CN115870510A - Method for preparing superfine silver nanowires with assistance of moisture - Google Patents
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- CN115870510A CN115870510A CN202211505285.5A CN202211505285A CN115870510A CN 115870510 A CN115870510 A CN 115870510A CN 202211505285 A CN202211505285 A CN 202211505285A CN 115870510 A CN115870510 A CN 115870510A
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 239000002042 Silver nanowire Substances 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 23
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 246
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 51
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims abstract description 50
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims abstract description 48
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 40
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000008367 deionised water Substances 0.000 claims abstract description 32
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 32
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 20
- 239000011780 sodium chloride Substances 0.000 claims abstract description 20
- 238000002360 preparation method Methods 0.000 claims abstract description 3
- NIYNMSUOZKOTCX-UHFFFAOYSA-M sodium;ethane-1,2-diol;chloride Chemical compound [Na+].[Cl-].OCCO NIYNMSUOZKOTCX-UHFFFAOYSA-M 0.000 claims description 13
- UGWRVHSFESMVND-UHFFFAOYSA-N silver;ethane-1,2-diol;nitrate Chemical compound [Ag+].OCCO.[O-][N+]([O-])=O UGWRVHSFESMVND-UHFFFAOYSA-N 0.000 claims description 8
- GUCNKGGPYGRQIO-UHFFFAOYSA-M sodium ethane-1,2-diol bromide Chemical compound [Na+].[Br-].OCCO GUCNKGGPYGRQIO-UHFFFAOYSA-M 0.000 claims description 8
- 238000002604 ultrasonography Methods 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 229920005862 polyol Polymers 0.000 abstract description 3
- 150000003077 polyols Chemical class 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- 239000002070 nanowire Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 79
- 239000011521 glass Substances 0.000 description 20
- 239000000460 chlorine Substances 0.000 description 5
- 238000010791 quenching Methods 0.000 description 5
- 230000000171 quenching effect Effects 0.000 description 5
- 239000011550 stock solution Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000009210 therapy by ultrasound Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 2
- 229910052794 bromium Inorganic materials 0.000 description 2
- 239000010946 fine silver Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- ZYDVNTYVDVZMKF-UHFFFAOYSA-N [Cl].[Ag] Chemical compound [Cl].[Ag] ZYDVNTYVDVZMKF-UHFFFAOYSA-N 0.000 description 1
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 description 1
- 239000012965 benzophenone Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 238000004917 polyol method Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- -1 sodium bromide sodium chloride-ethylene glycol Chemical compound 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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Abstract
The invention discloses a method for preparing superfine silver nanowires with the assistance of moisture, and belongs to the technical field of nanowire materials. The invention discloses a method for preparing silver nanowires by using a polyol reduction method, which comprises the following steps: step 1, preparing a silver nitrate glycol solution, a PVP glycol solution, a sodium chloride glycol solution and a sodium bromide glycol solution, and adding a certain amount of deionized water into the four solutions after the preparation is finished; and 2, uniformly mixing the silver nitrate glycol solution, the PVP glycol solution, the sodium chloride glycol solution and the sodium bromide glycol solution prepared in the step 1, heating for a certain time, and then adding a certain amount of deionized water to grow the silver nanowires to obtain the ultrafine silver nanowires with the diameter less than 20nm. The invention inhibits the lateral growth of the silver nanowire by a deionized water assisted method, thereby obtaining the superfine silver nanowire with smaller diameter, and the invention has the advantages of simple design and easy manufacture.
Description
Technical Field
The invention belongs to the technical field of nanowire materials, and particularly relates to a method for preparing ultrafine silver nanowires with the assistance of moisture.
