CN109663905B - Preparation method of core-shell silver nanowire based on conductive polymer - Google Patents
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Abstract
The invention relates to the technical field of flexible electronic materials, and particularly discloses a preparation method of a core-shell silver nanowire based on a conductive polymer. The method comprises the following steps: preparing a conductive polymer nanowire and depositing a nano-silver shell layer on the surface of the conductive polymer nanowire; preparing a conductive polymer nanowire precursor solution and a nano-silver precursor solution, and initiating the reaction of monomers in the conductive polymer nanowire precursor solution by adopting an electrochemical polymerization method to convert the monomers into a conductive polymer nanowire; in the nano-silver precursor liquid, the nano-silver is deposited on the conducting polymer nanowire by an electrochemical reduction method, and finally the core-shell silver nanowire is formed. The cost of the conductive polymer is very low, and the silver amount required by the core-shell silver nanowire is much lower than that of the traditional silver nanowire, so that the flexible transparent electrode with low cost can be obtained.
Description
Technical Field
The invention relates to the technical field of flexible electronic materials, in particular to a preparation method of core-shell silver nanowires based on a conductive polymer.
Background
When the traditional method is used for preparing the silver nanowire flexible transparent electrode, the biggest problem is that: silver is used as a noble metal, the cost per se is high, the material cost required for forming a unit silver nanowire is higher, and the large-area application of the flexible transparent electrode in flexible electronics is further limited.
According to the reports of the IDTechex corporation, flexible electronic devices will be sold in the market for approximately $ 500 billion in 2021. In 2017 only, the NanoMarket company predicted that the flexible transparent electrodes needed for only high-end applications were more than 5 hundred million square meters, the market value would be as high as $ 76 million, and the annual growth rate was 45%. Therefore, the market value of the high-quality flexible transparent electrode is very huge. Flexible transparent electrodes, which play a key role in flexible electronic devices, have the characteristics of transparency, conductivity, bending resistance, light weight, and the like. At present, indium tin oxide is still used as the most mature transparent electrode and widely applied to traditional electronic devices, but because the content of indium element in earth crust is low, the indium tin oxide is brittle and the preparation process is complex, the application requirement of flexible electronics is difficult to meet. Among potential alternatives to indium tin oxide, flexible transparent electrodes of silver nanowires have the most practical application potential. However, silver is a precious metal, and the cost of the nano-wire is higher, which limits the large-area application of the silver nano-wire flexible transparent electrode in flexible electronics. Therefore, there is a necessary trend to reduce the material cost per unit silver nanowire. The chinese patent application No. 201610028723.1 discloses a method for preparing a copper/silver core-shell structured nanowire, which comprises synthesizing a copper nanowire based on a system of ethylenediamine, copper nitrate and sodium hydroxide; by utilizing the reduction and replacement action of copper on silver ions, a dense silver layer is wrapped on the copper nanowire shell to form a core-shell structure, so that the core-shell structure is used for replacing the silver nanowires applied to the flexible transparent electrode. The chinese patent application No. 201580038664.X discloses a chemical method of synthesizing copper nanowires by using piperazine or hexamethylenediamine, then coating silver on the surface by using a chemical plating method, and obtaining a flexible transparent electrode with good conductivity and light transmittance by coating.
However, the copper/silver core-shell nanowires using flexible transparent electrodes still have the following problems: although copper is a non-noble metal and is relatively lower in cost than silver, its absolute cost is still high. Therefore, the copper/silver core-shell nanowire still cannot fundamentally solve the problem of high cost of the flexible transparent electrode.
Disclosure of Invention
In view of the above, there is a need to provide a method for preparing core-shell silver nanowires based on conductive polymers. The invention wraps a thin silver shell layer on the surface of the prepared conductive polymer nanowire to form the core-shell silver nanowire, and the cost of the conductive polymer is very low, and the silver amount required by the core-shell silver nanowire is much lower than that of the traditional silver nanowire, so that the material cost of the unit nanowire can be greatly reduced, and the flexible transparent electrode with low cost can be obtained.
