CN109065874B - MoO (MoO)3/rGO-N nano composite material and preparation method and application thereof - Google Patents
MoO (MoO)3/rGO-N nano composite material and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to the technical field of nano materials, in particular to MoO3The preparation method of the/rGO-N nano composite material and the application of the nano composite material in a lithium ion battery. MoO of the invention3In the/rGO-N nano composite material, the three-dimensional nitrogen-doped reduced graphene oxide composite sheet layer provides a substrate for the growth of molybdenum trioxide, the molybdenum trioxide can be uniformly dispersed and grown on the surface of the three-dimensional nitrogen-doped reduced graphene oxide, and the MoO with the structure3the/rGO-N nano composite material combines good conductivity of three-dimensional nitrogen-doped reduced graphene oxide and MoO3The nano-sheet has the advantages of short ion and electron transmission distance, can improve the overall conductivity of the material, can effectively relieve the volume change and aggregation of the molybdenum trioxide nano-particles in the charging/discharging process, keeps good structural integrity, has good electrochemical performance, and can be used as a negative electrode material of a lithium battery. The preparation method has simple process, high yield and easy production expansion.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a MoO3The preparation method of the/rGO-N nano composite material and the application of the nano composite material in a lithium ion battery.
Background
Current lithium ion battery cathode materialMainly made of graphite materials, but the energy density of the graphite materials is low, so that the rapid development of the lithium battery industry is severely restricted. The transition metal oxide is considered to be a lithium ion battery cathode material with great development prospect due to the advantages of high theoretical capacity, easy mass preparation, environmental friendliness and the like. So far, a great number of transition metal oxides with different shapes, different sizes and different structures, including molybdenum oxide, cobalt oxide, iron oxide, nickel oxide, manganese oxide, zinc oxide and the like, have been successfully prepared, and the transition metal oxides as the negative electrode materials of the lithium ion batteries all show ultrahigh lithium storage performance. Among these transition metal oxides, MoO3Has higher theoretical capacity (1117mA h g)-1) Thereby arousing the research interest of researchers. But MoO3The electron conductivity is low, the polarization is serious, and huge volume change can be generated in the charging and discharging process, so that MoO is seriously restricted3The practical application of (1). In order to solve the problems, researchers have conducted a great deal of research, and in summary, the research mainly includes two points, namely, MoO3Down to the nanometer level. MoO3Not only can obviously increase MoO by nano-crystallization3Contact area with electrolyte and can reduce electrons in MoO3Internal transmission distance. Secondly, MoO3And compounding with carbon material with better conductivity. The carbon material can not only improve the conductivity of the electrode, but also relieve MoO3The volume change in the charging and discharging process further promotes the MoO3Cycling stability and rate capability.
Graphene, as an advanced carbon material, is considered to be an ideal component of a lithium ion battery composite electrode material due to its advantages of high electrical conductivity, large specific surface area, high thermal conductivity, and the like. But graphene is a material consisting of carbon atoms in sp2The hybrid orbit forms a hexagonal honeycomb-shaped two-dimensional carbon nano material, the surface of the two-dimensional carbon nano material is relatively stable, and the two-dimensional carbon nano material is not beneficial to forming stable chemical bonds with transition metal oxides, sulfides, phosphides and the like, so that only one mixed material can be formed when the two-dimensional carbon nano material is compounded with a lithium battery material, and the requirement of an ideal composite material cannot be met.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides MoO in which molybdenum trioxide can be uniformly dispersed and can grow on the surface or in the interior of three-dimensional nitrogen-doped reduced graphene oxide3a/rGO-N composite; and preparation of MoO from cheap and easily available raw materials3The preparation method of the/rGO-N composite material has the advantages of simple process, high yield and easy production expansion; MoO of the invention3the/rGO-N composite material has good conductive performance, can keep good structural integrity in the charging and discharging processes, and can be used as a negative electrode material of a lithium battery.
In order to achieve the purpose, the invention adopts the following technical scheme.
