CN114284489A - Preparation method of nickel-metal hydride battery positive electrode material, positive electrode piece and nickel-metal hydride battery - Google Patents
Preparation method of nickel-metal hydride battery positive electrode material, positive electrode piece and nickel-metal hydride battery Download PDFInfo
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Abstract
The invention provides a preparation method of a nickel-metal hydride battery anode material, which comprises the following steps: preparing a cobalt sulfate solution; adding the cobalt sulfate solution and spherical nickel hydroxide into a stirring kettle, and then adding a sodium hydroxide solution for full reaction to prepare spherical cobalt-coated nickel hydroxide coated with a mixed crystal layer of nickel hydroxide and cobalt hydroxide; washing and drying the spherical cobalt-coated nickel hydroxide; and pouring the dried spherical cobalt-coated nickel hydroxide into a sealed tank, and adding oxygen to oxidize and reduce the surface of the spherical cobalt-coated nickel hydroxide into black conductive powder to obtain the final cathode material. The preparation method of the nickel-metal hydride battery positive electrode material, the positive electrode piece and the nickel-metal hydride battery provided by the invention can form a cobalt-coated layer which is tightly combined and has good electrochemical properties, and the prepared final positive electrode material has low cost and excellent electrochemical performance.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to the technical field of batteries, in particular to a preparation method of a nickel-metal hydride battery positive electrode material, a positive electrode piece and a nickel-metal hydride battery.
[ background of the invention ]
The spherical nickel hydroxide is widely applied as the anode material of the nickel-hydrogen battery. The common nickel hydroxide is a semiconductor, has poor conductivity and low charge-discharge efficiency, and various additives are usually added to improve the conductivity among spherical nickel hydroxide particles, between an active substance and a conductive framework and between the active substance and an electrolyte and improve the performance of an electrode, wherein the cobalt additive is effective, and the addition of cobaltous oxide can increase the activity of the material.
In the prior nickel-hydrogen battery, when spherical nickel hydroxide is used as a positive active material, CoO and other conductive materials are doped in the nickel hydroxide active material mainly in a mechanical mixing mode, and due to the limitation of mechanical mixing process conditions, the nickel hydroxide active material and the conductive materials cannot be mixed uniformly, so that the improvement effect is limited.
In view of the above, it is actually necessary to provide a novel method for preparing a positive electrode material of a nickel-metal hydride battery, a positive electrode plate and a nickel-metal hydride battery to overcome the above-mentioned drawbacks.
[ summary of the invention ]
The invention aims to provide a preparation method of a nickel-metal hydride battery positive electrode material, a positive electrode piece and a nickel-metal hydride battery, which can form a cobalt-coated layer with tight combination and good electrochemical properties, and the prepared final positive electrode material has low cost and excellent electrochemical performance.
In order to achieve the purpose, the invention provides a preparation method of a nickel-metal hydride battery positive electrode material, which comprises the following steps: preparing a cobalt sulfate solution; adding the cobalt sulfate solution and spherical nickel hydroxide into a stirring kettle, and then adding a sodium hydroxide solution for full reaction to prepare spherical cobalt-coated nickel hydroxide coated with a mixed crystal layer of nickel hydroxide and cobalt hydroxide; washing and drying the spherical cobalt-coated nickel hydroxide; and pouring the dried spherical cobalt-coated nickel hydroxide into a sealed tank, and adding oxygen to oxidize and reduce the surface of the spherical cobalt-coated nickel hydroxide into black conductive powder to obtain the final cathode material.
In a preferred embodiment, the mass fraction of cobalt sulfate in the cobalt sulfate solution is 1.0-1.2%.
In a preferred embodiment, the sodium hydroxide solution has a sodium hydroxide mass fraction of 30%.
In a preferred embodiment, the content of cobalt hydroxide in the mixed-crystal layer increases in a direction away from the surface of the spherical nickel hydroxide.
In a preferred embodiment, the step of washing and drying the spherical cobalt-coated nickel hydroxide comprises: and carrying out solid-liquid separation on the suspension after reaction in the stirring kettle by multiple washing and filter pressing methods.
