CN115028217A - Nickel disulfide crossed nanoflower material and preparation method and application thereof - Google Patents
Nickel disulfide crossed nanoflower material and preparation method and application thereof Download PDFInfo
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- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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Abstract
The invention belongs to the field of sodium ion battery electrode materials, and discloses a preparation method and application of a nickel disulfide crossed nanoflower material. The material is prepared by a simple one-step hydrothermal method. The nickel disulfide cross nanoflower material anchored on the graphene has a very large specific surface area. When the lithium ion battery negative electrode is applied to a sodium ion battery negative electrode, more sodium ions can be loaded, so that the battery capacity is improved. In addition, the unique flower-shaped structure of the nickel disulfide can improve the mobility of electrons and ions in the charging and discharging process, and after the graphene is wrapped, the ionic and electronic conductivity of the material is further improved, so that the cycle performance and the rate capability of the battery are improved; in addition, the material can prevent the appearance of polysulfide in the charge and discharge process, and the flower-like structure of the material can improve the mechanical property of the battery by adapting to volume shrinkage and expansion in the cycle process.
Description
Technical Field
The invention belongs to the technical field of novel energy materials, and particularly relates to a preparation method of a nickel disulfide crossed nanoflower material anchored on graphene and application of the nickel disulfide crossed nanoflower material in a sodium-ion battery.
Background
Due to the characteristics of abundant resources, low price, environmental friendliness and the like, Sodium Ion Batteries (SIBs) are currently considered to be the most promising substitutes for Lithium Ion Batteries (LIBs) and are applied to next-generation novel energy storage systems. However, the lack of suitable anode materials is one of the major obstacles limiting the large-scale use of SIBs. Among the anode materials currently being developed, metal disulfides (MS) 2 ) It is of great interest because of its high theoretical capacity and abundant natural resources. However, the problems of large volume change, low conductivity and slow diffusion kinetics of sodium ions limit their wide application. Strategies such as introducing conductive carbon, optimizing electrolyte, adjusting cut-off voltage, or designing nanocomposite structures are generally employed to improve their electrochemical performance.
Disclosure of Invention
In order to solve the defects of the prior art, the invention aims to provide a nickel disulfide crossed nanoflower material anchored on graphene, wherein the unique crossed flower-shaped structure of the material has a larger specific surface, so that the material has extremely high capacity, and the problems of large volume change, low conductivity, slow sodium ion diffusion kinetics and the like in the process of sodium intercalation/sodium deintercalation after the graphene is compounded are solved, so that the cycle performance and rate capability of the material in a sodium ion battery can be effectively enhanced;
another objective of the present invention is to provide a method for preparing the nickel disulfide crossed nanoflower material anchored on graphene, wherein the method is simple, low in cost, high in yield, and suitable for mass production;
the invention further aims to provide application of the nickel disulfide crossed nanoflower material anchored on the graphene.
The purpose of the invention is realized by the following technical steps:
a nickel disulfide cross nanoflower material is in a nickel disulfide cross nanoflower structure anchored on graphene.
Preferably, the raw materials synthesized by the nickel disulfide cross nanoflower structure anchored on the graphene comprise: nickel chloride hexahydrate, a vulcanizing agent L-cysteine and graphene in a mass ratio of 1:4: 1.
a preparation method of a nickel disulfide crossed nanoflower material comprises the following steps:
s1: 1mmol of nickel chloride hexahydrate (NiCl) was weighed 2 ·6H 2 O) is poured into 30ml of deionized water and stirred until the nickel chloride hexahydrate is completely dissolved;
s2: weighing 1mmol of urea, adding the urea into the deionized water in which the nickel chloride hexahydrate is dissolved in the S1, and stirring until the urea is completely dissolved;
s3: weighing 4mmol of L-cysteine, adding the L-cysteine into the solution obtained after the operation of S2, and stirring until the L-cysteine is completely dissolved;
s4: adding the solution processed in the step S3 into 50ml of graphene solution (2mg/ml), and then carrying out ultrasonic treatment for 1 h;
s5: adding the solution processed in the step S4 into a high-temperature high-pressure reaction kettle with a 100ml polytetrafluoroethylene lining, and reacting for 24 hours at 210 ℃;
s6: centrifuging the solution generated after the step of S5 in a centrifuge for a period of time, and washing with deionized water (30mL) and ethanol (30mL) for 6 times;
s7: drying the precipitate obtained in the step S6 in a vacuum oven at 60 ℃ for 24 hours to obtain a product of nickel disulfide crossed nano flower;
preferably, in the preparation method of the nickel disulfide crossed nanoflower material anchored on the graphene, the mass ratio of the weighed nickel chloride hexahydrate, the vulcanizing agent L-cysteine and the graphene is 1:4: 1; the step S1 is carried out for 2-3 min by magnetic stirring; the step S2 is carried out for 2-3 min by magnetic stirring; the step S3 is that the magnetic stirring time is 5-10 min; the hydrothermal reaction temperature is 200 ℃, and the reaction time is 24 hours; and the rotating speed and the time of the S6 centrifugal treatment are 4000-4500 r/min and 5-10 min respectively.
