CN102951634A - Oversized isostatic pressing graphite and production method thereof - Google Patents
Oversized isostatic pressing graphite and production method thereof Download PDFInfo
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- CN102951634A CN102951634A CN2012104752997A CN201210475299A CN102951634A CN 102951634 A CN102951634 A CN 102951634A CN 2012104752997 A CN2012104752997 A CN 2012104752997A CN 201210475299 A CN201210475299 A CN 201210475299A CN 102951634 A CN102951634 A CN 102951634A
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Abstract
The invention discloses oversized isostatic pressing graphite and a production method thereof. The following raw materials are taken by weight part: 35-60 parts of pitch coke powder, 30-55 parts of needle coke powder, 5-20 parts of graphite powder, 10-20 parts of intermediate-phase small spheres, 30-50 parts of coal pitch, 1-3 parts of surface active agents and 1-3 parts of modifying agents. The raw materials are subjected to grinding, mixing and pinching, vibration molding, isostatic pressing molding, roasting, dipping, secondary roasting and graphitizing, so that the oversized isostatic pressing graphite is obtained. A once raw material treating and molding method is adopted by the invention; compared with a method of secondarily coking raw materials adopted in China at present, the production method has the advantages of short manufacturing cycle, low energy consumption, and the like; the isostatic pressing graphite product in the size being above phi 700*700mm produced according to the production method has excellent isotropy, high volume density, high mechanical strength and high heat conductivity; the resistivity and the coefficient of thermal expansion are reduced; and a design thought is excellently reflected.
Description
Technical field
The invention belongs to the graphite production field, particularly a kind of super large-scale isostatic pressing formed graphite and production method thereof.
Background technology
The isostatic pressing formed graphite material usually because of molding mode former because cylinder material or rectangular parallelepiped material, the technical process of producing because of isostatic pressing formed graphite is dipping-roasting process repeatedly, the volume density of cylinder material or rectangular parallelepiped material is with inhomogeneous, position volume density near product surface is high, and is then lower near the volume density of core.This density unevenness of product brings very large difficulty can for the heat treatment processes such as roasting, greying, and simultaneously, the such volume density inequality of product is used to the user and brought larger puzzlement, even in use therefore has an accident.Therefore, common isostatic pressing formed graphite technique is difficult to guarantee yield rate and the quality of super large-scale isostatic pressing formed graphite material.
Use in the isostatic pressing formed graphite material at single crystal silicon thermal field, the topmost consumable material of thermal field is graphite three lobe crucible and graphite heaters.And these two kinds of consumable materials all are to carry out feeding in the outside of material usually, development along with photovoltaic industry, demand to 22 inch, the above size graphite three lobe crucibles of 24 inch, well heater also constantly increases, and this is also so that the isostatic pressing formed graphite material must the super large-scale isostatic pressing formed graphite material of production specification more than Φ 700 * 700mm.
At present the most ripe isostatic pressing formed graphite production technology adopts secondary Jiao's method to make starting material obtain preferably isotropy, the present invention is by adding the method for superfine graphite powder (powder particles is 1-10 μ m) and mesophasespherule, simultaneously various raw-material granularities are carried out refinement, can be just so that product has preferably isotropy on the basis of primary treatment, shortened technical process, reduce dipping, roasting number of times, by the impregnating by pressure mode under the super large pressure (2.0MPa), so that the inside and outside quality of product is more even, also saved the energy.
Summary of the invention
The invention provides that a kind of volume density is evenly distributed, isostatic pressing formed graphite and the production method thereof of specification more than Φ 700 * 700mm.
In order to solve above-mentioned technical problem, the present invention takes following technical scheme:
A kind of super large-scale isostatic pressing formed graphite is comprised of the component of following weight ratio: pitch coke powder 35-60 part; Needle-like coke powder 30-55 part; Graphite Powder 99 5-20 part; Mesophasespherule 10-20 part; Coal-tar pitch 30-50 part; Tensio-active agent 1-3 part; Properties-correcting agent 1-3 part.
Further technical scheme is: described tensio-active agent is stearic acid.
Further technical scheme is: described properties-correcting agent is Vinylstyrene.
Further technical scheme is: the production method of described super large-scale isostatic pressing formed graphite may further comprise the steps:
A, get raw material by following weight ratio: pitch coke powder 35-60 part; Needle-like coke powder 30-55 part; Graphite Powder 99 5-20 part; Mesophasespherule 10-20 part; Coal-tar pitch 30-50 part; Tensio-active agent 1-3 part; Properties-correcting agent 1-3 part.
B, pitch coke powder, needle-like coke powder are ground respectively, make its particle diameter be not more than 15 μ m.
