CN103855400A - Lithium silicate ferrous/graphene composite and its preparation method and application - Google Patents
Lithium silicate ferrous/graphene composite and its preparation method and application Download PDFInfo
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- CN103855400A CN103855400A CN201210504706.2A CN201210504706A CN103855400A CN 103855400 A CN103855400 A CN 103855400A CN 201210504706 A CN201210504706 A CN 201210504706A CN 103855400 A CN103855400 A CN 103855400A
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- lithium
- composite material
- graphene composite
- ferrosilicon silicate
- graphene
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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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- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
-
- 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
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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 invention belongs to the field of electrochemical materials, and discloses a lithium silicate ferrous / graphene composite and its preparation method and application; the composite consists of 50-90wt% of lithium silicate ferrous and 10-50wt% of graphene. According to the lithium silicate ferrous / graphene composite, the graphene is high in conductivity, and after compounding with the lithium silicate ferrous, the problem that the electronic and ionic conductivity of a lithium silicate ferrous material are not high can be solved effectively, and the reversible capacity is improved; at the same time, the composite discharge specific capacity can reach 145mAh / g which is close to the theoretical capacity of 166mAh / g; lithium ion batteries prepared by the composite can be charged and discharged at a current density of 5C, and the capacity retention rate can reach 62.8-80%.
Description
Technical field
The present invention relates to electrochemical material field, relate in particular to a kind of ferrosilicon silicate of lithium/graphene composite material and its preparation method and application.
Background technology
Along with the development of various new forms of energy, the miniaturization development of portable electric appts and the widespread demand of electric automobile to large-capacity high-power chemical power source.Current commercial lithium ion battery adopts inorganic positive pole/graphite system mostly, and wherein these positive electrodes are mainly LiFePO4s, LiMn2O4, cobalt acid lithium, the system of lithium nickelate and mixing.Although the chemical property excellence of this class system, due to itself capacity lower (as the theoretical 170mAh/g of LiFePO4), complicated process of preparation, the shortcoming that high in cost of production is many.So the positive electrode of other kind of development of new has been subject to people's attention widely.
Li
2feSiO
4series lithium ion battery positive electrode, with advantages such as ABUNDANT NATUREAL RESOURSES, environmental friendliness, high security and stable circulations, has good application prospect.Li at present
2feSiO
4be the research ground zero of positive electrode, need further research to improve the performance of this type of material.Because the form existing in silicate is more, at Li
2feSiO
4in the building-up process of material, easily there is impurity, synthetic pure phase Li
2feSiO
4more difficult.Li simultaneously
2feSiO
4exist similar problem: Li
2feSiO
4there is very low electronic conductivity and lithium ion diffusion coefficient is little, make the deintercalation invertibity of lithium ion in material poor, cause Li
2feSiO
4low specific discharge capacity and poor high rate performance.
Summary of the invention
Problem to be solved by this invention be to provide a kind of reversible capacity and specific discharge capacity higher, and forthright good ferrosilicon silicate of lithium/graphene composite material doubly.
Technical scheme of the present invention is as follows:
A kind of ferrosilicon silicate of lithium/graphene composite material, calculates according to mass percent, comprises 50 ~ 90% ferrosilicon silicate of lithium and 10 ~ 50% Graphene.
The preparation method of above-mentioned ferrosilicon silicate of lithium/graphene composite material, comprises the steps:
The source compound of iron, lithium metasilicate and graphite oxide are ground, obtain mixed powder; Wherein, the source compound of iron and the addition of lithium metasilicate are that 1:1 carries out according to ferro element and element silicon mol ratio, and the addition of graphite oxide is 0.333 ~ 3 times of lithium metasilicate quality;
Under reducing atmosphere, at 800 ~ 1000 ℃, to mixed powder calcining 6 ~ 24 hours, obtain described ferrosilicon silicate of lithium/graphene composite material.
