Method for preparing pure nickel substance through electrolytic method and prepared pure nickel substance
By controlling the current density and stirring speed through electrolysis and using an electrolyte containing nickel salts and additives, dendritic nickel powder and nickel film were successfully generated simultaneously on the cathode, solving the problems of complex preparation process and high cost in the existing technology and realizing an efficient and low-cost preparation method.
Patent Information
- Application Number
- CN202510842560.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-23
- Publication Date
- 2025-09-16
AI Technical Summary
It is difficult to simultaneously and efficiently prepare dendritic nickel powder and nickel thin film with existing technologies, and the preparation process is complex and costly.
The electrolysis method is adopted to generate dendritic nickel powder and nickel film by controlling the current density and stirring speed, using an electrolyte containing nickel salt, ammonium chloride and additives, and performing an electrolytic reaction between the cathode and the anode.
The simultaneous preparation of dendritic nickel powder and nickel film is achieved, the process is simple, the cost is low, the nickel powder is dendritic, the nickel film has a smooth surface and good conductivity, and is suitable as an electrode substrate or active material carrier.
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Abstract
Description
Technical Field
[0001] The present invention relates to the field of electrolytic coating methods, and in particular to a method for preparing pure nickel material by electrolysis and the prepared pure nickel material. Background Art
[0002] Dendritic nickel powder, due to its high purity, high activity, and unique physical and chemical properties, has broad application value in various fields. Nickel thin films are widely used in solar cells, electronic devices, and integrated circuits. Currently, there are many technologies for preparing dendritic nickel powder and nickel thin films separately, but there is no method for preparing both simultaneously. Separate preparation processes are complex and costly. Therefore, developing a method for simultaneously preparing both dendritic nickel powder and nickel thin films is crucial.
[0003] Chinese invention patent application CN111270275A discloses a bright black nickel plating solution, its preparation method, and its application. The solution utilizes a nickel source composed of imidazole and chitosan complexes, which exhibit good adsorption and coordination properties for nickel and cobalt ions, allowing nickel to be deposited on electrode surfaces. However, it cannot simultaneously produce nickel powder and nickel film. Chinese invention patent CN118374802B discloses a process for electroless deposition of a nickel-containing coating using a low-temperature solution. The solution utilizes a noble metal salt, a silane coupling agent, a stabilizer, and nano-nickel powder. The components interact to increase the reduction deposition rate of the coating, but the use of noble metals results in high production costs. Summary of the Invention
[0004] In order to develop a method for simultaneously preparing dendritic nickel powder and nickel film, the first aspect of the present invention provides a method for preparing pure nickel material by electrolysis, comprising the following steps:
[0005] S1: prepare electrolyte;
[0006] S2: Electrolysis reaction: Metal plate I is the cathode, and metal plate II is the anode. The distance between the cathode and anode is adjusted, the current density is controlled, and the electrolysis temperature is maintained. The cathode and anode are inserted into the electrolyte, and the electrolyte undergoes electrolysis reaction under continuous stirring;
[0007] S3: Product separation: After the reaction is completed, the product is stripped from the cathode and the pure nickel material is collected;
[0008] The pure nickel material includes dendritic nickel powder and nickel film.
[0009] As an embodiment, the electrolyte includes at least ammonium chloride, nickel salt, additives and water, and the concentration of the nickel salt in the electrolyte is 1-50 g / L.
[0010] As an embodiment, the concentration of ammonium chloride in the electrolyte is 1-20 g / L.
[0011] As an embodiment, the nickel salt includes at least one of nickel sulfate, nickel chloride, nickel sulfamate or nickel acetate.
[0012] As an embodiment, the additive is a sulfur-containing additive, and the concentration of the additive in the electrolyte is 0.01-0.2 g / L.
[0013] As an embodiment, the additive includes at least one of sodium lauryl sulfate, gelatin, thiourea or saccharin.
[0014] As an embodiment, the metal plate I includes at least one of a titanium plate, a stainless steel plate or a pure nickel plate; the metal plate II is an inert metal plate or a pure nickel plate.
