CN113903965A - Novel zinc-iodine aqueous solution battery and preparation method thereof - Google Patents
Novel zinc-iodine aqueous solution battery and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a novel zinc-iodine aqueous solution battery and a preparation method thereof. The novel zinc-iodine aqueous solution battery is composed of three chambers, a new chamber is added between the two conventional chambers and is respectively isolated by an anion/cation membrane, and the intermediate chamber realizes the separation and convergence of anions/cations and has the characteristic of determining the performance of the battery. The working electrode of the invention adopts a graphite felt processed by carbon quantum dots, the middle chamber is a zinc-iodine solution with a certain concentration, the anolyte is a zinc-containing ion solution, and the catholyte is an iodine-containing ion solution. The zinc-iodine battery can well inhibit the self-discharge phenomenon of the zinc-iodine battery, improve the working stability of the battery, well inhibit the generation of zinc dendrites and improve the cyclicity of the zinc-iodine battery. Compared with the prior art, the aqueous solution zinc-iodine battery with the structure has excellent cycle performance and energy storage stability. The invention is helpful to expand the application range of the zinc ion battery with aqueous solution.
Description
Technical Field
The invention belongs to the field of aqueous solution battery energy storage, in particular to a zinc-iodine battery structure design method and a zinc-iodine battery manufacturing method, and belongs to the field of material science and engineering.
Background
Compared with the lithium ion battery which dominates the market, the nonaqueous battery of the aqueous battery is more nonaqueous than the organic electrolyte which is used at presentThe lithium ion, sodium ion and potassium ion batteries are safer, and the water system electrolyte also shows great competitiveness, (1) the cost is low, oxygen-free and dry assembly lines are not needed, and the electrolyte and the manufacturing cost are low; (2) non-volatility due to water, thus exhibiting non-toxicity and non-flammability; (3) the ability to charge rapidly and with high power density due to the high ionic conductivity of aqueous media; (4) and high resistance to electrical and mechanical mishandling, and the like, and therefore aqueous ion secondary batteries still have a great development and development space. Zinc iodide (ZnI) electrolyte used in zinc-iodine battery2) Is an environment-friendly material, is non-toxic and is not easy to burn, so the material is widely concerned by researchers at home and abroad. In 2015, Li bin and its team of the national laboratories in the northwest pacific of the united states first proposed the concept of water-based zinc-iodine flow batteries [ Li, b.et al. ambipolar zinc-polymeric electrolyte for a high-energy dense aqueous flow battery. com.6, 6303 such as]The electrolyte of the battery adopts 5 mol per liter of zinc iodide solution, and the discharge energy density is up to 167 watt-hour per liter. In recent years, the development of static zinc-iodine batteries has attracted attention (patent: a zinc-iodine battery structure, CN201711142958.4), and the new zinc-iodine battery can reduce the complexity of the device structure and eliminate the liquid circulation system, however, the self-discharge problem and the circulation stability of the zinc-iodine battery still greatly hinder the application of the zinc-iodine battery system.
Disclosure of Invention
The invention aims to provide a novel zinc-iodine aqueous solution battery which is composed of three chambers, wherein the chambers are separated by an anion/cation membrane, and a graphene quantum dot modified graphite felt is used as a working electrode. By means of the technical scheme, the novel zinc-iodine battery is produced, the middle cavity realizes the separation and the convergence of anions and cations, and the characteristics of determining the performance of the battery are achieved, so that the zinc-iodine battery with the structure can inhibit the generation of zinc dendrites, the cycle performance of the battery is improved, and the self-discharge phenomenon of the zinc-iodine battery is well inhibited.
In order to achieve the purpose, the invention adopts the technical scheme that:
a novel zinc-iodine aqueous solution battery comprises three chambers, wherein the middle chamber is a buffer solution, and the other two chambers are respectively an anode solution and a cathode solution; the anode solution is separated from the anode by a cation membrane CEM, and the cathode solution is separated from the cathode by an anion membrane AEM; and a power supply or a device is connected between the anode and the cathode. By means of the technical scheme, the novel zinc-iodine battery is constructed.
The buffer solution is a zinc-iodine solution with a certain concentration, and the concentration variation range of the zinc-iodine solution is 1-7 mol per liter. The anolyte is zinc ion-containing solution, the catholyte is iodine ion-containing solution, the anolyte is zinc ion-containing aqueous solution, the electrolyte can be zinc sulfate, zinc fluoride, zinc bromide, zinc chloride, zinc acetate and the like with different solution concentrations, the catholyte is iodine ion-containing aqueous solution, and the electrolyte can be lithium iodide, sodium iodide, potassium iodide and the like with different solution concentrations.