With pitch coke powder, needle coke grinding to median size be not more than 15 μ m be because super large-scale isostatic pressing formed graphite material in roasting process easily because insufficient strength cracks, and powder particles is less in the isostatic pressing formed graphite, then the intensity of product is higher.Adopt superfine mill can reach above-mentioned granularity requirements.Powder particles is less simultaneously, and the long-width ratio of raw material is less, and then the isotropy trend of product is stronger.
C, Graphite Powder 99, mesophasespherule are ground respectively, making its particle diameter is 1-10 μ m.
The interpolation mesophasespherule is for the isotropy that improves material and the intensity after improving the product contraction.
D, the powder that B, C step are made mix, and other raw materials that add in the A step carry out kneading.
Add the coking rate that superfine graphite powder and properties-correcting agent can make thickener in the kneading process obtain kneading effect preferably and improve pitch in roasting process.
E, D step products obtained therefrom is ground after cooling, make its particle diameter be not more than 15 μ m.
F, will E step gained powder drop in the mould and carry out vibratory compaction, the density of vibratory compaction is not more than 1.45g/cm
3
G, F step products obtained therefrom is carried out isostatic pressing, moulding top pressure 160MPa, the time of waiting static pressure is 2-4h.
Adopt vibratory compaction and isostatic pressing can reduce the porosity of raw material, simultaneously because all directions are shunk simultaneously in moulding process, further improve the isotropy of product, so that product can shrink and coking uniformly, improve simultaneously product density in roasting process.
H, G step gained die mould product are carried out roasting, 1000 ℃ of roasting top temperatures, temperature rise rate is 1-40 ℃/h, roasting time is 400-500h.
I, H step gained roasting product is flooded, steeping fluid is impregnating pitch, and impregnation pressure 2.0MPa, dipping time are 3-6h; Repeat the H step behind the dipping and carry out re-baking.
J, with I step gained re-baking product put into the induction graphitizing furnace carry out greying, 2800 ℃ of graphitization temperatures; Products obtained therefrom is the finished product after the greying.
The present invention adopts primary material processing-forming method, compares with the burnt processing of the at present domestic secondary that generally adopts starting material to have the manufacturing cycle weak point, the low remarkable advantage that waits of energy consumption.And by the refinement coke fines size, add the isotropy that the measures such as superfine graphite powder and mesophasespherule improve products, the poor inherent defect of product isotropy degree of having avoided once shaped to bring.The isostatic pressing formed graphite product of specification more than Φ 700 * 700mm of producing through the present invention has isotropy degree excellence, volume density, physical strength, thermal conductivity height; Resistivity, thermal expansivity reduce, and have embodied well mentality of designing.
Embodiment
Embodiment 1
The present embodiment production specification is that Φ 810 * 730mm isostatic pressing formed graphite manufacturing raw material and production method are as follows:
A, get raw material by following weight ratio: 40 parts of pitch coke powders; 50 parts of needle-like coke powders; 10 parts of Graphite Powder 99s; 15 parts of mesophasespherules; 45 parts of coal-tar pitch; 2 parts in tensio-active agent; 1 part of properties-correcting agent;
B, pitch coke powder, needle-like coke powder are ground respectively, make its particle diameter be not more than 15 μ m;
C, Graphite Powder 99, mesophasespherule are ground respectively, making its particle diameter is 1-10 μ m;
D, the powder that B, C step are made mix, and other raw materials that add in the A step carry out kneading;
E, D step products obtained therefrom is ground after cooling, make its particle diameter be not more than 15 μ m;
F, will E step gained powder drop in the mould and carry out vibratory compaction, the density of vibratory compaction is not more than 1.45g/cm3;
G, F step products obtained therefrom is carried out isostatic pressing, moulding top pressure 160MPa, the time of waiting static pressure is 2-4h;
H, G step gained die mould product are carried out roasting, 1000 ℃ of roasting top temperatures, temperature rise rate is 1-40 ℃/h, roasting time is 400-500h;
I, H step gained roasting product is flooded, steeping fluid is impregnating pitch, and impregnation pressure 2.0MPa, dipping time are 3-6h; Repeat the H step behind the dipping and carry out re-baking;
J, with I step gained re-baking product put into the induction graphitizing furnace carry out greying, 2800 ℃ of graphitization temperatures.According to one embodiment of present invention, greying adopts and send some technology controlling and process graphite furnace temperature and a temperature rise rate.
Products obtained therefrom is the finished product after the greying.
Embodiment 2
The present embodiment production specification is that Φ 810 * 730mm isostatic pressing formed graphite manufacturing raw material and production method are as follows:
Get raw material by following weight ratio: 35 parts of pitch coke powders; 55 parts of needle-like coke powders; 5 parts of Graphite Powder 99s; 10 parts of mesophasespherules; 40 parts of coal-tar pitch; 2 parts in tensio-active agent; 1 part of properties-correcting agent;
The B-J of other production stage production stage as described in example 1 above.
