CN102974837B - The preparation method of flaky nanometer silver powder - Google Patents
The preparation method of flaky nanometer silver powder Download PDFInfo
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- CN102974837B CN102974837B CN201210500911.1A CN201210500911A CN102974837B CN 102974837 B CN102974837 B CN 102974837B CN 201210500911 A CN201210500911 A CN 201210500911A CN 102974837 B CN102974837 B CN 102974837B
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 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
- 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
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 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
- 239000012266 salt solution Substances 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
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims abstract description 3
- 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 abstract description 3
- 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
- 238000000034 method Methods 0.000 abstract description 21
- 230000035484 reaction time Effects 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 10
- 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
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 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
- IMBKASBLAKCLEM-UHFFFAOYSA-L ferrous ammonium sulfate (anhydrous) Chemical compound [NH4+].[NH4+].[Fe+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O IMBKASBLAKCLEM-UHFFFAOYSA-L 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
- 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
- 239000002671 adjuvant Substances 0.000 description 1
- 230000001476 alcoholic effect Effects 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
- 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
- 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
- 239000000843 powder Substances 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
- 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
Abstract
The invention discloses a kind of preparation method of flaky nanometer silver powder, it is obtained by reacting at the temperature of 0 ~ 100 DEG C by the silver salt solution and ferrous salt solution containing surfactant.Described silver salt is silver nitrate, silver sulfate or silver acetate.Described surfactant is polyvinylpyrrolidone, softex kw, lauryl sodium sulfate or polyethylene glycol.Described ferrous salt is iron ammonium sulfate or ferrous sulfate.The weight ratio of described silver salt and described ferrous salt is 2: 1 ~ 1: 4.The weight ratio of described silver salt and described surfactant is 50: 1 ~ 1: 2.The flaky nanometer silver powder pattern that method of the present invention finally obtains is single, and purity is high.The advantages such as method of the present invention also has that the reaction time is short, efficiency is high, reaction condition is gentle, Processes and apparatus is simple, production cost is low, easy and simple to handle, green non-pollution, are particularly suitable for industrialization large-scale 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 flaky nanometer silver powder.
Background technology
Flaky nanometer silver powder due to its surface area relatively large, between particle be face contact or linear contact lay, so resistance is relatively low, electric conductivity is better.In addition, the surface plasma resonance performance that flaky nanometer silver powder is special, makes it show and spheroidal particle and the distinct optical property of body phase material.Therefore, flaky nanometer 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 flaky nanometer silver powder mainly contains reduction ball-milling method, solution reduction, light inducible, thermal transition method, crystal seed method, template, solvent-thermal method, microwave irradiation and ultrasonic wave added method etc.Wherein solution reduction is the most conventional at present is also one of preparation method of most potentiality.
Chinese patent literature CN1935422A discloses a kind of preparation method of single dispersion triangular nano silver slice, and the method is mixed in the ternary solution system be made up of water, PVP and n-amyl alcohol by silver nitrate alcoholic solution, obtains triangular nano silver slice through heat treatment.
Chinese patent literature 1958197A discloses a kind of preparation method of Nano silver piece, the method first silver-colored source is obtained by reacting Nano silver grain seed with sodium borohydride under the existence of coating agent, and then this seed and Yin Yuan, coating agent and weak reductant reacted prepare 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 first mixed with trisodium citrate and polyvinylpyrrolidone by oxyacid silver, then add sodium borohydride and carry out reduction reaction, then add hydrogen peroxide reaction, obtain triangular silver nanosheet.
Chinese patent literature CN102632246A discloses a kind of a large amount of method preparing series Nano silver piece, the method is that high molecular surfactant, halogen-containing slaine and cupric inorganic salts adjuvant are mixed to get solution A, metal silver salt is added in the mixed solvent by polyalcohol and dimethyl formamide component, obtain solution B, solution A and solution B are mixed and heated to back flow reaction and obtain Nano silver piece.
Above-mentioned various some course of reaction of method preparing flake nano silver is loaded down with trivial details, 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 silver powder that these methods obtain 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 high and pattern is single, Processes and apparatus is simple, reaction condition is gentle and the method preparing flaky nanometer silver powder that the time is short.
The technical scheme realizing the object of the invention is: a kind of preparation method of flaky nanometer silver powder, is obtained by reacting at the temperature of 0 ~ 100 DEG C by the silver salt solution and ferrous salt solution containing surfactant.
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).
Above-mentioned reaction temperature preferably 40 DEG C ~ 80 DEG C.
