CN111312999A - Preparation method of graphene-coated nickel-iron bimetallic sulfide sodium-ion battery negative electrode material - Google Patents
Preparation method of graphene-coated nickel-iron bimetallic sulfide sodium-ion battery negative electrode material Download PDFInfo
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- 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
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
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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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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
The invention relates to a preparation method of a sodium ion battery cathode material with selectively etched nickel-iron bimetallic sulfide coated by graphene. Firstly synthesizing a precursor of NiFe-PBA Prussian blue, then preparing PBA with multiple active sites by an ammonia etching method, performing hydrothermal vulcanization, and calcining in Ar atmosphere to obtain (NiFe)9S8The structure of @ GO, thereby improving the ion diffusion dynamics and the electronic conductivity. And pure (NiFe)9S8Comparison, use (NiFe)9S8The SIB with @ GO as the negative electrode has a significantly improved specific capacity, showing excellent cycling stability and rate performance. The invention overcomes the disadvantages ofIn the prior art, the volume of the sodium ion battery cathode material expands in the charging and discharging processes, so that the cycle performance of the battery is effectively improved, and meanwhile, the conductivity of the battery can be improved by the external carbon layer, so that the specific capacity and the stability of the battery are improved.
Description
Technical Field
The technical scheme of the invention relates to a preparation method of a sodium ion battery cathode material with selectively etched nickel-iron bimetallic sulfide coated by graphene, belonging to the field of material chemistry.
Background
With the continuous consumption of fossil resources and the aggravation of environmental pollution, renewable and pollution-free energy storage resources are urgently needed to be found. Lithium ion batteries have been successfully commercialized in portable mobile electronic devices due to their advantages of high safety, high energy density, long cycle life, and the like. Although lithium ion batteries have been widely used, the high cost due to the very limited storage of metallic lithium on the earth has further hindered the future development of lithium ion batteries. The storage capacity of metallic sodium on the earth is very large, and lithium ions and sodium ions have similar reaction mechanisms, so that the metallic sodium is in wide attention. Sodium ion batteries are considered to be the most promising alternative to lithium ion batteries as a new generation of energy storage devices. However, conventional graphite anode materials cannot be used directly in sodium ion batteries because the radius of sodium ions is much larger than that of lithium ions. It is very important to find a suitable sodium ion battery anode material. Among the numerous negative electrode materials, transition metal sulfides are considered as the most promising negative electrode material for high-performance sodium ion batteries because of their various structural types and excellent electrochemical activity. As shown in the study, NiS2And FeS2The sodium storage mechanism of (a) involves a conversion process, however, the performance in terms of cycle life and stability performance is poor because the battery undergoes a large volume change during charge and discharge.
Based on some existing theoretical foundations, the invention provides a simple and convenient method for synthesizing (NiFe)9S8@ GO negative electrode material to enhance the electrochemical properties of sodium ion batteries.
Disclosure of Invention
The invention aims to solve the problems and provides a preparation method of a sodium-ion battery cathode material for selectively etching nickel-iron bimetallic sulfide by coating graphene. The method comprises the steps of firstly synthesizing a NiFe-PBA nanocube as a precursor, etching 8 corners of the nanocube by using a selective etching method to obtain a hollow structure, dispersing the etched Prussian blue nanocube in a graphene aqueous solution, carrying out hydrothermal vulcanization on the graphene aqueous solution and thioacetamide, then carrying out carbonization and calcination in an Ar atmosphere to obtain a graphene coated ferronickel bimetallic sulfide, and applying the material to a sodium ion battery cathode.
Due to the existence of the graphene, amorphous carbon can be formed in the calcining process, the conductivity of the material can be enhanced, and meanwhile, due to the existence of the carbon layer, the volume expansion of the sodium-ion battery in the charging and discharging process can be effectively inhibited. The hollow ferronickel has more active sites, and the active sites of sodium ions are increased, so that the stability and the capacity of the battery are improved. Compared with a pure NiFeS sample, the structure designed by the invention can more effectively improve the cycle performance and the coulombic efficiency of the sodium-ion battery.
