CN103236528B - A kind of germanium carbon graphite alkene composite material and its preparation method and application - Google Patents
A kind of germanium carbon graphite alkene composite material and its preparation method and application Download PDFInfo
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- CN103236528B CN103236528B CN201310140777.3A CN201310140777A CN103236528B CN 103236528 B CN103236528 B CN 103236528B CN 201310140777 A CN201310140777 A CN 201310140777A CN 103236528 B CN103236528 B CN 103236528B
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- 239000002131 composite material Substances 0.000 title claims abstract description 53
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 39
- 239000010439 graphite Substances 0.000 title claims abstract description 39
- -1 germanium carbon graphite alkene Chemical class 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 49
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium dioxide Chemical compound O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 claims abstract description 29
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 24
- 229910052732 germanium Inorganic materials 0.000 claims abstract description 18
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 17
- 229940119177 germanium dioxide Drugs 0.000 claims abstract description 12
- 239000002245 particle Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000011258 core-shell material Substances 0.000 claims abstract description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000001301 oxygen Substances 0.000 claims abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 4
- 239000002244 precipitate Substances 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims description 16
- 229910001416 lithium ion Inorganic materials 0.000 claims description 14
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 12
- 238000000498 ball milling Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 4
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 3
- 230000001476 alcoholic effect Effects 0.000 claims description 3
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 3
- 230000006872 improvement Effects 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 claims description 3
- 230000009467 reduction Effects 0.000 claims description 3
- 239000011257 shell material Substances 0.000 description 7
- 230000004087 circulation Effects 0.000 description 5
- KCFIHQSTJSCCBR-UHFFFAOYSA-N [C].[Ge] Chemical compound [C].[Ge] KCFIHQSTJSCCBR-UHFFFAOYSA-N 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000012876 topography Methods 0.000 description 4
- 239000011149 active material Substances 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910005793 GeO 2 Inorganic materials 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000006253 efflorescence Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000713 high-energy ball milling Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 235000012054 meals Nutrition 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 206010037844 rash Diseases 0.000 description 1
- 239000000758 substrate 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 kind of germanium carbon graphite alkene composite material, the carbon cotton-shaped by nano level germanium, germanium dioxide, group and redox graphene are composited, and wherein, the top layer that germanium dioxide is coated on germanium forms nucleocapsid, forms nano core-shell particle; Described nano core-shell uniform particles ground Dispersed precipitate is in the carbon that group is cotton-shaped, and reduced oxygen functionalized graphene network institute is coated.The invention also discloses preparation method and the application of above-mentioned germanium carbon graphite alkene composite material.Germanium carbon graphite alkene composite material prepared by the present invention has taken into account high power capacity, high magnification and high cyclical stability feature, and preparation process technique is simple, and power consumption is few, and output is high, pollution-free.
Description
Technical field
The present invention relates to lithium ion battery negative material, particularly a kind of germanium carbon graphite alkene composite material and its preparation method and application.
Background technology
Lithium ion battery has important strategic importance at new energy field, is the hot spot technology of current generation economic development and governmental support.The selection of negative material system and performance thereof are one of key factors determining performance of lithium ion battery of new generation.The capacity of traditional business-like carbon negative pole material reaches capacity, and the problem of its essence is the low (372mAhg of the theoretical capacity of material with carbon element
-1).In numerous non-carbon negative material system after deliberation, not only capacity is high as lithium ion battery negative material for metal Ge system, and lithium ion diffusion coefficient is large, it is 400 times of Si, good conductivity, can meet at present for high power capacity, high magnification, eco-friendly lithium ion battery growth requirement.But owing to there is larger change in volume in embedding lithium and de-lithium process, and efflorescence gradually, depart from collector and cause active material to lose efficacy.For overcoming this obstacle, nanometer can be adopted to reduce size (nano wire, nanotube, film etc.), doping inert matter with fixing active material, carbon coated shell or admixed graphite alkene with strategies such as buffer volumes expansions.In numerous strategy, simple nanometer or alloying effect are not remarkable and cost is higher, are not suitable for industrial applications.And the best method that the carbonaceous material with high conductivity and better ductility is used to cushion Metal Substrate active material volumetric expansion and improves its cycle performance.Particularly there is the Graphene of high conductivity, bigger serface, outstanding heat and chemical stability and good mechanical performance, more can effectively as the pressure-reducing pad of germanium base negative material in charge and discharge process change in volume, and conductance that whole electrode is high and lithium ion diffusion rate can be kept, while making germanium base lithium ion cell negative electrode material keep high power capacity, significantly can improve again circulation and high rate performance.
