CN117798372A - Method for synthesizing silver nanowires by converting particles - Google Patents
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- CN117798372A CN117798372A CN202211162115.1A CN202211162115A CN117798372A CN 117798372 A CN117798372 A CN 117798372A CN 202211162115 A CN202211162115 A CN 202211162115A CN 117798372 A CN117798372 A CN 117798372A
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 239000002042 Silver nanowire Substances 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 35
- 239000002245 particle Substances 0.000 title claims abstract description 24
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 11
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims abstract description 58
- 238000006243 chemical reaction Methods 0.000 claims abstract description 47
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229910052709 silver Inorganic materials 0.000 claims abstract description 36
- 239000004332 silver Substances 0.000 claims abstract description 36
- 239000002105 nanoparticle Substances 0.000 claims abstract description 30
- 239000008367 deionised water Substances 0.000 claims abstract description 24
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 24
- 239000007787 solid Substances 0.000 claims abstract description 20
- 238000005406 washing Methods 0.000 claims abstract description 18
- 239000006185 dispersion Substances 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 230000001105 regulatory effect Effects 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 43
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 40
- 239000007864 aqueous solution Substances 0.000 claims description 30
- 239000003638 chemical reducing agent Substances 0.000 claims description 17
- 239000003223 protective agent Substances 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000005119 centrifugation Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 239000001509 sodium citrate Substances 0.000 claims description 7
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims description 7
- 229940038773 trisodium citrate Drugs 0.000 claims description 7
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- AYKOTYRPPUMHMT-UHFFFAOYSA-N silver;hydrate Chemical compound O.[Ag] AYKOTYRPPUMHMT-UHFFFAOYSA-N 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 3
- -1 and in the step 3) Inorganic materials 0.000 claims description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 2
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 239000008103 glucose Substances 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical group N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 2
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- 239000012266 salt solution Substances 0.000 claims 1
- 238000009826 distribution Methods 0.000 abstract description 4
- 239000003153 chemical reaction reagent Substances 0.000 abstract 2
- 239000013078 crystal Substances 0.000 description 19
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical group [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 12
- 239000002159 nanocrystal Substances 0.000 description 10
- 230000015572 biosynthetic process Effects 0.000 description 8
- 239000002070 nanowire Substances 0.000 description 6
- 229910001961 silver nitrate Inorganic materials 0.000 description 6
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 5
- 230000007547 defect Effects 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 239000008346 aqueous phase Substances 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 229920005862 polyol Polymers 0.000 description 3
- 150000003077 polyols Chemical class 0.000 description 3
- 238000001308 synthesis method Methods 0.000 description 3
- 239000003513 alkali Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Abstract
The invention discloses a method for synthesizing silver nanowires by converting particles, which comprises the following steps: mixing a reducing reagent, a protecting reagent and water, regulating the pH value to 7-13 to obtain a reaction solution, heating the reaction solution to 60-100 ℃, adding silver salt water solution into the reaction solution under the stirring condition, continuously stirring for 1-5 h to obtain silver nanoparticle sol, cooling the silver nanoparticle sol to room temperature, centrifuging, washing and centrifuging the obtained solid, and dispersing the washed solid in deionized water to obtain silver nanoparticle dispersion; the method is simple, the reaction conditions are easy to control, the diameter distribution can be within 20-220nm, the length distribution can be within 1-20 mu m, and the superfine silver nanowires can be prepared.
Description
Technical Field
The invention belongs to the technical field of nanowire preparation, and particularly relates to a method for synthesizing silver nanowires through particle transformation.
Background
The flexible electronic industry has huge market scale reaching the billions of dollars, and has reuse application in the fields of flexible display, wearable equipment, intelligent home and the like. Silver nanowires are a key material in flexible electronics, and are cores for realizing the performances of flexibility, conductivity, light transmittance and the like of the materials. The diameter and length of the silver nanowire are closely related to the performance of the flexible electronic equipment, and key performances such as conductivity, flexibility and the like are directly determined. In general, flexible electrons, especially transparent conductive films, prepared from silver nanowires with longer lengths and finer diameters can have higher conductivity, higher optical transmittance and lower haze.
The current preparation method of silver nanowires mainly uses a polyol reduction method. The method for preparing the silver nanowires needs to be under high temperature conditions and utilizes organic solvents such as polyalcohols and the like. The development of the low-temperature preparation method based on the aqueous phase system can avoid the massive use of organic matters and the high-temperature environment, develop the green synthesis method and reduce the environmental pollution and the energy consumption. In addition, silver nanowires produced by the polyol reduction process are often accompanied by a large number of silver nanoparticles. The pure silver nanowire is obtained by a complicated purification process, so that the synthesis cost of the silver nanowire is greatly increased.
