CN113714509B - Urea-reduced silver nanowire and preparation method and application thereof - Google Patents
Urea-reduced silver nanowire and preparation method and application thereof Download PDFInfo
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- CN113714509B CN113714509B CN202111022770.2A CN202111022770A CN113714509B CN 113714509 B CN113714509 B CN 113714509B CN 202111022770 A CN202111022770 A CN 202111022770A CN 113714509 B CN113714509 B CN 113714509B
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- 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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- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
Abstract
The invention discloses a silver nanowire reduced by urea and a preparation method and application thereof, belonging to the technical field of synthesis of nano materials. The preparation method of the silver nanowire reduced by urea comprises the following steps: preparing a solution, adding urea and silver nitrate into ethylene glycol, stirring at normal temperature for 30-40min until the urea and the silver nitrate are dissolved, carrying out ultrasonic treatment for 10-20min to obtain a solution A, and carrying out continuous ice bath on the solution A for later use; adding polyvinylpyrrolidone into ethylene glycol, and stirring at normal temperature for 30-40min until the polyvinylpyrrolidone is dissolved to obtain a solution B for later use; then carrying out high-temperature reaction, preheating the solution B at 150-180 ℃, carrying out heat preservation, dripping the solution A into the reaction solution, and introducing N 2 Stirring, standing and preserving heat to obtain silver nanowire mother liquor; and finally, processing the silver nanowire mother liquor to obtain the silver nanowires. The preparation method is simple and convenient, has good repeatability, and the prepared silver nanowire has high purity, less associated silver nanoparticles and low preparation cost.
Description
Technical Field
The invention relates to the technical field of synthesis of nano materials, in particular to a silver nanowire reduced by urea and a preparation method and application thereof.
Background
Silver is the medium conductivity of metal (6.3X 10) 7 S/m) and a metal having the highest thermal conductivity (412W/m.K, 100 ℃), and is soft and ductile. Silver nanomaterials have better electrical and thermal conductivity than bulk silver, silver nanowires (AgNWs) are one-dimensional nanomaterials radially confined to the nanometer scale (less than 200nm), typically 10-200nm in diameter and 5-100 μm in length. The aspect ratio is one of the most important criteria for evaluating the AgNWs, the aspect ratio of AgNWs should be generally more than 50, and the nano-structure with the aspect ratio less than 50 is called silver nano-rod (AgNRs). Researchers have discovered silver nanowires (AgNWs)) The material not only meets the requirements of the conductive material on excellent electrical conductivity and thermal conductivity, but also has good flexibility, chemical stability and mechanical stability. The porous network composed of AgNWs has very excellent light transmission, so that the application of the porous network in transparent electronic devices is possible. The surface effects of the silver nano material such as macroscopic quantum tunneling effect, size effect and the like widen the application field of the silver nano material, so the silver nano material is widely applied to the fields of photoelectric devices, diodes, sensors, organic solar cells, energy storage devices and the like. AgNWs with high heat are expected in other fields, and are one of the most promising metal nanowire materials. In the prior art, a mixed polyol method is a common and general technology, and scholars use benzoin as a reducing agent to realize preparation of superfine silver nanowires, but generally, the method has relatively high cost, and is difficult to apply and popularize in the later development period of many years, so that the cost becomes a main barrier of silver nanowire ink in application. The invention adopts urea with long industrialization time and huge yield as a reducing agent, and the core aim is to reduce the cost.