Summary of the invention
In order to overcome the above-mentioned shortcoming of prior art with not enough, the object of the present invention is to provide a kind of germanium carbon graphite alkene composite material (GeGeO
2c/RGO, wherein represent that shell is coated ,/expression mixes mutually, and Ge represents germanium particle, GeO
2represent germanium dioxide, C represents carbon phase, and RGO represents redox graphene), take into account high power capacity, high magnification and high cyclical stability feature.
Another object of the present invention is to the preparation method providing above-mentioned germanium carbon graphite alkene composite material, germanium carbon proportion speed is easily weighed, and step is simple, easily realizes suitability for industrialized production.
Another object of the present invention is the application providing above-mentioned germanium carbon graphite alkene composite material.
Object of the present invention is achieved through the following technical solutions:
A kind of germanium carbon graphite alkene composite material, the carbon cotton-shaped by nano level germanium, germanium dioxide, group and redox graphene (RGO) are composited, and wherein, the top layer that germanium dioxide is coated on germanium forms nucleocapsid, and germanium and germanium dioxide form nano core-shell particle; Described nano core-shell uniform particles ground Dispersed precipitate is in the carbon that group is cotton-shaped, and reduced oxygen functionalized graphene network institute is coated.
A preparation method for germanium carbon graphite alkene composite material, comprises the following steps:
(1) adopt high energy pendulum shake ball mill (QC-3M) to carry out ball milling to pure germanium raw material and graphite raw material under oxidizing atmosphere, obtain GeGeO
2c composite; Described GeGeO
2c composite by have germanium dioxide shell the disperse of Ge uniform particles formed in the cotton-shaped carbon of the group of being distributed in;
(2) by GeGeO
2c composite and redox graphene carry out ultrasonic mixing in alcoholic solution, obtain germanium carbon graphite alkene composite material, i.e. GeGeO after vacuumize
2c/RGO composite material.
The mass ratio of described pure germanium raw material and graphite raw material is 1:0.1 ~ 1.
Described GeGeO
2the mass ratio of C composite and redox graphene is 1:0.1 ~ 0.8.
The time of described ball milling is 4 ~ 10h.
The preparation method of described redox graphene is as follows: adopt improvement Hummers method to prepare graphite oxide, obtain redox graphene with hydrazine hydrate reduction.
Described germanium carbon graphite alkene composite material GeGeO
2c/RGO is as lithium ion battery negative material.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) GeGeO for preparing of the present invention
2c/RGO composite material, has three-layer protection structure, when as lithium ion battery negative material, and the similar structures that relative chemical legal system is standby, the Li formed after the oxide shell layer had more and Li react
2o, plays fixing Ge particle, and prevent reunion and the first line of defence as change in volume in germanium charge and discharge process, the redox graphene network of the cotton-shaped carbon-coating of the group formed after high-energy ball milling and mixing is respectively as second and the 3rd road shell.Germanium carbon graphite alkene composite material prepared by the present invention has taken into account high power capacity, high magnification and excellent cyclical stability feature.
(2) GeGeO for preparing of the present invention
2the preparation process technique of C/RGO composite material is simple, and power consumption is few, and output is high, pollution-free.
(3) GeGeO for preparing of the present invention
2c/RGO composite material can not only meet the requirement that lithium ion battery instantly develops to high-energy-density high magnification, and more easily extensible is used for other matrix negative materials.
Accompanying drawing explanation
Fig. 1 is germanium carbon composite construction GeGeO prepared by embodiments of the invention 1
2the SEM figure of C.
Fig. 2 is the SEM figure of redox graphene RGO prepared by embodiments of the invention 1.
Fig. 3 is the GeGeO that formed after the germanium carbon prepared of embodiments of the invention 1 and redox graphene compound
2the XRD spectra of C/RGO composite material.
Fig. 4 is GeGeO prepared by embodiments of the invention 1
2the SEM figure of C/RGO composite material.
Fig. 5 is GeGeO prepared by embodiments of the invention 1
2the cycle performance curve chart of C/RGO composite material.
