CN102795859A - SiC-Si3N4 high temperature ceramic furnace bottom plate for annular furnace and preparation method thereof - Google Patents

SiC-Si3N4 high temperature ceramic furnace bottom plate for annular furnace and preparation method thereof Download PDF

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Publication number
CN102795859A
CN102795859A CN201210295924XA CN201210295924A CN102795859A CN 102795859 A CN102795859 A CN 102795859A CN 201210295924X A CN201210295924X A CN 201210295924XA CN 201210295924 A CN201210295924 A CN 201210295924A CN 102795859 A CN102795859 A CN 102795859A
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sic
preparation
drop
parts
powder
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祝洪喜
骆中汉
邓承继
汪盛明
张小东
彭玮珂
程明
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HUBEI HONGHUA HIGH TEMPERATURE MATERIAL CO Ltd
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HUBEI HONGHUA HIGH TEMPERATURE MATERIAL CO Ltd
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Abstract

The invention relates to a SiC-Si3N4 high temperature ceramic furnace bottom plate for an annular furnace and a preparation method thereof; the preparation method comprises the following steps: on a basis of a total weight part of 100 parts, weighing 25-75 parts of Si powder and the balance of SiC powder; adding 3-8 parts of a sintering aid and 4-9 parts of a binder, wherein the sintering aid is Y2O3, or a mixture of Y2O3 and Al2O3; performing material mixing, molding, sintering, silicon immersion, and machining to prepare the SiC-Si3N4 high temperature ceramic furnace bottom plate for an annular furnace. The preparation method is simple in process and low in cost, and the obtained product has the characteristics of high temperature resistance, good creep resistance, large high-temperature strength, good thermal shock resistance, and the like, can meet working condition requirements for annular furnace production, and can effectively solve the problems of poor high temperature resistance of metal furnace bottom plates, furnace bottom plate bending deformation due to a large material high-temperature creep rate, furnace bottom plate cracking damage due to a large material thermal expansion rate, and low service life.

