CN111276678A - Single-layer graphene coated FeS2Preparation method and application of carbon nanotube material - Google Patents
Single-layer graphene coated FeS2Preparation method and application of carbon nanotube material Download PDFInfo
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Abstract
The invention relates to a single-layer graphene coated FeS2The preparation method of the/carbon nano tube composite material comprises the following steps: preparation of Na2S2A solution; dispersing graphene oxide in water to obtain a graphene oxide turbid liquid, and dispersing carbon nanotubes in water to obtain a carbon nanotube turbid liquid; dissolving ferric sulfite in water, adding ascorbic acid, then adding uniformly dispersed graphene oxide turbid liquid and carbon nano tube turbid liquid, and finally adding Na2S2Obtaining a reaction mixed solution from the solution; the reaction mixture is added with nitrogenReflux reaction is carried out in the atmosphere, and the reaction product is cooled, subjected to solid-liquid separation, washed and dried to obtain the single-layer graphene coated FeS2A carbon nanotube composite material. Compared with the prior art, the lithium ion battery cathode material prepared by the method has the advantages of high specific capacity, excellent cycling stability, low cost and the like.
Description
Technical Field
The invention belongs to the technical field of material science and electrochemistry, and particularly relates to a single-layer graphene coated FeS2A preparation method and application of a/carbon nano tube composite material.
Background
As a new clean energy with high efficiency, lithium ion batteries have attracted much attention and have been rapidly developed because of their numerous advantages. Compared with the traditional secondary battery, the lithium ion battery has the advantages of large specific energy density, high working voltage, long cycle life and the like. In practical applications, lithium ion secondary batteries have been successfully commercialized as a main energy source for computers, mobile phones, new energy vehicles, and the like.
Transition Metal Disulfides (TMDs) have attracted considerable attention in the fields of energy storage and conversion, electronic devices, and the like due to their physicochemical properties such as unique crystal structures, excellent mechanical properties, and the like. In terms of technology, TMDs have the advantages of excellent large-current charging and discharging capacity, long cycle life, wide working temperature range and the like, and are a rich and cheap environment-friendly natural resource. Therefore, research on TMDs materials (especially natural minerals) has become one of the most popular topics in the advanced energy field at present.
Pyrite (FeS)2) Is a semiconductor composed of geologically abundant elements (sulfur and iron) due to its high theoretical capacity (890mAh g)-1) Low cost and environmental protection. In fact, Li/FeS2The battery has been commercialized as a primary battery because itHas higher capacity and service life. However, as a negative electrode for rechargeable lithium-ion batteries, the material causes large volume changes and severe capacity fading during charge/discharge cycles, which prevents its use in rechargeable batteries. The common method is to dope carbon material with excellent conductivity to form FeS with reasonable structure2The/carbon composite material effectively buffers the volume change problem and improves the overall conductivity of the material, thereby improving the electrical property of the active material.
Graphene, as a carbon material having a unique two-dimensional planar structure, has structural characteristics such as high electrical conductivity, good ductility, excellent mechanical properties, and the like. Therefore, the electrochemical performance of the electrode material can be effectively improved through the synergistic effect after the graphene is compounded with the cathode material.
Chinese patent CN 105932256A discloses graphene-based FeS2Nano material and its preparation and application. The preparation method comprises the following steps: ultrasonically dispersing graphene oxide in water to obtain a graphene oxide turbid liquid, and adding a reducing agent for ultrasonic treatment to obtain a graphene turbid liquid; mixing Na2Adding S and S into water, heating, stirring and dissolving uniformly to obtain Na2S2A solution; FeSO (ferric oxide) is added4Dissolving in water, mixing with the graphene suspension, and adding Na2S2Heating the solution to 100 ℃, carrying out reflux reaction for 0.5-3 h in an inert gas atmosphere, and carrying out centrifugal separation, drying and grinding on a reaction product to obtain the graphene-based FeS2A nanomaterial; however, when the technology disclosed in the patent is used as a negative electrode material of a lithium ion battery, the conductivity is insufficient, and the electrical properties are to be further improved.
Disclosure of Invention
The invention aims to overcome the defect of poor conductivity in the prior art and provide the single-layer graphene-coated FeS2Preparation method and application of carbon nanotube material.
