CN111900385A - Novel negative electrode material of potassium ion battery and preparation method thereof - Google Patents
Novel negative electrode material of potassium ion battery and preparation method thereof Download PDFInfo
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- 229910001414 potassium ion Inorganic materials 0.000 title claims abstract description 44
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 239000007773 negative electrode material Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 150000001875 compounds Chemical class 0.000 claims abstract description 33
- 239000002243 precursor Substances 0.000 claims abstract description 16
- 239000002073 nanorod Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002135 nanosheet Substances 0.000 claims abstract description 3
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 3
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 3
- 238000004073 vulcanization Methods 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 20
- 229910002555 FeNi Inorganic materials 0.000 claims description 18
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 17
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 13
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 12
- 239000004202 carbamide Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000013302 MIL-88A Substances 0.000 claims description 10
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 8
- 239000001530 fumaric acid Substances 0.000 claims description 8
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 7
- 238000003763 carbonization Methods 0.000 claims description 7
- 239000012300 argon atmosphere Substances 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 5
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 5
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 2
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 2
- 238000000643 oven drying Methods 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052799 carbon Inorganic materials 0.000 abstract description 5
- 238000007599 discharging Methods 0.000 abstract description 5
- 239000010406 cathode material Substances 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 3
- 239000007795 chemical reaction product Substances 0.000 description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 4
- 238000004146 energy storage Methods 0.000 description 4
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- 229910052700 potassium Inorganic materials 0.000 description 4
- 239000011591 potassium Substances 0.000 description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000001351 cycling effect Effects 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 229910052960 marcasite Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052683 pyrite Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000012621 metal-organic framework Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- -1 transition metal sulfides Chemical class 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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Abstract
The invention belongs to the technical field of potassium ion batteries, and particularly relates to a novel negative electrode material of a potassium ion battery and a preparation method thereof. The novel cathode material of the potassium ion battery is a NiFeS compound. Firstly, synthesizing Fe-MIL88A nano-rods as precursors; then growing a layer of nickel nanosheet on the surface of the precursor Fe-MIL88A nanorod by a hydrothermal method; and finally, carrying out high-temperature vulcanization to obtain the NiFeS compound. The novel negative electrode material overcomes the defect of volume expansion of the conventional negative electrode material of the potassium ion battery in the charging and discharging processes, and effectively improves the cycle performance of the battery; meanwhile, the coated carbon layer can also increase the conductivity of the battery, and improve the specific capacity and stability of the battery.
Description
Technical Field
The invention belongs to the technical field of potassium ion batteries, and particularly relates to a novel negative electrode material of a potassium ion battery and a preparation method thereof.
Background
In recent years, lithium ion batteries are widely applied to portable energy storage devices, electric vehicles and power grids, however, the further development of the lithium ion batteries is limited due to the high price of lithium sources, researchers begin to research and explore energy storage systems for replacing the lithium ion batteries, potassium ions in the energy storage systems have the same electrochemical working principle as the lithium ion batteries, and the energy storage systems are low in price and environmentally friendly, so that the attention is drawn; in addition, potassium has a standard hydrogen potential (-2.93V) similar to that of lithium (-3.04V), which means that potassium has a high operating voltage and a high energy density. However, the severe volume expansion can occur in the charging and discharging process, which leads to the rapid specific capacity attenuation and poor rate capability, and hinders the further development and application of the potassium ion battery. Therefore, a suitable potassium ion battery cathode material is found, and the improvement of the performance of the potassium ion battery is very urgent.
In the process of exploring a negative electrode material, transition metal sulfides are considered as a negative electrode material of a high-performance potassium ion battery due to various structural types and excellent electrochemical activity. As shown in the study, NiS2And FeS2The potassium storage mechanism of (a) involves a conversion process, but is inferior in cycle life and stability performance because the battery undergoes a large volume change during charge and discharge. Therefore, a new negative electrode material for potassium ion batteries is needed to overcome the above-mentioned drawbacks.
Disclosure of Invention
The invention aims to provide a novel negative electrode material of a potassium ion battery and a preparation method thereof aiming at the defects, the novel negative electrode material overcomes the defect of volume expansion of the negative electrode material of the existing potassium ion battery in the charging and discharging processes, and the cycle performance of the battery is effectively improved; meanwhile, the coated carbon layer can also increase the conductivity of the battery, and improve the specific capacity and stability of the battery.
The technical scheme of the invention is as follows: a novel cathode material of a potassium ion battery is a NiFeS compound.
