KR101780306B1 - method of preparing a silver nanowire and a silver nanowire prepared by using the same - Google Patents
method of preparing a silver nanowire and a silver nanowire prepared by using the same Download PDFInfo
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- KR101780306B1 KR101780306B1 KR1020150191315A KR20150191315A KR101780306B1 KR 101780306 B1 KR101780306 B1 KR 101780306B1 KR 1020150191315 A KR1020150191315 A KR 1020150191315A KR 20150191315 A KR20150191315 A KR 20150191315A KR 101780306 B1 KR101780306 B1 KR 101780306B1
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- silver nanowires
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 91
- 239000002042 Silver nanowire Substances 0.000 title claims abstract description 86
- 238000000034 method Methods 0.000 title claims description 19
- 229910052709 silver Inorganic materials 0.000 claims abstract description 39
- 238000010438 heat treatment Methods 0.000 claims abstract description 37
- 238000004519 manufacturing process Methods 0.000 claims abstract description 31
- 239000007787 solid Substances 0.000 claims abstract description 28
- 229910001316 Ag alloy Inorganic materials 0.000 claims abstract description 22
- 238000001816 cooling Methods 0.000 claims abstract description 21
- 239000000203 mixture Substances 0.000 claims abstract description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000011734 sodium Substances 0.000 description 70
- 239000000243 solution Substances 0.000 description 21
- 229910052708 sodium Inorganic materials 0.000 description 20
- 239000002070 nanowire Substances 0.000 description 15
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 9
- 239000003795 chemical substances by application Substances 0.000 description 9
- 150000003839 salts Chemical class 0.000 description 9
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 8
- 239000007791 liquid phase Substances 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- 239000007790 solid phase Substances 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 239000002243 precursor Substances 0.000 description 5
- 239000004332 silver Substances 0.000 description 5
- 239000012153 distilled water Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000011780 sodium chloride Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000006911 nucleation Effects 0.000 description 3
- 238000010899 nucleation Methods 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 229910052746 lanthanum Inorganic materials 0.000 description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 229920005862 polyol Polymers 0.000 description 2
- 150000003077 polyols Chemical class 0.000 description 2
- 229920006316 polyvinylpyrrolidine Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 101710134784 Agnoprotein Proteins 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 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 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Images
Classifications
-
- 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
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
-
- B22F1/0003—
-
- B22F1/0018—
-
- 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
- B22F2201/00—Treatment under specific atmosphere
- B22F2201/20—Use of vacuum
-
- 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
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/25—Noble metals, i.e. Ag Au, Ir, Os, Pd, Pt, Rh, Ru
- B22F2301/255—Silver or gold
Abstract
The present invention relates to a method of manufacturing silver nanowires, and more particularly, to a method of manufacturing a silver nanowire including a first step of preparing a mixture in which Ag or Ag alloy is melted in an Na solution by adding a molten Na solution to Ag or an Ag alloy; A second step of heating the mixture in a vacuum state and then cooling it to produce a Na coagulated solid containing wire-shaped Ag; And a third step of preparing a silver nanowire by liquefying coagulated solid by adding alcohol to the coagulated solid and then purifying the coagulated solid to remove Na. .
Description
The present invention relates to a method of manufacturing silver nanowires, and more particularly, to a method of manufacturing silver nanowires by which molten Na is added to Ag or an Ag alloy to heat and cool the silver nanowire .
Nanowires are expected to be used in a variety of applications due to their high chemical stability, excellent electrical conductivity, flexibility and permeability.
In particular, it has been found that in the case of silver (Ag) nanowires, the electrical and thermal conductivity of silver (Ag) can be improved by the optical properties and chemical stability, which exhibit the highest surface enhancement Raman efficiency in the visible region, The present invention can be applied to a transparent electrode using a conductive material for various electronic products such as a sensor, a display, a solar cell, and a mobile device.
A method for the manufacture of silver nanowires has been developed. Korean Patent Laid-Open No. 10-2012-0066544 discloses a nanoporous polyvinyl pyrrolidine (PVP) capping agent which induces wire formation in a polyol solvent such as heated propylene glycol (PG) Disclose the preparation of silver nanowires in such solutions by adding a silver salt or a salt containing NaCl as a catalyst and then adding a metal compound (silver precursor).
