CN109336611A - A kind of pressureless sintering silicon carbide nozzle and preparation method thereof - Google Patents
A kind of pressureless sintering silicon carbide nozzle and preparation method thereof Download PDFInfo
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- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—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
- C04B35/62605—Treating the starting powders individually or as mixtures
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- C04B35/626—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
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62695—Granulation or pelletising
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
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Abstract
The present invention relates to a kind of pressureless sintering silicon carbide nozzles and preparation method thereof, the bocca wall thickness is 3-10mm: bocca height is 150-800mm, is the raw material by following parts by weight through isostatic pressing, pressureless sintering forms, 80-150 parts of silicon carbide micro-powder, 0.5-4 parts of boron carbide micro powder, 2-12 parts of high-purity carbon black, 5-20 parts of phenolic resin, 0.6-5 parts of graphite, analyze pure ammonium hydroxide 9-20 parts, 0.2-5 parts of tributyl phosphate, 45-80 parts of deionized water.Bocca bulk density produced by the present invention is 3.02~3.12g/cm3, vickers microhardness > 25GPa, fracture toughness > 4.5MPam1/2.Based on without pressure pelletizing, solve that blank cracking, product wall unevenness is even, density is low, drying deformation quantity is big in conjunction with equal pressing equipment, it is difficult to the problem of mass production.
Description
Technical field
The present invention relates to a kind of pressureless sintering silicon carbide nozzles and preparation method thereof, belong to Industrial Stoves temperature-resistant material technology
Field.
Background technique
Silicon carbide burner nozzle is the ideal flame kiln furnitures of tunnel oven, shuttle kiln, roller kilns, and it is straight to be also applied to open fire
In the Industrial Stoves for connecing heating and radiant tube indirect heating system.
Domestic silicon carbide burner nozzle is generally adopted by silicon carbide reaction-sintered bocca, blank molding mode be slip casting at
Type.For pressureless sintering bocca, temperature tolerance, thermal shock resistance, resists corrosion resistance silicon carbide reaction-sintered bocca
It is lower for pressureless sintering bocca in oxidation susceptibility, consistency.
Summary of the invention
In view of the deficiencies of the prior art, in order to solve existing silicon carbide reaction-sintered bocca heatproof, consistency, anti-thermal shock
Performance, corrosion-resistant, antioxygenic property deficiency, the present invention provide a kind of pressureless sintering silicon carbide nozzle and preparation method thereof.
Technical scheme is as follows:
A kind of pressureless sintering silicon carbide nozzle, the bocca wall thickness are 3-10mm: bocca height is 150-800mm,
It is the raw material by following parts by weight through isostatic pressing, pressureless sintering forms, and 80-150 parts of silicon carbide micro-powder, boron carbide micro powder 0.5-
4 parts, 2-12 parts of high-purity carbon black, 5-20 parts of phenolic resin, 0.6-5 parts of graphite, pure ammonium hydroxide 9-20 parts are analyzed, tributyl phosphate 0.2-
5 parts, 45-80 parts of deionized water.
Preferred according to the present invention, the silicon carbide micro-powder average grain diameter is 0.45 μm, purity >=98.5%.
Preferred according to the present invention, the boron carbide micro powder average grain diameter is 1.5-3.5 μm, purity >=93.5%.
Preferred according to the present invention, the high-purity carbon black average grain diameter is 1-3 μm, purity >=92%.
Preferred according to the present invention, the graphite average grain diameter is 4-6 μm, purity >=93%.
It is preferred according to the present invention, the viscosity 700-1200mpa.s of the phenolic resin, remaining carbon >=40%.
Preferred according to the present invention, a kind of pressureless sintering silicon carbide nozzle is the raw material by following parts by weight through waiting static pressure
System, pressureless sintering form:
100 parts of silicon carbide micro-powder, 0.5-2 parts of boron carbide micro powder, 2-8 parts of high-purity carbon black, 5-16 parts of phenolic resin, graphite
0.6-3 parts, analyze pure ammonium hydroxide 9-12 parts, 0.2-1 parts of tributyl phosphate, 45-60 parts of deionized water.
Bocca thickness 3-10mm of the invention;Length and width dimensions select die size as needed, it can be achieved that long 150-
The silicon carbide burner nozzle product preparation of 800mm, diameter 20-300mm.