[0015] As an embodiment, the inert metal plate includes but is not limited to at least one of a tin-antimony-titanium plate or a pure nickel plate.
[0016] As an embodiment, the distance between the cathode and the anode is 15-45 mm, the electrolysis temperature is 30-60° C., the electrolysis time is 15-60 min, and the stirring speed of the electrolyte is 200-800 r / min.
[0017] In the present invention, the electrolyte is stirred at a constant speed of 200-800 r / min and a sulfur-containing additive is added to maintain a stable concentration of the electrolyte, prevent extreme concentration differences, and avoid affecting the uniformity and speed of nickel deposition near the electrode.
[0018] As an embodiment, the current density is 50-150A / m 2 , including 150A / m 2 , a nickel film is generated on the inner surface of the cathode, and neither nickel powder nor nickel film is generated on the outer surface of the cathode.
[0019] As an embodiment, the current density is 150-360A / m 2 , excluding 150A / m 2 , including 360A / m 2 , dendritic nickel powder and nickel film are generated on the inner surface of the cathode, and neither nickel powder nor nickel film is generated on the outer surface of the cathode.
[0020] As an embodiment, the current density is 360-560A / m 2 , excluding 360A / m 2 , including 560A / m 2 , dendritic nickel powder is generated on the inner surface of the cathode, and a nickel film is generated on the outer surface of the cathode.
[0021] As an embodiment, the current density is greater than 560A / m 2 , dendritic nickel powder is generated on the inner surface of the cathode, and neither nickel powder nor nickel film is generated on the outer surface of the cathode.
[0022] The present invention produces dendritic nickel powder and nickel film by electrolyzing nickel salt solution. The anode is an inert metal plate, and the cathode is a titanium plate, stainless steel plate or pure nickel plate. The constant current method is used for electrodeposition. The nickel ions obtain electrons on the cathode surface and are reduced to elemental nickel Ni. 2 ++2e - →Ni, anions migrate toward the anode, undergoing an oxidation reaction. Ion migration forms a closed circuit, maintaining a continuous current. A large electric field exists on the inner surface of the cathode facing the anode. The nickel microstructure is affected by this field, preferentially growing in the direction of the field, forming dendritic nickel powder. The outer surface facing away from the anode has a weak or absent electric field, forming a nickel film.
[0023] The second aspect of the present invention provides a pure nickel material, which is prepared by the above-mentioned method for preparing pure nickel material by electrolysis. The thickness of the prepared nickel film is 4-6 μm, and the average resistivity of the prepared nickel film is 12-18 μΩ·cm.
[0024] Compared with the prior art, the present invention has the following beneficial effects:
[0025] (1) The method for preparing pure nickel material by electrolysis of the present invention is to adjust the current density to 150-360A / m 2 or 360-560A / m 2 , dendritic nickel powder and nickel film can be obtained on the cathode at the same time, the production process is simple and the cost is low.
[0026] (2) The method for preparing pure nickel material by electrolysis of the present invention can maintain the concentration of the electrolyte stable by stirring the electrolyte at a constant speed of 200-800 r / min and adding a sulfur-containing additive, so that nickel is stably and evenly deposited near the cathode.
[0027] (3) The electrolytic method for preparing pure nickel material described in the present invention uses an electrolyte containing 1-50g / L nickel salt. The prepared nickel powder has a dendritic shape with a conical tip and a uniform branching density; the surface of the nickel film is smooth, continuous and crack-free, and has a low resistivity.
[0028] (4) The method for preparing pure nickel material by electrolysis described in the present invention produces dendritic nickel powder that is nano-scale nickel powder, and the nickel film produced has good electrical conductivity.
[0029] (5) The method for preparing pure nickel material by electrolysis described in the present invention has a dendritic nickel powder with a high specific surface area and high electrochemical reaction activity. The prepared nickel film has a uniform and dense structure, and its conductivity and mechanical integrity are better, making it suitable as an electrode substrate or active material carrier. BRIEF DESCRIPTION OF THE DRAWINGS
[0030] Figure 1 This is a picture of the electrolysis device used in the method for preparing pure nickel material by electrolysis described in the present invention.
