CN109686497B - Method for preparing copper nano grid transparent electrode based on gas phase reduction of copper oxide - Google Patents
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Abstract
The invention relates to the technical field of semiconductors; in particular to a method for preparing a copper nano grid transparent electrode based on gas phase reduction of copper oxide; preparing a spinning precursor solution by using copper nitrate, preparing a copper nitrate composite nanowire through electrostatic spinning, and heating and oxidizing the prepared copper nitrate composite nanowire to obtain a copper oxide nanofiber; finally, placing the obtained copper oxide nano fiber into a closed reaction kettle, wherein the closed reaction kettle contains gaseous alcohols, and then placing the reaction kettle at the temperature of 200-; the method for reducing the copper oxide nano-fiber by the solvent gas phase not only keeps the shape of the nano-fiber, but also completely reduces the copper oxide; the problem that the nano-grid transparent electrode is easy to break in the existing alcohol reduction process is solved; the method is safe, low in cost and excellent in reduction effect, ensures the transmittance and the conductivity, and finally obtains the copper grid transparent electrode with excellent performance.
Description
Technical Field
The invention belongs to the technical field of semiconductors, and particularly relates to a method for preparing a copper nano grid transparent electrode by gas phase reduction electrospinning copper oxide nano fibers, which has important potential application in a novel flexible electronic technology.
Background
The flexible transparent electrode is an essential important component in the flexible electronic device, and has extremely important influence on the absorption of light and the performance of the device. At present, the representative transparent electrode material is an ITO film, and the preparation technology is mature and the performance is stable. However, with the rapid development of devices such as flat panel displays and solar cells in the last two decades and the limited storage of indium element in the earth's crust, the price of ITO has rapidly increased, and the use of tin element in the new flexible electronics industry has been limited due to the easy poisoning of the substrate by tin element and the brittle nature of ITO. The new flexible transparent electrode material is conductive polymer, metal network, metal oxide, graphene, carbon nanotube and the like, wherein the metal network structure is the most promising material for replacing ITO (indium tin oxide) by virtue of excellent photoelectric properties.
The metal grid structure is prepared by a template method, a solution method, an electrostatic spinning method and the like. The template method has regular shape, but has high cost and the size is limited by the template process; the solution method has low cost, but the grid shape is irregular, and the conductivity is reduced. The nano-wire prepared by electrostatic spinning has the characteristics of high long-diameter ratio, wide spinnable material and controllable appearance. The reserves on the copper earth are large, the conductivity is second to silver, the preparation is easy, and the light transmittance is high. Therefore, the preparation of the copper nano grid transparent electrode by electrospinning becomes a powerful competitor of the future transparent electrode. In 2006, Michael boggnitzki firstly adopts electrostatic spinning to prepare copper nanofibers, firstly, PVB- (CuNO3)2 composite nanofibers are electrospun, the diameter is 550 nm, then, annealing is carried out in air at 450 ℃ for 2h to obtain CuO nanofibers, and finally, reduction is carried out in hydrogen at 300 ℃ for 2h to obtain Cu nanofibers (document Advanced Materials, vol. 18, 2384, 2006). In 2010, the Wu.H project is assembled with PVA copper acetate nanowires, dark brown copper oxide nanowires are obtained by oxidizing for 2h at 500 ℃, and red copper nanowires are obtained by reducing for 1h at 300 ℃ in hydrogen. The performance parameters of 90% at 50 Ω/sq are obtained after optimization (Nano letters, vol. 10, 4242, 2010). In 2015, electrospun PVA/Cuacetate and PVB/Cu nitrate trihydrate nanofiber from sunguul Kim system, also reduced with hydrogen gas to obtain copper nanowires with excellent performance (documents RSC Advances, vol. 5, 53275, 2015).
