CN103073048A - Method for preparing patterned ZnO film by liquid phase self-assembly technology - Google Patents
Method for preparing patterned ZnO film by liquid phase self-assembly technology Download PDFInfo
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- CN103073048A CN103073048A CN2012105663755A CN201210566375A CN103073048A CN 103073048 A CN103073048 A CN 103073048A CN 2012105663755 A CN2012105663755 A CN 2012105663755A CN 201210566375 A CN201210566375 A CN 201210566375A CN 103073048 A CN103073048 A CN 103073048A
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Abstract
The invention discloses a method for preparing a patterned ZnO film by a liquid phase self-assembly technology. Zn(NO3)2.6H2O and NH4F, as raw materials, are dissolved in distilled water to prepare precursor liquid; a substrate is dipped in OTS-toluene solution to prepare an OTS-SAMs; after being dried, the OTS-SAMs film is irradiated under ultraviolet light to obtain a substrate which is provided with a functionalized OTS-SAMs film on the surface; the surface of the substrate with the functionalized OTS-SAMs film is downwards suspended on the surface of the precursor liquid at the temperature of 70-80 DEG C, so that the functionalized OTS-SAMs film is contacted with the precursor liquid; an amorphous state ZnO film is prepared by depositing for 20 hours through the reverse absorption method; and after being dried, the amorphous state film is insulated at the temperature of 300 DEG C and is annealed to obtain the crystallized and patterned ZnO film. The method has simple technique and lower experimental condition requirements; and the obtained ZnO film is uniform and compact. The method is applied in the preparation of the patterned ZnO film, and has wide application prospects in the microelectronic field.
Description
[technical field]
The invention belongs to field of functional materials, be specifically related to the method that a kind of liquid phase self-assembling technique prepares the ZnO film of patterning.
[background technology]
In the last few years, along with the tremendous development of information science technology, semiconductor material with wide forbidden band is owing to it has caused people's extensive concern in the potential application aspect superpower and high-frequency element, ultraviolet detector, short-wave long light-emitting diode, laser apparatus and the related device thereof.Have the characteristics such as energy gap is large, the electronic drift saturating speed is high, specific inductivity is little as third generation semiconductor material ZnO.It is a kind of novel II-IV family semiconductor material with wide forbidden band, and band gap 3.37eV is typical directly wide band gap semiconducter.This character makes it at field of photoelectric devices very large application prospect be arranged.And the ZnO film emission wavelength is also shorter than the blue light wavelength of GaN, can further improve the density of optical storage.ZnO is abundant, cheap with its source, toxicity is little, and having again many good over-all propertieies such as very high thermostability and chemical stability has become the new generation broadband gap semiconductor material.These excellent specific properties that ZnO film has make it obtain comparatively extensively and effectively using in the various fields such as photoelectric device, solar cell, surface acoustic wave device, nonlinear optics device, ultraviolet light detector, gas sensor, humidity-sensitive material, pressure-sensitive device.
Different application is respectively had any different to the requirement of the character such as crystalline orientation, film thickness, surface finish and the photoelectricity of ZnO film, piezoelectricity.These differences are to be determined by different technologies of preparing and processing parameter, and various preparation technologies respectively have its relative merits.So in order to prepare the ZnO film of different performance, be from various techniques preparation characteristic separately.The preparation method of ZnO film mainly contains at present: magnetron sputtering method, metal-organic chemical vapor deposition equipment, pulsed laser deposition, spraying thermolysis, sol-gel method, molecular beam epitaxy, electrochemical deposition etc.
Self-assembled monolayer (self-assembled monolayers) technology (being called for short the SAMs technology) is the core technology of bionical synthesis technique, it is by producing chemisorption between an activity base of tensio-active agent and the substrate, the orderly molecule assembled layers of spontaneous formation on the interface.The SAMs technology at first is applied to the very thin super film of field of polymer technology preparation.Because to be that organic molecule (perhaps organic molecule steam) in solution is spontaneous be adsorbed on formed ultra-thin organic membrane on the solid substrate by chemical bond to SAMs securely, so it has the spontaneous formation of original position, becomes that the key high-sequential is arranged, defective is few, bonding force is strong, be characteristics such as " crystal forms ".Because the distinctive advantage of SAMs technology, its utilization is also more and more wider, especially in the utilization of film preparation.For self-assembling technique making ZnO film, be in the stage of fumbling, prepared ZnO film also is not observed it and has dielectric properties.
