CN103259024A - Composite negative plate of cerium and zinc redox flow cell and preparation method of plate - Google Patents
Composite negative plate of cerium and zinc redox flow cell and preparation method of plate Download PDFInfo
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- CN103259024A CN103259024A CN2013101799394A CN201310179939A CN103259024A CN 103259024 A CN103259024 A CN 103259024A CN 2013101799394 A CN2013101799394 A CN 2013101799394A CN 201310179939 A CN201310179939 A CN 201310179939A CN 103259024 A CN103259024 A CN 103259024A
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Abstract
The invention provides a composite negative plate of a cerium and zinc redox flow cell and a preparation method of the plate, and belongs to the field of electrochemical cells. The composite negative plate comprises a metallic titanium plate and a surface active layer, wherein the surface active layer comprises a binding agent, an activating agent and an additive; polyvinylidene fluoride or polytetrafluoroethylene is used as the binding agent; the mixture of zinc powder and conducting material is used as the activating agent; and one or more of indium oxide, tin oxide, bismuth oxide, titanium oxide or cerium oxide is/are used as the additive; and the ratio of the binding agent to the activating agent to the additive is (5 to 15):(50 to 90):(5 to 50) in weight part. The invention also discloses a preparation method of the composite negative plate of the cerium and zinc redox flow cell. The cell assembled by the composite negative plate is subjected to charge-discharge testing through 100mA current, the number of cycles of the cell reaches more than 550, the average voltage efficiency of the cell is 88.4 percent, the average coulomb efficiency is 96.4 percent, and the average energy efficiency is 82.9 percent.
Description
Technical field
The invention belongs to field of electrochemical batteries, be particularly related to a kind of cerium zinc redox flow batteries composite negative plate and preparation method thereof.
Technical background
In the research of cerium zinc flow battery, generally use graphite, graphite felt or pure zinc as the negative material of battery.As 2011, people such as P.K.Leung are at Journal of Power Sources 196(2011) reported the achievement in research about the cerium zinc flow battery among the 5174-5185, it uses carbon-polyethylene combination electrode as battery cathode in assembled battery, discovery is in the long-time running of battery, pH in the negative pole electrolyte can reduce, the anticathode deposition zinc has bigger corrosiveness, and finally capacity and the cycle life to battery exerts an influence.Thanking to the will roc in 2011 has used pure zinc metal sheet to make the negative pole of battery in its thesis for the doctorate " research of the anodal electrolyte of zinc-cerium flow battery ", after the battery operation several cycles, because the zinc overpotential of hydrogen evolution is lower, the negative pole zinc metal sheet dissolves, and battery cycle life is shorter.In addition, use when more common graphite felt electrode is done negative pole at present, zinc can be deposited on the staggered position of graphite felt fiber in the charging process, and the dissolving of zinc when being unfavorable for discharging causes the reduction of capacity, influences the performance of battery.
Summary of the invention
The present invention seeks in order to solve the easily problem of dissolving of existing cerium zinc flow battery negative plate zinc metal sheet, and a kind of cerium zinc redox flow batteries composite negative plate and preparation method thereof is provided.
The present invention at first provides a kind of cerium zinc redox flow batteries composite negative plate, this composite negative plate comprises metallic titanium plate and surface activity layer, described surface activity layer is by binding agent, activator and additive are formed, described binding agent is Kynoar (PVDF) or polytetrafluoroethylene (PTFE), activator is the mixture of zinc powder and electric conducting material, additive is indium oxide, tin oxide, bismuth oxide, in titanium oxide or the cerium oxide one or more, described binding agent, activator and weight of additive portion rate are (5～15): (50～90): (5～50).
Preferably, the ratio of weight and number of zinc powder and electric conducting material is (1～5) in the described activator: 1.
Preferably, described electric conducting material is selected from one or more in active carbon, Graphene or the acetylene black.
Preferably, described binding agent, activator and weight of additive portion rate are (5～10): (60～80): (20～40).
Preferably, described surface activity layer is 50～300mg/cm in the amount of being coated with of pickling metal titanium plate
2
The present invention also provides a kind of preparation method of cerium zinc redox flow batteries composite negative plate, comprises as follows:
1) according to the weight fraction meter, binding agent, activator and additive are mixed, obtain the active layer slurry; Described binding agent is Kynoar (PVDF) or polytetrafluoroethylene (PTFE), activator is the mixture of zinc powder and electric conducting material, additive is one or more in indium oxide, tin oxide, bismuth oxide, titanium oxide or the cerium oxide, and described binding agent, activator and weight of additive portion rate are (5～15): (50～90): (5～50);
2) the active layer slurry that step 1) is obtained is coated in a side of metallic titanium plate, obtains cerium zinc redox flow batteries composite negative plate behind the vacuum drying.
