CN105552354A - Method for preparing lithium ion battery cathode material - Google Patents

Method for preparing lithium ion battery cathode material Download PDF

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CN105552354A
CN105552354A CN201610151315.5A CN201610151315A CN105552354A CN 105552354 A CN105552354 A CN 105552354A CN 201610151315 A CN201610151315 A CN 201610151315A CN 105552354 A CN105552354 A CN 105552354A
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nano particle
sio
lithium ion
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water
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CN105552354B (en
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刘伟良
杨婷婷
赵丹
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Qilu University of Technology
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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
    • 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
    • H01M4/36—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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • 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

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
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  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)
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Abstract

The invention discloses a method for preparing a lithium ion battery cathode material. The cathode material is a composite microsphere of a special yolk structure, the nuclear layer of the composite microsphere is Fe3O4, the shell layer of the composite microsphere is a C-N layer containing mesoporous, and a cavity formed after etching is located between the nuclear layer and the shell layer. The preparing method comprises the steps of firstly, synthesizing SiO2 nano particles with the sol-gel method, and synthesizing Fe3O4 nano particles with the hydrothermal method; then coating Fe3O4 with a layer of SiO2, and coating the SiO2 layer with a composite shell composed of SiO2 nano particles and melamine resin; finally, obtaining the composite microsphere of the special yolk structure through calcination and etching. The material is novel in structure, the volume effect of the Fe3O4 particles can be inhibited by the cavity, the lithium ion diffusion velocity can be increased through the mesoporous so that the electrochemical reaction rate can be increased, and multiplying power and cycle performance can also be improved while the conductivity and specific capacity of the material are improved.

