CN106099037B - A kind of high-performance electrode composite material and preparation method - Google Patents
A kind of high-performance electrode composite material and preparation method Download PDFInfo
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- CN106099037B CN106099037B CN201610595956.XA CN201610595956A CN106099037B CN 106099037 B CN106099037 B CN 106099037B CN 201610595956 A CN201610595956 A CN 201610595956A CN 106099037 B CN106099037 B CN 106099037B
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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
- H01M4/364—Composites as mixtures
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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
- H01M4/06—Electrodes for primary cells
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/06—Electrodes for primary cells
- H01M4/08—Processes of manufacture
Abstract
The invention discloses a kind of high-performance electrode composite material and preparation method, which is prepared by the raw material of following parts by weight: two oxalic acid hydrates are ferrous, and 90~100 parts；Lithium dihydrogen phosphate, 110~120 parts；Vanadic anhydride, 2~4 parts；Titanium dioxide, 1~3 part；Manganese dioxide, 2~4 parts；Copper oxide, 0.5~1.5 part；Lithium stearate, 0.5~1.5 part；Ferroso-ferric oxide, 1~3 part；The weight ratio of tricresyl phosphate and totally 7~9 parts of aluminium isopropoxide, tricresyl phosphate and aluminium isopropoxide is 6~8:1.The result shows that electrode composite material capacity provided by the invention is high, good cycle, and preparation process is easy, raw material sources are abundant, at low cost, safety and environmental protection, compared with prior art, has substantive distinguishing features outstanding and significant progress.
Description
Technical field
The invention belongs to field of compound material, and in particular to a kind of high-performance electrode composite material and preparation method.
Background technique
With social development, energy and material increasingly highlights its critical role.
Develop that a kind of preparation process is easy, raw material sources are abundant, at low cost, safety and environmental protection, capacity are high, good cycle
High performance electrode material be always field of energy source materials scientific worker make great efforts target.
Summary of the invention
The first object of the present invention is to provide a kind of high-performance electrode composite material；
The second object of the present invention is to provide the preparation method of above-mentioned electrode composite material.
Above-mentioned purpose of the invention is achieved by following technical solution:
A kind of high-performance electrode composite material, is prepared by the raw material of following parts by weight: two oxalic acid hydrates are ferrous, and 90
~100 parts；Lithium dihydrogen phosphate, 110~120 parts；Vanadic anhydride, 2~4 parts；Titanium dioxide, 1~3 part；Manganese dioxide, 2~4
Part；Copper oxide, 0.5~1.5 part；Lithium stearate, 0.5~1.5 part；Ferroso-ferric oxide, 1~3 part；Tricresyl phosphate and isopropyl
Totally 7~9 parts of aluminium alcoholates, the weight ratio of tricresyl phosphate and aluminium isopropoxide is 6~8:1.
Further, the high-performance electrode composite material is prepared by the raw material of following parts by weight: two hydrations
Ferrous oxalate, 95 parts；Lithium dihydrogen phosphate, 115 parts；Vanadic anhydride, 3 parts；Titanium dioxide, 2 parts；Manganese dioxide, 3 parts；Oxidation
Copper, 1 part；Lithium stearate, 1 part；Ferroso-ferric oxide, 2 parts；Tricresyl phosphate and totally 8 parts of aluminium isopropoxide, tricresyl phosphate and
The weight ratio of aluminium isopropoxide is 7:1.
Further, the high-performance electrode composite material is prepared by the raw material of following parts by weight: two hydrations
Ferrous oxalate, 90 parts；Lithium dihydrogen phosphate, 110 parts；Vanadic anhydride, 2 parts；Titanium dioxide, 1 part；Manganese dioxide, 2 parts；Oxidation
Copper, 0.5 part；Lithium stearate, 0.5 part；Ferroso-ferric oxide, 1 part；Tricresyl phosphate and totally 7 parts of aluminium isopropoxide, tricresol phosphate
The weight ratio of ester and aluminium isopropoxide is 6:1.
