CN101412510A - Composite graphite for lithium secondary battery and manufacturing method thereof - Google Patents
Composite graphite for lithium secondary battery and manufacturing method thereof Download PDFInfo
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- CN101412510A CN101412510A CNA2007101635505A CN200710163550A CN101412510A CN 101412510 A CN101412510 A CN 101412510A CN A2007101635505 A CNA2007101635505 A CN A2007101635505A CN 200710163550 A CN200710163550 A CN 200710163550A CN 101412510 A CN101412510 A CN 101412510A
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Abstract
The invention discloses composite graphite used for a lithium secondary battery and a production method thereof. The production method is as follows: spherical graphite is taken as a substrate, preheated by a heating mixing roll until the temperature of powder is between 55 and 85 DEG C, added with a clad material (a mixed liquid which consists of coal tar, maltha and liquid resin, and fully mixed; and the mixture is filled into a graphite container for macromolecular treatment, sent into a direct-fired cemented carbonized oven for carbonizing treatment, and subjected to screen stencil or airflow classification to obtain composite graphite powder. The production method simplifies the production procedure and saves the production cost; the product is taken as a cathode material of the lithium secondary battery, so that the lithium secondary battery has high initial charging and discharging efficiency and large discharge quantity.
Description
Technical field
The present invention relates to a kind of composite graphite and manufacture method thereof that is used for lithium secondary battery, be meant that especially a kind of simplification manufacturing process saves cost of manufacture, obtain the negative material of lithium secondary battery, its battery of making obtains higher loading capacity, and has high discharging efficiency.
Background technology
Along with the electronic technology develop rapidly with reach its maturity, people in light weight, energy is high, adaptable power supply has proposed new requirement, well known lithium ion battery is big because of the potential difference of positive and negative electrode material, can improve its energy density, reach the characteristic that volume is little, electric weight is high, and can satisfy the demand of electronic product.
The negative material of lithium ion battery is a raw material with graphite all generally, with graphite, and graphite product such as synthetic graphite after most of employing natural graphite, coke type high temp are handled and pitch-based carbon fiber.Wherein, the most convenient with obtaining of natural graphite, yet natural graphite is because of the removal of impurity, the restriction of purification worker method generally is to be consideration with the crystalline flake graphite, but with crystalline flake graphite as lithium cell cathode material, though can reach higher loading capacity demand, but because of its specific shape, contacting with ionogen in the battery can't be as the safety of approximate globe, and causes at the high speed charge-discharge characteristic low.Simultaneously with natural flake graphite during as the negative material of lithium cell, in the early stage in the charge and discharge process, the lithium complex compound that causes lithium ion and electrolytic solution reaction to be produced because of its crystallinity is high easily is attached to its surface, forms solid state electrolyte SEI film, causes the low phenomenon of initial charge.
For addressing the above problem, relevant dealer and researchist drop into this important function for of research one after another both at home and abroad, wherein as TaiWan, China patent announcement number No. 587350 patent, it mainly contains the manufacture method about the three-layer type composite graphite, but its worker method complex steps, need various equipment to carry out each step, cause manufacturing cost high.
In addition as TaiWan, China patent announcement number I262617 patent, mainly utilize liquid hybrid system that liquid resin is coated on the spherical graphite, and be heat-treated to 800-1200 ℃, make resin be cracked into amorphous carbon, suppress graphite peeling off in battery charge and discharge process, to reach the efficiency for charge-discharge at raising initial stage.Though simple with the more above-mentioned patent of its manufacturing process, but still belong to complexity, at first go spherical graphite, liquid resin and organic solvent uniform mixing, remove organic solvent with vacuum-drying again, separate broken again through Overheating Treatment 800-1200 ℃.With regard to its whole worker's method, the carrying capacity of environment that is produced at necessity, the cost burden of the interpolation of organic solvent and removal and when removing organic solvent is all worth thinking deeply about.Simultaneously, when doing cover material with single liquid resin, after the thermal treatment since the carbon stratum reticulare on pore too much, and when heat-treating with 800-1200 ℃, make the top layer amorphous carbon produce to melt and lump, coating carbon material taking place easily in separating broken process peel off, and causes specific surface area excessive and then influence the characteristic of battery.And if aspect thermal treatment temperature, time when deficiency is arranged, also cause battery distortion of materials in charge and discharge process to differ easily and cause the phenomenon of peeling off of base material and cover material, make that equally the loading capacity of battery and efficiency for charge-discharge are low.
