CN104108699A - Preparation method of lithium ion battery graphite negative electrode material with high capacity and high compaction density - Google Patents
Preparation method of lithium ion battery graphite negative electrode material with high capacity and high compaction density Download PDFInfo
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- CN104108699A CN104108699A CN201310161457.6A CN201310161457A CN104108699A CN 104108699 A CN104108699 A CN 104108699A CN 201310161457 A CN201310161457 A CN 201310161457A CN 104108699 A CN104108699 A CN 104108699A
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- graphite
- lithium ion
- ion battery
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 239000010439 graphite Substances 0.000 title claims abstract description 80
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 68
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000005056 compaction Methods 0.000 title abstract 5
- 239000007773 negative electrode material Substances 0.000 title abstract 3
- 239000000463 material Substances 0.000 claims abstract description 30
- 238000000746 purification Methods 0.000 claims abstract description 22
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 10
- 238000005087 graphitization Methods 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 16
- 230000008569 process Effects 0.000 claims description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims description 14
- 230000008859 change Effects 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 7
- 230000000630 rising effect Effects 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 7
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 6
- 239000000460 chlorine Substances 0.000 claims description 6
- 229910052801 chlorine Inorganic materials 0.000 claims description 6
- 239000010406 cathode material Substances 0.000 claims description 5
- 240000003936 Plumbago auriculata Species 0.000 claims 1
- 229910021382 natural graphite Inorganic materials 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract 1
- 241000209456 Plumbago Species 0.000 description 11
- 238000011068 loading method Methods 0.000 description 7
- 239000007770 graphite material Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 239000008151 electrolyte solution Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 230000000875 corresponding effect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000009831 deintercalation Methods 0.000 description 1
- 230000009189 diving Effects 0.000 description 1
- 238000006253 efflorescence Methods 0.000 description 1
- 238000005213 imbibition Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- -1 lithium forms lithium-compound Chemical class 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000005453 pelletization Methods 0.000 description 1
- 206010037844 rash Diseases 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
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- Battery Electrode And Active Subsutance (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a preparation method of a lithium ion battery graphite negative electrode material with high capacity and high compaction density. The preparation method comprises the following steps: 1, carrying out spheroidization of natural graphite with the fixed carbon content of 80-99%; and 2, carrying out purification and graphitization, and thus obtaining the required graphite negative electrode material. The obtained material has high compaction density, the compaction density of a powder is 1.8-2.1 g/cm<3>, the compaction density of a pole piece is 1.75-1.95 g/cm<3>, the discharge specific capacity is high and greater than 370 mAh/g, the average particle size is 5-30 [mu]m, the liquid absorbing performance is good, and requirements of high specific capacity and high multiplying power of a lithium ion battery are fitted.
Description
Technical field
The present invention relates to a kind of preparation method of high compacted density graphite negative material of lithium ion battery.
Background technology
The electronic information epoch make the demand rapid growth to portable power source, because lithium ion battery has the significant advantage of high-voltage, heavy body, and have extended cycle life, safety performance is good, it is had broad application prospects in many-sides such as portable electric appts, electromobile, space technology, national defense industry, become the study hotspot of widely paying close attention in recent years.Current commercial lithium ion battery negative material is mainly carbon material, wherein natural graphite good conductivity, degree of crystallinity is high, have good laminate structure, the embedding-deintercalation that is applicable to lithium forms lithium-compound between graphite layers, and charge/discharge capacity is high, efficiency for charge-discharge is high, irreversible capacity is low, has good charge and discharge potential platform, becomes the negative material that current lithium ion battery applications is maximum.But the shortcoming of graphite material is also clearly, the one, graphite spacing d
002≤ 0.34nm, is less than the spacing d=0.37nm of graphite intercalation compound Li-GIC, causes in charge and discharge process, and graphite layers is apart from change, causes that graphite ink sheet peels off, efflorescence, causes electric cycle performance undesirable; The 2nd, poor with the consistency of electrolytic solution; The 3rd, its tap density is lower.In order to overcome the above-mentioned deficiency of graphite material, graphite material is carried out to modification and become the focus of carbon negative pole research in recent years.