Further, the high-performance electrode composite material is prepared by the raw material of following parts by weight: two hydrations
Ferrous oxalate, 100 parts；Lithium dihydrogen phosphate, 120 parts；Vanadic anhydride, 4 parts；Titanium dioxide, 3 parts；Manganese dioxide, 4 parts；Oxidation
Copper, 1.5 parts；Lithium stearate, 1.5 parts；Ferroso-ferric oxide, 3 parts；Tricresyl phosphate and totally 9 parts of aluminium isopropoxide, tricresol phosphate
The weight ratio of ester and aluminium isopropoxide is 8:1.
The preparation method of above-mentioned high-performance electrode composite material, includes the following steps:
Step S1 carries out ball milling mixing to raw material using three-dimensional high-speed concussion ball mill, forms raw material mixed uniformly
Powder；
Step S2 calcines the mixed-powder after ball milling under nitrogen protection effect, and calcination temperature is 600~800
℃。
Further, step S1 specifically: ball milling mixing, ball grinder are carried out to raw material using three-dimensional high-speed concussion ball mill
Interior ball load is no more than the one third of tank total volume, and raw material total amount is no more than the one third of tank total volume, Ball-milling Time
It is 2 hours, shimmy frequency is 1000 revs/min.
Further, step S2 specifically: high temperature sintering is carried out using dual temperature area rotary furnace to the mixed-powder after ball milling,
2 revs/min of boiler tube revolving speed of setting, intermittent time are 1 minute, are first led to nitrogen 30 minutes before sintering, nitrogen flow rate is standard state
Lower 0.14L/min is passed through pure nitrogen gas in sintering process and is protected, nitrogen flow 0.05L/min, and sintering temperature is 800 DEG C,
The electrode composite material of pure phase is obtained after sintering.
Advantages of the present invention:
Electrode composite material preparation process provided by the invention is easy, raw material sources are abundant, at low cost, safety and environmental protection, appearance
Amount is high, good cycle, has substantive distinguishing features outstanding and significant progress.
Specific embodiment
Essentiality content of the invention is further illustrated below with reference to embodiment, but present invention protection model is not limited with this
It encloses.Although the invention is described in detail with reference to the preferred embodiments, those skilled in the art should understand that, it can be right
Technical solution of the present invention is modified or replaced equivalently, without departing from the spirit and scope of technical solution of the present invention.
Embodiment 1: the preparation of electrode composite material
Parts by weight of raw materials ratio:
Two oxalic acid hydrates are ferrous, and 95 parts；Lithium dihydrogen phosphate, 115 parts；Vanadic anhydride, 3 parts；Titanium dioxide, 2 parts；Dioxy
Change manganese, 3 parts；Copper oxide, 1 part；Lithium stearate, 1 part；Ferroso-ferric oxide, 2 parts；Tricresyl phosphate and totally 8 parts of aluminium isopropoxide,
The weight ratio of tricresyl phosphate and aluminium isopropoxide is 7:1.
Preparation method:
Step S1 carries out ball milling mixing to raw material using three-dimensional high-speed concussion ball mill, and ball load is no more than in ball grinder
Tank total volume one third, raw material total amount be no more than tank total volume one third, ball milling 2 hours, shimmy frequency be 1000 turns/
Minute；
Step S2 carries out high temperature sintering using dual temperature area rotary furnace to the mixed-powder after ball milling, sets boiler tube revolving speed 2
Rev/min, the intermittent time is 1 minute, is first led to nitrogen 30 minutes before sintering, and nitrogen flow rate is 0.14L/min under standard state, is burnt
It is passed through pure nitrogen gas during knot to be protected, nitrogen flow 0.05L/min, sintering temperature is 800 DEG C, is sintered to obtain the final product.
Embodiment 2: the preparation of electrode composite material
Parts by weight of raw materials ratio:
Two oxalic acid hydrates are ferrous, and 90 parts；Lithium dihydrogen phosphate, 110 parts；Vanadic anhydride, 2 parts；Titanium dioxide, 1 part；Dioxy
Change manganese, 2 parts；Copper oxide, 0.5 part；Lithium stearate, 0.5 part；Ferroso-ferric oxide, 1 part；Tricresyl phosphate and aluminium isopropoxide totally 7
Part, the weight ratio of tricresyl phosphate and aluminium isopropoxide is 6:1.
