CN114409403B - Graphite crucible - Google Patents
Graphite crucible Download PDFInfo
- Publication number
- CN114409403B CN114409403B CN202210145848.8A CN202210145848A CN114409403B CN 114409403 B CN114409403 B CN 114409403B CN 202210145848 A CN202210145848 A CN 202210145848A CN 114409403 B CN114409403 B CN 114409403B
- Authority
- CN
- China
- Prior art keywords
- resin
- heating
- crucible
- graphite crucible
- graphene
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
- B32B37/1207—Heat-activated adhesive
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
- B32B9/005—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile
- B32B9/007—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile comprising carbon, e.g. graphite, composite carbon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
- B32B9/04—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
-
- 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
- C04B35/528—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 obtained from carbonaceous particles with or without other non-organic components
- C04B35/532—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 obtained from carbonaceous particles with or without other non-organic components containing a carbonisable binder
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
- B32B37/1207—Heat-activated adhesive
- B32B2037/1215—Hot-melt adhesive
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2255/00—Coating on the layer surface
- B32B2255/26—Polymeric coating
Abstract
The invention discloses a graphite crucible, which is represented by the following percentage by mass: 50-60% of graphitized coke, 35-45% of asphalt and 5-15% of a coating layer, wherein the coating layer comprises resin and pyridine; manufacturing an inert coating net by using resin and pyridine, wherein the inert coating net is adhered to graphene through coating, the other side of the graphene is coated with the resin, and the graphene is adhered to the prepared graphite crucible through melting the resin to cover the whole graphite crucible; in the invention, nitrogen is uniformly stirred with the resin to be uniformly attached to the surface of the resin to form a reticular nitrogen net, so that the oxidation resistance of the surface of the resin is improved, and the amount of free carbon is reduced.
Description
Technical Field
The invention belongs to the technical field of graphite materials, and particularly relates to a graphite crucible.
Background
Graphite is a crystalline carbon, a non-metallic material, silver gray in color, soft in texture, and metallic in luster. The graphite has a very high melting point, and begins to soften at 3000 ℃ in vacuum and then begins to evaporate and sublimate at 3500 ℃. The strength of general material is gradually reduced at high temp., while the strength of graphite is about doubled when it is heated to 2000 deg.C rather than normal temp.. Graphite has a relatively high thermal and electrical conductivity, which is about 4 times higher than stainless steel, about 2 times higher than carbon steel, and about 100 times higher than general non-metals. The thermal conductivity of the graphite material is not only higher than that of metal materials such as steel, iron and lead, but also the thermal conductivity coefficient is reduced along with the increase of temperature, which is different from the common metal materials, and graphite even tends to be in a heat insulation state at extremely high temperature. Therefore, the heat insulating properties of graphite are very reliable under ultra-high temperature conditions. The graphite has good lubricity and plasticity, the friction coefficient of the graphite is less than 0.1, the graphite can be expanded into a breathable and light-transmitting sheet, and the hardness of the high-strength graphite is very high, so that the graphite is difficult to process by using a diamond cutter. The graphite has chemical stability, and can resist acid, alkali and organic solvent corrosion. Graphite has many excellent properties, so graphite is widely used in modern industry.
The graphite crucible can be classified into graphite-clay material, graphite-silicon carbide material, and artificial graphite material. The graphite-clay crucible is prepared by using natural crystalline flake graphite and clay as main components, and is only used when cast iron and cast steel are melted at high temperature and a small amount of noble metal and the like are melted at present. In 1955, for the first time, japan, kokusai, developed and produced a graphite silicon carbide crucible, which was mainly prepared from natural crystalline flake graphite, silicon carbide, and a binder as main components, and which was superior in durability to a graphite-clay crucible because of its excellent durability, and which was used in place of the graphite-clay crucible, and in which most of nonferrous metals such as copper alloys and aluminum alloys were melted. The artificial graphite crucible is a crucible processed by graphite electrode blank, and plays an irreplaceable role in the aspects of smelting or high-temperature treatment of industrial products with special requirements. However, at present, most of domestic artificial graphite crucibles are processed by electrodes broken off on an electric arc furnace or a resistivity furnace, and the crucibles have the common defects of large granularity, low strength, high thermal expansion coefficient, high conductivity, large ash content and the like. In the industries of neodymium, praseodymium and polycrystalline silicon, the following main problems generally exist when the existing artificial graphite crucible is adopted: the service performance is poor: in the using process, because the graphite crucible is poor in corrosion resistance and oxidation resistance and free carbon elements exist on the surface of the graphite crucible, the graphite crucible can react with metal steam to generate carbide in the process of smelting metal at high temperature, so that the crucible and a metal block are bonded.
