CN113798505A - Silver nanowire containing lavender extract and preparation method and application thereof - Google Patents

Silver nanowire containing lavender extract and preparation method and application thereof Download PDF

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CN113798505A
CN113798505A CN202111014808.1A CN202111014808A CN113798505A CN 113798505 A CN113798505 A CN 113798505A CN 202111014808 A CN202111014808 A CN 202111014808A CN 113798505 A CN113798505 A CN 113798505A
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lavender extract
lavender
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extract
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王立惠
吴迎港
耿小红
吴博竞
陈同祥
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Zhongshuo Industry Shanghai Co ltd
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Abstract

The invention provides silver nanowires containing lavender extract and a preparation method and application thereof. The silver nanowire containing the lavender extract is prepared from the following raw materials: lavender extract, copper salt and silver salt. According to the invention, the lavender extract is used as a reducing agent, so that the lavender extract can be used as a reducing agent in the reaction synthesis process, the introduction of organic alcohol in a polyol synthesis method is avoided, most of compounds in the lavender plant extract are saponin and glycoside compounds, the lavender plant extract can serve as a surfactant to guide the interaction of Cu (II) and intermolecular sugar, the silver surface is passivated, the growth of a one-dimensional silver nanostructure is supported, and the silver nanowire with high length, diameter and good conductivity is synthesized. In addition, the copper ions avoid the dissolution of twin seeds caused by oxidation etching by removing oxygen on the surfaces of the twin seeds, promote the growth of multi-twin seeds, facilitate the formation of silver nanowires and improve the synthesis yield.

Description

Silver nanowire containing lavender extract and preparation method and application thereof
Technical Field
The invention belongs to the technical field of photoelectrons, and particularly relates to a silver nanowire containing a lavender extract, a preparation method and an application thereof, in particular to a silver nanowire containing a lavender extract, which is prepared from the lavender extract, and a preparation method and an application thereof.
Background
With the development of the times and the progress of science and technology, people have higher and higher requirements on future electronic products. Future electronic products may be bent, stretched, compressed, twisted and deformed into complex non-planar shapes. At the same time, they must also maintain good performance. The core component of electronic products such as touch screens, liquid crystal displays, organic light-emitting diodes, solar cells and the like is a transparent electrode.
Currently, the most widely used and most demanded transparent electrode material in the global electronic industry is Indium Tin Oxide (ITO). The ITO has good light transmittance, low thickness, easy etching into an electrode pattern, high hardness and wear resistance. Meanwhile, the method also has the defects that the cost is high, the method is not beneficial to producing the bent screen, the toxicity is not beneficial to environmental protection and the like. Therefore, ITO is gradually being replaced by next-generation flexible transparent materials such as Carbon Nanotubes (CNTs), graphene, and metal nanowires. Among the candidate materials, the metal nanowires, especially the silver nanowires containing the lavender extract, have the advantages of good conductivity, good light transmittance, excellent bending property, low cost, good stability, no moire and the like compared with materials such as ITO, metal grids, carbon nanotubes, conductive polymers, graphene and the like, and all indexes are all totipotent.
CN104616833A discloses a method for preparing a silver nanowire transparent electrode containing a lavender extract in a large area and the silver nanowire transparent electrode containing the lavender extract, a proper amount of silver nanowire solution containing the lavender extract is taken, a centrifuge is used for separating the silver nanowire containing the lavender extract and a solvent, after the solvent is removed, the silver nanowire containing the lavender extract at the bottom is doped into photoresist, and the photoresist is vibrated until the silver nanowire containing the lavender extract is uniformly dispersed therein to form silver nanowire-photoresist suspension containing the lavender extract; uniformly spin-coating the suspension on a clean transparent substrate to form a silver nanowire-photoresist film containing lavender extract; immersing the transparent substrate coated with the silver nanowire-photoresist film containing the lavender extract into a photoresist removing solution to remove the surface photoresist; and taking out the transparent substrate, and after the surface solution is volatilized, leaving the silver nanowires containing the lavender extract on the transparent substrate to form a uniform silver nanowire network containing the lavender extract, namely the silver nanowire transparent electrode containing the lavender extract.