Preparation method:
Step S1 carries out ball milling mixing to raw material using three-dimensional high-speed concussion ball mill, and ball load is no more than in ball grinder
Tank total volume one third, raw material total amount be no more than tank total volume one third, ball milling 2 hours, shimmy frequency be 1000 turns/
Minute；
Step S2 carries out high temperature sintering using dual temperature area rotary furnace to the mixed-powder after ball milling, sets boiler tube revolving speed 2
Rev/min, the intermittent time is 1 minute, is first led to nitrogen 30 minutes before sintering, and nitrogen flow rate is 0.14L/min under standard state, is burnt
It is passed through pure nitrogen gas during knot to be protected, nitrogen flow 0.05L/min, sintering temperature is 800 DEG C, is sintered to obtain the final product.
Embodiment 3: the preparation of electrode composite material
Parts by weight of raw materials ratio:
Two oxalic acid hydrates are ferrous, and 100 parts；Lithium dihydrogen phosphate, 120 parts；Vanadic anhydride, 4 parts；Titanium dioxide, 3 parts；Two
Manganese oxide, 4 parts；Copper oxide, 1.5 parts；Lithium stearate, 1.5 parts；Ferroso-ferric oxide, 3 parts；Tricresyl phosphate and aluminium isopropoxide
Totally 9 parts, the weight ratio of tricresyl phosphate and aluminium isopropoxide is 8:1.
Preparation method:
Step S1 carries out ball milling mixing to raw material using three-dimensional high-speed concussion ball mill, and ball load is no more than in ball grinder
Tank total volume one third, raw material total amount be no more than tank total volume one third, ball milling 2 hours, shimmy frequency be 1000 turns/
Minute；
Step S2 carries out high temperature sintering using dual temperature area rotary furnace to the mixed-powder after ball milling, sets boiler tube revolving speed 2
Rev/min, the intermittent time is 1 minute, is first led to nitrogen 30 minutes before sintering, and nitrogen flow rate is 0.14L/min under standard state, is burnt
It is passed through pure nitrogen gas during knot to be protected, nitrogen flow 0.05L/min, sintering temperature is 800 DEG C, is sintered to obtain the final product.
Embodiment 4: the preparation of electrode composite material
Parts by weight of raw materials ratio:
Two oxalic acid hydrates are ferrous, and 95 parts；Lithium dihydrogen phosphate, 115 parts；Vanadic anhydride, 3 parts；Titanium dioxide, 2 parts；Dioxy
Change manganese, 3 parts；Copper oxide, 1 part；Lithium stearate, 1 part；Ferroso-ferric oxide, 2 parts；Tricresyl phosphate and totally 8 parts of aluminium isopropoxide,
The weight ratio of tricresyl phosphate and aluminium isopropoxide is 6:1.
Preparation method:
Step S1 carries out ball milling mixing to raw material using three-dimensional high-speed concussion ball mill, and ball load is no more than in ball grinder
Tank total volume one third, raw material total amount be no more than tank total volume one third, ball milling 2 hours, shimmy frequency be 1000 turns/
Minute；
Step S2 carries out high temperature sintering using dual temperature area rotary furnace to the mixed-powder after ball milling, sets boiler tube revolving speed 2
Rev/min, the intermittent time is 1 minute, is first led to nitrogen 30 minutes before sintering, and nitrogen flow rate is 0.14L/min under standard state, is burnt
It is passed through pure nitrogen gas during knot to be protected, nitrogen flow 0.05L/min, sintering temperature is 800 DEG C, is sintered to obtain the final product.
Embodiment 5: the preparation of electrode composite material
Parts by weight of raw materials ratio:
Two oxalic acid hydrates are ferrous, and 95 parts；Lithium dihydrogen phosphate, 115 parts；Vanadic anhydride, 3 parts；Titanium dioxide, 2 parts；Dioxy
Change manganese, 3 parts；Copper oxide, 1 part；Lithium stearate, 1 part；Ferroso-ferric oxide, 2 parts；Tricresyl phosphate and totally 8 parts of aluminium isopropoxide,
The weight ratio of tricresyl phosphate and aluminium isopropoxide is 8:1.
