CN105198440B - Resistance to heat shocks silicon carbide crucible and its manufacture craft - Google Patents

Resistance to heat shocks silicon carbide crucible and its manufacture craft Download PDF

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CN105198440B
CN105198440B CN201510731195.1A CN201510731195A CN105198440B CN 105198440 B CN105198440 B CN 105198440B CN 201510731195 A CN201510731195 A CN 201510731195A CN 105198440 B CN105198440 B CN 105198440B
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resistance
crucible
silicon carbide
heat shocks
mesh
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CN105198440A (en
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马兰
杨绍利
刘坤
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Fuyang Keyou Testing Technology Co., Ltd
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Panzhihua University
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Abstract

The invention belongs to crucible production field, and in particular to resistance to heat shocks silicon carbide crucible and its manufacture craft.The technical problem to be solved in the present invention is that the silicon carbide crucible sintering cost that existing method makes is high, and thermal coefficient of expansion is big, and elasticity is small, and resistance to heat shocks is poor, causes the easy fragmentation of crucible under the conditions of rapid heat cycle.The scheme that the present invention solves above-mentioned technical problem is to provide a kind of resistance to heat shocks silicon carbide crucible and its manufacture craft.Above-mentioned resistance to heat shocks silicon carbide crucible, its constituent content are (by mass percentage):Carborundum 75%~85%, oxygen scavenger 7%~17%, additive 0.7%~1%, binding agent 2%~7%, surplus are releasing agent.Resistance to heat shocks silicon carbide crucible provided by the invention, there is good thermal shock resistance, >=1200 DEG C of burner hearths can be passed in and out, crucible is not burst, meanwhile, the manufacture craft of resistance to heat shocks silicon carbide crucible provided by the invention is simple and easy, has the potentiality of large-scale production.