Disclosure of Invention
The invention aims to provide a graphite crucible, wherein nitrogen is uniformly stirred with resin to be uniformly attached to the surface of the resin to form a net-shaped nitrogen net, so that the oxidation resistance of the surface of the resin is improved, and the amount of free carbon is reduced.
In order to achieve the purpose, the invention provides the following technical scheme: a graphite crucible, expressed in percentage by mass as: the graphite crucible coating method comprises the following steps of 50-60% of graphitized coke, 35-45% of asphalt and 5-15% of a coating layer, wherein the coating layer comprises resin and pyridine, an inert coating net is manufactured by utilizing the resin and the pyridine, the inert coating net is bonded to graphene through coating, the other side of the graphene is coated with the resin, and the graphene is bonded to a prepared graphite crucible through melting the resin, so that the whole graphite crucible is covered.
The surface of the existing graphite crucible is coated and bonded with an inert coating net which has the functions of oxidation resistance and free carbon element reduction, the inert coating net is mainly prepared by adding pyridine, the pyridine is gasified at the temperature of 500-700 ℃, a carbon-carbon single bond in the pyridine is decomposed to fully release the nitrogen element, and a gasified mixture consists of water, the nitrogen element and the carbon element, so that the nitrogen element obtained after distillation is uniformly stirred with resin, the nitrogen element is uniformly attached to the surface of the resin to form a net-shaped nitrogen net, the oxidation resistance of the surface of the resin is improved, meanwhile, the surface of the crucible is covered by the resin, and when being bonded, the resin is melted and simultaneously heated to 600-700 ℃, the free carbon element on the surface of the crucible can be cracked, the free carbon element on the surface of the crucible is removed, and the amount of the free carbon element on the surface of the crucible is reduced.
Preferably, the resin is one of polyethylene, polypropylene and the like, and the mass ratio of the resin to the pyridine is as follows: 2:1-1.5.
Adopt above-mentioned scheme: the mass ratio of the resin and the pyridine is optimized, and the load uniformity of the carbon element on the resin is further improved.
Preferably, the preparation of the graphite crucible comprises the following steps:
(1) preparing a graphite crucible, adding graphitized coke and asphalt according to the mass ratio, respectively screening the graphitized coke and the asphalt, kneading after screening, performing compression molding after kneading to form a semi-finished blank, further roasting to form a semi-finished roasted blank, and finally machining to form a crucible matrix;
(2) preparing an inert coating net, adding pyridine into a beaker according to the mass ratio, and adding a dispersing agent into the beaker, wherein the mass volume ratio of the pyridine to the dispersing agent is 2:9-15;
(3) mixing the collected distilled solution B with resin with corresponding mass after the prepared inert coating net is cooled to room temperature, and stirring at constant temperature of 50-70 ℃ for 2-3 h; obtaining a mixture C;
(4) pressing the graphene into a laminar object with the thickness of 1-1.5 mm;
(5) uniformly coating the mixture C prepared in the step (3) on one side surface of the graphene layer prepared in the step (4) at 50-70 ℃;
(6) and uniformly coating resin on the other side surface of the graphene, completely covering the coated graphene on the surface of the crucible substrate, and performing compression molding to complete the preparation.
Preferably, the thickness of the mixture C in the step (5) is 0.8 to 1mm.
Preferably, the specific steps of step (6) are as follows: heating and melting the surface of the graphene layer with the resin, wherein the heating temperature is 50-60 ℃, directly bonding the resin in a molten state to the outside of the crucible matrix, and further adopting mechanical pressing.
Adopt above-mentioned scheme: the combination degree of the graphene layer and the crucible is improved.
Preferably, the crucible matrix prepared in the step (1) is subjected to a high-temperature heating process, heated to 600-700 ℃ for 12-14h, and then cooled to room temperature for use.
