CN114029481A - Coating method of rare earth hydrogen storage alloy powder for carbon nanotube coated nickel-hydrogen battery cathode - Google Patents
Coating method of rare earth hydrogen storage alloy powder for carbon nanotube coated nickel-hydrogen battery cathode Download PDFInfo
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Abstract
The invention discloses a coating method of rare earth hydrogen storage alloy powder for a carbon nanotube coated nickel-hydrogen battery cathode, and relates to the technical field of nickel-hydrogen battery cathode materials. The invention adopts an ultrasonic stirring method to coat the surface of the rare earth hydrogen storage material with the polyethyleneimine and the carbon nano tube to directly obtain the carbon nano tube coated and modified nickel-hydrogen battery cathode materialAnd (5) feeding. The method obtains LaY uniformly coated with carbon nanotubes2Ni9.7Mn0.5Al0.3(A2B7Type) rare earth hydrogen storage materials show better cycle performance than uncoated modified materials under high rate current density of 5C discharge rate, play an important role in stabilizing the crystal structure of negative electrode materials and greatly improve the electrochemical performance of the negative electrode materials.
Description
Technical Field
The invention belongs to the field of nickel-hydrogen battery cathode materials, and particularly relates to a coating method of rare earth hydrogen storage alloy powder for a carbon nanotube coated nickel-hydrogen battery cathode.
Background
Nickel-hydrogen battery is a short name for nickel-metal hydride battery. Nickel-hydrogen battery negative electrode materials generally include: hydrogen storage alloy powder as active material, conductive carbon black as three agents, carbonyl nickel powder, glue material as adhesive, and foam nickel or nickel-plated steel band as current collector or negative electrode skeleton of current collector, wherein:
hydrogen absorbing alloy powder as active material, most commercially used is AB5Type, in recent years, due to A2B7The hydrogen storage alloy powder has high capacity, and can be used in batteries or partially used in the market2B7The amount of hydrogen absorbing alloy powder is also increasing.
The conductive carbon black and the carbonyl nickel powder as the three agents are used for adding the conductive carbon black and the carbonyl nickel powder into a wet-process slurry negative electrode of the nickel-hydrogen battery as a conductive agent, a yielding agent and a dispersing agent. Those skilled in the art are well aware of: acetylene black produced from industrial acetylene has poor conductivity and needs to be processed into conductive carbon black for use in batteries. Acetylene black is generally chemically treated with inexpensive polypyrrole or the like industrially, whereby industrial conductive carbon black useful for batteries is obtained.
In recent years, "nano-thermal" and "graphene thermal" have stirred the traditional battery industry, and researchers have found that carbon nanotubes with acceptable price have better efficacy as a "conductive agent" and a "yielding agent" than traditional conductive carbon black in a nickel-hydrogen battery negative plate. However, when the carbon nanotubes are used in the battery pole piece, if the carbon nanotubes are not subjected to the conductive treatment like acetylene black, the carbon nanotubes are not well wetted with components such as hydrogen storage alloy powder and glue, and the carbon nanotubes are difficult to play a role of a uniform dispersing agent.
The invention patent with application number 201610850225.5, which is disclosed by the Chinese patent office in 2018, 4 and 3, is a nickel-metal hydride battery capable of being used in extremely cold environment and a preparation method thereof, and has good effect, but has the following defects: a is to be2B7The alloy powder and the carbon nano tube are forcibly processed into the pole piece, the surface binding property is poor, the wettability is poor, the powder falling phenomenon is obvious, and the processing technology and the service life of the battery are seriously influenced.
On the contrary, the patent of 'a preparation method of a carbon nano composite nickel-hydrogen power battery negative pole piece and application thereof' applied by the Chinese patent office with the application number of 200710030263.7 does not avoid the problem that the surface of the carbon nano tube is not wetted with components such as hydrogen storage alloy powder, glue and the like, and the inventor adopts mixed acid in strong acid to coarsen or sensitize the surface of the carbon nano tube and increase the wettability of the carbon nano tube on the pole piece, but the application is restricted by negative effects such as environmental unfriendliness caused by the treatment of the mixed acid.