At present, the copper oxide nano-fiber is generally prepared by hydrogen high-temperature reduction, the cost is high, and hydrogen is explosive gas, so that the further research and application of the copper nano-grid transparent electrode are hindered. Copper oxide can be subjected to reduction reaction with alcohols under the heating condition, but the early experimental result shows that copper oxide nano-fibers can be reduced to obtain copper by adding the copper oxide nano-fibers into the alcohols or adding the alcohols into the copper oxide nano-fibers, but the appearance of the fibers is damaged.
Disclosure of Invention
The invention overcomes the defects in the prior art and provides a method for preparing a copper nano grid transparent electrode based on gas phase reduction of copper oxide. The method solves the problems that the reaction fiber of the copper oxide nano fiber in alcohol is easy to break and the appearance is damaged, and simultaneously, the safe and low-cost copper grid transparent electrode is prepared.
The invention is realized by the following technical scheme.
The method for preparing the copper nano grid transparent electrode based on gas phase reduction of copper oxide comprises the following steps:
a) preparing a spinning precursor solution by using copper nitrate, and preparing the copper nitrate composite nanowire through electrostatic spinning.
b) And heating and oxidizing the prepared copper nitrate composite nanowire to obtain the copper oxide nanofiber.
c) Gas-phase reduction: and placing the obtained copper oxide nano fiber into a closed reaction kettle, wherein the closed reaction kettle contains gaseous alcohols, and then placing the reaction kettle at the temperature of 200-250 ℃ for reaction for 3-5h to obtain the copper nano grid transparent electrode.
Preferably, the reaction kettle is placed at the temperature of 200 ℃ and 250 ℃ for reaction for 3-5h, and then the reaction kettle is placed in a vacuum drying oven for drying for 15-25 min.
Preferably, a spinning aid is added when the spinning precursor solution is prepared, and the spinning aid is glacial acetic acid.
Preferably, the prepared copper nitrate composite nanowire is heated and oxidized to obtain the copper oxide nanofiber, the heating temperature is 450-500 ℃, and the oxidation time is 2.5-3.5 h.
Preferably, the gaseous alcohol is ethanol or methanol, and the volume of the gaseous alcohol accounts for 5-10% of the volume of the reaction kettle.
Compared with the prior art, the invention has the beneficial effects that.
According to the invention, composite fibers are prepared through electrostatic spinning calculation, then the polymer is removed through heating to obtain copper oxide fibers, and the copper nano grid transparent electrode is prepared through solvent gas phase reduction. The reduction speed and the growth speed of the nano-fiber are coordinated by controlling the temperature and time conditions of the gas-phase reduction reaction. The method for reducing the copper oxide nano-fiber by the solvent gas phase not only keeps the shape of the nano-fiber, but also completely reduces the copper oxide. The problem that the nano-grid transparent electrode is easy to break in the existing alcohol reduction process is solved. The method is safe, low in cost and excellent in reduction effect, ensures the transmittance and the conductivity, and finally obtains the copper grid transparent electrode with excellent performance.
Drawings
Fig. 1 is a flow chart of the preparation of the copper nano-grid transparent electrode.
FIG. 2 is a schematic diagram of a copper grid transparent electrode prepared by ethanol gas phase reduction.
Fig. 3 is an optical micrograph of a copper grid prepared prior to gas phase reduction in example 1.
Fig. 4 is an optical micrograph of a copper grid prepared after gas phase reduction in example 1.
Fig. 5 is an SEM image of a copper mesh transparent electrode prepared by gas phase reduction in example 1.
FIG. 6 is a UV-visible absorption spectrum of a copper grid prepared by gas phase reduction in example 1.
FIG. 7 is an XRD spectrum of a copper grid prepared by gas phase reduction in example 1.
Fig. 8 is a transmission spectrum of a copper mesh transparent electrode prepared by gas phase reduction in example 1.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail with reference to the embodiments and the accompanying drawings. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. The technical solutions of the present invention are described in detail below with reference to the embodiments and the drawings, but the scope of protection is not limited thereto.
