CN110759333A - Graphene-coated electrode material Ni5P4@ rGO and preparation method and application thereof - Google Patents
Graphene-coated electrode material Ni5P4@ rGO and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses an electrode material Ni wrapped by graphene5P4@ rGO and its preparation and application. Ni5P4The nanoparticles are uniformly encapsulated by rGO nanoplatelets. Preparation procedureAdding nickel salt and graphene oxide into a mixed solvent of methanol and DMF (dimethyl formamide) for hydrothermal reaction to obtain a precursor of graphene nickel. Then, an electrode material Ni coated by graphene is obtained through phosphating treatment5P4@ rGO. Overcomes the problem that pure-phase pentanickel tetraphosphorylation is often not obtained before. The material is used as the negative electrode material of the sodium ion battery for the first time, and shows good cycle performance and rate capability, which has positive significance for realizing industrialization of the sodium ion battery. Meanwhile, the preparation process is simple, the cost is low, the yield is high, and the efficiency is high.
Description
Technical Field
The invention belongs to the technical field of electrode materials, and particularly relates to a graphene-coated electrode material Ni5P4@ rGO and a preparation method and application thereof.
Background
Since the new century, lithium ion batteries have been widely used in people's daily lives, such as electric vehicles, portable electronic products, etc., but further development of lithium ion batteries has been limited due to lack of lithium resources on earth. Sodium, as a "sister" of lithium, not only has similar physicochemical properties to lithium, but also the sodium content far exceeds that of lithium, which makes sodium-ion batteries increasingly popular with researchers. However, the radius of sodium ions (1.02A) is 1.3 times that of lithium ions (0.76A), resulting in poor rate and cycling performance.
Transition metal phosphides are of great interest because of their high theoretical specific capacity. In particular Ni5P4Has a theoretical specific capacity of 767mA h/g and can be considered as a very promising anode material. But at present Ni5P4There have been no reports on sodium ion batteries. Mainly because of the difficulty in synthesizing pure phases, Ni is generally synthesized5P4And NiP2Or Ni5P4And Ni2P, as in the literature "Structure of Nickel-phosphorus Compound negative electrode Material for lithium ion batteriesIn the research of modulation and electrochemical modification, pure-phase Ni is synthesized by a three-step method5P4@ C, the performance is attenuated after fifty cycles of running in the lithium ion battery, and the problems of low conductivity and overlarge volume change of the transition metal phosphide in the process of inserting/embedding lithium ions are not solved.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a graphene-coated electrode material Ni5P4@ rGO and a preparation method and application thereof. The method utilizes graphene to wrap Ni5P4The material prevents volume transition expansion caused in the process of sodium insertion and sodium removal, thereby reducing performance attenuation.
The object of the present invention is achieved by at least one of the following technical means.
Graphene-coated electrode material Ni5P4The preparation method of @ rGO comprises the following steps:
(1) dissolving nickel salt and graphene oxide in a solvent, and stirring and mixing to obtain a light green solution;
(2) adding urea into the light green solution, and then heating in a closed pressure-resistant reaction gas for reaction;
(3) cooling, collecting the precipitate, washing and drying to obtain a precursor of the graphene nickel;
(4) placing the precursor of the graphene nickel and sodium hypophosphite in a tubular furnace, arranging the sodium hypophosphite upstream, and introducing Ar/H into the reaction furnace2The airflow reacts to finally obtain the electrode material Ni5P4@rGO。
Further, in the step (1), the solvent is a mixed solvent of methanol and N, N-dimethylformamide; the nickel salt is nickel chloride, nickel nitrate or nickel sulfate.
Further, the volume ratio of methanol to DMF is 2.5-3.5: 1.
further, in the step (1), the concentration of nickel salt in the light green solution is 10-13 mg/ml, and the concentration of graphene oxide is 0.2-2.5 mg/ml.
Further, in the step (2), the molar ratio of urea to nickel salt is 0.35-0.45: 1.
further, in the step (2), the reaction temperature is 140-160 ℃, and the reaction time is 120-720 min.
Further, in the step (3), the freeze drying temperature is-60 to-30 ℃, and the time is 12 to 24 hours.
Further, in the step (4), the mass ratio of the sodium hypophosphite to the precursor of the graphene nickel is 1: 18 to 22.
Further, in the step (4), the reaction temperature is 350-450 ℃, and the reaction time is 1.8-2.2 h.
