CN116160011A - Silver nanowire and manufacturing method thereof - Google Patents
Silver nanowire and manufacturing method thereof Download PDFInfo
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- CN116160011A CN116160011A CN202310167507.5A CN202310167507A CN116160011A CN 116160011 A CN116160011 A CN 116160011A CN 202310167507 A CN202310167507 A CN 202310167507A CN 116160011 A CN116160011 A CN 116160011A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0547—Nanofibres or nanotubes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a silver nanowire manufacturing method, which comprises the following steps: s1, completely dissolving polyvinylpyrrolidone in ethylene glycol; s2, respectively dissolving sodium chloride and sodium bromide in the hexanediol; s3, respectively taking 0.14-0.16 weight parts of sodium chloride solution and sodium bromide solution, and respectively adding the sodium chloride solution and the sodium bromide solution into 85-95 weight parts of ethylene glycol for dilution; s4, mixing a sodium chloride solution and a sodium bromide solution with the polyvinylpyrrolidone ethylene glycol solution, and simultaneously adding a silver nitrate glycerol solution; s5, transferring the mixed solution into a Teflon lining autoclave, and reacting for 2.5-3.5 hours at the temperature of 168-172 ℃. The silver nanowire obtained by the silver nanowire manufacturing method has small wire diameter; the length of the wire is long; the distribution is concentrated; can be produced in batches and can meet the actual needs.
Description
Technical Field
The invention relates to the technical field of silver nanowire manufacturing, in particular to a silver nanowire and a manufacturing method thereof.
Background
Silver nanowires are the most important one of one-dimensional nano materials, have excellent conductivity, light transmittance and bending resistance, have great potential in flexible screens, and have great advantages in process manufacturing by simple production process and high yield. Meanwhile, the conductive film manufactured by the silver wire technology can achieve higher light transmittance compared with the film manufactured by the prior art due to smaller line width, and has smaller resistance change rate in bending, so that the conductive film has more advantages in being applied to curved-surface and flexible display equipment.
The preparation method of the silver nanowire is the most classical and mature method by using a polyalcohol synthesis method, but the method also has a certain amount of nano particles, nano rods and other impurities, and the impurities have great influence on the sheet resistance and the haze of the silver nanowire conductive film. The traditional purification method of silver nanowire mother liquor mostly adopts methods such as centrifugation, acetone or ethyl acetate precipitation, natural sedimentation and the like; wherein the method of natural sedimentation is time consuming. Centrifugal method or acetone treatment, such as the patent of the invention with publication number CN100342064, discloses a synthesis method of silver nanowires, which comprises synthesizing silver nitrate and ethylene glycol to obtain silver nanowire mother liquor, washing with acetone, centrifuging, and purifying, wherein the purification method is easy to cause aggregation of silver nanowires, and has poor separation effect
However, the silver nanowires and the method for manufacturing the same currently used have the following problems:
1. the diameter of the obtained silver nanowire is thick; the length of the wire; the distribution is wide;
2. and the mass production is difficult, and the actual requirements cannot be met.
Based on the above situation, the present invention provides a silver nanowire and a manufacturing method thereof, which can effectively solve the above problems.
Disclosure of Invention
The invention aims to provide a silver nanowire manufacturing method. The silver nanowire obtained by the silver nanowire manufacturing method has the statistical wire length of 36.3 micrometers, the particle size of 39.5 nanometers and the wire diameter ratio of most silver nanowires is more than 1000. The silver nanowire obtained by the method for manufacturing the silver nanowire is characterized in that the wire diameter of most silver nanowires is smaller than 50 nanometers, the wire length is larger than 15 micrometers, the yield is larger than 52%, and the method is suitable for batch preparation.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a method of manufacturing silver nanowires, comprising the steps of:
s1, adding 140-160 parts by weight of ethylene glycol into a reaction container, heating to 64-66 ℃, starting stirring, adding 6.8-7.1 parts by weight of polyvinylpyrrolidone, and stirring until the polyvinylpyrrolidone is completely dissolved in the ethylene glycol to obtain a polyvinylpyrrolidone ethylene glycol solution;
s2, respectively dissolving 0.24-0.26 weight part of sodium chloride and 0.21-0.22 weight part of sodium bromide in 4.5-5.5 weight parts of glycol to respectively obtain a sodium chloride solution and a sodium bromide solution;
s3, respectively taking 0.14-0.16 weight parts of sodium chloride solution and sodium bromide solution, and respectively adding the sodium chloride solution and the sodium bromide solution into 85-95 weight parts of ethylene glycol for dilution to obtain diluted sodium chloride solution and sodium bromide solution;
s4, adding the diluted sodium chloride solution and sodium bromide solution into the reaction container in the step S1, mixing with the polyvinylpyrrolidone ethylene glycol solution, and simultaneously adding 10-12 parts by weight of silver nitrate glycerol solution;
s5, after stirring for 9-12 minutes at room temperature, transferring the mixed solution into a Teflon lining autoclave, and heating to 168-172 ℃ within 30 minutes; then the reaction is carried out for 2.5 to 3.5 hours under heat preservation, and then the mixture is cooled to room temperature;
s6, the silver nanowire is obtained by the latest purification treatment.
