CN103413925B - Curling molybdenum trioxide nano band of Graphene and its preparation method and application - Google Patents
Curling molybdenum trioxide nano band of Graphene and its preparation method and application Download PDFInfo
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Abstract
The present invention relates to curling molybdenum trioxide nano band of Graphene and preparation method thereof, it can be used as anode material for lithium-ion batteries, include following steps: the 1) preparation of molybdenum colloidal sol: measure hydrogenperoxide steam generator and be placed in beaker, molybdenum powder is joined in hydrogen peroxide slowly, whole process is carried out in cold bath, after molybdenum powder adds completely, stir, obtain molybdenum colloidal sol; 2) graphene dispersing solution that Hummer legal system is standby is measured, and molybdenum colloidal sol prepared by step 1), stirring in water bath, is transferred in reactor, carries out hydro-thermal reaction, then naturally cool to room temperature in insulating box; 3) by step 2) put into baking oven after the product absolute ethanol washing that obtains and dry and get final product.The invention has the beneficial effects as follows: during positive electrode as lithium ion battery, show excellent multiplying power, higher specific capacity and good cyclical stability.Present invention process is simple, and economical and practical.
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, seeking new energy storage system has become a current challenge to overcome traditional fuel energy storage.Due to the low price of chargeable lithium cell, long circulation life, high-energy-density and good reversible feature, 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, Flied emission, catalysis, sensor field.Particularly in electrochemical energy storage application, just because of its stability, high power capacity and by good high rate performance, be 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.
But molybdenum trioxide comes with some shortcomings, such as poor dynamic performance or in cyclic process (particularly more high magnification under) capacity go down, the problems such as low conductivity.Therefore, the conductivity how effectively strengthening molybdenum trioxide nano band is used to the effective ways of the circulation ability strengthened 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 a kind of technique simple, meet the requirement of Green Chemistry, the curling molybdenum trioxide nano band of Graphene with good electric chemical property and its preparation method and application.
The present invention solves the problems of the technologies described above adopted technical scheme: the curling molybdenum trioxide nano band of Graphene, it is be attached to the molybdenum trioxide nano band above Graphene with single-size, described molybdenum trioxide nano band bandwidth is 200 to 300 nanometers, belt length is 5 to 6 microns, Graphene average thickness is 0.7 ~ 0.9 nanometer, Graphene is that curling shape is wound around parcel molybdenum trioxide nano band, for adopting following method to obtain product, includes following steps:
1) preparation of molybdenum colloidal sol: measure 30-40mL hydrogenperoxide steam generator and be placed in beaker, joined slowly in hydrogen peroxide by 3.8-4.2g molybdenum powder, whole process is carried out in cold bath, after molybdenum powder adds completely, in cold bath, stir 4-6 hour, obtain molybdenum colloidal sol;
2) graphene dispersing solution that 3-5mL Hummer legal system is standby is measured, and molybdenum colloidal sol prepared by 27-33mL step 1), stirring in water bath, is transferred in reactor, carries out hydro-thermal reaction, then naturally cool to room temperature in insulating box;
3) by step 2) put into 80 DEG C of baking ovens after the product absolute ethanol washing that obtains 3-4 time and dry and namely obtain the curling molybdenum trioxide nano band of Graphene.
By such scheme, described Graphene is individual layer, and size uniformity.
By such scheme, step 2) described in the temperature of stirring in water bath be 60 ~ 80 DEG C, mixing time is 4-6h.
By such scheme, step 2) described in the temperature of hydro-thermal reaction be 170-190 DEG C, 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 30-40mL hydrogenperoxide steam generator and be placed in beaker, joined slowly in hydrogen peroxide by 3.8-4.2g molybdenum powder, whole process is carried out in cold bath, after molybdenum powder adds completely, in cold bath, stir 4-6 hour, obtain molybdenum colloidal sol;
2) graphene dispersing solution that 3-5mL Hummer legal system is standby is measured, and molybdenum colloidal sol prepared by 27-33mL step 1), stirring in water bath, is transferred in reactor, carries out hydro-thermal reaction, then naturally cool to room temperature in insulating box;
3) by step 2) put into 80 DEG C of baking ovens after the product absolute ethanol washing that obtains 3-4 time and dry and namely obtain the curling molybdenum trioxide nano band of Graphene.
