CN113328060A - Method for preparing flexible electrode on nano needle cone nickel substrate - Google Patents
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- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
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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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- 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
- C25D3/22—Electroplating: Baths therefor from solutions of zinc
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- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/10—Electroplating with more than one layer of the same or of different metals
- C25D5/12—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium
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- C25D7/00—Electroplating characterised by the article coated
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- C25D9/00—Electrolytic coating other than with metals
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- C25D9/06—Electrolytic coating other than with metals with inorganic materials by anodic processes
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
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Abstract
The invention relates to a method for preparing a flexible electrode on a nano needle cone nickel substrate, belonging to the technical field of electrode materials. The method adopts a constant-current cathode electrodeposition mode to prepare the nano needle cone nickel, and regulates the size and the distribution uniformity of the nano needle cone nickel array by the crystallization regulator, so that the prepared nickel nano needle cone has uniform size and uniform distribution, and the size is about 150nm to 200 nm. Preparing the nanometer-sized manganese oxide anode material on the nanometer needle cone nickel by adopting a constant-current anode electrodeposition mode. After a conical nickel array grows on a flat substrate, the nano-sized manganese oxide adheres to the conical nickel to grow to form a flexible manganese oxide anode, and the flexible manganese oxide anode is assembled into a zinc-manganese secondary battery, wherein the specific discharge capacity reaches 210 mAh/g. The invention can relieve the problems of falling and pulverization of the anode and cathode materials, and improves the stability of the anode and cathode materials and the electrochemical performance of the battery, thereby having certain value for the practical application of the zinc ion battery.
Description
Technical Field
The invention belongs to the technical field of electrode materials, and particularly relates to a method for preparing a flexible electrode on a nano needle cone nickel substrate.
Background
Lithium ion batteries are widely used in various energy storage devices, but because lithium negative electrode metals of the lithium ion batteries are easy to oxidize and spontaneously combust, certain potential safety hazards exist. In recent years, battery safety is receiving more and more attention, and zinc ion batteries have received wide attention because of their characteristics such as high safety performance, large theoretical capacity, and low cost, compared with lithium ion batteries.
The zinc ion battery has certain advantages in the aspect of replacing the lithium ion battery, but the pulverization, the falling off and the like of the zinc ion anode and cathode materials are important influence factors for restricting the electrical performance of the zinc ion battery. The zinc ion battery can generate certain structural change in the circulating process, so that the problems of falling, pulverization and the like of active substances of positive and negative electrode materials are caused, the capacity of the battery can be quickly attenuated, and the practical application of the zinc ion battery is influenced. At present, most of researches are carried out to solve the problems of falling off, pulverization and the like of active substances of positive and negative electrode materials in modes of coating nano materials, preparing various nanospheres, nanorods and the like. For example, by adding graphene, carbon capsule coating, depositing conductive polymers and other substances, and adopting in-situ growth, hydrothermal synthesis and other modes, a conductive network is formed on the surface of the active substance, so that the material falling loss is reduced, and the structural stability of the active substance is protected. Therefore, a method with simple preparation process and low cost is needed to reduce the problems of falling off, pulverization and the like of active substances of the anode and cathode materials and improve the stability of the anode and cathode materials and the electrochemical performance of the battery.
Disclosure of Invention
The invention aims to solve the technical problem of poor binding force between anode and cathode materials and a substrate in the prior art and provides a method for preparing a flexible electrode on a nano needle cone nickel substrate.
In order to solve the above technical problems, an embodiment of the present invention provides a method for preparing a flexible electrode on a nickel substrate with a nano needle cone, including the following steps:
s1: preparing the nano needle-cone nickel on the flexible conductive substrate by adopting a constant-current cathode electrodeposition mode, which specifically comprises the following steps: the positive pole adopts pure nickel board, and the negative pole adopts flexible electrically conductive basement, and the plating solution adopts the deionized water configuration, and the composition of plating solution is: the main salt of the plating solution is 1.5mol/L of nickel chloride, the buffer is 0.5mol/L of boric acid, and the content of the crystallization regulator is 4 mol/L;
s2: the manganese oxide electrode material is prepared on the nanometer needle cone nickel by adopting a constant current anodic electrodeposition mode, and specifically comprises the following steps: the positive pole adopts nanometer needle cone nickel, and the negative pole adopts rhodium plating insoluble titanium net electrode, and the plating solution adopts the deionized water configuration, and the composition of plating solution is: the main salt of the plating solution is 0.3mol/L manganese sulfate, and the buffering agent is 0.5mol/L boric acid;
s3: preparing a zinc electrode material on the nano needle-cone nickel by adopting a constant-current cathode electrodeposition mode, which comprises the following steps: the positive pole adopts pure zinc plate, and the negative pole adopts nanometer needle awl nickel, and the plating solution adopts the deionized water configuration, and the composition of plating solution is: the main salt of the plating solution is 0.5mol/L zinc sulfate, the buffering agent is 0.5mol/L boric acid, and the conductive salt is 0.5mol/L sodium sulfate.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, step S1 is preceded by step S0: and sequentially carrying out oil removal treatment, microetching treatment and presoaking treatment on the flexible conductive substrate.
