CN102173409B - Preparation method for graphite carbon material - Google Patents
Preparation method for graphite carbon material Download PDFInfo
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Abstract
The invention provides a preparation method for a graphite carbon material, wherein, the graphite carbon material is prepared from the following required components in parts by weight:. 99-101 parts of calcined petroleum coke dry material and 20-25 parts of melting asphalt. The preparation method comprises the following steps: (1) mixing and kneading the dry material and an adhesive and then cooling and molding the mixture; (2) calcining for the first time; (3) soaking for the first time; (4) clacining for the second time; (5) soaking for the second time; (6) calcining for the third time; and (7) carrying out a graphitization process. The novel graphite carbon material prepared in accordance with the invention has the advantages of antioxidation, good heat and corrosion resistance, excellent conductivity and good thermal shock resistance, so that the lifetime is as over three times as that of a common graphite anode.
Description
Technical field:
The present invention relates to a kind of production method of carbon element of graphite material, particularly relate to a kind of belong to a kind of anti-oxidant, high temperature resistant, corrosion-resistant, physical strength is high, electroconductibility is strong and the production method of the carbon materials that thermal shock resistance is good.
Background technology
Smelt the special-purpose high purity graphite anode of rare earth and belong to nonmetal field new tool material, be widely used in making anode in the electrolytic furnace of electrolysis rare earth metal and use.The re metal electrolyzing stove is to add the iron cover with a rectangle graphite of high purity graphite plate processing and manufacturing pond to make, put into rare-earth oxide in the stove, insert the tungsten bar energising above and make negative electrode, the arc graphite product that four quadrntnt tubes of crucible wall suspension surround plays conduction and reductive action as anode, it makes, and carbon atom reacts in Sauerstoffatom in the rare-earth oxide and the graphite anode, displaces rare earth metal simple substance or alloy.So, smelt rare earth special graphite anode and belong to a kind of continuous consumption material, that graphite anode only possesses is anti-oxidant, high temperature resistant, corrosion-resistant, electroconductibility and characteristics such as thermal shock resistance is good, long service life, unit consumption is few, output is big, could use the lower high-quality rare earth metal of cost output.
The smelting rare earth special graphite anode of Chu Shouing mostly is waste and old electrode greatly and processes through mechanical cutting in the market, its quality instability, particles of aggregates is big, redox reaction is incomplete, consumption is big, the final product carbon residue content often exceeds standard, and other impurity also may exceed standard.In addition, the fine structure graphite anode on the market, though long service life, anti-consumption, production cost height, complex process.
Summary of the invention
The objective of the invention is to provide high-density, high purity, resistance to oxidation for smelting rare earth metal, electroconductibility is strong, thermal shock resistance good and the desirable new high-tech product of advantage such as long service life, to satisfy rare-earth industry carbon materials demand for development.
Purpose of the present invention is implemented by following technical scheme: it is described by weight, with every 99-101 part calcined petroleum coke siccative, add and dissolve pitch 20-25 part, pinch, vacuumize extrusion molding, bakes to burn the article, single-steeping, re-baking, double-steeping, three roastings and graphitization technique through preparing burden, mixing and make, its concrete making step is as follows:
(1), siccative and binding agent mix pinch, cool material, moulding
A. the preparation of calcined petroleum coke siccative: the calcined petroleum coke siccative is formulated by the calcined petroleum coke powder of 3 particle size fractions, comprising: the 1.5mm particle size fraction, and wherein granularity is that the calcined petroleum coke powder of 1.5mm accounts for 95%; 0.5mm particle size fraction, wherein granularity is that the calcined petroleum coke powder of 0.5mm accounts for 95% and the 0.074mm particle size fraction, and wherein granularity is that the calcined petroleum coke powder of 0.074mm accounts for 85%, the calcined petroleum coke powder of 3 particle size fractions by weight percentage, the calcined petroleum coke powder of 1.5mm particle size fraction is 10-12%; 0.5mm the calcined petroleum coke powder of particle size fraction is 48-50%; 0.074mm the calcined petroleum coke powder of particle size fraction is 38-40%; The percentage composition of the calcined petroleum coke powder of above-mentioned each particle size fraction is 100%; B. siccative and binding agent mix and to pinch: the siccative that above-mentioned a step is prepared and binding agent are softening temperature at 85-90 ℃ medium temperature coal pitch, at two cutter kneading machine internal heating that stir to 180-190 ℃, mix and pinched 2.5-3 hour, wherein by weight, per 99 parts of-101 parts of calcined petroleum coke siccatives add the binding agent of 20-25 part, by the cold material, extrusion molding when vacuumizing to 0.076mpa;
