CN107895800B - Method for preparing electrodeposited cobalt activated carbon anode by one-step method - Google Patents
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- CN107895800B CN107895800B CN201711002357.3A CN201711002357A CN107895800B CN 107895800 B CN107895800 B CN 107895800B CN 201711002357 A CN201711002357 A CN 201711002357A CN 107895800 B CN107895800 B CN 107895800B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
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- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
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- H—ELECTRICITY
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- H01M4/8896—Pressing, rolling, calendering
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Abstract
The invention discloses a method for preparing an electrodeposited cobalt activated carbon anode by a one-step method, which comprises the following steps: (1) a reference electrode jack and a counter electrode jack are arranged on the top wall, foam nickel is arranged on a side hole of the deposition container, the side wall of the deposition container is provided with a side wall hole, and the foam nickel is connected with a nickel wire; adding an aqueous solution of cobalt nitrate to the deposition vessel; inserting a reference electrode into the reference electrode jack and inserting a counter electrode into the counter electrode jack; connecting a nickel wire, a reference electrode and a counter electrode with an electrochemical workstation, depositing, taking out the foam nickel deposited on one side, and naturally drying; (2) mixing activated carbon powder with absolute ethyl alcohol, ultrasonically stirring, dropwise adding 60% polytetrafluoroethylene emulsion, ultrasonically stirring and uniformly mixing, heating in a water bath to obtain a muddy mixture, paving the muddy mixture on one side where the foamed nickel is deposited, pressing by using a roller press, and naturally drying in the air to obtain the electrodeposited cobalt activated carbon anode. The method has the advantages of simple production process, high production efficiency, less required equipment and low cost.
Description
Technical Field
The invention belongs to the technical field of fuel cells, and particularly relates to a method for preparing an electrodeposited cobalt activated carbon anode by a one-step method.
Background
With the rapid increase of energy demand, global industrialization and increasingly serious environmental problems, the development of new energy is more and more urgent. Fuel cells have attracted attention in recent years as a typical, efficient, environmentally friendly alternative energy source. Carbohydrates are one of the hydrogen carriers of high energy density, with the potential to address the problem of hydrogen storage, with glucose being of particular interest. Glucose fuel cells are largely classified into three types: direct Glucose Alkaline Fuel Cells (DGAFC), microbial fuel cells (MGFC), glucose and Enzyme Glucose Fuel Cells (EGFC). Compared with MGFC and EGFC, DGAFC has the advantages of high stability, durability and simple structure. However, the development of DGAFC has been hampered by three major problems, cost, susceptibility to metal catalyst poisoning, and low reaction kinetics.
In the preparation of the electrode of the fuel cell, a metal catalyst is often doped to improve the performance of the electrode, but the manufacturing steps of the catalyst are complicated and difficult to control, and time and energy are consumed. Compared with a catalyst doping mode, the method has the advantages that by using an electrodeposition mode, the electrode can be soaked in a metal salt solution for electroplating, required metal is rapidly deposited on the electrode, and a deposition layer which is firmly and compactly combined with the electrode and can be used practically is obtained.
Since the discovery, the metal cobalt is widely applied to various electrochemical catalysis experiments due to the characteristics of low price, easy obtaining, corrosion resistance, strong magnetism, high melting point and the like. The smelting of cobalt basically adopts a wet smelting technology, and the electrodeposition of cobalt is an important part for extracting cobalt by the wet smelting. In the research of cobalt-containing electrodes, lead-based alloy anodes, graphite anodes or inert cobalt alloy anodes are frequently used in the past, but these anodes have the defects of high overpotential, easy corrosion, pollution to cathode products and the like. Therefore, research to reduce the possibility of cobalt corrosion and to produce high performance insoluble anodes has been a major concern for researchers.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for preparing an electrodeposited cobalt activated carbon anode by a one-step method.