Background
Silver nanowires have been widely used as transparent conductive electrodes in flexible, stretchable electronic devices, and have recently attracted great interest in academia and industry. There is theoretical and experimental evidence that ultra-fine silver nanowires with an average diameter of less than 20nm or finer would be one of the most promising candidates in competition with the most advanced Indium Tin Oxide (ITO) transparent conductive films. In recent years, many researchers have been devoted to the synthesis of ultrafine silver nanowires, and for example, a high-pressure hydrothermal method of synthesizing ultrafine silver nanowires having a diameter of 15 to 20nm, a magnetoionic-liquid assisted polyol method of synthesizing ultrafine silver nanowires having an average diameter of 20nm, and 23 benzophenone-derived radicals as mild reducing agents of synthesizing ultrafine silver nanowires having an average diameter of 13nm have been proposed, but it is still difficult to expand the production of ultrafine silver nanowires using these methods. In recent years, various groups have used an improved polyol reduction method to synthesize ultrafine silver nanowires. The essence of the method is to utilize Cl - And Br - The ions control the nucleation and growth of the superfine silver nanowires simultaneously. The method has been popularized by a plurality of research groups to the synthesis of superfine silver nanowires. Although this approach is scalable, the diameter of the resulting ultra-fine silver nanowires is still difficult to be below 20nm. The invention is realized by regulatingThe natural factor of the water content in the formation process further reduces the size of the superfine silver nanowires.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a method for preparing ultrafine silver nanowires with the assistance of moisture, which does not need to add redundant elements and can obviously reduce the diameter of the ultrafine silver nanowires by adding a certain amount of deionized water.
The invention is realized by the following technical scheme:
a method for preparing superfine silver nanowires with the assistance of moisture comprises the following steps:
1) Respectively preparing a silver nitrate glycol solution, a PVP glycol solution, a sodium chloride glycol solution and a sodium bromide glycol solution, and respectively adding a certain amount of deionized water into the solutions after the preparation is finished;
2) Taking ethylene glycol, firstly adding a certain amount of deionized water, and then sequentially adding the silver nitrate ethylene glycol solution, the PVP ethylene glycol solution, the sodium chloride ethylene glycol solution and the sodium bromide ethylene glycol solution prepared in the step 1), uniformly mixing, and heating to grow the silver nanowires.
Further, in the step 1), the silver nitrate glycol solution is prepared in an ice bath at 0-5 ℃ for 5-10min by ultrasonic treatment.
Further, in the step 1), the PVP ethylene glycol solution is heated and dissolved at the high temperature of 100-130 ℃ for 20-50min to prepare the PVP ethylene glycol solution.
Further, in the step 1), the sodium chloride glycol solution and the sodium bromide glycol solution are heated and dissolved at a high temperature of 130-160 ℃ for 10-30min to prepare the sodium bromide sodium chloride-ethylene glycol solution.
Further, in the step 1), the volume ratio of deionized water to ethylene glycol added into each ethylene glycol solution is (0.1-0.5): 100.
further, in the step 2), the temperature range for heating and growing the silver nanowires is 130-150 ℃.
Further, in the step 2), the volume ratio of the deionized water to the ethylene glycol is (0.5-1): 100.
Compared with the prior art, the invention has the beneficial effects that:
the invention reduces the diameter of the superfine silver nanowire in a moisture-assisted manner, and the superfine silver nanowire prepared by the modified polyol reduction method mainly depends on Cl - And Br - To adjust the diameter of the superfine silver nanowires, but free Cl in the solution - And Br - Is not a main factor for regulating and controlling the diameter of the superfine silver nano-wire, and only Cl in the synthesized bromine-rich chlorine silver ore seed - And Br - The diameter of the superfine silver nano-wire is greatly influenced, and the existence of the water in the glycol solution influences the Cl in the bromine-rich silver chloride ore seeds to a certain extent - And Br - The content of the silver nano-wire is beneficial to further reducing the diameter of the superfine silver nano-wire, and the superfine silver nano-wire with the diameter of 15-20nm is finally obtained, so that the requirements of the transparent conductive electrode on the excellent conductivity and light transmittance of the silver nano-wire can be met, and the application range of the silver nano-wire is further widened. The method has simple design and easy manufacture. At present, no report is available in the literature and the patent on reducing the diameter of the superfine silver nanowires by a moisture-assisted mode.
Drawings
Fig. 1 is a SEM pictorial view of the silver nanowires synthesized in example 2;
fig. 2 is a SEM pictorial view of silver nanowires synthesized in comparative example 1;
fig. 3 is a SEM pictorial view of the silver nanowire synthesized in comparative example 2.
