CN110459748A - A kind of carbon coating ferrous acid lithium material and preparation method thereof - Google Patents
A kind of carbon coating ferrous acid lithium material and preparation method thereof Download PDFInfo
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- CN110459748A CN110459748A CN201910769367.2A CN201910769367A CN110459748A CN 110459748 A CN110459748 A CN 110459748A CN 201910769367 A CN201910769367 A CN 201910769367A CN 110459748 A CN110459748 A CN 110459748A
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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
- 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
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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
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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
- H01M4/52—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
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- 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 present invention relates to lithium battery anodes to mend lithium material technical field, discloses a kind of preparation method of carbon coating ferrous acid lithium material, method includes the following steps: (1) mixes source of iron and lithium source, sintering, obtain ferrous acid lithium, wherein the molar ratio of lithium source and source of iron is 5-25:1；(2) ferrous acid lithium obtained in step (1) is crushed；(3) ferrous acid lithium smashed in step (2) is subjected to gas phase cladding with carbon source, obtains carbon coating ferrous acid lithium material.The carbon coating ferrous acid lithium material of method preparation can effectively make up the active lithium lost during lithium battery first charge-discharge through the invention, external environment can be completely cut off simultaneously, the water or carbon dioxide exposure in ferrous acid lithium and air are avoided, the stability of carbon coating ferrous acid lithium material is improved.Carbon coating ferrous acid lithium material of the present invention is used to prepare lithium battery, lithium battery first charge-discharge specific capacity can be improved, improves first charge-discharge efficiency.
Description
Technical field
The present invention relates to lithium battery anodes to mend lithium material technical field, and in particular to a kind of carbon coating ferrous acid lithium material and its
Preparation method.
Background technique
Lithium ion battery can generate one layer of boundary layer containing lithium (SEI), the boundary in negative terminal surface during first charge-discharge
Face has the property of solid-state electrolytic solution, most important for the performance of performance of lithium ion battery.SEI film has organic solvent insoluble
Property, it can be stabilized in organic electrolyte, can effectively prevent the total insertion of solvent molecule, to improve the cyclicity of electrode
Energy and service life.However, the formation of SEI can consume the active lithium in battery, lead to the loss of battery reversible capacity.Currently,
Commercialized graphite cathode head effect is usually 90% or so, and the higher silicon based anode material head effect of specific capacity is smaller, usually
85% or so is even lower.
In order to make up the active lithium lost during first charge-discharge, at present the technology of mainstream include anode mend lithium technique and
Cathode mends two kinds of lithium technique.From technical maturity, it is currently undertaken by metal Li powder, Li foil mends lithium associated materials and equipment is raw
It produces, and the producer of benefit lithium technical study is more, industrial maturity is higher.But cathode mends requirement of the lithium to equipment and environment
Higher, safety is also difficult to ensure.As a comparison, the safety of anode benefit lithium technique is good, does not have shadow to existing production technology
It rings.Currently, be engaged in anode mend lithium material research producer and scientific research institution it is relatively fewer, about the related preparation for mending lithium material,
Improvement that is modified and mending lithium technique still requires study.
For ferrous acid lithium as a kind of rich lithium material, theoretical specific capacity 867mAh/g, operating voltage is moderate, raw after first charge-discharge
At inert substance be not involved in subsequent electrochemical process, be it is a kind of it is ideal anode mend lithium additive.
Summary of the invention
The purpose of the invention is to overcome ferrous acid lithium of the existing technology to be easy and the moisture and dioxy in environment
The problem of changing carbon reaction, provides a kind of carbon coating ferrous acid lithium material and preparation method thereof, the iron in the carbon coating ferrous acid lithium material
Sour lithium is a kind of ideal anode benefit lithium additive, while amorphous carbon layer can completely cut off external environment, avoid ferrous acid lithium and sky
Water or carbon dioxide exposure in gas, improve the stability of material.