CN110128883A discloses a conductive ink of a silver nanowire film containing a lavender extract with an ultra-low haze, a preparation method and an application thereof, wherein the conductive ink prepared by the preparation method is used for manufacturing the silver nanowire film containing the lavender extract with the ultra-low haze, the diameter of the silver nanowire containing the lavender extract obtained by the preparation method is 20 nanometers, and the length-diameter ratio of the silver nanowire is 1000; the optical transmittance of the film made of the conductive ink is higher than 95%, and the haze is lower than 0.5%.
CN112893862A discloses a silver nanowire containing lavender extract, a preparation method thereof and a conductive film prepared from the silver nanowire containing lavender extract, wherein the preparation method of the silver nanowire containing lavender extract comprises (1) preparing PVP polyalcohol solution, halide salt polyalcohol solution and silver nitrate polyalcohol solution respectively; (2) adding a part of prepared silver nitrate polyalcohol solution into a halide salt polyalcohol solution to react to prepare seed solution; (3) uniformly mixing the rest silver nitrate polyalcohol solution and PVP polyalcohol solution, dropwise adding the mixture into the seed solution for reaction, and standing for reaction after dropwise adding is finished to obtain silver nanowires containing lavender extract; and step four, washing the silver nanowires containing the lavender extract obtained in the step three, and then fixing the volume and dispersing the silver nanowires in a solvent.
The method for synthesizing silver nanowires containing lavender extract mainly comprises a solvothermal method, a wet chemical synthesis method, an environmental solution phase method, a polyol synthesis method, a hydrothermal method, an ultraviolet irradiation method, a template method, a seed crystal method and the like. The polyol process is currently the most commonly used process. The method has high requirements on reaction conditions, and simultaneously, chemical reagents such as ethylene glycol, PVP and the like which are easy to pollute the environment are inevitably introduced.
Therefore, the synthesis of silver nanowires containing lavender extract under mild conditions by using abundant green biomass resources and without adding other chemical reagents becomes one of the directions for which researchers are urgently in need of breakthrough.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide silver nanowires containing lavender extract, and a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides silver nanowires containing lavender extract, wherein the silver nanowires containing lavender extract are prepared from the following raw materials: lavender extract, copper salt and silver salt.
In the invention, the lavender extract is used as a reducing agent, the main components in the lavender plant extract are compounds such as kaempferol and ferulic acid, and the polyphenol compounds and flavonoid substances have good reducibility and can serve as the reducing agent in the reaction synthesis process, so that the introduction of organic alcohol in a polyol synthesis method is avoided. And most of compounds in the lavender plant extract are saponin and glucoside compounds, can serve as a surfactant to guide the interaction of Cu (II) and intermolecular sugar, passivate a silver surface, support the growth of a one-dimensional silver nanostructure, avoid using PVP (polyvinyl pyrrolidone) which is difficult to remove, and synthesize the silver nanowire with high length, diameter and good conductivity. And the Cu (II) avoids the dissolution of twin seeds caused by oxidation etching by removing oxygen on the surfaces of the twin seeds, promotes the growth of multi-twin seeds, is beneficial to forming silver nanowires and improves the synthesis yield.
Preferably, the lavender extract accounts for 5-15% of the total mass of the silver nanowires containing the lavender extract, and may be, for example, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, and the like.
Preferably, the molar ratio of the silver salt to the copper salt is 1 (0.5-3), and may be, for example, 1:0.5, 1:0.6, 1:0.8, 1:1, 1:1.2, 1:1.5, 1:1.7, 1:2, 1:2.2, 1:1.2.5, 1:2.8, 1:3, and the like. .
Preferably, the copper salt comprises any one of copper sulfate, basic copper carbonate, copper nitrate or copper chloride or a combination of at least two of them, preferably copper sulfate.
Preferably, the silver salt comprises any one or a combination of at least two of silver nitrate, silver sulfate, silver phosphate or silver chloride, preferably silver nitrate.
Preferably, the length of the silver nanowire containing lavender extract is 30-100 μm, such as 30 μm, 35 μm, 40 μm, 45 μm, 50 μm, 55 μm, 60 μm, 65 μm, 70 μm, 75 μm, 80 μm, 85 μm, 90 μm, 95 μm, 100 μm and the like, and the diameter of the silver nanowire containing lavender extract is 30-130nm, such as 30nm, 35nm, 40nm, 45nm, 50nm, 55nm, 60nm, 65nm, 70nm, 75nm, 80nm, 85nm, 90nm, 95nm, 100nm, 105nm, 110nm, 115nm, 120nm, 125nm, 130nm and the like.