MoO (MoO)3the/rGO-N composite material comprises nitrogen-doped redox graphene and flaky MoO growing on the surface of the nitrogen-doped redox graphene3The composite material has a three-dimensional porous structure.
MoO (MoO)3The preparation method of the/rGO-N composite material comprises the following steps:
s1, placing the aqueous solution of the graphene oxide, the molybdate and the ammonium salt in an environment of 100-160 ℃, and heating and refluxing for 2-6h to obtain a uniformly dispersed mixed solution; the mass ratio of the graphene oxide to the molybdate to the ammonium salt is 1: (4-8): (20-60).
Preferably, the aqueous solution of graphene oxide, molybdate and ammonium salt is placed in an oil bath at the temperature of 100-160 ℃ for heating and refluxing.
Preferably, the concentration of the graphene oxide in the aqueous solution is 0.5-2.5 mg/mL.
Preferably, the molybdate is at least one selected from ammonium molybdate, sodium molybdate and potassium molybdate.
Preferably, the ammonium salt is at least one selected from ammonium chloride, ammonium nitrate and ammonium bromide.
S2, heating the mixed solution to 150 ℃ and 210 ℃, and reacting for 16-24 h.
And S3, filtering the mixed solution after the reaction in the step S2, washing a filter cake, and drying the filter cake to obtain black powder.
Preferably, the filter cake is dried by placing the filter cake in a vacuum oven at 80 ℃.
And S4, calcining the black powder at high temperature in an inert atmosphere to obtain the composite material.
Preferably, the calcination temperature of the high-temperature calcination is 550-800 ℃, and the calcination time is 4-8 h.
The preparation method of the graphene oxide comprises the following steps:
adding natural graphite powder into concentrated sulfuric acid with the mass fraction of 98%, and stirring at room temperature to add sodium nitrate; then potassium permanganate is continuously added under stirring, and the temperature of the suspension is kept below 20 ℃ during the period of adding the potassium permanganate; then the suspension is stirred for 18-22h at room temperature to form thick slurry; then adding water into the thick slurry and stirring, then adding hydrogen peroxide to change the color of the mixture from brown to yellow and continuously stirring for more than 0.5 h; and then the mixture is taken over, and a filter cake is washed and dried to obtain the graphene oxide.
The volume ratio of the mass of the natural graphite powder to concentrated sulfuric acid is 1g:30 mL; the mass ratio of the natural graphite powder to the sodium nitrate to the potassium permanganate is 1:0.75: 20; the mass ratio of the natural graphite powder to the volume of water is 1g:128 mL.
The above-mentioned MoO3the/rGO-N composite material is used as a lithium ion battery cathode material.
Compared with the prior art, the invention has the beneficial effects that:
according to the method, cheap and easily-obtained raw materials are used for preparing the three-dimensional graphene oxide, the aqueous solution of the graphene oxide, molybdate and ammonium salt is subjected to a first-stage heating reaction at a relatively low temperature, and the amount of molybdate and ammonium salt is changed to regulate and control the attachment amount of molybdate radicals and ammonium radicals on the surface of the graphene oxide; then, a secondary heating reaction with relatively high temperature is carried out, so that nitrogen atoms in ammonium ions replace oxygen-containing functional groups in graphene oxide to form nitrogen-doped graphene, and in addition, molybdate radicals are decomposed into molybdenum trioxide at high temperature and high pressure to form MoO3the/rGO-N nano composite material enables molybdenum trioxide to be uniformly dispersed and grow on the surface of three-dimensional nitrogen-doped reduced graphene oxide, and then Mo with excellent lithium storage performance is obtained through high-temperature calcinationO3a/rGO-N nanocomposite. Compared with pure graphene, the three-dimensional nitrogen-doped reduced graphene oxide has more functional groups so that the property of the three-dimensional nitrogen-doped reduced graphene oxide is more active, and the three-dimensional nitrogen-doped reduced graphene oxide can be compounded with molybdenum trioxide to form high-performance MoO3a/rGO-N nanocomposite. In MoO3In the/rGO-N nano composite material, the three-dimensional nitrogen-doped reduced graphene oxide sheet layer provides a substrate for the growth of molybdenum trioxide, the molybdenum trioxide can be uniformly dispersed and grown on the surface of the three-dimensional nitrogen-doped reduced graphene oxide, and the MoO with the structure3the/rGO-N nano composite material combines good conductivity of three-dimensional nitrogen-doped reduced graphene oxide and MoO3The nano-sheet has the advantages of short ion and electron transmission distance, can improve the overall conductivity of the material, can effectively relieve the volume change and aggregation of the molybdenum trioxide nano-particles in the charging/discharging process, keeps good structural integrity, has good electrochemical performance, and can be used as a negative electrode material of a lithium battery.