From current present Research, the loading capacity performance of unit weight carbon material has approached theoretical value, therefore the in the situation that of battery given volume, if obtain higher energy density per unit volume, need higher compacted density, and existing material, under high compacting, under condition, there is imbibition deficiency, there is no enough passages that discharges and recharges, the problems such as diving that capacity is brought into play not exclusively and circulation is expanded, therefore around how to ensure that improving compacted density under the good prerequisite of heavy body cycle performance has launched research widely, as Xie Qiusheng, Qiao Yongmin etc. add catalyzed graphitization mode to be coated charing has made compacted density and has been not less than 1.70g/cm
3graphite cathode material (Chinese patent Granted publication CN102339988A), but the compacted density of its negative material making or not high enoughly (be less than 1.8g/cm
3), and capacity performance do not arrive 370mAh/g yet, fail to fully demonstrate the advantage of high compacting heavy body, and making processes bothers, cost is higher.
Summary of the invention
The object of this invention is to provide a kind of preparation method of high compacted density graphite negative material of lithium ion battery, the problem that solve is to make negative material have higher loading capacity and compacted density.
Material choice fixed carbon content, 80%～90%, needs enough impurity to ensure that it leaves corresponding hole while effusion; Nodularization can change its chemical property, then by purification of graphite, graphite-structure is become in order by unordered, has increased the describing property of itself and electrolytic solution, and the specific storage of material is brought into play better.
The present invention is by the following technical solutions: high ash content natural flake graphite is carried out to nodularization, make spherical graphite, again spherical graphite is carried out to high temperature purification and high temperature graphitization processing, the micropore that utilizes its ash content to overflow in the time of high temperature purification to stay obtains the high graphite cathode material that holds high compacting of a kind of porous;
Affiliated preparation method comprises the following steps:
(1) use ultramicron pelletizer to carry out nodularization to natural flake graphite, when nodularization, speed of grinding plate is 2000-4800rpm/min, and the nodularization time is 20-40min, makes the spherical graphite of median size 5-30 μ m;
(2) spherical graphite making being put into purification of graphite equipment processes; Concrete processing mode is material to be put into the plumbago crucible of body of heater, speed with 5-200 DEG C/min heats up, in the time that temperature in stove reaches 1000-1500 DEG C, flow with 1-5m3/h passes into nitrogen, continue to be warming up to 1500-2200 DEG C with the speed of 5-200 DEG C/min, pass into chlorine with the flow of 1-5m3/h simultaneously, until temperature stops heating while rising to 2200-3300 DEG C, insulation 5h, change again with the flow of 1-5m3/h and pass into nitrogen, 5-15h, purification of graphite process completes, and makes required graphite negative material of lithium ion battery.
The fixed carbon content of described natural flake graphite is 80%～90%, and median size is 60-100 μ m, and largest particle can pass through 80 eye mesh screens.
Described purification of graphite equipment is acheson furnace.
The graphite cathode material making by the present invention, compacted density is high, pole piece compacted density is between 1.75-1.95g/cm3, and powder body compacted density is between 1.8-2.1g/cm3, and specific discharge capacity is high, be greater than 370mAh/g, median size is 5-30 μ m, and absorbent is good, is applicable to current lithium ion battery to height ratio capacity and the forthright requirement of high power, and cheap, simple to operate.
Brief description of the drawings
Below in conjunction with the correlated performance of brief description of the drawings material of the present invention.
Fig. 1 is the ultramicron pelletizing structural scheme of mechanism that the present invention uses.Mark in figure: 1, chuck (heating, cooling), 2, stator, 3, circulation loop, 4, dog-house, 5, bleeder valve, 6, discharge port, 7, abrading block, 8, rotor.