[summary of the invention]
The purpose of this invention is to provide the method that a kind of liquid phase self-assembling technique prepares the ZnO film of patterning, prepare the ZnO film with (002) and (101) crystal face preferential growth; The inventive method requirement for experiment condition is lower, the ZnO film even compact that obtains, and First Observation has good dielectric properties to the ZnO film by the self-assembling method preparation.
For achieving the above object, the technical solution used in the present invention is:
A kind of liquid phase self-assembling technique prepares the method for the ZnO film of patterning, may further comprise the steps:
Step 1: the configuration of precursor liquid: with Zn (NO
3)
26H
2O and NH
4F is dissolved in the distilled water, is made into Zn (NO
3)
26H
2O concentration is 0.05mol/L, NH
4F concentration is the mixed solution of 0.2 ~ 0.3mol/L, and the pH value of regulating mixed solution is 5.5, mixes liquid under the room temperature to fully clarification, obtains precursor liquid;
Step 2: the functionalization of substrate: with the substrate washes clean, be to soak preparation OTS-SAMs film in 1% the OTS-toluene solution in volumetric concentration, with under UV-light, shining behind the dry removal of the OTS-SAMs film organism, obtain the substrate that the surface has the OTS-SAMs film of functionalization;
Step 3: the deposition of film: facing down and be suspended in the precursor liquid surface of functionalization OTS-SAMs film of substrate that the surface is had the OTS-SAMs film of functionalization, functionalization OTS-SAMs film is contacted with precursor liquid, prepare noncrystalline membrane 70 ℃～80 ℃ depositions;
Step 4: the crystallization of film: put into retort furnace after the noncrystalline membrane drying with preparation, obtain the ZnO film of the patterning of crystallization in 300 ℃ of insulation annealing 120min.
The present invention further improves and is: adopting concentration in the step 1 is the HNO of 4mol/L
3Solution and concentration are that the NaOH solution of 3mol/L is regulated the pH of mixed value.
The present invention further improves and is: the concrete operations of substrate washing are in the step 2: substrate is placed respectively deionized water, acetone, dehydrated alcohol supersound washing 10min.
The present invention further improves and is: the time that substrate soaks in volumetric concentration is 1% OTS-toluene solution in the step 2 is 30min, shines 20min through under the UV-light first before the immersion.
The present invention further improves and is: the OTS-SAMs film is to shine 40min under the UV-light of 184.9nm at wavelength in the step 2.
The present invention further improves and is: dry actual conditions is at 120 ℃ of dry 5min in the step 2.
The present invention further improves and is: depositing time is 20h in the step 3.
The present invention further improves and is: the drying in the step 4 is at room temperature carried out.
The present invention further improves and is: cover photomask at the OTS-SAMs film when OTS-SAMs film shines under UV-light in the step 2.
With respect to prior art, the present invention has following beneficial effect:
The present invention proposes a kind of technology of novel making ZnO film: at first prepare precursor liquid, then utilize the liquid phase self-assembling technique to prepare the OTS-SAMs film, the recycling UV-irradiation is carried out functional modification to the OTS-SAMs film, functionalization OTS-SAMs film after the modification is contacted with precursor liquid, prepare the ZnO film of patterning by reverse adsorption at the OTS-SAMs of functionalization film.The present invention by reverse adsorption, prepares the ZnO film with (002) and (101) crystal face preferential growth in conjunction with the advantage of liquid phase self-assembly.Technique of the present invention is simple, and requirement for experiment condition is lower, the ZnO film even compact that obtains.The present invention is the successful Application to autonomous packing technique, also is a kind of breakthrough progress of ZnO film technology of preparing simultaneously.Method of the present invention is applied to the preparation of patterning ZnO film, has broad application prospects at microelectronic.
