CN102054961A - Active negative pole piece and preparation method thereof - Google Patents
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Abstract
An active negative pole piece comprises a metal substrate, an active material layer coated on the metal substrate and a buffer layer coated on the active material layer, wherein, the active material layer and the buffer layer are prepared through the magnetron sputtering technology; the active layer is made of Si and one of such doped chemical elements as H, C, Al, Ni, Co and Cu; the buffer layer is made of C and one of such chemical elements as Al, B, Fe, Cu and Ag; and the thickness of the active material layer ranges from 1 to 20 Mu m. The preparation method of the active negative pole piece comprises the following steps: the metal substrate and a target material are placed in a magnetron sputtering device; the sputtering power is selected between 1000 and 5000W; the temperature of the metal substrate is maintained between 100 and 300 DEG C; and the sputtering time is between 3 and 6.5 hours, wherein, the Si target sputtering time accounts for 80% to 90% of the total sputtering time. Through the Si membrane doping and the great improvement of the magnetron sputtering power, a prepared Li-ion secondary battery has the advantages of high charge-discharge capacity, superior cycle performance and excellent electrochemical performance. Compared with the previously reported silicon substrate membrane negative pole pieces, the initial charge-discharge efficiency and the discharge capacity of the prepared Li-ion secondary battery are greatly improved. Moreover, the manufacture process is simple, and the production efficiency is improved.
Description
Technical field
The present invention relates to lithium ion battery, particularly a kind of active cathode pole piece and preparation method thereof.
Background technology
Lithium rechargeable battery is a notebook computer, camera, and the vital power supply of mobile phone and other communication devices, and will be used for automobile and other vehicles as green energy resource.Thereby the battery that need have high-energy-density and high power density, need to obtain the lithium rechargeable battery that size is littler, weight is lighter, energy storage capability is higher, charge-discharge performance is more excellent.
The silica-base film negative material reaches lower embedding lithium current potential and causes concern widely with its higher storage lithium capacity, satisfies the lithium rechargeable battery demand of development at present.But the first charge-discharge efficiency of silica-base material is lower, and under the condition of height removal lithium embedded, exists serious bulk effect, structural instability when its reason mainly is the lithium alloy removal lithium embedded.Improve the first charge-discharge efficiency of silica-base material, the cycle performance that improves material is the main direction of studying of present silica-base film negative material.
Sputtering method utilizes high energy particle (the normally cation that is quickened by electric field) to impact the surface of solids exactly, the atom of the surface of solids, molecule and these high energy particles exchange kinetic energy, thereby splashed out by the surface of solids, these particles are deposited on substrate surface (negative pole) and form film.
The negative material of lithium ion battery remains traditional carbon-based material at present, for example hard carbon, Delanium.Silica-base material as the shortcoming of the negative material of lithium ion battery is: irreversible capacity is big and cycle performance is poor first, and particularly first charge-discharge efficiency and graphite electrode differs greatly.Basic reason is: the reaction mechanism of silicon-based anode material is different from graphite cathode material.Graphite cathode material has special stratiform open architecture, and when carrying out the doff lithium reaction, reconstruct does not take place structure, and the pucker ﹠ bloat of volume only takes place.The silicon-based anode material can form Li when the doff lithium reaction takes place
12Si
7, Li
7Si
3, Li
13Si
4And Li
22Si
5The Li-Si alloy of four kinds of phases, when compound formed, reconstruct can take place in the structure of component crystal, and is accompanied by big volumetric expansion; Simultaneously, owing to the reasons such as electrical conductivity variation that transformation mutually, surperficial dangling bonds and particle volume variation cause, irreversible capacity is big during first charge-discharge.In non-crystalline material, be that even if expansion and contraction are reversible, the variation of volume also can produce very big irreversible capacity uniformly though lithium embeds the volumetric expansion that causes.Therefore, need improve,, improve the structure of material, reduce the influence of volumetric expansion, reduce the irreversible capacity that discharges and recharges of material simultaneously the generation of material so that improve the chemical property of silicon-based anode material to preparation methods and processing technology.