Summary of the invention
Main purpose of the present invention aims to provide a kind of composite graphite and manufacture method thereof that is used for lithium secondary battery, and its fabrication steps can effectively be simplified flow process, and reduces production costs.
A time purpose of the present invention aims to provide a kind of composite graphite and manufacture method thereof that is used for lithium secondary battery, can further reach the reduction caking rate, avoids battery distortion of materials in charge and discharge process material that is produced that differs to peel off.
In order to achieve the above object, the present invention is a kind of composite graphite and manufacture method thereof that is used for lithium secondary battery, and it comprises the following step:
1. choose spherical graphite as base material, above-mentioned base material with the in addition preheating of heating muller, is preheated to default preheating temperature at a preheating setting-up time, drop into cover material and also give thorough mixing, said mixture is packed in the crystal vessel;
2. above-mentioned crystal vessel is delivered to and carried out high molecular in the hot blast constant temperature recirculation still of a preset temp and handle;
3. move into straight the baked wheaten cake in the knot charring furnace after high temperature cabonization is handled again, be warming up to a preset temp and keep a Preset Time and be cooled to room temperature;
4. at last through sieving or air classification is handled and to be obtained composite graphite.
Wherein, above-mentioned graphite is to choose fixed carbon 〉=99.9%, and the crystallization aspect is d at interval
002The high pure spherical graphite of≤0.337nm is as base material.
In possible embodiments, above-mentioned base material preheating setting-up time 〉=30 minutes, its default preheating temperature is 55-85 ℃, and will mix 10 to 40 minutes in the cover material input heating muller with in the base material, above-mentioned cover material is coal tar or the viscid bitumen of softening temperature below 65 ℃, or with above-mentioned two kinds of materials and liquid resinous mixed solution, blending ratio is with (coal tar or viscid bitumen)/liquid resin=100/0-50/50, and the covering material usage ratio is about 10-40%[covering material usage ratio=cover material weight/(base material weight+batch cover material weight)].
Again, the mixture filling rate that fills in crystal vessel is 70-90%; Above-mentioned crystal vessel material degree of porosity 〉=3cc/cm
2Min, material density 〉=1.65g/cc, thermal conductivity 〉=120W/mk.
In possible embodiments, above-mentioned base material is carried out the treating processes of high molecular, setting roasting condition in its stove is, oxygen level in the stove 〉=15%, its furnace pressure is-the 10-10mm water colunm pressure that constant temperature keeps 210 ℃ in the stove, when above-mentioned crystal vessel passes through the polymer stove, crystal vessel with per hour 10-30 ℃ be warming up to Celsius≤210 ℃, overall treatment time≤15 hour.
Moreover, in the carbonization process, the straight roasting condition of burning the knot charring furnace, furnace pressure is set at 0.1-10mm water colunm pressure, air-fuel ratio 0.8-0.99, oxygen level≤300ppm, with per hour 20-120 ℃ be warming up to 1000-1600 Celsius ℃, holding temperature is 〉=2 hours the time, again it is cooled to room temperature.
