CN110148736A - A kind of silicon/carbon nanotube/cobalt composite material preparation method and applications - Google Patents

A kind of silicon/carbon nanotube/cobalt composite material preparation method and applications Download PDF

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Publication number
CN110148736A
CN110148736A CN201910477183.9A CN201910477183A CN110148736A CN 110148736 A CN110148736 A CN 110148736A CN 201910477183 A CN201910477183 A CN 201910477183A CN 110148736 A CN110148736 A CN 110148736A
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silicon
composite material
carbon nanotube
cobalt
melamine
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范立双
张宇
张乃庆
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Harbin Institute of Technology
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Harbin Institute of Technology
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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
    • C01B32/158—Carbon nanotubes
    • 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
    • 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
    • H01M4/386—Silicon or alloys based on silicon
    • 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
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
    • 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
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • 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
    • 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)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Nanotechnology (AREA)
  • Organic Chemistry (AREA)
  • Composite Materials (AREA)
  • Manufacturing & Machinery (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses a kind of silicon/carbon nanotube/cobalt composite material preparation method and applications, and described method includes following steps: (1) using wet ball grinding mixing silicon, melamine and nitric acid cobalt dust, obtain silicon/melamine/nitric acid cobalt precursor；(2) use inert gas as protective gas; 700 ~ 900 DEG C are raised to from room temperature with the heating rate of 0.5 ~ 2 DEG C/min; high-temperature heat treatment silicon/melamine/nitric acid 2 ~ 6h of cobalt precursor with this condition, naturally cools to room temperature, obtains silicon/carbon nanotube/cobalt composite material.Composite material exhibits prepared by the present invention have gone out high reversible specific capacity and cyclical stability, the preparation suitable for height ratio capacity lithium ion battery negative material.

