CN111453761A - Preparation method of ZnO nano particle film - Google Patents
Preparation method of ZnO nano particle film Download PDFInfo
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- CN111453761A CN111453761A CN202010378640.1A CN202010378640A CN111453761A CN 111453761 A CN111453761 A CN 111453761A CN 202010378640 A CN202010378640 A CN 202010378640A CN 111453761 A CN111453761 A CN 111453761A
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- 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
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Abstract
A preparation method of a ZnO nano-particle film. The preparation method comprises the steps of preparing solution and sol, treating a substrate, spin-coating a film and performing heat treatment. The method is used for preparing the ZnO nano-particle film.
Description
The technical field is as follows:
the invention relates to a preparation method of a ZnO nano particle film.
Background art:
the ZnO nano particle film switch has the characteristics of simple structure, attractive and flat appearance, light and thin finished product, good sealing effect, light touch connection type, long service life and the like, but the problem that how to manufacture a ZnO nano particle film suitable for the film switch needs to be solved.
The invention content is as follows:
the invention aims to provide a preparation method of a ZnO nanoparticle film, which is suitable for a ZnO nanoparticle film switch and has a good using effect.
The above purpose is realized by the following technical scheme:
a process for preparing the nano ZnO particle film includes such steps as preparing solution and sol, treating substrate, spin coating and heat treating.
A preparation method of a ZnO nanoparticle film comprises the steps of firstly weighing a plurality of Zn (CH3COO) 2.2H 20 on an electronic balance, dissolving the Zn (CH3COO) 2.2H 20 in 25 ml of absolute ethyl alcohol, fully stirring at 60 ℃ for 60min to form a transparent homogeneous zinc solution with the concentration of Zn2+ of 0.8 mol/L, taking 5 ml of 0.8 mol/L ZnO sol by a micropipette, taking O.2 ml of O.5 mol/L prepared according to a reaction metering ratio, dripping NaOH into the ZnO sol, transferring the mixed solution into a reaction kettle, covering and sealing, putting the reaction kettle into a 80 ℃ constant-temperature water bath kettle for heating for 24 hours, after the reaction is finished, taking out the reaction kettle, naturally cooling the reaction kettle to room temperature, pouring out an upper clear solution, obtaining a mixed substance of white Zn O nanoparticles and certain organic residues, drying at 50 ℃ for 30min to volatilize organic matters to obtain white powder, centrifuging the obtained particle product, washing with water, washing alcohol for multiple times, oscillating the white Zn O nanoparticles, and dispersing the white pure organic residues in the ethanol by ultrasound.
The preparation method of the ZnO nano-particle film comprises the steps of treating a substrate, firstly cleaning the substrate, and ultrasonically cleaning transparent conductive glass for 7-13 min by using a cleaning solution; boiling with deionized water twice, and ultrasonically oscillating with hot deionized water for 7-13 min; washing off residual inorganic matters and organic matters on the ITO transparent conductive glass substrate; then sequentially ultrasonically oscillating for 7-13 min by using acetone, absolute ethyl alcohol, deionized water and absolute ethyl alcohol respectively; and finally, the cleaned ITO transparent conductive glass is placed on a heating platform to be dried at 90-110 ℃ with the conductive surface facing upwards determined by a multimeter.
The preparation method of the ZnO nano-particle film comprises the steps of treating a substrate, firstly cleaning the substrate, and ultrasonically cleaning transparent conductive glass for 10min by using a cleaning solution; boiling with deionized water twice, and ultrasonically oscillating with hot deionized water for 10 min; washing off residual inorganic matters and organic matters on the ITO transparent conductive glass substrate; then sequentially ultrasonically oscillating for 10min by using acetone, absolute ethyl alcohol, deionized water and absolute ethyl alcohol respectively; and finally, the cleaned ITO transparent conductive glass is placed on a heating platform to be dried at the temperature of 100 ℃ with the conductive surface facing upwards determined by a multimeter.
According to the preparation method of the ZnO nano particle film, the film is spin-coated and is subjected to heat treatment, and a KW-4A type spin coater is selected for preparing a film sample; adjusting the rotating speed of the spin coater to obtain the required thickness of the film; uniformly mixing the obtained sol on a spin coater at a speed of 1300-; and finally, putting the coated substrate in a box furnace for annealing treatment at the heat treatment temperature of 200-300 ℃ for 20-40min, preserving the heat for 5-15min, naturally cooling, and taking out the sample to obtain the ZnO nano particle film.