(2), bakes to burn the article carries out roasting with the green compact of compression moulding by bakes to burn the article technology, sinter process is: furnace temperature was raised to 350 ℃ with 12 hours from room temperature, at 12-60 hour, on average per hour heat up 5 ℃, at 60-276 hour, on average per hour heat up 1-2 ℃, at 276-432 hour, the highest flame temperature 1250-1260 ℃ of the 2-3 ℃ of roasting for the first time that on average per hour heat up, obtains baked article through 432-440 hour heating by products temperature 810-890 ℃;
(3), single-steeping
The roasting product that obtains is preheating to 300-320 ℃, 11-12 hour warm up time, it is airtight that the product of preheating is put into the high-pressure impregnation jar, and the medium temperature coal pitch by precipitation is dissolved in injection, flood the product of preheating with medium temperature coal pitch, vacuumized vacuum tightness 0.08mpa 30-40 minute, be 4.5-5 hour clamping time, and weightening finish is not less than 20% of roasting product behind the single-steeping;
(4), re-baking
Impregnated goods are carried out re-baking, re-baking technology is: furnace temperature was raised to 350 ℃ with 12 hours from room temperature, at 12-60 hour, on average per hour heat up 5 ℃, at 60-228 hour, on average per hour heat up 1-2 ℃, at 228-276 hour, on average per hour heat up 2-3 ℃, at 276-312 hour, on average per hour heat up 5-6 ℃, kept constant temperature at 312-324 hour, at 324-336 hour, on average per hour heat up 10-11 ℃, kept constant temperature at 336-360 hour, the highest flame temperature 1250-1260 ℃ of roasting for the second time, products temperature is 800-810 ℃,, obtain roasting product through 360 hours heating;
(5), double-steeping
With carrying out double-steeping with the same method of single-steeping, weightening finish is not less than 12% of roasting product behind the double-steeping;
(6) three roastings
With carrying out three roastings with the same technology of re-baking, obtain roasting product;
(7), graphitization technique
To pack in the graphitizing furnace through the goods after twice dipping, three roastings, goods have been put by the combustion chamber sectional area, under airtight situation, switch on, send according to batch, carry out pyroprocessing, require the combustion chamber temperature of graphitizing furnace at 2400-2500 ℃, namely get this carbon element of graphite material, its front tile shape.
The invention has the advantages that: 1, mix at siccative and binding agent and pinch, adopt the method that vacuumizes extrusion molding in the cool material, moulding process, can make goods internal structure even compact, internal particle gap pore reduces, and gas permeability reduces, and improves volume density.When 2, formulating the roasting curve, in the fugitive constituent discharge phase, strict control products temperature per hour heats up goods and is no more than 0.5 ℃, and making binding agent even charing in goods is net distribution, generates good graphite microcrystal, prevents that crackle from producing, and improves yield rate; 3, promote the every physical and chemical index of product through dipping, roasting and graphitization technique again.All do not appear in the newspapers at home through vacuumizing the high purity graphite anode product that hot extrusion molding makes, belong to leading domestic, and every physical and chemical index all is better than detecting the physical and chemical index of product report; 4, technology of the present invention is simple, is convenient to operation, and production cost is low.
Embodiment:
Embodiment 1: specification is (430mm * 950mm * 70mm)
(1), siccative and binding agent mix pinch, cool material, moulding
With true density more than 2.08%, the powder of 1.5mm, 0.5mm that the ash content high-quality calcined petroleum coke that (comprises 0.3) below 0.3 obtains after abrasive dust, screening, three particle size fractions of 0.074mm is according to 74kg, 350kg and 276kg proportioning, do to mix through 45 minutes, be the 700kg siccative after being heated to 180 ℃; Add softening temperature again at 85 ℃-90 ℃ medium temperature coal pitch 147kg, mixing the press of packing into after pinching 2.5 hours under 185 ℃, vacuumize the 0.076mpa extrusion molding.