In the electrode material research in early days, Bourderau S etc. adopt the amorphous silicon membrane of vapour deposition process preparation, 3 times Xun Huan discharge capacity reaches 1000mAh/g, but cycle performance remains to be improved [Bo urderau S, Brousse T, Schleich D M.Amorphous silicon as a pos sible anode material for Li-ion batteries[Jl.J Power Sources, 1999,81-82:233 236].Structural unstable shortcoming when solving the lithium alloy doff lithium, improve the cycle performance of silica-base material, the researcher has taked multiple measure, employing high-energy ball milling methods such as G.X.Wang have prepared the Sn/C composite material, discharge capacity can reach 1080mAh/g first, but irreversible capacity is higher first, very low [the Wang G X of capability retention, Ahn J H, Lindsay M J, e t al.Graphite-tin composites as anode materialsfor lithiunr-ion batteries[J] .J Power Sources, 2001,97-98:211-215], there is the researcher to adopt alloy or the intermetallic compound of high energy ball mill method with active material and inert metal reaction generation respective metal, in the electric conductivity that has improved material, also improved cycle performance.At present, employing high energy ball mill methods such as Wang Pu have prepared the Si-Cu/C composite material as lithium ion battery negative material, utilize the relative smaller volume of cupro silicon good electrical conductivity to change the bulk effect that cushions silicon with graphite, the change in volume of overall electrode is controlled at reasonable levels, thereby improve the cycle performance [Wang Pu of composite material, exert beautiful swallow Na, Yang Jun. the preparation and the performance study of high power capacity Si-Cu/C composite negative pole material in the lithium ion battery. rare metal .2007,31 (1), 63-66].But in circulation first, the embedding lithium capacity of Si-Cu/C composite material is 1021mAh/g, and reversible capacity is 524mAh/g only first, and irreversible capacity is bigger.Khomenko V G etc. are coated on native graphite surface (or evenly spread in graphite matrix ultra-fine silicon particle) with amorphous nano-silicon, coat silicon/graphite material with amorphous carbon again, carbon/silicon/graphite the lithium ion battery negative material of preparation, its reversible capacity is 604mAh/g, irreversible capacity loss has only 8.1%[Khomenko V G, Barsukov V Z, Dorlaiger J E.J PowerSources[J], 2007,165 (2): 598-608].
Therefore, the lithium rechargeable battery of prior art fill diligent capacitance and cycle performance is still poor, can not satisfy people's various demands far away.
Summary of the invention
For improving the chemical property of Si negative material, the invention provides a kind of active cathode pole piece and preparation method thereof.
The active cathode pole piece of the present invention is to cover a resilient coating again after covering an active material layer on the metal substrate, and active material layer and resilient coating adopt the magnetron sputtering technique preparation.
Described active layer is one of silicon and doped chemical hydrogen, carbon, aluminium, nickel, cobalt, copper.
Described cushioning layer material is one of carbon and aluminium, boron, iron, copper, silver.
The thickness of described active material layer is 1-20 μ m.
The active cathode pole piece preparation method of the present invention comprises the steps:
1) in magnetic control sputtering device, lays metal substrate and target;
2) sputtering power is selected 1000-5000W;
3) keep the metal substrate temperature between 100-300 ℃;
4) sputtering time 3-6.5 hour, wherein Si target sputtering time took 80-90%.
Active cathode pole piece of the present invention and preparation method thereof, mix and increase substantially magnetron sputtering power by the Si film, prepared lithium rechargeable battery has high charge-discharge capacity and excellent cycle performance, chemical property is good, and the silica-base film cathode pole piece that efficiency for charge-discharge and discharge capacity are all reported before is greatly improved; First and manufacturing process simple, improved production efficiency.
Description of drawings
Fig. 1 is in active cathode pole piece cross sectional representation.
Fig. 2 is cathode pole piece cycle performance and the efficiency for charge-discharge curve chart of embodiment 1.
Fig. 3 is cathode pole piece cycle performance and the efficiency for charge-discharge curve chart of embodiment 2.
Fig. 4 is cathode pole piece cycle performance and the efficiency for charge-discharge curve chart of embodiment 3.
