrafine powder is 3 parts, clay 2
The 10 parts of progress fine powder premixings of part and 200 mesh of metallic silicon power, incorporation time is 30 minutes.The carbon that coarseness is 1-3mm is taken again
25 parts of SiClx, 0.5-1mm are 45 parts.
Maximum temperature be 1400 DEG C at, be incubated 4 hours.
Embodiment 3
Step is substantially the same manner as Example 1, and difference is：
Mullite fabric：40 parts of mullite, about 35 parts of 200 mesh mullite fine powder, 325 mesh for taking coarseness to be 0.2-1mm do not come
The clay that 20 parts and 5 parts of stone.
The black material of silicon nitride combined silicon carbide：To take 325 mesh carbide fine powders be 10 parts, silicon carbide ultrafine powder is 3 parts, clay 2
The 15 parts of progress fine powder premixings of part and 200 mesh of metallic silicon power, incorporation time is 30 minutes.The carbon that coarseness is 1-3mm is taken again
25 parts of SiClx, 0.5-1mm are 45 parts.
Maximum temperature is at 1420 DEG C, insulation 3 hours can
The load bearing board physical property contrast that examples detailed above is obtained is shown in Table 1：
The load bearing board physical property of table 1 detects table
Proposition of the present invention substitutes silicon-carborundum for a long time with nitride combined silicon carbide and is used as sandwich setter plate
Intermediate layer, instead of original oxidation and sinter system using brand-new nitriding atmosphere sintering schedule.
It should be understood by those skilled in the art that, the present invention is not limited to the above embodiments, above-described embodiment and explanation
Merely illustrating the principles of the invention described in book, without departing from the spirit and scope of the present invention, the present invention also have
Various changes and modifications, these changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention
By appended claims and its equivalent thereof.
Claims (5)
1. a kind of nitride bonded sandwich setter plate, it is characterised in that including mullite sealer, silicon nitride bonded silicon carbon
SiClx is intermediate layer；Each layer by following raw material by weight：
Mullite protective layer：Coarseness is 0.2-1mm 40 parts -50 parts of mullite, 200 10 parts -40 parts of mesh mullite fine powders,
325 10 parts -20 parts of mesh mullites and 1 part -5 parts of clay, 0.1 part -1 part of organic bond；
Silicon nitride combined silicon carbide intermediate layer：The carborundum that coarseness is 1-3mm is 20 parts -50 parts, 0.5-1mm is 10 part -40
Part, 325 mesh carbide fine powders be 10 parts -20 parts, silicon carbide ultrafine powder be 1 part -10 parts, 1 part -5 parts of clay and metallic silicon power
325 5 parts -20 parts of mesh, 0.1 part -1 part of organic bond.
2. a kind of nitride bonded sandwich setter plate according to claim 1, it is characterised in that：The organic bond
For sodium carboxymethylcellulose, the yellow starch gum solution mixture of 20 parts of concentration.
3. a kind of nitride bonded sandwich setter plate according to claim 1, it is characterised in that：The clay is Suzhou
Mud one.
4. a kind of preparation method of nitride bonded sandwich setter plate according to claim 1, it is characterised in that：Bag
Include following steps：
（1）It is prepared by raw material
Mullite fabric：Take coarseness be 0.2-1mm 40 parts -50 parts of mullite, 200 10 parts -40 parts of mesh mullite fine powders,
1 part -5 parts of 325 10 parts -20 parts of mesh mullites and clay are poured into edge runner and stirred 10 minutes, add organic bond 0.1
Part -1 part carries out wet stone roller with 1 part -10 parts of water, is then placed in stainless steel bucket old；
The black material of silicon nitride combined silicon carbide：To take 325 mesh carbide fine powders be 10 parts -20 parts, silicon carbide ultrafine powder is 1 part -10 parts,
5 parts -20 parts of 1 part -5 parts of clay and 325 mesh of metallic silicon power are put into Double cone mixer, add zirconium oxide abrasive ball, are carried out thin
Powder is pre-mixed, and incorporation time is 30 minutes.
5. the carborundum for taking coarseness to be 1-3mm again is 20 parts -50 parts, 0.5-1mm is 10 parts -40 parts and is put into edge runner and stirs
10 minutes, water, 0.1 part -1 part of the organic bond of 1 part -10 parts of addition remixed 10 minutes, are subsequently added the thin of premixing
Powder, wet stone roller 25 minutes, is finally putting into stainless steel bucket old；
（2）Shaping
Add load weighted mullite fabric in a mold and strike off rapidly, then pour into the black material of carborundum and strike off rapidly, and with pressure
Flitch flicking once, makes black material have certain orthostatic, then pours into mullite fabric again and strikes off rapidly, finally starts shooting
It is compressing；
（3）Dry
Sandwich setter plate after forming is put into electric drying chamber, dried to 1 part of moisture content ＜；
（4）Burn till
By on the loading kiln car of dried green compact in order, enter kiln and burnt till, because intermediate layer is silicon nitride combined silicon carbide,
Burning till environment must be sintered in a nitrogen atmosphere, and the kiln burnt till is full-automatic vacuum-pumping formula nitrogen firing furnace, and calcining system is pressed
Carried out according to silicon nitride combined silicon carbide material, maximum temperature is incubated 3-8 hours between 1350 DEG C -1450 DEG C.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107935576A (en) * | 2017-12-06 | 2018-04-20 | 郑州大学 | Silicon nitride bonded silicon mullite composite silicon carbide ceramic material and preparation method thereof |
| CN109748594A (en) * | 2019-03-12 | 2019-05-14 | 宜兴市恒祥耐火材料有限公司 | A kind of coke dry quenching furnace bracket refractory protection material and preparation method thereof |
| CN111747771A (en) * | 2019-03-29 | 2020-10-09 | 日本碍子株式会社 | Clamp for firing |
| CN111892403A (en) * | 2020-08-03 | 2020-11-06 | 福赛特(唐山)新材料有限公司 | High-temperature anti-bending silicon nitride combined silicon carbide slab and preparation method thereof |
| CN115368143A (en) * | 2022-05-30 | 2022-11-22 | 宜兴市拓邦耐火科技有限公司 | Silicon nitride microcrystal plate and its production process |
| CN115872756A (en) * | 2021-11-10 | 2023-03-31 | 济源市耐火炉业有限公司 | Composite checker brick for large coke oven and preparation method thereof |
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| US5980699A (en) * | 1997-10-24 | 1999-11-09 | Southwest Research Institute | Method for preparing silicon nitride and silicon nitride composites |
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| CN107935576A (en) * | 2017-12-06 | 2018-04-20 | 郑州大学 | Silicon nitride bonded silicon mullite composite silicon carbide ceramic material and preparation method thereof |
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| CN111747771A (en) * | 2019-03-29 | 2020-10-09 | 日本碍子株式会社 | Clamp for firing |
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| CN115872756A (en) * | 2021-11-10 | 2023-03-31 | 济源市耐火炉业有限公司 | Composite checker brick for large coke oven and preparation method thereof |
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