CN110093602B - Method for preparing silver nanowire array by utilizing capillary wetting action - Google Patents
Method for preparing silver nanowire array by utilizing capillary wetting action Download PDFInfo
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- CN110093602B CN110093602B CN201910426112.6A CN201910426112A CN110093602B CN 110093602 B CN110093602 B CN 110093602B CN 201910426112 A CN201910426112 A CN 201910426112A CN 110093602 B CN110093602 B CN 110093602B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
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- B82Y40/00—Manufacture or treatment of nanostructures
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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Abstract
A method for preparing a silver nanowire array by utilizing capillary wetting action relates to a method for preparing a silver nanowire array. The invention aims to solve the technical problems that the existing silver nanowire array is complex in preparation process and poor in binding property with a target matrix. The invention comprises the following steps: firstly, mixing Ag powder and CuO powder; secondly, heating; and thirdly, carrying out hydrothermal reaction. The invention provides a method for preparing a silver nanowire array on the surface of inert metal or ceramic by utilizing capillary wetting, which is simple and effective to operate, and simultaneously provides a method for removing an AAO template after phase change by corrosion, and has good application prospect.
Description
Technical Field
The invention relates to a method for preparing a silver nanowire array.
Background
The silver nanowire array has unique photoelectric property, high detection sensitivity and good catalytic performance, thereby having wide application prospect. At present, the preparation of silver nanowire arrays mainly adopts an electrochemical deposition mode, firstly, a layer of Au is deposited or sputtered on the surface of an anodic aluminum oxide template (AAO) to enable the Au to be conductive, then the AAO is used as an electrode, and Ag is contained in the Ag-containing nanowire arrays+The silver nanowire array is prepared by performing electrodeposition in the solution, preparing silver nanowires in nano holes of the AAO, and removing the AAO template by adopting acid or alkali solution to obtain the silver nanowire array. However, the electrodeposition method is complicated in process operation, the obtained silver nanowire array needs to be transferred onto a target substrate subsequently, a good connection method is lacked for the substrate, and the connection strength is poor. In addition, the chemical components of the AAO are amorphous alumina, and can be removed by acid or alkali solution at normal temperature and normal pressure, but after being heated, the AAO can generate phase change and has stronger acid-base corrosion resistance, and the conventional method cannot remove the AAOAnd (4) removing.
The capillary wetting phenomenon means that in a small-sized tubule, if the liquid has good wettability with the wall of the tubule, the liquid level in the tubule is a concave liquid level, and the liquid in the tubule rises under the action of the tension of the liquid surface. In the current research, some polymers and nitrates can be filled into the nanopores of the AAO template under the action of capillary wetting, and then corresponding nanostructures are obtained. But metals including Ag cannot penetrate into the AAO pores using a similar simple method because the liquid pure metal does not achieve good wetting with the inner walls of the AAO nanopores.
Disclosure of Invention
The invention provides a method for preparing a silver nanowire array by utilizing capillary wetting action, aiming at solving the technical problems of complex preparation process and poor binding property with a target matrix of the existing silver nanowire array.
The method for preparing the silver nanowire array by utilizing the capillary wetting action is carried out according to the following steps:
firstly, mixing powder: putting Ag powder and CuO powder into a ball milling tank, adding absolute ethyl alcohol to completely immerse the Ag powder and the CuO powder, performing wet mixing and ball milling for 6-12 h in a planetary ball mill, taking out, drying in a water bath at 90-95 ℃ to obtain Ag-CuO mixed powder, and then preparing the Ag-CuO mixed powder into Ag-CuO sheets under the pressure of a hydraulic press by using a tabletting mold; the molar fraction of CuO in the Ag-CuO mixed powder is 1-8%;
secondly, heating: polishing the base material, and then ultrasonically cleaning the base material for 5-10 min by using absolute ethyl alcohol; washing the anodic alumina template in absolute ethyl alcohol, and naturally airing; stacking the cleaned base material, the Ag-CuO sheet prepared in the step one and the aired anodic alumina template in sequence from bottom to top, placing the stacked base material, the Ag-CuO sheet and the aired anodic alumina template in a muffle furnace, heating the base material to 950-1000 ℃ from room temperature under the condition that the heating rate is 10-15 ℃/min, preserving the heat for 5-30 min, and then cooling the base material to room temperature under the condition that the cooling rate is 5-8 ℃/min;
thirdly, hydrothermal reaction: putting the sample obtained in the step two into a high-pressure hydrothermal reaction kettle, adding 0.2-0.3 mol/L NaOH aqueous solution, heating the mixture to 190-250 ℃ from room temperature under the condition that the heating rate is 6.5-7 ℃/min, keeping the temperature for 30-120 min for removing the anodic alumina template, taking the mixture out of the reaction kettle after cooling, and sequentially washing the mixture by using 5-6 mol/L NaOH aqueous solution, 1-1.2 mol/L phosphoric acid aqueous solution and deionized water to obtain a silver nanowire array; the volume of the 0.2 mol/L-0.3 mol/L NaOH aqueous solution is 50-55% of the volume of the high-pressure hydrothermal reaction kettle.
