CN103413925A - Graphene curled molybdenum trioxide nano-ribbons, and preparation method and application thereof - Google Patents
Graphene curled molybdenum trioxide nano-ribbons, and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to graphene curled molybdenum trioxide nano-ribbons, and a preparation method and an application thereof. The nano-ribbons can be used as a lithium ion battery positive electrode material. The method comprises the steps that: (1) a molybdenum sol is prepared, wherein excessive hydrogen peroxide solution is weighed and placed into a beaker; molybdenum powder is slowly added into the hydrogen peroxide, wherein the entire process is carried out under a cold water bath; when the molybdenum powder is completely added, the materials are stirred, such that molybdenum sol is obtained; (2) a graphene dispersion prepared with a Hummer method and the molybdenum sol prepared in the step (1) are weighed and are stirred under water bath; the mixture is transferred to a reaction kettle, and is subjected to a hydrothermal reaction in a thermostat; the material is naturally cooled to room temperature; (3) the product obtained in the step (2) is washed by using anhydrous ethanol, and is dried in a drying oven. The nano-ribbons and the method have the advantages that: when the material is adopted as a lithium ion battery positive electrode material, excellent rate performance, high specific capacity, and good circulation stability are shown. The process is simple and economical.
Description
Technical field
The invention belongs to nano material and technical field of electrochemistry, be specifically related to curling molybdenum trioxide nano band of a kind of Graphene and preparation method thereof, it can be used as anode material for lithium-ion batteries.
Background technology
Growing along with to energy demand, seek new energy storage system and overcome the traditional fuel energy storage and become a current challenge.Due to low price, long circulation life, high-energy-density and good reversible feature of chargeable lithium cell, it has become the focus of many research.
In transition metal oxide, molybdenum trioxide, as a kind of critical material, is furtherd investigate in optics, an emission, catalysis, sensor field.Particularly in electrochemical energy storage application, just because of its stability, high power capacity and by good high rate performance are able to application and research widely.The molybdenum trioxide of many structures is synthesized in succession as nano wire, nanometer sheet, nanobelt and nanometer rods.
Yet molybdenum trioxide comes with some shortcomings, for example poor dynamic performance or in cyclic process (particularly more high magnification under) capacity go down, the problems such as low conductivity.Therefore, the conductivity that how effectively to strengthen the molybdenum trioxide nano band is the effective ways that strengthen the circulation ability in high rate performance and electrochemical applications.It is reported, graphite is rare has good conductivity and multiple special nature, can solve the problem of the poorly conductive of metal oxide.
Summary of the invention
The object of the present invention is to provide that a kind of technique is simple, the requirement that meets Green Chemistry, have curling molybdenum trioxide nano band of Graphene of good electric chemical property and its preparation method and application.
The present invention solves the problems of the technologies described above the technical scheme adopted: the curling molybdenum trioxide nano band of Graphene, it is to be attached to above Graphene the molybdenum trioxide nano band with single-size, described molybdenum trioxide nano band bandwidth is 200 to 300 nanometers, belt length is 5 to 6 microns, the Graphene average thickness is 0.7～0.9 nanometer, Graphene is curling shape and is wound around parcel molybdenum trioxide nano band, makes product for adopting following method, includes following steps:
1) preparation of molybdenum colloidal sol: measure the 30-40mL hydrogenperoxide steam generator and be placed in beaker, the 3.8-4.2g molybdenum powder is joined in hydrogen peroxide slowly, and whole process is carried out in cold bath, after molybdenum powder adds fully, in cold bath, stir 4-6 hour, obtain molybdenum colloidal sol;
2) measure the standby graphene dispersing solution of 3-5mL Hummer legal system, reach molybdenum colloidal sol prepared by the 27-33mL step 1), stirring in water bath, be transferred in reactor, in insulating box, carries out hydro-thermal reaction, then naturally cools to room temperature;
3) by step 2) product that obtains dries and namely obtains the curling molybdenum trioxide nano band of Graphene with after absolute ethanol washing 3-4 time, putting into 80 ℃ of baking ovens.
Press such scheme, described Graphene is individual layer, and the size homogeneous.
Press such scheme, step 2) temperature of described stirring in water bath is 60～80 ℃, mixing time is 4-6h.