The further beneficial effect of the present invention is: the present invention adopts the short wave ultraviolet light radiation instrument as ultraviolet source, it is the ultraviolet ray of 184.9nm that wavelength is provided, under the covering of photomask, OTS-SAMs film on the substrate is carried out etching (modification), so that the OTS-SAMs film is subjected to the zone of UV-irradiation owing to the formation of silanol, matrix surface is good wetting ability; And be not the alkyl zone by the zone of UV-irradiation, matrix surface presents original hydrophobicity, obtain the OTS-SAMs film of the patterning of functionalization, and utilize the liquid phase self-assembling technique to prepare the patterning ZnO film at the OTS-SAMs of the patterning of functionalization film, method of the present invention is applied to the preparation of patterning ZnO film, has broad application prospects at microelectronic.
[description of drawings]
Fig. 1 is the metallurgical microscopic of the ZnO film of the patterning that obtains of the embodiment of the invention 1;
Fig. 2 is the metallurgical microscopic of the ZnO film of the patterning that obtains of the embodiment of the invention 2;
Fig. 3 is the metallurgical microscopic of the ZnO film of the patterning that obtains of the embodiment of the invention 3;
Fig. 4 is the XRD figure spectrum of the ZnO film of the patterning that obtains of embodiments of the invention, (a) be that embodiment 3, (b) are embodiment 1 for embodiment 2, (c);
Fig. 5 is the SEM figure of the ZnO film of the patterning that obtains of the embodiment of the invention 2;
Fig. 6 is the metallurgical microscopic of the ZnO film of the patterning that obtains of the embodiment of the invention 6;
Fig. 7 is the metallurgical microscopic of the ZnO film of the patterning that obtains of the embodiment of the invention 7.
[embodiment]
The invention will be further described below in conjunction with embodiment and accompanying drawing.
Embodiment 1
A kind of liquid phase self-assembling technique prepares the method for the ZnO film of patterning, may further comprise the steps:
Step 1: the configuration of precursor liquid: with the Zn (NO of 0.0025mol
3)
26H
2The NH of O and 0.01mol
4F is dissolved in the 50ml distilled water, is made into Zn (NO
3)
26H
2O concentration is 0.05mol/L, NH
4F concentration is the mixed solution of 0.2mol/L, is the HNO of 4mol/L with concentration
3Solution and concentration are that the pH value of the NaOH solution adjusting mixed solution of 3mol/L is 5.5, mix liquid under the room temperature to fully clarification, get precursor liquid.
Step 2: the functionalization of substrate: substrate is placed respectively deionized water, acetone, dehydrated alcohol supersound washing 10min.Behind irradiation 20min under the UV-light, be to soak 30min in 1% the OTS-toluene solution to prepare the OTS-SAMs film in volumetric concentration, (λ=184.9nm) shine down 40min obtains the substrate that the surface has functionalization OTS-SAMs film in UV-light after 120 ℃ of dry 5min remove organism with the OTS-SAMs film.
Step 3: the deposition of film: facing down and be suspended in the precursor liquid surface of functionalization OTS-SAMs film of substrate that the surface is had the OTS-SAMs film of functionalization, functionalization OTS-SAMs film is contacted with precursor liquid, prepare noncrystalline membrane at 80 ℃ of deposition 20h.
Step 4: the crystallization of film: the noncrystalline membrane of preparation is put into retort furnace after drying at room temperature, obtain the ZnO film of the patterning of crystallization in 300 ℃ of insulation annealing 120min.
The ZnO film of the patterning of the liquid phase self-assembling technique preparation that embodiment 1 is obtained carries out the metallography microscope test and XRD tests, and Fig. 1 is the metallurgical microscopic of the ZnO film of the patterning that obtains of the embodiment of the invention 1; The XRD figure spectrum of the ZnO film of the patterning that the curve among Fig. 4 (c) obtains for embodiments of the invention 1, the ZnO film of embodiment 1 preparation is the ZnO film of (002) and (101) crystal face preferential growth as can be seen from Figure 4.