Detailed Description
The present invention will be further described with reference to specific examples in order to better understand the technical solution.
Example 1
PVP/ethylene glycol solution: weigh 5.04g PVP (K90) into a 100mL Erlenmeyer flask, then add 90mL of ethylene glycol, set the heating plate to a temperature of 105 deg.C, and place the Erlenmeyer flask on the heating plate for 45min until the PVP is completely dissolved, resulting in a colorless PVP/ethylene glycol solution, then add 0.18mL deionized water.
Sodium chloride ethylene glycol solution: 0.2466g of sodium chloride was weighed into a brown glass bottle, 20mL of ethylene glycol was added, the hot plate was set to 135 deg.C, and the brown glass bottle was placed on the hot plate for 25min until the sodium chloride was completely dissolved, resulting in a colorless sodium chloride ethylene glycol solution, followed by the addition of 0.04mL of deionized water.
Sodium bromide glycol solution: 0.4572g of sodium bromide was weighed into a brown glass bottle, 20mL of ethylene glycol was added, the heating plate was set to 135 deg.C, and the brown glass bottle was placed on the heating plate for 25min until the sodium bromide was completely dissolved, resulting in a colorless sodium bromide ethylene glycol solution, followed by the addition of 0.04mL of deionized water.
Silver nitrate glycol solution: taking a centrifuge tube, adding 0.6765g of silver nitrate, pouring 15mL of ethylene glycol, placing the centrifuge tube in an ice bath at 2 ℃, standing for 1min, still performing 100HZ ultrasound in the ice bath for 7min to obtain a colorless silver nitrate ethylene glycol solution, and then adding 0.03mL of deionized water.
Adding 0.69mL of deionized water, 1mL of sodium bromide glycol solution, 2mL of sodium chloride glycol solution and 15mL of PVP/glycol solution into 115mL of ethylene glycol, quickly injecting the mixture into the single-neck round-bottom flask, finally injecting 15mL of silver nitrate glycol solution, uniformly mixing, reacting at 135 ℃ for 60min, taking out the single-neck round-bottom flask, and putting the single-neck round-bottom flask into cold water for quenching to obtain the gray-green superfine silver nanowire stock solution.
Example 2
PVP/ethylene glycol solution: weigh 5.04g PVP (K90) into a 100mL Erlenmeyer flask, then add 90mL ethylene glycol, set the hotplate to 130 deg.C, and place the Erlenmeyer flask on the hotplate for 20min until the PVP is completely dissolved, resulting in a colorless PVP/ethylene glycol solution, then add 0.45mL deionized water.
Sodium chloride ethylene glycol solution: 0.2466g of sodium chloride was weighed into a brown glass bottle, 20mL of ethylene glycol was added, the hot plate was set to 150 ℃ and the brown glass bottle was placed on the hot plate for 13min until the sodium chloride was completely dissolved, giving a colorless sodium chloride ethylene glycol solution, followed by the addition of 0.10mL of deionized water.
Sodium bromide glycol solution: 0.4572g of sodium bromide was weighed into a brown glass bottle, 20mL of ethylene glycol was added, the heating plate was set to 150 ℃ and the brown glass bottle was placed on the heating plate for 13min until the sodium bromide was completely dissolved, resulting in a colorless sodium bromide ethylene glycol solution, followed by the addition of 0.10mL of deionized water.
Silver nitrate glycol solution: taking a centrifuge tube, adding 0.6765g of silver nitrate, pouring 15mL of ethylene glycol, placing the centrifuge tube in an ice bath at 5 ℃ for standing for 1min, still performing 100HZ ultrasonic treatment in the ice bath for 10min to obtain a colorless silver nitrate ethylene glycol solution, and then adding 0.06mL of deionized water.
Adding 1.03mL of deionized water, 1mL of sodium bromide glycol solution, 2mL of sodium chloride glycol solution and 15mL of PVP/glycol solution into 115mL of ethylene glycol, quickly injecting the mixture into the single-neck round-bottom flask, finally injecting 15mL of silver nitrate glycol solution, uniformly mixing, reacting at 150 ℃ for 60min, taking out the single-neck round-bottom flask, and putting the single-neck round-bottom flask into cold water for quenching to obtain a gray-green superfine silver nanowire stock solution. The diameters of the silver nanowires were measured as shown in fig. 1.