Fig. 6 is GeGeO prepared by embodiments of the invention 2
2the SEM figure of C/RGO composite material.
Fig. 7 is GeGeO prepared by embodiments of the invention 3
2the cycle performance curve chart of C/RGO condensation material.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1
The preparation method of the germanium carbon graphite alkene composite material of the present embodiment, comprises the following steps:
(1) adopt high energy pendulum shake ball mill (QC-3M) to carry out ball milling to pure germanium raw material and graphite raw material under oxidizing atmosphere, germanium forms micro-germanium dioxide shell on its surface in nanometer process, and wherein the mass ratio of pure germanium raw material and graphite raw material is 1:1; Abrading-ball and raw meal mass ratio are 20:1, and Ball-milling Time is 10h, the GeGeO obtained
2c composite, its surface topography is as shown in Figure 1;
(2) adopt improvement Hummers method to prepare graphite oxide, obtain redox graphene with hydrazine hydrate reduction, its surface topography as shown in Figure 2;
(3) the germanium carbon complex nucleus shell material GeGeO will prepared after ball milling
2c and redox graphene in mass ratio 1:0.1 carry out ultrasonic mixing in alcoholic solution, obtain germanium carbon graphite alkene composite material GeGeO after the slow drying of vacuum
2c/RGO:, as shown in Figure 3, surface topography is as shown in Figure 4 for its XRD spectra.
GeGeO prepared by the known the present embodiment in Fig. 1 ~ 4
2c/RGO composite material is composited by the cotton-shaped carbon of nano level germanium, germanium dioxide, group and redox graphene, and wherein, the top layer that germanium dioxide is coated on germanium forms nucleocapsid, and germanium and germanium dioxide form nano core-shell particle; Described nano core-shell uniform particles ground Dispersed precipitate is in the carbon that group is cotton-shaped, and reduced oxygen functionalized graphene network institute is coated.
Below to GeGeO prepared by the present embodiment
2the performance of C/RGO composite material is tested:
By dried GeGeO
2c/RGO composite powder, conductive agent super-p and binding agent Pvdf in mass ratio 8:1:1 mixes to be coated on Copper Foil and is made into electrode slice.In argon gas atmosphere glove box, using lithium metal as to electrode, ethylene carbonate (EC)+dimethyl carbonate (DMC)+1MLiPF
6for electrolyte, be assembled into button cell and test.Test condition is: charging and discharging currents density is 200mA/g and 1000mA/g, discharge and recharge by voltage be 0.01V ~ 1.5V (vs.Li
+/ Li).
Fig. 5 is GeGeO prepared by the present embodiment
2c/RGO composite material cycle performance curve is (with GeGeO
2c:RGO1:0.1wt%, Ball-milling Time 10h, discharge-rate 0.2C are example), known, GeGeO prepared by the present embodiment
2the discharge capacity first of C/RGO composite material is 2665mAhg
-1, after 50 circulations, discharge capacity is 875mAhg
-1.
Embodiment 2
The preparation method of the germanium carbon graphite alkene composite material of the present embodiment, except the mass ratio of pure germanium raw material and graphite raw material is 1:0.1, GeGeO
2the mass ratio of C composite and redox graphene is outside 1:0.8, and all the other features and embodiment 1 are together.
GeGeO prepared by the present embodiment
2the surface topography of C/RGO composite material as shown in Figure 6.
The germanium carbon graphite alkene composite material prepared by the present embodiment is made lithium ion battery negative electrode slice and under 2C charge-discharge magnification condition, carries out charge-discharge test after assembled battery.The GeGeO of preparation
2c/RGO composite material its first discharge capacity be 1060mAhg
-1, after 100 circulations, capacity remains on 413mAhg
-1.
Embodiment 3
The preparation method of the germanium carbon graphite alkene composite material of the present embodiment, except the mass ratio of pure germanium raw material and graphite raw material be 1:0.5, Ball-milling Time is except 4h, all the other features and embodiment 1 with.
The germanium carbon graphite alkene composite material prepared by the present embodiment is made lithium ion battery negative electrode slice and under 2C charge-discharge magnification condition, carries out charge-discharge test after assembled battery, and as shown in Figure 7, known discharge capacity is first 1841mAhg to circulation performance curve
-1, after 100 circulations, capacity remains on 575mAhg
-1.
