Nothing Special   »   [go: up one dir, main page]

CN108417780A - A kind of preparation and its application of anode material of lithium-ion battery stainless (steel) wire load carbon covered stannum rice structure - Google Patents

A kind of preparation and its application of anode material of lithium-ion battery stainless (steel) wire load carbon covered stannum rice structure Download PDF

Info

Publication number
CN108417780A
CN108417780A CN201810128510.5A CN201810128510A CN108417780A CN 108417780 A CN108417780 A CN 108417780A CN 201810128510 A CN201810128510 A CN 201810128510A CN 108417780 A CN108417780 A CN 108417780A
Authority
CN
China
Prior art keywords
steel
stainless
wire
solution
tin oxide
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201810128510.5A
Other languages
Chinese (zh)
Inventor
锁国权
李丹
杨艳玲
侯小江
冯雷
毕雅欣
王祎
占胜
左玉
李妍欣
陈进耿
石小燕
朱建锋
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shaanxi University of Science and Technology
Original Assignee
Shaanxi University of Science and Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shaanxi University of Science and Technology filed Critical Shaanxi University of Science and Technology
Priority to CN201810128510.5A priority Critical patent/CN108417780A/en
Publication of CN108417780A publication Critical patent/CN108417780A/en
Pending legal-status Critical Current

Links

Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/13Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139Processes of manufacture
    • H01M4/1391Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/054Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/04Processes of manufacture in general
    • H01M4/0471Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/04Processes of manufacture in general
    • H01M4/049Manufacturing of an active layer by chemical means
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/362Composites
    • H01M4/366Composites as layered products
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/483Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/62Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/62Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624Electric conductive fillers
    • H01M4/625Carbon or graphite
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Nanotechnology (AREA)
  • Materials Engineering (AREA)
  • Composite Materials (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Inorganic Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

A kind of preparation and its application of anode material of lithium-ion battery stainless (steel) wire load carbon covered stannum rice structure, sodium hydroxide is dissolved in deionized water and obtains solution A;Stannic chloride is added into solution A and obtains solution B;Ammonium fluoride is added into solution B and obtains solution or emulsion C;Solution C is transferred to hydrothermal reaction kettle, the clean stainless (steel) wire of pre-wash is placed in solution C and carries out hydro-thermal reaction, is cooled down after reaction, dry stainless (steel) wire carrying tin oxide nanostructure under certain temperature;Stainless (steel) wire carrying tin oxide nanostructure is placed in organic solution, stainless (steel) wire load Coated with Organic Matter tin oxide nano structure is reacted to obtain;Stainless (steel) wire load Coated with Organic Matter tin oxide nano structure is placed in tube furnace and reacts to obtain stainless (steel) wire load carbon coating tin oxide nano structure;The present invention improves discharge and recharge, high rate performance and the cycle performance of sodium-ion battery.

