CN113210623B - Preparation method for synthesizing pure silver nanowire with controllable length-diameter ratio by microwave assistance - Google Patents

Preparation method for synthesizing pure silver nanowire with controllable length-diameter ratio by microwave assistance Download PDF

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CN113210623B
CN113210623B CN202110481865.4A CN202110481865A CN113210623B CN 113210623 B CN113210623 B CN 113210623B CN 202110481865 A CN202110481865 A CN 202110481865A CN 113210623 B CN113210623 B CN 113210623B
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nitrate
silver nanowire
silver
glycol
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CN113210623A (en
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秦发祥
许�鹏
沈雯钰
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Wuxi Xianfa New Material Technology Co ltd
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Abstract

The invention discloses a method for preparing pure silver nanowires with controllable length-diameter ratio by microwave-assisted synthesis. According to the method, a solvent heat-microwave assisted synthesis method is adopted, a glycol solution of silver nitrate and halide is heated and then is put into a microwave digestion instrument, and parameters such as microwave reaction temperature, time and power are controlled, and the stable pure silver nanowire with controllable length-diameter ratio is obtained after centrifugal washing. Compared with the traditional method for preparing the silver nanowire by using the polyol method, the method does not need to introduce high molecular polymers such as insulating polyvinylpyrrolidone, shortens the experimental period, improves the yield, realizes rapid synthesis of the silver nanowire with consistent size by utilizing the characteristics of high heating speed, uniform heating and the like of the microwave method synthesis, and controls the length-diameter ratio of the silver nanowire by controlling the microwave temperature.

