CN111087249A - Graphite porous crucible and preparation method thereof - Google Patents
Graphite porous crucible and preparation method thereof Download PDFInfo
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- CN111087249A CN111087249A CN201911378832.6A CN201911378832A CN111087249A CN 111087249 A CN111087249 A CN 111087249A CN 201911378832 A CN201911378832 A CN 201911378832A CN 111087249 A CN111087249 A CN 111087249A
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- 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
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Abstract
The invention relates to a preparation method of a graphite porous crucible, which comprises solid raw materials and modified asphalt, wherein the solid raw materials comprise, by weight, 52% -64% of graphitized calcined coke and 36-48% of graphitized heat-insulating material, and the modified asphalt accounts for 20-24% of the solid raw materials by mass. The graphite porous crucible is not easy to crack, low in resistivity and excellent in mechanical property, the prepared graphite crucible is high in compactness, the volume density is 1.62-1.64g/cm3, the resistivity is 20-25 u.omega.m, and the breaking strength is not less than 5.7 Mpa; the graphite crucible is gradually and compactly stacked under the action of self weight and external force by adopting a horizontal vibration molding process to form a compact blank, so that the compactness of the graphite crucible is greatly improved; the warm roasting mode can greatly reduce the problems of bulging, cracks and the like of the crucible caused by overhigh temperature rise or too fast temperature reduction in the roasting process and the cooling process of the graphite crucible.
Description
Technical Field
The invention relates to the technical field of crucibles, in particular to a graphite porous crucible and a preparation method thereof.
Background
With the innovation and development of preparation technology of high-temperature materials, the modern society puts higher requirements on crucibles under high-temperature environments. The crucible can be divided into three categories of ceramic crucible, clay crucible and metal crucible according to the material composition, wherein the ceramic crucible has wide application, can be used for smelting various steel, nonferrous metal and alloy thereof, and has become an indispensable tool in modern metallurgical industry. The crucible not only needs to have good high temperature resistance, but also needs to have good vibration resistance and stronger corrosion resistance, and the crucible prepared by the traditional method is difficult to meet the requirements.
Graphite has good chemical stability and strong chemical inertia under certain conditions, and is not easy to be impregnated and dissolved after being contacted with a melt and a solid-phase substance under a high-temperature condition, so that the graphite serving as a crucible material can greatly improve the erosion resistance of the crucible to molten slag. In general, in order to ensure the overall compactness and high-temperature sintering requirement of the crucible, the crucible material needs to be subjected to compression molding and then high-temperature roasting to obtain the crucible. However, the crucible is obtained by adopting a mould pressing process and a high-temperature roasting mode, the graphite material has poor bonding performance, mould pressing and pressure maintaining are carried out by needing larger pressure intensity, the problems of breakage and the like are easily caused by roasting and cooling of the crucible, and the production efficiency and the yield of the crucible are greatly reduced.
Disclosure of Invention
The invention aims to solve the problems of the prior art and provides a graphite crucible which is used for solving the problems of low compactness, high resistivity and low breaking strength of the prior crucible.
In order to achieve the purpose, the invention adopts the following technical scheme:
a graphite porous crucible comprises raw materials of solid raw materials and modified asphalt, wherein the solid raw materials comprise, by weight, 52% -64% of graphitized calcined coke and 36-48% of graphitized heat-insulating materials, and the modified asphalt accounts for 20-24% of the mass fraction of the solid raw materials.
Preferably, the crucible raw material comprises a solid raw material and modified asphalt, the solid raw material comprises 58% of graphitized calcined coke and 42% of graphitized heat-insulating material by weight, and the modified asphalt accounts for 21% -22% of the solid raw material by weight.
