CN114515836B - Synthesis method of water-phase low-temperature nano silver wire - Google Patents
Synthesis method of water-phase low-temperature nano silver wire Download PDFInfo
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- CN114515836B CN114515836B CN202011204338.0A CN202011204338A CN114515836B CN 114515836 B CN114515836 B CN 114515836B CN 202011204338 A CN202011204338 A CN 202011204338A CN 114515836 B CN114515836 B CN 114515836B
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 238000001308 synthesis method Methods 0.000 title description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 27
- 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 22
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 21
- 239000000243 solution Substances 0.000 claims abstract description 18
- 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
- 230000002194 synthesizing effect Effects 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
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229930003268 Vitamin C Natural products 0.000 claims abstract description 11
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 11
- 235000019154 vitamin C Nutrition 0.000 claims abstract description 11
- 239000011718 vitamin C Substances 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 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
- 238000005406 washing Methods 0.000 claims abstract description 4
- 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
- 230000008569 process Effects 0.000 claims description 7
- 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
- 239000003638 chemical reducing agent Substances 0.000 abstract description 5
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 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
- 239000012071 phase Substances 0.000 description 8
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 6
- 239000002042 Silver nanowire Substances 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000002070 nanowire Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 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
- 238000010438 heat treatment 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
- 239000006250 one-dimensional material Substances 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
Abstract
The invention relates to the technical field of nano silver wires, in particular to a method for synthesizing a water-phase low-temperature nano silver wire. The method comprises the following steps: (1) Preparing a silver nitrate precursor solution by taking deionized water as a solvent; (2) Sodium bicarbonate, glucose and 1-allyl-3-methylimidazole are added into the precursor solution and stirred uniformly; (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 (3) respectively washing the obtained product with deionized water and ethanol, and drying to obtain the nano silver wire. According to the method, vitamin C is used as a reducing agent, glucose is used as a surfactant, 1-allyl-3-methylimidazole is used as a nucleation control agent, a silver nitrate precursor is reduced in a water phase environment, and the nano silver wire can be obtained at a reaction temperature of 0-90 ℃, and the method is simple to operate, environment-friendly, low in production cost and suitable for large-scale popularization and application.
Description
Technical Field
The invention relates to the technical field of nano silver wires, in particular to a method for synthesizing a water-phase low-temperature nano silver wire.
Background
In recent years, low-dimensional nanomaterials, particularly one-dimensional materials such as nanowires, nanofibers, nanorods, and the like, have been widely used in the fields of energy, catalysis, biology, electronics, and the like due to their unique mechanical, electrical, thermal, optical, and the like properties. The nano silver wire is used as one of nano materials, and has been widely accepted in the fields of electronic industry, antibacterial materials, organic catalysis, energy conservation, environmental protection and the like due to the excellent electrical, optical, antibacterial and catalytic functions.
The current methods for preparing silver nanowires are mainly divided into two main types. The template method, such as porous anodic alumina, carbon nano tube, etc., has the advantages of being capable of realizing strict control of the shape and the size of the nano wire, but has high cost and limited yield, and is difficult to adapt to industrial mass production. The other class uses more non-template methods, which typically represent wet chemical reduction methods using polyols as solvents, but these methods generally require above 120 ℃ and the solvents are costly, and most use polyvinylpyrrolidone, which is costly in terms of subsequent washing and purification steps.
At present, high temperature and high pressure are generally required for a method for synthesizing nano silver wires in water, for example, journal of Material chemistry A (Journal of Materials Chemistry A.2016, volume 4, page 11366) reports a method for hydrothermally synthesizing silver wires by taking glucose as a reducing agent, which specifically comprises the following steps: preparing silver nitrate, sodium chloride, glucose and polyvinylpyrrolidone (PVP) into aqueous solutions respectively, adding the glucose solution into the silver nitrate solution, stirring uniformly, adding the PVP solution after 5-10 minutes, stirring for 20 minutes, adding the sodium chloride solution dropwise, transferring the solution into a 50mL reaction kettle, heating at 160 ℃ for 22 hours, taking out, and cooling to room temperature to obtain the silver nanowire. However, the silver nanowires synthesized by the method have small quantity and high reaction temperature.
Disclosure of Invention
Aiming at the technical problems, the invention provides a method for synthesizing the nano silver wire, which is used for preparing the nano silver wire in a water phase low-temperature environment, and is simple to operate and environment-friendly.
The invention adopts the following technical scheme:
the water phase low temperature nanometer silver wire synthesizing process includes the following steps:
(1) Preparing a silver nitrate precursor solution by taking deionized water as a solvent;
(2) Sodium bicarbonate, glucose and 1-allyl-3-methylimidazole are added into the precursor solution and stirred uniformly;
(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 (3) respectively washing the obtained product with deionized water and ethanol, and drying to obtain the nano silver wire.
Further, the mass ratio of the silver salt to the vitamin C is 1 (1-10).
Further, the mass ratio of the silver salt to the glucose is 1 (1-10).
Further, the mass ratio of the silver salt to the 1-allyl-3-methylimidazole is 1 (0.02-0.067).
Further, the mass ratio of the silver salt to the sodium bicarbonate is 1 (0.3-1).
Further, the stirring rate in the step (4) is 1 to 100rpm, preferably 5 to 50rpm.