The purpose of the invention can be realized by the following technical scheme:
single-layer graphene coated FeS2The preparation method of the/carbon nano tube composite material comprises the following steps:
preparation of Na2S2A solution;
dispersing graphene oxide in water to obtain a graphene oxide turbid liquid, and dispersing carbon nanotubes in water to obtain a carbon nanotube turbid liquid;
dissolving ferric sulfite in water, adding ascorbic acid, then adding uniformly dispersed graphene oxide turbid liquid and carbon nano tube turbid liquid, and finally adding Na2S2Obtaining a reaction mixed solution from the solution;
carrying out reflux reaction on the reaction mixed solution in a nitrogen atmosphere, and cooling, carrying out solid-liquid separation, washing and drying on a reaction product to obtain the single-layer graphene coated FeS2A carbon nanotube composite material.
The mass ratio of the graphene oxide to the carbon nano tube is 1.2-2.4: 1; said Na2The ratio of S to graphene oxide is 1 mmol: 0.03-0.06 g.
The mass ratio of the ascorbic acid to the graphene oxide is 1: 1.5-2.
The preparation of Na2S2The solution is prepared by adding sodium sulfide and sulfur powder in equal molar weight into deionized water, heating, stirring and dissolving to obtain Na2S2And (3) solution.
The sodium sulfide is Na2S·9H2O。
The graphene oxide and the carbon nano tube are dispersed in water through ultrasound.
The reaction time of the reflux reaction is 0.5-1.5 hours, preferably 1 hour.
The solid-liquid separation method is centrifugation; the washing method is to centrifugally wash the solid by using deionized water and ethanol.
The invention also provides the single-layer graphene coated FeS prepared by the preparation method2Application of/carbon nanotube composite material, and single-layer graphene coated FeS2And uniformly stirring and mixing the carbon nanotube composite material and the binder, coating the mixture on a copper foil, and drying to obtain the lithium ion battery cathode.
Said single layerGraphene coated FeS2The mass ratio of the carbon nanotube composite material to the binder is 9: 1; the binder is PVDF.
The invention further introduces the carbon nano tube into the system, and the reversible energy density of the carbon nano tube is matched with the common graphite anode material, so the carbon nano tube can be used as the primary choice of the electrode material of the lithium ion battery. The volume expansion problem of the battery can be relieved by using the material. In addition, the battery improved by using the carbon nano tube has excellent stability and cycle performance, the discharge capacity of the lithium ion battery is obviously improved, and the battery performance is also improved.
Therefore, in the further preparation of the lithium ion negative electrode material, the composite material and the binder are only required to be mixed, and the conductive carbon is not added, so that the specific gravity of the active substance is increased.
Compared with the prior art, the invention has the following advantages:
(1) preparation of single-layer graphene coated FeS by liquid phase deposition2Method for preparing/carbon nanotube composite material capable of making FeS2The particles and the carbon nano tubes are coated in the middle of the graphene sheet layer, so that the method is simple and convenient and is easy to operate;
(2) the method takes the graphene and the carbon nano tube as raw materials, so that the method has designability and low cost;
(3) the single-layer graphene coated FeS prepared by the method2The carbon nanotube composite material has high specific capacity and rate capability, and has wide application prospect in the field of rechargeable batteries;
(4) the composite material provided by the invention has excellent electrochemical performance as a lithium ion battery cathode, and has the characteristics of high specific capacity, excellent cycling stability, low cost and the like; the method conforms to the green development trend of the lithium ion battery, and has good application prospect in the fields of energy batteries, mobile portable small batteries and the like.
Drawings
FIG. 1 shows a single-layer graphene-coated FeS obtained in example 12SEM photograph of the/carbon nanotube composite material;
FIG. 2 shows single-layer graphene-coated FeS obtained in examples 1 to 32The/carbon nanotube composite material is used as a cycle performance diagram of the lithium ion battery cathode material;
FIG. 3 shows single-layer graphene-coated FeS obtained in examples 1 to 32The multiplying power performance diagram of the carbon nanotube composite material as the lithium ion battery cathode material.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
Single-layer graphene coated FeS2The preparation method of the carbon nanotube composite material is characterized in that the prepared composite material is used as a lithium ion battery cathode material, and the electrochemical performance of the lithium ion battery cathode material is tested.