Preferably, the particle size of the graphitized calcined coke is 0-8 mm;
preferably, the particle size of the graphitized heat preservation material is 0-2 mm;
the invention also provides a preparation method of the graphite porous crucible, which is used for solving the problem that the crucible obtained by the existing preparation method is easy to crack.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a graphite porous crucible comprises the following steps:
1) mechanically crushing the graphitized calcined coke into granules, and grinding the graphitized heat-insulating material into powder;
2) preheating a kneading pot to 140 ℃, adding the graphitized calcined coke and the graphitized heat-insulating material into the kneading pot under normal pressure, heating to 120 ℃ of 115 ℃ for dry mixing for 30min, discharging water in the material, adding modified asphalt, and discharging the obtained paste material into a hopper after wet mixing for 45 min;
3) putting the paste in the hopper into a material airing stirring cylinder with the preheating temperature of 80 ℃, and stirring and airing the material for 10-15 min;
4) vibrating and molding the paste material after stirring and airing by adopting a horizontal vibration molding process to prepare an electrode green body, wherein the diameter of the electrode green body is 860mm, and the length of the electrode green body is 2350 mm;
5) calcining the electrode green body by adopting a ring type calcining furnace under the conditions of vacuum and protective medium to prepare a carbon electrode;
6) and transversely cutting the electrode roasted product after the electrode roasted product is qualified to obtain a crucible blank, and processing the excircle and the inner hole of the crucible blank to obtain the graphite porous crucible.
Preferably, the vibration molding time in the step 4) is 150-180s, and the pressure maintaining time is 8-20 min.
Preferably, the air-isolated roasting time in the step 5) is 576h, the roasting mode is variable-temperature roasting, the lowest roasting temperature is not lower than 235 ℃, and the highest roasting temperature is not higher than 800 ℃.
Compared with the prior art, the invention has the following beneficial effects: the graphite porous crucible is not easy to crack, the resistivity is low, the mechanical property is excellent, the prepared graphite crucible is high in compactness, and the volume density is 1.62-1.64g/cm3The resistivity is between 20 and 25 u.omega.m, and the flexural strength is not less than 5.7 MPa. According to the preparation method of the graphite porous crucible, the graphite porous crucible is gradually stacked and compacted under the action of self weight and external force by adopting a horizontal vibration molding process to form a compact blank, so that the compactness of the graphite porous crucible is greatly improved; and the warm roasting mode can greatly reduce the problems of bulging, cracks and the like of the crucible caused by overhigh temperature rise or too fast temperature reduction in the roasting process and the cooling process of the graphite crucible, and greatly improve the yield and the yield of the graphite crucible.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the functions of the invention clearer and easier to understand, the invention is further described by combining the following specific embodiments:
the graphite porous crucible and the preparation method thereof provided by the invention adopt a pressure maintaining process, and continuously pressurize the paste material in a pressure maintaining mode to increase the density of the paste material. Meanwhile, the temperature of the die is about 120 ℃ in the pressure maintaining stage, so that the phenomenon that the paste at the contact part of the die is cooled too fast in the pressure maintaining stage to cause the curing of the edge of the paste is effectively avoided, the internal resistance of the die is increased, and the compactness is reduced.
The preheating of the die in the vibration molding process can greatly improve the mold-entering temperature of the paste, shorten the time for the paste to reach the optimal fluidity and the molding period, further improve the uniformity of the internal and external temperatures of the paste, improve the uniformity of the fluidity of the paste, reduce the pressure of compression molding and improve the physical and mechanical properties of products.
The horizontal vibration molding process is adopted, so that the insides of the paste materials can mutually impact under the vibration effect, the static friction among the paste materials is changed into the dynamic friction, the paste materials are changed into particles with fluidity, and the particles are gradually stacked under the action of self weight and external force to form a compact blank body. And during vibration molding, due to the energy output by vibration, the particles have the activity of three-dimensional space, are densely filled in all corners of the model and expel air, so that the paste density is improved in a smaller molding space. Compared with compression molding, the vibration molding temperature is shorter, a long-time material airing process is not needed, and the material can be filled into a mold for vibration molding only by cooling for ten minutes.