Preparation method:
Step S1 carries out ball milling mixing to raw material using three-dimensional high-speed concussion ball mill, and ball load is no more than in ball grinder
Tank total volume one third, raw material total amount be no more than tank total volume one third, ball milling 2 hours, shimmy frequency be 1000 turns/
Minute；
Step S2 carries out high temperature sintering using dual temperature area rotary furnace to the mixed-powder after ball milling, sets boiler tube revolving speed 2
Rev/min, the intermittent time is 1 minute, is first led to nitrogen 30 minutes before sintering, and nitrogen flow rate is 0.14L/min under standard state, is burnt
It is passed through pure nitrogen gas during knot to be protected, nitrogen flow 0.05L/min, sintering temperature is 800 DEG C, is sintered to obtain the final product.
Embodiment 6: comparative example
Parts by weight of raw materials ratio:
Two oxalic acid hydrates are ferrous, and 95 parts；Lithium dihydrogen phosphate, 115 parts；Vanadic anhydride, 3 parts；Titanium dioxide, 2 parts；Dioxy
Change manganese, 3 parts；Copper oxide, 1 part；Lithium stearate, 1 part；Ferroso-ferric oxide, 2 parts；Tricresyl phosphate and totally 8 parts of aluminium isopropoxide,
The weight ratio of tricresyl phosphate and aluminium isopropoxide is 5:1.
Preparation method:
Step S1 carries out ball milling mixing to raw material using three-dimensional high-speed concussion ball mill, and ball load is no more than in ball grinder
Tank total volume one third, raw material total amount be no more than tank total volume one third, ball milling 2 hours, shimmy frequency be 1000 turns/
Minute；
Step S2 carries out high temperature sintering using dual temperature area rotary furnace to the mixed-powder after ball milling, sets boiler tube revolving speed 2
Rev/min, the intermittent time is 1 minute, is first led to nitrogen 30 minutes before sintering, and nitrogen flow rate is 0.14L/min under standard state, is burnt
It is passed through pure nitrogen gas during knot to be protected, nitrogen flow 0.05L/min, sintering temperature is 800 DEG C, is sintered to obtain the final product.
Embodiment 7: comparative example
Parts by weight of raw materials ratio:
Two oxalic acid hydrates are ferrous, and 95 parts；Lithium dihydrogen phosphate, 115 parts；Vanadic anhydride, 3 parts；Titanium dioxide, 2 parts；Dioxy
Change manganese, 3 parts；Copper oxide, 1 part；Lithium stearate, 1 part；Ferroso-ferric oxide, 2 parts；Tricresyl phosphate and totally 8 parts of aluminium isopropoxide,
The weight ratio of tricresyl phosphate and aluminium isopropoxide is 9:1.
Preparation method:
Step S1 carries out ball milling mixing to raw material using three-dimensional high-speed concussion ball mill, and ball load is no more than in ball grinder
Tank total volume one third, raw material total amount be no more than tank total volume one third, ball milling 2 hours, shimmy frequency be 1000 turns/
Minute；
Step S2 carries out high temperature sintering using dual temperature area rotary furnace to the mixed-powder after ball milling, sets boiler tube revolving speed 2
Rev/min, the intermittent time is 1 minute, is first led to nitrogen 30 minutes before sintering, and nitrogen flow rate is 0.14L/min under standard state, is burnt
It is passed through pure nitrogen gas during knot to be protected, nitrogen flow 0.05L/min, sintering temperature is 800 DEG C, is sintered to obtain the final product.
Embodiment 8: effect example
The meso-position radius of the electrode composite material of Examples 1 to 7 preparation is 2.8~3.2 μm, and particle size is moderate.
First discharge specific capacity and fade performance are as follows: under 1C discharge-rate
| First discharge specific capacity | Attenuation percentage after circulation 300 times | |
| Embodiment 1 | 168.8mAh/g | Basically no attenuation |
| Embodiment 2 | 165.6mAh/g | Basically no attenuation |
| Embodiment 3 | 164.7mAh/g | Basically no attenuation |
| Embodiment 4 | 165.3mAh/g | Basically no attenuation |
| Embodiment 5 | 164.9mAh/g | Basically no attenuation |
| Embodiment 6 | 125.5mAh/g | 23% |
| Embodiment 7 | 131.4mAh/g | 21% |
The above results show that electrode composite material capacity provided by the invention is high, good cycle, and preparation process letter
Just, raw material sources are abundant, at low cost, safety and environmental protection, compared with prior art, have substantive distinguishing features outstanding and significantly into
Step.