The nickel disulfide crossed nanoflower material can be applied to the field of sodium ion battery negative electrode materials of sodium ion batteries.
In summary, compared with the prior art, the invention has the beneficial effects that:
1. the nickel disulfide cross nanoflower anchored on the graphene has a simple structure, is convenient to use, and has extremely high capacity, cycle performance and rate capability when used for a sodium ion battery cathode; and the unique flower-like structure can prevent the occurrence of byproducts, and the graphene is anchored on graphene, so that the problems of large volume change, low conductivity, slow sodium ion diffusion kinetics and the like in the sodium intercalation/sodium deintercalation process can be solved to improve the electrochemical performance of the sodium ion battery.
2. The invention has simple manufacturing method, low cost and high yield and is suitable for batch production.
Drawings
Figure 1 is an SEM image of nickel disulfide crossed nanoflower material anchored on graphene.
Figure 2 is an SEM image of nickel disulfide crossed nanoflower material.
Figure 3 is a comparison of the cycling performance of an example of nickel disulfide crossed nanoflower material anchored to graphene with a comparative example.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the embodiments of the present invention are not limited thereto. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art. The practice, methods and apparatus of the present invention are those conventional in the art, except as otherwise indicated.
Example 1
Step 1, adding NiCl 2 ·6H 2 O、CH 4 N 2 O、HSCH 2 CH(NH 2 )CO 2 H is represented by 1: after mixing according to the stoichiometric ratio of 1:4, stirring for 5min by magnetic force to completely melt the mixture in 20ml of deionized water;
step 2, adding 50ml of graphene solution (2mg/ml) into the solution obtained in the step 1, and carrying out ultrasonic cleaning for 1 h;
step 3, pouring the solution obtained in the step 2 into a high-temperature high-pressure reaction kettle with a 100ml polytetrafluoroethylene lining, and reacting for 24 hours at 210 ℃;
step 4, when the solution reacted in the step 3 is cooled to room temperature, centrifuging for 5min at the speed of 4000 r/min;
step 5, washing the solution after centrifugation for 3 times by using 30ml of deionized water, and then washing for three times by using 30ml of ethanol solution;
step 6, putting the precipitate washed in the step 5 into a vacuum drying oven at 60 ℃ for drying for 24 hours to obtain a nickel disulfide crossed nano flower material;
and 7, mixing the nickel disulfide crossed nanoflower material obtained in the 6 processes, SP and PVDF according to the ratio of 75: 15: 10 and adding NMP for mixing, coating the obtained electrode slurry on a copper foil with the thickness of 100 microns, and carrying out vacuum drying at 60 ℃ for a whole night; taking out and cutting into negative pole pieces with the diameter of 1 mm;
step 8, mounting the negative pole piece prepared in the step 7 into a button battery in a vacuum glove box, and carrying out an electrochemical performance test on an electrochemical workstation after the negative pole piece is placed aside for 12 hours;
and 9, performing other steps without changing the nickel disulfide cross nanoflower, wherein SP is that PVDF is 75: x: y, X + Y25; carrying out repeated experiments according to the steps in sequence, wherein X is 5, 10 and 20; 3 sets of experiments were repeated and are designated as examples 2-4.
Fig. 1 is an SEM image of a nickel disulfide crossed nanoflower material anchored on graphene, from which it is evident that nickel disulfide of the interdigitated nanoflower-like structure grows on graphene; the lithium ion battery has an extremely large specific surface area, can contain a large amount of sodium ions, and further optimizes the electrochemical performance of the battery.
Comparative example 1
Step 1, adding NiCl 2 ·6H 2 O、CH 4 N 2 O、HSCH 2 CH(NH 2 )CO 2 H is represented by 1: after mixing according to the stoichiometric ratio of 1:4, stirring for 5min by magnetic force to completely melt the mixture in 20ml of deionized water;
step 2, adding 50ml of deionized water into the solution obtained in the step 1, and ultrasonically cleaning for 1 h;
step 3, pouring the solution obtained in the step 2 into a high-temperature high-pressure reaction kettle with a 100ml polytetrafluoroethylene lining, and reacting for 24 hours at 210 ℃;
step 4, when the solution reacted in the step 3 is cooled to room temperature, centrifuging for 5min at the speed of 4000 r/min;
step 5, washing the solution after centrifugation for 3 times by using 30ml of deionized water, and then washing for three times by using 30ml of ethanol solution;
step 6, putting the precipitate washed in the step 5 into a vacuum drying oven at 60 ℃ for drying for 24 hours to obtain a nickel disulfide crossed nano flower material;
and 7, mixing the nickel disulfide crossed nanoflower material obtained in the 6 processes, SP and PVDF according to the ratio of 75: 15: 10 and adding NMP for mixing, coating the obtained electrode slurry on a copper foil with the thickness of 100 microns, and carrying out vacuum drying at 60 ℃ for a whole night; taking out and cutting into negative pole pieces with the diameter of 1 mm;
and 8, mounting the negative pole piece prepared in the step 7 into a button battery in a vacuum glove box, and carrying out an electrochemical performance test on an electrochemical workstation after the negative pole piece is placed aside for 12 hours.
