CN110814361A - Silver nanowire purification method - Google Patents
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- CN110814361A CN110814361A CN201911089510.XA CN201911089510A CN110814361A CN 110814361 A CN110814361 A CN 110814361A CN 201911089510 A CN201911089510 A CN 201911089510A CN 110814361 A CN110814361 A CN 110814361A
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention relates to the technical field of nano material purification, and discloses a silver nanowire purification method, which comprises the following steps: (1) dispersing the silver nanowire stock solution into a first solvent to obtain a silver nanowire dispersion solution, adding a surfactant, standing, and removing upper-layer liquid after the silver nanowires are settled to the bottom; (2) adding deionized water or alcohol into the silver nanowires settled at the bottom in the step (1), adding a surfactant, standing, removing the upper-layer liquid after the silver nanowires are settled at the bottom, and repeating for 2-6 times; (3) finally, dispersing the silver nanowires settled to the bottom in the step (2) into deionized water or alcohol to obtain purified silver nanowire dispersion liquid; the silver nanowire purification method is simple and convenient to operate, does not adopt organic solvents such as acetone and the like, is low in toxicity, has low requirements on the working environment in the production process, and has small influence on human health.
Description
Technical Field
The invention relates to the technical field of nano material purification, in particular to a silver nanowire purification method.
Background
One-dimensional nanomaterials, such as nanowires, nanofibers, nanorods, nanobelts, etc., all have unique physical and chemical properties such as electrical, optical, magnetic, etc., and are widely used in nano-electronic devices, nano-lasers, nano-chemical and biological sensors, nano-probes, nano-composites, etc. The silver nanowire is the most important one of the one-dimensional nanometer materials, has excellent electrical conductivity, light transmittance and bending resistance, has great potential in flexible screens, and has great advantages in process procedures due to simple production process and high yield. Meanwhile, due to the fact that the line width is small, compared with a conductive film manufactured in the prior art, the conductive film manufactured by the silver wire technology can achieve higher light transmittance, the resistance change rate is small when the conductive film is bent, and the conductive film has advantages when being applied to equipment with curved surfaces and flexible display.
The preparation method of the silver nanowire is the most classical method and the most mature method by using a polyol synthesis method, but the method also has a certain amount of impurities such as nano particles, nano rods and the like, and the impurities have great influence on the sheet resistance and the haze of the silver nanowire conductive film. The traditional method for purifying the silver nanowire mother liquor mostly adopts the methods of centrifugation, acetone or ethyl acetate precipitation, natural sedimentation and the like; wherein the natural sedimentation method is time-consuming. Centrifugal method or acetone treatment, such as the invention patent with the publication number of CN100342064, discloses a silver nanowire synthesis method, which comprises the steps of synthesizing silver nitrate and ethylene glycol to obtain silver nanowire mother liquor, washing with acetone, centrifugally separating and purifying, wherein the purification method is easy to cause silver nanowire agglomeration and has poor separation effect; for example, the invention patent with the application publication number of CN105345022A discloses a method for purifying silver nanowires, which adopts polyvinylpyrrolidone aqueous solution for dispersion, then uses acetone for washing and standing for separation, and uses a large amount of organic solvents such as acetone, etc. simultaneously, the treatment cost is high; the acetone has inhibitory and anesthetic effects on the central nervous system, and damage to liver, kidney and pancreas may occur to human body when contacting with high concentration.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a silver nanowire purification method, which is simple and convenient to operate, does not adopt organic solvents such as acetone and the like, has low toxicity, has low requirement on the working environment in the production process and has small influence on the human health.
In order to achieve the above purpose, the invention provides the following technical scheme:
a silver nanowire purification method comprises the following steps:
(1) dispersing the silver nanowire stock solution into a first solvent to obtain a silver nanowire dispersion solution, adding a surfactant, standing, and removing upper-layer liquid after the silver nanowires are settled to the bottom;
(2) adding deionized water or alcohol into the silver nanowires settled at the bottom in the step (1), adding a surfactant, standing, removing the upper-layer liquid after the silver nanowires are settled at the bottom, and repeating for 2-6 times;
(3) and (3) finally, dispersing the silver nanowires settled in the step (2) to the bottom into deionized water or alcohol to obtain purified silver nanowire dispersion liquid.