Adopt above-mentioned scheme: when the graphene layer is adhered to the crucible, the free carbon elements on the surface of the crucible can be cracked simultaneously, and the amount of the free carbon elements is reduced.
Compared with the prior art, the invention has the beneficial effects that: the surface of the existing graphite crucible is coated and bonded with a layer of inert coating net which has the functions of resisting oxidation and reducing free carbon elements, the inert coating net is mainly prepared by adding pyridine, the pyridine is gasified at the temperature of 500-700 ℃, carbon-carbon single bonds in the pyridine are disintegrated to fully release nitrogen elements, and the gasified mixture consists of water, the nitrogen elements and the carbon elements, so that the nitrogen elements are uniformly stirred with resin to be uniformly attached to the surface of the resin to form a net-shaped nitrogen net, the oxidation resistance of the surface of the resin is improved, and the amount of the free carbon elements is reduced.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a technical scheme that: a graphite crucible.
Expressed by mass percentage as: 50-60% of graphitized coke, 35-45% of asphalt and 5-15% of a coating layer, wherein the coating layer comprises resin and pyridine, the resin and the pyridine are used for manufacturing an inert coating net, the inert coating net is adhered to graphene through coating, the other side of the graphene is coated with the resin, and the graphene is adhered to the prepared graphite crucible through melting the resin so as to cover the whole graphite crucible.
The pyridine can be replaced by organic matters with high nitrogen content such as biuret, and the organic matters with high nitrogen content can provide a large amount of free nitrogen elements, so that the oxidation resistance is improved, and the cost investment can be reduced.
Wherein the resin is one of polyethylene, polypropylene and the like, and the mass ratio of the resin to the pyridine is as follows: 2:1-1.5.
The preparation method comprises the following steps:
(1) preparing a graphite crucible, adding graphitized coke and asphalt according to the mass ratio, respectively screening the graphitized coke and the asphalt, kneading after screening, performing compression molding to form a semi-finished blank after kneading, further roasting to form a semi-finished roasted blank, and finally machining to form a crucible matrix;
(2) preparing an inert coating net, adding pyridine into a beaker according to the mass ratio, and adding a dispersing agent into the beaker, wherein the mass volume ratio of the pyridine to the dispersing agent is 2:9-15;
(3) magnetically stirring the mixture in the beaker in the step (2), wherein the magnetic stirring speed is 25-35 r/min, and the stirring time is 60-80 min, so as to obtain a mixed solution A;
the pyridine is dispersed sufficiently for subsequent processing and fabrication, wherein the magnetic stirring can be replaced by an ultrasonic stirrer.
(4) Heating the mixed solution A, connecting a distillation tube on a beaker during heating, wherein the heating temperature is 500-700 ℃, the heating time is 8-12 h, and collecting a distilled solution B;
(5) mixing the collected distilled solution B with resin with corresponding mass after the distilled solution B is cooled to room temperature, and stirring at constant temperature of 50-70 ℃ for 2-3 h; obtaining a mixture C;
because the pyridine is gasified at the temperature of 500-700 ℃, the carbon-carbon single bond in the pyridine is decomposed, the nitrogen element is fully released, and the gasified mixture consists of water, the nitrogen element and the carbon element, the nitrogen element and the resin are uniformly stirred, so that the nitrogen element is uniformly attached to the surface of the resin to form a nitrogen net with a net shape, the oxidation resistance of the surface of the resin is improved, and the amount of the free carbon element is reduced.
(6) Pressing the graphene into a laminar object with the thickness of 1-1.5 mm;
(7) uniformly coating the mixture C prepared in the step (3) on one side surface of the graphene layer prepared in the step (4) at the temperature of 50-70 ℃;
(8) and uniformly coating resin on the other side surface of the graphene, completely covering the coated graphene on the surface of the crucible substrate, and performing compression molding to complete the preparation.
Wherein, the thickness of the mixture C in the step (7) is 0.8-1 mm.
Wherein, the specific steps of the step (8) are as follows: heating and melting the surface of the graphene layer with the resin, wherein the heating temperature is 50-60 ℃, directly bonding the resin in a molten state to the outside of the crucible matrix, and further adopting mechanical pressing.
Wherein, the crucible matrix prepared in the step (1) is heated to 600-700 ℃ for 12-14h at a high temperature, and then cooled to room temperature for use.