Description

A kind of anode material of lithium-ion battery stainless (steel) wire load carbon covered stannum rice structure It prepares and its applies
Technical field
The present invention relates to secondary power battery material technical field, more particularly to a kind of anode material of lithium-ion battery is stainless Steel mesh loads the preparation and its application of carbon covered stannum rice structure.
Background technology
Oil, natural gas and coal are not the inexhaustible energy, and the gas of combustion of fossil fuel discharge Serious Global Environmental Problems can be brought.In addition, national security can be threatened by relying on non-renewable resources import for a long time.Therefore generation New, clean, green fungible energy source and energy conversion and storage system are all being found by Jie Ge states.Wherein chemical-electrical Source is one of most important research direction, lithium ion battery be exactly grow up along with metal secondary batteries it is a kind of novel Electrochmical power source.But content is few during elemental lithium is expensive and the earth's crust, with increasing for lithium ion battery applications, the demand of lithium Also it greatly increases.Therefore it needs to develop other power alkali metal-ion batteries.
Sodium element is located in the periodic table of elements immediately below elemental lithium, has similar physicochemical properties, and sodium with lithium It is the 6th abundant element of reserves in the earth's crust, it is widely distributed, therefore develop the sodium-ion battery technology tool of extensive stored energy application There is important strategic importance.The raw material of sodium-ion battery is extensive, cheap, has become the heat of novel battery energy storage technology at present Point.Sodium ion radius (0.98) is more than lithium ion radius (0.69) so that overcomes needed for sodium ion diffusion in charge and discharge process Potential barrier bigger, to make diffusion rate substantially reduce, therefore need to find suitable battery cathode storage sodium material.Currently, The sodium ion negative material of research mainly has carbon material, conversion class material etc..It is oxide material mostly to convert class material, is not had Its corresponding metallic conductivity is high, while volume occurs for the insertion with abjection of sodium ion in single carbon-coated nano structural material Expansion ratio oxide is small.Therefore sodium-ion battery first charge-discharge amount, cyclical stability and conductivity are improved.
Stainless (steel) wire loads carbon covered stannum rice structure as a kind of novel sodium-ion battery negative electrode active material, prepares Method and correlative study work yet there are no report.
Invention content
In order to overcome the above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of anode material of lithium-ion batteries Stainless (steel) wire loads the preparation and its application of carbon covered stannum rice structure, invention enhances the electric conductivity of sodium-ion battery, Modulation slurry is eliminated simultaneously and applies blade technolgy, avoids the performance that battery is influenced using binder.
To achieve the goals above, the technical solution adopted by the present invention is:
A kind of preparation of anode material of lithium-ion battery stainless (steel) wire load carbon covered stannum rice structure, including following step Suddenly:
Step 1:
0.625g~1.808g sodium hydroxides will be proportionally dissolved in 40mL deionized waters and obtain solution A;
Step 2:
Under magnetic stirring, stannic chloride is added into above-mentioned solution A and obtains solution B, the mass ratio of sodium hydroxide and stannic chloride It is 2:1~4:1;
Step 3:
Under magnetic stirring, ammonium fluoride is added into above-mentioned solution B and obtains solution or emulsion C, sodium hydroxide and ammonium fluoride Mass ratio be 12:1~36:1;
Step 4:
Above-mentioned solution C is transferred to hydrothermal reaction kettle, the clean stainless (steel) wire of pre-wash is placed in solution C, is carried out Hydro-thermal reaction cools down after reaction, and stainless (steel) wire is cleaned with deionized water and ethyl alcohol, dry under certain temperature, obtains stainless steel Net carrying tin oxide nanostructure;
Step 5:
Above-mentioned stainless (steel) wire carrying tin oxide nanostructure is placed in organic solution, reacts a timing at a certain temperature Between, obtain stainless (steel) wire load Coated with Organic Matter tin oxide nano structure;
Step 6:
Above-mentioned stainless (steel) wire load Coated with Organic Matter tin oxide nano structure is placed in tube furnace, is roasted at a certain temperature Certain time is burnt, calcination atmosphere is argon gas, obtains stainless (steel) wire load carbon coating tin oxide nano structure;
Step 7:
Above-mentioned carbon stainless steel net load carbon coating tin oxide nano structure is placed in tube furnace, in reducing gas hydrogen It is made annealing treatment under atmosphere and predetermined temperature and just obtains final product stainless (steel) wire load carbon covered stannum rice structure after a certain period of time.
In the step 4, hydrothermal temperature be 160~200 DEG C, the reaction time be 0.5~for 24 hours.
In the step 5, organic carbon source is glucose, dopamine and beta-cyclodextrin etc., and reaction temperature is 160 DEG C~200 DEG C, 4 hours.
In the step 6, annealing temperature is 600 DEG C~750 DEG C, and annealing time is 1~4h, the flow velocity of argon gas is 10~ 100sccm。
In the step 7, annealing temperature is 600~750 DEG C, and annealing time is 1~4h, the flow velocity of hydrogen is 300~ 400sccm。
A kind of application of anode material of lithium-ion battery stainless (steel) wire load carbon covered stannum rice structure, stainless (steel) wire is born It carries carbon covered stannum rice structural material and is washed into a diameter of 8mm disks as active material electrode, sodium is used as to electrode, and electrolyte is (volume ratio of EC and DMC are 1 for the ethylene carbonate (EC) of 1M sodium hexafluoro phosphates and the solution of carbonic acid dioctyl phthalate (DMC):1), gather Propylene microcellular film is battery diaphragm, is assembled into button cell;After assembled button cell is stood 12 hours, LANDCT2100A carries out electrochemical property test.Test voltage is 0.01V~2.6V, current density 50mA/g.
Beneficial effects of the present invention:
Invention enhances the electric conductivities of sodium-ion battery, while eliminating modulation slurry and applying blade technolgy, avoid making The performance of battery is influenced with binder.By controlling the proportioning of reaction dissolvent, sintering temperature and soaking time improve the present invention The size of substance, pattern and structure.The specific surface area of stainless (steel) wire load carbon coating tin oxide nano structure prepared by the present invention Greatly, very large space stores sodium ion in charge and discharge process, carbon-coated rock-steady structure to be not easy in charge and discharge process It caves in.Surfactant NH is used in the present invention4F can obtain the carbon-coated nano structure of size uniformity on stainless (steel) wire Array stannic oxide.
Description of the drawings
Fig. 1 stainless (steel) wires load carbon covered stannum rice structure preparation process schematic diagram.
Specific implementation mode
Invention is further described in detail below in conjunction with the accompanying drawings.
Embodiment 1
A kind of preparation method of stainless (steel) wire load carbon covered stannum rice structure, includes the following steps:
1) sodium hydroxide that quality is 0.625g, under magnetic stirring, is dissolved in 40ml deionized waters and obtains solution A;
2) 0.47g stannic chlorides, under magnetic stirring, are added into above-mentioned solution A and obtain solution B;
3) 0.05g ammonium fluorides, under magnetic stirring, are added into B solution and obtain solution or emulsion C;
4), solution C is transferred in stainless steel cauldron, while the clean stainless (steel) wire of pre-wash is placed in solution In, hydro-thermal reaction is carried out, stainless (steel) wire is cleaned with deionized water and ethyl alcohol, after being reacted 24 hours at a temperature of 200 DEG C, just obtained Stainless (steel) wire carrying tin oxide nanostructure;
5), 4) the stainless (steel) wire tin supported nanostructure obtained in is placed in 3.6g glucose 40mL deionized waters, 180 The glucose cladding tin oxide nano structure of stainless (steel) wire load is obtained after being impregnated 4 hours in DEG C;
6), 3) the stainless (steel) wire load organic carbon source cladding tin oxide nano structure obtained in is placed in tube furnace, Just final product stainless (steel) wire load carbon coating oxidation sijna is obtained after being made annealing treatment 2 hours at a temperature of 700 DEG C in argon gas atmosphere Rice structure;
7), 4) the stainless (steel) wire load carbon coating tin oxide nano structure obtained in is placed in tube furnace, in hydrogen gas 650 DEG C of temperatures just obtain final product stainless (steel) wire load carbon covered stannum rice structure in atmosphere after 1 hour;
