CN112573508A - Preparation method, product and application of graphene-coated core-shell stannous oxide @ tin oxide material - Google Patents
Preparation method, product and application of graphene-coated core-shell stannous oxide @ tin oxide material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 41
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 37
- 239000011258 core-shell material Substances 0.000 title claims abstract description 31
- 229910001887 tin oxide Inorganic materials 0.000 title claims abstract description 30
- QHGNHLZPVBIIPX-UHFFFAOYSA-N tin(II) oxide Inorganic materials [Sn]=O QHGNHLZPVBIIPX-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000000047 product Substances 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 16
- 239000000725 suspension Substances 0.000 claims abstract description 16
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000012467 final product Substances 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical class [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims abstract description 5
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 6
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 4
- 239000008103 glucose Substances 0.000 claims description 4
- 229910052744 lithium Inorganic materials 0.000 claims description 4
- 239000007773 negative electrode material Substances 0.000 claims description 4
- 229960005070 ascorbic acid Drugs 0.000 claims description 3
- 235000010323 ascorbic acid Nutrition 0.000 claims description 3
- 239000011668 ascorbic acid Substances 0.000 claims description 3
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 3
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 14
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 14
- 238000000034 method Methods 0.000 abstract description 8
- 239000003792 electrolyte Substances 0.000 abstract description 6
- 230000002238 attenuated effect Effects 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000007086 side reaction Methods 0.000 abstract description 3
- 238000003760 magnetic stirring Methods 0.000 abstract 1
- 238000010586 diagram Methods 0.000 description 6
- 239000010406 cathode material Substances 0.000 description 3
- CQMNNMLVXSWLCH-UHFFFAOYSA-B 2-hydroxypropane-1,2,3-tricarboxylate;tin(4+) Chemical compound [Sn+4].[Sn+4].[Sn+4].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O CQMNNMLVXSWLCH-UHFFFAOYSA-B 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- YJGJRYWNNHUESM-UHFFFAOYSA-J triacetyloxystannyl acetate Chemical compound [Sn+4].CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O YJGJRYWNNHUESM-UHFFFAOYSA-J 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
- C01G19/02—Oxides
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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
- 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
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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
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- 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
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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- 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
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Abstract
The invention provides a preparation method of a graphene-coated core-shell stannous oxide @ tin oxide material, and a product and application thereof, wherein graphene oxide and soluble tin salt are dissolved in deionized water, strong base is added into the solution, and the solution is stirred by magnetic force; adding a weak reducing agent into the suspension, and carrying out magnetic stirring, centrifuging and washing to obtain a product; dispersing the product in hydrogen peroxide, magnetically stirring, centrifuging and drying to obtain the final product. The structure has larger specific surface area and better conductivity, can prevent the electrolyte from corroding the material to generate side reaction, and further can improve the electrochemical performance of the material. Under the condition of 1C multiplying power, the first discharge specific capacity is about 223 mAh/g; after 50 times of circulation, the discharge specific capacity is 180 mAh/g. The problem that the specific capacity is attenuated relatively quickly and the electrochemical performance is relatively poor in the cycle process of the lithium ion battery is solved. And the preparation method is simple, the process conditions are easy to realize, the energy consumption is low, and the preparation is pollution-free.
Description
Technical Field
The invention relates to the technical field of lithium ion battery cathode materials, in particular to a preparation method of a graphene-coated core-shell stannous oxide @ tin oxide material, and a product and application thereof.
Background
With the development of society, lithium ion batteries are receiving much attention. The lithium ion battery is the most ideal rechargeable battery in the world at present, and has the advantages of high energy density, long cycle life, no memory effect, small pollution and the like. With the progress of technology, lithium ion batteries are widely applied to the fields of electric automobiles, aerospace, biomedicine and the like, so that the research and development of lithium ion batteries for power and related materials have great significance. For power lithium ion batteries, the key is to increase the power density and energy density, and the improvement of the power density and energy density is fundamentally the improvement of electrode materials, particularly negative electrode materials.
Since the early 90 s of the last century, the japanese scientists developed carbon materials with layered structures, which were the first materials studied by people and applied to the commercialization of lithium ion batteries, and still remain one of the major points of attention and research, but carbon negative electrode materials have some defects: when the battery is formed, the electrolyte reacts with the electrolyte to form an SEI film, so that the electrolyte is consumed and the first coulombic efficiency is low; when the battery is overcharged, metal lithium may be precipitated on the surface of the carbon electrode to form lithium dendrite to cause short circuit, so that the temperature is increased and the battery explodes; in addition, the diffusion coefficient of lithium ions in the carbon material is small, so that the battery cannot realize large-current charging and discharging, and the application range of the lithium ion battery is limited.