[0031] Figure 1 In: 1. Cathode; 2. Anode; 3. Electrolyte; 4. Power supply.
[0032] Figure 2 The nickel powder and nickel film obtained in Example 1 of the present invention, from left to right are the state of nickel powder on the cathode, the state of nickel film on the cathode, the scraped nickel powder, and the peeled nickel film.
[0033] Figure 3 XRD patterns of nickel powder and nickel film obtained in Example 1 of the present invention, left: nickel powder; right: nickel film.
[0034] Figure 4 This is the XPS spectrum of the nickel thin film obtained in Example 1 of the present invention, including (a) Ni 2p, (b) O1s, (c) full spectrum XPS spectrum, and (d) C1s standard spectrum.
[0035] Figure 5 These are SEM images of nickel powder and nickel film obtained in Example 1 of the present invention, left: nickel powder; right: nickel film.
[0036] Figure 6 This is an SEM image of the nickel thin film obtained in Example 2 of the present invention, left: low magnification; right: high magnification.
[0037] Figure 7 This is an SEM image of the nickel thin film obtained in Example 3 of the present invention, left: low magnification; right: high magnification.
[0038] Figure 8 These are SEM images of nickel powder and nickel film obtained in Example 4 of the present invention, left: nickel powder; right: nickel film.
[0039] Figure 9 This is an SEM image of the nickel powder obtained in Example 5 of the present invention, left: low magnification; right: high magnification.
[0040] Figure 10 The right side is an SEM image of the nickel thin film obtained in Example 6 of the present invention, low magnification; the right side is a high magnification.
[0041] Figure 11The right side is an SEM image of the nickel thin film obtained in Example 7 of the present invention, low magnification; the right side is a high magnification.
[0042] Figure 12 This is a graph showing the charge and discharge performance of the nickel film obtained in Examples 1 and 8 of the present invention as a current collector for lithium-ion batteries;
[0043] From left to right are the specific capacity diagram of the 4μm nickel film prepared in Example 1 as a lithium-ion battery current collector during the charge and discharge process, the specific capacity diagram of the 6μm nickel film prepared in Example 8 as a lithium-ion battery current collector during the charge and discharge process, and the impedance spectra of the 4μm nickel film and the 6μm nickel film as lithium-ion battery current collectors. DETAILED DESCRIPTION
[0044] The electrolysis device used in the method for preparing pure nickel material by electrolysis according to the present invention is shown in the figure Figure 1 .
[0045] Example 1
[0046] A method for preparing pure nickel material by electrolysis comprises the following steps:
[0047] S1: preparing electrolyte 3;
[0048] S2: Electrolysis reaction: Metal plate I is cathode 1, and metal plate II is anode 2. The distance between cathode and anode 2 is adjusted, and the current density is controlled by power supply 4 to maintain the electrolysis temperature. Cathode 1 and anode 2 are inserted into the electrolyte, and the electrolyte undergoes electrolysis reaction under continuous stirring.
[0049] S3: Separation of products: After the reaction is completed, the products are stripped from the cathode 1 and collected to obtain pure nickel material;
[0050] The pure nickel material includes dendritic nickel powder and nickel film.
[0051] The electrolyte 3 includes ammonium chloride, nickel salt, additives and water, wherein the concentration of the nickel salt in the electrolyte 3 is 22.33 g / L, the concentration of the additive in the electrolyte 3 is 0.15 g / L, and the concentration of ammonium chloride in the electrolyte 3 is 10 g / L.
[0052] The nickel salt is nickel sulfate hexahydrate, and the additive is sodium lauryl sulfate.
[0053] The metal plate I is a titanium plate, and the metal plate II is a pure nickel plate.
[0054] The distance between the cathode 1 and the anode 2 is 30 mm, the electrolysis temperature is 40° C., the electrolysis time is 30 min, and the stirring speed of the electrolyte 3 is 300 r / min.
[0055] The current density is 460A / m2 , dendritic nickel powder is generated on the inner surface of cathode 1, and a nickel film is generated on the outer surface of cathode 1, and the thickness of the nickel film is 4 μm.