Preferably, the ratio of weight and number of zinc powder and electric conducting material is (1～5) in the described activator: 1.
Preferably, described electric conducting material is selected from one or more in active carbon, Graphene or the acetylene black.
Preferably, described binding agent, activator and weight of additive portion rate are (5～10): (60～80): (20～40).
Preferably, described surface activity layer is 50～300mg/cm in the amount of being coated with of pickling metal titanium plate
2
Beneficial effect of the present invention
The present invention at first provides a kind of cerium zinc redox flow batteries composite negative plate, this composite negative plate is to apply the high activity layer in the higher pickling metal titanium plate of corrosion resistance, because the metallic titanium plate mechanical property is higher, be conducive to the battery pile assembling, active layer has higher conductivity and high overpotential of hydrogen evolution, described activator is the mixture of zinc powder and electric conducting material, the adding of zinc powder is to guarantee that zinc is when deposition, electrode surface has had more nucleating point, thereby can save the deposition time of zinc, improve the deposition efficiency of zinc, the interpolation of electric conducting material not only can improve the activity of electrode, can also improve the conductivity of electrode, reduce the internal resistance of battery, improve battery efficiency; The additive effect mainly is the overpotential of hydrogen evolution that improves electrode, suppresses the formation of zinc dendrite and the cross section CURRENT DISTRIBUTION of optimization battery charge and discharge process.Compare with the metallic zinc electrode with the graphite-like electrode of present use, composite negative plate of the present invention has electro-chemical activity height, hydrogen-evolution overpotential height, can obviously improve energy efficiency and the useful life of battery, experimental result shows: composite negative plate of the present invention is assembled into battery, use the 100mA electric current to carry out charge-discharge test, the cycle-index of battery reaches more than 550 times, and battery average voltage efficient is 88.4%, average enclosed pasture efficient is 96.4%, and average energy efficient is 82.9%.
The present invention also provides a kind of preparation method of cerium zinc redox flow batteries composite negative plate, this method is utilized binding agent Kynoar (PVDF) or polytetrafluoroethylene (PTFE) zinc powder and the electric conducting material that activity is higher, cooperate additives such as an amount of bismuth oxide, indium oxide, titanium oxide, cerium oxide, be coated in the higher titanium of corrosion resistance or titanium alloy material plate, preparation cerium zinc flow battery composite negative plate, this preparation method's technology is simple, with low cost.
Description of drawings
Fig. 1 is cerium zinc redox flow batteries composite negative plate monolithic electrode schematic diagram of the present invention;
Wherein, 1, metallic titanium plate, 2, surface activity layer.
Embodiment
The present invention at first provides a kind of cerium zinc redox flow batteries composite negative plate, as shown in Figure 1, this composite negative plate comprises metallic titanium plate 1 and surface activity layer 2, described surface activity layer 2 is by binding agent, activator and additive are formed, described binding agent is Kynoar (PVDF) or polytetrafluoroethylene (PTFE), activator is the mixture of zinc powder and electric conducting material, described electric conducting material is preferably selected from active carbon, in Graphene or the acetylene black one or more, more preferably active carbon or acetylene black, the ratio of weight and number of zinc powder and electric conducting material is preferably (1～5) in the described activator: 1, more preferably (1.5～3): 1; Additive is one or more in indium oxide, tin oxide, bismuth oxide, titanium oxide or the cerium oxide, described binding agent, activator and weight of additive portion rate are (5～15): (50～90): (5～50) are preferably (5～10): (60～80): (20～40).
Described surface activity layer is preferably 50～300mg/cm in the amount of being coated with of pickling metal titanium plate
2, 100～200mg/cm more preferably
2, most preferably be 120～160mg/cm
2
Metallic titanium plate mechanical property of the present invention is higher, be conducive to the battery pile assembling, active layer has higher conductivity and high overpotential of hydrogen evolution, described activator is the mixture of zinc powder and electric conducting material, the adding of zinc powder is to guarantee that zinc is when deposition, electrode surface has had more nucleating point, thereby can save the deposition time of zinc, improve the deposition efficiency of zinc, the interpolation of electric conducting material not only can improve the activity of electrode, can also improve the conductivity of electrode, reduce the internal resistance of battery, improve battery efficiency; The additive effect mainly contains 3 points: the one, and it is deposited on zinc surface than the current potential height of zinc in charge and discharge process, can avoid the dissolving of zinc; The 2nd, have higher overpotential of hydrogen evolution, its existence can not promote hydrogen release, but may suppress hydrogen reaction; The 3rd, can make the deposition of zinc more even.