Example 1
Preparation of PVP- (CuNO) by electrospinning3)2And (3) oxidizing the composite nanowire for 3h at 480 ℃, and reducing the copper oxide nanofiber by adopting ethanol gas phase to obtain the copper nano grid transparent electrode. FIG. 1 is a schematic diagram of a copper nano-grid transparent electrodePreparing a flow chart.
Firstly, preparing an electrospinning precursor solution: 0.68g PVP powder was dissolved in 8ml absolute ethanol and stirred well by magnetic stirrer. Then 0.39g (CuNO) is added3)2•3H2And (4) performing particle O, and continuing stirring. Meanwhile, 1ml of glacial acetic acid is slowly added dropwise to help dissolution, and the glacial acetic acid is used as a spinning aid. The solution was stirred at room temperature until it was transparent and viscous, and the prepared spinning precursor solution was sucked up with a 2.5ml medical syringe, which was placed in an electrospinning syringe. 12KV positive high pressure, 10cm curing distance and 0.075mm/min injection speed are adopted, and the temperature and the humidity of spinning are respectively controlled at 25 ℃ and 20%. Through electrostatic spinning, PVP/(CuNO)3)2The composite nanowires are collected on a cleaned glass sheet. Drying the composite nanowire at 120 ℃ for 30min to remove water; and oxidizing for 3 hours at 480 ℃ to remove organic components, wherein the copper nitrate nanowires are oxidized into brown CuO NWs.
The CuO NWs is put in a high-pressure closed reaction kettle containing 8 percent of ethanol, the reaction kettle is put in an oven, and the reaction temperature and the pressure intensity are controlled by the temperature of the oven. Fig. 2 is a schematic view of a vapor phase reduced copper mesh transparent electrode. The reduction is carried out for 4h at 230 ℃, and the ethanol and the copper oxide react with the chemical formula (1). And finally, drying in a vacuum drying oven for 20min to obtain red Cu NWs. Fig. 3 and 4 are optical micrographs of copper mesh transparent electrodes prepared before and after vapor phase reduction, and it can be seen that the morphology of the fibers is well preserved before and after reduction. FIG. 5 is an SEM image of a copper grid transparent electrode prepared by vapor phase reduction, and the SEM image shows that the copper grid transparent electrode prepared by the method is excellent in uniformity and is expected to be applied to preparation of large-area devices. Fig. 6 and 7 are the ultraviolet-visible absorption spectrum and XRD spectrum of the vapor-phase-reduced copper mesh transparent electrode, from which it can be seen that the copper fibers are completely reduced without remaining other impurities. And finally, characterizing the prepared copper grid transparent electrode, wherein the average diameter of the nanowire is 220 nm, the transmittance of the transparent electrode is more than 80%, and the square resistance reaches 94.3 Ω/mouth (as shown in figure 8).
C2H5OH+ CuO→Cu+H2O+CH3CHO （1）
Example 2
Preparation of PVP- (CuNO) by electrospinning3)2And (3) oxidizing the composite nanowire for 3.5 hours at 450 ℃, and reducing the copper oxide nanofiber by adopting ethanol gas phase to obtain the copper nano grid transparent electrode. Fig. 1 is a flow chart of the preparation of the copper nano-grid transparent electrode.
Firstly, preparing an electrospinning precursor solution: 0.68g PVP powder was dissolved in 8ml absolute ethanol and stirred well by magnetic stirrer. Then 0.39g (CuNO) is added3)2•3H2And (4) performing particle O, and continuing stirring. Meanwhile, 1ml of glacial acetic acid is slowly added dropwise to help dissolution, and the glacial acetic acid is used as a spinning aid. The solution was stirred at room temperature until it was transparent and viscous, and the prepared spinning precursor solution was sucked up with a 2.5ml medical syringe, which was placed in an electrospinning syringe. 12KV positive high pressure, 10cm curing distance and 0.075mm/min injection speed are adopted, and the temperature and the humidity of spinning are respectively controlled at 25 ℃ and 20%. Through electrostatic spinning, PVP/(CuNO)3)2The composite nanowires are collected on a cleaned glass sheet. Drying the composite nanowire at 120 ℃ for 30min to remove water; and (3) oxidizing for 3.5h at the temperature of 450 ℃ to remove organic components, wherein the copper nitrate nanowires are oxidized into brown CuO NWs.