The preparation method of described ferrosilicon silicate of lithium/graphene composite material, wherein, the source compound of described iron is one or more in iron oxide, ferrous oxide and tri-iron tetroxide.
The preparation method of described ferrosilicon silicate of lithium/graphene composite material, wherein, grinding is to carry out in ball mill, and milling time is 1 ~ 10 hour.
The preparation method of described ferrosilicon silicate of lithium/graphene composite material, wherein, the gas of described reducing atmosphere is that volume ratio is the mist of the hydrogen of 90:10 and the mist of argon gas or hydrogen and nitrogen.
The invention still further relates to a kind of anode, comprise aluminium foil, and be coated in the positive electrode on aluminium foil, this positive electrode comprises that mass ratio is ferrosilicon silicate of lithium/graphene composite material, Kynoar and the acetylene black of 85:5:10; Calculate according to mass percent, described ferrosilicon silicate of lithium/graphene composite material comprises 50 ~ 90% ferrosilicon silicate of lithium and 10 ~ 50% Graphene.
Above-mentioned anode can be applied to lithium ion cell positive field.
Ferrosilicon silicate of lithium/graphene composite material of the present invention, Graphene has very high conductivity, can effectively solve the problem that ferrosilicon silicate of lithium material electronics conductivity and ionic conductivity are not high with ferrosilicon silicate of lithium after compound, and then improves reversible capacity; Meanwhile, this composite material specific discharge capacity can reach 145mAh/g, approaches theoretical capacity 166mAh/g; Lithium ion battery prepared by this material can discharge and recharge under the current density of 5C, and capacity retention can reach 62.8 ~ 80% simultaneously.
Accompanying drawing explanation
Fig. 1 is preparation technology's flow chart of ferrosilicon silicate of lithium/graphene composite material of the present invention.
Embodiment
A kind of active material that can be used for lithium ion cell positive provided by the invention, i.e. ferrosilicon silicate of lithium/graphene composite material, wherein, calculates ferrosilicon silicate of lithium (Li according to mass percent
2feSiO
4) mass content accounts for 50 ~ 90%, Graphene accounts for 10 ~ 50%.
The preparation method of above-mentioned ferrosilicon silicate of lithium/graphene composite material, as shown in Figure 1, comprises the steps:
S1, the source compound of iron, lithium metasilicate and graphite oxide are put into ball mill, ball milling 1 ~ 10h, obtains mixed powder; Wherein, the source compound of iron and the addition of lithium metasilicate are that 1:1 carries out according to ferro element and element silicon mol ratio, and the addition of graphite oxide is 0.333 ~ 3 times of lithium metasilicate quality;
S2, mixed powder is put into the Muffle furnace of reducing atmosphere, 800 ~ 1000 ℃ of calcinings 6 ~ 24 hours, obtain ferrosilicon silicate of lithium/graphene composite material.
Above-mentioned preparation method, in step S1, the source compound of iron can be one or more in iron oxide, ferrous oxide and tri-iron tetroxide.
Above-mentioned preparation method, in step S2, the gas of described reducing atmosphere is that volume ratio is the mist of the hydrogen of 90:10 and the mist of argon gas or hydrogen and nitrogen, i.e. the mist of 90v% hydrogen and 10v% argon gas or 90v% hydrogen and 10v% nitrogen mixture body.
The application of ferrosilicon silicate of lithium/graphene composite material: be generally used for the positive electrode of lithium ion battery, as:
A kind of anode, comprises aluminium foil, and is coated in the positive electrode on aluminium foil, this positive electrode comprises that mass ratio is ferrosilicon silicate of lithium/graphene composite material, Kynoar and the acetylene black of 85:5:10; Calculate according to mass percent, described ferrosilicon silicate of lithium/graphene composite material comprises 50 ~ 90% ferrosilicon silicate of lithium and 10 ~ 50% Graphene.
Above-mentioned anode can be applied to lithium ion cell positive field.