The design principle of the invention is as follows:
the chemical component of the AAO template is aluminum oxide (Al)2O3) While liquid pure Ag is in Al2O3The wetting angle is larger than 90 degrees, and the filling height of the liquid pure Ag in the nano holes of the AAO template is smaller than 0, namely the liquid pure Ag is not filled, which is calculated according to a capillary wetting height formula.
When liquid Ag is heated in the air, a small amount of oxygen is fused into the Ag, and the liquid Ag can be promoted in Al to a certain extent2O3The wetting angle is still about 90 degrees, which is not enough for Ag to fill in the template to prepare the nano-wire.
In air reaction brazing of macroscopic materials, CuO is generally used to improve the wettability of liquid Ag on the ceramic surface. At high temperature, CuO can form pseudo solid solution with Ag and Al2O3Reaction of the ceramic to form CuAl2O4Or CuAlO2And so on, CuO can reduce the content of liquid Ag in Al2O3Wetting angle of the surface. According to the invention, an Ag-CuO system is introduced into the field of nanowire array preparation by a template method, and according to a capillary wetting height formula, when the wetting angle between Ag and the inner wall of the AAO aperture is less than 90 degrees, the Ag-CuO system can be filled into the AAO aperture, so that the silver nanowire array is obtained.
According to the invention, a small amount of CuO is added into Ag, so that the wettability of liquid Ag on the inner wall of the AAO nano-pore can be greatly improved, and therefore, under the action of the surface tension of liquid, the liquid Ag can rise in the nano-pore and can form a solid Ag nano-wire after solidification. And removing the AAO template to prepare the Ag nanowire array.
The invention has the following beneficial effects:
1. the method is simple and effective to operate, and the substrate, the Ag-CuO and the AAO template are sequentially stacked and heated in the air, so that the Ag-CuO can permeate into the nano-pores of the template;
2. according to the invention, the CuO component is added into the Ag, so that the wettability of the liquid Ag in the holes of the AAO template is improved, and the penetration of the liquid Ag is promoted;
3. according to the invention, while the liquid Ag-CuO permeates into the template nano-pores, the liquid Ag-CuO and the matrix material can realize firm metallurgical bonding, so that the silver nanowire array can have good bonding strength with the matrix;
4. in the third step of the invention, the AAO template after phase change can be removed by using the high-temperature and high-pressure NaOH aqueous solution in the reaction kettle, and the Ag nanowire array is not damaged, and the concrete reasons are as follows:
the conventional method for removing the AAO template is to adopt NaOH aqueous solution or phosphoric acid solution and heat the aqueous solution in a water bath under normal pressure. Because the boiling point of water is 100 ℃ under the standard atmospheric pressure, the temperature of the corrosive liquid is 100 ℃ at most, which is not enough to remove the AAO template after high-temperature phase transition. Some researchers used hydrofluoric acid (HF) to remove the AAO template after heating at 800 ℃, but HF is very corrosive and can damage various metals including Ag nanowires.
In the invention, the NaOH aqueous solution is adopted in the hydrothermal reaction kettle to remove the AAO template after phase change, and because the boiling point of the liquid is increased along with the increase of the pressure, the temperature of the NaOH aqueous solution can be far higher than 100 ℃ in the sealed reaction kettle, and the air pressure above the liquid is also higher than the standard atmospheric pressure. With the increase of temperature, the chemical reaction rate can be improved, and under the conditions of high temperature and high pressure hydrothermal, the ionization constant of water is increased, the hydrolysis reaction is intensified, and the oxidation-reduction potential is obviously changed. In addition, the NaOH aqueous solution does not react with the metal Ag, and the prepared Ag nanowire array cannot be damaged.
The invention provides a method for preparing a silver nanowire array on the surface of inert metal or ceramic by utilizing capillary wetting, which is simple and effective to operate, and simultaneously provides a method for removing an AAO template after phase change by corrosion, and has good application prospect.
