CN105895890A - Application of Sn3O4 solar catalyst in negative electrode material of lithium ion battery - Google Patents

Application of Sn3O4 solar catalyst in negative electrode material of lithium ion battery Download PDF

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CN105895890A
CN105895890A CN201610394431.XA CN201610394431A CN105895890A CN 105895890 A CN105895890 A CN 105895890A CN 201610394431 A CN201610394431 A CN 201610394431A CN 105895890 A CN105895890 A CN 105895890A
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solution
lithium ion
ion battery
powder
sn3o4
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黄英
陈雪芳
张开创
冯玄圣
李素萍
闫靖
张娜
王明月
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Northwestern Polytechnical University
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Northwestern Polytechnical University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/058—Construction or manufacture
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • 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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Abstract

The invention provides application of a Sn3O4 solar catalyst in a negative electrode material of a lithium ion battery. The application comprises the following steps of adding stannous chloride dihydrate to deionized water, sequentially adding trisodium citrate and a sodium hydroxide solution, heating the obtained solution, naturally cooling the obtained solution, washing a solid in the obtained product with the deionized water for several times, and drying and grinding the product after washing to obtain Sn3O4 powder; and preparing an electrode with the Sn3O4 powder by a tape casting method, and assembling the electrode to obtain a CR2016 battery. When the Sn3O4 material prepared according to the invention is applied to the negative electrode material of the lithium ion battery, convenient transmission of carriers in the charging and discharging processes is ensured by gaps between nanosheet layers, moreover, the volume change caused by charging and discharging is effectively relieved, considerable capacity and favorable cycle performance are shown, and the research field of the novel negative electrode material of the lithium ion battery is further developed.