Below introduce the method that uses this material to be made into lithium ion battery.
1, prepare anode
First, select ferrosilicon silicate of lithium/graphene composite material prepared by above method as positive electrode;
Secondly, the ratio that is 85:5:10 according to mass ratio, ferrosilicon silicate of lithium/graphene composite material, Kynoar binding agent and conductive agent acetylene black are mixed, obtain slurry;
Finally, slurry is coated on aluminium foil, drying, roll film, trimming processing, make based lithium-ion battery positive plate.
2, preparation battery cathode
First, the ratio that is 85:5:10 according to mass ratio, graphite, Kynoar binding agent and conductive agent acetylene black are mixed, obtain slurry;
Secondly, slurry is coated on Copper Foil paper tinsel, drying, roll film, trimming processing, make anode plate for lithium ionic cell.
3, the assembling of lithium ion battery
By positive plate, barrier film, negative plate in order stack of laminations dress up battery core, then use battery housing seal battery core, in battery container, inject electrolyte by the liquid injection port being arranged on battery container subsequently, sealing liquid injection port, obtains lithium ion battery.
The concentration of electrolyte is generally 1mol/L, and the solute in electrolyte adopts LiPF
6, LiBF
4, LiTFSI (LiN (SO
2cF
3)
2), LiFSI (LiN (SO
2f)
2) etc., the solvent in electrolyte adopts one or more mixing in dimethyl carbonate, diethyl carbonate, propene carbonate, ethylene carbonate and acetonitrile.
Ferrosilicon silicate of lithium/graphene composite material of the present invention, Graphene has very high conductivity, can effectively solve the problem that ferrosilicon silicate of lithium material electronics conductivity and ionic conductivity are not high with ferrosilicon silicate of lithium after compound, and then improves reversible capacity; Meanwhile, this composite material specific discharge capacity can reach 145mAh/g, approaches theoretical capacity 166mAh/g; Lithium ion battery prepared by this material can discharge and recharge under the current density of 5C, and capacity retention can reach 62.8 ~ 80% simultaneously.
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in further detail.
Embodiment 1 ~ 4th, the preparation method of ferrosilicon silicate of lithium/graphene composite material, embodiment 5 ~ 8th, the material of embodiment 1 ~ 4 preparation is as the application of lithium ion cell positive.
Embodiment 1
(1) 72g FeO, 90g lithium metasilicate and 30g graphite oxide are put into ball mill, ball milling 1h for mixing;
(2) the ball milling mixture (1) being obtained is put into the Muffle furnace of the hydrogen-argon-mixed protection of hydrogen 90%, at 800 ℃, calcines 24h, obtains the ferrosilicon silicate of lithium/graphene composite material containing ferrosilicon silicate of lithium 90%.
Embodiment 2
(1) 80g iron oxide, 90g lithium metasilicate and 270g graphite oxide are put into ball mill, ball milling 10h for mixing;
(2) the ball milling mixture (1) being obtained is put into the Muffle furnace of the hydrogen-argon-mixed protection of hydrogen 90%, at 1000 ℃, calcines 6h, obtains the ferrosilicon silicate of lithium/graphene composite material containing ferrosilicon silicate of lithium 50%.
Embodiment 3
(1) 77g tri-iron tetroxide, 90g lithium metasilicate and 60g graphite oxide are put into ball mill, ball milling 3h for mixing;
(2) the ball milling mixture (1) being obtained is put into the Muffle furnace of the hydrogen nitrogen mixed gas protection of hydrogen 90%, at 900 ℃, calcines 12h, obtains the ferrosilicon silicate of lithium/graphene composite material containing ferrosilicon silicate of lithium 82%.
Embodiment 4
(1) just 72g ferrous oxide, 90g lithium metasilicate and 150g graphite oxide are put into ball mill, ball milling 6h for mixing;
(2) the ball milling mixture (1) being obtained is put into the Muffle furnace of the hydrogen nitrogen mixed gas protection of hydrogen 90%, at 950 ℃, calcines 18h, obtains the ferrosilicon silicate of lithium/graphene composite material containing ferrosilicon silicate of lithium 64.3%.