In addition to the polyol synthesis method, there is also reported a patent (application No. 201610945221.5) for synthesizing silver nanowires in aqueous phase, which induces seed crystals by blue light illumination, simultaneously screens the seed crystals with hydrogen peroxide, and subsequently obtains ultrafine silver nanowires through multiple rounds of growth. The hydrogen peroxide used in the method is used for screening decahedron seed crystals, so that the yield of the nanowires is improved, but the formation of particles and other morphologies cannot be completely prevented, and the silver nanowire products with higher purity can be obtained only after separation and purification treatment is still needed. In addition, the method needs blue light irradiation, hydrogen peroxide screening seed crystal, multiple circulation growth, complicated process, difficulty in improving production efficiency and adverse mass synthesis. Therefore, there is a need to optimize and improve the synthesis method of the aqueous phase silver nanowires, and improve the synthesis efficiency of the silver nanowires, so as to adapt to the industrial development requirements of the silver nanowires.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for synthesizing silver nanowires by converting particles, which is based on a water phase system to convert the particle nano silver into silver nanowires, and can convert silver salt particles with particle morphology into silver nanowires with one-dimensional morphology by utilizing hydrogen peroxide in water solution, so that the water phase synthesis of the silver nanowires is realized, the technical route adopted by the method is simple, and the reaction process is easy to control.
The aim of the invention is achieved by the following technical scheme.
A method for synthesizing silver nanowires by conversion of particles, comprising the steps of:
1) Mixing a reducing agent, a protecting agent and water, and regulating the pH value to 7-13 to obtain a reaction solution, wherein the reducing agent is one or more than two of formaldehyde, glucose, hydroxylamine and trisodium citrate, the protecting agent is one or more than two of trisodium citrate, polyvinylpyrrolidone (PVP) and Sodium Dodecyl Sulfate (SDS), the concentration of the reducing agent in the reaction solution is 0.02-0.20M, and the concentration of the protecting agent in the reaction solution is 0.10-2.00 wt%;
in the step 1), the concentration of the reducing agent in the reaction solution is 0.1M, and the concentration of the protecting agent in the reaction solution is 0.5wt%.
In the step 1), the pH value is regulated to 12 by adopting alkali, wherein the alkali is ammonia water or sodium hydroxide.
2) Heating the reaction solution to 60-100 ℃, adding silver salt water solution into the reaction solution under stirring, and continuing stirring for 1-5 h to obtain silver nanoparticle sol, wherein the concentration of silver salt in the silver salt water solution is 0.025-0.080M, and the silver salt water solution is 3-6% of the reaction solution by volume;
in the step 2), the silver salt aqueous solution is a mixture of silver salt and water, and the size of silver salt particles in the silver salt aqueous solution is 20-200 nm.
In the step 2), the concentration of silver salt in the silver salt aqueous solution is 0.045M.
In the step 2), the silver salt is silver nitrate.
In the step 2), the temperature of the reaction solution is raised to 80 to 90 ℃.
3) Cooling the silver nanoparticle sol to room temperature, centrifuging, washing and centrifuging the obtained solid, and dispersing the washed solid in deionized water to obtain silver nanoparticle dispersion liquid;
in the step 3), deionized water is used for the washing.
In the step 3), the room temperature is 20 to 25 ℃.
In the step 3), the speed of the centrifugation is 3000 to 10000rpm, preferably 5000 to 10000rpm.
In the step 3), the centrifugation time is 5 to 30 minutes, preferably 10 minutes.
In the step 3), the ratio (0.002-0.01) of the parts by volume of the silver in the silver salt aqueous solution to the parts by volume of the deionized water in the step 3): 1, wherein the unit of the parts by volume of the substances is mol, and the unit of the parts by volume is L.
In the above technical solution, the ratio of the parts by weight of silver in the silver salt aqueous solution to the parts by volume of deionized water in the step 3) is 0.005:1.
4) Dropwise adding hydrogen peroxide aqueous solution with the concentration of 10-30wt% into the silver nanoparticle dispersion obtained in the step 3) to obtain silver nanowire sol, centrifuging, washing and centrifuging the obtained solid to obtain silver nanowires, wherein the hydrogen peroxide aqueous solution is 3-10wt% of the silver nanoparticle dispersion liquid by volume.
