CN111354935A - Defect-rich rhenium sulfide/nitrogen-doped biomass-based carbon fiber composite material and preparation method thereof - Google Patents

Defect-rich rhenium sulfide/nitrogen-doped biomass-based carbon fiber composite material and preparation method thereof Download PDF

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CN111354935A
CN111354935A CN202010211101.9A CN202010211101A CN111354935A CN 111354935 A CN111354935 A CN 111354935A CN 202010211101 A CN202010211101 A CN 202010211101A CN 111354935 A CN111354935 A CN 111354935A
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nitrogen
carbon fiber
based carbon
composite material
fiber composite
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刘天西
宗伟
赖飞立
缪月娥
欧阳玥
郭和乐
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Donghua University
National Dong Hwa University
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Donghua 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
    • H01M4/362—Composites
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/51—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof
    • D06M11/53—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with hydrogen sulfide or its salts; with polysulfides
    • 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
    • H01M4/58—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
    • H01M4/581—Chalcogenides or intercalation compounds thereof
    • H01M4/5815—Sulfides
    • 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
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/40—Fibres of carbon
    • 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 discloses a defect-rich rhenium sulfide/nitrogen-doped biomass-based carbon fiber composite material which is characterized in that a defect-rich rhenium sulfide/nitrogen-doped biomass-based carbon fiber composite material is obtained by growing a rhenium sulfide nanosheet on the surface of a nitrogen-doped biomass-based carbon fiber in situ. The rhenium sulfide nanosheets in the composite material prepared by the method uniformly grow on the surface of the nitrogen-doped biomass-based carbon fiber, the composite material has the advantages of large specific surface area, good conductivity, stable physical and chemical properties and the like, and the defect-rich structure provides more effective ways for the rapid transmission of lithium ions, so that the composite material has excellent electrochemical performance.

