CN107221635B - Carbon fiber/MoS with wire structure2/MoO2Flexible electrode material and preparation method thereof - Google Patents
Carbon fiber/MoS with wire structure2/MoO2Flexible electrode material and preparation method thereof Download PDFInfo
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- 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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Abstract
The invention discloses a carbon fiber/MoS with an electric wire structure2/MoO2A flexible electrode material and a preparation method thereof belong to the field of electrochemistry and new energy materials. The inner layer of the electrode material structure is carbon fiber, the middle layer is molybdenum sulfide, the outermost layer is molybdenum oxide, and the three layers cover the wire structure. The inner-layer carbon fiber is used as an electron and ion transmission path, the middle-layer molybdenum sulfide provides high capacity, and the outer-layer molybdenum oxide coating can improve the capacity of the material and the conductivity of the material. The wire structure material is used as a lithium ion battery cathode material. According to the invention, the wet tissue is subjected to impurity removal treatment and then is calcined at high temperature, the wet tissue is carbonized at high temperature to form flexible carbon fibers, and then the flexible carbon fibers are hydrothermally formed with sodium molybdate and thiourea to form carbon fiber/MoS2A composite material. The composite material is further calcined in oxygen at low temperature to form the carbon fiber/MoS with the wire structure2/MoO2A flexible electrode material. The three-layer coated wire structure material obviously improves the specific capacity and the cycling stability of the material.
Description
Technical Field
The invention discloses a carbon fiber/MoS with an electric wire structure2/MoO2A flexible electrode material and a preparation method thereof belong to the field of electrochemistry and new energy materials.
Background
The flexible electronic device capable of being bent and folded is widely favored by people in recent years, and the flexible lithium ion battery is a core component of the flexible electronic device. The traditional lithium ion battery negative electrode material takes copper foil as a current collector, and the energy density of the battery is reduced by the copper foil current collector. Under the condition of large bending deformation, the active material is easy to separate from the current collector, and the electrochemical performance of the material is further influenced. The self-supporting flexible electrode material without the binder, the conductive agent and the current collector can obviously improve the energy density of the material and the electrochemical performance under the bending condition.
The molybdenum sulfide is used as a lithium ion battery cathode material, the characteristic of large interlayer spacing is beneficial to the diffusion of lithium ions, and the molybdenum sulfide has the advantage of high capacity when used as a lithium ion battery cathode material. But molybdenum sulfide shows poor stability and fast energy attenuation due to a lithium intercalation/lithium deintercalation reaction mechanism in the charging and discharging processes. The electrochemical resistance in the nanometer material is reduced through the coating of the molybdenum oxide, so that the conductivity and the stability of the material are increased. The CN201611175666.6 patent discloses a core-shell spherical MoO3/MoS2And preparation method thereof, and prepared core-shell spherical MoO3/MoS2Has excellent photocatalytic effect, and is added with a small amount of core-shell spherical MoO3/MoS2The full photocatalytic degradation of the organic dye can be finished in a short time. The invention discloses a tubular molybdenum disulfide nano material in the patent of CN201610323796.3, the molybdenum disulfide nano material prepared by the invention has the advantages of high specific surface area, high purity and uniform appearance, has higher energy density and better circulation stability when being used as an electrode material of a lithium ion battery, effectively improves the agglomeration phenomenon, reduces the structural damage and further improves the circulation stability of the battery. The CN201610799898.2 patent discloses a carbon nanotube/molybdenum disulfide nanosphere composite material, which shows excellent electrochemical performance as a super-capacitor electrode material, has a simple preparation process, is green and environment-friendly, and has huge potential application in the field of super-capacitors, lithium ion batteries and other equipment as a novel energy material. Comprehensive MoS2And MoO2The invention relates to a wire structure carbon fiber/MoS2/MoO2A flexible electrode material and a preparation method thereof. The material structure is similar to an electric wire structure, the inner layer is carbon fiber, the middle layer is molybdenum sulfide, the outermost layer is molybdenum oxide, and the electric wire structure is coated by three layers. The three-layer coated wire structure effectively improves the specific capacity and the rate capability of the materialAnd cycle performance.