Disclosure of Invention
Aiming at the problems, the invention provides a silver nanowire reduced by urea and a preparation method and application thereof, urea with long industrialization time and huge yield is taken as a reducing agent, the cost is reduced, the synthesis steps are simple and convenient, the repeatability is good, the purity of the prepared silver nanowire is higher,
the first purpose of the invention is to provide a preparation method of silver nanowires reduced by urea, which comprises the following steps:
Adding urea and silver nitrate into ethylene glycol, stirring at normal temperature for 30-40min until dissolving, performing ultrasonic treatment for 10-20min to obtain solution A, and performing ice bath on the solution A for later use; wherein, the concentration of the urea is 3.2-4.4g/L, and the concentration of the silver nitrate is 17 g/L;
adding polyvinylpyrrolidone into ethylene glycol, and stirring at normal temperature for 30-40min until the polyvinylpyrrolidone is dissolved to obtain a solution B for later use; wherein the concentration of the polyvinylpyrrolidone is 6.25-9.38 g/L;
Preheating the solution B at the temperature of 150 ℃ and 180 ℃, preserving the heat, dripping the solution A into the reaction solution, and introducing N 2 Stirring, standing and preserving heat to obtain silver nanowire mother liquor;
and 3, centrifuging the silver nanowire mother liquor to obtain a precipitate, and purifying the precipitate to obtain the silver nanowires.
Preferably, step 3 is performed according to the following method:
adding ethanol into the silver nanowire mother liquor, and performing ultrasonic treatment until the mixture is uniformly dispersed to obtain a mixed solution A; centrifuging the mixed solution to obtain a precipitate, wherein the precipitate is X1;
step (2), adding ethanol into X1, and performing ultrasonic treatment until the mixture is uniformly dispersed to obtain a mixed solution B; centrifuging the mixed solution to obtain a precipitate, wherein the precipitate is X2;
and (3) repeating the step (2) for 2-4 times to obtain the purified silver nanowire.
Preferably, in step 2, the volume ratio of the solution A to the solution B is 1: 1.
Preferably, in step 2, the instillation rate of the solution A is 0.15mL/min, and the instillation time is 10 min.
Preferably, in step 2, N is 2 The flow rate of (2) was 65 mL/min.
Preferably, in step 2, the stirring rate in step (1) and step (2) is 400 rpm.
Preferably, solution B is preheated to 150 ℃ and incubated for 30min in step 2.
Preferably, in the step 2, the standing and heat preservation time in the step 2 is 1.5 h.
It is a second object of the present invention to provide silver nanowires having an average diameter of 82 to 87.45nm and a length of 32 to 35 μm according to the above method.
A third object of the present invention is to provide a use of silver nanowires in the preparation of transparent electric heaters.
Compared with the prior art, the invention has the following beneficial effects:
(1) in the synthesis process of the silver nanowires, Ag is used as transition metal,the electron arrangement is [ Kr]4d 10 5s 1 Positive valence to monovalent Ag + d the track is completely filled. When Ag is present + When an electron from a ligand is received to form a coordinate bond, one 5s orbital and a 5p orbital are hybridized and changed into two degenerate sp orbitals, the two degenerate sp orbitals can receive a lone electron pair provided by urea to form a complex, and a carbonyl group on the urea can form a complex with Ag + And (4) matching. C of carbonyl in urea is electropositive, so that p-pi conjugation exists between lone-pair electrons of amino and pi bond of carbonyl, the O electron density is increased, and Ag + coordinated with O is influenced by the electron density of coordinated O atoms, and Ag + Become easily reduced, facilitating the reduction of Ag + And (3) carrying out the reaction.
(2) According to the invention, urea is used for replacing halogen ions as a control agent, so that the purity of the synthesized silver nanowire is higher, and the associated silver nanoparticles are fewer.
(3) The synthesis steps for preparing the silver nanowires are simple and convenient, and the repeatability is good.
Drawings
Fig. 1 is sem (a) and XRD patterns (b) of silver nanowires prepared in example 1 of the present invention;
FIG. 2 is SEM (a) and TEM images (b) of silver nanowires prepared in example 2 of the present invention;
FIG. 3 is an SEM of silver nanowires prepared according to example 3 of the present invention, with a scale of 5 μm;
FIG. 4 is an SEM image of silver nanowires prepared in example 3 of the present invention, with scales of 7 μm (a) and an EDS image (b);
fig. 5 is an sem (a) and diameter distribution histogram (b) of silver nanowires prepared in example 4 of the present invention;
fig. 6 is a UV-vis (a) and SEM image (b) of silver nanowires prepared in example 5 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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.