Description

Defect-rich rhenium sulfide/nitrogen-doped biomass-based carbon fiber composite material and preparation method thereof
Technical Field
The invention belongs to the technical field of metal sulfide-carbon materials, and particularly relates to a defect-rich rhenium sulfide/nitrogen-doped biomass-based carbon fiber composite material and a preparation method thereof.
Background
The wide application of the lithium ion battery is a cornerstone developed by many industries at present, most portable electronic devices need the lithium ion battery to provide electric energy at present, and higher requirements are provided for the energy density and the power density of the lithium ion battery. However, the capacity of conventional electrode materials has almost reached a bottleneck. Therefore, research and development of the high-specific-capacity negative electrode material are the key points for improving the energy/power density of the lithium ion battery, and are important bases for development and application of the lithium ion battery. However, high specific capacity negative electrode materials represented by transition metal sulfides and the like are accompanied by severe electrode volume expansion and contraction during charging and discharging, thereby causing collapse and destruction of an electrode structure, resulting in poor cycle stability and rate capability. Therefore, the development and commercial application of high specific capacity anode materials are greatly limited.
Rhenium sulfide (ReS)2) As an emerging member of transition metal sulfides, there are typically two-dimensional layered structures. On the premise of ensuring the efficient diffusion and transmission of lithium ions, the extremely weak van der waals interaction between the rhenium sulfide layers greatly relieves the volume expansion effect brought by the lithium ion embedding/removing process, and brings new eosin for the development of the next generation of lithium ion battery electrode material. Therefore, it is very important to reasonably design the rhenium sulfide material and study the electrochemical behavior of the rhenium sulfide material in the working of the lithium ion battery.
Disclosure of Invention
The invention aims to solve the technical problem of providing a defect-rich rhenium sulfide/nitrogen-doped biomass-based carbon fiber composite material with simple preparation process, low cost and excellent lithium ion battery performance and a preparation method thereof.
In order to achieve the purpose, the invention provides a defect-rich rhenium sulfide/nitrogen-doped biomass-based carbon fiber composite material, which is characterized in that a defect-rich rhenium sulfide/nitrogen-doped biomass-based carbon fiber composite material is obtained by growing a rhenium sulfide nanosheet on the surface of a nitrogen-doped biomass-based carbon fiber in situ.
The invention also provides a preparation method of the defect-rich rhenium sulfide/nitrogen-doped biomass-based carbon fiber composite material, which is characterized by comprising the following steps of: dissolving ammonium perrhenate, thiourea and hydroxylamine hydrochloride in deionized water, and performing ultrasonic treatment to uniformly disperse the ammonium perrhenate, the thiourea and the hydroxylamine hydrochloride to obtain a mixed solution; adding the nitrogen-doped biomass-based carbon fiber into the mixed solution; transferring the mixture into a hydrothermal kettle to heat for hydrothermal reaction; and after the reaction is finished, cooling to room temperature, washing the product by using a mixed solution of ethanol and water, and drying to obtain the defect-rich rhenium sulfide/nitrogen-doped biomass-based carbon fiber composite material.
Preferably, the molar ratio of the ammonium perrhenate to the thiourea to the hydroxylamine hydrochloride is (1-3) to (1-5) to (1-3).
More preferably, the molar ratio of the ammonium perrhenate, the thiourea and the hydroxylamine hydrochloride is 1:2.2: 2.
Preferably, the hydrothermal reaction temperature is 180-220 ℃, and the reaction time is 20-26 h.
More preferably, the hydrothermal reaction temperature is 200 ℃ and the reaction time is 24 h.
Preferably, the drying is at 80 ℃ for 10-14 h.
More preferably, the drying is at 80 ℃ for 12 h.
The invention also provides application of the defect-rich rhenium sulfide/nitrogen-doped biomass-based carbon fiber composite material in a lithium ion battery.
The defect-rich rhenium sulfide nanosheets in the composite material prepared by the method uniformly grow on the surface of the nitrogen-doped biomass-based carbon fiber, so that the problem that rhenium sulfide is easy to agglomerate in the synthesis process is solved. The active surface area of the rhenium sulfide is greatly increased, so that the composite material has the advantages of large specific surface area, good conductivity, stable physical and chemical properties and the like. The defect-rich structure of the rhenium sulfide nanosheet in the composite material provides more effective ways for the rapid transmission of lithium ions, so that the composite material shows excellent electrochemical performance.
Compared with the prior art, the invention has the following remarkable advantages:
1. the invention introduces a defect structure into the conventional rhenium sulfide, and is a simple and efficient modification method.
2. The nitrogen-doped biomass-based carbon fiber is used as a substrate, and the rhenium sulfide nanosheets are uniformly grown on the surface of the substrate, so that the problem that rhenium sulfide is easy to agglomerate in the synthesis process is avoided, and the active surface area of rhenium sulfide is greatly increased.
3. The defect-rich rhenium sulfide/nitrogen-doped biomass-based carbon fiber composite material prepared by the invention has the advantages of large specific surface area, good conductivity, stable physical and chemical properties and the like. Meanwhile, abundant defect structures in rhenium sulfide provide more effective ways for the rapid transmission of lithium ions, so that the rhenium sulfide has excellent electrochemical performance.
4. The invention prepares a rhenium sulfide/nitrogen-doped biomass-based carbon fiber composite material rich in defects based on rhenium sulfide with a defect-rich structure and a strategy of taking nitrogen-doped biomass-based carbon fibers as a substrate. Meanwhile, the existence of the nitrogen-doped biomass-based carbon fiber substrate not only avoids the serious agglomeration phenomenon of rhenium sulfide, but also greatly improves the conductivity of the composite material; the defect-rich structure in the rhenium sulfide can also obviously improve the electrochemical performance of the rhenium sulfide as the electrode material of the lithium ion battery. The composite material developed based on the design strategy has a good application prospect in the field of alkali metal-based battery cathode materials.
Drawings
FIG. 1 is a flow diagram of the preparation of a defect-rich rhenium sulfide/nitrogen doped biomass-based carbon fiber composite of the present invention;
fig. 2 is an X-ray diffraction (XRD) pattern of a deficient enriched rhenium sulfide/nitrogen doped biomass-based carbon fiber composite prepared in example 2 of the present invention;
FIG. 3 is a Scanning Electron Microscope (SEM) image of a defect-rich rhenium sulfide/nitrogen doped biomass-based carbon fiber composite prepared in example 2 of the invention;
fig. 4 is a performance spectrum of a lithium ion battery obtained when the defect-rich rhenium sulfide/nitrogen-doped biomass-based carbon fiber composite material prepared in example 2 of the invention is used as an electrode material of the lithium ion battery; wherein, the curve a is a cyclic voltammetry Curve (CV) curve of the obtained defect-rich rhenium sulfide/nitrogen-doped biomass-based carbon fiber composite material, and the curve b is a corresponding rate performance curve.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
The reagents used in the examples of the invention were as follows:
ammonium perrhenate (national chemical group, chemical reagent limited), thiourea (national chemical group, chemical reagent limited), hydroxylamine hydrochloride (national chemical group, chemical reagent limited); reference to a method for preparing nitrogen-doped biomass-based carbon fibers (Small2017,13,1602866).
Example 1
As shown in fig. 1, this example provides a defect-rich rhenium sulfide/nitrogen-doped biomass-based carbon fiber composite material, which includes the following specific steps:
dissolving ammonium perrhenate, thiourea and hydroxylamine hydrochloride in deionized water according to the molar ratio of 1:2.2:3, and performing ultrasonic treatment for 10min to uniformly disperse the ammonium perrhenate, the thiourea and the hydroxylamine hydrochloride to obtain a mixed solution; adding the nitrogen-doped biomass-based carbon fiber into the mixed solution, and carrying out ultrasonic treatment for 1 h; transferring the mixture into a hydrothermal kettle, heating the mixture to perform hydrothermal reaction at the temperature of 200 ℃ for 24 hours; after the reaction is finished, cooling to room temperature, washing the product by using a mixed solution of ethanol and water, and drying at 80 ℃ for 12 hours; obtaining the defect-rich rhenium sulfide/nitrogen-doped biomass-based carbon fiber composite material.
Example 2
The embodiment provides a defect-rich rhenium sulfide/nitrogen-doped biomass-based carbon fiber composite material, which comprises the following specific steps:
dissolving ammonium perrhenate, thiourea and hydroxylamine hydrochloride in deionized water according to the molar ratio of 1:2.2:2, and performing ultrasonic treatment for 10min to uniformly disperse the ammonium perrhenate, the thiourea and the hydroxylamine hydrochloride to obtain a mixed solution; adding the nitrogen-doped biomass-based carbon fiber into the mixed solution, and carrying out ultrasonic treatment for 1 h; transferring the mixture into a hydrothermal kettle, heating the mixture to perform hydrothermal reaction at the temperature of 200 ℃ for 24 hours; after the reaction is finished, cooling to room temperature, washing the product by using a mixed solution of ethanol and water, and drying at 80 ℃ for 12 hours; obtaining the defect-rich rhenium sulfide/nitrogen-doped biomass-based carbon fiber composite material.
The defect-rich rhenium sulfide/nitrogen-doped biomass-based carbon fiber composite material obtained in example 2 is characterized and tested by using X-ray diffraction, a scanning electron microscope and an electrochemical workstation, and the structure and the performance of the preparation method are as follows:
(1) XRD test results show that: as shown in fig. 2, the results of XRD patterns indicate that the defect-rich rhenium sulfide/nitrogen-doped biomass-based carbon fiber composite obtained in the experiment shows distinct 4 diffraction patterns at 2 θ ═ 14.5 °, 33.2 °, 43.3 °, and 57.9 °, which proves the successful preparation of the defect-rich rhenium sulfide/nitrogen-doped biomass-based carbon fiber composite, and this also directly illustrates that the preparation method provided by the present invention is feasible.
(2) The SEM test results show that: as shown in fig. 3, the defect-rich rhenium sulfide nanosheets are uniformly coated on the surface of the nitrogen-doped biomass-based carbon fiber, so that agglomeration of the rhenium sulfide nanosheets is avoided, and the diameter of the composite material is about 100 nm.
(4) The electrochemical test results show that: the close coincidence of the CV curves of the second circle and the fifth circle in fig. 4a indicates that the defect-rich rhenium sulfide/nitrogen-doped biomass-based carbon fiber composite material has good electrochemical reversibility; fig. 4b shows that the defect-rich rhenium sulfide/nitrogen-doped biomass-based carbon fiber composite material has good rate capability.

