CN106435533A - Method for preparing high-performance AZO transparent conductive thin film - Google Patents
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/1208—Oxides, e.g. ceramics
- C23C18/1216—Metal oxides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1254—Sol or sol-gel processing
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1295—Process of deposition of the inorganic material with after-treatment of the deposited inorganic material
Abstract
The invention discloses a method for preparing a high-performance AZO transparent conductive thin film. The method comprises three main steps which are respectively a precursor sol preparation step, a thin film preparation step adopting a spin-coating method, and a vacuum annealing and anti-sputtering washing step. The method specifically comprises the following steps: step (1) dissolving a certain amount of octan zinecnaty in an ethylene glycol monomethyl ether solvent or a glycol ether solvent, subsequently adding a stabilizing agent monoethanolamine and doping ions aluminum nitrate nonahydrate into the solution, performing water-bath stirring, and ageing at room temperature to obtain uniform and stable precursor sol; step (2) spin-coating and depositing the precursor wet soil on substrates such as a glass substrate, a quartz substrate and a silicon substrate by adopting a sol-gel spin-coating method, drying and performing low-temperature thermal treatment to obtain an AZO thin film with certain thickness; step (3) firstly annealing the AZO thin film under a medium-vacuum-degree condition and subsequently performing anti-sputtering washing on the surface of the thin film by using Ar<+>. By the three steps, the method disclosed by the invention is capable of obtaining an AZO transparent conductive thin film which is extremely low in resistance rate and quite high in visual light and ultraviolet light penetration rate.
Description
Technical field
The present invention relates to membrane material preparing technical field, particularly relate to one and conduct electricity very well, pass through in visible-range
The high transparent conductive oxide film of rate (TCO), specifically, is that a kind of employing sol-gal process (Sol-Gel method) spin coating becomes
Film, and through vacuum annealing and Ar+Backwash cleans the method preparing high performance AZO film.
Background technology
Transparent conductive oxide (TCO) film because of its in visible-range high permeability, there is high reflection to infrared light
Rate and relatively low resistivity, at field of photoelectric devices such as solar cell, plate of flat liquid crystal display, light emitting diodes (LED)
Show its wide application prospect.At present commercial TCO thin film, using most is tin-doped indium oxide film (ITO), but
It is that the phosphide element in ito thin film is expensive and poisonous.Meanwhile, to have raw material wide for Al-Doped ZnO film (AZO)
The advantages such as general, low price, asepsis environment-protecting, become the splendid replacer of ito thin film.The method preparing AZO film mainly has：Electricity
Son bundle vacuum evaporation, magnetron sputtering, chemical meteorology deposition, pulsed laser deposition, molecular beam epitaxy, spray pyrolysis, atomic layer deposition
Amass and collosol and gel spin-coating method.In these methods, sol-gal process prepares AZO film not only simply but also inexpensively, has technique
Process is simple, be not required to the equipment of complex and expensive, become that film uniformity is good, crystallization temperature is low and be easy to carry out accurate doping etc. numerous
Advantage.
Compared with other preparation methods, AZO film prepared by sol-gal process needs subsequent treatment process to reduce sample
Resistivity could meet the requirement of actual application.For using sol-gal process to prepare AZO film, subsequent treatment is to obtain height
The critical process of performance transparency conductive film.Currently, various subsequent treatment process are to the improvement of AZO film performance disunity,
Not possessing the condition being widely popularized, for example with concentration relatively low strong acid, film being carried out surface suede, this type of technology is thin to AZO
It though the electrical and optical performance of film has clear improvement, but is also difficult to meet the requirement of reality application.
Content of the invention
It is an object of the invention to provide in one and anneal and with Ar under vacuum+It is transparent that backwash cleans preparation high-performance AZO
The method of conductive film, uses collosol and gel spin-coating method to pass through at the deposition on substrate AZO films such as sheet glass, quartz, silicon, film
Annealing and Ar under follow-up middle vacuum degree condition+Backwash cleans, it is thus achieved that resistivity is extremely low, visible ray and black light pass through
The very high AZO transparent conductive film of rate.
The method that the present invention provides, is divided into the preparation of precursor sol, and it is clear that spin-coating method prepares film, Thin-film anneal and backwash
Wash three big steps.