Electrode material Ni prepared by the above preparation method5P4@rGO。
Another object of the present invention is to provide a negative electrode sheet for a battery, wherein the active material of the negative electrode sheet is the above-mentioned electrode material Ni5P4@rGO。
Another object of the present invention is to provide a sodium ion battery, wherein the active material of the negative electrode sheet of the sodium ion battery is the above-mentioned electrode material Ni5P4@rGO。
Method for preparing electrode material of the present invention and conventional Ni5P4The preparation method is simpler, the obtained phase is pure, the cost is low, the yield is high, and the efficiency is high. And is applied to sodium ion batteries for the first time, and Ni is added to solve the problem of volume transition expansion of transition metal phosphide after sodium insertion and sodium removal5P4And compounding with graphene. The material is used as the cathode material of the sodium ion battery to show good cycle performance and rate performance, which has positive significance for realizing industrialization of the sodium ion battery.
Drawings
FIG. 1 shows Ni prepared in example 15P4XRD pattern of (a);
FIG. 2 shows Ni prepared in example 15P4SEM picture of (1);
FIG. 3 shows Ni, a material prepared in example 25P4The XRD pattern of @ rGO;
FIG. 4 shows an embodimentExample 2 preparation of material Ni5P4SEM picture of @ rGO;
FIG. 5 shows Ni as a precursor of example 35P4And Ni5P4The rate performance graph of the sodium ion battery with @ rGO as a negative electrode material and different current densities;
FIG. 6 shows Ni as a component of example 35P4And Ni5P4@ rGO is used as a negative electrode material, and the long cycle performance of the sodium ion battery with the current density of 0.2A/g is shown.
Detailed Description
The invention is further described with reference to the following figures and detailed description of embodiments.
Example 1
Weighing 30mL of methanol, pouring 10mL of N, N-dimethylformamide into a 50mL beaker, stirring for three minutes to obtain a uniformly mixed solution, weighing 475.38mg (2mmol) of nickel chloride hexahydrate into the mixed solution, stirring for ten minutes to dissolve the nickel chloride hexahydrate to obtain a light green solution, adding 300mg (5mmol) of urea into the mixed solution while stirring, stirring for twenty minutes, transferring the uniformly obtained solution into a 50mL Teflon-lined autoclave, sealing the autoclave, keeping the oven at 150 ℃ for 720 minutes, naturally cooling to room temperature, collecting the generated green precipitate, washing with water for three times, putting the sample into a freeze dryer at-40 ℃ for drying for 12 hours to obtain a precursor α Ni (OH)2。
0.1g of prepared precursor α Ni (OH)2And 2.0g of sodium hypophosphite (NaH)2PO2·H2O) in two separate quartz boats, the tube furnace being charged upstream with NaH2PO2·H2And O. At Ar/H2Heating at 400 deg.C for 2 hr under air flow to obtain Ni5P4。
As shown in FIG. 1, Ni prepared in example 15P4XRD pattern of (a). The diffraction peak of the synthesized material and hexagonal phase Ni can be known by comparing with a standard card5P4Complete agreement of (PDF No.18-0883), indicating that pure phase Ni has been synthesized5P4。
As shown in the figure2, it can be seen by Scanning Electron Microscope (SEM) that the above method produces Ni5P4Nanoparticles.
Example 2
30ml of methanol and 10ml of N, N-dimethylformamide were weighed into a 50ml beaker and stirred for three minutes to obtain a uniformly mixed solution. 475.38mg (2mmol) of nickel chloride hexahydrate and 80mg of graphene oxide were weighed into the mixed solution and stirred for ten minutes so that the nickel chloride hexahydrate was dissolved to obtain a pale green solution. To the mixed solution was added 300mg (5mmol) of urea with stirring, and the mixture was further stirred for twenty minutes. The resulting homogeneous solution was transferred to a 50mL teflon lined autoclave. The autoclave was sealed, held in an oven at 150 degrees celsius for 720 minutes, and then allowed to cool naturally to room temperature. Collecting the generated green precipitate, washing with water for three times, and drying the sample in a freeze dryer at-40 ℃ for 12h to obtain the precursor of the graphene nickel.
0.1g of prepared precursor of graphene nickel and 2.0g of sodium hypophosphite (NaH)2PO2·H2O) in two separate quartz boats, the tube furnace being charged upstream with NaH2PO2·H2And O. At Ar/H2Heating at 400 deg.C for 2 hr under air flow to obtain Ni5P4@rGO。
As shown in FIG. 4, it can be seen from a Scanning Electron Microscope (SEM) that Ni was produced5P4Is wrapped by the rGO nano-sheet to form a three-dimensional network structure.
As shown in fig. 3, i.e., Ni prepared in example 25P4@ rGO @ atlas. Also by comparison with a standard card, the diffraction peak of the synthesized material and hexagonal phase Ni can be seen5P4(PDF No.18-0883) and the appearance of a broad diffraction peak around 25 ℃ corresponds to that of graphene, indicating that pure-phase Ni has been synthesized5P4@rGO。
Example 3
The electrode materials of example 1 and example 2 were respectively ground into powders, super P, PVDF and NMP were added to the powders, the powders were ground into slurry, the slurry was coated on a copper foil, a battery was placed in a glove box, and a sodium ion battery cycle performance test was performed using a blue electricity system.