Description

Resistance to heat shocks silicon carbide crucible and its manufacture craft
Technical field
The invention belongs to crucible production field, and in particular to resistance to heat shocks silicon carbide crucible and its manufacture craft.
Background technology
Because the research to crucible is constantly goed deep into, novel high-quality crucible emerges in an endless stream.But with scientific and technological further Development, crucible of high quality and at a reasonable price do not catch up with demand increasingly, and due to carborundum stable chemical performance, thermal conductivity factor is high, heat is swollen Swollen coefficient is low, so silicon carbide crucible is also gradually suggested and developed.But up to the present, the technology of silicon carbide crucible General to use hot pressing vacuum-sintering, sintering cost is high, and thermal coefficient of expansion is big, and elasticity is small, and resistance to heat shocks is poor, causes rapid heat cycle bar The easy fragmentation of crucible under part.
The content of the invention
The technical problem to be solved in the present invention is that the silicon carbide crucible sintering cost that existing method makes is high, thermal coefficient of expansion Greatly, elasticity is small, and resistance to heat shocks is poor, causes the easy fragmentation of crucible under the conditions of rapid heat cycle.
The scheme that the present invention solves above-mentioned technical problem is to provide a kind of resistance to heat shocks silicon carbide crucible and its manufacture craft.
Above-mentioned resistance to heat shocks silicon carbide crucible, its constituent content are (by mass percentage):Carborundum 75%~85%, Oxygen scavenger 7%~17%, additive 0.7%~1%, binding agent 2%~7%, surplus are releasing agent.
In above-mentioned resistance to heat shocks silicon carbide crucible, the carborundum is by 60~80 mesh, 100~200 mesh and 300~325 mesh Carborundum composition.Wherein, the mass ratio between the carborundum of 60~80 mesh, 100~200 mesh and 300~325 mesh is 1~3 ︰ 2 ~4 ︰ 1~2.
In above-mentioned resistance to heat shocks silicon carbide crucible, the oxygen scavenger is at least one in graphite powder, aluminium powder, magnesium powder or iron powder Kind.
In above-mentioned resistance to heat shocks silicon carbide crucible, the additive is in aluminum oxide, yittrium oxide, zirconium oxide or iron oxide It is one or two kinds of.
In above-mentioned resistance to heat shocks silicon carbide crucible, the binding agent is waterglass, clay, PVA (polyvinyl alcohol) or CMC Any one in (sodium carboxymethylcellulose).
In above-mentioned resistance to heat shocks silicon carbide crucible, described releasing agent is in graphite powder, talcum powder, mica powder or paraffin It is at least one.
The manufacture craft of above-mentioned resistance to heat shocks silicon carbide crucible, comprises the following steps:
A, by carborundum 75%~85%, oxygen scavenger 7%~17%, additive 0.7%~1%, binding agent 2%~7% Mixed with the releasing agent of surplus;
B, the material of mixing is put into mould, it is compressing, spontaneously dry 2~3 days, obtain crucible base;
C, by crucible base at 1350~1450 DEG C, normal pressure-sintered 18~24h, after furnace cooling, resistance to heat shocks carbonization is obtained Silica crucible.
In the manufacture craft of above-mentioned resistance to heat shocks silicon carbide crucible, need to be incubated during normal pressure-sintered described in step c. The operation of the insulation is:60 minutes are incubated when temperature is raised to 400 DEG C, temperature is incubated 60 minutes when being raised to 600 DEG C, temperature liter 120~150 minutes are incubated at 800 DEG C, temperature is incubated 60 minutes when being raised to 1000 DEG C, is 1250~1350 DEG C of insulations in temperature 120~150 minutes.
Resistance to heat shocks silicon carbide crucible provided by the invention, there is good thermal shock resistance, 1200 DEG C of stoves of > can be passed in and out Thorax, tolerance time >=30 hour, crucible are not burst, reusable more than 3 times.Meanwhile resistance to heat shocks carbon provided by the invention SiClx crucible manufacture craft is simple and easy.
Embodiment
Resistance to heat shocks silicon carbide crucible, its constituent content are (by mass percentage):Carborundum 75%~85%, deoxygenation Agent 7%~17%, additive 0.7%~1%, binding agent 2%~7%, surplus are releasing agent.
In above-mentioned resistance to heat shocks silicon carbide crucible, the carborundum is by 60~80 mesh, 100~200 mesh and 300~325 mesh Carborundum composition.Wherein, the mass ratio between the carborundum of 60~80 mesh, 100~200 mesh and 300~325 mesh is 1~3 ︰ 2 ~4 ︰ 1~2.The present invention uses the carborundum mass ratio of specific different meshes, and the crucible for making to obtain has larger base substrate close Degree;Moreover, the carborundum mass ratio of specific different meshes, can make crucible have larger thermal shock resistance;Meanwhile specific difference The carborundum mass ratio of mesh number, can reduce crucible cost.
In above-mentioned resistance to heat shocks silicon carbide crucible, the oxygen scavenger is at least one in graphite powder, aluminium powder, magnesium powder or iron powder Kind.
In above-mentioned resistance to heat shocks silicon carbide crucible, the additive is in aluminum oxide, yittrium oxide, zirconium oxide or iron oxide It is one or two kinds of.
In above-mentioned resistance to heat shocks silicon carbide crucible, the binding agent is waterglass, clay, PVA (polyvinyl alcohol) or CMC Any one in (sodium carboxymethylcellulose).
