CN113511647A - Preparation method of nickel diselenide/reduced graphene oxide composite material derived from nickel-based metal organic framework - Google Patents
Preparation method of nickel diselenide/reduced graphene oxide composite material derived from nickel-based metal organic framework Download PDFInfo
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Abstract
The invention provides a preparation method of nickel diselenide/reduced graphene oxide composite material derived from a nickel-based metal organic framework.
Description
Technical Field
The invention relates to a preparation method of a nickel diselenide/reduced graphene oxide composite material derived from a nickel-based metal organic framework.
Background
The super capacitor is a novel energy storage device, and has the characteristics of high power density, short charging time, long service life, good temperature characteristic, energy conservation, environmental protection and the like, so the super capacitor has wide application. The excellent electrochemical performance of the transition metal oxide makes the transition metal oxide an ideal choice for high-performance pseudocapacitance electrode materials. Among them, nickel oxide-based materials are considered to be promising electrode materials due to their excellent electrochemical stability and higher theoretical specific capacitance, and their advantages of low toxicity, low cost and abundant resources. However, their use in electrochemical energy storage materials is limited due to poor electrical conductivity. The transition metal selenide serving as an electrode material has high theoretical specific capacitance and higher conductivity compared with the same family sulfide, but can fall off due to expansion and contraction of the electrode material in the charge-discharge cycle process.
Disclosure of Invention
The invention aims to provide a preparation method of nickel diselenide/reduced graphene oxide composite material derived from a nickel-based metal organic framework. Transition metal selenides, as a class of electrode materials, have high theoretical specific capacitance and higher electrical conductivity than that of the same family of sulfides, but can also fall off due to expansion and contraction of the electrode materials in the charge-discharge cycle process. The nickel-based metal organic framework material can be self-assembled on the surface of a graphene oxide sheet to obtain nickel-based MOFs nano particles which are uniformly distributed, and the graphene has high specific surface area and excellent mechanical and electrical properties and can effectively improve the cycling stability of the electrode material.
In order to realize the purpose, the technical scheme is as follows: a preparation method of nickel-based metal organic framework derived nickel diselenide/reduced graphene oxide composite material comprises the following steps:
(1) dissolving nickel nitrate hexahydrate and hexa (4-carboxyphenoxy) cyclotriphosphazene in a first organic solvent, and uniformly mixing at room temperature to obtain a solution A;
ultrasonically dispersing graphene oxide in a second organic solvent to obtain a solution B;
(2) adding the solution B into the solution A, and stirring and refluxing at 160-170 ℃ to obtain a mixed solution C;
(3) and (3) calcining the precursor obtained by centrifuging, washing and drying the mixed solution C and selenium powder at the temperature of 450-550 ℃ in a protective atmosphere to obtain the nickel diselenide/reduced graphene oxide composite material derived from the nickel-based metal organic framework.
The graphene has unique two-position morphology, high conductivity and large specific surface area, and has outstanding advantages in the field of electrochemical energy storage. The graphene oxide sheet can be stably dispersed in an organic solvent, because the surface of the graphene oxide sheet has a large number of functional groups, such as hydroxyl, epoxy, carboxyl and the like, and the functional groups can be used as anchor points of a metal organic framework material growing on the surface of graphene.
Therefore, graphene with a nickel-based metal organic framework material growing on the surface is obtained through high-temperature reflux, and the graphene and selenium powder can be converted into a selenide/carbon composite material through one-step simple calcination, so that an electrode material with excellent performance is prepared.
When the calcination temperature in the step (3) is not lower than 650 ℃, the nickel diselenide/reduced graphene oxide composite material cannot be obtained.
Preferably, the weight ratio of nickel nitrate hexahydrate to hexa (4-carboxyphenoxy) cyclotriphosphazene in step (1) is 133: 146-133: 148. more preferably, the weight ratio of nickel nitrate hexahydrate to hexa (4-carboxyphenoxy) cyclotriphosphazene in step (1) is 133: 146.
preferably, the first organic solvent in step (1) comprises at least one of N, N-dimethylformamide and dimethyl sulfoxide, and the second organic solvent is at least one of N, N-dimethylformamide and dimethyl sulfoxide.
