CN101937994A - Graphene/aluminum composite cathode material of lithium ion battery and preparation method thereof - Google Patents
Graphene/aluminum composite cathode material of lithium ion battery and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a graphene/aluminum composite cathode material of lithium ion battery and a preparation method thereof and belongs to the cathode material technology of lithium ion battery technology. The cathode material comprises grapheme and aluminum in a mass ratio of 1:0.1-100, and the capacity is between 600 and 1,200 mAh/g. The preparation process of the cathode material comprises the following steps of: uniformly mixing the grapheme and the aluminum according to the mass ratio; pressing the mixed material on a copper foil current collector so as to obtain an electrode plate; assembling a battery by using the lithium plate; and performing the charge and discharge for 1 to 100 cycles for curing under a current density of 1 to 500 mA/mg so as to obtain the graphene/aluminum cathode material of the lithium ion battery. The graphene/aluminum cathode material of lithium ion battery and the preparation method have the advantages that: the preparation process is simple; the capacity and the circulation performance are much higher than those of a pure-aluminum and pure-graphene cathode material as well as the conventional commercial cathode material; and the graphene/aluminum cathode material is easy to realize and can widely promoted.
Description
Technical field
The present invention relates to Graphene/aluminium composite negative pole material of a kind of lithium ion battery and preparation method thereof, belong to lithium-ion electric pool technology negative material technology.
Background technology
The world today, fossil energy is day by day short, environmental pollution is serious day by day, the harmonious development of the energy, resource, environment and human society becomes the focus of social concerns day by day, the harmonious development of seek renewable and clean energy resource, seeking human and environment progressively becomes the theme in epoch, therefore has the object that high power density and high-energy-density, pollution-free, reusable lithium ion battery become national governments and scientific research institution's common concern.At present, material with carbon element is owing to having better performance, advantage such as inexpensive and nontoxic aspect safety and the cycle life, be applied to lithium ion battery industry as negative material widely.
In order further to improve the energy density of negative pole, people begin to turn one's attention to the material that can form alloy with elemental lithium.Metallic aluminium and lithium ion react and generate the Li-Al alloy, and (theoretical specific capacity is 993mAhg to have bigger specific capacity
-1), the negative material that can be used as lithium ion battery uses.Y.Homan[Y.Homan, T.Brousse, F.Jousse et al.Journal of Power Sources, 2001,97-98:185-187.] etc. this is studied in great detail, find that when using pure metallic aluminium as lithium ion battery negative material, its specific capacity is relevant with the thickness of employed aluminium foil, along with reducing of aluminum foil thickness, its specific capacity constantly increases; But, form " dendrite " in the electrochemical reaction process easily and sting barrier film, the cycle performance extreme difference of battery when pure metallic aluminum during as lithium ion battery negative.2004, Geim etc. prepared Graphene first, thereby had drawn back the prelude of Graphene research; 2009, employing low temperature expanding methods such as inventor Yang Quan is red have realized the low-cost magnanimity preparation of Graphene, obtained having the grapheme material of good nanostructure and energy storage character, thereby for the industrialization of Graphene and at energy storage Application for Field [the Wei Lv that lays the first stone, Dai-Ming Tang, Yan-Bing He et al., ACSNano, 2009,3 (11): 3730-3736. Yang Quan is red, Lv Wei, Sun Hui, high electrochemistry capacitance oxidization plumbago alkene and low temperature preparation method thereof and application, CN 200810151807.X].Meanwhile, [Peng Guo such as Song Huaihe, Huaihe Song, Xiaohong Chen., Electrochemistry Communications, 2009,11:1320-1324.] and Guoxiu Wang[Guoxiu Wang, Xiaoping Shen, Jane Yao et al., Carbon, 2009,47:2049-2053.] respectively it is furtherd investigate as lithium ion battery negative, find that it has bigger charge ratio capacity, but in the charging and discharging curve not platform occur, influenced Graphene as negative material in the lithium ion battery Application for Field.Graphene is particularly splendid at the effect of lithium ion cell positive additive agent field, under the situation of adding very in a small amount, just can reach or surmount effect [the Fang-Yuan Su of general commercial li-ion battery conductive additive, Conghui You, Yan-BingHe, et al.J.Mater.Chem., 2010.Yang Quanhong; Lv Wei; He Yanbing etc. are the electrode of conductive additive and the application in lithium ion battery with the Graphene, CN101794874A].
