CN114243166B - High-power-density metal-air battery and preparation method thereof - Google Patents
High-power-density metal-air battery and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-power density metal-air battery and a preparation method thereof, wherein anhydrous sodium carbonate powder is dissolved in deionized water, and konjak glucomannan powder is added for solidification to obtain uniform and stable productA fixed gel solid A; dissolving sodium hydroxide, zinc oxide and sodium stannate in deionized water to obtain a solution B, and soaking the gel solid A in the solution B to obtain a gel electrolyte; and taking metal as a negative electrode, taking waterproof carbon cloth loaded with C/N/MnO as an air positive electrode, and respectively placing the waterproof carbon cloth on two sides of the gel electrolyte to assemble the metal-air battery. The gel electrolyte with high electric power density is prepared from konjak glucomannan under the conditions of anhydrous sodium carbonate serving as a cross-linking agent and heating, and has the advantages of porous thermal stability, high alkali absorption, excellent high-current discharge performance of the assembled gel aluminum-air battery and high power density up to 90.7 mW cm ‑2 The requirements of the metal-air battery can be met; the preparation process is simple, low in cost and environment-friendly.
Description
Technical Field
The invention belongs to the technical field of metal-air batteries, and relates to a high-power density metal-air battery and a preparation method thereof.
Background
Metal Fuel Cells (MFC), also known as metal air cells, are new concepts of fuel cells formed by replacing hydrogen with metal fuel, and provide metals such as zinc, aluminum, etc., like fuel hydrogen, to reaction sites in the cells, which together with oxygen form a continuous electric energy generating device.
The aluminum-air battery has higher theoretical energy density (8100 Wh kg -1 ) The advantages of innocuity, environmental protection, etc. are paid attention to widely, and the high-performance aluminum-air battery assembled by the alkaline gel electrolyte prepared by the high polymer canThe advantages of preventing electrolyte leakage, being high in safety, convenient to carry, effectively inhibiting aluminum corrosion and the like are widely studied.
Gel Polymer Electrolytes (GPEs) are a new type of electrolyte and are a hot spot for research. Polyvinyl alcohol (PVA) and polyacrylic acid (PAA) are applied to aluminum air cells by Yang et al, polyvinyl alcohol (PVA) is applied to zinc air cells by romiro et al, and many studies on the use of polymer electrolytes in metal air cells have been conducted. The most commonly used high polymer material is PVA, and the defects of high conductivity, low price, simple preparation process, poor interface contact, unstable discharge performance and the like are needed to be solved.
Konjak glucomannan (konjac glucomannan, KGM) is a water-soluble polysaccharide widely existing in konjak tubers and is also a natural and renewable high-molecular polysaccharide. The molecular structure is an extended semi-flexible straight chain molecule, and a branched chain structure is not present, but the molecule has flexibility. Is a high molecular compound formed by connecting glucose and mannose by beta-1, 4 glycosidic bond, and acetyl groups are also arranged at the C-6 position of the mannose, and the existence of the acetyl groups determines the water solubility of KGM molecules.
Generally, KGM molecules can not generate gel in neutral and acid solutions, and can form thermally irreversible gel under the treatment of hot alkali, but konjak gel caused by hot alkali has the problems of easy water separation, insufficient gel strength and the like, and further application of konjak gel in the aspect of energy devices is limited. ZHOU et al (ZHOU Y, JIANG R S, PERKINS W S, CHENG Y Q. Morphology evolution and gelation mechanism of alkali induced konjac glucomannan hydro gel. Food Chemistry, 2018, 269:80-88.) studied and found that when a konjac gum solution was mixed with sodium carbonate and heated to 70℃or higher, the konjac gum molecules immediately deacetylated, inducing gelation of the solution.
KGM has a large number of-OH groups, gel shows good hydrophilicity and swelling property, and can form high-viscosity solution when dissolved in water, and has excellent hydrophilicity, gel property, thickening property and the like, so that the KGM is widely applied to the fields of foods, medicines, papermaking, environmental protection, high polymer materials and the like. Has certain alkali resistance and provides a foundation for the research and development of the alkaline gel aluminum-air battery.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the high-power density metal-air battery and the preparation method thereof, and the preparation process is simple, the cost is low, the used raw materials are low in price, and the environment is protected.