The effect of above-described embodiment indicates that essentiality content of the invention, but protection of the invention is not limited with this
Range.Those skilled in the art should understand that can with modification or equivalent replacement of the technical solution of the present invention are made,
Without departing from the essence and protection scope of technical solution of the present invention.
Claims (2)
1. a kind of high-performance electrode composite material, it is characterised in that:
Be made up of the raw material of following parts by weight: two oxalic acid hydrates are ferrous, and 95 parts；Lithium dihydrogen phosphate, 115 parts；Vanadic anhydride,
3 parts；Titanium dioxide, 2 parts；Manganese dioxide, 3 parts；Copper oxide, 1 part；Lithium stearate, 1 part；Ferroso-ferric oxide, 2 parts；Tripotassium phosphate
The weight ratio of phenolic ester and totally 8 parts of aluminium isopropoxide, tricresyl phosphate and aluminium isopropoxide is 7:1；
Or be made up of the raw material of following parts by weight: two oxalic acid hydrates are ferrous, 90 parts；Lithium dihydrogen phosphate, 110 parts；Five oxidations two
Vanadium, 2 parts；Titanium dioxide, 1 part；Manganese dioxide, 2 parts；Copper oxide, 0.5 part；Lithium stearate, 0.5 part；Ferroso-ferric oxide, 1 part；
The weight ratio of tricresyl phosphate and totally 7 parts of aluminium isopropoxide, tricresyl phosphate and aluminium isopropoxide is 6:1；
Or be made up of the raw material of following parts by weight: two oxalic acid hydrates are ferrous, 100 parts；Lithium dihydrogen phosphate, 120 parts；Five oxidations two
Vanadium, 4 parts；Titanium dioxide, 3 parts；Manganese dioxide, 4 parts；Copper oxide, 1.5 parts；Lithium stearate, 1.5 parts；Ferroso-ferric oxide, 3 parts；
The weight ratio of tricresyl phosphate and totally 9 parts of aluminium isopropoxide, tricresyl phosphate and aluminium isopropoxide is 8:1.
2. the preparation method of high-performance electrode composite material described in a kind of claim 1, which comprises the steps of:
Step S1 carries out ball milling mixing to raw material using three-dimensional high-speed concussion ball mill, raw material is made to form mixed uniformly powder；
Step S2 calcines the mixed-powder after ball milling under nitrogen protection effect, and calcination temperature is 600~800 DEG C；
Wherein, step S1 specifically: ball milling mixing, ball load in ball grinder are carried out to raw material using three-dimensional high-speed concussion ball mill
No more than the one third of tank total volume, raw material total amount is no more than the one third of tank total volume, and Ball-milling Time is 2 hours,
Shimmy frequency is 1000 revs/min；Step S2 specifically: high temperature is carried out using dual temperature area rotary furnace to the mixed-powder after ball milling
Sintering sets 2 revs/min of boiler tube revolving speed, and the intermittent time is 1 minute, is first led to nitrogen 30 minutes before sintering, nitrogen flow rate is standard
0.14L/min under state is passed through pure nitrogen gas in sintering process and is protected, nitrogen flow 0.05L/min, and sintering temperature is
800 DEG C, the electrode composite material of pure phase is obtained after sintering.
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| CN105047879A (en) * | 2015-07-17 | 2015-11-11 | 河北省科学院能源研究所 | Composite electrode material and preparation method thereof |
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| WO2012081543A1 (en) * | 2010-12-14 | 2012-06-21 | 協立化学産業株式会社 | Battery electrode or separator surface protective agent, battery electrode or separator protected by same, and battery having battery electrode or separator |
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Effective date of registration: 20190801 Address after: 523000 Guangcheng Street Venture Community, Dongguan City, Guangdong Province 1309 Baida Center Office Building, No. 9 Guantai Road Patentee after: Dongguan Tianzheng Enterprise Management Consulting Co., Ltd. Address before: 523112 Guangdong province Dongguan City Bridge Village Yinzhu road Dongcheng District Dongcheng Street No. 26 Patentee before: Dongguan Crystal New Material Technology Co., Ltd. |