The NiFeS compound is of a hollow nanorod structure, and a sheet structure is formed on the surface of the nanorod.
Firstly, synthesizing a Fe-MIL88A nano rod as a precursor; then growing a layer of nickel nanosheet on the surface of the precursor Fe-MIL88A nanorod by a hydrothermal method; and finally, carrying out high-temperature vulcanization to obtain the NiFeS compound.
The preparation method of the novel negative electrode material of the potassium ion battery comprises the following steps:
(1) preparing an iron-based metal framework precursor Fe-MIL-88A: firstly, measuring DMF, and then adding Fe (NO) into the DMF3)3∙9H2Stirring the O and the fumaric acid, and carrying out oil bath reaction after uniformly stirring; after the reaction is finished, washing and drying for later use;
(2) preparation of FeNi @ LDH: firstly, dispersing a precursor Fe-MIL-88A prepared in the step (1) and nickel nitrate in water by an ultrasonic dispersion method; then adding urea and ammonium fluoride, stirring until the urea and the ammonium fluoride are completely dissolved, and carrying out hydrothermal reaction after uniformly stirring; after the reaction is finished, washing and drying to obtain FeNi @ LDH;
(3) preparation of NiFeS compound: and (3) placing the FeNi @ LDH compound obtained in the step (2) and sulfur powder in a tube furnace under an argon atmosphere for high-temperature carbonization to obtain a NiFeS compound.
In the step (1), DMF is 8mL, and Fe (NO)3)3∙9H20.16g of O and 0.042g of fumaric acid; in the step (2), 0.1-0.2 g of cobalt nitrate, 100mL of water, 0.3g of urea and 0.05-0.1 g of ammonium fluoride are added; and (3) 0.2g of sulfur powder.
Stirring for 30min in the step (1); performing oil bath reaction for 1-2 h at 110 ℃; washing the mixture for 3 times by adopting DMF and methanol respectively, and drying the mixture at the temperature of 60-70 ℃.
Carrying out hydrothermal reaction at 110 ℃ for 5-10 h in the step (2); washing with water and ethanol for three times, and oven drying at 70 deg.C.
And (3) calcining the high-temperature carbonization in the step (3) at 400-500 ℃ for 2 h.
The invention has the beneficial effects that: the metal organic framework in the preparation raw materials of the novel cathode material of the potassium ion battery contains carbon, and amorphous carbon is formed in the calcining process, so that the conductivity of the material can be enhanced; meanwhile, due to the existence of the carbon layer, the volume expansion of the potassium ion battery in the charging and discharging process can be effectively inhibited. Hollow nano-rod has moreThe active sites are increased, so that the sites of potassium ions are increased, and the stability and the capacity of the battery are improved. Relative to FeS2In particular, the potassium ion battery using the NiFeS compound as the negative electrode material has significantly improved specific capacity, and the designed structure can improve the diffusion kinetics of potassium ions, improve the electron conductivity, and show excellent cycling stability and coulombic efficiency. Has the following advantages:
(1) the novel negative electrode material is reasonably designed through the preparation method, a hollow nanorod structure is synthesized, a sheet structure is formed on the surface of a nanorod, the sheet structure can provide more active sites for the potassium ion battery, the obtained hollow structure can also provide more active sites, and the potassium ion battery can have high specific capacity. The formed structure can provide more electronic channels for the battery, and is beneficial to the electrochemical reaction of the battery.
(2) In the charging and discharging process of the battery, due to the existence of the outer carbon layer, the volume expansion caused by the potassium ion potassium intercalation and potassium ion removal processes is effectively inhibited, the conductivity of the potassium ion battery can be increased, and the specific capacity and the stability of the potassium ion battery are improved. The reasonably designed nano structure can provide extra buffer space and pressure, and has important significance for the cycle performance of the potassium ion battery.
The preparation method of the invention is simple, convenient and effective to synthesize the NiFeS compound, and enhances the cycle performance and the stability of the potassium ion battery.
Drawings
FIG. 1 is a scanning electron micrograph of FeNi @ LDH from example 1.
FIG. 2 is a scanning electron microscope image of NiFeS in example 1.
FIG. 3 shows that NiFeS prepared in example 1 and example 2 respectively is used as a negative electrode material for a potassium ion battery, and the current density is 1A ∙ g-1Electrochemical cycling profile under discharge conditions.
Detailed Description
The present invention will be described in detail below with reference to examples. The raw materials involved are all available from Aladdin reagents, Inc. and Michelin reagents, Inc.