The chemical reagents adopted by the invention are all commercially available chemicals, and the purity is AR grade.
Example 1
(1) Preparing a graphite crucible, adding 50g of graphitized coke and 35g of asphalt according to the mass ratio, respectively screening the graphitized coke and the asphalt, carrying out kneading after screening, carrying out compression molding after kneading to form a semi-finished blank, further roasting to form a semi-finished baked blank, finally machining to form a crucible base body, carrying out a high-temperature heating process on the crucible base body, heating to 600 ℃, heating for 12 hours, and cooling to room temperature for use after heating;
(2) preparing an inert coating net, adding pyridine into a beaker according to a mass ratio, and adding a dispersing agent into the beaker, wherein the mass volume ratio of the pyridine to the dispersing agent is 2;
(3) magnetically stirring the mixture in the beaker in the step (2), wherein the magnetic stirring speed is 30r/min, and the stirring time is 60min to obtain a mixed solution A;
the pyridine is sufficiently dispersed for subsequent processing and manufacturing, wherein the magnetic stirring can be replaced by an ultrasonic stirrer.
(4) Heating the mixed solution A, connecting a distillation tube to a beaker during heating, heating at the temperature of 600 ℃ for 10 hours, and collecting a distilled solution B;
(5) mixing the collected distilled solution B with resin with corresponding mass after the distilled solution B is cooled to room temperature, and stirring at constant temperature of 60 ℃ for 2 hours; obtaining a mixture C;
(6) pressing the graphene into a laminar object with the thickness of 1 mm;
(7) uniformly coating the mixture C prepared in the step (5), wherein the thickness of the mixture C is 0.8mm, on one side surface of the graphene layer prepared in the step (6) at the temperature of 60 ℃;
(8) and evenly coating resin on the other side surface of the graphene, completely covering the coated graphene on the surface of the crucible substrate, heating and melting the surface of the graphene layer with the resin, wherein the heating temperature is 60 ℃, directly bonding the resin in a molten state to the outside of the crucible substrate, and then preparing the graphene by adopting mechanical compression molding.
Example 2
(1) Preparing a graphite crucible, adding 55g of graphitized coke and 40g of asphalt according to the mass ratio, respectively screening the graphitized coke and the asphalt, carrying out kneading after screening, carrying out compression molding after kneading to form a semi-finished blank, further roasting to form a semi-finished baked blank, finally machining to form a crucible base body, carrying out a high-temperature heating process on the crucible base body, heating to 600 ℃, heating for 12 hours, and cooling to room temperature for use after heating;
(2) preparing an inert coating net, adding pyridine into a beaker according to a mass ratio, and adding a dispersing agent into the beaker, wherein the mass volume ratio of the pyridine to the dispersing agent is 2;
(3) magnetically stirring the mixture in the beaker in the step (2), wherein the magnetic stirring speed is 30r/min, and the stirring time is 60min, so as to obtain a mixed solution A;
the pyridine is sufficiently dispersed for subsequent processing and manufacturing, wherein the magnetic stirring can be replaced by an ultrasonic stirrer.
(4) Heating the mixed solution A, connecting a distillation tube on a beaker during heating, wherein the heating temperature is 600 ℃, the heating time is 10 hours, and collecting a distilled solution B;
(5) mixing the collected distilled solution B with resin with corresponding mass after the distilled solution B is cooled to room temperature, and stirring at constant temperature of 60 ℃ for 2 hours; obtaining a mixture C;
(6) pressing the graphene into a laminar object with the thickness of 1 mm;
(7) uniformly coating the mixture C prepared in the step (5), wherein the thickness of the mixture C is 0.8mm, on one side surface of the graphene layer prepared in the step (6) at the temperature of 60 ℃;
(8) and evenly coating resin on the other side surface of the graphene, completely covering the coated graphene on the surface of the crucible substrate, heating and melting the surface of the graphene layer with the resin, wherein the heating temperature is 60 ℃, directly bonding the resin in a molten state to the outside of the crucible substrate, and then preparing the graphene by adopting mechanical compression molding.