In order to achieve the purpose, the invention adopts the following technical scheme:
the preparation method of the core-shell silver nanowire based on the conductive polymer comprises the following steps: preparing a conductive polymer nanowire and depositing a nano-silver shell layer on the surface of the conductive polymer nanowire; the method comprises the following specific steps:
s1, stirring and dissolving a conductive polymer monomer at room temperature into a phosphate buffer solution to obtain a conductive polymer monomer solution of 0.05-0.4 mol/L, and adding a dopant with a molar concentration of 5-40 mmol/L to form a conductive polymer nanowire precursor solution;
s2, stirring and mixing silver salt and sodium salt at room temperature to prepare a mixed aqueous solution with the molar concentration of silver salt being 1-10 mmol/L and the molar concentration of sodium salt being 0.1-0.7 mol/L, and adding a polymer stabilizer according to the mass concentration of 2-16 g/L to form nano-silver precursor liquid;
s3), transferring the conductive polymer nanowire precursor liquid obtained in the step S1) into an electrochemical cell, forming a three-electrode system of a working electrode, a counter electrode (the counter electrode is a metal sheet, such as a copper sheet, a platinum sheet or a silver sheet) and a reference electrode (the reference electrode can be a saturated calomel electrode, a silver/silver chloride electrode or a mercury/mercurous sulfate electrode) by taking a metal substrate as the working electrode, initiating a conductive polymer monomer reaction by adopting an electrochemical polymerization method, and centrifugally washing the formed conductive polymer nanowire for multiple times by using water;
s4, transferring the conductive polymer nanowire obtained in the step S3) to the nano-silver precursor liquid obtained in the step S2), standing and soaking for 0.5-2 h, and depositing nano-silver on the surface of the conductive polymer nanowire in situ by adopting an electrochemical reduction method in the three-electrode system of the step S3) to form the core-shell silver nanowire with the nano-silver layer wrapping the conductive polymer nanowire.
Further, the conductive polymer monomer in step S1) is one of pyrrole, aniline, and ethylenedioxythiophene.
Further, the concentration of the phosphate buffer solution in the step S1) is 0.1-1 mol/L, and the pH value is 6.5-8.0.
Further, the dopant in step S1) is one of naphthalene sulfonic acid, camphor sulfonic acid, and poly-p-styrene sulfonic acid.
Further, the silver salt in step S2) is one of silver sulfate, silver nitrate and silver carbonate.
Further, the sodium salt in step S2) is one of sodium chloride, sodium nitrate and sodium sulfate.
Further, the polymer stabilizer in step S2) is one of polyvinylpyrrolidone, polyethylene glycol, chitosan, and dextran.
Further, the metal substrate in step S3) is one of stainless steel, titanium and platinum.
Further, the electrochemical polymerization method in the step S3) is a constant current method or a constant voltage method; the working parameter of the constant current method is 0.3-1.5 mA, and the constant current method lasts for 5-30 min; the working parameter of the constant pressure method is 0.7-2.0V and lasts for 5-30 min.
Further, the electrochemical reduction method in the step S4) is a constant current method or a constant voltage method; the working parameter of the constant current method is 0.2-1.0 mA, and the deposition time is 2-9 min; the working parameter of the constant pressure method is-1.5 to-3.2V deposition for 2 to 9 min.
The invention has the beneficial effects that:
the invention firstly prepares the conductive polymer nanowire precursor liquid and the nano-silver precursor liquid. Initiating the reaction of monomers in the precursor liquid of the conducting polymer nanowire by adopting an electrochemical polymerization method to convert the monomers into the conducting polymer nanowire; in the nano-silver precursor liquid, the nano-silver is deposited on the conducting polymer nanowire by an electrochemical reduction method, and finally the core-shell silver nanowire is formed.
The electrochemical reduction method of the invention deposits the nano silver on the surface of the conductive polymer nanowire in situ, and compared with other methods, the electrochemical method has higher controllability and greenness in the formation of the nano material.
The cost of the conductive polymer is very low, and the silver amount required by the core-shell silver nanowire is much lower than that of the traditional silver nanowire, so that the material cost of the unit nanowire can be greatly reduced, and the flexible transparent electrode with low cost can be obtained.