(2), bakes to burn the article
The green compact of compression moulding are carried out roasting by bakes to burn the article technology, sinter process is: furnace temperature was raised to 350 ℃ with 12 hours from room temperature, at 12-60 hour, on average per hour heat up 5 ℃, at 60-276 hour, on average per hour heat up 1-2 ℃, at 276-432 hour, the highest flame temperature 1250-1260 ℃ of the 2-3 ℃ of roasting for the first time that on average per hour heat up, 810 ℃ of products temperatures obtain baked article through 432 hours heating;
(3), single-steeping
The roasting product that obtains is preheating to 300 ℃, 11 hours warm up time, it is airtight that the product of preheating is put into the high-pressure impregnation jar, and the medium temperature coal pitch by precipitation is dissolved in injection, flood the product of preheating with medium temperature coal pitch, vacuumized vacuum tightness 0.08mpa 30 minutes, be 5 hours clamping time, and weightening finish is not less than 20% of roasting product behind the single-steeping;
(4), re-baking
Impregnated goods are carried out re-baking, re-baking technology is: furnace temperature was raised to 350 ℃ with 12 hours from room temperature, at 12-60 hour, on average per hour heat up 5 ℃, at 60-228 hour, on average per hour heat up 1-2 ℃, at 228-276 hour, on average per hour heat up 2-3 ℃, at 276-312 hour, on average per hour heat up 5-6 ℃, kept constant temperature at 312-324 hour, at 324-336 hour, on average per hour heat up 10-11 ℃, kept constant temperature at 336-360 hour, 1250 ℃ of the highest flame temperatures of roasting for the second time, products temperature is 800 ℃, obtains roasting product through 360 hours heating;
(5), double-steeping
The re-baking product that obtain are preheating to 300 ℃, 11 hours warm up time, it is airtight that the product of preheating is put into the high-pressure impregnation jar, and the medium temperature coal pitch by precipitation is dissolved in injection, flood the product of preheating with medium temperature coal pitch, vacuumized vacuum tightness 0.08mpa 30 minutes, be 5 hours clamping time, and weightening finish is not less than 12% of roasting product behind the double-steeping;
(6) three roastings
Impregnated goods are carried out three roastings, three times sinter process is: furnace temperature was raised to 350 ℃ with 12 hours from room temperature, at 12-60 hour, on average per hour heat up 5 ℃, at 60-228 hour, on average per hour heat up 1-2 ℃, at 228-276 hour, on average per hour heat up 2-3 ℃, at 276-312 hour, on average per hour heat up 5-6 ℃, kept constant temperature at 312-324 hour, at 324-336 hour, on average per hour heat up 10-11 ℃, kept constant temperature at 336-360 hour, 1250 ℃ of three the highest flame temperatures of roasting, products temperature is 800 ℃, obtains roasting product three times through 360 hours heating
(7), graphitization technique
To pack in the graphitizing furnace through the goods after twice dipping, three roastings, put goods by the combustion chamber sectional area, under airtight situation, switch on, send according to batch, carry out pyroprocessing, require the combustion chamber temperature of graphitizing furnace at 2400 ℃, namely get this carbon element of graphite material.
Embodiment 2: specification is (430mm * 950mm * 70mm)
(1), siccative and binding agent mix pinch, cool material, moulding
With true density more than 2.08%, the powder of 1.5mm, 0.5mm that the ash content high-quality calcined petroleum coke that (comprises 0.3) below 0.3 obtains after abrasive dust, screening, three particle size fractions of 0.074mm is according to 84kg, 336kg and 280kg proportioning, do to mix through 45 minutes, be the 700kg siccative after being heated to 180 ℃; Add softening temperature again at 85 ℃-90 ℃ medium temperature coal pitch 147kg, mixing the press of packing into after pinching 3 hours under 185 ℃, vacuumize the 0.076mpa extrusion molding.
