CN105290420B - The method for preparing flaky nanometer silver powder - Google Patents
The method for preparing flaky nanometer silver powder Download PDFInfo
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- CN105290420B CN105290420B CN201510819711.6A CN201510819711A CN105290420B CN 105290420 B CN105290420 B CN 105290420B CN 201510819711 A CN201510819711 A CN 201510819711A CN 105290420 B CN105290420 B CN 105290420B
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- silver
- salt
- ferrous
- flaky nanometer
- silver powder
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 24
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical group [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 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 14
- 239000004094 surface-active agent Substances 0.000 claims abstract description 11
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 10
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 8
- 229920000036 polyvinylpyrrolidone Polymers 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
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 238000009938 salting Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 14
- 238000006243 chemical reaction Methods 0.000 abstract description 12
- 229910000359 iron(II) sulfate Inorganic materials 0.000 abstract description 5
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 abstract description 4
- 230000035484 reaction time Effects 0.000 abstract description 4
- 229920001223 polyethylene glycol Polymers 0.000 abstract description 3
- 239000002202 Polyethylene glycol Substances 0.000 abstract description 2
- 239000011790 ferrous sulphate Substances 0.000 abstract description 2
- 235000003891 ferrous sulphate Nutrition 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 abstract description 2
- 229940071536 silver acetate Drugs 0.000 abstract description 2
- YPNVIBVEFVRZPJ-UHFFFAOYSA-L silver sulfate Chemical compound [Ag+].[Ag+].[O-]S([O-])(=O)=O YPNVIBVEFVRZPJ-UHFFFAOYSA-L 0.000 abstract description 2
- 229910000367 silver sulfate Inorganic materials 0.000 abstract description 2
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 abstract 1
- ZLXPLDLEBORRPT-UHFFFAOYSA-M [NH4+].[Fe+].[O-]S([O-])(=O)=O Chemical group [NH4+].[Fe+].[O-]S([O-])(=O)=O ZLXPLDLEBORRPT-UHFFFAOYSA-M 0.000 abstract 1
- 229940010514 ammonium ferrous sulfate Drugs 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 11
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 8
- 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
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 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
- -1 Sodium alkyl sulfate Chemical class 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 239000012153 distilled water 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
- 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
- 239000000843 powder Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 239000002253 acid Substances 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
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 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
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- UMEAURNTRYCPNR-UHFFFAOYSA-N azane;iron(2+) Chemical group N.[Fe+2] UMEAURNTRYCPNR-UHFFFAOYSA-N 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
- 235000013339 cereals Nutrition 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent 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
- 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 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 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
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000012798 spherical particle 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
- 238000001291 vacuum drying Methods 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, and it is reacted by the silver salt solution containing surfactant with ferrous salt solution at a temperature of 0~100 DEG C obtains.Described silver salt is silver nitrate, silver sulfate or silver acetate.Described surfactant is polyvinylpyrrolidone, cetyl trimethylammonium bromide, 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 the method for the present invention finally gives is single, and purity is high.The method of the present invention also has the advantages that short reaction time, efficiency high, reaction condition is gentle, Processes and apparatus is simple, production cost is low, easy to operate, green non-pollution, is particularly suitable for industrialization large-scale production.
Description
The application is Application No. 201210500911.1, and the applying date is on November 29th, 2012, and invention and created name is
The divisional application of the application for a patent for invention of " preparation method of flaky nanometer silver powder ".
Technical field
The present invention relates to a kind of preparation method of metal dust, and in particular to a kind of preparation method of flaky nanometer silver powder.
Background technology
Flaky nanometer silver powder is face contact or linear contact lay between particle, so resistance phase because its surface area is relatively large
To relatively low, electric conductivity is preferable.In addition, the surface plasma resonance performance that flaky nanometer silver powder is special, make its show with it is spherical
Particle and the completely different optical property of body phase material.Therefore, flaky nanometer silver powder microelectronics, catalysis, surface-enhanced Raman,
The fields such as metal-enhanced fluorescence, infrared therapeutic, biomarker, nano conductive adhesive, electronic package material, which have, greatly applies valency
Value.
The preparation method of flaky nanometer silver powder mainly have 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 presently the most normal
With being also one of most potential preparation method.
Chinese patent literature CN1935422A discloses a kind of preparation method of single dispersion triangular nano silver slice, and this method is
Silver nitrate alcoholic solution is mixed in the ternary solution system being made up of water, PVP and n-amyl alcohol, the thermally treated triangle that obtains is received
Rice silver strip.
Chinese patent literature 1958197A discloses a kind of preparation method of Nano silver piece, and this method is first to wrap silver-colored source
Wrap up in and react to obtain Nano silver grain seed with sodium borohydride in the presence of agent, then again by the seed and Yin Yuan, coating agent and
Weak reductant reaction prepares Nano silver piece, and wherein weak reductant is hydrazine hydrate, ascorbic acid, HAS, HAN.
Chinese patent literature 101947655A discloses a kind of preparation method of triangular silver nanosheet, this method be by containing
Oxygen acid silver first mixes with trisodium citrate and polyvinylpyrrolidone, then adds sodium borohydride and carries out reduction reaction, then adds
Enter hydrogen peroxide reaction, obtain triangular silver nanosheet.
Chinese patent literature CN102632246A discloses a kind of method for largely preparing serial Nano silver piece, and this method is
High molecular surfactant, halogen-containing metal salt and cupric inorganic salts adjuvant are mixed to get solution A, by metal silver salt
The in the mixed solvent by polyalcohol and dimethylformamide component is added, solution B is obtained, solution A and solution B is mixed and heated to
Back flow reaction obtains Nano silver piece.