In the step 4), the concentration of the aqueous hydrogen peroxide solution is 18wt%.
In the step 4), the rate of dropping the aqueous hydrogen peroxide solution is 0.1 to 10mL/min, preferably 1mL/min.
In the step 4), deionized water is used for washing.
Silver nanowires obtained by the above method.
In the technical scheme, the diameter of the silver nanowire is 20-220nm, and the average diameter of the silver nanowire is 40nm.
Compared with the prior art, the method is simple, the reaction condition is easy to control, the diameter distribution of the method can be within the range of 20-220nm, the length distribution of the method is within the range of 1-20 mu m, and the method can be used for preparing the superfine silver nanowires.
Drawings
FIG. 1 is an SEM of silver nanowires prepared in example 1;
FIG. 2 is an SEM of silver nanowires prepared in example 2;
fig. 3 is an SEM of silver nanowires prepared in example 3.
Detailed Description
The technical scheme of the invention is further described below with reference to specific embodiments.
Deionized water was used for the water in the examples below.
The drugs in the examples described below were purchased from the national drug group and were chemically pure (AR).
Example 1
A method for synthesizing silver nanowires by conversion of particles, comprising the steps of:
1) Mixing a reducing agent, a protecting agent and water, adding ammonia water with the concentration of 22wt% to adjust the pH value to 9.4, and obtaining a reaction solution with stronger reducing capability, wherein the reducing agent is formaldehyde, the protecting agent is trisodium citrate, the concentration of the reducing agent in the reaction solution is 100mM, and the concentration of the protecting agent in the reaction solution is 0.5wt%;
2) Heating the reaction solution to 80 ℃, adding silver salt aqueous solution into the reaction solution under stirring, and continuing stirring for 1h to obtain silver nanoparticle sol, wherein the size of silver salt particles in the silver salt aqueous solution is 20-200 nm, and the silver salt particles are approximately spherical, the silver salt aqueous solution is a mixture of silver salt and water, the silver salt is silver nitrate, the concentration of the silver salt in the silver salt aqueous solution is 0.045M, and the silver salt aqueous solution is 5% of the reaction solution by volume;
3) Cooling the silver nanoparticle sol to room temperature of 20-25 ℃, centrifuging at 5000rpm for 10min, washing the solid obtained by centrifugation by adopting deionized water, and dispersing the solid obtained by washing in the deionized water to obtain silver nanoparticle dispersion liquid, wherein the ratio of the parts by volume of silver in the silver salt aqueous solution in the step 2) to the parts by volume of the deionized water used for dispersing the solid in the step 3) is 0.005:1, the unit of the parts by weight of substances is mol, and the unit of the parts by volume is L;
4) And 3) dropwise adding an aqueous hydrogen peroxide solution with the concentration of 18wt% into the silver nanoparticle dispersion obtained in the step 3), generating a large amount of bubbles in the dropwise adding process to obtain silver nanowire sol, centrifuging, washing and centrifuging the obtained solid by deionized water to obtain silver nanowires, wherein the aqueous hydrogen peroxide solution is 5% of the silver nanoparticle dispersion by volume, and the speed of dropwise adding the aqueous hydrogen peroxide solution is 1mL/min (the dropwise adding is completed in 10 min).
Silver nanowires as shown in fig. 1, the silver nanowires were about 70nm in diameter and 8.0 μm in average length.
Example 2
A method for synthesizing silver nanowires by conversion of particles, comprising the steps of:
1) Mixing a reducing agent, a protecting agent and water, and adding sodium hydroxide to adjust the pH value to 12 to obtain a reaction solution with stronger reducing capability, wherein the reducing agent is formaldehyde, the protecting agent is trisodium citrate, the concentration of the reducing agent in the reaction solution is 100mM, and the concentration of the protecting agent in the reaction solution is 0.5wt%;
2) Heating the reaction solution to 90 ℃, adding silver salt aqueous solution into the reaction solution under stirring, and continuing stirring for 1h to obtain silver nanoparticle sol, wherein the size of silver salt particles in the silver salt aqueous solution is 20-200 nm, and the silver salt particles are approximately spherical, the silver salt aqueous solution is a mixture of silver salt and water, the silver salt is silver nitrate, the concentration of the silver salt in the silver salt aqueous solution is 0.045M, and the silver salt aqueous solution is 5% of the reaction solution by volume;
3) Cooling the silver nanoparticle sol to room temperature of 20-25 ℃, centrifuging at 10000rpm for 10min, washing the solid obtained by centrifugation by adopting deionized water, and dispersing the solid obtained by washing in the deionized water to obtain silver nanoparticle dispersion liquid, wherein the ratio of the parts by volume of silver in the silver salt aqueous solution in the step 2) to the parts by volume of the deionized water used for dispersing the solid in the step 3) is 0.005:1, the unit of the parts by weight of substances is mol, and the unit of the parts by volume is L;
4) And 3) dropwise adding an aqueous hydrogen peroxide solution with the concentration of 18wt% into the silver nanoparticle dispersion obtained in the step 3), generating a large amount of bubbles in the dropwise adding process to obtain silver nanowire sol, centrifuging, washing and centrifuging the obtained solid by deionized water to obtain silver nanowires, wherein the aqueous hydrogen peroxide solution is 5% of the silver nanoparticle dispersion by volume, and the speed of dropwise adding the aqueous hydrogen peroxide solution is 1mL/min (the dropwise adding is completed in 10 min). The silver nanowires are shown in FIG. 2, and the diameter of the silver nanowires can be as thin as 24nm, and the length of the silver nanowires is 15 mu m.
