CN102034975A - Nitrogen-doped graphite carbon serving as anode material of lithium ion battery, and preparation method and application thereof - Google Patents
Nitrogen-doped graphite carbon serving as anode material of lithium ion battery, and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a nitrogen-doped graphite carbon, which is obtained by calcining a graphite carbon material in a nitrogen-containing micromolecule material or atmosphere of the nitrogen-containing micromolecule material. When a pole piece which is prepared from the nitrogen-doped graphite carbon material is used as an electrode material of the lithium ion battery, the specific capacity of the material reaches 450 to 1,100mAh/g, and the material has high multiplying power performance and cycle performance. A preparation method of the nitrogen-doped graphite carbon is convenient to operate, and is easy and practicable; the prepared material has stable and excellent performance, and is the anode material of the lithium ion battery, which has good application prospect.
Description
Technical field
The invention belongs to energy and material and technical field of electrochemistry, relate to a kind of lithium ion battery negative material nitrogen doped graphite carbon particularly.
The invention still further relates to the preparation method of above-mentioned nitrogen doped graphite carbon.
The invention still further relates to the application of above-mentioned nitrogen doped graphite carbon.
Background technology
Negative material is one of critical material of lithium ion battery, and carbonaceous material is research of people's early start and the material that is applied to lithium ion battery negative, still is subjected to extensive concern so far.Graphite be use in the lithium ion battery carbon material the earliest, that research is maximum is a kind of, has complete layered crystal structure, interlamellar spacing is 0.335nm, the interlayer that lithium embeds graphite forms Li
xC
6Intercalation compound.When x=1, single order lithium compound between graphite layers just, its theoretical specific capacity is 372mAh/g.But the graphitic carbon high rate during charging-discharging is low, influences its power performance.Research to the carbon negative pole mainly is to adopt various means that the graphitic carbon material is improved at present, emphasis is a better utilization cheap raw material native graphite for example how from now on, and it is carried out the graphitic carbon material that high-energy-density and high power density are developed in effective modification.
Graphitic carbon can carry out modification by several different methods, to reach different effects.Doping is a kind of method commonly used, by doping nitrogen or boron element, can change the electronic property of semi-conducting material.Dacheng Wei etc. (Synthesis of N-Doped Graphene by Chemical VaporDeposition and Its Electrical Properties[J] .Nano Lett 9 (2009): 1752-1758) adopt the CVD method to prepare nitrogen-doped graphene.Nan Li etc. (Large scale synthesis of N-dopedmulti-layered graphene sheets by simple arc-discharge method[J] .Carbon 48 (2010): 255-259) utilize arc discharge method to obtain the grapheme material that nitrogen mixes, graphitic carbon material band structure after wherein mixing changes, conductivity improves, and the graphitic carbon material after therefore mixing has bigger development space than original graphitic carbon material.
The cellular lattice structure of bidimensional cycle that Graphene is made up of the carbon hexatomic ring, it can warpage becomes the fullerene of zero dimension, is rolled into the carbon nano-tube of one dimension or is stacked to three-dimensional graphite.Graphene (Highly efficient and large-scale synthesis of graphene by electrolyticexfoliation[J] .Carbon 47 (2009): 3242-3246) several characteristics are arranged: be zero gap semiconductor, can be used as the detector material; The performance of Graphene does not vary with temperature, and is highly stable, and conductivity is good; In addition, Graphene also shows good electro-chemical activity, is the energy storage material of excellent performance, has huge application space as the high power density lithium ion battery negative material.Patent CN101572327A discloses with the negative material of Graphene as lithium ion battery, and its capacity remains on 380-450mAh/g after through 20-30 circulation.Yet nitrogen-doped graphene is not also reported as lithium ion battery negative material at present.
Can the application of nitrogen doped graphite material with carbon element be achieved, and depends on the development innovation of its mass preparation technology.CN 101708837A has proposed a kind of method for preparing nitrogen-doped graphene, is that organic explosive substance and the carbon nitrogen additive that will contain nitro obtains by explosive reaction.
Summary of the invention
The object of the present invention is to provide a kind of lithium ion battery negative material nitrogen doped graphite carbon.
Another purpose of the present invention is to provide a kind of method for preparing above-mentioned nitrogen doped graphite carbon.
For achieving the above object, nitrogen doped graphite carbon provided by the invention is to obtain after the graphitic carbon material is placed the atmosphere calcining of nitrogenous small molecule material or nitrogenous small molecule material.
Described nitrogen doped graphite carbon, wherein the graphitic carbon material is graphene oxide, reduction Graphene, native graphite, electrographite, expanded graphite or carbonaceous mesophase spherules graphite.