At present, for the use of carbon nanotubes in the field of nickel-hydrogen batteries, the existing technical methods are not mature, and new technologies and new methods are needed to improve technical support, thereby promoting the development of the nickel-hydrogen battery industry.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a coating method of rare earth hydrogen storage alloy powder for a carbon nanotube coated nickel-hydrogen battery cathode, and A obtained by the coating method2B7The rare earth hydrogen storage negative electrode material has excellent cycling stability and rate capability.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:
the invention provides a coating method of rare earth hydrogen storage alloy powder for a cathode of a carbon nanotube coated nickel-hydrogen battery, which comprises the following steps:
the method comprises the following steps: a is to be2B7Putting the type rare earth hydrogen storage material into a polyethyleneimine water solution, and stirring and ultrasonically treating to obtain a mixture;
step two: filtering the mixture obtained in the step one, removing redundant polyethyleneimine, washing, and dispersing into deionized water to obtain polyethyleneimine-coated A2B7A type rare earth hydrogen storage material;
step three: coating the polyethyleneimine A obtained in the step two2B7And putting the type rare earth hydrogen storage material into the uniformly dispersed carbon nano tube aqueous solution, stirring, mixing, filtering, and drying in vacuum to obtain the rare earth hydrogen storage alloy powder for the cathode of the nickel-hydrogen battery coated with the carbon nano tube.
Preferably, A in the first step2B7LaY A rare earth hydrogen storage material2Ni9.7Mn0.5Al0.3。
Preferably, the polyethyleneimine and A in the first step2B7The mass ratio of the rare earth hydrogen storage material is (1+ a):1, wherein a is 0-0.5, and the volume of the polyethyleneimine water solution is 50-200 mL.
Preferably, the time of the ultrasound in the step one is 0.5-2 h.
Preferably, the solution washed in the second step is a deionized water solution, and the volume of the solution dispersed in the deionized water solution is 50-200 mL.
Preferably, the length of the carbon nano tube in the third step is 0.5-5 μm, the concentration of the aqueous solution is 0.02-0.05 mg/mL, and the total amount of the solution is 200mL of deionized water solution.
Preferably, the stirring time of the third step is 5-24 h.
Preferably, the temperature of vacuum drying in the third step is 40-60 ℃, and the heat preservation time is 8-15 h.
The invention has the advantages of
The invention provides a coating method of rare earth hydrogen storage alloy powder for a cathode of a nickel-hydrogen battery coated with a carbon nanotube, which is directly obtained by coating polyethyleneimine and the carbon nanotube on the surface of a rare earth hydrogen storage material through ultrasonic stirring. Meanwhile, the method for coating and modifying the surface of the alloy can improve the protective capacity of the surface of the alloy, is beneficial to reducing the oxidation speed, prolonging the service life of the alloy, improving the electrocatalytic activity and the corrosion resistance, and effectively improving the electrochemical performance of the battery, especially the high-rate discharge performance.
The experimental results show that: the rare earth hydrogen storage alloy powder for the cathode of the nickel-hydrogen battery coated by the carbon nano tube obtained by the method keeps the appearance of the alloy well, and the carbon nano tube is uniformly coated on the surface of the alloy. Example 1A prepared by the method described above2B7The surface of the rare earth hydrogen storage material is coated with polyethyleneimine, and the discharge capacity of the negative electrode material of 0.025mg/mL carbon nano tube after circulating for 300 circles under the voltage range of 0.8-16V and the current density of 1C is 269.1mAh g-1. The discharge specific capacity is 267.2mAh g under the high-rate current density of 5C discharge rate-1Exhibit better cycling performance than the uncoated modified material.
Therefore, the rare earth hydrogen storage alloy powder for the cathode of the nickel-hydrogen battery coated by the carbon nanotube prepared by the method has excellent charge-discharge cycle stability and high-rate discharge performance, can be widely applied to cathode materials of the nickel-hydrogen battery, and is suitable for popularization and application.