See through the negative material that above-mentioned manufacture method is made, have following rerum natura, obtain volume percent at size distribution≤25 μ m[d (0.5)≤25 μ m of 50%], specific surface area≤5m
2/ g, tap density 〉=1.0g/cc, the x100% of degree of graphitization 〉=90%[(0.344000-d002)/(0.34400-0.33538)], and in the Ar Laser light Raman spectrum of wavelength 514.4nm, have 1350-1370cm
-1Peak strength I in the scope
D, to there being 1570-1630cm
-1The peak strength I of scope
GRatio I
D/ I
GThe composite stone ink powder of≤0.5 surperficial coating carbon material.
Description of drawings
Fig. 1 is the schematic flow sheet of the manufacture method of ion secondary battery cathode material lithium of the present invention;
Fig. 2 is the test loop life-span compare figure of the present invention with embodiment and battery that comparative example is made;
Fig. 3 is the cycle charge-discharge graphic representation of the embodiment of the invention-1;
Fig. 4 is the cycle charge-discharge graphic representation of the embodiment of the invention-2;
Fig. 5 is the cycle charge-discharge graphic representation of comparative example-1.
Embodiment
For further darker one deck being arranged to structure of the present invention, use and feature thereof, clearly,
Preferred embodiment is enumerated in full and accurate understanding and understanding, cooperates graphic being described in detail as follows:
At first see also shown in Figure 1ly, the present invention is a kind of composite graphite and manufacture method thereof that is used for lithium secondary battery, and it comprises following manufacturing step:
Choose fixed carbon fixed carbon 〉=99.9% earlier, the crystallization aspect is d at interval
002The high pure spherical graphite of≤0.337nm is as base material, be preheated to preset temp with the heating-type muller, drop into cover material in base material, and mixed, again said mixture is adorned Zhen and go into crystal vessel, sending into hot blast constant temperature recirculation still handles the mixture high molecular, the inner roasting of above-mentioned hot blast constant temperature recirculation still impose a condition into, oxygen level in the stove 〉=15%, its furnace pressure is-the 10-10mm water colunm pressure, constant temperature keeps 210 ℃ in the stove, and above-mentioned crystal vessel is during by the polymer stove, crystal vessel with per hour 10-30 ℃ be warming up to Celsius≤210 ℃.
Move into the straight knot charring furnace of burning again and carry out carbonizing treatment, the roasting condition of charring furnace is set in the above-mentioned carbonization process, furnace pressure is the 0.1-10mm water colunm pressure, air-fuel ratio 0.8-0.99, oxygen level≤300ppm, with per hour 20-120 ℃ be warming up to Celsius≤1000-1600 ℃, keep temperature-time for again it is cooled to room temperature after 〉=2 hours.
Handle with air-flow or screen fractionation at last, obtain volume percent at size distribution≤25 μ m[d (0.5)≤25 μ m of 50%], specific surface area≤5m
2/ g, tap density 〉=1.0g/cc, the x100% of degree of graphitization 〉=90%[(0.344000-d002)/(0.34400-0.33538)], and in the Ar Laser light Raman spectrum of wavelength 514.4nm, have 1350-1370cm
-1Peak strength I in the scope
D, to there being 1570-1630cm
-1The peak strength I of scope
GRatio I
D/ I
GThe composite stone ink powder of≤0.5 surperficial coating carbon material is in order to the negative material as lithium secondary battery.
In possible embodiments, base material warm up time 〉=30 minute, its default preheating temperature is 55-85 ℃, and in the cover material input heating muller with base material in the time of mixing be 10 to 40 minutes, above-mentioned cover material is coal tar or the viscid bitumen of softening temperature below 65 ℃, or with above-mentioned two kinds of materials and liquid resinous mixed solution, blending ratio is with (coal tar or viscid bitumen)/liquid resin=100/0-50/50, and the covering material usage ratio is about 10-40% (with the ratio of base material addition).
In possible embodiments, the mixture filling rate that mixture fills in crystal vessel is 70-90%; Above-mentioned crystal vessel material degree of porosity 〉=3cc/cm
2Min, material density 〉=1.65g/cc, thermal conductivity 〉=120W/mk.