Fig. 5 is the cycle performance curve chart of the cathode pole piece of comparative example 1.
Fig. 6 is the efficiency for charge-discharge curve chart of the cathode pole piece of comparative example 1.
Fig. 7 is cathode pole piece cycle performance and the efficiency for charge-discharge curve chart of embodiment 4.
Fig. 8 is cathode pole piece cycle performance and the efficiency for charge-discharge curve chart of embodiment 5.
Fig. 9 is cathode pole piece and the LiCoO of embodiment 5: the cycle performance and the efficiency for charge-discharge curve chart of the button cell of coupling back preparation.
Figure 10 is the cycle performance curve chart of the cathode pole piece of embodiment 6.
Figure 11 is the efficiency for charge-discharge curve chart of the cathode pole piece of embodiment 6.
Figure 12 is the cycle performance curve chart of the cathode pole piece of embodiment 7.
Figure 13 is the efficiency for charge-discharge curve chart of the cathode pole piece of embodiment 7.
Embodiment
Below in conjunction with embodiment the present invention is carried out more detailed explanation.
The active cathode pole piece structure of the present invention as shown in Figure 1, be coated with negative electrode material layer 2 on the metal substrate 1 of cathode pole piece, in negative electrode material layer 2, in order to improve the performance of battery, often also has doped chemical 3, for example H element, C element, and the present invention prepares negative electrode material layer on the cathode pole piece by the high-power magnetically controlled sputter method that adopts 1000-5000W, thickness is 1-20 μ m, obtained high performance cathode pole piece and lithium rechargeable battery, will further be explained and illustrated by each embodiment below the present invention.
Embodiment 1
Adopt the magnetically controlled DC sputtering technology, be target with crystal Si target and C target respectively, at thickness be on the Cu paper tinsel of 12 μ m two layers of laminated film of deposition Si-C as negative electrode material layer, wherein, the Si layer is an active material layer, covering the C layer that needs on the Si layer is resilient coating, thereby forms the cathode pole piece of lithium rechargeable battery.Wherein, in sputter procedure, cavity heats up naturally, and the temperature of Cu paper tinsel is about 140 ℃ during to temperature stabilization, and two kinds of target as sputter power are all 1500W, and working gas Ar flow is 50sccm, impurity gas H
2Flow be 10sccm, pressure is about 0.6Pa in the sputtering chamber, total sputtering time is 4.5 hours, wherein, Si target sputtering time is 4 hours.
Gained film cathode pole piece and metal Li composition half-cell are carried out electrochemical property test, at current density 0.9m/cm
2Under carry out charge and discharge cycles, the charging/discharging voltage scope is at 0-1.0V, discharge platform is about 0.2V, charging platform is about 0.25V.Test result as shown in Figure 2, wherein a is the efficiency for charge-discharge curve, b is the cycle performance curve, as can see from Figure 2, the specific discharge capacity of this cathode pole piece can reach 2687.7mAh/g, and first charge-discharge efficiency is 90.8%, and capacity remains on about 89% after 75 charge and discharge cycles.
Utilize magnetron sputtering technique, be target with crystal Si target and C target respectively, at thickness be on the metal substrate Cu paper tinsel of 12 μ m deposition Si-C laminated film as negative electrode material layer, wherein, the Si layer is an active material layer, the C layer that covers on the Si layer is a resilient coating, thereby forms the negative pole of lithium rechargeable battery.Wherein, in sputter procedure, cavity heats up naturally, and during to temperature stabilization, the temperature of Cu paper tinsel is about 120 ℃, and two kinds of target as sputter power are all 1300W, and working gas Ar flow is 50sccm, impurity gas C
2H
2Flow be 3sccm, pressure is about 1.6Pa in the sputtering chamber, total sputtering time is 4.5 hours, wherein, Si target sputtering time is 4 hours.