Further, the plating conditions in step S1 are: the temperature of the electro-deposition plating solution is 55 ℃, the current density is 1.5A/dm2, the electro-deposition plating solution is electrified and then is electroplated for 5 minutes, and the cathode is taken out and washed by deionized water, and then is dried and stored.
Further, the plating conditions in step S2 are: and (3) electrifying the electro-deposition plating solution at the temperature of 25 ℃ and the current density of 0.5A/dm2, electroplating for 1 minute, taking out the anode, washing with deionized water, and blow-drying for storage.
Further, the plating conditions in step S3 are: and (3) electroplating for 30 minutes after electrifying the electro-deposition plating solution at the temperature of 25 ℃ and the current density of 0.25A/dm 2-4A/dm2, taking out the cathode, washing with deionized water, and drying and storing.
Further, the oil removing treatment specifically comprises: soaking in 50 deg.C deoiling liquid for 3min, and washing with deionized water.
Further, the microetching treatment specifically comprises: soaking in 25 deg.C microetching solution for 30s, and washing with deionized water.
Further, the prepreg is specifically: soaking in 25 deg.C pickling solution for 1min, and washing with deionized water.
Further, the size of the nano needle cone nickel is 150nm to 200 nm.
In order to solve the technical problem, an embodiment of the present invention provides a zinc ion battery, which includes a manganese oxide electrode material and a zinc electrode material, where the manganese oxide electrode material and the zinc electrode material are prepared according to the method for preparing a flexible electrode on a nano needle cone nickel substrate.
Compared with the prior art, the invention has the beneficial effects that:
firstly, the nano needle cone nickel array structure is prepared in an aqueous solution in a manner of direct electrodeposition of the aqueous solution, the method is simple to operate, and the size and uniformity of the nano needle cone nickel array can be regulated and controlled by adjusting current density and a crystallization regulator.
Secondly, the manganese oxide anode material and the zinc cathode material are prepared on the nano needle cone nickel array in a mode of directly electrodepositing the aqueous solution, and the method is convenient to operate, low in cost and easy to implement. The manganese oxide with the nano structure is obtained by direct electrodeposition growth on the nano conical nickel array, the contact area of the manganese oxide and the zinc and nickel substrate is large, the binding force is good, the loss of the material in the circulation process is reduced, the manganese oxide anode material and the zinc cathode material prepared by the method can be assembled into a zinc-manganese secondary battery, and the discharge specific capacity reaches 210 mAh/g.
Thirdly, the invention deposits active substances on the prepared nano needle cone nickel array structure by changing the structure of the nickel current collector, reduces the problems of falling off, pulverization and the like of the active substances of the anode and cathode materials, and improves the stability of the anode and cathode materials and the electrochemical performance of the battery.
Drawings
Fig. 1 is an SEM image of nanoneedle-cone nickel and manganese oxide prepared on a flexible conductive substrate according to a first embodiment of the present invention, wherein fig. 1(a) is an SEM image of a flexible conductive substrate, fig. 1(b) is an SEM image of nanoneedle-cone nickel, and fig. 1(c) is an SEM image of manganese oxide;
fig. 2 is a diagram of the charge and discharge performance of a zinc ion battery composed of flexible electrodes prepared on a nano needle cone nickel substrate according to a first embodiment of the present invention;
fig. 3 is an EIS diagram of a zinc ion battery composed of flexible electrodes fabricated on a nanoneedle-cone nickel substrate according to a first embodiment of the present invention, wherein fig. 3(b) is a partially enlarged view of a square frame in fig. 3 (a);
FIG. 4 is an SEM image of nanoneedle-cone nickel prepared under different crystallization modifier concentrations according to the first embodiment of the invention; in FIG. 4(a), the crystallization modifier is 1mol/L, the crystallization modifier is 2mol/L in FIG. 4(b), and the crystallization modifier is 4mol/L in FIG. 4 (c).
