CN101414674A - Cathode material for lithium ion battery tin/carbon nanometer multilayer film, and preparation method and application thereof - Google Patents
Cathode material for lithium ion battery tin/carbon nanometer multilayer film, and preparation method and application thereof Download PDFInfo
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- CN101414674A CN101414674A CNA2008100300049A CN200810030004A CN101414674A CN 101414674 A CN101414674 A CN 101414674A CN A2008100300049 A CNA2008100300049 A CN A2008100300049A CN 200810030004 A CN200810030004 A CN 200810030004A CN 101414674 A CN101414674 A CN 101414674A
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Abstract
The invention provides a preparation method for a tin/carbon nano multilayer film cathode material of a lithium ion cell. The preparation method comprises the following steps: (1) preprocessing a substrate, a tin target, a graphite target and a vacuum coating chamber; (2) placing the substrate, the tin target and the graphite target into the vacuum coating chamber, and charging argon into the vacuum chamber after vacuumizing; (3) turning on a DC power supply to bomb the substrate; (4) turning on a radio frequency power supply to pre-sputter the target materials; and (5) formally sputtering, coating and alternately depositing the tin film and the carbon film. The invention also provides the tin/carbon nano multilayer film cathode material of the lithium ion cell prepared by the method and an application thereof. Compared with the prior art, the cathode material largely improves the cycle stability and the charge efficiency and discharge efficiency of an electrode, has the advantages of simple method and convenient operation, provides a reference to the industrialized production, and has the significant use value and good application prospect.
Description
Technical field
The present invention relates to the lithium ion battery material field, particularly a kind of as lithium ion battery negative pole, have tin/carbon nanometer multilayered film material of height ratio capacity and high cyclical stability and its production and application.
Technical background
Lithium ion battery has voltage height, specific energy height, the life-span is long, self discharge is little and advantage such as memory-less effect, has been widely used in fields such as photoelectricity, information, traffic and national defense and military.Lithium ion battery has become one of modern and following important new forms of energy along with the continuous expansion of its purposes.
Negative material is the key factor of decision lithium ion battery combination property quality, therefore, try to explore the specific capacity height, have extended cycle life, security performance well and the wide new type lithium ion battery negative material system of temperature applicable range, become the current crucial common problem of researching and developing the high performance lithium ion battery material in the world.
At present, the subject matter of commercialization carbon negative pole material existence is: (1) actual specific capacity is low, is about 300～330mAh/g; (2) form solid electrolyte interface (SEI) film because lithium irreversibly embeds lattice and is consumed in, cause bigger initial stage irreversible capacity loss; (3) be subjected to lithium ion (Li
+) diffusion coefficient (about 10
-10Cm
2/ s) restriction, its multiplying power discharging property is poor.
Although people are by carrying out doping vario-property or surface treatment to material with carbon element, because the lower theoretical specific capacity (372mAh/g) of material with carbon element has still limited increasing substantially of actual specific capacity.
Tin base cathode material has height ratio capacity and advantage cheaply, has now become at present one of main flow negative material of research in the world.Tin (Sn) and lithium (Li) can form the Li of high atomic ratio
22Sn
5Alloy phase has the theoretical specific capacity up to 990mAh/g, and this is the basis of exploitation high-performance tin negative pole material.But the subject matter of tin negative pole material existence at present is that tin matrix is at Li
+Generation enormousness variation in the process is taken off in embedding, thereby causes the mechanical disintegration of tin matrix, causes distortion and cracking, thereby avalanche and efflorescence inefficacy gradually shows relatively poor charge-discharge performance.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art part, a kind of lithium ion battery tin/carbon nanometer multilayer film negative material with height ratio capacity and high cyclical stability is provided.
Another object of the present invention is to provide a kind of method for preparing above-mentioned lithium ion battery tin/carbon nanometer multilayer film negative material.
A further object of the present invention is to provide the application of above-mentioned lithium ion battery tin/carbon nanometer multilayer film negative material.
Purpose of the present invention realizes by following technical proposal: a kind of preparation method of lithium ion battery tin/carbon nanometer multilayer film negative material comprises following concrete steps:
(1) preliminary treatment of substrate, tin target and graphite target and vacuum film coating chamber;
(2) substrate, tin target and graphite target are put into vacuum film coating chamber, vacuumize the back and feed argon gas in vacuum chamber;
(3) open DC power supply, the bombardment substrate;
(4) open radio-frequency power supply, pre-sputtering target material;
(5) formal sputtering plated film, alternating deposit tin layer and carbon-coating;
(6) with the stove cooling, promptly obtain this product.