The standing time is 2-48 h.
Compared with the existing method, the total consumption of the purification method is longer, but post-treatment processes such as solvent removal and the like are not needed, water is used as a solvent, and the price is low. In the existing method, acetone and other organic solvents are used, the acetone is a dangerous product easy to prepare toxin, waste liquid needs to be recycled by a professional company, and the silver nanowires are easily broken by repeated washing processes, so that the loss of the silver nanowires is determined and reaches up to 20%.
In the present invention, preferably, the silver nanowire stock solution in step (1) is synthesized by a polyol method. The polyhydric alcohol used in the above-mentioned polyhydric alcohol method is a polyhydric alcohol such as ethylene glycol, propylene glycol, butylene glycol, pentylene glycol, or glycerin. For example: the invention patent with the publication number of CN100342064 is named as silver nanowire mother liquor synthesized by silver nitrate and ethylene glycol in a silver nanowire synthesis method.
The method for synthesizing the silver nanowire by using the polyalcohol is a one-pot method, is simple to operate and high in production efficiency, and the silver nanowire obtained by the existing method for synthesizing the silver nanowire by using the polyalcohol still contains some impurities such as nano particles, nano rods and the like, and the impurities have great influence on the sheet resistance and the haze of the silver nanowire conducting film.
In the present invention, it is preferable that the silver nanowire stock solution contains silver nanowires with an average diameter of 10nm to 100nm and an average length of 2 μm to 50 μm.
In the present invention, preferably, the first solvent is water or alcohol or a combination of both; water or alcohol is used as solvent, so it has no toxicity and low cost. In the invention, the alcohol is one of methanol, ethanol and propylene glycol.
In the present invention, it is preferable that the amount of the surfactant added in the steps (1) and (2) is 0.005 to 10% of the total amount of the silver nanowire dispersion.
In the present invention, it is preferable that the volume ratio of the silver nanowire stock solution to the first solvent in step (1) is 1:1 to 20.
In the present invention, it is preferable that deionized water or alcohol is added to the step (2) in a volume 5 to 10 times that of the first solvent in the step (1).
In the present invention, preferably, the concentration of the silver nanowires in the purified silver nanowire dispersion obtained in step (3) is 0.1% to 1%.
In the present invention, preferably, the surfactant is one or more of a fluorocarbon surfactant, a cationic surfactant, an anionic surfactant, a nonionic surfactant, and an amphoteric surfactant.
In the present invention, preferably, the fluorocarbon surfactant is a nonionic fluorocarbon surfactant and/or an ionic fluorocarbon surfactant.
Further, the surfactant is a commercially available product, such as nonionic fluorocarbon surfactant, a commercially available product from komu corporation: capsule toneTMFS-3100、CapstoneTMOne or a combination of two of FS-30; the ionic fluorocarbon surfactant is CapstoneTMFS-10、CapstoneTMOne or a combination of two of FS-61; the cationic surfactant is one or more of octadecyl trimethyl ammonium chloride, dodecyl dimethyl benzyl ammonium chloride, didodecyl dimethyl ammonium chloride and polyquaternium cationic polymer; the anionic surfactant is one or more of ethoxy alkyl sodium sulfate, ethoxy ammonium alkyl sulfate, sodium dodecyl sulfate and ammonium dodecyl sulfate; the nonionic surfactant is one or more of alkylphenol polyoxyethylene, polyoxyethylene alkylamine and polyoxyethylene alkylolamide; the zwitterionic surfactant is dodecyl dimethyl betaine,One or a combination of two of cocamidopropyl betaine. In the method, the added surfactant enables the silver nanowires to be fully wetted, permeated and dispersed, thereby avoiding aggregation of the silver nanowires during sedimentation and accelerating sedimentation of the silver nanowires, and improving the purification purity of the silver nanowires.