The method of the above-mentioned nitrogen doped graphite of preparation provided by the invention carbon, its key step is:
Place the atmosphere calcining of nitrogenous small molecule material or nitrogenous small molecule material to carry out nitrogen treatment the graphitic carbon material.
Described preparation method, wherein the graphitic carbon material is graphene oxide, reduction Graphene, native graphite, electrographite, expanded graphite or carbonaceous mesophase spherules graphite.
Described preparation method, wherein nitrogenous small molecule material be in hydrazine class, pure ammonia, organic amine, organic amine salt, the nitrogen one or more.
Described preparation method, the volumn concentration ratio of wherein nitrogenous small molecule material is 10～99%.
Described preparation method, wherein the temperature of nitrogen treatment is 300～1500 ℃, nitridation time is 0.1～72 hour.
Described preparation method, wherein programming rate is 1～20 ℃/min during nitrogen treatment, and molecular concentration is 0.1～10M, and gas flow rate is 1～200sccm.
Nitrogen doped graphite carbon of the present invention can be used as lithium ion battery negative material, and nitrogen doped graphite carbon and conductive black, polyvinylidene fluoride are mixed into pulpous state, is applied on the Copper Foil, and vacuum drying obtains the lithium ion battery negative pole piece then.
The present invention is by nitrogenous micromolecule pyroreaction facture; the graphitic carbon material that obtains the nitrogen doping is as lithium ion battery negative material; it is low, easy to operate that this method has a cost; be easy to advantages such as large-scale production; simultaneously can be by changing raw material, the material that obtains different nitrogen doping is as lithium ion battery negative material.
Description of drawings
Fig. 1 is the charging and discharging curve figure of nitrogen-doped graphene of the present invention when current density is 42mA/g.
Fig. 2 is the cycle performance and the high rate performance figure of nitrogen-doped graphene of the present invention.
Fig. 3 is the x-ray diffraction pattern of nitrogen doping electrographite of the present invention.
Fig. 4 is the sem photograph of graphite oxide of the present invention after nitrogenize.
Embodiment
The object of the present invention is to provide a kind of new type lithium ion battery nitrogen doped graphite carbon negative pole material preparation method and application thereof, this material capacity is higher, and high rate performance is better, and preparation process is simple, and application prospect is extensive.
The preparation method of nitrogen doped graphite carbon negative pole material of the present invention, be to be raw material with the graphitic carbon material, be placed in nitrogenous small molecule material or the nitrogenous small molecule material atmosphere calcining and carry out nitrogen treatment, obtain lithium ion battery negative material nitrogen doped graphite carbon.
Graphitic carbonaceous materials of the present invention is graphite type material such as graphene oxide, reduction Graphene, native graphite, electrographite, expanded graphite or carbonaceous mesophase spherules.
Nitrogenous small molecule material of the present invention be in pure ammonia, organic amine, organic amine salt, the nitrogen isoreactivity material one or more, its volumn concentration ratio is 1～99%.
Nitriding temperature of the present invention is 300～1100 ℃, and nitridation time is 0.1～72 hour.
Programming rate is 1～20 ℃/min during nitrogenize of the present invention, and gas flow rate is 1～200sccm.
It is as follows that the present invention carries out the charge-discharge performance test process to the material of preparation:
(1) preparation of cathode pole piece: the material of preparation and conductive black, polyvinylidene fluoride in N-methyl pyrrolidone is mixed into pulpous state according to mass ratio at 85: 10: 5, be applied on the Copper Foil, then with it at 120 ℃ of following vacuum dryings, obtain cathode pole piece.
(2) assembled battery: lithium sheet just very, electrolyte is the lithium hexafluoro phosphate electrolyte that lithium ion battery is used, and is assembled into button cell in being connected with the glove box of argon gas.
The present invention has the following advantages:
(1) material preparation process is simple, easy operating;
(2) the reversible capability of charging and discharging height of material, good rate capability has very big application potential aspect lithium ion battery.
Further set forth the present invention with embodiment below, but the present invention is not so limited.
Adopt the Hummer method that Delanium is carried out oxidation, obtain graphite oxide, with hydrazine hydrate graphite oxide is reduced again, obtain reducing Graphene.The reduction Graphene of preparation is put into and is connected with ammonia/helium/hydrazine gaseous mixture (ammonia 10%-50%; Helium 90%-40%; Hydrazine in tube furnace 0-10%), was calcined 6 hours down, is obtained the grapheme material that nitrogen mixes for 700 ℃.With the nitrogen doped graphite material for preparing according to mass ratio 85: 10: 5 and conductive black, polyvinylidene fluoride mixes in the N-methyl pyrrolidone and is applied on the Copper Foil collector, 120 ℃ of vacuum dryings obtain cathode pole piece, be assembled into button cell then and test in glove box.The capacity that test obtains is 750mAh/g, and the charging and discharging curve of resulting material is illustrated in Fig. 1.