Preferably, in step S1, 150 parts by weight of ethylene glycol is added to the reaction vessel, heated to 65℃and stirring is started, and 6.95 parts by weight of polyvinylpyrrolidone is added.
Preferably, in step S1, the polyvinylpyrrolidone has a weight average molecular weight of 35000 to 37000.
Preferably, in step S2, 0.25 parts by weight of sodium chloride and 0.215 parts by weight of sodium bromide are dissolved in 5 parts by weight of glycol, respectively.
Preferably, in step S3, 0.15 parts by weight of the sodium chloride solution and the sodium bromide solution are then taken, respectively, and added to 90 parts by weight of ethylene glycol, respectively, for dilution.
Preferably, in step S4, the molar concentration of the silver nitrate glycerol solution is 0.01 to 0.8.
Preferably, in step S5, after stirring at room temperature for 10 minutes, the mixed solution is transferred to a teflon-lined autoclave and heated to 170 ℃ within 30 minutes.
Preferably, in step S5, the reaction is then incubated for 3 hours.
Preferably, in step S6, the purification treatment is to precipitate the nanowires using a large amount of acetone, and then an ethanol solution containing 0.5% pvp is added to redisperse the nanowires.
To purify silver nanowires, the nanowires were precipitated using a large amount of acetone, and then an ethanol solution containing 0.5% pvp was added to redisperse the nanowires. This process may be repeated three times to remove the particles. For transparent electrode applications, an additional centrifugation process is required to remove PVP residues and re-disperse the silver nanowires in ethanol or water for further use. For screen printing, the acetone washed silver nanowire precipitate is directly redispersed with a small amount of solution (e.g. 5 to 10ml ethanol and 5% pvp). Additional organics, such as PVP, are required to increase the viscosity of the silver nanowire ink for screen printing. The specific parameters need to be further modified according to the morphology and resistance of the printed sample.
The invention also provides a silver nanowire manufactured by adopting the silver nanowire manufacturing method.
Compared with the prior art, the invention has the following advantages:
the silver nanowire obtained by the silver nanowire manufacturing method has the statistical wire length of 36.3 micrometers, the particle size of 39.5 nanometers and the wire diameter ratio of most silver nanowires is more than 1000. The silver nanowire obtained by the method for manufacturing the silver nanowire is characterized in that the wire diameter of most silver nanowires is smaller than 50 nanometers, the wire length is larger than 15 micrometers, the yield is larger than 52%, and the method is suitable for batch preparation.
Detailed Description
In order that those skilled in the art will better understand the technical solution of the present invention, preferred embodiments of the present invention will be described below with reference to specific examples, but should not be construed as limiting the present patent.