Products obtained therefrom is the finished product after the greying.
Table 1 has been listed the physical and chemical index of the isostatic pressing formed graphite of embodiment of the invention production.
Table 1: the physical and chemical index of embodiment of the invention isostatic pressing formed graphite
The present invention adopts ultra-fine grain and the prescription of uniqueness and the molding mode of vibratory compaction-isostatic pressing, so that the isotropy of Φ 810 * 730mm super large-scale isostatic pressing formed graphite material, the material physical and chemical index meets or exceeds the performance requriements of the single crystal silicon thermal field usefulness isostatic pressing formed graphite of domestic present production, simultaneously by disposable processing raw material and special molding mode, improve the isotropy degree of isostatic pressing formed graphite material, greatly saved the production time, shortened technical process, saved the energy, improved the utilization ratio of single crystal silicon thermal field with the isostatic pressing formed graphite material.Because of its excellent performance, also can improve the work-ing life of this graphite material simultaneously.Although only provided Φ 810 * 730mm super large-scale isostatic pressing formed graphite and production method thereof in the embodiments of the invention, apparent, the present invention also can produce the isostatic pressing formed graphite of other specifications more than Φ 700 * 700mm.
Above-described embodiment is the better embodiment of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other are any not to deviate from change, modification, replacement, combination, the simplification of doing under spirit of the present invention and the principle; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (4)
1. a super large-scale isostatic pressing formed graphite is characterized in that being comprised of the component of following weight ratio: pitch coke powder 35-60 part; Needle-like coke powder 30-55 part; Graphite Powder 99 5-20 part; Mesophasespherule 10-20 part; Coal-tar pitch 30-50 part; Tensio-active agent 1-3 part; Properties-correcting agent 1-3 part.
2. super large-scale isostatic pressing formed graphite according to claim 1 is characterized in that described tensio-active agent is stearic acid.
3. super large-scale isostatic pressing formed graphite according to claim 1 is characterized in that described properties-correcting agent is Vinylstyrene.
4. the production method of the described super large-scale isostatic pressing formed graphite of each claim according to claim 1-3 is characterized in that may further comprise the steps:
A, get raw material by following weight ratio: pitch coke powder 35-60 part; Needle-like coke powder 30-55 part; Graphite Powder 99 5-20 part; Mesophasespherule 10-20 part; Coal-tar pitch 30-50 part; Tensio-active agent 1-3 part; Properties-correcting agent 1-3 part;
B, pitch coke powder, needle-like coke powder are ground respectively, make its particle diameter be not more than 15 μ m;
C, Graphite Powder 99, mesophasespherule are ground respectively, making its particle diameter is 1-10 μ m;
D, the powder that B, C step are made mix, and other raw materials that add in the A step carry out kneading;
E, D step products obtained therefrom is ground after cooling, make its particle diameter be not more than 15 μ m;
F, will E step gained powder drop in the mould and carry out vibratory compaction, the density of vibratory compaction is not more than 1.45g/cm
3
G, F step products obtained therefrom is carried out isostatic pressing, moulding top pressure 160MPa, the time of waiting static pressure is 2-4h;
H, G step gained die mould product are carried out roasting, 1000 ℃ of roasting top temperatures, temperature rise rate is 1-40 ℃/h, roasting time is 400-500h;
I, H step gained roasting product is flooded, steeping fluid is impregnating pitch, and impregnation pressure 2.0MPa, dipping time are 3-6h; Repeat the H step behind the dipping and carry out re-baking;
J, with I step gained re-baking product put into the induction graphitizing furnace carry out greying, 2800 ℃ of graphitization temperatures.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103449426A (en) * | 2013-09-06 | 2013-12-18 | 辽宁大化国瑞新材料有限公司 | Wear-resisting graphite and preparation technology thereof |
| CN103586562A (en) * | 2013-07-15 | 2014-02-19 | 王国珍 | Copper-plating-free air-gouging carbon bar and process method thereof |