The instrument information used in the present invention is as follows:
the electronic balance is an electronic balance manufactured by Mettler-Tollido instruments Inc. and having a model of ME104E, the magnetic heating stirrer is a magnetic heating stirrer manufactured by Aika (Guangzhou) instruments and equipment Inc. and having a model of IKA RCT basic, the desk-top high-speed centrifuge is a desk-top high-speed centrifuge manufactured by Hunan instruments laboratory Inc. and having a model of TG16-WS, the ultrasonic cleaner is an ultrasonic cleaner manufactured by Kunshan ultrasonic instruments Inc. and having a model of KQ5200, the vacuum drying oven is a vacuum drying oven manufactured by Shanghai Hengscience instruments Inc. and having a model of DZK-6250, the ultraviolet spectrophotometer is an ultraviolet spectrophotometer manufactured by UV-8010 PLUS manufactured by Japan Shimadzu corporation, the scanning electron microscope is a scanning electron microscope manufactured by HITACHI and having a model of SU 0, and an X-ray Energy Dispersive Spectrometer (EDS) is used for analyzing the elemental composition of a sample.
The reagent information used in the present invention is as follows:
urea of the formula CO (NH) 2 ) 2 The manufacturer is an alatin reagent; the purity of the reagent is AR, the silver nitrate and the molecular formula is AgNO 3 The purity of the reagent is more than or equal to 99.8 percent, and the manufacturer is a majo chemical reagent factory in Tianjin; ethylene Glycol (EG) of the formula (CH) 2 OH) 2 The purity of the reagent is more than or equal to 98.5 percent, and the manufacturer is a majo chemical reagent factory in Tianjin; polyvinylpyrrolidone (PVP) of formula (C) 6 H 9 NO) n The purity of the reagent is AR, and the manufacturer is an Aladdin reagent; absolute ethyl alcohol with molecular formula C 2 H 5 OH, the purity of the reagent AR is more than or equal to 99.7 percent, and the manufacturer is Tianjin Daimao chemical reagent factory.
Example 1
Step 3, purifying and separating AgNWs stock solution: purification was carried out as follows:
transferring the prepared AgNWs mother liquor to a 50.00mL centrifuge tube, adding ethanol with the volume equivalent to 3 times of the volume of the AgNWs mother liquor, performing ultrasonic treatment for 10min to uniformly disperse the AgNWs mother liquor to obtain a mixture A, performing centrifugal separation for 10min at the rotating speed of 4000rpm, and removing supernatant to obtain a precipitate X1;
step (2), adding ethanol with the volume equivalent to 3 times of that of X1 into X1, performing ultrasonic treatment for 10min to uniformly disperse the ethanol to obtain a mixture B,
and (3) repeating the step (2) for 3 times to obtain the purified silver nanowires.
The purified AgNWs are dispersed in a small amount of ethanol and are characterized by a scanning electron microscope, and the result is shown in figure 1, and the AgNWs synthesized under the condition has high purity reaching 92%. From the XRD pattern, it can be seen that AgNWs is crystalline intact and in a decahedral structure.
Example 2
Step 3, purifying and separating AgNWs stock solution: purification was carried out as follows:
transferring the prepared AgNWs mother liquor to a 50.00mL centrifuge tube, adding ethanol with the volume equivalent to 3 times of the volume of the AgNWs mother liquor, performing ultrasonic treatment for 10min to uniformly disperse the AgNWs mother liquor to obtain a mixture A, performing centrifugal separation for 10min at the rotating speed of 4000rpm, and removing supernatant to obtain a precipitate X1;
step (2), adding ethanol with the volume equivalent to 3 times of that of X1 into X1, performing ultrasonic treatment for 10min to uniformly disperse the ethanol to obtain a mixture B,
and (3) repeating the step (2) for 3 times to obtain the purified silver nanowire.