Description

A kind of ring furnace is used SiC-Si 3N 4Matter pyroceramic drop-bottom and preparation method thereof
Technical field
The invention belongs to the pyroceramic technical field, be specifically related to a kind of ring furnace and use SiC-Si 3N 4Matter pyroceramic drop-bottom and preparation method thereof.
Background technology
In the ring furnace of metallurgy and machinofacture factory, need a large amount of heat-resisting steel drop-bottom carrying coil of strip and steel parts of using to carry out hot-work production usually.Existing ring furnace base plate generally all is to adopt the high temperature alloy manufacturing; For example for a long time more than 950 ℃ even surpass making metal furnaces base plate under 1000 ℃ the working condition of high temperature and loading, the resistance to elevated temperatures of the high temperature alloy of products obtained therefrom particularly hot strength and creep resistance may not satisfy the requirement of actual condition.This is owing to the high temperature creep rate of metallic substance causes drop-bottom flexural deformation gradually greatly, and the material coefficient of thermal expansion rate is big and cause the drop-bottom cracking to damage.In addition, factors such as creep and cracking cause work-ing life of steel drop-bottom of high temperature alloy preparation lower, the more important thing is that the drop-bottom of distortion can influence the thermal treatment quality and the yield rate of institute's coil of strip that carries and steel part, the reduction productivity effect.Compare with high temperature steel; High temperature ceramic material has advantages such as hot strength height, creep-resistant property is good, coefficient of thermal expansion is little; Not only can effectively improve work-ing life, the reduction base plate use cost of base plate; And can guarantee the thermal treatment quality and the yield rate of the coil of strip that carries and steel part, increase economic efficiency.
Summary of the invention
The present invention is intended to overcome the defective of existing ring furnace steel drop-bottom, and purpose provides the ring furnace that a kind of technology is simple, use properties is good and uses SiC-Si 3N 4The technology of preparing of matter pyroceramic drop-bottom; The pyroceramic drop-bottom of using this technology to prepare is high temperature resistant, creep-resistant property good, hot strength is big, good thermal shock, and the resistance to elevated temperatures high temperature creep rate poor, material that can solve the metal furnaces base plate effectively causes drop-bottom flexural deformation, material coefficient of thermal expansion rate to cause damage of drop-bottom cracking and work-ing life than the problem of hanging down greatly greatly.
For realizing above-mentioned purpose, preparing method's step of the present invention is following:
(1) batching: take by weighing 25 ~ 75 parts of Si powder in 100 parts of total weight parts, surplus is the SiC powder; Add 3 ~ 8 component sintering additives and 4 ~ 9 parts of wedding agents; Said sintering aid is Y 2O 3, or Y 2O 3And Al 2O 3Mixture; Said wedding agent is selected from resol, silicon sol or water glass;
(2) batch mixing: process pug with mixing to grind in the adding of the batching in the step (1) mixing pan;
(3) moulding: the pug of step (2) die for molding of packing into is processed the drop-bottom slab;
(4) sintering: said slab is incubated 1 ~ 30h at nitrogen atmosphere with under 1270 ~ 1430 ℃ of conditions earlier, under nitrogen atmosphere, continues to be warmed up to 1450 ℃ ~ 1700 ℃ again, insulation 3 ~ 12h makes nitridation sintered base;
(5) oozing stain silicon handles: will said nitridation sintered base temperature be 1700 ~ 1850 ℃ with the condition of vacuum tightness less than 100Pa under ooze the processing of stain silicon, the treatment time is 2 ~ 20 hours, makes SiC-Si 3N 4Matter pyroceramic drop-bottom blank;
(6) blank is carried out machining processes, make ring furnace and use SiC-Si 3N 4Matter pyroceramic drop-bottom.
In the present invention, the purity of preferably described Si powder is >=95wt% that granularity is less than 0.1mm; The purity of described SiC powder is >=90wt% that granularity is less than 5mm.
In the present invention, preferably described Y 2O 3Purity>=95wt%, Al 2O 3Purity>=95wt%; Y 2O 3Or Al 2O 3Granularity less than 0.01mm.
In the present invention, described forming method is ramming process or vibratory compaction.
The invention still further relates to the prepared ring furnace of above-mentioned preparation method and use SiC-Si 3N 4Matter pyroceramic drop-bottom.
Below with more detailed description technical scheme of the present invention.
The present invention provides a kind of ring furnace to use SiC-Si 3N 4The preparation method of matter pyroceramic drop-bottom, step is following:
(1) batching: by weight, take by weighing 25 ~ 75 parts of Si powder and 25 ~ 75 parts of SiC powder, and the gross weight of Si powder and SiC powder is 100 parts.Add 3 ~ 8 component sintering additives and 4 ~ 9 parts of wedding agents again.Generally in the art, sintering aid and wedding agent are referred to as admixture.Said sintering aid is Y 2O 3, or Y 2O 3And Al 2O 3Mixture.Said wedding agent is selected from resol, silicon sol or water glass.
Among the present invention, Y 2O 3Be a kind of rare-earth oxide, introduce stupalith, help to increase density of material, reduction sintering temperature and time, raising thermal conductivity as sintering aid.For example adopt Dongguan City gold source rare-earth metal material to sell the yttrium oxide product that ltd sells.
In the present invention, the Si powder is meant the small particle size dust of from the blast furnace flue of smelting the silicon metal, collecting, or is called SILICA FUME or silicon ash.Staple is a vitreous state silicon-dioxide, mixes to make it have high-strength, anti-impact mill, excellent properties such as durable in the concrete.Preferably should use purity to be not less than the Si powder of 95wt%, its granularity is preferably less than 0.1mm, for example the SILICA FUME product of the bright blue silica flour in Shandong Materials Co., Ltd production and sales.
