CN107369834A - Compound fluorocarbons positive electrode and its production and use - Google Patents

Compound fluorocarbons positive electrode and its production and use Download PDF

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Publication number
CN107369834A
CN107369834A CN201710564406.6A CN201710564406A CN107369834A CN 107369834 A CN107369834 A CN 107369834A CN 201710564406 A CN201710564406 A CN 201710564406A CN 107369834 A CN107369834 A CN 107369834A
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positive electrode
preparation
compound
fluorocarbons
fluorocarbons positive
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CN107369834B (en
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伏萍萍
宋英杰
马倩倩
徐宁
吴孟涛
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Tianjin B&M Science and Technology Co Ltd
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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
    • H01M4/58—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
    • H01M4/36—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
    • H01M4/5835—Comprising fluorine or fluoride salts
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M6/00—Primary cells; Manufacture thereof

Abstract

The invention discloses a kind of compound fluorocarbons positive electrode and its production and use, the compound fluorocarbons positive electrode, molecular formula is M (CFx)n, wherein, any one or a few in M Co, Ni, Mn, Fe, Al, Ag and Cu；X=1~1.25, n >=1, n are natural numbers；Meanwhile M, C are dispersed.Its preparation method comprises the following steps：First transition metal fluorides are well mixed with expansible graphite powder, then are pressed into bulk, in kiln, the high-temperature process under fluoro-gas atmosphere, finally by crushing material after high-temperature process, produce product.The compound fluorocarbons positive electrode is applied to lithium primary battery, has good big high rate performance；Its preparation method has carried out metallic element doping to fluorocarbons, effectively improves the electrical conductivity of material；And synthesis technique is simple, process conditions are easily controllable, it is easy to accomplish industrialized mass production.