Example 1:
a method of manufacturing silver nanowires, comprising the steps of:
s1, adding 140-160 parts by weight of ethylene glycol into a reaction container, heating to 64-66 ℃, starting stirring, adding 6.8-7.1 parts by weight of polyvinylpyrrolidone, and stirring until the polyvinylpyrrolidone is completely dissolved in the ethylene glycol to obtain a polyvinylpyrrolidone ethylene glycol solution;
s2, respectively dissolving 0.24-0.26 weight part of sodium chloride and 0.21-0.22 weight part of sodium bromide in 4.5-5.5 weight parts of glycol to respectively obtain a sodium chloride solution and a sodium bromide solution;
s3, respectively taking 0.14-0.16 weight parts of sodium chloride solution and sodium bromide solution, and respectively adding the sodium chloride solution and the sodium bromide solution into 85-95 weight parts of ethylene glycol for dilution to obtain diluted sodium chloride solution and sodium bromide solution;
s4, adding the diluted sodium chloride solution and sodium bromide solution into the reaction container in the step S1, mixing with the polyvinylpyrrolidone ethylene glycol solution, and simultaneously adding 10-12 parts by weight of silver nitrate glycerol solution;
s5, after stirring for 9-12 minutes at room temperature, transferring the mixed solution into a Teflon lining autoclave, and heating to 168-172 ℃ within 30 minutes; then the reaction is carried out for 2.5 to 3.5 hours under heat preservation, and then the mixture is cooled to room temperature;
s6, the silver nanowire is obtained by the latest purification treatment.
Preferably, in step S1, 150 parts by weight of ethylene glycol is added to the reaction vessel, heated to 65℃and stirring is started, and 6.95 parts by weight of polyvinylpyrrolidone is added.
Preferably, in step S1, the polyvinylpyrrolidone has a weight average molecular weight of 35000 to 37000.
Preferably, in step S2, 0.25 parts by weight of sodium chloride and 0.215 parts by weight of sodium bromide are dissolved in 5 parts by weight of glycol, respectively.
Preferably, in step S3, 0.15 parts by weight of the sodium chloride solution and the sodium bromide solution are then taken, respectively, and added to 90 parts by weight of ethylene glycol, respectively, for dilution.
Preferably, in step S4, the molar concentration of the silver nitrate glycerol solution is 0.01 to 0.8.
Preferably, in step S5, after stirring at room temperature for 10 minutes, the mixed solution is transferred to a teflon-lined autoclave and heated to 170 ℃ within 30 minutes.
Preferably, in step S5, the reaction is then incubated for 3 hours.
Preferably, in step S6, the purification treatment is to precipitate the nanowires using a large amount of acetone, and then an ethanol solution containing 0.5% pvp is added to redisperse the nanowires.
The invention also provides a silver nanowire manufactured by adopting the silver nanowire manufacturing method.
Example 2:
a method of manufacturing silver nanowires, comprising the steps of:
s1, adding 140 parts by weight of ethylene glycol into a reaction container, heating to 64 ℃, starting stirring, adding 6.8 parts by weight of polyvinylpyrrolidone, and stirring until the polyvinylpyrrolidone is completely dissolved in the ethylene glycol to obtain a polyvinylpyrrolidone ethylene glycol solution;
s2, respectively dissolving 0.24 weight part of sodium chloride and 0.21 weight part of sodium bromide in 4.5 weight parts of glycol to respectively obtain a sodium chloride solution and a sodium bromide solution;
s3, respectively taking 0.14 weight parts of the sodium chloride solution and the sodium bromide solution, and respectively adding the sodium chloride solution and the sodium bromide solution into 85 weight parts of ethylene glycol for dilution to obtain diluted sodium chloride solution and sodium bromide solution;
s4, adding the diluted sodium chloride solution and sodium bromide solution into the reaction container in the step S1, mixing with the polyvinylpyrrolidone ethylene glycol solution, and simultaneously adding 10 parts by weight of silver nitrate glycerol solution;
s5, after stirring for 9 minutes at room temperature, transferring the mixed solution into a Teflon lining autoclave, and heating to 168 ℃ within 30 minutes; then the reaction is kept for 2.5 hours, and then the mixture is cooled to room temperature;
s6, the silver nanowire is obtained by the latest purification treatment.
In this embodiment, in step S1, the weight average molecular weight of the polyvinylpyrrolidone is 35000.
In this example, in step S4, the molar concentration of the silver nitrate glycerol solution is 0.01.
In this example, in step S6, the purification treatment is to precipitate the nanowires using a large amount of acetone, and then an ethanol solution containing 0.5% pvp is added to redisperse the nanowires.
In this embodiment, there is also provided a silver nanowire manufactured using the silver nanowire manufacturing method as described above.