Resol (phenolic resin is called for short PF) is mainly used in produces molding powder, stratified plastics; Make varnish or insulation, corrosion resistant coating; Make daily necessities, ornamental; Making sound insulation, lagging material, wood-based plate, casting, refractory materials etc., is can buy the acquisition product on the market.
Silicon sol (Silica solution) is a kind of colloidal solution, and odorless, nontoxic is the dispersion liquid of silica dioxide granule in water or in the solvent.Because the SiO in the silicon sol 2Silicon sol contains a large amount of water and hydroxyl, so also can be expressed as SiO 2NH 2O.
Water glass is the aqueous solution of water glass, has characteristics such as cohesive force is strong, intensity is higher, acid resistance, good heat resistance, alkali resistance.
(2) batch mixing: process pug with mixing to grind in the adding of the batching in the step (1) mixing pan.
Mixing pan is a mixing equipment common on the market, the wheeled mixing pan of the long-range Harmann Berstorff, Maschinenbau GmbH in for example state-run Henan production and sales.
(3) moulding: the pug of step (2) die for molding of packing into is processed the drop-bottom slab.
(4) sintering: said slab is incubated certain time length at nitrogen atmosphere with under 1270 ~ 1430 ℃ of conditions earlier, and common 1 ~ 30h allows, and then under nitrogen atmosphere, continue to be warmed up to 1450 ℃ ~ 1700 ℃, insulation 3 ~ 12h makes nitridation sintered base;
(5) oozing stain silicon handles: will said nitridation sintered base temperature be 1700 ~ 1850 ℃ with the condition of vacuum tightness less than 100Pa under ooze the processing of stain silicon, the treatment time is 2 ~ 20 hours, makes SiC-Si 3N 4Matter pyroceramic drop-bottom blank;
(6) blank is carried out machining processes, make ring furnace and use SiC-Si 3N 4Matter pyroceramic drop-bottom.
In the present invention, the purity of preferably described Si powder is >=95wt% that granularity is less than 0.1mm; The purity of described SiC powder is >=90wt% that granularity is less than 5mm.
In the present invention, preferably described Y 2O 3Purity should be less than 95wt%, Al 2O 3Purity should be less than 95wt%; Y 2O 3Or Al 2O 3Granularity less than 0.01mm.
In the present invention, described forming method is ramming process or vibratory compaction.
The invention still further relates to the prepared ring furnace of above-mentioned preparation method and use SiC-Si 3N 4Matter pyroceramic drop-bottom.
Compared with prior art, the present invention has following major advantage:
This preparing method's technology is simple, cost is low, and prepared ring furnace is used SiC-Si 3N 4High temperature resistant, characteristics such as creep-resistant property good, hot strength is big, good thermal shock that matter pyroceramic drop-bottom has; Replace heat-resisting steel drop-bottom with it; Can satisfy the working condition requirement that ring furnace is produced, the resistance to elevated temperatures high temperature creep rate poor, material that can solve the metal furnaces base plate effectively causes drop-bottom flexural deformation, material coefficient of thermal expansion rate to cause the problem of hanging down in damage of drop-bottom cracking and work-ing life greatly greatly.
Embodiment
Like no specified otherwise, all adopt weight ratio between each component in the present invention.
In order to understand the present invention better, below in conjunction with embodiment the present invention is further described, but content of the present invention not only is confined to following embodiment.
Embodiment 1
Take by weighing SiC powder 63kg, Si powder 37kg, 3kg Y 2O 3With 4kg resol, in mixing pan, mix to grind and process pug.Pug is packed in the mould, adopt conventional ramming process method moulding to make the furnace bottom slab.
Slab is being incubated 30h under the nitrogen atmosphere under 1270 ℃ of conditions, under nitrogen atmosphere, is continuing to be warmed up to 1700 ℃ again, insulation 3h makes nitridation sintered base.
Nitridation sintered base is oozed stain silicon under 1800 ℃, 30Pa vacuum tightness handle and made the drop-bottom blank in 15 hours.Blank is carried out machining processes, make ring furnace and use SiC-Si 3N 4Matter pyroceramic drop-bottom.
Embodiment 2
Take by weighing SiC powder 55kg, Si powder 45kg, 4kgY 2O 3With 6kg resol, mix the stone roller base like embodiment 1.
Slab is being incubated 5h under the nitrogen atmosphere under 1430 ℃ of conditions, under nitrogen atmosphere, is continuing to be warmed up to 1650 ℃ again, insulation 8h makes nitridation sintered base.
Nitridation sintered base is oozed stain silicon under 1850 ℃, 60Pa vacuum tightness handle and made the drop-bottom blank in 20 hours.Blank is carried out machining processes, make ring furnace and use SiC-Si 3N 4Matter pyroceramic drop-bottom.
Embodiment 3
Take by weighing SiC powder 75kg, Si powder 25kg, 8kgY 2O 3With the 9kg silicon sol, mix the stone roller base like embodiment 1.
Slab is being incubated 5h under the nitrogen atmosphere under 1430 ℃ of conditions, under nitrogen atmosphere, is continuing to be warmed up to 1650 ℃ again, insulation 8h makes nitridation sintered base.
Nitridation sintered base is oozed stain silicon under 1850 ℃, 60Pa vacuum tightness handle and made the drop-bottom blank in 20 hours.Blank is carried out machining processes, make ring furnace and use SiC-Si 3N 4Matter pyroceramic drop-bottom.
Embodiment 4
Take by weighing SiC powder 25kg, Si powder 275kg, 3kgY 2O 3, 3kgAl 2O 3With 6kg water glass, mix the stone roller base like embodiment 1.
Slab is being incubated 1h under the nitrogen atmosphere under 1430 ℃ of conditions, under nitrogen atmosphere, is continuing to be warmed up to 1450 ℃ again, insulation 12h makes nitridation sintered base.
Nitridation sintered base is oozed stain silicon under 1700 ℃, 10Pa vacuum tightness handle and made the drop-bottom blank in 2 hours.Blank is carried out machining processes, make ring furnace and use SiC-Si 3N 4Matter pyroceramic drop-bottom.

