CN116102355B - Carbon crucible with small thermal expansion coefficient and preparation method thereof - Google Patents
Carbon crucible with small thermal expansion coefficient and preparation method thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 101
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 55
- 239000010439 graphite Substances 0.000 claims abstract description 55
- 239000002245 particle Substances 0.000 claims abstract description 36
- 239000002270 dispersing agent Substances 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000000725 suspension Substances 0.000 claims abstract description 23
- 239000011230 binding agent Substances 0.000 claims abstract description 21
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 239000004927 clay Substances 0.000 claims abstract description 14
- 229920002401 polyacrylamide Polymers 0.000 claims abstract description 12
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 12
- -1 carbonaceous Substances 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims description 59
- 238000003756 stirring Methods 0.000 claims description 31
- 239000002002 slurry Substances 0.000 claims description 30
- 238000005245 sintering Methods 0.000 claims description 27
- 239000011248 coating agent Substances 0.000 claims description 26
- 238000000576 coating method Methods 0.000 claims description 26
- 239000010426 asphalt Substances 0.000 claims description 9
- 239000012153 distilled water Substances 0.000 claims description 9
- 238000009766 low-temperature sintering Methods 0.000 claims description 9
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 5
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 5
- 150000002148 esters Chemical class 0.000 claims description 5
- 239000000194 fatty acid Substances 0.000 claims description 5
- 229930195729 fatty acid Natural products 0.000 claims description 5
- 150000004665 fatty acids Chemical class 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000004513 sizing Methods 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 10
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 abstract description 7
- 239000007787 solid Substances 0.000 abstract description 7
- 239000002184 metal Substances 0.000 abstract description 5
- 229910052751 metal Inorganic materials 0.000 abstract description 5
- 239000006185 dispersion Substances 0.000 abstract description 4
- 239000007791 liquid phase Substances 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 238000009736 wetting Methods 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 239000011269 tar Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 89
- 239000000203 mixture Substances 0.000 description 15
- 239000007962 solid dispersion Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- 230000006872 improvement Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 230000003064 anti-oxidating effect Effects 0.000 description 3
- 239000002689 soil Substances 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000007767 bonding agent Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 229910001369 Brass Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- CNLWCVNCHLKFHK-UHFFFAOYSA-N aluminum;lithium;dioxido(oxo)silane Chemical compound [Li+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O CNLWCVNCHLKFHK-UHFFFAOYSA-N 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000010951 brass Substances 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910052570 clay Inorganic materials 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010433 feldspar Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910052642 spodumene Inorganic materials 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 235000012222 talc Nutrition 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- 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
- C04B35/52—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 carbon, e.g. graphite
- C04B35/522—Graphite
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- 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
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/349—Clays, e.g. bentonites, smectites such as montmorillonite, vermiculites or kaolines, e.g. illite, talc or sepiolite
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- 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
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3817—Carbides
- C04B2235/3826—Silicon carbides
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- 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
- C04B2235/422—Carbon
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
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- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Mold Materials And Core Materials (AREA)
- Crucibles And Fluidized-Bed Furnaces (AREA)
Abstract
The invention relates to the technical field of graphite crucibles, in particular to a carbon crucible with a small thermal expansion coefficient and a preparation method thereof. The preparation method comprises the following raw materials: natural crystalline flake graphite, carbonaceous, clay, silicon carbide, tar, dispersant and binder. According to the invention, the dispersing agent and the binder are added to help increase the wettability of graphite particles and dissociate aggregates, ensure uniform mixing of the components, bond the components to form the components and have certain mechanical strength, the carboxyl in a polyacrylamide molecular chain can reduce the surface tension, help the wetting of water to solids, fully wet and uniformly disperse the solid dispersed particles in suspension by liquid phase, and improve the hydrophobicity of the polycrystalline graphite, so that the uniform dispersion of the polycrystalline graphite is facilitated to form a compact oxidation-resistant film, the problem that a crucible is oxidized can be avoided, and the polycrystalline graphite has a lower thermal expansion coefficient than metal and higher chemical stability, thereby being beneficial to reducing the thermal expansion coefficient of the crucible.
Description
Technical Field
The invention relates to the technical field of graphite crucibles, in particular to a carbon crucible with a small thermal expansion coefficient and a preparation method thereof.