A preparation method of a sodium ion battery cathode material with selectively etched nickel-iron bimetallic sulfide coated by graphene. The method specifically comprises the following steps:
(1) preparation of NiFe-PBA nanocubes:
dissolving a proper amount of nickel nitrate hexahydrate and sodium citrate dihydrate into deionized water, dissolving a proper amount of potassium ferricyanide into the deionized water, mixing the two solutions together, and stirring under the condition of a water bath to obtain a yellow turbid solution. Standing the turbid solution for 24h, and then performing centrifugal separation to obtain a NiFe-PBA nanocube;
(2) preparation of NiFe-PBA @ etching nanocube
Dissolving the NiFe-PBA nanocube prepared in the step (1) in a mixed solution of deionized water and ethanol, performing ultrasonic treatment for 5min, stirring for 2-3h, performing centrifugal separation, collecting a sample, washing with methanol for three times, and drying in an oven at 60 ℃ to obtain the NiFe-PBA @ etching nanocube;
(3) preparation (NiFe)9S8@ GO negative electrode material
Dissolving the NiFe-PBA @ etching nanocube prepared in the step (2) in a graphene aqueous solution for ultrasonic treatment, adding thioacetamide, uniformly stirring, transferring the obtained solution into a reaction kettle for heating reaction, performing centrifugal separation after the reaction is finished, collecting a sample, and respectively using water and ethanolWashed three times and dried in an oven at 60 ℃. Placing the obtained sample into a tube furnace, calcining under Ar atmosphere, and cooling to room temperature to obtain (NiFe)9S8The @ GO negative electrode material is a sodium ion battery negative electrode material obtained by selectively etching nickel-iron bimetallic sulfide through graphene coating.
Further, in the step (1), the mass concentration of the nickel nitrate is 8.80g/L, the mass concentration of the sodium citrate dihydrate is 18.75g/L, and the mass concentration of the potassium ferricyanide is 4.90 g/L.
Further, in the step (1), the water bath stirring speed is 400r/min, the time is 60min, and the temperature is 85 ℃.
Further, in the step (2), the mass volume ratio of the NiFe-PBA material to the deionized water is 2g/L, and the volume ratio of the ethanol to the deionized water is 1: 5.
Further, in the step (3), the concentration of the graphene aqueous solution is 1mg/mL, the ultrasonic treatment time is 20min, and the thioacetamide is added and stirred for at least 10 min.
Further, in the step (3), the mass ratio of the NiFe-PBA @ ething nanocubes to thioacetamide is 1: 2, the reaction temperature is 180-190 ℃, and the reaction time is 12 h.
Further, in the step (3), the calcination temperature is 500 ℃ in the Ar atmosphere, the calcination time is 2 hours, and the temperature rise rate is 2 DEG/min.
Further, in the steps (1) to (3), the centrifugal speed is 10000r/min during centrifugal separation, and the time is 2 min.
Compared with the prior art, the invention has the following beneficial effects:
first, the synthesized structure can provide more electron transport channels for the battery, which is beneficial to the proceeding of electrochemical reaction. Secondly, in the process of charging and discharging, due to the existence of graphene, the volume expansion caused by the process of sodium ion sodium insertion and sodium removal is effectively inhibited. Thirdly, the ferronickel sulfide has higher specific capacity. The nano structure designed by the invention can provide extra buffer space and pressure, and is consistent with volume expansion brought by the charge and discharge process. Has important significance for the cycle performance of the sodium ion battery. Fourthly, the prepared sodium ion battery cathode material of the sulfide obviously improves the cycle performance of the sodium ion battery due to the combined action of multiple aspects, improves the capacity and the service life of the battery, and has positive significance for realizing the industrialization of the sodium ion battery.
Drawings
FIG. 1 is a scanning electron microscope image of the NiFe-PBA material in example 1.
FIG. 2 shows the composition of example 1 after vulcanization (NiFe)9S8Scanning electron micrograph of @ GO.
FIG. 4 shows the composition of example 1 after vulcanization (NiFe)9S8The XRD pattern of @ GO.
FIG. 3 is a ZnS @ CoS prepared in example 12@ C as negative electrode material of sodium ion battery and with current density of 1Ag-1Electrochemical cycling profile under discharging conditions.
The specific implementation mode is as follows:
the invention is further described with reference to the drawings and the detailed description.
Example 1:
(1) preparation of NiFe-PBA nanocubes:
1.76g of nickel nitrate hexahydrate and 3.75g of sodium citrate dihydrate were dissolved in 200mL of deionized water, 0.98g of potassium ferricyanide was dissolved in another 200mL of water, and the two solutions were mixed together and stirred in a water bath at 85 ℃ for 60min, to obtain a yellow cloudy solution. The solution was then allowed to stand for 24 h. After standing, centrifugally separating to prepare a NiFe-PBA nanocube; as can be seen from FIG. 1, the prepared structure is a cubic structure with uniform size and a diameter of about 200 nm.