Gained film cathode pole piece and metal Li composition half-cell are carried out electrochemical property test, and measuring current density is 1.2mA/cm
2, the charging/discharging voltage scope is at 0-1.0V, and discharge platform is about 0.2V, and charging platform is about 0.25V.Test result as shown in Figure 3, wherein a is the efficiency for charge-discharge curve, b is the cycle performance curve, as can see from Figure 3, the specific discharge capacity of cathode pole piece can reach 2521.3mAh/g, and first charge-discharge efficiency is 82.7%, and capacity is not decayed yet after 60 charge and discharge cycles.
Embodiment 3
Utilize the magnetically controlled DC sputtering technology, be target with crystal Si target and C target respectively, at thickness be on the metal substrate Cu paper tinsel of 12 μ m deposition Si-C laminated film as negative electrode material layer, wherein, the Si layer is an active material layer, the C layer that covers on the Si layer is a resilient coating, thereby forms the negative pole of lithium rechargeable battery.Wherein, the temperature of Cu paper tinsel is 150 ℃, and two kinds of target as sputter power are all 1400W, and working gas Ar flow is 46sccm, impurity gas C
2H: flow be 3sccm, pressure is 1.6Pa in the sputtering chamber, total sputtering time is 4.5 hours, wherein, Si target sputtering time is 4 hours.
Gained film cathode pole piece and metal Li composition half-cell are carried out electrochemical property test, and measuring current density is 1.1mA/cm
2, the charging/discharging voltage scope is at 0-1.0V.Test result as shown in Figure 4, wherein a is the efficiency for charge-discharge curve, b is the cycle performance curve, as can see from Figure 4, the specific discharge capacity of cathode pole piece can reach 2486.2mAh/g, and first charge-discharge efficiency is 84.5%, and capacity does not see that sorrow subtracts after 60 charge and discharge cycles.
Comparative example 1
In this comparative example in the preparation process of cathode pole piece, except sputtering power is that 450W and total sputtering time are 6.5 hours, other conditions are identical with embodiment 3 with step.
Gained film cathode pole piece and metal Li composition half-cell are carried out electrochemical property test, at current density 0.9mA/cm
2Under carry out charge and discharge cycles, the charging/discharging voltage scope is at 0-1.0V, discharge platform is about 0.2V, charging platform is about 0.25V.Test result as shown in Figure 5 and Figure 6, wherein, Fig. 5 is the cycle performance curve, the specific discharge capacity that therefrom can see cathode pole piece is 1751.1mAh/g, Fig. 6 is the efficiency for charge-discharge curve, can see that therefrom first charge-discharge efficiency is 63.96%, not decay of capacity after 75 charge and discharge cycles.
Can see from above-mentioned comparative example 1, compare that the present invention can improve specific discharge capacity and first charge-discharge efficiency significantly by the power that improves magnetron sputtering with embodiment 3.
Utilize the magnetically controlled DC sputtering technology, be target with crystal Si target and C target respectively, at thickness be on the metal substrate Cu paper tinsel of 12 μ m deposition Si-C laminated film as negative electrode material layer, wherein, the Si layer is an active material layer, the C layer that covers on the Si layer is a resilient coating, thereby forms the negative pole of lithium rechargeable battery.Wherein, the temperature of Cu paper tinsel is 150 ℃. two kinds of target as sputter power are all 1800W, and working gas Ar flow is 46sccm, the flow of impurity gas C2H2 is 11.3sccm, and pressure is 0.55Pa in the sputtering chamber, and total sputtering time is 4.5 hours, wherein, Si target sputtering time is 4 hours.
Gained film cathode pole piece and metal Li composition half-cell are carried out electrochemical property test, and measuring current density is 0.65mA/cm
2, the charging/discharging voltage scope is at 0-1.0V.Test result as shown in Figure 7, wherein a is the efficiency for charge-discharge curve, b is the cycle performance curve, as can see from Figure 7, the specific discharge capacity of cathode pole piece can reach 2600.4mAh/g, and first charge-discharge efficiency is 88.5%, and capacity remains on about 93% after 100 charge and discharge cycles.