Disclosure of Invention
The invention aims to provide a carbon fiber/MoS with a wire structure2/MoO2A flexible electrode material. The material is prepared by pretreating commercial wet paper towel, calcining at 800 ℃ for 4h under nitrogen atmosphere to obtain flexible carbon fiber paper, hydrothermally mixing the flexible carbon fiber paper with sodium molybdate and thiourea in a certain ratio, drying, and calcining at low temperature for 1h under oxygen atmosphere. Finally forming the carbon fiber/MoS of the wire structure2/MoO2Flexible electrode material, carbon fiber/MoS of the wire structure2/MoO2The flexible electrode material can be directly used as a lithium ion battery cathode material, and a binder and a current collector are not required to be added, so that the energy density of the whole electrode is effectively improved.
The purpose of the invention is realized as follows: carbon fiber/MoS with wire structure2/MoO2The preparation method of the flexible electrode material comprises the following process steps:
(1) 1mol L of wet tissue-1Then transferring the wet tissue into a mixed solution of absolute ethyl alcohol/acetone (1: 1) to be soaked for 6 hours. And then washing the obtained wet tissue with absolute ethyl alcohol and deionized water for 3-5 times, and then drying in a drying oven at 60 ℃ for 12h to obtain the processed wet tissue. The purpose of treating wet tissue is to remove impurities contained in the wet tissue.
(2) And (3) calcining the material in the step (2) for 4h at 800 ℃ in a nitrogen atmosphere to form the flexible carbon fiber.
(3) And (3) placing the flexible carbon fiber obtained in the step (2), 0.24g of sodium molybdate (molybdenum source) and 0.76g of thiourea (sulfur source) in a hydrothermal kettle, performing hydrothermal treatment at 200 ℃ for 24 hours to obtain molybdenum sulfide coated on the surface of the carbon fiber, and further drying. Molybdenum sulfide is attached to the surface of the carbon fiber to obtain the carbon fiber/MoS with the wire structure2A flexible electrode material. The mass ratio of the carbon fiber paper to the sodium molybdate to the thiourea is 1: 2-5: 5-10.
(4) Mixing carbon fiber/MoS2Calcining the material for 1h at 500 ℃ in an oxygen atmosphere to form a molybdenum oxide-coated molybdenum sulfide three-layer structure, and finally obtaining the carbon fiber with the wire structurevitamin/MoS2/MoO2A flexible electrode material.
The wet tissue is a wet tissue of a Weida brand.
The invention provides a wire structure carbon fiber/MoS2/MoO2The flexible electrode material has the following beneficial effects:
(1) the prepared material electrode combines MoS2And MoO2The two advantages are used as the lithium ion battery cathode material, and are beneficial to improving the conductivity and the cycling stability of the electrode material.
(2) The electric wire structure carbon fiber/MoS prepared by the method2/MoO2The flexible electrode material has a three-layer wire conductive structure, provides a channel for the transmission of lithium ions, and improves the stability and the conductivity of the material because molybdenum sulfide is coated by molybdenum oxide.
(3) The electric wire structure carbon fiber/MoS prepared by the method2/MoO2The flexible electrode material does not need additives such as a metal current collector, a binder, conductive carbon and the like, is directly used as an electrode material, is beneficial to improving the energy density and the power density of an electrode, and can also be used as a light-weight flexible current collector.
Drawings
FIG. 1 shows a carbon fiber/MoS wire structure prepared in example 1 of the present invention2/MoO2A flexible electrode material.
FIG. 2 shows a carbon fiber/MoS wire structure prepared in example 1 of the present invention2/MoO2Flexible electrode material and carbon fiber/MoS2An X-ray diffraction (XRD) pattern of the material.
FIG. 3 shows a carbon fiber/MoS wire structure prepared in example 1 of the present invention2/MoO2Scanning Electron Micrographs (SEM) of flexible electrode material at different magnifications.