(2) Preparation of NiFe-PBA @ etching nanocube
Dissolving 0.1g of the NiFe-PBA nanocube prepared in the step (1) in a mixed solution of 50mL of deionized water and 10mL of ethanol, carrying out ultrasonic treatment for 5min, stirring for 2h, carrying out centrifugal separation, collecting a sample, washing with methanol for three times, and drying in an oven at 60 ℃ to obtain NiFe-PBA @ etching;
(3) preparation of (N)iFe)9S8@ GO negative electrode material
Dissolving the NiFe-PBA @ etching sample prepared in the step (2) in 1mg/mL graphene aqueous solution, performing ultrasonic treatment for 20min, adding thioacetamide, stirring for 10min, transferring the obtained solution into a reaction kettle, reacting for 12h at 180 ℃, performing centrifugal separation after the reaction is finished, collecting the sample, washing with water and ethanol for three times respectively, and drying in an oven at 60 ℃. The obtained sample is placed in a tube furnace and calcined in Ar atmosphere, and (NiFe) is obtained after the reaction is finished9S8The @ GO negative electrode material is the sodium ion battery negative electrode material of the nickel-iron bimetal sulfide.
As can be seen from fig. 2, the etched cubes are tightly coated with graphene.
As can be seen in fig. 3, the peaks of the standard card and the sample are perfectly aligned, indicating successful synthesis.
As shown in fig. 4, the prepared material has high charge-discharge specific capacity and is stable. But pure (NiFe)9S8The capacity is relatively low and also less stable and the decay is relatively fast.
Example 2:
(1) preparation of NiFe-PBA nanocubes:
1.76g of nickel nitrate hexahydrate and 3.75g of sodium citrate dihydrate were dissolved in 200mL of deionized water, 0.98g of potassium ferricyanide was dissolved in another 200mL of water, and the above two solutions were mixed together and stirred in a water bath at 85 ℃ for 60min, to obtain a yellow cloudy solution. The solution was then allowed to stand for 24 h. After standing, centrifugally separating to prepare a NiFe-PBA nanocube;
(2) preparation of NiFe-PBA @ etching nanocube
Dissolving 0.1g of the NiFe-PBA nanocube prepared in the step (1) in a mixed solution of 50mL of deionized water and 10mL of ethanol, carrying out ultrasonic treatment for 5min, stirring for 2h, carrying out centrifugal separation, collecting a sample, washing with methanol for three times, and drying in an oven at 60 ℃ to obtain NiFe-PBA @ etching;
(3) preparation (NiFe)9S8@ GO negative electrode material
Dissolving the NiFe-PBA @ etching sample prepared in the step (2) in 1mg/mL graphene aqueous solution, performing ultrasonic treatment for 20min, adding thioacetamide, stirring for 10min, transferring the obtained solution into a reaction kettle, reacting for 12h at 190 ℃, performing centrifugal separation after the reaction is finished, collecting the sample, washing with water and ethanol for three times respectively, and drying in an oven at 60 ℃. The obtained sample is placed in a tube furnace and calcined in Ar atmosphere, and (NiFe) is obtained after the reaction is finished9S8The @ GO negative electrode material is the sodium ion battery negative electrode material of the nickel-iron bimetal sulfide.
Example 3:
(1) preparation of NiFe-PBA nanocubes:
1.76g of nickel nitrate hexahydrate and 3.75g of sodium citrate dihydrate were dissolved in 200mL of deionized water, 0.98g of potassium ferricyanide was dissolved in another 200mL of water, and the above two solutions were mixed together and stirred in a water bath at 85 ℃ for 60min to obtain a yellow turbid liquid. The solution was then allowed to stand for 24 h. After standing, centrifugally separating to prepare a NiFe-PBA nanocube;
(2) preparation of NiFe-PBA @ etching nanocube
Dissolving 0.1g of the NiFe-PBA nanocube prepared in the step (1) in a mixed solution of 50mL of deionized water and 10mL of ethanol, carrying out ultrasonic treatment for 5min, stirring for 3h, carrying out centrifugal separation, collecting a sample, washing with methanol for three times, and drying in an oven at 60 ℃ to obtain NiFe-PBA @ etching;
(3) preparation (NiFe)9S8@ GO negative electrode material
Dissolving the NiFe-PBA @ etching sample prepared in the step (2) in 1mg/mL graphene aqueous solution, performing ultrasonic treatment for 20min, adding thioacetamide, stirring for 10min, transferring the obtained solution into a reaction kettle, reacting for 12h at 180 ℃, performing centrifugal separation after the reaction is finished, collecting the sample, washing with water and ethanol for three times respectively, and drying in an oven at 60 ℃. The obtained sample is placed in a tube furnace and calcined in Ar atmosphere, and (NiFe) is obtained after the reaction is finished9S8The @ GO negative electrode material is the sodium ion battery negative electrode material of the nickel-iron bimetal sulfide.
The above-mentioned method for preparing the negative electrode material for sodium ion battery, wherein the raw materials are all purchased from the group consisting of Aladdin reagent Co., Ltd and Michelin reagent Co., Ltd, and the equipment and process used are well known to those skilled in the art.
The invention is not the best known technology.
