CN112979180A - ITO glass processing method and application thereof - Google Patents
ITO glass processing method and application thereof Download PDFInfo
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- CN112979180A CN112979180A CN201911294217.7A CN201911294217A CN112979180A CN 112979180 A CN112979180 A CN 112979180A CN 201911294217 A CN201911294217 A CN 201911294217A CN 112979180 A CN112979180 A CN 112979180A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/42—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating of an organic material and at least one non-metal coating
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/08—Fuel cells with aqueous electrolytes
- H01M8/083—Alkaline fuel cells
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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Abstract
The invention relates to a processing method of ITO glass and application thereof, belonging to the field of fuel cells. The main technical scheme is as follows: ultrasonically cleaning PET-ITO with deionized water, acetone and ethanol for 30min, placing in an ultraviolet ozone cleaning machine with the conductive surface facing upwards, and treating for 30 min; and after treatment, self-assembly is carried out, and the specific layer number is set according to the requirement. According to the ITO glass treatment method provided by the invention, ozone treatment is adopted, organic matters on the surface are decomposed by ultraviolet irradiation, an oxygen-rich layer is formed on the surface and carries a large number of hydroxyl groups, so that the glass surface has negative charges, and direct electrostatic alternative self-assembly is facilitated. The polyelectrolyte multilayer film can form nano-pores and micro-pores under certain conditions, so that the polyelectrolyte multilayer film has a large specific surface area and an open pore structure, and provides a template for electrodeposition.
Description
Technical Field
The invention relates to the field of fuel cells, in particular to a method for processing ITO glass and application thereof.
Background
The ITO conductive glass is formed by depositing an ITO (indium tin oxide) film with the thickness of 20-30nm on the surface of ultrathin glass by a vacuum magnetron sputtering method under the high-vacuum environment by utilizing the basic principle of plasma discharge on the basis of soda-lime-based or silicon-boron-based substrate glass. ITO conductive glass is a focus of global attention due to its excellent optical and electronic properties. The ITO conductive glass can be widely applied to the field of semiconductors, such as Thin Film Transistor (TFT), fuel cell, Solar cell (Solar cell) and sensor, and gradually becomes basic materials of computer liquid product display screens, mobile phone display screens and the like. Because the surface smoothness of the ITO conductive glass is very high, but ITO is easy to scrap due to the phenomena of pockmarks, microcrystalline gaps and the like, and meanwhile, the ITO film layer also has strong water absorption and can absorb moisture and carbon dioxide in the air and generate chemical reaction to generate 'mildew'. In addition, if the ITO film layer contacts with the active positive ion solution, ion replacement reaction is easy to generate, and other defects of electric conduction are formed.
Disclosure of Invention
In order to make up the defects of the prior art, the surface of the indium tin oxide is self-assembled, so that the surface is uniform. The films with different layers can be modified according to different scales of deposited metal particles, so that the particle size of the crystal can be regulated and controlled. The technical scheme adopted by the invention is as follows: a method for processing ITO glass comprises the following steps in sequence:
(1) testing the ITO glass conductive surface with a multimeter, wherein the conductive surface faces downwards, and cutting with a glass cutter;
(2) placing the ITO glass in a container filled with deionized water, placing the container in an ultrasonic instrument, wherein the ultrasonic instrument lasts for 30min at the temperature of 15 ℃, and taking out nitrogen for drying;
(3) placing ITO glass in a container, injecting acetone, sealing the container opening with tinfoil, placing in an ultrasonic instrument for 30min at 15 ℃, taking out nitrogen and drying;
(4) placing ITO glass in a container, injecting ethanol, sealing the container opening with tinfoil, placing in an ultrasonic instrument for 30min at 15 ℃, taking out nitrogen and drying;
(5) placing ITO glass in an ultraviolet ozone cleaning machine, wherein the conductive surface is upward, and after ozone treatment is carried out for 25-35min, organic matters on the surface of the ITO glass are decomposed by ultraviolet irradiation, an oxygen-rich layer is formed on the surface and carries a large number of hydroxyl groups, and the surface of the glass is provided with negative charges;
(6) placing the ITO glass in a PDDA (polydiene dimethyl ammonium chloride solution) solution to be soaked for 5min, taking out the ITO glass, washing the ITO glass with deionized water, drying the ITO glass by blowing with nitrogen, placing the PDDA/ITO glass in a PSS (poly (4-sodium styrene sulfonate)) solution to be soaked for 5min, and carrying out self-assembly to obtain a layer of PDDA/PSS self-assembled film;
(7) and (5) repeating the step (6) to prepare the ITO glass with layer-by-layer self-assembly.