Description

A kind of four oxidation three stannum solar energy catalyst application in lithium ion battery negative material
Technical field
The present invention relates to the application at lithium ion battery negative material of a kind of solar energy reforming catalyst.
Background technology
Tin-based material is considered to have extensively due to its high theoretical capacity, low cost, hypotoxicity, broad practicality The lithium ion battery negative material of general development prospect.
Document " " ACS Applied Materials Interfaces ", 2014,6:3790-3793 " discloses employing hydro-thermal method Four oxidation three stannum solar energy catalyst materials of synthesis, method is by SnCl2·2H2O and trisodium citrate are dissolved in deionization In water, adding NaOH solution after stirring 5 minutes, prepared homogeneous mixture solotion is put in water heating kettle, is placed on electric heating Being down to room temperature after 180 DEG C of heating 12h in stove, products therefrom is dried through filtration washing and ambient temperature in vacuum, is had There are four oxidation three stannum solar energy catalyst materials of flower-like structure.Research shows, under visible light illumination (λ > 400nm), Water is separated and shows significant photocatalysis performance by this material.The calculated results shows, the enhancing of reactivity is summed up In: under visible light, Sn2+And Sn4+Common existence can be that water decomposition provides a preferable band gap and band edge Position, Sn3O4The discovery of material promotes the research of visible ray sensitive catalyst.
But, current document has no Sn3O4Material is as the report of lithium ion battery negative material.
Summary of the invention
In order to overcome the deficiencies in the prior art, the present invention provides a kind of Sn that will be applied to solar energy reforming catalyst3O4 It is applied to the electrochemical research of lithium ion battery negative material.
The technical solution adopted for the present invention to solve the technical problems comprises the following steps:
(1) adding in deionized water by two hydrated stannous chlorides, stirring is to being completely dissolved；
(2) trisodium citrate is added in the solution of step (1) gained, trisodium citrate and two hydrated stannous chlorides Mol ratio be (2～3): 1, stirring to being completely dissolved, formed homogeneous solution；
(3) it is 0.2molL by molar concentration-1Sodium hydroxide solution add step (2) gained solution in, two water The mol ratio closing stannous chloride and sodium hydroxide more than 0 and is less than 5, keeps magnetic agitation 0.5-1h；
(4) solution of step (3) gained is warming up to 180 DEG C with the heating rate of 8-10 DEG C/min, reacts 10-12h After naturally cool to room temperature；
(5) solid in step (4) products therefrom is washed with deionized several times, the product after washing is put It is dried in 50-60 DEG C of vacuum drying oven to constant weight, grinds and obtain Sn3O4Powder；
(6) the tape casting is used to prepare electrode, by Sn3O4Powder, PVDF, conductive black and 1-methyl-2-pyrrolidine Ketone is mixed to form slurry, and the substrate of electrode film is metal copper foil；Wherein, Sn3O4Powder, PVDF, conductive black with The mass ratio of 1-Methyl-2-Pyrrolidone is 65:20:15:(410～820)；
(7) with lithium sheet for electrode, with polypropylene porous film as barrier film, it is the LiPF of 1mol/L by concentration6Carbonic acid Vinyl acetate solution and concentration are the LiPF of 1mol/L6Dimethyl carbonate solution equal-volume mix as electrolyte, at argon Compression ring border completes the assembling of CR2016 battery.
In described step (1), SnCl2·2H2O is 2:(270～290 with the mol ratio of deionized water).
In described step (6), when preparing single electrode, Sn3O4Powder, PVDF, conductive black gross mass are 0.5g, 1-Methyl-2-Pyrrolidone (NMP) volume is 2～4ml.
The invention has the beneficial effects as follows:
1. the present invention is successfully prepared with reference to the preparation methoies of four oxidation three stannum solar energy catalyst and is made up of nanometer sheet Sn3O4Material, when being applied to lithium ion battery negative material, the space between nanoscale twins not only ensure that in charge and discharge The convenient transmission of carrier in electric process, and effectively alleviate change in volume caused during discharge and recharge.
2. by prepared Sn3O4It is applied to lithium ion battery negative material, shows considerable capacity and good circulation Performance, has opened up the research field of new negative electrode materials for lithium secondary batteries further.
Accompanying drawing explanation
Fig. 1 is the method flow schematic diagram of the present invention
Fig. 2 is the product Sn in embodiment 13O4XRD figure spectrum；
Fig. 3 is product Sn in embodiment 23O4SEM figure, wherein, (a) is 500nm resolution, and (b) is 100nm Resolution；
