CN116618642B - Nickel powder with large particles and low apparent density and preparation method and application thereof - Google Patents

Nickel powder with large particles and low apparent density and preparation method and application thereof Download PDF

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CN116618642B
CN116618642B CN202310855221.6A CN202310855221A CN116618642B CN 116618642 B CN116618642 B CN 116618642B CN 202310855221 A CN202310855221 A CN 202310855221A CN 116618642 B CN116618642 B CN 116618642B
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nickel powder
particle size
powder
nickel
particles
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CN116618642A (en
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匡怡新
米甘露
陈彬
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CHANGSHA LIYOU METAL MATERIALS CO LTD
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CHANGSHA LIYOU METAL MATERIALS CO LTD
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
    • B01D39/2027—Metallic material
    • B01D39/2031—Metallic material the material being particulate
    • B01D39/2034—Metallic material the material being particulate sintered or bonded by inorganic agents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
    • B01D39/2027—Metallic material
    • B01D39/2051—Metallic foam
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
    • B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
    • C09J9/02—Electrically-conducting adhesives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/045—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by other means than ball or jet milling
    • B22F2009/046—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by other means than ball or jet milling by cutting
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/045—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by other means than ball or jet milling
    • B22F2009/047—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by other means than ball or jet milling by rolling
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention relates to a large-particle nickel powder with low apparent density, a preparation method and application thereof, wherein the nickel powder has a micro porous structure, wide particle size distribution and low apparent density, and the nickel powder is only 0.70-0.95 g/m 3 The method comprises the steps of carrying out a first treatment on the surface of the The purity of the nickel powder is more than or equal to 99.5%, the oxygen content is 0.3-0.4%, and the resistivity is 0.01-0.02 ohms; the nickel powder can be used in products such as conductive adhesive, conductive slurry, sintering activator, metal filtration, battery and the like. Compared with the nickel powder, the invention has wide particle size distribution range, good particle size concentration of a certain specification, can meet the requirements of different glue thicknesses of conductive glue products, can meet the special performances of no sedimentation of the nickel powder mixed with glue in the conductive glue, the nickel powder particles are compressible and easy to deform, the conductive channel stability is good, and the like, and can realize stable application in a large scale. The nickel powder preparation method provided by the invention is simple to operate, and the production and discharge of waste water in the production process are extremely small, so that the nickel powder preparation method is environment-friendly.

Description

Nickel powder with large particles and low apparent density and preparation method and application thereof
Technical Field
The invention belongs to the field of powder metallurgy, relates to a preparation process of nickel powder, and in particular relates to large-particle nickel powder with low apparent density and a preparation method thereof.
Background
The nickel powder has the characteristics of good oxidation resistance, high conductivity, small electric mobility and the like, and has wide application in the aspects of products such as catalysts, sintering activators, conductive slurry, conductive adhesive, metal filtration, batteries and the like.
Currently, the preparation method of nickel powder used in conductive adhesive mainly comprises the following steps: the method has the advantages of simple process, low cost and high powder purity, but has poor crystallinity, easy sintering of the powder and severe toxicity of the hydroxy nickel; the evaporation-condensation method has high purity, good cleanliness and strong oxidation resistance, but has complex equipment, low production efficiency and high cost; gamma-ray radiation synthesis method, the process is immature; the CVD method has the advantages that the powder is in a regular sphere shape, the particle size distribution is uniform, the size is controllable, the crystallinity is good, but special requirements are imposed on the design of the reactor, and the cost is high; high pressure hydrogen reduction process. In addition, there are liquid phase reduction method, microemulsion method, ultrasonic atomization-thermal decomposition method, hydrogen protection mechanical ball milling method and electrolytic method, and the shape and size of electrolytic method are easy to be controlled by current, and the powder is coarse and the energy consumption is high. Some of the above preparation methods have been applied in the industry, but most remain in the test stage and have some drawbacks, requiring products that are not targeted for conductive coupling, low bulk density, large particle size characteristics to meet their application.
For the large-granularity nickel powder which is generally selected for conductive adhesive products and metal filtering products, the requirement on the expansion pore-forming capability of the powder is high, meanwhile, the fluidity of the powder is required to be good, the particle size distribution interval of the nickel powder in the existing products is narrow, and the expansion pore-forming capability of the powder cannot meet the product requirement. The powder prepared by the prior art CN105081347B has a loose ratio of 0.2-0.9 g/m < 3 >, but the nickel powder is superfine nickel powder, the primary particle size is below 1 micron, and the product requirement cannot be met; in addition, substances such as ammonium sulfate, ammonia water, ammonium salt, surfactant and the like are used in the preparation process, so that great wastewater treatment problem is caused.
Therefore, products with large particles and low apparent density are urgently needed in conductive adhesive and metal filtering products, and special requirements of downstream products on raw materials are solved.
Disclosure of Invention
Aiming at the problems, the research team of the invention obtains the novel nickel powder through a large number of experiments, has porous large granularity and low apparent density, and has more excellent performance while meeting the product requirements after long-term research. Meanwhile, research and development personnel continuously optimize the process to determine the preparation method of the novel nickel powder.
Therefore, in one aspect, the invention provides a large-particle nickel powder with low apparent density, wherein the particle size distribution range of the nickel powder is 5-250 mu m, the nickel powder is of a micro-porous structure, and the apparent density is 0.70-0.95 g/m3;
further, the nickel powder has particles with the particle size distribution of 30-250 mu m and the proportion of 40-80%; the total amount of iron, copper, aluminum and manganese in the nickel powder is less than or equal to 0.05wt percent, and the balance is nickel; the oxygen content of the nickel powder is 0.33-0.40wt% and the resistivity is 0.01-0.02 ohms.
Further, the micro-porous structure of the nickel powder disclosed by the invention is a porous sponge-like structure.