Background
The carbon crucible is a kind of crucible which is made up by using graphite, clay, silica and wax stone as raw materials and is also called graphite crucible, and is mainly used for smelting non-ferrous metals of red copper, brass, gold, silver, zinc and lead, etc. and its alloy, and is applicable to casting formation of various moulds.
The high-performance low-expansion crucible as described in CN106083017B and the preparation method thereof are composed of a crucible base material and a crucible coating material, wherein the crucible base material comprises the following components in percentage by mass: 40-60% of leaf feldspar, 5-15% of spodumene, 5-15% of Suzhou soil, 1-3% of wood-saving soil, 1-5% of black talcum, 10-25% of Guizhou soil, 0-3% of white carbon black and 5-10% of zirconia micropowder, wherein the crucible coating material comprises the following components: the preparation method comprises the steps of mixing ingredients, ball milling, sieving, press filtration and dehydration, vacuum pugging, forming and drying to obtain a crucible blank, spraying a crucible coating material on the inner surface of a crucible base body, and finally sintering to obtain a crucible product, wherein the preparation method mainly comprises the steps of adding a high-performance low-expansion material to prepare a coating, coating the inner surface of the crucible blank, and carrying out smelting on the crucible, wherein the coating is worn at high temperature to influence the low expansion performance of the crucible.
Disclosure of Invention
The invention aims to provide a carbon crucible with a small thermal expansion coefficient and a preparation method thereof, so as to solve the problems in the background technology.
In order to achieve the above object, in one aspect, the present invention provides a carbon crucible having a small thermal expansion coefficient, comprising the following raw materials in parts by weight: 40-60 parts by weight of natural crystalline flake graphite, 5-12 parts by weight of carbon, 8-18 parts by weight of clay, 3-9 parts by weight of silicon carbide, 2-6 parts by weight of tar, 1-3 parts by weight of dispersing agent and 2-7 parts by weight of binder.
As a further improvement of the technical scheme, the dispersing agent comprises polyacrylamide and fatty acid polyoxyethylene ester.
As a further improvement of the present technical solution, the binder includes pitch and polycrystalline graphite.
On the other hand, the invention also provides a preparation method for preparing the carbon crucible with small thermal expansion coefficient, which comprises the following steps:
s1, taking natural crystalline flake graphite and carbon, crushing into particles, adding tar and distilled water, and stirring to generate suspension;
s2, preheating the suspension, adding a dispersing agent and clay, stirring, adding the mixture into a crucible mold, and heating to mold a blank;
s3, adding silicon carbide and a binder into the container, adding water, mixing and stirring to form slurry, and coating the slurry on the surface of the blank;
s4, sintering the blank at a high temperature after sintering the blank at a low temperature until the blank is solidified to form the crucible.
As a further improvement of the technical scheme, in the step S1, the size of particles formed after crushing is 32-80 meshes.
As a further improvement of the technical scheme, in the step S2, the stirring rotation speed is 15-30rpm/min.
As a further improvement of the technical scheme, in the step S3, the coating thickness of the slurry on the surface of the blank is 1-4mm.
As a further improvement of the technical scheme, in S4, the low-temperature sintering includes a pre-heating stage and a low-temperature dewatering stage, wherein the heating temperature in the pre-heating stage is 150-280 ℃, and the heating temperature in the low-temperature dewatering stage is 350-550 ℃.
As a further improvement of the technical scheme, in the step S4, the high-temperature sintering comprises a medium-temperature stage and a high-temperature stage, wherein the heating temperature in the medium-temperature stage is 600-800 ℃, and the heating temperature in the high-temperature stage is 900-1200 ℃.
According to the invention, the dispersing agent is added to help increase the wettability of graphite particles and dissociate aggregates, so that uniform mixing of all components is ensured, carboxyl groups are contained in a polyacrylamide molecular chain, the effect of reducing surface tension is realized, the wetting of water to solids is facilitated, solid dispersion particles in suspension are fully wetted and uniformly dispersed by liquid phase, the fatty acid polyoxyethylene ester serving as a nonionic dispersing agent can assist the polyacrylamide to wet the solid dispersion particles, the full mixing of all components is ensured, all components can be bonded by adding a bonding agent to form the solid dispersion particles and have certain mechanical strength, asphalt can bond the solid dispersion particles, all layers are bonded into a whole, and the polycrystalline graphite can bond natural crystalline flake graphite under the bonding effect of asphalt, wherein the hydrophobicity of the polycrystalline graphite can be improved under the effect of the carboxyl groups of the polyacrylamide, so that the uniform dispersion of the polycrystalline graphite is facilitated to form a compact anti-oxidation film, the problem that the crucible is oxidized can be avoided, and the thermal expansion coefficient of the polycrystalline graphite is lower than that of metal, the chemical stability is higher, and the thermal expansion coefficient of the polycrystalline graphite is facilitated to be reduced.