According to the preparation method of the ZnO nano particle film, the film is spin-coated and is subjected to heat treatment, and a KW-4A type spin coater is selected for preparing a film sample; adjusting the rotating speed of the spin coater to obtain the required thickness of the film; homogenizing the obtained sol on a homogenizing machine at 1500 r/min for 5S, homogenizing at 3000 r/min for 30S, and drying in a drying oven at 80 deg.C for 15 min; and finally, putting the coated substrate in a box furnace for annealing treatment, annealing at the heat treatment temperature of 250 ℃ for 30min, preserving the heat for 10min, naturally cooling, and taking out the sample to obtain the ZnO nano particle film.
Has the advantages that:
1. the film switch mainly comprises a ZnO nano particle film, a conductive silver paste circuit layer, an insulating ink layer and the like, wherein the circuit of the film switch is formed by printing a conductive silver paste circuit and has the function of serving as a transmission medium of an electric signal, and the distribution uniformity of the conductive silver paste layer directly influences the resistance characteristic of the conductive silver paste layer, so that the film switch can be produced quickly, and the production efficiency is improved; the light-cured insulating ink is tried to be used, so that the color difference of a finished product caused by hot air interference during the heat curing of an oven is avoided; proper process parameters are selected, so that the uniform thickness, the resistance matching and the small sawtooth edge effect of the conductive silver paste circuit are ensured.
Description of the drawings:
FIG. 1 is a schematic diagram of the preparation process of the metal oxide thin film device.
FIG. 1 (A) conductive substrate cleaning; (B) dropwise adding of metal oxide gel: (C) spin coating of a metal oxide film: (D) annealing and drying to obtain a metal oxide film; (E) the film is tested for electrical properties.
The specific implementation mode is as follows:
the technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings of the present invention.
Example 1:
a process for preparing the nano ZnO particle film includes such steps as preparing solution and sol, treating substrate, spin coating and heat treating.
Example 2:
the preparation method of the ZnO nanoparticle film described in example 1 comprises the steps of firstly weighing a plurality of Zn (CH3COO) 2.2H 20 on an electronic balance, dissolving the Zn (CH3COO) 2.2H 20 in 25 ml of absolute ethyl alcohol, fully stirring at 60 ℃ for 60min to form a transparent homogeneous zinc solution with Zn2+ concentration of 0.8 mol/L, taking 5 ml of 0.8 mol/L ZnO sol by a micropipette, taking O.2 ml of O.5 mol/L prepared according to the reaction metering ratio, dripping NaOH into the ZnO sol, transferring the mixed solution into a reaction kettle, covering and sealing the reaction kettle, placing the reaction kettle into a 80 ℃ constant-temperature water bath kettle to heat for 24 hours, taking out the reaction kettle after the reaction is completed, naturally cooling the reaction kettle to room temperature, pouring off supernatant clear liquid to obtain a mixed substance of white Zn O nanoparticles and certain organic residues, drying the organic substances at 50 ℃ for 30min to volatilize the organic substances to obtain white powder, washing the obtained particles with water, standby alcohol, washing the white water, ultrasonically oscillating the ZnO and ultrasonically dispersing the white nanoparticles to obtain pure organic nanoparticles.
Example 3:
the preparation method of the ZnO nano-particle film in the embodiment 1, the substrate is treated, firstly, the substrate is cleaned, and the transparent conductive glass is cleaned by ultrasonic for 7-13 min by using a cleaning solution; boiling with deionized water twice, and ultrasonically oscillating with hot deionized water for 7-13 min; washing off residual inorganic matters and organic matters on the ITO transparent conductive glass substrate; then sequentially ultrasonically oscillating for 7-13 min by using acetone, absolute ethyl alcohol, deionized water and absolute ethyl alcohol respectively; and finally, the cleaned ITO transparent conductive glass is placed on a heating platform to be dried at 90-110 ℃ with the conductive surface facing upwards determined by a multimeter.