Above-mentioned chart is a composite graphite powder experimental data of the present invention, and embodiment-1 data presentation in chart enforcement and analysis content is to select fixed carbon 〉=99.9%, and the crystallization aspect is d at interval
002The high pure spherical graphite of≤0.337nm is as base material, and after 45 minutes, the powder temperature reaches about 70 ℃ with its preheating, drops into batch cover material (coal tar) 20% again, mixes to stir after 10 minutes that mixture is filled in the crystal vessel, and its mixture filling rate is 80%.
When the high molecular treating processes, be warming up to 210 ℃ by room temperature, in 7.5 hours treatment times, oxygen level is=17.1%.
When carbonization process, top temperature is set 1450 ℃, and temperature rise rate is 40-100 ℃, and its air-fuel ratio schedules 0.85-0.95, measure of oxygen content 150ppm, and outward appearance is the Powdered loose block that has after the carbonization.
Sieve with 270 eye mesh screens at last, its screen cloth yield is 91.3%, the composite stone ink powder of gained, and median size is 17.11 μ m, specific surface area is 1.48m
2/ g, true density numerical value are 2.22g/cc, and X-ray diffraction analysis (d002) is 0.33570nm, degree of graphitization 96.29%, initial stage loading capacity 365.2mAh/g, initial charge 92.2%.
In a preferred embodiment, embodiment-2 adopts above-mentioned generation step to make composite graphite, and following data are its experimental data, are to select fixed carbon 〉=99.9%, and the crystallization aspect is d at interval
002The high pure spherical graphite of≤0.337nm is as base material, after 45 minutes, the powder temperature reaches 69 ℃ with its preheating, drops into batch cover material (coal tar and resin compound ratio are 50/50) 20% again, mix to stir after 10 minutes that mixture is filled in the crystal vessel, its mixture filling rate is 80%.
When the high molecular treating processes, be warming up to 210 ℃ by room temperature, in 7.5 hours treatment times, oxygen level is=16.8%.
When carbonization process, top temperature is set 1000 ℃, and temperature rise rate is 40-100 ℃, and its air-fuel ratio schedules 0.85-0.95, measure of oxygen content 195ppm, and outward appearance is the Powdered loose block that has after the carbonization.
Sieve with 270 eye mesh screens at last, its screen cloth yield is 90.8%, the composite stone ink powder of gained, and median size is 16.92 μ m, specific surface area is 2.73m
2/ g, true density numerical value are 2.27g/cc, and X-ray diffraction analysis (d002) is 0.33595nm, degree of graphitization 93.39%, initial stage loading capacity 363.8mAh/g, initial charge 91.8%.
Comparative example-1 is directly to make battery with spheroidal graphite materials, and its median size is 15.09 μ m, and specific surface area is 6.63m
2/ g, true density numerical value are 2.24g/cc, and X-ray diffraction analysis (d002) is 0.33558nm, degree of graphitization 97.68%, initial stage loading capacity 360.9mAh/g, initial charge 86.1%.
Comparative example-2 is to be batch produced composite graphite powder of cover material with resin, its roasting condition and fabrication steps and embodiment-2 is identical, sieves with 270 eye mesh screens, and its screen cloth yield is 63.3%, composite stone ink powder median size is 16.53 μ m, and specific surface area is 18.41m
2/ g, true density numerical value are 2.32g/cc, and X-ray diffraction analysis (d002) is 0.33657nm, degree of graphitization 86.19%, and solid content is too low when crossing the large electrode making because of specific surface area, and battery is made failure, can't electrically assess, and analyzes termination so accuse.
By relatively following of chart data, according to the negative material that the present invention generated, specific surface area is much smaller than comparative example-1 and comparative example-2, the screen cloth yield is higher than comparative example-2, its initial stage loading capacity, initial charge and cycle life that makes behind the negative material of button-type battery all is higher than comparative example-1 directly makes battery with spherical graphite negative material, when the composite graphite of comparative example-2 output then caused pole piece to make because of specific surface area is excessive, solid content was crossed the low manufacturing that can't finish pole piece.