In the embodiment, under the condition of higher pH value, the reduction speed of the silver nitrate is high, and the silver nitrate can be quickly subjected to nuclear growth to obtain the nanocrystalline particles with smaller diameters, wherein the nanocrystalline particles comprise multiple twin crystals, single twin crystals and monocrystalline silver nanoparticles. During the conversion of the particles into silver nanowires, multiple twins of smaller diameter enable finer silver nanowires to be obtained.
Silver has very low stacking fault defect energy, and various defect structures based on stacking fault defects are very easy to form in a nucleation stage, wherein the defect structures comprise single-twin crystal structures, multiple-twin crystal structures and single-crystal structure nanocrystals. After growth, the single twin structure nanocrystals can grow into a two-dimensional platelet morphology, such as a triangular nanoplatelet. And the multiple twin crystal structure nano crystal is grown to obtain a one-dimensional nano rod or nano wire. The single crystal structure nanocrystalline can be converted into a cube or octahedral polyhedron shape through growth. The method of the invention utilizes the reducing agent to quickly reduce and obtain the silver nano-particles, and the obtained silver nano-particles have various structures, including single crystal nano-crystals, single twin crystal nano-crystals, five twin crystal nano-crystals and the like. The preparation of the nanowire is realized by utilizing the one-dimensional growth habit of the decahedron nanocrystalline (multiple twin crystals). The formation of decahedral nanocrystals is related to nucleation rate, and the synthesized silver nanoparticles often contain a certain proportion of decahedral nanocrystals.
Under certain conditions, hydrogen peroxide may be either oxidizing or reducing. Under proper conditions, single twin and single crystalsNanocrystals are unstable in the presence of hydrogen peroxide and are easily oxidized to metal ions (Ag + ) The hydrogen peroxide is subjected to this process to obtain electrons, which form hydroxide ions (OH). The formation of hydroxide ions enhances the reducing power of hydrogen peroxide, which in turn can re-reduce the ag+ formed to metal. Therefore, the total reaction in the solution is that the hydrogen peroxide oxidizes unstable particles in the metal nano-particles into metal ions, and simultaneously reduces the newly formed metal ions into a growth source of stable metal particles (multiple twin crystals), namely, the reaction is used for sacrificing unstable single crystals and single twin crystal nano-crystals, so that the stable growth of the multiple twin crystal nano-crystals is realized, and finally, the synthesis of the nano-wires is obtained.
Example 3
A method for synthesizing silver nanowires by conversion of particles, comprising the steps of:
1) Mixing a reducing agent, a protecting agent and water, adding ammonia water with the concentration of 22wt% to adjust the pH value to 9.4, and obtaining a reaction solution with stronger reducing capability, wherein the reducing agent is formaldehyde, the protecting agent is trisodium citrate, the concentration of the reducing agent in the reaction solution is 100mM, and the concentration of the protecting agent in the reaction solution is 0.5wt%;
2) Heating the reaction solution to 80 ℃, adding silver salt aqueous solution into the reaction solution under stirring, and continuing stirring for 1h to obtain silver nanoparticle sol, wherein the size of silver salt particles in the silver salt aqueous solution is 20-200 nm, and the silver salt particles are approximately spherical, the silver salt aqueous solution is a mixture of silver salt and water, the silver salt is silver nitrate, the concentration of the silver salt in the silver salt aqueous solution is 0.045M, and the silver salt aqueous solution is 5% of the reaction solution by volume;
3) Cooling the silver nanoparticle sol to room temperature of 20-25 ℃, centrifuging at 5000rpm for 10min, washing the solid obtained by centrifugation by adopting deionized water, and dispersing the solid obtained by washing in the deionized water to obtain silver nanoparticle dispersion liquid, wherein the ratio of the parts by volume of silver in the silver salt aqueous solution in the step 2) to the parts by volume of the deionized water used for dispersing the solid in the step 3) is 0.005:1, the unit of the parts by weight of substances is mol, and the unit of the parts by volume is L;
4) And 3) dropwise adding an aqueous hydrogen peroxide solution with the concentration of 18wt% into the silver nanoparticle dispersion obtained in the step 3), generating a large amount of bubbles in the dropwise adding process to obtain silver nanowire sol, centrifuging, washing and centrifuging the obtained solid by deionized water to obtain silver nanowires, wherein the aqueous hydrogen peroxide solution is 10% of the silver nanoparticle dispersion by volume, and the speed of dropwise adding the aqueous hydrogen peroxide solution is 1mL/min (the dropwise adding is completed in 10 min).
