CN116921689A - Synthesis method of silver nanowire with ultrahigh length-diameter ratio - Google Patents
Synthesis method of silver nanowire with ultrahigh length-diameter ratio Download PDFInfo
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 239000002042 Silver nanowire Substances 0.000 title claims abstract description 67
- 238000001308 synthesis method Methods 0.000 title claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 38
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 38
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 38
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 32
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 30
- 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 16
- 239000008103 glucose Substances 0.000 claims abstract description 16
- 239000011780 sodium chloride Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 15
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 15
- 238000007789 sealing Methods 0.000 claims abstract description 8
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 58
- 238000003756 stirring Methods 0.000 claims description 35
- 239000008367 deionised water Substances 0.000 claims description 28
- 229910021641 deionized water Inorganic materials 0.000 claims description 28
- 239000000203 mixture Substances 0.000 claims description 16
- -1 polytetrafluoroethylene Polymers 0.000 claims description 10
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 9
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 9
- 238000000746 purification Methods 0.000 claims description 8
- 230000035484 reaction time Effects 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 239000012467 final product Substances 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 230000015572 biosynthetic process Effects 0.000 abstract description 10
- 238000003786 synthesis reaction Methods 0.000 abstract description 9
- 239000011248 coating agent Substances 0.000 abstract description 6
- 238000000576 coating method Methods 0.000 abstract description 6
- 239000002086 nanomaterial Substances 0.000 abstract description 4
- 238000010899 nucleation Methods 0.000 abstract description 4
- 230000006911 nucleation Effects 0.000 abstract description 3
- 230000001737 promoting effect Effects 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 238000004140 cleaning Methods 0.000 abstract 1
- 238000007865 diluting Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 238000002474 experimental method Methods 0.000 description 20
- 238000004090 dissolution Methods 0.000 description 12
- 238000005303 weighing Methods 0.000 description 8
- 239000000047 product Substances 0.000 description 7
- 239000013078 crystal Substances 0.000 description 6
- 239000002070 nanowire Substances 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- 238000005530 etching Methods 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 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 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000000024 high-resolution transmission electron micrograph Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000002667 nucleating agent Substances 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 238000004917 polyol method Methods 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 238000009417 prefabrication Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000010900 secondary nucleation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Classifications
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- 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
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0547—Nanofibres or nanotubes
-
- 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 belongs to the technical field of nano material synthesis, and particularly relates to a method for synthesizing silver nanowires with ultra-high length-diameter ratio. The synthesis method comprises the following steps: respectively preparing a silver nitrate solution, a sodium chloride solution, a glucose solution and a polyvinylpyrrolidone solution by taking water as a solvent; uniformly mixing the solutions, pouring the solutions into a reaction kettle, and reacting for a certain time after sealing; pouring out, diluting, cleaning and centrifuging. According to the invention, polyvinylpyrrolidone with different molecular weights is used, and polyvinylpyrrolidone chains with small molecular weights can enter gaps of polyvinylpyrrolidone chains with large molecular weights, so that the coating surface is longer, the coating surface is more compact, the length of the coating surface on the surface of the silver wire is increased, and the possibility of damaging the silver nanowire caused by secondary or multiple nucleation is also inhibited. Thereby better promoting the silver nanowire to grow anisotropically and have ultrahigh length-diameter ratio.
Description
Technical Field
The invention belongs to the technical field of nano material synthesis, and particularly relates to a synthesis method of silver nanowires with ultra-high length-diameter ratio.
Background
Silver nanowires are a typical one-dimensional metallic nanomaterial that not only have the small-size effect of the nanomaterial itself, but also have excellent thermal conductivity, electrical conductivity, and flexibility of the silver metal itself. Under the development hot trend of the current flexible wearable equipment, the silver nanowire is used as a base material of a high-performance flexible electrode, and has a wide application prospect. In general, transparent electrodes made from silver nanowires with high aspect ratios have better photovoltaic properties. Therefore, the silver nanowire with high purity and high length-diameter ratio is prepared efficiently by adopting a low-cost solution synthesis method, and has important scientific and economic significance.