The invention further controls the electrochemical process parameters to ensure the integrity and the density of the nano silver shell layer.
Drawings
FIG. 1 is a scanning electron microscope image of polypyrrole nanowires;
fig. 2 is a scanning electron microscope image of core-shell silver nanowires.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions of the present invention will be further clearly and completely described below with reference to the embodiments of the present invention. It should be noted that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Dissolving pyrrole in phosphate buffer solution with the molar concentration of 0.2mol/L, PH of 7.4 by stirring at room temperature to form pyrrole solution with the molar concentration of 0.1mol/L, and then adding naphthalene sulfonic acid to ensure that the molar concentration of the naphthalene sulfonic acid in the solution is 10mmol/L to form conductive polymer nanowire precursor liquid; stirring and mixing silver nitrate and sodium nitrate at room temperature to prepare a mixed aqueous solution with the molar concentration of the silver nitrate being 3mmol/L and the molar concentration of the sodium nitrate being 0.2mol/L, and adding polyvinylpyrrolidone according to the mass concentration of 2g/L to form nano-silver precursor liquid; transferring the conductive polymer nanowire precursor liquid into an electrochemical cell, forming a three-electrode system by taking a stainless steel sheet as a working electrode, a copper sheet as a counter electrode and a saturated calomel electrode as a reference electrode, and adopting a constant current method: 0.6mA, and after 10min, the formed polypyrrole nanowires (shown in figure 1) are washed three times by water centrifugation; and (3) transferring the obtained polypyrrole nanowires to a nano-silver precursor solution, standing and soaking for 1.5h, and then performing a constant current method in the same three-electrode system: and (3) carrying out 0.5mA electrodeposition for 5min to deposit nano silver on the surface of the polypyrrole nanowire in situ, and preparing the core-shell silver nanowire (shown in figure 2) with the nano silver layer wrapping the polypyrrole nanowire.
Example 2
Stirring and dissolving aniline at room temperature in a phosphate buffer solution with the concentration of 0.2mol/L, pH being 6.8 to form a 0.3mol/L mixed solution, and adding naphthalenesulfonic acid according to the concentration of 20mmol/L to form a conductive polymer nanowire precursor solution; stirring and mixing silver sulfate and sodium nitrate at room temperature to prepare a mixed aqueous solution with the molar concentration of silver sulfate being 6mmol/L and the molar concentration of sodium nitrate being 0.2mol/L, and adding polyvinylpyrrolidone according to the mass concentration of 2g/L to form nano-silver precursor liquid; transferring the conductive polymer nanowire precursor liquid into an electrochemical cell, taking a stainless steel sheet as a working electrode, a copper sheet as a counter electrode and a saturated calomel electrode as a reference electrode to form a three-electrode system, wherein the constant pressure method comprises the following steps: 1.0V, and after 15min, centrifugally washing the formed polyaniline nanowires for three times by using water; and (3) transferring the obtained polyaniline nanowires to a nano-silver precursor solution, standing and soaking for 1.5h, and then performing a constant current method in the same three-electrode system: and (3) depositing nano silver on the surface of the polyaniline nanowire in situ at 0.5mA for 5min to prepare the core-shell silver nanowire with the nano silver layer wrapping the polyaniline nanowire.
Example 3
Dissolving pyrrole in phosphate buffer solution with the concentration of 8.0 in 0.6mol/L, pH under stirring at room temperature to form 0.1mol/L mixed solution, and adding camphorsulfonic acid with the molar concentration of 10mmol/L to form conductive polymer nanowire precursor solution; stirring and mixing silver nitrate and sodium nitrate at room temperature to prepare a silver nitrate and sodium nitrate mixed aqueous solution with the molar concentration of 3mmol/L and 0.6mol/L respectively, and adding chitosan according to the mass concentration of 5g/L to form nano-silver precursor liquid; transferring the conductive polymer nanowire precursor liquid into an electrochemical cell, forming a three-electrode system by taking a titanium sheet as a working electrode, a copper sheet as a counter electrode and a saturated calomel electrode as a reference electrode, and adopting a constant-current method: centrifuging and washing the polypyrrole nanowires formed after 0.6mA lasts for 10min for three times by using water; and (3) transferring the obtained polypyrrole nanowires to a nano-silver precursor liquid, standing and soaking for 1.5h, and then in the same three-electrode system, performing a constant pressure method: and (3) depositing the nano silver on the surface of the polypyrrole nanowire in situ at-1.5V for 8min to prepare the core-shell silver nanowire with the nano silver layer wrapping the polypyrrole nanowire.