Description

Preparation method for synthesizing pure silver nanowire with controllable length-diameter ratio by microwave assistance
Technical Field
The invention relates to a preparation method for synthesizing pure silver nanowires with controllable length-diameter ratio by microwave assistance, belonging to the technical field of nano material preparation.
Background
Silver nanowires have attracted the eyes of many material researchers due to their high conductivity, flexibility, chemical stability, and excellent optical properties. At present, most of silver nanowires are synthesized by adopting a chemical method, using polyalcohol as a solvent and a reducing agent, and reducing silver nitrate in the presence of polyvinylpyrrolidone (PVP) and halogen elements to prepare the silver nanowires. The weak reducing agent is used, so that the reaction time required by the solvothermal method is too long, and the required time is as long as several hours or even tens of hours. For example, in chinese patent publication No. CN111922359B (publication No. 2020.11.13), the heating reaction time required is 6-10 hours, and long preparation time may reduce the preparation efficiency of silver nanowires. In addition, most methods for preparing silver nanowires greatly reduce the yield of silver nanowires because the { 11 } crystal plane of silver is covered with insulating polyvinylpyrrolidone, which introduces a washing step for removing polyvinylpyrrolidone to the experiment. For example, in chinese patent publication No. CN105834454a (publication No. 2016.08.10), polyvinylpyrrolidone and ethylene glycol are added in a volume ratio of 1:5 to 1:10, the prepared silver nanowire is firstly washed three times by using acetone to remove polyvinylpyrrolidone and ethylene glycol, and then washed three times by using deionized water to remove the acetone, and the excessive washing times can reduce the yield of the silver nanowire, and the acetone has the advantages of high toxicity, low boiling point, easy volatilization and easy environmental pollution, and is not suitable for industrial mass production.
Disclosure of Invention
The invention aims to provide a preparation method of pure silver nanowires with different length-diameter ratios, which is rapid to manufacture, simple in process, good in stability and controllable, aiming at the defects of the existing method for synthesizing silver nanowires by using polyalcohol. The method starts with a solvothermal-microwave auxiliary synthesis method, solves the problems that the productivity and the conductivity of the prepared silver nanowire are reduced by adopting insulating polyvinylpyrrolidone in the traditional process, greatly reduces the preparation time of the silver nanowire by adopting a microwave synthesis method, and simultaneously controls the length-diameter ratio of the silver nanowire by changing the microwave temperature.
The technical scheme adopted by the invention is as follows:
the invention firstly discloses a preparation method for synthesizing pure silver nanowires with controllable length-diameter ratio by microwave assistance, which comprises the following steps: heating glycol, uniformly mixing with glycol solution of halide and glycol solution of nitrate, and preserving heat; mixing with glycol solution of silver nitrate, placing into a microwave digestion instrument for microwave heating, regulating microwave parameters, washing and centrifuging the obtained solution, and then re-dispersing in a solvent to obtain stably dispersed silver nanowires.
Further, the added halide is NaCl and CuCl 2 NaBr and FeCl 3 One or more of the following.
Further, the nitrate added is Fe (NO 3 ) 3 、Cu(NO 3 ) 3 And Na (NO) 3 ) 3 One or more of the following.
Preferably, the temperature of the ethylene glycol in the step S1 is 120 ℃, and the solution is in a stirring state.
Further, the halide and the nitrate are dissolved in the glycol first and then added into the glycol which is heated and kept warm for uniform mixing.
Further, the concentration of the halide in the glycol solution of the halide is 8-10 mmol/L, and the concentration of the nitrate in the glycol solution of the nitrate is 20-50 mmol/L; the volume ratio of the heated and heat-preserving glycol, the halide glycol solution and the nitrate glycol solution is 20:1.2:1.
Further, the concentration of the silver nitrate in the ethylene glycol solution of the silver nitrate is 10-30 mg/mL.
Further, the volume ratio of the heated and heat-preserving glycol to the glycol solution of silver nitrate is 1:1.
further, the microwave parameters are as follows: the microwave temperature is 110-150 ℃, the microwave frequency is 300-900 w, and the microwave time is 30-60 minutes.
Further, the rotational speed of the centrifugation is 6000-10000 revolutions per minute, the centrifugation time is 5-10 min, and the centrifugation times are 2 times; the dispersant selected is ethanol.
The invention also discloses the silver nanowire prepared by the method, the length-diameter ratio of the silver nanowire is controllable to 20-500, and the surface of the silver nanowire is not coated with insulation.
Compared with the prior art, the invention has the following beneficial effects:
1) The pure silver nanowire with controllable length-diameter ratio is prepared by the solvothermal-microwave auxiliary synthesis method, and the selected synthesis method is the solvothermal-microwave auxiliary synthesis method, so that the temperature is quickly increased, the heating is uniform, the preparation period of the silver nanowire is greatly shortened, the preparation efficiency of the material is improved, the prepared material is more uniform, and the preparation stability of the silver nanowire material is ensured.
2) The silver nanowire provided by the invention does not use polyvinylpyrrolidone, so that the experimental steps are reduced, the purity and conductivity of the silver nanowire are improved, and the performances of conductive electrodes, sensors, electromagnetic devices, energy storage, energy conversion and other application fields can be effectively improved.
3) The solvothermal-microwave assisted synthesis method prepares the pure silver nanowire with the controllable length-diameter ratio, and the silver nanowire with the controllable length-diameter ratio is effectively controlled by changing the microwave reaction temperature, so that the distribution and the utilization rate of the nano material are more accurately and effectively controlled on the raw material.
Drawings
FIG. 1 is an SEM image of silver nanowires prepared according to example 1;
FIG. 2 is an SEM image of silver nanowires prepared according to example 2;
FIG. 3 is an SEM image of silver nanowires prepared according to example 3;
fig. 4 is an XRD pattern of the silver nanowire prepared in example 1.
Detailed Description
The invention is further illustrated and described below with reference to the drawings and detailed description. Unless otherwise specified, all experimental reagents used in the invention are commercially available.
Example 1
The silver nanowire material is prepared by the specific preparation method as follows:
1) Analytically pure ethylene glycol was selected and 20mL of ethylene glycol was poured into a three-necked flask and heated with stirring to 120 ℃ for 1 hour.
2) Sequentially adding 1mL of FeCl with the concentration of 8mmol/L 3 Ethylene glycol solution, 0.2mL NaBr ethylene glycol solution with a concentration of 8mmol/L and 1mL Fe (NO) with a concentration of 40mmol/L 3 ) 3 Glycol solution was added to solution 1) and incubated for 20 minutes.
3) 20mL of ethylene glycol-dissolved silver nitrate (0.2 g) was slowly dropped into solution 2, and stirring was stopped.
4) Transferring the solution into a microwave digestion tank, setting the microwave heating time to be 1 hour, and setting the temperature to be 110 ℃ and the power to be 300w.
5) After the reaction of 4) was completed, the reaction product was washed twice with ethanol at 6000 rpm in a centrifuge and stored redispersed in ethanol.
The scanning electron microscope of the silver nanowire prepared in the embodiment is shown in fig. 1, fig. 4 is an XRD representation of the silver nanowire prepared in the embodiment 1, and it can be seen from fig. 4 that the prepared silver nanowire has a complete structure, an average diameter of 80nm, an average length of over 30 μm, and an aspect ratio of over 375 without insulating coating.
Example 2
The silver nanowire material is prepared by the specific preparation method as follows:
1) Analytically pure ethylene glycol was selected and 20mL of ethylene glycol was poured into a three-necked flask and heated with stirring to 120 ℃ for 1 hour.
2) Sequentially adding 1mL of FeCl with the concentration of 8mmol/L 3 Ethylene glycol solution, 0.2mL NaBr ethylene glycol solution with a concentration of 8mmol/L and 1mL Fe (NO) with a concentration of 40mmol/L 3 ) 3 Glycol solution was added to solution 1) and incubated for 20 minutes.
3) 20mL of ethylene glycol-dissolved silver nitrate (0.2 g) was slowly dropped into solution 2, and stirring was stopped.
4) Transferring the solution into a microwave digestion tank, setting the microwave heating time to be 1 hour, and setting the temperature to be 130 ℃ and the power to be 300w.
5) After the reaction of 4) was completed, the reaction product was washed twice with ethanol at 6000 rpm in a centrifuge and stored redispersed in ethanol.
FIG. 2 is a scanning electron microscope image of the silver nanowires prepared in example 2, wherein the average diameter of the silver nanowires is 100nm, the average length is more than 30 μm, the length-diameter ratio is more than 300, and the surface is not coated with insulation.
Example 3
The silver nanowire material prepared in the embodiment 3 is specifically prepared by the following steps:
1) Analytically pure ethylene glycol was selected and 20mL of ethylene glycol was poured into a three-necked flask and heated with stirring to 120 ℃ for 1 hour.
2) Sequentially adding 1mL of FeCl with the concentration of 8mmol/L 3 Ethylene glycol solution, 0.2mL NaBr ethylene glycol solution with a concentration of 8mmol/L and 1mL Fe (NO) with a concentration of 40mmol/L 3 ) 3 Glycol solution was added to solution 1) and incubated for 20 minutes.
3) 20mL of ethylene glycol-dissolved silver nitrate (0.2 g) was slowly dropped into solution 2, and stirring was stopped.
4) Transferring the solution into a microwave digestion tank, setting the microwave heating time to be 30 minutes, setting the temperature to be 150 ℃ and setting the power to be 300w.
5) After the reaction of 4) was completed, the reaction product was washed twice with ethanol at 6000 rpm in a centrifuge and stored redispersed in ethanol.
FIG. 3 is a scanning electron microscope image of silver nanowires prepared in example 3, the average diameter of the silver nanowires is 150nm, the average length is more than 3 μm, the length-diameter ratio is more than 20, and the surface is not coated with insulation.
The above-described embodiments are only preferred embodiments of the present invention, but are not intended to limit the present invention. Various changes and modifications may be made by one of ordinary skill in the pertinent art without departing from the spirit and scope of the present invention. Therefore, all the technical schemes obtained by adopting the equivalent substitution or equivalent transformation are within the protection scope of the invention.