Currently, the polyol process is the dominant method for synthesizing silver nanowires. For the synthesis of longer nanowires, common methods are mainly oxide etching, pre-seeding, low temperature synthesis and hydrothermal methods. Oxidizing etching, i.e., etching the seed crystal by adding oxidizing substances such as iron ions, copper ions, hydrogen peroxide, nitric acid, etc., to remove small-sized seed crystals and reduce the number of seed crystals, but the diameter is generally larger while obtaining longer nanowires. Prefabrication of seed, i.e. separately preparing seed, adjusts nanowire size by controlling seed size and concentration, silver ion supply, however secondary nucleation is more difficult to avoid and adds complexity to the process. The low-temperature synthesis utilizes low temperature to inhibit nucleation number and promote stable growth of the nanowire to obtain a longer nanowire, but the reduction of the polyol at low temperature is weak, so that the temperature reduction is limited, the length of the nanowire is limited to increase, and the reaction time is greatly prolonged due to the low-temperature reaction, so that the efficiency is low. The hydrothermal method is to synthesize longer silver nanowires by using water as a solvent, glucose as a reducing agent, polyvinylpyrrolidone as a morphology control agent and sodium chloride as a nucleating agent, but the silver nanowires synthesized by the hydrothermal method have thicker diameters and nonuniform diameters.
Disclosure of Invention
The invention aims to provide a method for synthesizing the silver nanowire with the ultrahigh length-diameter ratio, which has the advantages of simple synthesis process, high purity of the synthesized silver nanowire, high yield and uniform length and diameter.
The invention provides a method for synthesizing silver nanowires with ultra-high length-diameter ratio, which comprises the following specific steps:
step 1: dissolving silver nitrate in deionized water, and stirring and dissolving to form a silver nitrate solution with the concentration of 0.02-0.025M;
step 2: dissolving glucose in deionized water, and stirring and dissolving to form a glucose solution with the concentration of 0.02 g/mL-0.03 g/mL;
step 3: dissolving polyvinylpyrrolidone in deionized water, and stirring and dissolving to form polyvinylpyrrolidone solution with the concentration of 0.06 g/mL-0.1 g/mL; the polyvinylpyrrolidone is a mixture of K30, K60 and K88-96, and the mass ratio of the polyvinylpyrrolidone to the K30 to the K60 to the K88-96 is (0.8-1.2) to (0.8-1.2);
step 4: dissolving sodium chloride in deionized water, and stirring and dissolving to form a sodium chloride solution with the concentration of 0.12M-0.2M;
step 5: transferring the two solutions in the step 1 and the step 2 into a container, slowly adding the solution in the step 3, stirring for 30-35 minutes, and slowly dripping the solution in the step 4 to fully and uniformly mix the solutions;
step 6: transferring the mixed solution obtained in the step 5 into a polytetrafluoroethylene lining, sealing, and then placing the sealed polytetrafluoroethylene lining into a constant-temperature blast oven for reaction;
step 7: and after the reaction is finished, taking out the reaction kettle, putting the reaction kettle in an ice bath, rapidly cooling the reaction kettle to room temperature, and performing centrifugal washing and purification by a centrifugal machine to obtain a final product.
Further, the polyvinylpyrrolidone in the step 3 is a mixture of K30, K60 and K88-96, preferably the mass ratio of the three is k30:k60:k88-96=1:1:1.
Further, in the step 6, the reaction temperature is 150-170 ℃ and the reaction time is 10-24 hours.
In the present invention, the ultra-high aspect ratio silver nanowire means that the length-to-diameter ratio of the silver nanowire is 800 or more, preferably 1000 or more.
