CN114784284A - Zinc anode modified by silk fibroin coating, preparation method and application thereof - Google Patents
Zinc anode modified by silk fibroin coating, preparation method and application thereof Download PDFInfo
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Abstract
A zinc anode modified by a silk fibroin coating, a preparation method and an application thereof belong to the technical field of energy materials. The invention firstly prepares zinc anode (Zn-SF) coated by silk fibroin, and then prepares ZnxV2O5·nH2O cathode material, cathode assembled in CR2025 button cell, Zn-SF as anode, glass fiber diaphragm and 2M ZnSO4As a separator and an electrolyte, assembling to obtain (Zn-SF) -ZnxV2O5·nH2And O, fully charging the battery. SF coating modified zinc anodes provide high ratesPerformance and longer cycle stability, with ZnxV2O5·nH2The full cell combined by the O cathode provides a method for constructing a zinc anode on an interface, is used for a high-rate water system zinc ion cell, and improves the electrochemical performance and the cycle life of the cell.
Description
Technical Field
The invention belongs to the technical field of energy materials, and particularly relates to a zinc anode modified by a silk fibroin coating, a preparation method and application thereof.
Background
The water system zinc ion battery has huge potential in a large-scale energy storage system due to the advantages of high theoretical capacity, low oxidation-reduction potential and natural abundance. However, as an important part of the battery, zinc anodes always suffer from serious problems such as dendrite growth, hydrogen evolution reaction and the formation of by-products, which greatly reduce their cycle life and raise safety concerns. Therefore, in order to obtain stable zinc anodes, researchers have proposed a number of methods including anode structural adjustment (three-dimensional current collector or alloy), electrolyte optimization (additives/high concentration salts) and surface protective coatings. The anode structure adjustment strategy enlarges the specific surface area, greatly reduces the local current density, and the introduction of the zinc-philic sites hopefully reduces the nucleation potential barrier, induces the uniform deposition of zinc ions and has high coulombic efficiency. The electrolyte optimization strategy adjusts the solvation structure of zinc ions, reduces the activity of water and promotes the uniform distribution of the zinc ions. As an alternative strategy, the establishment of a surface protection layer on the surface of the zinc anode has the common advantage of simplicity and high practical value. The compact solid barrier on the zinc anode can separate water/protons from the aqueous electrolyte, optimize the flux of zinc ions, and promote desolvation of zinc, thereby eliminating dendrites and inhibiting side reactions. Inorganic coatings with nanostructured morphology have been extensively studied, however, brittleness and weak adhesion may cause the protective layer to crack after repeated deposition/peeling cycles. In contrast, the polymer coating provides strong adhesion and flexibility to accommodate changes in anode volume over long-term cycling. In addition, the abundant polar groups on the surface provide nucleation sites, which are beneficial to zinc hexahydrateDesolvation of the ions adjusts the uniform distribution of zinc ions on a molecular scale. However, since the organic coating is more strongly chemisorbed to zinc ions than water molecules, the interfacial resistance is increased, resulting in severe polarization phenomena at high current densities. High polarization voltage causes instability of the anode interface and aggravation of side reactions, resulting in rapid capacity fade at high rates. Therefore, reducing the polarization voltage of the zinc anode is key to stabilizing the anode interface and improving the rate capability, and can be achieved by accelerating the deposition/stripping process of zinc ions. Negative charge can be induced by establishing ohmic contact (Zn-CeO)2) Or introduced to the surface of the coating using a cation exchange membrane, which can attract the inward diffusion of cations, accelerating the zinc ion stripping process. Although charged protective layers have proven promising for improving the zinc ion deposition/stripping process, a single charged surface may only be beneficial for the particular process of stripping or deposition, adversely affecting the reverse process. Therefore, the development of the amphoteric charged protective coating can dynamically adjust the stripping and deposition processes, further reduce the anode polarization and improve the rate capability of the anode.