Compared with the prior art, the invention has the beneficial effects that:
according to the carbon crucible with the small thermal expansion coefficient and the preparation method thereof, the dispersing agent and the binder are added to help increase the wettability of graphite particles and dissociate aggregates, so that uniform mixing of the components is ensured, the components are bonded to form the carbon crucible with certain mechanical strength, the surface tension of carboxyl groups in a polyacrylamide molecular chain can be reduced, the wetting of water to solids is facilitated, the solid dispersion particles in suspension can be fully wetted and uniformly dispersed by liquid phase, and the polycrystalline graphite can be bonded with natural crystalline flake graphite under the cementing effect of asphalt, wherein the hydrophobicity of the polycrystalline graphite can be improved under the action of carboxyl groups of polyacrylamide, so that the uniform dispersion of the polycrystalline graphite is facilitated to form a compact anti-oxidation film, the problem that the crucible is oxidized can be avoided, and the thermal expansion coefficient of the polycrystalline graphite is lower than that of metal, so that the chemical stability is higher, and the thermal expansion coefficient of the crucible is facilitated to be reduced.
Drawings
FIG. 1 is a flow chart of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
On one hand, the invention provides a carbon crucible with a small thermal expansion coefficient and a preparation method thereof, and the carbon crucible comprises the following raw materials in parts by weight: 40-60 parts by weight of natural crystalline flake graphite, 5-12 parts by weight of carbon, 8-18 parts by weight of clay, 3-9 parts by weight of silicon carbide, 2-6 parts by weight of tar, 1-3 parts by weight of dispersing agent and 2-7 parts by weight of binder.
In the invention, the dispersing agent comprises polyacrylamide and fatty acid polyoxyethylene ester, and the dispersing agent is added to help increase the wettability of graphite particles and dissociate aggregates, so that the components are uniformly mixed.
Further, the binder comprises asphalt and polycrystalline graphite, the components can be bonded by adding the binder to form the composite material and the composite material has certain mechanical strength, the asphalt can bond the solid dispersed particles and bond all layers into a whole, and the polycrystalline graphite can bond the natural crystalline flake graphite under the bonding action of the asphalt.
According to the invention, the dispersing agent is added to help increase the wettability of graphite particles and dissociate aggregates, so that uniform mixing of all components is ensured, carboxyl groups are contained in a polyacrylamide molecular chain, the effect of reducing surface tension is realized, the wetting of water to solids is facilitated, solid dispersion particles in suspension are fully wetted and uniformly dispersed by liquid phase, the fatty acid polyoxyethylene ester serving as a nonionic dispersing agent can assist the polyacrylamide to wet the solid dispersion particles, the full mixing of all components is ensured, all components can be bonded by adding a bonding agent to form the solid dispersion particles and have certain mechanical strength, asphalt can bond the solid dispersion particles, all layers are bonded into a whole, and the polycrystalline graphite can bond natural crystalline flake graphite under the bonding effect of asphalt, wherein the hydrophobicity of the polycrystalline graphite can be improved under the effect of the carboxyl groups of the polyacrylamide, so that the uniform dispersion of the polycrystalline graphite is facilitated to form a compact anti-oxidation film, the problem that the crucible is oxidized can be avoided, and the thermal expansion coefficient of the polycrystalline graphite is lower than that of metal, the chemical stability is higher, and the thermal expansion coefficient of the polycrystalline graphite is facilitated to be reduced.