Among the preparation method of above-mentioned lithium ion battery tin/carbon nanometer multilayer film negative material, described substrate is meant Copper Foil; Described tin target purity is more than 99.9%; Described graphite target purity is more than 99.9% and graphite target damascene copper pedestal; The preliminary treatment of described substrate is in order with anhydrous propanone ultrasonic waves for cleaning, rinsed with deionized water, dilute sulfuric acid rinsing, rinsed with deionized water and dry up; The preliminary treatment of described tin target, graphite target and vacuum film coating chamber is meant that adopting anhydrous propanone to put on the skin washes.
Described the vacuumizing of step (2) is meant vacuum degree≤2 * 10
-3Pa, described purity of argon is more than 99.999%.
The described bombardment substrate of step (3) is at 80～160W power bombardment substrate, 5～10min.
The described pre-sputtering target material of step (4) is the pre-sputtering target material 5～10min of 100～200W power.
The described sputter coating of step (5), alternating deposit tin layer and carbon-coating are meant and adopt radio frequency or magnetically controlled DC sputtering tin target earlier, obtain certain thickness pure tin rete; After cooling, on the tin film that is obtained, adopt radio frequency or magnetically controlled DC sputtering graphite target again; So repeatedly, prepare several modulation periods, in the disposable preparation of finishing tin/carbon nanometer sandwich construction film of vacuum chamber.The power of described radio frequency or magnetically controlled DC sputtering is 100～400W; Time is got 2～30min.Described certain thickness is: 0～3 μ m; Be meant described several modulation periods: 1～10 modulation period.
The lithium ion battery tin/carbon nanometer multilayer film negative material that is obtained by method for preparing has the metallic tin layer and graphite linings is alternately piled up the sandwich construction that forms.
The lithium ion battery tin/carbon nanometer multilayer film negative material that is obtained by method for preparing can be applicable to prepare lithium ion battery; With a kind of buckle type lithium-ion battery is example, concrete application mode is: with the electrode of tin/carbon nanometer multilayer film as lithium ion battery, for being that electrolyte, microporous polyethylene or polypropylene screen are barrier film, promptly be assembled into a kind of buckle type lithium-ion battery with pour lithium slice to electrode, the conventional organic electrolyte that contains lithium ion.
Principle of the present invention is: the inventor at tin electrode in embedding/when taking off lithium, because of volumetric expansion/contraction causes tin matrix cracking and efflorescence this problem that lost efficacy, propose to make up the conception of tin/carbon nanometer sandwich construction film, the high power capacity of comprehensive utilization tin and the support structure effect of carbon, on copper foil substrate, prepare tin/carbon nanometer multilayer film, as the lithium ion battery negative material.The multi-layer film structure of graphite and tin more helps Li
+Embedding is taken off, and more embedding lithium passage and embedding lithium position can be provided.Simultaneously, graphite linings has been brought into play the effect of structural support, has elastomer and electric transmission network function.Graphite linings has been alleviated the electrode avalanche that tin electrode causes owing to volumetric expansion at charge and discharge process as elastomer; As the network of electric transmission, kept tin electrode in the high utilance in degree of depth circulation back.
Based on the foregoing invention principle, the present invention compared with prior art has the following advantages and beneficial effect: relative pure tin electrode, the tin/carbon nanometer multilayer film electrode has improved its cyclical stability and efficiency for charge-discharge significantly.Tin/carbon two layer membrane electrode are compared with the pure tin electrode, and after 20 charge and discharge cycles, the capacity of tin/carbon two layer membrane electrode maintains the capacity 270mAh/g that 515mAh/g is higher than the pure tin electrode; Coulombic efficiency is 73% first, is higher than the coulombic efficiency first 57% of pure tin electrode.This shows, the compound tin electrode of graphite alleviates or change in volume causes when having suppressed the tin doff lithium internal stress, has postponed the film cracking, has avoided the film efflorescence to lose efficacy, and is keeping more complete film initial configuration, has improved the cyclical stability of electrode.In addition, the inventive method is simple, easy and simple to handle, for suitability for industrialized production provides foundation, has significant practical value and good prospects for application.
Description of drawings
Fig. 1 is the preparation flow figure of lithium ion battery tin/carbon nanometer multilayer film negative material of the present invention.
Fig. 2 is prepared pure tin film and the first charge-discharge curve chart of tin/carbon two layer membrane electrode when charge-discharge magnification is C/5 of embodiment 1.
Fig. 3 is the prepared pure tin film of embodiment 1 and the cycle performance curve chart of tin/carbon two layer membrane electrode.