Example 3
(1) Preparing a graphite crucible, adding 55g of graphitized coke and 35g of asphalt according to the mass ratio, respectively screening the graphitized coke and the asphalt, carrying out kneading after screening, carrying out compression molding after kneading to form a semi-finished blank, further roasting to form a semi-finished baked blank, finally machining to form a crucible base body, carrying out a high-temperature heating process on the crucible base body, heating to 600 ℃, heating for 12 hours, and cooling to room temperature for use after heating;
(2) preparing an inert coating net, adding pyridine into a beaker according to the mass ratio, and adding a dispersing agent into the beaker, wherein the mass volume ratio of the pyridine to the dispersing agent is 2;
(3) magnetically stirring the mixture in the beaker in the step (2), wherein the magnetic stirring speed is 30r/min, and the stirring time is 60min to obtain a mixed solution A;
the pyridine is dispersed sufficiently for subsequent processing and fabrication, wherein the magnetic stirring can be replaced by an ultrasonic stirrer.
(4) Heating the mixed solution A, connecting a distillation tube on a beaker during heating, wherein the heating temperature is 600 ℃, the heating time is 10 hours, and collecting a distilled solution B;
(5) mixing the collected distilled solution B with resin with corresponding mass after the distilled solution B is cooled to room temperature, and stirring at constant temperature of 60 ℃ for 2 hours; obtaining a mixture C;
(6) pressing the graphene into a laminar object with the thickness of 1 mm;
(7) uniformly coating the mixture C prepared in the step (5), wherein the thickness of the mixture C is 0.8mm, on one side surface of the graphene layer prepared in the step (6) at the temperature of 60 ℃;
(8) and evenly coating resin on the other side surface of the graphene, completely covering the coated graphene on the surface of the crucible substrate, heating and melting the surface of the graphene layer with the resin, wherein the heating temperature is 60 ℃, directly bonding the resin in a molten state to the outside of the crucible substrate, and then preparing the graphene by adopting mechanical compression molding.
Comparative example 1
Preparing a graphite crucible, adding 50g of graphitized coke and 35g of asphalt according to the mass ratio, respectively screening the graphitized coke and the asphalt, carrying out kneading after screening, carrying out compression molding after kneading to form a semi-finished blank, further roasting to form a semi-finished baked blank, finally machining to form a crucible base body, carrying out a high-temperature heating process on the crucible base body, heating to 600 ℃, heating for 12 hours, and cooling to room temperature for use after heating.
Comparative example 2
Preparing a graphite crucible, adding 50g of graphitized coke and 35g of asphalt according to the mass ratio, respectively screening the graphitized coke and the asphalt, carrying out kneading after screening, carrying out compression molding after kneading to form a semi-finished blank, further roasting to form a semi-finished baked blank, and finally machining to form a crucible base body.
Placing industrial aluminum powder in the graphite crucible prepared in the embodiment and the comparative example, carrying out an aluminum melting test according to a metal melting standard, wherein the maximum temperature is 720 ℃, the vacuum degree is 3.08X 10 < -2 > Pa, the industrial aluminum powder is melted into liquid aluminum in the aluminum melting process and is coated on the central position of the graphite crucible, after cooling and solidification, taking out the graphite crucible to investigate the demolding effect of the silicon block, wherein the demolding effect is expressed by the mass ratio of the residual aluminum block adhered to the inside of the graphite crucible to the aluminum block solidified integrally, and the result is shown in the following table 1:
TABLE 1
| Ratio (%) | |
| Example 1 | 0.083 |
| Example 2 | 0.012 |
| Example 3 | 0.069 |
| Comparative example 1 | 0.656 |
| Comparative example 2 | 1.023 |
The contents of free carbon on the surfaces of the graphite crucibles prepared in the above examples and comparative examples were measured by a gas volumetric method, and the results are shown in the following table 2:
| content (%) | |
| Example 1 | 0.053 |
| Example 2 | 0.046 |
| Example 3 | 0.060 |
| Comparative example 1 | 0.072 |
| Comparative example 2 | 0.235 |
As can be seen from the above table 1, when the addition amount of pyridine is 10g, the demolding effect is optimal, and the graphite crucible can be effectively prevented from being bonded; as can be seen from table 2 above, when the amount of pyridine added is 10g, the demolding effect is optimal, and the graphite crucible can be effectively prevented from being bonded, and after the crucible base body is subjected to the high-temperature heating process, the free carbon element is greatly reduced, and the formation of carbide at the bottom of the crucible when the crucible is used is avoided, so that the formation of a bonding layer can be avoided.