Example 3:
a method of manufacturing silver nanowires, comprising the steps of:
s1, adding 160 parts by weight of ethylene glycol into a reaction container, heating to 66 ℃, starting stirring, adding 6.8-7.1 parts by weight of polyvinylpyrrolidone, and stirring until the polyvinylpyrrolidone is completely dissolved in the ethylene glycol to obtain a polyvinylpyrrolidone ethylene glycol solution;
s2, respectively dissolving 0.26 weight part of sodium chloride and 0.22 weight part of sodium bromide in 5.5 weight parts of glycol to respectively obtain a sodium chloride solution and a sodium bromide solution;
s3, respectively taking 0.16 weight parts of the sodium chloride solution and the sodium bromide solution, and respectively adding the sodium chloride solution and the sodium bromide solution into 95 weight parts of ethylene glycol for dilution to obtain diluted sodium chloride solution and sodium bromide solution;
s4, adding the diluted sodium chloride solution and sodium bromide solution into the reaction container in the step S1, mixing with the polyvinylpyrrolidone ethylene glycol solution, and simultaneously adding 12 parts by weight of silver nitrate glycerol solution;
s5, after stirring at room temperature for 12 minutes, the mixed solution was transferred to a teflon-lined autoclave and heated to 172 ℃ within 30 minutes; then the reaction is kept for 3.5 hours, and then the mixture is cooled to room temperature;
s6, the silver nanowire is obtained by the latest purification treatment.
In this embodiment, in step S1, the polyvinylpyrrolidone has a weight average molecular weight of 37000.
In this example, in step S4, the molar concentration of the silver nitrate glycerol solution is 0.8.
In this example, in step S6, the purification treatment is to precipitate the nanowires using a large amount of acetone, and then an ethanol solution containing 0.5% pvp is added to redisperse the nanowires.
In this embodiment, there is also provided a silver nanowire manufactured using the silver nanowire manufacturing method as described above.
Example 4:
a method of manufacturing silver nanowires, comprising the steps of:
s1, adding 140-160 parts by weight of ethylene glycol into a reaction container, heating to 64-66 ℃, starting stirring, adding 6.8-7.1 parts by weight of polyvinylpyrrolidone, and stirring until the polyvinylpyrrolidone is completely dissolved in the ethylene glycol to obtain a polyvinylpyrrolidone ethylene glycol solution;
s2, respectively dissolving 0.24-0.26 weight part of sodium chloride and 0.21-0.22 weight part of sodium bromide in 4.5-5.5 weight parts of glycol to respectively obtain a sodium chloride solution and a sodium bromide solution;
s3, respectively taking 0.14-0.16 weight parts of sodium chloride solution and sodium bromide solution, and respectively adding the sodium chloride solution and the sodium bromide solution into 85-95 weight parts of ethylene glycol for dilution to obtain diluted sodium chloride solution and sodium bromide solution;
s4, adding the diluted sodium chloride solution and sodium bromide solution into the reaction container in the step S1, mixing with the polyvinylpyrrolidone ethylene glycol solution, and simultaneously adding 10-12 parts by weight of silver nitrate glycerol solution;
s5, after stirring for 9-12 minutes at room temperature, transferring the mixed solution into a Teflon lining autoclave, and heating to 168-172 ℃ within 30 minutes; then the reaction is carried out for 2.5 to 3.5 hours under heat preservation, and then the mixture is cooled to room temperature;
s6, the silver nanowire is obtained by the latest purification treatment.
In this example, in step S1, 150 parts by weight of ethylene glycol was added to the reaction vessel, heated to 65℃and stirring was started, and 6.95 parts by weight of polyvinylpyrrolidone was added.
In this embodiment, in step S1, the polyvinylpyrrolidone has a weight average molecular weight of 36000.
In this example, in step S2, 0.25 parts by weight of sodium chloride and 0.215 parts by weight of sodium bromide were dissolved in 5 parts by weight of glycol, respectively.
In this example, in step S3, 0.15 parts by weight of the sodium chloride solution and the sodium bromide solution were then taken, respectively, and added to 90 parts by weight of ethylene glycol, respectively, for dilution.
In this embodiment, in step S4, the molar concentration of the silver nitrate glycerol solution is 0.56.
In this example, in step S5, after stirring at room temperature for 10 minutes, the mixed solution was transferred to a teflon-lined autoclave and heated to 170 ℃ within 30 minutes.