Claims (5)

1. The preparation method for synthesizing the pure silver nanowire with the controllable length-diameter ratio by microwave assistance is characterized by comprising the following steps of: heating glycol, uniformly mixing with glycol solution of halide and glycol solution of nitrate, and preserving heat; mixing with ethylene glycol solution of silver nitrate, placing into a microwave digestion instrument for microwave heating, regulating microwave parameters, washing and centrifuging the obtained solution, and then re-dispersing in a solvent to obtain stably dispersed silver nanowires;
the halide and the nitrate are dissolved in glycol firstly and then added into the glycol which is heated and kept warm for uniform mixing; the concentration of the halide in the glycol solution of the halide is 8-10 mmol/L, and the concentration of the nitrate in the glycol solution of the nitrate is 20-50 mmol/L; heating and maintaining the volume ratio of glycol, glycol solution of halide and glycol solution of nitrate at 20:1.2:1; the concentration of the silver nitrate in the ethylene glycol solution of the silver nitrate is 10-30 mg/mL; the volume ratio of the heated and heat-preserving glycol to the glycol solution of silver nitrate is 1:1, a step of;
the microwave parameters are as follows: the microwave temperature is 110-150 ℃, the microwave frequency is 300-900 w, and the microwave time is 30-60 minutes.
2. The method for preparing the pure silver nanowire with controllable length-diameter ratio by microwave-assisted synthesis according to claim 1, wherein the added halide is NaCl or CuCl 2 NaBr and FeCl 3 One or more of the following.
3. The method for preparing pure silver nanowires with controllable aspect ratio by microwave-assisted synthesis according to claim 1, wherein the nitrate added is Fe (NO 3 ) 3 。
4. The method for preparing the pure silver nanowire with the controllable length-diameter ratio by microwave-assisted synthesis according to claim 1, wherein the rotation speed of centrifugation is 6000-10000 revolutions per minute, and the centrifugation time is 5-10 min; the dispersant selected is ethanol.
5. A silver nanowire prepared by the method according to any one of claims 1 to 4, wherein the aspect ratio is controlled to be 20 to 500, and the surface is not coated with insulation.
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