CN107275603A - MoSe2The preparation of OMC compounds and its application in lithium ion battery - Google Patents

MoSe2The preparation of OMC compounds and its application in lithium ion battery Download PDF

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Publication number
CN107275603A
CN107275603A CN201710434576.2A CN201710434576A CN107275603A CN 107275603 A CN107275603 A CN 107275603A CN 201710434576 A CN201710434576 A CN 201710434576A CN 107275603 A CN107275603 A CN 107275603A
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omc
compounds
mose
preparation
ion battery
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魏明灯
郑成
陈聪荣
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Fuzhou University
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Fuzhou University
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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
    • 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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • 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)
  • Manufacturing & Machinery (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses a kind of MoSe2The preparation method of OMC compounds and its application in lithium ion battery, it is that a certain amount of molybdenum source is loaded into OMC by nanometer casting method（Ordered mesopore carbon）In, it is then MoSe by molybdenum source converted in-situ by high-temperature process2, obtain the MoSe2OMC compounds.The synthetic method of compound of the present invention is simple, favorable reproducibility, and it stores up lithium excellent performance, has good cyclical stability and big high rate performance as lithium ion battery negative material.

Description

MoSe2The preparation of-OMC compounds and its application in lithium ion battery
Technical field
The invention belongs to field of material preparation, and in particular to a kind of MoSe2- ordered mesopore carbon（OMC）The preparation of compound And its application in lithium ion battery.
Background technology
MoSe2As a kind of typical two-dimensional material, with special Se-Mo-Se sandwich layer structures, inside layer with Covalent bond is connected, and interlayer is attracted each other with Van der Waals force, has similar structure to graphite.And compared to for graphite, MoSe2Layer Spacing is bigger（About 0.65 nm）, the insertion and abjection of ion are especially suitable for, is considered as a kind of lithium storage materials of great prospect.But It is, MoSe2Electric conductivity itself is poor, so as to influence its big high rate performance, can occur volume change during Li insertion extraction in addition Change so that MoSe2Easily come off from collector, cause the rapid decay of capacity.
The content of the invention
It is an object of the invention to provide a kind of MoSe2The preparation of-OMC compounds and its answering in lithium ion battery With its synthetic method is simple, favorable reproducibility, and the storage lithium excellent performance of gained compound, as negative electrode of lithium ion battery Material has good cyclical stability and big high rate performance.
To achieve the above object, the present invention is adopted the following technical scheme that：
A kind of MoSe2The preparation method of-OMC compounds, it comprises the following steps：
1）50-100mg ordered mesopore carbons are washed into 1h with concentrated nitric acid, is then washed respectively with deionized water and ethanol and centrifuges 3 It is secondary, it is standby；
2）50-100mg phosphomolybdic acids are dissolved in 1-10mL ethanol, step 1 is then added）The ordered mesopore carbon pre-processed, Stirring is volatilized completely to ethanol, with after drying in 70 DEG C of baking ovens；
3）By step 2）Gained sample is placed in tube furnace simultaneously with 50-200mg selenium powders, in H2/ Ar mixed atmospheres（Volume ratio 5: 95）In, in calcining 1-12h at 500-800 DEG C, after after tube furnace natural cooling, produce the MoSe2- OMC compounds.
Prepared MoSe2Application of-OMC the compounds in as lithium ion battery negative material.
The remarkable advantage of the present invention is：The present invention is calcined using simple nanometer casting method and later stage, has synthesized one kind MoSe2- ordered mesoporous carbon complex, its synthetic method is simple, favorable reproducibility, and gained compound storage lithium excellent performance, by it There is excellent cyclical stability and big high rate performance as lithium ion battery negative material.After testing, assembled by the compound Lithium ion battery there is 451 mAh/g capacity when current density is 2 A/g after charge and discharge cycles 1000 times.
Brief description of the drawings
Fig. 1 is present invention gained MoSe2The XRD of-OMC compounds.
Fig. 2 is present invention gained MoSe2The SEM figures of-OMC compounds.
Fig. 3 is present invention gained MoSe2The TEM figures of-OMC compounds.
Fig. 4 is present invention gained MoSe2The chemical property figure of-OMC compounds.
Embodiment