Silicon carbide micro-powder used in the present invention, boron carbide micro powder, phenolic resin, high-purity carbon black, graphite can be in market institute energy
The technical grade raw material of purchase.
A kind of preparation method of pressureless sintering silicon carbide nozzle, comprises the following steps that
(1) ceramic slurry is prepared
Deionized water is weighed according to the ratio, phenolic resin ball milling is sufficiently mixed 6-10 hours, then it is added boron carbide, graphite,
High-purity carbon black, ball milling are sufficiently mixed 6-10 hours, and silicon carbide micro-powder, ammonium hydroxide is added, and tributyl phosphate ball milling is sufficiently mixed 18-24
Pulp after hour;Obtain ceramic slurry;
(2) mist projection granulating
Ceramic slurry made from step (1) is added in agitator tank, by spray drying tower at 280 DEG C of inlet temperature, out
110 DEG C of temperature of mouth, atomization frequency are 34 hertz, and material pump frequency is 39 hertz, and tower body negative pressure is 130 megapascal, the grain composition of system
2%, 60-80 mesh is accounted for for 40-50 mesh accounting for 20%, 80-200 mesh and account for 78%, particle surface is mellow and full, and imperforate granular powder;
(3) powder loads
The common abrasive rubber set of wall thickness 3-15mm is fixed on alloy core model, by granular powder made from step (2)
It is even to be filled between rubber sleeve and core model, finally feeding port is sealed with rubber block;
(4) static pressure suppressions such as
It is put into the mold after step (3) filling powder obtained in equal static pressure cylinders body, the static pressure suppressions such as carries out, obtain hair
Base,
(5) it dries
Blank is made in step (4) to dry;
(6) vehicle base
Blank after step (5) drying is cut away into the irregular part in end on the lathe that revolving speed is 300-600n/min,
Obtain silicon carbide green body;
(7) it is sintered
Silicon carbide green body is placed in graphite vacuum high temperature furnace, under protective atmosphere, 1- is sintered at a temperature of 2100-2200 DEG C
3 hours, densification pressureless sintering silicon carbide nozzle is made.
Gained bocca thickness 3-10mm produced by the present invention;The carbonization of long 150-800mm, diameter 20-300mm can be achieved
Silicon bocca product, and be able to maintain and do not crack, deformation quantity it is small;Bulk density is 3.02~3.12g/cm3, vickers microhardness >
25GPa, fracture toughness > 4.5MPam1/2。
It is preferred according to the present invention, ceramic slurry is prepared in step (1), and phenolic resin matter is added before phenolic resin mixing
System is added after 80% deionized water agitation and dilution of amount.
Preferred according to the present invention, granular powder moisture content is 0.01%-0.3% in step (2).
Preferred according to the present invention, powder packed process described in step (3) needs mold to be placed on shock platforms vibration
Feeding port is sealed after compacting powder.
It is preferred according to the present invention, the static pressure suppressions such as described in step (4) specifically: 120 megapascal of press secondary pressurized is protected
The pressure time 5 minutes, pressure release to 80mpa, pressure maintaining 20 minutes, pressure release to 70mpa, pressure maintaining 10 minutes, pressure release 55mpa, pressure maintaining 5 seconds,
Depanning after natural pressure release to 0mpa.
Preferred according to the present invention, drying described in step (5) is dried to be put into the drying box that temperature is 140-160 DEG C
48 hours, drying box was the drying box with air blast function, and drying box is discharged in product moisture as far as possible.
It is preferred according to the present invention, in vehicle system described in step (6), needs to make nylon tooling according to blank, to the greatest extent may be used
It can be reduced vibration of the external stress to blank.
Preferred according to the present invention, vacuum sintering furnace described in step (7), calandria is generated heat using isostatic pressing formed graphite
Body, fever bulk resistor reach 50-70 ohm.Make thermal field the temperature difference range ± 2.5 degree as uniform as possible in furnace.
Beneficial effect
1, the present invention solves blank cracking, product wall unevenness in conjunction with equal pressing equipment based on without pressure pelletizing
It is even, density is low, drying deformation quantity is big, it is difficult to the problem of mass production.
2, the present invention uses ball milling material by wet type mixing, mist projection granulating production without powder compact, the powder porosity used in product≤
0.2%.
3, the present invention uses shock platforms powder filling method, makes the idiosome wall thickness homogeneity deviation ± 0.1mm suppressed.