In the case of the above production method, there is an advantage that the reaction temperature is lowered by using a propylene glycol solvent excellent in reducing power, and the formation of a wire is facilitated while reducing the amount of the capping agent by using a sun salt or a purified salt as a catalyst.
However, in the above-mentioned production method, the capping agent content is lowered by the use of the catalyst, capping agent must be essentially contained in order to prevent agglomeration of substances in the solvent and to form nanowires. In addition, There is a problem that the material or the impurities formed by the above can not be completely removed from the resulting nanowire.
Korean Patent Laid-Open No. 10-2015-0077601 discloses a method for improving the production efficiency of silver nanowires by using a lanthanum-based metal salt as an additive in the production of the nanowire, and suppressing the generation of impurities and particles accompanying it. However, the above manufacturing method uses a lanthanum-based metal salt instead of a salt of sodium chloride or a salt of salt containing NaCl, and still uses a camping agent and a polyol solvent so that the material or the material formed from the obtained nanowire There is a problem that the impurities can not be completely removed.
Conventionally, nanowire manufacturing methods are limited in salt selection. That is, there is a problem that most of the precursors used are limited to silver nitrate (AgNO 3 ) in order to obtain a satisfactory yield in the production of silver nanowires.
Korean Patent Laid-Open Publication No. 10-2015-0072518 discloses a silver nanowire using various silver precursors, so that nanowires can be easily produced even when insoluble or low-solubility precursors are used. do.
However, in the case of the above-mentioned invention, various silver precursors are used, but still water-soluble polymers of NaCl or halides and polyvinylpyrrolidone are used.
SUMMARY OF THE INVENTION Accordingly, it is an object of the present invention to provide a method for manufacturing silver nanowires using molten Na, which can easily produce silver nanowires without using solvents, capping agents and catalysts .
Another object of the present invention is to provide a silver nanowire produced by the above method.
Another object of the present invention is to provide an electronic device manufactured using the silver nanowire.
According to an aspect of the present invention,
A first step of preparing a mixture in which an Ag or Ag alloy is melted in an Na solution by adding a molten Na solution to Ag or an Ag alloy;
A second step of heating the mixture in a vacuum state and then cooling it to produce a Na coagulated solid containing wire-shaped Ag; And
And a third step of preparing a silver nanowire by liquefying coagulated solid by adding alcohol to the coagulated solid and then purifying the solid to remove Na, do.
In another aspect of the present invention, there is provided a silver nanowire produced by the method.
According to another aspect of the present invention, there is provided an electronic device manufactured using the silver nanowire.
According to the silver nanowire production method of the present invention, molten Na solution is added to Ag or Ag alloy having powder or bulk size and heated to 97.7 ~ 880 캜 for at least 1 minute and then cooled to 15 캜 / sec It is possible to produce silver nanowires without the use of a capping agent.
The manufacturing method of the present invention simplifies the manufacturing process compared to the conventional silver nanowire manufacturing method, thereby improving work efficiency, There is an advantage that impurities are not formed on the silver nanowires by preparing silver nanowires using only molten Na without using a solvent, a capping agent and a catalyst.
According to the silver nanowire production method of the present invention, the silver nanowire diameter and length can be changed by controlling the content of Ag or Ag alloy and Na, and controlling the heating temperature and the holding time within the heating temperature range. There is an advantage that silver nanowires of various sizes can be easily manufactured.
1 is a photograph showing a manufacturing process of a silver nanowire according to the present invention.
FIG. 2 is a graph showing a product and a phase change according to a temperature change in the process of manufacturing silver nanowires according to the present invention.
FIG. 3 is a SEM photograph of silver nanowires prepared with different contents of Ag and Na according to an embodiment of the present invention.
FIG. 4 is a histogram showing the diameter and length of silver nanowires prepared by varying the content of Ag and Na according to an embodiment of the present invention.
5 is a SEM photograph of a silver nanowire fabricated at different heating temperatures according to an embodiment of the present invention.
FIG. 6 is a histogram showing the diameter and length of silver nanowires manufactured at different heating temperatures according to an embodiment of the present invention.
FIG. 7 is a SEM photograph of a silver nanowire fabricated with different heating temperature holding times according to an embodiment of the present invention.
FIG. 8 is a histogram showing the diameter and length of silver nanowires manufactured by different heating temperature holding times according to an embodiment of the present invention.
9 is a SEM photograph of silver nanowires manufactured at different cooling rates according to an embodiment of the present invention.
