CN102672199A - Preparation method of silver particle with sheet-strip integrated structural shape - Google Patents
Preparation method of silver particle with sheet-strip integrated structural shape Download PDFInfo
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- CN102672199A CN102672199A CN2012101797483A CN201210179748A CN102672199A CN 102672199 A CN102672199 A CN 102672199A CN 2012101797483 A CN2012101797483 A CN 2012101797483A CN 201210179748 A CN201210179748 A CN 201210179748A CN 102672199 A CN102672199 A CN 102672199A
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Abstract
The invention relates to a preparation method of a silver particle with a sheet-strip integrated structural shape. The preparation method of the silver particle with the sheet-strip integrated structural shape comprises the following step of preparing the silver particle with the sheet-strip integrated structural shape by a chemical liquid-phase reduction method by taking deionized water or distilled water as a solvent, a soluble silver salt as a silver source, an organic acid and/ or an organic acid salt and an inorganic acid as main shape controlling agents, a small molecular alcohol and/ or ketone as a modifier, and ascorbic acid and/ or ascorbate as a reductant, wherein the silver particle has an integral structure consisting of silver by sheet-shaped silver and strip-shaped silver; the width of the sheet-shaped silver is between 2-20 microns and adjustable; the thickness of the sheet-shaped silver is 100-300 nanometers and adjustable; the length of the strip-shaped silver is 5-50 microns and adjustable; the width of the strip-shaped silver is 200-500 nanometers and adjustable; and the thickness of the strip-shaped silver is 100-300 nanometers and adjustable. The preparation method of the silver particle with the sheet-strip integrated structural shape is mild in preparation conditions; and prepared silver particles are high in yield and high in purity.
Description
Technical field
The present invention relates to a kind of preparation method of special appearance silver granular materials, particularly the preparation method of the silver-colored particle of a kind of band integrative-structure pattern.
Background technology
Because silver powder has performances such as good conduction, heat conduction and catalysis, therefore can be widely used in fields such as electronics industry, catalysis, antibiotic, electromagnetic protection.In electronics industry; Silver powder is mainly as conductive filler; Be prepared into conductive silver paste, electrically-conducting paint, conductive silver glue, conductive silver ink etc., combine oven dry, sintering process to be prepared into conducting wire, conductive pattern, electronic device etc. through technologies such as serigraphy, spraying, inkjet printings.
The preparation method of argent powder mainly contains thermal decomposition method, electrochemical process, atomization, polishing and chemical reduction method.Mostly the silver powder of thermal decomposition method preparation is porous, reunion shape.The silver powder size of electrochemical process preparation is generally bigger, appearance with dendritic be main.Mostly atomization is large-size particle shape silver powder if obtaining.The silver powder pattern that polishing obtains has graininess and sheet etc.Chemical reduction method is to prepare super fine silver powder to adopt maximum methods, and chemical reduction method can carry out accuracy controlling to the pattern and the size of silver powder, obtains the silver powder of various patterns and size.