Further, the total amount of iron, copper, aluminum and manganese in the nickel powder is 0.02-0.03wt%, wherein the copper content is less than or equal to 0.015wt%.
Furthermore, the purity of the nickel powder is more than or equal to 99.5 percent.
The particle size distribution range of the nickel powder is wide, and the nickel powder is expanded from 10 mu m to 250 mu m, so that the selectivity of the product is enlarged. Meanwhile, more researches focus on the direction of superfine nickel powder, and the application of large-particle nickel powder is focused on a small amount, and the application range of the nickel powder is affected.
The nickel powder is porous powder, has high specific surface, and has large granularity control interval selectivity and small apparent density compared with atomized nickel powder/electrolytic nickel powder. And the number of powder particles in the same particle size range is 2-4 times of that of atomized nickel powder and 1.5-2 times of that of electrolytic nickel powder.
The main impurity metals in the nickel powder of the invention are iron, copper, aluminum and manganese, and the content of metal impurities is controlled below 0.05 percent. On the one hand, impurities can affect the physical properties of nickel powder, especially the content control of impurity copper, and when the copper content exceeds 0.015%, copper can generate copper compounds under the acidic formula condition of the adhesive tape product to form spots, thereby affecting the adhesive tape performance. And simultaneously affects the conductivity and the expansion pore-forming capability of the nickel powder.
On the other hand, the invention also provides a preparation method of the large-particle nickel powder with low apparent density, which sequentially comprises the following steps: wet mixing, drying, multi-stage shearing crushing, granulating, low-temperature reduction, rolling-scattering, heating, solid-phase diffusion sintering, crushing, screening and vacuum packaging.
Further, the raw material wet mixing step in the preparation method of the nickel powder comprises the following steps: mixing a proper amount of nickel carbonyl powder with an oxalic acid solution with the concentration of 5% -20%, adding a proper amount of hydrogen peroxide as an oxidant, and reacting for 2.5-3 hours to form a gray green slurry; the temperature of the gray green slurry is 30-50 ℃; the temperature of the oxalic acid solution is 70-95 ℃, and the proportion of the hydroxy nickel powder and the oxalic acid solution is such that no oxalic acid is separated out from the mixed solution.
Further, in the preparation method of the nickel powder, the particle size of the carbonyl nickel powder is 1-3 mu m, belongs to superfine nickel powder, and is treated by reducing gas atmosphere at the low temperature of 380-450 ℃; the mass fraction of the hydrogen peroxide in the reaction solution is 0.05-0.1%.
The reaction of the hydroxy nickel powder and oxalic acid is exothermic, the reaction speed of the oxidant is accelerated, and the nickel powder subjected to reduction treatment at the temperature of 380-450 ℃ can form a certain counter balance with the oxidant by adding 70-95 ℃ oxalic acid solution, so that the two can control the reaction speed, and the bulk density of the nickel powder is further controlled by combining the control of the reaction time. The proportion of the hydroxy nickel powder to the oxalic acid is only needed to observe that no oxalic acid is separated out from the mixed solution, so that the process difficulty is reduced. The concentration, temperature, reaction time, etc. of the oxalic acid solution form a key link for reducing the bulk density. In this step, the particle size of the raw ultrafine nickel powder is inversely related to the concentration of oxalic acid.
Further, the drying step in the preparation method of the nickel powder of the invention comprises the following steps: and (3) placing the slurry into a static electric heating oven, heating the oven to 150-220 ℃ at a speed of 35-55 ℃/h, and baking for 12-16h to finish drying to obtain a slurry block.
The drying process can be carried out after the reacted slurry is cooled to room temperature, or can be carried out directly by drying the gray green slurry at 30-50 ℃. The drying process cannot be performed at an excessively high temperature rise rate, otherwise the pore density of the nickel powder is affected, and the final bulk density and strength of the nickel powder are further affected.
Further, in the preparation method of the nickel powder, the slurry block is subjected to multistage shearing crushing to obtain nickel powder microparticles with the granularity of less than 2 mu m; and granulating by adopting granulating equipment to obtain coarse nickel powder particles.
In the preparation method of the nickel powder, the dried slurry is still a block, and the preparation method adopts multistage shearing type crushing, so that the production efficiency is high, and fine particles can be produced.
Further, in the rolling-scattering step in the preparation method of the nickel powder, quick feeding is adopted to pass through rolling equipment; wherein the feeding speed is 1.25-1.8kg/min, the double-roller clearance of the rolling equipment is 1.5-3mm, and the rotating speed is 25-30r/min.
The particles are rolled in a rolling-scattering mode, so that the feeding speed, the roller rotating speed and the roller gap are well controlled, and the pore and fluffy state of the particles can be better kept. The feeding speed and the rotating speed of the roller are in a certain matching relationship, so that the bulk of the particles is ensured on one hand, and the production efficiency is ensured on the other hand.
Further, in the preparation method of the nickel powder, the crushing stage number in the multistage shear type crushing step is 3-5, and the particle size distribution of the crushed nickel powder microparticles is 1-1.5 mu m.
In the preparation method of the nickel powder, the low-temperature reduction step adopts hydrogen to reduce the nickel powder microparticles, the reduction temperature is 355-480 ℃, the reduction time is 2-4 hours, and the reduced nickel powder microparticles are obtained and are in a bulk shape or a small loose block shape.
The reduction temperature in the low-temperature reduction step cannot be too high, particles can be hardened in a very short time when the reduction temperature exceeds 480 ℃, and the particles can be hardened when the reduction time is too long, so that the required particle size cannot be obtained. If the temperature is too low or the time is insufficient, there is a phenomenon that reduction is not performed or insufficient and uneven reduction occurs. Further, the preferable reduction temperature is 380-450 ℃ and the reduction time is 2-2.5h.
