CN106876678A - A kind of metal and its oxide and carbon composite production technology - Google Patents

A kind of metal and its oxide and carbon composite production technology Download PDF

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Publication number
CN106876678A
CN106876678A CN201710201327.9A CN201710201327A CN106876678A CN 106876678 A CN106876678 A CN 106876678A CN 201710201327 A CN201710201327 A CN 201710201327A CN 106876678 A CN106876678 A CN 106876678A
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metal
oxide
sintering
carbon
powder
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***
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Suzhou Carrying Powerful New Mstar Technology Ltd
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Suzhou Carrying Powerful New Mstar Technology Ltd
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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
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • 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
    • H01M4/04—Processes of manufacture in general
    • 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
    • H01M4/04—Processes of manufacture in general
    • H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
    • 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
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • 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
    • 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
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative electrodes
    • 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

Abstract

The invention discloses a kind of metal and its oxide and carbon composite production technology, including the preparation of preparation of powder, slurry, mist projection granulating, modified surface, preliminary sintering, pyrolysis shelling, cooling and shaping, air-flow crushing, composite negative pole material；The carbon source includes any one in sucrose, polyvinyl alcohol, starch macromolecular material or two or more mixtures；The metal-powder includes any one in tin (Sn), zinc (Zn), aluminium (Al) metal material or two or more mixtures；The metal-oxide powder includes any one in tin oxide, zinc oxide, alundum (Al2O3) oxide powder or two or more mixtures；The thickener is sodium carboxymethylcellulose；Carbon source and metallic tin, zinc, aluminium and its oxide are carried out cladding treatment by the present invention, prepare the composite negative pole material of ball-type core shell structure, and the expansion of metal inner core negative pole is limited by pyrolytic carbon shell, and effectively delay metal negative electrode to be peeled off with foil.

