CN113714509A - 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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- 239000002042 Silver nanowire Substances 0.000 title claims abstract description 98
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000004202 carbamide Substances 0.000 title claims abstract description 32
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000243 solution Substances 0.000 claims abstract description 89
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 66
- 238000003756 stirring Methods 0.000 claims abstract description 38
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 16
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 16
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 16
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 90
- 239000012452 mother liquor Substances 0.000 claims description 27
- 238000009210 therapy by ultrasound Methods 0.000 claims description 27
- 239000000203 mixture Substances 0.000 claims description 19
- 239000002244 precipitate Substances 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 11
- 239000011259 mixed solution Substances 0.000 claims description 8
- 230000009467 reduction Effects 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 8
- 229910052709 silver Inorganic materials 0.000 abstract description 8
- 239000004332 silver Substances 0.000 abstract description 8
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 238000003786 synthesis reaction Methods 0.000 abstract description 5
- 239000010413 mother solution Substances 0.000 abstract 2
- 239000002245 particle Substances 0.000 abstract 1
- 150000003672 ureas Chemical class 0.000 abstract 1
- 235000019441 ethanol Nutrition 0.000 description 28
- 239000003153 chemical reaction reagent Substances 0.000 description 11
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 8
- 238000000746 purification Methods 0.000 description 7
- 238000000926 separation method Methods 0.000 description 7
- 239000011550 stock solution Substances 0.000 description 7
- 239000006228 supernatant Substances 0.000 description 7
- 238000012986 modification Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000004626 scanning electron microscopy Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- ISAOCJYIOMOJEB-UHFFFAOYSA-N benzoin Chemical compound C=1C=CC=CC=1C(O)C(=O)C1=CC=CC=C1 ISAOCJYIOMOJEB-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 244000028419 Styrax benzoin Species 0.000 description 1
- 235000000126 Styrax benzoin Nutrition 0.000 description 1
- 235000008411 Sumatra benzointree Nutrition 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229960002130 benzoin Drugs 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000021615 conjugation Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000019382 gum benzoic Nutrition 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- -1 halogen ions Chemical class 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 238000004917 polyol method Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 230000005641 tunneling Effects 0.000 description 1
- 238000002211 ultraviolet spectrum Methods 0.000 description 1
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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
- 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
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heating 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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
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Abstract
本发明公开一种尿素还原的银纳米线及其制备方法和用途，属于纳米材料合成技术领域。这种尿素还原的银纳米线的制备方法是：先配置溶液，将尿素与硝酸银加入乙二醇中，常温下搅拌30‑40min直至溶解，超声10‑20min后，得到溶液A，对溶液A持续冰浴，备用；将聚乙烯吡咯烷酮加入乙二醇中，常温下搅拌30‑40min直至溶解，得到溶液B，备用；然后进行高温反应，将溶液B预热150‑180℃并进行保温，将溶液A滴注到反应溶液中，通入N2并进行搅拌，静置保温，得到银纳米线母液；最后，对银纳米线母液进行处理得到银纳米线。本发明制备方法简便，重复性好，制备的银纳米线纯度高，伴生的银纳米颗粒较少，制备成本低。
The invention discloses a urea-reduced silver nanowire, a preparation method and application thereof, and belongs to the technical field of nanomaterial synthesis. The preparation method of this urea-reduced silver nanowires is: first configure a solution, add urea and silver nitrate into ethylene glycol, stir at room temperature for 30-40min until dissolving, after ultrasonic 10-20min, obtain solution A, to solution A Continue the ice bath for standby; add polyvinylpyrrolidone to ethylene glycol, stir at room temperature for 30-40min until dissolved, and obtain solution B, which is for later use; then carry out high-temperature reaction, preheat solution B to 150-180 ℃ and keep warm, and Solution A is dripped into the reaction solution, poured into N 2 and stirred, and kept at rest to obtain a silver nanowire mother solution; finally, the silver nanowire mother solution is processed to obtain silver nanowires. The preparation method of the invention has the advantages of simple and convenient preparation method, good repeatability, high purity of the prepared silver nanowires, less accompanying silver nanometer particles, 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)7S/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 having a diameter of 10-200nm and a length of 5-100 μm. 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 found that silver nanowires (AgNWs) not only satisfy excellent electrical conductivity and thermal conductivity required for conductive materials, but also have good flexibility, chemical 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 nucleusThe central goal is to reduce costs.
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 150-2Stirring, 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 processed 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 is2The 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 the use of silver nanowires for the preparation of transparent electric heaters.
Compared with the prior art, the invention has the following beneficial effects:
(1) during the synthesis of silver nanowires, Ag is used as a transition metal, and the electrons of Ag are arranged as [ Kr]4d105s1Positive valence to monovalent Ag+d the track is completely filled. When Ag is present+When an electron from a ligand is accepted to form a coordination bond, one 5s orbital and a 5p orbital are hybridized to be 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, so that O electron density is increased, and Ag + coordinated with O is influenced by electron density of coordinated O atom, so that 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 a 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 development 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 Nippon Shimadzu corporation and having a model of UV-3600PLUS, the scanning electron microscope is a scanning electron microscope manufactured by HITACHICHI and having a model of SU8010, and the elemental composition of the sample is analyzed by an X-ray Energy Dispersive Spectrometer (EDS).
The reagent information used in the present invention is as follows:
urea of the formula CO (NH)2)2The manufacturer is an alatin reagent; the purity of the reagent is AR, silver nitrate and the molecular formula is AgNO3The 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)2OH)2The 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)6H9NO)nThe purity of the reagent is AR, and the manufacturer is an Aladdin reagent; absolute ethyl alcohol with molecular formula C2H5OH, 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 nanowire.
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 were 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 FIG. 6, the AgNWs synthesized under the condition has a sharp and narrow shape and detects an AgNWs ultraviolet absorption peak at 380nm, which indicates 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, performing 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 nanowire.
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, performing 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 (10)
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, 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; 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 150-2Stirring, 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 N2The 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 for preparing silver nanowires through urea reduction according to claim 6, wherein the solution B is preheated to 150 ℃ and kept for 30min in the step 2.
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.
9. Silver nanowires produced by the method of any one of claims 1 to 8, wherein the silver nanowires have an average diameter of 82 to 87.45nm and a length of 32 to 35 μm.
10. Use of a silver nanowire as defined in claim 9 for the preparation of a transparent electric heater.
Priority Applications (1)
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| CN116275084A (en) * | 2023-03-28 | 2023-06-23 | 西北大学 | A kind of silver nanoparticle that urea participates in and its preparation method and application |
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