CN102974837A - Preparation method for flaky nanometer silver powder - Google Patents
Preparation method for flaky nanometer silver powder Download PDFInfo
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- CN102974837A CN102974837A CN2012105009111A CN201210500911A CN102974837A CN 102974837 A CN102974837 A CN 102974837A CN 2012105009111 A CN2012105009111 A CN 2012105009111A CN 201210500911 A CN201210500911 A CN 201210500911A CN 102974837 A CN102974837 A CN 102974837A
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- silver
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- silver powder
- ferrous
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 14
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical group [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000004094 surface-active agent Substances 0.000 claims abstract description 12
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 6
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 6
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 4
- 239000011790 ferrous sulphate Substances 0.000 claims abstract description 3
- 235000003891 ferrous sulphate Nutrition 0.000 claims abstract description 3
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 claims abstract description 3
- 229940071536 silver acetate Drugs 0.000 claims abstract description 3
- YPNVIBVEFVRZPJ-UHFFFAOYSA-L silver sulfate Chemical compound [Ag+].[Ag+].[O-]S([O-])(=O)=O YPNVIBVEFVRZPJ-UHFFFAOYSA-L 0.000 claims abstract description 3
- 229910000367 silver sulfate Inorganic materials 0.000 claims abstract description 3
- 229940010514 ammonium ferrous sulfate Drugs 0.000 claims abstract 2
- 239000000843 powder Substances 0.000 claims description 24
- 239000012266 salt solution Substances 0.000 claims description 4
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 2
- ZLXPLDLEBORRPT-UHFFFAOYSA-M [NH4+].[Fe+].[O-]S([O-])(=O)=O Chemical group [NH4+].[Fe+].[O-]S([O-])(=O)=O ZLXPLDLEBORRPT-UHFFFAOYSA-M 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 20
- 239000000243 solution Substances 0.000 abstract description 11
- 230000035484 reaction time Effects 0.000 abstract description 4
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 abstract description 3
- IMBKASBLAKCLEM-UHFFFAOYSA-L ferrous ammonium sulfate (anhydrous) Chemical group [NH4+].[NH4+].[Fe+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O IMBKASBLAKCLEM-UHFFFAOYSA-L 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 abstract 1
- 239000007864 aqueous solution Substances 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 6
- 229920003081 Povidone K 30 Polymers 0.000 description 6
- 238000006722 reduction reaction Methods 0.000 description 6
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 239000012279 sodium borohydride Substances 0.000 description 3
- 229910000033 sodium borohydride Inorganic materials 0.000 description 3
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical group OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 241000792859 Enema Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- -1 Silver salt Silver nitrate Silver nitrate Silver nitrate Silver sulfate Silver acetate Chemical compound 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 239000000090 biomarker Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000013872 defecation Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007920 enema Substances 0.000 description 1
- 229940095399 enema Drugs 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 239000000829 suppository Substances 0.000 description 1
- 230000001225 therapeutic effect Effects 0.000 description 1
- 230000010512 thermal transition Effects 0.000 description 1
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 1
- 229940038773 trisodium citrate Drugs 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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Abstract
The invention discloses a preparation method for flaky nanometer silver powder. The flaky nanometer silver powder is prepared by performing reaction on a surfactant-containing aqueous solution of silver salt and a solution of ferrous salt at temperature of 0 to 100 DEG C, wherein the silver salt is silver nitrate, silver sulfate or silver acetate; a surfactant is polyvinylpyrrolidone, hexadecyl trimethyl ammonium bromide, sodium dodecyl sulfate or polyethylene glycol; the ferrous salt is ammonium ferrous sulfate or ferrous sulfate; the weight ratio of the silver salt to the ferrous salt is 2:1 to 1:4; and the weight ratio of the silver salt to the surfactant is 50:1 to 1:2. The flaky nanometer silver powder finally obtained by the method has an undiversified shape and high purity. The method also has the advantages of short reaction time, high efficiency, mild reaction conditions, simple process and equipment, low production cost, convenience for operation, no pollution and the like, and is particularly suitable for industrial production.
Description
Technical field
The present invention relates to a kind of preparation method of metal dust, be specifically related to a kind of preparation method of flake nano silver powder.
Background technology
Flake nano silver powder is face contact or line contact between particle because its surface area is relatively large, so resistance is relatively low, electric conductivity is better.In addition, the surface plasma resonance performance that flake nano silver powder is special shows and spheroidal particle and the distinct optical property of body phase material it.Therefore, flake nano silver powder has great using value in fields such as microelectronics, catalysis, surface-enhanced Raman, metal-enhanced fluorescence, infrared therapeutic, biomarker, nano conductive adhesive, electronic package materials.