FIG. 5 is a contact angle test chart of the nanoneedle-cone nickel prepared in the first embodiment of the present invention; fig. 5(a) is a contact angle test chart of the PI substrate, fig. 5(b) is a contact angle test chart of the flexible conductive substrate, fig. 5(c) is a contact angle test chart of the watt nickel, and fig. 5(d) is a contact angle test chart of the nano needle cone nickel.
Fig. 6 is an SEM image of zinc anodes prepared at different current densities according to the first embodiment of the present invention; in FIG. 6(a), the current density was 0.25A/dm2In FIG. 6(b), the current density was 0.5A/dm2In FIG. 6(c), the current density is 4A/dm2Then (c) is performed.
Detailed Description
The principles and features of this invention are described below in conjunction with the following drawings, which are set forth by way of illustration only and are not intended to limit the scope of the invention.
The method for preparing the flexible electrode on the nano needle cone nickel substrate provided by the first embodiment of the invention comprises the following steps:
(1) pretreatment of electrodes
And (3) pretreating the flexible copper-clad substrate to remove an oxide layer, oil stains and the like on the flexible substrate so as to avoid influencing the growth of the cone nickel in the electrodeposition process. The pretreatment process mainly comprises three steps of oil removal, microetching and presoaking. The oil removing process is to soak the flexible substrate in oil removing liquid at 50 ℃ for 3min and wash the flexible substrate clean by deionized water, and the oil removing process is mainly to clean oil stains, organic substances and the like on the surface of the substrate; the microetching process is to soak the flexible substrate in microetching liquid at 25 ℃ for 30s and wash the flexible substrate clean by deionized water, and the microetching process can remove an oxide layer on the surface of the substrate and can improve the binding force with a plating layer; the pre-dipping process is to soak the flexible substrate in a pickling solution at 25 ℃ for 1min and wash the flexible substrate with deionized water, and the oxide layer on the surface of the substrate can be further removed in the pre-dipping process.
(2) Preparation of nano needle cone nickel
And (3) taking the pretreated flexible copper-clad substrate as an electroplating cathode, communicating the electroplating cathode with a power supply cathode, communicating the anode with a pure nickel plate, communicating the electroplating cathode with a power supply anode, and preparing the nano needle-cone nickel on the flexible conductive substrate by adopting a constant-current cathodic electrodeposition mode.
In the preparation process of nanometer needle awl nickel, the raw materials that adopt are analytic pure chemical reagent, all adopt deionized water to prepare when the plating solution is prepared, and the composition of plating solution is: the main salt of the plating solution is 1.5mol/L of nickel chloride, the buffer is 0.5mol/L of boric acid, and the crystallization regulator is 4 mol/L. The temperature of the electrodeposition coating liquid is 55 ℃ and the current density is 1.5A/dm2And electrifying, electroplating for 5 minutes, taking out the cathode, washing with deionized water, blow-drying and storing to finish the preparation of the nano conical nickel on the cathode substrate.
(3) Preparation of flexible manganese oxide positive electrode
The manganese oxide electrode material is prepared on the nano needle cone nickel by adopting a constant current anode electrodeposition mode, the main salt of the electroplating solution is 0.3mol/L manganese sulfate, the buffering agent is 0.5mol/L boric acid, and the buffering agent mainly plays a role in maintaining the relative stability of the pH value of the solution. The anode is prepared nano needle-cone nickel and communicated with the anode, the cathode is a rhodium-plated insoluble titanium mesh electrode and communicated with the cathode, the temperature of the plating solution is 25 ℃, and the current density is 0.5A/dm2And electroplating for 1 minute after electrifying, taking out the anode, washing with deionized water, drying and storing to finish the preparation of the manganese oxide anode. The shapes of the manganese oxide anode material in the preparation process are shown in figure 1, after a conical nickel array grows on a flat copper substrate, the nano-sized manganese oxide adheres to the nano-conical nickel to grow, and the flexible manganese oxide anode is formed.
(3) Preparation of flexible zinc cathode
Preparing zinc electrode material on the nanometer needle cone nickel by constant current cathode electrodeposition, wherein the anode is pure zinc plate and is communicated with the anode, the cathode is prepared nanometer cone nickel and is communicated with the cathode, the temperature of the plating solution is 25 ℃, and the current density is 4A/dm2Electroplating for 30 minutes after electrificationAnd (5) taking out the cathode, washing with deionized water, drying and storing. The main salt of the plating solution is 0.5mol/L zinc sulfate, the buffering agent is 0.5mol/L boric acid, and the conductive salt is 0.5mol/L sodium sulfate.