(1) 4mmol of Na2S·9H2O and 4mmol of sulfur powder are put into a beaker filled with 50mL of deionized water, and magnetic stirring is carried out while heating until a brown yellow solution A is formed. 0.12g of graphene oxide solution and 0.1g of carbon nanotubes are respectively dissolved in a 20mL beaker for uniform ultrasonic dispersion. 2mmolFeSO4·7H2Dissolving O in 20mL of deionized water, adding 0.06g of ascorbic acid, and then adding the uniformly dispersed graphene oxide solution and the carbon nano tubes for mixing. Finally adding the solution A in N2Refluxing for 1h under atmosphere gave a black precipitate. Naturally cooling the black precipitate to room temperature, centrifuging the material by using deionized water and ethanol, and drying at 60 ℃ to obtain rGO-coated mesoporous single-layer graphene-coated FeS2Carbon nanotube composite material, denoted FeS2a/CNTs/rGO-1 composite material. The single-layer graphene-coated FeS2SEM photograph of/CNTs/rGO-1 composite material is shown in FIG. 1, and it can be seen from FIG. 1 that the shaded part of black color is FeS2Particles, the sides of which have been covered with stonesShading of graphene sheets, FeS indicated in the figure2The particles and the carbon nanotubes are coated in the middle of the graphene sheet layer.
(2) Uniformly stirring the composite material and the binder (PVDF) according to the proportion of 9:1 by magnetic force, coating the mixture on a copper foil, drying and cutting the copper foil into pole pieces with uniform size. The obtained composite material is used as a negative electrode material of the lithium ion battery to assemble a lithium ion button type half battery, and a pure lithium sheet is used as a counter electrode. Mixing 1M LiPF6The electrolyte is prepared by dissolving the materials in a mixed solution of Ethylene Carbonate (EC) and dimethyl carbonate (DMC) (the volume ratio is 1:1), electrochemical tests are carried out by using a button type half cell, and the cycle performance graph and the rate performance graph are respectively shown in figures 2 and 3.
Example 2
Single-layer graphene coated FeS2The preparation method of the carbon nanotube composite material is characterized in that the prepared composite material is used as a lithium ion battery cathode material, and the electrochemical performance of the lithium ion battery cathode material is tested.
(1) 4mmol of Na2S·9H2O and 4mmol of sulfur powder are put into a beaker filled with 50mL of deionized water, and magnetic stirring is carried out while heating until a brown yellow solution A is formed. 0.18g of graphene oxide solution and 0.1g of carbon nanotubes are dissolved in a 20mL beaker and uniformly dispersed by ultrasonic. 4mmol of FeSO4·7H2Dissolving O in 20mL of deionized water, adding 0.12g of ascorbic acid, and then adding the uniformly dispersed graphene oxide solution for mixing. Finally adding the solution A in N2Refluxing for 1h under atmosphere gave a black precipitate. Naturally cooling the black precipitate to room temperature, centrifuging the material by using deionized water and ethanol, and drying at 60 ℃ to obtain rGO-coated mesoporous single-layer graphene-coated FeS2Carbon nanotube composite material, denoted FeS2a/CNTs/rGO-2 composite material. The single-layer graphene coated FeS2SEM photographs of the/CNTs/rGO-2 composite material are shown in FIG. 1;
(2) uniformly stirring the composite material and the binder (PVDF) according to the proportion of 9:1 by magnetic force, coating the mixture on a copper foil, drying and cutting the copper foil into pole pieces with uniform size. The obtained composite material is used as a negative electrode material of a lithium ion battery to be assembled into a lithium ion button type half battery, and a pure lithium sheet is usedAs a counter electrode. Mixing 1M LiPF6The electrolyte is prepared by dissolving the materials in a mixed solution of Ethylene Carbonate (EC) and dimethyl carbonate (DMC) (the volume ratio is 1:1), electrochemical tests are carried out by using a button type half cell, and the cycle performance graph and the rate performance graph are respectively shown in figures 2 and 3.
Example 3
Single-layer graphene coated FeS2The preparation method of the carbon nanotube composite material is characterized in that the prepared composite material is used as a lithium ion battery cathode material, and the electrochemical performance of the lithium ion battery cathode material is tested.