Summary of the invention
The object of the present invention is to provide Graphene/aluminium composite negative pole material of a kind of lithium ion battery and preparation method thereof, the lithium ion battery specific volume for preparing with this negative material is big, the charging/discharging voltage platform is low, good cycle, and its preparation method process is simple.
To achieve these goals, technical scheme of the present invention is as follows: a kind of Graphene of lithium ion battery/aluminium composite negative pole material, it is characterized in that this composite negative pole material is 1: 0.1～100 to be made up of Graphene and aluminium by mass ratio, its capacity reaches 600～1200mAh/g.
The preparation method of the Graphene of above-mentioned lithium ion battery/aluminium composite negative pole material is characterized in that comprising following process:
(1) is 1: 0.1～100 by Graphene and metallic aluminium powder mass ratio, takes by weighing Graphene and metallic aluminium powder, adopt ball milling, stirring or the ultrasonic dispersion material that is uniformly mixed;
(2) Graphene/aluminium powder composite material that mixing in the step (1) is obtained is compressed on the Copper Foil collector and prepares electrode slice, with the lithium sheet is positive pole, be assembled into battery, then under the current density of 1-500mA/mg, discharge and recharge 1-100 circulation and carry out slaking, obtain silicon/carbon/graphite in lithium ion batteries alkene/aluminium negative material after the slaking.
The present invention has following advantage: preparation process is simple, the capacity and the cycle performance of the lithium ion battery of Graphene of the present invention/aluminium composite negative pole material preparation not only are higher than fine aluminium and pure Graphene negative material far away, and be higher than existing business-like negative material, and as graphite, carbon nano-tube etc.Of the present invention being easy to realized, extensively promoted.
Description of drawings
Fig. 1 is the lithium ion battery charging and discharging curve with the Graphene of preparation in the embodiment of the invention 3/aluminium negative material preparation.As can be seen from Figure 1, the present invention is different from other grapheme material, takes off the lithium capacity first and can reach 1100mAhg
-1And voltage platform is lower, is about 0.48V vs Li
+/ Li.
Fig. 2 is for being that the lithium ion battery of negative material preparation and Comparative Examples 2 are the charge-discharge performance comparison diagram of three kinds of lithium ion batteries of the lithium ion battery for preparing of negative material with the fine aluminium with the lithium ion battery of the Graphene/aluminium negative material preparation of preparation in the embodiment of the invention 3 and Comparative Examples 1 with pure Graphene.Wherein the curve that couples together with ■ is that Graphene/aluminium composite material is the lithium ion battery cycle performance curve of negative pole, with ▲ curve that couples together is that pure aluminum material is the lithium ion battery cycle performance curve of negative pole, with ● the curve that couples together is that pure grapheme material is carry out of the lithium ion battery cycle performance curve of negative pole along with cycle charge-discharge.
Fig. 3 is the sem photograph with the Graphene/aluminium negative material of preparation in the embodiment of the invention 3.The aluminium nano particle is scattered in the Graphene surface comparatively equably.
Embodiment
Take by weighing Graphene 2g, aluminium powder 200mg, place ball mill, after the ball milling 5h, obtain mixing sufficient Graphene/aluminium composite material continuously; Take by weighing this composite material 540mg, concentration is that 60% polytetrafluoroethylene (PTFE) ethanol emulsion 386mg packs in the small beaker of 100ml, add the 40ml absolute ethyl alcohol again said mixture is mixed pulp, press the battery pole plates manufacture craft when baking is extremely half-dried, it is compressed on the Copper Foil collector makes negative plate, be placed on then in the vacuum drying chamber in 150 ℃ of oven dry down, with the lithium sheet is positive pole, form lithium ion battery with above-mentioned material, material is discharged and recharged 2 circulation slakings under the current density of 10mA/mg, obtain Graphene/aluminium composite negative pole material.