Further, the step (5) is ozone treatment for 30 min.
The invention also discloses application of the ITO glass treatment method in construction of an ethanol fuel cell.
The method comprises the steps of taking a NiNPs/AuNPs/ITO electrode as a working electrode, an Ag/AgCl electrode as a reference electrode and a platinum wire as an auxiliary electrode to form a three-electrode system, placing the three-electrode system in an ethanol solution and a supporting electrolyte, setting the potential to be-0.2-1.3V, recording a cyclic voltammetry curve of 100mmol/L ethanol with the scanning speed range of 20-100 mV/S, and analyzing the control process of the electrode in the electrocatalytic oxidation of the ethanol solution by using a standard curve method.
Further, the supporting electrolyte contains 1mol/LKOH and has a pH of 14.
Further, the NiNPs/AuNPs/ITO electrode comprises: indium tin oxide conductive glass (ITO) is used as a substrate and a conductive layer, nano nickel gold particles are electrochemical deposition layers, the nano nickel particles are deposited on the nano gold particles, and the nano gold particles are deposited on the ITO.
The invention has the beneficial effects that:
(1) PDDA is positively charged and PSS is negatively charged. The PSS is placed on the outermost layer, and as the PSS is negatively charged and the metal ions are positively charged, a large amount of metal ions can be enriched around the substrate, the concentration of the metal ions around the substrate is high, and during electrodeposition, more crystal nuclei are formed, and crystals grow large and fast. When PDDA is placed on the outermost layer, the PDDA is positively charged, metal ions are positively charged, the metal ions around the substrate are few, the metal ion concentration around the substrate is low, and the electrodeposition is carried out, so that crystal nuclei are few, and crystals are small and slow. The size of the crystals can thus be controlled by this method.
(2) The substrate also has a certain guiding effect on the appearance of the sediment, the polyelectrolyte with opposite charges can be alternately adsorbed by electrostatic action to obtain a self-assembled multilayer film, and the polyelectrolyte multilayer film can form nano-pores and micro-pores under certain conditions, so that the polyelectrolyte multilayer film has a large specific surface area and an open pore structure, and provides a template for electrodeposition. Through the electrodeposition process, the nano structure is subjected to restrictive growth in the pore channel, so that the uniformly dispersed nano structure is obtained, and the catalytic performance of the material is improved.
(3) After the ITO glass is treated by ozone, organic matters on the surface are decomposed by ultraviolet irradiation, an oxygen-rich layer is formed on the surface and carries a large number of hydroxyl groups, so that the glass surface has negative charges, and direct electrostatic alternative self-assembly is facilitated.
Drawings
FIG. 1 is a surface topography diagram of a nano-gold/nano-nickel composite electrode based on ITO.
FIG. 2 is a comparison of cyclic voltammograms of an ethanol solution and a blank solution;
wherein: a. ethanol solution, b, blank solution.
FIG. 3 is a plot of cyclic voltammetry for different sweep rates of ethanol solution;
wherein: a. 100mV/s, b, 80mV/s, c, 60mV/s, d, 40mV/s, e, 20 mV/s.
FIG. 4 is a standard curve of ethanol at different sweep rates;
wherein: a. 100mmol/L, b, 80mmol/L, c, 60mmol/L, d, 40mmol/L, e, 20 mmol/L.