In a preferred embodiment, the step of washing and drying the spherical cobalt-coated nickel hydroxide comprises: and heating the spherical cobalt-coated nickel hydroxide to 150-160 ℃ under the protection of nitrogen to ensure that the water content of the spherical cobalt-coated nickel hydroxide is below 0.8 percent.
In a second aspect, the invention further provides a nickel-metal hydride battery positive electrode plate, which comprises a positive electrode substrate and a positive electrode material prepared by the preparation method of the nickel-metal hydride battery positive electrode material, wherein the positive electrode material is coated on the positive electrode substrate.
In a preferred embodiment, the positive electrode substrate is foamed nickel.
In a third aspect, the invention further provides a nickel-metal hydride battery, which comprises the positive pole piece of the nickel-metal hydride battery.
Compared with the prior art, the preparation method of the nickel-metal hydride battery positive electrode material, the positive electrode piece and the nickel-metal hydride battery provided by the invention have the advantages that the prepared cobalt sulfate solution and the spherical nickel hydroxide are added into the stirring kettle, the sodium hydroxide solution is added for full reaction to prepare the spherical cobalt-coated nickel hydroxide coated with the mixed crystal layer of the nickel hydroxide and the cobalt hydroxide, and then the spherical cobalt-coated nickel hydroxide is washed, dried and reduced by oxygen, so that the spherical nickel hydroxide is treated by an electrochemical process, a mixed crystal layer of the nickel hydroxide and the cobalt hydroxide is formed on the surface of the spherical nickel hydroxide and covers the surface of the nickel hydroxide to form a cobalt-coated layer which is tightly combined and has good electrochemical properties.
In order to make the aforementioned and other objects, features and advantages of the present invention comprehensible, preferred embodiments accompanied with figures are described in detail below.
[ description of the drawings ]
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is a flow chart of a method for preparing a positive electrode material of a nickel-metal hydride battery provided by the invention.
[ detailed description ] embodiments
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the present invention provides a method for preparing a positive electrode material of a nickel-metal hydride battery, which is used for preparing a positive electrode material with low cost and excellent performance. Specifically, the preparation method of the nickel-metal hydride battery positive electrode material comprises the following steps:
step S10: a cobalt sulfate solution was prepared. Specifically, cobalt sulfate and deionized water are mixed and stirred for 2-3 hours according to a proper proportion to prepare a cobalt sulfate solution. And the mass fraction of the cobalt sulfate in the cobalt sulfate solution is 1.0-1.2%.
Step S20: and adding the cobalt sulfate solution and the spherical nickel hydroxide into a stirring kettle, and then adding a sodium hydroxide solution for full reaction to prepare the spherical cobalt-coated nickel hydroxide coated with a mixed crystal layer of nickel hydroxide and cobalt hydroxide. Specifically, prepared cobalt sulfate solution and spherical nickel hydroxide are added into a synthesis stirring kettle according to a proper flow, sodium hydroxide solution is added for stirring and full reaction, heating is carried out for continuous reaction, a mixed crystal layer of nickel hydroxide and cobalt hydroxide is covered on the surface of the spherical nickel hydroxide, the content of cobalt in the formed mixed crystal layer is gradually increased from inside to outside due to the dominance of cobalt ions, the mixed crystal layer is in gradient distribution, namely the content of cobalt hydroxide in the mixed crystal layer is gradually increased in the direction far away from the surface of the spherical nickel hydroxide, and the outmost layer of the spherical nickel hydroxide is a cobalt-coated layer of cobalt hydroxide. It will be appreciated that the thickness of the cobalt cladding layer may be controlled by controlling the total amount of cobalt sulphate. In the present embodiment, the mass fraction of sodium hydroxide in the sodium hydroxide solution is 30%.