Description

A kind of silicon/carbon nanotube/cobalt composite material preparation method and applications
Technical field
The invention belongs to technical field of composite materials, be related to a kind of silicon/carbon nanotube/cobalt composite material preparation method and Its application in lithium ion battery.
Background technique
Since lithium ion battery has high-energy density, long circulation life, operating voltage high and environmentally friendly etc. many Advantage has been achieved for being widely applied popularization in current energy storage market.But with all kinds of electronic devices and electric car Rapid development, for the energy density of currently used lithium ion battery, more stringent requirements are proposed.Due to currently making extensively The theoretical specific capacity of graphite cathode is only 374 mAh g-1, be no longer satisfied the next-generation high specific energy lithium ion battery of development Capacity of negative plates demand.Therefore, exploitation height ratio capacity cathode new material is for realizing that lithium ion battery is prominent in energy density It breaks most important.Silicium cathode has up to 4200 mAh g-1Theoretical specific capacity；Meanwhile silicon is second abundant yuan in the earth's crust Element, widely distributed on earth, abundant raw material is environmentally friendly, and therefore, silicium cathode is considered as developing next-generation high specific energy lithium The ideal negative electrode material of ion battery.However, silicon can occur biggish volume and become due to during lithium ion is embedded in and is deviate from Change, and then the dusting of electrode material is caused to inactivate, causes the rapid decay of capacity.In addition to this, the poor electric conductivity of silicon itself So that silicon materials are difficult to play the advantage of height ratio capacity.Aiming at the problem that volume change existing for the silicium cathode and poorly conductive, It can be by the way that it be carried out with carbon material compound to improve its chemical property.Introducing carbon material not only can effectively improve silicon material The electric conductivity of material accelerates related electrochemical reaction dynamics；And carbon material can also serve as silicon materials and be embedded in lithium ion The buffer medium of volume expansion in journey avoids the dusting of active material silicon from inactivating, improves the cycle life of battery.
Carbon nanotube is a kind of one-dimensional carbon material with excellent draw ratio, can be cross-linked with each other in electrode whole interior, The electron-transport network for forming electronics high-speed transfer, greatly improves the electric conductivity of overall electrode, the carbon nanotube of internal crosslinking Introduce the cycle performance and high rate performance for significantly improving active material.
Summary of the invention
The object of the present invention is to provide a kind of silicon/carbon nanotube/cobalt composite material preparation method and applications, use is wet Method ball-milling method prepares silicon/melamine/nitric acid cobalt precursor, then is heat-treated to obtain silicon/carbon at high temperature, in inert atmosphere Nanotube/cobalt composite material, and then study its chemical property.The result shows that silicon/carbon nanotube/cobalt prepared by the present invention is multiple Condensation material shows stable cycle life and high rate performance.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of silicon/carbon nanotube/cobalt composite material preparation method, includes the following steps:
(1) wet ball grinding mixing silicon, melamine and nitric acid cobalt dust are used, silicon/melamine/nitric acid cobalt precursor is obtained；
In this step, wet ball grinding solvent for use selects dehydrated alcohol, and rotational speed of ball-mill is 300 ~ 600 r/min, Ball-milling Time control System is in 12 ~ 24 h；Silicon materials are nano silica fume, and average grain diameter is between 100 ~ 500 nm；Melamine/cobalt nitrate quality Than for 10:1, silicon/cobalt nitrate mass ratio is between 1:1 ~ 5:1；
(2) use inert gas (argon gas or nitrogen) as protective gas, from room temperature with the heating rate liter of 0.2 ~ 2 DEG C/min To 700 ~ 900 DEG C, high-temperature heat treatment silicon/melamine/2 ~ 6 h of nitric acid cobalt precursor, naturally cools to room with this condition Temperature obtains silicon/carbon nanotube/cobalt composite material.
Silicon/carbon nanotube/cobalt composite material that the above method is prepared can be used as cathode apply in lithium ion battery and In solid state battery.
Compared with the prior art, the present invention has the advantage that
1, carbon nanotube/cobalt introduces the electric conductivity that can effectively improve electrode, improves removal lithium embedded dynamics, plays silicium cathode The characteristics of height ratio capacity.
2, the introducing of carbon nanotube/cobalt can alleviate silicium cathode volume change during removal lithium embedded, avoid electrode material Dusting inactivation, improve the cyclical stability of battery.
3, composite material exhibits prepared by the present invention have gone out high reversible specific capacity and cyclical stability, are suitable for Fabrication of High Specific Capacitance Measure the preparation of lithium ion battery negative material.
Detailed description of the invention
Fig. 1 is silicon/carbon nanotube/cobalt composite material of the preparation of embodiment 1 in 0.5 A g-1Current density under circulation Performance map.