FIG. 5 shows the response of different electrodes to ethanol;
wherein: a. Ni/Au, b, Ni.
Detailed Description
The technical solutions of the present invention are further described below with reference to the drawings and the specific embodiments, but the present invention is not limited to the embodiments in any way. In the examples, unless otherwise specified, the experimental methods are all conventional methods; unless otherwise indicated, the experimental reagents and materials were commercially available.
EXAMPLE 1 treatment of ITO glass
(1) And taking a piece of ITO glass to be used, testing the conductive surface of the ITO glass by using a universal meter, ensuring that the conductive surface faces downwards, and cutting the ITO glass with the size of 10 x 20mm for later use by using a glass cutter.
(2) The ITO glass is carefully placed in a clean beaker, preferably without stacking. Deionized water was slowly injected along the walls of the beaker until the glass was submerged or a little more. The beaker with the glass is placed in an ultrasonic instrument. The time length of the ultrasonic instrument is set for 30min, and the temperature is set to be 15 ℃. The beaker was placed in an ultrasonic instrument to observe whether the beaker floated. If floating, add the right amount of deionized water or subtract a small amount of water in the ultrasonic instrument. After 30min, the ITO glass is carefully clamped out by a pair of tweezers, and the glass is dried by nitrogen.
(3) The blow-dried glass was placed in a clean beaker and acetone was injected along the beaker wall until the glass was submerged or a little bit more. And (4) ultrasonic treatment. The beaker mouth was wrapped with tinfoil and placed in an ultrasonic instrument. The time length of the ultrasonic instrument is set for 30min, and the temperature is set to be 15 ℃. The beaker was placed in an ultrasonic instrument to observe whether the beaker floated. If floating, add appropriate amount of acetone. After 30min, the ITO glass is carefully clamped out by a pair of tweezers, and the glass is dried by nitrogen.
(4) The blow-dried glass is placed in a clean beaker, and ethanol is injected along the wall of the beaker until the glass is submerged or a little bit more. And (4) ultrasonic treatment. The beaker was placed in an ultrasonic instrument. The time length of the ultrasonic instrument is set for 30min, and the temperature is set to be 15 ℃. The beaker was placed in an ultrasonic instrument to observe whether the beaker floated. If floating, add appropriate amount of ethanol. After 30min, the ITO glass is carefully clamped out by a pair of tweezers, and the glass is blown dry by nitrogen. And placing the mixture in a culture dish for later use.
(5) And (3) placing the ITO glass in a PDDA (polydiene dimethyl ammonium chloride solution) solution for soaking for 5min, taking out, washing with deionized water, and drying by nitrogen. And putting the PDDA/ITO glass into a PSS (poly (4-styrene sodium sulfonate)) solution for self-assembly to obtain a layer of (PDDA/PSS) self-assembled film.
(6) And (5) repeating the step (5) to prepare six layers of self-assembled ITO glass.
Example 2 ITO/Nano Nickel-gold composite electrode preparation
The preparation method of the ITO/nano nickel-gold composite electrode comprises the following specific steps:
(1) flower-like nano gold deposition
Adopting a three-electrode system, and immersing an ITO electrode modified by a PDDA/PSS multilayer film into H2SO4(0.5M) and KAuCl4(1mg/mL) ofIn the mixture, a platinum electrode was used as a counter electrode and Ag/AgCl as a reference electrode. Setting the voltage to be-0.2V and the time to be 800s, and carrying out underpotential deposition. And (5) carrying out nitrogen protection on the electrode after deposition, and standing for standby after three days.
(2) Preparation of Ni-Au/ITO composite electrode
A three-electrode system is adopted, Au/ITO glass with a nano structure is used as a working electrode, an Ag/AgCl electrode and a platinum wire electrode are used as reference electrodes, and a counter electrode is placed in an electrolytic cell filled with nickel sulfate solution. Setting electrodeposition parameters of an electrochemical workstation by adopting a chronoamperometry method: voltage-1V, time 300 s. And immediately taking out the electrode, washing the electrode with deionized water for multiple times, and standing the electrode for later use under the protection of nitrogen after deposition.