Silver nanowires as shown in fig. 3, the silver nanowires have a diameter of about 200nm and an average length of 2.0 μm. A large amount of hydrogen peroxide is rapidly added, resulting in thicker and shorter nanowires.
The foregoing has described exemplary embodiments of the invention, it being understood that any simple variations, modifications, or other equivalent arrangements which would not unduly obscure the invention may be made by those skilled in the art without departing from the spirit of the invention.
Claims (10)
1. A method for synthesizing silver nanowires by converting particles, comprising the steps of:
1) Mixing a reducing agent, a protecting agent and water, and regulating the pH value to 7-13 to obtain a reaction solution, wherein the reducing agent is one or more than two of formaldehyde, glucose, hydroxylamine and trisodium citrate, the protecting agent is one or more than two of trisodium citrate, polyvinylpyrrolidone and sodium dodecyl sulfate, the concentration of the reducing agent in the reaction solution is 0.02-0.20M, and the concentration of the protecting agent in the reaction solution is 0.10-2.00 wt%;
2) Heating the reaction solution to 60-100 ℃, adding silver salt water solution into the reaction solution under stirring, and continuing stirring for 1-5 h to obtain silver nanoparticle sol, wherein the concentration of silver salt in the silver salt water solution is 0.025-0.080M, and the silver salt water solution is 3-6% of the reaction solution by volume;
3) Cooling the silver nanoparticle sol to room temperature, centrifuging, washing and centrifuging the obtained solid, and dispersing the washed solid in deionized water to obtain silver nanoparticle dispersion liquid;
4) Dropwise adding hydrogen peroxide aqueous solution with the concentration of 10-30wt% into the silver nanoparticle dispersion obtained in the step 3) to obtain silver nanowire sol, centrifuging, washing and centrifuging the obtained solid to obtain silver nanowires, wherein the hydrogen peroxide aqueous solution is 3-10wt% of the silver nanoparticle dispersion liquid by volume.
2. The method according to claim 1, wherein in the step 1), a base is used to adjust the pH, and the base is ammonia or sodium hydroxide.
3. The method according to claim 1, wherein in the step 2), the silver salt aqueous solution is a mixture of silver salt and water, and the silver salt particles in the silver salt aqueous solution have a size of 20 to 200nm.
4. The method according to claim 1, wherein in the step 2), the reaction solution is heated to 80 to 90 ℃, and in the step 3), deionized water is used for the washing.
5. The method according to claim 1, characterized in that in step 3) the speed of centrifugation is 3000-10000 rpm, preferably 5000-10000 rpm, and the time of centrifugation is 5-30 min.
6. The method according to claim 1, wherein in the step 3), a ratio of parts by weight of silver in the silver salt aqueous solution to parts by volume of deionized water in the step 3) (0.002 to 0.01): 1, wherein the unit of the parts by volume of the substances is mol, and the unit of the parts by volume is L.
7. The method of claim 6, wherein the ratio of the parts by volume of silver in the aqueous silver salt solution to the parts by volume of deionized water in step 3) is 0.005:1.
8. the method according to claim 1, wherein in the step 4), the rate of dropping the aqueous hydrogen peroxide solution is 0.1 to 10mL/min; in the step 4), deionized water is used for washing.
9. Silver nanowires obtainable by the process according to any of claims 1 to 8.
10. The silver nanowire according to claim 9, characterized in that the diameter of the silver nanowire is 20-220nm, and the average number of diameters of the silver nanowire is 40nm.
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