In above-mentioned resistance to heat shocks silicon carbide crucible, described releasing agent is in graphite powder, talcum powder, mica powder or paraffin It is at least one.
The manufacture craft of above-mentioned resistance to heat shocks silicon carbide crucible, comprises the following steps:
A, by carborundum 75%~85%, oxygen scavenger 7%~17%, additive 0.7%~1%, binding agent 2%~7% Mixed with the releasing agent of surplus;
B, the material of mixing is put into mould, it is compressing, spontaneously dry 2~3 days, obtain crucible base;
C, by crucible base at 1350~1450 DEG C, normal pressure-sintered 18~24h, after furnace cooling, resistance to heat shocks carbonization is obtained Silica crucible.
In the manufacture craft of above-mentioned resistance to heat shocks silicon carbide crucible, need to be incubated during normal pressure-sintered described in step c. The operation of the insulation is:60 minutes are incubated when temperature is raised to 400 DEG C, temperature is incubated 60 minutes when being raised to 600 DEG C, temperature liter 120~150 minutes are incubated at 800 DEG C, temperature is incubated 60 minutes when being raised to 1000 DEG C, is 1250~1350 DEG C of insulations in temperature 120~150 minutes.
Embodiment 1
The resistance to heat shocks silicon carbide crucible of the present embodiment, including following component and each component content (by mass percentage) It is as follows:85% carborundum, 7% graphite powder, 1% aluminum oxide, 5% waterglass, surplus are mica powder releasing agent.
In the present embodiment, the carborundum is made up of three kinds of 60~80 mesh, 100~200 mesh and 300~325 mesh specifications, its In 60~80 mesh, 100~200 mesh and 300~325 mesh carborundum between mass ratio be 2:3:1.
Resistance to heat shocks silicon carbide crucible in the present embodiment is made by following technique:Raw material is mixed first and is sufficiently stirred It is even then powder is compressing by press, it is then charged into high temperature furnace, is incubated 60 minutes when temperature is raised to 400 DEG C, temperature 60 minutes are incubated when being raised to 600 DEG C, temperature is incubated 120 minutes when being raised to 800 DEG C, and temperature is incubated 60 minutes when being raised to 1000 DEG C, It is 1250 DEG C in temperature and is incubated 120 minutes, with stove natural cooling.
The porosity of resistance to heat shocks silicon carbide crucible obtained by the present embodiment is 4%, and tolerable temperature is 1200 DEG C, during tolerance Between be 1 hour, reusable 5 times.
Embodiment 2
The resistance to heat shocks silicon carbide crucible of the present embodiment, including following component and each component content (by mass percentage) It is as follows:80% carborundum, 12% graphite powder, 0.8% yittrium oxide, 7% PVA, surplus are graphite powder releasing agent.
In the present embodiment, the carborundum is made up of three kinds of 60~80 mesh, 100~200 mesh and 300~325 mesh specifications, its In mass ratio between 60~80 mesh, 100~200 mesh and 300~325 mesh carborundum be 1.5:4:2.
The resistance to heat shocks silicon carbide crucible of the present embodiment is made by following technique:Raw material is mixed first and is sufficiently stirred It is even then powder is compressing by press, it is then charged into high temperature furnace and sinters, 60 minutes is incubated when temperature is raised to 400 DEG C, Temperature is incubated 60 minutes when being raised to 600 DEG C, and temperature is incubated 150 minutes when being raised to 800 DEG C, and temperature is incubated 60 points when being raised to 1000 DEG C Clock, it is 1350 DEG C in temperature and is incubated 150 minutes, with stove natural cooling.
The porosity of resistance to heat shocks silicon carbide crucible obtained by the present embodiment is 5.5%, and tolerable temperature is 1250 DEG C, tolerance Time is 1.5 hours, reusable 4 times.
Embodiment 3
The resistance to heat shocks silicon carbide crucible of the present embodiment, including following component and each component content (by mass percentage) It is as follows:82% carborundum, 10% graphite powder, 0.6% zirconium oxide, 6% waterglass, surplus are talcum powder releasing agent.
In the present embodiment, the carborundum is made up of three kinds of 60~80 mesh, 100~200 mesh and 300~325 mesh specifications, its In 60~80 mesh, 100~200 mesh and 300~325 mesh carborundum between mass ratio be 1:3:1.5.
Resistance to heat shocks silicon carbide crucible in the present embodiment is made by following technique:Raw material is mixed first and is sufficiently stirred It is even then powder is compressing by press, sintering (not vacuumizing) in high temperature furnace is then charged into, when temperature is raised to 400 DEG C Insulation 60 minutes, temperature are incubated 60 minutes when being raised to 600 DEG C, and temperature is incubated 125 minutes when being raised to 800 DEG C, and temperature is raised to 1000 DEG C when be incubated 60 minutes, temperature be 1350 DEG C be incubated 125 minutes, with stove natural cooling.
The porosity that resistance to heat shocks silicon carbide crucible is made in the present embodiment is 7%, and tolerable temperature is 1300 DEG C, tolerance time For 2 hours, reusable 3 times.
Resistance to heat shocks silicon carbide crucible provided by the invention, there is good thermal shock resistance, >=1200 DEG C of stoves can be passed in and out Thorax, crucible are not burst.