Description

A kind of preparation method of lithium ion battery negative material
Technical field
The invention belongs to energy technology field and technical field of lithium ion, be specifically related to a kind of preparation method of lithium ion battery negative material.
Background technology
In recent years, graphite because of its charge-discharge performance stablize, theoretical specific capacity is 372mAhg 1, be widely used in the research of lithium ion battery negative material, but along with development that is scientific and technical and electronic product, existing electric energy storage device has been difficult to the satisfied new market demand.Data show, nano level transition metal oxide (M xo y, M=Mn, Fe, Co, Ni etc.) and theoretical specific capacity is higher, large as new energy materials development space.Wherein Fe 3o 4theoretical capacity is 924mAhg 1, good stability, low price, wide material sources, are used as lithium ion battery negative material gradually.But Fe 3o 4conductivity own is low, and the phenomenons such as cohesion and bulk effect easily occur circulation time, needs further modification to meet reality need as negative material.
The people such as WangJian-Gan have made the coated Mn oxide lithium ion battery negative material of N doping C, illustrate that the material with carbon element that N adulterates has higher electronic transmission performance.Patent of invention CN104779378A describes the preparation method of a kind of germanium-mesoporous carbon fiber composite lithium cell cathode material, for solving the volumetric expansion problem of germanium in removal lithium embedded process, water-soluble etching method is utilized to prepare the matrix of carbon fiber as lithium cell cathode material of special meso-hole structure, and be compounded to form GeMCF composite material with germanium source, effectively cushion the volumetric expansion of germanium in removal lithium embedded process, improve specific capacity and the cycle performance of lithium cell cathode material simultaneously.For the lithium cell cathode material of project organization novelty provides imagination space.
For lithium ion battery negative material structural instability in prior art, the shortcoming of cycle performance difference, the present invention proposes a kind of Fe with special construction 3o 4the preparation method of composite material.The Fe of prepared by the present invention have special construction 3o 4composite material, stratum nucleare is Fe 3o 4material, shell is containing mesoporous C, N layer.Stratum nucleare has higher theoretical capacity, and the mesoporous of shell has high specific area and homogeneous mesopore orbit, for the transmission of lithium ion provides passage.The present invention is intended to for the research of lithium cell cathode material provides new approaches.
Summary of the invention
For the above fact, the preparation method of a kind of lithium ion battery negative material provided by the invention, comprises the following steps:
(1) ferric trichloride six water, anhydrous sodium acetate and natrium citricum are mixed with a certain amount of ethylene glycol, join in autoclave, react 10 ~ 12 hours at 180 ~ 200 DEG C, by magnet by precipitate and separate, use absolute ethyl alcohol and water washing successively, dry, obtain Fe 3o 4nano particle;
(2) absolute ethyl alcohol and ammoniacal liquor are mixed, again tetraethoxysilane was dropped in above-mentioned mixed solution in 20 ~ 30 minutes under mechanical agitation, react 10 ~ 12 hours at 20 ~ 30 DEG C, use absolute ethyl alcohol and water washing successively, dry, obtain SiO 2nano particle;
(3) by step (1) gained Fe 3o 4nano particle, absolute ethyl alcohol and ammoniacal liquor mix, and at 20 ~ 25 DEG C, mechanical agitation dripped a certain amount of tetraethoxysilane after 30 ~ 60 minutes, and mechanical agitation 10 ~ 12 hours, by magnet by precipitate and separate, uses absolute ethyl alcohol and water washing successively, dry, obtain Fe 3o 4siO 2nano particle;
(4) melamine is dissolved in 37% formalin under 50 ~ 60 DEG C of water-baths, obtains the mixed solution of homogeneous transparent;
(5) by step (2) gained SiO 2after nano particle and water mix, add gained mixed solution and catalyst in step (4), react 0.5 ~ 3 hour under 50 ~ 60 DEG C of water-baths.After by step (3) gained Fe 3o 4siO 2nano particle adds in above-mentioned mixed solution, continues to react 2 ~ 4 hours under these conditions, by magnet by precipitate and separate, washes with water, dry, obtains Fe 3o 4siO 2(SiO 2with melamine resin composite bed) nano particle;
(6) gained solid product in step (5) is sintered 4 ~ 6 hours in 600 ~ 850 DEG C of inert gas shielding atmosphere, obtain Fe 3o 4siO 2(SiO 2with C-N composite bed);
(7) by gained Fe in step (6) 3o 4siO 2(SiO 2with C-N composite bed) nano particle solid product, etching agent and water mixes, and reacts 4 ~ 8 hours, by magnet by precipitate and separate, wash with water at 60 ~ 85 DEG C, dry, obtains Fe 3o 4cavity (the mesoporous layer of C-N nano particle) nano particle.