Embodiment 2
A kind of liquid phase self-assembling technique prepares the method for the ZnO film of patterning, may further comprise the steps:
Step 1: the configuration of precursor liquid: with the Zn (NO of 0.0025mol
3)
26H
2The NH of O and 0.0125mol
4F is dissolved in the 50ml distilled water, is made into Zn (NO
3)
26H
2O concentration is 0.05mol/L, NH
4F concentration is the mixed solution of 0.25mol/L, is the HNO of 4mol/L with concentration
3Solution and concentration are that the pH value of the NaOH solution adjusting mixed solution of 3mol/L is 5.5, mix liquid under the room temperature to fully clarification, get precursor liquid.
Step 2: the functionalization of substrate: substrate is placed respectively deionized water, acetone, dehydrated alcohol supersound washing 10min.Behind irradiation 20min under the UV-light, be to soak 30min in 1% the OTS-toluene solution to prepare the OTS-SAMs film in volumetric concentration, (λ=184.9nm) shine down 40min obtains the glass substrate that the surface has functionalization OTS-SAMs film in UV-light after 120 ℃ of dry 5min remove organism with the OTS-SAMs film.
Step 3: the deposition of film: the surface has facing down and be suspended in the precursor liquid surface of functionalization OTS-SAMs film of substrate of the OTS-SAMs film of functionalization, and functionalization OTS-SAMs film is contacted with precursor liquid, prepares noncrystalline membrane at 80 ℃ of deposition 20h.
Step 4: the crystallization of film: the noncrystalline membrane of preparation is put into retort furnace after drying at room temperature, obtain the ZnO film of the patterning of crystallization in 300 ℃ of insulation annealing 120min.
The ZnO film of the patterning that embodiment 2 is obtained carries out metallography microscope test, XRD test and SEM test, and Fig. 2 is the metallurgical microscopic of the ZnO film of the patterning that obtains of the embodiment of the invention 2; The XRD figure spectrum of the ZnO film of the patterning that the curve among Fig. 4 (b) obtains for embodiments of the invention 2, the ZnO film of embodiment 2 preparations is the ZnO film of (002) and (101) crystal face preferential growth as can be seen from Figure 4; Fig. 5 is the SEM figure of the ZnO film of the patterning that obtains of the embodiment of the invention 2.
Embodiment 3
A kind of liquid phase self-assembling technique prepares the method for the ZnO film of patterning, may further comprise the steps:
Step 1: the configuration of precursor liquid: with the Zn (NO of 0.0025mol
3)
26H
2The NH of O and 0.0150mol
4F is dissolved in the 50ml distilled water, is made into Zn (NO
3)
26H
2O concentration is 0.05mol/L, NH
4F concentration is the mixed solution of 0.3mol/L, is the HNO of 4mol/L with concentration
3Solution and concentration are that the pH value of the NaOH solution adjusting mixed solution of 3mol/L is 5.5, mix liquid under the room temperature to fully clarification, get precursor liquid.
Step 2: the functionalization of substrate: substrate is placed respectively deionized water, acetone, dehydrated alcohol supersound washing 10min.Behind irradiation 20min under the UV-light, be to soak 30min in 1% the OTS-toluene solution to prepare the OTS-SAMs film in volumetric concentration, (λ=184.9nm) shine down 40min obtains the substrate that the surface has functionalization OTS-SAMs film in UV-light after 120 ℃ of dry 5min remove organism with the OTS-SAMs film.
Step 3: the deposition of film: the surface has facing down and be suspended in the precursor liquid surface of functionalization OTS-SAMs film of substrate of the OTS-SAMs film of functionalization, and functionalization OTS-SAMs film is contacted with precursor liquid, prepares noncrystalline membrane at 80 ℃ of deposition 20h.
Step 4: the crystallization of film: the noncrystalline membrane of preparation is put into retort furnace after drying at room temperature, obtain the ZnO film of the patterning of crystallization in 300 ℃ of insulation annealing 120min.