8), the assembling of button cell, using stainless (steel) wire load carbon covered stannum rice structure be washed into a diameter of 8mm disks as Active material electrode, sodium are used as to electrode, and electrolyte is the ethylene carbonate (EC) and carbonic acid dioctyl phthalate of 1M sodium hexafluoro phosphates (DMC) (volume ratio of EC and DMC are 1 to solution:1), microporous polypropylene membrane is battery diaphragm, is assembled into button cell;
9) after, assembled button cell stands 24 hours, electrochemical property test is carried out in LANDCT2100A.Test Voltage is 0.01V~2.6V, current density 50mA/g.
Embodiment 2
A kind of preparation method of stainless (steel) wire load carbon covered stannum rice structure, includes the following steps:
1) sodium hydroxide that quality is 0.9375g, under magnetic stirring, is dissolved in 40ml deionized waters and obtains solution A;
2) 0.47g stannic chlorides, under magnetic stirring, are added into above-mentioned solution A and obtain solution B;
3) 0.05g ammonium fluorides, under magnetic stirring, are added into B solution and obtain solution or emulsion C;
4), solution C is transferred in stainless steel cauldron, while the clean stainless (steel) wire of pre-wash is placed in solution In, hydro-thermal reaction is carried out, stainless (steel) wire is cleaned with deionized water and ethyl alcohol, after being reacted 24 hours at a temperature of 200 DEG C, just obtained Stainless (steel) wire carrying tin oxide nanostructure;
5), 4) the stainless (steel) wire tin supported nanostructure obtained in is placed in 3.6g glucose 40mL deionized waters, 180 The glucose cladding tin oxide nano structure of stainless (steel) wire load is obtained after being impregnated 4 hours in DEG C;
6), 3) the stainless (steel) wire load organic carbon source cladding tin oxide nano structure obtained in is placed in tube furnace, Just final product stainless (steel) wire load carbon coating oxidation sijna is obtained after being made annealing treatment 2 hours at a temperature of 700 DEG C in argon gas atmosphere Rice structure;
7), 4) the stainless (steel) wire load carbon coating tin oxide nano structure obtained in is placed in tube furnace, in hydrogen gas 650 DEG C of temperatures just obtain final product stainless (steel) wire load carbon covered stannum rice structure in atmosphere after 1 hour;
8), the assembling of button cell, using stainless (steel) wire load carbon covered stannum rice structure be washed into a diameter of 8mm disks as Active material electrode, sodium are used as to electrode, and electrolyte is the ethylene carbonate (EC) and carbonic acid dioctyl phthalate of 1M sodium hexafluoro phosphates (DMC) (volume ratio of EC and DMC are 1 to solution:1), microporous polypropylene membrane is battery diaphragm, is assembled into button cell;
9) after, assembled button cell stands 24 hours, electrochemical property test is carried out in LANDCT2100A.Test Voltage is 0.01V~2.6V, current density 50mA/g.
Embodiment 3
A kind of preparation method of stainless (steel) wire load carbon covered stannum rice structure, includes the following steps:
1) sodium hydroxide that quality is 1.25g, under magnetic stirring, is dissolved in 40ml deionized waters and obtains solution A;
2) 0.47g stannic chlorides, under magnetic stirring, are added into above-mentioned solution A and obtain solution B;
3) 0.05g ammonium fluorides, under magnetic stirring, are added into B solution and obtain solution or emulsion C;
4), solution C is transferred in stainless steel cauldron, while the clean stainless (steel) wire of pre-wash is placed in solution In, hydro-thermal reaction is carried out, stainless (steel) wire is cleaned with deionized water and ethyl alcohol, after being reacted 24 hours at a temperature of 200 DEG C, just obtained Stainless (steel) wire carrying tin oxide nanostructure;
5), 4) the stainless (steel) wire tin supported nanostructure obtained in is placed in 3.6g glucose 40mL deionized waters, 180 The glucose cladding tin oxide nano structure of stainless (steel) wire load is obtained after being impregnated 4 hours in DEG C;
6), 3) the stainless (steel) wire load organic carbon source cladding tin oxide nano structure obtained in is placed in tube furnace, Just final product stainless (steel) wire load carbon coating oxidation sijna is obtained after being made annealing treatment 2 hours at a temperature of 700 DEG C in argon gas atmosphere Rice structure;
7), 4) the stainless (steel) wire load carbon coating tin oxide nano structure obtained in is placed in tube furnace, in hydrogen gas 650 DEG C of temperatures just obtain final product stainless (steel) wire load carbon covered stannum rice structure in atmosphere after 1 hour;