Further, in the preparation method of the nickel powder, the granulating step adopts a rolling method, a centrifugal method or a high-speed stirring method, ethylene glycol or wax is used as a binder, the addition amount of the binder is 35-110mL/kg, and the particle size distribution of the prepared nickel powder coarse particles is 1.0-3.5mm.
In the metal powder granulating process, along with the increase of the addition amount of the binder, the particle size of the particles becomes larger, the granulating rate is increased sharply, and the fine powder rate is reduced; when the binder is added to a certain amount, the granulation rate is highest, and the particle shape is good; thereafter, as the amount of the binder added increases, the granulation rate increases slowly. The particles become longer on the sides and the flowability of the particles becomes worse. The size and strength of the metal particles increase with the increase of the binder, but too much binder can damage the granulating equipment, and the binding force of different metal particles to the binder is different. On the other hand, the apparent density of the nickel powder and the addition amount of the binder also show a certain linear relation. Finally, various factors are combined to obtain the optimal addition amount of the binder.
Further, in the preparation method of the nickel powder of the invention, the heating solid-phase diffusion sintering step comprises the following steps: and (3) placing the rolled material obtained in the rolling-scattering step in a reducing atmosphere, and sintering at 680-750 ℃ for 3-5h.
The temperature required for the warming solid phase diffusion step is approximately 2 times the reduction temperature in the above-mentioned low temperature reduction step. Because the nickel powder particles after rolling and scattering can be in a high-activity state at the high temperature of 680-750 ℃, the particles can be further fused, the structure is more stable, and the strength of the nickel powder is improved.
In the preparation method of the nickel powder, the crushing step adopts a hammer crusher to carry out rapid crushing, and the screening step adopts a vibrating screen to carry out particle size separation, so that 3-6 particle size distribution grades are separated.
The invention also provides application of the large-particle low-apparent-density nickel powder in conductive adhesive products.
The invention also provides another application of the large-particle nickel powder with low apparent density, and the nickel powder is used for conductive adhesive products.
Compared with the prior art, the invention has the following beneficial technical effects:
the nickel powder has good powder fluidity, is porous powder, has small loose density and high specific surface; the number of powder particles per unit weight in the same granularity range is 2-4 times that of atomized nickel powder, and the number of the nickel powder is 1.5-2 times that of electrolytic nickel powder. The particle size distribution range of the nickel powder is wide, compared with the particle size control interval selectivity of atomized nickel powder and electrolytic nickel powder, the selectivity of the product is enlarged, and the application range of large particles is further widened. In addition, the nickel powder of the present invention has high strength.
Compared with the nickel powder product prepared by the conventional electrolytic nickel powder and carbonyl nickel powder process, the nickel powder disclosed by the invention has the advantages that the expansion pore-forming capability of the nickel powder is obviously improved by 2-2.5 times, and the structural strength, the pore uniformity, the pore throughout and the pore diameter uniformity of the product are all improved.
The nickel powder disclosed by the invention has the advantages of larger particle size distribution range and larger interval selectivity, realizes the thickness specification application of more types of glue in the application of conductive glue products, meets various special requirements of non-sedimentation of conductive particles and glue in the conductive glue products, compressive deformability of product particles, stability of conductive channels and the like, and realizes the stable application in a large scale. The nickel powder can also be used in products such as conductive slurry, sintering activator, battery and the like.
The invention has simple preparation process, little waste water generation and discharge in the production process, and environmental protection and green.
Drawings
FIG. 1 is a diagram of the process steps of the present invention;
FIG. 2 is a 200-fold magnification microscopic morphology of nickel powder according to the present invention;
FIG. 3 is a graph of the microscopic morphology of the nickel powder of the present invention at 5000 times magnification.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments and examples.
Specifically, the invention provides large-particle nickel powder with low apparent density, the nickel powder is of a micro-porous structure, the particle size distribution range of the nickel powder is 5-250 mu m, and the apparent density is 0.70-0.95 g/m < 3 >; wherein, the particle size distribution of the nickel powder is 30-250 μm, and the proportion of the particles is 40-80%; the total amount of iron, copper, aluminum and manganese in the nickel powder is less than or equal to 0.05wt percent, and the balance is nickel; the oxygen content of the nickel powder is 0.33-0.40wt% and the resistivity is 0.01-0.02 ohms. As shown in fig. 2 and 3, a microscopic topography of the nickel powder is shown.
The micro porous structure of the nickel powder is a porous sponge structure, and the total amount of iron, copper, aluminum and manganese in the nickel powder is 0.02-0.03wt%, wherein the copper content is less than or equal to 0.015wt%.
As shown in FIG. 1, the invention also provides a preparation method of the large-particle nickel powder with low apparent density, which sequentially comprises the following steps: wet mixing, drying, multi-stage shearing crushing, granulating, low-temperature reduction, rolling-scattering, heating, solid-phase diffusion sintering, crushing, screening and vacuum packaging;
the wet mixing step of the raw materials comprises the following steps: mixing a proper amount of nickel carbonyl powder with an oxalic acid solution with the concentration of 5% -20%, adding a proper amount of hydrogen peroxide as an oxidant, and reacting for 2.5-3 hours to form a gray green slurry with the temperature of 30-50 ℃; the temperature of the oxalic acid solution is 70-95 ℃; the particle size of the carbonyl nickel powder is 1-3 mu m, and the carbonyl nickel powder is treated by a reducing gas atmosphere at the low temperature of 380-450 ℃; the mass fraction of the hydrogen peroxide in the reaction solution is 0.05-0.1%.
In addition, the proportion of the hydroxy nickel powder to the oxalic acid solution has no specific requirement, and is determined according to the required quantity; but the proportion of the hydroxy nickel powder and the oxalic acid solution satisfies the best condition that no oxalic acid is precipitated in the mixed solution.