Above-described embodiment is the present invention's preferably execution mode; but embodiments of the present invention are not limited by the examples; change, the modification done under other any does not deviate from Spirit Essence of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (4)
1. a preparation method for germanium carbon graphite alkene composite material, is characterized in that, comprise the following steps:
(1) adopt high energy pendulum shake ball mill to carry out ball milling to pure germanium raw material and graphite raw material under oxidizing atmosphere, obtain GeGeO
2c composite; Described GeGeO
2c composite by have germanium dioxide shell the disperse of Ge uniform particles formed in the cotton-shaped carbon of the group of being distributed in;
The mass ratio of described pure germanium raw material and graphite raw material is 1:0.1 ~ 1;
(2) by GeGeO
2c composite and redox graphene carry out ultrasonic mixing in alcoholic solution, obtain germanium carbon graphite alkene composite material after vacuumize; Described GeGeO
2the mass ratio of C composite and redox graphene is 1:0.1 ~ 0.8;
Described germanium carbon graphite alkene composite material, the carbon cotton-shaped by nano level germanium, germanium dioxide, group and redox graphene are composited, and wherein, the top layer that germanium dioxide is coated on germanium forms nucleocapsid, and germanium and germanium dioxide form nano core-shell particle; Described nano core-shell uniform particles ground Dispersed precipitate is in the carbon that group is cotton-shaped, and reduced oxygen functionalized graphene network institute is coated.
2. the preparation method of germanium carbon graphite alkene composite material described in claim 1, is characterized in that, the time of described ball milling is 4 ~ 10h.
3. the preparation method of germanium carbon graphite alkene composite material described in claim 1, it is characterized in that, the preparation method of described redox graphene is as follows: adopt improvement Hummers method to prepare graphite oxide, obtain redox graphene with hydrazine hydrate reduction.
4. the application of germanium carbon graphite alkene composite material for preparing of the preparation method of the germanium carbon graphite alkene composite material of claim 1, as lithium ion battery negative material.
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104733707A (en) * | 2013-12-24 | 2015-06-24 | 中国电子科技集团公司第十八研究所 | Preparation method of germanium-based cathode material for lithium ion battery |
| CN104733719A (en) * | 2013-12-24 | 2015-06-24 | 中国电子科技集团公司第十八研究所 | Method for preparing germanium-based cathode material for lithium ion battery by adopting carbothermic reduction method |
| CN104466104A (en) * | 2014-11-19 | 2015-03-25 | 东莞市翔丰华电池材料有限公司 | Germanium-graphene composite cathode material for lithium ion battery and preparation method thereof |
| CN104659346A (en) * | 2015-02-11 | 2015-05-27 | 深圳新宙邦科技股份有限公司 | Germanium/carbon composite negative electrode material and preparation method thereof |
| CN105006551B (en) * | 2015-06-03 | 2017-06-06 | 中南大学 | A kind of sodium-ion battery phosphorization tin/Graphene anode material and preparation method thereof |
| CN108281627B (en) * | 2018-01-03 | 2021-05-25 | 中国科学院上海硅酸盐研究所 | Germanium-carbon composite negative electrode material for lithium ion battery and preparation method thereof |
| CN111540745A (en) * | 2020-05-13 | 2020-08-14 | 复旦大学 | Low-power-consumption two-dimensional material semi-floating gate memory and preparation method thereof |
| CN111640927B (en) * | 2020-06-17 | 2021-10-01 | 中国人民解放军国防科技大学 | Graphene-bridged polythiophene-coated germanium nanoparticle composite material and preparation method and application thereof |
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| CN101331630A (en) * | 2006-05-23 | 2008-12-24 | 索尼株式会社 | Negative electrode and method for producing same, and battery and method for producing same |
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| CN101331630A (en) * | 2006-05-23 | 2008-12-24 | 索尼株式会社 | Negative electrode and method for producing same, and battery and method for producing same |
| CN102427127A (en) * | 2011-12-02 | 2012-04-25 | 华南理工大学 | Stannum oxide/stannum-carbon composite material, and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
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| Ding-Jiang Xue et al.Improving the Electrode Performance of Ge through GeC Core−Shell Nanoparticles and Graphene Networks.《Journal of the American Chemical Society》.2012,第134卷2512−2515. * |
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