Silk Fibroin (SF), a naturally occurring protein, forms a secondary conformation composed of hydrophobic β -sheets through intermolecular hydrogen bonding. Because of the existence of ionized side chain/end chain (-NH) on the surface of protein2and-COOH), SF possesses an amphoteric charge under different pH conditions, being electrically neutral at the isoelectric point (below isoelectric point: -NH2+H+＝>-NH3 +(ii) a Above isoelectric point: -COOH + -OH-＝>-COO-)。
Disclosure of Invention
The invention aims to provide a zinc metal anode modified by a silk fibroin coating, a preparation method and application thereof, and aims to solve the problems of anode instability and over-high polarization under high current density of zinc, so that the rate performance and the cycling stability of a battery are improved, and the service life of the battery is prolonged.
Preparation of zinc anode coated with silk fibroin: firstly, 4-6 g of silkworm cocoon is cut into small pieces, and the pieces are placed in a volume of 40-60 ml and 0.02M of Na2CO3Boiling the aqueous solution for 30-40 minutes, taking out the silkworm cocoons, thoroughly cleaning the silkworm cocoons with distilled water, and drying the silkworm cocoons in the air at room temperature to obtain silkworm fibroin; then, polishing the surface of the zinc foil by using sand paper, and cleaning by using deionized water and ethanol to obtain a cleaned zinc foil; dissolving 0.2-0.4 g of anhydrous calcium chloride in 10-20 ml of anhydrous formic acid (HCOOH) to obtain a uniform transparent solution; finally, adding 0.6-1.2 g of dried silk fibroin into the transparent solution under vigorous stirring (600rpm) until the silk fibroin is completely dissolved; and coating the obtained mixed solution on a cleaned zinc foil by using a scraper, drying for 10-20 hours to obtain a silk fibroin coating with the thickness of 2-10 mu m on the zinc foil, and soaking the zinc anode modified by the coating in water to induce the formation of beta-sheets and pores, thereby obtaining the zinc anode (Zn-SF anode) coated with the silk fibroin.
ZnxV2O5·nH2Preparing an O cathode material: zn is synthesized by hydrothermal reactionxV2O5·nH2And O. Firstly, 0.535-0.55 g V2O5Dispersing in 60-80 ml of deionized water, and stirring at room temperature (400rpm) for 15-25 minutes; 0.5-2 mL of H2O2And 50-80mg Zn (NO)3)2Is added to V2O5The dispersion solution is stirred vigorously (600rpm) for 20-30 minutes; then transferring the obtained mixed solution into an autoclave with a teflon lining, and heating for 9-12 hours at 170-190 ℃; cooling the reaction product to room temperature, centrifuging (2000-5000 r/min), washing the centrifuged product with deionized water for 3-5 times, and drying in vacuum at 55-65 ℃ to obtain ZnxV2O5·nH2O cathode material powder.
Preparation of Zn// Zn or Zn-SF// Zn-SF symmetrical cells: the symmetrical cells were assembled by using two pure Zn electrodes or two Zn-SF electrodes (diameter 12 mm, thickness 100 μm) in CR2025 coin cells, respectively. 2M ZnSO4The aqueous solution and a glass fiber membrane (GF/C, Whatman) were used as an electrolyte and a membrane, respectively, and the volume of the electrolyte was 200. mu.l.
Zn-ZnxV2O5·nH2O or (Zn-SF) -ZnxV2O5·nH2Preparing an O full cell: zn is reacted withxV2O5·nH2O cathode material powder, acetylene black and Polytetrafluoroethylene (PTFE) are mixed according to the weight ratio of 7-14: 2-4: 1-3, pressing on a stainless steel net to prepare a self-supporting film, drying in vacuum at room temperature, and cutting into squares (1x1 cm)2) As a cathode; zn on stainless steel netxV2O5·nH2The load mass of the O cathode active material is 1.5-3.0 mg/cm2(ii) a Assembling the cathode in a CR2025 coin cell with pure Zn or Zn-SF as the anode, glass fiber separator (GF/C, Whatman) and 2M ZnSO4(200. mu.L) was used as a separator and an electrolyte, and the volume of the electrolyte added was 200. mu.L.
