CN111842925A - Preparation method of silver nanowire and silver nanowire prepared by same - Google Patents
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- CN111842925A CN111842925A CN202010702904.4A CN202010702904A CN111842925A CN 111842925 A CN111842925 A CN 111842925A CN 202010702904 A CN202010702904 A CN 202010702904A CN 111842925 A CN111842925 A CN 111842925A
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Abstract
The invention provides a preparation method of a silver nanowire, which comprises the following steps: providing a polyol solution of a metal chloride; providing a polyol solution of an organic protectant; providing a polyol solution of a silver precursor; mixing the polyalcohol solution of the silver precursor with the polyalcohol solution of the organic protective agent to obtain a first mixed solution; mixing the polyalcohol solution of the metal chloride with the first mixed solution to prepare a second mixed solution; and (3) reacting the second mixed solution at the temperature of 110-150 ℃ for 6-10 h to prepare a solid-liquid mixture, and separating the solid-liquid mixture to remove the upper solution to prepare the silver nanowire. The average length of the prepared silver nanowires reaches more than 30 micrometers, even the silver nanowires with the length of about 120 micrometers can be prepared, and the prepared silver nanowires are controllable in length and uniform in size.
Description
Technical Field
The invention relates to the technical field of nano material preparation, in particular to a preparation method of a silver nanowire and the prepared silver nanowire.
Background
Transparent Conductive Electrodes (TCEs) are important components of photovoltaic devices such as solar cells, liquid crystal displays, Organic Light Emitting Diodes (OLEDs), touch screens, organic EL panels, and the like. Indium Tin Oxide (ITO) is widely used as a TCE material due to its high optical transparency and low sheet resistance. With the development of photovoltaic or photoelectric devices in the aspects of miniaturization, portability, flexibility and the like, ITO cannot meet the requirements of future applications due to the characteristics of weak chemical and thermal stability, high brittleness, toxicity and the like. Transparent conductive thin films such as carbon nanotubes, metal gates, graphene, thin metal films, etc. have been widely studied, but the transmittance, conductivity and stability of the transparent conductive thin films cannot simultaneously satisfy the requirements of TCE.
Silver nanowires (AgNWs), which are considered promising candidates for replacing ITO for flexible or bendable displays in TCE production, are of great interest because of their highest electrical and thermal conductivity among all metals and potential application in the fabrication of nanoscale electronic devices. However, the silver nanowires prepared by the traditional method cannot generate silver nanowires with uniform states, and the lengths of the silver nanowires are not long.
Disclosure of Invention
Based on this, the invention provides a novel silver nanowire preparation method and a silver nanowire prepared by the method, which are necessary to solve the technical problems of non-uniform state and short length of the silver nanowire prepared by the traditional method.
The invention provides a preparation method of a silver nanowire, which comprises the following steps:
providing a polyol solution of a metal chloride;
providing a polyol solution of an organic protectant;
providing a polyol solution of a silver precursor;
mixing the polyalcohol solution of the silver precursor with the polyalcohol solution of the organic protective agent to obtain a first mixed solution;
mixing the polyalcohol solution of the metal chloride with the first mixed solution to prepare a second mixed solution;
and (3) reacting the second mixed solution at the temperature of 110-150 ℃ for 6-10 h to prepare a solid-liquid mixture, and separating the solid-liquid mixture to remove the upper solution to prepare the silver nanowire.
In one embodiment, the polyol solution of the silver precursor and the polyol solution of the organic protective agent are mixed in a manner that the polyol solution of the silver precursor is added dropwise into the polyol solution of the organic protective agent; the mixing mode of the polyol solution of the metal chloride and the first mixed solution is that the polyol solution of the metal chloride is dripped into the first mixed solution.
In one embodiment, the metal chloride includes any one of ferric chloride, cupric chloride and sodium chloride, the organic protective agent is polyvinylpyrrolidone, the silver precursor is silver nitrate or silver acetate, and the polyol is selected from ethylene glycol or glycerol.
In one embodiment, the molar concentration of the polyol solution of the metal chloride is 5-55 μmol/L.
In one embodiment, when the metal chloride is ferric chloride, the molar concentration of the polyhydric alcohol solution of the metal chloride is 5-35 mu mol/L; when the metal chloride is copper chloride, the molar concentration of the polyalcohol solution of the metal chloride is 9-51 mu mol/L; when the metal chloride is sodium chloride, the molar concentration of the polyalcohol solution of the metal chloride is 30-37.5 mu mol/L.
In one embodiment, the mass concentration of the polyalcohol solution of the organic protective agent is 2 g/L-10 g/L; the mass concentration of the polyalcohol solution of the silver precursor is 2 g/L-10 g/L.