Fig. 4 is the film SEM shape appearance figure after the prepared pure tin film of embodiment 1 and 20 circulations of tin/carbon two layer membrane electrode; Wherein a is the pure tin film; B is tin/carbon two tunics.
Fig. 5 is 30 cycle performance curve charts of prepared tin/carbon ten layer membrane electrode of embodiment 4.
Embodiment
The present invention is described in further detail below in conjunction with embodiment and accompanying drawing, but embodiments of the present invention are not limited only to this.
Embodiment 1
The RFMS-4 sputter that present embodiment adopts is a self design, partly is made up of vacuum system, vacuum film coating chamber, radio-frequency power supply, three DC power supply, air supply system etc.Establish four water-cooled magnetic controlled sputtering targets in the vacuum chamber, a built-in water-cooled substrate holder can carry out the multistation rotation, and the distance between substrate and target surface is adjustable, and the adjustable distance scope is 20mm.Have two substrate lids to exchange according to required plated film area, substrate lid diameter is 50mm, and the machining area diameter is 40mm; Another substrate lid diameter is 40mm, and the machining area diameter is 30mm.The target diameter is 59mm, and effectively the machining area diameter is 50mm, and target thickness is 1～5mm.Each target is furnished with permanent magnet assembly, radome, cooling water system and sealing system.Vacuum system is made up of mechanical pump and diffusion pump, and maximum vacuum can reach 1 * 10
-4Pa.Utilize the various combination of three DC power supply and a radio-frequency power supply can prepare metal and nonmetal nano-multilayer film, membrana granulosa, gradient film etc.
Fig. 1 shows the preparation flow of tin/carbon nanometer multilayer film negative material, specifically comprises following operating procedure:
(1) preliminary treatment of substrate, target and vacuum chamber
Substrate is selected Copper Foil for use, and size is Φ 50mm, and thickness is 10 μ m; Tin target purity 99.9%, specification are Φ 59 * 4mm; Graphite target purity 99.9%, specification are Φ 52 * 5mm, graphite target damascene copper pedestal.Above material provides by Shenzhen Ou Lai sputtering target material Co., Ltd.Following handling procedure is adopted in the preliminary treatment of Copper Foil: anhydrous propanone ultrasonic waves for cleaning 20min → rinsed with deionized water → dilute sulfuric acid rinsing 1min → rinsed with deionized water → dry up; The preliminary treatment of target and vacuum film coating chamber is adopted anhydrous propanone to put on the skin and is washed.
(2) clamping substrate and target → open cooling water, start → be evacuated to 2 * 10
-3Pa → in vacuum chamber, feed argon gas (99.999%, 60ml/min).
(3) open DC power supply, bombardment substrate 5min (100W power).
(4) open radio-frequency power supply, the pre-sputter 10min of target (100W power).
(5) on copper foil substrate, (99.9%, Φ 59 * 4mm), and the time is 20min, obtain the pure tin film to adopt magnetically controlled DC sputtering 250W sputter tin target earlier; And then (99.95%, Φ 52 * 5mm), and the time is 10min, obtain tin/carbon two tunics to adopt the rf magnetron sputtering graphite target on the tin film that is obtained.
(6) with stove cooling 40min, close vacuum system, shut down, close cooling water and power supply.
After tested, tin thickness is 320nm.In order to contrast, be the work electrode of lithium ion battery with pure tin film and tin/carbon two tunics respectively, to electrode be pour lithium slice, electrolyte is the conventional organic electrolyte, the barrier film that contain lithium ion and is microporous polyethylene or polypropylene screen, be assembled into button cell, and in the voltage range of 0～1.5V, on the charge-discharge test instrument, carry out charge-discharge test with the multiplying power of C/5.Test result as shown in Figures 2 and 3.
The result shows that behind the composite graphite layer, the lithium embedding behavior of taking off of tin electrode obviously is improved.After 20 circulations, the capacity of pure tin electrode is 270mAh/g, and the capacity of tin/carbon two layer membrane electrode also maintains 515mAh/g, and coulombic efficiency is 73% first, is higher than the coulomb 57% first of pure tin electrode.
Fig. 4 is the surface topography map contrast of the film after pure tin film and 20 circulations of tin/carbon two layer membrane electrode.The result shows, behind the composite graphite layer, has postponed film cracking and efflorescence and has lost efficacy, and when the basic efflorescence of tin electrode was lost efficacy, tin/carbon electrode was still keeping more complete film initial configuration, thereby has improved the cycle performance of electrode.
Embodiment 2
Present embodiment except that following characteristics with embodiment 1:
The described bombardment substrate of step (3) is at 80W power bombardment substrate 10min.