Inspired by the specific recognition function and reversible surface charge of organisms, the invention provides a biological inspired protective coating with reversible amphoteric charge, which accelerates the deposition/stripping process of zinc ions and stabilizes a zinc anode by adjusting the dynamic change of the pH value of an interface. During stripping, as the pH of the coating surface increases, the coating surface is detected as negatively charged, attracting cations to diffuse into the coating and repelling sulfate anions. During the deposition process, as the pH value of the surface of the coating is reduced, the surface charge is positive, and the diffusion of zinc ions from the coating to the anode is accelerated. Importantly, the coating effectively inhibits hydrogen evolution reactions by isolating the anode from water/protons, thereby enhancing interface stability during cycling. The polar group peptide bonds (-O ═ C-N-H) at the coating surface further provide rich nucleation sites, promoting desolvation of zinc hexahydrate ions, resulting in uniform zinc nucleation and growth. Due to these unique functions, SF coating modified zinc anodes provide high rate capability and longer cycling stability, with ZnxV2O5·nH2The O cathode combined full cell provides a method for constructing a zinc anode at an interface, and is used for a high-rate water system zinc ion battery.
Drawings
FIG. 1: Zn-SF (b) and pure Zn (a) symmetrical batteries have constant current charge-discharge test curves under different multiplying power currents.
FIG. 2 is a schematic diagram: Zn-SF (b) and pure Zn (a) symmetrical cell at 1mA cm-2Constant current charge-discharge test curves of 1h for charging and discharging under current density.
FIG. 3: Zn-SF (b) and pure Zn (a) symmetrical cell at 10mA cm-2Constant current charge-discharge test curves of 0.2h each for charge-discharge at current density.
FIG. 4: Zn-SF (a) electrochemical AC impedance plot for different cycling conditions of symmetric cells as compared to pure Zn (b).
FIG. 5: tafel test curve of single electrode of Zn-SF and pure Zn anode.
FIG. 6: Zn-SF and pure Zn anode, ZnxV2O5·nH2Cyclic voltammogram of a full cell assembled with O as the cathode.
As shown in FIG. 1, 2M ZnSO was used40.5-20mA cm of electrolyte-2The rate capability of Zn-SF symmetrical cell was tested within the range (total charge/discharge capacity 0.5mAh cm)-2). The results show that the voltage-time curve remains stable with increasing current rate, with a slight increase in polarization voltage at high current rates due to the effect of the SF coating. When restored to the initial current rate, the Zn-SF anode shows similar voltage hysteresis, indicating that it has good rate performance. In contrast, pure Zn anodes exhibit similar overpotentials at lower current rates, while the poling voltage rapidly increases at high current rates, exhibiting severe voltage fluctuations, with the difficulty of exfoliation/deposition increasing gradually as byproducts block the ion transport channel, and pure Zn exhibits unstable voltage polarization and cannot be recovered.
As shown in FIG. 2, at 1mA cm-2Under the condition of charging/discharging for 1h, the pure Zn symmetrical cell has the cycle time of more than 70h, generates severe voltage fluctuation, and generates short circuit after 300h, and the polarization voltage of the Zn-SF symmetrical cell is still maintained at 32mV until 1500h and slightly increases.
As shown in FIG. 3, even at 10mA cm-2Under the high current density charge/discharge condition of 0.2h, it is still observed that the Zn-SF battery has a charge/discharge time of more than 500hThe stable cycle characteristic is obviously compared with a pure Zn symmetrical battery (200h, the voltage fluctuates sharply), and the anode modified by the coating is more stable under the high current multiplying power.
As shown in fig. 4, the charge transfer resistance of the pure Zn symmetric cell increases sharply with the number of cycles in the electrochemical ac impedance plot. It is worth noting that the charge transfer resistance of Zn-SF symmetric cells does not change much after 100 cycles and is much lower than that of pure Zn symmetric cells due to the effective protection of SF coating, while the uneven deposition with a large amount of by-products leads to increased charge transfer difficulty of pure Zn symmetric cells.