Claims (8)
1. A preparation method of a sodium ion battery cathode material for selectively etching nickel-iron bimetallic sulfide by coating graphene comprises the following steps:
(1) preparation of NiFe-PBA nanocubes:
dissolving a proper amount of nickel nitrate hexahydrate and sodium citrate dihydrate into deionized water, dissolving a proper amount of potassium ferricyanide into the deionized water, mixing the two solutions together, stirring in a water bath to obtain a yellow turbid solution, standing the turbid solution for 24 hours, and performing centrifugal separation to obtain a NiFe-PBA nanocube;
(2) preparation of NiFe-PBA @ etching nanocubes:
putting the NiFe-PBA nanocubes prepared in the step (1) into a mixed solution of deionized water and ethanol, performing ultrasonic treatment for 5min, stirring for 2-3h, performing centrifugal separation, collecting samples, washing with methanol for three times, and drying in an oven at 60 ℃ to obtain the NiFe-PBA @ etching nanocubes;
(3) preparation (NiFe)9S8@ GO negative electrode materials:
dissolving the NiFe-PBA @ etching nanocube prepared in the step (2) in a graphene aqueous solution for ultrasonic treatment, adding thioacetamide, uniformly stirring, transferring the obtained mixed solution into a reaction kettle for heating reaction, performing centrifugal separation after the reaction is finished, collecting a sample, washing the sample with water and ethanol for three times respectively, drying the sample in an oven at the temperature of 60 ℃, putting the obtained sample into a tubular furnace, calcining the sample in the Ar atmosphere, and cooling the sample to the room temperature to obtain (NiFe)9S8The @ GO negative electrode material is the sodium ion battery negative electrode material of the nickel-iron bimetal sulfide.
2. The production method according to claim 1, wherein in the step (1), the mass concentration of nickel nitrate is 8.80g/L, the mass concentration of sodium citrate dihydrate is 18.75g/L, and the mass concentration of potassium ferricyanide is 4.90 g/L.
3. The method according to claim 1 or 2, wherein in the step (1), the stirring speed of the water bath is 400r/min, the time is 60min, and the temperature is 85 ℃.
4. The preparation method according to claim 1, wherein in the step (2), the mass-to-volume ratio of the NiFe-PBA material to the deionized water is 1g/L, and the volume ratio of the ethanol to the deionized water is 3: 10.
5. the preparation method according to claim 1, wherein in the step (3), the concentration of the graphene aqueous solution is 1mg/mL, the ultrasonic separation time is 20min, and the thioacetamide is added and then stirred for at least 10 min.
6. The preparation method according to claim 1, wherein in the step (3), the mass ratio of NiFe-PBA @ etching nanocubes to thioacetamide is 1: 2, the temperature of the heating reaction is 180-190 ℃, and the time is 12 h.
7. The production method according to claim 1 or 6, wherein in the step (3), the calcination temperature in the Ar atmosphere is 500 ℃, the calcination time is 2 hours, and the temperature increase rate is 2 °/min.
8. The method according to claim 1, wherein in the steps (1) to (3), the centrifugal speed is 10000r/min and the time is 2 min.
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| CN113422155A (en) * | 2021-05-25 | 2021-09-21 | 复旦大学 | Preparation method of multifunctional diaphragm coating for lithium-sulfur battery |
| CN114512666A (en) * | 2022-03-04 | 2022-05-17 | 哈尔滨工业大学 | Preparation method of sodium ion battery cathode material for in-situ growth of transition bimetallic chalcogenide on flexible carbon cloth substrate |
| CN114975926A (en) * | 2022-05-24 | 2022-08-30 | 东莞理工学院 | Double-active-site Prussian blue type sodium ion negative electrode material and preparation method thereof |
| CN115634698A (en) * | 2022-11-08 | 2023-01-24 | 江南大学 | Micro/nano graded flower-shaped direct Z-shaped heterojunction visible light catalyst and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113422155A (en) * | 2021-05-25 | 2021-09-21 | 复旦大学 | Preparation method of multifunctional diaphragm coating for lithium-sulfur battery |
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| CN114512666A (en) * | 2022-03-04 | 2022-05-17 | 哈尔滨工业大学 | Preparation method of sodium ion battery cathode material for in-situ growth of transition bimetallic chalcogenide on flexible carbon cloth substrate |
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| CN115634698A (en) * | 2022-11-08 | 2023-01-24 | 江南大学 | Micro/nano graded flower-shaped direct Z-shaped heterojunction visible light catalyst and preparation method thereof |
| CN115634698B (en) * | 2022-11-08 | 2024-03-01 | 江南大学 | Micro/nano hierarchical flower-like direct Z-shaped heterojunction visible light catalyst and preparation method thereof |
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Application publication date: 20200619 |
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