Referring to fig. 1, in another aspect, the present invention further provides a method for preparing the carbon crucible with a small thermal expansion coefficient, which comprises the following specific steps:
s1, taking 40-60 parts by weight of natural crystalline flake graphite and 5-12 parts by weight of carbon, crushing the natural crystalline flake graphite and the carbon into particles with the particle size of 32-80 meshes, adding 2-6 parts by weight of tar and distilled water, stirring the mixture to generate suspension, and crushing the natural crystalline flake graphite and the carbon into particles with smaller particle size so as to facilitate full contact and mixing of materials and increase the contact area with the tar;
s2, preheating the suspension, adding 1-3 parts by weight of dispersing agent and 8-18 parts by weight of clay, stirring at a rotating speed of 15-30rpm/min, adding the mixture into a crucible mold, heating to mold a blank, and stirring to facilitate the dispersing agent and the clay to be fully mixed into the suspension, so that the dispersing agent can conveniently increase the wettability of solid ions, and the uniform mixing of all components is ensured;
s3, adding 3-9 parts by weight of silicon carbide and 2-7 parts by weight of binder into a container, adding water, mixing and stirring to form slurry, coating the slurry on the surface of a blank, wherein the coating thickness of the slurry on the surface of the blank is 1-4mm, and coating the slurry on the surface of the blank to enable the slurry to form a compact antioxidant film on the surface of the blank during subsequent high-temperature curing;
s4, sintering the blank at a low temperature until the blank is solidified to form a crucible, wherein the low-temperature sintering comprises a pre-heating stage and a low-temperature dewatering stage, the heating temperature in the pre-heating stage is 150-280 ℃, the heating temperature in the low-temperature dewatering stage is 350-550 ℃, in order to avoid cracks of the prepared crucible, the crucible is heated and dewatered in the pre-heating stage, residual moisture in the crucible is removed through the rising temperature in the low-temperature dewatering stage, the high-temperature sintering comprises a medium-temperature stage and a high-temperature stage, the heating temperature in the medium-temperature stage is 600-800 ℃, the heating temperature in the high-temperature stage is 900-1200 ℃, the graphite components and other components in the crucible are integrally connected and solidified as a whole and slurry coated on the surface of the blank is gradually melted to form a film to seal or cover the surface of the blank, and the blank is completely solidified and the slurry is completely melted to form an oxidation-resistant film of the sealed blank in the high-temperature stage, so that the hardening of the crucible is facilitated.
The carbon crucible with small thermal expansion coefficient prepared by the invention is further described by the following specific examples according to the differences of raw material consumption and process parameters in the preparation process.
Example 1
S1, taking 40 parts by weight of natural crystalline flake graphite and 5 parts by weight of carbon, crushing the natural crystalline flake graphite and the carbon into particles with the particle size of 32 meshes, adding 2 parts by weight of tar and distilled water, and stirring the mixture to generate suspension;
s2, preheating the suspension, adding 1 part by weight of dispersing agent and 8 parts by weight of clay, stirring at a rotating speed of 15rpm/min, and adding the mixture into a crucible mold to heat and mold a blank;
s3, adding 3 parts by weight of silicon carbide and 2 parts by weight of binder into the container, adding water, mixing and stirring to form slurry, and coating the slurry on the surface of the blank, wherein the coating thickness of the slurry on the surface of the blank is 1mm;
s4, sintering the blank at a low temperature, and sintering the blank at a high temperature until the blank is solidified to form a crucible, wherein the low temperature sintering comprises a pre-heating stage and a low temperature dewatering stage, the heating temperature in the pre-heating stage is 150 ℃, the heating temperature in the low temperature dewatering stage is 350 ℃, the high temperature sintering comprises a medium temperature stage and a high temperature stage, the heating temperature in the medium temperature stage is 600 ℃, and the heating temperature in the high temperature stage is 900 ℃.
Example 2
S1, taking 50 parts by weight of natural crystalline flake graphite and 8 parts by weight of carbon, crushing the natural crystalline flake graphite and the carbon into particles with 60 meshes, adding 4 parts by weight of tar and distilled water, and stirring the mixture to generate suspension;
s2, preheating the suspension, adding 2 parts by weight of dispersing agent and 13 parts by weight of clay, stirring at a rotating speed of 25rpm/min, and adding the mixture into a crucible mold to heat and mold a blank;
s3, adding 6 parts by weight of silicon carbide and 4 parts by weight of binder into the container, adding water, mixing and stirring to form slurry, and coating the slurry on the surface of the blank, wherein the coating thickness of the slurry on the surface of the blank is 3mm;
s4, sintering the blank at a low temperature, and sintering the blank at a high temperature until the blank is solidified to form a crucible, wherein the low temperature sintering comprises a pre-heating stage and a low temperature dewatering stage, the heating temperature in the pre-heating stage is 220 ℃, the heating temperature in the low temperature dewatering stage is 400 ℃, the high temperature sintering comprises a medium temperature stage and a high temperature stage, the heating temperature in the medium temperature stage is 700 ℃, and the heating temperature in the high temperature stage is 1100 ℃.