The purified AgNWs were dispersed in a small amount of ethanol and characterized by scanning electron microscopy, see FIG. 2, under which conditions AgNWs had an average diameter of 82nm and an average length of 35 μm.
Example 3
Step 3, purifying and separating AgNWs stock solution: purification was carried out as follows:
transferring the prepared AgNWs mother liquor to a 50.00mL centrifuge tube, adding ethanol with the volume equivalent to 3 times of the volume of the AgNWs mother liquor, performing ultrasonic treatment for 10min to uniformly disperse the AgNWs mother liquor to obtain a mixture A, performing centrifugal separation for 10min at the rotating speed of 4000rpm, and removing supernatant to obtain a precipitate X1;
step (2), adding ethanol with the volume equivalent to 3 times of that of X1 into X1, performing ultrasonic treatment for 10min to uniformly disperse the ethanol to obtain a mixture B,
and (3) repeating the step (2) for 3 times to obtain the purified silver nanowire.
The purified AgNWs was dispersed in a small amount of ethanol and characterized by scanning electron microscopy, and the results are shown in fig. 3 and fig. 4, where the scale of the scan of fig. 3 is 5 μm and the scale of the scan of fig. 4 is 7 μm, and where the EDS result of fig. 4b was obtained from the scan of fig. 4a, the prepared AgNWs was associated with fewer silver nanoparticles, and the mass fraction of AgNWs was 87%.
Example 4
Step 3, purifying and separating AgNWs stock solution: purification was carried out as follows:
transferring the prepared AgNWs mother liquor to a 50.00mL centrifuge tube, adding ethanol with the volume equivalent to 3 times of the volume of the AgNWs mother liquor, performing ultrasonic treatment for 10min to uniformly disperse the AgNWs mother liquor to obtain a mixture A, performing centrifugal separation for 10min at the rotating speed of 4000rpm, and removing supernatant to obtain a precipitate X1;
step (2), adding ethanol with the volume equivalent to 3 times of that of X1 into X1, performing ultrasonic treatment for 10min to uniformly disperse the ethanol to obtain a mixture B,
and (3) repeating the step (2) for 3 times to obtain the purified silver nanowire.
The purified AgNWs was dispersed in a small amount of ethanol and characterized by scanning electron microscopy, and the results are shown in fig. 5, from which it can be seen that the AgNWs had an average diameter of 87.45nm and a length of 32 μm.
Example 5
Step 3, purifying and separating AgNWs stock solution: purification was carried out as follows:
transferring the prepared AgNWs mother liquor to a 50.00mL centrifuge tube, adding ethanol with the volume equivalent to 3 times of the volume of the AgNWs mother liquor, performing ultrasonic treatment for 10min to uniformly disperse the AgNWs mother liquor to obtain a mixture A, performing centrifugal separation for 10min at the rotating speed of 4000rpm, and removing supernatant to obtain a precipitate X1;
step (2), adding ethanol with the volume equivalent to 3 times of that of X1 into X1, performing ultrasonic treatment for 10min to uniformly disperse the ethanol to obtain a mixture B,
and (3) repeating the step (2) for 3 times to obtain the purified silver nanowire.
The purified AgNWs are dispersed in a small amount of ethanol, and are characterized by an ultraviolet spectrum and a scanning electron microscope, and the result is shown in figure 6, the AgNWs synthesized under the condition detects an AgNWs ultraviolet absorption peak at 380nm, and the shape of the AgNWs is sharp and narrow, which shows that the purity of the AgNWs is high.