The graphene-coated core-shell stannous oxide @ tin oxide material is used as a lithium ion battery cathode material, and has high Li + storage capacity through the coating and core-shell structure of graphene. The material is considered to be a promising lithium ion battery cathode material.
The invention provides a preparation method of a graphene-coated core-shell stannous oxide @ tin oxide material, wherein the graphene can improve the conductivity of the material, and the core-shell stannous oxide @ tin oxide material has larger specific surface area and conductivity, and is further favorable for improving the electrochemical performance of the material. The preparation process is relatively simple and easy to operate.
The invention provides a preparation method of a graphene-coated core-shell stannous oxide @ tin oxide material. The structure has larger specific surface area and better conductivity, can prevent the electrolyte from corroding the material to generate side reaction, and further can improve the electrochemical performance of the material. The problem that the specific capacity is attenuated relatively quickly and the electrochemical performance is relatively poor in the cycle process of the lithium ion battery is solved. And the preparation method is simple, the process conditions are easy to realize, the energy consumption is low, and the preparation is pollution-free.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method of a graphene-coated core-shell stannous oxide @ tin oxide material.
Yet another object of the present invention is to: the graphene-coated core-shell stannous oxide @ tin oxide material product prepared by the method is provided.
Yet another object of the present invention is to: applications of the above products are provided.
The invention aims to realize the following scheme, and the preparation method of the graphene-coated core-shell stannous oxide @ tin oxide material is characterized by comprising the following steps of,
the first step is as follows: dissolving 40 mg of graphene oxide and 2 mmol of soluble tin salt in 100 mL of deionized water, and ultrasonically dispersing for 30-60 min to mark as suspension A;
the second step is that: adding 4-6M strong base into the solution A, and magnetically stirring until the solution A is uniform for 10-30 min, wherein the solution A is marked as suspension B;
the third step: adding 1 g of weak reducing agent into the suspension, magnetically stirring for 30-60 min, centrifuging, and washing with deionized water and ethanol for several times to obtain a product C;
the fourth step: and dispersing the product C in 100 mL of hydrogen peroxide with the mass fraction of 15%, magnetically stirring for 6-10 h, centrifuging, and drying at 60-80 ℃ for 0.5-2 h to obtain a final product.
The tin salt is one or the combination of tin chloride, tin acetate or tin citrate.
The strong base is one or the combination of potassium hydroxide or sodium hydroxide.
The weak reducing agent is one or the combination of glucose or ascorbic acid.
The invention provides a graphene-coated core-shell stannous oxide @ tin oxide material which is prepared according to any one of the methods.
The invention provides an application of a graphene-coated core-shell stannous oxide @ tin oxide material in preparation of a lithium battery negative electrode material.
The invention provides a preparation method of a graphene-coated core-shell stannous oxide @ tin oxide material. The structure has larger specific surface area and better conductivity, can prevent the electrolyte from corroding the material to generate side reaction, and further can improve the electrochemical performance of the material. Under the condition of 1C multiplying power, the first discharge specific capacity is about 223 mAh/g; after 50 times of circulation, the discharge specific capacity is 180 mAh/g. The problem that the specific capacity is attenuated relatively quickly and the electrochemical performance is relatively poor in the cycle process of the lithium ion battery is solved. And the preparation method is simple, the process conditions are easy to realize, the energy consumption is low, and the preparation is pollution-free.
Drawings
FIG. 1 is a cycle performance diagram of the graphene-coated core-shell stannous oxide @ tin oxide material of example 1;
FIG. 2 is a cycle performance diagram of the graphene-coated core-shell stannous oxide @ tin oxide material of example 2;
fig. 3 is a cycle performance diagram of the graphene-coated core-shell stannous oxide @ tin oxide material of example 3.
Detailed Description
The present invention is described in detail by the following specific examples, but the scope of the present invention is not limited to these examples.
Example 1
A graphene-coated core-shell stannous oxide @ tin oxide material is prepared by the following steps:
the first step is as follows: dissolving 40 mg of graphene oxide and 2 mmol of stannic chloride in 100 mL of deionized water, and ultrasonically dispersing for 30min to mark as suspension A;
the second step is that: adding 6M strong base sodium hydroxide into the solution A, magnetically stirring for 10 min to obtain suspension B;
the third step: adding 1 g of glucose serving as a weak reducing agent into the suspension B, magnetically stirring for 30min, centrifuging, and washing with deionized water and ethanol for several times to obtain a product C;
the fourth step: and dispersing the product C in 100 mL of hydrogen peroxide with the mass fraction of 15%, magnetically stirring for 6 h, centrifuging, and drying at 80 ℃ for 0.5 h to obtain a final product graphene coated core-shell stannous oxide @ tin oxide material.