Embodiment 5
Utilize the magnetically controlled DC sputtering technology, be target with crystal Si target and C target respectively, at thickness be on the metal substrate Cu paper tinsel of 12 μ m deposition Si-C laminated film as negative electrode material layer, wherein, the Si layer is an active material layer, the C layer that covers on the Si layer is a resilient coating, thereby forms the negative pole of lithium rechargeable battery.Wherein, the temperature of Cu paper tinsel is 150 ℃, and two kinds of target as sputter power are all 1800W, and working gas Ar flow is 50sccm, impurity gas C
2H
2Flow be 4.8sccm, pressure is 0.55Pa in the sputtering chamber, total sputtering time is 4.5 hours, wherein, Si target sputtering time is 4 hours.
Gained film cathode pole piece and metal Li composition half-cell are carried out electrochemical property test, and measuring current density is 0.71mA/cm
2, the charging/discharging voltage scope is at 0-1.0V.Test result as shown in Figure 8, wherein a is the efficiency for charge-discharge curve, b is the cycle performance curve, as can see from Figure 8, the specific discharge capacity of cathode pole piece can reach 2623.8mAh/g, and first charge-discharge efficiency is 84.6%, and capacity remains on about 95% after 100 charge and discharge cycles.
With the cathode pole piece of present embodiment preparation and with LiCoO
2Be the anode pole piece of positive electrode active materials, the assembling button cell according to the conventional method preparation.Positive plate is of a size of Φ 14mm
2, test result as shown in Figure 9, the first discharge specific capacity of gained battery is 131mAh/g, 100 times circulation volume remains on about 81%.
Above-mentioned positive electrode pole piece can prepare according to following method: utilize solvent such as N-N-methyl-2-2-pyrrolidone N-(NMP), disperse the mixture LiMO of composite oxides
2(wherein M is at least a transition metal) is as Li
XCoO
2, Li
XNiO
2, LiMn
2O
4, Li
XMnO
3Deng, use electric conducting material such as carbon black and binding agent such as Kynoar (PVDF) simultaneously, adopt the mixture that forms to be coated in above the metal substrate.
Utilizing magnetron sputtering technique, is target with crystal Si target, at thickness be on the metal substrate Cu paper tinsel of 12 μ m the pure Si film active material of deposition as negative electrode material layer, thereby form the negative pole of lithium rechargeable battery.Wherein, the temperature of Cu paper tinsel is 250 ℃, and two kinds of target as sputter power are all 1000W, and working gas Ar flow is 25sccm, impurity gas C
2H
2Flow be 1.0sccm, pressure is 0.55Pa in the sputtering chamber, total sputtering time is 2 hours.
Gained film cathode pole piece and metal Li composition half-cell are carried out electrochemical property test, and measuring current density is 0.8mA/cm
2, the charging/discharging voltage scope is at 0-1.0V, and discharge platform is about 0.2V, and charging platform is about 0.3V.Test result as shown in Figure 10 and Figure 11, wherein Figure 10 is the cycle performance curve, Figure 11 is the efficiency for charge-discharge curve, as we can see from the figure, the specific discharge capacity of cathode pole piece can reach 2209.3mAh/g, first charge-discharge efficiency is 93.4%, and capacity still remains on about 93.5% after 65 charge and discharge cycles.
Embodiment 7
Utilize magnetron sputtering technique, be target with Si-AI alloys target and C target respectively, at thickness be on the metal substrate Cu paper tinsel of 12 μ m the deposition laminated film as negative electrode material layer, wherein, the Si-AI alloy-layer is an active material layer, the C layer that covers on the Si-AI alloy active material layer is a resilient coating, thereby forms the negative pole of lithium rechargeable battery.Wherein, the temperature of Cu paper tinsel is 200 ℃, and two kinds of target as sputter power are all 1300W, and working gas Ar flow is 63sccm, and pressure is 3.6Pa in the sputtering chamber, and total sputtering time is 6.5 hours, and wherein, Si-AI alloys target sputtering time is 6 hours.