The present invention also provides a kind of preparation method of cerium zinc redox flow batteries composite negative plate, comprises as follows:
1) according to the weight fraction meter, binding agent, activator and additive are mixed, obtain the active layer slurry; Described binding agent is Kynoar (PVDF) or polytetrafluoroethylene (PTFE), activator is the mixture of zinc powder and electric conducting material, described electric conducting material is preferably selected from one or more in active carbon, Graphene or the acetylene black, more preferably active carbon or acetylene black, the ratio of weight and number of zinc powder and electric conducting material is preferably (1～5) in the described activator: 1, more preferably (1.5～3): 1; Additive is one or more in indium oxide, tin oxide, bismuth oxide, titanium oxide or the cerium oxide, described binding agent, activator and weight of additive portion rate are (5～15): (50～90): (5～50) are preferably (5～10): (60～80): (20～40);
2) the active layer slurry that step 1) is obtained is coated in a side of metallic titanium plate, obtains cerium zinc redox flow batteries composite negative plate behind the vacuum drying.
The described active layer slurry of step 1) of the present invention when binding agent is Kynoar, is added to binding agent, activator and additive in the organic solvent and dissolves, and obtains the active layer slurry, and described organic solvent is preferably the N-methyl pyrrolidone; When binding agent is polytetrafluoroethylene, directly ptfe emulsion, activator and additive are mixed, namely obtain the active layer slurry.
Surface activity layer of the present invention is preferably 50～300mg/cm in the amount of being coated with of pickling metal titanium plate
2, 100～200mg/cm more preferably
2, most preferably be 120～160mg/cm
2
The metallic titanium plate that the present invention will be coated with the active layer slurry carries out vacuum drying, and described bake out temperature is preferably 50～120 ℃, and the time is 5～24h, and vacuum degree is 1 * 10
-1～1 * 10
-3MPa, pressurize cools to room temperature then, obtains cerium zinc redox flow batteries composite negative plate.
Below in conjunction with specific embodiment the present invention is done further detailed description.
1) take by weighing binding agent Kynoar 0.1g, zinc powder 0.5g, activated carbon 0.4g, acetylene black 0.05g, each 0.1g of indium oxide, tin oxide and titanium oxide, the N-methyl pyrrolidone that adds 2000ml grinds dissolving, obtains the active layer slurry;
2) method of adopt brushing is coated in a side of metallic titanium plate uniformly with above-mentioned active layer slurry, the preparation active layer, and active layer is 140mg/cm in the amount of being coated with of pickling metal titanium plate
2, the metallic titanium plate that is coated with active layer being carried out the vacuum high-temperature oven dry handle, bake out temperature is 70 ℃, and the time is 15h, and the relative vacuum degree is 1 * 10
-1MPa, pressurize cools to room temperature, obtains cerium zinc redox flow batteries composite negative plate.As shown in Figure 1.
The cerium zinc redox flow batteries composite negative plate that embodiment 1 is obtained cooperates assembled battery with anodal graphite felt electrode, use the 40mA electric current to discharge and recharge, the cycle-index of battery reaches more than 200 times, battery average voltage efficient is 87.1%, average enclosed pasture efficient is 94.7%, and average energy efficient is 80.4%.
1) take by weighing binding agent Kynoar 0.08g, zinc powder 0.6g, activated carbon 0.15g, acetylene black 0.05g, each 0.1g of tin oxide, bismuth oxide, titanium oxide and cerium oxide, the N-methyl pyrrolidone that adds 2000ml grinds dissolving, obtains the active layer slurry;
2) method that adopts blade coating is coated in a side of metallic titanium plate uniformly with above-mentioned active layer slurry, the preparation active layer, and active layer is 135mg/cm in the amount of being coated with of pickling metal titanium plate
2, the metallic titanium plate that is coated with active layer being carried out vacuum drying handle, bake out temperature is 80 ℃, and the time is 10h, and the relative vacuum degree is 1 * 10
-3MPa, pressurize cools to room temperature, obtains cerium zinc redox flow batteries composite negative plate.
The cerium zinc redox flow batteries composite negative plate that embodiment 2 is obtained cooperates assembled battery with anodal graphite electrode, use the 80mA electric current to discharge and recharge, the cycle-index of battery reaches more than 100 times, battery average voltage efficient is 84.1%, average enclosed pasture efficient is 90.4%, and average energy efficient is 75.7%.