In order that content of the present invention easily facilitates understanding, with reference to embodiment to of the present invention Technical scheme is described further, but the present invention is not limited only to this.
Embodiment 1
1）50mg ordered mesopore carbons are washed into 1h with concentrated nitric acid, is then washed and centrifuged 3 times with deionized water and ethanol respectively, it is standby With；
2）100mg phosphomolybdic acids are dissolved in 10mL ethanol, step 1 is then added）The ordered mesopore carbon pre-processed, stirring is extremely Ethanol volatilizees completely, with after drying in 70 DEG C of baking ovens；
3）By step 2）Gained sample is placed in tube furnace simultaneously with 200mg selenium powders, in H2/ Ar mixed atmospheres（Volume ratio 5:95） In, in calcining 1h at 800 DEG C, after after tube furnace natural cooling, produce MoSe2- OMC compounds.
Embodiment 2
1）100mg ordered mesopore carbons are washed into 1h with concentrated nitric acid, is then washed and centrifuged 3 times with deionized water and ethanol respectively, It is standby；
2）50mg phosphomolybdic acids are dissolved in 1mL ethanol, step 1 is then added）The ordered mesopore carbon pre-processed, stirring to second Alcohol volatilizees completely, with after drying in 70 DEG C of baking ovens；
3）By step 2）Gained sample is placed in tube furnace simultaneously with 50mg selenium powders, in H2/ Ar mixed atmospheres（Volume ratio 5:95） In, in calcining 12h at 500 DEG C, after after tube furnace natural cooling, produce MoSe2- OMC compounds.
Embodiment 3
1）80mg ordered mesopore carbons are washed into 1h with concentrated nitric acid, is then washed and centrifuged 3 times with deionized water and ethanol respectively, it is standby With；
2）70mg phosphomolybdic acids are dissolved in 5mL ethanol, step 1 is then added）The ordered mesopore carbon pre-processed, stirring to second Alcohol volatilizees completely, with after drying in 70 DEG C of baking ovens；
3）By step 2）Gained sample is placed in tube furnace simultaneously with 150mg selenium powders, in H2/ Ar mixed atmospheres（Volume ratio 5:95） In, in calcining 6h at 600 DEG C, after after tube furnace natural cooling, produce MoSe2- OMC compounds.
Fig. 1 is the gained MoSe of embodiment 32The XRD of-OMC compounds.It can be seen that MoSe2- OMC compounds by MoSe2With semi-graphited carbon composition, wherein MoSe2Belong to hexagonal crystal system, match with standard card 077-1715.
Fig. 2 is the gained MoSe of embodiment 32The SEM figures of-OMC compounds.It can be seen that MoSe2- OMC compounds are presented Micron order Rod-like shape.
Fig. 3 is the gained MoSe of embodiment 32The TEM figures of-OMC compounds.It can be seen that the MoSe of layer structure2Nanometer It is distributed in the duct of ordered mesopore carbon uniform particle.
Battery is assembled：By the gained MoSe of embodiment 32- OMC compounds and Kynoar, acetylene black in mass ratio 80: 10:Work electrode be equably coated on copper foil after 10 mixed grindings, reference electrode and be lithium metal to electrode, electrolyte is 1M LiPF6EC+DMC+EMC（Volume ratio：EC/DMC/EMC=1/1/1）Solution, test is used as using CR2025 type button cells Carrier（All assemblings are carried out in the glove box with inert atmosphere protection）.
Fig. 4 is the gained MoSe of embodiment 32The chemical property figure of-OMC compounds.It can be seen that by the lithium of its assembling Ion battery still has 451 mAh/g capacity when current density is 2 A/g after charge and discharge cycles 1000 times, while also showing Go out good high rate performance.
The foregoing is only presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with Modification, should all belong to the covering scope of the present invention.

Claims (4)

1. a kind of MoSe2The preparation method of-OMC compounds, it is characterised in that：Comprise the following steps：
1）Ordered mesopore carbon is washed into 1h with concentrated nitric acid, is then washed and centrifuged 3 times with deionized water and ethanol respectively, it is standby；
2）By phosphomolybdic acid dissolving in ethanol, step 1 is then added）The ordered mesopore carbon pre-processed, is stirred complete to ethanol Volatilization, with after 70 DEG C of drying；
3）By step 2）Gained sample is placed in tube furnace simultaneously with selenium powder, in reducibility gas atmosphere, at 500-800 DEG C 1-12h is calcined, after after tube furnace natural cooling, the MoSe is produced2- OMC compounds.
2. MoSe according to claim 12The preparation method of-OMC compounds, it is characterised in that：Ordered mesopore carbon used, phosphorus The weight ratio of molybdic acid and selenium powder is 1-2:1-2:1-4.
3. MoSe according to claim 12The preparation method of-OMC compounds, it is characterised in that：The reducibility gas is by H2 Gas and Ar gas by volume 5:95 mix.
4. MoSe prepared by a kind of method as claimed in claim 12- OMC compounds are in as lithium ion battery negative material Using.
CN201710434576.2A 2017-06-09 2017-06-09 MoSe2The preparation of OMC compounds and its application in lithium ion battery Pending CN107275603A (en)