The roasting time of the ring-type roasting furnace is 576 hours, variable-temperature roasting is adopted, the roasting temperature range is 235-800 ℃, low-temperature roasting is firstly carried out, redundant moisture in the material is discharged, then high-temperature roasting is carried out, the reaction in the paste is promoted, finally the temperature is gradually reduced, the internal structure of the electrode roasted product is stabilized, internal bulging or cracks of the electrode roasted product caused by variable temperature are avoided, and the mechanical property of the electrode roasted product is stabilized.
Example 1:
selecting 52 parts of graphitized calcined coke, 48 parts of graphitized heat-insulating material and 20 parts of modified asphalt, mechanically crushing and grinding the graphitized calcined coke and the graphitized heat-insulating material to obtain graphitized calcined coke with the particle size of 0-8mm and the graphitized heat-insulating material with the particle size of 0-2mm, kneading by using a 3000L medium-sized kneader, preheating a kneading pot to 140 ℃, adding the graphitized calcined coke and the graphitized heat-insulating material into the kneading pot under normal pressure, heating to 115 ℃, dry-mixing for 30min, discharging water in the materials, adding the modified asphalt into the kneading pot, and discharging the obtained paste into a hopper after wet mixing for 45 min; placing the paste in a hopper into a preheated material airing stirring cylinder with the preheating temperature of 80 ℃, stirring and airing the material for 10min, performing vibration molding by adopting a horizontal vibration molding process for 150s, and then maintaining the pressure for 8min to obtain an electrode green body with the diameter of 860mm and the length of 2350 mm; roasting by adopting a ring roasting furnace, and roasting the electrode green body for 576h in an air-isolated manner under the protection of metallurgical coke particles, wherein the roasting mode is variable-temperature roasting to obtain an electrode roasted product; and transversely cutting the electrode roasted product after the electrode roasted product is qualified to obtain a crucible blank, and processing the excircle and the inner hole of the crucible blank to obtain the graphite porous crucible A.
Example 2:
selecting 52 parts of graphitized calcined coke, 48 parts of graphitized heat-insulating material and 20 parts of modified asphalt, mechanically crushing and grinding the graphitized calcined coke and the graphitized heat-insulating material to obtain graphitized calcined coke with the particle size of 0-8mm and the graphitized heat-insulating material with the particle size of 0-2mm, kneading by using a 3000L medium-sized kneader, preheating a kneading pot to 140 ℃, adding the graphitized calcined coke and the graphitized heat-insulating material into the kneading pot under normal pressure, heating to 117 ℃, dry-mixing for 30min, discharging water in the materials, adding the modified asphalt into the kneading pot, and discharging the obtained paste into a hopper after wet mixing for 45 min; placing the paste in a hopper into a preheated material airing stirring cylinder with the preheating temperature of 80 ℃, stirring and airing the materials for 12min, performing vibration molding by adopting a horizontal vibration molding process for 165s, and then maintaining the pressure for 14min to obtain an electrode green body with the diameter of 860mm and the length of 2350 mm; roasting by adopting a ring roasting furnace, and roasting the electrode green body for 576h in an air-isolated manner under the protection of a metallurgical coke material, wherein the roasting mode is variable-temperature roasting to obtain an electrode roasted product; and transversely cutting the electrode roasted product after the electrode roasted product is qualified to obtain a crucible blank, and processing the excircle and the inner hole of the crucible blank to obtain the graphite porous crucible B.