In one embodiment, the mass ratio of the organic protective agent to the silver precursor in the first mixed solution is 1: 3-3: 1.
In one embodiment, the volume ratio of the polyol solution of the metal chloride to the first mixed solution is 1: 100.
The invention also provides a silver nanowire prepared by the preparation method.
In one embodiment, the silver nanowires have an average length of 30 μm to 120 μm.
According to the preparation method of the silver nanowires, the silver nanowires are prepared by inducing the metal chloride, the average length of the prepared silver nanowires is more than 30 micrometers, even the silver nanowires with the length of about 120 micrometers can be prepared, and the prepared silver nanowires are controllable in length and uniform in size. In addition, the preparation method of the silver nanowire is simple, mild in reaction condition, easy to control and good in repeatability.
Drawings
Fig. 1 is an SEM image of silver nanowires prepared in example 1 of the present invention;
FIG. 2 is an SEM image of silver nanowires prepared in example 2 of the present invention;
FIG. 3 is an SEM image of silver nanowires prepared in example 3 of the present invention;
fig. 4 is an XRD pattern of silver nanowires prepared in examples 1, 2 and 3 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the detailed description and specific examples, while indicating the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
The reagents used in the following examples are all commercially available reagents having chemical purity or higher.
Different from the understanding of the influence of the traditional preparation method of the silver nanowires on the types of metal chlorides and the selection and the recognition of the organic protective agent on the product, the research of the invention finds that the organic protective agent not only inhibits the grain diameter increase of the silver nanowires in the reaction, but also has important influence on the preparation length of the silver nanowires due to the average molecular weight of the organic protective agent, and the organic protective agents with different average molecular weights are selected, so that the prepared silver nanowires have great length difference. In addition, the kind of metal chloride also has an important influence on the length, uniformity, yield of the prepared silver nanowire, and is confirmed by the following examples and comparative examples.
Example 1
An ethylene glycol solution of ferric chloride having a molar concentration of 12.5. mu. mol/L, an ethylene glycol solution of polyvinylpyrrolidone having a mass concentration of 6g/L (average molecular weight of 1300000), and an ethylene glycol solution of silver nitrate having a mass concentration of 4g/L were prepared, respectively. 50mL of silver nitrate glycol solution is dripped into 50mL of ethylene glycol solution of vinyl pyrrolidone to prepare a first mixed solution, 1mL of ferric chloride glycol solution is dripped into the first mixed solution, and then the reaction is carried out for 8h at the temperature of 130 ℃. And placing the solid-liquid mixture obtained after the reaction in a centrifuge, centrifuging for 5min at the rotating speed of 4000rpm, washing the solid for 2-3 times by using absolute ethyl alcohol, removing the upper-layer liquid, and storing the lower-layer precipitate, namely the silver nanowires in the absolute ethyl alcohol. The detection shows that the yield of the prepared silver nanowire is 72.5%.
Referring to fig. 1, which is an SEM image of the silver nanowires obtained in example 1, it can be seen that the diameters of the prepared silver nanowires are uniform, the average length of the silver nanowires is 30 μm, and the percentage of the silver nanowires with lengths of 25 μm to 35 μm in the product is 94% by detection.
Example 2
An ethylene glycol solution of copper chloride having a molar concentration of 18.75 μmol/L, an ethylene glycol solution of polyvinylpyrrolidone having a mass concentration of 6g/L (average molecular weight of 1300000), and an ethylene glycol solution of silver nitrate having a mass concentration of 4g/L were prepared, respectively. 50mL of silver nitrate glycol solution is dripped into 50mL of ethylene glycol solution of vinyl pyrrolidone to prepare a first mixed solution, 1mL of ferric chloride glycol solution is dripped into the first mixed solution, and then the reaction is carried out for 8h at the temperature of 130 ℃. And placing the solid-liquid mixture obtained after the reaction in a centrifuge, centrifuging for 5min at the rotating speed of 4000rpm, washing the solid for 2-3 times by using absolute ethyl alcohol, removing the upper-layer liquid, and storing the lower-layer precipitate, namely the silver nanowires in the absolute ethyl alcohol. The detection shows that the yield of the prepared silver nanowire is 81.3%.
Referring to fig. 2, which is an SEM image of the silver nanowires obtained in example 2, it can be seen that the diameters of the prepared silver nanowires are uniform, the average length of the silver nanowires is 50 μm, and the percentage of the silver nanowires having a length of 45 μm to 45 μm in the product is 96% by detection.