See also Fig. 2 to Fig. 5, be the button-type battery of being done as negative material with above-mentioned powdered graphite, the test that the process cycle charge-discharge is 20 times, embodiment-1 and embodiment-2 its loading capacities still maintain and are higher than other comparative example more than 80%, and comparative example-1 is through behind the cycle charge-discharge 20 times, the battery recession level can be demonstrated by Fig. 5, behind above-mentioned cycle charge discharge electrical testing, obviously find out the battery that the composite graphite that generated with step of the present invention is done, have higher loading capacity and good cycle charge discharge electrical efficiency.
By step of the present invention, simplify the making worker method of the negative material of lithium secondary battery, and reduced production cost, need not separate broken processing, save and separate the facility investment and the manpower of broken processing; And see through selecting for use of cover material, battery efficiency is promoted, reduce caking rate, avoid battery distortion of materials in charge and discharge process material that is produced that differs to peel off, and then effectively promote the charge/discharge capacity of battery.
The above person, it only is preferred embodiment of the present invention, can not limit scope of the invention process with this, promptly the simple equivalent of being done according to the present patent application claim and description of the invention content substantially changes and modifies, and must be included in the present patent application claim.
Claims (11)
1, a kind of composite graphite and manufacture method thereof that is used for lithium secondary battery, this manufacture method comprises the following step:
1). choose spherical graphite as base material, above-mentioned base material with default preheating temperature preheating one a preheating setting-up time, is dropped into cover material again and gives thorough mixing, said mixture is packed in the crystal vessel;
2). crystal vessel sent into carry out high molecular in the recirculation still and handle;
3). with above-mentioned crystal vessel after having handled, put into carbide furnace and carry out high temperature cabonization again and handle, wait to be warming up to a preset temp and keep a Preset Time and be cooled to room temperature by high molecular;
4). at last through sieving or air classification is handled and to be obtained composite graphite.
2, a kind of composite graphite and manufacture method thereof that is used for lithium secondary battery according to claim 1, wherein, above-mentioned base material preheating setting-up time 〉=30 minutes, default preheating temperature is 55-85 ℃.
3, a kind of composite graphite and manufacture method thereof that is used for lithium secondary battery according to claim 1, wherein, criticizing cover material is coal tar or the viscid bitumen of softening temperature below 65 ℃, or above two kinds of materials and liquid resinous mixed solution, and the weight percent that this cover material uses is 10%-40%.
4, a kind of composite graphite and manufacture method thereof according to claim 1 with the what lithium secondary battery, wherein, the degree of porosity 〉=3cc/cm of above-mentioned crystal vessel
2Min, material density 〉=1.65g/cc, thermal conductivity 〉=120W/mk.
5, a kind of composite graphite and manufacture method thereof that is used for lithium secondary battery according to claim 1 wherein, carried out above-mentioned high molecular when handling, oxygen level 〉=15% of setting in the recirculation still.
6, a kind of composite graphite and manufacture method thereof that is used for lithium secondary battery according to claim 1 wherein, carried out above-mentioned high molecular when handling, and the recirculation still internal pressure is-the 10mm-10mm water colunm pressure.
7, a kind of composite graphite and manufacture method thereof that is used for lithium secondary battery according to claim 1 wherein, carried out above-mentioned high molecular when handling, and crystal vessel per hour heats up 10-30 ℃, the institute top temperature that rises≤210 ℃.
8, a kind of composite graphite and manufacture method thereof that is used for lithium secondary battery according to claim 1, wherein, when carrying out above-mentioned carbonizing treatment, the oxygen level≤300ppm that sets in the carbide furnace, air-fuel ratio is 0.8-0.99.
9, a kind of composite graphite and manufacture method thereof that is used for lithium secondary battery according to claim 1, wherein, when carrying out above-mentioned carbonizing treatment, the pressure in the carbide furnace is water colunm pressure 0.1mm-10mm.