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Cited By (8)

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Publication number Priority date Publication date Assignee Title
CN108767223A (en) * 2018-05-28 2018-11-06 福州大学 A kind of preparation method of micro-nano structure algaroth-carbon complex lithium ion battery negative material
CN109742368A (en) * 2019-01-08 2019-05-10 福建师范大学 A kind of preparation for lacking the compound anode material of lithium-ion battery of layer with the long-life
CN109742361A (en) * 2019-01-08 2019-05-10 福建师范大学 A kind of preparation method and application of compound anode material of lithium-ion battery
CN109742362A (en) * 2019-01-08 2019-05-10 福建师范大学 A kind of tin dope induction synthesis mixed phase molybdenum disulfide-derivative carbon composite preparation of chlorella and application
CN109742360A (en) * 2019-01-08 2019-05-10 福建师范大学 There is one kind high capacity selenizing molybdenum-chlorella derived carbon to lack the preparation of layer compound cell negative electrode material
CN110265637A (en) * 2019-05-18 2019-09-20 福建师范大学福清分校 A kind of synthetic method and application of the derivative porous carbon complex anode material of lithium-ion battery of the tungsten selenide of excellent properties-collagen
CN110635112A (en) * 2019-09-25 2019-12-31 福州大学 Molybdenum selenide-graphite-based bi-ion battery and preparation method thereof
CN113948703A (en) * 2021-10-15 2022-01-18 海南大学 MoSe used as lithium ion battery cathode2/NC submicron sphere composite material

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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108767223A (en) * 2018-05-28 2018-11-06 福州大学 A kind of preparation method of micro-nano structure algaroth-carbon complex lithium ion battery negative material
CN109742360B (en) * 2019-01-08 2022-03-29 福建师范大学 Preparation method of high-capacity molybdenum selenide-chlorella derived carbon-less-layer composite battery anode material
CN109742368A (en) * 2019-01-08 2019-05-10 福建师范大学 A kind of preparation for lacking the compound anode material of lithium-ion battery of layer with the long-life
CN109742361A (en) * 2019-01-08 2019-05-10 福建师范大学 A kind of preparation method and application of compound anode material of lithium-ion battery
CN109742362A (en) * 2019-01-08 2019-05-10 福建师范大学 A kind of tin dope induction synthesis mixed phase molybdenum disulfide-derivative carbon composite preparation of chlorella and application
CN109742360A (en) * 2019-01-08 2019-05-10 福建师范大学 There is one kind high capacity selenizing molybdenum-chlorella derived carbon to lack the preparation of layer compound cell negative electrode material
CN109742361B (en) * 2019-01-08 2021-09-28 福建师范大学 Preparation method and application of composite sodium-ion battery negative electrode material
CN109742362B (en) * 2019-01-08 2021-09-28 福建师范大学 Preparation and application of tin-doped induced synthesized 1T-2H mixed phase few-layer molybdenum disulfide-chlorella derived carbon composite material
CN109742368B (en) * 2019-01-08 2022-02-22 福建师范大学 Preparation of long-life few-layer composite sodium-ion battery negative electrode material
CN110265637A (en) * 2019-05-18 2019-09-20 福建师范大学福清分校 A kind of synthetic method and application of the derivative porous carbon complex anode material of lithium-ion battery of the tungsten selenide of excellent properties-collagen
CN110265637B (en) * 2019-05-18 2022-07-12 福建师范大学福清分校 Synthesis method and application of tungsten selenide-collagen derived porous carbon composite sodium ion battery cathode material with excellent performance
CN110635112A (en) * 2019-09-25 2019-12-31 福州大学 Molybdenum selenide-graphite-based bi-ion battery and preparation method thereof
CN110635112B (en) * 2019-09-25 2022-05-24 福州大学 Molybdenum selenide-graphite-based bi-ion battery and preparation method thereof
CN113948703A (en) * 2021-10-15 2022-01-18 海南大学 MoSe used as lithium ion battery cathode2/NC submicron sphere composite material

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