Drawings
FIG. 1 is SEM pictures of materials obtained in example 1 of the present invention and comparative example 1. Wherein FIG. 1a isLaY of uncoated carbon nanotubes2Ni9.7Mn0.5Al0.3Rare earth hydrogen storage material, FIG. 1b is LaY coated with carbon nanotubes2Ni9.7Mn0.5Al0.3Rare earth hydrogen storage materials.
FIG. 2 is a discharge curve diagram of the cycle of using sintered alpha-nickel hydroxide as the positive electrode, using a sulfonated polypropylene graft membrane as the separator, activating 10 cycles at a current density of 0.2C and a current density of 1C in a voltage range of 0.8-1.6V, in the case of preparing the negative electrode by mixing the materials obtained in example 1 and comparative example 1 of the present invention with nickel carbonyl powder.
FIG. 3 is a graph showing rate discharge characteristics of batteries assembled from the materials obtained in example 1 of the present invention and comparative example 1.
Detailed Description
The invention provides a coating method of rare earth hydrogen storage alloy powder for a cathode of a carbon nanotube coated nickel-hydrogen battery, which comprises the following steps:
the method comprises the following steps: a is to be2B7Putting the type rare earth hydrogen storage material into a polyethyleneimine water solution, and stirring and ultrasonically treating to obtain a mixture;
a is described2B7The rare earth hydrogen storage material is preferably LaY2Ni9.7Mn0.5Al0.3Grinding, and sieving with 200 mesh sieve;
the polyethyleneimine source is commercially available;
the polyethyleneimine and A2B7The mass ratio of the rare earth hydrogen storage material is preferably (1+ a):1, wherein a is 0-0.5, the volume of water in the polyethyleneimine water solution is 50-200 mL, and the ultrasonic time is preferably 0.5-2 h, more preferably 1 h;
step two: filtering the mixture obtained in the step one, removing redundant polyethyleneimine, washing, and dispersing into deionized water to obtain polyethyleneimine-coated A2B7A type rare earth hydrogen storage material;
the washed solution is a deionized water solution, and the volume of the solution dispersed into the deionized water solution is 50-200 mL.
Step three: coating the polyethyleneimine A obtained in the step two2B7And putting the type rare earth hydrogen storage material into the uniformly dispersed carbon nano tube aqueous solution, stirring, mixing, filtering, and drying in vacuum to obtain the carbon nano tube coated and modified rare earth hydrogen storage material for the nickel-metal hydride battery cathode.
The length of the carbon nano tube is preferably 0.5-5 mm, the concentration of the water solution is 0.02-0.05 mg/mL, the total amount of the solution is 200mL of deionized water solution, the carbon nano tube water solution is obtained by ultrasonically dispersing the carbon nano tube in water, the ultrasonic dispersion time is preferably 1-3 h, and the ultrasonic temperature is not higher than 30 ℃. The stirring time is preferably 5-24 h; the temperature of the vacuum drying is preferably 40-60 ℃, and the heat preservation time is preferably 8-15 h.
Other aspects, features and advantages of the present invention will become apparent from the following detailed description, which, when taken in conjunction with the drawings, illustrate by way of example the principles of the invention. But this example does not limit the invention.
Example 1
1) LaY will be mixed2Ni9.7Mn0.5Al0.3Fully grinding the rare earth hydrogen storage material in a mortar, sieving with a 200-mesh sieve, weighing 2g of polyethyleneimine, dissolving in 100mL of deionized water solution, and adding 1.5g of LaY2Ni9.7Mn0.5Al0.3Ultrasonically stirring the rare earth hydrogen storage material for 1h to obtain a mixture;
2) leaching and washing the uniformly mixed raw materials to remove redundant polyethyleneimine, and dispersing the cleaned raw materials into deionized water to obtain polyethyleneimine-coated A2B7A type rare earth hydrogen storage material;
3) weighing 5mg of commercially available carbon nano tube, dissolving the commercially available carbon nano tube in 200mL of deionized water solution, and performing ultrasonic treatment for 2h to obtain polyethyleneimine-coated A2B7Dispersing the type rare earth hydrogen storage material in a carbon nano tube solution with good ultrasonic, stirring for 12h, filtering, washing, drying in a vacuum drying oven at 60 ℃ for 10h, cooling, and obtaining the modified A for the nickel-metal hydride battery cathode coated with the carbon nano tube2B7Rare earth hydrogen storage material.