The surface topography based on the ITO/nano nickel-gold composite electrode is shown in figure 1: the nano-particle size and distribution on the electrode are uniform, and the electrocatalysis performance is particularly outstanding.
Example 3 comparison of Cyclic voltammograms of ethanol solution and blank solution
Firstly, placing a three-electrode system in a KOH solution with the pH of 1 and the concentration of 1mol/L, scanning within a potential range of-0.2-1.3V by using a cyclic voltammetry method, and recording a cyclic voltammetry curve of a blank solution; then, the three-electrode system is placed in 100mmol/L ethanol solution to be detected containing 1mol/L KOH solution with the pH value of 14 as supporting electrolyte, and scanning is carried out within the potential range of-0.2-1.3V by using cyclic voltammetry, and the cyclic voltammetry curve of ethanol is recorded. As shown in fig. 2: the catalytic effect of the Au-Ni electrode at 100mmol/L ethanol was tested at a scan rate of 100 mV/s. From the figure, it can be seen that Au-Ni electrode has good catalytic activity to ethanol. The fuel composed of the Ni-Au/ITO electrode can efficiently convert the biological energy into the electric energy.
Example 4 Cyclic voltammetric response of NiNPs/AuNPs/ITO electrode to the same concentration of ethanol at different sweep rates
Sequentially placing the three-electrode system in 100mm ethanol solution to be tested containing 1mol/L KOH solution with the pH of 14 as supporting electrolyte, testing the ethanol solutions with different sweep rates at the same concentration, wherein the sweep rates are respectively 20mV/s, 40mV/s, 60mV/s, 80mV/s and 100mV/s, and scanning within a potential range of-0.2-1.3V by utilizing a cyclic voltammetry. Recording the cyclic voltammetry curves of ethanol with the same concentration and different sweep rates. As shown in the attached figure 3: as can be seen from the figure, with the continuous increase of the sweep rate, the oxidation current of the nano electrode in the ethanol solution is also continuously increased, the oxidation peak is also continuously increased, and a good linear response for catalyzing ethanol is presented, so that the Au-Ni electrode can be proved to be used for catalyzing ethanol to be diffusion control.
Example 5 cyclic voltammetry response of a NiNPs/AuNPs/ITO electrode to ethanol of different concentrations A three-electrode system was sequentially placed in 20mM, 40mM, 60mM, 80mM, 100mM ethanol solutions to be tested containing 0.1mol/L NaOH solution with pH 14 as supporting electrolyte, and scanned within a potential range of-0.2 to 1.3V using cyclic voltammetry. Cyclic voltammograms were recorded for no concentration of ethanol. As shown in fig. 4: as can be seen from the figure, with the increasing concentration, the oxidation current of the nano electrode in the ethanol solution also increases continuously, the oxidation peak also rises continuously, and the good linear response of catalyzing ethanol is presented.
Example 4 response of different electrodes to ethanol
Firstly, placing a three-electrode system in a KOH solution with the pH of 14 and the concentration of 1mol/L, scanning within a potential range of-0.2-1.3V by using a cyclic voltammetry method, and recording a cyclic voltammetry curve of ethanol. Then, changing a working electrode, taking a NiNPs/ITO electrode as the working electrode, scanning within a potential range of-0.2-1.3V by using cyclic voltammetry, and recording a cyclic voltammetry curve, as shown in the attached figure 5: the catalytic effect of the NiNPs/AuNPs/ITO electrode and the NiNPs/ITO electrode in a 1mol/L KOH solution with a pH of 14 as supporting electrolyte in a 100mm ethanol solution was tested at a scanning speed of 100 mV/s. It can be seen by comparing the voltammetry curves that the catalytic effect of the NiNPs/AuNPs/ITO electrode is far greater than that of the NiNPs/ITO electrode, so that the catalytic activity of the NiNPs/AuNPs/ITO electrode on ethanol is good. The fuel composed of the NiNPs/AuNPs/ITO electrode can efficiently convert the biological energy into the electric energy.