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 preparation individual layer and there is the Graphene of excellent conductive performance, together with well attached with the molybdenum trioxide with single-size, during the positive electrode of this electrode as lithium ion battery, show excellent multiplying power, higher specific capacity and good cyclical stability.Present invention process is simple, and economical and practical, and material requested is all prepare voluntarily substantially, is got final product synthesis of high purity, is evenly attached to molybdenum trioxide nano band on Graphene, meet the requirement of Green Chemistry, be beneficial to the marketization and promote by one step hydro thermal method.
Accompanying drawing explanation
Fig. 1 is the XRD of embodiment 1 and infrared figure;
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 the present invention better, illustrate content of the present invention further below in conjunction with embodiment, but content of the present invention is not only confined to the following examples.
Adopt the graphene dispersing solution that Hummer legal system is standby: by 1g graphite and 23mL concentrated sulfuric acid mix and blend 24 hours, then put into 40 DEG C of water-baths, add 100mL sodium nitrate, stir 5 minutes; Then temperature is risen to 45 DEG C, and slowly add 500mg potassium permanganate, stir 30 minutes.3mL water is added above-mentioned solution, after 5 minutes, adds other 3mL.After 5 minutes, add 40mL water.After 15 minutes, solution is taken out cooling, adds 140mL deionized water and 10mL30% hydrogen peroxide simultaneously, and centrifuge washing.Finally, be scattered in by centrifugal products therefrom in 100mL deionized water, ultrasonic 60 minutes, with 5000 revs/min of speed washings, gained brown suspension is graphene dispersing solution.
Embodiment 1:
One step hydro thermal method prepares Graphene curling molybdenum trioxide nano charged pool positive electrode, comprises the steps:
1) preparation of molybdenum colloidal sol: measure 40mL hydrogenperoxide steam generator and be placed in 100mL beaker, joined slowly in hydrogen peroxide by 4g molybdenum powder, whole process is carried out in cold bath.After molybdenum powder adds completely, stir 4 hours in cold bath;
2) graphene dispersing solution that 5mLHummer legal system is standby is measured, and the molybdenum colloidal sol prepared in 30mL step 1), at 70 DEG C of stirred in water bath 4h, be transferred in 50mL reactor, in insulating box, 180 DEG C of insulation 6h, then naturally cool to room temperature;
3) by step 2) put into 80 DEG C of baking ovens after the product absolute ethanol washing that obtains 3-4 time and dry and namely obtain the curling molybdenum trioxide nano band of Graphene.
As shown in Figure 1, XRD proves the molybdenum trioxide nano band having synthesized pure phase, and the existence of Graphene does not have an impact to the structure of molybdenum trioxide.Infrared test proves to there is Graphene in end product.
As shown in Figure 2, the Graphene that atomic force microscope (AFM) demonstrates synthesis is individual layer, and thickness is at about 0.7nm.
As shown in Figure 3, the graphene uniform observed out clearly in ESEM (SEM) in curling shape is wound around the molybdenum trioxide nano belt surface being wrapped in size uniformity.
As shown in Figure 4, high resolution TEM (HRTEM) further demonstrates 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 carry out the assembling of battery in glove box.Cyclic voltammetry shows, under the discharge and recharge of 0.5A/g, capacity still reaches 289mAh/g, and under 0.5 current density to 2A/g, battery capacity is respectively 289,238and138mAh/g.Have higher capacity and cyclical stability based on the molybdenum trioxide nano charged pool that Graphene is curling compared with pure molybdenum trioxide nano charged pool, its conductivity increases significantly.
As shown in Figure 6, under the discharge and recharge of high current density (1A/g), Graphene compound molybdenum trioxide nano charged pool still has high capacity 200mAh/g and good stability, the capability retention of 99%, and 500 circles that circulate under high current density.Graphene compound molybdenum trioxide nano band has excellent high rate performance simultaneously, and tool has greatly improved compared with pure molybdenum trioxide.
As Fig. 7, Design Mechanism of the present invention, there is a large amount of unsaturated bonds in the graphenic surface of preparation, there is a large amount of peroxide bridges combine with on the peroxo-polymolybdic acid in the molybdenum colloidal sol of preparation, by hydro thermal method, make this combination become more firm, thus define the structure of the curling molybdenum trioxide of Graphene, this Structure composing continuous print conductive channel, substantially increases the conductivity of pure phase molybdenum trioxide, thus improves chemical property and cycle life.