Embodiment 2
The grapheme material that example 1 prepares is put into the tube furnace that is connected with ammonia/allylamine gaseous mixture, calcined 2 hours down, obtain the nitrogen-doped graphene material for 800 ℃.With the nitrogen-doped graphene material for preparing according to mass ratio 85: 10: 5 and conductive black, polyvinylidene fluoride mixes in the N-methyl pyrrolidone and is applied on the Copper Foil collector, 120 ℃ of vacuum dryings obtain cathode pole piece, be assembled into button cell then and test in glove box.The specific capacity of nitrogenize Graphene when current density is 42mA/g that this method prepares is 1150mAh/g, and the specific capacity when current density is 210mA/g is 440mAh/g.The high rate performance and the cycle performance of resulting material are illustrated in Fig. 2.
Embodiment 3
Electrographite is put into the tube furnace that is connected with methyl amine, and gas flow rate is 80sccm, and programming rate is 2 ℃/min, calcines 2 hours down at 700 ℃, obtains the graphite cathode material that nitrogen mixes.The material for preparing is assembled into button cell tests, obtaining the specific capacity of nitrogenize graphite cathode material when 0.1C discharges and recharges is 450mAh/g.The X-ray diffraction of nitrogenize graphite is illustrated in Fig. 3.
Embodiment 4
Adopt the Hummer method that Delanium is carried out oxidation, obtain the graphite oxide material.The graphite oxide that obtains is put into the tube furnace that is connected with ammonia/argon gas/vinylamine gaseous mixture (v/v 10%), calcined 4 hours down, obtain the graphite material that nitrogen mixes at 900 ℃.The material for preparing is assembled into button cell tests, obtaining the specific capacity of nitrogenize graphite cathode material when 0.1C discharges and recharges is 650mAh/g.The ESEM of gained material is illustrated in Fig. 4.
Claims (10)
1. nitrogen doped graphite carbon is to obtain after the graphitic carbon material is placed the atmosphere calcining of nitrogenous small molecule material or nitrogenous small molecule material.
2. nitrogen doped graphite carbon according to claim 1, wherein, the graphitic carbon material is graphene oxide, reduction Graphene, native graphite, electrographite, expanded graphite or carbonaceous mesophase spherules graphite.
3. method for preparing the described nitrogen doped graphite of claim 1 carbon, its key step is:
Place the atmosphere calcining of nitrogenous small molecule material or nitrogenous small molecule material to carry out nitrogen treatment the graphitic carbon material.
4. preparation method according to claim 3, wherein, the graphitic carbon material is graphene oxide, reduction Graphene, native graphite, electrographite, expanded graphite or carbonaceous mesophase spherules graphite.
5. preparation method according to claim 3, wherein, nitrogenous small molecule material be in hydrazine class, pure ammonia, organic amine, organic amine salt, the nitrogen one or more.
6. preparation method according to claim 3, wherein, the volumn concentration of nitrogenous small molecule material ratio is 10～99%.
7. preparation method according to claim 3, wherein, the temperature of nitrogen treatment is 300～1500 ℃, nitridation time is 0.1～72 hour.
8. according to claim 3 or 7 described preparation methods, wherein, programming rate is 1～20 ℃/min during nitrogen treatment, and molecular concentration is 0.1～10M, and gas flow rate is 1～200sccm.
9. the described nitrogen doped graphite of claim 1 carbon is as the application of lithium ion battery negative material.
10. application according to claim 9 is mixed into pulpous state with nitrogen doped graphite carbon and conductive black, the polyvinylidene fluoride of claim 1, is applied on the Copper Foil, and vacuum drying obtains the lithium ion battery negative pole piece then.
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| CN102956864A (en) * | 2011-08-29 | 2013-03-06 | 海洋王照明科技股份有限公司 | Preparation method of nitrogen-doped graphene electrode |
| CN103183330A (en) * | 2013-04-02 | 2013-07-03 | 中国矿业大学 | Controllable synthesis method for nitrogen and phosphorus co-doped graphitized carbon ball with hollow structure |
| CN103682357A (en) * | 2012-09-24 | 2014-03-26 | 海洋王照明科技股份有限公司 | Graphene composite electrode material and preparation method thereof, lead-carbon battery negative electrode lead plaster and preparation method thereof as well as lead-carbon battery |
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| CN104201385A (en) * | 2014-08-14 | 2014-12-10 | 中国科学技术大学 | Preparation method of high-nitrogen-doped graphene nanoparticles and application of high-nitrogen-doped graphene nanoparticles as negative material of lithium ion battery |
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