4, the present invention uses isostatic pressing formed graphite heater, passes through test fever bulk resistor, assembling fever group.Make furnace body thermal field
Uniformly, the temperature difference range ± 2.5 degree.
Specific embodiment
Below with reference to embodiment, technical scheme is described further, but institute's protection scope of the present invention is not limited to
This.
The silicon carbide micro-powder average grain diameter is 0.45 μm, purity >=98.5%;The boron carbide micro powder average grain diameter is
1.5-3.5 μm, purity >=93.5%;Commercial products.
Embodiment 1:
A kind of pressureless sintering silicon carbide nozzle, the bocca wall thickness are 3-10mm: bocca height is 150-800mm,
It is the raw material by following parts by weight through isostatic pressing, pressureless sintering forms, and 100 parts of silicon carbide micro-powder, 0.5 part of boron carbide micro powder,
2 parts of high-purity carbon black, 5 parts of phenolic resin, 0.6 part of graphite, analyze 9 parts of pure ammonium hydroxide, 0.2 part of tributyl phosphate, 45 parts of deionized water.
Preparation method, steps are as follows:
1) ball milling mixing
Deionized water is weighed according to the ratio, and phenolic resin ball milling is sufficiently mixed 8 hours, and boron carbide is then added, and graphite is high-purity
Carbon black, ball milling are sufficiently mixed 12 hours, and silicon carbide micro-powder, ammonium hydroxide is added, and tributyl phosphate ball milling goes out after being sufficiently mixed 20 hours
Slurry.
2) mist projection granulating
Slurry made from step (1) is added in agitator tank, by spray drying tower at 280 degree of inlet temperature, outlet temperature
110 degree of degree is atomized 34 hertz of frequency, expects 39 hertz of pump frequency, 130 megapascal of tower body negative pressure, the grain composition of system is 40 mesh or more
2%, 60-80 mesh 20%, 80-200 mesh 78%, particle surface is mellow and full, and the granular powder that the porosity is low.
3) powder loads
The common abrasive rubber set of wall thickness 3-15mm is fixed on alloy core model.Pelletizing made from step (2) is even
It is filled between rubber sleeve and core model, finally seals feeding port with rubber block.
4) isostatic pressing
It by the mold after step (3) filling powder obtained, is put into and waits in static pressure cylinders body, pass through 120 megapascal pressure and suppress.
5) it dries
Blank is made 150 degree in baking oven in step (4), is dried 48 hours.
6) vehicle embryo
Blank cuts away the irregular part in end at center lathe revolving speed 300-600n/min after step (5) drying.
7) it is sintered
Step (6) is obtained in silicon carbide green body merging graphite vacuum high temperature furnace, under protective atmosphere, 2100-2200 DEG C
At a temperature of keep the temperature 1-3 hours, the static pressure suppressions pressureless sintering silicon carbide burner nozzle such as densification is made.
Through detecting, the bulk density of gained thyrite is 3.10g/cm3, vickers microhardness 26.7Gpa, break
Split toughness 5.57MPam1/2。
Embodiment 2:
A kind of pressureless sintering silicon carbide nozzle is the raw material by following parts by weight through isostatic pressing, and pressureless sintering forms,
It 100 parts of silicon carbide micro-powder, 2 parts of boron carbide micro powder, 8 parts of high-purity carbon black, 16 parts of phenolic resin, 3 parts of graphite, analyzes pure
12 parts of ammonium hydroxide, 1 part of tributyl phosphate, 60 parts of deionized water.
The preparation method is the same as that of Example 1.
Through detecting, the bulk density of gained thyrite is 3.12g/cm3, vickers microhardness 28.1Gpa, break
Split toughness 6.14MPam1/2。
Claims (9)
1. a kind of pressureless sintering silicon carbide nozzle, the bocca wall thickness is 3-10mm: bocca height is 150-800mm, is
By the raw material of following parts by weight through isostatic pressing, pressureless sintering is formed, and 80-150 parts of silicon carbide micro-powder, boron carbide micro powder 0.5-4
Part, 2-12 parts of high-purity carbon black, 5-20 parts of phenolic resin, 0.6-5 parts of graphite, pure ammonium hydroxide 9-20 parts are analyzed, tributyl phosphate 0.2-5
Part, 45-80 parts of deionized water.
