CN101286556A - Graphitic cladding method by nano-scale mesophase asphalt - Google Patents
Graphitic cladding method by nano-scale mesophase asphalt Download PDFInfo
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- CN101286556A CN101286556A CNA200710021378XA CN200710021378A CN101286556A CN 101286556 A CN101286556 A CN 101286556A CN A200710021378X A CNA200710021378X A CN A200710021378XA CN 200710021378 A CN200710021378 A CN 200710021378A CN 101286556 A CN101286556 A CN 101286556A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to a preparation method for secondary battery cathode material, more particularly to a preparation method thereof which is formed by coating graphite by using nano-intermediate phase asphalt. The key point of the method is that nano-processing is carried out to the intermediate phase asphalt which is in semi-liquid state, the nano-intermediate phase asphalt in the semi-liquid state is sprayed on the substrate surface of the graphite by a nano-spray device, then even coating is realized, finally, the secondary battery cathode material is obtained by the traditional processes of drying, carbonization and graphitization. The adoption of the method can improve the coating evenness and the spherical completeness in a greater degree, thus further reducing the first-time irreversible capacity of the graphite, improving the cyclical stability and having the advantages that the charging and discharging voltage of the secondary battery is low, the charging and discharging platform is long and the cycle life is good.
Description
Technical field
The present invention relates to secondary battery cathode material preparation method, especially with the preparation method of nanoscale mesophase pitch secondary battery cathode material that coated graphite is formed.
Background technology
Secondary cell has been that the battery of new generation after Ni-MH battery is representative with the lithium ion battery since the eighties of last century the nineties, because of its have operating voltage height, energy density big, have extended cycle life, advantages such as self discharge is little, memory-less effect, become the chemical power source of present high-grade consumer electronics first-selection, and be penetrated into sophisticated technology fields such as Aero-Space, military affairs.Be accompanied by the demand that it grows with each passing day, secondary cell is just becoming the emphasis and the focus of new century scientific and technical research and exploitation.
Wherein the charge/discharge capacity of native graphite Yin Qigao, favorable charge-discharge platform, wide material sources, cost is low and the extensive use that obtains.But because the degree of graphitization of native graphite is higher, the edge of its crystallite and the crystal structure between the bottom surface and other physicochemical properties difference are bigger, mainly occur in the marginal portion of crystallite with the decomposition reaction of electrolyte.So the compactness of the purification membrane that generates is relatively poor, in charging process, the common embedding of solvation lithium ion takes place easily, causes the expansion and the collapse of graphite linings, has increased irreversible capacity.After native graphite is handled through physics or chemical method in addition, exist the shortcoming with the adhesive property difference of pole plate, be easy to come off in the cycle charge discharge electric process, influenced cycle life, especially reduced the cycle life of high current charge-discharge from pole plate.
In order to improve the chemical property of natural graphite material, people carry out physical and chemical modified and finishing by the whole bag of tricks to native graphite, and obtained corresponding effects, as native graphite is pulverized, classification and be processed into spheric granules, improved tap density, adopt the method for various surface modifications to improve the chemical property of graphite in addition in addition, a kind of employing thermal oxidation graphite powder is disclosed as Japan Patent No.2000-261046, change the surface state of graphite powder, though improved the reactivity of negative material and electrolyte, discharge capacity is lower than native graphite.United States Patent (USP) U.S.Pat.No.6403259 discloses a kind of employing and has ground native graphite or Delanium surface coating one deck material with carbon element, improved the high temperature self-discharge performance and the cryogenic property of negative material, but the performance of others is not fully up to expectations.Also have United States Patent (USP) U.S.Pat.No.5908715 to adopt organic solvent dissolution epoxy resin, polyparaphenylene to coat pyrolytic carbon in addition at graphite surface, Chinese patent CN1224251A adopts ethanol dissolving phenolic resins or Lauxite coated graphite, Chinese patent CN1304187A is with the organic solvent solution coated graphite of polyacrylonitrile, Kynoar, epoxy resin etc., there is environmental pollution in said method, coat that the back graphite granule is easy to bond and pulverization process afterwards in be easy to cause the breakage that comes off of coating layer, influenced the overall performance of negative material.
More than several method for coating excessive and the graphite microparticles below the 15 μ m often had can't be configured as sphere and cause coating uneven phenomenon and produce because of the coating molecule.
Adopt nanometer materials coated graphite formation secondary battery cathode material and this material preparation method to become an important channel that addresses the above problem, adopt accurate nano carbon material in one dimension that native graphite is carried out modification as mentioning among the Chinese patent CN1670991, but this patent application does not provide specific interphase material to combine the formed concrete negative material product in back with graphite, does not provide how to make the effective concrete preparation method who combines of carbon nano-material and graphite substrate yet.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method who adopts the secondary battery cathode material of nanoscale mesophase pitch coated graphite.