[0056] Example 2
[0057] A method for preparing pure nickel material by electrolysis comprises the following steps:
[0058] S1: preparing electrolyte 3;
[0059] S2: Electrolysis reaction: Metal plate I is cathode 1, and metal plate II is anode 2. The distance between cathode 1 and anode 2 is adjusted, the current density is controlled, and the electrolysis temperature is maintained. Cathode 1 and anode 2 are inserted into electrolyte 3, and electrolyte 3 undergoes electrolysis reaction under continuous stirring.
[0060] S3: Separation of products: After the reaction is completed, the products are stripped from the cathode 1 and collected to obtain pure nickel material;
[0061] The pure nickel material is a nickel film.
[0062] The electrolyte 3 includes ammonium chloride, nickel salt, additives and water, wherein the concentration of the nickel salt in the electrolyte 3 is 22.33 g / L, the concentration of the additive in the electrolyte 3 is 0.05 g / L, and the concentration of ammonium chloride in the electrolyte 3 is 10 g / L.
[0063] The nickel salt is nickel sulfate hexahydrate, and the additive is thiourea additive.
[0064] The metal plate I is a stainless steel plate, and the metal plate II is a pure nickel plate.
[0065] The distance between the cathode 1 and the anode 2 is 30 mm, the electrolysis temperature is 40° C., the electrolysis time is 50 min, and the stirring speed of the electrolyte 3 is 300 r / min.
[0066] The current density is 120A / m 2 , a nickel film is formed on the inner surface of cathode 1.
[0067] Example 3
[0068] A method for preparing pure nickel material by electrolysis comprises the following steps:
[0069] S1: preparing electrolyte 3;
[0070] S2: Electrolysis reaction: Metal plate I is cathode 1, and metal plate II is anode 2. The distance between cathode 1 and anode 2 is adjusted, the current density is controlled, and the electrolysis temperature is maintained. Cathode 1 and anode 2 are inserted into electrolyte 3, and electrolyte 3 undergoes electrolysis reaction under continuous stirring.
[0071] S3: Separation of products: After the reaction is completed, the products are stripped from the cathode 1 and collected to obtain pure nickel material;
[0072] The pure nickel material is a nickel film.
[0073] The electrolyte 3 includes ammonium chloride, nickel salt, additives and water, wherein the concentration of the nickel salt in the electrolyte 3 is 22.33 g / L, the concentration of the additive in the electrolyte 3 is 0.05 g / L, and the concentration of ammonium chloride in the electrolyte 3 is 5 g / L.
[0074] The nickel salt is nickel sulfate hexahydrate, and the additive is gelatin additive.
[0075] The metal plate I is a pure nickel plate, and the metal plate II is a tin-antimony-titanium plate.
[0076] The distance between the cathode 1 and the anode 2 is 30 mm, the electrolysis temperature is 40° C., the electrolysis time is 60 min, and the stirring speed of the electrolyte 3 is 300 r / min.
[0077] The current density is 120A / m 2 , a nickel film is formed on the inner surface of cathode 1.
[0078] Example 4
[0079] A method for preparing pure nickel material by electrolysis comprises the following steps:
[0080] S1: preparing electrolyte 3;
[0081] S2: Electrolysis reaction: Metal plate I is cathode 1, and metal plate II is anode 2. The distance between cathode 1 and anode 2 is adjusted, the current density is controlled, and the electrolysis temperature is maintained. Cathode 1 and anode 2 are inserted into electrolyte 3, and electrolyte 3 undergoes electrolysis reaction under continuous stirring.
[0082] S3: Separation of products: After the reaction is completed, the products are stripped from the cathode 1 and collected to obtain pure nickel material;
[0083] The pure nickel material includes dendritic nickel powder and nickel film.
[0084] The electrolyte 3 includes ammonium chloride, nickel salt, additives and water, wherein the concentration of the nickel salt in the electrolyte 3 is 18 g / L, the concentration of the additive in the electrolyte 3 is 0.15 g / L, and the concentration of ammonium chloride in the electrolyte 3 is 8 g / L.