The drying step comprises the following steps: and (3) placing the green-gray slurry into a static electric heating oven, heating the oven to 150-220 ℃ at a speed of 35-55 ℃/h, and baking for 12-16h to finish drying to obtain a slurry block.
Carrying out multistage shearing crushing on the slurry block to obtain nickel powder microparticles with the granularity of less than 2 mu m; in the multistage shearing type crushing step, the crushing stage number is 3-5, and the particle size distribution of the nickel powder microparticles obtained by crushing is 1-1.5 mu m.
Granulating by adopting granulating equipment to obtain coarse nickel powder particles; the granulating step adopts a rolling method, a centrifugal method or a high-speed stirring method, ethylene glycol or wax is used as a binder, the addition amount of the binder is 40-100mL/kg, and the particle size distribution of the nickel powder coarse particles is 1.0-3.5mm.
The low-temperature reduction step adopts hydrogen to reduce the nickel powder microparticles, the reduction temperature is 355-480 ℃, the reduction time is 2-4 hours, and the reduced nickel powder microparticles are obtained and are in a bulk shape or a small loose block shape.
In the rolling-scattering step, quick feeding is adopted to pass through rolling equipment; wherein the feeding speed is 1.25-1.8kg/min, the double-roller clearance of the rolling equipment is 1.5-3mm, and the rotating speed is 25-30r/min.
The heating solid phase diffusion sintering step comprises the following steps: and (3) placing the rolled material obtained in the rolling-scattering step in a reducing atmosphere, and sintering at 680-750 ℃ for 3-5h.
The crushing step adopts a hammer crusher to carry out rapid crushing, and adopts a vibrating screen to carry out particle size sorting in the screening step, so as to separate 3-6 particle size grades.
The preparation method of the nickel powder can obtain the nickel powder microstructure shown in fig. 2 and 3.
The invention also provides application of the large-particle nickel powder with low apparent density, and the nickel powder is used for porous metal filtering products. Another use of the nickel powder is provided for the conductive adhesive product.
Specific embodiments are described in further detail.
Example 1
The large-particle nickel powder with low apparent density has the particle size distribution range of 5-250 mu m, is of a micro-porous structure and has the apparent density of 0.70-0.95 g/m < 3 >; the proportion of particles with the particle size distribution of 30-250 μm in the nickel powder is 40-80%; the total amount of iron, copper, aluminum and manganese in the nickel powder is less than or equal to 0.05wt percent, and the balance is the nickel powder; the oxygen content of the nickel powder is 0.33-0.40wt% and the resistivity is 0.01-0.02 ohms.
The nickel powder is adopted to sinter and prepare the metal filter element in the porous metal filter product.
The nickel powder of the embodiment has good powder fluidity, is porous powder, has small loose density and high specific surface; the number of powder particles per unit weight in the same granularity range is 2-4 times that of atomized nickel powder, and the number of the nickel powder is 1.5-2 times that of electrolytic nickel powder. The particle size distribution range of the nickel powder is wide, compared with the particle size control interval selectivity of atomized nickel powder and electrolytic nickel powder, the selectivity of the product is enlarged, and the application range of large particles is further widened. In addition, the nickel powder of the present invention has high strength.
Compared with the metal filter element product prepared by sintering the nickel powder prepared by the conventional electrolytic nickel powder and carbonyl nickel powder process, the expansion pore-forming capability of the nickel powder is obviously improved by 2-2.5 times, and the structural strength, the pore uniformity, the pore throughout and the pore diameter consistency of the product are all improved.
Example 2
The large-particle nickel powder with low apparent density has the particle size distribution range of 5-250 mu m, is of a micro-porous structure and has the apparent density of 0.70-0.95 g/m < 3 >; the proportion of particles with the particle size distribution of 30-250 μm in the nickel powder is 40-80%; the total amount of iron, copper, aluminum and manganese in the nickel powder is less than or equal to 0.05wt percent, and the balance is the nickel powder; the oxygen content of the nickel powder is 0.33-0.40wt% and the resistivity is 0.01-0.02 ohms.
The 150-250 mu m nickel powder is adopted to prepare the conductive adhesive with the thickness of 0.2 mm.
The nickel powder of the embodiment has good powder fluidity, is porous powder, has small loose density and high specific surface; the number of powder particles per unit weight in the same granularity range is 2-4 times that of atomized nickel powder, and the number of the nickel powder is 1.5-2 times that of electrolytic nickel powder. The particle size distribution range of the nickel powder is wide, compared with the particle size control interval selectivity of atomized nickel powder and electrolytic nickel powder, the selectivity of the product is enlarged, and the application range of large particles is further widened. In addition, the nickel powder of the present invention has high strength.
The conductive adhesive prepared from the nickel powder can meet various special requirements of non-settlement of conductive particles and glue in conductive adhesive products, compressibility deformability of product particles, stability of conductive channels and the like, and can be stably applied in a large scale.
Example 3
This embodiment differs from embodiment 2 only in that: the conductive adhesive with the thickness of 0.04mm is prepared by adopting the nickel powder with the thickness of 5-50 mu m.
The nickel powder of the embodiment has good powder fluidity, is porous powder, has small loose density and high specific surface; the number of powder particles per unit weight in the same granularity range is 2-4 times that of atomized nickel powder, and the number of the nickel powder is 1.5-2 times that of electrolytic nickel powder. The particle size distribution range of the nickel powder is wide, compared with the particle size control interval selectivity of atomized nickel powder and electrolytic nickel powder, the selectivity of the product is enlarged, and the application range of large particles is further widened. In addition, the nickel powder of the present invention has high strength.
The conductive adhesive prepared from the nickel powder can meet various special requirements of non-settlement of conductive particles and glue in conductive adhesive products, compressibility deformability of product particles, stability of conductive channels and the like, and can be stably applied in a large scale.
Example 4
This embodiment differs from embodiment 1 only in that: the micro porous structure of the nickel powder is a porous sponge structure. The total content of iron, copper, aluminum and manganese in the nickel powder is 0.02-0.03wt%, wherein the copper content is less than or equal to 0.015wt%.
The nickel powder of the embodiment has good powder fluidity, is porous powder, has small loose density and high specific surface; the number of powder particles per unit weight in the same granularity range is 2-4 times that of atomized nickel powder, and the number of the nickel powder is 1.5-2 times that of electrolytic nickel powder. The particle size distribution range of the nickel powder is wide, compared with the particle size control interval selectivity of atomized nickel powder and electrolytic nickel powder, the selectivity of the product is enlarged, and the application range of large particles is further widened. In addition, the nickel powder of the present invention has high strength.
Compared with the metal filter element product prepared by sintering the nickel powder prepared by the conventional electrolytic nickel powder and carbonyl nickel powder process, the expansion pore-forming capability of the nickel powder is obviously improved by 2-2.5 times, and the structural strength, the pore uniformity, the pore throughout and the pore diameter consistency of the product are all improved.
Example 5
This embodiment differs from embodiment 2 only in that: the micro porous structure of the nickel powder is a porous sponge structure. The total content of iron, copper, aluminum and manganese in the nickel powder is 0.02-0.03wt%, wherein the copper content is less than or equal to 0.015wt%.
The nickel powder of the embodiment has good powder fluidity, is porous powder, has small loose density and high specific surface; the number of powder particles per unit weight in the same granularity range is 2-4 times that of atomized nickel powder, and the number of the nickel powder is 1.5-2 times that of electrolytic nickel powder. The particle size distribution range of the nickel powder is wide, compared with the particle size control interval selectivity of atomized nickel powder and electrolytic nickel powder, the selectivity of the product is enlarged, and the application range of large particles is further widened. In addition, the nickel powder of the present invention has high strength.
The conductive adhesive prepared from the nickel powder can meet various special requirements of non-settlement of conductive particles and glue in conductive adhesive products, compressibility deformability of product particles, stability of conductive channels and the like, and can be stably applied in a large scale.
Example 6
Embodiment 6 of the present invention is a method for preparing the above large-particle nickel powder with low bulk density, which sequentially comprises the following steps: wet mixing, drying, multi-stage shearing crushing, granulating, low-temperature reduction, rolling-scattering, heating, solid-phase diffusion sintering, crushing, screening and vacuum packaging.
The wet mixing step of the raw materials comprises the following steps: mixing a proper amount of nickel carbonyl powder with an oxalic acid solution with the concentration of 5% -20%, adding a proper amount of hydrogen peroxide as an oxidant, and reacting for 2.5-3 hours to form a gray green slurry; the temperature of the gray green slurry is 30-50 ℃; the temperature of the oxalic acid solution is 70-95 ℃, and the proportion of the hydroxyl nickel powder and the oxalic acid solution is satisfied that no oxalic acid is separated out from the mixed solution.
The particle size of the carbonyl nickel powder is 1-3 mu m, belongs to superfine nickel powder, and is treated in a reducing gas atmosphere at a low temperature of 380-450 ℃; the mass fraction of the hydrogen peroxide in the reaction solution is 0.05-0.1%.
The drying step comprises the following steps: and (3) placing the slurry into a static electric heating oven, heating the oven to 150-220 ℃ at a speed of 35-55 ℃/h, and baking for 12-16h to finish drying to obtain a slurry block.
Carrying out multistage shearing crushing on the slurry block to obtain nickel powder microparticles with the granularity of less than 2 mu m; and granulating by adopting granulating equipment to obtain coarse nickel powder particles. The dried slurry is still in a block shape, and is crushed by adopting multistage shearing type, wherein the crushing stage number in the multistage shearing type crushing step is 3-5, so that the gap and fluffy state of particles can be better kept.
In the rolling-scattering step, quick feeding is adopted to pass through rolling equipment; wherein the feeding speed is 1.25-1.8kg/min, the double-roller clearance of the rolling equipment is 1.5-3mm, and the rotating speed is 25-30r/min. And the solid-phase sintering step is to place the rolled material obtained in the rolling-scattering step in a reducing atmosphere, and sinter the rolled material for 3 to 5 hours at 680 to 750 ℃. And (3) performing a low-temperature reduction step, namely reducing the nickel powder microparticles by adopting hydrogen at 355-480 ℃ for 2-4 hours to obtain reduced nickel powder microparticles which are in a bulk or small loose block shape. Then granulating, rolling, centrifuging or stirring at high speed, using ethylene glycol or wax as binder, wherein the binder is added at 40-100mL/kg, and the particle size distribution of coarse nickel powder particles is 1.0-3.5mm. Then a hammer crusher is adopted to carry out rapid crushing, and a vibrating screen is used to carry out granularity screening and sorting, and 3-6 nickel powder particles with granularity grades are separated.
The nickel powder with large particles and low apparent density is prepared by the embodiment, the particle size distribution range of the nickel powder is 5-250 mu m, the nickel powder is of a micro porous structure, and the apparent density is 0.70-0.95 g/m3; the proportion of particles with the particle size distribution of 30-250 μm in the nickel powder is 40-80%; the total amount of iron, copper, aluminum and manganese in the nickel powder is less than or equal to 0.05wt percent, and the purity of the nickel powder is more than or equal to 99.5 percent; the oxygen content of the nickel powder is 0.33-0.40wt% and the resistivity is 0.01-0.02 ohms.
Example 7
This embodiment differs from embodiment 6 only in that: mixing a proper amount of nickel carbonyl powder with an oxalic acid solution with the concentration of 20%, and adding a proper amount of hydrogen peroxide as an oxidant to react for 2.5 hours; the temperature of the oxalic acid solution is 80-95 ℃, and the mass fraction of hydrogen peroxide in the reaction solution is 0.05%.
The nickel powder with large particles and low apparent density is prepared in the embodiment, the particle size distribution range of the nickel powder is 5-250 mu m, and the apparent density is 0.75-0.88g/m < 3 >; the particle ratio of particles with the particle size distribution of 30-250 μm in the nickel powder is 45-80%; the total amount of iron, copper, aluminum and manganese in the nickel powder is 0.03 weight percent, and the copper content is less than or equal to 0.010 weight percent; the oxygen content of the nickel powder was 0.33wt% and the resistivity was 0.01 ohm.
Example 8
This embodiment differs from embodiment 6 only in that: mixing a proper amount of nickel carbonyl powder with an oxalic acid solution with the concentration of 15%, adding a proper amount of hydrogen peroxide as an oxidant, and reacting for 2.5 hours, wherein the temperature of the oxalic acid solution is 75-85 ℃. The carbonyl nickel powder is superfine nickel powder with the diameter of 1-3 mu m, and is treated in the atmosphere of reducing gas at the low temperature of 450 ℃; the mass fraction of hydrogen peroxide in the reaction solution is 0.08%.
The nickel powder with large particles and low apparent density is prepared in the embodiment, the particle size distribution range of the nickel powder is 5-250 mu m, and the apparent density is 0.80-0.95 g/m3; the proportion of particles with the particle size distribution of 30-250 μm in the nickel powder is 40-80%; the total weight of iron, copper, aluminum and manganese in the nickel powder is 0.02 percent, and the copper content is less than or equal to 0.010 percent; the oxygen content of the nickel powder was 0.40wt% and the resistivity was 0.018 ohms.
Example 9
This embodiment differs from embodiment 6 only in that: mixing a proper amount of nickel carbonyl powder with 5% oxalic acid solution, adding a proper amount of hydrogen peroxide as an oxidant, and reacting for 3 hours; the temperature of the oxalic acid solution was 95 ℃. The carbonyl nickel powder is superfine nickel powder with the diameter of 1-3 mu m, and is treated in the atmosphere of reducing gas at the low temperature of 380 ℃; the mass fraction of hydrogen peroxide in the reaction solution is 0.1%.
The nickel powder with large particles and low apparent density is prepared in the embodiment, the particle size distribution range of the nickel powder is 5-250 mu m, and the apparent density is 0.70-0.95 g/m3; the particle ratio of particles with the particle size distribution of 30-250 μm in the nickel powder is 45-75%; the total amount of iron, copper, aluminum and manganese in the nickel powder is less than or equal to 0.03wt%; the oxygen content of the nickel powder was 0.38wt% and the resistivity was 0.02 ohms.
Example 10
This embodiment differs from embodiment 6 only in that: mixing a proper amount of nickel carbonyl powder with an oxalic acid solution with the concentration of 10%, and adding a proper amount of hydrogen peroxide as an oxidant to react for 3 hours; the temperature of the oxalic acid solution was 90 ℃. The nickel carbonyl powder is superfine nickel powder with the diameter of 1-3 mu m, and is treated in the atmosphere of reducing gas at the low temperature of 400 ℃; the mass fraction of hydrogen peroxide in the reaction solution is 0.09%.
The nickel powder with large particles and low apparent density is prepared in the embodiment, the particle size distribution range of the nickel powder is 15-250 mu m, the nickel powder is of a micro porous structure, and the apparent density is 0.78-0.93 g/m3; the proportion of particles with the particle size distribution of 30-250 mu m in the nickel powder is 50-80%; the total amount of iron, copper, aluminum and manganese in the nickel powder is 0.03wt%, the oxygen content of the nickel powder is 0.40wt% and the resistivity is 0.02 ohm.
Example 11
This embodiment differs from embodiment 6 only in that: the particle size distribution of the nickel powder microparticles obtained by multistage shearing crushing is 1.2-1.5 mu m.
The particle size distribution range of the nickel powder is 10-250 mu m, the nickel powder is of a micro porous structure, and the loose density is 0.70-0.87 g/m < 3 >; the particle ratio of particles with the particle size distribution of 30-250 μm in the nickel powder is 48-76%; the total amount of iron, copper, aluminum and manganese in the nickel powder is less than or equal to 0.05wt percent, and the balance is the nickel powder; the oxygen content of the nickel powder is 0.33-0.40wt% and the resistivity is 0.01-0.02 ohms.
Example 12
This embodiment differs from embodiment 6 only in that: the reduction temperature in the low-temperature reduction step is 360 ℃ and the reduction time is 4 hours.
The nickel powder with large particles and low apparent density is prepared by the embodiment, the particle size distribution range of the nickel powder is 5-250 mu m, the nickel powder is of a micro porous structure, and the apparent density is 0.77-0.93 g/m3; the particle ratio of particles with the particle size distribution of 30-250 μm in the nickel powder is 54-68%; the total amount of iron, copper, aluminum and manganese in the nickel powder was 0.028wt%, the oxygen content of the nickel powder was 0.33wt%, and the resistivity was 0.01 ohm.
Example 13
This embodiment differs from embodiment 6 only in that: the reduction temperature in the low-temperature reduction step is 480 ℃ and the reduction time is 2.5h.
The nickel powder with large particles and low apparent density is prepared in the embodiment, the particle size distribution range of the nickel powder is 5-250 mu m, the nickel powder is of a micro-porous structure, and the apparent density is 0.70-0.83 g/m3; the particle ratio of particles with the particle size distribution of 30-250 μm in the nickel powder is 56-75%; the total amount of iron, copper, aluminum and manganese in the nickel powder was 0.02wt%, the oxygen content of the nickel powder was 0.33wt%, and the resistivity was 0.01 ohm.
Example 14
This embodiment differs from embodiment 6 only in that: in the rolling-scattering step, the feeding speed is 1.7kg/min, the double-roller gap of the rolling equipment is 3mm, and the rotating speed is 25r/min.
The nickel powder with large particles and low apparent density is prepared by the embodiment, the particle size distribution range of the nickel powder is 5-200 mu m, the nickel powder is of a micro-porous structure, and the apparent density is 0.70-0.85 g/m3; the particle ratio of particles with the particle size distribution of 30-200 mu m in the nickel powder is 56-80%; the total amount of iron, copper, aluminum and manganese in the nickel powder is less than or equal to 0.05 weight percent, the oxygen content of the nickel powder is 0.33-0.40 weight percent, and the resistivity is 0.01-0.02 ohms.
Example 15
This embodiment differs from embodiment 6 only in that: in the rolling-scattering step, the feeding speed was 1.3kg/min, the twin-roll gap of the rolling apparatus was 2.5mm, and the rotational speed was 27r/min.
The nickel powder with large particles and low apparent density is prepared in the embodiment, the particle size distribution range of the nickel powder is 10-220 mu m, the nickel powder is of a micro-porous structure, and the apparent density is 0.75-0.90 g/m3; the proportion of particles with the particle size distribution of 30-220 mu m in the nickel powder is 50-70%; the total amount of iron, copper, aluminum and manganese in the nickel powder is less than or equal to 0.03 weight percent, the oxygen content of the nickel powder is 0.33-0.40 weight percent, and the resistivity is 0.01-0.02 ohms.
Example 16
This embodiment differs from embodiment 6 only in that: in the solid-phase sintering step, the reduction treatment temperature is 750 ℃ and the sintering treatment is 4.5 hours.
The nickel powder with large particles and low apparent density is prepared in the embodiment, the particle size distribution range of the nickel powder is 5-250 mu m, and the apparent density is 0.70-0.85 g/m3; the proportion of particles with the particle size distribution of 30-250 μm in the nickel powder is 40-60%; the total amount of iron, copper, aluminum and manganese in the nickel powder is less than or equal to 0.03 weight percent, and the balance is the nickel powder; the oxygen content of the nickel powder is 0.35-0.40wt% and the resistivity is 0.01-0.02 ohms.
Example 17
This embodiment differs from embodiment 6 only in that: in the solid-phase sintering step, the reduction treatment temperature is 680 ℃ and the sintering treatment is carried out for 5 hours.
The nickel powder with large particles and low apparent density is prepared in the embodiment, the particle size distribution range of the nickel powder is 5-250 mu m, and the apparent density is 0.85-0.95 g/m3; the proportion of particles with the particle size distribution of 30-250 μm in the nickel powder is 40-50%; the total amount of iron, copper, aluminum and manganese in the nickel powder is less than or equal to 0.03 weight percent, the oxygen content of the nickel powder is 0.33-0.40 weight percent, and the resistivity is 0.01-0.02 ohms.
Example 18:
the large-particle nickel powder with low apparent density is used for porous metal filtering products.
Example 19:
the large-particle nickel powder with low apparent density is used for conductive adhesive products.
Comparative example 1
This comparative example differs from example 6 only in that: mixing a proper amount of nickel carbonyl powder with an oxalic acid solution with the concentration of 30%, and adding a proper amount of hydrogen peroxide as an oxidant to react for 1h; the temperature of the oxalic acid solution was 55 ℃.
The nickel carbonyl powder is 10 mu m powder, and is treated in a reducing gas atmosphere at a low temperature of 550 ℃; the mass fraction of hydrogen peroxide in the reaction solution is 0.7%.
The comparative example produced large particle nickel powder with low bulk density, the particle size distribution range of the nickel powder was 100-150 μm, the bulk density was 2.5 g/m3, the total of iron, copper, aluminum, manganese in the nickel powder was 0.18wt%, the oxygen content of the nickel powder was 0.8wt%, and the resistivity was 0.08 ohms.
Comparative example 2
This comparative example differs from example 6 only in that: mixing a proper amount of nickel carbonyl powder with an oxalic acid solution with the concentration of 4%, and adding a proper amount of hydrogen peroxide as an oxidant for reaction for 5 hours; the temperature of the oxalic acid solution was 120 ℃.
The nickel carbonyl powder is 0.5 mu m powder, and is treated in a reducing gas atmosphere at a low temperature of 350 ℃; the mass fraction of hydrogen peroxide in the reaction solution is 0.3%.
The comparative example produced large particle nickel powder with low bulk density, the particle size distribution range of the nickel powder was 10-50 μm, the bulk density was 1.2g/m3, the total of iron, copper, aluminum, manganese in the nickel powder was 0.1wt%, the oxygen content of the nickel powder was 0.5wt%, and the resistivity was 0.06 ohms.
Comparative example 3
This comparative example differs from example 6 only in that: in the rolling-scattering step, the feeding speed is 2kg/min, the double-roller gap of the rolling equipment is 5mm, and the rotating speed is 38 r/min.
The comparative example produced large particle low bulk density nickel powder having a bulk density of 2.3 g/m3.
Comparative example 4
This comparative example differs from example 6 only in that: in the solid-phase sintering step, the reduction treatment temperature is 700 ℃ and the sintering treatment is carried out for 2 hours.
The comparative example produced large particle low bulk density nickel powder having a bulk density of 2.5 g/m3; the oxygen content of the nickel powder was 0.6wt% and the resistivity was 0.1 ohm.
The nickel powder prepared in the embodiments 6-17 has good powder fluidity, is porous powder, has small loose density and high specific surface; the number of powder particles per unit weight in the same granularity range is 2-4 times that of atomized nickel powder, and the number of the nickel powder is 1.5-2 times that of electrolytic nickel powder. The nickel powder has wide particle size distribution range, and compared with atomized nickel powder and electrolytic nickel powder, the nickel powder has large particle size control interval selectivity, and can be used in conductive slurry, sintering activator, battery and other products. In addition, the nickel powder of the present invention has high strength.
In the production and application of the porous metal filtering product, compared with the nickel powder product prepared by the conventional electrolytic nickel powder and carbonyl nickel powder process, the nickel powder prepared by the method has the advantages that the expansion pore-forming capacity of the nickel powder is obviously improved by 2-2.5 times, and the structural strength, the pore uniformity, the pore throughout and the pore diameter consistency of the product are all improved.
The nickel powder prepared in the embodiments 6-17 has larger particle size distribution range and interval selectivity, realizes the thickness specification application of more glue in the application of conductive glue products, meets various special requirements of non-sedimentation of conductive particles and glue in the conductive glue products, the compressibility deformability of product particles, the stability of conductive channels and the like, and realizes the stable application in a large scale.
The preparation process of the nickel powder in the embodiments 6-17 is simple, the generation and the discharge of waste water in the production process are few, and the environment is protected.
The foregoing description of the preferred embodiments of the present disclosure is not intended to limit the disclosure to the particular embodiments disclosed, but on the contrary, the intention is to cover all modifications, equivalents, alternatives, and alternatives falling within the spirit and principles of the disclosure. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from its scope. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.
It will be appreciated that the present disclosure is not limited to the features already described above and that various modifications or changes may be made without departing from the scope thereof. The scope of the present disclosure is limited only by the appended claims.

Claims (9)

1. The nickel powder with large particles and low apparent density is characterized in that the nickel powder has a micro porous structure, the particle size distribution range of the nickel powder is 5-250 mu m, and the apparent density is 0.70-0.95 g/m 3 The method comprises the steps of carrying out a first treatment on the surface of the Wherein, the particle size distribution of the nickel powder is 30-250 μm, and the proportion of the particles is 40-80%; the total amount of iron, copper, aluminum and manganese in the nickel powder is less than or equal to 0.05wt percent, and the balance is nickel; the oxygen content of the nickel powder is 0.33-0.40wt% and the resistivity is 0.01-0.02 ohms.
2. The nickel powder according to claim 1, wherein the micro porous structure is a porous sponge structure, and the total amount of iron, copper, aluminum and manganese in the nickel powder is 0.02-0.03wt%, wherein the copper content is less than or equal to 0.015wt%.
3. A process for producing the large-particle low-bulk nickel powder according to any one of claims 1 or 2, characterized in that: the preparation method sequentially comprises the following steps: wet mixing, drying, multi-stage shearing crushing, granulating, low-temperature reduction, rolling-scattering, heating, solid-phase diffusion sintering, crushing, screening and vacuum packaging;
the raw material wet mixing step comprises the following steps: mixing a proper amount of nickel carbonyl powder with an oxalic acid solution with the concentration of 5% -20%, adding a proper amount of hydrogen peroxide as an oxidant, and reacting for 2.5-3 hours to form a gray green slurry with the temperature of 30-50 ℃; the temperature of the oxalic acid solution is 70-95 ℃; the particle size of the carbonyl nickel powder is 1-3 mu m, and the carbonyl nickel powder is treated by a reducing gas atmosphere at the low temperature of 380-450 ℃; the mass fraction of the hydrogen peroxide in the reaction solution is 0.05-0.1%;
the drying step includes: placing the gray green slurry into a static electric heating oven, heating the oven to 150-220 ℃ at a speed of 35-55 ℃/h, and baking for 12-16h to finish drying to obtain a slurry block;
the slurry block is subjected to multistage shearing crushing to obtain nickel powder microparticles with the granularity of less than 2 mu m; granulating by adopting granulating equipment to obtain coarse nickel powder particles;
in the rolling-scattering step, quick feeding is adopted to pass through rolling equipment; wherein the feeding speed is 1.25-1.8kg/min, the double-roller gap of the rolling equipment is 1.5-3mm, and the rotating speed is 25-30r/min;
the heating solid phase diffusion sintering step comprises the following steps: and (3) placing the rolled material obtained in the rolling-scattering step in a reducing atmosphere, and sintering at 680-750 ℃ for 3-5h.
4. The method according to claim 3, wherein the number of crushing stages in the multi-stage shearing crushing step is 3 to 5, and the size distribution of the fine particles of the nickel powder obtained by crushing is 1 to 1.5. Mu.m.
5. The method for preparing nickel powder according to claim 4, wherein the low-temperature reduction step adopts hydrogen gas to reduce the nickel powder microparticles, the reduction temperature is 355-480 ℃, the reduction time is 2-4 hours, and the reduced nickel powder microparticles are obtained and are in a bulk shape or a small loose block shape.
6. The method for preparing nickel powder according to claim 5, wherein the granulating step adopts a rolling method, a centrifugation method or a high-speed stirring method, ethylene glycol or wax is used as a binder, the addition amount of the binder is 40-100mL/kg, and the particle size distribution of the coarse particles of the nickel powder is 1.0-3.5mm.
7. The method for preparing nickel powder according to claim 6, wherein the crushing step is performed by a hammer crusher, and the sieving step is performed by a vibrating screen for particle size separation, and 3-6 particle size distribution grades are separated.
8. Use of large particle low bulk density nickel powder according to any of claims 1-7 for porous metal filtration articles.
9. Use of large-particle low-apparent-density nickel powder for conductive paste products according to any one of claims 1 to 7.
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