The ZnO film of the patterning that embodiment 3 is obtained carries out the metallography microscope test and XRD tests, and Fig. 3 is the metallurgical microscopic of the ZnO film of the patterning that obtains of the embodiment of the invention 3; The XRD figure spectrum of the ZnO film of the patterning that the curve among Fig. 4 (a) obtains for embodiments of the invention 3, the ZnO film of embodiment 3 preparations is the ZnO film of (002) and (101) crystal face preferential growth as can be seen from Figure 4.
Embodiment 4
A kind of liquid phase self-assembling technique prepares the method for the ZnO film of patterning, may further comprise the steps:
Step 1: the configuration of precursor liquid: with the Zn (NO of 0.0025mol
3)
26H
2The NH of O and 0.011mol
4F is dissolved in the 50ml distilled water, is made into Zn (NO
3)
26H
2O concentration is 0.05mol/L, NH
4F concentration is the mixed solution of 0.22mol/L, is the HNO of 4mol/L with concentration
3Solution and concentration are that the pH value of the NaOH solution adjusting mixed solution of 3mol/L is 5.5, mix liquid under the room temperature to fully clarification, get precursor liquid.
Step 2: the functionalization of substrate: substrate is placed respectively deionized water, acetone, dehydrated alcohol supersound washing 10min.Behind irradiation 20min under the UV-light, be to soak 30min in 1% the OTS-toluene solution to prepare the OTS-SAMs film in volumetric concentration, (λ=184.9nm) shine down 40min obtains the glass substrate that the surface has functionalization OTS-SAMs film in UV-light after 120 ℃ of dry 5min remove organism with the OTS-SAMs film.
Step 3: the deposition of film: the surface has facing down and be suspended in the precursor liquid surface of functionalization OTS-SAMs film of substrate of the OTS-SAMs film of functionalization, and functionalization OTS-SAMs film is contacted with precursor liquid, prepares noncrystalline membrane at 70 ℃ of deposition 20h.
Step 4: the crystallization of film: the noncrystalline membrane of preparation is put into retort furnace after drying at room temperature, obtain the ZnO film of the patterning of crystallization in 300 ℃ of insulation annealing 120min.
Embodiment 5
A kind of liquid phase self-assembling technique prepares the method for the ZnO film of patterning, may further comprise the steps:
Step 1: the configuration of precursor liquid: with the Zn (NO of 0.0025mol
3)
26H
2The NH of O and 0.014mol
4F is dissolved in the 50ml distilled water, is made into Zn (NO
3)
26H
2O concentration is 0.05mol/L, NH
4F concentration is the mixed solution of 0.28mol/L, is the HNO of 4mol/L with concentration
3Solution and concentration are that the pH value of the NaOH solution adjusting mixed solution of 3mol/L is 5.5, mix liquid under the room temperature to fully clarification, get precursor liquid.
Step 2: the functionalization of substrate: substrate is placed respectively deionized water, acetone, dehydrated alcohol supersound washing 10min.Behind irradiation 20min under the UV-light, be to soak 30min in 1% the OTS-toluene solution to prepare the OTS-SAMs film in volumetric concentration, (λ=184.9nm) shine down 40min obtains the substrate that the surface has functionalization OTS-SAMs film in UV-light after 120 ℃ of dry 5min remove organism with the OTS-SAMs film.
Step 3: the deposition of film: the surface has facing down and be suspended in the precursor liquid surface of functionalization OTS-SAMs film of substrate of the OTS-SAMs film of functionalization, and functionalization OTS-SAMs film is contacted with precursor liquid, prepares noncrystalline membrane at 75 ℃ of deposition 20h.
Step 4: the crystallization of film: the noncrystalline membrane of preparation is put into retort furnace after drying at room temperature, obtain the ZnO film of the patterning of crystallization in 300 ℃ of insulation annealing 120min.