Fig. 2 is an SEM image of a nickel disulfide crossed nanoflower material, from which it is apparent that nickel disulfide is in a cross nanoflower-like structure.
Figure 3 is a comparison of the cycling performance of an example of nickel disulfide crossed nanoflower material anchored to graphene with a comparative example. It can be clearly seen from the figure that the nickel disulfide cross nanoflower material anchored on graphene has higher sample cycling stability than the nickel disulfide cross nanoflower material, demonstrating the feasibility of example 1;
the above examples are illustrative of the preferred embodiments of the present invention, but the present invention is not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and they are included in the scope of the present invention.
Claims (7)
1. A nickel disulfide cross nanoflower material is characterized in that the material is in a nickel disulfide cross nanoflower structure anchored on graphene.
2. The nickel disulfide cross nanoflower material of claim 1, wherein the raw materials synthesized by the nickel disulfide cross nanoflower structure anchored on graphene comprise: nickel chloride hexahydrate, a vulcanizing agent L-cysteine and graphene in a mass ratio of 1:4: 1.
3. a method of making the nickel disulfide interdigitated nanoflower material of claim 1, comprising the steps of:
s1, weighing nickel chloride hexahydrate, urea and L-cysteine powder, respectively adding the nickel chloride hexahydrate, the urea and the L-cysteine powder into deionized water, magnetically stirring the mixture uniformly, then adding the mixture into a graphene solution, and carrying out ultrasonic cleaning treatment to obtain a solution A;
s2: adding the solution A obtained in the step S1 into a high-temperature high-pressure reaction kettle with a polytetrafluoroethylene lining for hydrothermal reaction to obtain a mixed solution A;
s3: the mixed solution a obtained after the treatment of S2 was centrifuged and then filtered.
4. The method for preparing nickel disulfide crossed nanoflower material according to claim 3, wherein magnetic stirring time of nickel chloride hexahydrate and urea in step S1 is 2-3 min, and magnetic stirring time of L-cysteine powder is 5-10 min.
5. The method for preparing nickel disulfide crossed nanoflower material according to claim 3, wherein the temperature of the hydrothermal reaction in the step S2 is 200 ℃, and the reaction time is 24 h.
6. The method for preparing the nickel disulfide crossed nanoflower material according to claim 3, wherein the rotation speed and the time of the centrifugal treatment in the step S3 are 4000r/min and 5-10 min respectively.
7. The application of the nickel disulfide cross nanoflower material as claimed in claim 1, wherein the nickel disulfide cross nanoflower material can be applied to the field of negative electrode materials of sodium-ion batteries.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20160119912A (en) * | 2015-04-06 | 2016-10-17 | 울산과학기술원 | Preparing method of graphene oxide dopeded with cobalt disulfide |
| CN106207127A (en) * | 2016-08-30 | 2016-12-07 | 安徽师范大学 | The preparation method of a kind of nickel sulfide/graphene nanocomposite material, lithium ion battery negative, lithium ion battery |
| CN110911684A (en) * | 2019-11-22 | 2020-03-24 | 广东工业大学 | Antimony-doped cobalt disulfide-loaded graphene and preparation method and application thereof |
| CN113346064A (en) * | 2021-06-02 | 2021-09-03 | 齐鲁工业大学 | Sulfur-doped graphene-coated bimetallic sulfide composite material, preparation method and application thereof in sodium-ion battery |
| CN114497541A (en) * | 2022-01-27 | 2022-05-13 | 广东工业大学 | Preparation and application of hollow nickel disulfide ball |
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- 2022-05-27 CN CN202210587971.5A patent/CN115028217A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20160119912A (en) * | 2015-04-06 | 2016-10-17 | 울산과학기술원 | Preparing method of graphene oxide dopeded with cobalt disulfide |
| CN106207127A (en) * | 2016-08-30 | 2016-12-07 | 安徽师范大学 | The preparation method of a kind of nickel sulfide/graphene nanocomposite material, lithium ion battery negative, lithium ion battery |
| CN110911684A (en) * | 2019-11-22 | 2020-03-24 | 广东工业大学 | Antimony-doped cobalt disulfide-loaded graphene and preparation method and application thereof |
| CN113346064A (en) * | 2021-06-02 | 2021-09-03 | 齐鲁工业大学 | Sulfur-doped graphene-coated bimetallic sulfide composite material, preparation method and application thereof in sodium-ion battery |
| CN114497541A (en) * | 2022-01-27 | 2022-05-13 | 广东工业大学 | Preparation and application of hollow nickel disulfide ball |
Non-Patent Citations (1)
| Title |
|---|
| QIANNAN CHEN等: "L-Cysteine-assisted hydrothermal synthesis of nickel disulfide/graphene composite with enhanced electrochemical performance for reversible lithium storage", JOURNAL OF POWER SOURCES, vol. 294, pages 51 - 58 * |
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