In a second aspect, the present invention provides a method for preparing silver nanowires containing lavender extract according to the first aspect, the method comprising the following steps:
(1) dissolving lavender extract, copper salt and silver salt respectively to obtain lavender extracting solution, copper salt solution and silver salt solution;
(2) mixing the lavender extract obtained in the step (1) with a copper salt solution, stirring for the first time, then dropwise adding a silver salt solution, and stirring for the second time to obtain a mixed solution;
(3) and (3) heating the mixed solution obtained in the step (2) for reaction to obtain the silver nanowires containing the lavender extract.
In the invention, in the whole process of synthesizing the silver nanowires containing the lavender extract by using the lavender extract, no chemical reagent which pollutes the environment such as ethylene glycol is used as a solvent, but water is used as the solvent, so that the product does not have the residue of the chemical reagent, and the purity of the silver nanowires containing the lavender extract is ensured.
Preferably, in step (1), the dissolving solvent is water.
Preferably, in step (1), the concentration of the lavender extract is 0.01-0.04g/mL, for example, 0.01g/mL, 0.015g/mL, 0.02g/mL, 0.025g/mL, 0.03g/mL, 0.035g/mL, 0.04g/mL, or the like.
Preferably, in step (1), the concentration of the copper salt solution is 8 to 12mmol/L, and may be, for example, 8mmol/L, 8.5mmol/L, 9mmol/L, 9.5mmol/L, 10mmol/L, 10.5mmol/L, 11mmol/L, 11.5mmol/L, 12mmol/L, or the like.
Preferably, in step (1), the concentration of the silver salt solution is 0.5 to 10mmol/L, and may be, for example, 0.5mmol/L, 1mmol/L, 2mmol/L, 3mmol/L, 4mmol/L, 5mmol/L, 6mmol/L, 7mmol/L, 8mmol/L, 9mmol/L, 10mmol/L or the like.
Preferably, the volume ratio of the lavender extract to the copper salt solution to the silver salt solution is (11-44): (33-66);
wherein, the first "11-44" can be, for example, 11, 15, 20, 25, 30, 35, 40, 44, etc.;
wherein, the second "11-44" can be, for example, 11, 15, 20, 25, 30, 35, 40, 44, etc.;
the "33 to 66" may be 33, 40, 45, 50, 55, 60, 66, etc., for example.
Preferably, in the step (2), the temperature of the primary stirring is 25-30 ℃, for example, 25 ℃, 26 ℃, 27 ℃, 28 ℃, 29 ℃, 30 ℃ and the like, the time of the primary stirring is 8-12h, for example, 8h, 8.5h, 9h, 9.5h, 10h, 10.5h, 11h, 11.5h, 12h and the like, and the rotation speed of the primary stirring is 600-800rpm, for example, 600rpm, 650rpm, 700rpm, 750rpm, 800rpm and the like.
Preferably, in step (2), the dropping rate of the silver salt solution is 0.3-0.8mL/min, and may be, for example, 0.3mL/min, 0.4mL/min, 0.5mL/min, 0.6mL/min, 0.7mL/min, 0.8mL/min, or the like.
Preferably, in the step (2), the temperature of the secondary stirring is 25-30 ℃, for example, 25 ℃, 26 ℃, 27 ℃, 28 ℃, 29 ℃, 30 ℃ and the like, the time of the secondary stirring is 2-4h, for example, 2h, 2.5h, 3h, 3.5h, 4h and the like, and the rotation speed of the secondary stirring is 350-550rpm, for example, 350rpm, 400rpm, 450rpm, 500rpm, 550rpm and the like.
Preferably, in the step (3), the temperature of the heating reaction is 40-60 ℃, for example, 40 ℃, 45 ℃, 50 ℃, 55 ℃, 60 ℃ and the like, and the time of the heating reaction is 36-72h, for example, 36h, 40h, 45h, 50h, 55h, 60h, 65h, 70h, 72h and the like.