8), the assembling of button cell, using stainless (steel) wire load carbon covered stannum rice structure be washed into a diameter of 8mm disks as Active material electrode, sodium are used as to electrode, and electrolyte is the ethylene carbonate (EC) and carbonic acid dioctyl phthalate of 1M sodium hexafluoro phosphates (DMC) (volume ratio of EC and DMC are 1 to solution:1), microporous polypropylene membrane is battery diaphragm, is assembled into button cell;
9) after, assembled button cell stands 24 hours, electrochemical property test is carried out in LANDCT2100A.Test Voltage is 0.01V~2.6V, current density 50mA/g.
Embodiment 4
A kind of preparation method of stainless (steel) wire load carbon covered stannum rice structure, includes the following steps:
1) sodium hydroxide that quality is 1.808g is dissolved in 40ml deionized waters and obtains solution A;
2) 0.47g stannic chlorides, under magnetic stirring, are added into above-mentioned solution A and obtain solution B;
3) 0.05g ammonium fluorides, under magnetic stirring, are added into B solution and obtain solution or emulsion C;
4), solution C is transferred in stainless steel cauldron, while the clean stainless (steel) wire of pre-wash is placed in solution In, hydro-thermal reaction is carried out, stainless (steel) wire is cleaned with deionized water and ethyl alcohol, after being reacted 24 hours at a temperature of 200 DEG C, just obtained Stainless (steel) wire carrying tin oxide nanostructure;
5), 4) the stainless (steel) wire tin supported nanostructure obtained in is placed in 3.6g glucose 40mL deionized waters, 180 The glucose cladding tin oxide nano structure of stainless (steel) wire load is obtained after being impregnated 4 hours in DEG C;
6), 3) the stainless (steel) wire load organic carbon source cladding tin oxide nano structure obtained in is placed in tube furnace, Just final product stainless (steel) wire load carbon coating oxidation sijna is obtained after being made annealing treatment 2 hours at a temperature of 700 DEG C in argon gas atmosphere Rice structure;
7), 4) the stainless (steel) wire load carbon coating tin oxide nano structure obtained in is placed in tube furnace, in hydrogen gas 650 DEG C of temperatures just obtain final product stainless (steel) wire load carbon covered stannum rice structure in atmosphere after 1 hour;
8), the assembling of button cell, using stainless (steel) wire load carbon covered stannum rice structure be washed into a diameter of 8mm disks as Active material electrode, sodium are used as to electrode, and electrolyte is the ethylene carbonate (EC) and carbonic acid dioctyl phthalate of 1M sodium hexafluoro phosphates (DMC) (volume ratio of EC and DMC are 1 to solution:1), microporous polypropylene membrane is battery diaphragm, is assembled into button cell;
9) after, assembled button cell stands 24 hours, electrochemical property test is carried out in LANDCT2100A.Test Voltage is 0.01V~2.6V, current density 50mA/g.
As shown in Figure 1:
1), the sodium hydroxide of certain mass, which is dissolved in 40mL deionized waters, obtains solution A;
2) stannic chloride, under magnetic stirring, is added into above-mentioned solution A and obtains solution B;
3) ammonium fluoride, under magnetic stirring, is added into above-mentioned solution B and obtains solution or emulsion C;
4) above-mentioned solution C, is transferred to hydrothermal reaction kettle, the clean stainless (steel) wire of pre-wash is placed in solution C, into Row hydro-thermal reaction.It cools down after reaction, stainless (steel) wire is cleaned with deionized water and ethyl alcohol, dry under certain temperature, is obtained stainless Steel mesh carrying tin oxide nanostructure;
5), above-mentioned stainless (steel) wire carrying tin oxide nanostructure is placed in organic solution, reacts one at a certain temperature It fixes time, obtains stainless (steel) wire load Coated with Organic Matter tin oxide nano structure;
6), above-mentioned stainless (steel) wire load Coated with Organic Matter tin oxide nano structure is placed in tube furnace, in certain temperature Lower roasting certain time, calcination atmosphere are argon gas, obtain stainless (steel) wire load carbon coating tin oxide nano structure;
7), above-mentioned carbon stainless steel net load carbon coating tin oxide nano structure is placed in tube furnace, in reducing gas hydrogen It is made annealing treatment under the atmosphere and predetermined temperature of gas and just obtains final product stainless (steel) wire load carbon covered stannum rice after a certain period of time Structure.