Example 3
S1, taking 60 parts by weight of natural crystalline flake graphite and 12 parts by weight of carbon, crushing the natural crystalline flake graphite and the carbon into particles with the particle size of 80 meshes, adding 6 parts by weight of tar and distilled water, and stirring the mixture to generate suspension;
s2, preheating the suspension, adding 3 parts by weight of dispersing agent and 18 parts by weight of clay, stirring at a rotating speed of 30rpm/min, and adding the mixture into a crucible mold to heat and mold a blank;
s3, adding 9 parts by weight of silicon carbide and 7 parts by weight of binder into the container, adding water, mixing and stirring to form slurry, and coating the slurry on the surface of the blank, wherein the coating thickness of the slurry on the surface of the blank is 4mm;
s4, sintering the blank at a low temperature, and sintering the blank at a high temperature until the blank is solidified to form a crucible, wherein the low temperature sintering comprises a pre-heating stage and a low temperature dewatering stage, the heating temperature in the pre-heating stage is 280 ℃, the heating temperature in the low temperature dewatering stage is 550 ℃, the high temperature sintering comprises a medium temperature stage and a high temperature stage, the heating temperature in the medium temperature stage is 800 ℃, and the heating temperature in the high temperature stage is 1200 ℃.
Example 4
S1, taking 48 parts by weight of natural crystalline flake graphite and 10 parts by weight of carbon, crushing the natural crystalline flake graphite and the carbon into particles with the particle size of 70 meshes, adding 2 parts by weight of tar and distilled water, and stirring the mixture to generate suspension;
s2, preheating the suspension, adding 1 part by weight of dispersing agent and 10 parts by weight of clay, stirring at a rotating speed of 25rpm/min, and adding the mixture into a crucible mold to heat and mold a blank;
s3, adding 8 parts by weight of silicon carbide and 4 parts by weight of binder into the container, adding water, mixing and stirring to form slurry, and coating the slurry on the surface of the blank, wherein the coating thickness of the slurry on the surface of the blank is 2mm;
s4, sintering the blank at a low temperature, and sintering the blank at a high temperature until the blank is solidified to form a crucible, wherein the low temperature sintering comprises a pre-heating stage and a low temperature dewatering stage, the heating temperature in the pre-heating stage is 200 ℃, the heating temperature in the low temperature dewatering stage is 500 ℃, the high temperature sintering comprises a medium temperature stage and a high temperature stage, the heating temperature in the medium temperature stage is 700 ℃, and the heating temperature in the high temperature stage is 1000 ℃.
Table 1 comparison of the amounts of the respective raw materials in examples 1 to 4
Table 2 comparative process parameters in examples 1-4
Comparative example 1
The comparative example adopts the preparation method of example 1, only lacks dispersing agent, and the rest is unchanged, and the specific steps are as follows:
s1, taking 40 parts by weight of natural crystalline flake graphite and 5 parts by weight of carbon, crushing the natural crystalline flake graphite and the carbon into particles with the particle size of 32 meshes, adding 2 parts by weight of tar and distilled water, and stirring the mixture to generate suspension;
s2, preheating the suspension, adding 8 parts by weight of clay, stirring at a rotating speed of 15rpm/min, and adding the mixture into a crucible mold to heat and mold a blank;
s3, adding 3 parts by weight of silicon carbide and 2 parts by weight of binder into the container, adding water, mixing and stirring to form slurry, and coating the slurry on the surface of the blank, wherein the coating thickness of the slurry on the surface of the blank is 1mm;
s4, sintering the blank at a low temperature, and sintering the blank at a high temperature until the blank is solidified to form a crucible, wherein the low temperature sintering comprises a pre-heating stage and a low temperature dewatering stage, the heating temperature in the pre-heating stage is 150 ℃, the heating temperature in the low temperature dewatering stage is 350 ℃, the high temperature sintering comprises a medium temperature stage and a high temperature stage, the heating temperature in the medium temperature stage is 600 ℃, and the heating temperature in the high temperature stage is 900 ℃.