(2), bakes to burn the article
The green compact of compression moulding are carried out roasting by bakes to burn the article technology, sinter process is: furnace temperature was raised to 350 ℃ with 12 hours from room temperature, at 12-60 hour, on average per hour heat up 5 ℃, at 60-276 hour, on average per hour heat up 1-2 ℃, at 276-432 hour, 1260 ℃ of the 2-3 ℃ of the highest flame temperatures of roasting for the first time that on average per hour heat up, 890 ℃ of products temperatures obtain baked article through 432 hours heating;
(3), single-steeping
The roasting product that obtains is preheating to 320 ℃, 11 hours warm up time, it is airtight that the product of preheating is put into the high-pressure impregnation jar, and the medium temperature coal pitch by precipitation is dissolved in injection, flood the product of preheating with medium temperature coal pitch, vacuumized vacuum tightness 0.08mpa 40 minutes, be 4.5 hours clamping time, and weightening finish is not less than 20% of roasting product behind the single-steeping;
(4), re-baking
Impregnated goods are carried out re-baking, re-baking technology is: furnace temperature was raised to 350 ℃ with 12 hours from room temperature, at 12-60 hour, on average per hour heat up 5 ℃, at 60-228 hour, on average per hour heat up 1-2 ℃, at 228-276 hour, on average per hour heat up 2-3 ℃, at 276-312 hour, on average per hour heat up 5-6 ℃, kept constant temperature at 312-324 hour, at 324-336 hour, on average per hour heat up 10-11 ℃, kept constant temperature at 336-360 hour, 1260 ℃ of the highest flame temperatures of roasting for the second time, products temperature is 810 ℃, obtains roasting product through 360 hours heating;
(5), double-steeping
The re-baking product that obtain are preheating to 320 ℃, 12 hours warm up time, it is airtight that the product of preheating is put into the high-pressure impregnation jar, and the medium temperature coal pitch by precipitation is dissolved in injection, flood the product of preheating with medium temperature coal pitch, vacuumized vacuum tightness 0.08mpa 40 minutes, be 4.5 hours clamping time, and weightening finish is not less than 12% of roasting product behind the double-steeping;
(6) three roastings
Impregnated goods are carried out three roastings, three times sinter process is: furnace temperature was raised to 350 ℃ with 12 hours from room temperature, at 12-60 hour, on average per hour heat up 5 ℃, at 60-228 hour, on average per hour heat up 1-2 ℃, at 228-276 hour, on average per hour heat up 2-3 ℃, at 276-312 hour, on average per hour heat up 5-6 ℃, kept constant temperature at 312-324 hour, at 324-336 hour, on average per hour heat up 10-11 ℃, kept constant temperature at 336-360 hour, 1260 ℃ of three the highest flame temperatures of roasting, products temperature is 810 ℃, obtains roasting product three times through 360 hours heating
(7), graphitization technique
To pack in the graphitizing furnace through the goods after twice dipping, three roastings, put goods by the combustion chamber sectional area, under airtight situation, switch on, send according to batch, carry out pyroprocessing, require the combustion chamber temperature of graphitizing furnace at 2500 ℃, namely get this carbon element of graphite material.
Embodiment 3: specification is (430mm * 950mm * 70mm)
(1), siccative and binding agent mix pinch, cool material, moulding
With true density more than 2.08%, the powder of 1.5mm, 0.5mm that the ash content high-quality calcined petroleum coke that (comprises 0.3) below 0.3 obtains after abrasive dust, screening, three particle size fractions of 0.074mm is according to 84kg, 343kg and 273kg proportioning, do to mix through 45 minutes, be the 700kg siccative after being heated to 180 ℃; Add softening temperature again at 85 ℃-90 ℃ medium temperature coal pitch 147kg, mixing the press of packing into after pinching 3 hours under 185 ℃, vacuumize the 0.076mpa extrusion molding.
