CN114515836A - Method for synthesizing aqueous-phase low-temperature nano silver wire - Google Patents
Method for synthesizing aqueous-phase low-temperature nano silver wire Download PDFInfo
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 34
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 17
- 239000008346 aqueous phase Substances 0.000 title claims abstract description 15
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 30
- 238000003756 stirring Methods 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000000243 solution Substances 0.000 claims abstract description 21
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229930003268 Vitamin C Natural products 0.000 claims abstract description 15
- 235000019154 vitamin C Nutrition 0.000 claims abstract description 15
- 239000011718 vitamin C Substances 0.000 claims abstract description 15
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 14
- 239000008103 glucose Substances 0.000 claims abstract description 14
- 239000002243 precursor Substances 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 12
- PBIDWHVVZCGMAR-UHFFFAOYSA-N 1-methyl-3-prop-2-enyl-2h-imidazole Chemical compound CN1CN(CC=C)C=C1 PBIDWHVVZCGMAR-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 9
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 239000012071 phase Substances 0.000 claims abstract description 5
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims abstract description 4
- 239000002042 Silver nanowire Substances 0.000 claims description 11
- 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 description 8
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- 238000001308 synthesis method Methods 0.000 claims description 2
- 239000003638 chemical reducing agent Substances 0.000 abstract description 5
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 230000006911 nucleation Effects 0.000 abstract description 3
- 238000010899 nucleation Methods 0.000 abstract description 3
- 239000004094 surface-active agent Substances 0.000 abstract description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000002070 nanowire Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
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- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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Abstract
The invention relates to the technical field of nano silver wires, in particular to a method for synthesizing a nano silver wire at a low water phase temperature. The method comprises the following steps: (1) preparing a silver nitrate precursor solution by taking deionized water as a solvent; (2) adding sodium bicarbonate, glucose and 1-allyl-3-methylimidazole into the precursor solution, and uniformly stirring; (3) slowly adding vitamin C, and stirring to obtain mixed solution; (4) placing the mixed solution in a constant-temperature water bath at 0-90 ℃, and slowly stirring for reaction; (5) and respectively washing the obtained product with deionized water and ethanol, and drying to obtain the nano silver wire. According to the method, the vitamin C is used as a reducing agent, the glucose is used as a surfactant, the 1-allyl-3-methylimidazole is used as a nucleation control agent, the silver nitrate precursor is reduced in an aqueous phase environment, and the nano silver wire can be obtained at the reaction temperature of 0-90 ℃.
Description
Technical Field
The invention relates to the technical field of nano silver wires, in particular to a method for synthesizing a nano silver wire at a low water phase temperature.
Background
In recent years, low-dimensional nanomaterials, especially one-dimensional nanomaterials, such as nanowires, nanofibers, nanorods, etc., are widely used in the fields of energy, catalysis, biology, electronics, etc., due to their unique mechanical, electrical, thermal, optical, etc. properties. The nano silver wire is one of nano materials, and has excellent electrical, optical, antibacterial and catalytic functions, so that the nano silver wire is widely accepted in the fields of electronic industry, antibacterial materials, organic catalysis, energy conservation, environmental protection and the like.
There are two main categories of current methods for preparing silver nanowires. One is a template method, such as porous anodic aluminum oxide, carbon nanotubes and the like, and the method has the advantages that the shape and the size of the nanowire can be strictly controlled, but the method has high cost and limited yield and is difficult to adapt to industrial large-scale production. The other method adopts a lot of non-template methods, which is typically represented by a wet chemical reduction method using polyhydric alcohol as a solvent, but the methods generally need more than 120 ℃, the cost of the solvent is high, polyvinylpyrrolidone is mostly used, and the subsequent cleaning and purification steps are many and the cost is high.
At present, a method for aqueous synthesis of a silver nanowire generally requires high temperature and high pressure, and as reported in Journal of Materials Chemistry a (Journal of Materials Chemistry a.2016, page 4, 11366), a method for hydrothermal synthesis of a silver nanowire with glucose as a reducing agent specifically comprises the following steps: respectively preparing silver nitrate, sodium chloride, glucose and polyvinylpyrrolidone (PVP) into water solutions, then adding the glucose solution into the silver nitrate solution and uniformly stirring, adding the PVP solution after 5-10 minutes, stirring for 20 minutes, finally dropwise adding the sodium chloride solution, then transferring the solution into a 50mL reaction kettle, heating at 160 ℃ for 22 hours, taking out the solution, and cooling to room temperature to obtain the silver nanowire. However, the method has the advantages of small amount of synthesized silver nanowires and high reaction temperature.
Disclosure of Invention
Aiming at the technical problems, the invention provides a method for synthesizing a nano silver wire, which is used for preparing the nano silver wire in a water-phase low-temperature environment, is simple to operate and is environment-friendly.