Compared with the prior art, the invention has the following beneficial effects:
compared with the previous researchers using polyvinylpyrrolidone with single molecular weight to synthesize silver nanowires (J. Mater. Chem. A, 2016, 4, 11365), the method for synthesizing the silver nanowires with ultra-high length-diameter ratio according to the invention uses high molecular weight polyethyleneWhen the polyvinylpyrrolidone is added, polyvinylpyrrolidone with small molecular weight is added, and polyvinylpyrrolidone with small molecular weight can enter gaps of polyvinylpyrrolidone with large molecular weight, so that the coating surface is longer, the coating surface is more compact, the length of the coating surface on the surface of the silver wire is increased, and the possibility of damaging the silver nanowire caused by secondary or multiple nucleation is also inhibited. Thereby better promoting the silver nanowires to grow anisotropically and have higher length-diameter ratio. At the same time, high concentration of Cl - Can co-act with oxygen in the solution to form Cl - /O 2 Other seed crystals can be selectively etched, and the yield of the silver nanowires is effectively improved. Experimental results show that the synthesis method provided by the invention can finally synthesize silver nanowires with average diameter of about 35nm and average length of about 350 mu m, and the length-diameter ratio of the silver nanowires is up to 10000 times.
The synthesis method disclosed by the invention is simple in process, high in purity, high in yield, uniform in length and diameter, good in repeatability and obvious in advantages in the application aspect of the flexible transparent conductive film.
Drawings
Fig. 1 is a low-magnification scanning electron micrograph of the silver nanowires obtained in example 1.
Fig. 2 is a high-magnification scanning electron micrograph of the silver nanowires obtained in example 1.
Fig. 3 is a high-power transmission electron micrograph of the silver nanowires obtained in example 2.
Fig. 4 is a high resolution transmission electron micrograph of the silver nanowires obtained in example 3.
Fig. 5 shows the X-ray diffraction analysis result (XRD) of the silver nanowire obtained in example 4, which is consistent with JCPDS:04-0783, and shows that the silver nanowire synthesized by the method example 1 has a higher purity, and the synthesized silver nanowire still has the same face-centered cubic structure as bulk silver.
FIG. 6 is an ultraviolet absorption spectrum (UV-Vis) of the silver nanowire synthesized in example 5, further demonstrating that the synthesized product is silver nanowire and that there are two characteristic peaks in the image, 350nm and 390nm, respectively. The peak at 350nm is related to the plasmon response of the silver nanowires, the peak at 390nm is due to the lateral plasmon mode of AgNWs, whereas the characteristic peak of the silver nanoparticles at 410nm is not detected in this spectrum.
Description of the embodiments
The invention is further described below by way of examples with reference to the accompanying drawings. The described embodiments are only some, but not all, embodiments of the invention. 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 be within the scope of the invention.
Examples
Step 1: weighing 125mg of silver nitrate, dissolving in 30 mL deionized water, and stirring to form silver nitrate solution with the concentration required by an experiment;
step 2: weighing 240mg of glucose, dissolving in 10 mL deionized water, and stirring to form glucose solution with concentration required by experiments;
step 3: 2g of polyvinylpyrrolidone is weighed and dissolved in 30 mL deionized water, and polyvinylpyrrolidone solution with the concentration required by the experiment is formed after stirring and dissolution; the polyvinylpyrrolidone is a mixture of K30, K60 and K88-96, and the mass ratio is K30:K 60:K 88-96=1:1:1;
step 4: 70mg of sodium chloride is weighed and dissolved in 10 mL deionized water, and sodium chloride solution with the concentration required by an experiment is formed after stirring and dissolution;
step 5: transferring the two solutions in the step 1 and the step 2 into a beaker, slowly adding the solution in the step 3, stirring for 30 minutes, and slowly dripping the solution in the step 4 to fully and uniformly mix the solutions;
step 6: transferring the mixed solution obtained in the step 5 into a polytetrafluoroethylene lining of 100 mL, sealing, and then placing into a constant-temperature blast oven, wherein the reaction temperature is 150 ℃ and the reaction time is 10 hours;
step 7: and after the reaction is finished, taking out the reaction kettle, putting the reaction kettle in an ice bath, rapidly cooling the reaction kettle to room temperature, and performing centrifugal washing and purification by a centrifugal machine to obtain a final product.
The synthesis method provided in the embodiment 1 of the invention can finally synthesize silver nanowires with average diameter of about 35nm and average length of about 350 μm, and the length-diameter ratio of the silver nanowires is up to 10000 times.