Embodiment
Below in conjunction with embodiment, the present invention is described in further details
Embodiment 1
(1) to fixed carbon content be 90%, the natural flake graphite of median size 80 μ m uses ultramicron pelletizer to carry out nodularization, when nodularization, speed of grinding plate is 3000rpm/min, the nodularization time is 35min, makes the spherical graphite of median size 23 μ m; (2) spherical graphite making is put into purification of graphite equipment and process, processing mode is material to be put into the plumbago crucible of body of heater, heats up, with the speed of 20 DEG C/min in the time that the temperature of plumbago crucible in stove reaches 1000 DEG C, with 3m
3the flow of/h passes into nitrogen, continues to be warming up to 1500 DEG C with the speed of 50 DEG C/min, simultaneously with 3m
3the flow of/h passes into chlorine, until temperature stops heating while rising to 2000 DEG C, and insulation 5h, then change with 3m
3the flow of/h passes into nitrogen, 5h, and purification of graphite process completes.The negative material obtaining, loading capacity 370.5mAh/g, powder-compacting 1.92g/cm
3, pole piece compacted density 1.83g/cm
3.
Embodiment 2
(1) to fixed carbon content be 80%, the natural flake graphite of median size 90 μ m uses ultramicron pelletizer to carry out nodularization, when nodularization, speed of grinding plate is 4200rpm/min, the nodularization time is 30min, makes the spherical graphite of median size 17 μ m; (2) spherical graphite making is put into purification of graphite equipment and process, processing mode is material to be put into the plumbago crucible of body of heater, heats up, with the speed of 50 DEG C/min in the time that the temperature of plumbago crucible in stove reaches 1200 DEG C, with 3m
3the flow of/h passes into nitrogen, continues to be warming up to 1800 DEG C with the speed of 50 DEG C/min, simultaneously with 3m
3the flow of/h passes into chlorine, until temperature stops heating while rising to 2500 DEG C, and insulation 5h, then change with 3m
3the flow of/h passes into nitrogen, 10h, and purification of graphite process completes.The negative material obtaining, loading capacity 372.1mAh/g, powder-compacting 1.98g/cm
3, pole piece compacted density 1.88g/cm
3.
Embodiment 3
(1) to fixed carbon content be 85%, the natural flake graphite of median size 65 μ m uses ultramicron pelletizer to carry out nodularization, when nodularization, speed of grinding plate is 4500rpm/min, the nodularization time is 35min, makes the spherical graphite of median size 15 μ m; (2) spherical graphite making is put into purification of graphite equipment and process, processing mode is material to be put into the plumbago crucible of body of heater, heats up, with the speed of 50 DEG C/min in the time that the temperature of plumbago crucible in stove reaches 1500 DEG C, with 3m
3the flow of/h passes into nitrogen, continues to be warming up to 2000 DEG C with the speed of 50 DEG C/min, simultaneously with 3m
3the flow of/h passes into chlorine, until temperature stops heating while rising to 3200 DEG C, and insulation 5h, then change with 3m
3the flow of/h passes into nitrogen, 15h, and purification of graphite process completes.The negative material obtaining, loading capacity 370.2mAh/g, powder-compacting 2.01g/cm
3, pole piece compacted density 1.90g/cm
3.
Embodiment 4
(1) to fixed carbon content be 83%, the natural flake graphite of median size 70 μ m uses ultramicron pelletizer to carry out nodularization, when nodularization, speed of grinding plate is 4000rpm/min, the nodularization time is 35min, makes the spherical graphite of median size 19 μ m; (2) spherical graphite making is put into purification of graphite equipment and process, processing mode is material to be put into the plumbago crucible of body of heater, heats up, with the speed of 50 DEG C/min in the time that the temperature of plumbago crucible in stove reaches 1200 DEG C, with 3m
3the flow of/h passes into nitrogen, continues to be warming up to 1500 DEG C with the speed of 50 DEG C/min, simultaneously with 3m
3the flow of/h passes into freonll-11, until temperature stops heating while rising to 3200 DEG C, and insulation 5h, then change with 3m
3the flow of/h passes into nitrogen, 15h, and purification of graphite process completes.The negative material obtaining, loading capacity 371.1mAh/g, powder-compacting 2.07g/cm
3, pole piece compacted density 1.93g/cm
3.