Fig. 1 is a cycle performance diagram of a graphene-coated core-shell stannous oxide @ tin oxide material. Under the condition of 1C multiplying power, the first discharge specific capacity is about 217 mAh/g; after 50 times of circulation, the discharge specific capacity is 178 mAh/g.
Example 2
The graphene-coated core-shell stannous oxide @ tin oxide material is prepared by the following steps, similar to the steps in example 1:
the first step is as follows: dissolving 40 mg of graphene oxide and 2 mmol of soluble tin acetate in 100 mL of deionized water, and ultrasonically dispersing for 30min to mark as suspension A;
the second step is that: adding 6M potassium hydroxide into the solution A, magnetically stirring the solution A until the solution A is uniform for 10 min, and marking the solution A as suspension B;
the third step: adding 1 g of ascorbic acid into the suspension, magnetically stirring for 60 min, centrifuging, and washing with deionized water and ethanol for several times to obtain a product C;
the fourth step: dispersing the product C in 100 mL of hydrogen peroxide with the mass fraction of 15%, magnetically stirring for 10 h, then centrifuging and drying at 60 ℃ for 1 h to obtain the final product.
Fig. 2 is a cycle performance diagram of the graphene-coated core-shell stannous oxide @ tin oxide material. Under the condition of 1C multiplying power, the first discharge specific capacity is about 215 mAh/g; after 50 times of circulation, the specific discharge capacity is 171 mAh/g.
Example 3
The graphene-coated core-shell stannous oxide @ tin oxide material is prepared by the following steps, similar to the steps in example 1:
the first step is as follows: dissolving 40 mg of graphene oxide and 2 mmol of soluble tin citrate in 100 mL of deionized water, and ultrasonically dispersing for 30min to mark as suspension A;
the second step is that: adding 6M potassium hydroxide into the solution A, magnetically stirring the solution A until the solution A is uniform for 30min, and marking the solution A as suspension B;
the third step: adding 1 g of glucose into the suspension, magnetically stirring for 30min, centrifuging, and washing with deionized water and ethanol for several times to obtain a product C;
the fourth step: dispersing the product C in 100 mL of hydrogen peroxide with the mass fraction of 15%, magnetically stirring for 10 h, then centrifuging and drying at 60 ℃ for 1 h to obtain the final product.
Fig. 3 is a cycle performance diagram of the graphene coated core-shell stannous oxide @ tin oxide material. Under the condition of 1C multiplying power, the first discharge specific capacity is about 223 mAh/g; after 50 times of circulation, the discharge specific capacity is 180 mAh/g.
Claims (6)
1. A preparation method of a graphene-coated core-shell stannous oxide @ tin oxide material is characterized by comprising the following steps of,
the first step is as follows: dissolving 40 mg of graphene oxide and 2 mmol of soluble tin salt in 100 mL of deionized water, and ultrasonically dispersing for 30-60 min to mark as suspension A;
the second step is that: adding 4-6M strong base into the solution A, and magnetically stirring until the solution A is uniform for 10-30 min, wherein the solution A is marked as suspension B;
the third step: adding 1 g of weak reducing agent into the suspension B, magnetically stirring for 30-60 min, centrifuging, and washing with deionized water and ethanol for several times to obtain a product C;
the fourth step: and dispersing the product C in 100 mL of hydrogen peroxide with the mass fraction of 15%, magnetically stirring for 6-10 h, centrifuging, and drying at 60-80 ℃ for 0.5-2 h to obtain a final product.
2. The preparation method of the graphene-coated core-shell stannous oxide @ tin oxide material as claimed in claim 1, wherein in the first step, the tin salt is one or a combination of stannic chloride, stannic acetate and stannic citrate.
3. The preparation method of the graphene coated core-shell stannous oxide @ tin oxide material as claimed in claim 1, wherein in the second step, the strong base is one or a combination of potassium hydroxide and sodium hydroxide.
4. The preparation method of the graphene-coated core-shell stannous oxide @ tin oxide material as claimed in claim 1, wherein in the third step, the weak reducing agent is one or a combination of glucose and ascorbic acid.
5. A graphene-coated core-shell stannous oxide @ tin oxide material, characterized by being prepared according to any one of claims 1-4.
6. The application of the graphene-coated core-shell stannous oxide @ tin oxide material in the preparation of a lithium battery negative electrode material according to claim 5.
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