Step S30: and washing and drying the spherical cobalt-coated nickel hydroxide. Specifically, the suspension obtained after the reaction in the stirred tank of step S20 is subjected to multiple washing and filter pressing processes to perform solid-liquid separation. It is understood that after the reaction of step S20, the spherical cobalt-coated nickel hydroxide is suspended in the mother liquor and is obtained by filtration. And then heating the filtered spherical cobalt-coated nickel hydroxide to 150-160 ℃ under the protection of nitrogen, so that the water content of the spherical cobalt-coated nickel hydroxide is below 0.8 percent, and the aim of drying is fulfilled.
Step S40: and pouring the dried spherical cobalt-coated nickel hydroxide into a sealed tank, and adding oxygen to oxidize and reduce the surface of the spherical cobalt-coated nickel hydroxide into black conductive powder to obtain the final cathode material. Specifically, after the spherical cobalt-coated nickel hydroxide is subjected to oxygen reduction, the spherical cobalt-coated nickel hydroxide with a tightly combined coating layer and good electrical properties can be prepared.
Therefore, the preparation method of the nickel-hydrogen battery anode material provided by the invention is characterized in that the prepared cobalt sulfate solution and spherical nickel hydroxide are added into a stirring kettle, sodium hydroxide solution is added for full reaction to prepare spherical cobalt-coated nickel hydroxide coated with a mixed crystal layer of nickel hydroxide and cobalt hydroxide, and then the spherical cobalt-coated nickel hydroxide is washed, dried and reduced by oxygen, so that the spherical nickel hydroxide is processed by an electrochemical process to form a mixed crystal layer of nickel hydroxide and cobalt hydroxide on the surface of the spherical nickel hydroxide and cover the mixed crystal layer on the surface of the nickel hydroxide to form a cobalt-coated layer which is tightly combined and has good electrochemical properties.
The following examples and comparative examples were used to test the spherical cobalt-coated nickel hydroxide positive electrode material prepared by the method for preparing a positive electrode material for a nickel-metal hydride battery provided by the present invention:
example (b):
the positive electrode substrate adopts foamed nickel, the positive electrode active material comprises 99g of spherical cobalt-coated nickel hydroxide and 1g of ytterbium oxide, the negative electrode substrate adopts a copper mesh, the negative electrode hydrogen storage alloy powder comprises 54.0g of nickel, 2.0g of cobalt, 540g of manganese, 1.0g of aluminum and 0.5g of additive, and the additive is a mixture of cerium and praseodymium; the electrolyte is a mixed solution formed by 5% KOH solution, 28% NaOH solution and 1% NaLiOH solution.
The manufacturing method of the positive plate comprises the following steps: a1, preparing a positive electrode material: uniformly mixing the positive electrode active material and the additive to prepare a positive electrode material; a2, coating of positive electrode material: uniformly coating the positive electrode material prepared in the step a1 on a positive electrode substrate; a3, positive electrode tabletting: and c, pressing the positive electrode substrate coated with the positive electrode material in the step a2 to obtain the positive electrode sheet. Specifically, the size of the positive electrode plate is as follows: 41 x 95 x 0.65 mm.
The preparation of the negative plate comprises the following steps: b1, coating of negative electrode material: uniformly coating the alloy powder on a copper mesh; b2, negative electrode pellet: and c, pressing the copper mesh coated with the alloy powder in the step b1 to obtain the negative plate. Specifically, the size of the negative electrode sheet is as follows: 41 x 128 x 0.28 mm.
Dissolving an alkaline electrolyte in a solvent to prepare an electrolyte; and injecting the prepared electrolyte into the shell, wherein the using amount of the electrolyte is 2.5-2.6 g, and thus obtaining the nickel-metal hydride battery. And finally, carrying out charge and discharge tests on the nickel-metal hydride battery according to a formation pre-charging process, wherein the specific charge and discharge process comprises the following steps: charging at 0.02C for 5 hours and charging at 0.1C for 6 hours; discharging the battery to 1.0V at 0.2C, charging the battery for 1.2 hours at 0.5C, and discharging and grading the battery at 1C to obtain the capacity change of the battery.