To achieve the goals above, one aspect of the present invention provides a kind of preparation method of carbon coating ferrous acid lithium material, should
Method the following steps are included:
(1) source of iron and lithium source are mixed, sintering obtains ferrous acid lithium, wherein the molar ratio of lithium source and source of iron is 5-25:1；
(2) ferrous acid lithium obtained in step (1) is crushed；
(3) ferrous acid lithium smashed in step (2) is subjected to gas phase cladding with carbon source, obtains carbon coating ferrous acid lithium material.
Preferably, in step (1), the source of iron is di-iron trioxide, ferroso-ferric oxide, FeOOH, ferric nitrate
With one of ironic citrate or a variety of.
Preferably, in step (1), the lithium source is one of lithium carbonate, monohydrate lithium hydroxide and lithia or more
Kind.
Preferably, in step (1), the sintering process are as follows: source of iron, lithium source mixture are placed in sintering furnace, in nitrogen
Under gas shielded, sintering temperature is warming up to preset heating rate and is sintered.
Preferably, the preset heating rate is 1-10 DEG C/min.
Preferably, the sintering temperature is 650-1000 DEG C；The sintering time is 3-72h.
Preferably, in step (2), it is 2-50 μm that the ferrous acid lithium, which is crushed to average grain diameter,.
Preferably, in step (3), the carbon source be one of methane, ethane, propane, ethylene, acetylene and butylene or
It is a variety of.
Preferably, in step (3), the gas phase coats process are as follows: smashed ferrous acid lithium is placed in CVD rotary furnace
It is warming up to preset temperature, carbon source is passed through with preset flow, stops being passed through carbon source after gas phase cladding is carried out under preset temperature, cool down
After obtain carbon coating ferrous acid lithium material.
Preferably, the default temperature of plate is 600-800 DEG C.
Preferably, the preset flow is 2.5-7mL/min.
Preferably, the gas phase cladding time is 2-8h.
Another aspect of the present invention provides a kind of carbon coating ferrous acid lithium material prepared by previously described method.
Preferably, the content of carbon is 0.5-5 weight % in the carbon coating ferrous acid lithium material.
The carbon coating ferrous acid lithium material of method preparation can effectively make up lithium battery and fill for the first time through the invention
The active lithium lost in discharge process, while external environment can be completely cut off, avoid water or carbon dioxide in ferrous acid lithium and air
Contact improves the stability of carbon coating ferrous acid lithium material.Carbon coating ferrous acid lithium material of the present invention is used to prepare lithium electricity
Lithium battery first charge-discharge specific capacity can be improved in pond, improves first charge-discharge efficiency.
Detailed description of the invention
Fig. 1 is the stereoscan photograph of the carbon coating ferrous acid lithium material prepared in embodiment 1.
Specific embodiment
Below in conjunction with attached drawing, detailed description of the preferred embodiments.It should be understood that this place is retouched
The specific embodiment stated is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or
Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively
It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more
New numberical range, these numberical ranges should be considered as specific open herein.
One aspect of the present invention provides a kind of preparation method of carbon coating ferrous acid lithium material, method includes the following steps:
(1) source of iron and lithium source are mixed, sintering obtains ferrous acid lithium, wherein the molar ratio of lithium source and source of iron is 5-25:1；
(2) ferrous acid lithium obtained in step (1) is crushed；
(3) ferrous acid lithium smashed in step (2) is subjected to gas phase cladding with carbon source, obtains carbon coating ferrous acid lithium material.
Ferrous acid lithium advantages of good crystallization in the carbon coating ferrous acid lithium material of method preparation through the invention, no miscellaneous phase, energy
It is enough effectively to make up the active lithium lost during lithium battery first charge-discharge, and the amorphous carbon layer of ferrous acid lithium surface covering
External environment can be completely cut off, avoid water or carbon dioxide exposure in ferrous acid lithium and air, improve carbon coating ferrous acid lithium material
Stability.