Embodiment 5
1, prepare anode
First, select ferrosilicon silicate of lithium/graphene composite material prepared by embodiment 1 as positive electrode;
Secondly, the ratio that is 85:5:10 according to mass ratio, ferrosilicon silicate of lithium/graphene composite material, Kynoar binding agent and conductive agent acetylene black are mixed, obtain slurry;
Finally, slurry is coated on aluminium foil, drying, roll film, trimming processing, make based lithium-ion battery positive plate.
2, preparation battery cathode
First, the ratio that is 85:5:10 according to mass ratio, graphite, Kynoar binding agent and conductive agent acetylene black are mixed, obtain slurry;
Secondly, slurry is coated on Copper Foil paper tinsel, drying, roll film, trimming processing, make anode plate for lithium ionic cell.
3, the assembling of lithium ion battery
By positive plate, barrier film, negative plate in order stack of laminations dress up battery core, then use battery housing seal battery core, subsequently by being arranged on liquid injection port on battery container toward the LiPF that injects 1mol/L in battery container
6/ dimethyl carbonate electrolyte, sealing liquid injection port, obtains lithium ion battery.
Embodiment 6 ~ 8 difference from Example 5 are:
Cell positive material adopts respectively the prepared ferrosilicon silicate of lithium/graphene composite material out of embodiment 2 ~ 4; And electrolyte is respectively the LiBF of 1mol/L
4the LiTFSI/ propene carbonate electrolyte of/diethyl carbonate electrolyte, 1mol/L, LiFSI/ ethylene carbonate+acetonitrile electrolyte of 1mol/L.
Composite material to embodiment 1 ~ 4 preparation carries out conductivity test, and test result is as shown in table 1.
Table 1
| ? | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Conductivity s/cm | 5.2×10 -7 | 8.7×10 -8 | 2.1×10 -7 | 9.410 -8 |
Under room temperature, the electronic conductivity of ferrosilicon silicate of lithium, far below other positive electrode, is approximately 6 × 10
-14s/cm, ferrosilicon silicate of lithium/graphene composite material that the present invention prepares is far above 6 × 10
-14s/cm.
Embodiment 5 ~ 8 is carried out under the electric current of 0.1C and 5C to charge-discharge test, it is as shown in the table for test result.
Table 2
Ferrosilicon silicate of lithium/graphene composite material energy the conductivity that adopts the present invention to prepare is improved, and the capacity that this material can have been given play to is improved, and reaches 145mAh/g, approaches theoretical capacity 166mAh/g; Lithium ion battery prepared by this material can discharge and recharge under the current density of 5C, and capacity retention can reach 62.8 ~ 80% simultaneously.
Should be understood that, the above-mentioned statement for preferred embodiment of the present invention is comparatively detailed, can not therefore think the restriction to scope of patent protection of the present invention, and scope of patent protection of the present invention should be as the criterion with claims.
Claims (7)
1. ferrosilicon silicate of lithium/graphene composite material, is characterized in that, calculates according to mass percent, comprises 50 ~ 90% ferrosilicon silicate of lithium and 10 ~ 50% Graphene.
2. a preparation method for ferrosilicon silicate of lithium/graphene composite material, is characterized in that, comprises the steps:
The source compound of iron, lithium metasilicate and graphite oxide are ground, obtain mixed powder; Wherein, the source compound of iron and the addition of lithium metasilicate are that 1:1 carries out according to ferro element and element silicon mol ratio, and the addition of graphite oxide is 0.333 ~ 3 times of lithium metasilicate quality;
Under reducing atmosphere, at 800 ~ 1000 ℃, to mixed powder calcining 6 ~ 24 hours, obtain described ferrosilicon silicate of lithium/graphene composite material.