Preferably, in step (3), after the heating reaction is finished, post-treatment is further performed: the reaction solution is centrifuged with acetone and/or ethanol, and the product is dispersed and stored.
Preferably, in step (3), the rotation speed of the centrifugation is 10000-15000rpm, such as 10000rpm, 11000rpm, 12000rpm, 13000rpm, 14000rpm, 15000rpm and the like, and the time of the centrifugation is 5-30min, such as 5min, 6min, 8min, 10min, 12min, 14min, 16min, 18min, 20min, 22min, 24min, 26min, 28min, 30min and the like.
Preferably, the preparation method of the silver nanowires containing the lavender extract comprises the following steps:
(1) dissolving lavender extract, copper salt and silver salt with water respectively to obtain 0.01-0.04g/mL lavender extract, 8-12mmol/L copper salt solution and 0.5-10mmol/L silver salt solution;
(2) mixing the lavender extract obtained in the step (1) with a copper salt solution, stirring for the first time, then dropwise adding a silver salt solution at a rate of 0.3-0.8mL/min, and stirring for the second time to obtain a mixed solution;
wherein the volume ratio of the lavender extracting solution to the copper salt solution to the silver salt solution is (11-44): (33-66);
(3) heating the mixed solution obtained in the step (2) in a water bath to 40-60 ℃, reacting for 36-72h, centrifuging the reaction solution with acetone and/or ethanol after the reaction is finished, and dispersing and storing the product to obtain the silver nanowire containing the lavender extract.
In a third aspect, the present invention provides a use of the silver nanowires containing lavender extract according to the first aspect in the preparation of a transparent electrode.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the invention, the lavender extract is introduced into the preparation raw material of the silver nanowires containing the lavender extract, the main components in the lavender plant extract are compounds such as kaempferol and ferulic acid, and the polyphenol compounds and flavonoid substances have good reducibility, can serve as reducing agents in the reaction synthesis process, avoid the introduction of organic alcohol in a polyol synthesis method, and are more green and environment-friendly;
(2) most of compounds in the lavender plant extract are saponin and glucoside compounds, can serve as a surfactant to guide the interaction of Cu (II) and intermolecular sugar, passivate a silver surface, support the growth of a one-dimensional silver nanostructure, avoid using PVP (polyvinyl pyrrolidone) which is difficult to remove, and synthesize silver nanowires with high length, diameter and good conductivity;
(3) according to the invention, copper salt is introduced in the preparation process, and the Cu (II) removes oxygen on the surface of the twin crystal seeds, so that the twin crystal seeds are prevented from being dissolved due to oxidation etching, the growth of multiple twin crystal seeds is promoted, the formation of silver nanowires is facilitated, and the synthesis yield is improved.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The present embodiment provides silver nanowires containing lavender extract, which are prepared by the following preparation method:
(1) adding 2g of lavender extract dry powder into 100mL of deionized water, magnetically stirring at 60 ℃ until the lavender extract dry powder is completely dissolved, cooling to room temperature, and filtering to obtain 20g/L of lavender plant extract; respectively weighing a certain amount of AgNO3And CuSO4·5H2Dissolving O in deionized water, and magnetically stirring until the O is completely dissolved to obtain AgNO with concentration of 5mmol/L3Solution and CuSO with concentration of 10mmol/L4·5H2O solution;
(2) mixing Lavender plant extractive solution and CuSO4·5H2Mixing the O solution, magnetically stirring at the rotation speed of 700rpm at 25 ℃ for 10h, and then dropwise adding AgNO at 0.35mL/min3Stirring the solution at the same time at the temperature of 25 ℃ and the rotating speed of 450rpm for 2 hours to obtain a mixed solution;
wherein, 25 vol% of lavender plant extract and CuSO4·5H2Deionized water solution of O25 vol%, AgNO350 vol% of deionized water solution;
(3) heating the mixed solution in water bath to 50 ℃, and reacting for 72 hours; and centrifuging the silver nanowire stock solution twice at 12000rpm by using acetone and ethanol respectively, wherein each time is 5min, and dispersing the product in absolute ethyl alcohol for storage to obtain the silver nanowire with the length of 80-100 mu m and the diameter of 30-50 nm.