Example 3
PVP/ethylene glycol solution: weigh 5.04g PVP (K90) into a 100mL Erlenmeyer flask, then add 90mL ethylene glycol, set the heating plate at 130 deg.C, and place the Erlenmeyer flask on the heating plate for 60min until the PVP is completely dissolved, resulting in a colorless PVP/ethylene glycol solution, then add 0.36mL deionized water.
Sodium chloride ethylene glycol solution: 0.2466g of sodium chloride was weighed into a brown glass bottle, 20mL of ethylene glycol was added, the hot plate was set to 145 deg.C, and the brown glass bottle was placed on the hot plate for 16min until the sodium chloride was completely dissolved, resulting in a colorless sodium chloride ethylene glycol solution, followed by 0.08mL of deionized water.
Sodium bromide glycol solution: 0.4572g of sodium bromide was weighed into a brown glass bottle, 20mL of ethylene glycol was added, the hot plate was set to 145 deg.C, and the brown glass bottle was placed on the hot plate for 16min until the sodium bromide was completely dissolved, resulting in a colorless sodium bromide ethylene glycol solution, followed by 0.08mL of deionized water.
Silver nitrate glycol solution: taking a centrifuge tube, adding 0.6765g of silver nitrate, pouring 15mL of ethylene glycol, placing the centrifuge tube in an ice bath at 4 ℃ for standing for 1min, still performing 100HZ ultrasonic treatment in the ice bath for 9min to obtain a colorless silver nitrate ethylene glycol solution, and then adding 0.05mL of deionized water.
Adding 0.92mL of deionized water, 1mL of sodium bromide glycol solution, 2mL of sodium chloride glycol solution and 15mL of PVP/glycol solution into 115mL of ethylene glycol, quickly injecting the mixture into the single-neck round-bottom flask, finally injecting 15mL of silver nitrate glycol solution, uniformly mixing, reacting at 145 ℃ for 60min, taking out the single-neck round-bottom flask, and putting the single-neck round-bottom flask into cold water for quenching to obtain the gray-green superfine silver nanowire stock solution.
Comparative example 1
PVP/ethylene glycol solution: weigh 5.04g PVP (K90) into a 100mL Erlenmeyer flask, then add 90mL ethylene glycol, set the heating plate to 110 deg.C, and place the Erlenmeyer flask on the heating plate for 40min until the PVP is completely dissolved, resulting in a colorless PVP/ethylene glycol solution, then add 0.09mL deionized water.
Sodium chloride ethylene glycol solution: 0.2466g of sodium chloride was weighed into a brown glass bottle, 20mL of ethylene glycol was added, the hot plate was set at 140 ℃ and the brown glass bottle was placed on the hot plate for 20min until the sodium chloride was completely dissolved, giving a colorless sodium chloride ethylene glycol solution, followed by 0.02mL of deionized water.
Sodium bromide glycol solution: 0.4572g of sodium bromide was weighed into a brown glass bottle, 20mL of ethylene glycol was added, the hot plate was set at 140 deg.C, and the brown glass bottle was placed on the hot plate for 20min until the sodium bromide was completely dissolved, resulting in a colorless sodium bromide ethylene glycol solution, followed by 0.02mL of deionized water.
Silver nitrate glycol solution: taking a centrifuge tube, adding 0.6765g of silver nitrate, pouring 15mL of ethylene glycol, placing the centrifuge tube in an ice bath at 3 ℃, standing for 1min, still performing 100HZ ultrasound in the ice bath for 8min to obtain a colorless silver nitrate ethylene glycol solution, and then adding 0.02mL of deionized water.