Example 4:
the preparation method of the ZnO nanoparticle thin film in embodiment 3, wherein the substrate is treated by firstly cleaning the substrate, and ultrasonically cleaning transparent conductive glass for 10min by using a cleaning solution; boiling with deionized water twice, and ultrasonically oscillating with hot deionized water for 10 min; washing off residual inorganic matters and organic matters on the ITO transparent conductive glass substrate; then sequentially ultrasonically oscillating for 10min by using acetone, absolute ethyl alcohol, deionized water and absolute ethyl alcohol respectively; and finally, the cleaned ITO transparent conductive glass is placed on a heating platform to be dried at the temperature of 100 ℃ with the conductive surface facing upwards determined by a multimeter.
Example 5:
the preparation method of the ZnO nanoparticle film of embodiment 1, spin-coating the film and heat-treating, selecting a KW-4A type spin coater to prepare the film sample; adjusting the rotating speed of the spin coater to obtain the required thickness of the film; uniformly mixing the obtained sol on a spin coater at a speed of 1300-; and finally, putting the coated substrate in a box furnace for annealing treatment at the heat treatment temperature of 200-300 ℃ for 20-40min, preserving the heat for 5-15min, naturally cooling, and taking out the sample to obtain the ZnO nano particle film.
Example 6:
the method for preparing a ZnO nanoparticle thin film of embodiment 5, wherein the spin coating of the thin film and the heat treatment are carried out by preparing a thin film sample by using a KW-4A type spin coater; adjusting the rotating speed of the spin coater to obtain the required thickness of the film; homogenizing the obtained sol on a homogenizing machine at 1500 r/min for 5S, homogenizing at 3000 r/min for 30S, and drying in a drying oven at 80 deg.C for 15 min; and finally, putting the coated substrate in a box furnace for annealing treatment, annealing at the heat treatment temperature of 250 ℃ for 30min, preserving the heat for 10min, naturally cooling, and taking out the sample to obtain the ZnO nano particle film.
Example 7:
the preparation method of the ZnO nanoparticle thin film in embodiment 3, wherein the substrate is treated by firstly cleaning the substrate, and ultrasonically cleaning transparent conductive glass for 7min by using a cleaning solution; boiling with deionized water twice, and ultrasonically oscillating with hot deionized water for 7 min; washing off residual inorganic matters and organic matters on the ITO transparent conductive glass substrate; then sequentially ultrasonically oscillating for 7min by using acetone, absolute ethyl alcohol, deionized water and absolute ethyl alcohol respectively; and finally, the cleaned ITO transparent conductive glass is placed on a heating platform to be dried at 90 ℃ with the conductive surface facing upwards determined by a multimeter.
Example 8:
the preparation method of the ZnO nanoparticle thin film in embodiment 3, wherein the substrate is treated by firstly cleaning the substrate, and ultrasonically cleaning transparent conductive glass for 13 min by using a cleaning solution; boiling with deionized water twice, and ultrasonically oscillating with hot deionized water for 13 min; washing off residual inorganic matters and organic matters on the ITO transparent conductive glass substrate; then sequentially ultrasonically oscillating for 13 min by using acetone, absolute ethyl alcohol, deionized water and absolute ethyl alcohol respectively; and finally, the cleaned ITO transparent conductive glass is placed on a heating platform to be dried at the temperature of 110 ℃ with the conductive surface facing upwards determined by a multimeter.
Example 9:
the method for preparing a ZnO nanoparticle thin film of embodiment 5, wherein the spin coating of the thin film and the heat treatment are carried out by preparing a thin film sample by using a KW-4A type spin coater; adjusting the rotating speed of the spin coater to obtain the required thickness of the film; homogenizing the obtained sol on a homogenizing machine at 1300 r/min for 5S, homogenizing at 2800 r/min for 20S, and drying in a drying oven at 70 deg.C for 10 min; and finally, putting the coated substrate in a box furnace for annealing treatment, annealing at the heat treatment temperature of 200 ℃ for 20min, preserving the heat for 5min, naturally cooling, and taking out the sample to obtain the ZnO nano particle film.