The invention adopts the following technical scheme:
a method for synthesizing a nano silver wire at a low aqueous phase temperature comprises the following steps:
(1) preparing a silver nitrate precursor solution by taking deionized water as a solvent;
(2) adding sodium bicarbonate, glucose and 1-allyl-3-methylimidazole into the precursor solution, and uniformly stirring;
(3) slowly adding vitamin C, and stirring to obtain mixed solution;
(4) placing the mixed solution in a constant-temperature water bath at 0-90 ℃, and stirring for reaction;
(5) and respectively washing the obtained product with deionized water and ethanol, and drying to obtain the nano silver wire.
Furthermore, the mass ratio of the silver salt to the vitamin C is 1 (1-10).
Furthermore, the mass ratio of the silver salt to the glucose is 1 (1-10).
Furthermore, the mass ratio of the silver salt to the 1-allyl-3-methylimidazole is 1 (0.02-0.067).
Furthermore, the mass ratio of the silver salt to the sodium bicarbonate is 1 (0.3-1).
Further, the stirring speed in the step (4) is 1-100 rpm, preferably 5-50 rpm.
Further, the reaction time in the step (4) is 10-60 hours.
On the other hand, the invention also provides the nano silver wire prepared by the synthesis method, wherein the diameter of the nano silver wire is 15-100 nm, and the length of the nano silver wire is 10-200 mu m.
The method for synthesizing the aqueous-phase low-temperature nano silver wire takes vitamin C as a reducing agent, glucose as a surfactant and 1-allyl-3-methylimidazole as a nucleation control agent, reduces a silver nitrate precursor in an aqueous-phase environment, and can obtain the nano silver wire at a reaction temperature of 0-90 ℃.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a scanning electron microscope image of a silver nanowire prepared in example 1 of the present invention;
FIG. 2 is a scanning electron microscope image of the silver nanowires prepared in example 2 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A method for synthesizing a nano silver wire at a low aqueous phase temperature comprises the following steps:
(1) using deionized water as a solvent, preparing 500mL of silver nitrate precursor solution with the concentration of 20mmol/L, and uniformly stirring;
(2) adding 1.5 g of sodium bicarbonate, 5 g of glucose and 0.1 g of 1-allyl-3-methylimidazole into the precursor solution, and uniformly stirring;
(3) slowly adding 50mL of vitamin C with the concentration of 0.5mol/L, and stirring for 10 minutes to uniformly mix the vitamin C and the vitamin C to obtain a mixed solution;
(4) placing the mixed solution in a constant-temperature water bath at 60 ℃, and stirring and reacting for 15h at the stirring speed of 50 rpm;
(5) and (3) washing the obtained product with deionized water and ethanol for one time respectively, and drying to obtain the nano silver wire, wherein a scanning electron microscope image of the nano silver wire is shown in figure 1.
The diameter of the nano silver wire prepared by the embodiment is 18-28 nm, and the length of the nano silver wire is 20-35 mu m.
Example 2
A method for synthesizing a nano silver wire at a low aqueous phase temperature comprises the following steps:
(1) preparing 1000mL of silver nitrate precursor solution with the concentration of 50mmol/L by taking deionized water as a solvent, and uniformly stirring;
(2) adding 3 g of sodium bicarbonate, 90 g of glucose and 0.2 g of 1-allyl-3-methylimidazole into the precursor solution, and uniformly stirring;
(3) slowly adding 100mL of vitamin C with the concentration of 1mol/L, and stirring for 10 minutes to uniformly mix the vitamin C and the vitamin C to obtain a mixed solution;
(4) placing the mixed solution in a constant-temperature water bath at 0 ℃, and stirring and reacting for 60 hours at a stirring speed of 80 rpm;
(5) and washing the obtained product with deionized water and ethanol for one time respectively, and drying to obtain the nano silver wire, wherein a scanning electron microscope image of the nano silver wire is shown in figure 2.
The diameter of the nano silver wire prepared by the embodiment is 25-35 nm, and the length is 35-60 mu m.
Example 3
A method for synthesizing a nano silver wire at a low aqueous phase temperature comprises the following steps:
(1) preparing 800mL of silver nitrate precursor solution with the concentration of 40mmol/L by taking deionized water as a solvent, and uniformly stirring;
(2) adding 2 g of sodium bicarbonate, 50 g of glucose and 0.15 g of 1-allyl-3-methylimidazole into the precursor solution, and uniformly stirring;
(3) slowly adding 50mL of vitamin C with the concentration of 1mol/L, and stirring for 10 minutes to uniformly mix the mixture to obtain a mixed solution;
(4) placing the mixed solution in a constant-temperature water bath at 90 ℃, and stirring and reacting for 10 hours at the stirring speed of 5 rpm;
(5) and washing the obtained product with deionized water and ethanol for one time respectively, and drying to obtain the nano silver wire.
