CN112408355B - Preparation method of tin simple substance/Prussian blue framework @ carbon composite material - Google Patents
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Abstract
The invention provides a preparation method of a tin simple substance/Prussian blue framework @ carbon composite material, which comprises the following steps: (1) Dissolving potassium hexacyanoferrate in deionized water, and performing ultrasonic treatment until red particles are completely dissolved; then adding polyvinylpyrrolidone, carrying out ultrasonic dissolution, placing the solution in a forced air oven for reaction, centrifuging, washing with water, and drying to obtain blue-black precursor powder; (2) Dissolving water-soluble tin salt in deionized water, then adding the blue-black precursor powder into the solution, stirring in a water bath, centrifuging, washing with water, and drying to obtain a blue reaction product; (3) Taking the blue reaction product, carrying out in-situ polymerization on the blue reaction product to obtain blue-gray powder, transferring the blue-gray powder into an argon-hydrogen mixed atmosphere for reduction reaction to obtain a black final reaction product, and collecting the black final reaction product to obtain the tin simple substance/Prussian blue framework @ carbon composite material. The invention also provides application of the material as a potassium ion battery negative electrode material.
Description
Technical Field
The invention belongs to the technical field of preparation of electrode materials of potassium ion batteries, and particularly relates to a preparation method and application of a tin simple substance/Prussian blue framework @ carbon composite material.
Background
Because the potassium (K) content in the earth crust is higher (the potassium content is 1.5 percent, and the lithium content is 0.0017 percent), the natural content richness K is obviously better than that of lithium, and K/K is superior to that of lithium in Lithium Ion Batteries (LIBs) + With Li/Li + Such that Potassium Ion Batteries (PIBs) are considered a low cost energy storage system. Although K will be + The graphite-embedded negative electrode contributes to the compactness of PIBsActually developed, but the capacity obtained by the method is usually less than 250mAh g -1 . Conversion alloy/reaction based anode materials tend to have higher theoretical specific capacities. The tin (Sn) simple substance is used as the alloy reaction type potassium ion battery cathode material and has the g of up to 560mAh -1 But due to K + Size ratio of (A) to (B) Li + Much larger, in practical PIBs, the problem of pulverization of Sn metal anodes based on alloying reactions is particularly severe. Therefore, a major challenge for stable elemental Sn-based cathodes in high performance PIBs is to repeatedly insert/extract K + During which inevitable volume expansion is cushioned and structural integrity is maintained. Among them, researchers have proposed that a rigid coating based on conductive carbon covering the surface of a conversion/alloy negative electrode can reduce the interface resistance and improve the overall electron conductivity. However, due to the insertion of a large number of K + Causing a large volume change, cracking and structural damage of the carbon layer, which in turn leads to a decrease in electrochemical performance. The approach of two-dimensional (2D) material confinement helps to improve electron conductivity and maintain electrode integrity, but does not prevent the pulverization of the confined transformation/alloy anode material. To achieve robustness and high structural stability of the volumetrically varied electrode material, combining conductive encapsulation with 2D material confinement may be an effective strategy.
The invention provides a preparation method of a tin simple substance/Prussian blue framework @ carbon composite material, which comprises the following main contents and innovation points: the invention utilizes Sn 4+ /Sn 2+ And a precursor Fe 3+ Ion exchange reaction of (2), with Sn 4+ /Sn 2+ Encapsulation into a precursor, subsequent carbon coating, and final reduction of Sn by gas phase 4+ /Sn 2+ The Sn simple substance in the composite material can provide considerable specific capacity, the carbon and the Prussian blue framework can provide a reliable barrier for inhibiting the volume effect for the Sn simple substance, in addition, the electronic conductivity of the whole material can be improved by the carbon tightly coated on the surface of the nano particles, and the obtained material has higher capacity, superior rate capability and cycle performance, and is particularly suitable for being used as potassium ion IIAnd (3) a negative electrode material of the secondary battery.
Disclosure of Invention
The invention aims to provide a preparation method of a tin simple substance/Prussian blue framework @ carbon composite material
In order to achieve the purpose, the invention adopts a three-step method to prepare a tin simple substance/Prussian blue framework @ carbon composite material, namely (S1) a nanoparticle precursor is prepared; (S2) preparation of Encapsulated Sn 4+ /Sn 4+ The precursor nanoparticles of (a); (S3) carrying out gas-phase reduction on the tin simple substance/Prussian blue framework @ carbon.