Example 2
The present embodiment provides silver nanowires containing lavender extract, which are prepared by the following preparation method:
(1) adding 2.5g of lavender extract dry powder into 100mL of deionized water, magnetically stirring at 60 ℃ until the lavender extract dry powder is completely dissolved, cooling to room temperature, and filtering to obtain 25g/L of lavender plant extract; respectively weighing a certain amount of AgNO3And CuSO4·5H2Dissolving O in deionized water, and magnetically stirring until the O is completely dissolved to obtain AgNO with the concentration of 3mmol/L3Solution and CuSO with concentration of 10mmol/L4·5H2O solution;
(2) mixing Lavender plant extractive solution and CuSO4·5H2Mixing the O solution, magnetically stirring at 650rpm at 30 deg.C for 12h, and adding AgNO dropwise at 0.5mL/min3Stirring the solution at the same time at the temperature of 30 ℃ for 4 hours at the rotating speed of 500rpm to obtain a mixed solution;
wherein, 25 vol% of lavender plant extract and CuSO4·5H2Deionized water solution of O25 vol%, AgNO350 vol% of deionized water solution;
(3) heating the mixed solution in water bath to 40 ℃, and reacting for 72 hours; and centrifuging the silver nanowire stock solution twice at 12000rpm by using acetone and ethanol respectively, wherein each time is 5min, and dispersing the product in absolute ethanol for storage to obtain the silver nanowires with the length of 40-60 mu m and the diameter of 100-130 nm.
Example 3
The present embodiment provides silver nanowires containing lavender extract, which are prepared by the following preparation method:
(1) adding 1g of lavender extract dry powder into 100mL of deionized water, magnetically stirring at 60 ℃ until the lavender extract dry powder is completely dissolved, cooling to room temperature, and filtering to obtain 10g/L of lavender plant extract; respectively weighing a certain amount of AgNO3And CuSO4·5H2Dissolving O in deionized water, and magnetically stirring until the O is completely dissolved to obtain AgNO with the concentration of 7mmol/L3Solution and CuSO with concentration of 10mmol/L4·5H2O solution;
(2) mixing Lavender plant extractive solution and CuSO4·5H2Mixing the O solution, magnetically stirring at the rotation speed of 600rpm for 12h at 25 ℃, then dropwise adding a silver nitrate solution at 0.4mL/min, and simultaneously stirring at the rotation speed of 400rpm for 2h at 25 ℃ to obtain a mixed solution;
wherein, the lavender plant extract is 11 vol%, and CuSO4·5H2Deionized water solution of O23 vol%, AgNO366 vol% of deionized water;
(3) heating the mixed solution in water bath to 60 ℃, and reacting for 48 hours; and centrifuging the silver nanowire stock solution twice at 12000rpm by using acetone and ethanol respectively, wherein each time is 5min, and dispersing the product in absolute ethanol for storage to obtain the silver nanowires with the length of 30-40 mu m and the diameter of 80-100 nm.
Example 4
The present embodiment provides silver nanowires containing lavender extract, which are prepared by the following preparation method:
(1) adding 4g of lavender extract dry powder into 100mL of deionized water, magnetically stirring at 60 ℃ until the lavender extract dry powder is completely dissolved, cooling to room temperature, and filtering to obtain 40g/L of lavender plant extract; respectively weighing a certain amount of AgNO3And CuSO4·5H2Dissolving O in deionized water, and magnetically stirring until the O is completely dissolved to obtain AgNO with concentration of 10mmol/L3Solution and CuSO with concentration of 10mmol/L4·5H2O solution;
(2) mixing Lavender plant extractive solution and CuSO4·5H2Mixing the O solution, magnetically stirring at the rotation speed of 700rpm at 25 ℃ for 12h, and then dropwise adding AgNO at 0.55mL/min3Stirring the solution at the rotation speed of 450rpm for 3 hours at the temperature of 25 ℃ to obtain a mixed solution;
wherein, the lavender plant extract is 23 vol%, and the CuSO is4·5H2Deionized water solution of O11 vol%, AgNO366 vol% of deionized water;
(3) heating the mixed solution in a water bath to 60 ℃, reacting for 72 hours, centrifuging the silver nanowire stock solution twice at 12000rpm by using acetone and ethanol respectively, 5min each time, and dispersing the product in absolute ethyl alcohol for storage to obtain the silver nanowires with the length of 50-70 mu m and the diameter of 60-80 nm.