2. pressureless sintering silicon carbide nozzle according to claim 1, which is characterized in that the silicon carbide micro-powder average grain diameter
It is 0.45 μm, purity >=98.5%, the boron carbide micro powder average grain diameter is 1.5-3.5 μm, and purity >=93.5% is described high-purity
Carbon black average grain diameter is 1-3 μm, purity >=92%, and the graphite average grain diameter is 4-6 μm, purity >=93%.
3. pressureless sintering silicon carbide nozzle according to claim 1, which is characterized in that the viscosity 700- of the phenolic resin
1200mpa.s, remaining carbon >=40%.
4. a kind of pressureless sintering silicon carbide nozzle is the raw material by following parts by weight through isostatic pressing, pressureless sintering is formed:
100 parts of silicon carbide micro-powder, 0.5-2 parts of boron carbide micro powder, 2-8 parts of high-purity carbon black, 5-16 parts of phenolic resin, graphite 0.6-3
Part, analyze pure ammonium hydroxide 9-12 parts, 0.2-1 parts of tributyl phosphate, 45-60 parts of deionized water.
5. a kind of preparation method of pressureless sintering silicon carbide nozzle, comprises the following steps that
(1) ceramic slurry is prepared
Deionized water is weighed according to the ratio, and phenolic resin ball milling is sufficiently mixed 6-10 hours, and boron carbide is then added, and graphite is high-purity
Carbon black, ball milling are sufficiently mixed 6-10 hours, and silicon carbide micro-powder, ammonium hydroxide is added, and tributyl phosphate ball milling is sufficiently mixed 18-24 hours
Pulp afterwards;Obtain ceramic slurry;
(2) mist projection granulating
Ceramic slurry made from step (1) is added in agitator tank, by spray drying tower at 280 DEG C of inlet temperature, outlet temperature
110 DEG C of degree, atomization frequency are 34 hertz, and material pump frequency is 39 hertz, and tower body negative pressure is 130 megapascal, and the grain composition of system is 40-
50 mesh, which account for 2%, 60-80 mesh and account for 20%, 80-200 mesh, accounts for 78%, and particle surface is mellow and full, and imperforate granular powder;
(3) powder loads
It is fixed on the common abrasive rubber set of wall thickness 3-15mm on alloy core model, fills out granular powder is even made from step (2)
It fills between rubber sleeve and core model, finally seals feeding port with rubber block;
(4) static pressure suppressions such as
It is put into the mold after step (3) filling powder obtained in equal static pressure cylinders body, the static pressure suppressions such as carries out, obtain blank,
(5) it dries
Blank is made in step (4) to dry;
(6) vehicle base
Blank after step (5) drying is cut away into the irregular part in end on the lathe that revolving speed is 300-600n/min, obtains carbon
SiClx green body;
(7) it is sintered
Silicon carbide green body is placed in graphite vacuum high temperature furnace, it is small that 1-3 is sintered under protective atmosphere, at a temperature of 2100-2200 DEG C
When, densification pressureless sintering silicon carbide nozzle is made.
6. preparation method according to claim 5, which is characterized in that granular powder moisture content is in step (2)
0.01%-0.3%.
7. preparation method according to claim 5, which is characterized in that the static pressure suppressions such as described in step (4) specifically: pressure
120 megapascal of machine secondary pressurized, the dwell time 5 minutes, pressure release to 80mpa, pressure maintaining 20 minutes, pressure release to 70mpa, pressure maintaining 10 divided
Clock, pressure release 55mpa, pressure maintaining 5 seconds, depanning after natural pressure release to 0mpa.
8. preparation method according to claim 5, which is characterized in that drying described in step (5) is to be put into temperature to be
It is dried 48 hours in 140-160 DEG C of drying box, drying box is the drying box with air blast function, and product moisture is discharged as far as possible
Drying box.
9. preparation method according to claim 5, which is characterized in that vacuum sintering furnace described in step (7), calandria
Using isostatic pressing formed graphite heater, bulk resistor of generating heat reaches 50-70 ohm.Make thermal field the temperature difference range as uniform as possible in furnace ±
2.5 degree.
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Cited By (1)
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CN116003135A (en) * | 2022-12-26 | 2023-04-25 | 何思义 | Preparation method of reaction sintering silicon carbide ceramic granulating powder |
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