As shown in FIG. 5, Ni prepared in examples 1 and 25P4And Ni5P4The cycling performance of @ rGO at different current densities, as can be seen from the figure, Ni at different current densities5P4Performance ratio of @ rGO Ni5P4Excellent and shows excellent rate performance.
As shown in FIG. 6, Ni prepared in examples 1 and 25P4And Ni5P4Circulation performance of @ rGO composite material at 0.2A/g current, Ni5P4The specific capacity of @ rGO reaches 304mA h/g relative to Ni5P4The good is that the wrapping of graphene helps to improve the conductivity of the material and alleviate the problem of volume expansion during the circulation process.
Example 4
30ml of methanol and 10ml of N, N-dimethylformamide were weighed into a 50ml beaker and stirred for three minutes to obtain a uniformly mixed solution. 400mg (1.7mmol) of nickel chloride hexahydrate and 8mg of graphene oxide were weighed out into the mixed solution and stirred for ten minutes so that the nickel chloride hexahydrate was dissolved to obtain a pale green solution. To the mixed solution was added 300mg (5mmol) of urea with stirring, and the mixture was further stirred for twenty minutes. The resulting homogeneous solution was transferred to a 50mL teflon lined autoclave. The autoclave was sealed, held in an oven at 150 degrees celsius for 720 minutes, and then allowed to cool naturally to room temperature. Collecting the generated green precipitate, washing with water for three times, and drying the sample in a freeze dryer at-40 ℃ for 12h to obtain the precursor of the graphene nickel.
0.1g of prepared precursor of graphene nickel and 2.0g of sodium hypophosphite (NaH)2PO2·H2O) in two separate quartz boats, the tube furnace being charged upstream with NaH2PO2·H2And O. At Ar/H2Heating at 450 deg.C for 2 hr under air flow to obtain Ni5P4@rGO。
Example 5
30ml of methanol and 10ml of N, N-dimethylformamide were weighed into a 50ml beaker and stirred for three minutes to obtain a uniformly mixed solution. 475.38mg (2mmol) of nickel chloride hexahydrate and 100mg of graphene oxide were weighed into the mixed solution and stirred for ten minutes so that the nickel chloride hexahydrate was dissolved to obtain a pale green solution. 267mg (4.4mmol) of urea was added to the mixed solution with stirring, and the mixture was further stirred for twenty minutes. The resulting homogeneous solution was transferred to a 50mL teflon lined autoclave. The autoclave was sealed, held in an oven at 150 degrees celsius for 720 minutes, and then allowed to cool naturally to room temperature. Collecting the generated green precipitate, washing with water for three times, and drying the sample in a freeze dryer at-40 ℃ for 12h to obtain the precursor of the graphene nickel.
0.1g of prepared precursor of graphene nickel and 2.2g of sodium hypophosphite (NaH)2PO2·H2O) in two separate quartz boats, the tube furnace being charged upstream with NaH2PO2·H2And O. At Ar/H2Heating at 350 deg.C for 1.8 hr under air flow to obtain Ni5P4@rGO。
Example 6
30ml of methanol and 10ml of N, N-dimethylformamide were weighed into a 50ml beaker and stirred for three minutes to obtain a uniformly mixed solution. 520mg (2.19mmol) of nickel chloride hexahydrate and 20mg of graphene oxide were weighed into the mixed solution and stirred for ten minutes so that the nickel chloride hexahydrate was dissolved to obtain a pale green solution. 375mg (6.26mmol) of urea was added to the mixed solution with stirring, and stirred for twenty minutes. The resulting homogeneous solution was transferred to a 50mL teflon lined autoclave. The autoclave was sealed, held in an oven at 140 degrees celsius for 720 minutes, and then allowed to cool naturally to room temperature. Collecting the generated green precipitate, washing with water for three times, and drying the sample in a freeze dryer at-60 ℃ for 12h to obtain the precursor of the graphene nickel.
0.1g of prepared precursor of graphene nickel and 1.8g of sodium hypophosphite (NaH)2PO2·H2O) in two separate quartz boats, the tube furnace being charged upstream with NaH2PO2·H2And O. At Ar/H2Heating at 400 deg.C for 2 hr under air flow to obtain Ni5P4@rGO。
Example 7
30ml of methanol and 10ml of N, N-dimethylformamide were weighed into a 50ml beaker and stirred for three minutes to obtain a uniformly mixed solution. 475.38mg (2mmol) of nickel chloride hexahydrate and 20mg of graphene oxide were weighed into the mixed solution and stirred for ten minutes so that the nickel chloride hexahydrate was dissolved to obtain a pale green solution. To the mixed solution was added 300mg (5mmol) of urea with stirring, and the mixture was further stirred for twenty minutes. The resulting homogeneous solution was transferred to a 50mL teflon lined autoclave. The autoclave was sealed, held in an oven at 160 degrees celsius for 120 minutes, and then allowed to cool naturally to room temperature. Collecting the generated green precipitate, washing with water for three times, and drying the sample in a freeze dryer at-30 ℃ for 24h to obtain the precursor of the graphene nickel.