(2), bakes to burn the article
The green compact of compression moulding are carried out roasting by bakes to burn the article technology, sinter process is: furnace temperature was raised to 350 ℃ with 12 hours from room temperature, at 12-60 hour, on average per hour heat up 5 ℃, at 60-276 hour, on average per hour heat up 1-2 ℃, at 276-432 hour, 1255 ℃ of the 2-3 ℃ of the highest flame temperatures of roasting for the first time that on average per hour heat up, 860 ℃ of products temperatures obtain baked article through 432 hours heating;
(3), single-steeping
The roasting product that obtains is preheating to 320 ℃, 11 hours warm up time, it is airtight that the product of preheating is put into the high-pressure impregnation jar, and the medium temperature coal pitch by precipitation is dissolved in injection, flood the product of preheating with medium temperature coal pitch, vacuumized vacuum tightness 0.08mpa 36 minutes, be 4.7 hours clamping time, and weightening finish is not less than 20% of roasting product behind the single-steeping;
(4), re-baking
Impregnated goods are carried out re-baking, re-baking technology is: furnace temperature was raised to 350 ℃ with 12 hours from room temperature, at 12-60 hour, on average per hour heat up 5 ℃, at 60-228 hour, on average per hour heat up 1-2 ℃, at 228-276 hour, on average per hour heat up 2-3 ℃, at 276-312 hour, on average per hour heat up 5-6 ℃, kept constant temperature at 312-324 hour, at 324-336 hour, on average per hour heat up 10-11 ℃, kept constant temperature at 336-360 hour, 1256 ℃ of the highest flame temperatures of roasting for the second time, products temperature is 807 ℃, obtains roasting product through 360 hours heating;
(5), double-steeping
The re-baking product that obtain are preheating to 312 ℃, 11 hours warm up time, it is airtight that the product of preheating is put into the high-pressure impregnation jar, and the medium temperature coal pitch by precipitation is dissolved in injection, flood the product of preheating with medium temperature coal pitch, vacuumized vacuum tightness 0.08mpa 37 minutes, be 4.5 hours clamping time, and weightening finish is not less than 12% of roasting product behind the double-steeping;
(6) three roastings
Impregnated goods are carried out three roastings, three times sinter process is: furnace temperature was raised to 350 ℃ with 12 hours from room temperature, at 12-60 hour, on average per hour heat up 5 ℃, at 60-228 hour, on average per hour heat up 1-2 ℃, at 228-276 hour, on average per hour heat up 2-3 ℃, at 276-312 hour, on average per hour heat up 5-6 ℃, kept constant temperature at 312-324 hour, at 324-336 hour, on average per hour heat up 10-11 ℃, kept constant temperature at 336-360 hour, 1256 ℃ of three the highest flame temperatures of roasting, products temperature is 806 ℃, obtains roasting product three times through 360 hours heating
(7), graphitization technique
To pack in the graphitizing furnace through the goods after twice dipping, three roastings, put goods by the combustion chamber sectional area, under airtight situation, switch on, send according to batch, carry out pyroprocessing, require the combustion chamber temperature of graphitizing furnace at 2460 ℃, namely get this carbon element of graphite material.
Embodiment 4:
The carbon element of graphite material that embodiment 1-3 makes, its carbon content is respectively after testing: 99.6%, 99.58%, 99.8%, all greater than 99.5%; Volume density is respectively: 1.77g/cm
3, 1.79g/cm
3, 1.76g/cm
3, all greater than 1.75g/cm
3Be respectively than resistance: 6.8 μ Ω m, 6.9 μ Ω m, 6.4 μ Ω m, all less than 7 μ Ω m; Folding strength is respectively: 41MPa, 40.7MPa, 42MPa, all greater than 40MPa; The unit consumption time is respectively: 83 hours, 81 hours, 84 hours, and respectively greater than 80 hours.
The advanced index contrast of this carbon element of graphite material technology index and domestic same industry situation is as shown in the table:
| Index name | Quality index | Advanced index of the same trade |
| Carbon content (purity) | ≥99.5％ | ≥98％ |
| Volume density | ≥1.75g/cm 3 | ≥1.68g/cm 3 |
| Compare resistance | ≤7μΩm | ≤8.5μΩm |
| Folding strength | ≥40MPa | ≥38MPa |
| The unit consumption time | 〉=80 hours | 〉=50 hours |
As can be seen from the above table, the graphite anode product performance index that makes of present method has reached leading domestic level.