Compared with the prior art, the invention has the beneficial effects that:
the silver nanowire purification method provided by the invention is provided aiming at the method for synthesizing silver nanowires by using polyhydric alcohols, and the method for synthesizing silver nanowires by using polyhydric alcohols is a one-pot method, so that the operation is simple and the production efficiency is high; the purification method is simple and convenient to operate, not only can purify the silver nanowire stock solution obtained by the similar polyol synthesis method, but also can be applied to the purification of the silver nanowire stock solution obtained by the mixed polyol synthesis method, effectively removes impurities such as nano particles, nano rods and the like in the silver nanowire stock solution, accelerates the sedimentation of the silver nanowires while avoiding the aggregation of the silver nanowires during sedimentation, improves the purification purity of the silver nanowires, and obviously reduces the sheet resistance and the haze of the purified silver nanowire conductive film.
The silver nanowire purification method does not adopt organic solvents such as acetone and the like, has low toxicity, low requirement on the working environment in the production process and small influence on the human health.
Drawings
Fig. 1 is an SEM electron micrograph of the purified silver nanowires of example 2.
Fig. 2 is an SEM electron micrograph of the purified silver nanowires of comparative example 1.
Detailed Description
In order to make the technical means, the creation features, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the embodiment. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1:
a silver nanowire purification method comprises the following specific steps: 10ml of silver nanowire stock solution with the average diameter of 10nm and the average length of 15 mu m obtained by an ethylene glycol synthesis method is dispersed into 200ml of water to obtain silver nanowire dispersion liquid, 0.03g of surfactant is added to enable the silver nanowires to be settled after dispersion, standing is carried out for 6h, and after the silver nanowires are settled to the bottom, the upper liquid is removed;
adding 1000ml of deionized water into the silver nanowires settled at the bottom, adding 0.03g of surfactant, standing for 6 hours, removing the upper-layer liquid after the silver nanowires are settled at the bottom, and repeating for 2 times;
and finally dispersing the silver nanowires settled to the bottom into 200ml of deionized water to obtain the purified silver nanowire dispersion liquid.
In this example, the surfactant is CapstoneTMFS-3100。
Example 2:
a silver nanowire purification method comprises the following specific steps: 100ml of silver nanowire stock solution with the average diameter of 20nm and the average length of 20 mu m, which is synthesized by a polyalcohol method, is dispersed in 100ml of water to obtain silver nanowire dispersion liquid, 2.5g of surfactant is added to enable the silver nanowires to be dispersed and then settled, the mixture is kept stand for 8 hours, and after the silver nanowires are settled to the bottom, the upper liquid is removed;
adding 500ml of deionized water into the silver nanowires settled at the bottom, adding 0.5g of surfactant, standing for 8 hours, removing the upper-layer liquid after the silver nanowires are settled at the bottom, and repeating for 2 times;
and finally dispersing the silver nanowires settled to the bottom into 200ml of deionized water to obtain the purified silver nanowire dispersion liquid.
In this example, the surfactant is octadecyl trimethyl ammonium chloride.
Example 3:
a silver nanowire purification method comprises the following specific steps: 100ml of silver nanowire stock solution with the average diameter of 60nm and the average length of 30 mu m, which is synthesized by a polyalcohol method, is dispersed into 100ml of ethanol solution with the volume fraction of 50% to obtain silver nanowire dispersion, 2g of surfactant is added to disperse the silver nanowires, then the silver nanowires are settled and kept stand for 30min, and after the silver nanowires are settled to the bottom, the upper liquid is removed;
adding 800ml of ethanol into the silver nanowires settled at the bottom, adding 0.05g of surfactant, standing for 2 hours, removing the upper-layer liquid after the silver nanowires are settled at the bottom, and repeating for 5 times;
and finally dispersing the silver nanowires settled to the bottom into 800ml of deionized water to obtain the purified silver nanowire dispersion liquid.