The described pre-sputtering target material of step (4) is the pre-sputtering target material 5min of 200W power.
The described sputter tin of step (5) target is to adopt radio frequency sputtering, and power is 150W, and the time is 15min; The time of sputter graphite target is 5min; Step is evacuated to 1 * 10 in (2)
-4Pa, the argon gas of feeding 99.9999%.
The tin of gained/carbon two membranes electrode discharge capacity first is 778mAh/g, and first charge-discharge efficiency is 69%, and through 20 circulations, capacity remains 330mAh/g, and coulombic efficiency maintains more than 90%.
Embodiment 3
Present embodiment except that following characteristics with embodiment 2:
The described bombardment substrate of step (3) is at 160W power bombardment substrate 5min.
The described pre-sputtering target material of step (3) is the pre-sputtering target material 7min of 150W power.
The time of the described sputter graphite target of step (5) changes 20min into.
The tin of gained/carbon two membranes electrode discharge capacity first is 670mAh/g, and first charge-discharge efficiency is 90%, and through 20 circulations, capacity remains 550mAh/g, and coulombic efficiency maintains more than 95%.
Embodiment 4
On the basis of embodiment 1, step among the preparation method of tin/carbon nanometer multilayer film negative material (5) changes into:
(5) on copper foil substrate, (99.9%, Φ 59 * 4mm), and sputtering power is 150W, and sputtering time is 5min to adopt rf magnetron sputtering tin target earlier; Behind the cooling 20min, and then (99.95%, Φ 52 * 5mm), and sputtering power is 150W, and sputtering time is 2min to adopt the rf magnetron sputtering graphite target on the tin film that is obtained; So repeatedly, prepare 10 modulation periods, in the disposable preparation of finishing ten layers of structural membrane of tin/carbon of vacuum chamber.
All the other preparation technology's flow processs and embodiment 1 obtain lithium ion battery tin/carbon ten tunic negative materials thus.
With tin/carbon ten tunic negative materials of obtaining work electrode as lithium ion battery, with pour lithium slice for being that electrolyte, microporous polyethylene or polypropylene screen are barrier film to electrode, the conventional organic electrolyte that contains lithium ion, be assembled into button cell, and in the voltage range of 0～1.5V, multiplying power with C/5 is carried out charge-discharge test on the charge-discharge test instrument, get its cycle performance curve as shown in Figure 5.
Test result shows that the lithium of the embedding first capacity of tin/carbon ten layer membrane electrode is 693mAh/g, and 30 times circulation back embedding lithium capacity is 310mAh/g, keeps 45% of capacity first; Coulombic efficiency 82% first, after this maintains 95～97%.This shows that ten tunic structures of graphite and tin more help Li
+Embedding is taken off, and more embedding lithium passage and embedding lithium position can be provided, and has improved the cyclical stability and the efficiency for charge-discharge of tin electrode significantly.
Embodiment 5
Among the embodiment 4 among the preparation method of tin/carbon nanometer multilayer film negative material, the technological parameter that the technological parameter of the described sputter tin of step (5) target changes " adopting rf magnetron sputtering; sputtering power is 250W; the time is 15min ", sputter graphite target into changes " adopting rf magnetron sputtering; sputtering power is 250W; the time is 5min " into, and all the other are with embodiment 1.
The lithium of the embedding first capacity of tin/carbon ten layer membrane electrode of gained is 670mAh/g, and 30 times circulation back embedding lithium capacity is 412mAh/g, keeps 62% of capacity first; Coulombic efficiency 86% first, after this maintains 95～100%.
Embodiment 6
Among the embodiment 4 among the preparation method of tin/carbon nanometer multilayer film negative material, technological parameter when the technological parameter during the described sputter tin of step (5) target changes " adopting magnetically controlled DC sputtering; sputtering power is 100W; the time is 10min ", sputter graphite target into changes " adopting rf magnetron sputtering; sputtering power is 400W; the time is 5min " into, and all the other are with embodiment 1.
The lithium of the embedding first capacity of tin/carbon ten layer membrane electrode of gained is 684mAh/g, and 30 times circulation back embedding lithium capacity is 380mAh/g, keeps 55% of capacity first; Coulombic efficiency 77% first, after this maintains 93～97%.
Embodiment 7
Among the embodiment 4 among the preparation method of tin/carbon nanometer multilayer film negative material, technological parameter when the technological parameter during the described sputter tin of step (5) target changes " adopting magnetically controlled DC sputtering; sputtering power is 400W; the time is 30min ", sputter graphite target into changes " adopting rf magnetron sputtering; sputtering power is 300W; the time is 5min " into, changes " preparing 5 modulation periods " modulation period into, and all the other are with embodiment 1.