The preparation method of flake nano silver powder mainly contains reduction ball-milling method, solution reduction, photo-induction inducing defecation by enema and suppository, thermal transition method, crystal seed method, template, solvent-thermal method, microwave irradiation and ultrasonic auxiliary law etc.Wherein solution reduction be at present commonly used also be one of the preparation method of tool potentiality.
Chinese patent literature CN1935422A discloses a kind of preparation method of single dispersion triangular nano silver slice, and the method is that the silver nitrate alcoholic solution is mixed in the ternary solution system that is comprised of water, PVP and n-amyl alcohol, obtains triangular nano silver slice through heat treatment.
Chinese patent literature 1958197A discloses a kind of preparation method of Nano silver piece, the method is first silver-colored source to be obtained the Nano silver grain seed with the sodium borohydride reaction in the presence of coating agent, and then with this seed and Yin Yuan, coating agent and weak reductant reaction preparation Nano silver piece, wherein weak reductant is hydrazine hydrate, ascorbic acid, HAS, HAN.
Chinese patent literature 101947655A discloses a kind of preparation method of triangular silver nanosheet, the method is that oxyacid silver is mixed with trisodium citrate and polyvinylpyrrolidone first, then add sodium borohydride and carry out reduction reaction, add again the hydrogen peroxide reaction, obtain triangular silver nanosheet.
Chinese patent literature CN102632246A discloses a kind of a large amount of method for preparing the series Nano silver piece, the method is that high molecular surfactant, halogen-containing slaine and cupric inorganic salts assistant are mixed to get solution A, in the mixed solvent of metal silver salt adding by polyalcohol and dimethyl formamide component, obtain solution B, solution A and solution B are mixed and heated to back flow reaction obtain Nano silver piece.
Above-mentioned various some course of reaction of method for preparing flake nano silver is loaded down with trivial details, and is higher for equipment requirement; Some operation is complicated, and reaction condition is higher, and the reaction time is longer; Some also uses the reagent of contaminated environment; Most importantly the flake nano aluminium powder that obtains of these methods is easy to reunite and grow up, and pattern is not single.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, provide a kind of product purity height and pattern is single, Processes and apparatus is simple, reaction condition is gentle and the time the is short method for preparing flake nano silver powder.
The technical scheme that realizes the object of the invention is: a kind of preparation method of flake nano silver powder, reacted under 0～100 ℃ temperature by the silver salt solution that contains surfactant and ferrous salt solution and to obtain.
Described silver salt is silver nitrate, silver sulfate or silver acetate.
Described surfactant is polyvinylpyrrolidone (PVP), softex kw (CTAB), lauryl sodium sulfate (SDS) or polyethylene glycol (PEG).
Described ferrous salt is iron ammonium sulfate (also can be described as six ferrous sulfate hydrate ammoniums) or ferrous sulfate (also can be described as green vitriol).
Preferred 40 ℃～80 ℃ of above-mentioned reaction temperature.
The weight ratio of described silver salt and described ferrous salt is 2: 1～1: 4, preferred 1: 1～1: 2.
The weight ratio of described silver salt and described surfactant is 50: 1～1: 2, preferred 10: 1～5: 1.
The good effect that the present invention has: (1) method of the present invention does not adopt the reducing agent of the common reduction silver salt such as sodium borohydride, hydrazine hydrate, but adopts ferrous salt reduction soluble silver salt, and the flake nano silver powder pattern that finally obtains is single, and purity is high.(2) method reaction time weak point of the present invention, efficient is high, and reaction condition is gentle.(3) method Processes and apparatus of the present invention is simple, and production cost is low, and easy and simple to handle, and green non-pollution is particularly suitable for large-scale industrialization production.
Description of drawings
Fig. 1 is SEM (SEM) figure of the flake nano silver powder that makes of embodiment 1.
The specific embodiment
(embodiment 1)
The preparation method of the flake nano silver powder of present embodiment is as follows:
1. the silver nitrate of 0.20g and the PVP-K30 of 0.04g are joined in the distilled water of 15mL, abundant stirring and dissolving obtains containing the liquor argenti nitratis ophthalmicus of PVP-K30.
2. six ferrous sulfate hydrate ammoniums with 0.40g join in the distilled water of 15mL, and fully stirring and dissolving obtains l ferrous ammonium sulfate solution.
3. the l ferrous ammonium sulfate solution that 2. step is obtained slowly is added drop-wise in the liquor argenti nitratis ophthalmicus that contains PVP-K30 that 1. step obtain, and is warming up to 60 ℃, insulation reaction 30min.
4. after reaction finishes, leave standstill 1h, then product is carried out centrifugation, with absolute ethyl alcohol and distilled water solid product is washed three times successively, place at last vacuum drying chamber vacuum drying under 80 ℃ temperature, namely get flake nano silver powder.
The SEM figure of the flake nano silver powder that present embodiment makes sees Fig. 1, and as seen from Figure 1, it is high that present embodiment makes flake nano silver powder purity, and pattern is single.