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 core-shell silver nanowires based on conductive polymers is characterized by comprising the following steps: preparing a conductive polymer nanowire and depositing a nano-silver shell layer on the surface of the conductive polymer nanowire; the method comprises the following specific steps:
s1, stirring and dissolving a conductive polymer monomer at room temperature into a phosphate buffer solution to obtain a conductive polymer monomer solution of 0.05-0.4 mol/L, and adding a dopant with a molar concentration of 5-40 mmol/L to form a conductive polymer nanowire precursor solution;
s2, stirring and mixing silver salt and sodium salt at room temperature to prepare a mixed aqueous solution with the molar concentration of silver salt being 1-10 mmol/L and the molar concentration of sodium salt being 0.1-0.7 mol/L, and adding a polymer stabilizer according to the mass concentration of 2-16 g/L to form nano-silver precursor liquid;
s3), transferring the conductive polymer nanowire precursor liquid obtained in the step S1) into an electrochemical cell, forming a three-electrode system of a working electrode, a counter electrode and a reference electrode by taking a metal substrate as the working electrode, initiating a conductive polymer monomer reaction by adopting an electrochemical polymerization method, and centrifugally washing the formed conductive polymer nanowire by using water;
s4, transferring the conductive polymer nanowire obtained in the step S3) to the nano-silver precursor liquid obtained in the step S2), standing and soaking for 0.5-2 h, and depositing nano-silver on the surface of the conductive polymer nanowire in situ by adopting an electrochemical reduction method in the three-electrode system of the step S3) to form the core-shell silver nanowire with the nano-silver layer wrapping the conductive polymer nanowire.
2. The method for preparing core-shell silver nanowires based on conductive polymers according to claim 1, wherein the conductive polymer monomer in step S1) is one of pyrrole, aniline, and ethylenedioxythiophene.
3. The method for preparing core-shell silver nanowires based on conductive polymers according to claim 1, wherein the concentration of the phosphate buffer solution in the step S1) is 0.1-1 mol/L, and the pH value is 6.5-8.0.
4. The method of preparing core-shell silver nanowires based on conductive polymers of claim 1, wherein the dopant of step S1) is one of naphthalene sulfonic acid, camphor sulfonic acid and poly-p-styrene sulfonic acid.
5. The method for preparing core-shell silver nanowires based on conductive polymers as claimed in claim 1, wherein the silver salt in step S2) is one of silver sulfate, silver nitrate and silver carbonate.
6. The method for preparing core-shell silver nanowires based on conductive polymers according to claim 1, wherein the sodium salt in step S2) is one of sodium chloride, sodium nitrate and sodium sulfate.
7. The method for preparing core-shell silver nanowires based on conductive polymers according to claim 1, wherein the polymer stabilizer in step S2) is one of polyvinylpyrrolidone, polyethylene glycol, chitosan and dextran.
8. The method for preparing core-shell silver nanowires based on conductive polymers according to claim 1, wherein the metal substrate in step S3) is one of stainless steel, titanium and platinum.
9. The method for preparing core-shell silver nanowires based on conductive polymers according to claim 1, wherein the electrochemical polymerization method in step S3) is a constant current method or a constant voltage method; the working parameter of the constant current method is 0.3-1.5 mA, and the constant current method lasts for 5-30 min; the working parameter of the constant pressure method is 0.7-2.0V and lasts for 5-30 min.
10. The method for preparing core-shell silver nanowires based on conductive polymers according to claim 1, wherein the electrochemical reduction method in step S4) is a constant current method or a constant voltage method; the working parameter of the constant current method is 0.2-1.0 mA, and the deposition time is 2-9 min; the working parameter of the constant pressure method is-1.5 to-3.2V deposition for 2 to 9 min.
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