Example 1
The novel negative electrode material of the potassium ion battery is a NiFeS compound. The NiFeS compound is of a hollow nanorod structure, and a sheet structure is formed on the surface of the nanorod.
The preparation method of the novel negative electrode material of the potassium ion battery comprises the following steps:
(1) preparing an iron-based metal framework precursor Fe-MIL-88A: first, 8ml of DMF was taken and placed in a round bottom flask, and then 0.16g of Fe (NO) was added to DMF3)3∙9H2Stirring O and 0.042g of fumaric acid for 30min, uniformly stirring, and transferring to a 110 ℃ oil bath kettle for reaction for 1 h; after the reaction is finished, washing the mixture for 3 times by adopting DMF and methanol respectively, and drying the mixture in a drying oven at the temperature of 70 ℃ for later use;
(2) preparation of FeNi @ LDH compounds: firstly, dispersing a precursor Fe-MIL-88A prepared in the step (1) and 0.1g of nickel nitrate into 100mL of water by an ultrasonic dispersion method; then adding 0.3g of urea and 0.05g of ammonium fluoride, stirring until the urea and the ammonium fluoride are completely dissolved, uniformly stirring, and transferring the mixture to a 110 ℃ oven for reaction for 6 hours; after the reaction is finished, respectively washing the reaction product by using water and ethanol for three times, and drying the reaction product in an oven at the temperature of 70 ℃ to obtain a FeNi @ LDH compound;
(3) preparation of NiFeS compound: and (3) putting the FeNi @ LDH compound obtained in the step (2) and 0.2g of sulfur powder into a tubular furnace in an argon atmosphere for high-temperature carbonization at the calcining temperature of 400 ℃ for 2 hours to obtain the NiFeS compound.
As can be seen from figure 1, a layer of sheet structure grows on the surface of the prepared FeNi @ LDH, and the size is uniform.
As can be seen in fig. 2, the surface sheet thickness of the NiFeS compound increases due to the reaction of sublimed sulfur and FeNi @ LDH to form sulfide.
Example 2
The preparation method of the novel negative electrode material of the potassium ion battery comprises the following steps:
(1) preparing an iron-based metal framework precursor Fe-MIL-88A: first, 8ml of DMF was taken and placed in a round bottom flask, and then 0.16g of Fe (NO) was added to DMF3)3∙9H2O and 0.042g of fumaric acid is stirred for 30min, and the fumaric acid is transferred to an oil bath kettle at 110 ℃ after being uniformly stirred to react for 1 h; after the reaction is finished, washing the mixture for 3 times by adopting DMF and methanol respectively, and drying the mixture in a drying oven at the temperature of 70 ℃ for later use;
(2) preparation of FeNi @ LDH compounds: firstly, dispersing a precursor Fe-MIL-88A prepared in the step (1) and 0.1g of nickel nitrate into 100mL of water by an ultrasonic dispersion method; then adding 0.3g of urea and 0.05g of ammonium fluoride, stirring until the urea and the ammonium fluoride are completely dissolved, uniformly stirring, and transferring the mixture to a 110 ℃ oven for reaction for 10 hours; after the reaction is finished, respectively washing the reaction product by using water and ethanol for three times, and drying the reaction product in an oven at the temperature of 70 ℃ to obtain a FeNi @ LDH compound;
(3) preparation of NiFeS compound: and (3) putting the FeNi @ LDH compound obtained in the step (2) and 0.2g of sulfur powder into a tubular furnace in an argon atmosphere for high-temperature carbonization at the calcination temperature of 450 ℃ for 2 hours to obtain the NiFeS compound.
It can be seen from fig. 3 that the specific capacity can be maintained at about 500mAh/g after 500 cycles, while the capacity is somewhat attenuated after the temperature is increased to 450 ℃, which is not as stable as 400 ℃, and the specific capacity is possibly reduced due to the structural damage of the material caused by high temperature.