The technical scheme of the invention is summarized as follows:
the method for preparing the electrodeposited cobalt activated carbon anode by the one-step method comprises the following steps:
(1) a reference electrode jack and a counter electrode jack are arranged on the top wall, foam nickel is arranged on a side hole of the deposition container, the side wall of the deposition container is provided with a side wall hole, and the foam nickel is connected with a nickel wire; adding 100 ml-500 ml of 0.05M-0.2M cobalt nitrate aqueous solution into the deposition container; inserting a reference electrode into the reference electrode jack and inserting a counter electrode into the counter electrode jack; connecting a nickel wire, a reference electrode and a counter electrode with an electrochemical workstation, enabling the deposition voltage to be-0.6V-1.2V, depositing for 600 s-1200 s, taking out the foamed nickel deposited on one side, and naturally drying;
(2) weighing 1-2 g of activated carbon powder, mixing with 20-40 ml of absolute ethyl alcohol, ultrasonically stirring for 25-30 min, dropwise adding 0.5-1 g of 60% polytetrafluoroethylene emulsion, ultrasonically stirring for 25-30 min, uniformly mixing, heating in a water bath at 70-90 ℃ for 20-30 min to obtain a mud-like mixture, paving on one side where foam nickel is deposited, pressing to the thickness of 4-6 mm by using a roller press, and naturally air-drying to obtain the electrodeposited cobalt activated carbon anode.
Preferably, the reference electrode is a saturated calomel electrode, and the counter electrode is a platinum wire.
The invention has the advantages that:
1. the method has simple production process, does not need expensive noble metal or electronic transfersome, has high production efficiency, needs less equipment and low cost, and is suitable for small-scale or large-scale production;
2. the method has the advantages that cobalt is electrodeposited on the foam nickel net with the three-dimensional structure, the characteristic of large surface area of the three-dimensional structure of the foam nickel can be fully exerted, the active carbon pressed on the foam nickel can be fully contacted with the deposited cobalt, and the conductivity and the catalysis performance of the electrode are enhanced.
3. The active carbon layer is rolled on one side of the deposited cobalt through a rolling method, so that the contact between the cobalt and electrolyte can be reduced to a certain extent, the possibility of corrosion of the cobalt is reduced, and the application life of the anode is prolonged.
4. The roll pressing method is used for preparing the fuel cell of the electrodeposited cobalt, is successfully applied to the glucose alkaline fuel cell and obtains good performance.
Drawings
FIG. 1 is a schematic diagram of an apparatus for preparing an electrodeposited cobalt activated carbon anode.
Figure 2 is a plot of anodic Linear Sweep Voltammetry (LSV) versus different cobalt nitrate deposition concentrations.
Fig. 3 is a plot of anodic Linear Sweep Voltammetry (LSV) versus time for cobalt nitrate deposition.
Fig. 4 is a plot of anodic Linear Sweep Voltammetry (LSV) versus different cobalt nitrate deposition voltages.
Detailed Description
The present invention will be further described with reference to the following specific examples.
The device for preparing the electrodeposited cobalt activated carbon anode comprises a deposition container 6, wherein a reference electrode jack 8 and a counter electrode jack 9 are arranged on the top wall of the deposition container 6, a side wall hole 11 is arranged on the side wall of the deposition container 6, a foamed nickel 5 is arranged on the side wall hole of the deposition container, the foamed nickel is connected with a nickel wire 7, the foamed nickel 5 is transversely pressed by a gasket 4, the gasket 4 is pressed by a gasket 3, a fixing plate 1 presses the gasket 3, a bolt 2 sequentially penetrates through small holes in the fixing plate, and the small holes in the gasket and the small holes in the deposition container are screwed by a nut 10.
The above apparatus is described in order to enable those skilled in the art to better understand the present invention, but not to limit the present invention in any way.
The reference electrode is a saturated calomel electrode, and the counter electrode is a platinum wire.
Example 1
The method for preparing the electrodeposited cobalt activated carbon anode by the one-step method comprises the following steps:
(1) a reference electrode jack and a counter electrode jack are arranged on the top wall, foam nickel is arranged on a side hole of the deposition container, the side wall of the deposition container is provided with a side wall hole, the diameter of the foam nickel is 3cm, and the foam nickel is connected with a nickel wire; adding 250ml of 0.1M cobalt nitrate aqueous solution into the deposition container; inserting a reference electrode into the reference electrode jack and inserting a counter electrode into the counter electrode jack; connecting a nickel wire, a reference electrode and a counter electrode with an electrochemical workstation, enabling the deposition voltage to be-0.8V, depositing for 800s, taking out the foamed nickel deposited on one side, and naturally drying for 12 h;
(2) weighing 1g of activated carbon powder, mixing with 20ml of absolute ethyl alcohol, ultrasonically stirring for 30min, dropwise adding 0.5g of 60% polytetrafluoroethylene emulsion, ultrasonically stirring for 30min, uniformly mixing, heating in a water bath at 80 ℃ for 20min to obtain a pasty mixture, paving the pasty mixture on one side where foam nickel is deposited, pressing the mixture to the thickness of 5mm by using a roller press, and naturally air-drying for 9h to obtain the electrodeposited cobalt activated carbon anode.