Example 5
The present embodiment provides silver nanowires containing lavender extract, which are prepared by the following preparation method:
(1) adding 1.5g Lavender extract dry powder into 100mL deionized water, magnetically stirring at 60 deg.C until completely dissolved, cooling to room temperature, and filtering to obtain 15g/L Lavender plantExtracting solution; respectively weighing a certain amount of AgNO3And CuSO4·5H2Dissolving O in deionized water, and magnetically stirring until the O is completely dissolved to obtain AgNO with concentration of 8mmol/L3Solution and CuSO with concentration of 10mmol/L4·5H2O solution;
(2) mixing Lavender plant extractive solution and CuSO4·5H2Mixing the O solution, magnetically stirring at 650rpm at 28 deg.C for 9h, and adding AgNO dropwise at 0.8mL/min3Stirring the solution at the same time at the rotation speed of 500rpm for 4 hours at the temperature of 28 ℃ to obtain a mixed solution;
wherein, the lavender plant extract is 23 vol%, and the CuSO is4·5H2Deionized water solution of O44 vol%, AgNO333 vol% of deionized water;
(3) heating the mixed solution in a water bath to 60 ℃, reacting for 36h, centrifuging the silver nanowire stock solution twice at 12000rpm by using acetone and ethanol respectively, 5min each time, and dispersing the product in absolute ethyl alcohol for storage to obtain the silver nanowires with the length of 30-40 mu m and the diameter of 110-130 nm.
Example 6
This example provides silver nanowires containing lavender extract, which are different from example 1 only in that CuSO is added4·5H2Replacement of O by Cu (CH)3COO)2·H2O, the other steps are the same as in example 1.
Example 7
This example provides silver nanowires containing lavender extract, which are different from example 1 only in that silver nitrate is replaced with silver chloride, and the other steps are the same as example 1.
Example 8
This example provides silver nanowires containing lavender extract, which is different from example 1 only in that, in step (1), the concentration of the copper salt solution is 8 mmol/L.
Example 9
This example provides silver nanowires containing lavender extract, which is different from example 1 only in that, in step (1), the concentration of the copper salt solution is 12 mmol/L.
Example 10
This example provides silver nanowires containing lavender extract, which is different from example 1 only in that, in the step (2), the dropping speed is 0.2 mL/min.
Example 11
This example provides silver nanowires containing lavender extract, which are different from example 1 only in that, in step (2), the dropping rate is 0.9 mL/min.
Example 12
This example provides silver nanowires containing lavender extract, which is different from example 1 only in that, in step (3), the reaction is carried out at 35 ℃ for 80 hours.
Example 13
This example provides silver nanowires containing lavender extract, which is different from example 1 only in that, in step (3), the reaction is carried out at 65 ℃ for 30 hours.
Comparative example 1
The present comparative example provides a method for preparing a silver nanowire, the method specifically comprising the steps of:
(1) respectively weighing a certain amount of AgNO3And CuSO4·5H2Dissolving O in deionized water, and magnetically stirring until the O is completely dissolved to obtain AgNO with concentration of 5mmol/L3Solution and CuSO with concentration of 10mmol/L4·5H2O solution;
(2) mixing AgNO3Solution and CuSO4·5H2Mixing the O solution, and uniformly stirring to obtain a mixed solution;
wherein, AgNO3Solution 50 vol%, CuSO4·5H250 vol% of deionized water solution of O;
(3) heating the mixed solution in water bath to 50 ℃, and reacting for 72 hours; and centrifuging the silver nanowire stock solution twice at 12000rpm by using acetone and ethanol respectively, wherein each time is 5min, dispersing the product in absolute ethanol for storage, and obtaining the product without silver nanowires.