Preferably, the weight ratio of the product obtained by reacting nickel nitrate hexahydrate and hexa (4-carboxyphenoxy) cyclotriphosphazene in the step (2) to graphene oxide is 100: 2.9-100: 3.1; more preferably, the weight ratio of the product obtained by reacting nickel nitrate hexahydrate and hexa (4-carboxyphenoxy) cyclotriphosphazene in the step (2) to graphene oxide is 100: 3.
Preferably, the stirring reflux time in the step (2) is 2-2.5 h. More preferably, the stirring reflux time in the step (2) is 2 h.
Preferably, the calcination time in the step (3) is 2-4 h, and the temperature rise rate of the calcination is 1-2 ℃/min.
Preferably, the protective atmosphere in step (3) is argon or nitrogen.
Preferably, the weight ratio of the precursor to the selenium powder in the step (3) is 1: 4-1: 5. more preferably, the weight ratio of the precursor to the selenium powder in the step (3) is 1: 5.
preferably, the drying in the step (3) is vacuum drying.
The invention provides a nickel diselenide/reduced graphene oxide composite material derived from a nickel-based metal organic framework, which is prepared by adopting the preparation method.
The invention provides application of the nickel diselenide/reduced graphene oxide composite material in the field of supercapacitors or energy storage.
Has the advantages that:
1. according to the invention, nitrogen, phosphorus and oxygen co-doped ligand hexa (4-carboxyphenoxy) cyclotriphosphazene (4-carboxyphenyloxy) -cyclotriphosphazene, CTP-COOH), nickel nitrate hexahydrate and graphene oxide are refluxed and stirred at 160 ℃ to synthesize graphene with a nickel-based metal organic framework material growing on the surface, wherein metal ions and organic matters are respectively converted into nickel-based oxide and a carbon material, and a nanoparticle structure with mutual connection is formed on the surface of the graphene. And calcining the graphene with the nickel-based metal organic framework material growing on the surface and selenium powder at high temperature to generate the composite material of nickel diselenide/reduced graphene oxide. Based on the characteristics of the size of the nano particles, more active sites are exposed, and the reaction area of ions is effectively increased; the graphene has high specific surface area and excellent mechanical and electrical properties, and can effectively improve the cycling stability of the electrode material; the nickel diselenide as an electrode material has high theoretical specific capacitance and higher conductivity compared with the same family sulfide. The nickel diselenide/reduced graphene oxide is compounded as the electrode material of the super capacitor, so that not only can higher specific capacity be obtained, but also the electrochemical stability of the super capacitor can be obviously improved.
2. According to the invention, the nickel diselenide/reduced graphene oxide composite material can be obtained by controlling the reaction conditions, the obtained composite material has a nanoparticle structure, small size and large specific surface area, and the nanoparticles and the graphene sheets are self-assembled, so that the ion transmission rate can be effectively increased, and the cycle stability of the composite material is improved.
3. In the preparation process provided by the invention, the nickel-based metal organic framework material/reduced graphene oxide precursor (namely, graphene with the surface growing nickel-based metal organic framework material) is prepared by reflux stirring, and then the precursor and selenium powder are calcined in one step to prepare the electrode material, so that the reaction condition is convenient to control, the operation is simple, the production cost is low, and the industrial production is easy to realize.
Drawings
FIG. 1 is a nickel-based metal organic framework-derived nickel diselenide/reduced graphene oxide composite (NiSe) prepared in example 12/rGO-450).
FIG. 2 is a nickel-based metal organic framework-derived nickel diselenide/reduced graphene oxide composite (NiSe) prepared in example 12/rGO-450).
FIG. 3 is a nickel-based metal organic framework-derived nickel diselenide/reduced graphene oxide composite (NiSe) prepared in example 22/rGO-550).
FIG. 4 is a nickel-based metal organic framework-derived nickel diselenide/reduced graphene oxide composite (NiSe) prepared in example 22/rGO-550).
FIG. 5 is a nickel-based metal organic framework-derived nickel diselenide/reduced graphene oxide composite (NiSe) prepared in example 22/rGO-550) cycle performance plot.
FIG. 6 shows NiSe in the Ni-based MOFs-derived nickel diselenide/reduced graphene oxide composites prepared in examples 1-42PerGO-550 rate performance diagram.