Press such scheme, step 2) temperature of described hydro-thermal reaction is 170-190 ℃, the hydro-thermal reaction time is 4-6h.
The preparation method of the curling molybdenum trioxide nano band of Graphene is characterized in that including following steps:
1) preparation of molybdenum colloidal sol: measure the 30-40mL hydrogenperoxide steam generator and be placed in beaker, the 3.8-4.2g molybdenum powder is joined in hydrogen peroxide slowly, and whole process is carried out in cold bath, after molybdenum powder adds fully, in cold bath, stir 4-6 hour, obtain molybdenum colloidal sol;
2) measure the standby graphene dispersing solution of 3-5mL Hummer legal system, reach molybdenum colloidal sol prepared by the 27-33mL step 1), stirring in water bath, be transferred in reactor, in insulating box, carries out hydro-thermal reaction, then naturally cools to room temperature;
3) by step 2) product that obtains dries and namely obtains the curling molybdenum trioxide nano band of Graphene with after absolute ethanol washing 3-4 time, putting into 80 ℃ of baking ovens.
The curling molybdenum trioxide nano band of Graphene is as the application of the active material of lithium ion battery.
The invention has the beneficial effects as follows: based on the individual layer of preparation and have the Graphene of excellent conductive performance, together well attached with the molybdenum trioxide with single-size, this electrode is during as the positive electrode of lithium ion battery, shows excellent multiplying power, higher specific capacity and good cyclical stability.Technique of the present invention is simple, and economical and practical, and material requested is all to prepare voluntarily basically, gets final product synthesis of high purity, evenly is attached to the molybdenum trioxide nano band on Graphene by one step hydro thermal method, meets the requirement of Green Chemistry, is beneficial to the marketization and promotes.
The accompanying drawing explanation
Fig. 1 is XRD and the infrared figure of embodiment 1;
Fig. 2 is the AFM figure of embodiment 1;
Fig. 3 is the SEM figure of embodiment 1;
Fig. 4 is the TEM figure of embodiment 1;
Fig. 5 is the chemical property figure of embodiment 1;
Fig. 6 is cycle performance and the multiplying power figure of embodiment 1;
Fig. 7 is the structural design drawing of embodiment 1.
Embodiment
In order to understand better the present invention, below in conjunction with embodiment, further illustrate content of the present invention, but content of the present invention not only is confined to the following examples.
Adopt the standby graphene dispersing solution of Hummer legal system: by 1g graphite and 23mL concentrated sulfuric acid mix and blend 24 hours, then put into 40 ℃ of water-baths, add 100mL sodium nitrate, stirred 5 minutes; Then temperature is risen to 45 ℃, and slowly add 500mg potassium permanganate, stirred 30 minutes.3mL water is added to above-mentioned solution, after 5 minutes, add other 3mL.After 5 minutes, add 40mL water.After 15 minutes, solution is taken out cooling, add simultaneously 140mL deionized water and 10mL30% hydrogen peroxide, and centrifuge washing.Finally, centrifugal products therefrom is scattered in the 100mL deionized water, ultrasonic 60 minutes, with 5000 rev/mins of speed washings, the gained brown suspension was graphene dispersing solution.
Embodiment 1:
One step hydro thermal method prepares the curling molybdenum trioxide nano charged pool of Graphene positive electrode, comprises the steps:
1) preparation of molybdenum colloidal sol: measure the 40mL hydrogenperoxide steam generator and be placed in the 100mL beaker, the 4g molybdenum powder is joined in hydrogen peroxide slowly, whole process is carried out in cold bath.After molybdenum powder adds fully, stirred 4 hours in cold bath;
2) measure the standby graphene dispersing solution of 5mLHummer legal system, and the molybdenum colloidal sol prepared in the 30mL step 1), at 70 ℃ of stirred in water bath 4h, being transferred in the 50mL reactor, 180 ℃ of insulation 6h, then naturally cool to room temperature in insulating box;
3) by step 2) product that obtains dries and namely obtains the curling molybdenum trioxide nano band of Graphene with after absolute ethanol washing 3-4 time, putting into 80 ℃ of baking ovens.