Above-mentioned various some courses of reaction of the method for preparing flake nano silver are cumbersome, higher for equipment requirement；Some are anti-
Complex operation is answered, reaction condition is higher, and the reaction time is longer；Some are also using the reagent of pollution environment；Most importantly these
The flake nano silver powder that method obtains is easy to reunite and grown up, and pattern is not single.
The content of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide, a kind of product purity is high and pattern is single, technique
And the method for the preparation flaky nanometer silver powder that equipment is simple, reaction condition is gentle and the time is short.
Realizing the technical scheme of the object of the invention is：A kind of preparation method of flaky nanometer silver powder, by containing surfactant
Silver salt solution react and obtain at a temperature of 0~100 DEG C with ferrous salt solution.
Described silver salt is silver nitrate, silver sulfate or silver acetate.
Described surfactant is polyvinylpyrrolidone（PVP）, cetyl trimethylammonium bromide（CTAB）, 12
Sodium alkyl sulfate（SDS）Or polyethylene glycol（PEG）.
Described ferrous salt is iron ammonium sulfate（Alternatively referred to as six ferrous sulfate hydrate ammoniums）Or ferrous sulfate（Also can claim
For green vitriol）.
Preferably 40 DEG C~80 DEG C of above-mentioned reaction temperature.
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：（1）The method of the present invention does not use the common reduction such as sodium borohydride, hydrazine hydrate
The reducing agent of silver salt, but ferrous salt reduction soluble silver salt is used, the flaky nanometer silver powder pattern finally given is single, purity
It is high.（2）The method reaction time of the present invention is short, efficiency high, and reaction condition is gentle.（3）The present invention method technique and set
Standby simple, production cost is low, and easy to operate, green non-pollution, is particularly suitable for industrialization large-scale production.
Brief description of the drawings
Fig. 1 is the SEM of flaky nanometer silver powder made from embodiment 1（SEM）Figure.
Embodiment
（Embodiment 1）
The preparation method of the flaky nanometer silver powder of the present embodiment is as follows：
1. the PVP-K30 of 0.20g silver nitrate and 0.04g is added in 15mL distilled water, dissolving is sufficiently stirred, is obtained
To the silver nitrate solution containing PVP-K30.
2. 0.40g six ferrous sulfate hydrate ammoniums are added in 15mL distilled water, dissolving is sufficiently stirred, obtains sulfuric acid
Ferrous ammonium salt solution.
3. 2. l ferrous ammonium sulfate solution that step is obtained is slowly dropped to the 1. silver nitrate containing PVP-K30 that step obtains
In solution, 60 DEG C are warming up to, insulation reaction 30min.
After 4. reaction terminates, 1h is stood, then product is centrifuged, successively with absolute ethyl alcohol and distilled water to solid
Body product washs three times, is finally placed in vacuum drying chamber and is dried in vacuo at a temperature of 80 DEG C, produces flaky nanometer silver powder.
The SEM figures of flaky nanometer silver powder made from the present embodiment are shown in Fig. 1, and as seen from Figure 1, sheet is made in the present embodiment
Nano-silver powder purity is high, and pattern is single.
（2~embodiment of embodiment 5）
The preparation method of each embodiment is substantially the same manner as Example 1, and difference is shown 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 |
（6~embodiment of embodiment 9）
The preparation method of each embodiment is substantially the same manner as Example 1, and difference is shown 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 (1)
- A kind of 1. method for preparing flaky nanometer silver powder, it is characterised in that：By the silver salt solution containing surfactant and ferrous iron Salting liquid reacts at a temperature of 0~100 DEG C to be obtained；The weight ratio of described silver salt and described surfactant for 10: 1~ 5∶1；Described silver salt is silver nitrate；Described surfactant is polyvinylpyrrolidone；Described ferrous salt is that sulfuric acid is sub- Iron ammonium.
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| 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 |
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|---|---|---|---|---|
| SU1488134A1 (en) * | 1987-11-17 | 1989-06-23 | Предприятие П/Я А-3481 | Method of producing silver powder |
| CN1958197A (en) * | 2006-11-16 | 2007-05-09 | 中国科学院长春应用化学研究所 | Method for preparing Nano silver piece |
| CN101823153A (en) * | 2009-03-06 | 2010-09-08 | 五邑大学 | Technology for preparing flake nano silver with overlarge area |
| CN101890504A (en) * | 2010-07-07 | 2010-11-24 | 江苏技术师范学院 | Method for preparing flaky nano copper powder |
| CN101947655A (en) * | 2010-10-25 | 2011-01-19 | 江苏技术师范学院 | Preparation method of triangular silver nanosheet |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102974837A (en) | 2013-03-20 |
| CN105268993B (en) | 2019-01-25 |
| CN105268993A (en) | 2016-01-27 |
| CN105290420A (en) | 2016-02-03 |
| CN102974837B (en) | 2016-01-06 |
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Address after: No. 1801 Zhong Wu Avenue, Changzhou, Jiangsu Province, Jiangsu Patentee after: JIANGSU University OF TECHNOLOGY Address before: 213001 1801 Zhong Wu Avenue, Zhong Lou District, Changzhou, Jiangsu Patentee before: Jiangsu University of Technology |
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Application publication date: 20160203 Assignee: LIYANG LIFANG PRECIOUS METALS MATERIAL Co.,Ltd. Assignor: JIANGSU University OF TECHNOLOGY Contract record no.: X2023980054514 Denomination of invention: Method for preparing sheet-like nano silver powder Granted publication date: 20171121 License type: Common License Record date: 20240102 |