Gained film cathode pole piece and metal Li composition half-cell are carried out electrochemical property test, and measuring current density is 0.45mA/cm
2, the charging/discharging voltage scope is at 0-1.0V, and discharge platform is about 0.2V, and charging platform is about 0.4V.Test result such as Figure 12 and shown in Figure 13, wherein Figure 12 is the cycle performance curve, Figure 13 is the efficiency for charge-discharge curve, as we can see from the figure, the specific discharge capacity of cathode pole piece can reach 2786.5mAh/g, first charge-discharge efficiency is 87.5%, and capacity is not decayed after 50 charge and discharge cycles.
Embodiment 8-14
Utilize magnetron sputtering technique, be target with Si target, Al target and C target respectively, at thickness be on the metal substrate Cu paper tinsel of 12 μ m the deposition laminated film as negative electrode material layer, wherein, Si layer and Al layer are together as active material layer, the C layer that covers on the active material layer is a resilient coating, thereby forms the negative pole of lithium rechargeable battery.Wherein, the temperature of Cu paper tinsel is about 300 ℃, and working gas Ar flow is 50sccm, and pressure is 0.55Pa in the sputtering chamber, total sputtering time is 3.5 hours, wherein, Si target and Al target co-sputtered, sputtering time is 3 little right, under these conditions, the power that changes magnetron sputtering carries out electrochemical property test to gained film cathode pole piece and metal Li composition half-cell, at current density 0.9mA/cm from 2000W-5000W
2Under carry out charge and discharge cycles, the charging/discharging voltage scope is at 0-1.0V, the electrochemical property test result of each cathode pole piece as shown in Table 1.
Table 1:
From table, can see that the cathode pole piece for preparing has very high specific discharge capacity and first charge-discharge efficiency under the magnetron sputtering power of 2000W-5000W.
Claims (7)
1. an active cathode pole piece is characterized in that: cover a resilient coating again after covering an active material layer on the metal substrate, active material layer and the preparation of resilient coating employing magnetron sputtering technique.
2. active cathode pole piece according to claim 1 is characterized in that: described active layer is one of silicon and doped chemical hydrogen, carbon, aluminium, nickel, cobalt, copper.
3. active cathode pole piece according to claim 2 is characterized in that: described cushioning layer material is one of carbon and aluminium, boron, iron, copper, silver.
4. active cathode pole piece according to claim 3 is characterized in that: the thickness of described active material layer is 1-20 μ m.
5. active cathode pole piece preparation method, it is characterized in that: described method comprises the steps:
1) in magnetic control sputtering device, lays metal substrate and target;
2) sputtering power is selected 1000-5000W;
3) keep the metal substrate temperature between 100-300 ℃;
4) sputtering time 3-6.5 hour, wherein Si target sputtering time took 80-90%.
6. active cathode pole piece preparation method according to claim 5 is characterized in that: described target is Si-doped chemical hybrid target and C target.
7. active cathode pole piece preparation method according to claim 6 is characterized in that: described sputter work atmosphere is Ar, H
2Or C
2H
2Gas.
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| CN103050667A (en) * | 2012-12-13 | 2013-04-17 | 中南大学 | Composite anode of multi-layer structure for lithium-sulfur rechargeable battery and preparation method |
| CN104347842A (en) * | 2013-07-23 | 2015-02-11 | 华为技术有限公司 | Composite negative electrode sheet of lithium ion secondary battery, preparation method thereof, and lithium ion secondary battery |
| CN104347842B (en) * | 2013-07-23 | 2017-08-25 | 华为技术有限公司 | A kind of lithium rechargeable battery composite negative plate and preparation method thereof and lithium rechargeable battery |
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| CN108075105A (en) * | 2016-11-18 | 2018-05-25 | 中国科学院金属研究所 | A kind of preparation method of lithium ion battery silicon-based anode |
| CN110034278A (en) * | 2018-01-12 | 2019-07-19 | 中南大学 | A kind of SnS2Film lithium cell cathode and its preparation and application |
| CN111313002A (en) * | 2020-02-27 | 2020-06-19 | 桂林电子科技大学 | Composite negative electrode, and preparation method and application thereof |
| CN111313002B (en) * | 2020-02-27 | 2021-12-28 | 桂林电子科技大学 | Composite negative electrode, and preparation method and application thereof |
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Application publication date: 20110511 |