The preparation method has simple process, high yield and easy production expansion.
Drawings
FIG. 1 is MoO in example 13A scanning electron micrograph of the/rGO-N nano composite material A1 under the magnification of 1 ten thousand times;
FIG. 2 is MoO in example 13The X-ray diffraction spectrogram of/rGO-N nano composite material A1;
FIG. 3 is MoO in example 13Constant current cycle plot of/rGO-N nanocomposite a 1;
FIG. 4 is MoO in example 23A scanning electron micrograph of the/rGO-N nano composite material A2 under the magnification of 1 ten thousand times;
FIG. 5 is MoO in example 33Scanning electron micrograph of/rGO-N nano composite material A3 under 1 ten thousand times magnification.
Detailed Description
In order to more fully understand the technical contents of the present invention, the technical solutions of the present invention will be further described and illustrated with reference to the following specific embodiments.
Example 1
The present embodiment provides a MoO3/rGO-N composite material and MoO thereof3A preparation method of/rGO-N composite material.
MoO described in this example3the/rGO-N composite material comprises nitrogen-doped redox graphene and flaky MoO growing on the surface of the nitrogen-doped redox graphene3The composite material has a three-dimensional porous structure, and the preparation method comprises the following specific steps:
(1) preparation of Graphene Oxide (GO): 5g of natural graphite powder was added to 150mL of concentrated sulfuric acid (mass fraction w: 98%), and 3.75g of sodium nitrate was added thereto with stirring at room temperature. Under vigorous stirring, 20g of potassium permanganate were added slowly, during which time the temperature of the suspension was kept below 20 ℃, after which the reaction was transferred to room temperature and stirred for about 20h, forming a thick slurry. Under the condition of uniform stirring, 640mL of deionized water is slowly added, then 30mL of hydrogen peroxide (mass fraction w is 30%) is slowly added, the color of the solution is changed from brown to yellow, the mixture is continuously stirred for 0.5h, then the mixture is filtered, washed by deionized water, impurities such as metal ions are removed, and the graphene oxide is obtained after drying.
(2) Adding 125mg of GO into 50ml of deionized water, magnetically stirring for 30min and carrying out ultrasound treatment for 6h (controlling the water temperature to be below 40 ℃), so that the graphene oxide is completely dispersed in the aqueous solution. Subsequently, 0.75g of ammonium molybdate and 3.75g of ammonium chloride were added thereto, and the mixture was stirred with heating in an oil bath at 120 ℃ for 4 hours. And transferring the obtained mixed solution into a reaction kettle, reacting at 180 ℃ for 20 hours, cooling the reaction kettle to room temperature, filtering the mixed solution, washing the product by using a large amount of deionized water, and drying the product in a vacuum drying oven at 80 ℃ to obtain black powder. Transferring the obtained black powder into a porcelain boat, calcining for 6h in a tube furnace at the temperature of 750 ℃ in a nitrogen atmosphere to obtain MoO3the/rGO-N nano composite material is marked as A1.
For the MoO prepared in this example3The following tests were carried out for the/rGO-N composite a1 and the test results are as follows:
(1) a1 was examined by scanning electron microscopy using Hitachi S-4800, and the results are shown in FIG. 1. As can be seen from FIG. 1, A1 is MoO3And a three-dimensional nitrogen-doped reduced graphene oxide.