Fig. 4 is product Sn in embodiment 33O4TEM figure, wherein, (a) is 500nm resolution, and (b) is 100nm Resolution；
Fig. 5 is the product Sn in each embodiment3O4In electric current density 60mAg-1(0-2.0V) the cycle performance figure under the conditions of.
Detailed description of the invention
The present invention is further described with embodiment below in conjunction with the accompanying drawings, and the present invention includes but are not limited to following embodiment.
The invention discloses and one four is aoxidized three stannum (Sn3O4) solar energy reforming catalyst be applied to lithium ion battery bear The technical scheme of pole material, this material shows the chemical property of excellence as lithium ion battery negative material.
The present invention includes the Sn being applied to solar energy reforming catalyst3O4Preparation and the assembling of CR2016 button cell, Specifically comprise the following steps that
(1) by 20mmol SnCl2·2H2O is dissolved in 50mL deionized water, stirs to being completely dissolved simultaneously；
(2) according to nTrisodium citrate: nTwo hydrated stannous chlorides=2-3, adds trisodium citrate in (1) solution, and stirring is to completely Dissolve, form homogeneous solution；
(3) according to nSodium hydroxide: nTwo hydrated stannous chlorides=1:(0-5), it is 0.2molL by the molar concentration of preparation-1Sodium hydroxide Solution adds (2) solution, and keeps magnetic agitation 0.5-1h；
(4) (3) solution of mix homogeneously is transferred to water heating kettle, be placed in resistance furnace, with the liter of 8-10 DEG C/min Temperature ramp, to 180 DEG C, naturally cools to room temperature after reaction 10-12h；
(5) solid in products therefrom is washed with deionized for several times, and the product after washing is placed in 50-60 DEG C of vacuum Drying baker is dried to constant weight, grinds and obtain Sn3O4Powder.
(6) using the tape casting to prepare electrode, by mass percentage=65%:20%:15%, by Sn3O4Powder, PVDF, Conductive black and a certain amount of 1-Methyl-2-Pyrrolidone (NMP) are mixed to form slurry, and the substrate of electrode film is metallic copper Paper tinsel.Wherein, Sn3O4Powder, PVDF, conductive black gross mass are 0.5g, 1-Methyl-2-Pyrrolidone (NMP) body Amass as 2-4ml.
(7) CR2016 button cell it is assembled into, with lithium sheet (Φ=16 purity > 99.9%) for electrode, with poly-third Alkene perforated membrane (Φ=18) is barrier film, with LiPF6Ethylene carbonate (EC) and dimethyl carbonate (DMC) (VEC:VDMC=1:1, concentration is 1mol/L) mixed solution as electrolyte, in the glove box of full argon Complete the assembling of CR2016 battery.
Embodiment 1
(1) by 20mmolSnCl2·2H2O is dissolved in 50mL deionized water, stirs to being completely dissolved simultaneously；
(2) according to nTrisodium citrate: nTwo hydrated stannous chlorides=2.5, trisodium citrate is added in (1) solution, stirring is to completely Dissolve, form homogeneous solution；
(3) according to nSodium hydroxide: nTwo hydrated stannous chlorides=1:1, is 0.2molL by the molar concentration of preparation-1Sodium hydroxide molten Liquid adds in (2) solution, and keeps magnetic agitation 0.5h；
(4) (3) solution by mix homogeneously transfers to the water heating kettle of 200ml politef, with the intensification of 10 DEG C/min Ramp is to 180 DEG C, and naturally cools to room temperature after 180 DEG C of reaction 12h；
(5) solid in products therefrom is washed with deionized for several times, and is dried 12h in 60 DEG C of vacuum drying ovens, Grinding obtains Sn3O4Powder.
(6) using the tape casting to prepare electrode, by mass percentage=65%:20%:15%, by Sn3O4Powder, PVDF, Conductive black and a certain amount of 1-Methyl-2-Pyrrolidone (NMP) are mixed to form slurry, and the substrate of electrode film is metallic copper Paper tinsel.Wherein, Sn3O4Powder, PVDF, conductive black gross mass are 0.5g, 1-Methyl-2-Pyrrolidone (NMP) body Amass as 2-4ml.
(7) CR2016 button cell it is assembled into, with lithium sheet (Φ=16 purity > 99.9%) for electrode, with poly-third Alkene perforated membrane (Φ=18) is barrier film, with LiPF6Ethylene carbonate (EC) and dimethyl carbonate (DMC) (VEC:VDMC=1:1) mixed solution as electrolyte, the glove box of full argon completes CR2016 battery Assemble.
The XRD figure of product is as shown in Figure 2.As shown in Figure 2, the position at the XRD peak of product and intensity are all and anorthic system The Sn of crystal structure3O4(PDF 16 0737) is consistent.There is no other impurity peaks, show to be successfully prepared Sn3O4。
In electric current density 60mAg-1Under the conditions of, the CR2016 button cell assembling the product in embodiment carries out charge and discharge Electric performance test, charging/discharging voltage scope is 0-2.0V.Cycle performance is as shown in Figure 5.As seen from the figure, product is first Discharge capacity can reach 1156mAhg-1, initial charge capacity 977mAhg-1, after 50 circulations, discharge capacity is protected Hold 471.2mAhg-1Left and right.
Embodiment 2