As shown in Figure 1, the XRD proof has been synthesized the molybdenum trioxide nano band of pure phase, and the existence of Graphene does not affect the structure generation of molybdenum trioxide.There is Graphene in the infrared test proof in end product.
As shown in Figure 2, atomic force microscope (AFM) has proved that synthetic Graphene is individual layer, and thickness is in the 0.7nm left and right.
As shown in Figure 3, in ESEM (SEM), observe out the graphene uniform that is curling shape clearly and be wound around the molybdenum trioxide nano belt surface that is wrapped in the size homogeneous.
As shown in Figure 4, high-resolution transmission electron microscope (HRTEM) has further proved the composite construction of Graphene and molybdenum trioxide nano band, and test shows, product is mono-crystalline structures.
As shown in Figure 5, Graphene prepared by the present invention and molybdenum trioxide nano band, carry out charge-discharge test after the assembling carrying out battery in glove box.Cyclic voltammetry shows, capacity still reaches 289mAh/g under the discharging and recharging of 0.5A/g, and under the current density of 2A/g, battery capacity is respectively 289,238and138mAh/g 0.5.With pure molybdenum trioxide nano charged pool, compare based on the curling molybdenum trioxide nano charged pool of Graphene and have higher capacity and cyclical stability, its conductivity increases significantly.
As shown in Figure 6, under the discharging and recharging of high current density (1A/g), the compound molybdenum trioxide nano charged pool of Graphene still has high capacity 200mAh/g and good stability, 99% capability retention, and circulation 500 is enclosed under high current density.The compound molybdenum trioxide nano band of Graphene has excellent high rate performance simultaneously, with pure molybdenum trioxide, compares tool and has greatly improved.
As Fig. 7, Design Mechanism of the present invention, there is a large amount of unsaturated bonds in the Graphene surface of preparation, with the preparation molybdenum colloidal sol in the peroxide molybdic acid on exist a large amount of peroxide bridges to combine, by hydro thermal method, make this combination become more firm, thereby formed the structure of the curling molybdenum trioxide of Graphene, this structure has formed continuous conductive channel, has greatly improved the conductivity of pure phase molybdenum trioxide, thereby has improved chemical property and cycle life.
Embodiment 2:
One step hydro thermal method prepares the curling molybdenum trioxide nano charged pool of Graphene positive electrode, comprises the steps:
1) preparation of molybdenum colloidal sol: measure the 40mL hydrogenperoxide steam generator and be placed in the 100mL beaker, the 4g molybdenum powder is joined in hydrogen peroxide slowly, whole process is carried out in cold bath.After molybdenum powder adds fully, stirred 4 hours in cold bath;
2) measure the standby graphene dispersing solution of 5mL Hummer legal system, and the molybdenum colloidal sol prepared in the 30mL step 1), at 70 ℃ of stirred in water bath 4h, being transferred in the 50mL reactor, 170 ℃ of insulation 6h, then naturally cool to room temperature in insulating box;
3) by step 2) product that obtains dries and namely obtains the curling molybdenum trioxide nano band of Graphene with after absolute ethanol washing 3-4 time, putting into 80 ℃ of baking ovens.
The curling molybdenum trioxide nano band of Graphene prepared by the present invention, carry out charge-discharge test after the assembling carrying out battery in glove box.In cyclic voltammetry, show, under the discharging and recharging of high current density (1 A/g), the compound molybdenum trioxide nano charged pool of Graphene still has high capacity 200mAh/g and good capability retention, and circulation 500 is enclosed under high current density.The compound molybdenum trioxide nano band of Graphene has excellent high rate performance simultaneously, with pure molybdenum trioxide, compares tool and has greatly improved.
Embodiment 3:
One step hydro thermal method prepares the curling molybdenum trioxide nano charged pool of Graphene positive electrode, comprises the steps:
1) preparation of molybdenum colloidal sol: measure the 40mL hydrogenperoxide steam generator and be placed in the 100mL beaker, the 4g molybdenum powder is joined in hydrogen peroxide slowly, whole process is carried out in cold bath.After molybdenum powder adds fully, stirred 4 hours in cold bath;
2) measure the standby graphene dispersing solution of 5mL Hummer legal system, and the molybdenum colloidal sol prepared in the 30mL step 1), at 80 ℃ of stirred in water bath 4h, being transferred in the 50mL reactor, 190 ℃ of insulation 6h, then naturally cool to room temperature in insulating box;
3) by step 2) product that obtains dries and namely obtains the curling molybdenum trioxide nano band of Graphene with after absolute ethanol washing 3-4 time, putting into 80 ℃ of baking ovens.