Example 6
Step 3, purifying and separating AgNWs stock solution: purification was carried out as follows:
transferring the prepared AgNWs mother liquor to a 50.00mL centrifuge tube, adding ethanol with the volume equivalent to 3 times of the volume of the AgNWs mother liquor, performing ultrasonic treatment for 10min to uniformly disperse the AgNWs mother liquor to obtain a mixture A, performing centrifugal separation for 10min at the rotating speed of 4000rpm, and removing supernatant to obtain a precipitate X1;
step (2), adding ethanol with the volume equivalent to 3 times of that of X1 into X1, carrying out ultrasonic treatment for 10min to uniformly disperse the ethanol to obtain a mixture B,
and (3) repeating the step (2) for 2 times to obtain the purified silver nanowires.
Example 7
Step 3, purifying and separating AgNWs stock solution: purification was carried out as follows:
transferring the prepared AgNWs mother liquor to a 50.00mL centrifuge tube, adding ethanol with the volume equivalent to 3 times of the volume of the AgNWs mother liquor, performing ultrasonic treatment for 10min to uniformly disperse the AgNWs mother liquor to obtain a mixture A, performing centrifugal separation for 10min at the rotating speed of 4000rpm, and removing supernatant to obtain a precipitate X1;
step (2), adding ethanol with the volume equivalent to 3 times of that of X1 into X1, carrying out ultrasonic treatment for 10min to uniformly disperse the ethanol to obtain a mixture B,
and (3) repeating the step (2) for 5 times to obtain the purified silver nanowire.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (8)
1. A preparation method of silver nanowires reduced by urea is characterized by comprising the following steps:
step 1, preparing a solution
Adding urea and silver nitrate into ethylene glycol, stirring at normal temperature until the urea and the silver nitrate are dissolved, performing ultrasonic treatment for 10-20min to obtain a solution A, and performing continuous ice bath on the solution A for later use; wherein, the concentration of the urea is 3.2-4.4g/L, and the concentration of the silver nitrate is 17 g/L;
adding polyvinylpyrrolidone into ethylene glycol, and stirring at normal temperature until the polyvinylpyrrolidone is dissolved to obtain a solution B for later use; wherein the concentration of the polyvinylpyrrolidone is 6.25-9.38 g/L;
step 2, high temperature reaction
Preheating the solution B at the temperature of 150- 2 Stirring, standing and preserving heat to obtain silver nanowire mother liquor;
and 3, centrifuging the silver nanowire mother liquor to obtain a precipitate, and purifying the precipitate to obtain the silver nanowires.
2. The method of claim 1, wherein step 3 comprises the following steps:
adding ethanol into the silver nanowire mother liquor, and performing ultrasonic treatment until the mixture is uniformly dispersed to obtain a mixed solution A; centrifuging the mixed solution to obtain a precipitate, wherein the precipitate is X1;
step (2), adding ethanol into X1, and performing ultrasonic treatment until the mixture is uniformly dispersed to obtain a mixed solution B; centrifuging the mixed solution to obtain a precipitate, wherein the precipitate is X2;
and (3) repeating the step (2) for 2-4 times to obtain the purified silver nanowire.
3. The method for preparing silver nanowires through urea reduction according to claim 1, wherein in the step 2, the volume ratio of the solution A to the solution B is 1: 1.
4. The method according to claim 3, wherein in the step 2, the dripping rate of the solution A is 0.15mL/min, and the dripping time is 10 min.
5. The method of claim 4, wherein in step 2, N is N 2 The flow rate of (2) was 65 mL/min.
6. The method for preparing urea-reduced silver nanowires according to claim 5, wherein in the step 2, the stirring speed in the steps (1) and (2) is 400 rpm.
7. The method of claim 6, wherein in step 2, solution B is preheated to 150 ℃ and incubated for 30 min.
8. The method for preparing silver nanowires through urea reduction according to claim 7, wherein in the step 2, the standing and heat preservation time in the step 2 is 1.5 h.
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| CN104870361A (en) * | 2012-12-14 | 2015-08-26 | 率路技术株式会社 | Method for manufacturing silver nanowires using ionic liquid |
| CN103203468B (en) * | 2013-04-17 | 2016-05-25 | 苏州冷石纳米材料科技有限公司 | A kind of preparation method of nano silver wire |
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