Claims (1)
1. the production method of a carbon element of graphite material, it is characterized in that, described by weight, with every 99-101 part calcined petroleum coke siccative, add and dissolve pitch 20-25 part, pinch, vacuumize extrusion molding, bakes to burn the article, single-steeping, re-baking, double-steeping, three roastings and graphitization technique through preparing burden, mixing and make, its concrete making step is as follows:
(1), siccative and binding agent mix pinch, cool material, moulding
A. the preparation of calcined petroleum coke siccative: the calcined petroleum coke siccative is formulated by the calcined petroleum coke powder of 3 particle size fractions, comprising: the 1.5mm particle size fraction, and wherein granularity is that the calcined petroleum coke powder of 1.5mm accounts for 95%; 0.5mm particle size fraction, wherein granularity is that the calcined petroleum coke powder of 0.5mm accounts for 95% and the 0.074mm particle size fraction, wherein granularity be the calcined petroleum coke powder of 0.074mm account for 85%, 3 particle size fraction the calcined petroleum coke powder by weight percentage: the calcined petroleum coke powder of 1.5mm particle size fraction is 10-12%; 0.5mm the calcined petroleum coke powder of particle size fraction is 48-50%; 0.074mm the calcined petroleum coke powder of particle size fraction is 38-40%; The percentage composition of the calcined petroleum coke powder of above-mentioned each particle size fraction is 100%;
B. siccative and binding agent mix and to pinch: the siccative that above-mentioned a step is prepared and binding agent are softening temperature at 85-90 ℃ medium temperature coal pitch, at two cutter kneading machine internal heating that stir to 180-190 ℃, mix and pinched 2.5-3 hour, wherein by weight, per 99 parts-101 parts calcined petroleum coke siccative adds the binding agent of 20-25 part, by the cold material, extrusion molding when vacuumizing to 0.076mpa;
(2), bakes to burn the article
The green compact of compression moulding are carried out roasting by bakes to burn the article technology, sinter process is: furnace temperature was raised to 350 ℃ with 12 hours from room temperature, at 12-60 hour, on average per hour heat up 5 ℃, at 60-276 hour, on average per hour heat up 1-2 ℃, at 276-432 hour, on average per hour heat up 2-3 ℃ the highest flame temperature 1250-1260 ℃ of roasting for the first time, products temperature 890-900 ℃, obtain the bakes to burn the article goods through 432-440 hour heating;
(3), single-steeping
The bakes to burn the article goods that obtain are preheating to 300 ℃-320 ℃, 11-12 hour warm up time, it is airtight that the product of preheating is put into the high-pressure impregnation jar, and the medium temperature coal pitch by precipitation is dissolved in injection, flood the product of preheating with medium temperature coal pitch, vacuumized 30-40 minute, when vacuum tightness reaches 0.08mpa, be 4.5-5 hour clamping time, and weightening finish is not less than 20% of roasting product behind the single-steeping;
(4), re-baking
Impregnated goods are carried out re-baking, re-baking technology is: furnace temperature was raised to 350 ℃ with 12 hours from room temperature, at 12-60 hour, on average per hour heat up 5 ℃, at 60-228 hour, on average per hour heat up 1-2 ℃, at 228-276 hour, on average per hour heat up 2-3 ℃, at 276-312 hour, on average per hour heat up 5-6 ℃, kept constant temperature at 312-324 hour, at 324-336 hour, on average per hour heat up 10-11 ℃, kept constant temperature at 336-360 hour, the highest flame temperature 1250-1260 ℃ of roasting for the second time, products temperature is 800-810 ℃, obtains the re-baking product through 360-365 hour heating;
(5), double-steeping
With with the same method of single-steeping the re-baking product being carried out double-steeping, weightening finish is not less than 12% of re-baking product behind the double-steeping;
(6) three roastings
With with the same technology of re-baking the re-baking product of double-steeping being carried out three roastings, obtain roasting product three times;
(7), graphitization technique
To pack in the graphitizing furnace through three roasting products after twice dipping, three roastings, put goods by the combustion chamber sectional area, under airtight situation, switch on, send according to batch, carry out pyroprocessing, require the combustion chamber temperature of graphitizing furnace at 2400-2500 ℃, namely get this carbon element of graphite material.
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| CN112745123A (en) * | 2021-01-25 | 2021-05-04 | 焦作钧菲津材科技有限公司 | Preparation method of carbon material |
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| CN1885598A (en) * | 2006-07-10 | 2006-12-27 | 深圳市贝特瑞电子材料有限公司 | Composite carbon negative electrode material of lithium ion power battery and its preparation method |
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| US20050254545A1 (en) * | 2004-05-12 | 2005-11-17 | Sgl Carbon Ag | Graphite electrode for electrothermic reduction furnaces, electrode column, and method of producing graphite electrodes |
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| CN1048834A (en) * | 1990-05-18 | 1991-01-30 | 东新电碳厂 | The manufacture method of carbon materials |
| CN1885598A (en) * | 2006-07-10 | 2006-12-27 | 深圳市贝特瑞电子材料有限公司 | Composite carbon negative electrode material of lithium ion power battery and its preparation method |
| CN101417794A (en) * | 2007-10-26 | 2009-04-29 | 顾向宏 | Production manufacturing method of high rate lithium ionic cell cathode F series material |
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