After tested, tin thickness is about 3 μ m.The lithium of the embedding first capacity of tin/carbon five layer membrane electrode of gained is 698mAh/g, and 30 times circulation back embedding lithium capacity is 326mAh/g, keeps 48% of capacity first; Coulombic efficiency 75% first, after this maintains 94～97%.
Claims (9)
1, a kind of lithium ion battery tin/carbon nanometer multilayer film negative material is characterized in that: have metallic tin layer and graphite linings and alternately pile up the sandwich construction that forms.
2,, it is characterized in that may further comprise the steps according to the preparation method of the described lithium ion battery tin/carbon nanometer multilayer film negative material of claim 1:
(1) preliminary treatment of substrate, tin target and graphite target and vacuum film coating chamber;
(2) substrate, tin target and graphite target are put into vacuum film coating chamber, vacuumize the back and feed argon gas in vacuum chamber;
(3) open DC power supply, the bombardment substrate;
(4) open radio-frequency power supply, pre-sputtering target material;
(5) formal sputtering plated film, alternating deposit tin layer and carbon-coating;
(6) with the stove cooling, obtain finished product.
3, according to the preparation method of the described lithium ion battery tin/carbon nanometer multilayer film negative material of claim 2, it is characterized in that: described substrate is meant Copper Foil; Described tin target purity is more than 99.9%; Described graphite target purity is more than 99.9% and graphite target damascene copper pedestal; The preliminary treatment of described substrate is in order with anhydrous propanone ultrasonic waves for cleaning, rinsed with deionized water, dilute sulfuric acid rinsing, rinsed with deionized water and dry up; The preliminary treatment of described tin target, graphite target and vacuum film coating chamber is meant that adopting anhydrous propanone to put on the skin washes.
4, according to the preparation method of the described lithium ion battery tin/carbon nanometer multilayer film negative material of claim 2, it is characterized in that: described the vacuumizing of step (2) is meant vacuum degree≤2 * 10
-3Pa, described purity of argon is more than 99.999%; The described bombardment substrate of step (3) is at 80～160W power bombardment substrate, 5～10min; The described pre-sputtering target material of step (4) is the pre-sputtering target material 5～10min of 100～200W power.
5, according to the preparation method of the described lithium ion battery tin/carbon nanometer multilayer film negative material of claim 2, it is characterized in that: the described sputter coating of step (5), alternating deposit tin layer and carbon-coating are meant and adopt radio frequency or magnetically controlled DC sputtering tin target earlier, obtain certain thickness pure tin rete; After cooling, on the tin film that is obtained, adopt radio frequency or magnetically controlled DC sputtering graphite target again; So repeatedly, prepare several modulation periods, in the disposable preparation of finishing tin/carbon nanometer sandwich construction film of vacuum chamber.
6, the preparation method of lithium ion battery tin/carbon nanometer multilayer film negative material according to claim 5 is characterized in that: the power of described radio frequency or magnetically controlled DC sputtering is 100～400W; Time is got 2～30min.
7, the preparation method of lithium ion battery tin/carbon nanometer multilayer film negative material according to claim 5 is characterized in that: described certain thickness is: 0～3 μ m; Be meant described several modulation periods: 1～10 modulation period.
8, lithium ion battery tin/carbon nanometer multilayer film negative material according to claim 1 is made the application in field at lithium ion battery.
9, lithium ion battery tin/carbon nanometer multilayer film negative material according to claim 8 is made the application in field at lithium ion battery, it is characterized in that: with the electrode of tin/carbon nanometer multilayer film as lithium ion battery, for being that electrolyte, microporous polyethylene or polypropylene screen are barrier film, be assembled into the buckle type lithium-ion battery with pour lithium slice to electrode, the conventional organic electrolyte that contains lithium ion.
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| CN108493402A (en) * | 2018-04-12 | 2018-09-04 | 太原科技大学 | The method for preparing lithium-sulphur cell positive electrode piece using ion beam sputtering technology |
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| WO2020207363A1 (en) * | 2019-04-08 | 2020-10-15 | 青岛九环新越新能源科技股份有限公司 | Multilayer electrode based on mass transfer reduction and diffusion control, and an energy storage device |
| CN112599735A (en) * | 2020-12-11 | 2021-04-02 | 合肥国轩高科动力能源有限公司 | Modified NCM622 ternary cathode material and preparation method thereof |
| CN112599735B (en) * | 2020-12-11 | 2022-02-18 | 合肥国轩高科动力能源有限公司 | Modified NCM622 ternary cathode material and preparation method thereof |
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