| CN104876581A (en) * | 2015-05-14 | 2015-09-02 | 湖南省长宇新型炭材料有限公司 | Preparation method of low-resistivity isotropic graphite |
| CN105000545A (en) * | 2015-07-09 | 2015-10-28 | 山西大学 | Method for preparing lithium ion battery artificial graphite/coke anode material |
| CN105174251A (en) * | 2015-09-22 | 2015-12-23 | 成都炭素有限责任公司 | Preparation method of isostatic pressing formed graphite of ultra-thin structure |
| CN106892428A (en) * | 2017-03-27 | 2017-06-27 | 凤城市宝山炭素有限公司 | A kind of method that short route produces isotropic hyperfine structure isostatic pressing formed graphite |
| CN108933232A (en) * | 2018-07-17 | 2018-12-04 | 大同新成新材料股份有限公司 | A kind of preparation process of lithium battery silicon-carbon cathode |
| CN110642248A (en) * | 2019-11-19 | 2020-01-03 | 平顶山市天宝特种材料有限公司 | Production method of fine-structure high-purity graphite with changed molecular arrangement combination |
| CN112521152A (en) * | 2020-10-21 | 2021-03-19 | 大同宇林德石墨新材料股份有限公司 | Preparation process of phi 700mm ultrahigh-power graphite electrode |
| CN113603487A (en) * | 2021-08-24 | 2021-11-05 | 郑州丰毅新材料科技有限公司 | Graphite with large specification and fine granularity and preparation process thereof |
| CN115124345A (en) * | 2022-05-16 | 2022-09-30 | 中核龙原科技有限公司 | Nuclear graphite for fast neutron value-added reactor nuclear measurement system and preparation method thereof |
| CN115284422A (en) * | 2022-08-11 | 2022-11-04 | 中钢集团南京新材料研究院有限公司 | Isostatic pressing impregnation method for carbon material |
| CN115403383A (en) * | 2021-05-28 | 2022-11-29 | 成都炭素有限责任公司 | Manufacturing method of graphite mold material for hot bending of curved-surface glass |
| CN116655387A (en) * | 2023-06-01 | 2023-08-29 | 潍坊华美智能科技有限公司 | High-heat-conductivity silicon carbide ceramic and preparation method thereof |
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- 2012-11-21 CN CN2012104752997A patent/CN102951634A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103586562A (en) * | 2013-07-15 | 2014-02-19 | 王国珍 | Copper-plating-free air-gouging carbon bar and process method thereof |
| CN103586562B (en) * | 2013-07-15 | 2016-03-02 | 王国珍 | Not copper facing gouge carbon-point and process thereof |
| CN103449426A (en) * | 2013-09-06 | 2013-12-18 | 辽宁大化国瑞新材料有限公司 | Wear-resisting graphite and preparation technology thereof |
| CN103449426B (en) * | 2013-09-06 | 2015-11-18 | 辽宁大化国瑞新材料有限公司 | A kind of wear-resisting graphite and manufacturing process thereof |
| CN104876581A (en) * | 2015-05-14 | 2015-09-02 | 湖南省长宇新型炭材料有限公司 | Preparation method of low-resistivity isotropic graphite |
| CN105000545A (en) * | 2015-07-09 | 2015-10-28 | 山西大学 | Method for preparing lithium ion battery artificial graphite/coke anode material |
| CN105174251A (en) * | 2015-09-22 | 2015-12-23 | 成都炭素有限责任公司 | Preparation method of isostatic pressing formed graphite of ultra-thin structure |
| CN106892428A (en) * | 2017-03-27 | 2017-06-27 | 凤城市宝山炭素有限公司 | A kind of method that short route produces isotropic hyperfine structure isostatic pressing formed graphite |
| CN108933232A (en) * | 2018-07-17 | 2018-12-04 | 大同新成新材料股份有限公司 | A kind of preparation process of lithium battery silicon-carbon cathode |
| CN110642248A (en) * | 2019-11-19 | 2020-01-03 | 平顶山市天宝特种材料有限公司 | Production method of fine-structure high-purity graphite with changed molecular arrangement combination |
| CN112521152A (en) * | 2020-10-21 | 2021-03-19 | 大同宇林德石墨新材料股份有限公司 | Preparation process of phi 700mm ultrahigh-power graphite electrode |
| CN115403383A (en) * | 2021-05-28 | 2022-11-29 | 成都炭素有限责任公司 | Manufacturing method of graphite mold material for hot bending of curved-surface glass |
| CN113603487A (en) * | 2021-08-24 | 2021-11-05 | 郑州丰毅新材料科技有限公司 | Graphite with large specification and fine granularity and preparation process thereof |
| CN115124345A (en) * | 2022-05-16 | 2022-09-30 | 中核龙原科技有限公司 | Nuclear graphite for fast neutron value-added reactor nuclear measurement system and preparation method thereof |
| CN115284422A (en) * | 2022-08-11 | 2022-11-04 | 中钢集团南京新材料研究院有限公司 | Isostatic pressing impregnation method for carbon material |
| CN115284422B (en) * | 2022-08-11 | 2023-09-29 | 中钢集团南京新材料研究院有限公司 | Isostatic pressing impregnation method for carbon material |
| CN116655387A (en) * | 2023-06-01 | 2023-08-29 | 潍坊华美智能科技有限公司 | High-heat-conductivity silicon carbide ceramic and preparation method thereof |
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Application publication date: 20130306 |