In method of the present invention, in step (1), the source of iron can be the conventional selection of this field, specifically
Ground, the source of iron are di-iron trioxide (Fe2O3), ferroso-ferric oxide (Fe3O4), FeOOH (FeOOH), ferric nitrate and lemon
One of lemon acid iron is a variety of, and under preferable case, the source of iron is di-iron trioxide.
In method of the present invention, in step (1), the lithium source can be the conventional selection of this field, specifically
Ground, the lithium source are lithium carbonate (Li2CO3), monohydrate lithium hydroxide (LiOHH2O), lithia (Li2O one of) or more
Kind, under preferable case, the lithium source is LiOHH2O。
In order to guarantee that source of iron and lithium source can sinter the ferrous acid lithium with high-crystallinity into, rubbing lithium source and source of iron is needed
You are than controlling in suitable range.In method of the present invention, in step (1), the lithium source and the source of iron
Molar ratio can be 5-25:1, specifically, such as can be 5:1,10:1,15:1,20:1 or 25:1, it is preferable that in step (1)
In, the molar ratio of the lithium source and the source of iron can be 15:1.
In method of the present invention, in step (1), the sintering process are as follows: be placed in source of iron, lithium source mixture
In sintering furnace, under nitrogen protection, sintering temperature is warming up to preset heating rate and is sintered.
In the sintering process, the sintering furnace is the conventional selection of this field, and under preferable case, the sintering furnace is
Batch-type furnace.The preset heating rate be 1-10 DEG C/min, specifically, for example, can for 1 DEG C/min, 2 DEG C/min, 3 DEG C/min,
4 DEG C/min, 5 DEG C/min, 6 DEG C/min, 7 DEG C/min, 8 DEG C/min, 9 DEG C/min or 10 DEG C/min, it is preferable that the default heating
Speed is 5 DEG C/min.The sintering temperature is 650-1000 DEG C, specifically, such as can be 650 DEG C, 700 DEG C, 750 DEG C, 800
DEG C, 850 DEG C, 900 DEG C, 950 DEG C or 1000 DEG C, under preferable case, the sintering temperature be 800 DEG C.The sintering time is 3-
72h, it is preferable that the sintering time is 10-60h, it is highly preferred that the sintering time is 20-50h.
In method of the present invention, in step (2), it is 2-50 μm that the ferrous acid lithium, which is crushed to average grain diameter,；
It specifically, such as can be 2 μm, 5 μm, 10 μm, 15 μm, 20 μm, 25 μm, 30 μm, 35 μm, 40 μm, 45 μm or 50 μm；It is preferred that
Ground, in step (2), it is 25 μm that the ferrous acid lithium, which is crushed to average grain diameter,.
In order to improve amorphous carbon layer in the coating efficiency on ferrous acid lithium surface, in step (3), the carbon source is gas-phase carbon
Source, specifically, the gas phase carbon source are one of methane, ethane, propane, ethylene, acetylene and butylene or a variety of, it is preferable that
The gas phase carbon source is methane, ethylene or acetylene.
In method of the present invention, in step (3), the gas phase coats process are as follows: by smashed ferrous acid lithium
It is placed in CVD rotary furnace and is warming up to preset temperature, carbon source is passed through with preset flow, stop after carrying out gas phase cladding under preset temperature
It is only passed through carbon source, carbon coating ferrous acid lithium material is obtained after cooling.
During gas phase cladding, the CVD rotary furnace is produced by Xianyang Research & Design Institute of Ceramics, model KY-
R-SJQ3.The default temperature of plate is 600-800 DEG C, specifically, such as can for 600 DEG C, 650 DEG C, 700 DEG C, 750 DEG C or
800 DEG C, under preferable case, the default temperature of plate is 750 DEG C.The preset flow is 2.5-7mL/min, specifically, example
It such as can be 2.5mL/min, 3mL/min, 3.5mL/min, 4mL/min, 4.5mL/min, 5mL/min, 5.5mL/min, 6mL/
Min, 6.5mL/min or 7mL/min, under preferable case, the preset flow is 5mL/min.The gas phase cladding time is 2-
8h specifically, such as can be 2,3,4,5,6,7 or 8h, and under preferable case, the gas phase cladding time is 3h.