(1) 4mmol of Na2S·9H2O and 4mmol of sulfur powder are put into a beaker filled with 50mL of deionized water, and magnetic stirring is carried out while heating until a brown yellow solution A is formed. 0.24g of graphene oxide solution and 0.1g of carbon nanotubes are dissolved in a 20mL beaker and uniformly dispersed by ultrasonic. 4mmol of FeSO4·7H2Dissolving O in 20mL of deionized water, adding 0.12g of ascorbic acid, and then adding the uniformly dispersed graphene oxide solution for mixing. Finally adding the solution A in N2Refluxing for 1h under atmosphere gave a black precipitate. Naturally cooling the black precipitate to room temperature, centrifuging the material by using deionized water and ethanol, and drying at 60 ℃ to obtain rGO-coated mesoporous single-layer graphene-coated FeS2Carbon nanotube composite material, denoted FeS2a/CNTs/rGO-3 composite material. The single-layer graphene coated FeS2SEM photograph of/CNTs/rGO-3 composite material is shown in FIG. 1;
(2) uniformly stirring the composite material and the binder (PVDF) according to the proportion of 9:1 by magnetic force, coating the mixture on a copper foil, drying and cutting the copper foil into pole pieces with uniform size. The obtained composite material is used as a negative electrode material of the lithium ion battery to assemble a lithium ion button type half battery, and a pure lithium sheet is used as a counter electrode. Mixing 1M LiPF6The electrolyte is prepared by dissolving the materials in a mixed solution of Ethylene Carbonate (EC) and dimethyl carbonate (DMC) (the volume ratio is 1:1), electrochemical tests are carried out by using a button type half cell, and the cycle performance graph and the rate performance graph are respectively shown in figures 2 and 3.
As can be seen from fig. 2, as the addition amount of graphene increases, the FeS is coated with the single-layer graphene2The performance of the/CNTs/rGO composite material is improved along with the improvement, and FeS is obtained after 50 cycles of circulation2the/CNTs/rGO-3 can still maintain the specific discharge capacity of 745mAh/g, while the FeS2CNTs/rGO-1 and FeS2The FeS is caused by the fact that the addition amount of the/CNTs/rGO-2 is too small2The material is not well coated, resulting in the reduction of electrochemical performance; it can be seen from fig. 3 that the FeS is coated with the single-layer graphene as the addition amount of the graphene increases2The performance of the/CNTs/rGO composite material is improved along with the performance of the FeS under different current densities2The specific discharge capacity of/CNTs/rGO-3 can still be well maintained without special reduction.
Example 4
Single-layer graphene coated FeS2The preparation method of the/carbon nano tube composite material comprises the following steps: adding 4mmol of Na2S·9H2O and 4mmol of sulfur powder are put into a beaker filled with 50mL of deionized water, and magnetic stirring is carried out while heating until a brown yellow solution A is formed. 0.12g of graphene oxide solution and 0.1g of carbon nanotubes are respectively dissolved in a 20mL beaker for uniform ultrasonic dispersion. 2mmolFeSO4·7H2Dissolving O in 20mL of deionized water, adding 0.06g of ascorbic acid, and then adding the uniformly dispersed graphene oxide solution and the carbon nano tubes for mixing. Finally adding the solution A in N2Refluxing for 0.5h under atmosphere gave a black precipitate. Naturally cooling the black precipitate to room temperature, centrifuging the material by using deionized water and ethanol, and drying at 60 ℃ to obtain rGO-coated mesoporous single-layer graphene-coated FeS2Carbon nanotube composite material, denoted FeS2a/CNTs/rGO-1 composite material. The single-layer graphene-coated FeS2SEM photograph of/CNTs/rGO-4 composite material is shown in FIG. 1, and it can be seen from FIG. 1 that the shaded part of black color is FeS2The particles, which have been shaded alongside graphene sheets, show FeS2The particles and the carbon nanotubes are coated in the middle of the graphene sheet layer.