In order to solve the technical problems, the invention adopts the following technical scheme:
the method for preparing the high-power density gel electrolyte and assembling the battery by using konjak glucomannan, zinc oxide and sodium stannate comprises the following steps:
(1) At room temperature, dissolving anhydrous sodium carbonate powder in deionized water, then adding konjak glucomannan powder to obtain a mixed solution, and solidifying the mixed solution to obtain uniform and stable gel solid A;
(2) Dissolving sodium hydroxide, zinc oxide and sodium stannate in deionized water to prepare a stable solution B, and soaking the gel solid A prepared in the step (1) in the solution B to obtain a gel electrolyte;
(3) And (3) taking metal as an anode, taking C/N/MnO-loaded waterproof carbon cloth as an air anode, and respectively placing the waterproof carbon cloth on two sides of the gel electrolyte prepared in the step (2) to assemble the metal-air battery.
Further, the mass concentration of sodium carbonate in the mixed solution in the step (1) is 0.3% -0.5%, the molecular weight of the konjak glucomannan is 200-2000 kDa, and the mass concentration of the konjak glucomannan in the mixed solution is 2.8% -3.2%.
Further, in the step (1), the mass ratio of the anhydrous sodium carbonate to the konjac glucomannan is 12:100.
Further, the curing temperature in the step (1) is 90-95 ℃, preferably 90 ℃.
Further, the concentration of sodium hydroxide in the solution B in the step (2) is 7mol/L, the concentration of zinc oxide is 7mol/L, and the concentration of sodium stannate is 7 mol/L.
Further, the soaking temperature in the step (2) is normal temperature, and the soaking time is 48 and h.
The high-power-density metal-air battery prepared by the preparation method has the structure that an aluminum foil/plate is used as a negative electrode, alkaline konjak glucomannan is used as a gel electrolyte, and waterproof carbon cloth coated with a C/N/MnO catalyst is used as a positive electrode.
The prepared electrolyte is porous, has high thermal stability and high alkaline absorption, and the assembled gel aluminum air battery has excellent high-current discharge performance, and the power density is as high as 90.7 mW cm -2 The small gel aluminum-air battery is 1 mAcm -2 The discharge time is 13.8 and h under the current density, and the large gel aluminum-air battery is 20 mAcm -2 The discharge time is 118h under the current density, and the requirements of the metal-air battery can be met.
The invention has the beneficial effects that: the konjak glucomannan gel electrolyte prepared by the invention has larger network holes, and the electrochemical performance, the power density and the discharge performance of the alkaline gel electrolyte are improved through the network structure. The gel electrolyte has stable structure and strong alkali absorbing capacity, can meet the discharge of an aluminum-air battery under the high current density, and has excellent electrochemical performance. The alkaline KGM gel electrolyte prepared by the invention can solve the interface problem and serious side reaction of the current gel aluminum-air battery by assembling the battery, and has excellent discharge performance under high current density. The corrosion inhibitor is added into the electrolyte, so that the electrochemical performance of the battery is effectively improved, and a foundation is laid for the practical application of the metal-air battery.
Drawings
FIG. 1 is a schematic diagram showing an aluminum air cell assembled from the gel electrolyte prepared in comparative example 1 of the present invention at 1mA cm -2 Discharge performance at current density.
FIG. 2 is a schematic diagram showing an aluminum air cell assembled from the gel electrolyte prepared in example 1 of the present invention at 1mA cm -2 Discharge performance at current density.
Fig. 3 is an Open Circuit Potential (OCP) diagram of an assembled aluminum air battery of the gel electrolyte prepared in comparative example 2 of the present invention.
Fig. 4 is an Open Circuit Potential (OCP) diagram of an assembled aluminum air cell of the gel electrolyte prepared in example 1 of the present invention.
Fig. 5 is a graph showing the results of linear voltammetry (LSV) of the gel electrolyte prepared in comparative example 3 according to the present invention assembled into an aluminum air cell.
Fig. 6 is a graph of linear voltammogram (LSV) results of the gel electrolyte prepared in example 1 of the present invention assembled into an aluminum air cell.
FIG. 7 is a graph showing that the gel electrolyte prepared in comparative example 4 of the present invention was assembled into an aluminum air cell at 20mA cm -2 Discharge performance at current density.
FIG. 8 is a graph showing that the gel electrolyte prepared in example 1 of the present invention was assembled into an aluminum air cell at 20mA cm -2 Discharge performance at current density.
Fig. 9 is an Open Circuit Potential (OCP) diagram of an assembled aluminum air cell of the gel electrolyte prepared in comparative example 5 of the present invention.