Drawings
FIG. 1 is a photograph of the cross-sectional structure of the calcined product in step two of experiment one;
fig. 2 is an SEM image of the silver nanowire array obtained in step three of experiment one.
Detailed Description
The first embodiment is as follows: the embodiment is a method for preparing a silver nanowire array by utilizing capillary wetting, which is specifically carried out according to the following steps:
firstly, mixing powder: putting Ag powder and CuO powder into a ball milling tank, adding absolute ethyl alcohol to completely immerse the Ag powder and the CuO powder, performing wet mixing and ball milling for 6-12 h in a planetary ball mill, taking out, drying in a water bath at 90-95 ℃ to obtain Ag-CuO mixed powder, and then preparing the Ag-CuO mixed powder into Ag-CuO sheets under the pressure of a hydraulic press by using a tabletting mold; the molar fraction of CuO in the Ag-CuO mixed powder is 1-8%;
secondly, heating: polishing the base material, and then ultrasonically cleaning the base material for 5-10 min by using absolute ethyl alcohol; washing the anodic alumina template in absolute ethyl alcohol, and naturally airing; stacking the cleaned base material, the Ag-CuO sheet prepared in the step one and the aired anodic alumina template in sequence from bottom to top, placing the stacked base material, the Ag-CuO sheet and the aired anodic alumina template in a muffle furnace, heating the base material to 950-1000 ℃ from room temperature under the condition that the heating rate is 10-15 ℃/min, preserving the heat for 5-30 min, and then cooling the base material to room temperature under the condition that the cooling rate is 5-8 ℃/min;
thirdly, hydrothermal reaction: putting the sample obtained in the step two into a high-pressure hydrothermal reaction kettle, adding 0.2-0.3 mol/L NaOH aqueous solution, heating the mixture to 190-250 ℃ from room temperature under the condition that the heating rate is 6.5-7 ℃/min, keeping the temperature for 30-120 min for removing the anodic alumina template, taking the mixture out of the reaction kettle after cooling, and sequentially washing the mixture by using 5-6 mol/L NaOH aqueous solution, 1-1.2 mol/L phosphoric acid aqueous solution and deionized water to obtain a silver nanowire array; the volume of the 0.2 mol/L-0.3 mol/L NaOH aqueous solution is 50-55% of the volume of the high-pressure hydrothermal reaction kettle.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the molar fraction of CuO in the Ag-CuO mixed powder in the first step is 1%. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the base material in the second step is a high-temperature stable ceramic material, in particular Al2O3Or BSCF, BCFN or BCFZ. The others are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: the base material in the second step is a metal material with high melting point and stable chemical property, specifically Pt, Crofer22APU, AISI310S or AISI 314. The rest is the same as one of the first to third embodiments.
The fifth concrete implementation mode: the fourth difference between this embodiment and the specific embodiment is that: the thickness of the anodic aluminum oxide template in the second step is 30-60 μm, and the aperture is 40-100 nm. The rest is the same as the fourth embodiment.
The invention was verified with the following tests:
test one: the test is a method for preparing a silver nanowire array by utilizing capillary wetting, and the method is specifically carried out according to the following steps:
firstly, mixing powder: putting Ag powder and CuO powder into a ball milling tank, adding absolute ethyl alcohol to completely immerse the Ag powder and the CuO powder, carrying out wet mixing and ball milling for 12 hours in a planetary ball mill at the ball milling speed of 700 revolutions per minute, then taking out, drying in a water bath at 90 ℃ to obtain Ag-CuO mixed powder, and then preparing the Ag-CuO mixed powder into Ag-CuO sheets under the pressure of a hydraulic press by using a sheet pressing mould; the molar fraction of CuO in the Ag-CuO mixed powder is 1%;
secondly, heating: polishing the base material, and then ultrasonically cleaning the base material for 10min by using absolute ethyl alcohol; washing the anodic alumina template in absolute ethyl alcohol, and naturally airing; stacking the cleaned base material, the Ag-CuO sheet prepared in the step one and the aired anodized aluminum template together in sequence from bottom to top, and placingHeating the mixture to 970 ℃ from room temperature in a muffle furnace at the heating rate of 10 ℃/min, preserving the heat for 30min, and then cooling the mixture to room temperature at the cooling rate of 5 ℃/min; the matrix material is Al2O3(ii) a The thickness of the anodic aluminum oxide template is 60 mu m, and the aperture is 40 nm-60 nm;
thirdly, hydrothermal reaction: putting the sample obtained in the step two into a high-pressure hydrothermal reaction kettle, adding 0.2mol/L NaOH aqueous solution to completely immerse the sample obtained in the step two, heating the sample to 250 ℃ from room temperature under the condition that the heating rate is 6.5 ℃/min, preserving the heat for 30min to remove the anodic alumina template, taking the sample out of the reaction kettle after cooling, and sequentially washing the sample with 5mol/L NaOH aqueous solution, 1mol/L phosphoric acid aqueous solution and deionized water to obtain a silver nanowire array; the volume of the 0.2mol/L NaOH aqueous solution is 50 percent of the volume of the high-pressure hydrothermal reaction kettle.