The zinc-iodine battery can inhibit the generation of zinc-zinc dendrites, improve the cyclicity of the zinc-iodine battery, and well inhibit the self-discharge phenomenon of the zinc-iodine battery.
The preparation method of the novel zinc-iodine aqueous solution battery comprises the following steps:
firstly, cutting a graphite felt into small pieces of 1cm multiplied by 1cm as a base material, ultrasonically cleaning the base material in ethanol and deionized water, and then drying the base material for 24 hours at the temperature of 60 ℃;
secondly, 2-10 g of citric acid is put into a crucible and heated at the temperature of 100-400 ℃ until the citric acid is melted and shows orange color. Dropwise adding the orange liquid into 10-50mL of NaOH solution with the mass concentration of 2-10mg/mL under vigorous stirring, and neutralizing the pH value of the solution to 7.0 by using NaOH with the same mass concentration to finally form graphene quantum dot solution;
and thirdly, putting the graphene quantum dot solution into a centrifuge tube, adding 10-25mL of deionized water, and putting the cleaned graphite felt into the centrifuge tube. And then placing the centrifugal tube in an ultrasonic bath for 1-10h to enable the graphene quantum dots to be attached to the surface of the graphite felt, and finally washing the sample clean with deionized water and drying. Finally preparing a graphene quantum dot modified graphite felt;
fourthly, constructing a zinc-iodine battery with three chambers, wherein the three chambers are separated by an anion/cation membrane, the middle chamber is a zinc-iodine solution with a certain concentration (the concentration range is 1-7 mol/L), the anolyte is a zinc-ion-containing solution, and the catholyte is an iodine-ion-containing solution;
and fifthly, changing the water solutions with different electrolytes and concentrations in the negative/positive chambers to construct zinc-iodine water solution batteries with different structures, and stably testing the charge and discharge performance of the batteries after standing and activating.
Compared with the prior art, the invention has the following beneficial effects:
the zinc-iodine battery with the novel structure well inhibits the generation of zinc dendrites, so that the cycle performance of the zinc-iodine battery is obviously improved.
The zinc-iodine battery with the novel structure can well inhibit the complexation of zinc/iodine ions by introducing the middle cavity, and the self-discharge phenomenon of the zinc-iodine battery is inhibited.
According to the novel zinc-iodine aqueous solution battery, a new transition chamber is added into two conventional chambers and is respectively isolated by an anion/cation membrane, the middle chamber is a zinc-iodine solution with a certain concentration, the anolyte is a zinc-ion-containing solution, and the catholyte is an iodine-ion-containing solution, so that the cost can be reduced by selecting a proper solution.
Drawings
Fig. 1 is a schematic diagram of a zinc-iodine cell (top panel).
In the figure, 1-power supply or device; 2-anode 3-cathode; 4-cationic membrane (CEM); 5-anionic membranes (AEM); 6-anode solution; 7-intermediate buffer solution; 8-cathode solution.
Fig. 2 shows a 3 cycle charge and discharge curve for a zinc-iodine cell, comparing a two chamber (top) zinc-iodine cell with a three chamber (bottom) zinc-iodine cell, where the solution is 2 moles per liter of zinc-iodine solution and the charge and discharge current is 2 ma. (2M ZnI two chamber (upper) and three chamber (lower) zinc-iodine cell first three cycle charge-discharge curve, charge-discharge current is and 2mA)
FIG. 3 shows a charge/discharge curve of a zinc-iodine cell, comparing a two-chamber (top) zinc-iodine cell with a three-chamber (bottom) zinc-iodine cell, where the solution is 5 mol/L zinc-iodine solution and the charge/discharge current is 2 mA. (5M ZnI two chamber (upper) and three chamber (lower) charging and discharging curves with charging and discharging current of 2mA)
Fig. 4 shows a 50 cycle charge and discharge curve for a zinc-iodine cell, comparing a two chamber (top) zinc-iodine cell with a three chamber (bottom) zinc-iodine cell, where the solution is 5 moles per liter of zinc-iodine solution and the charge and discharge current is 2 ma.
Figure 5 stability testing of zinc-iodine cells, comparison of two-chamber (top) and three-chamber (bottom) zinc-iodine cells, solution 5 moles per liter of zinc-iodine solution, charge and discharge current 2 milliamps.
FIG. 6 shows the stability test of the three-chamber zinc-iodine battery, and the standing time is prolonged to 12-15 hours. The chamber solution is 5 mol per liter of zinc-iodine solution, and the charging and discharging current is 2 milliamperes.
