CN108500289A - The preparation method of flake silver powder in a kind of alkaline medium - Google Patents
The preparation method of flake silver powder in a kind of alkaline medium Download PDFInfo
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- CN108500289A CN108500289A CN201810237830.4A CN201810237830A CN108500289A CN 108500289 A CN108500289 A CN 108500289A CN 201810237830 A CN201810237830 A CN 201810237830A CN 108500289 A CN108500289 A CN 108500289A
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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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- 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
- B22F1/17—Metallic particles coated with metal
Abstract
The present invention provides a kind of preparation method of flake silver powder, this method is using water, silver salt, complexing agent, silver-plating brightener, dispersant, alkali, the crystallization of sheet alkali compounds and reducing agent as raw material, using the method for chemical plating, it is silver-plated in sheet alkali compounds crystal surface, up to silver ion, the reaction was complete, after reaction, by separating-purifying and Treatment technique for processing process, without ball milling, flake silver 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 flake silver powder technique, industrialization prospect is good.
Description
Technical field
The present invention relates to a kind of preparation methods of flake silver powder in alkaline medium, belong to the technology of preparing of metal powder material
Field.
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 provides one kind with water, silver salt, complexing agent, silver-plating brightener, dispersant, alkali, sheet alkali compounds knot
Crystal template and reducing agent are raw material, the method for preparing flake silver powder.This method is with low energy consumption, environmental pollution is small, production technology
Simply, production process route is short, the feature that small, product purity is high and yield is high is invested in large-scale production, and industrialization prospect is good.
Currently, this method is there is not yet document report.
Invention content
The preparation method of flake silver powder in a kind of alkaline medium of the present invention, provides a kind of preparation side of flake silver powder
Method, this method is with water, silver salt, complexing agent, silver-plating brightener, dispersant, alkali, sheet alkali compounds crystallization template and reducing agent
For raw material, using the method for chemical plating, silver-plated in sheet alkali compounds crystallization template surface, up to silver ion, the reaction was complete,
After reaction, through separating-purifying and Treatment technique for processing process to get to flake silver powder.
1, in a kind of alkaline medium of the present invention flake silver powder preparation method, it is characterised in that the system of flake silver powder
It is standby to adopt the following technical scheme that：
1. sheet alkali compounds crystallizes the preparation of template：According to surfactant, the matter of alkali compounds crystallization and water
It is (0.1%~30.0%): (0.1%~30.0%): the ratio of (55.0%~95.0%) to measure percentage, first by water and surface
Activating agent mixes, to get to aqueous surfactant solution after stirring and dissolving is complete；Aqueous surfactant solution is heated to boiling
It rises, alkali compounds crystallization stirring is added to abundant dissolving, the saturated solution of alkali compounds crystallization is obtained by filtration while hot；By alkali
Property compound crystallization saturated solution be placed in temperature control crystallisation by cooling in 50 DEG C of insulating box, after temperature of charge drops to 50 DEG C,
Material is taken out from insulating box, then allows material cooled to room temperature, keeps crystallization complete；Material filtering obtains sheet alkalinity chemical combination
Object crystallizes crude product, filters mother liquid obtained recycling, and sheet alkali compounds crystallizes crude product and presses its quality again, separately take 1~
Crystallization is obtained by filtration in 0~5 DEG C of cold water wash crystallization of 10 times of crystalline qualities 2~3 times, and crystallization, which is dried, obtains sheet alkalinity
Compound crystallizes template；
2. alkali compounds containing sheet crystallizes the preparation of the alkaline mixt of template and silver salt：According to water, silver salt, complexing
The mass percent that agent, silver-plating brightener, dispersant, alkali and sheet alkali compounds crystallize template is (35.0%~95.0%)
: (0.1%~30.0%): (0.1%~30.0%): (0.001%~30.0%): (0.1%~30.0%): (0.1%~
30.0%): the ratio of (0.1~30.0%) first mixes water, silver salt, complexing agent, silver-plating brightener, dispersant and alkali, stirring
Be completely dissolved to all materials, add sheet alkali compounds crystallization template, stir and with ultrasonic echography processing 1~
Sheet alkali compounds crystallization template is ground into the flaky crystal that grain size is 0.5~20.0 μm by 60min with ultrasonic echography
Afterwards to get to alkali compounds containing sheet crystallize template and silver salt alkaline mixt；
3. 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；