(2) X-ray diffraction spectrum detection is carried out on A1 by a D8 advanced X-ray power differential spectrometer, the result is shown in figure 2, and the MoO in A1 is shown by comparing figure 2 with a standard card3MoO in hexagonal phase3。
(3) Using a Mikrouna, Super (1220/750/900) glove box (H)2O<0.1ppm，O2<0.1ppm) assembled button half cells, followed by a novyi cell tester at 200mA g for A1 samples-1The constant current charge and discharge test was performed 50 times at the current density of (1), and the results are shown in FIG. 3. As can be seen from FIG. 3, the capacity of A1 still remained 565mAh g after 50 cycles-1The material has good cycling stability.
Example 2
The present embodiment provides a MoO3/rGO-N composite material and MoO thereof3A preparation method of/rGO-N composite material.
MoO described in this example3the/rGO-N composite material comprises nitrogen-doped redox graphene and flaky MoO growing on the surface of the nitrogen-doped redox graphene3The composite material has a three-dimensional porous structure, and the preparation method comprises the following specific steps:
(1) the preparation of Graphene Oxide (GO) was the same as in example 1.
(2) Adding 125mg of GO into 50ml of deionized water, magnetically stirring for 30min and carrying out ultrasound treatment for 6h (controlling the water temperature to be below 40 ℃), so that the graphene oxide is completely dispersed in the aqueous solution. Subsequently, 0.75g of sodium molybdate and 3.75g of ammonium chloride were added thereto, and the mixture was stirred with heating in an oil bath at 120 ℃ for 4 hours. And transferring the obtained mixed solution into a reaction kettle, reacting at 180 ℃ for 20 hours, cooling the reaction kettle to room temperature, filtering the mixed solution, washing the product by using a large amount of deionized water, and drying the product in a vacuum drying oven at 80 ℃ to obtain black powder. Transferring the obtained black powder into a porcelain boat, calcining for 6h in a tube furnace at the temperature of 750 ℃ in a nitrogen atmosphere to obtain MoO3the/rGO-N nano composite material is marked as A2.
MoO prepared in this example by Hitachi S-48003The result of the scanning electron microscope detection of the/rGO-N composite material A2 is shown in figure 4. As can be seen from FIG. 4, A2 is MoO3And a three-dimensional nitrogen-doped reduced graphene oxide.
Example 3
The present embodiment provides a MoO3/rGO-N composite material and MoO thereof3A preparation method of/rGO-N composite material.
MoO described in this example3the/rGO-N composite material comprises nitrogen-doped redox graphene and flaky MoO growing on the surface of the nitrogen-doped redox graphene3The composite material has a three-dimensional porous structure, and the preparation method comprises the following specific steps:
(1) the preparation of Graphene Oxide (GO) was the same as in example 1.
(2) Adding 125mg of GO into 50ml of deionized water, magnetically stirring for 30min and carrying out ultrasound treatment for 6h (controlling the water temperature to be below 40 ℃), so that the graphene oxide is completely dispersed in the aqueous solution. Subsequently, 0.75g of potassium molybdate and 3.75g of ammonium chloride were added thereto, and the mixture was stirred with heating in an oil bath at 120 ℃ for 4 hours. And transferring the obtained mixed solution into a reaction kettle, reacting at 180 ℃ for 20 hours, cooling the reaction kettle to room temperature, filtering the mixed solution, washing the product by using a large amount of deionized water, and drying the product in a vacuum drying oven at 80 ℃ to obtain black powder. Transferring the obtained black powder into a porcelain boat, calcining for 6h in a tube furnace at the temperature of 750 ℃ in a nitrogen atmosphere to obtain MoO3the/rGO-N nano composite material is marked as A3.
MoO prepared in this example by Hitachi S-48003The result of the scanning electron microscope detection of the/rGO-N composite material A3 is shown in figure 5. As can be seen from FIG. 5, A3 is MoO3And a three-dimensional nitrogen-doped reduced graphene oxide.