The electrodeposited cobalt activated carbon anode was prepared in the same manner as in this example except that the 0.1M aqueous cobalt nitrate solution of this example was replaced with a 0.05M aqueous cobalt nitrate solution.
The electrodeposited cobalt activated carbon anode was prepared in the same manner as in this example except that the 0.1M aqueous cobalt nitrate solution of this example was replaced with a 0.15M aqueous cobalt nitrate solution.
The 0.1M cobalt nitrate aqueous solution of this example was replaced with a 0.2M cobalt nitrate aqueous solution, and an electrodeposited cobalt activated carbon anode was prepared in the same manner as in this example.
Example 2
The test electrolyte was 7ml of 3M potassium hydroxide and 7ml of 3M glucose solution and the test was performed after 12h of equilibration of the solution. The LSV can reflect the current and thus the battery performance, the larger the current, the better the performance, and it is observed that under the condition of different concentrations of the deposition solution (0.05M, 0.1M, 0.15M and 0.2M cobalt nitrate aqueous solution), the current (performance) corresponding to the anode is arranged in the sequence of-0.4V of applied voltage: 0.1M >0.15M >0.2M >0.05M > blank anodes (i.e. control group, preparation process was the same as other group experiments except that foamed nickel was not subjected to cobalt electrodeposition), see FIG. 2.
Example 3
The method for preparing the electrodeposited cobalt activated carbon anode by the one-step method comprises the following steps:
(1) a reference electrode jack and a counter electrode jack are arranged on the top wall, foam nickel is arranged on a side hole of the deposition container, the side wall of the deposition container is provided with a side wall hole, the diameter of the foam nickel is 3cm, and the foam nickel is connected with a nickel wire; adding 100ml of 0.1M cobalt nitrate aqueous solution into the deposition container; inserting a reference electrode into the reference electrode jack and inserting a counter electrode into the counter electrode jack; connecting a nickel wire, a reference electrode and a counter electrode with an electrochemical workstation, enabling the deposition voltage to be-0.8V, depositing for 800s, taking out the foamed nickel deposited on one side, and naturally drying for 12 h;
(2) weighing 2g of activated carbon powder, mixing with 40ml of absolute ethyl alcohol, ultrasonically stirring for 30min, dropwise adding 1g of 60% polytetrafluoroethylene emulsion, ultrasonically stirring for 25min, uniformly mixing, heating in a water bath at 70 ℃ for 30min to obtain a muddy mixture, paving on one side of a foam nickel for deposition, pressing to the thickness of 4mm by using a roller press, and naturally air-drying for 6h to obtain the electrodeposited cobalt activated carbon anode.
The electrodeposition 600s was used in place of 800s in this example, and other examples were carried out to prepare an electrodeposited cobalt activated carbon anode.
The 1000s deposition was used instead of 800s in this example, and other steps were carried out in the same manner as in this example to prepare an electrodeposited cobalt activated carbon anode.
The electrodeposited cobalt activated carbon anode was prepared by using 1200s of deposition instead of 800s of this example, which is otherwise the same as this example.
Example 4
The test electrolyte was 7ml of 3M potassium hydroxide and 7ml of 3M glucose solution and the test was performed after 12h of equilibration of the solution. The LSV can reflect the current magnitude and thus the battery performance, the larger the current, the better the performance, and it can be observed that under different deposition time (600s, 800s, 1000s, 1200s) and at the applied voltage of-0.4V, the current magnitude (performance height) corresponding to the anode is arranged in the order: 800s >1000s >1200s >600s > blank anode, see fig. 3.
Example 5
The method for preparing the electrodeposited cobalt activated carbon anode by the one-step method comprises the following steps:
(1) a reference electrode jack and a counter electrode jack are arranged on the top wall, foam nickel is arranged on a side hole of the deposition container, the side wall of the deposition container is provided with a side wall hole, the diameter of the foam nickel is 3cm, and the foam nickel is connected with a nickel wire; adding 500ml of 0.1M cobalt nitrate aqueous solution into the deposition container; inserting a reference electrode into the reference electrode jack and inserting a counter electrode into the counter electrode jack; connecting a nickel wire, a reference electrode and a counter electrode with an electrochemical workstation, enabling the deposition voltage to be-0.8V, depositing for 800s, taking out the foamed nickel deposited on one side, and naturally drying for 12 h;
(2) weighing 1g of activated carbon powder, mixing with 20ml of absolute ethyl alcohol, ultrasonically stirring for 25min, dropwise adding 0.5g of 60% polytetrafluoroethylene emulsion, ultrasonically stirring for 30min, uniformly mixing, heating in a water bath at 90 ℃ for 20min to obtain a pasty mixture, flatly paving on one side where foam nickel is deposited, pressing to the thickness of 6mm by using a roller press, and naturally air-drying for 12h to obtain the electrodeposited cobalt activated carbon anode.