In this example, the surfactant is CapstoneTMFS-10。
Example 4:
a silver nanowire purification method comprises the following specific steps: 100ml of silver nanowire stock solution with the average diameter of 100nm and the average length of 50 mu m, which is synthesized by a polyalcohol method, is dispersed into 300ml of ethanol to obtain silver nanowire dispersion liquid, 20g of surfactant is added to disperse the silver nanowires, then the silver nanowires are settled and kept stand for 48h, and after the silver nanowires are settled to the bottom, the upper liquid is removed;
adding 3000ml of ethanol into the silver nanowires settled at the bottom, adding 1g of surfactant, standing for 8 hours, removing the upper-layer liquid after the silver nanowires settled at the bottom, and repeating for 6 times;
and finally dispersing the silver nanowires settled to the bottom into 1000ml of ethanol to obtain the purified silver nanowire aqueous solution.
In this example, the surfactant is CapstoneTMFS-30、CapstoneTMFS-61, octadecyl trimethyl ammonium chloride, a mixture of sodium dodecyl sulfate and dodecyl dimethyl betaine, and the weight ratio of the mixture is 1:1:1:1: 1.
Comparative example 1:
a silver nanowire purification method is disclosed in the invention patent with application publication number CN105345022A, and comprises the following specific steps: dispersing 0.02g of silver nanowires with the average diameter of 20nm and the average length of 60 mu m, which are synthesized by a polyalcohol method, in 10mL of polyvinylpyrrolidone (PVP) aqueous solution with the mass fraction of 0.5% to obtain silver nanowire dispersion liquid, adding acetone, wherein the volume of the acetone is 4 times that of the silver nanowire dispersion liquid, aggregating the silver nanowires, standing for 10min, and removing the upper layer liquid. Repeating the steps for 3 times to obtain the purified silver nanowire.
Two parts of 100g of silver nanowire stock solution are taken and purified by the methods of the embodiment 2 and the comparative example 1 respectively to obtain 1.01g of purified silver nanowire in the embodiment 2 and 0.80g of purified silver nanowire in the comparative example 1, and the silver nanowire loss is 20.8 percent compared with the silver nanowire loss in the embodiment 2.
By comparing the electron micrographs of the example 2 and the comparative example 1, the purified silver nanowires of the example 2 are uniformly dispersed and have high purity, and the purified silver nanowires hardly contain impurities such as nanoparticles and nanorods; although the total time consumption of the purification method in the embodiment 2 is longer than that of the comparative example 1, post-treatment processes such as solvent removal and the like are not needed, water is used as a solvent, the price is low, acetone used in the comparative example 1 is a dangerous product which is easy to prepare toxin, waste liquid needs to be recycled by a professional company, the silver nanowires are easy to break after repeated washing processes, and the consumption of the silver nanowires reaches 20.8%.
Comparative example 2:
a silver nanowire purification method, which is different from example 2 only in that a surfactant is not added. The method comprises the following specific steps: 100ml of silver nanowire stock solution with the average diameter of 20nm and the average length of 20 mu m, which is synthesized by a polyalcohol method, is dispersed in 100ml of water to obtain silver nanowire dispersion liquid, the silver nanowires are settled after being dispersed, the mixture is kept stand for 30 days, and after the silver nanowires are settled to the bottom, the upper liquid is removed;
adding 500ml of deionized water into the silver nanowires settled at the bottom, standing for 20 days, removing the upper liquid after the silver nanowires settle at the bottom, and repeating for 2 times;
and finally dispersing the silver nanowires settled to the bottom into 200ml of deionized water to obtain the purified silver nanowire dispersion liquid.
The properties of the purified aqueous silver nanowire solutions of examples 1-4 were examined by experiments as follows:
respectively adopting a silver nanowire stock solution and the purified silver nanowire aqueous solution of the examples 1 to 4, adding an auxiliary agent and a thickening agent, coating the mixture on a PET substrate through a Meyer rod to prepare a uniform film, then carrying out a haze test by adopting a photoelectric haze meter, wherein the haze data are shown in a table 1 under the condition that the sheet resistance is 50 omega:
TABLE 1
Note: the data are the average of 5 tests.