Description

A kind of metal and its oxide and carbon composite production technology
Technical field
The present invention relates to a kind of metal and the laminating material technical equipment field of carbon, more particularly to a kind of metal and its oxide With carbon composite production technology.
Background technology
The research of high-capacity secondary battery negative material has turned into the key for improving battery performance with application.In theory, Some can all can be used as secondary ion cell negative electrode material with the metal of ion component alloy system or metal and its oxide. These negative materials are referred to as alloy material of cathode.Al, Sn, Si and Sb isoreactivity storage elemental lithium are relatively conventional lithium ions two Primary cell metal negative electrode material.Zn is also relatively conventional secondary cell metal negative electrode material.
The shortcoming of alloy material of cathode is that irreversible capacity is larger and cycle performance is poor first.Basic reason is：Alloy When embedding dealkylation reaction is carried out, the structure of component crystal can be reconstructed negative material, and along with big volumetric expansion；Meanwhile, In crystalline material, the formation of intermetallic compound also results in two-phase borderline region and produces uneven Volume Changes, causes The rupture or efflorescence of active particle.This rupture and efflorescence can cause active particle and electrode to lose contact, or even cause negative pole Avalanche produce very big irreversible capacity.
In the prior art, in order to solve this problem, enterprise and research institution carried out it is various have tried to, its technology road Footpath is：Cladding treatment is carried out to inorganic material Si, and alloy anode is combined with carbon material, form the material of nucleocapsid structure Material；The expansion of metal negative electrode is limited by pyrolytic carbon shell, and delays metal negative electrode to be peeled off with foil.Because metal material exists Easily melted under the hot environment of carbon source pyrolysis, it is easy to the problem such as oxidation, for such as metallic tin (Sn), zinc (Zn), aluminium (Al) etc. The cladding treatment of metal material not yet has the maturation process of open report.
The content of the invention
In order to solve the above technical problems, producing work with carbon composite the invention provides a kind of metal and its oxide Skill, for deficiency of the prior art, optimized production process is coated using carbon source with metallic tin, zinc, aluminium and its oxide Treatment, prepares the negative material of ball-type core shell structure, and the expansion of metal inner core negative pole is limited by pyrolytic carbon shell, and effectively prolongs Slow metal negative electrode is peeled off with foil.
To reach above-mentioned purpose, technical scheme is as follows：A kind of metal and its oxide are given birth to carbon composite Production. art, including the preparation of preparation of powder, slurry, mist projection granulating, modified surface, preliminary sintering, pyrolysis shelling, cooling and shaping, gas Stream is crushed, composite negative pole material, it is characterised in that：
1st, the preparation of powder, composition and the proportioning of the powder are：In percentage by weight；
The carbon source includes any one in sucrose, polyvinyl alcohol, starch macromolecular material or two or more Mixture；
The metal-powder includes any one in tin (Sn), zinc (Zn), aluminium (Al) metal material or two or more Mixture；
The metal-oxide powder includes any one in tin oxide, zinc oxide, alundum (Al2O3) oxide powder Or two or more mixtures；
The thickener is sodium carboxymethylcellulose；
2nd, prepared by the slurry, by the powder material input ball mill in step 1, is stirred point with distilled water solution Dissipate, and be sufficiently mixed, under the grinding in ball milling face, obtain slurry；
3rd, mist projection granulating, the slurry in step 2 is pumped into spray drying tower by conveying carries out spray drying granulation, control The Parameter Conditions of spray drying tower processed, the grain diameter of granulation is more than or equal to 100 microns, obtain it is spherical by carbon source coat Grain aggregate；
4th, surface is modified, and the aggregate in step 3 is transferred in kiln, and using being divided in the atmosphere of starvation Section sintering；It is preferred that pure nitrogen gas are used as protective gas, it is 200 DEG C -400 DEG C, the sintering in the sintering range of the sintering Time range be -6 hours 4 hours；The sintering temperature makes carbon source decompose formation pyrolytic carbon shell completely, while will not make again The metal of kernel melts；The sintering time also meets makes carbon source decompose formation pyrolytic carbon shell completely, while will not make kernel again Metal melt the two conditions；The multi-steps sintering includes preliminary sintering, pyrolysis shelling, cooling and shaping；
5th, the sintering range of the preliminary sintering is 200 DEG C -300 DEG C；Soaking time scope is at least 2 hours；
6th, the sintering range of the pyrolysis shelling is 300 DEG C -400 DEG C；Soaking time scope is at least 1 hour；
7th, the cooling and shaping, under nitrogen holding, cooling down to room temperature；Obtain the ball that metal inner core is coated with carbon shell Core-shell structure composite material particle；In the composite material granular, the proportion of metal and its oxide surface carbon coated is Between 2% -50%；The real density of the composite material granular reaches 0.5g/cm3More than；
8th, the air-flow crushing, the composite material granular for obtaining in step 7 is transferred in airslide disintegrating mill, with common empty Gas is source of the gas, and spheroidization pulverization process is carried out to composite material granular by airslide disintegrating mill, forms 10 microns -100 microns Composite negative pole material；
9th, the composite negative pole material, the composite negative pole material in step 8 is detected, dispensed, is put in storage.
By above-mentioned technical proposal, the beneficial effect of technical solution of the present invention is：By disperseing slurrying, drying-granulating, table The modified sintering in face and air-flow crushing production technology, cladding treatment is carried out by carbon source and metallic tin, zinc, aluminium and its oxide, is prepared The negative material of ball-type core shell structure, the expansion of metal inner core negative pole is limited by pyrolytic carbon shell, and effectively delays metal to bear Pole is peeled off with foil, obtains high performance high-capacity secondary battery alloy composite anode material.
1st, metal of the present invention and its oxide and carbon composite production technology, solve metal dust is carried out in a solvent It is easy to the problem for settling, processing characteristics is poor during dispersion；
2nd, the alloy material of cathode of present invention process manufacture, is electrolysed in blocking battery by the pyrolytic carbon layer of surface compact There is the path of side reaction with active material in liquid, significantly reduce the gas production problems of too that electrolyte decomposition is caused；