[0085] The nickel salt is nickel sulfate hexahydrate, and the additive is sodium lauryl sulfate.
[0086] The metal plate I is a titanium plate, and the metal plate II is a pure nickel plate.
[0087] The distance between the cathode 1 and the anode 2 is 30 mm, the electrolysis temperature is 40° C., the electrolysis time is 50 min, and the stirring speed of the electrolyte 3 is 300 r / min.
[0088] The current density is 460A / m 2 , dendritic nickel powder is generated on the inner surface of cathode 1, and a nickel film is generated on the outer surface of cathode 1.
[0089] Example 5
[0090] A method for preparing pure nickel material by electrolysis, the specific implementation method is the same as Example 1, except that the metal plate I is a pure nickel plate, and the metal plate II is a tin-antimony-titanium plate.
[0091] The current density is 1200A / m 2 , dendritic nickel powder is generated on the inner surface of cathode 1.
[0092] Example 6
[0093] A method for preparing pure nickel material by electrolysis, the specific implementation method is the same as Example 1, except that the metal plate I is a stainless steel plate, and the metal plate II is a tin-antimony-titanium-nickel plate.
[0094] The electrolysis time is 60 min.
[0095] The current density is 120A / m 2 , a nickel film is formed on the inner surface of cathode 1.
[0096] Example 7
[0097] A method for preparing pure nickel material by electrolysis comprises the following steps:
[0098] S1: preparing electrolyte 3;
[0099] S2: Electrolysis reaction: Metal plate I is cathode 1, and metal plate II is anode 2. The distance between cathode 1 and anode 2 is adjusted, the current density is controlled, and the electrolysis temperature is maintained. Cathode 1 and anode 2 are inserted into electrolyte 3, and electrolyte 3 undergoes electrolysis reaction under continuous stirring.
[0100] S3: Separation of products: After the reaction is completed, the products are stripped from the cathode 1 and collected to obtain pure nickel material;
[0101] The pure nickel material is a nickel film.
[0102] The electrolyte 3 includes ammonium chloride, nickel salt, additives and water, wherein the concentration of the nickel salt in the electrolyte 3 is 22.33 g / L, the concentration of the additive in the electrolyte 3 is 0.15 g / L, and the concentration of ammonium chloride in the electrolyte 3 is 5 g / L.
[0103] The nickel salt is nickel sulfate hexahydrate, and the additive is gelatin additive.
[0104] The metal plate I is a pure nickel plate, and the metal plate II is a pure nickel plate.
[0105] The distance between the cathode 1 and the anode 2 is 30 mm, the electrolysis temperature is 40° C., the electrolysis time is 30 min, and the stirring speed of the electrolyte 3 is 300 r / min.
[0106] The current density is 90A / m 2 , a nickel film is formed on the inner surface of cathode 1.
[0107] Example 8
[0108] A method for preparing pure nickel material by electrolysis, the specific implementation method is the same as Example 1, except that the electrolysis time is 40 minutes.
[0109] Performance Testing
[0110] The film thickness was tested using a step profiler, and the film resistivity and square resistance were tested using a four-probe test method.
[0111] The nickel films prepared in Example 1 and Example 8 were used in lithium-ion batteries. The nickel films were used as current collectors and assembled into lithium-ion batteries using a button cell packaging process. The lithium-ion performance of the batteries was tested using an electrochemical workstation and a blue battery test system. The specific capacity and impedance during the charge and discharge process were tested. The specific capacity and impedance diagrams are shown in Figure 12 .
[0112] The resistivity and sheet resistance of the nickel films of Examples 1-4, 6-8 were tested. The test results are shown in Table 1.