Embodiment 2:
One step hydro thermal method prepares Graphene curling molybdenum trioxide nano charged pool positive electrode, comprises the steps:
1) preparation of molybdenum colloidal sol: measure 40mL hydrogenperoxide steam generator and be placed in 100mL beaker, joined slowly in hydrogen peroxide by 4g molybdenum powder, whole process is carried out in cold bath.After molybdenum powder adds completely, stir 4 hours in cold bath;
2) graphene dispersing solution that 5mL Hummer legal system is standby is measured, and the molybdenum colloidal sol prepared in 30mL step 1), at 70 DEG C of stirred in water bath 4h, be transferred in 50mL reactor, in insulating box, 170 DEG C of insulation 6h, then naturally cool to room temperature;
3) by step 2) put into 80 DEG C of baking ovens after the product absolute ethanol washing that obtains 3-4 time and dry and namely obtain the curling molybdenum trioxide nano band of Graphene.
The curling molybdenum trioxide nano band of Graphene prepared by the present invention, carries out charge-discharge test after carry out the assembling of battery in glove box.Show in cyclic voltammetry, under the discharge and recharge of high current density (1 A/g), Graphene compound molybdenum trioxide nano charged pool still has high capacity 200mAh/g and good capability retention, and 500 circles that circulate under high current density.Graphene compound molybdenum trioxide nano band has excellent high rate performance simultaneously, and tool has greatly improved compared with pure molybdenum trioxide.
Embodiment 3:
One step hydro thermal method prepares Graphene curling molybdenum trioxide nano charged pool positive electrode, comprises the steps:
1) preparation of molybdenum colloidal sol: measure 40mL hydrogenperoxide steam generator and be placed in 100mL beaker, joined slowly in hydrogen peroxide by 4g molybdenum powder, whole process is carried out in cold bath.After molybdenum powder adds completely, stir 4 hours in cold bath;
2) graphene dispersing solution that 5mL Hummer legal system is standby is measured, and the molybdenum colloidal sol prepared in 30mL step 1), at 80 DEG C of stirred in water bath 4h, be transferred in 50mL reactor, in insulating box, 190 DEG C of insulation 6h, then naturally cool to room temperature;
3) by step 2) put into 80 DEG C of baking ovens after the product absolute ethanol washing that obtains 3-4 time and dry and namely obtain the curling molybdenum trioxide nano band of Graphene.
The curling molybdenum trioxide nano band of Graphene prepared by the present invention, carries out charge-discharge test after carry out the assembling of battery in glove box.Show in cyclic voltammetry, under the discharge and recharge of high current density (1A/g), Graphene compound molybdenum trioxide nano charged pool still has high capacity 200 mAh/g and good capability retention, and 500 circles that circulate under high current density.Graphene compound molybdenum trioxide nano band has excellent high rate performance simultaneously, and tool has greatly improved compared with pure molybdenum trioxide.
Embodiment 4:
One step hydro thermal method prepares Graphene curling molybdenum trioxide nano charged pool positive electrode, comprises the steps:
1) preparation of molybdenum colloidal sol: measure 40mL hydrogenperoxide steam generator and be placed in 100mL beaker, joined slowly in hydrogen peroxide by 4g molybdenum powder, whole process is carried out in cold bath.After molybdenum powder adds completely, stir 4 hours in cold bath;
2) graphene dispersing solution that 5mL Hummer legal system is standby is measured, and the molybdenum colloidal sol prepared in 30mL step 1), at 80 DEG C of stirred in water bath 6h, be transferred in 50mL reactor, in insulating box, 180 DEG C of insulation 6h, then naturally cool to room temperature;
3) by step 2) put into 80 DEG C of baking ovens after the product absolute ethanol washing that obtains 3-4 time and dry and namely obtain the curling molybdenum trioxide nano band of Graphene.
The curling molybdenum trioxide nano band of Graphene prepared by the present invention, carries out charge-discharge test after carry out the assembling of battery in glove box.Show in cyclic voltammetry, under the discharge and recharge of high current density (1 A/g), Graphene compound molybdenum trioxide nano charged pool still has high capacity 200mAh/g and good capability retention, and 500 circles that circulate under high current density.Graphene compound molybdenum trioxide nano band has excellent high rate performance simultaneously, and tool has greatly improved compared with pure molybdenum trioxide.