Described in upper step (4), the mol ratio of melamine and 37% formalin is 1:1 ~ 5.
Catalyst described in upper step (5) is the one in formic acid, glacial acetic acid or NaOH.
Etching agent described in upper step (7) is the one in hydrofluoric acid or NaOH.
Be compared with the prior art, preparation method's tool of a kind of lithium ion battery negative material provided by the invention has the following advantages:
(1) magnetic responsiveness that the present invention makes full use of magnetic material is separated, simply easy to operate;
(2) Fe prepared by the present invention 3o 4cavity (the mesoporous layer of C-N nano particle) nano particle structure is unique, and cavity can suppress Fe 3o 4the bulk effect of particle, the mesoporous diffusion velocity accelerating lithium ion, improves electrochemical reaction speed;
(3) Fe prepared by the present invention 3o 4cavity (the mesoporous layer of C-N nano particle) nano particle, shell C, N content are high, are used as lithium ion battery negative material, excellent electrical property.
Embodiment
Below by way of specific embodiment foregoing of the present invention be further illustrated but this should be interpreted as content of the present invention is only limitted to following example.
Embodiment 1:
(1) be dissolved in 40ml ethylene glycol by 2.1g ferric trichloride six water, 2.4g anhydrous sodium acetate and 0.35g natrium citricum, ultrasonic disperse forms uniform suspension in 1 hour.By this suspension mechanical agitation 1 hour under normal temperature, join afterwards in the reactor of 100ml in 180 DEG C of reactions 10 hours.By magnet by precipitate and separate, respectively wash 3 times successively with absolute ethyl alcohol and distilled water, at 40 DEG C, drying 8 hours, obtains Fe 3o 4nano particle;
(2) 150ml absolute ethyl alcohol and 10ml ammoniacal liquor are mixed, then dropwised in 25 minutes by 5ml tetraethoxysilane, react 10 hours, respectively wash 3 times successively with absolute ethyl alcohol and distilled water at 25 DEG C, at 40 DEG C, drying 10 hours, obtains SiO 2nano particle;
(3) by step (1) gained Fe 3o 40.15g, 100ml absolute ethyl alcohol and 6ml ammoniacal liquor mixing and stirring, under 25 DEG C of water-baths, mechanical agitation is after 40 minutes, slowly drips 4ml tetraethoxysilane, continues mechanical agitation 10 hours, and solution slowly becomes white.By magnet by precipitate and separate, respectively wash 3 times successively with absolute ethyl alcohol and distilled water, at 40 DEG C, drying 10 hours, obtains Fe 3o 4siO 2nano particle;
(4) get 1.2g melamine and 3ml37% formalin, 60 DEG C of lower magnetic forces stir and dissolve completely to melamine for 30 minutes, obtain the mixed solution of homogeneous transparent;
(5) step (2) gained SiO is got 2after nano particle 0.1g and 100ml distilled water mix, add formalin and 1.5mL glacial acetic acid that step (4) gained is dissolved with melamine, mechanic whirl-nett reaction 1 hour under 50 DEG C of water-baths.Again by step (3) gained Fe 3o 4siO 2nano particle 0.2g adds in above-mentioned mixed solution, continues reaction 2 hours under the same terms.By magnet by precipitate and separate, be washed with distilled water to few 3 times, at 60 DEG C, drying 10 hours, obtains Fe 3o 4siO 2(SiO 2with melamine resin composite bed) nano particle;
(6) by step (5) gained nano particle mortar grinder powdered, be placed in crucible, adopt tube furnace to carry out roast, condition is: Ar atmosphere is enclosed, 600 DEG C, and be incubated 4 hours, heating rate is 1 DEG C/min.Treat that temperature is down to initial temperature, taken out by crucible, black solid is Fe 3o 4cavity (the mesoporous layer of C-N nano particle) nano particle;
(7) step (6) gained Fe is got 3o 4cavity (the mesoporous layer of C-N nano particle) nano particle 0.2g and 1.0g NaOH are dissolved in 100ml water, and ultrasonic disperse obtains even suspension-turbid liquid in 30 minutes, react 4 hours at 60 DEG C.By magnet by precipitate and separate, with distilled water washing, at 40 DEG C, drying 10 hours, is Fe with mortar grinder powdered 3o 4cavity (the mesoporous layer of C-N nano particle) powder.
Embodiment 2:
(1) be dissolved in 50ml ethylene glycol by 1.8g ferric trichloride six water, 2.0g anhydrous sodium acetate and 0.3g natrium citricum, ultrasonic disperse forms uniform suspension in 1 hour.By this suspension mechanical agitation 2 hours under normal temperature, join afterwards in the reactor of 100ml in 180 DEG C of reactions 12 hours.By magnet by precipitate and separate, respectively wash 3 times successively with absolute ethyl alcohol and distilled water, at 40 DEG C, drying 10 hours, obtains Fe 3o 4nano particle;
(2) 120ml absolute ethyl alcohol and 8ml ammoniacal liquor are mixed, then dropwised in 20 minutes by 4ml tetraethoxysilane, react 10 hours, respectively wash 3 times successively with absolute ethyl alcohol and distilled water at 30 DEG C, at 40 DEG C, drying 12 hours, obtains SiO 2nano particle;