The curling molybdenum trioxide nano band of Graphene prepared by the present invention, carry out charge-discharge test after the assembling carrying out battery in glove box.In cyclic voltammetry, show, under the discharging and recharging of high current density (1A/g), the compound molybdenum trioxide nano charged pool of Graphene still has high capacity 200 mAh/g and good capability retention, and circulation 500 is enclosed under high current density.The compound molybdenum trioxide nano band of Graphene has excellent high rate performance simultaneously, with pure molybdenum trioxide, compares tool and has greatly improved.
Embodiment 4:
One step hydro thermal method prepares the curling molybdenum trioxide nano charged pool of Graphene positive electrode, comprises the steps:
1) preparation of molybdenum colloidal sol: measure the 40mL hydrogenperoxide steam generator and be placed in the 100mL beaker, the 4g molybdenum powder is joined in hydrogen peroxide slowly, whole process is carried out in cold bath.After molybdenum powder adds fully, stirred 4 hours in cold bath;
2) measure the standby graphene dispersing solution of 5mL Hummer legal system, and the molybdenum colloidal sol prepared in the 30mL step 1), at 80 ℃ of stirred in water bath 6h, being transferred in the 50mL reactor, 180 ℃ of insulation 6h, then naturally cool to room temperature in insulating box;
3) by step 2) product that obtains dries and namely obtains the curling molybdenum trioxide nano band of Graphene with after absolute ethanol washing 3-4 time, putting into 80 ℃ of baking ovens.
The curling molybdenum trioxide nano band of Graphene prepared by the present invention, carry out charge-discharge test after the assembling carrying out battery in glove box.In cyclic voltammetry, show, under the discharging and recharging of high current density (1 A/g), the compound molybdenum trioxide nano charged pool of Graphene still has high capacity 200mAh/g and good capability retention, and circulation 500 is enclosed under high current density.The compound molybdenum trioxide nano band of Graphene has excellent high rate performance simultaneously, with pure molybdenum trioxide, compares tool and has greatly improved.
Embodiment 5:
One step hydro thermal method prepares the curling molybdenum trioxide nano charged pool of Graphene positive electrode, comprises the steps:
1) preparation of molybdenum colloidal sol: measure the 40mL hydrogenperoxide steam generator and be placed in the 100mL beaker, the 4g molybdenum powder is joined in hydrogen peroxide slowly, whole process is carried out in cold bath.After molybdenum powder adds fully, stirred 4 hours in cold bath;
2) measure the standby graphene dispersing solution of 5mL Hummer legal system, and the molybdenum colloidal sol prepared in the 30mL step 1), at 70 ℃ of stirred in water bath 4h, being transferred in the 50mL reactor, 190 ℃ of insulation 4h, then naturally cool to room temperature in insulating box;
3) by step 2) product that obtains dries and namely obtains the curling molybdenum trioxide nano band of Graphene with after absolute ethanol washing 3-4 time, putting into 80 ℃ of baking ovens.
The curling molybdenum trioxide nano band of Graphene prepared by the present invention, carry out charge-discharge test after the assembling carrying out battery in glove box.In cyclic voltammetry, show, under the discharging and recharging of high current density (1 A/g), the compound molybdenum trioxide nano charged pool of Graphene still has high capacity 200mAh/g and good capability retention, and circulation 500 is enclosed under high current density.The compound molybdenum trioxide nano band of Graphene has excellent high rate performance simultaneously, with pure molybdenum trioxide, compares tool and has greatly improved.