3rd, the alloy material of cathode of present invention process manufacture, electrolyte is blocked repeatedly by the pyrolytic carbon layer of surface compact With the possibility that reactive species interface occurs side reaction, it is to avoid the battery capacity loss risk that thus results in；
4th, production technology is coated by Carbon Materials of the invention, is solved bonding between foil and active material in battery The relatively low problem of intensity, solves active material recirculation gas stripper Problem of Failure.
Brief description of the drawings
Technical scheme in order to illustrate more clearly the embodiments of the present invention, below will be in embodiment or description of the prior art The required accompanying drawing for using is briefly described, it should be apparent that, drawings in the following description are only some realities of the invention Example is applied, for those of ordinary skill in the art, on the premise of not paying creative work, can also be according to these accompanying drawings Obtain other accompanying drawings.
Fig. 1 is that a kind of metal and its oxide disclosed in the embodiment of the present invention show with the carbon composite technological process of production It is intended to.
Specific embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.It is based on Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of creative work is not made Embodiment, belongs to the scope of protection of the invention.
According to Fig. 1, match somebody with somebody the invention provides a kind of metal and its oxide and carbon composite production technology, including powder System, slurry preparation, mist projection granulating, modified surface, preliminary sintering, pyrolysis shelling, cooling and shaping, air-flow crushing, composite negative pole material Material；
1st, the preparation of powder, composition and the proportioning of the powder are：In percentage by weight；
The carbon source includes any one in sucrose, polyvinyl alcohol, starch macromolecular material or two or more Mixture；The metal-powder includes any one in tin (Sn), zinc (Zn), aluminium (Al) metal material or two or more Mixture；The metal-oxide powder include tin oxide, zinc oxide, alundum (Al2O3) oxide powder in any one or The two or more mixture of person；The thickener is sodium carboxymethylcellulose；
2nd, prepared by the slurry, by the powder material input ball mill in step 1, is stirred point with distilled water solution Dissipate, and be sufficiently mixed, under the grinding in ball milling face, obtain slurry；
3rd, mist projection granulating, the slurry in step 2 is pumped into spray drying tower by conveying carries out spray drying granulation, control The Parameter Conditions of spray drying tower processed, the grain diameter of granulation is more than or equal to 100 microns, obtain it is spherical by carbon source coat Grain aggregate；
4th, surface is modified, and the aggregate in step 3 is transferred in kiln, and using being divided in the atmosphere of starvation Section sintering；It is preferred that pure nitrogen gas are used as protective gas, the sintering temperature makes carbon source decompose formation pyrolytic carbon shell completely, while again not Can melt the metal of kernel；The sintering time also meets makes carbon source decompose formation pyrolytic carbon shell completely, while will not make again The metal of kernel melts the two conditions；The multi-steps sintering includes preliminary sintering, pyrolysis shelling, cooling and shaping；
5th, the sintering range of the preliminary sintering is 200 DEG C -300 DEG C；Soaking time scope is at least 2 hours；Institute The sintering range for stating pyrolysis shelling is 300 DEG C -400 DEG C；Soaking time scope is at least 1 hour；The cooling and shaping, Under nitrogen holding, cooling down to room temperature；Obtain the spherical shell structure composite material granular that metal inner core is coated with carbon shell；It is described In composite material granular, the proportion of metal and its oxide surface carbon coated is between 2% -50%；The composite The real density of particle reaches 0.5g/cm3More than；
6th, the air-flow crushing, the composite material granular for obtaining in step 5 is transferred in airslide disintegrating mill, with common empty Gas is source of the gas, and spheroidization pulverization process is carried out to composite material granular by airslide disintegrating mill, forms 10 microns -100 microns Composite negative pole material；The composite negative pole material, the composite negative pole material in step 8 is detected, dispensed, is put in storage.
Specific implementation process operating procedure of the invention is：1st, according to proportioning, activated carbon, thickener, carbon source, metal are weighed And its oxide；The mixture 10% of activated carbon and other adding ingredients；70% zinc metal fine powder, 10% zinc oxide ultra_fine powderses with 10% carbon source mixes, and carbon source can be sucrose, resin Polymer material；By carbon source and activated carbon in dispersing apparatus, or Activated carbon is stirred dispersion with adding ingredient, zinc powder and oxide powder and zinc mixture；Treat after the completion of ball milling, take out slurry, lead to Cross spray drying tower and be dried granulation as aggregate, size controlling is more than 100 μm in making particle；2nd, activated carbon aggregate Surface modification treatment：The activated carbon aggregate that surface covers organic carbon source is sintered in kiln, 400 degree of sintering temperature, 4-6 hours of sintering time, the carbon source on surface is set to be pyrolyzed to form pyrolytic carbon.The cladding that one side pyrolytic carbon is formed can strengthen The structural strength of aggregate, on the other hand, the outer layer pyrolytic carbon of spherical shell structure can also reduce active material and the pair of electrolyte is anti- Should occur；3rd, the crushing of activated carbon aggregate, spheroidization pulverization process is carried out by the material input air flow pulverizer after sintering, its Middle source of the gas is normal air, forms 10 microns to 100 microns of composite negative pole raw material；The material because be compounded with activated carbon and Pyrolytic carbon, forms height than table loose structure, and imbibition ability strengthens, while reducing apparent gravity, it is easier to suspend in a solvent, Improve the processing characteristics of negative material.
By above-mentioned specific embodiment, the beneficial effects of the invention are as follows：It is modified by disperseing slurrying, drying-granulating, surface Sintering and air-flow crushing production technology, cladding treatment is carried out by carbon source and metallic tin, zinc, aluminium and its oxide, prepares ball-type core The negative material of shell structure, the expansion of metal inner core negative pole is limited by pyrolytic carbon shell, and effectively delays metal negative electrode and paper tinsel Material is peeled off, and obtains high performance high-capacity secondary battery alloy composite anode material.
The foregoing description of the disclosed embodiments, enables professional and technical personnel in the field to realize or uses the present invention. Various modifications to these embodiments will be apparent for those skilled in the art, as defined herein General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, the present invention The embodiments shown herein is not intended to be limited to, and is to fit to and principles disclosed herein and features of novelty phase one The scope most wide for causing.