Example 3:
selecting 52 parts of graphitized calcined coke, 48 parts of graphitized heat-insulating material and 20 parts of modified asphalt, mechanically crushing and grinding the graphitized calcined coke and the graphitized heat-insulating material to obtain graphitized calcined coke with the particle size of 0-8mm and the graphitized heat-insulating material with the particle size of 0-2mm, kneading by using a 3000L medium-sized kneader, preheating a kneading pot to 140 ℃, adding the graphitized calcined coke and the graphitized heat-insulating material into the kneading pot under normal pressure, heating to 120 ℃, dry-mixing for 30min, discharging water in the materials, adding the modified asphalt into the kneading pot, and discharging the obtained paste into a hopper after wet mixing for 45 min; placing the paste in a hopper into a preheated material airing stirring cylinder with the preheating temperature of 80 ℃, stirring and airing the materials for 15min, performing vibration molding by adopting a horizontal vibration molding process for 180s, and then maintaining the pressure for 20min to obtain an electrode green body with the diameter of 860mm and the length of 2350 mm; roasting by adopting a ring roasting furnace, and roasting the electrode green body for 576h in an air-isolated manner under the protection of a metallurgical coke material, wherein the roasting mode is variable-temperature roasting to obtain an electrode roasted product; and transversely cutting the electrode roasted product after the electrode roasted product is qualified to obtain a crucible blank, and processing the excircle and the inner hole of the crucible blank to obtain the graphite porous crucible C.
Example 4:
selecting 58 parts of graphitized calcined coke, 42 parts of graphitized heat-insulating material and 21 parts of modified asphalt, mechanically crushing and grinding the graphitized calcined coke and the graphitized heat-insulating material to obtain graphitized calcined coke with the particle size of 0-8mm and a graphitized heat-insulating material with the particle size of 0-2mm, kneading by using a 3000L medium-sized kneader, preheating a kneading pot to 140 ℃, adding the graphitized calcined coke and the graphitized heat-insulating material into the kneading pot under normal pressure, heating to 115 ℃, dry-mixing for 30min, discharging water in the materials, adding the modified asphalt into the kneading pot, and discharging the obtained paste into a hopper after wet mixing for 45 min; placing the paste in a hopper into a preheated material airing stirring cylinder with the preheating temperature of 80 ℃, stirring and airing the material for 10min, performing vibration molding by adopting a horizontal vibration molding process for 150s, and then maintaining the pressure for 8min to obtain an electrode green body with the diameter of 860mm and the length of 2350 mm; roasting by adopting a ring roasting furnace, and roasting the electrode green body for 576h in an air-isolated manner under the protection of a metallurgical coke material, wherein the roasting mode is variable-temperature roasting to obtain an electrode roasted product; and transversely cutting the electrode roasted product after the roasting is qualified to obtain a crucible blank, and processing the excircle and the inner hole of the crucible blank to obtain the graphite porous crucible D.
Example 5:
selecting 58 parts of graphitized calcined coke, 42 parts of graphitized heat-insulating material and 22 parts of modified asphalt, mechanically crushing and grinding the graphitized calcined coke and the graphitized heat-insulating material to obtain graphitized calcined coke with the particle size of 0-8mm and a graphitized heat-insulating material with the particle size of 0-2mm, kneading by using a 3000L medium-sized kneader, preheating a kneading pot to 140 ℃, adding the graphitized calcined coke and the graphitized heat-insulating material into the kneading pot under normal pressure, heating to 118 ℃, dry-mixing for 30min, discharging water in the materials, adding the modified asphalt into the kneading pot, and discharging the obtained paste into a hopper after wet mixing for 45 min; placing the paste in a hopper into a preheated material airing stirring cylinder with the preheating temperature of 80 ℃, stirring and airing the materials for 13min, performing vibration molding by adopting a horizontal vibration molding process for 165s, and then maintaining the pressure for 8min to obtain an electrode green body with the diameter of 860mm and the length of 2350 mm; roasting by adopting a ring roasting furnace, and roasting the electrode green body for 576h in an air-isolated manner under the protection of a metallurgical coke material, wherein the roasting mode is variable-temperature roasting to obtain an electrode roasted product; and transversely cutting the electrode roasted product after the roasting is qualified to obtain a crucible blank, and processing the excircle and the inner hole of the crucible blank to obtain the graphite porous crucible E.