Claims (6)

1. a ring furnace is used SiC-Si 3N 4The preparation method of matter pyroceramic drop-bottom is characterized in that step is following:
(1) batching: take by weighing 25 ~ 75 parts of Si powder in 100 parts of total weight parts, surplus is the SiC powder; Add 3 ~ 8 component sintering additives and 4 ~ 9 parts of wedding agents; Said sintering aid is Y 2O 3, or Y 2O 3And Al 2O 3Mixture; Said wedding agent is selected from resol, silicon sol or water glass;
(2) batch mixing: process pug with mixing to grind in the adding of the batching in the step (1) mixing pan;
(3) moulding: the pug of step (2) die for molding of packing into is processed the drop-bottom slab;
(4) sintering: said slab is incubated 1 ~ 30h at nitrogen atmosphere with under 1270 ~ 1430 ℃ of conditions earlier, under nitrogen atmosphere, continues to be warmed up to 1450 ℃ ~ 1700 ℃ again, insulation 3 ~ 12h makes nitridation sintered base;
(5) oozing stain silicon handles: will said nitridation sintered base temperature be 1700 ~ 1850 ℃ with the condition of vacuum tightness less than 100Pa under ooze the processing of stain silicon, the treatment time is 2 ~ 20 hours, makes SiC-Si 3N 4Matter pyroceramic drop-bottom blank;
(6) blank is carried out machining processes, make ring furnace and use SiC-Si 3N 4Matter pyroceramic drop-bottom.
2. preparation method according to claim 1 is characterized in that the purity of described Si powder is >=95wt%, and granularity is less than 0.1mm.
3. preparation method according to claim 1 is characterized in that the purity of described SiC powder is >=90wt%, and granularity is less than 5mm.
4. preparation method according to claim 1 is characterized in that described Y 2O 3Purity>=95wt%, Al 2O 3Purity>=95wt%; Y 2O 3Or Al 2O 3Granularity less than 0.01mm.
5. preparation method according to claim 1 is characterized in that described forming method is ramming process or vibratory compaction.
6. the ring furnace for preparing according to the described preparation method of each claim in the claim 1 ~ 5 is used SiC-Si 3N 4Matter pyroceramic drop-bottom.
CN201210295924XA 2012-08-17 2012-08-17 SiC-Si3N4 high temperature ceramic furnace bottom plate for annular furnace and preparation method thereof Pending CN102795859A (en)

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Cited By (15)

* Cited by examiner, † Cited by third party
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CN103232245A (en) * 2013-02-16 2013-08-07 东北大学 Method for preparing silicon nitride compound silicon carbide ceramic from crystalline silicon cutting waste materials
CN103641484A (en) * 2013-12-16 2014-03-19 武汉科技大学 Method for preparing Si3N4/SiC composite ceramic powder from biomass power plant ash
CN103896593A (en) * 2014-03-05 2014-07-02 武汉科技大学 Silicon nitride combined silicon carbide complex-phase high-temperature-resistant material and preparation method thereof
CN104150940A (en) * 2013-05-14 2014-11-19 中国科学院上海硅酸盐研究所 Silicon nitride/silicon carbide complex phase porous ceramic and preparation method thereof
CN104150910A (en) * 2013-05-14 2014-11-19 中国科学院上海硅酸盐研究所 Method for preparing silicon nitride and silicon carbide complex phase porous ceramic by virtue of polycrystalline Si cutting wastes
CN104311102A (en) * 2014-10-22 2015-01-28 山东理工大学 Preparation method of silicon nitride and silicon carbide combined lanthanum hexaboride foamed ceramic
CN104311101A (en) * 2014-10-22 2015-01-28 山东理工大学 Preparation method of silicon nitride and silicon carbide combined tantalum boride foamed ceramic
CN104311133A (en) * 2014-10-22 2015-01-28 山东理工大学 Preparation method of silicon nitride, silicon carbide combined molybdenum boride foamed ceramics
CN104311103A (en) * 2014-10-22 2015-01-28 山东理工大学 Preparation method of silicon nitride and silicon carbide combined tungsten bloride foamed ceramic
CN106083055A (en) * 2016-06-08 2016-11-09 武汉钢铁股份有限公司 A kind of annular furnace Si N Al C complex fire resistant ceramics furnace base plate and preparation method
CN106083076A (en) * 2016-06-08 2016-11-09 武汉钢铁股份有限公司 A kind of annular furnace drop-bottom Si SiC complex fire resistant is ceramic and prepares drop-bottom method
CN108585917A (en) * 2018-05-08 2018-09-28 中国人民解放军国防科技大学 Preparation method of silicon nitride-silicon carbide complex phase porous ceramic
CN110964228A (en) * 2019-11-25 2020-04-07 西北工业大学 Silicon carbide-boron nitride nanosheet heterogeneous filler and preparation method thereof, and epoxy resin heat-conducting composite material and preparation method thereof
CN111892410A (en) * 2020-08-04 2020-11-06 山东嘉和耐火材料有限责任公司 Preparation process and equipment of novel low-creep inorganic nonmetal new material
CN115894038A (en) * 2022-12-30 2023-04-04 山东中鹏特种陶瓷有限公司 Manufacturing process of large-size silicon carbide sand mill lining