For achieving the above object, technical scheme of the present invention is, adopts the nanoscale mesophase pitch that graphite is coated, and its method step is as follows:
(1) graphite microparticles of 60%-90% is put in the pyroreaction still that adds inert gas shielding earlier, pyroreaction still heating rate is to heat up that 100 ℃, warm-up time are 3-5 hour, to make the temperature in the pyroreaction still be 300 ℃-500 ℃ in per 1 hour, the mixing speed of pyroreaction still is 60-300 rev/min, graphite microparticles bone dry and burn some pollutants in the pyroreaction still;
(2) make the pyroreaction still be cooled to 200 ℃-300 ℃, this pyroreaction temperature in the kettle near but be no more than the softening point of nanoscale mesophase pitch;
(3) the 10%-40% nanoscale mesophase pitch that will be used for coating layer is input to heat pipe and heats 3-10 second, making the nanoscale mesophase pitch temperature through superheater tube is 200 ℃-350 ℃, this temperature is a little more than the softening point of nanoscale mesophase pitch, thereby obtains nanoscale semiliquid mesophase pitch;
(4) will deliver to nano-nozzle through the superheater tube semiliquid nanoscale mesophase pitch that obtains of heating, the nanoscale mesophase pitch droplet that sprays at a high speed through nano-nozzle enters into described pyroreaction still, the mixing speed of pyroreaction still is 60-300 rev/min, in the pyroreaction still, nanoscale mesophase pitch droplet mixing coated graphite microparticles 2-3 hour, this process pyroreaction temperature in the kettle is 200 ℃-300 ℃, this temperature near but be no more than the softening point of nanoscale mesophase pitch, the pressure in the pyroreaction still is 10
-5-10
-3Pa;
(5) coated graphite is sent into vacuum drying oven from the pyroreaction still by the road, is filled with inert gas (helium, neon, argon) in the vacuum drying oven, and temperature is at 400 ℃-500 ℃ in the vacuum drying oven, and the vacuumize furnace pressure is 10
-5-10
-3Pa, be 2-3 hour drying time;
(6) coated graphite after the dry reprocessing is sent into the high temperature cabonization vacuum furnace by the road again, is filled with inert gas in the high temperature cabonization vacuum furnace, and the pressure in the high temperature cabonization vacuum furnace is 10
-4-10
-1Pa, the temperature rise rate of high temperature cabonization vacuum furnace is for per hour heating up 100 ℃, and the temperature that makes the high temperature cabonization vacuum furnace is 700-1300 ℃, and the carbonisation time is 12-20 hour;
(7) coated graphite after the carbonization treatment is sent into the high temperature graphitization vacuum furnace by the road again, is filled with inert gas (helium, neon, argon) in the high temperature graphitization vacuum furnace, and the pressure in the high temperature graphitization vacuum furnace is 10
-4-10
-1Pa, the temperature rise rate of high temperature graphitization vacuum furnace is for per hour heating up 100 ℃, and the temperature that makes the high temperature graphitization vacuum furnace is 1800-3000 ℃, and the graphitizing process time is 12-20 hour, obtains uniform coated graphite microparticles.
In above-mentioned preparation method, described inert gas is helium or neon or argon gas, He-Ne gaseous mixture, helium is argon-mixed, neon is argon-mixed, He-Ne is argon-mixed.
In above-mentioned preparation method, described nanoscale mesophase pitch is mesophase pitch to be immersed nano-milled machine carry out obtaining in wet lapping 2-3 hour, and the granularity of grinding the back mesophase pitch is 30nm to 50nm.
In above-mentioned preparation method, described graphite microparticles is natural micro crystal graphite, amorphous graphite, amorphous graphite, crystalline flake graphite, electrographite, and granularity is between 5-40 μ m.
The invention has the beneficial effects as follows, adopt nanoscale mesophase pitch coated graphite can go up largely to improve and coat the uniformity and spherical integrity degree, yet further reduce the irreversible capacity first of graphite, improve cyclical stability, kept low to charging/discharging of secondary cell voltage, charge and discharge platform is long, the advantage that cycle life is good.
Description of drawings:
Fig. 1 is the Electronic Speculum figure (multiplication factor is 1000 times) before graphite microparticles coats without the nanoscale mesophase pitch.
Fig. 2 is the Electronic Speculum figure (multiplication factor is 1000 times) after mesophase pitch coating of graphite microparticles process nanoscale and the carbonization.