Claims (1)

1. a kind of metal and its oxide and carbon composite production technology, it is characterised in that including preparation of powder, slurry system Standby, mist projection granulating, modified surface, preliminary sintering, pyrolysis shelling, cooling and shaping, air-flow crushing, composite negative pole material；The gold Category and its oxide are with the concrete technology flow process of carbon composite production technology：
1.1st, the preparation of powder, composition and the proportioning of the powder are：In percentage by weight；
The carbon source includes any one in sucrose, polyvinyl alcohol, starch macromolecular material or two or more mixing Thing；
The metal-powder include in tin (Sn), zinc (Zn), aluminium (Al) metal material any one or it is two or more mixed Compound；
The metal-oxide powder include tin oxide, zinc oxide, alundum (Al2O3) oxide powder in any one or Two or more mixtures；
The thickener is sodium carboxymethylcellulose；
1.2nd, prepared by the slurry, by the powder material input ball mill in step 1.1, is stirred point with distilled water solution Dissipate, and be sufficiently mixed, under the grinding in ball milling face, obtain slurry；
1.3rd, mist projection granulating, the slurry in step 1.2 is pumped into spray drying tower by conveying carries out spray drying granulation, control The Parameter Conditions of spray drying tower processed, the grain diameter of granulation is more than or equal to 100 microns, obtain it is spherical by carbon source coat Grain aggregate；
1.4th, surface is modified, and the aggregate in step 1.3 is transferred in kiln, and using being divided in the atmosphere of starvation Section sintering；It is preferred that pure nitrogen gas are used as protective gas, it is 200 DEG C -400 DEG C, the sintering in the sintering range of the sintering Time range be -6 hours 4 hours；The sintering temperature makes carbon source decompose formation pyrolytic carbon shell completely, while will not make again The metal of kernel melts；The sintering time also meets makes carbon source decompose formation pyrolytic carbon shell completely, while will not make kernel again Metal melt the two conditions；The multi-steps sintering includes preliminary sintering, pyrolysis shelling, cooling and shaping；
1.5th, the sintering range of the preliminary sintering is 200 DEG C -300 DEG C；Soaking time scope is at least 2 hours；
1.6th, the sintering range of the pyrolysis shelling is 300 DEG C -400 DEG C；Soaking time scope is at least 1 hour；
1.7th, the cooling and shaping, under nitrogen holding, cooling down to room temperature；Obtain the spherical shell that metal inner core is coated with carbon shell Structural composite material particle；In the composite material granular, the proportion of metal and its oxide surface carbon coated for 2%- Between 50%；The real density of the composite material granular reaches 0.5g/cm3More than；
1.8th, the air-flow crushing, the composite material granular for obtaining in step 7 is transferred in airslide disintegrating mill, with normal air It is source of the gas, spheroidization pulverization process is carried out to composite material granular by airslide disintegrating mill, forms 10 microns -100 microns and answer Close negative material；
1.9th, the composite negative pole material, the composite negative pole material in step 8 is detected, dispensed, is put in storage.
CN201710201327.9A 2017-03-30 2017-03-30 A kind of metal and its oxide and carbon composite production technology Pending CN106876678A (en)

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Publication number Priority date Publication date Assignee Title
US20200287207A1 (en) * 2019-03-06 2020-09-10 Nanotek Instruments, Inc. Process for producing porous particulates of graphene shell-protected alkali metal, electrodes, and alkali metal battery
CN111653760A (en) * 2020-04-30 2020-09-11 中南大学 Two-dimensional metal sheet and preparation method and application thereof
CN114927675A (en) * 2022-06-30 2022-08-19 宜春瑞富特新能源材料技术有限公司 Composite metal-coated silicon carbide-based negative electrode material and preparation method and application thereof

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20200287207A1 (en) * 2019-03-06 2020-09-10 Nanotek Instruments, Inc. Process for producing porous particulates of graphene shell-protected alkali metal, electrodes, and alkali metal battery
CN111653760A (en) * 2020-04-30 2020-09-11 中南大学 Two-dimensional metal sheet and preparation method and application thereof
CN111653760B (en) * 2020-04-30 2021-11-05 中南大学 Two-dimensional metal sheet and preparation method and application thereof
CN114927675A (en) * 2022-06-30 2022-08-19 宜春瑞富特新能源材料技术有限公司 Composite metal-coated silicon carbide-based negative electrode material and preparation method and application thereof

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Application publication date: 20170620