10 is a histogram showing the diameter and length of silver nanowires manufactured at different cooling rates according to an embodiment of the present invention.
The present invention relates to a method of manufacturing silver nanowires, and more particularly, to a method of manufacturing silver nanowires by which molten Na is added to Ag or an Ag alloy to heat and cool the silver nanowire .
Hereinafter, the present invention will be described in detail.
According to an aspect of the present invention,
A first step of preparing a mixture in which an Ag or Ag alloy is melted in an Na solution by adding a molten Na solution to Ag or an Ag alloy; A second step of heating the mixture in a vacuum state and then cooling it to produce a Na coagulated solid containing wire-shaped Ag; And a third step of preparing a silver nanowire by liquefying coagulated solid by reacting the coagulated solid with an alcohol and then purifying the coagulated solid to remove Na. / RTI >
FIG. 1 illustrates a manufacturing process of a silver nanowire according to the present invention. Referring to FIG. 1, a method of manufacturing a nanowire will be described.
In the present invention, the first step in the method for producing silver nanowires is a step of preparing a mixture in which Ag or Ag alloy is melted in an Na solution. This corresponds to steps (a) to (c) of FIG. 1, in which a molten Na solution is added to Ag or an Ag alloy to prepare a mixture in which an Ag or Ag alloy is melted in an Na solution.
In this case, Ag is characterized in that it has a powder or bulk size. Ag alloy is characterized in that Ag contains Sn, Cu, Zn, Pb, In or Bi.
Also, the content of Ag or Ag alloy and Na can be adjusted within a range of 0.01 to 99.99% considering the diameter and length of the nanowires to be manufactured.
Next, in the second step of the present invention, the mixture is heated in a vacuum state and then cooled to produce a Na coagulated solid containing wire-like Ag, which is obtained by the steps (d) and .
Specifically, in the second step, a mixture obtained by melting the Ag or Ag alloy in the Na solution prepared in the first step is heated to 97.7 to 880 캜 in a vacuum state and held (Fig. 1 (d)), / sec at a rate slower than that of the wire-shaped Ag-containing solid (Fig. 1 (e)).
At this time, when the heating temperature is set to 97.7 to 880 캜, there is a problem that Na is not reacted with Ag or Ag alloy when heated to less than 97.7 캜, and when heated to more than 880 캜, Na is vaporized This is because a problem occurs.
In the second step, the heating process is performed at a temperature of 97.7 to 880 캜, and then the heating temperature is maintained for 1 minute or more. This is because, when the heating temperature is maintained at less than 1 minute in the heating process, since the time for allowing the reaction of Na and Ag or Ag alloy is not sufficient, it is not produced in a wire form or is produced in a wire form This is a small amount.
In addition, the cooling process after the heating in the second step is performed at a rate slower than 15 ° C / sec. When the quenching is carried out at a rate higher than 15 ° C / sec after heating to 97.7-880 ° C, This is because Ag does not grow. Accordingly, it is preferable that the second cooling step is performed at a rate of 0.013 ° C / sec or more and less than 15 ° C / sec.
FIG. 2 shows the products and phase changes of the heating and cooling process of the second step of the present invention. More specifically, FIG. 2 is a graph showing changes in temperature and temperature during cooling after addition of molten Na solution to Ag, ≪ / RTI >
In the second step, when the mixture is heated and maintained at 880 ° C in the second step, it is present as a mixed solution of Ag and Na in a liquid phase. The mixture is maintained at 0.013 ° C / sec or more at 15 ° C / sec (Liquid (Ag) and Na (Na)) in liquid phase and liquid phase (Na) in liquid phase and liquid phase, respectively, (Liquid (Ag, Na)) + solid phase Ag, solid phase Ag + solid phase Ag 2 Na and solid phase Na + solid phase Ag 2 Na are changed.
More specifically, since the solid phase of Ag 2 Na produced in the cooling process is an unstable compound, when the Ag 2 Na is gradually cooled at a rate of 0.013 ° C / sec or more and less than 15 ° C / sec, Ag in the specific crystal direction of the Ag 2 Na So that silver nanowires are produced.
Finally, in the third step of the present invention, the coagulated solid is liquefied by adding alcohol to the coagulated solid, followed by refining to remove Na, thereby producing silver nanowires.