The weight ratio of described silver salt and described ferrous salt is 2: 1 ~ 1: 4, preferably 1: 1 ~ 1: 2.
The weight ratio of described silver salt and described surfactant is 50: 1 ~ 1: 2, preferably 10: 1 ~ 5: 1.
The good effect that the present invention has: the reducing agent of the reduction silver salt that (1) method of the present invention does not adopt sodium borohydride, hydrazine hydrate etc. common, but adopt ferrous salt reduction soluble silver salt, the flaky nanometer silver powder pattern finally obtained is single, and purity is high.(2) the method reaction time of the present invention is short, and efficiency 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, green non-pollution, is particularly suitable for industrialization large-scale production.
Accompanying drawing explanation
Fig. 1 is SEM (SEM) figure of the flaky nanometer silver powder that embodiment 1 obtains.
Detailed description of the invention
(embodiment 1)
The preparation method of the flaky nanometer silver powder of the 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, obtain the liquor argenti nitratis ophthalmicus containing PVP-K30.
2. join in the distilled water of 15mL by the six ferrous sulfate hydrate ammoniums of 0.40g, abundant stirring and dissolving, obtains l ferrous ammonium sulfate solution.
3. the l ferrous ammonium sulfate solution 2. step obtained slowly be added drop-wise to that 1. step obtain containing in the liquor argenti nitratis ophthalmicus of PVP-K30, be warming up to 60 DEG C, insulation reaction 30min.
4., after reaction terminates, leave standstill 1h, then centrifugation is carried out to product, with absolute ethyl alcohol and distilled water, three times are washed to solid product successively, be finally placed in vacuum drying chamber vacuum drying at the temperature of 80 DEG C, obtain flaky nanometer silver powder.
The SEM figure of the flaky nanometer silver powder that the present embodiment obtains is shown in Fig. 1, and as seen from Figure 1, it is high that the present embodiment obtains flaky nanometer 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 is in 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 is in 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 (8)
1. a preparation method for flaky nanometer silver powder, is characterized in that: be obtained by reacting at the temperature of 0 ~ 100 DEG C by the silver salt solution and ferrous salt solution that contain surfactant; The weight ratio of described silver salt and described surfactant is 50: 1 ~ 1: 2.
2. the preparation method of flaky nanometer silver powder according to claim 1, is characterized in that: described silver salt is silver nitrate, silver sulfate or silver acetate.
3. the preparation method of flaky nanometer silver powder according to claim 1, is characterized in that: described surfactant is polyvinylpyrrolidone, softex kw, lauryl sodium sulfate or polyethylene glycol.
4. the preparation method of flaky nanometer silver powder according to claim 1, is characterized in that: described ferrous salt is iron ammonium sulfate or ferrous sulfate.
5. the preparation method of flaky nanometer silver powder according to claim 1, is characterized in that: reaction temperature is 40 DEG C ~ 80 DEG C.
6. according to the preparation method of the flaky nanometer silver powder one of claim 1 to 5 Suo Shu, 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 flaky nanometer silver powder according to claim 6, is characterized in that: the weight ratio of described silver salt and described ferrous salt is 1: 1 ~ 1: 2.
8. the preparation method of flaky nanometer silver powder according to claim 1, is characterized in that: the weight ratio of described silver salt and described surfactant is 10: 1 ~ 5: 1.
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| CN201510819711.6A CN105290420B (en) | 2012-11-29 | 2012-11-29 | The method for preparing flaky nanometer silver powder |
| CN201210500911.1A CN102974837B (en) | 2012-11-29 | 2012-11-29 | The preparation method of flaky nanometer silver powder |
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| US10071420B2 (en) * | 2013-06-25 | 2018-09-11 | Kaken Tech Co., Ltd. | Flake-like silver powder, conductive paste, and method for producing flake-like silver 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 |
| KR101618093B1 (en) * | 2014-03-17 | 2016-05-09 | 주식회사 상보 | A Conductive Paste Composition for Forming Conductive Thin Film on a Flexible Substrate and a method for producing the same |
| CN104551007A (en) * | 2015-01-13 | 2015-04-29 | 山东大学 | Large-scale preparation method of silver nano-sheets |
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| 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 |
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Also Published As
| Publication number | Publication date |
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| CN105268993A (en) | 2016-01-27 |
| CN102974837A (en) | 2013-03-20 |
| CN105268993B (en) | 2019-01-25 |
| CN105290420B (en) | 2017-11-21 |
| CN105290420A (en) | 2016-02-03 |
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