S1, dissolving potassium hexacyanoferrate in deionized water, and performing ultrasonic treatment until red particles are completely dissolved; adding polyvinylpyrrolidone, ultrasonic dissolving, placing the solution in a blast oven at 60-90 deg.C for reaction for 1-24 hr, centrifuging, washing with water (3-4 times), and drying in an oven at 60 deg.C for 12 hr to obtain blue-black precursor powder;
s2, dissolving water-soluble tin salt in deionized water to prepare a water-soluble tin salt solution, then adding the blue-black precursor powder into the solution, stirring in a water bath at 40-80 ℃ for 1-24 hours, centrifugally washing (3-4 times), and then placing in a 60 ℃ oven for drying for 12 hours to obtain a blue reaction product;
and S3, carrying out in-situ polymerization on the blue reaction product to obtain blue-gray powder, then transferring the blue-gray powder into a tubular furnace in an argon-hydrogen mixed atmosphere to carry out reduction reaction for 1-12 hours at the temperature of 400-800 ℃, wherein the heating rate is 2-5 ℃/min, and after cooling, collecting a black final reaction product, namely the tin simple substance/Prussian blue frame @ carbon composite material. The invention also provides application of the material as a potassium ion battery negative electrode material.
Preferably, the polyvinylpyrrolidone in step S1 has an average molecular weight of 8000 to 1300000.
Preferably, the mass ratio of the potassium hexacyanoferrate to the polyvinylpyrrolidone in step S1 is 1:1 to 1.
Preferably, the water-soluble tin salt in step S2 is one of tin tetrachloride or stannous chloride.
Preferably, the mass ratio of the water-soluble tin salt to the black precursor powder in step S2 is 1: 0.1-1:2.
Preferably, in the in-situ polymerization in step S3, the pyrrole monomer is used as a raw material, sodium Dodecyl Sulfate (SDS) is used as a dispersant, and ammonium persulfate is used as an initiator.
Drawings
Fig. 1 is an SEM image of elemental tin/prussian blue framework @ carbon composite electrode material prepared in example 1;
fig. 2 is an SEM image of elemental tin/prussian blue framework @ carbon composite prepared in example 1;
FIG. 3 shows that the current density of the elemental tin/Prussian blue framework @ carbon composite material prepared in example 1 is 0.5A g -1 A graph of cyclic performance of time;
FIG. 4 shows that the current density of the elemental tin/Prussian blue framework @ carbon composite material prepared in the example 2 is 0.05-2A g -1 Graph of rate performance.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the concept of the invention. All falling within the scope of the present invention.
Example 1
Dissolving 1mmol of potassium hexacyanoferrate in 100mL of deionized water, and performing ultrasonic treatment for 1 hour until red particles are completely dissolved; then adding 1g of polyvinylpyrrolidone with the molecular weight of 45000, performing ultrasonic treatment for 1 hour until the polyvinylpyrrolidone is completely dissolved, putting the solution into a blast oven with the temperature of 80 ℃ for reaction for 16 hours, centrifugally washing (3-4 times), and then putting the solution into an oven with the temperature of 60 ℃ for drying for 12 hours to obtain blue-black precursor powder; dissolving 2mmol of crystallized tin tetrachloride in 100ml of deionized water to prepare a tin tetrachloride solution, then adding 0.1g of the blue-black precursor powder into the solution, stirring in a water bath at 60 ℃ for 12 hours, centrifugally washing (3-4 times), and then placing in an oven at 60 ℃ for drying for 12 hours to obtain a blue reaction product; taking 0.1g of the blue reaction product, adding the blue reaction product into a beaker containing 50mg and 5mg of SDS of pyrrole monomer, adding 10 after ultrasonic dispersion is uniform0mg of ammonium persulfate initiates polymerization of pyrrole to obtain a Ppy-coated precursor to obtain blue gray powder, then 0.1g of the blue gray powder is transferred to a tubular furnace in an argon-hydrogen mixed atmosphere to perform reduction reaction at 500 ℃ for 8 hours, the heating rate is 5 ℃/min, and after cooling, a black final reaction product, namely the tin simple substance/Prussian blue frame @ carbon composite material, is obtained. Scanning electron micrographs of the precursor and the final material are shown in fig. 1 and fig. 2, which show the regular nano-sphere morphology, and the final product is tightly coated with carbon. FIG. 4 shows a current density of 0.5A g -1 The multiplying power performance graph shows that the specific capacity of the composite material at the current density is 0.5A g -1 The time capacity is as high as 130mAh g -1 And after 120 cycles, the product can still maintain 155mAh g -1 The method provided by the invention is proved to be capable of obviously improving the cycle performance of the Sn simple substance.
Example 2
Dissolving 2mmol of potassium hexacyanoferrate in 100mL of deionized water, and carrying out ultrasonic treatment for 1 hour until red particles are completely dissolved; then adding 1g of polyvinylpyrrolidone with molecular weight of 8000, carrying out ultrasonic treatment for 1 hour until the polyvinylpyrrolidone is completely dissolved, placing the solution in a 60 ℃ forced air oven for reaction for 24 hours, carrying out centrifugal water washing (3-4 times), and placing in a 60 ℃ oven for drying for 12 hours to obtain blue-black precursor powder; dissolving 1mmol of stannous chloride in 100mL of deionized water to prepare a stannous chloride solution, then adding 0.1g of the blue-black precursor powder into the solution, stirring in a water bath at 80 ℃ for 24 hours, centrifugally washing (3-4 times), and drying in an oven at 60 ℃ for 12 hours to obtain a blue reaction product; taking 0.1g of the blue reaction product, adding the blue reaction product into a beaker containing 50mg of pyrrole monomer and 5mg of SDS, adding 120mg of ammonium persulfate after uniform ultrasonic dispersion to initiate the polymerization of pyrrole to obtain a Ppy-coated precursor, obtaining blue gray powder, transferring 0.1g of the blue gray powder into a tubular furnace in argon-hydrogen mixed atmosphere to perform reduction reaction for 6 hours at 800 ℃, wherein the temperature rise speed is 2 ℃/min, and collecting a black final reaction product, namely tin simple substance/Prussian blue frame @ carbon composite material after cooling. The specific capacity of the composite material at current density is 2A g -1 The time capacity is as high as 95mAh g -1 The rate capability is good.