Claims (9)

1. The defect-rich rhenium sulfide/nitrogen-doped biomass-based carbon fiber composite material is characterized in that a defect-rich rhenium sulfide/nitrogen-doped biomass-based carbon fiber composite material is obtained by growing a rhenium sulfide nanosheet on the surface of a nitrogen-doped biomass-based carbon fiber in situ.
2. The method of preparing a deficient enriched rhenium sulfide/nitrogen doped biomass-based carbon fiber composite of claim 1, comprising: dissolving ammonium perrhenate, thiourea and hydroxylamine hydrochloride in deionized water, and performing ultrasonic treatment to uniformly disperse the ammonium perrhenate, the thiourea and the hydroxylamine hydrochloride to obtain a mixed solution; adding the nitrogen-doped biomass-based carbon fiber into the mixed solution; transferring the mixture into a hydrothermal kettle to heat for hydrothermal reaction; and after the reaction is finished, cooling to room temperature, washing the product by using a mixed solution of ethanol and water, and drying to obtain the defect-rich rhenium sulfide/nitrogen-doped biomass-based carbon fiber composite material.
3. The method of making a deficient rich rhenium sulfide/nitrogen doped biomass-based carbon fiber composite of claim 2, wherein the molar ratio of ammonium perrhenate, thiourea, hydroxylamine hydrochloride is (1-3) to (1-5) to (1-3).
4. The method for preparing the enriched rhenium sulfide/nitrogen-doped biomass-based carbon fiber composite material as claimed in claim 3, wherein the molar ratio of the ammonium perrhenate, the thiourea and the hydroxylamine hydrochloride is 1:2.2: 2.
5. The method for preparing the rhenium/nitrogen-doped biomass-based carbon fiber composite material rich in defects as claimed in claim 2, wherein the hydrothermal reaction temperature is 180-220 ℃, and the reaction time is 20-26 h.
6. The method for preparing the rhenium/nitrogen-enriched doped biomass-based carbon fiber composite material with rich defects according to claim 6, wherein the hydrothermal reaction temperature is 200 ℃ and the reaction time is 24 h.
7. The method for preparing a rhenium/nitrogen-enriched doped biomass-based carbon fiber composite material as claimed in claim 2, wherein the drying is performed at 80 ℃ for 10-14 h.
8. The method of preparing a deficient enriched rhenium sulfide/nitrogen doped biomass-based carbon fiber composite of claim 8, wherein the drying is at 80 ℃ for 12 hours.
9. Use of the deficient enriched rhenium sulfide/nitrogen doped biomass-based carbon fiber composite of claim 1 in a lithium ion battery.
CN202010211101.9A 2020-03-24 2020-03-24 Defect-rich rhenium sulfide/nitrogen-doped biomass-based carbon fiber composite material and preparation method thereof Pending CN111354935A (en)

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