Fig. 10 is an Open Circuit Potential (OCP) diagram of an assembled aluminum air cell of the gel electrolyte prepared in example 2 of the present invention.
FIG. 11 is a graph showing that the gel electrolyte prepared in comparative example 6 of the present invention was assembled into an aluminum air cell at 5mA cm -2 Discharge performance at current density.
FIG. 12 is a graph showing that the gel electrolyte prepared in example 1 of the present invention was assembled into an aluminum air cell at 5mA cm -2 Discharge performance at current density.
FIG. 13 is a Scanning Electron Microscope (SEM) result of the gel electrolyte prepared in comparative example 7 of the present invention.
FIG. 14 is a Scanning Electron Microscope (SEM) result of the gel electrolyte prepared in example 1 of the present invention.
Fig. 15 is a structural view of a large gel aluminum-air battery according to the present invention.
FIG. 16 is a graph showing that the gel electrolyte prepared in comparative example 8 of the present invention was assembled into an aluminum air cell at 20mA cm -2 Discharge performance at current density.
FIG. 17 is a graph showing the assembly of the gel electrolyte prepared in example 2 of the present invention into an aluminum air cell at 20mA cm -2 At current densityIs a graph of discharge performance of (a).
Detailed Description
The invention will be further illustrated with reference to specific examples. It is to be understood that the following examples are intended to illustrate the present invention and are not to be construed as limiting the scope of the invention, and that numerous insubstantial modifications and adaptations can be made by those skilled in the art in light of the foregoing disclosure.
Example 1
The preparation method of the high-power-density metal-air battery of the embodiment is as follows:
0.36. 0.36 g anhydrous sodium carbonate (molecular weight 106) was weighed and dissolved in 100 mL deionized water at room temperature (25 ℃) and the glass rod was stirred continuously for about 10 minutes to complete dissolution. Then, 3 g konjak glucomannan (molecular weight 200-2000 kDa) was dispersed in the above solution, and the glass rod was continuously stirred for 20 minutes, and when the solution was in a non-flowing state, it was put in a water bath at 90℃to be solidified. After curing about 2h, the solid appeared pale yellow in color and had a relatively hard texture, which was allowed to stand at room temperature for about 24. 24 h. Finally, the gel was immersed in a mixed solution of sodium hydroxide, zinc oxide and sodium stannate (the concentration of sodium hydroxide, zinc oxide and sodium stannate in the mixed solution is 7 mol/L) for about 48 h to obtain an alkaline gel electrolyte.
Preparation of small (2 cm. Times.2 cm. Times.3 cm) cells: an aluminum foil with a thickness of 0.5. 0.5 mm was used as an anode, and 5mg of C/N/MnO was dispersed in 500. Mu.LH 2 O，500μLC 2 H 5 In a mixed solution of OH and 70 mu LNafion, and ultrasonic treatment was performed for 30min, after which 225 mu L of the uniform paint was applied to a carbon cloth having a water-repellent adhesive in an area of 1X 1 cm 2 Then baking in oven at 60deg.C for 30min to dry to obtain a load of 1.97 mg cm -2 Is provided. And respectively placing the two on two sides of the prepared gel electrolyte to assemble the gel aluminum-air battery.
Preparation of Large (12 cm. Times.4 cm. Times.10 cm) cell an aluminum plate with a thickness of 5. 5 mm was used as anode, 50mg of C/N/MnO was dispersed in 5000. Mu.LH 2 O，5000μLC 2 H 5 In a mixed solution of OH and 700 mu LNafion, and sonicated for 50min, after which a uniform coating thereof was applied to the toolThe coating area of the carbon cloth with waterproof glue is 10 multiplied by 10cm 2 Then baking in oven at 60deg.C for 30min to dry to obtain a load of 0.5 mg cm -2 Is provided. And respectively placing the two on two sides of the prepared gel electrolyte to assemble the gel aluminum-air battery.
The prepared gel electrolyte is soaked in deionized water, frozen at the temperature of minus 10 ℃ for 24 h, then freeze-dried in a freeze dryer (under the vacuum condition of minus 65 ℃) for 24 h, and the section of the obtained sample is stuck on a scanning sample table by conductive adhesive and subjected to metal spraying treatment for 100 s, thus being used for Scanning Electron Microscope (SEM) sample shooting.