The preparation of lithium ion cell positive: get positive active material cobalt acid lithium, Kynoar (PVDF) is respectively 100.0g, 11.8g with conductive carbon black and mixes with 5.9g, drip the N-N-methyl-2-2-pyrrolidone N-said mixture is mixed pulp, press the battery pole plates manufacture craft when baking is extremely half-dried, evenly be compressed on it on aluminum foil current collector, be placed on then in the vacuum drying chamber and dry down, make lithium ion cell positive in 150 ℃;
The assembling of lithium ion battery: in dry glove box, positive pole, negative pole, barrier film and electrolyte are assembled according to cell making process, obtained the lithium ion battery that Graphene/aluminium composite material is a negative material after shelving 8h.
Take by weighing Graphene 2g, aluminium powder 2g, place mixer, after the continuous stirring 1h, obtain mixing sufficient Graphene/aluminium composite material; Take by weighing this composite material 1.08g, concentration is that 60% polytetrafluoroethylene (PTFE) ethanol emulsion 0.45g packs in the small beaker of 100ml, add 40ml N-N-methyl-2-2-pyrrolidone N-again said mixture is mixed pulp, press the battery pole plates manufacture craft when baking is extremely half-dried, it is compressed on the Copper Foil collector makes negative plate, be placed on then in the vacuum drying chamber in 100 ℃ of oven dry down, with the lithium sheet is positive pole, form lithium ion battery with above-mentioned material, material is discharged and recharged 1 circulation slaking under the current density of 100mA/mg, obtain Graphene/aluminium composite negative pole material.
The preparation of lithium ion cell positive: get anode active material of phosphate iron lithium, Kynoar (PVDF) is respectively 125.0g, 14.8g with conductive carbon black and mixes with 7.4g, drip absolute ethyl alcohol said mixture is mixed pulp, press the battery pole plates manufacture craft when baking is extremely half-dried, evenly be compressed on it on aluminum foil current collector, be placed on then in the vacuum drying chamber and dry down, make lithium ion cell positive in 100 ℃;
The assembling of lithium ion battery: in dry glove box, positive pole, negative pole, barrier film and electrolyte are assembled according to cell making process, obtained the lithium ion battery that Graphene/aluminium composite material is a negative material after shelving 12h.
Take by weighing Graphene 2g, aluminium powder 6g, place ball mill, after the ball milling 3h, obtain mixing sufficient Graphene/aluminium composite material continuously; Take by weighing this composite material 540mg, concentration is that 60% polytetrafluoroethylene (PTFE) ethanol emulsion 100mg packs in the small beaker of 100ml, add 30ml N-N-methyl-2-2-pyrrolidone N-again said mixture is mixed pulp, press the battery pole plates manufacture craft when baking is extremely half-dried, it is compressed on the Copper Foil collector makes negative plate, be placed on then in the vacuum drying chamber in 100 ℃ of oven dry down, with the lithium sheet is positive pole, form lithium ion battery with above-mentioned material, under the current density of 30mA/mg, discharge and recharge 1 circulation, Graphene/aluminum is discharged and recharged slaking, obtain Graphene/aluminium composite negative pole material.
Lithium ion battery is the lithium sheet to electrode;
The assembling of lithium ion battery: in dry glove box, be electrode with the pole piece that makes, be assembled into lithium ion battery according to cell making process with the lithium sheet.Shelving that 12h obtains with Graphene/aluminium composite material is the lithium ion battery of electrode material.Carry out charge-discharge test, measuring current density is 50mAg
-1The first charge-discharge curve as shown in Figure 1, preceding 10 circulation cycle performances of battery as shown in Figure 2, the sem photograph of the Graphene/aluminium composite material after the slaking is as shown in Figure 3.