FIG. 4, a shows the carbon fiber/MoS wire structure prepared in example 12/MoO2Taking the flexible electrode material as a previous 3-time charge-discharge curve of the lithium ion battery cathode material; panel b is the preparation of carbon fiber/MoS of example 12The flexible electrode material is used as the previous 3-time charge-discharge curve of the lithium ion battery cathode material.
FIG. 5 shows a wire-structured carbon fiber/MoS prepared in example 1 of the present invention2/MoO2Flexible electrode material and carbon fiber/MoS2And comparing the cycle performance of the flexible electrode material.
FIG. 6 shows a wire-structured carbon fiber/MoS prepared in example 1 of the present invention2/MoO2Cyclic voltammogram of a flexible electrode material.
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1: wire structure carbon fiber/MoS2/MoO2Flexible electrode material I
Adding wet tissue in 1mol L-1Is soaked in dilute hydrochloric acid for 12 hours, and then the wet tissue is transferred to absolute ethyl alcohol/acetone in a volume ratio of 1:1 for 6 hours, then washing the obtained wet tissue with absolute ethyl alcohol and deionized water for 3-5 times, then putting the wet tissue into a drying oven at 60 ℃ for drying for 12 hours to obtain the processed wet tissue, then calcining the processed wet tissue in a tube furnace at 800 ℃ for 4 hours, and putting the wet tissue, 0.24g of sodium molybdate and 0.76g of thiourea into a hydrothermal kettle for hydrothermal reaction at 200 ℃ for 24 hours. During hydrothermal process, sodium molybdate and thiourea form MoS2Coating carbon fiber surface to obtain flexible carbon fiber/MoS2A flexible material. Finally, calcining the material in oxygen at the low temperature of 500 ℃ for 1h to finally form the carbon fiber/MoS with the wire structure2/MoO2A flexible electrode material. The electrode is directly used as a working electrode, a lithium sheet is used as a counter electrode, and the electrolyte is a universal lithium ion battery electrolyte 1M LiPF6EC =1: 1 DMC, a 2025 coin cell was prepared at 100mA g-1Charging and discharging the current density of (1). FIG. 1 shows a carbon fiber/MoS wire structure prepared2/MoO2The flexible electrode material is used for optical photos, and the electrode is a self-supporting electrode and can be directly used as an electrode. FIG. 2 shows a carbon fiber/MoS wire structure2/MoO2Flexible electrode material and carbon fiber/MoS2XRD diffraction pattern of the material shows that the carbon fiber/MoS2The material showed good MoS2Diffraction peaks, corresponding to cards 37-1492. Carbon fiber/MoS2The material is calcined in oxygen at 500 DEG CXRD pattern of the obtained material corresponds to MoS2And MoO2Mixed phases, corresponding to standard cards 37-1492 and 32-0671, respectively. The resulting material was further demonstrated to be carbon fiber/MoS2/MoO2The material, carbon fiber, is an amorphous structure. FIG. 3 is a carbon fiber/MoS2/MoO2Scanning electron microscope photograph of the material. As can be seen from the figure, the material is of a wire structure, the inner layer is made of carbon fiber, and the outer coating layer is made of MoS2A material. Due to MoS2Oxidation in oxygen to form MoO2So the outermost layer should be MoO2A material. The carbon fiber/MoS2/MoO2The flexible electrode material combines the excellent performances of molybdenum sulfide and molybdenum oxide and has a specific carbon fiber/MoS ratio2The material has better electrochemical performance. In FIG. 4, a and b are respectively the carbon fiber/MoS of the wire structure2/MoO2Flexible electrode material and wire structure carbon fiber/MoS2First three charge-discharge curves of the flexible electrode material. It can be seen that a in FIG. 4 shows carbon fiber/MoS2/MoO2The first discharge capacity of the composite material is 700.8mAh g-1The