Further, the reaction time in the step (4) is 10 to 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.
According to the aqueous phase low-temperature nano silver wire synthesis method, vitamin C is used as a reducing agent, glucose is used as a surfactant, 1-allyl-3-methylimidazole is used as a nucleation control agent, a silver nitrate precursor is reduced in an aqueous phase environment, and the nano silver wire can be obtained at a reaction temperature of 0-90 ℃, and the method is simple to operate, environment-friendly, low in production cost and suitable for large-scale popularization and application.
Drawings
For a clearer description of embodiments of the invention or of solutions in the prior art, the drawings which are used in the description of the embodiments or of the prior art will be briefly described, it being obvious that the drawings in the description below are only some embodiments of the invention, and that other drawings can be obtained from them without inventive effort for a person skilled in the art.
FIG. 1 is a scanning electron microscope image of the nano silver wire prepared in example 1 of the present invention;
fig. 2 is a scanning electron microscope image of the nano silver wire prepared in example 2 of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to fall within the scope of the invention.
Example 1
The water phase low temperature nanometer silver wire synthesizing process includes the following steps:
(1) Preparing 500mL of silver nitrate precursor solution with the concentration of 20mmol/L by taking deionized water as a solvent, 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) Then 50mL of vitamin C with the concentration of 0.5mol/L is slowly added, and the mixture is stirred for 10 minutes to be uniformly mixed 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 a stirring speed of 50 rpm;
(5) And cleaning 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 diagram of the nano silver wire is shown in figure 1.
The nano silver wire prepared by the embodiment has the diameter of 18-28 nm and the length of 20-35 mu m.
Example 2
The water phase low temperature nanometer silver wire synthesizing process includes 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) 3 g of sodium bicarbonate, 90 g of glucose and 0.2 g of 1-allyl-3-methylimidazole are added into the precursor solution and stirred uniformly;
(3) Then 100mL of vitamin C with the concentration of 1mol/L is slowly added, and the mixture is stirred for 10 minutes to be uniformly mixed 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) The obtained product is washed once by deionized water and ethanol respectively, and dried to obtain the nano silver wire, and a scanning electron microscope diagram of the nano silver wire is shown in figure 2.
The nano silver wire prepared in the embodiment has the diameter of 25-35 nm and the length of 35-60 mu m.
Example 3
The water phase low temperature nanometer silver wire synthesizing process includes 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) Then 50mL of vitamin C with the concentration of 1mol/L is slowly added, and the mixture is stirred for 10 minutes to be uniformly mixed 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 a stirring speed of 5 rpm;
(5) And (3) cleaning the obtained product with deionized water and ethanol for one time respectively, and drying to obtain the nano silver wire.
The nano silver wire prepared by the embodiment has the diameter of 40-60 nm and the length of 10-25 mu m.
According to the invention, the silver nanowire is prepared by reducing silver nitrate in a low-temperature water phase environment by taking vitamin C as a reducing agent, taking glucose as a surfactant and taking 1-allyl-3-methylimidazole as a nucleation control agent. Compared with the conventional alcohol thermal method with the reaction temperature above 100 ℃, the method reduces the reaction temperature, avoids the use of polyvinylpyrrolidone PVP, greatly simplifies the subsequent cleaning and purifying process, reduces the cost and improves the efficiency; and compared with ethylene glycol used in the conventional synthesis process, the pure water solvent is lower in cost and more environment-friendly.
The invention has been further described with reference to specific embodiments, but it should be understood that the detailed description is not to be construed as limiting the spirit and scope of the invention, but rather as providing those skilled in the art with the benefit of this disclosure with the benefit of their various modifications to the described embodiments.
Claims (4)
1. The water phase low temperature nano silver wire synthesizing process includes the following steps:
(1) Preparing a silver nitrate precursor solution by taking deionized water as a solvent;
(2) Sodium bicarbonate, glucose and 1-allyl-3-methylimidazole are added into the precursor solution and stirred uniformly;
(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) Washing the obtained product with deionized water and ethanol respectively, and drying to obtain nano silver wires;
the mass ratio of the silver salt to the vitamin C is 1 (1-10);
the mass ratio of the silver salt to the glucose is 1 (1-10);
the mass ratio of the silver salt to the 1-allyl-3-methylimidazole is 1 (0.02-0.067);
the mass ratio of the silver salt to the sodium bicarbonate is 1 (0.3-1).
2. The method for synthesizing the nano silver wire at the low temperature in the water phase according to claim 1, wherein the stirring speed in the step (4) is 1-100 rpm.
3. The method for synthesizing the nano silver wire at the low temperature in the water phase according to claim 1, wherein the reaction time in the step (4) is 10-60 hours.
4. The method for synthesizing the nano silver wire at the low temperature in the water phase according to claim 1, wherein the diameter of the nano silver wire is 15-100 nm and the length is 10-200 μm.
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| CN202011204338.0A CN114515836B (en) | 2020-11-02 | 2020-11-02 | Synthesis method of water-phase low-temperature nano silver wire |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011204338.0A CN114515836B (en) | 2020-11-02 | 2020-11-02 | Synthesis method of water-phase low-temperature nano silver wire |
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| CN114515836B true CN114515836B (en) | 2023-11-03 |
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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 |
-
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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