Carbon obtained in example 1Nanotube coating modified A2B7The SEM test result of the rare earth hydrogen storage material is shown in figure 1b, and the surface of the rare earth hydrogen storage material is uniformly coated with a carbon nanotube material.
Comparative example 1
LaY will be mixed2Ni9.7Mn0.5Al0.3The rare earth hydrogen storage material is fully ground in a mortar and sieved by a 200-mesh sieve.
LaY from comparative example 12Ni9.7Mn0.5Al0.3The SEM test result of the rare earth hydrogen storage material is shown in figure 1a, and the surface is smoother.
Application example 1
LaY prepared in example 1 and comparative example 12Ni9.7Mn0.5Al0.3The electrochemical performance of the rare earth hydrogen storage material is tested. The method comprises the following specific steps:
mixing a negative electrode active material and carbonyl nickel powder according to the mass ratio of 1:5, pressing a sheet under 15MPa, wrapping with foamed nickel, and welding a tab. The loading of the active material of the obtained pole piece is about 150 mg. The positive electrode adopts sintered a-nickel hydroxide, a polypropylene graft membrane subjected to sulfonation treatment is used as a diaphragm, the electrolyte is 6M KOH solution, and an electrochemical performance test is performed in a voltage range of 0.8-1.6V.
LaY obtained in example 1 and comparative example 12Ni9.7Mn0.5Al0.3The activation of the battery prepared by the rare earth hydrogen storage material in the voltage range of 0.8-1.6V under the current density of 0.2C and the discharge cycle performance of the battery under the current density of 1C are shown in figure 2, and can be seen: LaY2Ni9.7Mn0.5Al0.3The maximum discharge capacity of the rare earth hydrogen storage material under the current density of 0.2C is 384.2mAh g-1LaY coated with carbon nanotubes2Ni9.7Mn0.5Al0.3The maximum discharge capacity of the rare earth hydrogen storage material under the current density of 0.2C is 394.1mAh g-1After 300 cycles, LaY2Ni9.7Mn0.5Al0.3Rare earth hydrogen storage material and carbon nanotube coated LaY2Ni9.7Mn0.5Al0.3The discharge capacity of the rare earth hydrogen storage material is 249.4mAh g-1And 269.1mAh g-1。
LaY obtained in example 1 and comparative example 12Ni9.7Mn0.5Al0.3The multiplying power discharge cycle performance of the battery prepared by the rare earth hydrogen storage material under the current density of 0.2C, 0.5C, 1C, 2C and 5C in the voltage interval of 0.8-1.6V is shown in figure 3, and LaY can be seen2Ni9.7Mn0.5Al0.3The discharge capacities of the rare earth hydrogen storage material at current densities of 0.2C, 0.5C, 1C, 2C and 5C are 380 mAh g, 371.7 mAh, 358.8 mAh, 325.1 mAh and 64mAh g respectively-1Carbon nanotube coated LaY2Ni9.7Mn0.5Al0.3The discharge capacity of the rare earth hydrogen storage material at the current density of 0.2C, 0.5C, 1C, 2C and 5C is 386.6, 375.7, 367, 348.2 and 267.2mAh g respectively-1。
The above results show that LaY coated with carbon nanotubes2Ni9.7Mn0.5Al0.3The cycle stability and the large-current discharge performance of the rare earth hydrogen storage material are obviously superior to those of uncoated LaY2Ni9.7Mn0.5Al0.3Rare earth hydrogen storage material, which fully proves that the carbon nano tube coating is well stabilized LaY2Ni9.7Mn0.5Al0.3The surface structure stability of the rare earth hydrogen storage material improves the electrode activity and the corrosion resistance, thereby improving LaY under high current density2Ni9.7Mn0.5Al0.3The discharge cycle performance of the rare earth hydrogen storage material, therefore, the invention has more commercial popularization superiority.
