CN107342404B - Carbon modified MoS2/MoO2Two-phase composite material and preparation method thereof - Google Patents
Carbon modified MoS2/MoO2Two-phase composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a carbon modified MoS2/MoO2A two-phase composite material and a preparation method thereof belong to the field of electrochemistry and new energy materials. The method directly mixes the graphene oxide with the carbon nano tube, ammonium molybdate and thiourea, uses dilute hydrochloric acid and sodium hydroxide to adjust the pH value of the solution, and then carries out hydrothermal treatment after stirring and ultrasonic treatment. Washing the product obtained by the hydrothermal method with deionized water and absolute ethyl alcohol for several times, then carrying out vacuum drying at normal temperature, and then calcining under the protection of atmosphere to obtain the target product. MoS can be prepared in one step by adjusting the pH value of the mixed solution2/MoO2A two-phase foam-like composite. The layered graphene and the rod-shaped carbon nano tube form a stable three-dimensional conductive network in the material, the molybdenum disulfide provides high specific capacitance, and the molybdenum dioxide improves the conductivity of the material. The foam composite material is used as a lithium ion battery cathode material, and shows high specific capacity and excellent cycling stability.
Description
Technical Field
The invention discloses a carbon modified MoS2/MoO2A two-phase foam composite material and a preparation method thereof belong to the field of electrochemistry and new energy materials.
Background
The molybdenum dioxide has a rutile structure, and the main structure of the molybdenum dioxide is formed by molybdenum ions and oxygen ions through [ MoO ]6]The octahedron is formed by sharing corners, lithium ions with small radius can be embedded into the octahedron and can enter between the octahedrons without reforming the structure, and the theoretical lithium embedding capacity of the lithium ion battery is 838 mAh/g which is far higher than that of the current commercial graphite negative electrode material; simultaneously has low metal resistivity (8.8 multiplied by 10)-5Ω.cm), high melting point, high chemical stabilityThe two-dimensional layered nano material is widely concerned due to a new method leading to a low-dimensional system, the molybdenum disulfide is a quasi-two-dimensional layered structure and presents a typical S-Mo-S three-layered structure, all layers of the molybdenum disulfide are mutually acted by Van der Waals force to be beneficial to the insertion of lithium ions, the theoretical capacity of the lithium ion battery cathode is large (~ 670 mAh/g), the molybdenum disulfide can generate volume change in the charging and discharging processes to damage the structure of the material so as to reduce the cycling stability of the material, David Mitlin and the like modify porous three-dimensional MoO through sulfur2To prepare a multi-layered MoS2Covering MoO2The three-dimensional nano porous reticular composite material used as the negative electrode of the lithium ion battery shows excellent performance, the first discharge specific capacity reaches 1233 mAh/g under the current density of 100 mA/g, and 1171 mAh/g (after being circulated for 80 times)J. Phys. Chem. C 2014, 118, 18387−18396）。
Disclosure of Invention
The invention aims to provide a carbon modified MoS2/MoO2A two-phase foam composite material and a preparation method thereof. Uniformly mixing graphene oxide with a carbon nano tube, tetrahydrate, ammonium molybdate and thiourea, carrying out hydrothermal treatment, carrying out normal-temperature vacuum drying on a hydrothermal product, and calcining the hydrothermal product in a protective atmosphere to finally form carbon modified MoS2/MoO2A biphasic material.
The purpose of the invention is realized as follows: carbon modified MoS2/MoO2The preparation method of the two-phase foam composite material comprises the steps of uniformly mixing graphene oxide with treated carbon nano tubes, ammonium molybdate tetrahydrate and thiourea, adjusting the pH value of a solution by using hydrochloric acid and sodium hydroxide, stirring, carrying out ultrasonic treatment, carrying out hydrothermal reaction, cleaning a hydrothermal product for a plurality of times by using deionized water and absolute ethyl alcohol, then carrying out vacuum drying at normal temperature, and calcining the material dried at normal temperature in vacuum in nitrogen atmosphere to obtain a target product, namely the carbon-modified MoS2/MoO2A dual phase foam composite.
The hydrothermal reaction temperature is 180-220 ℃, and the hydrothermal reaction time is 20-30 h.
In order to maintain its three-dimensional porous foam structure, the hydrothermal product was freeze-dried under vacuum at-50 ℃ for 24 h. The samples after freeze-drying retained a three-dimensional foam structure.
The calcination temperature is 600-900 ℃, and the calcination time is 2-6 h.