As can be seen from the data in table 1, the haze of the aqueous solution of the silver nanowire obtained by purifying the stock solution of the silver nanowire in examples 1 to 4 is significantly reduced, and is reduced by 69.9% relative to the stock solution of the silver nanowire; and then, performing resistance test on the silver nanowire stock solution and the silver nanowire aqueous solution purified in the embodiment 1-4, wherein the resistance test shows that the silver nanowire stock solution is not conductive, and the resistance of the silver nanowire aqueous solution purified in the embodiment 1-4 is between 50 and 70 omega, which shows that the resistance of the silver nanowire aqueous solution obtained by purifying the silver nanowire stock solution in the embodiment 1-4 is also greatly reduced.
Meanwhile, in the comparison between the example 2 and the comparative example 2, the silver nanowires are purified without adding the surfactant, so that the addition of the surfactant is obviously better; the purified silver nanowire of the comparative example 2 is only reduced by 4.8 percent relative to the silver nanowire stock solution; in the comparative example 2, 20 to 30 days are needed for waiting for the silver nanowire to settle, and the time is long; therefore, the added surfactant can fully wet, permeate and disperse the silver nanowires, thereby avoiding the aggregation of the silver nanowires during sedimentation and accelerating the sedimentation of the silver nanowires, and improving the purification purity of the silver nanowires.
The above description is intended to describe in detail the preferred embodiments of the present invention, but the embodiments are not intended to limit the scope of the claims of the present invention, and all equivalent changes and modifications made within the technical spirit of the present invention should fall within the scope of the claims of the present invention.
Claims (10)
1. A silver nanowire purification method is characterized by comprising the following steps:
(1) dispersing the silver nanowire stock solution into a first solvent to obtain a silver nanowire dispersion solution, adding a surfactant, standing, and removing upper-layer liquid after the silver nanowires are settled to the bottom;
(2) adding deionized water or alcohol into the silver nanowires settled at the bottom in the step (1), adding a surfactant, standing, removing the upper-layer liquid after the silver nanowires are settled at the bottom, and repeating for 2-6 times;
(3) and (3) finally, dispersing the silver nanowires settled in the step (2) to the bottom into deionized water or alcohol to obtain purified silver nanowire dispersion liquid.
2. The method for purifying silver nanowires of claim 1, wherein the stock solution of silver nanowires in step (1) is synthesized by a polyol method.
3. The method for purifying silver nanowires of claim 2, wherein the silver nanowires contained in the silver nanowire stock solution have an average diameter of 10nm to 100nm and an average length of 2 μm to 50 μm.
4. The method of claim 1, wherein the first solvent is water or alcohol or a combination thereof.
5. The method for purifying silver nanowires of claim 1, wherein the volume ratio of the silver nanowire stock solution to the first solvent in the step (1) is 1: 1-20.
6. The method for purifying silver nanowires of claim 1, wherein the volume of deionized water or alcohol added in step (2) is 5-10 times that of the first solvent in step (1).
7. The method for purifying silver nanowires of claim 1, wherein the concentration of silver nanowires in the purified silver nanowire dispersion obtained in step (3) is 0.1% -1%.
8. The method for purifying silver nanowires of claim 1, wherein the ratio of the mass of the surfactant added in the steps (1) and (2) to the volume of the silver nanowire dispersion is 0.005-10%.
9. The method for purifying silver nanowires of claim 8, wherein the surfactant is one or more of a fluorocarbon surfactant, a cationic surfactant, an anionic surfactant, a nonionic surfactant and an amphoteric surfactant.
10. The method of claim 9, wherein the fluorocarbon surfactant is a non-ionic fluorocarbon surfactant and/or an ionic fluorocarbon surfactant.
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CN112605380A (en) * | 2020-11-30 | 2021-04-06 | 哈尔滨工业大学 | Filtering and purifying method of silver nanowires |
CN115283661A (en) * | 2022-08-09 | 2022-11-04 | 北京化工大学 | Method for purifying copper nanowire and copper nanowire prepared by same |
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