(3) by step (1) gained Fe 3o 40.2g, 150ml absolute ethyl alcohol and 8ml ammoniacal liquor mixing and stirring, under 20 DEG C of water-baths, mechanical agitation is after 50 minutes, slowly drips 5ml tetraethoxysilane, continues mechanical agitation 12 hours, and solution slowly becomes white.By magnet by precipitate and separate, respectively wash 3 times successively with absolute ethyl alcohol and distilled water, at 40 DEG C, drying 10 hours, obtains Fe 3o 4siO 2nano particle;
(4) get 1.5g melamine and 4ml37% formalin, 60 DEG C of lower magnetic forces stir and dissolve completely to melamine for 40 minutes, obtain the mixed solution of homogeneous transparent;
(5) step (2) gained SiO is got 2the above-mentioned formalin and the 1.0g NaOH that are dissolved with melamine is added, mechanic whirl-nett reaction 1 hour under 60 DEG C of water-baths after nano particle 0.15g and 120ml distilled water mix.Again by step (3) gained Fe 3o 4siO 2nano particle 0.1g adds in above-mentioned mixed solution, continues reaction 2 hours under the same terms.By magnet by precipitate and separate, be washed with distilled water to few 3 times, at 60 DEG C, drying 10 hours, obtains Fe 3o 4siO 2(SiO 2with melamine resin composite bed) nano particle;
(6) by step (5) gained nano particle mortar grinder powdered, be placed in crucible, adopt tube furnace to carry out roast, condition is: Ar atmosphere is enclosed, 700 DEG C, and be incubated 5 hours, heating rate is 1 DEG C/min.Treat that temperature is down to initial temperature, taken out by crucible, black solid is Fe 3o 4cavity (the mesoporous layer of C-N nano particle) nano particle;
(7) step (6) gained Fe is got 3o 4cavity (the mesoporous layer of C-N nano particle) nano particle 0.15g and 2ml hydrofluoric acid are dissolved in 120ml water, and ultrasonic disperse obtains even suspension-turbid liquid in 40 minutes, react 6 hours at 60 DEG C.By magnet by precipitate and separate, with distilled water washing, at 40 DEG C, drying 10 hours, is Fe with mortar grinder powdered 3o 4cavity (the mesoporous layer of C-N nano particle) powder.
Embodiment 3:
(1) be dissolved in 60ml ethylene glycol by 2.5g ferric trichloride six water, 3.0g anhydrous sodium acetate and 0.5g natrium citricum, ultrasonic disperse forms uniform suspension in 1 hour.By this suspension mechanical agitation 1 hour under normal temperature, join afterwards in the reactor of 150ml in 200 DEG C of reactions 10 hours.By magnet by precipitate and separate, respectively wash 3 times successively with absolute ethyl alcohol and distilled water, at 40 DEG C, drying 12 hours, obtains Fe 3o 4nano particle;
(2) 150ml absolute ethyl alcohol and 15ml ammoniacal liquor are mixed, then dropwised in 30 minutes by 5ml tetraethoxysilane, react 12 hours, respectively wash 3 times successively with absolute ethyl alcohol and distilled water at 25 DEG C, at 40 DEG C, drying 12 hours, obtains SiO 2nano particle;
(3) by step (1) gained Fe 3o 40.12g, 80ml absolute ethyl alcohol and 5ml ammoniacal liquor mixing and stirring, under 25 DEG C of water-baths, mechanical agitation is after 60 minutes, slowly drips 4ml tetraethoxysilane, continues mechanical agitation 10 hours, and solution slowly becomes white.By magnet by precipitate and separate, respectively wash 3 times successively with absolute ethyl alcohol and distilled water, at 40 DEG C, drying 12 hours, obtains Fe 3o 4siO 2nano particle;
(4) get 2.3g melamine and 18ml37% formalin, 60 DEG C of lower magnetic forces stir and dissolve completely to melamine for 30 minutes, obtain the mixed solution of homogeneous transparent;
(5) step (2) gained SiO is got 2the above-mentioned formalin and the 2.5mL glacial acetic acid that are dissolved with melamine is added, mechanic whirl-nett reaction 1 hour under 60 DEG C of water-baths after nano particle 0.3g and 150ml distilled water mix.Again by step (3) gained Fe 3o 4siO 2nano particle 0.15g adds in above-mentioned mixed solution, continues reaction 2 hours under the same terms.By magnet by precipitate and separate, be washed with distilled water to few 3 times, at 60 DEG C, drying 10 hours, obtains Fe 3o 4siO 2(SiO 2with melamine resin composite bed) nano particle;
(6) by step (5) gained nano particle mortar grinder powdered, be placed in crucible, adopt tube furnace to carry out roast, condition is: Ar atmosphere is enclosed, 800 DEG C, and be incubated 6 hours, heating rate is 1 DEG C/min.Treat that temperature is down to initial temperature, taken out by crucible, black solid is Fe 3o 4cavity (the mesoporous layer of C-N nano particle) nano particle;
(7) step (6) gained Fe is got 3o 4cavity (the mesoporous layer of C-N nano particle) nano particle 0.2g and 1.0g NaOH are dissolved in 100ml water, and ultrasonic disperse obtains even suspension-turbid liquid in 40 minutes, react 5 hours at 80 DEG C.By magnet by precipitate and separate, with distilled water washing, at 40 DEG C, drying 12 hours, is Fe with mortar grinder powdered 3o 4cavity (the mesoporous layer of C-N nano particle) powder.

