CN1827266A - Process for preparing nano nickel powder - Google Patents
Process for preparing nano nickel powder Download PDFInfo
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- CN1827266A CN1827266A CN 200610025552 CN200610025552A CN1827266A CN 1827266 A CN1827266 A CN 1827266A CN 200610025552 CN200610025552 CN 200610025552 CN 200610025552 A CN200610025552 A CN 200610025552A CN 1827266 A CN1827266 A CN 1827266A
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 181
- 239000000843 powder Substances 0.000 title claims description 46
- 238000004519 manufacturing process Methods 0.000 title description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 79
- 238000000034 method Methods 0.000 claims abstract description 55
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 39
- 230000008569 process Effects 0.000 claims abstract description 23
- 229910052751 metal Inorganic materials 0.000 claims abstract description 20
- 239000002184 metal Substances 0.000 claims abstract description 20
- 239000004020 conductor Substances 0.000 claims abstract description 12
- 239000000654 additive Substances 0.000 claims abstract description 11
- 230000000996 additive effect Effects 0.000 claims abstract description 11
- 238000001291 vacuum drying Methods 0.000 claims abstract description 6
- 230000000694 effects Effects 0.000 claims abstract description 5
- 230000009467 reduction Effects 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 23
- 239000002245 particle Substances 0.000 claims description 17
- 239000002243 precursor Substances 0.000 claims description 16
- 238000004806 packaging method and process Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 14
- 238000003487 electrochemical reaction Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- 239000003792 electrolyte Substances 0.000 claims description 11
- YFZDLRVCXDBOPH-UHFFFAOYSA-N tetraheptylazanium Chemical class CCCCCCC[N+](CCCCCCC)(CCCCCCC)CCCCCCC YFZDLRVCXDBOPH-UHFFFAOYSA-N 0.000 claims description 7
- 239000003153 chemical reaction reagent Substances 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 238000002848 electrochemical method Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 3
- 238000009826 distribution Methods 0.000 abstract description 2
- 239000008151 electrolyte solution Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 31
- 235000019441 ethanol Nutrition 0.000 description 23
- 239000007788 liquid Substances 0.000 description 12
- 239000000243 solution Substances 0.000 description 9
- 229910001453 nickel ion Inorganic materials 0.000 description 8
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 7
- 229920000915 polyvinyl chloride Polymers 0.000 description 7
- 239000004800 polyvinyl chloride Substances 0.000 description 7
- 238000007789 sealing Methods 0.000 description 7
- 230000003647 oxidation Effects 0.000 description 6
- 239000002699 waste material Substances 0.000 description 6
- 238000001914 filtration Methods 0.000 description 5
- 239000002912 waste gas Substances 0.000 description 5
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 4
- 238000005868 electrolysis reaction Methods 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- 229920003023 plastic Polymers 0.000 description 4
- 239000004033 plastic Substances 0.000 description 4
- 238000004064 recycling Methods 0.000 description 4
- 229910000838 Al alloy Inorganic materials 0.000 description 3
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 150000002815 nickel Chemical class 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 150000005846 sugar alcohols Polymers 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 229920005862 polyol Polymers 0.000 description 2
- 150000003077 polyols Chemical class 0.000 description 2
- 238000010301 surface-oxidation reaction Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000011255 nonaqueous electrolyte Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention relates to a method for preparing nanometer nickel powder, which comprises: inside the electrolytic tank, using the metal nickel plate as the anode, the conductive material as cathode, and the organic alcohol as electrolytic solution; adding certain additive, to attaint the nanometer nickel metastable phase predecessor material with high activity; then via the eccentric device, attaining the separated wet nanometer nickel powder to be dried by vacuum drying box; being processed to attain the nanometer metal nickel powder which meets the quality standard of national nanometer nickel. The invention has the advantages that: it has simple process, while the product quality can reach different levels of national nanometer nickel standards, without surface oxidization in long storage and normal temperature. The invention has lower cost, adjust producing amount, better power distribution property, and controllable quality.
Description
Technical Field
The invention relates to a method for preparing nano nickel powder, which can be used for civil or military use and belongs to the technical field of nano material preparation.
Background
The industrial production process of nanometer nickel powder belongs to high and new technology in the field of nanometer material preparation, and the current method for producing nanometer nickel powder at home and abroad mainly comprises the following steps:
method one, plasma (or laser) heating evaporation method:
the metal nickel is heated and volatilized by high-temperature plasma in a vacuum chamber, and the nickel steam is brought into a low-temperature collection chamber by inert gas or nitrogen. The method has the characteristics of capability of producing different nano metal powder, adjustable production capacity, good product dispersibility, large equipment investment, high cost, easy oxidation due to the fact that the surface is clean and not modified, and inflammable danger due to the fact that the product is exposed in the air.
The second method is a direct electrolytic reduction method:
the nickel is used as anode, the saturated aqueous solution of nickel salt is added with a certain amount of reducing agent and dispersant to be used as electrolyte, and the nano nickel powder is directly obtained at the cathode through electrolysis. The method has the characteristics of simple production process, unstable product quality, uneven particles, difficulty in obtaining powder below 50 nanometers, serious powder agglomeration and unsuitability for large-scale production of the nano nickel, and the method is suitable for being adopted under the laboratory state due to harsh conditions.
Method III, polyol reduction of Ni (OH)2The method comprises the following steps:
directly precipitating with nickel salt in alkaline solution to obtain Ni (OH)2And then reduction treatment is carried out under polyhydric alcohol, the method is researched moreat present, but the method is not applied to production, the production process is immature, powder particles are not uniform, in addition, the nano nickel powder is difficult to separate from the viscous polyhydric alcohol, and the product purity is low.
Disclosure of Invention
The invention aims to provide a novel and unique preparation method of nano nickel powder, which can reach the quality standard grade of national nano nickel, can not generate surface oxidation phenomenon when the product is stored for a long time at normal temperature, and has good dispersibility and adjustable size.
In order to achieve the above purpose, the technical scheme of the invention is characterized in that the electrochemical method of directly sacrificing anode metallic nickel by adopting non-aqueous electrolyte comprises the following specific processes:
the first step, electrochemical reaction process:
in an electrolytic bath, a metal nickel plate is used as an anode, a conductive material is used as a cathode, an electrolyte is an environment-friendly anhydrous industrial reagent ethanol, the concentration is 90-100%, the metal nickel plate and the conductive material are covered, a tetraheptyl ammonium salt TBA additive with the concentration of 0.1-10% and the ethanol ratio of 1: 8-800 is added, the TBA does not participate in chemical reaction, and in the electrochemical reaction, the high-activity tetraheptyl ammonium salt TBA is generatedMetastable phase precursor R of nano nickel2-Ni, taking out precursor particles of nickel;
step two, reduction heat treatment:
metastable phase precursor R of nano nickel2Ni, reducing alcohol with the concentration of 100 percent and organic anhydrous reducing liquid are sealed in a high-pressure kettle according to the proportion of 1: 10-100, the heat reduction heat treatment is carried out, the pressure is 50-100 atmospheric pressure (G), the temperature is 200-270 ℃, the time is 2-5 hours, and nano nickel powder which is dispersed in organic solution and is modified on the surface is obtained after the reduction;
step three, separation and drying:
separating the mixture of the nano nickel and the organic solution obtained after reduction by a centrifugal device to obtain wet nano nickel powder, drying the wet nano nickel powder by a vacuum drying oven at the temperature of 30-50 ℃, and directly obtaining a nano metallic nickel powder product meeting the national nano nickel quality standard after treatment;
fourthly, product packaging:
and weighing and packaging the finished product in a glove box, wherein a PVC (polyvinyl chloride) sealing packaging bag is adopted, a plastic bottle is additionally arranged, and more than 20 kg of the finished product is packaged by an aluminum alloy barrel.
The consumption of Ni, electrolyte and additive in the metal nickel plate can be determined according to the production scale.
In the invention, in an electrolytic cell, a metal nickel plate Ni is used as an anode, other conductive materials are used as a cathode, an electrolyte is an environment-friendly industrial reagent absolute ethyl alcohol, and tetraheptyl ammonium salt TBA is used as an additive which can be ionized in an ethanol solution, only plays a role in increasing the conductivity and does not participate in chemical reaction. In electrochemical reaction, anode nickel loses electrons and turns into nickel ions, which are combined with ethanol with weak negative electrode property to generate metastable phase precursor R of nano nickel with highactivity2Ni, taking out the nanometer precursor particles of the nickel through filtration, wherein no gas or liquid is discharged in the process, no heat is emitted in the reaction process, and the chemical reaction process comprises the following steps:
the invention leads the metastable phase of the nano nickel to be in front ofRepellent R2Sealing Ni and absolute ethyl alcohol in an autoclave, and addingThermal reduction treatment, except that there is certain low temperature heat to give off around the autoclave in the treatment process, there is not any waste gas, waste liquid to discharge in the whole treatment process, its reaction process is the reverse process of the first step, namely nickel ion obtains the electron that is lost from ethanol oxidation, reduce into the nickel atom, because under the organic solvent environment, the grain growth is inhibited, thus can get nanometer nickel powder, ethanol is oxidized into acetaldehyde, the reduction process is:
the surface of the obtained nano nickel powder is coated and modified by organic alcohol, so the nano nickel powder can be stored in the air for a long time without oxidation. The first step of electrochemical reaction is used to obtain R with high activity nano structure2Ni, so that the implementation of the second step reverse process is guaranteed.
Compared with the method I, namely a plasma heating evaporation method, the method has the characteristics of simple production process, low product cost and small equipment investment, and solves the problem of unavoidable oxidation of the surface of the nano nickel produced by the plasma heating evaporation method.
Compared with the second method, namely a direct electrolytic reduction method, the method has the advantages that the particle size of the produced nano nickel powder is easier to control, the particle distribution range is narrow, and the problem that the method is easy to agglomerate in the powder drying process is solved. The whole process is carried out in a non-aqueous solution, the parameters of the length of the particle nucleus are few, the control is easy, and the particles are surrounded by organic molecules and are not easy to agglomerate.
The invention and method three' polyol reduction Ni (OH)2Compared with the method, the method has the advantages of simple production process, no discharge of byproducts and wastes, low production cost and no introduction of any other impurity ions in the reaction process, so that the product has the characteristics of high purity, good dispersibility and small particles, and solves the problems that the nano nickel and the polyhydric alcohol are difficult to separate and the purity is low in the third methodAnd the problem of large particles.
The invention has the advantages that the produced nano nickel powder product completely reaches the quality standard grade of the national nano nickel, and the chemical components, the physical properties and the specific surface area of the nano nickel powder product can reach the national standard and also reach the quality grade of the international advanced level. Compared with products of the American quantum ball nano material company, the nano nickel powder produced by the method can not be subjected to surface oxidation after being stored for a long time at normal temperature.
Compared with other methods, the method has the following advantages under the condition of the same production scale: the investment is small, and the production cost is lower than 1000 yuan/kg; the production capacity can be adjusted at any time, and a producer can flexibly adjust the actual production capacity according to market supply and demand quotations; the finished product powder has good dispersibility and is easy to subpackage, store and transport; the production process has no emission of pollutants such as harmful waste gas, waste liquid and the like, and can realize the environment-friendly production order of new materials; the electrolyte after electrolytic filtration is returned to the electrolytic cell for recycling, and the residual acetaldehyde produced in the reduction heat treatment can be recycled or sold as a production raw material, so that the recycling economy can be realized. The method has controllable production quality and clean production environment in a factory.
Detailed description of the preferred embodiments
The present invention will be described in more detail with reference to examples, and the amount of Ni consumed in the metallic nickel plate electrode of the present invention may be determined according to the production scale.
Example 1 was prepared to produce 10 grams of product.
A preparation method of nano nickel powder adopts an electrochemical method, and the operation process of the method is as follows:
in the first step, electrochemical reaction:
in an electrolytic cell, 30 g of metal nickel plate Ni is used as an anode, conductive material carbon glass is used as a cathode, electrolyte is 160 g of absolute ethyl alcohol which is an environment-friendly industrial reagent, the concentration is 100%, the metal nickel plate and the conductive material are covered, 6 g of tetraheptyl ammonium salt TBA with theconcentration of 2% is added to serve as an additive, the additive can be ionized in an ethanol solution, and only the effect of increasing the conductivity is achievedElectric action, without participating in chemical reactions. In electrochemical reaction, anode nickel loses electrons and turns into nickel ions, which are combined with ethanol with weak negative electrode property to generate metastable phase precursor R of nano nickel with high activity2-Ni, taking out the nickel nanoprecursor particles by filtration; the chemical reaction process comprises the following steps:
step two, reduction heat treatment:
metastable phase precursor R of nano nickel2And (3) sealing Ni and 100% absolute ethyl alcohol in a high-pressure kettle according to the ratio of 1: 50, performing heating reduction treatment under the pressure of 65 atmospheric pressures and the temperature of 250 ℃ for 3 hours, and reducing to obtain the nano nickel powder with the surface modified by the ethyl alcohol. In the treatment process, except that a certain amount of low-temperature heat is emitted around the high-pressure kettle, no waste gas or waste liquid is discharged in the whole treatment process; the reaction process is the reverse process of the first step, namely, nickel ions obtain electrons which are lost by oxidation of ethanol and are reduced into nickel atoms. Because the particle growth is inhibited under the organic solvent environment, the nanoscale nickel powder can be obtained, ethanol is oxidized into acetaldehyde, and the chemical reaction process comprises the following steps:
step three, separation and drying:
separating the mixture of the reduced nano nickel and the organic solution by a centrifugal device to obtain wet nano nickel powder, drying the wet nano nickel powder by a vacuum drying oven at the temperature of 40 ℃, directly obtaining a nano metallic nickel powder product meeting the national quality standard after treatment, and continuously using the rest 20 g of nickel plate until complete electrolysis. The conversion rate of the block nickel plate into the nano nickel powder is more than 99 percent;
fourthly, product packaging:
and weighing and packaging the finished product in a glove box, and packaging the finished product by adopting a PVC sealing packaging bag or a plastic bottle.
Example 2 a production capacity of 1 ton per year, 200 working days per year (8 hour shift), calculated as 5 kg of finished product per day.
A method for preparing nano nickel powder adopts an electrochemical method, and comprises the following steps:
the first step, electrochemical reaction:
in a closed electrolytic cell, 15 kg of metal nickel plate Ni is used as an anode, a conductive material metal copper is used as a cathode, an electrolyte is 80 kg of absolute ethyl alcohol which is an environment-friendly industrial reagent, the metal nickel plate and the conductive material are covered, the concentration is 95%, 4 kg of tetraheptyl ammonium salt TBA with the concentration of 5% is added to be used as an additive, the additive can be ionized in an ethanol solution, only the function of increasing the conductivity is achieved, and the chemical reaction is not participated. In electrochemical reaction, anode nickel loses electrons and turns into nickel ions, which are combined with ethanol with weak negative electrode property to generate metastable phase precursor R of nano nickel with high activity2And Ni, the nano precursor particles of the nickel are taken out through filtering, and the filtered electrolyte can be directly sent back to the electrolytic cell for continuous recycling. In the process, no gas and liquid are discharged, no heat is emitted in the reaction process, and the chemical reaction process comprises the following steps:
step two, reduction heat treatment:
metastable phase precursor R of nano nickel2And (3) sealing Ni and 100% absolute ethyl alcohol in a high-pressure kettle according to the ratio of 1: 60, carrying out heating reduction treatment under the pressure of 80 atmospheric pressures and the temperature of 260 ℃ for 3 hours, and reducing to obtain the nano nickel powder with the surface modified by the ethyl alcohol. In the treatment process, except that a certain amount of low-temperature heat is emitted around the high-pressure kettle, no waste gas or waste liquid is discharged in the whole treatment process, and the reaction process is the reverse process of the first step, namely, nickel ions obtain electrons which are oxidized and lost from ethanol and are reduced into nickel atoms. Because the particle growth is inhibited in the organic solvent environment, the nano nickel powder can be obtained, and the ethanol is oxidized into acetaldehyde. The chemical reaction process is as follows:
step three, separation and drying:
separating the mixture of the nano nickel and the organic solution obtained after reduction by an industrial liquid centrifugal device to obtainwet nano nickel powder, and drying the wet nano nickel powder by using a vacuum drying oven at the temperature of 50 ℃ to directly obtain a nano metal nickel powder product meeting the national quality standard after treatment; the remaining 10 kg of nickel plate can be used continuously until complete electrolysis. The conversion rate of the block nickel plate to the nano nickel powder is more than 99 percent, and the separated liquid is collected and stored, separated and recycled after reaching a certain amount or sold as a production raw material.
Fourthly, product packaging:
and weighing and packaging the finished product in a glove box, wherein a PVC (polyvinyl chloride) sealing packaging bag is adopted, a plastic bottle is additionally arranged, and more than 20 kg of the finished product is packaged by an aluminum alloy barrel.
Example 3 production of 5 tons per year, 200 working days per year (16 h 2 shift), calculated as 25 kg of finished product per day.
A method for preparing nano nickel powder adopts an electrochemical method, and comprises the following steps:
in the first step, electrochemical reaction:
in a closed electrolytic cell, 75 kg of metal nickel plate Ni is used as an anode, metal nickel is used as a cathode, electrolyte is 240 kg of absolute ethyl alcohol which is an environment-friendly industrial reagent, the concentration of the absolute ethyl alcohol is 90%, the metal nickel plate and a conductive material are covered, 24 kg of tetraheptyl ammonium salt TBA with the concentration of 10% is added to serve as an additive, and the additive can be ionized in an ethanol solution, only plays a role in increasing the conductivity and does not participate in chemical reaction. In electrochemical reaction, anode nickel loses electrons and turns into nickel ions, which are combined with ethanol with weak negative electrode property to generate metastable phase precursor R of nano nickel with high activity2And (4) filtering to obtain nickel nano precursor particles, carrying out reduction treatment in the next step, and returning the filtered electrolyte to the electrolytic cell for continuous recycling. In the process, no gas and liquid are discharged and reactedThe process has no heat emission, and the chemical reaction process is as follows:
step two, reduction heat treatment:
metastable phase precursor R of nano nickel2Ni and absolute ethyl alcohol with the concentration of 100 percent are sealed in a high-pressure kettle according to the proportion of 1: 70 for heating reduction treatment, the pressure is 100 atmospheric pressures, the temperature is 270 ℃, the time is 3 hours, nano nickel powder with the surface modified by the ethyl alcohol is obtained after reduction, and except certain low-temperature heat dissipation around the high-pressure kettle in the treatment process, no waste gas and waste liquid are discharged in the whole treatment process; the reaction process is the reverse process of the first step, namely nickel ions obtain electrons lost from ethanol oxidation and are reduced into nickel atoms, and the particle growth is inhibited under the environment of an organic solvent, so that the nanoscale nickel powder can be obtained, ethanol is oxidized into acetaldehyde, and the chemical reaction process comprises the following steps:
step three, separation and drying:
separating the mixture of the reducednano nickel and the organic solution by a centrifugal device to obtain wet nano nickel powder, drying the wet nano nickel powder at 40 ℃ by a vacuum drying oven, and directly obtaining the nano metal nickel powder product meeting the national quality standard after treatment. The remaining 50 kg of nickel plate can be used continuously until complete electrolysis. The conversion rate of the block nickel plate into the nano nickel powder is more than 99 percent; the separated liquid is collected and stored, and is separated and recycled after reaching a certain amount or sold as a production raw material, and enters circular economy;
fourthly, product packaging:
and weighing and packaging the finished product in a glove box, wherein a PVC (polyvinyl chloride) sealing packaging bag is adopted, a plastic bottle is additionally arranged, and more than 20 kg of the finished product is packaged by an aluminum alloy barrel.
Product performance test comparison table of the method of the invention
The invention conforms to the national standard: GB/T19588 and 2004 nano nickel powder.
The detection results in the table are provided by the detection report of the national specified highest-quality nano nickel powder standard detection unit.
Claims (3)
1. A preparation method of nano nickel powder is characterized in that an electrochemical method is adopted, and the method comprises the following steps:
the first step, the electrochemical reaction process:
in an electrolytic bath, a metal nickel plate is used as an anode, a conductive material is used as a cathode, an electrolyte is an environment-friendly anhydrous industrial reagent ethanol with the concentration of 90-100%, the metal nickel plate and the conductive material are covered, a tetraheptyl ammonium salt TBA additive with the concentration of 0.1-10% and the ethanol ratio of 1: 8 to 1: 800 is added, the TBA does not participate in chemical reaction, and a metastable-phase precursor R of nano nickel with high activity is generated in electrochemical reaction2-Ni, taking out precursor particles of nickel;
step two, reduction heat treatment:
metastable phase precursor R of nano nickel2Ni and ethanol with the concentration of 100 percent are sealed in a high-pressure kettle according to the proportion of 1: 10-100, the heat reduction heat treatment is carried out, the pressure is 50-100 atmospheric pressure (G), the temperature is 200-270 ℃, the time is 2-5 hours, and the nano nickel powder with the surface modified by organic alcohol is obtained after the reduction;
thirdly, separation and drying:
separating the mixture of the nano nickel and the organic solution obtained after reduction by a centrifugal device to obtain wet nano nickel powder, drying the wet nano nickel powder by a vacuum drying oven at the temperature of 30-50 ℃, and directly obtaining a nano metallic nickel powder product meeting the national quality standard after treatment;
fourthly, product packaging:
and weighing and packaging the finished product in a glove box.
2. The method of claim 1, wherein the conductive material is selected from the group consisting of nickel, copper, and carbon glass.
3. The method according to claim 1, wherein the electrolytic bath is a closed electrolytic bath.
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| CN101428348B (en) * | 2008-07-29 | 2010-09-08 | 张建玲 | Process for producing spherical submicron metal with hydro-thermal treatment |
| CN101709489B (en) * | 2009-11-12 | 2011-03-23 | 中南大学 | Method for producing nickel powder from pure nickel sulfate solution through direct deposition |
| CN102196868A (en) * | 2008-10-24 | 2011-09-21 | 株式会社日清制粉集团本社 | Method for classifying powder |
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| JP4096645B2 (en) * | 2002-06-28 | 2008-06-04 | 株式会社村田製作所 | Nickel powder manufacturing method, nickel powder, conductive paste, and multilayer ceramic electronic component |
| JP4244883B2 (en) * | 2003-08-26 | 2009-03-25 | 株式会社村田製作所 | Method for producing nickel powder |
| JP2005240076A (en) * | 2004-02-24 | 2005-09-08 | Fujikura Ltd | Method for manufacturing oxide-containing nickel powder |
| JP3938770B2 (en) * | 2004-04-16 | 2007-06-27 | Ｔｄｋ株式会社 | Nickel powder manufacturing method, nickel powder manufacturing device and nickel powder manufacturing crucible |
| CN1631588A (en) * | 2004-11-18 | 2005-06-29 | 上海大学 | Method for manufacturing nanometer nickel |
| CN1319685C (en) * | 2005-01-13 | 2007-06-06 | 南京大学 | Production for nanometer nickel powder |
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| CN101428348B (en) * | 2008-07-29 | 2010-09-08 | 张建玲 | Process for producing spherical submicron metal with hydro-thermal treatment |
| CN102196868A (en) * | 2008-10-24 | 2011-09-21 | 株式会社日清制粉集团本社 | Method for classifying powder |
| CN102196868B (en) * | 2008-10-24 | 2014-04-23 | 株式会社日清制粉集团本社 | Method for classifying powder |
| CN101709489B (en) * | 2009-11-12 | 2011-03-23 | 中南大学 | Method for producing nickel powder from pure nickel sulfate solution through direct deposition |
| CN102586800A (en) * | 2011-01-17 | 2012-07-18 | 李小毛 | Preparation method of nano-copper powder |
| CN102586800B (en) * | 2011-01-17 | 2015-05-13 | 李小毛 | Preparation method of nano-copper powder |
| CN102634816A (en) * | 2011-02-14 | 2012-08-15 | 李小毛 | Preparation method of nanometer tin indium oxide powder |
| CN102634816B (en) * | 2011-02-14 | 2014-11-19 | 李小毛 | Preparation method of nanometer tin indium oxide powder |
| CN103464784A (en) * | 2013-09-27 | 2013-12-25 | 南开大学 | Preparation method of nano nickel supported on carbon |
| CN103464784B (en) * | 2013-09-27 | 2016-01-20 | 南开大学 | A kind of preparation method of carbon loaded with nano nickel |
| CN103722167A (en) * | 2013-12-10 | 2014-04-16 | 大连理工大学 | Method for preparing nano nickel powder through electrolytic deposition in ethanol solution of nickel chloride hexahydrate |
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