Another aspect of the present invention provides a kind of carbon coating ferrous acid lithium material prepared by previously described method.The carbon packet
Covering ferrous acid lithium material is a kind of good anode benefit lithium material.
In order to guarantee that amorphous carbon layer can avoid the water or carbon dioxide exposure in ferrous acid lithium and air, ferrous acid lithium completely
The amorphous carbon layer covering amount on surface must be enough, and the content of carbon should meet certain requirement in carbon coating ferrous acid lithium material.
Preferably, the content of carbon is 0.5-5 weight % in the carbon coating ferrous acid lithium material, it is highly preferred that the carbon coating ferrous acid lithium
The content of carbon is 1.5-5 weight % in material, it is further preferred that the content of carbon is 3-5 in the carbon coating ferrous acid lithium material
Weight %.
The carbon coating ferrous acid lithium material of method preparation can effectively make up lithium battery and fill for the first time through the invention
The active lithium lost in discharge process, while external environment can be completely cut off, avoid water or carbon dioxide in ferrous acid lithium and air
Contact improves the stability of carbon coating ferrous acid lithium material.Carbon coating ferrous acid lithium material of the present invention is used to prepare lithium electricity
Lithium battery first charge-discharge specific capacity can be improved in pond, improves first charge-discharge efficiency.
The present invention will be described in detail by way of examples below, but scope of protection of the present invention is not limited thereto.
Embodiment 1
By 232.2g LiOHH2O and 30g Fe2O3It is uniformly mixed, obtained mixture is put into van-type furnace, in nitrogen
Protection under, 850 DEG C of sintering 36h are warming up to 5 DEG C/min heating rate, will the obtained ferrous acid lithium of sintering crush after be put into CVD
It is warming up to 800 DEG C in rotary furnace, is passed through methane gas, the flow that control is passed through methane gas is 2.5mL/min, gas at 800 DEG C
Mutually stop being passed through methane gas after cladding 3h, after cooling, (the scanning of carbon coating ferrous acid lithium material of carbon coating ferrous acid lithium material is made
Electromicroscopic photograph is as shown in Figure 1).
Embodiment 2
By 271.3g Li2CO3With 50g Fe2O3It is uniformly mixed, obtained mixture is put into van-type furnace, in the guarantor of nitrogen
Under shield, 1000 DEG C of sintering 72h are warming up to 1 DEG C/min heating rate, CVD revolution is put into after the ferrous acid lithium that sintering obtains is crushed
It is warming up to 700 DEG C in furnace, is passed through acetylene gas, the flow that control is passed through acetylene gas is 5mL/min, and gas phase coats at 700 DEG C
Stop being passed through acetylene gas after 2h, after cooling, carbon coating ferrous acid lithium material is made.
Embodiment 3
By 84.9g LiOHH2O, 29.7g FeOOH is uniformly mixed, and obtained mixture is put into van-type furnace, in nitrogen
Protection under, 900 DEG C of sintering 48h are warming up to 10 DEG C/min heating rate, will the obtained ferrous acid lithium of sintering crush after be put into CVD
It is warming up to 750 DEG C in rotary furnace, is passed through ethylene gas, the flow that control is passed through ethylene gas is 7mL/min, gas phase at 750 DEG C
Stop being passed through ethylene gas after cladding 5h, after cooling, carbon coating ferrous acid lithium material is made.
Comparative example 1
According to method described in embodiment 1 prepare carbon coating ferrous acid lithium material, unlike, smashed ferrous acid lithium not into
Promoting the circulation of qi mutually coats.
Comparative example 2
Carbon coating ferrous acid lithium material is prepared according to method described in embodiment 1, unlike, with 5 DEG C/min heating rate
It is warming up to 500 DEG C of sintering for 24 hours.