first charge capacity was 497.7 mAh g-1Discharge plateaus of 1.2V and 0.7V, corresponding to Li, respectivelyXMoS2And SEI film formation. The charging platforms were 1.5V, 1.7V and 2.2V. 1.5V and 1.7V correspond to LiXMoO2Formation of (2) and LiXMoO2Conversion reactions between different phases, 2.2V for Li2Oxidation of S to form MoS2The reaction of (1). B in FIG. 4 shows carbon fiber/MoS2The first discharge capacity of the lithium secondary battery is 698.6 mAh g-1Discharge plateaus of 1.2V and 0.7V, corresponding to Li, respectivelyXMoS2And SEI film formation. The first charge capacity is 450.6 mAh g-1The charging platform is 2.2V, and 2.2V corresponds to Li2Oxidation of S to MoS2The reaction of (1). FIG. 5 is a carbon fiber/MoS2/MoO2Flexible electrode material and carbon fiber/MoS2The cycle performance curve of the flexible electrode material can show that the carbon fiber/MoS2/MoO2The material has better cycle performance due to MoO2The material is activated in the course of reaction, so that the capacity is 40 circlesThere is a tendency for the capacity to rise during cycling. Carbon fiber/MoS2/MoO2Still has 546.7 mAh g-1Reversible capacity of (2), carbon fiber/MoS2Only 251.9 mAh g-1The reversible capacity of (a). This is because the molybdenum oxide in the outer layer particles is continuously activated during the charging and discharging process, providing space for the storage sites for lithium ions, and the capacity is further improved with the increase of the number of cycles. FIG. 6 shows a carbon fiber/MoS wire structure2/MoO2The cyclic voltammetry curve of the flexible electrode material has a reduction peak of 0.4V, and a reduction peak of 1.1V, 1.2V, 1.5V, 1.7V, and an oxidation peak of 1.5V, 1.7V, 2.2V in the first turn, which are identical to the charge-discharge curve of a in fig. 4.
Example 2 wire construction carbon fiber/MoS2/MoO2Flexible electrode material II
Adding wet tissue in 1mol L-1Soaking the wet tissue in dilute hydrochloric acid for 12 hours, transferring the wet tissue into a mixed solution of absolute ethyl alcohol and acetone according to the volume ratio of 1:1, soaking for 6 hours, then washing the obtained wet tissue for 3-5 times by using the absolute ethyl alcohol and deionized water, then drying for 12 hours in a 60 ℃ drying box, calcining the treated wet tissue in a tube furnace at 800 ℃ for 4 hours, and then putting the calcined wet tissue, 0.24g of sodium molybdate and 0.76g of thiourea into a hydrothermal kettle for hydrothermal reaction at 200 ℃ for 24 hours. During hydrothermal process, sodium molybdate and thiourea form MoS2Coating carbon fiber surface to obtain flexible carbon fiber/MoS2A flexible material. Then the material is calcined in oxygen at the low temperature of 600 ℃ for 1h to finally form the carbon fiber/MoS with the wire structure2/MoO2A flexible electrode material. The electrode material was tested as described in example 1, 100mA g as a negative electrode material for a lithium ion battery-1Charging and discharging at current density, and first reversible capacity of 650 mAh g-1Reversible capacity after 40 cycles of 620 mAh g-1。
Example 3 wire construction carbon fiber/MoS2/MoO2Flexible electrode material III
Adding wet tissue in 1mol L-1Soaking the wet tissue in the dilute hydrochloric acid for 12 hours, then transferring the wet tissue into a mixed solution of absolute ethyl alcohol and acetone in a volume ratio of 1:1, soaking for 6 hours, and then soaking the obtained wet tissue in the absolute ethyl alcohol,Washing with deionized water for 3-5 times, drying in a 60 ℃ drying oven for 12h to obtain the treated wet tissue, calcining in a tube furnace at 800 ℃ for 4h, and putting the wet tissue, 0.24g of sodium molybdate and 0.76g of thiourea in a hydrothermal kettle for hydrothermal treatment at 200 ℃ for 24 h. During hydrothermal process, sodium molybdate and thiourea form MoS2Coating carbon fiber surface to obtain flexible carbon fiber/MoS2A flexible material. Then the material is calcined in oxygen at the low temperature of 400 ℃ for 1h to finally form the carbon fiber/MoS with the wire structure2/MoO2A flexible electrode material. The electrode material was tested as described in example 1, 100mA g as a negative electrode material for a lithium ion battery-1Charging and discharging at current density, the first reversible capacity is 630mAh g-1Reversible capacity after 40 cycles of 593 mAh g-1。