Comparative example 2
The present comparative example provides a method for preparing a silver nanowire, the method specifically comprising the steps of:
(1) adding 2g of lavender extract dry powder into 100mL of deionized water, magnetically stirring at 60 ℃ until the lavender extract dry powder is completely dissolved, cooling to room temperature, and filtering to obtain 20g/L of lavender plant extract; weighing a certain amount of AgNO3Dissolving in deionized water, and magnetically stirring until completely dissolving to obtain silver nitrate solution with concentration of 5 mmol/L;
(2) mixing Lavender plant extractive solution with AgNO3Mixing the solutions, and uniformly stirring to obtain a mixed solution;
wherein, 25 vol% of lavender plant extract and AgNO375 vol% of the solution;
(3) heating the mixed solution in water bath to 50 ℃, and reacting for 72 hours; and centrifuging the silver nanowire stock solution twice at 12000rpm by using acetone and ethanol respectively, wherein each time is 5min, and dispersing the product in absolute ethanol for storage to obtain the silver nanoparticles with the particle size of 80-100 nm.
Comparative example 3
This comparative example provides a method for preparing silver nanowires containing lavender extract, which is different from example 1 only in that the ethanol extract of lavender extract is replaced with 1mg/mL of 1-ethyl-3-methylimidazole chloride ethanol solution.
Performance testing
The following tests were carried out on the products shown in examples 1 to 13 and comparative examples 1 to 3, and the specific test methods were as follows:
(1) silver nano length, diameter and aspect ratio: scanning electron microscope (manufacturer: Nippon Hitachi, model: SU8020) was used;
(2) purity: scanning electron microscope (manufacturer: Nippon Hitachi, model: SU8020) was used;
(3) yield: the product silver wire is weighed after drying divided by the mass of silver nitrate times 108 divided by 169;
the specific test results are shown in table 1 below ("-" represents no nanowire formed):
TABLE 1
Figure BDA0003240033160000131
Figure BDA0003240033160000141
As shown in the test data in Table 1, the length of the silver nanowire containing the lavender extract is 30-100 μm, the diameter of the silver nanowire containing the lavender extract is 30-130nm, the length-diameter ratio is 200-3000, the purity is more than 90%, and the yield is more than 95%. Therefore, the method for synthesizing the silver nanowires containing the lavender extract by using the lavender extract is green and environment-friendly, low in cost and simple in process, and the uniform silver nanowires containing the lavender extract with high yield and high length-diameter ratio are prepared by using the lavender extract as a reducing agent and using an ethanol aqueous solution as a solvent and avoiding using ethylene glycol, PVP and other chemical reagents which are easy to pollute the environment.
It can be known from the comparison between example 1 and examples 6 and 7 that the copper salt is copper sulfate and the silver salt is silver nitrate, which can promote the growth of the one-dimensional nano structure and is more beneficial to the generation of longer silver nanowires.
As is clear from comparison between example 1 and examples 8 and 9, the alcohol solution of copper salt is too dilute or too concentrated, and thus it is impossible to generate more polytwinned seeds at the initial stage of the reaction, and the yield of silver nanowires is lowered, and by-products such as silver nanoparticles are generated more.
As is clear from comparison between example 1 and examples 10 and 11, the dropping speed is in the range of 0.3-0.8mL/min, and the obtained silver nanowires have a small and long diameter, i.e., a large aspect ratio, and cannot grow well even if the dropping speed is too fast or too slow.
As can be seen from the comparison between example 1 and examples 12 and 13, the heating reaction temperature is 40-60 ℃ and the heating reaction time is 36-72h, so that finer silver nanowires can be synthesized, otherwise, even if the temperature is reduced for a long time or the temperature is increased for a short time, uniform silver nanowires containing polyphenol compounds with high extension degree and high aspect ratio cannot be prepared.
As can be seen from the comparison of example 1 and comparative example 1, the reduction reaction could not be completed to prepare silver nanowires without adding lavender extract.
As is clear from the comparison between example 1 and comparative example 2, the product was silver nanoparticles having a large particle diameter (particle diameter of 80 to 100nm) without adding copper salt, and no silver nanowires were formed.
As can be seen from the comparison of example 1 and comparative example 3, the addition of other types of reducing agents failed to perform the reaction at a lower temperature, and no silver nanowires were generated.
The applicant states that the silver nanowires containing lavender extract, the preparation method and the application thereof are illustrated by the above examples, but the invention is not limited to the above examples, that is, the invention is not limited to the above examples. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.

Claims (10)

1. The silver nanowire containing the lavender extract is characterized in that the silver nanowire containing the lavender extract is prepared from the following raw materials: lavender extract, copper salt and silver salt.