Comparative example 2
The comparative example adopts the preparation method of example 2, only lacks dispersing agent, and the rest is unchanged, and the specific steps are similar to those of comparative example 1, and the comparative example is not repeated.
Comparative example 3
The comparative example adopts the preparation method of example 3, only lacks dispersing agent, and the rest is unchanged, and the specific steps are similar to those of comparative example 1, and the comparative example is not repeated.
Comparative example 4
The comparative example adopts the preparation method of example 4, only lacks dispersing agent, and the rest is unchanged, and the specific steps are similar to those of comparative example 1, and the comparative example is not repeated.
Table 3 comparison of the amounts of the respective raw materials in comparative examples 1 to 4
Comparative example 5
The comparative example uses the preparation method of example 1, only lacks the binder, and the rest is unchanged, and the specific steps are as follows:
s1, taking 40 parts by weight of natural crystalline flake graphite and 5 parts by weight of carbon, crushing the natural crystalline flake graphite and the carbon into particles with the particle size of 32 meshes, adding 2 parts by weight of tar and distilled water, and stirring the mixture to generate suspension;
s2, preheating the suspension, adding 1 part by weight of dispersing agent and 8 parts by weight of clay, stirring at a rotating speed of 15rpm/min, and adding the mixture into a crucible mold to heat and mold a blank;
s3, adding 3 parts by weight of silicon carbide into the container, adding water, mixing and stirring to form slurry, and coating the slurry on the surface of the blank, wherein the coating thickness of the slurry on the surface of the blank is 1mm;
s4, sintering the blank at a low temperature, and sintering the blank at a high temperature until the blank is solidified to form a crucible, wherein the low temperature sintering comprises a pre-heating stage and a low temperature dewatering stage, the heating temperature in the pre-heating stage is 150 ℃, the heating temperature in the low temperature dewatering stage is 350 ℃, the high temperature sintering comprises a medium temperature stage and a high temperature stage, the heating temperature in the medium temperature stage is 600 ℃, and the heating temperature in the high temperature stage is 900 ℃.
Comparative example 6
The comparative example adopts the preparation method of example 2, only lacks the binder, and the rest is unchanged, and the specific steps are similar to those of comparative example 5, and the comparative example is not repeated.
Comparative example 7
The comparative example adopts the preparation method of example 3, only lacks the binder, and the rest is unchanged, and the specific steps are similar to those of comparative example 5, and the comparative example is not repeated.
Comparative example 8
The comparative example adopts the preparation method of example 4, only lacks the binder, and the rest is unchanged, and the specific steps are similar to those of comparative example 5, and the comparative example is not repeated.
Table 4 comparison of the amounts of the respective raw materials in comparative examples 5 to 8
Table 5 comparative process parameters in comparative examples 1-8
Comparative example 9
The comparative example was similar to comparative example 1 in specific procedure except that the particle size was set to 25 mesh based on comparative example 1, and the details of the comparative example were not repeated.
Comparative example 10
The stirring rotation speed is set to be 50rpm/min on the basis of comparative example 2, the rest is unchanged, the specific steps are similar to those of comparative example 2, and the comparative example is not repeated.
Comparative example 11
The comparative example was set to 5mm in coating thickness based on comparative example 3, the rest was unchanged, and specific steps were similar to comparative example 3, and the comparative example will not be repeated.
Comparative example 12
The comparative example is based on comparative example 4, the pre-heating temperature is set to 300 ℃, the rest is unchanged, the specific steps are similar to comparative example 4, and the comparative example is not repeated.
Comparative example 13
The comparative example is based on comparative example 5, the low-temperature water removal temperature is set to 320 ℃, the rest is unchanged, the specific steps are similar to those of comparative example 5, and the comparative example is not repeated.
Comparative example 14
The comparative example is based on comparative example 6, the medium temperature is set to 850 ℃, the rest is unchanged, the specific steps are similar to those of comparative example 6, and the comparative example is not repeated.