Examples
Step 1: weighing 125mg of silver nitrate, dissolving in 30 mL deionized water, and stirring to form silver nitrate solution with the concentration required by an experiment;
step 2: weighing 240mg of glucose, dissolving in 10 mL deionized water, and stirring to form glucose solution with concentration required by experiments;
step 3: 2g of polyvinylpyrrolidone is weighed and dissolved in 30 mL deionized water, and polyvinylpyrrolidone solution with the concentration required by the experiment is formed after stirring and dissolution; the polyvinylpyrrolidone is a mixture of K30, K60 and K88-96, and the mass ratio is K30:K 60:K 88-96=1:0.8:0.8;
step 4: 70mg of sodium chloride is weighed and dissolved in 10 mL deionized water, and sodium chloride solution with the concentration required by an experiment is formed after stirring and dissolution;
step 5: transferring the two solutions in the step 1 and the step 2 into a beaker, slowly adding the solution in the step 3, stirring for 30 minutes, and slowly dripping the solution in the step 4 to fully and uniformly mix the solutions;
step 6: transferring the mixed solution obtained in the step 5 into a polytetrafluoroethylene lining of 100 mL, sealing, and then placing into a constant-temperature blast oven, wherein the reaction temperature is 160 ℃ and the reaction time is 12 hours;
step 7: and after the reaction is finished, taking out the reaction kettle, putting the reaction kettle in an ice bath, rapidly cooling the reaction kettle to room temperature, and performing centrifugal washing and purification by a centrifugal machine to obtain a final product.
The synthesis method provided in the embodiment 2 of the invention can finally synthesize silver nanowires with average diameter of about 35nm and average length of about 350 μm, and the length-diameter ratio of the silver nanowires is up to 10000 times.
Examples
Step 1: 120mg of silver nitrate is weighed and dissolved in 30 mL deionized water, and after stirring and dissolution, silver nitrate solution with the concentration required by an experiment is formed;
step 2: weighing 250mg of glucose, dissolving in 10 mL deionized water, and stirring to form glucose solution with concentration required by an experiment;
step 3: 2g of polyvinylpyrrolidone is weighed and dissolved in 30 mL deionized water, and polyvinylpyrrolidone solution with the concentration required by the experiment is formed after stirring and dissolution; the polyvinylpyrrolidone is a mixture of K30, K60 and K88-96, and the mass ratio is K30:K 60:K 88-96=1:1:1;
step 4: 80mg of sodium chloride is weighed and dissolved in 10 mL deionized water, and sodium chloride solution with the concentration required by an experiment is formed after stirring and dissolution;
step 5: transferring the two solutions in the step 1 and the step 2 into a beaker, slowly adding the solution in the step 3, stirring for 30 minutes, and slowly dripping the solution in the step 4 to fully and uniformly mix the solutions;
step 6: transferring the mixed solution obtained in the step 5 into a polytetrafluoroethylene lining of 100 mL, sealing, and then placing into a constant-temperature blast oven, wherein the reaction temperature is 170 ℃ and the reaction time is 10 hours;
step 7: and after the reaction is finished, taking out the reaction kettle, putting the reaction kettle in an ice bath, rapidly cooling the reaction kettle to room temperature, and performing centrifugal washing and purification by a centrifugal machine to obtain a final product.
The synthesis method provided in the embodiment 3 of the invention can finally synthesize silver nanowires with average diameters of about 35nm and average lengths of about 350 μm, and the length-diameter ratio of the silver nanowires is up to 10000 times.