Claims (6)

1. a kind of preparation of anode material of lithium-ion battery stainless (steel) wire load carbon covered stannum rice structure, which is characterized in that packet Include following steps:
Step 1:
0.625g~1.808g sodium hydroxides will be proportionally dissolved in 40mL deionized waters and obtain solution A;
Step 2:
Under magnetic stirring, stannic chloride is added into above-mentioned solution A and obtains solution B, the mass ratio of sodium hydroxide and stannic chloride is 2:1 ~4:1;
Step 3:
Under magnetic stirring, ammonium fluoride is added into above-mentioned solution B and obtains solution or emulsion C, the matter of sodium hydroxide and ammonium fluoride Amount is than being 12:1~36:1;
Step 4:
Above-mentioned solution C is transferred to hydrothermal reaction kettle, the clean stainless (steel) wire of pre-wash is placed in solution C, carries out hydro-thermal Reaction, cools down after reaction, and stainless (steel) wire is cleaned with deionized water and ethyl alcohol, dry under certain temperature, and it is negative to obtain stainless (steel) wire Carry tin oxide nano structure;
Step 5:
Above-mentioned stainless (steel) wire carrying tin oxide nanostructure is placed in organic solution, reacts certain time at a certain temperature, It obtains stainless (steel) wire and loads Coated with Organic Matter tin oxide nano structure;
Step 6:
Above-mentioned stainless (steel) wire load Coated with Organic Matter tin oxide nano structure is placed in tube furnace, roasts one at a certain temperature It fixes time, calcination atmosphere is argon gas, obtains stainless (steel) wire load carbon coating tin oxide nano structure;
Step 7:
Above-mentioned carbon stainless steel net load carbon coating tin oxide nano structure is placed in tube furnace, in the atmosphere of reducing gas hydrogen Final product stainless (steel) wire load carbon covered stannum rice structure is just obtained after a certain period of time with being made annealing treatment under predetermined temperature.
2. a kind of anode material of lithium-ion battery stainless (steel) wire load carbon covered stannum rice structure according to claim 1 Prepare, which is characterized in that in the step 4, hydrothermal temperature be 160~200 DEG C, the reaction time be 0.5~for 24 hours.
3. a kind of anode material of lithium-ion battery stainless (steel) wire load carbon covered stannum rice structure according to claim 1 It prepares, which is characterized in that in the step 5, organic carbon source is glucose, dopamine and beta-cyclodextrin etc., and reaction temperature exists 160 DEG C~200 DEG C, 4 hours.
4. a kind of anode material of lithium-ion battery stainless (steel) wire load carbon covered stannum rice structure according to claim 1 It prepares, which is characterized in that in the step 6, annealing temperature is 600 DEG C~750 DEG C, and annealing time is 1~4h, the stream of argon gas Speed is 10~100sccm.
5. a kind of anode material of lithium-ion battery stainless (steel) wire load carbon covered stannum rice structure according to claim 1 It prepares, which is characterized in that in the step 7, annealing temperature is 600~750 DEG C, and annealing time is 1~4h, the flow velocity of hydrogen For 300~400sccm.
6. a kind of application of anode material of lithium-ion battery stainless (steel) wire load carbon covered stannum rice structure, which is characterized in that will Stainless (steel) wire load carbon covered stannum rice structural material is washed into a diameter of 8mm disks as active material electrode, and sodium is used as to electricity Pole, electrolyte are the solution of the ethylene carbonate and carbonic acid dioctyl phthalate of 1M sodium hexafluoro phosphates, are by volume 1:1, polypropylene is micro- Pore membrane is battery diaphragm, is assembled into button cell;By assembled button cell stand 12 hours after, LANDCT2100A into Row electrochemical property test, test voltage are 0.01V~2.6V, current density 50mA/g.
CN201810128510.5A 2018-02-08 2018-02-08 A kind of preparation and its application of anode material of lithium-ion battery stainless (steel) wire load carbon covered stannum rice structure Pending CN108417780A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810128510.5A CN108417780A (en) 2018-02-08 2018-02-08 A kind of preparation and its application of anode material of lithium-ion battery stainless (steel) wire load carbon covered stannum rice structure