The treated carbon nanotube is the carbon nanotube in Ar/H2Calcining in atmosphere at 500-600 deg.c for 1-3 hr. Placing the calcined carbon nano-tube in HNO with the concentration of 70%3Soaking at 60 deg.C for 1-2 hr. The surface of the carbon nano tube after treatment contains oxygen-containing functional groups, and has good hydrophilicity.
The mass ratio of the graphene oxide to the treated carbon nano tube, ammonium molybdate tetrahydrate and thiourea is 1:1:1:2 ~ 7.
The pH value of the solution is adjusted to 3-12 by using hydrochloric acid and sodium hydroxide.
The invention provides a carbon modified MoS2/MoO2The two-phase foam composite material and the preparation method thereof have the following beneficial effects:
(1) the carbon modified MoS prepared by the method2/MoO2The two-phase foam composite material has simple experimental steps, namely, the two-phase material containing molybdenum disulfide and molybdenum dioxide is prepared by one-step hydrothermal method.
(2) The electrode material prepared by the method is a three-dimensional conductive network formed by graphene and carbon nanotubes, and can effectively improve the conductivity and the cycling stability of the material.
(3) Molybdenum sulfide provides high capacity, molybdenum oxide improves conductivity, and the two interact synergistically to improve the electrochemical performance of the composite material.
(4) The electrode material prepared by the method is a self-supporting flexible electrode material without a binder, a conductive agent and a current collector, and the energy density of the material can be remarkably improved.
(5) The electrode material prepared by the method is in a foam shape, and has light weight and good mechanical flexibility.
The invention adopts a simple method to prepare the carbon modified MoS2/MoO2The diphase foam composite material simultaneously contains molybdenum disulfide and molybdenum dioxide diphase, and the proportion of the molybdenum disulfide and the molybdenum dioxide can be controlled by adjusting the pH value of precursor mixed liquor. The material is in a foam shape, has lighter weight and better mechanical flexibility, and shows ultrahigh specific capacity and ultrahigh cycling stability performance when being used as a lithium ion battery cathode material. The method takes graphene and carbon nano tubes as modification materials, prepares molybdenum disulfide and molybdenum dioxide biphases by a hydrothermal method, and enables the molybdenum disulfide and the molybdenum dioxide biphases to grow on the surfaces of the carbon nano tubes. The method is not reported in any documents and patents.
Drawings
FIG. 1 shows a carbon modified MoS prepared in example 1 of the present invention2/MoO2Photograph of the two-phase foam composite.
FIG. 2 shows a carbon-modified MoS prepared in example 1 of the present invention2/MoO2An X-ray diffraction (XRD) pattern of the dual phase foam composite.
FIG. 3 shows a carbon modified MoS prepared in example 1 of the present invention2/MoO2Scanning Electron Micrographs (SEM) of the two-phase foam composite, wherein a is a drawing at a magnification of 30000 and b is a drawing at a magnification of 50000.
FIG. 4 shows a carbon modified MoS prepared in example 1 of the present invention2/MoO2First 2 charge and discharge curves for the dual phase foam composite.
FIG. 5 shows a carbon modified MoS prepared in example 1 of the present invention2/MoO2Cycling stability performance of the dual phase foam composite.
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1: carbon modified MoS2/MoO2Two-phase foam composite material and preparation method thereof
Mixing the prepared graphene oxide graphene (35 mL, 1 mg/mL) and the treated carbon nanotube (0.35 g), and tetrahydrate and ammonium molybdate (0.35 g), thiourea (0.8 g)Placing the mixture in a lining of a hydrothermal reaction kettle, and using dilute hydrochloric acid (1 mol L)-1) Adjusting the pH value of the precursor to be pH =6, stirring for 20 minutes, then carrying out ultrasonic treatment for 20 minutes, and then placing the precursor in a reaction kettle for hydrothermal treatment. The hydrothermal temperature is 200 ℃ and the hydrothermal time is 24 hours. Washing the hydrothermal product with deionized water and absolute ethyl alcohol for several times, freezing at low temperature, then carrying out normal-temperature vacuum drying for 24 hours, calcining the normal-temperature vacuum dried material in a nitrogen atmosphere at 800 ℃, and keeping the temperature for 4 hours to finally obtain the carbon modified MoS2/MoO2A dual phase foam composite. FIG. 1 is a schematic representation of the carbon modified MoS prepared2/MoO2Photograph of the two-phase foamed negative electrode material, it can be seen from the photograph that the material is foamed. FIG. 2 is a schematic representation of the carbon modified MoS prepared2/MoO2The XRD pattern of the two-phase foam cathode material can be compared with a standard card to prove that the material contains MoS2、MoO2Two phases. FIG. 3 is a carbon modified MoS prepared in2/MoO2SEM pictures of the two-phase foam composite material show that the graphene and the carbon nano tube form a conductive network. Meanwhile, a large number of carbon nanotubes are connected in a staggered manner from a high-power SEM, so that a good channel is provided for the transmission of electrons and the diffusion of ions. Prepared carbon modified MoS2/MoO2The dual phase foam composite material exhibits a higher specific capacity and excellent cycling stability performance. 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 100 mA g-1Charging and discharging the current density of (1). The first 2 charge-discharge curves of the electrode are shown in FIG. 5, and it can be seen that the first discharge capacity of the material is 700.8 mAh g-1First reversible charge capacity of 497 mAh g-1The second reversible capacity is 506.9 mAh g-1. After 150 cycles, the reversible charge capacity is 560 mAh g-1. As can be seen from the cycle performance chart, the material has good cycle performance.