1 (f) to (j). Specifically, by adding alcohol to the Na-containing solid containing the wire-shaped Ag, the alcohol and Na react to form liquefied (FIG. 1 f) and (g)), and silver nanowires are produced by purifying the silver nanowires (Fig. 1 (i) and (j)).
1 (f) and (g)). Then, distilled water is further added (FIG. 1 (h)) to remove impurities around the silver nanowires from the distilled water And the viscosity of the liquid phase is also lowered so as to be more easily purified.
In the third step, the purification method is not limited, but it is preferable to carry out vacuum electrolytic extraction.
As described above, according to the present invention, a method of manufacturing a nanowire is characterized in that a molten Na solution is added to Ag or an Ag alloy, heated to 97.7 to 880 캜, held for at least 1 minute and then cooled to 0.013 캜 / The silver nanowire can be manufactured without using a capping agent.
According to the silver nanowire production method of the present invention, the silver nanowire diameter and length can be controlled by adjusting the content of the Ag or Ag alloy and Na, and controlling the heating temperature and the holding time within the heating temperature range It is possible to easily manufacture silver nanowires of various sizes.
Accordingly, the present invention provides, in another aspect, a silver nanowire that is produced by the above-described method.
In another aspect, the present invention provides an electronic device, which is manufactured using the silver nanowire.
Hereinafter, the present invention will be described in more detail by way of examples, but the scope of the present invention is not limited by the examples.
<Examples>
≪ Example 1 > Production of silver nanowires according to the content of Ag and Na
A 99.9% molten Na solution was added to Ag having a purity of 99.0% or more to prepare a mixture in which Ag was melted in the Na solution. In this case, the content of Ag and Na was changed to 0.1 wt.% Ag + 99.9 wt.% Na, 4.0 wt.% Ag + 96.0 wt.% Na and 20.0 wt.% Ag + 80 wt.
Next, the mixture in which the Ag was melted in the Na solution was placed in an electric furnace and heated to 150 캜 in a vacuum atmosphere, and then maintained at the above temperature for 12 hours. After completion of the above process, the mixture was cooled in an electric furnace at a rate of 0.013 캜 / Respectively.
Next, the solid state was liquefied by adding ethanol solution to solid state Na in which solidified Ag solidified in the cooling process, and reacting with Na in solid state.
Thereafter, purified silver nanowires were obtained by adding distilled water to the liquid phase having a high viscosity and vacuum electrolytic extraction.
As described above, the silver nanowires obtained in this embodiment had a content ratio of Ag and Na of 0.1 wt.% Ag + 99.9 wt.% Na, 4.0 wt.% Ag + 96.0 wt.% Na and 20.0 wt. % Ag + 80 wt.% Na, respectively.
Example 2: Preparation of silver nanowire according to heating temperature
A 99.9% molten Na solution was added to Ag having a purity of 99.0% or more to prepare a solution of Ag in the Na solution having a content ratio of 0.3 wt.% Ag + 99.7% Na.
Next, 0.3 wt.% Ag + 99.7% Na mixture, which is a mixture of Ag in the Na solution, was heated at different temperatures of 150 ° C., 250 ° C. and 350 ° C., For 12 hours and then cooled in an electric furnace at a rate of 0.013 [deg.] C / sec after the above procedure was completed.
Next, the solid state was liquefied by adding ethanol solution to solid state Na in which solidified Ag solidified in the cooling process, and reacting with Na in solid state.
Thereafter, purified silver nanowires were obtained by adding distilled water to the liquid phase having a high viscosity and vacuum electrolytic extraction.
The silver nanowires obtained at this time were prepared for each of the above-mentioned temperatures as the heating temperature was changed to 150 캜, 250 캜 and 350 캜.
≪ Example 3 > Preparation of silver nanowire according to heating temperature holding time
Silver nanowires were prepared in the same manner as in Example 2, except that the heating temperature was changed to 150 ° C and the holding time was changed to 0.1hr, 12hr and 24hr.
Example 4 Preparation of silver nanowires according to cooling rate
After heating at a heating temperature of 150 ° C, the temperature is maintained at the above temperature for 24 hours. After completion of the above process, cooling is carried out at a rate of 0.013 ° C / sec in an electric furnace or at a rate of 15 ° C / sec in alcohol Silver nanowires were prepared in the same manner as in Example 2. [
<Analysis>
The silver nanowires with different contents of Ag and Na
FIG. 3 is a SEM photograph of silver nanowires prepared by varying the content ratio of Ag and Na according to Example 1, and FIG. 4 is a histogram showing the diameter and length of silver nanowires having different contents.