(1) by 20mmolSnCl2·2H2O is dissolved in 50mL deionized water, stirs to being completely dissolved simultaneously；
(2) according to nTrisodium citrate: nTwo hydrated stannous chlorides=2.5, trisodium citrate is added in (1) solution, stirring is to completely Dissolve, form homogeneous solution；
(3) according to nSodium hydroxide: nTwo hydrated stannous chlorides=1:2, is 0.2molL by the molar concentration of preparation-1Sodium hydroxide molten Liquid adds in (2) solution, and keeps magnetic agitation 0.5h；
(4) (3) solution by mix homogeneously transfers to the water heating kettle of 200ml politef, with the intensification of 10 DEG C/min Ramp is to 180 DEG C, and naturally cools to room temperature after 180 DEG C of reaction 12h；
(5) solid in products therefrom is washed with deionized for several times, and is dried 12h in 60 DEG C of vacuum drying ovens, Grinding obtains Sn3O4Powder.
(6) using the tape casting to prepare electrode, by mass percentage=65%:20%:15%, by Sn3O4Powder, PVDF, Conductive black and a certain amount of 1-Methyl-2-Pyrrolidone (NMP) are mixed to form slurry, and the substrate of electrode film is metallic copper Paper tinsel.Wherein, Sn3O4Powder, PVDF, conductive black gross mass are 0.5g, 1-Methyl-2-Pyrrolidone (NMP) body Amass as 2-4ml.
(7) CR2016 button cell it is assembled into, with lithium sheet (Φ=16 purity > 99.9%) for electrode, with poly-third Alkene perforated membrane (Φ=18) is barrier film, with LiPF6Ethylene carbonate (EC) and dimethyl carbonate (DMC) (VEC:VDMC=1:1) mixed solution as electrolyte, the glove box of full argon completes CR2016 battery Assemble.
The SEM of product schemes as shown in Figure 3.From the figure 3, it may be seen that product has the flower-shaped knot of obvious nanometer sheet composition Structure, and there is between nanoscale twins certain space, on the one hand can provide effective passage for the transmission of lithium ion, Make electrolyte be easier in entrance electrode material to be electrochemically reacted；On the other hand, the existence energy padded coaming in space Bulk effect in charge and discharge process.
In electric current density 60mAg-1Under the conditions of, the CR2016 button cell assembling the product in embodiment carries out charge and discharge Electric performance test, charging/discharging voltage scope is 0-2.0V.Cycle performance is as shown in Figure 5.As seen from the figure, product is first Discharge capacity can reach 1256mAhg-1, initial charge capacity 1083.1mAhg-1, discharge capacity after 50 circulations Keep 505.2mAhg-1Left and right.
Embodiment 3
(1) by 20mmolSnCl2·2H2O is dissolved in 50mL deionized water, stirs to being completely dissolved simultaneously；
(2) according to nTrisodium citrate: nTwo hydrated stannous chlorides=2.5, trisodium citrate is added in (1) solution, stirring is to completely Dissolve, form homogeneous solution；
(3) according to nSodium hydroxide: nTwo hydrated stannous chlorides=1:3, is 0.2molL by the molar concentration of preparation-1Sodium hydroxide molten Liquid adds in (2) solution, and keeps magnetic agitation 0.5h；
(4) (3) solution by mix homogeneously transfers to the water heating kettle of 200ml politef, with the intensification of 10 DEG C/min Ramp is to 180 DEG C, and naturally cools to room temperature after 180 DEG C of reaction 12h；
(5) solid in products therefrom is washed with deionized for several times, and is dried 12h in 60 DEG C of vacuum drying ovens, Grinding obtains Sn3O4Powder.
(6) using the tape casting to prepare electrode, by mass percentage=65%:20%:15%, by Sn3O4Powder, PVDF, Conductive black and a certain amount of 1-Methyl-2-Pyrrolidone (NMP) are mixed to form slurry, and the substrate of electrode film is metallic copper Paper tinsel.Wherein, Sn3O4Powder, PVDF, conductive black gross mass are 0.5g, 1-Methyl-2-Pyrrolidone (NMP) body Amass as 2-4ml.
(7) CR2016 button cell it is assembled into, with lithium sheet (Φ=16 purity > 99.9%) for electrode, with poly-third Alkene perforated membrane (Φ=18) is barrier film, with LiPF6Ethylene carbonate (EC) and dimethyl carbonate (DMC) (VEC:VDMC=1:1) mixed solution as electrolyte, the glove box of full argon completes CR2016 battery Assemble.
The TEM of product schemes as shown in Figure 4.As shown in Figure 4, product has and is significantly made up of two-dimensional nano sheet Flower-like structure, the thickness of nanometer sheet can carry for the transmission of lithium ion in the existence of 20-30nm. two-dimensional nano laminated structure Supply effective passage, simultaneously to a certain extent can padded coaming bulk effect in charge and discharge process.
In electric current density 60mAg-1Under the conditions of, the CR2016 button cell assembling the product in embodiment carries out charge and discharge Electric performance test, charging/discharging voltage scope is 0-2.0V.Cycle performance is as shown in Figure 5.As seen from the figure, product is first Discharge capacity can reach 1546.9mAhg-1, initial charge capacity 902mAhg-1, after 50 circulations, discharge capacity is protected Hold 469mAhg-1Left and right.