Fig. 3 coats through the nanoscale mesophase pitch to pass through graphited graphite microparticles Electronic Speculum figure (multiplication factor is 1000 times) again.
Fig. 4 is that preparation method's flow process of the present invention and preparation facilities are formed schematic diagram.
In the above accompanying drawing, the 1st, mesophase pitch raw material, the 2nd, graphite microparticles, the 3rd, nano-milled machine, the 4th, heat pipe, the 5th, nano-nozzle, the 6th, pyroreaction still, the 7th, vacuum drying oven, the 8th, high temperature cabonization vacuum furnace, the 9th, high temperature graphitization vacuum furnace, the 10th, coated graphite.
Embodiment
Embodiment one:
The equipment of this example is formed as shown in Figure 4.Complete equipment all is in whole sealing status by pipeline connection.Wherein nano-milled machine is selected the nano-milled machine of DRAIS PML-H/V universal type for use.
At first 75 kilograms of natural micro crystal graphites 2 are put in the pyroreaction still 6, charge into helium, neon, argon mixture gas in the pyroreaction still, the mixing speed of pyroreaction still is 220 rev/mins, per hour to rise 100 ℃ heating rate, heated 4 hours, the temperature in the pyroreaction still is risen to 400 ℃.Natural micro crystal graphite is finished drying in the pyroreaction still, the minute quantity pollutant is also burned clean.Heated in 4 hours finish after, make the pyroreaction still be cooled to 240 ℃, this temperature near but be no more than the softening point of nanoscale mesophase pitch so that natural micro crystal graphite can mix coating preferably with the nanoscale mesophase pitch droplet that sprays into.
With the above-mentioned steps while, 25 kilograms of mesophase pitch 1 are immersed in the nano-milled machine 2, adopt the wet lapping method, ground 2.5 hours, and, be the nanoscale mesophase pitch of 30nm to 50nm with phase granularity in the middle of guaranteeing with the granularity that the back mesophase pitch is ground in the detection of Mastersizer 2000-grain size analysis instrument.Be input in the heat pipe 4 and heated for 7 seconds with being about to the nanoscale mesophase pitch, making the nanoscale mesophase pitch temperature through superheater tube 4 is 240 ℃, this temperature near but be no more than the softening point of nanoscale mesophase pitch, thereby obtain nanoscale semiliquid mesophase pitch.Nanoscale semiliquid mesophase pitch is directly sprayed in the pyroreaction still by nano-nozzle, with natural micro crystal graphite mixing coating wherein, the mixing speed of pyroreaction still is 220 rev/mins, spraying mix the coating process through the time 2.5 hours, the pressure in the pyroreaction still is 10
-4Pa, temperature maintains 240 ℃ all the time.
Will be coated graphite send into vacuum drying oven 7 from pyroreaction still 6 by the road and carry out dried, be filled with helium, neon, argon mixed inert gas in the vacuum drying oven, temperature is at 450 ℃ in the vacuum drying oven, the vacuumize furnace pressure is 10
-4Pa, be 2.5 hours drying time.
Coated graphite after the dry reprocessing is sent into high temperature cabonization vacuum furnace 8 by the road again carry out carbonization treatment, be filled with helium, neon, argon mixed inert gas in the high temperature cabonization vacuum furnace, the pressure in the high temperature cabonization vacuum furnace is 10
-3Pa, the temperature rise rate of high temperature cabonization vacuum furnace is for per hour heating up 100 ℃, and the temperature that makes the high temperature cabonization vacuum furnace is 1200 ℃, and the carbonisation time is 17 hours.
Coated graphite after the carbonization treatment sent into by the road again carry out graphitization processing in the high temperature graphitization vacuum furnace 9, be filled with helium, neon, argon mixed inert gas in the high temperature graphitization vacuum furnace, the pressure in the high temperature graphitization vacuum furnace is 10
-3Pa, the temperature rise rate of high temperature graphitization vacuum furnace are for per hour heating up 100 ℃, and making the temperature in the high temperature graphitization vacuum furnace is 2500 ℃, and the graphitizing process time is 17 hours, obtains uniform coated graphite microparticles 10.
The coated graphite microparticles that present embodiment obtains is used for secondary battery cathode material, and its initial charge capacity (mAh/g) is 392.36, and discharge capacity (mAh/g) is that 365.20,500 circulation volumes remain 84.7% first.
Embodiment two:
Graphite microparticles drying in the present embodiment, nanoscale mesophase pitch form and semiliquidization, nanoscale mesophase pitch and graphite microparticles to mix all processes of coating identical with embodiment one, but when coated graphite carries out carbonization, carburizing temperature is 1250 ℃, 2800 ℃ of graphitization temperatures, resulting coated graphite microparticles is used for secondary battery cathode material, its initial charge capacity (mAh/g) is 390.52, discharge capacity (mAh/g) is that 368.51,500 circulation volumes remain 86.5% first.