As shown in fig. 5, in the single electrode test, compared to the pure Zn anode, the SF-coating-modified zinc anode has a more positive corrosion potential and a lower corrosion current density, indicating that the corrosion rate is lower, mainly due to the fact that the silk fibroin coating can reduce the direct contact of the electrolyte with the zinc anode, and reduce the generation of side reactions.
As shown in FIG. 6, at 0.2mV s-1Exhibits two pairs of characteristic peaks (V) typical of cyclic voltammograms at the scanning rate of (1)4 +/V3+And V5+/V4+). Assembled cells based on Zn-SF anodes exhibit higher current densities, establishing higher electrochemical capacities. Furthermore, a narrower voltage gap was observed between the two pairs of redox peaks in the CV curve, representing a lower electrochemical polarization, compared to a pure Zn-based cell.
Detailed Description
The following examples are provided for better understanding of the present invention, but the present invention is not limited to the following examples and should not be construed as being limited to the scope of the present invention.
Example 1:
preparation of zinc anode coated with silk fibroin: first, silk fibroin is prepared. Cutting Bombyx Bombycis (5 g) into small pieces, adding 50 ml of 0.02M Na2CO3The aqueous solution was boiled for 35 minutes, thoroughly washed with distilled water, and dried in air at room temperature. Subsequently, 0.4 g of anhydrous calcium chloride was dissolvedThe solution was dissolved in 15 ml of anhydrous formic acid (HCOOH) to obtain a uniform transparent solution, and then 0.8 g of dried silk fibroin was added to the above solution under vigorous stirring until complete dissolution. And (2) polishing the surface of the zinc foil by using sand paper, then cleaning the zinc foil by using deionized water and ethanol, drying the zinc foil at room temperature, coating the silk fibroin mixed solution on the zinc foil by using a scraper, wherein the thickness of the zinc foil is 6 mu m, drying the zinc foil overnight to prepare a solid silk fibroin coating, and soaking the dried silk fibroin coating in water to induce the formation of beta-sheets and pores, thereby preparing the silk fibroin-coated zinc anode, which is recorded as Zn-SF.
ZnxV2O5·nH2Preparation of O cathode material: zn is synthesized by hydrothermal reactionxV2O5·nH2And O. First, 0.55 g of V2O5Dispersed in 80 ml of deionized water and stirred (400rpm) at room temperature for 15 minutes; 2mL of H2O2And 80mg Zn (NO)3)2Is added to V2O5Is vigorously stirred (600rpm) for 30 minutes; then transferring the obtained mixed solution into a teflon-lined autoclave, and heating at 180 ℃ for 12 hours; cooling the reaction product to room temperature, centrifuging (5000 r/min), washing the centrifuged product with deionized water for 5 times, and vacuum drying at 65 ℃ to obtain ZnxV2O5·nH2O cathode material powder.
Example 2:
preparation of Zn// Zn (Zn-SF// Zn-SF) symmetrical cell: the symmetrical cell was assembled by using two pure Zn electrodes (or two Zn-SF electrodes as cathode and anode, respectively) with a diameter of 12 mm and a thickness of 100 μ M in a CR2025 coin cell4The aqueous solution and a glass fiber membrane (GF/C, Whatman) were used as an electrolyte and a membrane, respectively, and the volume of the electrolyte added was 200. mu.l.
Zn(Zn-SF)-ZnxV2O5·nH2Preparing an O full cell: zn is reacted withxV2O5·nH2O powder, acetylene black and Polytetrafluoroethylene (PTFE) were mixed at a mass ratio of 7:2:1 to prepare a self-supportingSupport film, pressed on stainless steel mesh, dried under vacuum at room temperature and cut into pieces (1X1 cm)2) As a cathode. The mass loading was measured to be 2mg cm-2. The cathode was assembled in a CR2025 coin cell, pure Zn or Zn-SF as anode, glass fiber membrane (GF/C, Whatman) and 2M ZnSO4(200. mu.L) was used as a separator and an electrolyte.