Claims (3)

1. an oxidation three stannum solar energy catalyst application in lithium ion battery negative material, it is characterised in that include Following step:
(1) adding in deionized water by two hydrated stannous chlorides, stirring is to being completely dissolved；
(2) trisodium citrate is added in the solution of step (1) gained, trisodium citrate and two hydrated stannous chlorides Mol ratio be (2～3): 1, stirring to being completely dissolved, formed homogeneous solution；
(3) it is 0.2molL by molar concentration-1Sodium hydroxide solution add step (2) gained solution in, two water The mol ratio closing stannous chloride and sodium hydroxide more than 0 and is less than 5, keeps magnetic agitation 0.5-1h；
(4) solution of step (3) gained is warming up to 180 DEG C with the heating rate of 8-10 DEG C/min, reacts 10-12h After naturally cool to room temperature；
(5) solid in step (4) products therefrom is washed with deionized several times, the product after washing is put It is dried in 50-60 DEG C of vacuum drying oven to constant weight, grinds and obtain Sn3O4Powder；
(6) the tape casting is used to prepare electrode, by Sn3O4Powder, PVDF, conductive black and 1-methyl-2-pyrrolidine Ketone is mixed to form slurry, and the substrate of electrode film is metal copper foil；Wherein, Sn3O4Powder, PVDF, conductive black with The mass ratio of 1-Methyl-2-Pyrrolidone is 65:20:15:(410～820)；
(7) with lithium sheet for electrode, with polypropylene porous film as barrier film, it is the LiPF of 1mol/L by concentration6Carbonic acid Vinyl acetate solution and concentration are the LiPF of 1mol/L6Dimethyl carbonate solution equal-volume mix as electrolyte, at argon Compression ring border completes the assembling of CR2016 battery.
Four oxidation three stannum solar energy catalyst application in lithium ion battery negative material the most according to claim 1, It is characterized in that: in described step (1), SnCl2·2H2O is 2:(270～290 with the mol ratio of deionized water).
Four oxidation three stannum solar energy catalyst application in lithium ion battery negative material the most according to claim 1, It is characterized in that: in described step (6), when preparing single electrode, Sn3O4Powder, PVDF, conduction charcoal Black gross mass is 0.5g, and 1-Methyl-2-Pyrrolidone (NMP) volume is 2～4ml.
CN201610394431.XA 2016-06-06 2016-06-06 Application of Sn3O4 solar catalyst in negative electrode material of lithium ion battery Pending CN105895890A (en)

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CN110530941A (en) * 2019-07-17 2019-12-03 济南大学 A kind of Cu doping Sn3O4Gas sensitive and its formaldehyde gas sensor and preparation method, application
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CN107317007A (en) * 2017-06-23 2017-11-03 西北工业大学 Lithium ion battery aoxidizes the preparation method of three tin negative pole materials with titanium dioxide/tetra-
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CN109682865A (en) * 2019-01-07 2019-04-26 北京工业大学 A kind of autoreduction preparation method of the stannic oxide nanometer flower gas sensitive of load gold nano grain
CN110530941A (en) * 2019-07-17 2019-12-03 济南大学 A kind of Cu doping Sn3O4Gas sensitive and its formaldehyde gas sensor and preparation method, application
CN110530941B (en) * 2019-07-17 2022-01-14 济南大学 Cu doped Sn3O4Gas sensitive material, formaldehyde gas sensor, preparation method and application thereof
CN110935437A (en) * 2019-12-18 2020-03-31 兰州大学 Synthetic method of Z-type tri-tin tetroxide/bismuth vanadate quantum dot composite photocatalyst capable of fully hydrolyzing water

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