The present invention includes, but is not limited to, the above embodiments, and any equivalent substitutions or partial modifications made under the principle of the spirit of the present invention are considered to be within the scope of the present invention.
Claims (8)
1. A coating method of rare earth hydrogen storage alloy powder for a carbon nanotube coated nickel-hydrogen battery cathode is characterized by comprising the following steps:
the method comprises the following steps: a is to be2B7Putting the type rare earth hydrogen storage material into a polyethyleneimine water solution, and stirring and ultrasonically treating to obtain a mixture;
step two: filtering the mixture obtained in the step one, removing redundant polyethyleneimine, washing, and dispersing into deionized water to obtain polyethyleneimine-coated A2B7A type rare earth hydrogen storage material;
step three: coating the polyethyleneimine A obtained in the step two2B7And putting the type rare earth hydrogen storage material into the uniformly dispersed carbon nano tube aqueous solution, stirring, mixing, filtering, and drying in vacuum to obtain the rare earth hydrogen storage alloy powder for the cathode of the nickel-hydrogen battery coated with the carbon nano tube.
2. The method for coating a rare earth hydrogen storage alloy powder for a carbon nanotube-coated nickel-hydrogen battery negative electrode according to claim 1, wherein the step A in the step one2B7LaY A rare earth hydrogen storage material2Ni9.7Mn0.5Al0.3。
3. The method for coating the rare earth hydrogen storage alloy powder for the cathode of the carbon nanotube-coated nickel-hydrogen battery according to claim 1, wherein the polyethyleneimine and A in the step one2B7The mass ratio of the rare earth hydrogen storage material is (1+ a):1, wherein a is 0-0.5, and the volume of the polyethyleneimine water solution is 50-200 mL.
4. The method for coating the rare earth hydrogen storage alloy powder for the carbon nanotube-coated nickel-hydrogen battery cathode according to claim 1, wherein the ultrasonic time in the first step is 0.5-2 h.
5. The method for coating the rare earth hydrogen storage alloy powder for the carbon nanotube-coated nickel-hydrogen battery cathode according to claim 1, wherein the solution washed in the second step is a deionized water solution, and the volume of the deionized water solution dispersed in the deionized water solution is 50-200 mL.
6. The method for coating the rare earth hydrogen storage alloy powder for the carbon nanotube-coated nickel-hydrogen battery cathode according to claim 1, wherein the length of the carbon nanotube in the third step is 0.5-5 μm, the concentration of the aqueous solution is 0.02-0.05 mg/mL, and the total amount of the solution is 200mL of deionized water solution.
7. The method for coating the rare earth hydrogen storage alloy powder for the carbon nanotube-coated nickel-hydrogen battery negative electrode according to claim 1, wherein the stirring time in the third step is 5-24 h.
8. The coating method of the rare earth hydrogen storage alloy powder for the carbon nanotube-coated nickel-hydrogen battery cathode according to claim 1, wherein the temperature of vacuum drying in the third step is 40-60 ℃, and the heat preservation time is 8-15 h.
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| CN113540427A (en) * | 2021-03-31 | 2021-10-22 | 有研工程技术研究院有限公司 | Preparation method of carbon-coated hydrogen storage alloy |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20100092868A1 (en) * | 2008-10-14 | 2010-04-15 | Hyung-Sun Kim | Carbon nanotube-coated silicon/metal composite particle, preparation method thereof, and anode for secondary battery and secondary battery using the same |
| US20110171531A1 (en) * | 2009-09-08 | 2011-07-14 | Northwestern University | Multifunctional Nanocomposites of Carbon Nanotubes and Nanoparticles Formed Via Vacuum Filtration |
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