Comparative example:
the positive electrode substrate adopts foamed nickel, the positive electrode active material is 93g of spherical nickel hydroxide, 6g of cobaltous hydroxide and 1g of ytterbium oxide, the negative electrode substrate adopts a copper mesh, the negative electrode hydrogen storage alloy powder consists of 54.0g of nickel, 2.0g of cobalt, 540g of manganese, 1.0g of aluminum and 0.5g of additive, and the additive is a mixture of cerium and praseodymium; the electrolyte is a mixed solution formed by 5% KOH solution, 28% NaOH solution and 1% NaLiOH solution.
The manufacturing method of the positive plate comprises the following steps: a1, preparing a positive electrode material: uniformly mixing a positive electrode active material (namely spherical cobalt-coated nickel hydroxide) and an additive to prepare a positive electrode material; a2, coating of positive electrode material: uniformly coating the positive electrode material prepared in the step a1 on a positive electrode substrate; a3, positive electrode tabletting: and c, pressing the positive electrode substrate coated with the positive electrode material in the step a2 to obtain the positive electrode sheet. Specifically, the size of the positive electrode plate is as follows: 41 x 95 x 0.65 mm.
The preparation of the negative plate comprises the following steps: b1, coating of negative electrode material: uniformly coating the alloy powder on a copper mesh; b2, negative electrode pellet: and c, pressing the copper mesh coated with the alloy powder in the step b1 to obtain the negative plate. Specifically, the size of the negative electrode sheet is as follows: 41 x 128 x 0.28 mm.
Dissolving an alkaline electrolyte in a solvent to prepare an electrolyte; and injecting the prepared electrolyte into the shell, wherein the using amount of the electrolyte is 2.5-2.6 g, and thus obtaining the nickel-metal hydride battery. And finally, carrying out charge and discharge tests on the nickel-metal hydride battery according to a formation pre-charging process, wherein the specific charge and discharge process comprises the following steps: charging at 0.02C for 5 hours and charging at 0.1C for 6 hours; discharging the battery to 1.0V at 0.2C, charging the battery for 1.2 hours at 0.5C, and discharging and grading the battery at 1C to obtain the capacity change of the battery.
The experimental data for the above examples and comparative examples are as follows:
under normal temperature storage, the capacity retention rate of the hydrogen-nickel battery prepared in the embodiment after one year is 80-82%, and the capacity retention rate of the hydrogen-nickel battery prepared in the comparative example after one year is 50-55%; and (3) capacity recovery: the capacity recovery rate of the nickel-hydrogen battery prepared in the example after one year is 90-95%, and the capacity recovery rate of the nickel-hydrogen battery prepared in the comparative example after one year is 70-85%. Therefore, in the embodiment, the spherical cobalt-coated nickel hydroxide prepared by the method is used as the positive electrode material, and the capacity retention rate and the capacity recovery rate of the battery are obviously superior to those of the comparative example.
The cycle life of the nickel-hydrogen battery prepared in the example is reduced to 80% at the current of 1C for 400 weeks, and the cycle life of the nickel-hydrogen battery prepared in the comparative example is reduced to 80% at the current of 1C for 250 weeks; the cycle life of the nickel-hydrogen cell prepared in the example was reduced to 80% at a current of 5C at 300 weeks, while the cycle life of the nickel-hydrogen cell prepared in the comparative example was reduced to 80% at a current of 5C at 150 weeks. Therefore, no matter under the current of 1C or 5C, the spherical cobalt-coated nickel hydroxide prepared by the invention is used as the cathode material in the embodiment, and the cycle life performance of the battery is obviously superior to that of the comparative example.
Furthermore, the cost of the prepared nickel-metal hydride battery is saved by 0.20 yuan/ton compared with the traditional battery by taking 38 ten thousand/ton of cobaltous oxide and 15 ten thousand yuan/ton of nickel as the anode materials in the embodiment, and the anode material prepared by the preparation method of the anode material of the nickel-metal hydride battery provided by the invention has lower cost.