The above description is only for the purpose of creating a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can substitute or change the technical solution and the inventive concept of the present invention within the technical scope of the present invention.
Claims (3)
1. The method for processing the ITO glass is characterized by comprising the following steps in sequence:
(1) testing the ITO glass conductive surface with a multimeter, wherein the conductive surface faces downwards, and cutting with a glass cutter;
(2) placing the ITO glass in a container filled with deionized water, placing the container in an ultrasonic instrument, wherein the ultrasonic instrument lasts for 30min at the temperature of 15 ℃, and taking out nitrogen for drying;
(3) placing ITO glass in a container, injecting acetone, sealing the container opening with tinfoil, placing in an ultrasonic instrument for 30min at 15 ℃, taking out nitrogen and drying;
(4) placing ITO glass in a container, injecting ethanol, sealing the container opening with tinfoil, placing in an ultrasonic instrument for 30min at 15 ℃, taking out nitrogen and drying;
(5) placing ITO glass in an ultraviolet ozone cleaning machine, wherein the conductive surface is upward, and after ozone treatment is carried out for 25-35min, organic matters on the surface of the ITO glass are decomposed by ultraviolet irradiation, an oxygen-rich layer is formed on the surface and carries a large number of hydroxyl groups, and the surface of the glass is provided with negative charges;
(6) placing the ITO glass in a polydiene dimethyl ammonium chloride solution for soaking for 5min, taking out, washing with deionized water, drying by blowing with nitrogen, placing the PDDA/ITO glass in a poly (4-sodium styrene sulfonate) solution for soaking for 5min for self-assembly, and obtaining a layer of PDDA/PSS self-assembled film;
(7) and (5) repeating the step (6) to prepare the ITO glass with layer-by-layer self-assembly.
2. The method for treating ITO glass according to claim 1, wherein the step (5) is an ozone treatment for 30 min.
3. Use of the method of treating ITO glass according to claim 1 in the construction of an ethanol fuel cell.
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Citations (4)
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| CN106198659A (en) * | 2016-07-15 | 2016-12-07 | 大连大学 | A kind of method depositing nanometer gold in micro-fluidic duct |
| CN108195911A (en) * | 2017-12-22 | 2018-06-22 | 大连大学 | A kind of preparation method and application that can be used repeatedly the Ag/AgCl microelectrodes based on PDMS |
| CN108982632A (en) * | 2018-07-26 | 2018-12-11 | 大连大学 | A kind of flexible electrode and preparation method thereof based on flower-like nanometer gold structure |
| CN109298060A (en) * | 2018-10-18 | 2019-02-01 | 大连大学 | A method of the preparation of the functionalized multi-wall carbonnanotubes modified electrode based on ITO and apply the determination of electrode uric acid |
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2019
- 2019-12-16 CN CN201911294217.7A patent/CN112979180A/en active Pending
Patent Citations (4)
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|---|---|---|---|---|
| CN106198659A (en) * | 2016-07-15 | 2016-12-07 | 大连大学 | A kind of method depositing nanometer gold in micro-fluidic duct |
| CN108195911A (en) * | 2017-12-22 | 2018-06-22 | 大连大学 | A kind of preparation method and application that can be used repeatedly the Ag/AgCl microelectrodes based on PDMS |
| CN108982632A (en) * | 2018-07-26 | 2018-12-11 | 大连大学 | A kind of flexible electrode and preparation method thereof based on flower-like nanometer gold structure |
| CN109298060A (en) * | 2018-10-18 | 2019-02-01 | 大连大学 | A method of the preparation of the functionalized multi-wall carbonnanotubes modified electrode based on ITO and apply the determination of electrode uric acid |
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| YUYING GAO ET AL: "Electrosynthesis of poly(3,4-ethylenedioxythiophene) microcups in the aqueous solution of LiClO4 and tri(ethylene glycol)", 《POLYMER》 * |
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