0.1g of prepared precursor of graphene nickel and 2.0g of sodium hypophosphite (NaH)2PO2·H2O) in two separate quartz boats, the tube furnace being charged upstream with NaH2PO2·H2And O. At Ar/H2Heating at 450 deg.C for 2.2 hr under air flow to obtain Ni5P4@rGO。
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any equivalent alterations, modifications or improvements made by those skilled in the art to the above-described embodiments using the technical solutions of the present invention are still within the scope of the technical solutions of the present invention.
Claims (10)
1. Graphene-coated electrode material Ni5P4The preparation method of @ rGO is characterized by comprising the following steps:
(1) dissolving nickel salt and graphene oxide in a solvent, and stirring and mixing to obtain a light green solution;
(2) adding urea into the light green solution, and then heating in a closed pressure-resistant reaction gas for reaction;
(3) cooling, collecting the precipitate, washing and drying to obtain a precursor of the graphene nickel;
(4) placing the precursor of the graphene nickel and sodium hypophosphite in a tubular furnace, wherein the sodium hypophosphite is arrangedIntroducing Ar/H into the reaction furnace at upstream2The airflow reacts to finally obtain the graphene-coated electrode material Ni5P4@rGO。
2. The production method according to claim 1, wherein in the step (1), the solvent is a mixed solvent of methanol and N, N-dimethylformamide, and the nickel salt is nickel chloride, nickel nitrate or nickel sulfate; in the step (1), the concentration of the nickel salt in the light green solution is 10-13 mg/ml, and the concentration of the graphene oxide is 0.2-2.5 mg/ml.
3. The preparation method according to claim 1, wherein in the step (2), the molar ratio of the nickel salt to the urea is 0.35-0.45: 1.
4. the method according to claim 1, wherein in the step (2), the reaction temperature is 140 to 160 ℃ and the reaction time is 120 to 720 min.
5. The preparation method according to claim 1, wherein in the step (3), the freeze-drying temperature is-60 to-30 ℃ and the time is 12 to 24 hours.
6. The preparation method according to claim 1, wherein in the step (4), the mass ratio of the sodium hypophosphite to the graphene nickel precursor is 1: 18 to 22.
7. The preparation method according to claim 1, wherein the reaction temperature in the step (4) is 350-450 ℃ and the reaction time is 1.8-2.2 h.
8. The graphene-coated pentanickel tetraphosphorate prepared by the method according to any one of claims 1 to 7.
9. A negative electrode plate of a battery is characterized in that the active substance of the negative electrode plate of the battery isObtaining the electrode material Ni coated by the graphene of 85P4@rGO。
10. A sodium-ion battery, characterized in that the active material of the negative plate of the sodium-ion battery is the graphene-coated electrode material Ni of claim 85P4@rGO。
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| CN107403911A (en) * | 2017-06-20 | 2017-11-28 | 江苏大学 | Graphene/transition metal phosphide/C-base composte material, preparation method and lithium ion battery negative electrode |
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| CN107403911A (en) * | 2017-06-20 | 2017-11-28 | 江苏大学 | Graphene/transition metal phosphide/C-base composte material, preparation method and lithium ion battery negative electrode |
| CN107665984A (en) * | 2017-09-13 | 2018-02-06 | 哈尔滨工业大学 | A kind of preparation method of the lithium sulfur battery anode material based on the graphene-supported phosphatization nickel material of phosphorus doping |
| CN109659544A (en) * | 2018-12-24 | 2019-04-19 | 肇庆市华师大光电产业研究院 | A kind of lithium/anode material of lithium-ion battery preparation method of graphene coated bimetallic sulfide |
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| Title |
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| HONGLEI WANG ET. AL.: ""Flower-Like Nickel Phosphide Microballs Assembled by Nanoplates with Exposed High-Energy (001) Facets: Efficient Electrocatalyst for the Hydrogen Evolution Reaction"", 《CHEMSUSCHEM》 * |
| JIANG J. ET. AL.: "One-pot synthesis of carbon-coated Ni5P4 nanoparticles and CoP nanorods for high-rate and high-stability lithium-ion batteries", 《JOURNAL OF MATERIALS CHEMISTRY A》 * |
| MA TG. ET. AL.: "Iron-Doped Ni5P4 Ultrathin Nanoporous Nanosheets for water Splitting and On-Demand Hydrogen Release via NaBH4 Hydrolysis", 《ACS APPLIED NANO MATERIALS》 * |
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