Fig. 7 electron micrographs of electrode samples after 1000 cycles comprising the anode (top left) and cathode (bottom left) of a two-chamber zinc-iodine cell, and the anode (top right) and cathode (bottom right) of a three-chamber zinc-iodine cell.
Fig. 8 changes the charge and discharge curves of the zinc-iodine cell with the positive and negative chamber solvents, the middle chamber is 1 mol per liter of zinc-iodine solution, the anode solution is 1 mol per liter of zinc sulfate solution, and the cathode solution is 1 mol per liter of potassium iodide solution. The first three cycles of the charge-discharge curve of the upper graph and the 100 cycles of the charge-discharge curve of the lower graph.
Detailed Description
The present invention will be further described with reference to the accompanying drawings, which will become apparent to those skilled in the art.
Example 1: charge-discharge test of three-chamber zinc-iodine battery
The invention provides a novel zinc-iodine aqueous solution battery, which is composed of three chambers, wherein the chambers are separated by an anion/cation membrane, and a graphene quantum dot modified graphite felt is used as a working electrode. By means of the technical scheme, a novel zinc-iodine battery (as shown in figure 1) is produced. The three chambers are all filled with 2 mol/l of zinc-iodine aqueous solution, and under the condition of two milliamperes of current, similar to the conventional zinc-iodine battery with two chambers, the stable charge-discharge curve can be realized (as shown in figure 2). A 5 mol/l zinc-iodine aqueous solution was injected into all three chambers, and a stable charge-discharge curve was also achieved at two milliamps current, similar to a conventional zinc-iodine cell with two chambers (as shown in fig. 3). And through a multi-cycle test curve (as shown in fig. 4), the three-chamber zinc-iodine cell achieved a greater discharge capacity (0.25 ma-hr) and was able to remain stable during the first 50 cycles.
Example 2: stability testing of three-chamber zinc-iodine batteries
In order to verify the stability problem of the three-chamber zinc-iodine battery after charging, the charging and discharging curves of the zinc-iodine battery after different standing times (0 to 20 hours) are tested to judge the stability problem of the zinc-iodine battery. As shown in fig. 5, in the conventional two-chamber zinc-iodine battery, after the standing time is half an hour, the efficiency (capacity) retention rate is still 50-60%, the proportional value of the efficiency (capacity) can be continued to the standing time for 4 hours, and once the standing time is longer than 4 hours, the efficiency (capacity) value is rapidly reduced, so that the stability of the capacity of the conventional two-chamber zinc-iodine battery can only be considered to be maintained for 4 hours. In the three-chamber zinc-iodine battery, after the three-chamber zinc-iodine battery is kept still for half an hour, the efficiency (capacity) retention rate is still 50-60%, the efficiency (capacity) retention rate is not attenuated until the three-chamber zinc-iodine battery is kept still for 6 hours, the standing time is continuously prolonged, the retention time of the charging capacity can reach 15 hours (as shown in figure 6), and the improvement of the battery stability of the three-chamber zinc-iodine battery by more than 3 times is proved.
Example 3: electrode surface topography testing
In order to observe the zinc deposition characteristics of the three-chamber zinc-iodine battery, the appearance of the surfaces of the positive and negative electrodes after 1000 cycles is observed by using an electron microscope, and compared with the zinc deposition on the surfaces of the positive and negative batteries of the two-chamber zinc-iodine battery (as shown in an upper graph of fig. 7), the deposition amount of the anode zinc is obviously reduced, and the generation of zinc dendrites is effectively inhibited. Even for the cathode, the electrode surface of the three-chamber zinc-iodine cell was very smooth and had no precipitates, while the electrode surface of the two-chamber zinc-iodine cell had some amount of zinc deposited. The three-chamber zinc-iodine battery is proved to be capable of well inhibiting the generation of zinc dendrites, which is very helpful for the stability work of the zinc-iodine battery.
Example 4: charge-discharge test of three-chamber zinc-iodine battery composed of different electrolytes
In order to verify the flexibility and variability of the three-cavity zinc-iodine battery and expand the application range of the three-cavity zinc-iodine battery, the novel zinc-iodine battery is constructed by changing the types of solutions of the three cavities. We can construct a new type of zinc-iodine battery by choosing a certain concentration of zinc-iodine solution (e.g. 1 mol/l) as the middle chamber, zinc-ion-containing solution (e.g. zinc sulfate) as the anolyte, and iodine-ion-containing solution (e.g. potassium iodide) as the catholyte. The test results are shown in fig. 8, the first three cycle charge-discharge curves of this cell show a stable discharge plateau, with a discharge voltage of about 1.1 v and maintaining 130 cycle stability.