Embodiment 6
A kind of liquid phase self-assembling technique prepares the method for the ZnO film of patterning, may further comprise the steps:
Step 1: the configuration of precursor liquid: with the Zn (NO of 0.0025mol
3)
26H
2The NH of O and 0.0125mol
4F is dissolved in the 50ml distilled water, is made into Zn (NO
3)
26H
2O concentration is 0.05mol/L, NH
4F concentration is the mixed solution of 0.25mol/L, is the HNO of 4mol/L with concentration
3Solution and concentration are that the pH value of the NaOH solution adjusting mixed solution of 3mol/L is 5.5, mix liquid under the room temperature to fully clarification, get precursor liquid.
Step 2: the functionalization of substrate: substrate is placed respectively deionized water, acetone, dehydrated alcohol supersound washing 10min.Behind irradiation 20min under the UV-light, be to soak 30min in 1% the OTS-toluene solution to prepare the OTS-SAMs film in volumetric concentration, the OTS-SAMs film is removed organism in 120 ℃ of dry 5min.Then with the OTS-SAMs film under the covering of photomask, UV-light (the lower irradiation of λ=184.9nm) 40min so that the OTS-SAMs film is subjected to the zone of UV-irradiation because the formation of silanol, matrix surface is good wetting ability; And be not the alkyl zone by the zone of UV-irradiation, matrix surface presents original hydrophobicity, obtains the substrate that the surface has functionalization OTS-SAMs film.
Step 3: the deposition of film: the surface has facing down and be suspended in the precursor liquid surface of functionalization OTS-SAMs film of substrate of the OTS-SAMs film of functionalization, and functionalization OTS-SAMs film is contacted with precursor liquid, prepares noncrystalline membrane at 70 ℃ of deposition 20h.
Step 4: the crystallization of film: the noncrystalline membrane of preparation is put into retort furnace after drying at room temperature, obtain the ZnO film of the patterning of crystallization in 300 ℃ of insulation annealing 120min.
The ZnO film of the patterning that embodiment 6 is obtained carries out the metallography microscope test, and Fig. 6 is the metallurgical microscopic of the ZnO film of the patterning that obtains of the embodiment of the invention 6.
Embodiment 7
A kind of liquid phase self-assembling technique prepares the method for the ZnO film of patterning, may further comprise the steps:
Step 1: the configuration of precursor liquid, with the Zn (NO of 0.0025mol
3)
26H
2The NH of O and 0.0125mol
4F is dissolved in the 50ml distilled water, is made into Zn (NO
3)
26H
2O concentration is 0.05mol/L, NH
4F concentration is the mixed solution of 0.25mol/L, is the HNO of 4mol/L with concentration
3Solution and concentration are that the pH value of the NaOH solution adjusting mixed solution of 3mol/L is 5.5, mix liquid under the room temperature to fully clarification, get precursor liquid.
Step 2: the functionalization of substrate: substrate is placed respectively deionized water, acetone, dehydrated alcohol supersound washing 10min.Behind irradiation 20min under the UV-light, be to soak 30min in 1% the OTS-toluene solution to prepare the OTS-SAMs film in volumetric concentration, the OTS-SAMs film is removed organism in 120 ℃ of dry 5min.Then with the OTS-SAMs film under the covering of photomask, UV-light (the lower irradiation of λ=184.9nm) 40min so that the OTS-SAMs film is subjected to the zone of UV-irradiation because the formation of silanol, matrix surface is good wetting ability; And be not the alkyl zone by the zone of UV-irradiation, matrix surface presents original hydrophobicity.Obtain the substrate that the surface has functionalization OTS-SAMs film.
Step 3: the deposition of film: the surface has facing down and be suspended in the precursor liquid surface of functionalization OTS-SAMs film of substrate of the OTS-SAMs film of functionalization, and functionalization OTS-SAMs film is contacted with precursor liquid, prepares noncrystalline membrane at 80 ℃ of deposition 20h.
Step 4: the crystallization of film: prepared noncrystalline membrane is put into retort furnace after drying at room temperature, obtain the ZnO film of the patterning of crystallization in 300 ℃ of insulation annealing 120min.
The ZnO film of the patterning that embodiment 7 is obtained carries out the metallography microscope test, and Fig. 7 is the metallurgical microscopic of the ZnO film of the patterning that obtains of the embodiment of the invention 7.