Example 5
Single-layer graphene coated FeS2The preparation method of the/carbon nano tube composite material comprises the following steps: adding 4mmol of Na2S·9H2O and 4mmol of sulfur powder are put into a chamber containing 50mL of deionized waterIn a beaker of water, magnetic stirring was carried out while heating until a brownish yellow solution A was formed. 0.12g of graphene oxide solution and 0.1g of carbon nanotubes are respectively dissolved in a 20mL beaker for uniform ultrasonic dispersion. 2mmolFeSO4·7H2Dissolving O in 20mL of deionized water, adding 0.06g of ascorbic acid, and then adding the uniformly dispersed graphene oxide solution and the carbon nano tubes for mixing. Finally adding the solution A in N2Reflux for 1.5h under ambient conditions gave a black precipitate. Naturally cooling the black precipitate to room temperature, centrifuging the material by using deionized water and ethanol, and drying at 60 ℃ to obtain rGO-coated mesoporous single-layer graphene-coated FeS2Carbon nanotube composite material, denoted FeS2a/CNTs/rGO-5 composite material. The single-layer graphene-coated FeS2SEM photograph of/CNTs/rGO-1 composite material is shown in FIG. 1, and it can be seen from FIG. 1 that the shaded part of black color is FeS2The particles, which have been shaded alongside graphene sheets, show FeS2The particles and the carbon nanotubes are coated in the middle of the graphene sheet layer.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (10)
1. Single-layer graphene coated FeS2The preparation method of the/carbon nano tube composite material is characterized by comprising the following steps:
preparation of Na2S2A solution;
dispersing graphene oxide in water to obtain a graphene oxide turbid liquid, and dispersing carbon nanotubes in water to obtain a carbon nanotube turbid liquid;
dissolving ferric sulfite in water, adding ascorbic acid, then adding uniformly dispersed graphene oxide turbid liquid and carbon nano tube turbid liquid, and finally adding Na2S2Obtaining a reaction mixed solution from the solution;
refluxing the reaction mixture in nitrogen atmosphere for reactionCooling, solid-liquid separating, washing and drying the product to obtain the single-layer graphene coated FeS2A carbon nanotube composite material.
2. The single-layer graphene-coated FeS according to claim 12The preparation method of the/carbon nanotube composite material is characterized in that the mass ratio of the graphene oxide to the carbon nanotube is 1.2-2.4: 1; said Na2The ratio of S to graphene oxide is 1 mmol: 0.03-0.06 g.
3. The single-layer graphene-coated FeS according to claim 12The preparation method of the/carbon nanotube composite material is characterized in that the mass ratio of the ascorbic acid to the graphene oxide is 1: 1.5-2.
4. The single-layer graphene-coated FeS according to claim 12The preparation method of the/carbon nano tube composite material is characterized in that the Na is prepared2S2The solution is prepared by adding sodium sulfide and sulfur powder in equal molar weight into deionized water, heating, stirring and dissolving to obtain Na2S2And (3) solution.
5. The single-layer graphene-coated FeS according to claim 42The preparation method of the/carbon nano tube composite material is characterized in that the sodium sulfide is Na2S·9H2O。
6. The single-layer graphene-coated FeS according to claim 12The preparation method of the/carbon nanotube composite material is characterized in that the graphene oxide and the carbon nanotube are dispersed in water through ultrasound.
7. The single-layer graphene-coated FeS according to claim 12The preparation method of the/carbon nano tube composite material is characterized in that the reaction time of the reflux reaction is 0.5-1.5 hoursIn this case, the time is preferably 1 hour.
8. The single-layer graphene-coated FeS according to claim 12The preparation method of the carbon nanotube composite material is characterized in that the solid-liquid separation method is centrifugation; the washing method is to centrifugally wash the solid by using deionized water and ethanol.
9. Single-layer graphene-coated FeS prepared by adopting preparation method of claim 12The application of the/carbon nano tube composite material is characterized in that the single-layer graphene coated FeS2And uniformly stirring and mixing the carbon nanotube composite material and the binder, coating the mixture on a copper foil, and drying to obtain the lithium ion battery cathode.
10. The single-layer graphene-coated FeS according to claim 92The application of the/carbon nano tube composite material is characterized in that the single-layer graphene coated FeS2The mass ratio of the carbon nanotube composite material to the binder is 9: 1; the binder is PVDF.
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| CN113140721B (en) * | 2021-04-21 | 2022-04-19 | 南京航空航天大学 | Self-supporting aluminum ion battery positive electrode material, preparation method thereof and aluminum-air battery |
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