Example 4
The present embodiment provides a MoO3/rGO-N composite material and MoO thereof3A preparation method of/rGO-N composite material.
MoO described in this example3the/rGO-N composite material comprises nitrogen-doped redox graphene and flaky MoO growing on the surface of the nitrogen-doped redox graphene3The composite material has a three-dimensional porous structure, and the preparation method comprises the following specific steps:
(1) the preparation of Graphene Oxide (GO) was the same as in example 1.
(2) Adding 125mg of GO into 50ml of deionized water, magnetically stirring for 30min and carrying out ultrasound treatment for 6h (controlling the water temperature to be below 40 ℃), so that the graphene oxide is completely dispersed in the aqueous solution. Subsequently, 0.75g of ammonium molybdate and 3.75g of ammonium nitrate were added thereto, and the mixture was stirred with heating in an oil bath at 120 ℃ for 4 hours. And transferring the obtained mixed solution into a reaction kettle, reacting at 180 ℃ for 20 hours, cooling the reaction kettle to room temperature, filtering the mixed solution, washing the product by using a large amount of deionized water, and drying the product in a vacuum drying oven at 80 ℃ to obtain black powder. Transferring the obtained black powder into a porcelain boat, calcining for 6h in a tube furnace at the temperature of 750 ℃ in a nitrogen atmosphere to obtain MoO3the/rGO-N nano composite material is marked as A4.
Example 5
The present embodiment provides a MoO3/rGO-N composite material and MoO thereof3A preparation method of/rGO-N composite material.
MoO described in this example3the/rGO-N composite material comprises nitrogen-doped redox graphene and flaky MoO growing on the surface of the nitrogen-doped redox graphene3The composite material has a three-dimensional porous structure, and the preparation method comprises the following specific steps:
(1) the preparation of Graphene Oxide (GO) was the same as in example 1.
(2) Adding 125mg of GO into 50ml of deionized water, magnetically stirring for 30min and carrying out ultrasound treatment for 6h (controlling the water temperature to be below 40 ℃), so that the graphene oxide is completely dispersed in the aqueous solution. Subsequently, 0.75g of ammonium molybdate and 3.75g of ammonium bromide were added thereto, and the mixture was stirred with heating in an oil bath at 120 ℃ for 4 hours. And transferring the obtained mixed solution into a reaction kettle, reacting at 180 ℃ for 20 hours, cooling the reaction kettle to room temperature, filtering the mixed solution, washing the product by using a large amount of deionized water, and drying the product in a vacuum drying oven at 80 ℃ to obtain black powder. Transferring the obtained black powder into a porcelain boat, calcining for 6h in a tube furnace at the temperature of 750 ℃ in a nitrogen atmosphere to obtain MoO3the/rGO-N nano composite material is marked as A5.
Example 6
The present embodiment provides a MoO3/rGO-N composite material and MoO thereof3A preparation method of/rGO-N composite material.
MoO described in this example3the/rGO-N composite material is marked as A6 and comprises nitrogen-doped redox graphene and flaky MoO growing on the surface of the nitrogen-doped redox graphene3The composite material has a three-dimensional porous structure, and the specific preparation steps are basically the same as those in example 1, except that the amounts of ammonium molybdate and ammonium chloride are changed, wherein the amount of ammonium molybdate is 0.5g and the amount of ammonium chloride is 2.5g in this example.
Example 7
The present embodiment provides a MoO3/rGO-N composite material and MoO thereof3A preparation method of/rGO-N composite material.
MoO described in this example3the/rGO-N composite material is marked as A7 and comprises nitrogen-doped redox graphene and flaky MoO growing on the surface of the nitrogen-doped redox graphene3The composite material has a three-dimensional porous structure, and the specific preparation steps are basically the same as those in example 1, except that the amounts of ammonium molybdate and ammonium chloride are changed, wherein the amount of ammonium molybdate is 0.5g and the amount of ammonium chloride is 7.5g in this example.