FIG. 1 is a photograph of the cross-sectional structure of the calcined product in the second step of the first test, in which the area A is an anodized aluminum template, the area B is Ag, and the area C is Al2O3The matrix, it can be seen that Ag has been filled into the AAO template (since the Cu content is very small, it is not marked in the figure).
Fig. 2 is an SEM image of the silver nanowire array obtained in the third step of the first test, and it can be seen that the Ag nanowire array prepared in the first test has a uniform size, is vertically upward, and has a low agglomeration degree.
Claims (7)
1. A method for preparing a silver nanowire array by utilizing capillary wetting is characterized in that the method for preparing the silver nanowire array by utilizing the capillary wetting is carried out according to the following steps:
firstly, mixing powder: putting Ag powder and CuO powder into a ball milling tank, adding absolute ethyl alcohol to completely immerse the Ag powder and the CuO powder, performing wet mixing and ball milling for 6-12 h in a planetary ball mill, taking out, drying in a water bath at 90-95 ℃ to obtain Ag-CuO mixed powder, and then preparing the Ag-CuO mixed powder into Ag-CuO sheets under the pressure of a hydraulic press by using a tabletting mold; the molar fraction of CuO in the Ag-CuO mixed powder is 1-8%;
secondly, heating: polishing the base material, and then ultrasonically cleaning the base material for 5-10 min by using absolute ethyl alcohol; washing the anodic alumina template in absolute ethyl alcohol, and naturally airing; stacking the cleaned base material, the Ag-CuO sheet prepared in the step one and the aired anodic alumina template in sequence from bottom to top, placing the stacked base material, the Ag-CuO sheet and the aired anodic alumina template in a muffle furnace, heating the base material to 950-1000 ℃ from room temperature under the condition that the heating rate is 10-15 ℃/min, preserving the heat for 5-30 min, and then cooling the base material to room temperature under the condition that the cooling rate is 5-8 ℃/min;
thirdly, hydrothermal reaction: putting the sample obtained in the step two into a high-pressure hydrothermal reaction kettle, adding 0.2-0.3 mol/L NaOH aqueous solution to completely immerse the sample obtained in the step two, heating the sample to 190-250 ℃ from room temperature under the condition that the heating rate is 6.5-7 ℃/min, preserving the heat for 30-120 min to remove the anodic alumina template, taking the sample out of the reaction kettle after cooling, and sequentially washing the sample with 5-6 mol/L NaOH aqueous solution, 1-1.2 mol/L phosphoric acid aqueous solution and deionized water to obtain a silver nanowire array; the volume of the 0.2 mol/L-0.3 mol/L NaOH aqueous solution is 50-55% of the volume of the high-pressure hydrothermal reaction kettle.
2. The method of claim 1, wherein the molar fraction of CuO in the Ag-CuO mixed powder in the first step is 1%.
3. The method of claim 1, wherein the substrate material in step two is a high temperature stable ceramic material, specifically Al2O3BSCF, BCFN or BCFZ.
4. The method of claim 1, wherein the base material in the second step is a metal material with high melting point and stable chemical properties, specifically Pt, Crofer22APU, AISI310S or AISI 314.
5. The method of claim 1, wherein the thickness of the anodized aluminum template in step two is 30 μm to 60 μm, and the pore size is 40nm to 100 nm.
6. The method for preparing silver nanowire array by capillary wetting according to claim 1, wherein the sample obtained in step two is placed in a high-pressure hydrothermal reaction kettle in step three, and 0.2mol/L NaOH aqueous solution is added to completely immerse the sample obtained in step two.
7. The method for preparing silver nanowire array by capillary wetting according to claim 1, wherein the temperature is raised from room temperature to 250 ℃ at a temperature raising rate of 6.5 ℃/min in the third step and is kept for 30min for removing the anodic alumina template.
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