Embodiment 3
1) take by weighing binding agent Kynoar 0.1g, zinc powder 0.5g, activated carbon 0.1g, acetylene black 0.1g, each 0.1g of indium oxide, titanium oxide and cerium oxide, the N-methyl pyrrolidone that adds 2000ml grinds dissolving, obtains the active layer slurry;
2) method of adopt brushing is coated in a side of metallic titanium plate uniformly with above-mentioned active layer slurry, the preparation active layer, and active layer is 120mg/cm in the amount of being coated with of pickling metal titanium plate
2, the metallic titanium plate that is coated with active layer being carried out hyperthermia drying handle, bake out temperature is 80 ℃, and the time is 12h, and the relative vacuum degree is 1 * 10
-2MPa, pressurize cools to room temperature, obtains cerium zinc redox flow batteries composite negative plate.
The cerium zinc redox flow batteries composite negative plate that embodiment 3 is obtained cooperates assembled battery with anodal graphite felt electrode, use the 100mA electric current to carry out charge-discharge test, the cycle-index of battery reaches more than 550 times, battery average voltage efficient is 88.4%, average enclosed pasture efficient is 96.4%, and average energy efficient is 82.9%.
Embodiment 4
1) take by weighing zinc powder 0.45g, activated carbon 0.2g, each 0.1g of bismuth oxide, titanium oxide and cerium oxide adds the 2000ml ptfe emulsion, obtains the active layer slurry, and wherein to contain the polytetrafluoroethylene quality be 0.1g to ptfe emulsion;
2) method of adopt brushing is coated in a side of metallic titanium plate uniformly with above-mentioned active layer slurry, the preparation active layer, and active layer is 160mg/cm in the amount of being coated with of pickling metal titanium plate
2, the metallic titanium plate that is coated with active layer being carried out the vacuum high-temperature oven dry handle, bake out temperature is 120 ℃, and the time is 20h, and the relative vacuum degree is 1 * 10
-2MPa, pressurize cools to room temperature, obtains cerium zinc redox flow batteries composite negative plate.
The cerium zinc redox flow batteries composite negative plate that embodiment 4 is obtained cooperates assembled battery with anodal graphite felt electrode, use the 100mA electric current to carry out charge-discharge test, the cycle-index of battery reaches more than 170 times, battery average voltage efficient is 84.4%, average enclosed pasture efficient is 97.4%, and average energy efficient is 82.0%.
Embodiment 5
1) take by weighing zinc powder 0.5g, activated carbon 0.1g, each 0.1g of indium oxide, titanium oxide and cerium oxide adds the 1500ml ptfe emulsion and obtains the active layer slurry, and wherein to contain the polytetrafluoroethylene quality be 0.075g to ptfe emulsion;
2) method of adopt brushing is coated in a side of metallic titanium plate uniformly with above-mentioned active layer slurry, the preparation active layer, and active layer is 160mg/cm in the amount of being coated with of pickling metal titanium plate
2, the metallic titanium plate that is coated with active layer being carried out the constant-pressure and high-temperature oven dry handle, bake out temperature is 120 ℃, and the time is 24h, and pressurize cools to room temperature, obtains cerium zinc redox flow batteries composite negative plate.
The cerium zinc redox flow batteries composite negative plate that embodiment 5 is obtained cooperates assembled battery with anodal graphite felt electrode, use the 100mA electric current to carry out charge-discharge test, the cycle-index of battery reaches more than 120 times, battery average voltage efficient is 78.2%, average enclosed pasture efficient is 90.1%, and average energy efficient is 68.4%.
Embodiment 6
1) take by weighing binding agent Kynoar 0.05g, zinc powder 0.3g, activated carbon 0.15g, acetylene black 0.05g, each 0.02g of indium oxide, titanium oxide and cerium oxide, the N-methyl pyrrolidone that adds 800ml grinds dissolving, obtains the active layer slurry;
2) method that adopts blade coating is coated in a side of metallic titanium plate uniformly with above-mentioned active layer slurry, the preparation active layer, and active layer is 120mg/cm in the amount of being coated with of pickling metal titanium plate
2, the metallic titanium plate that is coated with active layer being carried out vacuum drying handle, bake out temperature is 80 ℃, and the time is 10h, and the relative vacuum degree is 1 * 10
-3MPa, pressurize cools to room temperature, obtains cerium zinc redox flow batteries composite negative plate.
The cerium zinc redox flow batteries composite negative plate that embodiment 6 is obtained cooperates assembled battery with anodal graphite electrode, use the 80mA electric current to discharge and recharge, the cycle-index of battery reaches more than 80 times, battery average voltage efficient is 78.6%, average enclosed pasture efficient is 93.4%, and average energy efficient is 72.7%.