Example 3
The preparation method of the novel negative electrode material of the potassium ion battery comprises the following steps:
(1) preparing an iron-based metal framework precursor Fe-MIL-88A: first, 8ml of DMF was taken and placed in a round bottom flask, and then 0.16g of Fe (NO) was added to DMF3)3∙9H2Stirring O and 0.042g of fumaric acid for 30min, uniformly stirring, and transferring to a 110 ℃ oil bath kettle for reaction for 1 h; after the reaction is finished, washing the mixture for 3 times by adopting DMF and methanol respectively, and drying the mixture in a drying oven at the temperature of 70 ℃ for later use;
(2) preparation of FeNi @ LDH compounds: firstly, dispersing a precursor Fe-MIL-88A prepared in the step (1) and 0.2g of nickel nitrate into 100mL of water by an ultrasonic dispersion method; then adding 0.3g of urea and 0.1g of ammonium fluoride, stirring until the urea and the ammonium fluoride are completely dissolved, uniformly stirring, and transferring the mixture to a 110 ℃ oven for reaction for 5 hours; after the reaction is finished, respectively washing the reaction product by using water and ethanol for three times, and drying the reaction product in an oven at the temperature of 70 ℃ to obtain a FeNi @ LDH compound;
(3) preparation of NiFeS compound: and (3) putting the FeNi @ LDH compound obtained in the step (2) and 0.2g of sulfur powder into a tubular furnace in an argon atmosphere for high-temperature carbonization at the calcining temperature of 500 ℃ for 2 hours to obtain the NiFeS compound.
The invention is not the best known technology.
Claims (8)
1. A novel negative electrode material of a potassium ion battery is characterized in that the negative electrode material is a NiFeS compound.
2. The novel negative electrode material of the potassium ion battery as claimed in claim 1, wherein the NiFeS compound is a hollow nanorod structure, and a sheet structure is formed on the surface of the nanorod.
3. A preparation method of the novel negative electrode material of the potassium ion battery in claim 1 is characterized by firstly synthesizing Fe-MIL88A nano-rods as precursors; then growing a layer of nickel nanosheet on the surface of the precursor Fe-MIL88A nanorod by a hydrothermal method; and finally, carrying out high-temperature vulcanization to obtain the NiFeS compound.
4. The preparation method of the novel negative electrode material of the potassium ion battery as claimed in claim 3, characterized by comprising the following steps:
(1) preparing an iron-based metal framework precursor Fe-MIL-88A: firstly, measuring DMF, and then adding Fe (NO) into the DMF3)3∙9H2Stirring the O and the fumaric acid, and carrying out oil bath reaction after uniformly stirring; after the reaction is finished, washing and drying for later use;
(2) preparation of FeNi @ LDH: firstly, dispersing a precursor Fe-MIL-88A prepared in the step (1) and nickel nitrate in water by an ultrasonic dispersion method; then adding urea and ammonium fluoride, stirring until the urea and the ammonium fluoride are completely dissolved, and carrying out hydrothermal reaction after uniformly stirring; after the reaction is finished, washing and drying to obtain FeNi @ LDH;
(3) preparation of NiFeS compound: and (3) placing the FeNi @ LDH obtained in the step (2) and sulfur powder in a tube furnace in an argon atmosphere for high-temperature carbonization to obtain the NiFeS compound.
5. The preparation method of the novel negative electrode material of the potassium ion battery as claimed in claim 4, wherein the DMF in the step (1) is 8mL, and Fe (NO) is adopted3)3∙9H20.16g of O and 0.042g of fumaric acid; in the step (2), 0.1-0.2 g of cobalt nitrate, 100mL of water, 0.3g of urea and 0.05-0.1 g of ammonium fluoride are added; and (3) 0.2g of sulfur powder.
6. The preparation method of the novel negative electrode material of the potassium ion battery as claimed in claim 4, wherein the stirring in the step (1) is carried out for 30 min; performing oil bath reaction for 1-2 h at 110 ℃; washing the mixture for 3 times by adopting DMF and methanol respectively, and drying the mixture at the temperature of 60-70 ℃.
7. The preparation method of the novel negative electrode material of the potassium ion battery as claimed in claim 4, wherein in the step (2), the hydrothermal reaction is carried out for 5-10 h at 110 ℃; washing with water and ethanol for three times, and oven drying at 70 deg.C.
8. The preparation method of the novel negative electrode material of the potassium ion battery as claimed in claim 4, wherein the calcination temperature of the high-temperature carbonization in the step (3) is 400-500 ℃ and the calcination time is 2 hours.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20170125794A1 (en) * | 2014-04-21 | 2017-05-04 | Xiamen University | A sulfur-based transition metal composite and the negative electrode comprising the same and the battery comprising the same |
| CN109860593A (en) * | 2019-01-29 | 2019-06-07 | 陕西科技大学 | A kind of iron-nickel sulfide and preparation method thereof and sodium-ion battery using the same as negative electrode |
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