Claims (3)

1. resistance to heat shocks silicon carbide crucible, its constituent content are (by mass percentage):Carborundum 75%~85%, oxygen scavenger 7%~17%, additive 0.7%~1%, binding agent 2%~7%, surplus is releasing agent;The carborundum by 60~80 mesh, The carborundum of 100~200 mesh and 300~325 mesh forms, 60~80 mesh, 100~200 mesh, the quality of 300~325 mesh carborundum Than for the ︰ 1~2 of 1~3 ︰ 2~4;
The oxygen scavenger is at least one of graphite powder, aluminium powder, magnesium powder or iron powder;The additive be aluminum oxide, yittrium oxide, One or both of zirconium oxide or iron oxide;The binding agent is waterglass, clay, polyvinyl alcohol or sodium carboxymethylcellulose In any one;Described releasing agent is at least one of graphite powder, talcum powder, mica powder or paraffin.
2. the manufacture craft of resistance to heat shocks silicon carbide crucible, comprises the following steps described in claim 1:
A, by carborundum 75%~85%, oxygen scavenger 7%~17%, additive 0.7%~1%, binding agent 2%~7% and remaining The releasing agent of amount mixes;
B, the material of mixing is put into mould, it is compressing, spontaneously dry 2~3 days, obtain crucible base;
C, by crucible base at 1350~1450 DEG C, normal pressure-sintered 18~24h, after furnace cooling, resistance to heat shocks carborundum earthenware is obtained Crucible.
3. the manufacture craft of resistance to heat shocks silicon carbide crucible according to claim 2, it is characterised in that:Described in step c Need to be incubated during normal pressure-sintered;The operation of the insulation is:60 minutes are incubated when temperature is raised to 400 DEG C, temperature is raised to 60 minutes are incubated at 600 DEG C, temperature is incubated 120~150 minutes when being raised to 800 DEG C, and temperature is incubated 60 minutes when being raised to 1000 DEG C, It is 1250~1350 DEG C in temperature and is incubated 120~150 minutes.
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Publication number Priority date Publication date Assignee Title
CN105753498A (en) * 2016-01-26 2016-07-13 无锡强工机械工业有限公司 Preparation method of high-temperature-resisting silicon carbide-based composite material
CN105906369B (en) * 2016-04-18 2018-04-13 湖南浩威特科技发展有限公司 The sintering method of carborundum prefabricated component and the preparation method of aluminium silicon carbide plate
CN106187247B (en) * 2016-07-26 2019-11-08 唐山贝斯特高温材料有限公司 Metallic aluminium silicon carbide composite diphase material and preparation method thereof
CN107162612A (en) * 2017-05-26 2017-09-15 长兴华悦耐火材料厂 A kind of silicon carbide crucible and preparation method thereof
CN107686355A (en) * 2017-09-18 2018-02-13 佛山市高捷工业炉有限公司 The preparation method of high intensity crucible
CN107986804A (en) * 2017-12-11 2018-05-04 洛阳名力科技开发有限公司 A kind of neutral refractory
CN108840682A (en) * 2018-07-12 2018-11-20 佛山市高捷工业炉有限公司 A kind of high abrasion crucible ceramic material
CN109485429A (en) * 2018-11-13 2019-03-19 武汉美琪林新材料有限公司 A kind of silicon carbide ceramics soup ladle suspension setting rod and preparation method thereof
CN109485428A (en) * 2018-11-13 2019-03-19 武汉美琪林新材料有限公司 A kind of domestic ceramics silicon plate and preparation method thereof

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CN101973773A (en) * 2010-11-03 2011-02-16 淄博恒世科技发展有限公司 Preparation method of large crucible with combination of silicon nitride and silicon carbide
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CN103880455A (en) * 2014-02-12 2014-06-25 嘉兴皓特特种陶瓷有限公司 Preparation method of steel cord enhanced graphite silicon carbide crucible

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CN101318812A (en) * 2008-06-27 2008-12-10 中国铝业股份有限公司 Method for manufacturing high-alumina-quality high-temperature crucible pot
CN101973773A (en) * 2010-11-03 2011-02-16 淄博恒世科技发展有限公司 Preparation method of large crucible with combination of silicon nitride and silicon carbide
CN103298983A (en) * 2010-12-22 2013-09-11 施托伊勒太阳能有限公司 Crucibles
CN103880455A (en) * 2014-02-12 2014-06-25 嘉兴皓特特种陶瓷有限公司 Preparation method of steel cord enhanced graphite silicon carbide crucible

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Address before: 617000 Airport Road, Panzhihua, Sichuan, No. 10

Patentee before: PANZHIHUA University