Example 3
Dissolving 1mmol of potassium hexacyanoferrate in 100mL of deionized water, and performing ultrasonic treatment for 1 hour until red particles are completely dissolved; then adding 1g of polyvinylpyrrolidone with molecular weight of 8000, carrying out ultrasonic treatment for 1 hour until the polyvinylpyrrolidone is completely dissolved, placing the solution in a blast oven with the temperature of 70 ℃ for reaction for 12 hours, carrying out centrifugal water washing (3-4 times), and then placing in an oven with the temperature of 60 ℃ for drying for 12 hours to obtain blue-black precursor powder; dissolving 2mmol of stannic chloride in 100ml of deionized water to prepare stannic chloride solution, then adding 0.1g of the blue-black precursor powder into the solution, stirring in a water bath at 50 ℃ for 12 hours, centrifugally washing (3-4 times), and then placing in an oven at 60 ℃ for drying for 12 hours to obtain a blue reaction product; and taking 0.1g of the blue reaction product, adding the blue reaction product into a beaker containing 50mg and 5mg of SDS (sodium dodecyl sulfate), adding 10mg of ammonium persulfate after uniformly dispersing by ultrasound to initiate polymerization of pyrrole to obtain a Ppy-coated precursor, obtaining blue gray powder, transferring 0.1g of the powder into a tubular furnace in argon-hydrogen mixed atmosphere to perform reduction reaction for 4 hours at 600 ℃, wherein the heating rate is 4 ℃/min, and collecting a black final reaction product, namely the tin simple substance/Prussian blue framework @ carbon composite material after cooling. It is in the range of 0.5A g -1 The time capacity is up to 320mAh g -1 The capacity retention after 300 cycles was 90.7%, which was found to be 2A g -1 The specific capacity of the material under large-multiplying power charge and discharge reaches 105mAh g -1 。
Claims (8)
1. A preparation method of a tin simple substance @ carbon composite material comprises the following steps:
s1, dissolving potassium hexacyanoferrate in deionized water, and performing ultrasonic treatment until red particles are completely dissolved; adding polyvinylpyrrolidone, ultrasonically dissolving, placing the obtained solution in a blast oven at 60-90 ℃ for reacting for 1-24 hours, centrifugally washing for 3-4 times, and placing in an oven at 60 ℃ for drying for 12 hours to obtain blue-black precursor powder;
s2, dissolving water-soluble tin salt in deionized water to prepare a water-soluble tin salt solution, then adding the blue-black precursor powder into the solution, stirring in a water bath at 40-80 ℃ for 1-24 hours, centrifugally washing for 3-4 times, and then placing in a 60 ℃ oven for drying for 12 hours to obtain a blue reaction product;
and S3, carrying out in-situ polymerization on the blue reaction product by Ppy to obtain blue gray powder, then transferring the blue powder into a tubular furnace in an argon-hydrogen mixed atmosphere to carry out reduction reaction for 1-12 hours at 400-800 ℃, wherein the heating rate is 2-5 ℃/min, and collecting the black final reaction product, namely the tin simple substance @ carbon composite material after cooling.
2. The method of claim 1, wherein in step S1, the polyvinylpyrrolidone has an average molecular weight of 8000 to 1300000.
3. The method according to claim 1, wherein the ratio of potassium hexacyanoferrate to polyvinylpyrrolidone in step S1 is 1: [ 1-20 ].
4. The method according to claim 1, wherein in step S2, the water-soluble tin salt is one of tin tetrachloride or tin chloride.
5. The method according to claim 1, wherein the mass ratio of the water-soluble tin salt to the bluish black precursor powder in step S2 is 1: [ 0.1-2 ].
6. The preparation method according to claim 1, wherein in step S3, the in-situ polymerization uses pyrrole monomers as raw materials, sodium dodecyl sulfate as a dispersant, and ammonium persulfate as an initiator.
7. The simple tin @ carbon composite material prepared by the preparation method of any one of claims 1 to 6 is characterized by being prepared from a simple tin and carbon composite material.
8. The elemental tin @ carbon composite material prepared by the preparation method of any one of claims 1 to 6 is used as a potassium ion battery negative electrode material.
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