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Cited By (22)

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Publication number Priority date Publication date Assignee Title
CN103232245A (en) * 2013-02-16 2013-08-07 东北大学 Method for preparing silicon nitride compound silicon carbide ceramic from crystalline silicon cutting waste materials
CN104150940B (en) * 2013-05-14 2015-10-28 中国科学院上海硅酸盐研究所 Silicon nitride and silicon carbide complex phase porous ceramics and preparation method thereof
CN104150940A (en) * 2013-05-14 2014-11-19 中国科学院上海硅酸盐研究所 Silicon nitride/silicon carbide complex phase porous ceramic and preparation method thereof
CN104150910A (en) * 2013-05-14 2014-11-19 中国科学院上海硅酸盐研究所 Method for preparing silicon nitride and silicon carbide complex phase porous ceramic by virtue of polycrystalline Si cutting wastes
CN104150910B (en) * 2013-05-14 2016-03-23 中国科学院上海硅酸盐研究所 Polycrystalline Si cutting waste material is utilized to prepare the method for silicon nitride and silicon carbide complex phase porous ceramics
CN103641484A (en) * 2013-12-16 2014-03-19 武汉科技大学 Method for preparing Si3N4/SiC composite ceramic powder from biomass power plant ash
CN103896593A (en) * 2014-03-05 2014-07-02 武汉科技大学 Silicon nitride combined silicon carbide complex-phase high-temperature-resistant material and preparation method thereof
CN104311103B (en) * 2014-10-22 2016-02-24 山东理工大学 A kind of silicon nitride, silicon carbide are in conjunction with the preparation method of boronation two tungsten foamed ceramics
CN104311102B (en) * 2014-10-22 2016-04-20 山东理工大学 A kind of silicon nitride, silicon carbide are in conjunction with the preparation method of lanthanum hexaborane foamed ceramics
CN104311133A (en) * 2014-10-22 2015-01-28 山东理工大学 Preparation method of silicon nitride, silicon carbide combined molybdenum boride foamed ceramics
CN104311101A (en) * 2014-10-22 2015-01-28 山东理工大学 Preparation method of silicon nitride and silicon carbide combined tantalum boride foamed ceramic
CN104311133B (en) * 2014-10-22 2016-02-24 山东理工大学 A kind of silicon nitride, silicon carbide are in conjunction with the preparation method of boronation two molybdenum foamed ceramics
CN104311101B (en) * 2014-10-22 2016-02-24 山东理工大学 A kind of silicon nitride, silicon carbide are in conjunction with the preparation method of tantalum boride foamed ceramics
CN104311102A (en) * 2014-10-22 2015-01-28 山东理工大学 Preparation method of silicon nitride and silicon carbide combined lanthanum hexaboride foamed ceramic
CN104311103A (en) * 2014-10-22 2015-01-28 山东理工大学 Preparation method of silicon nitride and silicon carbide combined tungsten bloride foamed ceramic
CN106083055A (en) * 2016-06-08 2016-11-09 武汉钢铁股份有限公司 A kind of annular furnace Si N Al C complex fire resistant ceramics furnace base plate and preparation method
CN106083076A (en) * 2016-06-08 2016-11-09 武汉钢铁股份有限公司 A kind of annular furnace drop-bottom Si SiC complex fire resistant is ceramic and prepares drop-bottom method
CN108585917A (en) * 2018-05-08 2018-09-28 中国人民解放军国防科技大学 Preparation method of silicon nitride-silicon carbide complex phase porous ceramic
CN108585917B (en) * 2018-05-08 2020-06-26 中国人民解放军国防科技大学 Preparation method of silicon nitride-silicon carbide complex phase porous ceramic
CN110964228A (en) * 2019-11-25 2020-04-07 西北工业大学 Silicon carbide-boron nitride nanosheet heterogeneous filler and preparation method thereof, and epoxy resin heat-conducting composite material and preparation method thereof
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Application publication date: 20121128