Embodiment 7
1) take by weighing binding agent Kynoar 0.15g, zinc powder 0.5g, activated carbon 0.2g, acetylene black 0.2g, each 0.15g of indium oxide, titanium oxide and cerium oxide, the N-methyl pyrrolidone that adds 2200ml grinds dissolving, obtains the active layer slurry;
2) method that adopts blade coating is coated in a side of metallic titanium plate uniformly with above-mentioned active layer slurry, the preparation active layer, and active layer is 120mg/cm in the amount of being coated with of pickling metal titanium plate
2, the metallic titanium plate that is coated with active layer being carried out vacuum drying handle, bake out temperature is 80 ℃, and the time is 10h, and the relative vacuum degree is 1 * 10
-3MPa, pressurize cools to room temperature, obtains cerium zinc redox flow batteries composite negative plate.
The cerium zinc redox flow batteries composite negative plate that embodiment 7 is obtained cooperates assembled battery with anodal graphite electrode, use the 120mA electric current to discharge and recharge, the cycle-index of battery reaches more than 300 times, battery average voltage efficient is 87.2%, average enclosed pasture efficient is 85.2%, and average energy efficient is 73.8%.
The explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof.Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection range of claim of the present invention.
Claims (10)
1. cerium zinc redox flow batteries composite negative plate, it is characterized in that, this composite negative plate comprises metallic titanium plate and surface activity layer, described surface activity layer is made up of binding agent, activator and additive, described binding agent is Kynoar or polytetrafluoroethylene, activator is the mixture of zinc powder and electric conducting material, additive is one or more in indium oxide, tin oxide, bismuth oxide, titanium oxide or the cerium oxide, and described binding agent, activator and weight of additive portion rate are (5～15): (50～90): (5～50).
2. cerium zinc redox flow batteries composite negative plate according to claim 1 is characterized in that the ratio of weight and number of zinc powder and electric conducting material is (1～5) in the described activator: 1.
3. according to any one described cerium zinc redox flow batteries composite negative plate of claim 1-2, it is characterized in that described electric conducting material is selected from one or more in active carbon, Graphene or the acetylene black.
4. cerium zinc redox flow batteries composite negative plate according to claim 1 is characterized in that described binding agent, activator and weight of additive portion rate are (5～10): (60～80): (20～40).
5. cerium zinc redox flow batteries composite negative plate according to claim 1 is characterized in that described surface activity layer is 50～300mg/cm in the amount of being coated with of pickling metal titanium plate
2
6. the preparation method of cerium zinc redox flow batteries composite negative plate is characterized in that, comprises as follows:
1) according to the weight fraction meter, binding agent, activator and additive are mixed, obtain the active layer slurry; Described binding agent is Kynoar or polytetrafluoroethylene, activator is the mixture of zinc powder and electric conducting material, additive is one or more in indium oxide, tin oxide, bismuth oxide, titanium oxide or the cerium oxide, and described binding agent, activator and weight of additive portion rate are (5～15): (50～90): (5～50);
2) the active layer slurry that step 1) is obtained is coated in a side of metallic titanium plate, obtains cerium zinc redox flow batteries composite negative plate behind the vacuum drying.
7. the preparation method of cerium zinc redox flow batteries composite negative plate according to claim 6 is characterized in that, the ratio of weight and number of zinc powder and electric conducting material is (1～5) in the described activator: 1.
8. according to the preparation method of any one described cerium zinc redox flow batteries composite negative plate of claim 6-7, it is characterized in that described electric conducting material is selected from one or more in active carbon, Graphene or the acetylene black.
9. the preparation method of cerium zinc redox flow batteries composite negative plate according to claim 6 is characterized in that, described binding agent, activator and weight of additive portion rate are (5～10): (60～80): (20～40).
10. the preparation method of cerium zinc redox flow batteries composite negative plate according to claim 6 is characterized in that, described surface activity layer is 50～300mg/cm in the amount of being coated with of pickling metal titanium plate
2
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| CN108963241A (en) * | 2017-05-19 | 2018-12-07 | 苏州宝时得电动工具有限公司 | battery, battery pack and uninterruptible power supply |
| CN110364732A (en) * | 2018-04-10 | 2019-10-22 | 中国科学院上海硅酸盐研究所 | With the compound zinc load and preparation method and application of inorganic functional decorative layer in a kind of water system battery |
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| WO2023200652A1 (en) * | 2022-04-15 | 2023-10-19 | Washington University | Electrode-decoupled redox flow battery |
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| CN103259024B (en) | 2015-11-18 |
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