Example 6:
selecting 58 parts of graphitized calcined coke, 42 parts of graphitized heat-insulating material and 23 parts of modified asphalt, mechanically crushing and grinding the graphitized calcined coke and the graphitized heat-insulating material to obtain graphitized calcined coke with the particle size of 0-8mm and a graphitized heat-insulating material with the particle size of 0-2mm, kneading by using a 3000L medium-sized kneader, preheating a kneading pot to 140 ℃, adding the graphitized calcined coke and the graphitized heat-insulating material into the kneading pot under normal pressure, heating to 120 ℃, dry-mixing for 30min, discharging water in the materials, adding the modified asphalt into the kneading pot, and discharging the obtained paste into a hopper after wet mixing for 45 min; placing the paste in a hopper into a preheated material airing stirring cylinder with the preheating temperature of 80 ℃, stirring and airing the materials for 15min, performing vibration molding by adopting a horizontal vibration molding process for 180s, and then maintaining the pressure for 20min to obtain an electrode green body with the diameter of 860mm and the length of 2350 mm; roasting by adopting a ring roasting furnace, and roasting the electrode green body for 576h in an air-isolated manner under the protection of a metallurgical coke material, wherein the roasting mode is variable-temperature roasting to obtain an electrode roasted product; and transversely cutting the electrode roasted product after the electrode roasted product is qualified to obtain a crucible blank, and processing the excircle and the inner hole of the crucible blank to obtain the graphite porous crucible F.
Example 7:
selecting 64 parts of graphitized calcined coke, 36 parts of graphitized heat-insulating material and 24 parts of modified asphalt, mechanically crushing and grinding the graphitized calcined coke and the graphitized heat-insulating material to obtain graphitized calcined coke with the particle size of 0-8mm and a graphitized heat-insulating material with the particle size of 0-2mm, kneading by using a 3000L medium-sized kneader, preheating a kneading pot to 140 ℃, adding the graphitized calcined coke and the graphitized heat-insulating material into the kneading pot under normal pressure, heating to 115 ℃, dry-mixing for 30min, discharging water in the materials, adding the modified asphalt into the kneading pot, and discharging the obtained paste into a hopper after wet mixing for 45 min; placing the paste in a hopper into a preheated material airing stirring cylinder with the preheating temperature of 80 ℃, stirring and airing the material for 10min, performing vibration molding by adopting a horizontal vibration molding process for 150s, and then maintaining the pressure for 8min to obtain an electrode green body with the diameter of 860mm and the length of 2350 mm; roasting by adopting a ring roasting furnace, and roasting the electrode green body for 576h in an air-isolated manner under the protection of a metallurgical coke material, wherein the roasting mode is variable-temperature roasting to obtain an electrode roasted product; and transversely cutting the electrode roasted product after the electrode roasted product is qualified to obtain a crucible blank, and processing the excircle and the inner hole of the crucible blank to obtain the graphite porous crucible G.
Example 8:
selecting 64 parts of graphitized calcined coke, 36 parts of graphitized heat-insulating material and 24 parts of modified asphalt, mechanically crushing and grinding the graphitized calcined coke and the graphitized heat-insulating material to obtain graphitized calcined coke with the particle size of 0-8mm and a graphitized heat-insulating material with the particle size of 0-2mm, kneading by using a 3000L medium-sized kneader, preheating a kneading pot to 140 ℃, adding the graphitized calcined coke and the graphitized heat-insulating material into the kneading pot under normal pressure, heating to 118 ℃, dry-mixing for 30min, discharging water in the materials, adding the modified asphalt into the kneading pot, and discharging the obtained paste into a hopper after wet mixing for 45 min; placing the paste in a hopper into a preheated material airing stirring cylinder with the preheating temperature of 80 ℃, stirring and airing the materials for 13min, performing vibration molding by adopting a horizontal vibration molding process for 165s, and then maintaining the pressure for 14min to obtain an electrode green body with the diameter of 860mm and the length of 2350 mm; roasting by adopting a ring roasting furnace, and roasting the electrode green body for 576h in an air-isolated manner under the protection of a metallurgical coke material, wherein the roasting mode is variable-temperature roasting to obtain an electrode roasted product; and transversely cutting the electrode roasted product after the electrode roasted product is qualified to obtain a crucible blank, and processing the excircle and the inner hole of the crucible blank to obtain the graphite porous crucible H.