Example 10:
the method for preparing a ZnO nanoparticle thin film of embodiment 5, wherein the spin coating of the thin film and the heat treatment are carried out by preparing a thin film sample by using a KW-4A type spin coater; adjusting the rotating speed of the spin coater to obtain the required thickness of the film; homogenizing the obtained sol on a homogenizing machine at 1700 r/min for 5S, homogenizing at 3200 r/min for 40S, and drying in a drying oven at 90 deg.C for 20 min; and finally, putting the coated substrate in a box furnace for annealing treatment, annealing at the heat treatment temperature of 300 ℃ for 40min, preserving the heat for 15min, naturally cooling, and taking out the sample to obtain the ZnO nano particle film.
Example 11:
in the method for preparing a ZnO nanoparticle thin film described in embodiment 3, the substrate is treated by first cleaning the substrate, and the substrate for preparing an organic thin film includes indium tin oxide ITO transparent conductive glass and a microscope slide; the ITO transparent conductive glass was used for electrical property testing and SEM characterization, and the microscope slide was used for XRD characterization. The ITO transparent conductive glass is manufactured by coating a layer of indium tin oxide (commonly called ITO) film on a soda-lime-based or silicon-boron-based substrate glass by a magnetron sputtering method, is widely applied to the fields of liquid crystal displays, solar cells, photoelectrons and various optics, and also begins to be applied to experimental research as an electrode due to good light transmittance and electrical conductivity. The ITO transparent conductive glass (square resistance is 20D./cmz, transmittance is 90%. the surface state of the ITO transparent conductive glass directly influences the hole injection capability, the electronic state of an organic film interface and the film forming property of an organic material, because the cleanness and the flatness of a substrate have great influence on the film performance, and because the thickness of the organic film manufactured by the method is only dozens of nanometers, any foreign matter pollutes the substrate to cause the change of the film appearance, the cleaning of the ITO transparent conductive glass substrate is a very important process, the cleaning of the ITO transparent conductive glass adopts the following steps of ultrasonically cleaning the transparent conductive glass for 7-13 min by using a cleaning solution, boiling the transparent conductive glass twice by using deionized water, ultrasonically oscillating the transparent conductive glass for 7-13 min by using hot deionized water, washing off residual inorganic matters and organic matters on the ITO transparent conductive glass substrate, and respectively using acetone, acetone and water to clean the ITO transparent conductive glass, Sequentially ultrasonically oscillating anhydrous ethanol, deionized water and anhydrous ethanol for 7-13 min; and finally, the cleaned ITO transparent conductive glass is placed on a heating platform to be dried at 90-110 ℃ with the conductive surface facing upwards determined by a multimeter. All the above experiments were performed at room temperature. The cleaning process of the microscope slide is similar to the cleaning process of the ITO conductive glass.
Example 12:
in the preparation method of the ZnO nanoparticle thin film in embodiment 5, the thin film is spin-coated and heat-treated, and in the experiment of the item, a KW-4A type spin coater is selected to prepare a thin film sample; in the experiment, the required film thickness can be obtained by adjusting the rotating speed of a spin coater; homogenizing the obtained sol on a homogenizing machine at 1500 r/min for 5S, homogenizing at 3000 r/min for 30S, and drying in a drying oven at 80 deg.C for 15 min; and finally, putting the coated substrate in a box furnace for annealing treatment, annealing at the heat treatment temperature of 250 ℃ for 30min, preserving the heat for 10min, naturally cooling, and taking out the sample to obtain the ZnO nano particle film.
Example 13:
the preparation method of ZnO nanoparticle film described in example 2 is that 0.8 mol/L ZnO sol 5 ml is taken by micropipette, then 0.2 ml 0.5 mol/L prepared according to reaction metering ratio is taken, 1 NaOH is slowly dropped into ZnO sol, milky flocculent deposition appears when dropping, the mixed solution is transferred into a reaction kettle, covered and sealed, and put into an 80 ℃ constant temperature water bath kettle to be heated for 24 hours, the size of the particles has a close relation with the growth temperature and the growth time, if the temperature is too high or the growth time is too long, ZnO small particles will agglomerate to form particles with larger particle size, so we must strictly control the growth temperature and time of the nanoparticles, in the solution containing OH, ZnO nanoparticles are formed by two ways, one is a fast nucleation and growth process of ZnO particles under Zn2+ excess condition (1 → 2), the other is a slow nucleation and growth process under OH excess condition (1 → 3 → 4), the reaction is taken out for standby after the reaction, the reaction kettle is cooled to room temperature, white organic particles are obtained by natural washing, white organic particles are washed, and dried, white organic particles are obtained by shaking, and white organic particles are obtained by centrifugation, and the white organic particles are obtained by shaking.