The cell was tested for open circuit potential under conditions of a scan rate of 0.01 v/s and a scan time of 120 s. The power density of this cell was tested at an initial voltage of 1.5 v and a sweep rate of 0.01 v/s.
The cells were measured at 1-20 mA cm -2 And (3) carrying out a discharge test under the current density to obtain a stable discharge platform and effective working time of the battery.
The small gel aluminum-air battery assembled in the embodiment is 1 mAcm -2 As shown in fig. 2, the discharge performance at the current density of 13.8 h can be stably discharged; FIG. 4 is an open circuit voltage of an assembled aluminum cell, which is relatively stable and about 1.68V, and the linear voltammetry (LSV) results of FIG. 6 show that the power density of the aluminum cell is 90.7 mW cm -2 . As can be seen from FIG. 8, the temperature is 20mA cm -2 The aluminum-air battery can stably discharge 4.7 h at the current density of (a). At 5mA cm -2 The aluminum space cell can stably discharge 9.7. 9.7 h at the current density as shown in fig. 12. The result of a Scanning Electron Microscope (SEM) of the obtained alkaline gel electrolyte is shown in fig. 14, and the larger network holes can better store the liquid electrolyte, and simultaneously provide channels for the transmission of the electrolyte, so that the alkaline gel electrolyte has good electrochemical performance. The following is explained: the gel electrolyte assembled metal-air battery prepared by the invention has excellent electrochemical performance.
Example 2
The preparation method of the high-power-density metal-air battery of the embodiment is as follows:
2 g anhydrous sodium carbonate (molecular weight 106) was weighed into 400 mL deionized water at room temperature (25 ℃) and the glass rod was stirred continuously for about 10 min to complete dissolution. Then, 13 g konjak glucomannan (molecular weight 200-2000 kDa) was dispersed in the above solution, and the glass rod was continuously stirred for 40 min, and when the solution was in a non-flowing state, it was put in a water bath at 90℃to be solidified. After curing about 6 h, the solid appeared pale yellow in color and had a relatively hard texture, which was allowed to stand at room temperature for about 24. 24 h. Finally, it was immersed in a mixed solution of sodium hydroxide, zinc oxide and sodium stannate for about 48 h to obtain an alkaline gel electrolyte.
The assembly method is the same as in example 1.
Fig. 10 is an open circuit voltage of a large gel aluminum air cell assembled to be relatively stable and approximately 1.7V. The assembled large gel aluminum-air battery structure is shown in a physical diagram in FIG. 15, and can be seen from FIG. 17 at 20mA cm -2 The large gel aluminum void cell can be stably discharged 118h at a current density of (a). The following is explained: the large-sized metal-air battery assembled by the invention has excellent electrochemical performance.
Comparative example 1
The procedure of example 1 was repeated except that the konjac glucomannan of example 1 was replaced with polyvinyl alcohol (molecular weight: 205,000).
FIG. 1 shows a small gel aluminum air cell assembled in comparative example 1 at 1mA cm -2 The discharge test was carried out at a current density of about 4.1 hours, and compared with example 1, there was no good interface contact, which severely affected the service life of the battery, resulting in a large difference in electrochemical properties.
Comparative example 2
The curing temperature of this comparative example was 85℃and the rest of the procedure was as in example 1.
The Open Circuit Potential (OCP) of the resulting gel electrolyte, as seen from the third graph, was maintained at about 1.52V, with a certain difference from 1.68V of example 1.
Comparative example 3
In this comparative example, deionized water was used in an amount of 80% mL, and the rest of the procedure was as in example 1.
FIG. 5 is a graph showing the results of linear voltammetry (LSV) of the gel electrolyte prepared in comparative example 3, the highest power density of comparative example 3 being 27.4mW cm -2 Whereas the highest power density of example 1 was 90.7 mW cm -2 This illustrates: the alkaline gel polymer electrolyte prepared by the invention has excellent electrochemical performance.
Comparative example 4
The zinc oxide and sodium stannate in the mixed solution of example 1 were replaced with dihydrogen phosphate, wherein the concentration of the dihydrogen phosphate was 14mol/L, and the rest of the steps were the same as in example 1.
As can be seen from FIG. 7, comparative example 4 was conducted at 20mA cm -2 The aluminum space cell was able to discharge stably at about 0.5. 0.5 h, while the sample prepared in example 1 was able to discharge stably at 4.7. 4.7 h under the same conditions. The following is explained: the alkaline gel polymer electrolyte prepared by the corrosion inhibitor has excellent electrochemical performance.