As a result, in the case where the content ratio of Ag and Na was 0.1 wt.% Ag + 99.9 wt.% Na, 4.0 wt.% Ag + 96.0 wt.% Na and 20.0 wt.% Ag + 80 wt. It is possible to observe silver nanowires grown with Ag in the lateral direction using Ag 2 Na as a nucleation seed. By controlling the content of Ag and Na, it is possible to control the diameter of silver nanowires to 400 to 2,400 nm, Can be adjusted to 20 to 180 탆.
The silver nanowires
FIG. 5 is a SEM photograph of silver nanowires prepared at different heating temperatures according to Example 2, and FIG. 6 is a histogram showing diameter and length for each silver nanowire manufactured at different temperatures.
As a result, silver nanowires grown in the lateral direction with Ag 2 Na as nucleation seeds can be observed in all cases where the heating temperatures are 150 ° C., 250 ° C., and 350 ° C. By controlling the heating temperature The diameter of the nanowire can be adjusted to 400 to 2400 nm, and the length can be adjusted to 20 to 120 탆.
Silver nanowires with heating temperature holding time
FIG. 7 is a SEM image of silver nanowires prepared at different heating temperature holding times according to Example 3. FIG. 8 is a graph showing the diameter and length of each silver nanowire prepared at different heating temperature holding times It is a histogram.
7, when the heating temperature holding time is shortened to 0.1 hr, it can be confirmed that the yield of the nanowire is reduced as compared with the case where the heating temperature holding time is set to 12 hours or 24 hours, It can be seen that the yield of the wire is affected by the heating temperature holding time. Also, referring to FIG. 8, it can be seen that the diameter and length of the silver nanowire to be manufactured can be controlled by controlling the heating time holding time.
The silver nanowires
FIG. 9 is a SEM image of silver nanowires prepared at different cooling rates according to Example 4, and FIG. 10 is a histogram showing diameter and length of silver nanowires prepared at different cooling rates.
Referring to the SEM image of FIG. 9, it can be seen that when Ag is slowly cooled to 0.013 ° C / sec in the electric furnace (FIG. 9 (a)), Ag can grow sufficiently in the lateral direction using Ag 2 Na as a nucleation seed (Fig. 9 (b)) shows that when Ag is not sufficiently grown due to rapid cooling, the nanowire shows a point shape or rhombo shape instead of a wire shape. .
10, silver nanowires having diameters and lengths of 500 to 1200 nm and 20 to 120 μm, respectively, were produced when Ag was sufficiently grown at a cooling rate of 0.013 ° C / sec in an electric furnace, As shown in FIG. 9, when Ag rapidly grows at a cooling rate of 15 ° C / sec, it can be seen that most of the grains have diameters and lengths of 200 to 400 nm and 20 μm have.
While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments. It will be understood that various modifications and changes may be made without departing from the scope of the appended claims.
Claims (6)
A second step of heating the mixture in a vacuum state and then cooling it to produce a Na coagulated solid containing wire-shaped Ag; And
And a third step of preparing a silver nanowire by liquefying the coagulated solid by reacting the coagulated solid with an alcohol and then purifying the coagulated solid to remove Na.
Wherein the silver nanowire has a diameter of 400 to 2400 nm and a length of 20 to 180 탆.
Wherein the second step comprises heating the mixture to a temperature of from 97.7 to 880 캜 in a vacuum to maintain it at a cooling rate of less than 15 캜 / sec to produce a Na coagulated solid containing wire-shaped Ag A method of manufacturing a silver nanowire.
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| KR20190019350A (en) | 2017-08-17 | 2019-02-27 | 문경식 | Method for producing silver nanowires using AgCl solution |
| KR102596187B1 (en) | 2019-02-11 | 2023-10-31 | 주식회사 씨엔피솔루션즈 | Method for producing silver nanowires using AgCl dispersion |
| CN111014719A (en) * | 2019-12-26 | 2020-04-17 | 海泰纳鑫科技(成都)有限公司 | High-purity silver nanowire, preparation method thereof and silver nanowire conductive film |
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| KR101554927B1 (en) * | 2014-07-21 | 2015-09-22 | 주식회사 에이든 | Preparing method of silver nanowire and transparent electrode using it |
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