Description

Compound fluorocarbons positive electrode and its production and use
Technical field
The present invention relates to field of lithium ion battery anode, be specially related to a kind of compound fluorocarbons positive electrode and its Preparation method and purposes.
Background technology
Li/ is fluorinated carbon battery as a kind of lithium primary battery, has higher specific energy, energy density per unit volume and long storage Deposit the life-span.The baby batteries such as button cell can be not only assembled into applied to wrist-watch, pocket calculating machine, wearable device, memory etc., and And the big batteries such as cylindrical battery, square battery can be assembled into applied to memory, radio station receiver, photographic equipment etc..
(CF)nIt is 3.2V as a kind of positive electrode open-circuit voltage, operating voltage is 2.5V~2.7V, and theory reaches than energy To 2180Wh/kg, it is than energy highest in current solid positive electrode, therefore has been a great concern, application prospect is non- It is often tempting.But the maximum determination of fluorinated carbon material is that its electron conduction is poor, seriously reduces its high rate performance.Report at present Method to fluorocarbons battery performance is mainly carbon coating, metal and its compound cladding process, such as 104466177A pairs of patent Fluorination carbon surface has carried out nickel coated, and patent 105185959A has carried out carbon coating based on polyureas etc. to fluorination carbon surface, its Purpose is by carrying out conductive material cladding processing to fluorocarbons particle surface, to improve the electric conductivity of material.But wrap The shortcomings that covering means is to be only capable of improving the contact electrical conductivity between material microscopic particles, and coating technology presence covers uneven, bag The shortcomings that coating thickness control difficulty is big, it is difficult to realize the uniformity that electric conductivity improves in micro-scale.
The content of the invention
In order to solve the above-mentioned technical problem, the present invention provides a kind of compound fluorocarbons positive electrode and preparation method thereof and used On the way, the compound fluorinated carbon material is by designing being mutually bonded between metallic element, carbon and fluorine element atom, controlling Fluorination reaction, and a kind of advanced composite material (ACM) designed.Due to the covalent bond between the former fluorocarbons of introducing of metallic element by To perturbation, so that material intrinsic conductivity is improved, it is a kind of method for improving material conductivity from body phase.It is of the invention public The compound fluorocarbons positive electrode opened is applied to lithium primary battery, has good big high rate performance；By inflatable stone during preparation Ink carries out transient metal doped and fluorination so that product high rate performance is made and is improved.
Therefore, technical scheme is as follows：
A kind of compound fluorocarbons positive electrode, molecular formula are M (CFx)n, wherein, in M Co, Ni, Mn, Fe, Al, Ag and Cu Any one or a few；X=1~1.25, n >=1, n are natural numbers；Meanwhile M, C are dispersed.
A kind of preparation method of compound fluorocarbons positive electrode, comprises the following steps：
1) transition metal fluorides and expansible graphite powder are added into high speed mixer, is well mixed, obtains material I；
2) it is the material I is compressing, obtain the material II of bulk；
3) the material II is placed in kiln, the high-temperature process under fluoro-gas atmosphere, obtains material III；
4) the material III is crushed, produces product.
Further, the amount of the material of the metallic element in the transition metal fluorides and the carbon in expansible graphite powder The ratio between amount of material of element is 0.001~1：1.
Further, the transition metal fluorides are CoF3、NiF2、MnF2、MnF3、FeF2、FeF3、AlF3, AgF and CuF2 In one or more.
Further, used pressure is when compressing in step 2)：0.1~100MPa.
Further, the temperature of step 3) high temperature processing is 400~600 DEG C.
Further, in step 3) fluoro-gas atmosphere be hydrogen fluoride, fluorine gas, or both mixture.It is it is preferred that described fluorine-containing The content of hydrogen fluoride and fluorine gas at least accounts for the 5% of total gas volume in atmosphere.
Further, granularity is D after being crushed in step 4)50=0.1~30 μm.
A kind of purposes of compound fluorocarbons positive electrode, the compound fluorocarbons positive electrode are used for lithium primary battery positive pole material Material.
This method has carried out metallic element doping to fluorocarbons, effectively improves the electrical conductivity of material；And synthesis technique letter Single, process conditions are easily controllable, it is easy to accomplish industrialized mass production.
Brief description of the drawings
Fig. 1 is the process route chart of the preparation method of compound fluorocarbons positive electrode provided by the invention；
Fig. 2 is the XRD spectrum of high-rate type fluorocarbons positive electrode made from embodiment 1；