Comparative example 5
The procedure of example 1 was repeated except that zinc oxide and sodium stannate in the mixed solution of example 1 were replaced with sodium silicate, wherein the concentration of sodium silicate was 14 mol/L.
As can be seen from fig. 9, the Open Circuit Potential (OCP) of the resulting gel electrolyte was maintained at about 1.63V, which is lower than 1.68V of example 1, affecting the discharge performance.
Comparative example 6
The procedure of example 1 was followed except that zinc oxide and sodium stannate in the mixed solution of example 1 were replaced with calcium tartrate having a calcium tartrate concentration of 14 mol/L.
As can be seen from FIG. 11, comparative example 6 was conducted at 5mA cm -2 The aluminum space cell was able to discharge stably at about 2.7. 2.7 h, while the sample prepared in example 1 was able to discharge stably at 9.7. 9.7 h at the same current density. The following is explained: the alkaline gel polymer electrolyte prepared by the invention has excellent electrochemical performance.
Comparative example 7
The procedure of example 1 was repeated except that zinc oxide and sodium stannate in the mixed solution of example 1 were replaced with glucose, wherein the concentration of glucose was 14 mol/L.
Fig. 13 shows the Scanning Electron Microscope (SEM) results of comparative example 7, from which it can be seen that the internal structure of the gel is denser, and that there is no larger network pores that can store and transport the liquid electrolyte, compared to example 1, resulting in a larger gap in electrochemical performance.
Comparative example 8
The curing temperature of this comparative example was 85℃and the rest of the procedure was as in example 2.
FIG. 16 is a 20mA cm large gel aluminum air cell assembled in comparative example 8 -2 The discharge performance diagram under the current density is about 7.2h of discharge, which is far lower than that of the example 2 under the same condition, and the discharge platform is unstable, the utilization rate of the aluminum cathode is not high, and the service life of the battery is shortened.
The reagents and starting materials used in the examples were all commercially available conventional starting materials.
The foregoing has shown and described the basic principles and main features of the present invention and the advantages of the present invention. The present invention is not limited to the above-described embodiments, and the above-described embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made therein without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (3)
1. The preparation method of the high-power-density metal-air battery is characterized by comprising the following steps of:
(1) At room temperature, dissolving anhydrous sodium carbonate powder in deionized water, then adding konjak glucomannan powder to obtain a mixed solution, and solidifying the mixed solution to obtain uniform and stable gel solid A;
(2) Dissolving sodium hydroxide, zinc oxide and sodium stannate in deionized water to prepare a stable solution B, and soaking the gel solid A prepared in the step (1) in the solution B to obtain a gel electrolyte;
(3) Taking metal as a negative electrode, taking C/N/MnO-loaded waterproof carbon cloth as an air positive electrode, and respectively placing the waterproof carbon cloth on two sides of the gel electrolyte prepared in the step (2) to assemble a metal-air battery;
the mass ratio of the anhydrous sodium carbonate to the konjac glucomannan is 12:100;
the curing temperature in the step (1) is 90-95 ℃;
the concentration of sodium hydroxide in the solution B in the step (2) is 7mol/L, the concentration of zinc oxide is 7mol/L, and the concentration of sodium stannate is 7 mol/L.
2. The method of manufacturing a high power density metal-air battery according to claim 1, wherein: the soaking temperature in the step (2) is normal temperature, and the soaking time is 48 and h.
3. A high power density metal-air battery made by the method of making according to claim 1 or 2.
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| US5585208A (en) * | 1995-08-10 | 1996-12-17 | Lian; Keryn K. | Alkaline gel electrolyte for electrochemical cells |
| CN100419004C (en) * | 2006-08-31 | 2008-09-17 | 上海交通大学 | Gelation method of low concentration konjak glucomannan at low-temperature basic condition |
| CN108232109B (en) * | 2017-12-26 | 2020-07-24 | 华中科技大学 | Application of konjac glucomannan in adhesive |
| CN110085909B (en) * | 2019-05-05 | 2021-06-22 | 中南大学 | Composite solid electrolyte material and preparation method and application thereof |
| CN112713293B (en) * | 2021-01-25 | 2022-05-10 | 郑州大学 | High-conductivity gel polymer electrolyte applied to aluminum-air battery and preparation method and application thereof |
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