Examples
Step 1: weighing 115mg of silver nitrate, dissolving in 30 mL deionized water, and stirring to form silver nitrate solution with the concentration required by an experiment;
step 2: weighing 240mg of glucose, dissolving in 10 mL deionized water, and stirring to form glucose solution with concentration required by experiments;
step 3: 2g of polyvinylpyrrolidone is weighed and dissolved in 30 mL deionized water, and polyvinylpyrrolidone solution with the concentration required by the experiment is formed after stirring and dissolution; the polyvinylpyrrolidone is a mixture of K30, K60 and K88-96, and the mass ratio is K30:K 60:K 88-96=1:1:0.8;
step 4: 70mg of sodium chloride is weighed and dissolved in 10 mL deionized water, and sodium chloride solution with the concentration required by an experiment is formed after stirring and dissolution;
step 5: transferring the two solutions in the step 1 and the step 2 into a beaker, slowly adding the solution in the step 3, stirring for 30 minutes, and slowly dripping the solution in the step 4 to fully and uniformly mix the solutions;
step 6: transferring the mixed solution obtained in the step 5 into a polytetrafluoroethylene lining of 100 mL, sealing, and then placing into a constant-temperature blast oven, wherein the reaction temperature is 160 ℃ and the reaction time is 24 hours;
step 7: and after the reaction is finished, taking out the reaction kettle, putting the reaction kettle in an ice bath, rapidly cooling the reaction kettle to room temperature, and performing centrifugal washing and purification by a centrifugal machine to obtain a final product.
The synthesis method provided in example 4 of the present invention can finally synthesize silver nanowires with an average diameter of about 35nm and an average length of about 350 μm, and the aspect ratio of the silver nanowires is up to 10000 times.
Examples
Step 1: weighing 125mg of silver nitrate, dissolving in 30 mL deionized water, and stirring to form silver nitrate solution with the concentration required by an experiment;
step 2: 260mg of glucose is weighed and dissolved in 10 mL deionized water, and glucose solution with the concentration required by an experiment is formed after stirring and dissolution;
step 3: 2g of polyvinylpyrrolidone is weighed and dissolved in 30 mL deionized water, and polyvinylpyrrolidone solution with the concentration required by the experiment is formed after stirring and dissolution; the polyvinylpyrrolidone is a mixture of K30, K60 and K88-96, and the mass ratio is K30:K 60:K 88-96=1:0.8:1;
step 4: 70mg of sodium chloride is weighed and dissolved in 10 mL deionized water, and sodium chloride solution with the concentration required by an experiment is formed after stirring and dissolution;
step 5: transferring the two solutions in the step 1 and the step 2 into a beaker, slowly adding the solution in the step 3, stirring for 30 minutes, and slowly dripping the solution in the step 4 to fully and uniformly mix the solutions;
step 6: transferring the mixed solution obtained in the step 5 into a polytetrafluoroethylene lining of 100 mL, sealing, and then placing into a constant-temperature blast oven, wherein the reaction temperature is 150 ℃ and the reaction time is 10 hours;
step 7: and after the reaction is finished, taking out the reaction kettle, putting the reaction kettle in an ice bath, rapidly cooling the reaction kettle to room temperature, and performing centrifugal washing and purification by a centrifugal machine to obtain a final product.
The synthesis method provided in example 5 of the present invention can finally synthesize silver nanowires having an average diameter of about 35nm and an average length of about 350 μm, and the aspect ratio of the silver nanowires is up to 10000 times.
From examples 1 to 5, the synthesis method provided by the invention realizes the controllable synthesis of the silver nanowire with the ultra-high length-diameter ratio.
FIGS. 1 to 2 are scanning electron microscope images of the product obtained in example 1, and it can be seen that the average diameter of the silver nanowires is 35nm, no obvious impurity particles are generated, and the purity is high.
Fig. 3 is a transmission electron microscope image of the product obtained in this example 2, and it was found that the outer layer of the silver nanowires was coated with a light polyvinylpyrrolidone film having a thickness of about 1 a nm a. The layer of polyvinylpyrrolidone cannot be removed by adopting a centrifugal separation purification method, is firmly adsorbed on the surface of the silver nanowire through Ag-O coordination bonds, and can reduce the oxidation of AgNWs.
Fig. 4 is a high resolution transmission electron microscope image of the product obtained in this example 3, in which the crystal structure and sharp lattice fringes of silver nanowires are seen, and when the incident electron beam is perpendicular to the side surfaces of the wires, a moire pattern appears in the middle, with a lattice spacing as large as 0.38nm. This is caused by the superposition of the upper and lower monocrystalline subunits.