Claims (6)

1. a lithium ion battery negative material, is characterized in that, described negative material has yolk structure, and stratum nucleare is Fe 3o 4, shell is containing mesoporous C, N layer, the cavity for being formed after etching between stratum nucleare and shell.
2. a preparation method for lithium ion battery negative material, is characterized in that, comprises the following steps:
Ferric trichloride six water, anhydrous sodium acetate and natrium citricum are mixed with a certain amount of ethylene glycol, joins in autoclave, react 10 ~ 12 hours at 180 ~ 200 DEG C, by magnet by precipitate and separate, use absolute ethyl alcohol and water washing successively, dry, obtain Fe 3o 4nano particle;
Absolute ethyl alcohol and ammoniacal liquor are mixed, again tetraethoxysilane was dropped in above-mentioned mixed solution in 20 ~ 30 minutes under mechanical agitation, react 10 ~ 12 hours under room temperature, use absolute ethyl alcohol and water washing successively, dry, obtain SiO 2nano particle;
By step (1) gained Fe 3o 4nano particle, absolute ethyl alcohol and ammoniacal liquor mix, and at 20 ~ 25 DEG C, mechanical agitation dripped a certain amount of tetraethoxysilane after 30 ~ 60 minutes, and mechanical agitation 10 ~ 12 hours, by magnet by precipitate and separate, uses absolute ethyl alcohol and water washing successively, dry, obtain Fe 3o 4siO 2nano particle;
Melamine is dissolved in 37% formalin under 50 ~ 60 DEG C of water-baths, obtains the mixed solution of homogeneous transparent;
By step (2) gained SiO 2nano particle and water mix, and add gained mixed solution and catalyst in step (4), react step (3) gained Fe after 0.5 ~ 3 hour under 50 ~ 60 DEG C of water-baths 3o 4siO 2nano particle adds in above-mentioned mixed solution, continues to react 2 ~ 4 hours under these conditions, by magnet by precipitate and separate, washes with water, dry, obtains Fe 3o 4siO 2(SiO 2nano particle and melamine resin composite bed) nano particle;
Gained solid product in step (5) is sintered 4 ~ 6 hours in 600 ~ 850 DEG C of inert gas shielding atmosphere, obtains Fe 3o 4siO 2(SiO 2with C-N composite bed);
By gained Fe in step (6) 3o 4siO 2(SiO 2with C-N composite bed) nano particle solid product, etching agent and water mixes, and reacts 4 ~ 8 hours, by magnet by precipitate and separate, wash with water at 60 ~ 85 DEG C, dry, obtains Fe 3o 4cavity (the mesoporous layer of C-N nano particle) nano particle.
3. the preparation method of a kind of lithium ion battery negative material as claimed in claim 2, is characterized in that: the mol ratio of step (4) described melamine and 37% formalin is 1:1 ~ 5.
4. the preparation method of a kind of lithium ion battery negative material as claimed in claim 2, is characterized in that: the catalyst described in step (5) is the one in formic acid, glacial acetic acid or NaOH.
5. the preparation method of a kind of lithium ion battery negative material as claimed in claim 2, is characterized in that: the etching agent described in step (7) is the one in hydrofluoric acid or NaOH.
6. the preparation method of a kind of lithium ion battery negative material as claimed in claim 2, is characterized in that: the Fe described in step (7) 3o 4cavity (the mesoporous layer of C-N nano particle) nano particle, it is mesoporous that its shell is formed after containing etching.
CN201610151315.5A 2016-03-17 2016-03-17 A kind of preparation method of lithium ion battery negative material Expired - Fee Related CN105552354B (en)

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CN113636563A (en) * 2021-08-24 2021-11-12 郑州轻工业大学 SiO (silicon dioxide)2Preparation method of incompletely-coated magnetic nanoparticles

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Publication number Priority date Publication date Assignee Title
KR20200059714A (en) * 2018-11-21 2020-05-29 (주)파마오넥스 Method for manufacturing porous silica-iron-copper
CN113543616A (en) * 2021-07-16 2021-10-22 中原工学院 Hollow core-shell structure Fe3O4@SiO2@ PANI wave absorbing agent and preparation method thereof
CN113636563A (en) * 2021-08-24 2021-11-12 郑州轻工业大学 SiO (silicon dioxide)2Preparation method of incompletely-coated magnetic nanoparticles
CN113636563B (en) * 2021-08-24 2023-12-22 郑州轻工业大学 SiO (silicon dioxide) 2 Preparation method of incompletely coated magnetic nano particles

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