Embodiment 5
(1) to fixed carbon content be 88%, the natural flake graphite of median size 75 μ m uses ultramicron pelletizer to carry out nodularization, when nodularization, speed of grinding plate is 4000rpm/min, the nodularization time is 30min, makes the spherical graphite of median size 21 μ m; (2) spherical graphite making is put into purification of graphite equipment and process, processing mode is material to be put into the plumbago crucible of body of heater, heats up, with the speed of 50 DEG C/min in the time that the temperature of plumbago crucible in stove reaches 1200 DEG C, with 3m
3the flow of/h passes into nitrogen, continues to be warming up to 1500 DEG C with the speed of 50 DEG C/min, simultaneously with 3m
3the flow of/h passes into chlorine, until temperature stops heating while rising to 3000 DEG C, and insulation 5h, then change with 3m
3the flow of/h passes into nitrogen, 15h, and purification of graphite process completes.The negative material obtaining, loading capacity 370.8mAh/g, powder-compacting 2.05g/cm
3, pole piece compacted density 1.91g/cm
3.
Table 1 is the DCO data of above-described embodiment
Claims (4)
1. the preparation method of a high compacted density graphite negative material of lithium ion battery, it is characterized in that: high ash content natural flake graphite is carried out to nodularization, make spherical graphite, again spherical graphite is carried out to high temperature purification and high temperature graphitization processing, the micropore that utilizes its ash content to overflow in the time of high temperature purification to stay obtains the high graphite cathode material that holds high compacting of a kind of porous;
Affiliated preparation method comprises the following steps:
(1) use ultramicron pelletizer to carry out nodularization to natural flake graphite, when nodularization, speed of grinding plate is 2000-4800rpm/min, and the nodularization time is 20-40min, makes the spherical graphite of median size 5-30 μ m;
(2) spherical graphite making being put into purification of graphite equipment processes; Concrete processing mode is material to be put into the plumbago crucible of body of heater, heats up, with the speed of 5-200 DEG C/min in the time that temperature in stove reaches 1000-1500 DEG C, with 1-5m
3the flow of/h passes into nitrogen, continues to be warming up to 1500-2200 DEG C with the speed of 5-200 DEG C/min, simultaneously with 1-5m
3the flow of/h passes into chlorine, until temperature stops heating while rising to 2200-3300 DEG C, and insulation 5h, then change with 1-5m
3the flow of/h passes into nitrogen, 5-15h, and purification of graphite process completes, and makes required graphite negative material of lithium ion battery.
2. the preparation method of high compacted density graphite negative material of lithium ion battery according to claim 1, it is characterized in that: the fixed carbon content of described natural flake graphite is 80%～90%, median size is 60-100 μ m, and largest particle can pass through 80 eye mesh screens.
3. the preparation method of high compacted density graphite negative material of lithium ion battery according to claim 1, is characterized in that: described purification of graphite equipment is acheson furnace.
4. the preparation method of high compacted density graphite negative material of lithium ion battery according to claim 1, it is characterized in that: gained graphite cathode material, median size is 5-30 μ m, pole piece compacted density is 1.75-1.95g/cm3, powder body compacted density is 1.8-2.1g/cm3, and specific discharge capacity is greater than 370mAh/g.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310161457.6A CN104108699A (en) | 2013-04-22 | 2013-04-22 | Preparation method of lithium ion battery graphite negative electrode material with high capacity and high compaction density |
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| CN201310161457.6A CN104108699A (en) | 2013-04-22 | 2013-04-22 | Preparation method of lithium ion battery graphite negative electrode material with high capacity and high compaction density |
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Cited By (3)
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| CN105489893A (en) * | 2015-10-28 | 2016-04-13 | 江西正拓新能源科技股份有限公司 | Graphite anode material for lithium-ion battery and preparation method of graphite anode material |
| CN109652192A (en) * | 2019-01-11 | 2019-04-19 | 西安凯丰铁路机电设备有限公司 | A kind of aqua type coefficient of friction modifiers for rail tread |
| CN113161514A (en) * | 2020-01-07 | 2021-07-23 | 珠海冠宇电池股份有限公司 | Graphite composition, battery cathode and lithium ion battery |
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