Claims (4)
1. Carbon fiber/MoS with wire structure2/MoO2The preparation method of the flexible electrode material is characterized in that,
soaking wet tissue in 1mol/L dilute hydrochloric acid for 12h, transferring the wet tissue to a mixed solution of absolute ethyl alcohol and acetone according to the volume ratio of 1:1, soaking for 6h, then washing the obtained wet tissue for 3-5 times by using absolute ethyl alcohol and deionized water, then drying in a 60 ℃ drying box for 12h to obtain the treated wet tissue, calcining the treated wet tissue in a nitrogen atmosphere furnace at the temperature of 500 plus one year and 1200 ℃ for 1-10h, and then carrying out hydrothermal reaction with sodium molybdate and thiourea at the temperature of 90-200 ℃ for 1-24h to obtain the carbon fiber/MoS with the wire structure2The flexible electrode material is further calcined for 1-5h at the temperature of 200-500 ℃ in the oxygen atmosphere to obtain the carbon fiber/MoS with the wire structure2/MoO2The flexible electrode material is in a wire structure, the inner layer is carbon fiber, the middle layer is molybdenum sulfide, the outermost layer is molybdenum oxide, and the wire structure is coated by three layers.
2. Wire-structured carbon fiber/MoS according to claim 12/MoO2The preparation method of the flexible electrode material is characterized by comprising the following steps: and calcining the treated wet tissue paper at 800 ℃ under nitrogen to obtain the carbon fiber paper.
3. Wire-structured carbon fiber/MoS according to claim 22/MoO2The preparation method of the flexible electrode material is characterized by comprising the following steps: the mass ratio of the carbon fiber paper to the sodium molybdate to the thiourea is 1: 2-5: 5-10, mixing sodium molybdate, thiourea and carbon fiber paper for hydrothermal treatment, wherein the hydrothermal temperature is 200 ℃, the hydrothermal time is 24h, and the hydrothermal product is carbon fiber/MoS2A composite material.
4. Wire-structured carbon fiber/MoS according to claim 12/MoO2The preparation method of the flexible electrode material is characterized by comprising the following steps: carbon fiber/MoS2Calcining the flexible electrode material in oxygen at a low temperature of 500 ℃ for 1h to obtain the carbon fiber/MoS with the wire structure2/MoO2A flexible electrode material.
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| CN108636427B (en) * | 2018-04-27 | 2021-02-02 | 重庆文理学院 | Molybdenum disulfide-nitrogen sulfur doped graphite foil composite nanomaterial and preparation method thereof |
| CN111755672B (en) * | 2019-05-14 | 2021-11-12 | 中南大学 | Molybdenum disulfide coated molybdenum dioxide negative electrode material and preparation method and application thereof |
| CN111261430B (en) * | 2020-01-20 | 2022-04-26 | 陕西科技大学 | Nano needle-shaped cobalt nickel sulfide/carbon paper flexible electrode and preparation method thereof |
| CN114975941B (en) * | 2022-06-06 | 2023-12-15 | 郑州轻工业大学 | Tortoise-back bamboo-shaped MoO x /MoS 2 Hybrid material/C, preparation method and application thereof |
| CN114914098B (en) * | 2022-06-14 | 2023-05-12 | 湘潭大学 | Preparation method and application of waste wet towel derived nitrogen-oxygen-sulfur co-doped flexible carbon cloth |
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