Embodiment 5:
One step hydro thermal method prepares Graphene curling molybdenum trioxide nano charged pool positive electrode, comprises the steps:
1) preparation of molybdenum colloidal sol: measure 40mL hydrogenperoxide steam generator and be placed in 100mL beaker, joined slowly in hydrogen peroxide by 4g molybdenum powder, whole process is carried out in cold bath.After molybdenum powder adds completely, stir 4 hours in cold bath;
2) graphene dispersing solution that 5mL Hummer legal system is standby is measured, and the molybdenum colloidal sol prepared in 30mL step 1), at 70 DEG C of stirred in water bath 4h, be transferred in 50mL reactor, in insulating box, 190 DEG C of insulation 4h, then naturally cool to room temperature;
3) by step 2) put into 80 DEG C of baking ovens after the product absolute ethanol washing that obtains 3-4 time and dry and namely obtain the curling molybdenum trioxide nano band of Graphene.
The curling molybdenum trioxide nano band of Graphene prepared by the present invention, carries out charge-discharge test after carry out the assembling of battery in glove box.Show in cyclic voltammetry, under the discharge and recharge of high current density (1 A/g), Graphene compound molybdenum trioxide nano charged pool still has high capacity 200mAh/g and good capability retention, and 500 circles that circulate under high current density.Graphene compound molybdenum trioxide nano band has excellent high rate performance simultaneously, and tool has greatly improved compared with pure molybdenum trioxide.
Claims (3)
1. the curling molybdenum trioxide nano band of Graphene, it is be attached to the molybdenum trioxide nano band above Graphene with single-size, described molybdenum trioxide nano band bandwidth is 200 to 300 nanometers, belt length is 5 to 6 microns, Graphene average thickness is 0.7 ~ 0.9 nanometer, Graphene is that curling shape is wound around parcel molybdenum trioxide nano band, and described Graphene is individual layer, and size uniformity; For adopting following method to obtain product, include following steps:
1) preparation of molybdenum colloidal sol: measure 30-40mL hydrogenperoxide steam generator and be placed in beaker, joined slowly in hydrogen peroxide by 3.8-4.2g molybdenum powder, whole process is carried out in cold bath, after molybdenum powder adds completely, in cold bath, stir 4-6 hour, obtain molybdenum colloidal sol;
2) graphene dispersing solution that 3-5mL Hummer legal system is standby is measured, and 27-33mL step 1) the molybdenum colloidal sol prepared, stirring in water bath, is transferred in reactor, carries out hydro-thermal reaction, then naturally cool to room temperature in insulating box; The temperature of described stirring in water bath is 60 ~ 80 DEG C, and mixing time is 4-6h; The temperature of described hydro-thermal reaction is 170-190 DEG C, and the hydro-thermal reaction time is 4-6h;
3) by step 2) put into 80 DEG C of baking ovens after the product absolute ethanol washing that obtains 3-4 time and dry and namely obtain the curling molybdenum trioxide nano band of Graphene.
2. the preparation method of the curling molybdenum trioxide nano band of Graphene according to claim 1, is characterized in that including following steps:
1) preparation of molybdenum colloidal sol: measure 30-40mL hydrogenperoxide steam generator and be placed in beaker, joined slowly in hydrogen peroxide by 3.8-4.2g molybdenum powder, whole process is carried out in cold bath, after molybdenum powder adds completely, in cold bath, stir 4-6 hour, obtain molybdenum colloidal sol;
2) graphene dispersing solution that 3-5mL Hummer legal system is standby is measured, and 27-33mL step 1) the molybdenum colloidal sol prepared, stirring in water bath, is transferred in reactor, carries out hydro-thermal reaction, then naturally cool to room temperature in insulating box; The temperature of described stirring in water bath is 60 ~ 80 DEG C, and mixing time is 4-6h; The temperature of described hydro-thermal reaction is 170-190 DEG C, and the hydro-thermal reaction time is 4-6h;
3) by step 2) put into 80 DEG C of baking ovens after the product absolute ethanol washing that obtains 3-4 time and dry and namely obtain the curling molybdenum trioxide nano band of Graphene.
3. the curling molybdenum trioxide nano band of Graphene according to claim 1 is as the application of the active material of lithium ion battery.
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