Fig. 7 is an X-ray powder diffraction pattern of nickel-based metal organic framework-derived nickel diselenide/reduced graphene oxide composite prepared in example 1-2.
Fig. 8 is an SEM photograph of the nickel-based metal organic framework-derived nickel diselenide/reduced graphene oxide composite material prepared in example 1-2.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Example 1
The embodiment provides a preparation method of a nickel-based metal organic framework derived nickel diselenide/reduced graphene oxide composite material, which comprises the following steps:
(1) adding 133mg of nickel nitrate hexahydrate and 146mg of hexa (4-carboxyphenoxy) cyclotriphosphazene (CTP-COOH) into 28mL of N-N dimethylformamide solution, and stirring at room temperature for 10min to obtain a mixed solution A;
adding 5mL of graphene oxide solution (2mg/mL) into 23mL of N-N dimethylformamide solution, and performing ultrasonic treatment in a probe ice bath for 20min to obtain solution B;
(2) adding 20mL of the solution B into the mixed solution A, and refluxing and stirring for 2h at 160 ℃ to obtain a mixed solution C;
(3) and (2) respectively cleaning and centrifuging the mixed solution C by using N-N dimethylformamide and tetrahydrofuran solution for three times, then carrying out vacuum drying at room temperature for 6h to obtain a precursor, heating the precursor and selenium powder (in a weight ratio of 1: 5) in a nitrogen atmosphere at a speed of 1 ℃/min to 450 and calcining for 3h to obtain the nickel diselenide/reduced graphene oxide composite material derived from the nickel-based metal organic framework, wherein the label is NiSe 2/rGO-450.
Example 2
The embodiment provides a preparation method of a nickel-based metal organic framework derived nickel diselenide/reduced graphene oxide composite material, which comprises the following steps:
(1) adding 133mg of nickel nitrate hexahydrate and 146mg of hexa (4-carboxyphenoxy) cyclotriphosphazene (CTP-COOH) into 28mL of N-N dimethylformamide solution, and stirring at room temperature for 10min to obtain a mixed solution A;
adding 5mL of graphene oxide solution (2mg/mL) into 23mL of N-N dimethylformamide solution, and performing ultrasonic treatment in a probe ice bath for 20min to obtain solution B;
(2) adding 20mL of the solution B into the mixed solution A, and refluxing and stirring at 160 ℃ for 2 hours to obtain a mixed solution C;
(3) and respectively cleaning and centrifuging the mixed solution C by using N-N dimethylformamide and tetrahydrofuran solution for three times, drying the mixed solution C at room temperature for 6h in vacuum, heating the mixed solution C and selenium powder (the mass ratio is 1: 5) in a nitrogen atmosphere at the speed of 1 ℃/min to 550, and calcining the mixture for 3h to prepare the nickel diselenide/reduced graphene oxide composite material derived from the nickel-based metal organic framework, wherein the composite material is marked as NiSe 2/rGO-550.
Performance test methods and results: a piece of foamed nickel (size: 1.2X 4 cm) was placed at room temperature2) Putting into a beaker, sequentially carrying out ultrasonic treatment on the beaker with acetone, 0.5M hydrochloric acid, distilled water and absolute ethyl alcohol for 5 minutes, then drying in vacuum at 60 ℃ and weighing for later use. Grinding the nickel-based metal organic framework-derived nickel diselenide/reduced graphene oxide composite material, the superconducting carbon black and the polyvinylidene fluoride (the mass ratio is 8: 1: 1) in the embodiment 1-2 in a mortar for 30min, dropwise adding an N-methyl pyrrolidone solution, grinding until no granular sensation exists, uniformly coating the slurry on the cleaned and dried foamed nickel, drying in vacuum at 60 ℃ for 12h to obtain a positive working electrode, weighing, using 6M KOH as an electrolyte, a platinum electrode as a counter electrode and a mercury oxide electrode as a reference electrode to perform three-electrode electrochemical processThe test results correspond to fig. 1 to 8. According to the nickel-based metal organic framework derived nickel diselenide/reduced graphene oxide composite material prepared by the invention, nickel diselenide nano particles are uniformly distributed on the surface of a graphene sheet, so that the transmission rate of ions can be effectively improved, and the charge and discharge capacity is ensured not to be attenuated. The nickel-based metal organic framework derived nickel diselenide and the reduced graphene oxide are compounded to be used as the electrode material of the super capacitor, so that higher specific capacity can be obtained, and the electrochemical stability of the super capacitor can be obviously improved.