Example 9:
selecting 64 parts of graphitized calcined coke, 36 parts of graphitized heat-insulating material and 24 parts of modified asphalt, mechanically crushing and grinding the graphitized calcined coke and the graphitized heat-insulating material to obtain graphitized calcined coke with the particle size of 0-8mm and a graphitized heat-insulating material with the particle size of 0-2mm, kneading by using a 3000L medium-sized kneader, preheating a kneading pot to 140 ℃, adding the graphitized calcined coke and the graphitized heat-insulating material into the kneading pot under normal pressure, heating to 120 ℃, dry-mixing for 30min, discharging water in the materials, adding the modified asphalt into the kneading pot, and discharging the obtained paste into a hopper after wet mixing for 45 min; placing the paste in a hopper into a preheated material airing stirring cylinder with the preheating temperature of 80 ℃, stirring and airing the materials for 15min, performing vibration molding by adopting a horizontal vibration molding process for 180s, and then maintaining the pressure for 20min to obtain an electrode green body with the diameter of 860mm and the length of 2350 mm; roasting by adopting a ring roasting furnace, and roasting the electrode green body for 576h in an air-isolated manner under the protection of a metallurgical coke material, wherein the roasting mode is variable-temperature roasting to obtain an electrode roasted product; and transversely cutting the electrode roasted product after the electrode roasted product is qualified to obtain a crucible blank, and processing the excircle and the inner hole of the crucible blank to obtain the graphite porous crucible I.
The performance parameters of the prepared graphite porous crucible were compared to obtain the following data:
through the determination of the volume density, the resistivity and the flexural strength of the graphite porous crucible, the performance of the graphite porous crucible prepared by the formula and the method meets the standard conditions that the volume density is between 1.62 and 1.64g/cm3, the resistivity is between 20 and 25 u.omega.m, and the flexural strength is not less than 5.7Mpa, and the graphite porous crucible can be suitable for the application requirements of industrialized crucibles.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.
Claims (7)
1. The graphite porous crucible is characterized in that crucible raw materials comprise solid raw materials and modified asphalt, wherein the solid raw materials comprise, by weight, 52% -64% of graphitized calcined coke and 36-48% of graphitized heat-insulating materials, and the modified asphalt accounts for 20-24% of the solid raw materials by weight.
2. The graphite porous crucible as claimed in claim 1, wherein the crucible raw material comprises a solid raw material and modified pitch, the solid raw material comprises 58% of graphitized calcined coke and 42% of graphitized heat preservation material by weight, and the modified pitch accounts for 21% -22% of the solid raw material by weight.
3. A graphite porous crucible according to claim 1 or 2, wherein the graphitized calcined coke has a particle size of 0 to 8 mm.
4. The porous graphite crucible according to claim 1 or 2, wherein the graphitized insulating material has a particle size of 0 to 2 mm.
5. A method of making the graphite porous crucible of claim 1, comprising the steps of:
1) mechanically crushing the graphitized calcined coke into granules, and grinding the graphitized heat-insulating material into powder;
2) preheating a kneading pot to 140 ℃, adding the graphitized calcined coke and the graphitized heat-insulating material into the kneading pot under normal pressure, heating to 120 ℃ of 115 ℃ for dry mixing for 30min, discharging water in the material, adding modified asphalt, and discharging the obtained paste material into a hopper after wet mixing for 45 min;
3) putting the paste in the hopper into a material airing stirring cylinder with the preheating temperature of 80 ℃, and stirring and airing the material for 10-15 min;
4) vibrating and molding the paste material after stirring and airing by adopting a horizontal vibration molding process to prepare an electrode green body, wherein the diameter of the electrode green body is 860mm, and the length of the electrode green body is 2350 mm;
5) calcining the electrode green body by adopting a ring type calcining furnace under the conditions of vacuum and protective medium to prepare a carbon electrode;
6) and transversely cutting the electrode roasted product after the electrode roasted product is qualified to obtain a crucible blank, and processing the excircle and the inner hole of the crucible blank to obtain the graphite porous crucible.