FIG. 5 is an X-ray diffraction pattern of the product obtained in this example 4, and it was found that five of the main diffraction peaks (i.e., bragg diffraction angles) of the silver nanowires appear in the figure, respectively at 38.1 ° {111}, 44.3 ° {200}, 64.4 ° {220}, 77.5 ° {311}, and 81.5 ° {222}, which correspond to the X-ray diffraction standard spectrum card (JCPDS: 04-0783) of elemental silver, indicating that the synthesized product is elemental silver and has a face-centered cubic structure. From the graph information, the {111} plane is the highest in intensity among five characteristic peaks, which indicates that the {100} plane with stronger crystal energy is well coated by polyvinylpyrrolidone, and silver nanowires selectively grow along the {111} plane.
FIG. 6 is an ultraviolet-visible absorption spectrum of the product obtained in example 5, in which there are two characteristic peaks in the image, respectively 350nm and 390nm. The peak at 350nm is related to the plasmon response of AgNWs, the peak at 390nm is due to the lateral plasmon mode of AgNWs, whereas the characteristic peak of the silver nanoparticle at 410nm is not detected in this spectrum.
Under the synergistic effect of three polyvinylpyrrolidone with different molecular weights, the silver nanowire with the ultra-high length-diameter ratio can be obtained, which breaks through the diameter of the silver nanowire synthesized by the hydrothermal method reported in the past and provides a new reference for the synthesis process and the growth theory of the silver nanowire.
The synthesis method of the silver nanowire provided by the invention adopts specific raw materials, and combines specific synthesis steps, conditions and parameters to realize better interaction, so that the large-scale synthesis of the silver nanowire can be realized by one-step reaction, the method is simple, and the obtained silver nanowire is uniform in size, thereby providing a foundation for subsequent functional application.
It will be readily appreciated by those skilled in the art that the foregoing description is merely a preferred embodiment of the invention and is not intended to limit the invention, but any modifications, equivalents, improvements or alternatives falling within the spirit and principles of the invention are intended to be included within the scope of the invention.
Claims (3)
1. The synthesis method of the silver nanowire with the ultrahigh length-diameter ratio is characterized by comprising the following specific steps of:
step 1: dissolving silver nitrate in deionized water, and stirring and dissolving to form a silver nitrate solution with the concentration of 0.02-0.025M;
step 2: dissolving glucose in deionized water, and stirring and dissolving to form a glucose solution with the concentration of 0.02 g/mL-0.03 g/mL;
step 3: dissolving polyvinylpyrrolidone in deionized water, and stirring and dissolving to form polyvinylpyrrolidone solution with the concentration of 0.06 g/mL-0.1 g/mL; the polyvinylpyrrolidone is a mixture of K30, K60 and K88-96, and the mass ratio is K30:K 60:K 88-96=1: (0.8-1.2): (0.8-1.2);
step 4: dissolving sodium chloride in deionized water, and stirring and dissolving to form a sodium chloride solution with the concentration of 0.12M-0.2M;
step 5: transferring the two solutions in the step 1 and the step 2 into a container, slowly adding the solution in the step 3, stirring for 30-35 minutes, and slowly dripping the solution in the step 4 to fully and uniformly mix the solutions;
step 6: transferring the mixed solution obtained in the step 5 into a polytetrafluoroethylene lining, sealing, and then placing the sealed polytetrafluoroethylene lining into a constant-temperature blast oven for reaction;
step 7: and after the reaction is finished, taking out the reaction kettle, putting the reaction kettle in an ice bath, rapidly cooling to room temperature, and performing centrifugal washing and purification by a centrifugal machine to obtain a final product silver nanowire, wherein the length-diameter ratio of the silver nanowire is more than 800.
2. The method of synthesizing ultra-high aspect ratio silver nanowires according to claim 1, wherein the polyvinylpyrrolidone in step 3 is a mixture of K30, K60 and K88-96 and the mass ratio is k30:k60:k88-96=1:1:1.
3. The method for synthesizing the silver nanowire with the ultrahigh length-diameter ratio according to claim 1, wherein the reaction temperature in the step 6 is 150-170 ℃ and the reaction time is 10-24 hours.
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