Example 2A carbon modified MoS2/MoO2Two-phase foam composite material and preparation method II thereof
The prepared graphene (35 mL, 1 mg/mL) and treated carbon nanotubes (0.35 g), as well as tetrahydrate and ammonium molybdate (0.35 g), thiourea (0.8 g) were placed in the hydrothermal reaction kettle liner, diluted hydrochloric acid (1 mol L)-1) Adjusting the pH value of the precursor to be pH =5, stirring for 20 minutes, then carrying out ultrasonic treatment for 20 minutes, and then placing the precursor in a reaction kettle for hydrothermal treatment. The hydrothermal temperature is 200 ℃ and the hydrothermal time is 24 hours. Washing the hydrothermal product with deionized water and absolute ethyl alcohol for several times, freezing at low temperature, then carrying out normal-temperature vacuum drying for 24 hours, calcining the normal-temperature vacuum dried material in a nitrogen atmosphere at 800 ℃, and keeping the temperature for 4 hours to finally obtain the carbon modified MoS2/MoO2A dual phase foam composite. The electrode material was tested as described in example 1, using 100 mA g as the negative electrode material for lithium ion batteries-1The current density is charged and discharged, and the first reversible capacity is 620 mAh g-1The reversible capacity after 150 cycles was 530 m Ah g-1。
Example 3A carbon modified MoS2/MoO2Two-phase foam composite material and preparation method III thereof
The prepared graphene (35 mL, 1 mg/mL) and treated carbon nanotubes (0.35 g), as well as tetrahydrate and ammonium molybdate (0.35 g), thiourea (0.8 g) were placed in the hydrothermal reaction kettle liner, diluted hydrochloric acid (1 mol L)-1) Adjusting the pH value of the precursor to be pH =4, stirring for 20 minutes, then carrying out ultrasonic treatment for 20 minutes, and then placing the precursor in a reaction kettle for hydrothermal treatment. The hydrothermal temperature is 200 ℃ and the hydrothermal time is 24 hours. Washing the hydrothermal product with deionized water and absolute ethyl alcohol for several times, freezing at low temperature, then carrying out normal-temperature vacuum drying for 24 hours, calcining the normal-temperature vacuum dried material in a nitrogen atmosphere at 800 ℃, and keeping the temperature for 4 hours to finally obtain the carbon modified MoS2/MoO2A two-phase foam negative electrode material. The electrode material was tested as described in example 1, using 100 mA g as the negative electrode material for lithium ion batteries-1The current density is charged and discharged, and the first reversible capacity is 530 mAh g-1Reversible capacity after 150 cycles of420 mAh g-1。
Example 4A carbon modified MoS2/MoO2Two-phase foam composite material and preparation method IV thereof
The prepared graphene (35 mL, 1 mg/mL) and treated carbon nanotubes (0.35 g), as well as tetrahydrate and ammonium molybdate (0.35 g), thiourea (0.8 g) were placed in the hydrothermal reaction kettle liner, followed by sodium hydroxide (1 mol L)-1) Adjusting the pH value of the precursor to be pH =7, stirring for 20 minutes, then carrying out ultrasonic treatment for 20 minutes, and then placing the precursor in a reaction kettle for hydrothermal treatment. The hydrothermal temperature is 200 ℃ and the hydrothermal time is 24 hours. Washing the hydrothermal product with deionized water and absolute ethyl alcohol for several times, freezing at low temperature, then carrying out normal-temperature vacuum drying for 24 hours, calcining the normal-temperature vacuum dried material in a nitrogen atmosphere at 800 ℃, and keeping the temperature for 4 hours to finally obtain the carbon modified MoS2/MoO2A dual phase foam composite. The electrode material was tested as described in example 1, using 100 mA g as the negative electrode material for lithium ion batteries-1Charging and discharging at current density, and first reversible capacity of 690.5 mAh g-1And the reversible capacity after 150 cycles is 537 mAh g-1。
Example 5A carbon modified MoS2/MoO2Two-phase foam composite material and preparation method thereof