Take by weighing Graphene 100mg, aluminium powder 10g, place ball mill, after the ball milling 20h, obtain mixing sufficient Graphene/aluminium composite material continuously; Take by weighing this composite material 28.5g, concentration is that 60% polytetrafluoroethylene (PTFE) ethanol emulsion 2.5g packs in the small beaker of 100ml, add 40ml N-N-methyl-2-2-pyrrolidone N-again said mixture is mixed pulp, press the battery pole plates manufacture craft when baking is extremely half-dried, it is compressed on the Copper Foil collector makes negative plate, be placed on then in the vacuum drying chamber in 100 ℃ of oven dry down, with the lithium sheet is positive pole, form lithium ion battery with above-mentioned material, under the current density of 50mA/mg, discharge and recharge 10 circulations, Graphene/aluminum is discharged and recharged slaking, obtain Graphene/aluminium composite negative pole material.
The preparation of lithium ion cell positive: get the positive active material spinel lithium manganate, butadiene-styrene rubber is respectively 150.0g, 17.6g with conductive carbon black and mixes with 8.8g, drip absolute ethyl alcohol said mixture is mixed pulp, press cell making process when baking is extremely half-dried, evenly be compressed on it on aluminum foil current collector, with the 80 ℃ of oven dry down under vacuum of positive electrical pole plate, make lithium ion cell positive then;
The assembling of lithium ion battery: in dry glove box, positive pole, negative pole, barrier film and electrolyte are assembled according to cell making process, obtained the lithium ion battery that Graphene/aluminium composite material is a negative material after shelving 24h.
Comparative Examples 1
Take by weighing Graphene 54mg, concentration is that 60% polytetrafluoroethylene (PTFE) ethanol emulsion 10mg packs in the small beaker of 20ml, add the 5ml absolute ethyl alcohol again, beaker is placed in the ultrasonic concussion machine then and shake 1h, the slurry that obtains mixing is pressed the battery pole plates manufacture craft when baking is extremely half-dried, it is compressed on the Copper Foil collector makes negative plate, be placed on then in the vacuum drying chamber and dry down, obtain a pole piece of lithium ion battery in 100 ℃.In dry glove box, be electrode with the lithium sheet with the pole piece that makes, be assembled into lithium ion battery according to cell making process.Shelve and carry out the anticathode material behind the 12h and under the current density of 30mA/mg, discharge and recharge 2 circulations, discharge and recharge slaking.
Minimum with the capacity of the lithium ion battery of the Graphene of the above-mentioned embodiment of the invention/aluminium composite negative pole material preparation is 800mAhg
-1, good cycle; And this Comparative Examples is the lithium ion battery of negative material preparation with pure Graphene, no charge and discharge platform, and capacity is near 300mAhg
-1And cycle performance is poor.It serves to show that Graphene of the present invention/aluminium composite negative pole material performance is higher than pure Graphene negative electrode material far away.
Comparative Examples 2
Take by weighing aluminium powder 5g, concentration is that 60% polytetrafluoroethylene (PTFE) ethanol emulsion 500mg packs in the small beaker of 150ml, add the 100ml absolute ethyl alcohol again, beaker is placed in the ultrasonic concussion machine then and shake 1h, the slurry that obtains mixing is pressed the battery pole plates manufacture craft when baking is extremely half-dried, it is compressed on the Copper Foil collector makes negative plate, be placed on then in the vacuum drying chamber and dry down, obtain a pole piece of lithium ion battery in 100 ℃.In dry glove box, be electrode with the lithium sheet with the pole piece that makes, be assembled into lithium ion battery according to cell making process.Shelve and carry out the anticathode material behind the 12h and carry out under the current density of 30mA/mg, discharging and recharging 2 all slakings.