The CuO NWs is put in a high-pressure closed reaction kettle containing 10% isobutanol, the reaction kettle is put in an oven, and the reaction temperature and the pressure are controlled by the temperature of the oven. Reducing for 5h at 200 ℃, and finally drying in a vacuum drying oven for 20min to obtain red Cu NWs.
Example 3
Preparation of PVP- (CuNO) by electrospinning3)2And (3) oxidizing the composite nanowire for 2.5h at 500 ℃, and reducing the copper oxide nanofiber by adopting ethanol gas phase to obtain the copper nano grid transparent electrode. Fig. 1 is a flow chart of the preparation of the copper nano-grid transparent electrode.
Firstly, preparing an electrospinning precursor solution: 0.68g PVP powder was dissolved in 8ml absolute ethanol and stirred well by magnetic stirrer. Then 0.39g (CuNO) is added3)2•3H2And (4) performing particle O, and continuing stirring. Meanwhile, 1ml of glacial acetic acid is slowly added dropwise to help dissolution, and the glacial acetic acid is used as a spinning aid. Stirring at room temperatureThe solution is transparent and viscous, the prepared spinning precursor solution is absorbed by a 2.5ml medical injector, and the injector is placed in an electrostatic spinning injection device. 12KV positive high pressure, 10cm curing distance and 0.075mm/min injection speed are adopted, and the temperature and the humidity of spinning are respectively controlled at 25 ℃ and 20%. Through electrostatic spinning, PVP/(CuNO)3)2The composite nanowires are collected on a cleaned glass sheet. Drying the composite nanowire at 120 ℃ for 30min to remove water; and oxidizing for 2.5h at 500 ℃ to remove organic components, wherein the copper nitrate nanowires are oxidized into brown CuO NWs.
The CuO NWs is put in a high-pressure closed reaction kettle containing 5 percent of methanol, the reaction kettle is put in an oven, and the reaction temperature and the pressure intensity are controlled by the temperature of the oven. Reducing for 3h at 250 ℃, and finally drying in a vacuum drying oven for 20min to obtain red CuNWs.
While the invention has been described in further detail with reference to specific preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (4)
1. The method for preparing the copper nano grid transparent electrode based on gas phase reduction of copper oxide is characterized by comprising the following steps of:
a) preparing a spinning precursor solution by using copper nitrate, and preparing a copper nitrate composite nanowire through electrostatic spinning;
b) heating and oxidizing the prepared copper nitrate composite nanowire to obtain copper oxide nanofiber;
c) gas-phase reduction: and placing the obtained copper oxide nano fiber into a closed reaction kettle, wherein the closed reaction kettle contains gaseous alcohol, and then placing the reaction kettle at the temperature of 200-250 ℃ for reaction for 3-5h to obtain the copper nano grid transparent electrode, wherein the gaseous alcohol is ethanol or methanol, and the volume of the gaseous alcohol accounts for 5-10% of the volume of the reaction kettle.
2. The method for preparing a copper nano grid transparent electrode based on gas phase reduction of copper oxide as claimed in claim 1, wherein the reaction kettle is placed at 200-250 ℃ for reaction for 3-5h, and then the reaction kettle is placed in a vacuum drying oven for drying for 15-25 min.
3. The method for preparing the copper nano grid transparent electrode based on gas phase reduction of copper oxide according to claim 1, wherein a spinning aid is added during preparation of the spinning precursor solution, and the spinning aid is glacial acetic acid.
4. The method for preparing a copper nano grid transparent electrode based on gas phase reduction of copper oxide as claimed in claim 1, wherein the prepared copper nitrate composite nano wire is heated and oxidized to obtain the copper oxide nano fiber, the heating temperature is 450-.
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