the-1.0V deposition is used for replacing the-0.8V deposition of the embodiment, and the electrodeposited cobalt activated carbon anode is prepared by the same method as the embodiment.
the-0.8V of the embodiment is replaced by-0.6V, and the electrodeposited cobalt activated carbon anode is prepared by the same method as the embodiment.
the-1.2V deposition is used for replacing the-0.8V deposition of the embodiment, and the electrodeposited cobalt activated carbon anode is prepared by the same method as the embodiment.
Example 6
The test electrolyte was 7ml of 3M potassium hydroxide and 7ml of 3M glucose solution and the test was performed after 12h of equilibration of the solution. LSV can reflect the current magnitude and thus the battery performance, the larger the current, the better the performance, and it can be observed that under different deposition voltages (-0.8V, -1.0V, -0.6V, -1.2V), the current magnitude (performance magnitude) corresponding to the anode is arranged in the order of-0.4V under the applied voltage: -0.8V > -0.6V > -1.0V > -1.2V > blank anode, see FIG. 4.
60% Polytetrafluoroethylene emulsion manufacturer: shanghai Hesen electric Co., Ltd.
Electrochemical workstation manufacturer and model: shanghai Chenghua instruments Co., Ltd., CHI-660E.
Claims (2)
1. The method for preparing the electrodeposited cobalt activated carbon anode by the one-step method is characterized by comprising the following steps of:
(1) a reference electrode jack and a counter electrode jack are arranged on the top wall, foam nickel is arranged on a side hole of the deposition container, the side wall of the deposition container is provided with a side wall hole, and the foam nickel is connected with a nickel wire; adding 100 ml-500 ml of 0.05M-0.2M cobalt nitrate aqueous solution into the deposition container; inserting a reference electrode into the reference electrode jack and inserting a counter electrode into the counter electrode jack; connecting a nickel wire, a reference electrode and a counter electrode with an electrochemical workstation, enabling the deposition voltage to be-0.6V-1.2V, depositing for 600 s-1200 s, taking out the foamed nickel deposited on one side, and naturally drying;
(2) weighing 1-2 g of activated carbon powder, mixing with 20-40 ml of absolute ethyl alcohol, ultrasonically stirring for 25-30 min, dropwise adding 0.5-1 g of 60% polytetrafluoroethylene emulsion, ultrasonically stirring for 25-30 min, uniformly mixing, heating in a water bath at 70-90 ℃ for 20-30 min to obtain a mud-like mixture, paving on one side where foam nickel is deposited, pressing to the thickness of 4-6 mm by using a roller press, and naturally air-drying to obtain the electrodeposited cobalt activated carbon anode.
2. The method of claim 1, wherein the reference electrode is a saturated calomel electrode and the counter electrode is a platinum wire.
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| CN104167556A (en) * | 2014-08-19 | 2014-11-26 | 刘昊 | Air electrode of lithium air battery, preparation method of air electrode and lithium air battery |
| CN105762371A (en) * | 2016-04-14 | 2016-07-13 | 天津大学 | Biomass alkaline fuel cell anode with electron transporter and preparation method |
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| CN103346332B (en) * | 2013-05-31 | 2016-01-27 | 哈尔滨工程大学 | The three-dimensional porous H of all-metal of carbon-free binder free 2o 2the preparation method of electro-oxidizing-catalyzing electrode |
| CN105070525A (en) * | 2015-05-06 | 2015-11-18 | 成都理工大学 | In-situ preparation of NiCo2Sx and NiCo2O4 on conductive substrate and application of NiCo2Sx and NiCo2O4 in energy storage device |
| CN105448528B (en) * | 2015-10-27 | 2019-05-28 | 梧州三和新材料科技有限公司 | A kind of preparation method of metal-graphite alkene composite porous electrode material |
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| CN104167556A (en) * | 2014-08-19 | 2014-11-26 | 刘昊 | Air electrode of lithium air battery, preparation method of air electrode and lithium air battery |
| CN105762371A (en) * | 2016-04-14 | 2016-07-13 | 天津大学 | Biomass alkaline fuel cell anode with electron transporter and preparation method |
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