Embodiment 8
A kind of liquid phase self-assembling technique prepares the method for the ZnO film of patterning, may further comprise the steps:
Step 1: the configuration of precursor liquid: with the Zn (NO of 0.0025mol
3)
26H
2The NH of O and 0.01mol
4F is dissolved in the 50ml distilled water, is made into Zn (NO
3)
26H
2O concentration is 0.05mol/L, NH
4F concentration is the mixed solution of 0.2mol/L, is the HNO of 4mol/L with concentration
3Solution and concentration are that the pH value of the NaOH solution adjusting mixed solution of 3mol/L is 5.5, mix liquid under the room temperature to fully clarification, get precursor liquid.
Step 2: the functionalization of substrate: substrate is placed respectively deionized water, acetone, dehydrated alcohol supersound washing 10min.Behind irradiation 20min under the UV-light, be to soak 30min in 1% the OTS-toluene solution to prepare the OTS-SAMs film in volumetric concentration, the OTS-SAMs film is removed organism in 120 ℃ of dry 5min.Then with the OTS-SAMs film under the covering of photomask, UV-light (the lower irradiation of λ=184.9nm) 40min so that the OTS-SAMs film is subjected to the zone of UV-irradiation because the formation of silanol, matrix surface is good wetting ability; And be not the alkyl zone by the zone of UV-irradiation, matrix surface presents original hydrophobicity.Obtain the substrate that the surface has functionalization OTS-SAMs film.
Step 3: the deposition of film: the surface has facing down and be suspended in the precursor liquid surface of functionalization OTS-SAMs film of substrate of the OTS-SAMs film of functionalization, and functionalization OTS-SAMs film is contacted with precursor liquid, prepares noncrystalline membrane at 75 ℃ of deposition 20h.
Step 4: the crystallization of film: the noncrystalline membrane of preparation is put into retort furnace after drying at room temperature, obtain the ZnO film of the patterning of crystallization in 300 ℃ of insulation annealing 120min.
Embodiment 9
A kind of liquid phase self-assembling technique prepares the method for the ZnO film of patterning, may further comprise the steps:
Step 1: the configuration of precursor liquid, with the Zn (NO of 0.0025mol
3)
26H
2The NH of O and 0.015mol
4F is dissolved in the 50ml distilled water, is made into Zn (NO
3)
26H
2O concentration is 0.05mol/L, NH
4F concentration is the mixed solution of 0.3mol/L, is the HNO of 4mol/L with concentration
3Solution and concentration are that the pH value of the NaOH solution adjusting mixed solution of 3mol/L is 5.5, mix liquid under the room temperature to fully clarification, get precursor liquid.
Step 2: the functionalization of substrate: substrate is placed respectively deionized water, acetone, dehydrated alcohol supersound washing 10min.Behind irradiation 20min under the UV-light, be to soak 30min in 1% the OTS-toluene solution to prepare the OTS-SAMs film in volumetric concentration, the OTS-SAMs film is removed organism in 120 ℃ of dry 5min.Then with the OTS-SAMs film under the covering of photomask, UV-light (the lower irradiation of λ=184.9nm) 40min so that the OTS-SAMs film is subjected to the zone of UV-irradiation because the formation of silanol, matrix surface is good wetting ability; And be not the alkyl zone by the zone of UV-irradiation, matrix surface presents original hydrophobicity.Obtain the substrate that the surface has functionalization OTS-SAMs film.
Step 3: the deposition of film: the surface has facing down and be suspended in the precursor liquid surface of functionalization OTS-SAMs film of substrate of the OTS-SAMs film of functionalization, and functionalization OTS-SAMs film is contacted with precursor liquid, prepares noncrystalline membrane at 80 ℃ of deposition 20h.
Step 4: the crystallization of film: prepared noncrystalline membrane is put into retort furnace after drying at room temperature, obtain the ZnO film of the patterning of crystallization in 300 ℃ of insulation annealing 120min.