The invention also provides a nickel-metal hydride battery positive pole piece which comprises a positive pole substrate and the positive pole material prepared by the preparation method of the nickel-metal hydride battery positive pole material in any embodiment, wherein the positive pole material is coated on the positive pole substrate. Specifically, the positive electrode substrate is foamed nickel.
The invention also provides a nickel-metal hydride battery, which comprises the positive pole piece of the nickel-metal hydride battery in any one of the embodiments.
It can be understood that all embodiments of the method for preparing the nickel-metal hydride battery positive electrode material provided by the invention are applicable to the nickel-metal hydride battery positive electrode piece and the nickel-metal hydride battery provided by the invention, and can achieve the same or similar technical effects.
In summary, according to the preparation method of the nickel-metal hydride battery positive electrode material, the positive electrode plate and the nickel-metal hydride battery provided by the invention, the prepared cobalt sulfate solution and the spherical nickel hydroxide are added into the stirring kettle, the sodium hydroxide solution is added for sufficient reaction to prepare the spherical cobalt-coated nickel hydroxide coated with the mixed crystal layer of the nickel hydroxide and the cobalt hydroxide, and then the spherical cobalt-coated nickel hydroxide is washed, dried and reduced by oxygen, so that the spherical nickel hydroxide is treated by the electrochemical process, a nickel hydroxide and cobalt hydroxide mixed crystal layer is formed on the surface of the spherical nickel hydroxide and covers the surface of the nickel hydroxide to form a cobalt-coated layer which is tightly combined and has good electrochemical properties, and the prepared final positive electrode material has low cost and excellent electrochemical properties.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present specification and drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (9)
1. A preparation method of a nickel-metal hydride battery positive electrode material is characterized by comprising the following steps:
preparing a cobalt sulfate solution;
adding the cobalt sulfate solution and spherical nickel hydroxide into a stirring kettle, and then adding a sodium hydroxide solution for full reaction to prepare spherical cobalt-coated nickel hydroxide coated with a mixed crystal layer of nickel hydroxide and cobalt hydroxide;
washing and drying the spherical cobalt-coated nickel hydroxide;
and pouring the dried spherical cobalt-coated nickel hydroxide into a sealed tank, and adding oxygen to oxidize and reduce the surface of the spherical cobalt-coated nickel hydroxide into black conductive powder to obtain the final cathode material.
2. The method for preparing the positive electrode material for the nickel-metal hydride battery as claimed in claim 1, wherein the mass fraction of cobalt sulfate in the cobalt sulfate solution is 1.0-1.2%.
3. The method for producing a positive electrode material for a nickel-metal hydride battery according to claim 1, wherein the mass fraction of sodium hydroxide in the sodium hydroxide solution is 30%.
4. The method for producing a positive electrode material for a nickel-metal hydride battery according to claim 1, wherein the content of cobalt hydroxide in the mixed crystal layer increases in a direction away from the surface of the spherical nickel hydroxide.
5. The method of claim 1, wherein the step of washing and drying the spherical cobalt-coated nickel hydroxide comprises:
and carrying out solid-liquid separation on the suspension after reaction in the stirring kettle by multiple washing and filter pressing methods.
6. The method of claim 1, wherein the step of washing and drying the spherical cobalt-coated nickel hydroxide comprises:
and heating the spherical cobalt-coated nickel hydroxide to 150-160 ℃ under the protection of nitrogen to ensure that the water content of the spherical cobalt-coated nickel hydroxide is below 0.8 percent.
7. A positive pole piece of a nickel-metal hydride battery is characterized by comprising a positive pole substrate and a positive pole material prepared by the preparation method of the positive pole material of the nickel-metal hydride battery as claimed in any one of claims 1 to 6, wherein the positive pole material is coated on the positive pole substrate.
8. The positive electrode sheet of the nickel-metal hydride battery as claimed in claim 7, wherein the positive electrode substrate is foamed nickel.
9. A nickel-metal hydride battery comprising the positive electrode tab of claim 8 or 9.
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