The flexible manganese oxide positive electrode and the zinc negative electrode prepared in the first embodiment of the invention are assembled into a zinc ion battery, and the performance of the zinc ion battery is tested, and the performance and EIS test of the zinc ion battery composed of the manganese oxide positive electrode and the zinc negative electrode prepared on the nano needle cone nickel in the first embodiment of the invention are shown in figures 2 and 3.
Fig. 2 is a charge-discharge curve of a zinc ion battery composed of a manganese oxide positive electrode and a zinc negative electrode, wherein a square curve is a charge curve, a triangular curve is a discharge curve, the discharge specific capacity reaches 210mAh/g, the discharge specific capacity is good, and the charge-discharge voltage range is controlled between 1.0V and 1.9V. According to the charging and discharging curve, the battery has an obvious charging and discharging platform and has better charging and discharging performance.
Fig. 3 is an EIS diagram of a zinc ion battery composed of a manganese oxide positive electrode and a zinc negative electrode, and fig. 3(b) is a partially enlarged view of fig. 3(a), illustrating that the EIS diagram exists in two semicircles, corresponds to the processes of an SEI layer and charge transfer of the battery, the battery has an ohmic resistance of 6.7 Ω, and exists typical SEI layer, charge transfer and diffusion resistance processes, and illustrates that the prepared flexible manganese oxide positive electrode and zinc negative electrode can be used as the positive electrode and the negative electrode of a zinc ion secondary battery.
The following experiments were conducted by using different crystallization modifier concentrations to affect the growth of nanoneedle-cone nickel:
firstly, placing a pretreated flexible copper-clad substrate serving as an electroplating cathode into a plating solution, wherein the anode is a pure nickel plate, and then growing the nano needle-cone nickel by adopting a constant-current electrodeposition mode. The electroplating solution comprises the following components: nickel chloride with 1.5mol/L of main salt of plating solution, boric acid with 0.5mol/L of buffering agent, 55 ℃ of temperature of the electrodeposition plating solution, 5min of time and 1.5A/dm of current density2(ii) a And (5) washing with deionized water after the completion, and drying and storing. Wherein, the concentrations of the crystallization modifiers are 1mol/L, 2mol/L and 4mol/L respectively, and SEM images of the nano-needle cone nickel prepared by the crystallization modifiers with different concentrations are shown in FIG. 4. FIG. 5 is a prepared nanoThe contact angle test chart of the nickel with the needle cone is shown in the figures, wherein (a) to (d) respectively represent the contact angle test chart of a substrate PI, a substrate PI copper-clad plate, watt nickel and the nickel with the needle cone.
The experimental results show that when the concentration of the crystallization regulator is low, the nickel nanometer coniform is different in size and uneven in distribution, and when the concentration of the crystallization regulator reaches 4mol/L, the nickel nanometer coniform is uniform in size and even in distribution, and the size is about 150nm to 200 nm. The nano needle cone nickel has excellent hydrophilicity through a contact angle test surface, the water contact angle is 5.4 degrees which is far smaller than 48.8 degrees of common watt nickel and 68 degrees of a copper substrate, and the nano needle cone nickel is proved to be capable of well improving the hydrophilicity of the surface, is beneficial to full contact of a solid surface and a liquid surface and has a certain application value. Therefore, the nano nickel coniferous needle array with uniform growth can be obtained by changing the concentration of the crystallization regulator, and the obtained nano nickel coniferous needle has very good hydrophilicity.
FIG. 6 shows the respective current densities of 0.25A/dm2、0.5A/dm2And 4A/dm2The sheet structure of the zinc layer of the zinc cathode prepared below is increased along with the increase of the current density, which shows that the current density influences the particle size of zinc on the conical nickel substrate.
The method adopts a constant-current cathode electrodeposition mode to prepare the nano needle cone nickel, and regulates the size and the distribution uniformity of the nano needle cone nickel array by the crystallization regulator, so that the prepared nickel nano needle cone has uniform size and uniform distribution, and the size is about 150nm to 200 nm. Preparing the nanometer-sized manganese oxide anode material on the nanometer needle cone nickel by adopting a constant-current anode electrodeposition mode. The charging and discharging curve of the zinc ion battery composed of the manganese oxide anode and the zinc cathode prepared by the method shows that the discharging specific capacity reaches 210mAh/g, the battery has good discharging specific capacity, the charging and discharging voltage range is between 1.0V and 1.9V, and the battery has an obvious charging and discharging platform. EIS tests show that the battery has 6.7 omega ohmic impedance, a typical SEI layer, charge transfer and diffusion impedance process exists, and the prepared flexible manganese oxide anode and zinc cathode can be used as the anode and the cathode of a zinc ion secondary battery and have a certain application prospect. .