Comparative example 15
The comparative example is based on comparative example 7, the high temperature is set to 1400 ℃, the rest is unchanged, the specific steps are similar to comparative example 7, and the comparative example is not repeated.
Table 6 comparison of the amounts of the respective raw materials in comparative examples 9 to 15
Table 7 comparative Process parameter comparison in comparative examples 9-15
Test examples
Carbon crucibles were prepared according to the preparation method of a carbon crucible having a small thermal expansion coefficient provided in examples 1 to 4 and comparative examples 1 to 15, respectively, and the thermal expansion coefficients of the carbon crucibles were measured according to GB/T16535-1996 test method for thermal expansion coefficient of engineering ceramic wire, and the measured data were filled in Table 8.
Table 8 comparison of thermal expansion coefficients of carbon crucibles prepared in examples and comparative examples
| Coefficient of thermal expansion/(. Times.10) -6 /℃) | |
| Example 1 | 1.14 |
| Example 2 | 1.09 |
| Example 3 | 1.17 |
| Example 4 | 1.15 |
| Comparative example 1 | 1.25 |
| Comparative example 2 | 1.21 |
| Comparative example 3 | 1.31 |
| Comparative example 4 | 1.27 |
| Comparative example 5 | 1.27 |
| Comparative example 6 | 1.24 |
| Comparative example 7 | 1.34 |
| Comparative example 8 | 1.30 |
| Comparative example 9 | 1.26 |
| Comparative example 10 | 1.23 |
| Comparative example 11 | 1.32 |
| Comparative example 12 | 1.29 |
| Comparative example 13 | 1.28 |
| Comparative example 14 | 1.25 |
| Comparative example 15 | 1.36 |
As can be seen from Table 8, the carbon crucibles prepared in examples 1 to 4 have a lower thermal expansion coefficient than the carbon crucibles prepared in comparative examples 1 to 15, and the carbon crucibles prepared in examples have a thermal expansion coefficient of less than 1.17X10 -6 The carbon crucible prepared by adopting the comparative examples of different raw material consumption and process parameters has higher thermal expansion coefficient, so the carbon crucible prepared by the invention has lower thermal expansion coefficient.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the above-described embodiments, and that the above-described embodiments and descriptions are only preferred embodiments of the present invention, and are not intended to limit the invention, and that various changes and modifications may be made therein without departing from the spirit and scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (4)
1. The preparation method of the carbon crucible with small thermal expansion coefficient is characterized by comprising the following steps:
s1, taking 40-60 parts by weight of natural crystalline flake graphite and 5-12 parts by weight of carbon, crushing into particles, adding 2-6 parts by weight of tar and distilled water, and stirring to generate suspension;
s2, preheating the suspension, adding 1-3 parts by weight of dispersing agent and 8-18 parts by weight of clay, stirring, adding into a crucible mold, and heating to mold a blank;
s3, adding 3-9 parts by weight of silicon carbide and 2-7 parts by weight of binder into the container, adding water, mixing and stirring to form slurry, and coating the slurry on the surface of the blank;
s4, sintering the blank at a high temperature after sintering the blank at a low temperature until the blank is solidified to form a crucible;
wherein the dispersing agent comprises polyacrylamide and fatty acid polyoxyethylene ester;
the binder comprises asphalt and polycrystalline graphite;
in the step S3, the coating thickness of the sizing agent on the surface of the blank is 1-4mm;
in the step S4, the low-temperature sintering comprises a pre-heating stage and a low-temperature water removal stage, wherein the heating temperature in the pre-heating stage is 150-280 ℃, and the heating temperature in the low-temperature water removal stage is 350-550 ℃;
in the step S4, the high-temperature sintering comprises a medium-temperature stage and a high-temperature stage, wherein the heating temperature in the medium-temperature stage is 600-800 ℃, and the heating temperature in the high-temperature stage is 900-1200 ℃.
2. The method for producing a carbon crucible having a small thermal expansion coefficient according to claim 1, wherein: in the step S1, the size of particles formed after crushing is 32-80 meshes.
3. The method for producing a carbon crucible having a small thermal expansion coefficient according to claim 1, wherein: in the step S2, the stirring rotation speed is 15-30rpm/min.
4. A carbon crucible having a small thermal expansion coefficient prepared by the preparation method according to any one of claims 1 to 3.
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