3. the preparation method of ferrosilicon silicate of lithium/graphene composite material according to claim 2, is characterized in that, the source compound of described iron is one or more in iron oxide, ferrous oxide and tri-iron tetroxide.
4. the preparation method of ferrosilicon silicate of lithium/graphene composite material according to claim 2, is characterized in that, grinding is to carry out in ball mill, and milling time is 1 ~ 10 hour.
5. the preparation method of ferrosilicon silicate of lithium/graphene composite material according to claim 2, is characterized in that, the gas of described reducing atmosphere is that volume ratio is the mist of the hydrogen of 90:10 and the mist of argon gas or hydrogen and nitrogen.
6. an anode, comprise aluminium foil, and be coated in the positive electrode on aluminium foil, this positive electrode comprises that mass ratio is ferrosilicon silicate of lithium/graphene composite material, Kynoar and the acetylene black of 85:5:10, it is characterized in that, calculate according to mass percent, described ferrosilicon silicate of lithium/graphene composite material comprises 50 ~ 90% ferrosilicon silicate of lithium and 10 ~ 50% Graphene.
7. a lithium ion battery, is characterized in that, the positive pole of this lithium ion battery adopts anode claimed in claim 6.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108123120A (en) * | 2017-12-07 | 2018-06-05 | 成都新柯力化工科技有限公司 | A kind of lithium battery nanometer ferric metasilicate lithium/graphene anode material and preparation method thereof |
| CN109904393A (en) * | 2017-12-08 | 2019-06-18 | 浙江工业大学 | A kind of lithium ion battery graphene-supported transition metal silicate nano-sized membrane and preparation method thereof |
| CN112687464A (en) * | 2020-12-23 | 2021-04-20 | 上海大学 | Ferrous chloride modified graphene magnetic composite material and preparation method thereof |
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| CN102201275A (en) * | 2010-03-25 | 2011-09-28 | 海洋王照明科技股份有限公司 | Lithium salt and graphene composite material as well as preparation method and application thereof |
| CN102412396A (en) * | 2011-11-11 | 2012-04-11 | 深圳市德方纳米科技有限公司 | Lithium ion battery electrode material coated with non-continuous graphene |
| US20120205595A1 (en) * | 2011-02-14 | 2012-08-16 | Basf Se | Electrode materials and process for producing them |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102201275A (en) * | 2010-03-25 | 2011-09-28 | 海洋王照明科技股份有限公司 | Lithium salt and graphene composite material as well as preparation method and application thereof |
| US20120205595A1 (en) * | 2011-02-14 | 2012-08-16 | Basf Se | Electrode materials and process for producing them |
| CN102412396A (en) * | 2011-11-11 | 2012-04-11 | 深圳市德方纳米科技有限公司 | Lithium ion battery electrode material coated with non-continuous graphene |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108123120A (en) * | 2017-12-07 | 2018-06-05 | 成都新柯力化工科技有限公司 | A kind of lithium battery nanometer ferric metasilicate lithium/graphene anode material and preparation method thereof |
| CN108123120B (en) * | 2017-12-07 | 2020-07-21 | 成都新柯力化工科技有限公司 | Nano lithium iron silicate/graphene positive electrode material for lithium battery and preparation method thereof |
| CN109904393A (en) * | 2017-12-08 | 2019-06-18 | 浙江工业大学 | A kind of lithium ion battery graphene-supported transition metal silicate nano-sized membrane and preparation method thereof |
| CN109904393B (en) * | 2017-12-08 | 2020-12-25 | 浙江工业大学 | Graphene-loaded transition metal silicate nano-film material for lithium ion battery and preparation method thereof |
| CN112687464A (en) * | 2020-12-23 | 2021-04-20 | 上海大学 | Ferrous chloride modified graphene magnetic composite material and preparation method thereof |
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Application publication date: 20140611 |