[0113] Table 1
[0114] Film thickness / μm Resistivity / μΩ·cm Square resistance mΩ / □ Example 1 4 17.49 9.72 Example 2 8 14.1 17.68 Example 3 10 12.9 11.22 Example 4 8 16.56 11.6 Example 6 10 15.66 15.67 Example 7 4 17.86 13.5 Example 8 6 16.21 9.83
[0115] The nickel powder and nickel film obtained in Example 1 are shown in the following figure: Figure 2 The nickel powder on the cathode is granular and has a high specific surface area, which is conducive to the electrochemical reaction activity; the nickel film on the cathode has a uniform and dense structure, indicating that its conductivity and mechanical integrity are better, and it is suitable as an electrode substrate or active material carrier; the nickel powder scraped from the cathode has a small particle size and obvious particles; the nickel film scraped from the cathode still maintains good continuity and integrity, indicating that its bonding strength with the substrate is high, which can effectively alleviate the volume expansion during charging and discharging and improve the electrode stability.
[0116] The XRD patterns of the nickel powder and nickel film obtained in Example 1 are shown in FIG. Figure 3 ,Depend on Figure 3It can be seen that the crystal plane indices corresponding to the diffraction peaks of nickel powder and nickel film are (111), (200), and (220), and no other impurity peaks appear, indicating that the prepared nickel powder and nickel film are both nickel element.
[0117] The XPS images of nickel powder and nickel film obtained in Example 1 are shown in FIG. Figure 4 The main peak of the O1s spectrum is at 531.98 eV, corresponding to hydroxyl (-OH) or adsorbed water, rather than lattice oxygen (O 2- , ~ 529-530eV); Ni 2p has a main peak at 852.58eV (Ni 0 )、856.28eV(Ni 2+ ) and 873.88eV(Ni 2+ ) shows that the sample is a mixed phase of metallic nickel and nickel compounds, Ni 2+ 2p 3 / 2 (856.28 eV) and 2p 1 / 2 The main peak (873.88eV) indicates that the sample is mainly composed of nickel oxide (NiO) or hydroxide (Ni(OH)2). Satellite peaks: 879.88eV and 876.88eV are typical satellite peaks, generated by coordination effects or electronic interactions. The full spectrum (Survey) verifies the main elements: Ni, O, C, and no other impurity peaks, indicating that the sample composition is pure. The XPS data of the nickel film and the above-mentioned XRD data show that the bulk phase of the nickel film is pure nickel element, and nickel oxide (NiO) and a hydroxylated layer (Ni(OH)2) are formed on the surface of the nickel film due to environmental exposure. The main peak of the C1s binding energy spectrum as the standard spectrum is at 284.88eV.
[0118] The SEM images of the nickel powder and nickel film obtained in Example 1 are shown in FIG. Figure 5 ,Depend on Figure 5 It can be seen that the nickel powder is dendritic, with a conical tip and uniform branching density; the surface of the nickel film is relatively flat, continuous and crack-free, providing a low-impedance electronic conduction network, reducing polarization, and is conducive to improving power density.
[0119] The SEM image of the nickel film obtained in Example 2 is shown in FIG. Figure 6 , Figure 6 At low magnification, the surface of the medium nickel film appears relatively rough, with some granular or blocky objects scattered around, while at high magnification, it exhibits an obvious crack-like structure.
[0120] The SEM image of the nickel film obtained in Example 3 is shown in FIG. Figure 7 , Figure 7 At high magnification, the surface of the medium nickel film has obvious peeling and damaged areas, showing irregular block and flaky structures. At low magnification, the surface has many fine scratches and textures, which are relatively evenly distributed.
[0121] The SEM images of the nickel powder and nickel film obtained in Example 4 are shown in FIG. Figure 8 , Figure 8 The medium nickel powder exhibits an irregular, clustered aggregate morphology. The particles agglomerate to form a structure resembling a grape bunch or coral. The nickel film surface is relatively flat, but exhibits some gully-like or streaky textures, demonstrating a certain degree of directionality.
[0122] The SEM image of the nickel powder obtained in Example 5 is shown in FIG. Figure 9 , Figure 9 At medium and low magnifications, the nickel powder bifurcation is highly symmetrical, with complete network coverage and no agglomeration; at high magnification, the tip is perfectly conical and has no defects.
[0123] The SEM image of the nickel film obtained in Example 6 is shown in Figure 10 , Figure 10 At high magnification, the nickel film exhibits a nanoscale grain structure with good surface uniformity and contains pores or grain boundaries below the micron level. At low magnification, the film continuously covers the substrate with smooth edges and no obvious large-scale defects.