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810128510.5A CN108417780A (en) 2018-02-08 2018-02-08 A kind of preparation and its application of anode material of lithium-ion battery stainless (steel) wire load carbon covered stannum rice structure

Publications (1)

Publication Number Publication Date
CN108417780A true CN108417780A (en) 2018-08-17

Family

ID=63128073

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201810128510.5A Pending CN108417780A (en) 2018-02-08 2018-02-08 A kind of preparation and its application of anode material of lithium-ion battery stainless (steel) wire load carbon covered stannum rice structure

Country Status (1)

Country Link
CN (1) CN108417780A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109301229A (en) * 2018-11-12 2019-02-01 陕西科技大学 A kind of preparation method and application of kalium ion battery negative electrode material graphene coated tin oxide/stannic disulfide nano flower
CN113233497A (en) * 2021-05-18 2021-08-10 哈尔滨工业大学 Preparation method and application of carbon-coated tin dioxide material
CN114899375A (en) * 2022-05-09 2022-08-12 西安工业大学 Preparation method of PEDOT-coated sheet-shaped self-assembled FeNCN film

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101723315A (en) * 2009-11-26 2010-06-09 上海大学 Preparation method of Sn/C nano composite material with nucleocapsid structure
CN104022285A (en) * 2014-06-24 2014-09-03 武汉理工大学 SnO2@polymer coaxial heterogeneous nano rod array structural material as well as preparation method and application thereof
CN104157876A (en) * 2014-08-14 2014-11-19 上海交通大学 Preparation method of porous carbon-tin nanocomposite material for lithium battery cathode
CN106299306A (en) * 2016-09-30 2017-01-04 江苏长园华盛新能源材料有限公司 A kind of stannum/carbon composite of nanostructured and its preparation method and application
CN106935823A (en) * 2017-03-20 2017-07-07 郑州大学 A kind of lithium ion battery negative material Sn/C and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101723315A (en) * 2009-11-26 2010-06-09 上海大学 Preparation method of Sn/C nano composite material with nucleocapsid structure
CN104022285A (en) * 2014-06-24 2014-09-03 武汉理工大学 SnO2@polymer coaxial heterogeneous nano rod array structural material as well as preparation method and application thereof
CN104157876A (en) * 2014-08-14 2014-11-19 上海交通大学 Preparation method of porous carbon-tin nanocomposite material for lithium battery cathode
CN106299306A (en) * 2016-09-30 2017-01-04 江苏长园华盛新能源材料有限公司 A kind of stannum/carbon composite of nanostructured and its preparation method and application
CN106935823A (en) * 2017-03-20 2017-07-07 郑州大学 A kind of lithium ion battery negative material Sn/C and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
WEI-MING ZHANG等: "Tin-Nanoparticles Encapsulated in Elastic Hollow Carbon Spheres for High-Performance Anode Material in Lithium-Ion Batteries", 《ADVANCED MATERIALS》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109301229A (en) * 2018-11-12 2019-02-01 陕西科技大学 A kind of preparation method and application of kalium ion battery negative electrode material graphene coated tin oxide/stannic disulfide nano flower
CN109301229B (en) * 2018-11-12 2021-02-05 陕西科技大学 Preparation method and application of graphene-coated tin oxide/tin disulfide nanoflower serving as negative electrode material of potassium ion battery
CN113233497A (en) * 2021-05-18 2021-08-10 哈尔滨工业大学 Preparation method and application of carbon-coated tin dioxide material
CN114899375A (en) * 2022-05-09 2022-08-12 西安工业大学 Preparation method of PEDOT-coated sheet-shaped self-assembled FeNCN film

Similar Documents

Publication Publication Date Title
CN109004199B (en) Preparation method of biomass hard carbon material for negative electrode of sodium-ion battery
CN107579291B (en) Aqueous electrolyte and aqueous metal ion battery
CN107799757B (en) MoS2Nitrogen-doped carbon tube composite material and preparation method and application thereof
CN103219551A (en) Water-system alkali metal ion power storage device
CN107342421B (en) High-content pyridine nitrogen-doped porous carbon negative electrode material, and preparation method and application thereof
CN108598394B (en) Carbon-coated titanium manganese phosphate sodium microspheres and preparation method and application thereof
CN109686953A (en) A kind of lithium-sulfur battery composite cathode material and preparation method thereof
CN107946564B (en) Rich in Na4Mn2O5/Na0.7MnO2Composite material and preparation method and application thereof
CN106972162A (en) A kind of sodium-ion battery double-doped hard carbon microballoon of negative material phosphorus sulphur and preparation method thereof
CN112928343B (en) Water system copper ion battery suitable for large-scale energy storage application
CN113422153B (en) Preparation method of anode side interlayer material for lithium-sulfur battery
CN104795564A (en) Cathode material, electrode piece, secondary cell and application of aqueous-solution secondary cell
CN104064824A (en) Water system rechargeable battery
CN107968195A (en) Lithium-rich cathode material coated by lithium iron phosphate and preparation method thereof
CN114702614A (en) Cathode material for improving cycling stability of vulcanized polyacrylonitrile battery and preparation method thereof
CN110931779A (en) High-capacity long-life aqueous zinc ion battery positive electrode material and preparation method thereof
CN108390067A (en) A kind of preparation and its application of stainless (steel) wire load carbon coating tin oxide nano structure
CN108417780A (en) A kind of preparation and its application of anode material of lithium-ion battery stainless (steel) wire load carbon covered stannum rice structure
CN104241628A (en) Method for preparing titanium-dioxide-modified ferric oxide microspheres as well as produced product and use of titanium-dioxide-modified ferric oxide microspheres
CN110828799A (en) Water-system zinc ion battery MnOx@ C cathode material and preparation method thereof
CN111082162B (en) Aqueous sodium ion battery
CN102751503A (en) Carbon/lithium stannate/graphene composite cathode material of lithium battery and preparation method of material
CN105047870A (en) Nitrogen-doped carbon-coated silicon composite material and preparation method thereof
CN110854365A (en) Preparation method of polyaniline/carbon composite material for anode material of water-based zinc-ion battery
CN108281620B (en) Preparation method of negative electrode material titanium dioxide of sodium-ion battery

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20180817