Embodiment three:
Graphite microparticles drying in the present embodiment, nanoscale mesophase pitch form and semiliquidization, nanoscale mesophase pitch and graphite microparticles to mix all processes of coating identical with embodiment one, but when coated graphite carries out carbonization, carburizing temperature is 1300 ℃, 3000 ℃ of graphitization temperatures, resulting coated graphite microparticles is used for secondary battery cathode material, its initial charge capacity (mAh/g) is 388.40, discharge capacity (mAh/g) is that 369.32,500 circulation volumes remain 88.1% first.
Claims (4)
1, a kind of method of nanoscale mesophase pitch coated graphite is characterized in that:
(1) graphite microparticles of 60%-90% is put in the pyroreaction still that adds inert gas shielding earlier, pyroreaction still heating rate is to heat up that 100 ℃, warm-up time are 3-5 hour, to make the temperature in the pyroreaction still be 300 ℃-500 ℃ in per 1 hour, pyroreaction still mixing speed is 60-300 rev/min, graphite microparticles bone dry and burn some pollutants in the pyroreaction still;
(2) make the pyroreaction still be cooled to 200 ℃-300 ℃, this pyroreaction temperature in the kettle near but be no more than the softening point of nanoscale mesophase pitch;
(3) the 10%-40% nanoscale mesophase pitch that will be used for coating layer is input to heat pipe and heats 3-10 second, making the nanoscale mesophase pitch temperature through superheater tube is 200 ℃-350 ℃, this temperature is a little more than the softening point of nanoscale mesophase pitch, thereby obtains nanoscale semiliquid mesophase pitch;
(4) will deliver to nano-nozzle through the superheater tube semiliquid nanoscale mesophase pitch that obtains of heating, the nanoscale mesophase pitch droplet that sprays at a high speed through nano-nozzle enters into described pyroreaction still, the mixing speed of pyroreaction still is 60-300 rev/min, in the pyroreaction still, nanoscale mesophase pitch droplet mixing coated graphite microparticles 2-3 hour, this process pyroreaction temperature in the kettle is 200 ℃-300 ℃, this temperature near but be no more than the softening point of nanoscale mesophase pitch, the pressure in the pyroreaction still is 10
-5-10
-3Pa;
(5) coated graphite is sent into vacuum drying oven from the pyroreaction still by the road, is filled with inert gas (helium, neon, argon) in the vacuum drying oven, and temperature is at 400 ℃-500 ℃ in the vacuum drying oven, and the vacuumize furnace pressure is 10
-5-10
-3Pa, be 2-3 hour drying time;
(6) coated graphite after the dry reprocessing is sent into the high temperature cabonization vacuum furnace by the road again, is filled with inert gas in the high temperature cabonization vacuum furnace, and the pressure in the high temperature cabonization vacuum furnace is 10
-4-10
-1Pa, the temperature rise rate of high temperature cabonization vacuum furnace is for per hour heating up 100 ℃, and the temperature that makes the high temperature cabonization vacuum furnace is 700-1300 ℃, and the carbonisation time is 12-20 hour;
(7) coated graphite after the carbonization treatment is sent into the high temperature graphitization vacuum furnace by the road again, is filled with inert gas in the high temperature graphitization vacuum furnace, and the pressure in the high temperature graphitization vacuum furnace is 10
-4-10
-1Pa, the temperature rise rate of high temperature graphitization vacuum furnace is for per hour heating up 100 ℃, and the temperature that makes the high temperature graphitization vacuum furnace is 1800-3000 ℃, and the graphitizing process time is 12-20 hour, obtains uniform coated graphite microparticles.
2, the preparation method of nanoscale coated graphite according to claim 1 is characterized in that: described inert gas is helium or neon or argon gas, He-Ne gaseous mixture, helium is argon-mixed, neon is argon-mixed, He-Ne is argon-mixed.
3, the preparation method of nanoscale coated graphite according to claim 1, it is characterized in that: described nanoscale mesophase pitch is mesophase pitch to be immersed nano-milled machine carry out obtaining in wet lapping 2-3 hour, and the granularity of grinding the back mesophase pitch is 30nm to 50nm.
4, the preparation method of nanoscale coated graphite according to claim 1 is characterized in that: above-mentioned graphite microparticles is natural micro crystal graphite, amorphous graphite, amorphous graphite, crystalline flake graphite, electrographite, and granularity is between 5-40 μ m.
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