6. The method for preparing a graphite porous crucible as claimed in claim 5, wherein the vibration molding time in step 4) is 150-.
7. The method for preparing the graphite porous crucible according to claim 5, wherein the air-insulated roasting time in the step 5) is 576h, the roasting mode is temperature-variable roasting, the minimum roasting temperature is not lower than 235 ℃, and the maximum roasting temperature is not higher than 800 ℃.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114213127A (en) * | 2021-12-31 | 2022-03-22 | 吉林科工碳业有限公司 | Preparation method of graphite crucible |
| CN114409403A (en) * | 2022-02-17 | 2022-04-29 | 鞍山炭素有限公司 | Graphite crucible |
| CN115557732A (en) * | 2022-12-02 | 2023-01-03 | 石家庄中正碳素有限公司 | Special crucible forming preparation process for cathode powder |
| CN115609940A (en) * | 2022-12-20 | 2023-01-17 | 石家庄中正碳素有限公司 | Production process of graphite crucible |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1190579A (en) * | 1997-09-18 | 1999-04-06 | Nippon Karu Kk | Heat-shock resistant graphite die, and its manufacture |
| CN105218098A (en) * | 2015-10-29 | 2016-01-06 | 武陟县虹桥碳素有限责任公司 | A kind of negative material high temperature purification special graphite crucible manufacturing |
| CN105272287A (en) * | 2015-10-15 | 2016-01-27 | 大同新成新材料股份有限公司 | Method for preparing graphite crucible with recycled graphite |
| CN107032794A (en) * | 2016-11-03 | 2017-08-11 | 大同新成新材料股份有限公司 | A kind of preparation method of the graphite crucible purified for negative material |
| CN107140984A (en) * | 2017-05-11 | 2017-09-08 | 吉林科工碳业有限公司 | The manufacture method of disposal molding graphite crucible |
-
2019
- 2019-12-27 CN CN201911378832.6A patent/CN111087249A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1190579A (en) * | 1997-09-18 | 1999-04-06 | Nippon Karu Kk | Heat-shock resistant graphite die, and its manufacture |
| CN105272287A (en) * | 2015-10-15 | 2016-01-27 | 大同新成新材料股份有限公司 | Method for preparing graphite crucible with recycled graphite |
| CN105218098A (en) * | 2015-10-29 | 2016-01-06 | 武陟县虹桥碳素有限责任公司 | A kind of negative material high temperature purification special graphite crucible manufacturing |
| CN107032794A (en) * | 2016-11-03 | 2017-08-11 | 大同新成新材料股份有限公司 | A kind of preparation method of the graphite crucible purified for negative material |
| CN107140984A (en) * | 2017-05-11 | 2017-09-08 | 吉林科工碳业有限公司 | The manufacture method of disposal molding graphite crucible |
Non-Patent Citations (1)
| Title |
|---|
| 赵志凤: "《炭材料工艺基础》", 31 July 2017, 哈尔滨工业大学出版社 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114213127A (en) * | 2021-12-31 | 2022-03-22 | 吉林科工碳业有限公司 | Preparation method of graphite crucible |
| CN114409403A (en) * | 2022-02-17 | 2022-04-29 | 鞍山炭素有限公司 | Graphite crucible |
| CN114409403B (en) * | 2022-02-17 | 2022-10-28 | 鞍山炭素有限公司 | Graphite crucible |
| CN115557732A (en) * | 2022-12-02 | 2023-01-03 | 石家庄中正碳素有限公司 | Special crucible forming preparation process for cathode powder |
| CN115609940A (en) * | 2022-12-20 | 2023-01-17 | 石家庄中正碳素有限公司 | Production process of graphite crucible |
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