The diameter of the nano silver wire prepared by the embodiment is 40-60 nm, and the length of the nano silver wire is 10-25 mu m.
The invention realizes the preparation of silver nanowires by reducing silver nitrate in a low-temperature water phase environment by taking vitamin C as a reducing agent, glucose as a surfactant and 1-allyl-3-methylimidazole as a nucleation control agent. Compared with the conventional alcohol heating method for preparing the silver nanowires at the reaction temperature of more than 100 ℃, the method has the advantages that the reaction temperature is reduced, the use of polyvinylpyrrolidone (PVP) is avoided, the subsequent cleaning and purifying process is greatly simplified, the cost is reduced, and the efficiency is improved; and compared with ethylene glycol used in the conventional synthesis process, the pure water solvent has lower cost and is more environment-friendly.
The present invention has been further described with reference to specific embodiments, but it should be understood that the detailed description should not be construed as limiting the spirit and scope of the present invention, and various modifications made to the above-described embodiments by those of ordinary skill in the art after reading this specification are within the scope of the present invention.
Claims (8)
1. A method for synthesizing a nano silver wire with a low aqueous phase temperature is characterized by comprising the following steps:
(1) preparing a silver nitrate precursor solution by taking deionized water as a solvent;
(2) adding sodium bicarbonate, glucose and 1-allyl-3-methylimidazole into the precursor solution, and uniformly stirring;
(3) slowly adding vitamin C, and stirring to obtain mixed solution;
(4) placing the mixed solution in a constant-temperature water bath at 0-90 ℃, and stirring for reaction;
(5) and respectively washing the obtained product with deionized water and ethanol, and drying to obtain the nano silver wire.
2. The method for synthesizing the nano silver wire at the low temperature in the aqueous phase according to claim 1, wherein the mass ratio of the silver salt to the vitamin C is 1 (1-10).
3. The method for synthesizing the nano silver wire at the low temperature in the aqueous phase according to claim 1, wherein the mass ratio of the silver salt to the glucose is 1 (1-10).
4. The method for synthesizing the nano silver wire at the low temperature in the water phase according to claim 1, wherein the mass ratio of the silver salt to the 1-allyl-3-methylimidazole is 1 (0.02-0.067).
5. The method for synthesizing the nano silver wire at the low temperature in the aqueous phase according to claim 1, wherein the mass ratio of the silver salt to the sodium bicarbonate is 1 (0.3-1).
6. The method for synthesizing the nano silver wire with the low aqueous phase temperature according to claim 1, wherein the stirring speed in the step (4) is 1-100 rpm.
7. The method for synthesizing the nano silver wire at the low temperature of the aqueous phase according to claim 1, wherein the reaction time in the step (4) is 10 to 60 hours.
8. The silver nanowire obtained by the synthesis method according to any one of claims 1-7, wherein the silver nanowire has a diameter of 15-100 nm and a length of 10-200 μm.
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Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2012180589A (en) * | 2011-02-07 | 2012-09-20 | Sumitomo Chemical Co Ltd | Method for manufacturing metal nanowire |
CN104209538A (en) * | 2014-09-02 | 2014-12-17 | 北京化工大学 | Method for preparing silver nanowires in aqueous medium |
CN104690294A (en) * | 2015-03-27 | 2015-06-10 | 严锋 | High-length-diameter-ratio silver nanowire preparation method and silver nanowire prepared by same |
CN104854020A (en) * | 2012-12-14 | 2015-08-19 | 茵斯康科技株式会社 | Method for manufacturing silver nanowires using copolymer capping agents |
CN104870361A (en) * | 2012-12-14 | 2015-08-26 | 率路技术株式会社 | Method for manufacturing silver nanowires using ionic liquid |
CN110465653A (en) * | 2019-09-19 | 2019-11-19 | 安徽工业大学 | A kind of silver wire and preparation method thereof |
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2020
- 2020-11-02 CN CN202011204338.0A patent/CN114515836B/en active Active
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2012180589A (en) * | 2011-02-07 | 2012-09-20 | Sumitomo Chemical Co Ltd | Method for manufacturing metal nanowire |
CN104854020A (en) * | 2012-12-14 | 2015-08-19 | 茵斯康科技株式会社 | Method for manufacturing silver nanowires using copolymer capping agents |
CN104870361A (en) * | 2012-12-14 | 2015-08-26 | 率路技术株式会社 | Method for manufacturing silver nanowires using ionic liquid |
CN104209538A (en) * | 2014-09-02 | 2014-12-17 | 北京化工大学 | Method for preparing silver nanowires in aqueous medium |
CN104690294A (en) * | 2015-03-27 | 2015-06-10 | 严锋 | High-length-diameter-ratio silver nanowire preparation method and silver nanowire prepared by same |
CN110465653A (en) * | 2019-09-19 | 2019-11-19 | 安徽工业大学 | A kind of silver wire and preparation method thereof |
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