Example 8
The present embodiment provides a MoO3/rGO-N composite material and MoO thereof3A preparation method of/rGO-N composite material.
MoO described in this example3the/rGO-N composite material is marked as A8 and comprises nitrogen-doped redox graphene and flaky MoO growing on the surface of the nitrogen-doped redox graphene3The composite material has a three-dimensional porous structure, and the specific preparation steps are basically the same as those in example 1, except that the amounts of ammonium molybdate and ammonium chloride are changed, wherein the amount of ammonium molybdate is 1g and the amount of ammonium chloride is 2.5g in this example.
Example 9
The present embodiment provides a MoO3/rGO-N composite material and MoO thereof3Preparation method of/rGO-N composite material。
MoO described in this example3the/rGO-N composite material is marked as A9 and comprises nitrogen-doped redox graphene and flaky MoO growing on the surface of the nitrogen-doped redox graphene3The composite material has a three-dimensional porous structure, and the specific preparation steps are basically the same as those of the embodiment 1, except that:
1. and (3) the concentration of the graphene oxide in the aqueous solution is 0.5mg/mL, namely in the step (2), 125mg of GO is added into 250mL of deionized water, and the mixture is magnetically stirred for 30min and subjected to ultrasound treatment for 6h (the water temperature is controlled below 40 ℃) to completely disperse the graphene oxide in the aqueous solution.
2. The amounts of ammonium molybdate and ammonium chloride were varied, and in this example the amount of ammonium molybdate was 1g and the amount of ammonium chloride was 7.5 g.
Example 10
The present embodiment provides a MoO3/rGO-N composite material and MoO thereof3A preparation method of/rGO-N composite material.
MoO described in this example3the/rGO-N composite material is marked as A10 and comprises nitrogen-doped redox graphene and flaky MoO growing on the surface of the nitrogen-doped redox graphene3The composite material has a three-dimensional porous structure, and the specific preparation steps are basically the same as those of example 1, except that the time and temperature of oil bath in the step (2), the time and temperature of reactants in a reaction kettle, and the time and temperature of high-temperature calcination are changed as follows: heating and stirring the mixture solution in an oil bath at 160 ℃ for 2 hours; transferring the mixture solution to a reaction kettle, and reacting for 16h at 210 ℃; the black powder was transferred to a porcelain boat and calcined in a tube furnace at 800 ℃ for 4 hours in a nitrogen atmosphere.
Example 11
The present embodiment provides a MoO3/rGO-N composite material and MoO thereof3A preparation method of/rGO-N composite material.
MoO described in this example3the/rGO-N composite material is marked as A11 and comprises nitrogen-doped redox graphene and flaky MoO growing on the surface of the nitrogen-doped redox graphene3The composite material hasThe three-dimensional porous structure, the specific preparation steps are substantially the same as those of example 1, except that the time and temperature of the oil bath, the time and temperature of the reactants in the reaction kettle, and the time and temperature of the high-temperature calcination in step (2) are changed as follows: heating and stirring the mixture solution in an oil bath at 100 ℃ for 6 hours; transferring the mixture solution to a reaction kettle, and reacting at 150 ℃ for 24 hours; the black powder was transferred to a porcelain boat and calcined in a tube furnace at 550 ℃ for 8 hours in a nitrogen atmosphere.
The MoO prepared in examples 2-11 were tested separately3The electrochemical performance of the/rGO-N composite material A2-A11 is tested by the same method as the method for testing A1 prepared in example 1, and test results show that the A2-A11 prepared in examples 2-11 have better electrochemical performance and good cycling stability, and the capacity of the A2-A11 is still kept at 500mAhg after 50 cycles-1The above.
In addition, the results of scanning electron microscopy on A4-A11 prepared in examples 4-11 were conducted by Hitachi S-4800, and it was found that A2-A11 were all MoO3And a three-dimensional nitrogen-doped reduced graphene oxide.