Fig. 3 is the SEM photograph of high-rate type fluorocarbons positive electrode made from embodiment 1；
Fig. 4 is high-rate type fluorocarbons positive electrode made from embodiment 1, fluorocarbons positive electrode made from comparative example 1 Charging and discharging curve figure.
Embodiment
Technical scheme is described in detail below in conjunction with drawings and examples.
Embodiment 1
A kind of preparation method of compound fluorocarbons positive electrode, comprises the following steps：
1) according to mol ratio Co:C=0.001, weigh CoF3Powder and expansible graphite C powder, add high speed mixer, High speed dispersion mixing is carried out, obtains material I；
2) by material I under conditions of pressure 0.1MPa it is compressing, obtain bulk material II；
3) material II is placed in kiln, is passed through gas containing HF (HF volume content >=10%), is calcined at 400 DEG C 8h, obtain material III；
4) material III is put into jaw crusher successively, mechanical crusher crushes, Control granularity D50For 15 μm ± 1 μm, i.e., Obtain Co (CF1.25)1000Positive electrode.
Fig. 2 is the Co (CF that the present embodiment obtains1.25)1000The infrared absorption spectra of positive electrode, it can be seen that material exists C-F stretching vibration peaks be present in 1000 °~1400 ° scopes.
Fig. 3 is the Co (CF that the present embodiment obtains1.25)1000The stereoscan photograph of positive electrode, size are about 15 μ m。
Comparative example 1
The step 1) of embodiment 1 is changed to：Expanded graphite C powder is added into high speed mixer, carries out high speed dispersion mixing, Obtain material I；Remaining step with embodiment 1, obtains the fluorinated carbon material adulterated without metallic element.
Fig. 4 is the Co (CF that embodiment 1 obtains1.25)1000Positive electrode, comparative example 1 obtain without metal-doped (CF1.25)1000Positive electrode is assembled into the charging and discharging curve of button cell, it can be seen that the compound fluorocarbons that embodiment 1 obtains is just Pole material has more preferable 1C rate capabilities.
Embodiment 2
A kind of preparation method of compound fluorocarbons positive electrode, comprises the following steps：
1) according to mol ratio Mn:C=1：1, weigh MnF2Powder and expansible graphite C powder, add high speed mixer, enter Row high speed dispersion mixing, obtains material I；
2) by material I under conditions of pressure 100MPa it is compressing, obtain bulk material II；
3) material II is placed in kiln, is passed through gas containing HF (HF volume content >=10%), is calcined at 500 DEG C 8h, obtain material III；
4) material III is put into jaw crusher successively, mechanical crusher crushes, Control granularity D50For 20 μm ± 1 μm, i.e., Obtain Mn (CF) positive electrode.
Embodiment 3
A kind of preparation method of compound fluorocarbons positive electrode, comprises the following steps：
1) according to mol ratio Al:C=0.01：1, weigh AlF3Powder and expansible graphite C powder, add high speed batch mixing Machine, high speed dispersion mixing is carried out, obtains material I；
2) by material I under conditions of pressure 10MPa it is compressing, obtain bulk material II；
3) material II is placed in kiln, is passed through gas containing HF (HF volume content >=10%), is calcined at 600 DEG C 8h, obtain material III；
4) material III is put into jaw crusher successively, mechanical crusher crushes, Control granularity D50For 0.5 μm of ± 0.1 μ M, that is, obtain Al (CF1.1)100Positive electrode.
Embodiment 4
A kind of preparation method of compound fluorocarbons positive electrode, comprises the following steps：
1) according to mol ratio Ag:C=0.1：1, AgF powder and expansible graphite C powder are weighed, adds high speed mixer, High speed dispersion mixing is carried out, obtains material I；
2) by material I under conditions of pressure 10MPa it is compressing, obtain bulk material II；
3) material II is placed in kiln, is passed through gas containing HF (HF volume content >=10%), is calcined at 600 DEG C 8h, obtain material III；
4) material III is put into jaw crusher successively, mechanical crusher crushes, Control granularity D50For 5 μm ± 0.5 μm, Obtain Ag (CF1.2)10Positive electrode.
Experimental conditions：
Table 1 lists the multiplying power discharging that button cell is made using compound fluorocarbons positive electrode made from above-described embodiment Specific capacity.The test condition of button cell is：23 DEG C ± 2 DEG C, LR 2032, I=0.1C, 1C, 1.0~3.0V vs.Li/Li+。
Table 1 buckles electric multiplying power charging capacity contrast table
The compound fluorocarbons positive electrode that each embodiment obtains it can be seen from data in table 1, specific capacity reach The discharge capacity performance of battery is significantly better than the non-impurity-doped samples of comparative example 1 under more than 900mAh/g, 1C multiplying power.
In summary, present disclosure is not limited in the above embodiments, and the knowledgeable people in same area can Can propose other embodiments easily within the technological guidance's thought of the present invention, but this embodiment is included in this hair Within the scope of bright.