Adding 0.57mL of deionized water, 1mL of sodium bromide glycol solution, 2mL of sodium chloride glycol solution and 15mL of PVP/glycol solution into 115mL of ethylene glycol, quickly injecting the mixture into the single-neck round-bottom flask, finally injecting 15mL of silver nitrate glycol solution, uniformly mixing, reacting at 140 ℃ for 60min, taking out the single-neck round-bottom flask, and quenching in cold water to obtain the gray-green superfine silver nanowire stock solution. The measured diameters of the silver nanowires are shown in FIG. 2
Comparative example 2
PVP/ethylene glycol solution: weigh 5.04g PVP (K90) into a 100mL Erlenmeyer flask, then add 90mL ethylene glycol, set the heating plate at 130 deg.C, and place the Erlenmeyer flask on the heating plate for 20min until the PVP is completely dissolved, resulting in a colorless PVP/ethylene glycol solution.
Sodium chloride ethylene glycol solution: 0.2466g of sodium chloride is weighed and placed in a brown glass bottle, 20mL of ethylene glycol is added, the heating plate is set to 150 ℃, and the brown glass bottle is placed on the heating plate for 13min until the sodium chloride is completely dissolved, so that a colorless sodium chloride ethylene glycol solution is obtained.
Sodium bromide glycol solution: 0.4572g of sodium bromide is weighed and placed in a brown glass bottle, 20mL of ethylene glycol is added, the heating plate is set at 150 ℃, and the brown glass bottle is placed on the heating plate for 13min until the sodium bromide is completely dissolved, so that colorless sodium bromide ethylene glycol solution is obtained.
Silver nitrate glycol solution: taking a centrifuge tube, adding 0.6765g of silver nitrate, pouring 15mL of ethylene glycol, placing the centrifuge tube in an ice bath at 5 ℃ for standing for 1min, and performing 100HZ ultrasonic treatment in the ice bath for 10min to obtain a colorless silver nitrate ethylene glycol solution.
And (2) quickly injecting 115mL of ethylene glycol, 1mL of sodium bromide ethylene glycol solution, 2mL of sodium chloride ethylene glycol solution and 15mL of PVP/ethylene glycol solution into the single-neck round-bottom flask, finally injecting 15mL of silver nitrate ethylene glycol solution, reacting for 60min at 150 ℃ after uniformly mixing, taking out the single-neck round-bottom flask, and putting the single-neck round-bottom flask into cold water for quenching to obtain the grey-green superfine silver nanowire stock solution. The diameters of the silver nanowires were measured as shown in fig. 3.
Claims (7)
1. A method for preparing superfine silver nanowires with the assistance of moisture is characterized by comprising the following steps:
1) Respectively preparing a silver nitrate glycol solution, a PVP glycol solution, a sodium chloride glycol solution and a sodium bromide glycol solution, and respectively adding a certain amount of deionized water into the solutions after the preparation is finished;
2) Adding a certain amount of deionized water into ethylene glycol, and then sequentially adding the silver nitrate ethylene glycol solution, the PVP ethylene glycol solution, the sodium chloride ethylene glycol solution and the sodium bromide ethylene glycol solution prepared in the step 1), uniformly mixing and heating to grow the silver nanowires.
2. The method for preparing ultrafine silver nanowires with the assistance of moisture according to claim 1, wherein in step 1), the silver nitrate glycol solution is prepared by ultrasound in an ice bath at 0-5 ℃ for 5-10 min.
3. The method for preparing ultrafine silver nanowires with the assistance of moisture according to claim 1, wherein in step 1), PVP (polyvinyl pyrrolidone) glycol solution is heated and dissolved at a high temperature of 100-130 ℃ for 20-50 min.
4. The method for preparing ultrafine silver nanowires with the assistance of moisture according to claim 1, wherein in step 1), the solution of sodium chloride in ethylene glycol and the solution of sodium bromide in ethylene glycol are heated and dissolved at a high temperature of 130-160 ℃ for 10-30 min.
5. The method for preparing ultrafine silver nanowires with the aid of moisture according to claim 1, wherein in step 1), deionized water and ethylene glycol are added to each ethylene glycol solution in a volume ratio of (0.1-0.5): 100.
6. the method for preparing ultrafine silver nanowires with moisture assistance according to claim 1, wherein the temperature range for heating and growing the silver nanowires in step 2) is 130-150 ℃.
7. The method for preparing ultrafine silver nanowires with the aid of moisture according to claim 1, wherein in the step 2), the volume ratio of deionized water to ethylene glycol is (0.5-1): 100.
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