The above only is one embodiment of the present invention, it or not whole or unique embodiment, the conversion of any equivalence that those of ordinary skills take technical solution of the present invention by reading specification sheets of the present invention is claim of the present invention and contains.
Claims (9)
1. a liquid phase self-assembling technique prepares the method for the ZnO film of patterning, it is characterized in that, may further comprise the steps:
Step 1: the configuration of precursor liquid: with Zn (NO
3)
26H
2O and NH
4F is dissolved in the distilled water, is made into Zn (NO
3)
26H
2O concentration is 0.05mol/L, NH
4F concentration is the mixed solution of 0.2 ~ 0.3mol/L, and the pH value of regulating mixed solution is 5.5, mixes liquid under the room temperature to fully clarification, obtains precursor liquid;
Step 2: the functionalization of substrate: with the substrate washes clean, be to soak preparation OTS-SAMs film in 1% the OTS-toluene solution in volumetric concentration, with under UV-light, shining behind the dry removal of the OTS-SAMs film organism, obtain the substrate that the surface has the OTS-SAMs film of functionalization;
Step 3: the deposition of film: facing down and be suspended in the precursor liquid surface of functionalization OTS-SAMs film of substrate that the surface is had the OTS-SAMs film of functionalization, functionalization OTS-SAMs film is contacted with precursor liquid, prepare noncrystalline membrane 70 ℃～80 ℃ depositions;
Step 4: the crystallization of film: put into retort furnace after the noncrystalline membrane drying with preparation, obtain the ZnO film of the patterning of crystallization in 300 ℃ of insulation annealing 120min.
2. liquid phase self-assembling technique according to claim 1 prepares the method for the ZnO film of patterning, it is characterized in that: adopting concentration in the step 1 is the HNO of 4mol/L
3Solution and concentration are that the NaOH solution of 3mol/L is regulated the pH of mixed value.
3. liquid phase self-assembling technique according to claim 1 prepares the method for the ZnO film of patterning, it is characterized in that: the concrete operations of substrate washing are in the step 2: substrate is placed respectively deionized water, acetone, dehydrated alcohol supersound washing 10min.
4. liquid phase self-assembling technique according to claim 1 prepares the method for the ZnO film of patterning, it is characterized in that: the time that substrate soaks in volumetric concentration is 1% OTS-toluene solution in the step 2 is 30min, shines 20min through under the UV-light first before the immersion.
5. liquid phase self-assembling technique according to claim 1 prepares the method for the ZnO film of patterning, it is characterized in that: the OTS-SAMs film is to shine 40min under the UV-light of 184.9nm at wavelength in the step 2.
6. liquid phase self-assembling technique according to claim 1 prepares the method for the ZnO film of patterning, it is characterized in that: dry actual conditions is at 120 ℃ of dry 5min in the step 2.
7. liquid phase self-assembling technique according to claim 1 prepares the method for the ZnO film of patterning, it is characterized in that: depositing time is 20h in the step 3.
8. liquid phase self-assembling technique according to claim 1 prepares the method for the ZnO film of patterning, it is characterized in that: the drying in the step 4 is at room temperature carried out.
9. the liquid phase self-assembling technique according to claim 1-8 described in any one prepares the method for the ZnO film of patterning, it is characterized in that: cover photomask at the OTS-SAMs film when OTS-SAMs film shines under UV-light in the step 2.
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| CN106925256A (en) * | 2017-03-30 | 2017-07-07 | 陕西科技大学 | A kind of visible light-responded characteristic titanium oxide/pucherite hetero-junction thin-film and its preparation method and application |
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| CN106925256B (en) * | 2017-03-30 | 2019-05-10 | 陕西科技大学 | A kind of visible light-responded characteristic titanium oxide/pucherite hetero-junction thin-film and its preparation method and application |
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| CN106944037B (en) * | 2017-03-30 | 2019-10-29 | 陕西科技大学 | A kind of visible light-responded characteristic zinc oxide/pucherite hetero-junction thin-film and its preparation method and application |
| US10787366B2 (en) * | 2018-07-31 | 2020-09-29 | National Sun Yat-Sen University | Method for manufacturing graphitic sheet |
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