Minimum with the capacity of the lithium ion battery of the Graphene of the above-mentioned embodiment of the invention/aluminium composite negative pole material preparation is 800mAhg
-1, good cycle; And this Comparative Examples is the lithium ion battery of negative material preparation with the fine aluminium, and after two charge and discharge cycles slakings, the 3rd circulation time, capacity are almost near 0mAhg
-1, no practical value.It serves to show that Graphene of the present invention/aluminium composite negative pole material performance is higher than the pure aluminium cathode electrode material far away.
The foregoing description is preferred embodiment of the present invention, is not to be used for limiting the scope of the present invention, so all equivalences of being done with the described structure of claim of the present invention, feature and principle change or modify, all should be included within the claim scope of the present invention.
Claims (2)
1. the Graphene of a lithium ion battery/aluminium composite negative pole material is characterized in that, this composite negative pole material is 1: 0.1～100 to be made up of Graphene and aluminium by mass ratio, and capacity reaches 600～1200mAh/g.
2. method for preparing the Graphene/aluminium composite negative pole material of the described lithium ion battery of claim 1 is characterized in that comprising following process:
(1) is 1: 0.1～100 by Graphene and metallic aluminium powder mass ratio, takes by weighing Graphene and metallic aluminium powder, adopt ball milling, stirring or the ultrasonic dispersion material that is uniformly mixed;
(2) Graphene/aluminium powder composite material that step (1) mixing is obtained is compressed on the Copper Foil collector and prepares electrode slice, with the lithium sheet is positive pole, be assembled into battery, then under the current density of 1-500mA/mg, discharge and recharge 1-100 circulation and carry out slaking, obtain silicon/carbon/graphite in lithium ion batteries alkene/aluminium negative material after the slaking.
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| CN103000245A (en) * | 2012-12-03 | 2013-03-27 | 京东方科技集团股份有限公司 | Graphene metal hybrid electrode material and preparation method and applications thereof |
| CN103035891A (en) * | 2011-10-09 | 2013-04-10 | 海洋王照明科技股份有限公司 | Graphene nanometer sheet and silicon combined electrode material and preparation method of electrode material |
| CN103178244A (en) * | 2011-12-23 | 2013-06-26 | 财团法人工业技术研究院 | Hybrid energy storage element |
| CN104218225A (en) * | 2014-05-07 | 2014-12-17 | 江南石墨烯研究院 | Submicron graphene/lithium-rich lithium-nickel-cobalt-manganese oxide compound and preparation method thereof |
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| CN108326302A (en) * | 2018-02-26 | 2018-07-27 | 华南理工大学 | A kind of graphene enhancing aluminum alloy materials and preparation method thereof |
| CN109546083A (en) * | 2018-11-17 | 2019-03-29 | 广西中医药大学 | A kind of graphene battery negative plate and preparation method thereof |
| CN110380003A (en) * | 2019-07-02 | 2019-10-25 | 天津大学 | A kind of cathode of lithium battery and preparation method thereof, lithium battery |
| US10566623B2 (en) | 2017-06-22 | 2020-02-18 | Aselsan Elektronik Sanayi Ve Ticaret A.S | Thin cathode for micro-battery |
| WO2020076188A1 (en) * | 2018-10-11 | 2020-04-16 | Joint Stock Company "Irkutsk Electronetwork Company" (Jsc "Ienk") | Aluminum-ion battery |
| CN112563511A (en) * | 2020-12-10 | 2021-03-26 | 深圳中科瑞能实业有限公司 | Aluminum-containing negative electrode material, negative electrode plate and lithium ion secondary battery |
| CN115870496A (en) * | 2022-11-25 | 2023-03-31 | 湖南法恩莱特新能源科技有限公司 | Graphene-aluminum compound and preparation method and application thereof |
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| CN103178244A (en) * | 2011-12-23 | 2013-06-26 | 财团法人工业技术研究院 | Hybrid energy storage element |
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Application publication date: 20110105 |