4. the preparation of flake silver powder：The alkaline mixt room temperature that alkali compounds containing sheet is crystallized to template and silver salt is cold
Water-bath cooling makes reaction system maintain room temperature, under stirring condition, is gradually added reducing agent aqueous solution, by silver ion reduction at
Metallic silver and chemical plating are plated to sheet alkali compounds crystallization template surface, and up to silver ion, the reaction was complete；Due to sheet alkalinity
Compound crystallization template is only very slightly soluble in cold water, but is dissolved in hot water and boiling water, therefore, reaction product is heated to boiling, makes sheet
Alkali compounds crystallization template is dissolved in boiling water, silver strip crude product is obtained by filtration while hot, gained silver strip crude product is washed through multiple boiling water
After washing and filtering repetitive operation purification while hot, then warp plus water are dispersed with stirring, ultrasonic echography crushes 1~6h, filtering, absolute ethyl alcohol
Washing, filtering and dry technical process are to get being 0.5~3.0 μm to average grain diameter and piece that average thickness is 10~30nm
Shape silver powder；
Wherein, water used is any one of distilled water, deionized water, ultra-pure water and high purity water；
Wherein, alkali compounds used crystallization is any in antifebrin, para-totuidine, naphthalidine and 2- naphthylamines
Kind；
Wherein, ultrasonic wave used is the ultrasonic wave that frequency is 20KHz~1MHz, power is 30W~15KW.
2, in a kind of alkaline medium flake silver powder preparation method, it is characterised in that this method prepare flake silver powder technology
Index is：
1) appearance：Grey is to dark gray powder；
2) purity：>=99.9%；
3) particle size range：0.050~5 μm；
4) average grain diameter：0.5~3.0 μm；
5) thickness range：5~60nm；
6) average thickness：10~30nm；
7) apparent density：2.1~3.2g/cm3；
8) tap density：2.9~4.1g/cm3。
3, in a kind of alkaline medium flake silver powder preparation method, it is characterised in that this method has following significant excellent
Point：
(1) when preparing sheet alkali compounds crystallization template, the saturated solution that alkali compounds crystallizes is placed in temperature control and is existed
Crystallisation by cooling in 50 DEG C of insulating box is to reduce the cooling velocity of material by reducing the temperature difference of material and environment, to reduce
Crystallization rate, it is therefore an objective to keep the flaky crystal to be formed more regular；The sheet alkali compounds that material filtering obtains crystallizes crude product,
0~5 DEG C of cold water of 1~10 times of crystallization crude product quality is selected to wash 2~3 times, in order to reduce sheet alkalinity chemical combination
The loss of object crystallization improves the preparation efficiency of sheet alkali compounds crystallization template；The crystallization of sheet alkali compounds refers to the alkali
Property compound crystal shape be flaky crystal, crystallized as template with sheet alkali compounds, silver by chemical plating is plated to sheet
Alkali compounds crystallization template surface can form sheet silver, and the preparation process of sheet silver is simple；
(2) the sheet alkali compounds crystallization template selected must be slightly soluble in cold water, be dissolved in hot water and boiling water, in this way can be with
After reaction product is heated to boiling, sheet alkali compounds crystallization template is made to be dissolved in boiling water, after filtering while hot, then through repeatedly boiling
Water washing and repetitive operation is filtered while hot, you can remove impurity and sheet alkali compounds crystallizes template, impurity and template are easy to
It removes, purifying technique simply, quickly and efficiently, is conducive to the flake silver powder that high-purity is prepared, silver powder purity is reachable
99.9% or more, product purity is high；
(3) firstly, since the sheet alkali compounds crystallization template selected is slightly soluble in cold water, it is dissolved in hot water and boiling water, institute
With the preparation reaction of sheet silver is optimally maintained to be carried out at room temperature, is conducive to during the reaction, keep sheet alkalization in this way
The amount for closing object crystallization template is not reduced because of dissolving, and the amount of sheet alkali compounds crystallization template is just stablized, to flake silver powder thickness
The controllability of degree is with regard to strong；Secondly as the sheet alkali compounds crystallization template selected belongs to alkaloid compound, reaction must be
It is carried out under alkaline environment, so, reactant must keep pH ＞ 7, avoid the amount of sheet alkali compounds crystallization template in acidity
It is reduced because of acid-base neutralization reaction in environment, in this way, the amount of sheet alkali compounds crystallization template is just stablized, to flake silver powder thickness
The controllability of degree is with regard to strong；In the case that silver salt dosage determines, the use of template is crystallized by changing sheet alkali compounds for third
Amount adjusts the ratio of silver salt and sheet alkali compounds crystallization template, you can the effectively thickness of control flake silver powder；4th, it uses
Ultrasonic echography crushes the sheet silver that sheet alkali compounds crystallization template and chemical plating obtain, when adjusting ultrasonic echography crushing
Between, the grain size of flake silver powder can be effectively controlled, size controlling method is simple and effective；In short, the present invention both can effectively control sheet
The thickness of silver powder, and the grain size of flake silver powder can be effectively controlled, the flake silver powder of high-specific surface area, specific surface area can be prepared
It is 5~15 times of ball-milling method；
(4) in the preparation process of flake silver powder, the purpose of silver-plating brightener is added, is to keep chemical plating silver layer light flat
It is whole, improve the flatness and finish of flake silver powder particle surface；In the preparation process of flake silver powder, the mesh of complexing agent is added
, be in order to form the dynamic equilibrium of free silver ions and silver-colored complex ion in the reaction system, with the free silver of effective control from
The concentration of son, and then the deposition velocity of the reduction reaction speed and silver of silver ion is controlled, to obtain uniform silvering, and it is
Keep chemical plating silver layer light smooth, can also effectively improve the flatness and finish of flake silver powder particle surface；This is all advantageous
In improving the intergranular contact area of flake silver powder, the electric conductivity with the product of flake silver powder particle formulation is improved, and is not added
The flake silver powder that silver-plating brightener is prepared with complexing agent is added to compare, the electric conductivity of flake silver powder prepared by the present invention can be improved
35% or so, improvement effect is apparent；
(5) in the preparation process of flake silver powder, the purpose of dispersant is added, is particle agglomeration in order to prevent, improves sheet
The dispersibility of silver powder particles, so that flake silver powder is easily dispersed when preparing product with flake silver powder, user is easy to use, improves
The performance of flake silver powder；
(6) it compared with the thick product for using ball shape silver powder to prepare, is prepared using flake silver powder produced by the invention
Thick product, such as conductive adhesive, electrocondution slurry, conductive coating and electrically conductive ink, since flake silver powder is in sticky system
In have thixotropic property, make product sedimentation stability and storage stability improve 50% or so, the stability of product is good；
(7) silver belongs to soft metal, and silver powder particles are pressurized or are impacted and can be laminated agglomerating, therefore, ball mill grinding and grind
Be milled it is broken can cause to be laminated agglomerating and reunite between silver powder particles, the present invention is using ultrasonic echography comminuting method by silver strip powder
It is 0.5~3.0 μm of flake silver powder to be broken into average grain diameter, silver powder particles can be effectively prevent to reunite；
(8) after preparing flake silver powder the reaction was complete, when reaction product is heated to boiling, due to sheet alkali compounds
Crystallization template is slightly soluble in cold water, but is dissolved in hot water and boiling water, therefore, after silver strip is taken out in filtering while hot, sheet alkali compounds knot
Crystal template stays in the mother liquor of filtering gained, and after mother liquor cooling, sheet alkali compounds crystallization template crystallizes precipitation again, precipitation
Again with after the method separating-purifying of recrystallization, sheet alkali compounds crystallization template can recycle, and therefore, both save for crystallization
Template resource and production cost is reduced, and reduce the discharge of pollutant, improves economic benefit and environmental benefit；
(9) technological requirement that the mantle plate method reported prepares flake silver powder is high, severe reaction conditions, and control is improper often
What is obtained is graininess silver powder rather than flake silver powder, and therefore, the technique repetition stability that mantle plate method prepares flake silver powder is poor,
Unstable product quality, or even cannot get flake silver 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 silver powder
Problem, such as silver 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 flake silver powder；Biological template prepares flake silver 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 flake silver powder is 100%, and template easily removes, and product purity exists
99.9% or more, production cost is low, and production efficiency is high；
(10) technical solution of the present invention have low energy consumption, environmental pollution is small, simple production process, process route letter
Short, large-scale production equipment investment is small, and production efficiency is high, and production cost is low, the dispersion performance of product and the system that conducts electricity very well
Row advantage, is suitable for large-scale production, solves the problems, such as that existing ball-milling method and template prepare flake silver powder technique,
Industrialization prospect is good.
4, in a kind of alkaline medium of the present invention flake silver powder preparation method, it is characterised in that surface used live
Property agent is lauryl sodium sulfate, ammonium lauryl sulfate, dodecyl sulphate potassium, dodecyl sulphate monoethanolamine, 12
Alkylsurfuric acid diethanol amine, dodecyltriethanolamine sulfate, sodium hexadecyl sulfate, hexadecyl hydrosulfate ammonium, cetyl
Potassium sulfate, hexadecyl hydrosulfate monoethanolamine, hexadecyl hydrosulfate diethanol amine, hexadecyl hydrosulfate triethanolamine, dodecane
Base polyethenoxy ether sodium sulfate, dodecyl polyoxyethylene ether ammonium sulfate, dodecyl polyoxyethylene ether potassium sulfate, dodecyl
Polyoxyethylene ether diethanolamine, dodecyl polyoxyethylene ether sulfate, dodecyl polyoxyethylene ether sulfuric acid
Triethanolamine, sodium cetanesulfonate, cetyl ichthyodin, cetyl potassium sulfonate, cetyl sulfonic acid monoethanolamine, ten
Six alkyl sulfonic acid diethanol amine, cetyl sulfonic acid triethanolamine, neopelex, dodecyl benzene sulfonic acid ammonium, ten
Dialkyl benzene sulfonic acids potassium, dodecyl benzene sulfonic acid monoethanolamine, dodecyl benzene sulfonic acid diethanol amine, dodecyl benzene sulfonic acid three
Ethanol amine, nonylphenol polyoxyethylene ether sulfate, nonylphenol polyoxyethylene ether ammonium sulfate, nonylphenol polyoxyethylene ether potassium sulfate,
Nonylphenol polyoxyethylene ether diethanolamine, nonylphenol polyoxyethylene ether sulfate, nonylphenol polyoxyethylene ether sulphur
Triethylenetetraminehexaacetic acid hydramine, coconut oil alkanolamide, lauroylamidopropyl betaine, Cocoamidopropyl betaine, soyamide propyl
Glycine betaine, octadecyl dimethyl amine oxide and dodecyldimethylamine oxide it is any one or more.
5, in a kind of alkaline medium of the present invention flake silver powder preparation method, it is characterised in that silver salt used is
Silver fluoride, silver nitrate, silver citrate, actol, silver tartrate and silver acetate any one or more of.
6, in a kind of alkaline medium of the present invention flake silver powder preparation method, it is characterised in that complexing agent used
It is N-hydroxyethyl-ethylenediamine triacetic acid, N-hydroxyethyl-ethylenediamine triacetic acid trisodium, nitrilotriacetic acid, nitrilotriacetic acid trisodium salt, ethylenediamine
Tetraacethyl, disodium ethylene diamine tetraacetate, citric acid, sodium citrate, potassium citrate, ammonium citrate, tartaric acid, sodium tartrate, wine
Stone acid potassium, potassium antimony tartrate and ammonium tartrate any one or more of.
7, in a kind of alkaline medium of the present invention flake silver powder preparation method, it is characterised in that silver-plated light used
Bright dose be HL-SP201A/B, KYU AG-1 bright silvers additive, Silverstar NM-02 Bright Silver Plating Process silver photo etching,
Carbon disulfide, thiocarbamide, potassium xanthate, xanthic acid antimony, xanthic acid tin, sodium thiosulfate, ATS (Ammonium thiosulphate), sulfamic acid, grape
Saccharic acid antimony potassium, potassium antimony tartrate, sodium sulfocyanate, potassium rhodanide, ammonium thiocyanate, aminodithioformic acid, aminodithioformic acid
Sodium, ammonium dithiocarbamate, aminodithioformic acid potassium, thiocarbohydrazide, thioglycolic acid, 2 mercaptopropionic acid, 2- sulfydryls
Niacin, cystine, 2-mercaptothiazoline, 1- mercapto glycerols, thiosalicylic acid, thio-diethylene glycol, thioacetic acid, thio dipropyl
Acid, Thioproline, AG-300 plating silver additives and SILVER B/ST bright silver additive any one or more ofs.
8, in a kind of alkaline medium of the present invention flake silver powder preparation method, it is characterised in that dispersant used
It is polyvinylpyrrolidone, carboxymethyl cellulose, sodium carboxymethylcellulose, methylcellulose, hydroxyethyl cellulose, methylol fibre
Tie up element, hydroxypropyl cellulose, gelatin, polyacrylic acid, Sodium Polyacrylate, ammonium polyacrylate, polyacrylic acid potassium, polyvinyl alcohol, Ah
Draw uncle's natural gum and polyethylene glycol any one or more of.
9, in a kind of alkaline medium of the present invention flake silver powder preparation method, it is characterised in that alkali used is
Any one of ammonia, ammonium hydroxide, ethylenediamine, n-butylamine, n-amylamine, diethylenetriamine, triethylene tetramine and tetraethylenepentamine are more
Kind.
10, in a kind of alkaline medium of the present invention flake silver powder preparation method, it is characterised in that reduction used
Agent is azanol, ethanol amine, diethanol amine, triethanolamine, formaldehyde, acetaldehyde, glucose, ascorbic acid, sodium hypophosphite, hydrazine hydrate
With sodium borohydride any one or more 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 alkaline medium in flake silver powder preparation method nonlimiting examples, providing for these embodiments be only
Achieve the purpose that present invention is further described in detail, not to the present invention in any form with substantial limitation；It must
Note that it is assumed 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
It can also make several improvements, supplement and optimize, these are improved, supplement and optimization also should be regarded as protection scope of the present invention；Institute
Have and be familiar with those skilled in the art, in the case where not departing from the method for the present invention range, utilizes technical solution of the present invention
Process modification, scheme supplement and raw material proportioning optimization are carried out with technology contents, is accordingly to be regarded as the equivalent embodiment of the present invention；Meanwhile
Substantial technological any equivalent improvement, supplement and the optimization made for the present invention of all methods according to the present invention, also belong to this hair
The technical scope of bright method；In the examples below that, unless stated otherwise, all percentage all refers to mass percent.
Table one, Examples 1 to 9 raw material and proportioning
It notes [1]：Wang Chongguo, Chen Weidong.Influence of the ratio of grinding media to material to high density flake silver powder.It is Chinese metallurgical, 2015,25 (8)：
15-17。
According to the raw material and proportioning of Examples 1 to 9 in table one, the detailed technology scheme and preparation process of Examples 1 to 9 walk
It is rapid as follows：
1. sheet alkali compounds crystallizes the preparation of template：According to the surfactant of Examples 1 to 9, alkalinity in table one
Compound crystallizes and the mass percent of water, first mixes water with surfactant, lives to get to surface after stirring and dissolving is complete
Property agent aqueous solution；Aqueous surfactant solution is heated to boiling, alkali compounds crystallization stirring is added to abundant dissolving, while hot
The saturated solution of alkali compounds crystallization is obtained by filtration；The saturated solution that alkali compounds crystallizes is placed in perseverance of the temperature control at 50 DEG C
Crystallisation by cooling in incubator takes out material, then material is allowed to naturally cool to room after temperature of charge drops to 50 DEG C from insulating box
Temperature keeps crystallization complete；Material filtering obtains sheet alkali compounds crystallization crude product, filters mother liquid obtained recycling, sheet
Alkali compounds crystallizes crude product and presses its quality again, separately takes 0~5 DEG C of cold water wash crystallization 2~3 of 1~10 times of crystalline quality
It is secondary, crystallization is obtained by filtration, crystallization, which is dried, obtains sheet alkali compounds crystallization template；
2. alkali compounds containing sheet crystallizes the preparation of the alkaline mixt of template and silver salt：According to embodiment 1 in table one
~9 water, the mass percent of silver salt, complexing agent, silver-plating brightener, dispersant, alkali and sheet alkali compounds crystallization template,
First water, silver salt, complexing agent, silver-plating brightener, dispersant and alkali are mixed, stirring is completely dissolved to all materials, adds piece
Shape alkali compounds crystallizes template, stirs and handles 1~60min with ultrasonic echography, and sheet alkali compounds is crystallized template
It is after 0.5~20.0 μm of flaky crystal to get to the crystallizing mould of alkali compounds containing sheet to be ground into grain size with ultrasonic echography
The alkaline mixt of plate and silver salt；
3. the preparation of reducing agent aqueous solution：It, will according to the reducing agent of Examples 1 to 9 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；
4. the preparation of flake silver powder：The alkaline mixt room temperature that alkali compounds containing sheet is crystallized to template and silver salt is cold
Water-bath cooling makes reaction system maintain room temperature, under stirring condition, is gradually added reducing agent aqueous solution, by silver ion reduction at
Metallic silver and chemical plating are plated to sheet alkali compounds crystallization template surface, and up to silver ion, the reaction was complete；Due to sheet alkalinity
Compound crystallization template is only very slightly soluble in cold water, but is dissolved in hot water and boiling water, therefore, reaction product is heated to boiling, makes sheet
Alkali compounds crystallization template is dissolved in boiling water, silver strip crude product is obtained by filtration while hot, gained silver strip crude product is washed through multiple boiling water
After washing and filtering repetitive operation purification while hot, then warp plus water are dispersed with stirring, ultrasonic echography crushes 1~6h, filtering, absolute ethyl alcohol
Washing, filtering and dry technical process are to get being 0.5~3.0 μm to average grain diameter and piece that average thickness is 10~30nm
Shape silver powder；
Wherein, ultrasonic wave used is the ultrasonic wave that frequency is 20KHz~1MHz, power is 30W~15KW.
Claims (10)
1. the preparation method of flake silver powder in a kind of alkaline medium, it is characterised in that：
1. sheet alkali compounds crystallizes the preparation of template：According to surfactant, the quality hundred of alkali compounds crystallization and water
Divide than being (0.1%~30.0%): (0.1%~30.0%): the ratio of (55.0%~95.0%), first by water and surface-active
Agent mixes, to get to aqueous surfactant solution after stirring and dissolving is complete；Aqueous surfactant solution is heated to boiling, is added
Enter alkali compounds crystallization stirring to abundant dissolving, the saturated solution of alkali compounds crystallization is obtained by filtration while hot；By alkalization
The saturated solution for closing object crystallization is placed in temperature control crystallisation by cooling in 50 DEG C of insulating box, after temperature of charge drops to 50 DEG C, from perseverance
Material is taken out in incubator, then allows material cooled to room temperature, keeps crystallization complete；Material filtering obtains sheet alkali compounds knot
Brilliant crude product filters mother liquid obtained recycling, and sheet alkali compounds crystallizes crude product and presses its quality again, separately takes 1~10 times
In 0~5 DEG C of cold water wash crystallization 2~3 times of crystalline quality, crystallization is obtained by filtration, crystallization, which is dried, obtains sheet alkalinity chemical combination
Object crystallizes template；
2. alkali compounds containing sheet crystallizes the preparation of the alkaline mixt of template and silver salt：According to water, silver salt, complexing agent, plating
The mass percent that silver-colored brightener, dispersant, alkali and sheet alkali compounds crystallize template is (35.0%~95.0%):
(0.1%~30.0%): (0.1%~30.0%): (0.001%~30.0%): (0.1%~30.0%): (0.1%~
30.0%): the ratio of (0.1~30.0%) first mixes water, silver salt, complexing agent, silver-plating brightener, dispersant and alkali, stirring
Be completely dissolved to all materials, add sheet alkali compounds crystallization template, stir and with ultrasonic echography processing 1~
Sheet alkali compounds crystallization template is ground into the flaky crystal that grain size is 0.5~20.0 μm by 60min with ultrasonic echography
Afterwards to get to alkali compounds containing sheet crystallize template and silver salt alkaline mixt；
3. 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；
4. the preparation of flake silver powder：Alkali compounds containing sheet is crystallized to the alkaline mixt room temperature cold bath of template and silver salt
It is cooling, so that reaction system is maintained room temperature, under stirring condition, reducing agent aqueous solution is gradually added, by silver ion reduction at metal
Silver and chemical plating are plated to sheet alkali compounds crystallization template surface, and up to silver ion, the reaction was complete；Due to sheet alkalinity chemical combination
Object crystallization template is only very slightly soluble in cold water, but is dissolved in hot water and boiling water, therefore, reaction product is heated to boiling, and keeps sheet alkaline
Compound crystallization template is dissolved in boiling water, is obtained by filtration silver strip crude product while hot, gained silver strip crude product through the washing of multiple boiling water and
After the purification of filtering repetitive operation while hot, then through plus water is dispersed with stirring, ultrasonic echography crushes 1~6h, filtering, absolute ethyl alcohol are washed
The technical process such as wash, filter and dry to get being 0.5~3.0 μm to average grain diameter and sheet that average thickness is 10~30nm
Silver powder；
Wherein, water used is any one of distilled water, deionized water, ultra-pure water and high purity water；
Wherein, alkali compounds used crystallization is any one of antifebrin, para-totuidine, naphthalidine and 2- naphthylamines；
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 the technical indicator of the flake silver powder of preparation is：
1) appearance：Grey is to dark gray powder；
2) purity：>=99.9%；
3) particle size range：0.050~5 μm；
4) average grain diameter：0.5~3.0 μm；
5) thickness range：5~60nm；
6) average thickness：10~30nm；
7) apparent density：2.1~3.2g/cm3；
8) tap density：2.9~4.1g/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 surfactant used is lauryl sodium sulfate, 12
Alkylsurfuric acid ammonium, dodecyl sulphate potassium, dodecyl sulphate monoethanolamine, dodecyl sulphate diethanol amine, dodecyl
Sulfuric acid triethanolamine, sodium hexadecyl sulfate, hexadecyl hydrosulfate ammonium, hexadecyl hydrosulfate potassium, hexadecyl hydrosulfate monoethanol
Amine, hexadecyl hydrosulfate diethanol amine, hexadecyl hydrosulfate triethanolamine, dodecyl polyoxyethylene ether sodium sulphate, dodecane
Base polyoxyethylene ether ammonium sulfate, dodecyl polyoxyethylene ether potassium sulfate, dodecyl polyoxyethylene ether diethanolamine, ten
Dialkyl group laureth sulfate, dodecyl polyoxyethylene ether sulfuric acid triethanolamine, sodium cetanesulfonate, ten
Six alkyl sulfonic acid ammoniums, cetyl potassium sulfonate, cetyl sulfonic acid monoethanolamine, cetyl sulfonic acid diethanol amine, hexadecane
Base sulfonic acid triethanolamine, neopelex, dodecyl benzene sulfonic acid ammonium, Potassium dodecylbenzenesulfonate, detergent alkylate
Sulfonic acid monoethanolamine, dodecyl benzene sulfonic acid diethanol amine, dodecyl benzene sulfonic acid triethanolamine, nonylphenol polyoxyethylene ether sulphur
Sour sodium, nonylphenol polyoxyethylene ether ammonium sulfate, nonylphenol polyoxyethylene ether potassium sulfate, nonylphenol polyoxyethylene ether sulfuric acid monoethanol
Amine, nonylphenol polyoxyethylene ether sulfate, nonylphenol polyoxyethylene ether sulfuric acid triethanolamine, coconut oil alkanolamide,
Lauroylamidopropyl betaine, Cocoamidopropyl betaine, soyamide propyl betaine, octadecyl dimethyl amine oxide
With any one or more ofs such as dodecyldimethylamine oxide.
5. preparation method described in claim 1, it is characterised in that silver salt used is silver fluoride, silver nitrate, silver perchlorate, lemon
Lemon acid silver, actol, silver tartrate and silver acetate any one or more of.
6. 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, nitrilotriacetic acid, nitrilotriacetic acid trisodium salt, ethylenediamine tetra-acetic acid, disodium ethylene diamine tetraacetate, lemon
Lemon acid, sodium citrate, potassium citrate, ammonium citrate, tartaric acid, sodium tartrate, potassium tartrate, potassium antimony tartrate and ammonium tartrate
Etc. any one or more ofs.
7. preparation method described in claim 1, it is characterised in that silver-plating brightener used is HL-SP201A/B, KYU AG-
1 bright silver additive, Silverstar NM-02 Bright Silver Plating Process silver photo etching, carbon disulfide, thiocarbamide, potassium xanthate, Huang
Ortho acid antimony, xanthic acid tin, sodium thiosulfate, ATS (Ammonium thiosulphate), sulfamic acid, Pentostam potassium, potassium antimony tartrate, thiocyanic acid
It is sodium, potassium rhodanide, ammonium thiocyanate, aminodithioformic acid, nabam, ammonium dithiocarbamate, two thio
Potassium carbamate, thiocarbohydrazide, thioglycolic acid, 2 mercaptopropionic acid, 2- mercaptonicotinic acids, cystine, 2-mercaptothiazoline, 1-
Mercapto glycerol, thiosalicylic acid, thio-diethylene glycol, thioacetic acid, thio-2 acid, Thioproline, AG-300 are silver-plated to be added
Add any one or more ofs such as agent and SILVER B/ST bright silver additives.
8. 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
Any in acrylic acid, Sodium Polyacrylate, ammonium polyacrylate, polyacrylic acid potassium, polyvinyl alcohol, gum arabic and polyethylene glycol
Kind is a variety of.
9. preparation method described in claim 1, it is characterised in that alkali used is ammonia, ammonium hydroxide, ethylenediamine, n-butylamine, positive penta
Any one or more ofs such as amine, diethylenetriamine, triethylene tetramine and tetraethylenepentamine.
10. preparation method described in claim 1, it is characterised in that reducing agent used be azanol, ethanol amine, diethanol amine,
Any one of triethanolamine, formaldehyde, acetaldehyde, glucose, ascorbic acid, sodium hypophosphite, hydrazine hydrate and sodium borohydride are more
Kind.
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| CN201910158659.2A CN109663932B (en) | 2018-03-16 | 2019-02-28 | Preparation method of flaky silver powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109663932A (en) * | 2018-03-16 | 2019-04-23 | 南京林业大学 | A kind of preparation method of flake silver powder |
| CN110270693A (en) * | 2019-07-12 | 2019-09-24 | 刘松青 | A kind of silver nanowires continuous producing method that solvent recovery cycle utilizes |
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2018
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109663932A (en) * | 2018-03-16 | 2019-04-23 | 南京林业大学 | A kind of preparation method of flake silver powder |
| CN110270693A (en) * | 2019-07-12 | 2019-09-24 | 刘松青 | A kind of silver nanowires continuous producing method that solvent recovery cycle utilizes |
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