Placing the prepared graphene (35 mL, 1 mg/mL) and treated carbon nanotubes (0.35 g), tetrahydrate and ammonium molybdate (0.35 g) and thiourea (0.8 g) in a liner of a hydrothermal reaction kettle, adjusting the pH value of the precursor to be pH =8 by using sodium hydroxide, stirring for 20 minutes, performing ultrasonic treatment for 20 minutes, and then placing in the reaction kettle for hydrothermal treatment. The hydrothermal temperature is 200 ℃ and the hydrothermal time is 24 hours. Washing the hydrothermal product with deionized water and absolute ethyl alcohol for several times, freezing at low temperature, then carrying out normal-temperature vacuum drying for 24 hours, calcining the normal-temperature vacuum dried material in a nitrogen atmosphere at 800 ℃, and keeping the temperature for 4 hours to finally obtain the carbon modified MoS2/MoO2A two-phase foam negative electrode material. The electrode material was tested as a lithium ion battery under the conditions described in example 1Cell anode material at 100 mA g-1Charging and discharging at current density, and first reversible capacity of 510 mAh g-1And the reversible capacity after 150 cycles is 482 mAh g-1。
Claims (4)
1. Carbon modified MoS2/MoO2The preparation method of the two-phase foam composite material is characterized by comprising the following steps: uniformly mixing graphene oxide with treated carbon nano tubes, ammonium molybdate tetrahydrate and thiourea, adjusting the pH value of the solution by using hydrochloric acid and sodium hydroxide, stirring, performing ultrasonic hydrothermal reaction, cleaning the hydrothermal reaction product for several times by using deionized water and absolute ethyl alcohol, performing vacuum freeze drying at-50 ℃ for 24 hours, then performing vacuum drying at normal temperature, and calcining the material subjected to the vacuum drying at the normal temperature in a nitrogen atmosphere to obtain a target product, namely the carbon-modified MoS2/MoO2A dual phase foam composite; the treated carbon nanotube is the carbon nanotube in Ar/H2Calcining in atmosphere at 500-600 deg.C for 1-3 hr, and placing the calcined carbon nanotube in 70% HNO3Soaking at 60 deg.c for 1-2 hr to obtain carbon nanotube with oxygen-containing functional group on the surface and excellent hydrophilicity.
2. The carbon modified MoS of claim 1, wherein the carbon modified MoS comprises a carbon-modified carbon2/MoO2The preparation method of the two-phase foam composite material is characterized by comprising the following steps: the product after freeze drying needs to be calcined in nitrogen atmosphere, the calcining temperature is 600-900 ℃, and the calcining time is 2-6 h.
3. The carbon modified MoS of claim 1, wherein the carbon modified MoS comprises a carbon-modified carbon2/MoO2The preparation method of the two-phase foam composite material is characterized in that the mass ratio of the graphene oxide to the treated carbon nano tube, ammonium molybdate tetrahydrate and thiourea is 1:1:1:2 ~ 7.
4. The carbon modified MoS of claim 1, wherein the carbon modified MoS comprises a carbon-modified carbon2/MoO2Process for the preparation of a two-phase foam composite, characterized in thatThe method comprises the following steps: hydrochloric acid and sodium hydroxide are used for adjusting the pH value of the solution to 3-12.
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| CN102142538A (en) * | 2011-02-25 | 2011-08-03 | 浙江大学 | Lithium ion battery electrode made of graphene/ MoS2 and amorphous carbon and preparation method |
| CN105244482A (en) * | 2015-09-12 | 2016-01-13 | 复旦大学 | Nickel cobalt sulfide/graphene/carbon nanotube composite material and preparation method and application thereof |
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| CN102142538A (en) * | 2011-02-25 | 2011-08-03 | 浙江大学 | Lithium ion battery electrode made of graphene/ MoS2 and amorphous carbon and preparation method |
| CN105244482A (en) * | 2015-09-12 | 2016-01-13 | 复旦大学 | Nickel cobalt sulfide/graphene/carbon nanotube composite material and preparation method and application thereof |
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