Fig. 2 is (cathode) silicon/carbon nanotube/cobalt | | cobalt acid lithium (anode) full battery is in 0.5 A g-1It is recycled under current density Performance map.
Specific embodiment
Below with reference to embodiment, further description of the technical solution of the present invention, and however, it is not limited to this, all right Technical solution of the present invention is modified or replaced equivalently, and without departing from the spirit and scope of the technical solution of the present invention, should all be contained Lid is within the protection scope of the present invention.
Embodiment 1
Silicon/carbon nanotube/cobalt composite material is prepared according to the following steps in the present embodiment:
(1) under normal temperature and pressure, 10 mL ethyl alcohol, 200 mg nano silica fumes, 200 mg cobalt nitrates and 2 are separately added into ball grinder G melamine, 12 h of ball milling under the revolving speed of 500 r/min obtain silicon/melamine/nitric acid cobalt precursor.
(2) under protecting obtained silicon/melamine/nitric acid cobalt precursor in a nitrogen atmosphere, 800 are raised to from room temperature DEG C, heating rate is 1 DEG C/min, and soaking time is 4 h, naturally cools to room temperature, obtains silicon/carbon nanotube/cobalt composite wood Material.
Silicon/carbon nanotube/cobalt composite material manufactured in the present embodiment is prepared into Electrode, use metallic lithium foil as Reference electrode and to electrode, investigates the chemical property of composite material, in 0.5 A g-1Current density under cycle performance As shown in Figure 1.From fig. 1, it can be seen that silicon/carbon nanotube/cobalt composite material manufactured in the present embodiment is in 0.5 A g-1Current density After lower 200 circle of circulation, specific discharge capacity is 1208 mAh/g, capacity retention ratio 91%, has shown high specific capacity and excellent Cyclical stability.
Chemical property figure of the silicon/carbon nanotube/cobalt composite material manufactured in the present embodiment in lithium ion full battery is such as Shown in Fig. 2.
Embodiment 2
Silicon/carbon nanotube/cobalt composite material is prepared according to the following steps in the present embodiment:
(1) under normal temperature and pressure, 10 mL ethyl alcohol, 1 g nano silica fume, 200 mg cobalt nitrates and 2 g are separately added into ball grinder Melamine, 12 h of ball milling under the revolving speed of 500 r/min obtain silicon/melamine/nitric acid cobalt precursor.
(2) under protecting obtained silicon/melamine/nitric acid cobalt precursor in a nitrogen atmosphere, 800 are raised to from room temperature DEG C, heating rate is 1 DEG C/min, and soaking time is 4 h, naturally cools to room temperature, obtains silicon/carbon nanotube/cobalt composite wood Material.
Embodiment 3
Silicon/carbon nanotube/cobalt composite material is prepared according to the following steps in the present embodiment:
(1) under normal temperature and pressure, 10 mL ethyl alcohol, 500 mg nano silica fumes, 200 mg cobalt nitrates and 2 are separately added into ball grinder G melamine, 12 h of ball milling under the revolving speed of 500 r/min obtain silicon/melamine/nitric acid cobalt precursor.
(2) under protecting obtained silicon/melamine/nitric acid cobalt precursor in a nitrogen atmosphere, 800 are raised to from room temperature DEG C, heating rate is 1 DEG C/min, and soaking time is 4 h, naturally cools to room temperature, obtains silicon/carbon nanotube/cobalt composite wood Material.
Embodiment 4
Silicon/carbon nanotube/cobalt composite material is prepared according to the following steps in the present embodiment:
(1) under normal temperature and pressure, 10 mL ethyl alcohol, 200 mg nano silica fumes, 200 mg cobalt nitrates and 2 are separately added into ball grinder G melamine, 12 h of ball milling under the revolving speed of 500 r/min obtain silicon/melamine/nitric acid cobalt precursor.
(2) under protecting obtained silicon/melamine/nitric acid cobalt precursor in a nitrogen atmosphere, 900 are raised to from room temperature DEG C, heating rate is 1 DEG C/min, and soaking time is 4 h, naturally cools to room temperature, obtains silicon/carbon nanotube/cobalt composite wood Material.
Embodiment 5
Silicon/carbon nanotube/cobalt composite material is prepared according to the following steps in the present embodiment:
(1) under normal temperature and pressure, 10 mL ethyl alcohol, 200 mg nano silica fumes, 200 mg cobalt nitrates and 2 are separately added into ball grinder G melamine, 12 h of ball milling under the revolving speed of 500 r/min obtain silicon/melamine/nitric acid cobalt precursor.
(2) under protecting obtained silicon/melamine/nitric acid cobalt precursor in a nitrogen atmosphere, 700 are raised to from room temperature DEG C, heating rate is 1 DEG C/min, and soaking time is 4 h, naturally cools to room temperature and obtains silicon/carbon nanotube/cobalt composite material.
Embodiment 6
Silicon/carbon nanotube/cobalt composite material is prepared according to the following steps in the present embodiment:
(1) under normal temperature and pressure, 10 mL ethyl alcohol, 200 mg nano silica fumes, 200 mg cobalt nitrates and 2 are separately added into ball grinder G melamine, 12 h of ball milling under the revolving speed of 500 r/min obtain silicon/melamine/nitric acid cobalt precursor.
(2) under protecting obtained silicon/melamine/nitric acid cobalt precursor in a nitrogen atmosphere, 800 are raised to from room temperature DEG C, heating rate is 1 DEG C/min, and soaking time is 12 h, naturally cools to room temperature and obtains silicon/carbon nanotube/cobalt composite wood Material.