Test case
The carbon coating ferrous acid lithium material of the middle preparation of embodiment 1-3 and comparative example 1-2 is prepared into lithium ion battery and is examined
It surveys, detecting step is as follows: carbon coating ferrous acid lithium, Super-P and PVDF is dispersed in NMP according to mass ratio 8:1:1, control
Solid content is 40% or so, after Defoaming machine is uniformly dispersed, be coated in aluminium foil on, vacuum drying, be made anode pole piece after
The assembly of 2025 battery of button is carried out in glove box, electrolyte is the LiPF of 1.2mol/L6, wherein solvent volume ratio is EC:EMC=
3:7, diaphragm are Celgard polypropylene screen, use metal lithium sheet for electrode.By the half-cell assembled on new prestige tester
Volume test is carried out, charging is 4.5V, discharge cut-off voltage 2.0V, charge-discharge magnification 0.05C, test result by voltage
As shown in table 1.
Table 1
It can be seen that the carbon coating ferrous acid lithium material prepared using technical solutions according to the invention by the result of table 1
After being prepared into lithium battery, first charge-discharge specific capacity is significantly increased, and first charge-discharge efficiency also increases.
The preferred embodiment of the present invention has been described above in detail, and still, the present invention is not limited thereto.In skill of the invention
In art conception range, can with various simple variants of the technical solution of the present invention are made, including each technical characteristic with it is any its
Its suitable method is combined, and it should also be regarded as the disclosure of the present invention for these simple variants and combination, is belonged to
Protection scope of the present invention.
Claims (10)
1. a kind of preparation method of carbon coating ferrous acid lithium material, which is characterized in that method includes the following steps:
(1) source of iron and lithium source are mixed, sintering obtains ferrous acid lithium, wherein the molar ratio of lithium source and source of iron is 5-25:1；
(2) ferrous acid lithium obtained in step (1) is crushed；
(3) ferrous acid lithium smashed in step (2) is subjected to gas phase cladding with carbon source, obtains carbon coating ferrous acid lithium material.
2. the method according to claim 1, wherein the source of iron is di-iron trioxide, four in step (1)
One of Fe 3 O, FeOOH, ferric nitrate and ironic citrate are a variety of.
3. the method according to claim 1, wherein the lithium source is lithium carbonate, Dan Shuiqing in step (1)
One of lithia and lithia are a variety of.
4. the method according to claim 1, wherein in step (1), the sintering process are as follows: by source of iron, lithium
Source mixture is placed in sintering furnace, under nitrogen protection, is warming up to sintering temperature with preset heating rate and is sintered；
Preferably, the preset heating rate is 1-10 DEG C/min.
5. method according to claim 1 or 4, which is characterized in that the sintering temperature is 650-1000 DEG C；The sintering
Time is 3-72h.
6. the method according to claim 1, wherein the ferrous acid lithium is crushed to average grain in step (2)
Diameter is 2-50 μm.
7. the method according to claim 1, wherein the carbon source is methane, ethane, third in step (3)
One of alkane, ethylene, acetylene and butylene are a variety of.
8. the method according to claim 1, wherein the gas phase coats process are as follows: by powder in step (3)
Ferrous acid lithium after broken, which is placed in CVD rotary furnace, is warming up to preset temperature, is passed through carbon source with preset flow, carries out under preset temperature
Stop being passed through carbon source after gas phase cladding, carbon coating ferrous acid lithium material is obtained after cooling；
Preferably, the default temperature of plate is 600-800 DEG C；
Preferably, the preset flow is 2.5-7mL/min；
Preferably, the gas phase cladding time is 2-8h.
9. the carbon coating ferrous acid lithium material of the preparation of the method as described in any one of claim 1-8.
10. carbon coating ferrous acid lithium material according to claim 9, which is characterized in that in the carbon coating ferrous acid lithium material
The content of carbon is 0.5-5 weight %.
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