While the present invention has been described in detail by way of examples, it will be understood by those skilled in the art that various modifications and alterations can be made without departing from the principles of the present invention, such as changing the carbon-based material, changing the electrolyte of the solution, changing the membrane of the anion and cation, etc., and such modifications and alterations should also be construed as falling within the scope of the present invention.
Claims (4)
1. A novel zinc-iodine aqueous solution battery is characterized in that: the device comprises three chambers, wherein the middle chamber is buffer solution, and the other two chambers are anode solution and cathode solution respectively; the anode solution is separated from the anode by a cation membrane CEM, and the cathode solution is separated from the cathode by an anion membrane AEM; and a power supply or a device is connected between the anode and the cathode.
2. The novel zinc-iodine aqueous solution battery according to claim 1, characterized in that: the buffer solution is a zinc-iodine solution with a certain concentration, and the concentration variation range of the zinc-iodine solution is 1-7 mol per liter.
3. The novel zinc-iodine aqueous solution battery according to claim 1, characterized in that: the anolyte is zinc ion-containing solution, the catholyte is iodine ion-containing solution, the anolyte is zinc ion-containing aqueous solution, and the electrolyte is selected from zinc sulfate, zinc fluoride, zinc bromide, zinc chloride and zinc acetate with different solution concentrations; the cathode electrolyte is an iodine ion-containing aqueous solution, and the electrolyte is selected from lithium iodide, sodium iodide and potassium iodide with different solution concentrations.
4. A method of manufacturing a novel zinc-iodine aqueous battery as claimed in any one of claims 1 to 3, wherein: the method comprises the following steps:
firstly, cutting a graphite felt into small pieces of 1cm multiplied by 1cm as a base material, ultrasonically cleaning the base material in ethanol and deionized water, and then drying the base material for 24 hours at the temperature of 60 ℃;
secondly, 2-10 g of citric acid is put into a crucible and heated at the temperature of 100-400 ℃ until the citric acid is melted and shows orange color. Dropwise adding the orange liquid into 10-50mL of NaOH solution with the mass concentration of 2-10mg/mL under vigorous stirring, and neutralizing the pH value of the solution to 7.0 by using NaOH with the same mass concentration to finally form graphene quantum dot solution;
and thirdly, putting the graphene quantum dot solution into a centrifuge tube, adding 10-25mL of deionized water, and putting the cleaned graphite felt into the centrifuge tube. And then placing the centrifugal tube in an ultrasonic bath for 1-10h to enable the graphene quantum dots to be attached to the surface of the graphite felt, and finally washing the sample clean with deionized water and drying. Finally preparing a graphene quantum dot modified graphite felt;
fourthly, constructing a zinc-iodine battery with three chambers, wherein the three chambers are separated by an anion/cation membrane, the middle chamber is a zinc-iodine solution with a certain concentration (the concentration range is 1-7 mol/L), the anolyte is a zinc-ion-containing solution, and the catholyte is an iodine-ion-containing solution;
and fifthly, changing the water solutions with different electrolytes and concentrations in the negative/positive chambers to construct zinc-iodine water solution batteries with different structures, and stably testing the charge and discharge performance of the batteries after standing and activating.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115020756A (en) * | 2022-06-13 | 2022-09-06 | 燕山大学 | Zinc-bromine/iodine double flow battery |
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| CN105742656A (en) * | 2014-12-11 | 2016-07-06 | 中国科学院大连化学物理研究所 | Zinc-iodine flow battery |
| CN113224396A (en) * | 2021-07-08 | 2021-08-06 | 北京航空航天大学 | Zinc-polymer water system rechargeable battery with three-chamber structure and preparation method thereof |
| CN113437339A (en) * | 2021-05-10 | 2021-09-24 | 中国科学院金属研究所 | Positive electrode electrolyte for zinc-iodine flow battery |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105742656A (en) * | 2014-12-11 | 2016-07-06 | 中国科学院大连化学物理研究所 | Zinc-iodine flow battery |
| CN113437339A (en) * | 2021-05-10 | 2021-09-24 | 中国科学院金属研究所 | Positive electrode electrolyte for zinc-iodine flow battery |
| CN113224396A (en) * | 2021-07-08 | 2021-08-06 | 北京航空航天大学 | Zinc-polymer water system rechargeable battery with three-chamber structure and preparation method thereof |
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| GUO-MING WENG,ET AL: "Unlocking the capacity of iodide for high-energydensity zinc/polyiodide and lithium/polyiodide redox flow batteries", 《ENERGY & ENVIRONMENTAL SCIENCE》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115020756A (en) * | 2022-06-13 | 2022-09-06 | 燕山大学 | Zinc-bromine/iodine double flow battery |
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