[0124] The SEM image of the nickel film obtained in Example 7 is shown in Figure 11 , Figure 11 At high magnification, the nickel film exhibits a nanoscale grain structure with good surface uniformity and fine granularity. At low magnification, the film continuously covers the substrate with smooth edges and no obvious large-scale defects such as cracks or peeling.
[0125] The nickel films obtained in Example 1 and Example 8 were used as lithium ion battery current collectors for charge and discharge performance tests. The specific capacity of the 4 μm nickel film prepared in Example 1 as a lithium ion battery current collector during the charge and discharge test is shown in the figure. Figure 12 Left, the specific capacity diagram of the 6μm nickel film prepared in Example 8 as a lithium ion battery current collector during the charge and discharge test is shown in Figure 12 The impedance spectra of 4μm nickel film and 6μm nickel film as lithium ion battery current collector are shown in Figure 12 Right. Compared with 6μm nickel film, 4μm nickel film as current collector has higher specific capacity and better cycle performance. This is because 4μm nickel film has better electrical properties and stronger charge transport capability than 6μm nickel film.
Claims
1. A method for preparing pure nickel material by electrolysis, characterized in that: The following steps are involved: S1: prepare electrolyte; S2: Electrolysis reaction: Metal plate I is the cathode, and metal plate II is the anode. The distance between the cathode and anode is adjusted, the current density is controlled, and the electrolysis temperature is maintained. The cathode and anode are inserted into the electrolyte, and the electrolyte undergoes electrolysis reaction under continuous stirring; S3: Product separation: After the reaction is completed, the product is stripped from the cathode and the pure nickel material is collected; The pure nickel material includes dendritic nickel powder and nickel film.
2. The method for preparing pure nickel material by electrolysis according to claim 1, characterized in that: The electrolyte at least includes ammonium chloride, nickel salt, additives and water, and the concentration of the nickel salt in the electrolyte is 1-50 g / L.
3. The method for preparing pure nickel material by electrolysis according to claim 2, characterized in that: The nickel salt includes at least one of nickel sulfate, nickel chloride, nickel sulfamate or nickel acetate.
4. The method for preparing pure nickel material by electrolysis according to claim 2, characterized in that: The additive is a sulfur-containing additive, and the concentration of the additive in the electrolyte is 0.01-0.2 g / L.
5. The method for preparing pure nickel material by electrolysis according to claim 4, characterized in that: The additive includes at least one of sodium lauryl sulfate, gelatin, thiourea or saccharin.
6. The method for preparing pure nickel material by electrolysis according to claim 1, characterized in that: The metal plate I includes at least one of a titanium plate, a stainless steel plate or a pure nickel plate; the metal plate II is an inert metal plate.
7. The method for preparing pure nickel material by electrolysis according to claim 5, characterized in that: The distance between the cathode and the anode is 15-45 mm, the electrolysis temperature is 30-60° C., the electrolysis time is 15-60 min, and the stirring speed of the electrolyte is 200-800 r / min.
8. The method for preparing pure nickel material by electrolysis according to claim 6, characterized in that: The current density is 150-360A / m 2 , including 360A / m 2 , dendritic nickel powder and nickel film are generated on the inner surface of the cathode.
9. The method for preparing pure nickel material by electrolysis according to claim 6, characterized in that: The current density is 360-560A / m 2 , excluding 360A / m 2 , dendritic nickel powder is generated on the inner surface of the cathode, and a nickel film is generated on the outer surface of the cathode.
10. A pure nickel material, characterized in that The nickel powder is prepared by the method for preparing pure nickel material by electrolysis according to any one of claims 1 to 9. The nickel powder has a dendritic morphology, the thickness of the nickel film is 4-6 μm, and the average resistivity of the nickel film is 12-18 μΩ·cm.
Citation Information
Patent Citations
Bright black nickel plating electroplate solution and preparation method and application thereof
CN111270275A
A process for electroless deposition of nickel-containing coating using low temperature solution
CN118374802B