In the above table 1, when more pyridine is added, the ratio is higher, which is related to the formation of free carbon element by the cracking of excessive pyridine.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising a … …" does not exclude the presence of another identical element in a process, method, article, or apparatus that comprises the element.
The above description is only for illustrating the technical solution of the present invention and not for limiting, and other modifications or equivalent substitutions made by the technical solution of the present invention by those of ordinary skill in the art should be covered within the scope of the claims of the present invention as long as they do not depart from the spirit and scope of the technical solution of the present invention.
Claims (6)
1. A graphite crucible, characterized in that: the graphite crucible is represented by the following percentage by mass: 50-60% of graphitized coke, 35-45% of asphalt and 5-15% of a coating layer, wherein the coating layer comprises resin and pyridine; preparing an inert coating net by using resin and pyridine, wherein the inert coating net is adhered to graphene through coating, the other side of the graphene is coated with the resin, and the graphene is adhered to the prepared graphite crucible in a melting mode through the melting resin to cover the whole graphite crucible;
the preparation of the graphite crucible comprises the following steps:
(1) preparing a graphite crucible, adding graphitized coke and asphalt according to the mass ratio, respectively screening the graphitized coke and the asphalt, kneading after screening, performing compression molding after kneading to form a semi-finished blank, further roasting to form a semi-finished roasted blank, and finally machining to form a crucible matrix;
(2) adding pyridine into a beaker according to the mass ratio, and adding a dispersing agent into the beaker, wherein the mass-volume ratio of the pyridine to the dispersing agent is 2:9-15;
magnetically stirring the mixture in the beaker in the step (2), wherein the magnetic stirring speed is 25-35 r/min, and the stirring time is 60-80 min, so as to obtain a mixed solution A;
heating the mixed solution A, connecting a distillation tube on a beaker during heating, wherein the heating temperature is 500-700 ℃, the heating time is 8-12 h, and collecting a distilled solution B;
(3) after the distilled solution B is cooled to room temperature, mixing the collected distilled solution B with resin with corresponding mass, and stirring at constant temperature of 50-70 ℃ for 2-3 h; obtaining a mixture C;
(4) pressing the graphene into a laminar object with the thickness of 1-1.5 mm;
(5) uniformly coating the mixture C prepared in the step (3) on one side surface of the graphene layer prepared in the step (4) at the temperature of 50-70 ℃;
(6) and uniformly coating resin on the other side surface of the graphene, completely covering the coated graphene on the surface of the crucible substrate, and performing compression molding to complete the preparation.
2. A graphite crucible as set forth in claim 1, wherein: the resin is one of polyethylene and polypropylene, and the mass ratio of the resin to the pyridine is as follows: 2:1-1.5.
3. A graphite crucible as set forth in claim 1, wherein: the thickness of the mixture C in the step (5) is 0.8-1 mm.
4. A graphite crucible as set forth in claim 1, wherein: the specific steps of the step (6) are as follows: heating and melting the surface of the graphene layer with the resin, wherein the heating temperature is 50-60 ℃, directly bonding the resin in a molten state to the outside of the crucible matrix, and further adopting mechanical pressing.
5. A graphite crucible as set forth in claim 1, wherein: and (2) carrying out a high-temperature heating process on the crucible matrix prepared in the step (1), heating to 600-700 ℃, heating for 12-14h, and cooling to room temperature for use after heating.