Claims (8)
1. the curling molybdenum trioxide nano band of Graphene, it is to be attached to above Graphene the molybdenum trioxide nano band with single-size, described molybdenum trioxide nano band bandwidth is 200 to 300 nanometers, belt length is 5 to 6 microns, the Graphene average thickness is 0.7～0.9 nanometer, Graphene is curling shape and is wound around parcel molybdenum trioxide nano band, makes product for adopting following method, includes following steps:
1) preparation of molybdenum colloidal sol: measure the 30-40mL hydrogenperoxide steam generator and be placed in beaker, the 3.8-4.2g molybdenum powder is joined in hydrogen peroxide slowly, and whole process is carried out in cold bath, after molybdenum powder adds fully, in cold bath, stir 4-6 hour, obtain molybdenum colloidal sol;
2) measure the standby graphene dispersing solution of 3-5mL Hummer legal system, reach molybdenum colloidal sol prepared by the 27-33mL step 1), stirring in water bath, be transferred in reactor, in insulating box, carries out hydro-thermal reaction, then naturally cools to room temperature;
3) by step 2) product that obtains dries and namely obtains the curling molybdenum trioxide nano band of Graphene with after absolute ethanol washing 3-4 time, putting into 80 ℃ of baking ovens.
2. the curling molybdenum trioxide nano band of Graphene according to claim 1, is characterized in that described Graphene is individual layer, and the size homogeneous.
3. the curling molybdenum trioxide nano band of Graphene according to claim 1, is characterized in that step 2) temperature of described stirring in water bath is 60～80 ℃, mixing time is 4-6h.
4. the curling molybdenum trioxide nano band of Graphene according to claim 1, is characterized in that step 2) temperature of described hydro-thermal reaction is 170-190 ℃, the hydro-thermal reaction time is 4-6h.
5. the preparation method of the curling molybdenum trioxide nano band of Graphene claimed in claim 1 is characterized in that including following steps:
1) preparation of molybdenum colloidal sol: measure the 30-40mL hydrogenperoxide steam generator and be placed in beaker, the 3.8-4.2g molybdenum powder is joined in hydrogen peroxide slowly, and whole process is carried out in cold bath, after molybdenum powder adds fully, in cold bath, stir 4-6 hour, obtain molybdenum colloidal sol;
2) measure the standby graphene dispersing solution of 3-5mL Hummer legal system, reach molybdenum colloidal sol prepared by the 27-33mL step 1), stirring in water bath, be transferred in reactor, in insulating box, carries out hydro-thermal reaction, then naturally cools to room temperature;
3) by step 2) product that obtains dries and namely obtains the curling molybdenum trioxide nano band of Graphene with after absolute ethanol washing 3-4 time, putting into 80 ℃ of baking ovens.
6. the preparation method of the curling molybdenum trioxide nano band of Graphene according to claim 1, is characterized in that step 2) temperature of described stirring in water bath is 60～80 ℃, mixing time is 4-6h.
7. the preparation method of the curling molybdenum trioxide nano band of Graphene according to claim 1, is characterized in that step 2) temperature of described hydro-thermal reaction is 170-190 ℃, the hydro-thermal reaction time is 4-6h.
8. the curling molybdenum trioxide nano band of Graphene claimed in claim 1 is as the application of the active material of lithium ion battery.
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| CN106207141A (en) * | 2016-09-29 | 2016-12-07 | 柳州申通汽车科技有限公司 | The preparation method of new energy car battery negative material |
| CN106159245A (en) * | 2016-09-29 | 2016-11-23 | 柳州申通汽车科技有限公司 | A kind of preparation method of graphene battery negative plate |
| CN106129389A (en) * | 2016-09-29 | 2016-11-16 | 柳州申通汽车科技有限公司 | The preparation method of new energy car battery pole piece |
| CN110752302A (en) * | 2018-07-24 | 2020-02-04 | Tcl集团股份有限公司 | Composite material, preparation method thereof and quantum dot light-emitting diode |
| CN110752302B (en) * | 2018-07-24 | 2020-12-18 | Tcl科技集团股份有限公司 | Composite material, preparation method thereof and quantum dot light-emitting diode |
| CN110787829A (en) * | 2019-11-11 | 2020-02-14 | 深圳大学 | Mo nanosphere cocatalyst and preparation method and application thereof |
| CN113293395A (en) * | 2021-04-29 | 2021-08-24 | 齐齐哈尔大学 | Molybdenum selenide catalyst, preparation method thereof and application thereof in hydrogen evolution by electrolyzing water |
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