Claims (5)
1. A preparation method of a zinc anode modified by a silk fibroin coating is characterized by comprising the following steps: firstly, 4-6 g of silkworm cocoon is cut into small pieces, and the pieces are placed in a volume of 40-60 ml and 0.02M of Na2CO3Boiling the aqueous solution for 30-40 minutes, taking out the silkworm cocoons, thoroughly cleaning the silkworm cocoons with distilled water, and drying the silkworm cocoons in the air at room temperature to obtain silkworm fibroin; then, polishing the surface of the zinc foil by using sand paper, and cleaning by using deionized water and ethanol to obtain a cleaned zinc foil; dissolving 0.2-0.4 g of anhydrous calcium chloride in 10-20 ml of anhydrous formic acid to obtain a uniform transparent solution; then adding 0.6-1.2 g of dried silk fibroin into the transparent solution under vigorous stirring until the silk fibroin is completely dissolved; and finally, coating the obtained mixed solution on the cleaned zinc foil by using a scraper, drying for 10-20 hours to obtain a silk fibroin coating with the thickness of 2-10 mu m on the zinc foil, and soaking the zinc foil modified by the silk fibroin coating in water to induce the formation of beta-sheets and pores, thereby obtaining the silk fibroin-coated zinc anode which is marked as a Zn-SF anode.
2. A zinc anode modified by a silk fibroin coating is characterized in that: is prepared by the method of claim 1.
3. The method for preparing (Zn-SF) -Zn by using zinc anode modified by silk fibroin coating as claimed in claim 2xV2O5·nH2The application in O full cells.
4. The method for preparing (Zn-SF) -Zn from zinc anode modified by silk fibroin coating as claimed in claim 3xV2O5·nH2O allUse in a battery, characterized in that: is prepared by reacting ZnxV2O5·nH2O cathode material powder, acetylene black and polytetrafluoroethylene are mixed according to the weight ratio of 7-14: 2-4: 1-3, pressing the mixture on a stainless steel net to prepare a self-supporting film, drying the self-supporting film in vacuum at room temperature, and cutting the film into a square shape to be used as a cathode; zn on stainless steel netxV2O5·nH2The load mass of the O cathode material is 1.5-3.0 mg/cm2(ii) a Assembling the cathode in a CR2025 button cell, with Zn-SF as the anode, a glass fiber diaphragm and 2M ZnSO4As a separator and an electrolyte, thereby obtaining (Zn-SF) -ZnxV2O5·nH2And O, fully charging the battery.
5. The method for preparing (Zn-SF) -Zn from zinc anode modified by silk fibroin coating as claimed in claim 4xV2O5·nH2The application in the O full cell is characterized in that: firstly, 0.535-0.55 g of V2O5Dispersing in 60-80 ml of deionized water, and stirring for 15-25 minutes at room temperature to obtain V2O5A dispersion liquid; 0.5-2 mL of H2O2And 50-80mg Zn (NO)3)2Is added to V2O5In the dispersion liquid, stirring vigorously for 20-30 minutes; then transferring the obtained mixed solution into an autoclave with a teflon lining, and heating for 9-12 hours at 170-190 ℃; cooling the reaction product to room temperature, centrifuging, washing the centrifuged product with deionized water for 3-5 times, and drying at 55-65 ℃ in vacuum to obtain ZnxV2O5·nH2O cathode material powder.
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| CN107170967A (en) * | 2017-05-05 | 2017-09-15 | 武汉理工大学 | Pre- intercalated layered barium oxide nano material of bivalent metal ion and its preparation method and application |
| CN113143281A (en) * | 2020-01-22 | 2021-07-23 | 天津大学 | Silk-screen printing fibroin-based high-adhesion degradable flexible electrode and application thereof in human-computer interaction interface |
| CN112563446A (en) * | 2020-11-22 | 2021-03-26 | 扬州大学 | Electrode with biopolymer coating and method for making same |
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| JIAHUI LU ET AL.: "Silk Fibroin Coating Enables Dendrite-free Zinc Anode for Long-Life Aqueous Zinc-Ion Batteries", 《CHEMSUSCHEM》, vol. 15, no. 15, pages 202200656 * |
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