FIG. 1 is a nickel-based metal organic framework-derived nickel diselenide/reduced graphene oxide composite (NiSe) prepared in example 12/rGO-450). As can be seen from FIG. 1, the composite material NiSe2The cyclic voltammograms of/rGO-450 at different sweep rates all show a pair of redox peaks, demonstrating that the redox reaction occurs mainly. FIG. 2 is a nickel-based metal organic framework-derived nickel diselenide/reduced graphene oxide composite (NiSe) prepared in example 12/rGO-450). As can be seen from FIG. 2, the discharge time was about 250 seconds at the minimum current density of 1A/g and about 13 seconds at the maximum current density of 10A/g.
FIG. 3 is a nickel-based metal organic framework-derived nickel diselenide/reduced graphene oxide composite (NiSe) prepared in example 22/rGO-550). As can be seen from FIG. 3, the composite material NiSe2The cyclic voltammograms of/rGO-550 at different sweep rates all showed a pair of redox peaks, demonstrating that the redox reaction occurs primarily. FIG. 4 shows NiSe prepared in example 22Charge-discharge diagram of/rGO-550. As can be seen from FIG. 4, the discharge time was about 290 seconds at the minimum current density of 1A/g and about 23 seconds at the maximum current density of 10A/g. FIG. 5 is a nickel-based metal organic framework-derived nickel diselenide/reduced graphene oxide composite (NiSe) prepared in example 22/rGO-550) cycle performance plot. As can be seen from FIG. 5, NiSe2/rGO-550 at 5A g-1After 10000 cycles of circulation under the current density, the capacity retention rate is close to 76 percent.
FIG. 6 shows the nickel-based metals of examples 1-2NiSe in nickel diselenide/reduced graphene oxide composite material derived from machine frame2PerGO rate performance graph. As can be seen from FIG. 6, NiSe was observed at different current densities2The specific capacity of/rGO-550 is highest. Fig. 7 is an X-ray powder diffraction pattern of the nickel diselenide/reduced graphene oxide composite material derived from the nickel-based metal organic framework prepared in example 1-2, and it can be seen from the X-ray powder diffraction pattern that both samples exhibit high crystallization characteristics, similar peak patterns, and peak characteristics similar to those of the standard spectrum nickel diselenide (NiSe)2JCPDS No. 65-5016). Fig. 8 is an SEM photograph of the nickel-based metal organic framework-derived nickel diselenide/reduced graphene oxide composite prepared in example 1-2. Wherein, (a) NiSe2/rGO-450；(b) NiSe2/rGO-550. As can be seen from fig. 8, the nickel diselenide/reduced graphene oxide composite material derived from the nickel-based metal organic framework is prepared at 450-550 ℃, nickel diselenide particles are uniformly distributed on the surface of graphene, and the particle size is about 50 nm.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. A preparation method of nickel-based metal organic framework derived nickel diselenide/reduced graphene oxide composite material is characterized by comprising the following steps:
(1) dissolving nickel nitrate hexahydrate and hexa (4-carboxyphenoxy) cyclotriphosphazene in a first organic solvent, and uniformly mixing at room temperature to obtain a solution A;
ultrasonically dispersing graphene oxide in a second organic solvent to obtain a solution B;
(2) adding the solution B into the solution A, and stirring and refluxing at 160-170 ℃ to obtain a mixed solution C;
(3) and (3) centrifuging, washing and drying the mixed solution C to obtain a precursor, and calcining the precursor and selenium powder at 450-550 ℃ in a protective atmosphere to obtain the nickel diselenide/reduced graphene oxide composite material.
2. The method according to claim 1, wherein the weight ratio of nickel nitrate hexahydrate to hexa (4-carboxyphenoxy) cyclotriphosphazene in step (1) is 133: 146-133: 148; preferably, the weight ratio of nickel nitrate hexahydrate to hexa (4-carboxyphenoxy) cyclotriphosphazene in step (1) is 133: 146.