Claims (6)
1. A preparation method of a ZnO nano-particle film is characterized by comprising the steps of preparing solution and sol, treating a substrate, spin-coating the film and performing heat treatment.
2. The process of claim 1, wherein the preparation of the solution and sol comprises weighing several Zn (CH3COO) 2.2H 20 on an electronic balance, dissolving in 25 ml absolute ethanol, stirring at 60 deg.C for 60min to obtain a transparent homogeneous zinc solution with Zn2+ concentration of 0.8 mol/L, taking 5 ml ZnO sol with 0.8 mol/L mol, adding O.2 ml O.5 mol/L prepared according to the reaction ratio, dropping NaOH into the ZnO sol, transferring the mixed solution into a reaction kettle, sealing, heating in a 80 deg.C constant temperature water bath for 24 hr, reacting, cooling naturally to room temperature, pouring off the upper clear solution to obtain a mixture of white Zn O nanoparticles and some organic residues, drying at 50 deg.C for 30min to volatilize the organic matter to obtain white powder, washing the obtained particle product with water, washing with alcohol, and ultrasonic vibration to obtain white nano particles without water, and dispersing in ethanol.
3. The method for preparing the ZnO nano-particle film according to claim 1, wherein the substrate is treated by firstly cleaning the substrate, and ultrasonically cleaning transparent conductive glass for 7-13 min by using a cleaning solution; boiling with deionized water twice, and ultrasonically oscillating with hot deionized water for 7-13 min; washing off residual inorganic matters and organic matters on the ITO transparent conductive glass substrate; then sequentially ultrasonically oscillating for 7-13 min by using acetone, absolute ethyl alcohol, deionized water and absolute ethyl alcohol respectively; and finally, the cleaned ITO transparent conductive glass is placed on a heating platform to be dried at 90-110 ℃ with the conductive surface facing upwards determined by a multimeter.
4. The method for preparing the ZnO nano-particle film according to claim 3, wherein the treatment of the substrate comprises the steps of firstly cleaning the substrate, and ultrasonically cleaning transparent conductive glass for 10min by using a cleaning solution; boiling with deionized water twice, and ultrasonically oscillating with hot deionized water for 10 min; washing off residual inorganic matters and organic matters on the ITO transparent conductive glass substrate; then sequentially ultrasonically oscillating for 10min by using acetone, absolute ethyl alcohol, deionized water and absolute ethyl alcohol respectively; and finally, the cleaned ITO transparent conductive glass is placed on a heating platform to be dried at the temperature of 100 ℃ with the conductive surface facing upwards determined by a multimeter.
5. The preparation method of the ZnO nano-particle film according to claim 1, which is characterized in that the spin coating of the film and the heat treatment are carried out by preparing a film sample by using a KW-4A type spin coater; adjusting the rotating speed of the spin coater to obtain the required thickness of the film; uniformly mixing the obtained sol on a spin coater at a speed of 1300-; and finally, putting the coated substrate in a box furnace for annealing treatment at the heat treatment temperature of 200-300 ℃ for 20-40min, preserving the heat for 5-15min, naturally cooling, and taking out the sample to obtain the ZnO nano particle film.
6. The method for preparing the ZnO nano-particle film according to claim 5, which is characterized in that the spin coating of the film and the heat treatment are carried out by preparing a film sample by using a KW-4A type spin coater; adjusting the rotating speed of the spin coater to obtain the required thickness of the film; homogenizing the obtained sol on a homogenizing machine at 1500 r/min for 5S, homogenizing at 3000 r/min for 30S, and drying in a drying oven at 80 deg.C for 15 min; and finally, putting the coated substrate in a box furnace for annealing treatment, annealing at the heat treatment temperature of 250 ℃ for 30min, preserving the heat for 10min, naturally cooling, and taking out the sample to obtain the ZnO nano particle film.
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