Example 3
An ethylene glycol solution of sodium chloride having a molar concentration of 37.5. mu. mol/L, an ethylene glycol solution of polyvinylpyrrolidone having a mass concentration of 6g/L (average molecular weight of 1300000), and an ethylene glycol solution of silver nitrate having a mass concentration of 4g/L were prepared, respectively. 50mL of silver nitrate glycol solution is dripped into 50mL of ethylene glycol solution of vinyl pyrrolidone to prepare a first mixed solution, 1mL of ferric chloride glycol solution is dripped into the first mixed solution, and then the reaction is carried out for 8h at the temperature of 130 ℃. And placing the solid-liquid mixture obtained after the reaction in a centrifuge, centrifuging for 5min at the rotating speed of 4000rpm, washing the solid for 2-3 times by using absolute ethyl alcohol, removing the upper-layer liquid, and storing the lower-layer precipitate, namely the silver nanowires in the absolute ethyl alcohol. The detection shows that the yield of the prepared silver nanowire is 83.7%.
Referring to fig. 3, which is an SEM image of the silver nanowires obtained in example 3, it can be seen that the diameters of the prepared silver nanowires are uniform, the average length of the silver nanowires is 120 μm, and the percentage of the silver nanowires with the length of 115 μm to 125 μm in the product is 97%.
Fig. 4 is a XRD chart of the silver nanowires prepared in examples 1, 2 and 3 of the present invention. As can be seen from the figure, the prepared silver nanowires were completely crystallized.
Example 4
An ethylene glycol solution of sodium chloride having a molar concentration of 37.5. mu. mol/L, an ethylene glycol solution of polyvinylpyrrolidone having a mass concentration of 6g/L (average molecular weight: 58000), and an ethylene glycol solution of silver nitrate having a mass concentration of 4g/L were prepared, respectively. 50mL of silver nitrate glycol solution is dripped into 50mL of ethylene glycol solution of vinyl pyrrolidone to prepare a first mixed solution, 1mL of sodium chloride glycol solution is dripped into the first mixed solution, and then the reaction is carried out for 8h at the temperature of 130 ℃. And placing the solid-liquid mixture obtained after the reaction in a centrifuge, centrifuging for 5min at the rotating speed of 4000rpm, washing the solid for 2-3 times by using absolute ethyl alcohol, removing the upper-layer liquid, and storing the lower-layer precipitate, namely the silver nanowires in the absolute ethyl alcohol. Through detection, the yield of the prepared silver nanowires is 82.2%, the average length of the silver nanowires is 20 microns, and the proportion of the silver nanowires with the length of 15-25 microns in the product is 94%.
Example 5
An ethylene glycol solution of sodium chloride having a molar concentration of 37.5. mu. mol/L, an ethylene glycol solution of polyvinylpyrrolidone having a mass concentration of 6g/L (average molecular weight: 36000), and an ethylene glycol solution of silver nitrate having a mass concentration of 4g/L were prepared, respectively. 50mL of silver nitrate glycol solution is dripped into 50mL of ethylene glycol solution of vinyl pyrrolidone to prepare a first mixed solution, 1mL of sodium chloride glycol solution is dripped into the first mixed solution, and then the reaction is carried out for 8h at the temperature of 130 ℃. And placing the solid-liquid mixture obtained after the reaction in a centrifuge, centrifuging for 5min at the rotating speed of 4000rpm, washing the solid for 2-3 times by using absolute ethyl alcohol, removing the upper-layer liquid, and storing the lower-layer precipitate, namely the silver nanowires in the absolute ethyl alcohol. The detection shows that the yield of the prepared silver nanowires is 75.6%, the average length of the silver nanowires is 10 microns, and the proportion of the silver nanowires with the length of 5-5 microns in the product is 94%.
From the experimental results of examples 4 to 5, it can be seen that when the polyvinyl pyrrolidone having different average molecular weights is used, the length of the prepared silver nanowire is also significantly different, and the greater the average molecular weight of the polyvinyl pyrrolidone, the longer the length of the prepared silver nanowire is.
Comparative example 1
An ethylene glycol solution of sodium chloride having a molar concentration of 12.5. mu. mol/L, an ethylene glycol solution of potassium chloride having a molar concentration of 25. mu. mol/L, an ethylene glycol solution of polyvinylpyrrolidone having a mass concentration of 6g/L (average molecular weight of 1300000), and an ethylene glycol solution of silver nitrate having a mass concentration of 4g/L were prepared, respectively. 50mL of silver nitrate glycol solution is dripped into 50mL of vinyl pyrrolidone glycol solution to prepare a first mixed solution, 1mL of sodium chloride glycol solution and 1mL of potassium chloride glycol solution are dripped into the first mixed solution together, and then the mixture reacts for 8 hours at the temperature of 130 ℃. And placing the solid-liquid mixture obtained after the reaction in a centrifuge, centrifuging for 5min at the rotating speed of 4000rpm, washing the solid for 2-3 times by using absolute ethyl alcohol, removing the upper-layer liquid, and storing the lower-layer precipitate, namely the silver nanowires in the absolute ethyl alcohol. The detection shows that the yield of the prepared silver nanowires is 45.4%, the average length of the silver nanowires is 20 microns, and the proportion of the silver nanowires with the lengths of 25-35 microns in the product is 42%.