10, a kind of composite graphite and manufacture method thereof that is used for lithium secondary battery according to claim 1, wherein, when carrying out above-mentioned carbonizing treatment, per hour heat up 20-120 ℃, described preset temp is between 1000-1600 ℃, and the Preset Time that described high temperature keeps is 〉=2 hours.
11, a kind of composite graphite of lithium secondary battery and composite graphite that manufacture method is made thereof of being used for according to claim 1, have following rerum natura: its volume percent is size distribution≤25 μ m of 50% o'clock, specific surface area≤5m
2/ g, tap density 〉=1.0g/cc, degree of graphitization 〉=90%; And there is 1350-1370cm in it in the Ar Laser light Raman spectrum of wavelength 514.4nm
-1Peak strength (I in the scope
D) to there being 1570-1630cm
-1Peak strength (the I of scope
G) ratio (I
D/ I
G)≤0.5.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103560247A (en) * | 2013-11-08 | 2014-02-05 | 深圳市贝特瑞新能源材料股份有限公司 | Vehicle-mounted and energy-storage lithium ion battery cathode material and preparation method thereof |
| CN107954411A (en) * | 2017-11-06 | 2018-04-24 | 山西水木新碳材科技有限公司 | The Processes and apparatus of vertical continuous carbonization production lithium cell cathode material |
| CN109952672A (en) * | 2016-11-14 | 2019-06-28 | 日立化成株式会社 | Lithium ion secondary battery cathode material, lithium ion secondary battery cathode and lithium ion secondary battery |
| CN110495023A (en) * | 2017-04-13 | 2019-11-22 | 埃卡特有限公司 | The removing graphite composite material of ZnO nano particle coating, the preparation method of the composite material and its application in Li-ion batteries piles |
| CN111048785A (en) * | 2019-12-27 | 2020-04-21 | 深圳市金润能源材料有限公司 | Negative electrode material, preparation method thereof, electrode plate and battery |
| CN115395003A (en) * | 2022-10-28 | 2022-11-25 | 溧阳紫宸新材料科技有限公司 | Negative electrode material and preparation method and application thereof |
-
2007
- 2007-10-15 CN CNA2007101635505A patent/CN101412510A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103560247A (en) * | 2013-11-08 | 2014-02-05 | 深圳市贝特瑞新能源材料股份有限公司 | Vehicle-mounted and energy-storage lithium ion battery cathode material and preparation method thereof |
| CN103560247B (en) * | 2013-11-08 | 2017-02-01 | 深圳市贝特瑞新能源材料股份有限公司 | Vehicle-mounted and energy-storage lithium ion battery cathode material and preparation method thereof |
| CN109952672A (en) * | 2016-11-14 | 2019-06-28 | 日立化成株式会社 | Lithium ion secondary battery cathode material, lithium ion secondary battery cathode and lithium ion secondary battery |
| CN110495023A (en) * | 2017-04-13 | 2019-11-22 | 埃卡特有限公司 | The removing graphite composite material of ZnO nano particle coating, the preparation method of the composite material and its application in Li-ion batteries piles |
| CN107954411A (en) * | 2017-11-06 | 2018-04-24 | 山西水木新碳材科技有限公司 | The Processes and apparatus of vertical continuous carbonization production lithium cell cathode material |
| CN111048785A (en) * | 2019-12-27 | 2020-04-21 | 深圳市金润能源材料有限公司 | Negative electrode material, preparation method thereof, electrode plate and battery |
| CN115395003A (en) * | 2022-10-28 | 2022-11-25 | 溧阳紫宸新材料科技有限公司 | Negative electrode material and preparation method and application thereof |
| CN115395003B (en) * | 2022-10-28 | 2023-02-28 | 溧阳紫宸新材料科技有限公司 | Negative electrode material and preparation method and application thereof |
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Open date: 20090422 |