Claims (7)

1. a kind of silicon/carbon nanotube/cobalt composite material preparation method, it is characterised in that described method includes following steps:
(1) wet ball grinding mixing silicon, melamine and nitric acid cobalt dust are used, silicon/melamine/nitric acid cobalt precursor is obtained, Control melamine/cobalt nitrate mass ratio is 10:1, and silicon/cobalt nitrate mass ratio is between 1:1 ~ 5:1；
(2) it uses inert gas as protective gas, is raised to 700 ~ 900 DEG C from room temperature with the heating rate of 0.5 ~ 2 DEG C/min, High-temperature heat treatment silicon/melamine/2 ~ 6 h of nitric acid cobalt precursor with this condition, naturally cools to room temperature, obtains silicon/carbon and receives Mitron/cobalt composite material.
2. silicon according to claim 1/carbon nanotube/cobalt composite material preparation method, it is characterised in that the wet process Ball milling solvent for use selects dehydrated alcohol.
3. silicon according to claim 1/carbon nanotube/cobalt composite material preparation method, it is characterised in that the ball milling Revolving speed is 300 ~ 600 r/min.
4. silicon according to claim 1/carbon nanotube/cobalt composite material preparation method, it is characterised in that the ball milling Time controls in 12 ~ 24 h.
5. silicon according to claim 1/carbon nanotube/cobalt composite material preparation method, it is characterised in that the silicon material Material is nano silica fume, and average grain diameter is between 100 ~ 500 nm.
6. silicon according to claim 1/carbon nanotube/cobalt composite material preparation method, it is characterised in that the inertia Gas is argon gas or nitrogen.
7. silicon/carbon nanotube/cobalt composite material of claim 1-6 any claim the method preparation is as cathode in lithium Application in ion battery and solid state battery.
CN201910477183.9A 2019-06-03 2019-06-03 A kind of silicon/carbon nanotube/cobalt composite material preparation method and applications Withdrawn CN110148736A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113860288A (en) * 2021-11-05 2021-12-31 中国人民解放军国防科技大学 Silicon-carbon nanotube composite negative electrode material and preparation method and application thereof
CN114639828A (en) * 2020-12-16 2022-06-17 南京大学 Multi-lamellar flower-shaped network structure silicon-carbon composite material and preparation method and application thereof

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KR100731922B1 (en) * 2006-04-28 2007-06-25 전자부품연구원 Composite nano material for secondary battery and fabricating method for the same
CN104617261A (en) * 2015-01-23 2015-05-13 东莞市翔丰华电池材料有限公司 Method for preparing composite cathode material of silicon-carbon nanotube of lithium ion battery
CN104934573A (en) * 2014-03-19 2015-09-23 苏州格瑞动力电源科技有限公司 In-situ solid-phase synthesis method of silicon-graphene spheroidal composite material with multilevel structure and application thereof
CN109244432A (en) * 2018-11-15 2019-01-18 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of silico-carbo nanometer tube composite materials and products thereof and application
CN109585801A (en) * 2018-10-16 2019-04-05 湖南宸宇富基新能源科技有限公司 A kind of carbon nano-tube filled silicon/hollow carbon compound cathode materials and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100731922B1 (en) * 2006-04-28 2007-06-25 전자부품연구원 Composite nano material for secondary battery and fabricating method for the same
CN104934573A (en) * 2014-03-19 2015-09-23 苏州格瑞动力电源科技有限公司 In-situ solid-phase synthesis method of silicon-graphene spheroidal composite material with multilevel structure and application thereof
CN104617261A (en) * 2015-01-23 2015-05-13 东莞市翔丰华电池材料有限公司 Method for preparing composite cathode material of silicon-carbon nanotube of lithium ion battery
CN109585801A (en) * 2018-10-16 2019-04-05 湖南宸宇富基新能源科技有限公司 A kind of carbon nano-tube filled silicon/hollow carbon compound cathode materials and preparation method thereof
CN109244432A (en) * 2018-11-15 2019-01-18 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of silico-carbo nanometer tube composite materials and products thereof and application

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114639828A (en) * 2020-12-16 2022-06-17 南京大学 Multi-lamellar flower-shaped network structure silicon-carbon composite material and preparation method and application thereof
CN114639828B (en) * 2020-12-16 2024-04-30 南京大学 Multi-sheet flower-like network structure silicon-carbon composite material and preparation method and application thereof
CN113860288A (en) * 2021-11-05 2021-12-31 中国人民解放军国防科技大学 Silicon-carbon nanotube composite negative electrode material and preparation method and application thereof

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