Claims (10)

  1. A kind of 1. compound fluorocarbons positive electrode, it is characterised in that：Molecular formula is M (CFx)n, wherein, M Co, Ni, Mn, Fe, Any one or a few in Al, Ag and Cu；X=1~1.25, n >=1, n are natural numbers；Meanwhile M, C are dispersed.
  2. 2. the preparation method of compound fluorocarbons positive electrode as claimed in claim 1, it is characterised in that comprise the following steps：
    1) transition metal fluorides and expansible graphite powder are added into high speed mixer, is well mixed, obtains material I；
    2) it is the material I is compressing, obtain the material II of bulk；
    3) the material II is placed in kiln, the high-temperature process under fluoro-gas atmosphere, obtains material III；
    4) the material III is crushed, produces product.
  3. 3. preparation method as claimed in claim 2, it is characterised in that：The material of metallic element in the transition metal fluorides Amount and expansible graphite powder in the ratio between the amount of material of carbon be 0.001~1：1.
  4. 4. preparation method as claimed in claim 2, it is characterised in that：The transition metal fluorides are CoF3、NiF2、MnF2、 MnF3、FeF2、FeF3、AlF3, AgF and CuF2In one or more.
  5. 5. preparation method as claimed in claim 2, it is characterised in that：Used pressure is when compressing in step 2)：0.1 ~100MPa.
  6. 6. preparation method as claimed in claim 2, it is characterised in that：The temperature of step 3) high temperature processing is 400~600 DEG C.
  7. 7. preparation method as claimed in claim 2, it is characterised in that：In step 3) fluoro-gas atmosphere be hydrogen fluoride, fluorine gas or Both mixtures.
  8. 8. preparation method as claimed in claim 7, it is characterised in that：The content of hydrogen fluoride and fluorine gas in the fluoro-gas atmosphere At least account for the 5% of total gas volume.
  9. 9. preparation method as claimed in claim 2, it is characterised in that：Granularity is D after being crushed in step 4)50=0.1~30 μm.
  10. 10. the purposes of compound fluorocarbons positive electrode as claimed in claim 1, it is characterised in that：The compound fluorocarbons positive pole material Expect to be used for lithium primary battery positive electrode.
CN201710564406.6A 2017-07-12 2017-07-12 Composite carbon fluoride anode material and preparation method and application thereof Active CN107369834B (en)

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Cited By (6)

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Publication number Priority date Publication date Assignee Title
CN109037627A (en) * 2018-07-20 2018-12-18 浙江大学 A kind of alkali metal base composite negative pole and its application
CN109888283A (en) * 2017-12-06 2019-06-14 中国科学院大连化学物理研究所 A kind of modified fluorinated carbon quantum of hetero atom and preparation method thereof
CN112607724A (en) * 2020-12-18 2021-04-06 中国民航大学 Preparation method of carbon fluoride anode material based on covalent organic framework material
CN113410466A (en) * 2021-06-17 2021-09-17 贵州梅岭电源有限公司 Preparation method of carbon fluoride modified ferric trifluoride cathode material
CN113422059A (en) * 2021-06-17 2021-09-21 贵州梅岭电源有限公司 High-voltage carbon fluoride composite cathode material and preparation method thereof
CN115893471A (en) * 2022-11-10 2023-04-04 电子科技大学长三角研究院(湖州) Method for compounding silver oxide and carbon fluoride through plasma induction and application of lithium primary battery

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CN104466177A (en) * 2014-12-03 2015-03-25 湘潭大学 Nickel coated carbon fluoride positive electrode material and preparation method thereof
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CN104466177A (en) * 2014-12-03 2015-03-25 湘潭大学 Nickel coated carbon fluoride positive electrode material and preparation method thereof
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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109888283A (en) * 2017-12-06 2019-06-14 中国科学院大连化学物理研究所 A kind of modified fluorinated carbon quantum of hetero atom and preparation method thereof
CN109888283B (en) * 2017-12-06 2021-07-06 中国科学院大连化学物理研究所 Heteroatom modified carbon fluoride quantum dot and preparation method thereof
CN109037627A (en) * 2018-07-20 2018-12-18 浙江大学 A kind of alkali metal base composite negative pole and its application
CN109037627B (en) * 2018-07-20 2020-08-25 浙江大学 Alkali metal-based composite negative electrode and application thereof
CN112607724A (en) * 2020-12-18 2021-04-06 中国民航大学 Preparation method of carbon fluoride anode material based on covalent organic framework material
CN113410466A (en) * 2021-06-17 2021-09-17 贵州梅岭电源有限公司 Preparation method of carbon fluoride modified ferric trifluoride cathode material
CN113422059A (en) * 2021-06-17 2021-09-21 贵州梅岭电源有限公司 High-voltage carbon fluoride composite cathode material and preparation method thereof
CN113410466B (en) * 2021-06-17 2022-07-12 贵州梅岭电源有限公司 Preparation method of carbon fluoride modified ferric trifluoride cathode material
CN115893471A (en) * 2022-11-10 2023-04-04 电子科技大学长三角研究院(湖州) Method for compounding silver oxide and carbon fluoride through plasma induction and application of lithium primary battery

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