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A method for preparing a flexible electrode on a nano needle cone nickel substrate is characterized by comprising the following steps:
s1: preparing the nano needle-cone nickel on the flexible conductive substrate by adopting a constant-current cathode electrodeposition mode, which specifically comprises the following steps: the positive pole adopts pure nickel board, and the negative pole adopts flexible electrically conductive basement, and the plating solution adopts the deionized water configuration, and the composition of plating solution is: the main salt of the plating solution is 1.5mol/L of nickel chloride, the buffer is 0.5mol/L of boric acid, and the content of the crystallization regulator is 4 mol/L;
s2: the manganese oxide electrode material is prepared on the nanometer needle cone nickel by adopting a constant current anodic electrodeposition mode, and specifically comprises the following steps: the positive pole adopts nanometer needle cone nickel, and the negative pole adopts rhodium plating insoluble titanium net electrode, and the plating solution adopts the deionized water configuration, and the composition of plating solution is: the main salt of the plating solution is 0.3mol/L manganese sulfate, and the buffering agent is 0.5mol/L boric acid;
s3: preparing a zinc electrode material on the nano needle-cone nickel by adopting a constant-current cathode electrodeposition mode, which comprises the following steps: the positive pole adopts pure zinc plate, and the negative pole adopts nanometer needle awl nickel, and the plating solution adopts the deionized water configuration, and the composition of plating solution is: the main salt of the plating solution is 0.5mol/L zinc sulfate, the buffering agent is 0.5mol/L boric acid, and the conductive salt is 0.5mol/L sodium sulfate.
2. The method for preparing a flexible electrode on a nickel substrate with a nano needle cone as claimed in claim 1, wherein step S1 is preceded by step S0: and sequentially carrying out oil removal treatment, microetching treatment and presoaking treatment on the flexible conductive substrate.
3. The method for preparing the flexible electrode on the nickel substrate with the nanometer needle cones as claimed in claim 1, wherein the electroplating conditions in the step S1 are as follows: the temperature of the electrodeposition coating liquid is 55 ℃ and the current density is 1.5A/dm2And electrifying, electroplating for 5 minutes, taking out the cathode, washing with deionized water, drying and storing.
4. The method for preparing the flexible electrode on the nickel substrate with the nanometer needle cones as claimed in claim 1, wherein the electroplating conditions in the step S2 are as follows: the temperature of the electrodeposition coating liquid is 25 ℃ and the current density is 0.5A/dm2And electrifying, electroplating for 1 minute, taking out the anode, washing with deionized water, and blow-drying for storage.
5. The method for preparing the flexible electrode on the nickel substrate with the nanometer needle cones as claimed in claim 1, wherein the electroplating conditions in the step S3 are as follows: the temperature of the electrodeposition coating liquid is 25 ℃ and the current density is 0.25A/dm2～4A/dm2 .And electrifying, electroplating for 30 minutes, taking out the cathode, washing with deionized water, drying and storing.
6. The method for preparing the flexible electrode on the nickel substrate with the nanometer needle cones as claimed in claim 1, wherein the degreasing treatment specifically comprises: soaking in 50 deg.C deoiling liquid for 3min, and washing with deionized water.
7. The method for preparing the flexible electrode on the nickel substrate with the nanometer needle cones as claimed in claim 1, wherein the microetching treatment specifically comprises: soaking in 25 deg.C microetching solution for 30s, and washing with deionized water.
8. The method for preparing the flexible electrode on the nano needle cone nickel substrate according to claim 1, wherein the pre-dipping treatment is specifically as follows: soaking in 25 deg.C pickling solution for 1min, and washing with deionized water.
9. The method for preparing the flexible electrode on the nano needle cone nickel substrate as claimed in claim 1, wherein the size of the nano needle cone nickel is 150nm to 200 nm.
10. A zinc ion battery comprising a manganese oxide electrode material and a zinc electrode material, wherein the manganese oxide electrode material and the zinc electrode material are prepared according to the method for preparing a flexible electrode on a nanoneedle cone nickel substrate of any one of claims 1 to 9.
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| CN114540895A (en) * | 2022-03-01 | 2022-05-27 | 九牧厨卫股份有限公司 | Bactericidal gray composite coating, preparation method thereof and gray bactericidal product |
| CN115000348A (en) * | 2022-05-23 | 2022-09-02 | 上海交通大学 | Alkali metal negative electrode composite coating and preparation method and application thereof |
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