Comparative example 2
An ethylene glycol solution of copper chloride with a molar concentration of 12.5. mu. mol/L, an ethylene glycol solution of potassium chloride with a molar concentration of 12.5. mu. mol/L, an ethylene glycol solution of polyvinylpyrrolidone with a mass concentration of 6g/L (average molecular weight of 1300000), and an ethylene glycol solution of silver nitrate with a mass concentration of 4g/L were prepared, respectively. 50mL of silver nitrate glycol solution is dripped into 50mL of vinyl pyrrolidone glycol solution to prepare a first mixed solution, 1mL of copper chloride glycol solution and 1mL of potassium chloride glycol solution are dripped into the first mixed solution together, and then the reaction is carried out for 8 hours at the temperature of 130 ℃. And placing the solid-liquid mixture obtained after the reaction in a centrifuge, centrifuging for 5min at the rotating speed of 4000rpm, washing the solid for 2-3 times by using absolute ethyl alcohol, removing the upper-layer liquid, and storing the lower-layer precipitate, namely the silver nanowires in the absolute ethyl alcohol. The detection shows that the yield of the prepared silver nanowires is 51.0%, the average length of the silver nanowires is 20 microns, and the proportion of the silver nanowires with the length of 25-35 microns in the product is 38%.
As can be seen from examples 1 to 5 and comparative examples 1 and 2, when the metal chloride used is ferric chloride, cupric chloride or sodium chloride, the prepared silver nanowires have uniform length and high yield; and when the metal chloride contains potassium chloride, the uniformity of the length of the prepared silver nanowire is seriously influenced. The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A preparation method of silver nanowires is characterized by comprising the following steps:
providing a polyol solution of a metal chloride;
providing a polyol solution of an organic protectant;
providing a polyol solution of a silver precursor;
mixing the polyalcohol solution of the silver precursor with the polyalcohol solution of the organic protective agent to obtain a first mixed solution;
mixing the polyalcohol solution of the metal chloride with the first mixed solution to prepare a second mixed solution;
and (3) reacting the second mixed solution at the temperature of 110-150 ℃ for 6-10 h to prepare a solid-liquid mixture, and separating the solid-liquid mixture to remove the upper solution to prepare the silver nanowire.
2. The method for preparing silver nanowires of claim 1, wherein the polyol solution of the silver precursor and the polyol solution of the organic protective agent are mixed by dropping the polyol solution of the silver precursor into the polyol solution of the organic protective agent; the mixing mode of the polyol solution of the metal chloride and the first mixed solution is that the polyol solution of the metal chloride is dripped into the first mixed solution.
3. The method of preparing silver nanowires of claim 1, wherein the metal chloride comprises any one of ferric chloride, cupric chloride and sodium chloride, the organic protective agent is polyvinylpyrrolidone, the silver precursor is silver nitrate or silver acetate, and the polyol is selected from ethylene glycol or glycerol.
4. The method of preparing silver nanowires of any one of claims 1 to 3, wherein the molar concentration of the polyol solution of the metal chloride is 5 to 55 μmol/L.
5. The method for preparing silver nanowires of claim 4, wherein when the metal chloride is ferric chloride, the molar concentration of the polyol solution of the metal chloride is 5 to 35 μmol/L; when the metal chloride is copper chloride, the molar concentration of the polyalcohol solution of the metal chloride is 9-51 mu mol/L; when the metal chloride is sodium chloride, the molar concentration of the polyalcohol solution of the metal chloride is 30-37.5 mu mol/L.
6. The method for preparing silver nanowires of claim 5, wherein the mass concentration of the polyol solution of the organic protective agent is 2g/L to 10 g/L; the mass concentration of the polyalcohol solution of the silver precursor is 2 g/L-10 g/L.
7. The method for preparing silver nanowires of claim 6, wherein the mass ratio of the organic protective agent to the silver precursor in the first mixed solution is 1:3 to 3: 1.
8. The method for producing silver nanowires according to claim 7, wherein a volume ratio of the polyol solution of the metal chloride to the first mixed solution is 1: 100.
9. A silver nanowire prepared by the method according to any one of claims 1 to 8.
10. The silver nanowires of claim 9, wherein the silver nanowires have an average length of 30 μm to 120 μm.
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