2. The silver nanowires containing lavender extract according to claim 1, wherein the lavender extract accounts for 5-15% of the total mass of the silver nanowires containing lavender extract;
preferably, the molar ratio of the silver salt to the copper salt is 1 (0.5-3).
3. The silver nanowires containing lavender extract according to claim 1 or 2, wherein the copper salt comprises any one of copper sulfate, basic copper carbonate, copper nitrate or copper chloride or a combination of at least two of them, preferably copper sulfate;
preferably, the silver salt comprises any one or a combination of at least two of silver nitrate, silver sulfate, silver phosphate or silver chloride, preferably silver nitrate.
4. The lavender extract-containing silver nanowires according to any one of claims 1 to 3, wherein the length of the lavender extract-containing silver nanowires is 30 to 100 μm, and the diameter of the lavender extract-containing silver nanowires is 30 to 130 nm.
5. The method for preparing lavender extract-containing silver nanowires according to any one of claims 1-4, wherein the method for preparing lavender extract-containing silver nanowires comprises the following steps:
(1) dissolving lavender extract, copper salt and silver salt respectively to obtain lavender extracting solution, copper salt solution and silver salt solution;
(2) mixing the lavender extract obtained in the step (1) with a copper salt solution, stirring for the first time, then dropwise adding a silver salt solution, and stirring for the second time to obtain a mixed solution;
(3) and (3) heating the mixed solution obtained in the step (2) for reaction to obtain the silver nanowires containing the lavender extract.
6. The method for preparing silver nanowires containing lavender extract according to claim 5, wherein in the step (1), the dissolving solvent is water;
preferably, in the step (1), the concentration of the lavender extract is 0.01-0.04 g/mL;
preferably, in the step (1), the concentration of the copper salt solution is 8-12 mmol/L;
preferably, in the step (1), the concentration of the silver salt solution is 0.5-10 mmol/L.
7. The method for preparing silver nanowires containing lavender extract as claimed in claim 5 or 6, wherein in the step (2), the volume ratio of the lavender extract, the copper salt solution and the silver salt solution is (11-44): (33-66);
preferably, in the step (2), the temperature of the primary stirring is 25-30 ℃, the time of the primary stirring is 8-12h, and the rotation speed of the primary stirring is 600-800 rpm;
preferably, in the step (2), the dropping speed of the silver salt solution is 0.3-0.8 mL/min;
preferably, in the step (2), the temperature of the secondary stirring is 25-30 ℃, the time of the secondary stirring is 2-4h, and the rotation speed of the secondary stirring is 350-550 rpm.
8. The method for preparing silver nanowires containing lavender extract according to any one of claims 5-7, wherein in the step (3), the temperature of the heating reaction is 40-60 ℃, and the time of the heating reaction is 36-72 h;
preferably, in step (3), after the heating reaction is finished, post-treatment is further performed: centrifuging the reaction solution by using acetone and/or ethanol, and dispersing and storing the product;
preferably, in the step (3), the rotation speed of the centrifugation is 10000-.
9. The method for preparing lavender extract-containing silver nanowires according to any one of claims 5-8, wherein the method for preparing lavender extract-containing silver nanowires comprises the following steps:
(1) dissolving lavender extract, copper salt and silver salt with water respectively to obtain 0.01-0.04g/mL lavender extract, 8-12mmol/L copper salt solution and 0.5-10mmol/L silver salt solution;
(2) mixing the lavender extract obtained in the step (1) with a copper salt solution, stirring for the first time, then dropwise adding a silver salt solution at a rate of 0.3-0.8mL/min, and stirring for the second time to obtain a mixed solution;
wherein the volume ratio of the lavender extracting solution to the copper salt solution to the silver salt solution is (11-44): (33-66);
(3) heating the mixed solution obtained in the step (2) in a water bath to 40-60 ℃, reacting for 36-72h, centrifuging the reaction solution with acetone and/or ethanol after the reaction is finished, and dispersing and storing the product to obtain the silver nanowire containing the lavender extract.
10. Use of silver nanowires containing lavender extract according to any one of claims 1-4 for the preparation of transparent electrodes and/or antibacterial materials.
CN202111014808.1A 2021-08-31 2021-08-31 Silver nanowire containing lavender extract and preparation method and application thereof Pending CN113798505A (en)

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Application publication date: 20211217