In this example, in step S5, the reaction was then incubated for 3 hours.
In this example, in step S6, the purification treatment is to precipitate the nanowires using a large amount of acetone, and then an ethanol solution containing 0.5% pvp is added to redisperse the nanowires.
The silver nanowire obtained by the method for manufacturing the silver nanowire has the statistical wire length of 36.3 micrometers, the particle size of 39.5 nanometers and the wire diameter ratio of most silver nanowires is more than 1000. The silver nanowire obtained by the method for manufacturing the silver nanowire is characterized in that the wire diameter of most silver nanowires is smaller than 50 nanometers, the wire length is larger than 15 micrometers, the yield is larger than 52%, and the method is suitable for batch preparation.
The above is only a preferred embodiment of the present invention, and it should be noted that the above preferred embodiment should not be construed as limiting the present invention, and the scope of the present invention is defined by the appended claimsThe scope of the claims should be determined. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention and these modifications and adaptations are intended to be comprehended within the scope of the invention 。
Claims (10)
1. A method of manufacturing silver nanowires, comprising the steps of:
s1, adding 140-160 parts by weight of ethylene glycol into a reaction container, heating to 64-66 ℃, starting stirring, adding 6.8-7.1 parts by weight of polyvinylpyrrolidone, and stirring until the polyvinylpyrrolidone is completely dissolved in the ethylene glycol to obtain a polyvinylpyrrolidone ethylene glycol solution;
s2, respectively dissolving 0.24-0.26 weight part of sodium chloride and 0.21-0.22 weight part of sodium bromide in 4.5-5.5 weight parts of glycol to respectively obtain a sodium chloride solution and a sodium bromide solution;
s3, respectively taking 0.14-0.16 weight parts of sodium chloride solution and sodium bromide solution, and respectively adding the sodium chloride solution and the sodium bromide solution into 85-95 weight parts of ethylene glycol for dilution to obtain diluted sodium chloride solution and sodium bromide solution;
s4, adding the diluted sodium chloride solution and sodium bromide solution into the reaction container in the step S1, mixing with the polyvinylpyrrolidone ethylene glycol solution, and simultaneously adding 10-12 parts by weight of silver nitrate glycerol solution;
s5, after stirring for 9-12 minutes at room temperature, transferring the mixed solution into a Teflon lining autoclave, and heating to 168-172 ℃ within 30 minutes; then the reaction is carried out for 2.5 to 3.5 hours under heat preservation, and then the mixture is cooled to room temperature;
s6, the silver nanowire is obtained by the latest purification treatment.
2. The method of producing silver nanowires as recited in claim 1, wherein in step S1, 150 parts by weight of ethylene glycol is added to the reaction vessel, heated to 65 ℃, stirring is started, and 6.95 parts by weight of polyvinylpyrrolidone is added.
3. The method of producing silver nanowires as recited in claim 1, wherein in step S1, the polyvinylpyrrolidone has a weight average molecular weight of 35000 to 37000.
4. The method of manufacturing silver nanowires according to claim 1, wherein in step S2, 0.25 parts by weight of sodium chloride and 0.215 parts by weight of sodium bromide are dissolved in 5 parts by weight of glycol, respectively.
5. The method of manufacturing silver nanowires as recited in claim 1, wherein in step S3, 0.15 parts by weight of the sodium chloride solution and the sodium bromide solution are then taken, respectively, and added to 90 parts by weight of ethylene glycol, respectively, for dilution.
6. The method according to claim 1, wherein in step S4, the molar concentration of the silver nitrate glycerol solution is 0.01 to 0.8.
7. The method of manufacturing silver nanowires as recited in claim 1, wherein in step S5, after stirring at room temperature for 10 minutes, the mixed solution is transferred to a teflon-lined autoclave and heated to 170 ℃ within 30 minutes.
8. The method of manufacturing silver nanowires as recited in claim 7, wherein in step S5, the reaction is then performed for 3 hours with heat preservation.
9. The method of manufacturing silver nanowires as recited in claim 1, wherein in step S6, the purification treatment is to precipitate the nanowires using a large amount of acetone, and then an ethanol solution containing 0.5% pvp is added to redisperse the nanowires.
10. A silver nanowire manufactured by the silver nanowire manufacturing method according to any one of claims 1 to 9.
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