In other embodiments, when preparing graphene oxide, the suspension after addition of potassium permanganate is stirred at room temperature for about 20h (18-22h) to form a thick slurry.
The technical contents of the present invention are further illustrated by the examples, so as to facilitate the understanding of the reader, but the embodiments of the present invention are not limited thereto, and any technical extension or re-creation based on the present invention is protected by the present invention.
Claims (9)
1. MoO (MoO)3The preparation method of/rGO-N composite material is characterized in that the MoO is prepared3the/rGO-N composite material comprises nitrogen-doped redox graphene and flaky MoO growing on the surface of the nitrogen-doped redox graphene3The composite material has a three-dimensional porous structure;
the preparation method comprises the following steps:
s1, placing the aqueous solution of the graphene oxide, the molybdate and the ammonium salt in an environment of 100-160 ℃, and heating and refluxing for 2-6h to obtain a uniformly dispersed mixed solution; the mass ratio of the graphene oxide to the molybdate to the ammonium salt is 1: (4-8): (20-60);
s2, transferring the obtained mixed solution into a reaction kettle, heating to 150 ℃ and 210 ℃, and reacting for 16-24 h;
s3, filtering the mixed solution after the reaction in the step S2, washing a filter cake, and drying the filter cake to obtain black powder;
and S4, calcining the black powder at high temperature in an inert atmosphere to obtain the composite material.
2. The MoO of claim 13The preparation method of the/rGO-N composite material is characterized by comprising the following steps: in the step S1, the aqueous solution of graphene oxide, molybdate and ammonium salt is heated and refluxed in an oil bath at 100-160 ℃.
3. The MoO of claim 13The preparation method of the/rGO-N composite material is characterized by comprising the following steps: in the step S3, the filter cake is dried by placing the filter cake in a vacuum drying oven at 80 ℃.
4. The MoO of claim 13The preparation method of the/rGO-N composite material is characterized by comprising the following steps: in the step S4, the calcination temperature of the high-temperature calcination is 550-800 ℃, and the calcination time is 4-8 h.
5. The MoO of claim 13The preparation method of the/rGO-N composite material is characterized in that the preparation method of the graphene oxide is as follows:
adding natural graphite powder into concentrated sulfuric acid with the mass fraction of 98%, and stirring at room temperature to add sodium nitrate; then potassium permanganate is continuously added under stirring, and the temperature of the suspension is kept below 20 ℃ during the period of adding the potassium permanganate; then the suspension is stirred for 18-22h at room temperature to form thick slurry; then adding water into the thick slurry and stirring, then adding hydrogen peroxide to change the color of the mixture from brown to yellow and continuously stirring for more than 0.5 h; then filtering the mixture, washing a filter cake and drying to obtain graphene oxide;
the volume ratio of the mass of the natural graphite powder to concentrated sulfuric acid is 1g:30 mL; the mass ratio of the natural graphite powder to the sodium nitrate to the potassium permanganate is 1:0.75: 20; the mass ratio of the natural graphite powder to the volume of water is 1g:128 mL.
6. MoO according to any of claims 1 to 53The preparation method of the/rGO-N composite material is characterized by comprising the following steps: in step S1, the concentration of graphene oxide in the aqueous solution of graphene oxide, molybdate and ammonium salt is 0.5-2.5 mg/mL.
7. MoO according to any of claims 1 to 53The preparation method of the/rGO-N composite material is characterized by comprising the following steps: the molybdate is at least one of ammonium molybdate, sodium molybdate and potassium molybdate.
8. MoO according to any of claims 1 to 53The preparation method of the/rGO-N composite material is characterized by comprising the following steps: the ammonium salt is at least one selected from ammonium chloride, ammonium nitrate and ammonium bromide.
9. The MoO of claim 13MoO prepared by preparation method of/rGO-N composite material3the/rGO-N composite material is used as a lithium ion battery cathode material.
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| "MoO3纳米带/RGO复合材料的制备及其电化学性能研究";纪文旭，等;《无机化学学报》;20150430;第31卷(第4期);第659-665页 * |
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