The pattern of the silver-colored particle powder of the employing chemical reduction method preparation of being reported in patent and the document at present mainly contains sphere, regular sheet, amorphous sheet, wire, bar-shaped, and various patterns such as triangle sheet, dendroid, flower-shaped, cubic shaped are also arranged.Publication number is the technology that the Chinese patent of CN1401452 discloses a kind of chemical reduction method preparation micron flake silver powder; It is predecessor with the silver nitrate, and hydrogen peroxide is a reducing agent, in the blending agent of pure water; With the chloroplatinic acid is that catalyst, PVP are under protectant situation; The synthetic silver powder that obtains the monocrystalline hexagonal flake, the sheet footpath can reach 30～50 μ m, and sheet thickness is 0.1～0.5 μ m.Publication number is the preparation method that the Chinese patent of CN1958197 discloses a kind of Nano silver piece; Seed mediated growth method preparation monocrystal silver nanometer sheet under natrium citricum is assisted is adopted in this invention; Molar ratio between silver in the control seed and the silver-colored source of use; Can obtain the Nano silver piece of nanoscale, the size range that the method makes Nano silver piece is 25nm～500nm, and thickness is 10～30nm; Publication number is the synthetic method that the Chinese patent of CN1424163 discloses a kind of monocrystal silver nano line, and this is invented with AgNO
3The aqueous solution and N-N dimethyl formamide mixed liquor are precursor liquid, after butyl titanate and acetylacetone,2,4-pentanedione mix with AgNO
3Mix precursor liquid and add wherein, under 50～70 ℃, reacted 2～24 hours, obtain monocrystal silver nano line.Publication number is that the Chinese patent of CN1709791 discloses a kind of method for preparing nano silver wire; With quaternary ammonium salt cationic Gemini surfactant is template; With the hexamethylenetetramine is reducing agent, has prepared the nano silver wire of big L/D ratio, diameter homogeneous through hydrothermal synthesis method.At document Vasilev et al.Langmuir, Vol.21, No.26, in 2005, adopting 2-sulfydryl butyric acid is 100 ℃ of reduction gold chlorides down in temperature, obtain curling shape nanowires of gold and afterbody are the mix products of the nano wire of triangular plate.
But up to now, also do not see the report that is equipped with the silver-colored particle of sheet band integrative-structure pattern with the solution reduction legal system in the prior art.
Summary of the invention
The object of the present invention is to provide the preparation method of the silver-colored particle of a kind of band integrative-structure pattern, the integrative-structure that the silver-colored particle of this sheet band integrative-structure pattern is made up of sheet silver and banded silver.
The preparation method of the silver-colored particle of of the present invention band integrative-structure pattern adopts the chemical liquid phase reducing process.For obtaining the silver-colored particle of the uniform sheet band of size integrative-structure pattern; The present invention with deionized water or distilled water as solvent; With soluble silver salt is silver-colored source; With organic acid and/or acylate and inorganic acid is main morphology control agent, can add small molecule alcohol and/or little molecule ketone again as conditioning agent, is the silver-colored particle that reducing agent prepares sheet band integrative-structure pattern with ascorbic acid and/or ascorbate.
Preparation method of the present invention may further comprise the steps:
(1) soluble silver salt is dissolved in deionized water or the distilled water; Obtain the silver salt solution that concentration is 0.1～1mol/L; Add organic acid then and/or acylate obtains mixed solution, making organic acid and/or the acylate concentration in mixed solution is 0.02～1 * 10
-3Mol/L; Inorganic acid is joined in the above-mentioned mixed solution, making the concentration of inorganic acid in mixed solution is 0.01～1mol/L again; Can add small molecule alcohol and/or little molecule ketone as conditioning agent then again, making the deionized water of small molecule alcohol and/or little molecule ketone and above-mentioned dissolving soluble silver salt or the volume ratio of distilled water is 0～2, and the mixed solution that obtains is as oxidation liquid;
(2) ascorbic acid and/or the ascorbate got as reducing agent are dissolved in deionized water or the distilled water, and the solution that is mixed with concentration and is 0.15～1.5mol/L is as reducing solution;
(3) be 0～60 ℃ and stir under the condition of (the general speed that stirs is 100～600 rev/mins) in temperature; The reducing solution that oxidation liquid that step (1) is obtained and step (2) obtain is even for 1:0.5～1:1 rapid mixing in molar ratio, mixes back standing and reacting (time of general standing and reacting is 5～30 minutes); The collecting precipitation product fully carries out dried behind the washing precipitation product, can obtain the silver-colored particle of micron order sheet band integrative-structure pattern.
The integrative-structure that the silver-colored particle of described band integrative-structure pattern is made up of sheet silver and banded silver, wherein, the sheet width of sheet silver part is adjustable between 2～20 microns, and the sheet thickness of sheet silver part is adjustable between 100～300 nanometers; The length dimension of the band of banded silver part is adjustable between 5～50 microns, and the width of band is adjustable between 200～500 nanometers, and the thickness of band is adjustable between 100～300 nanometers.
Method of the present invention; Several kinds of conditions of a kind of conditioned disjunction in the content of the content of concentration, organic acid and/or acylate through changing silver salt solution and reducing solution, content, small molecule alcohol and/or the little molecule ketone of inorganic acid and the reaction temperature etc. can effectively be controlled the pattern and the size of the silver-colored particle of gained sheet band integrative-structure pattern.
The silver-colored particle of described band integrative-structure pattern is a crystal structure, and the type of crystal structure is the face-centered cubic mono-crystalline structures.The purity of the silver-colored particle of described band integrative-structure pattern is not less than 99.5%; The pattern and the size of the silver-colored particle of described band integrative-structure pattern are even, and yield reaches more than 99%.
Described soluble silver salt is silver nitrate or silver acetate etc.
Described reducing agent is ascorbic acid and/or ascorbate, and wherein ascorbate is selected from one or more in sodium ascorbate, potassium ascorbate and the Calcium Ascorbate etc.
Described inorganic acid is a nitric acid etc.
Described organic acid is an ammonia carboxylic class organic acid, is selected from ethylenediamine tetra-acetic acid, 1,2-diaminocyclohexane tetraacetic acid, ethylene glycol diethyl ether ethylenediamine tetraacetic acid (EDTA) and the aminotriacetic acid etc. one or more.
Described acylate is an ammonia carboxylic class acylate, is selected from disodium ethylene diamine tetraacetate, EDTAP dipotassium ethylene diamine tetraacetate, sodium versenate, tetrasodium ethylenediamine tetraacetate, ethylenediamine tetra-acetic acid tripotassium, ethylenediamine tetra-acetic acid four potassium, Ferric Sodium Edetate, 1,2-diaminocyclohexane tetraacetic acid disodium, 1,2-diaminocyclohexane tetraacetic acid dipotassium, aminotriacetic acid disodium, aminotriacetic acid dipotassium and the ethylene glycol diethyl ether edetate disodium etc. one or more.
Described small molecule alcohol is selected from one or more in the solubility small molecular alcohols such as ethanol, propyl alcohol, butanols and ethylene glycol.
Described little molecule ketone is an acetone.
The purpose of described stirring is that oxidation liquid is mixed with the reducing solution rapid and uniform.
Described collecting precipitation product fully carries out dried behind the washing precipitation product, and available water and ethanol wash respectively, filters back natural air drying or low temperature drying.
The main application of the silver-colored particle of the sheet band integrative-structure pattern of the present invention's preparation: can be used as conductive filler and in electrocondution slurry, conducting resinl, electrically-conducting paint, conductive film material, contact material, electromagnetic protection coating, use; Also can be used as catalyst and anti-biotic material uses.
Advantage of the present invention and good effect:
1. the pattern of the silver-colored particle of sheet band integrative-structure pattern and size homogeneous;
2. the productive rate of the silver-colored particle of sheet band integrative-structure pattern is high, and purity is high; The yield of the silver-colored particle of its sheet band integrative-structure pattern reaches more than 99%; Purity is not less than 99.5%;
3. the silver-colored particle of sheet band integrative-structure pattern conducts electricity very well good stability;
4. preparation process condition is gentle, and the output of silver-colored particle is big, and is with low cost;
The reaction temperature of silver-colored particle that the chemical liquid phase reducing process that the present invention adopts prepares sheet band integrative-structure pattern is moderate, and component is simple, and main salt concentration is high, and disposable output is big; Do not need special expensive raw material, therefore with low cost;
5. do not add any surfactant, be prone to washing and collect;
6. the reaction system equipment needed thereby is simple, need not special device, and the equipment input cost is low;
7. the reaction system component is simple, does not have strong toxicity raw material and accessory substance, and treatment cost of waste liquor is low.
Following combine accompanying drawing and embodiment further specify the present invention, but are not limitation of the present invention.
Description of drawings
Fig. 1. the electron scanning micrograph a of the silver-colored particle of the sheet band integrative-structure pattern of the embodiment of the invention 1 preparation and XRD figure spectrum b.
Fig. 2. electron scanning micrograph a, transmission electron microscope photo b and the electronic diffraction spot c of the silver-colored particle of the sheet band integrative-structure pattern of the embodiment of the invention 3 preparations.
Fig. 3. the electron scanning micrograph of the silver-colored particle of the sheet band integrative-structure pattern of the embodiment of the invention 4 preparations.
The specific embodiment
(1) the 2g silver nitrate is dissolved in the 20ml deionized water is mixed with liquor argenti nitratis ophthalmicus; Under stirring, 0.8ml nitric acid (mass concentration is 65～68%) is joined in the liquor argenti nitratis ophthalmicus; The disodium ethylene diamine tetraacetate that adds 0.001g again, the mixed solution that obtains is as oxidation liquid;
(2) get the 1.2g dissolution of ascorbic acid in the 8ml deionized water as reducing solution;
(3) be that 20 ℃ and mixing speed are under 400 rev/mins the condition in temperature, the Restore All liquid rapid mixing that whole oxidation liquid that step (1) is obtained and step (2) obtain is even, mixes the back standing and reacting 15 minutes; Stir the collecting precipitation product then, use washing with alcohol twice again after spending 3～5 precipitated products of deionised water, filter the silver-colored particle that the back low temperature drying obtains sheet band integrative-structure pattern.
Shown in the electron scanning micrograph of Fig. 1 a; The integrative-structure that the silver-colored particle of gained sheet band integrative-structure pattern is made up of sheet silver and banded silver; Wherein, the sheet width of sheet silver part is between 15～20 microns, and the sheet thickness of sheet silver part is between 200～300 nanometers; The length dimension of the band of banded silver part is between 20～30 microns, and the width dimensions of band is between 300～500 nanometers, and the thickness of band is between 200～300 nanometers.Shown in the XRD figure spectrum of Fig. 1 b, the silver-colored particle of described band integrative-structure pattern is a crystal structure, and the type of crystal structure is the face-centered cubic mono-crystalline structures.The purity of the silver-colored particle of described band integrative-structure pattern is not less than 99.5%; The pattern and the size of the silver-colored particle of described band integrative-structure pattern are even, and yield reaches more than 99%.
Embodiment 2
Basic identical with embodiment 1, different use when just preparing liquor argenti nitratis ophthalmicus to be the 1g silver nitrate use when preparing reducing solution is the 0.6g ascorbic acid.Use sem observation, the integrative-structure that the silver-colored particle of gained sheet band integrative-structure pattern is made up of sheet silver and banded silver, wherein, the sheet width of sheet silver part is between 8～10 microns, and the sheet thickness of sheet silver part is between 100～200 nanometers; The length dimension of the band of banded silver part is between 10～25 microns, and the width dimensions of band is between 200～400 nanometers, and the thickness of band is between 100～200 nanometers.
Embodiment 3
(1) the 1g silver nitrate is dissolved in the 15ml deionized water is mixed with liquor argenti nitratis ophthalmicus; Under stirring, 0.4ml nitric acid (mass concentration is 65～68%) is joined in the liquor argenti nitratis ophthalmicus; The disodium ethylene diamine tetraacetate that adds 0.001g again; And adding the 4ml absolute ethyl alcohol, the mixed solution that obtains is as oxidation liquid;
(2) get the 0.6g dissolution of ascorbic acid in the 6ml deionized water as reducing solution;
(3) be that 20 ℃ and mixing speed are under 200 rev/mins the condition in temperature, the Restore All liquid rapid mixing that whole oxidation liquid that step (1) is obtained and step (2) obtain is even, mixes the back standing and reacting 20 minutes; Filter the collecting precipitation product then, use 3～5 precipitated products of deionized water and washing with alcohol respectively, air dry obtains the silver-colored particle of sheet band integrative-structure pattern.
The crystal structure type of the silver-colored particle of described band integrative-structure pattern is the face-centered cubic mono-crystalline structures.Shown in Fig. 2 a, 2b, 2c, the integrative-structure that the silver-colored particle of gained sheet band integrative-structure pattern is made up of sheet silver and banded silver, wherein, the sheet width of sheet silver part is between 6～8 microns, and the sheet thickness of sheet silver part is between 100～150 nanometers; The length dimension of the band of banded silver part is between 10～20 microns, and the width dimensions of band is between 200～300 nanometers, and the thickness of band is between 100～200 nanometers.
Embodiment 4
Basic identical with embodiment 3, different what use when just preparing reducing solution is the 0.7g sodium ascorbate.Use sem observation; The integrative-structure that the silver-colored particle of gained sheet band integrative-structure pattern is made up of sheet silver and banded silver; Wherein, the sheet width of sheet silver part is between 10～15 microns, and the sheet thickness of sheet silver part is between 100～200 nanometers; The length dimension of the band of banded silver part is between 15～25 microns, and the width dimensions of band is between 200～350 nanometers, and the thickness of band is between 100～200 nanometers.
(1) the 1.6g silver nitrate is dissolved in the 31.6ml distilled water is mixed with liquor argenti nitratis ophthalmicus; Under stirring, 0.4ml nitric acid (mass concentration is 65～68%) is joined in the liquor argenti nitratis ophthalmicus; The ethylenediamine tetra-acetic acid that adds 0.001g again; And adding the 8ml absolute ethyl alcohol, the mixed solution that obtains is as oxidation liquid;
(2) get the 0.96g dissolution of ascorbic acid in the 12ml distilled water as reducing solution;
(3) be that 21 ℃ and mixing speed are under 400 rev/mins the condition in temperature, the Restore All liquid rapid mixing that whole oxidation liquid that step (1) is obtained and step (2) obtain is even, mixes the back standing and reacting 20 minutes; Filter the collecting precipitation product then, use 3～5 precipitated products of deionized water and washing with alcohol respectively, air dry obtains the silver-colored particle of sheet band integrative-structure pattern.
Shown in the electron scanning micrograph of Fig. 3; The integrative-structure that the silver-colored particle of gained sheet band integrative-structure pattern is made up of sheet silver and banded silver; Wherein, the sheet width of sheet silver part is between 4～6 microns, and the sheet thickness of sheet silver part is between 150～200 nanometers; The length dimension of the band of banded silver part is between 20～40 microns, and the width dimensions of band is between 200～400 nanometers, and the thickness of band is between 150～200 nanometers.The silver-colored particle of described band integrative-structure pattern is a crystal structure, and the type of crystal structure is the face-centered cubic mono-crystalline structures.
Embodiment 6
Basic identical with embodiment 4, different just reaction temperatures is that 10 ℃ of times with standing and reacting are 30 minutes.Use sem observation, the integrative-structure that the silver-colored particle of gained sheet band integrative-structure pattern is made up of sheet silver and banded silver, wherein, the sheet width of sheet silver part is between 3～6 microns, and the sheet thickness of sheet silver part is between 100～150 nanometers; The length dimension of the band of banded silver part is between 10～20 microns, and the width dimensions of band is between 150～200 nanometers, and the thickness of band is between 100～150 nanometers.
Embodiment 7
(1) the 1g silver nitrate is dissolved in the 20ml deionized water is mixed with liquor argenti nitratis ophthalmicus; Under stirring, 0.4ml nitric acid (mass concentration is 65～68%) is joined in the liquor argenti nitratis ophthalmicus; The disodium ethylene diamine tetraacetate that adds 0.001g again, the mixed solution that obtains is as oxidation liquid;
(2) get the 0.6g dissolution of ascorbic acid in the 6ml deionized water as reducing solution;
(3) be that 35 ℃ and mixing speed are under 400 rev/mins the condition in temperature, the Restore All liquid rapid mixing that whole oxidation liquid that step (1) is obtained and step (2) obtain is even, mixes the back standing and reacting 5 minutes; Stir the collecting precipitation product then, use 3～5 precipitated products of deionized water and washing with alcohol respectively, air dry obtains the silver-colored particle of sheet band integrative-structure pattern.
Use sem observation, the integrative-structure that the silver-colored particle of gained sheet band integrative-structure pattern is made up of sheet silver and banded silver, wherein, the sheet width of sheet silver part is between 4～8 microns, and the sheet thickness of sheet silver part is between 150～200 nanometers; The length dimension of the band of banded silver part is between 15～30 microns, and the width dimensions of band is between 150～250 nanometers, and the thickness of band is between 100～200 nanometers.The crystal structure type of the silver-colored particle of described band integrative-structure pattern is the face-centered cubic mono-crystalline structures.
Embodiment 8
(1) the 1.6g silver acetate is dissolved into is mixed with silver acetate solution in the 32ml deionized water; Under stirring, 0.8ml nitric acid (mass concentration is 65～68%) is joined in the silver acetate solution; The disodium ethylene diamine tetraacetate that adds 0.002g again; And adding the 8ml absolute ethyl alcohol, the mixed solution that obtains is as oxidation liquid;
(2) get the 0.96g dissolution of ascorbic acid in the 12ml deionized water as reducing solution;
(3) be that 22 ℃ and mixing speed are under 600 rev/mins the condition in temperature, the Restore All liquid rapid mixing that whole oxidation liquid that step (1) is obtained and step (2) obtain is even, mixes the back standing and reacting 20 minutes; Filter the collecting precipitation product then, use 3～5 precipitated products of deionized water and washing with alcohol respectively, air dry obtains the silver-colored particle of sheet band integrative-structure pattern.
Use sem observation, the integrative-structure that the silver-colored particle of gained sheet band integrative-structure pattern is made up of sheet silver and banded silver, wherein, the sheet width of sheet silver part is between 4～5 microns, and the sheet thickness of sheet silver part is between 200～300 nanometers; The length dimension of the band of banded silver part is between 15～20 microns, and the width dimensions of band is between 200～500 nanometers, and the thickness of band is between 200～300 nanometers.The crystal structure type of the silver-colored particle of described band integrative-structure pattern is the face-centered cubic mono-crystalline structures.
Embodiment 9
Basic identical with embodiment 8, different when just preparing oxidation liquid with 0.002g disodium ethylene diamine tetraacetate and ethylenediamine tetra-acetic acid (weight ratio is 1:1), when preparing reducing solution with 1g sodium ascorbate and ascorbic acid (weight ratio is 1:1).Use sem observation, the integrative-structure that the silver-colored particle of gained sheet band integrative-structure pattern is made up of sheet silver and banded silver, wherein, the sheet width of sheet silver part is between 4～8 microns, and the sheet thickness of sheet silver part is between 150～300 nanometers; The length dimension of the band of banded silver part is between 15～25 microns, and the width dimensions of band is between 200～400 nanometers, and the thickness of band is between 200～300 nanometers.
Claims (10)
1. the preparation method of the silver-colored particle of a sheet band integrative-structure pattern is characterized in that described preparation method may further comprise the steps:
(1) soluble silver salt is dissolved in deionized water or the distilled water; Obtain the silver salt solution that concentration is 0.1～1mol/L; Add organic acid then and/or acylate obtains mixed solution, making organic acid and/or the acylate concentration in mixed solution is 0.02～1 * 10
-3Mol/L; Inorganic acid is joined in the above-mentioned mixed solution, making the concentration of inorganic acid in mixed solution is 0.01～1mol/L again; And then add small molecular alcohol and/or little molecule ketone as conditioning agent, and making the deionized water of small molecular alcohol and/or little molecule ketone and above-mentioned dissolving soluble silver salt or the volume ratio of distilled water is 0～2, the mixed solution that obtains is as oxidation liquid;
(2) ascorbic acid and/or the ascorbate got as reducing agent are dissolved in deionized water or the distilled water, and the solution that is mixed with concentration and is 0.15～1.5mol/L is as reducing solution;
(3) under temperature is 0～60 ℃ and stirring condition, the reducing solution that oxidation liquid that step (1) is obtained and step (2) obtain mixes for 1:0.5～1:1 in molar ratio, mixes the back standing and reacting; The collecting precipitation product fully carries out dried behind the washing precipitation product, obtains the silver-colored particle of sheet band integrative-structure pattern;
Described organic acid is an ammonia carboxylic organic acid; Described acylate is an ammonia carboxylic acylate.
2. preparation method according to claim 1 is characterized in that: the time of described standing and reacting is 5～30 minutes.
3. preparation method according to claim 1 is characterized in that: the speed of described stirring is 100～600 rev/mins.
4. preparation method according to claim 1 is characterized in that: described soluble silver salt is silver nitrate or silver acetate.
5. preparation method according to claim 1 is characterized in that: described ascorbate is selected from one or more in sodium ascorbate, potassium ascorbate and the Calcium Ascorbate.
6. preparation method according to claim 1 is characterized in that: described inorganic acid is a nitric acid.
7. preparation method according to claim 1 is characterized in that: described ammonia carboxylic organic acid is selected from one or more in ethylenediamine tetra-acetic acid, 1,2-diaminocyclohexane tetraacetic acid, ethylene glycol diethyl ether ethylenediamine tetraacetic acid (EDTA) and the aminotriacetic acid;
Described ammonia carboxylic acylate is selected from one or more in disodium ethylene diamine tetraacetate, EDTAP dipotassium ethylene diamine tetraacetate, sodium versenate, tetrasodium ethylenediamine tetraacetate, ethylenediamine tetra-acetic acid tripotassium, ethylenediamine tetra-acetic acid four potassium, Ferric Sodium Edetate, 1,2-diaminocyclohexane tetraacetic acid disodium, 1,2-diaminocyclohexane tetraacetic acid dipotassium, aminotriacetic acid disodium, aminotriacetic acid dipotassium and the ethylene glycol diethyl ether edetate disodium.
8. preparation method according to claim 1 is characterized in that: described small molecular alcohol is selected from one or more in ethanol, propyl alcohol, butanols and the ethylene glycol; Described little molecule ketone is acetone.
9. preparation method according to claim 1; It is characterized in that: the integrative-structure that the silver-colored particle of described band integrative-structure pattern is made up of sheet silver and banded silver; Wherein, The sheet width of sheet silver part is between 2～20 microns, and the sheet thickness of sheet silver part is between 100～300 nanometers; The length dimension of the band of banded silver part is between 5～50 microns, and the width of band is between 200～500 nanometers, and the thickness of band is between 100～300 nanometers.
10. according to claim 1 or 9 described preparation methods, it is characterized in that: the silver-colored particle of described band integrative-structure pattern is a crystal structure, and the type of crystal structure is the face-centered cubic mono-crystalline structures.
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| CN101579746A (en) * | 2008-05-13 | 2009-11-18 | 中国科学院理化技术研究所 | Method for preparing micron-grade superfine silver powder with shape of pinecone, flower or tree |
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| CN101218051A (en) * | 2005-07-05 | 2008-07-09 | 三井金属矿业株式会社 | Highly crystalline silver powder and process for production of the same |
| CN101200004A (en) * | 2006-12-14 | 2008-06-18 | 中国科学院理化技术研究所 | Chemical preparing process for flake micron silver powder |
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| CN114985758A (en) * | 2022-07-29 | 2022-09-02 | 长春黄金研究院有限公司 | Preparation method of flake silver powder |
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