(embodiment 2～embodiment 5)
The preparation method of each embodiment is substantially the same manner as Example 1, and difference sees Table 1.
Table 1
| ? | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Silver salt | Silver nitrate | Silver nitrate | Silver nitrate | Silver sulfate | Silver acetate |
| Surfactant | PVP-K30 | PEG-10000 | SDS | PVP-K30 | CTAB |
| Ferrous salt | Six ferrous sulfate hydrate ammoniums | Green vitriol | Six ferrous sulfate hydrate ammoniums | Green vitriol | Six ferrous sulfate hydrate ammoniums |
(embodiment 6～embodiment 9)
The preparation method of each embodiment is substantially the same manner as Example 1, and difference sees Table 2.
Table 2
| ? | Embodiment 1 | Embodiment 6 | Embodiment 7 | Embodiment 8 | Embodiment 9 | Embodiment 10 | Embodiment 11 |
| Silver nitrate | 0.20g | 0.20g | 0.20g | 0.20g | 2.00g | 2.00g | 2.00g |
| PVP-K30 | 0.04g | 0.01g | 0.02g | 0.40g | 0.10g | 0.04g | 0.40g |
| Six ferrous sulfate hydrate ammoniums | 0.40g | 0.80g | 0.20g | 0.10g | 2.00g | 4.00g | 7.00g |
| Reaction temperature | 60℃ | 40℃ | 20℃ | 50℃ | 80℃ | 0℃ | 60℃ |
| Reaction time | 30min | 28min | 35min | 30min | 32min | 25min | 30min |
Claims (9)
1. the preparation method of a flake nano silver powder is characterized in that: reacted under 0～100 ℃ temperature by the silver salt solution that contains surfactant and ferrous salt solution and obtain.
2. the preparation method of flake nano silver powder according to claim 1, it is characterized in that: described silver salt is silver nitrate, silver sulfate or silver acetate.
3. the preparation method of flake nano silver powder according to claim 1, it is characterized in that: described surfactant is polyvinylpyrrolidone, softex kw, lauryl sodium sulfate or polyethylene glycol.
4. the preparation method of flake nano silver powder according to claim 1, it is characterized in that: described ferrous salt is iron ammonium sulfate or ferrous sulfate.
5. the preparation method of flake nano silver powder according to claim 1, it is characterized in that: reaction temperature is 40 ℃～80 ℃.
6. according to claim 1 to the preparation method of one of 5 described flake nano silver powder, it is characterized in that: the weight ratio of described silver salt and described ferrous salt is 2: 1～1: 4.
7. the preparation method of flake nano silver powder according to claim 6, it is characterized in that: the weight ratio of described silver salt and described ferrous salt is 1: 1～1: 2.
8. according to claim 1 to the preparation method of one of 5 described flake nano silver powder, it is characterized in that: the weight ratio of described silver salt and described surfactant is 50: 1～1: 2.
9. the preparation method of flake nano silver powder according to claim 8, it is characterized in that: the weight ratio of described silver salt and described surfactant is 10: 1～5: 1.
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| CN105050755A (en) * | 2013-06-25 | 2015-11-11 | 化研科技株式会社 | Flake-like silver powder, conductive paste, and method for producing flake-like silver powder |
| CN105050755B (en) * | 2013-06-25 | 2017-03-15 | 化研科技株式会社 | The manufacture method of laminar argentum powder, conductive paste and laminar argentum powder |
| CN103521777A (en) * | 2013-10-11 | 2014-01-22 | 南京邮电大学 | Method for preparing two-dimensional silver nanosheets of different shapes |
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| CN112355321A (en) * | 2020-10-09 | 2021-02-12 | 肇庆市华师大光电产业研究院 | Preparation method of kelp-like silver structure |
| CN112475310A (en) * | 2020-10-16 | 2021-03-12 | 湖南诺尔得材料科技有限公司 | Preparation method of silver powder with narrow particle size distribution |
| CN112475310B (en) * | 2020-10-16 | 2022-12-20 | 湖南中伟新银材料科技有限公司 | Preparation method of silver powder with narrow particle size distribution |
| CN114042929A (en) * | 2021-10-26 | 2022-02-15 | 西安交通大学 | High-concentration silver nano-micron sheet and synthesis method thereof |
| CN115488347A (en) * | 2022-09-09 | 2022-12-20 | 淮阴师范学院 | Preparation method of multilayer silver nanosheet |
| CN115488347B (en) * | 2022-09-09 | 2024-01-26 | 淮阴师范学院 | Preparation method of multilayer silver nano-sheet |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105290420B (en) | 2017-11-21 |
| CN102974837B (en) | 2016-01-06 |
| CN105268993B (en) | 2019-01-25 |
| CN105268993A (en) | 2016-01-27 |
| CN105290420A (en) | 2016-02-03 |
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