3. the method according to claim 1, wherein the first organic solvent in step (1) comprises at least one of N, N-dimethylformamide and dimethylsulfoxide, and the second organic solvent comprises at least one of N, N-dimethylformamide and dimethylsulfoxide.
4. The preparation method according to claim 1, wherein the weight ratio of the product obtained by reacting nickel nitrate hexahydrate and hexa (4-carboxyphenoxy) cyclotriphosphazene in the step (2) to graphene oxide is 100: 2.9-100: 3.1; preferably, the weight ratio of the product obtained by reacting nickel nitrate hexahydrate and hexa (4-carboxyphenoxy) cyclotriphosphazene in the step (2) to graphene oxide is 100: 3.
5. The preparation method according to claim 1, wherein the stirring reflux time in the step (2) is 2-2.5 h; preferably, the stirring reflux time in the step (2) is 2 h.
6. The preparation method according to claim 1, wherein the calcination time in the step (3) is 2-4 h, and the temperature rise rate of the calcination is 1-2 ℃/min.
7. The method according to claim 1, wherein the protective atmosphere in the step (3) is argon or nitrogen.
8. The preparation method according to claim 1, wherein the weight ratio of the precursor to the selenium powder in the step (3) is 1: 4-1: 5; preferably, the weight ratio of the precursor to the selenium powder in the step (3) is 1: 5.
9. a nickel-based metal organic framework-derived nickel diselenide/reduced graphene oxide composite material, which is characterized by being prepared by the preparation method of any one of claims 1 to 8.
10. Use of the nickel diselenide/reduced graphene oxide composite material of claim 9 in the field of supercapacitors or energy storage.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114471625A (en) * | 2021-11-30 | 2022-05-13 | 东北农业大学 | Preparation method and application of nickel selenide/tungsten trioxide/graphene photocatalytic composite material |
| CN114614032A (en) * | 2022-03-18 | 2022-06-10 | 江苏索普化工股份有限公司 | Anode composite nano catalyst material of methanol fuel cell and preparation method and application thereof |
| CN115058017A (en) * | 2022-06-28 | 2022-09-16 | 河北大学 | Preparation method of hexa (4-carboxyphenoxy) cyclotriphosphazene based zinc ion complex flame retardant and flame-retardant epoxy resin |
| CN115490211A (en) * | 2022-10-12 | 2022-12-20 | 武汉大学 | Method for preparing nitrogen-doped porous carbon nickel diselenide nanocomposite by nesting doll type microwave method |
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| CN112010360A (en) * | 2020-07-29 | 2020-12-01 | 北京理工大学 | Universal preparation method for synthesizing carbon-coated nickel metal compounds with various morphologies |
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| CN112010360A (en) * | 2020-07-29 | 2020-12-01 | 北京理工大学 | Universal preparation method for synthesizing carbon-coated nickel metal compounds with various morphologies |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114471625A (en) * | 2021-11-30 | 2022-05-13 | 东北农业大学 | Preparation method and application of nickel selenide/tungsten trioxide/graphene photocatalytic composite material |
| CN114471625B (en) * | 2021-11-30 | 2022-09-06 | 东北农业大学 | Preparation method and application of nickel selenide/tungsten trioxide/graphene photocatalytic composite material |
| CN114614032A (en) * | 2022-03-18 | 2022-06-10 | 江苏索普化工股份有限公司 | Anode composite nano catalyst material of methanol fuel cell and preparation method and application thereof |
| CN115058017A (en) * | 2022-06-28 | 2022-09-16 | 河北大学 | Preparation method of hexa (4-carboxyphenoxy) cyclotriphosphazene based zinc ion complex flame retardant and flame-retardant epoxy resin |
| CN115058017B (en) * | 2022-06-28 | 2024-02-06 | 河北大学 | Preparation method of hexa (4-carboxyphenoxy) cyclotriphosphazene zinc ion complex flame retardant and flame-retardant epoxy resin |
| CN115490211A (en) * | 2022-10-12 | 2022-12-20 | 武汉大学 | Method for preparing nitrogen-doped porous carbon nickel diselenide nanocomposite by nesting doll type microwave method |
| CN115490211B (en) * | 2022-10-12 | 2024-01-09 | 武汉大学 | Method for preparing nitrogen-doped porous carbon nickel diselenide nanocomposite by using nested doll type microwave method |
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