6. A graphite crucible as set forth in claim 1, wherein: the dispersing agent is one of ethylene glycol and propanol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210145848.8A CN114409403B (en) | 2022-02-17 | 2022-02-17 | Graphite crucible |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210145848.8A CN114409403B (en) | 2022-02-17 | 2022-02-17 | Graphite crucible |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114409403A CN114409403A (en) | 2022-04-29 |
| CN114409403B true CN114409403B (en) | 2022-10-28 |
Family
ID=81260881
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210145848.8A Active CN114409403B (en) | 2022-02-17 | 2022-02-17 | Graphite crucible |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114409403B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011042569A (en) * | 2007-04-04 | 2011-03-03 | Sony Corp | Porous carbon material, adsorbent, filler, mask, adsorbing sheet, and carrier |
| CN108022706A (en) * | 2017-12-22 | 2018-05-11 | 湖南工程学院 | A kind of preparation method of magnetic-functionalized graphene composite material |
| CN108046812A (en) * | 2017-12-12 | 2018-05-18 | 中国平煤神马能源化工集团有限责任公司 | A kind of Delanium crucible and preparation method thereof |
| CN109651649A (en) * | 2018-12-17 | 2019-04-19 | 四川大学 | A kind of graphene-based antioxidant and its preparation method and application |
| CN111087249A (en) * | 2019-12-27 | 2020-05-01 | 重庆东星炭素材料有限公司 | Graphite porous crucible and preparation method thereof |
| CN113716546A (en) * | 2021-08-31 | 2021-11-30 | 青岛海洋科学与技术国家实验室发展中心 | Graphene/mesoporous carbon/ZIF-derived carbon composite three-dimensional graded porous carbon material, and preparation method and application thereof |
-
2022
- 2022-02-17 CN CN202210145848.8A patent/CN114409403B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011042569A (en) * | 2007-04-04 | 2011-03-03 | Sony Corp | Porous carbon material, adsorbent, filler, mask, adsorbing sheet, and carrier |
| CN108046812A (en) * | 2017-12-12 | 2018-05-18 | 中国平煤神马能源化工集团有限责任公司 | A kind of Delanium crucible and preparation method thereof |
| CN108022706A (en) * | 2017-12-22 | 2018-05-11 | 湖南工程学院 | A kind of preparation method of magnetic-functionalized graphene composite material |
| CN109651649A (en) * | 2018-12-17 | 2019-04-19 | 四川大学 | A kind of graphene-based antioxidant and its preparation method and application |
| CN111087249A (en) * | 2019-12-27 | 2020-05-01 | 重庆东星炭素材料有限公司 | Graphite porous crucible and preparation method thereof |
| CN113716546A (en) * | 2021-08-31 | 2021-11-30 | 青岛海洋科学与技术国家实验室发展中心 | Graphene/mesoporous carbon/ZIF-derived carbon composite three-dimensional graded porous carbon material, and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114409403A (en) | 2022-04-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102294485B (en) | Composite electric contact material and preparation method thereof | |
| CN101524754B (en) | Rapid thermal pressed sintering molding process for titanium-aluminum alloy targets | |
| CN111910160B (en) | Preparation method of aluminum-scandium target material | |
| CN108046812A (en) | A kind of Delanium crucible and preparation method thereof | |
| CN110592421B (en) | Copper alloy, copper alloy sheet material, and preparation method and application thereof | |
| CN110511047B (en) | Method for preparing regenerated magnesia carbon brick by hydration impregnation treatment process | |
| CN101503302A (en) | Carboneous fire-resistant material for furnace brick lining and preparation thereof | |
| CN110684914A (en) | High-strength high-hardness aluminum alloy and preparation method thereof | |
| CN114409403B (en) | Graphite crucible | |
| US3408312A (en) | Electrically conductive cermet compositions | |
| US3011982A (en) | Refractory and method of making the same | |
| CN104032173A (en) | High-strength tin-brass alloy material and preparation method thereof | |
| CN114086179B (en) | Preparation method of diamond wear-resistant coating on surface of copper matrix | |
| JPH11256321A (en) | Zno base sintered compact | |
| WO2018028091A1 (en) | Copper-based composite material for mechanical part and preparation method therefor | |
| CN113502408B (en) | High-conductivity copper alloy containing tellurium and nickel and preparation method thereof | |
| CN113199024B (en) | Ternary layered compound, metal-based composite material, and preparation method and raw materials thereof | |
| CN114449695B (en) | Ultrahigh-power graphite electrode | |
| CN113186021A (en) | Solid lubricant and preparation method thereof | |
| KR101697941B1 (en) | Manufacturing method of grid for lead-acid battery | |
| CN113106302A (en) | Al-Re-Te ternary intermediate alloy and preparation method thereof | |
| CN113088774B (en) | High-resistance Al-Mg-Mn-Ti aluminum alloy and preparation process thereof | |
| CN109930176A (en) | A kind of method that fused salt prepares silicon nickel alloy | |
| CN110965081B (en) | Copper-steel composite cathode steel bar and manufacturing process thereof | |
| CN115041679B (en) | Diamond surface modification treatment method and application |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |