CN108356281A - A kind of preparation method of Nickel Powder - Google Patents
A kind of preparation method of Nickel Powder Download PDFInfo
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- CN108356281A CN108356281A CN201810237478.4A CN201810237478A CN108356281A CN 108356281 A CN108356281 A CN 108356281A CN 201810237478 A CN201810237478 A CN 201810237478A CN 108356281 A CN108356281 A CN 108356281A
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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
- 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
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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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
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/068—Flake-like particles
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
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- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
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- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The present invention provides a kind of preparation method of Nickel Powder, this method is using water, nickel salt, complexing agent, nickel plating brightener, dispersant, antioxidant, sublimable flaky compound crystallization template and reducing agent as raw material, using the method for chemical plating, template surface nickel plating is crystallized in sublimable flaky compound, up to nickel ion, the reaction was complete, after reaction, through separating-purifying and Treatment technique for processing process, without ball milling, Nickel Powder is directly obtained.Technical solution of the present invention is with low energy consumption; environmental pollution is small; simple production process, process route is brief, and large-scale production equipment investment is small; production efficiency is high; production cost is low, and the dispersion performance of product and the series of advantages such as conduct electricity very well are suitable for large-scale production; solve the problems, such as that ball-milling method prepares Nickel Powder technique, industrialization prospect is good.
Description
Technical field
The present invention relates to a kind of preparation methods of Nickel Powder, belong to the preparing technical field of metal powder material.
Background technology
Metal powder is divided into spherical shape, irregular granules shape, sheet and four kinds of threadiness by grain shape.With globular metallic powder and
Granulated metal powder is different, and flaky metal powder has excellent catalytic performance, excellent sintering character, excellent thixotropy
Energy, excellent adhesive force, good screen effect, excellent reflection of electromagnetic wave ability and splendid electric conductivity, make it change
The fields such as catalysis, powder metallurgy, conductive coating, conductive adhesive, electrically conductive ink and electrocondution slurry are learned to have a wide range of applications.
Currently, chemical catalysis, electromagnetic screen coating, reflection of radar wave coating, conductive coating, conductive adhesive, conductive oil
Ink and electrocondution slurry field use globular metallic powder or granulated metal powder mostly.In terms of electric conductivity, compared to piece
Shape metal powder, globular metallic powder and the intergranular contact of granulated metal powder are point contacts, and electric conductivity is poor, metal powder
Last dosage is big, and use cost is high；And flaky metal powder particle not only large specific surface area, and intergranular contact be line contact and
Face contacts so that the intergranular contact area of flaky metal powder increases considerably, therefore, with globular metallic powder and graininess
Metal powder is compared, and the amount that flaky metal powder particle forms flaky metal powder needed for the conductive channel of same conductivity energy is bright
It is aobvious to reduce, and also have thixotropic property, the settlement stability performance of product notable with the thickened product that flaky metal powder is prepared
It improves；So using flaky metal powder prepare conduction electrons material be both remarkably improved the electric conductivity of product, adhesive force and
Storage stability, and the dosage of metal powder can be greatly lowered, it economizes on resources, reduces production cost, increase economic efficiency.
In terms of chemical catalysis, electromagnetic shielding and reflection of radar wave, since flaky metal powder is obviously than globular metallic powder and graininess
The large specific surface area of metal powder shows excellent catalytic performance, capability of electromagnetic shielding and reflection of radar wave performance.Therefore,
The technology of preparing of flaky metal powder is concerned.
The technology report that chemical method prepares flaky metal powder is many, but these technology poor repeatabilities, can be used for industry
That changes is few.Currently, the flaky metal powder product of commercial type, is mostly to use globular metallic powder or granular metal powder
End is obtained through ball milling under given conditions, due to generally requiring inert gas shielding when ball milling, and must be added to lubrication appropriate
Agent and dispersant ball milling are then classified, surface polishing and surface are modified to required granularity, last purified to handle
To flaky metal powder；So ball-milling technology is generally all more complicated cumbersome, equipment requirement is high, and the production cycle is long, high energy consumption,
Production cost is high；And the obtained flaky metal powder product purity of ball milling is not often high, grain size is big, sheet-like particle concave-convex surface
Coarse, in irregular shape, became uneven, powder crack at edge, specific surface area is small.Therefore, it is prepared using new and effective method
Flaky metal powder product is concerned.
Chemical plating is a kind for the treatment of technology that the coat of metal can be formed in surfaces of various materials, and the technology is because of technique letter
Just, energy-saving and environmental protection and be increasingly subject to the concern of people.The principle of chemical plating is simple, different from plating, and chemical plating is that one kind is not required to
Electricity consumption, but in the solution containing reducing agent and metal ion, using oxidation-reduction reaction principle, metal ion is restored
The method that a variety of materials surface forms coating is deposited at metal.
Mostly it is in metallic conductor and non-metallic isolator material surface currently, having the chemical plating of document report
The chemical plating of progress mainly achievees the purpose that basis material is decorated and protected, on compound crystal surface
Learn the rarely seen document report of research of plating；Using flaky compound crystalline solid as template, sheet metal is prepared by the method for chemical plating
The research of powder is even more rarely seen document report.Therefore, it using flaky compound crystalline solid as the template of chemical plating, inquires into flaking
Reaction process condition and technical solution that object crystallization template surface carries out chemical plating are closed, inquires into and is carried from the separation of gained chemical plating product
Pure and mild processing obtains the technical process and technology of flaky metal powder, provides a kind of completely new side preparing flaky metal powder
Method is undoubtedly of great significance.
The present invention provide it is a kind of with water, nickel salt, complexing agent, nickel plating brightener, dispersant, antioxidant, sublimable
Shape compound crystallizes template and reducing agent is raw material, the method for preparing Nickel Powder.This method is with low energy consumption, environmental pollution
Small, simple production process, production process route are short, the feature that small, product purity is high and yield is high, industry are invested in large-scale production
Change promise well.Currently, this method is there is not yet document report.
Invention content
A kind of preparation method of Nickel Powder of the present invention provides a kind of preparation method of Nickel Powder, this method
With water, nickel salt, complexing agent, nickel plating brightener, dispersant, antioxidant, sublimable flaky compound crystallization template and reduction
Agent is raw material, using the method for chemical plating, template surface nickel plating is crystallized in sublimable flaky compound, until nickel ion reacts
Completely, after reaction, through separating-purifying and Treatment technique for processing process to get to Nickel Powder.
1, the preparation method of a kind of Nickel Powder of the present invention, it is characterised in that the preparation of Nickel Powder is using as follows
Technical solution：
1. crystallizing the preparation of the mixture of template and nickel salt containing sublimable flaky compound：According to water, nickel salt, complexing
Agent, nickel plating brightener, dispersant, antioxidant and sublimable flaky compound crystallization template mass percent be
(35.0%~95.0%): (0.1%~30.0%): (0.1%~30.0%): (0.001%~10.0%): (0.1%~
30.0%): (0.001%~10.0%): the ratio of (0.1~30.0%), first by water, nickel salt, complexing agent, nickel plating brightener,
Dispersant and antioxidant mixing, stirring are completely dissolved to all materials, add sublimable flaky compound crystallization template,
It stirs and handles 1~60min with ultrasonic echography, sublimable flaky compound crystallization template is ground into ultrasonic echography
Grain size is after 0.5~20.0 μm of flaky crystal to get to the mixing for crystallizing template and nickel salt containing sublimable flaky compound
Object；
2. the preparation of reducing agent aqueous solution：It is (0.1%~30.0%) according to the mass percent of reducing agent and water:
The ratio of (70.0%~99.9%) mixes water with reducing agent, to get to reducing agent aqueous solution after stirring and dissolving is complete；
3. the preparation of Nickel Powder：The mixture of template and nickel salt is crystallized in stirring condition containing sublimable flaky compound
Under, it is gradually added reducing agent aqueous solution, nickel ion is reduced into metallic nickel and chemical plating is plated to sublimable flaky compound knot
Crystal template surface, up to nickel ion, the reaction was complete；Solid matter of the reaction product through filtering gained is again through multiple water washing and mistake
Repetitive operation is filtered, obtains the sublimable flaky compound crystallization of nickel plating, the material is within the temperature range of 70~150 DEG C, warp
Decompression heat treatment makes sublimable flaky compound crystallization distillation, solidifying with cold-trap after sublimable flaky compound crystallization distillation
Magnificent recycle simultaneously can be recycled, until the crystallization of sublimable flaky compound obtains nickel sheet after eliminating, gained nickel sheet is again through adding nothing
Water-ethanol is dispersed with stirring, ultrasonic echography crushes 1~6h, filtering and the technical process of drying to get be 1.0 to average grain diameter~
5.0 μm are the Nickel Powder of 10~40m with average thickness；
Wherein, water used is any one of distilled water, deionized water, ultra-pure water and high purity water；
Wherein, ultrasonic wave used is the ultrasonic wave that frequency is 20KHz~1MHz, power is 30W~15KW.
2, a kind of preparation method of Nickel Powder, it is characterised in that this method prepare Nickel Powder technical indicator be：
1) appearance：Grey powder；
2) particle size range：0.2~10.0 μm；
3) average grain diameter：1.0~5.0 μm；
4) thickness range：5~70nm；
5) average thickness：10~40nm；
6) apparent density：1.8~2.7g/cm3；
7) tap density：2.4~3.2g/cm3。
3, a kind of preparation method of Nickel Powder, it is characterised in that this method has the advantages that following notable：
(1) sublimable flaky compound crystallization is selected to make template, it is therefore an objective to make chemical plating obtained solid product through multiple
After water washing and filtering repetitive operation remove water-solubility impurity, you can directly remove template using the method for distillation, template is easily
It removes, purifying technique very simple, quickly and efficiently；
(2) in the case that nickel salt dosage determines, the dosage of template is crystallized by changing sublimable flaky compound, is adjusted
The ratio of nickel salt and sublimable flaky compound crystallization template, you can the effectively thickness of control Nickel Powder；It is super with ultrasonic wave
Sound crushes the sheet nickel that sublimable flaky compound crystallization template and chemical plating obtain, and adjusts ultrasonic echography grinding time,
The grain size of Nickel Powder can be effectively controlled, size controlling method is simple and effective；Therefore, the present invention both can effectively control Nickel Powder
Thickness, and can effectively control the grain size of Nickel Powder, the Nickel Powder of high-specific surface area can be prepared, specific surface area is ball
3~5 times of shape nickel powder；
(3) in the preparation process of Nickel Powder, the purpose of nickel plating brightener is added, is to keep chemical Ni-plating layer light flat
It is whole, improve the flatness and finish of Nickel Powder particle surface；In the preparation process of Nickel Powder, the mesh of complexing agent is added
, be in order to form the dynamic equilibrium of free nickel ion and nickel complex ion in the reaction system, with it is effective control dissociate nickel from
The concentration of son, and then the deposition velocity of the reduction reaction speed and nickel of nickel ion is controlled, to obtain uniform nickel coating, and it is
Keep chemical Ni-plating layer light smooth, can also effectively improve the flatness and finish of Nickel Powder particle surface；
(4) in the preparation process of Nickel Powder, the purpose of dispersant is added, is particle agglomeration in order to prevent, improves sheet
The dispersibility of nickel powder particle, so that Nickel Powder is easily dispersed when preparing product with Nickel Powder, user is easy to use, improves
The performance of Nickel Powder；
(5) after preparing Nickel Powder the reaction was complete, reaction product filters obtained solid product through multiple water washing and mistake
After filtering repetitive operation removing water-solubility impurity, the sublimable flaky compound crystallization of nickel plating is obtained, the material is at 70~150 DEG C
Within the temperature range of, it is heat-treated through decompression, makes sublimable flaky compound crystallization distillation, sublimable flaky compound crystallization
It can be recycled with cold-trap recycling of sublimating after distillation, therefore, not only save template resource and reduced production cost, but also reduced
The discharge of pollutant, improves economic benefit and environmental benefit；
(6) technological requirement that the mantle plate method reported prepares Nickel Powder is high, severe reaction conditions, and control is improper often
What is obtained is graininess nickel powder rather than Nickel Powder, and therefore, the technique repetition stability that mantle plate method prepares Nickel Powder is poor,
Unstable product quality, or even cannot get Nickel Powder, production success rate is not high；The dura mater plate method reported prepares sheet
Complex process and the processing cost height etc. that remove, even can not remove or remove template is difficult to and there is template again in the technology of nickel powder
Problem, such as nickel powder is prepared as template using titanium dioxide, Woelm Alumina substance, template is not only difficult to remove, or even can not remove
Go, that is, complicated technology used to remove template, template is also difficult to cleared, and processing cost is high, and product purity is not high, and often also no
To Nickel Powder；Biological template prepares Nickel Powder operating procedure complexity, and control difficulty is high, and reaction process is slower, production
Efficiency is low.The success rate that technical solution of the present invention prepares Nickel Powder is 100%, and template easily removes, and production cost is low, raw
It produces efficient；
(7) it is to form one layer of protection on nickel coating surface to prepare during Nickel Powder using the purpose of antioxidant
Film is aoxidized with the nickel coating for preventing sublimable flaky compound from crystallizing template surface；
(8) technical solution of the present invention have low energy consumption, environmental pollution is small, and simple production process, process route is brief,
Large-scale production equipment investment is small, and production efficiency is high, and production cost is low, the dispersion performance of product and conducts electricity very well a series of excellent
Point, is suitable for large-scale production, solves the problems, such as that existing ball-milling method and template prepare Nickel Powder technique, industry
Change promise well.
4, the preparation method of a kind of Nickel Powder of the present invention, it is characterised in that ultrasonic wave used is that frequency is
20KHz~1MHz, the ultrasonic wave that power is 30W~15KW.
5, a kind of preparation method of Nickel Powder of the present invention, it is characterised in that sublimable sheet chemical combination used
It is any one of borneol, benzoic acid, naphthalene and anthracene that object, which crystallizes template,.
6, the preparation method of a kind of Nickel Powder of the present invention, it is characterised in that nickel salt used be citric acid nickel,
Nickel sulfate, nickel nitrate, tartaric acid nickel, nickel chloride and nickel acetate any one or more of.
7, the preparation method of a kind of Nickel Powder of the present invention, it is characterised in that antioxidant used is benzene a pair of horses going side by side three
Nitrogen azoles, mercapto benzothiazole, amineothiot, n-propyl mercaptan, isopropyl mercaptan, tert-butyl mercaptan, sec-butyl mercaptan, isobutyl group
Mercaptan, butyl mercaptan, tertiary butyl mercaptan, isoamyl mercaptan, n-amylmercaptane, n-hexyl mercaptan, n octylmercaptan, n-nonyl
Mercaptan, n-dodecyl mercaptan, tert-dodecylmercaotan, tetradecyl mercaptan, hexadecyl mercaptan, Stearyl mercaptan, benzyl
Base mercaptan and phenethyl mercaptan any one or more of；
8, the preparation method of a kind of Nickel Powder of the present invention, it is characterised in that complexing agent used is N- ethoxys
Ethylenediamine triacetic acid, N-hydroxyethyl-ethylenediamine triacetic acid trisodium salt, nitrilotriacetic acid, nitrilotriacetic acid trisodium salt, ethylenediamine tetra-acetic acid, second
Edetate disodium salt, citric acid, sodium citrate, potassium citrate, ammonium citrate, tartaric acid, sodium tartrate, potassium tartrate,
Sodium potassium tartrate tetrahydrate, glycerine, triethanolamine, potassium antimony tartrate and ammonium tartrate, sodium pyrophosphate, potassium pyrophosphate, ammonium pyrophosphate, lactic acid
Sodium, potassium lactate, ammonium lactate, sodium fluoride, potassium fluoride and ammonium fluoride any one or more of.
9, the preparation method of a kind of Nickel Powder of the present invention, it is characterised in that nickel plating brightener used is pyridine
Drone propoxyl group sulfobetaine, propane sulfonic acid pyridiniujm, pyridinium hydroxy propyl sulfobetaine, diethylin propargylamine, propilolic alcohol
Propoxylated compounds, propine alcohol ethoxylates, carboxyethyl thiocarbamide drone glycine betaine, diethyl thiourea, propargyl sodium sulfonate and
Sodium vinyl sulfonate any one or more of.
10, the preparation method of a kind of Nickel Powder of the present invention, it is characterised in that dispersant used is polyethylene
Pyrrolidones, carboxymethyl cellulose, sodium carboxymethylcellulose, methylcellulose, hydroxyethyl cellulose, hydroxymethyl cellulose, hydroxyl
Propyl cellulose, gelatin, polyacrylic acid, Sodium Polyacrylate, ammonium polyacrylate, polyacrylic acid potassium, polyvinyl alcohol, gum arabic
With polyethylene glycol any one or more of.
11, the preparation method of a kind of Nickel Powder of the present invention, it is characterised in that reducing agent used is time phosphorous
Any in sour sodium, ortho phosphorous acid, sodium borohydride, potassium borohydride, hydrazine, hydrazine sulfate, lignocaine borine and dimethylamino borine
Kind is a variety of.
Specific implementation mode
With reference to embodiment, present invention is further described in detail.It should be noted that being of the present invention below
A kind of Nickel Powder preparation method nonlimiting examples, these embodiments provide, it is only for reach to this
Invent the purpose that is described in further detail, not to the present invention in any form with substantial limitation；It must be noted that
For those skilled in the art, under the premise of not departing from the method for the present invention, those skilled in the art can also make
Several to improve, supplement and optimize, these are improved, supplement and optimization also should be regarded as protection scope of the present invention；It is all to be familiar with ability
The professional technician in domain utilizes technical solution of the present invention and technology contents in the case where not departing from the method for the present invention range
Process modification, scheme supplement and raw material proportioning optimization are carried out, the equivalent embodiment of the present invention is accordingly to be regarded as；Meanwhile it is all according to this hair
Substantial technological any equivalent improvement, supplement and the optimization made for the present invention of bright method, also belong to the skill of the method for the present invention
Art range；In the examples below that, unless stated otherwise, all percentage all refers to mass percent.
Table one, Examples 1 to 8 raw material and proportioning
It notes [1]：Zhao Jiachun, Fan Xingxiang, Li Bojie, etc..The experimental study of superfine spherical nickel powder is prepared using nickel sulfate.Nothing
Machine salt industrial, 2013,45 (1)：34-36.
According to the raw material and proportioning of Examples 1 to 8 in table one, the detailed technology scheme and preparation process of Examples 1 to 8 walk
It is rapid as follows：
1. crystallizing the preparation of the mixture of template and nickel salt containing sublimable flaky compound：According to embodiment 1 in table one
~8 water, nickel salt, complexing agent, nickel plating brightener, dispersant, antioxidant and sublimable flaky compound crystallizes template
Mass percent first mixes water, nickel salt, complexing agent, nickel plating brightener, dispersant and antioxidant, stirring to all materials
It is completely dissolved, adds sublimable flaky compound crystallization template, stir and handle 1~60min with ultrasonic echography, it can
The flaky compound crystallization template of distillation with ultrasonic echography be ground into grain size be after 0.5~20.0 μm of flaky crystal to get
To the mixture for crystallizing template and nickel salt containing sublimable flaky compound；
2. the preparation of reducing agent aqueous solution：It, will according to the reducing agent of Examples 1 to 8 in table one and the mass percent of water
Water is mixed with reducing agent, to get to reducing agent aqueous solution after stirring and dissolving is complete；
3. the preparation of Nickel Powder：The mixture of template and nickel salt is crystallized in stirring condition containing sublimable flaky compound
Under, it is gradually added reducing agent aqueous solution, nickel ion is reduced into metallic nickel and chemical plating is plated to sublimable flaky compound knot
Crystal template surface, up to nickel ion, the reaction was complete；Solid matter of the reaction product through filtering gained is again through repeatedly washing and filtering
Repetitive operation obtains the sublimable flaky compound crystallization of nickel plating, and the material is within the temperature range of 70~150 DEG C, through subtracting
Autoclaving makes sublimable flaky compound crystallization distillation, is sublimated with cold-trap after sublimable flaky compound crystallization distillation
It recycles and can be recycled, until the crystallization of sublimable flaky compound obtains nickel sheet after eliminating, gained nickel sheet is anhydrous through adding again
Ethyl alcohol is dispersed with stirring, ultrasonic echography crushes 1~6h, filtering and the technical process of drying to get be 1.0 to average grain diameter~
5.0 μm are the Nickel Powder of 10~40nm with average thickness；
Wherein, water used is any one of distilled water, deionized water, ultra-pure water and high purity water；
Wherein, ultrasonic wave used is the ultrasonic wave that frequency is 20KHz~1MHz, power is 30W~15KW.
Claims (10)
1. a kind of preparation method of Nickel Powder, it is characterised in that：
1. crystallizing the preparation of the mixture of template and nickel salt containing sublimable flaky compound：According to water, nickel salt, complexing agent, plating
Nickel brightener, dispersant, antioxidant and sublimable flaky compound crystallization template mass percent be (35.0%~
95.0%): (0.1%~30.0%): (0.1%~30.0%): (0.001%~10.0%): (0.1%~30.0%):
(0.001%~10.0%): the ratio of (0.1~30.0%), first by water, nickel salt, complexing agent, nickel plating brightener, dispersant and
Antioxidant mixes, and stirring is completely dissolved to all materials, adds sublimable flaky compound crystallization template, and stirring is used in combination
Ultrasonic echography handles 1~60min, and sublimable flaky compound crystallization template is ground into grain size with ultrasonic echography is
After 0.5~20.0 μm of flaky crystal to get to containing sublimable flaky compound crystallize template and nickel salt mixture；
2. the preparation of reducing agent aqueous solution：It is (0.1%~30.0%) according to the mass percent of reducing agent and water: (70.0%
~99.9%) ratio mixes water with reducing agent, to get to reducing agent aqueous solution after stirring and dissolving is complete；
3. the preparation of Nickel Powder：The mixture of template and nickel salt is crystallized containing sublimable flaky compound under agitation,
It is gradually added reducing agent aqueous solution, nickel ion is reduced into metallic nickel and chemical plating is plated to sublimable flaky compound crystallizing mould
Plate surface, up to nickel ion, the reaction was complete；Solid matter of the reaction product through filtering gained is repeated through repeatedly washing and filtering again
Operation obtains the sublimable flaky compound crystallization of nickel plating, and the material is within the temperature range of 70~150 DEG C, through decompression heat
Processing makes the crystallization distillation of sublimable flaky compound, is sublimated recycling with cold-trap after sublimable flaky compound crystallization distillation
And can be recycled, until the crystallization of sublimable flaky compound obtains nickel sheet after eliminating, gained nickel sheet is again through adding absolute ethyl alcohol
It is dispersed with stirring, ultrasonic echography crushes 1~6h, the technical process of filtering and drying is to get being 1.0~5.0 μm to average grain diameter
With the Nickel Powder that average thickness is 10~40nm；
Wherein, water used is any one of distilled water, deionized water, ultra-pure water and high purity water；
Wherein, ultrasonic wave used is the ultrasonic wave that frequency is 20KHz~1MHz, power is 30W~15KW.
2. preparation method described in claim 1, it is characterised in that this method prepare Nickel Powder technical indicator be：
1) appearance：Grey powder；
2) particle size range：0.2~10.0 μm；
3) average grain diameter：1.0~5.0 μm；
4) thickness range：5~70nm；
5) average thickness：10~40nm；
6) apparent density：1.8~2.7g/cm3；
7) tap density：2.4~3.2g/cm3。
3. preparation method described in claim 1, it is characterised in that ultrasonic wave used is that frequency is 20KHz~1MHz, power
For the ultrasonic wave of 30W~15KW.
4. preparation method described in claim 1, it is characterised in that sublimable flaky compound crystallization template used is ice
Any one of piece, benzoic acid, naphthalene and anthracene etc..
5. preparation method described in claim 1, it is characterised in that nickel salt used is citric acid nickel, nickel sulfate, nickel nitrate, wine
Stone acid nickel, nickel chloride and nickel acetate any one or more of.
6. preparation method described in claim 1, it is characterised in that antioxidant used is benzotriazole, sulfydryl benzene a pair of horses going side by side thiophene
Azoles, amineothiot, n-propyl mercaptan, isopropyl mercaptan, tert-butyl mercaptan, sec-butyl mercaptan, iso-butyl mercaptan, normal-butyl sulphur
Alcohol, tertiary butyl mercaptan, isoamyl mercaptan, n-amylmercaptane, n-hexyl mercaptan, n octylmercaptan, n-nonyl mercaptan, n-dodecane
Base mercaptan, tert-dodecylmercaotan, tetradecyl mercaptan, hexadecyl mercaptan, Stearyl mercaptan, benzyl mercaptan and phenethyl
Any one or more ofs such as mercaptan.
7. preparation method described in claim 1, it is characterised in that complexing agent used is N-hydroxyethyl-ethylenediamine triacetic acid, N-
Trisodium hydroxyethylene diamine triacetate salt, nitrilotriacetic acid, nitrilotriacetic acid trisodium salt, ethylenediamine tetra-acetic acid, disodium ethylene diamine tetraacetate
It is salt, citric acid, sodium citrate, potassium citrate, ammonium citrate, tartaric acid, sodium tartrate, potassium tartrate, sodium potassium tartrate tetrahydrate, sweet
Oil, triethanolamine, potassium antimony tartrate and ammonium tartrate, sodium pyrophosphate, potassium pyrophosphate, ammonium pyrophosphate, sodium lactate, potassium lactate, breast
Sour ammonium, sodium fluoride, potassium fluoride and ammonium fluoride any one or more of.
8. preparation method described in claim 1, it is characterised in that nickel plating brightener used is the thio sweet tea of pyridinium propoxyl group
Dish alkali, propane sulfonic acid pyridiniujm, pyridinium hydroxy propyl sulfobetaine, diethylin propargylamine, propilolic alcohol propoxylated compounds, third
In alkynol ethoxy compound, carboxyethyl thiocarbamide drone glycine betaine, diethyl thiourea, propargyl sodium sulfonate and sodium vinyl sulfonate
It is any one or more.
9. preparation method described in claim 1, it is characterised in that dispersant used is polyvinylpyrrolidone, carboxymethyl fibre
It ties up element, sodium carboxymethylcellulose, methylcellulose, hydroxyethyl cellulose, hydroxymethyl cellulose, hydroxypropyl cellulose, gelatin, gather
Appointing in acrylic acid, Sodium Polyacrylate, ammonium polyacrylate, polyacrylic acid potassium, polyvinyl alcohol, gum arabic and polyethylene glycol etc.
It is one or more.
10. preparation method described in claim 1, it is characterised in that reducing agent used is sodium hypophosphite, ortho phosphorous acid, boron
Any one or more ofs such as sodium hydride, potassium borohydride, hydrazine, hydrazine sulfate, lignocaine borine and dimethylamino borine.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810237478.4A CN108356281A (en) | 2018-03-16 | 2018-03-16 | A kind of preparation method of Nickel Powder |
| CN201910186579.8A CN109732101B (en) | 2018-03-16 | 2019-03-11 | Preparation method of flaky nickel powder |
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| CN201810237478.4A CN108356281A (en) | 2018-03-16 | 2018-03-16 | A kind of preparation method of Nickel Powder |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108588768A (en) * | 2018-05-29 | 2018-09-28 | 广州市华番盛化工科技有限公司 | Steel and iron parts alkalinity deep hole nickel-plating additive, pre-plating solution and pre-plating process |
| CN109732101A (en) * | 2018-03-16 | 2019-05-10 | 南京林业大学 | A kind of preparation method of Nickel Powder |
| CN112251740A (en) * | 2020-10-21 | 2021-01-22 | 广州三孚新材料科技股份有限公司 | Chemical nickel plating brightener for heterojunction solar cell and preparation method thereof |
| CN113264607A (en) * | 2021-05-14 | 2021-08-17 | 深圳市小荷环保技术有限公司 | Method for promoting reduction recovery of high-concentration nickel in chemical nickel plating waste liquid |
-
2018
- 2018-03-16 CN CN201810237478.4A patent/CN108356281A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109732101A (en) * | 2018-03-16 | 2019-05-10 | 南京林业大学 | A kind of preparation method of Nickel Powder |
| CN108588768A (en) * | 2018-05-29 | 2018-09-28 | 广州市华番盛化工科技有限公司 | Steel and iron parts alkalinity deep hole nickel-plating additive, pre-plating solution and pre-plating process |
| CN112251740A (en) * | 2020-10-21 | 2021-01-22 | 广州三孚新材料科技股份有限公司 | Chemical nickel plating brightener for heterojunction solar cell and preparation method thereof |
| CN113264607A (en) * | 2021-05-14 | 2021-08-17 | 深圳市小荷环保技术有限公司 | Method for promoting reduction recovery of high-concentration nickel in chemical nickel plating waste liquid |
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