The technical solution used in the present invention is：A kind of method preparing high-performance AZO transparent conductive film, including following step
Suddenly：
1) preparation of precursor sol：
Dissolving in a solvent two acetate hydrate zinc, the molar concentration making zinc ion is 0.2-1mol/L, at 25-40 DEG C of bar
It after stirring is extremely dissolved under part, in solution, is sequentially added into stabilizer and nine water aluminum nitrates, in molar ratio, Al3+:Zn2+=0.01-
0.05:1, mixed solution constant temperature stirring 3-4h in the water-bath of 70-80 DEG C, gained mixed solution is at room temperature aged 20-24h,
Obtain precursor sol；
2) preparation of AZO film：
By step 1) precursor sol that obtains, use spin-coating method to prepare AZO gel film on substrate, by obtain
AZO gel film in atmosphere, is dried 5-15 minute under the conditions of 90-110 DEG C；Then in atmosphere, heat under the conditions of 400-450 DEG C
Process 10-20 minute, obtain AZO film；
3) annealing of AZO film and Ar+Backwash cleans：
By step 2) the AZO film that obtains, put in the Sample Room of magnetic control sputtering system, be 1-300Pa in vacuum,
Make annealing treatment 2-3h under the conditions of 400-600 DEG C, after Sample Room naturally cools to room temperature, in Sample Room, be passed through backwash purgative gas
Body, under 1Pa, backwash cleans.
Above-mentioned method, step 1) in, described solvent is EGME or ethylene glycol ethyl ether.
Above-mentioned method, step 1) in, described stabilizer is MEA.
Above-mentioned method, step 1) in, in molar ratio, MEA：Zn2+=1:1.
Above-mentioned method, step 2) in, described substrate is glass, quartz or silicon chip.
Above-mentioned method, step 2) in, described spin-coating method technological parameter is：Rotating speed 3000rpm, spin-coating time 30s.
Above-mentioned method, step 2) repeat 7-10 time, obtain certain thickness AZO film.
Above-mentioned method, step 3) in, vacuum is 1-100Pa, and annealing temperature is 400-600 DEG C.
Above-mentioned method, step 3) in, described backwash purge gas is Ar gas or N2Gas.
Above-mentioned method, step 3) in, backwash scavenging period is 2-20min.
The invention has the beneficial effects as follows：
1) present invention uses two cheap acetate hydrate zinc, and nine water aluminum nitrates are as raw material, with EGME
Or the organic solution such as ethylene glycol ethyl ether is solvent, the cost of preparing transparent conductive film greatly reduces.
2) present invention uses collosol and gel spin-coating method film forming, is not required to the equipment of complexity, and technique is simple, can realize extensive work
Industry metaplasia is produced, additionally, sol-gal process can realize accurately adulterating, becomes film uniformity good.
3) annealing to AZO film for the present invention is carried out in the middle vacuum of 1-300Pa, and this vacuum only needs to use
Simple mechanical pump can realize, it is not necessary to the expensive diffusion pump even vacuum acquirement devices such as molecular pump.Only need simple
Post processing AZO film can be made to obtain splendid electric conductivity.
4) present invention uses nitrogen or Ar+Backwash cleaning treatment is carried out to AZO film surface, film can be reduced further
Resistivity, simultaneously can also carry out suede modification to film surface, this suede structure can promote incident sunshine reflection,
Incidence sunshine thus is distributed to all angles by refraction and scattering, effectively in enhancing solar cell light absorbing material to entering
Penetrating the capture of sunshine, the increase that light absorbs can increase the short circuit current of solar cell, finally realizes solar cell photoelectric
The raising of conversion efficiency.AZO film can be made as a kind of splendid electrode of solar battery.
Brief description
Fig. 1 is embodiment the 1st, embodiment the 2nd, embodiment the 3rd, comparative example 1 and the resistivity of AZO film of comparative example 2 preparation.
Fig. 2 a is the Optical transmission spectrum of the AZO film of annealing under different vacuum.
Fig. 2 b is the Optical transmission spectrum of the AZO film after different time backwash cleans.
Fig. 3 is the surface topography SEM figure of the AZO film that non-backwash cleans after cleaning 10 minutes with backwash,
Wherein, the non-backwash of (a) comparative example 1 cleans；B () embodiment 5 backwash cleans 10 minutes.
Detailed description of the invention
The present invention is described in detail with detailed description of the invention below in conjunction with the accompanying drawings.
Embodiment 1
(1) anneal and with Ar under vacuum in+Backwash cleans preparation AZO transparent conductive film
1) it is equipped with the two acetate hydrate zinc particles of 0.06mol in the beaker of 100ml EGME solvent, room temperature
Lower stirring is to being completely dissolved.Add and Zn with in backward solution2+Equimolar than MEA as stabilizer, after stirring
Add a certain amount of nine water aluminum nitrate particles in solution so that Al3+:Zn2+=0.02:1 (mol ratio).Then beaker is put
In the water-bath of 75 DEG C, constant temperature stirring 3h, obtains precursor liquid light yellow, transparent and homogeneous.
2) uncovered for precursor liquid placement is aged 24h in atmosphere, obtain having certain viscosity, stable homogeneous presoma molten
Glue.
3) glass substrate (also can be quartz or silicon chip) with deionized water ultrasonic cleaning several times, then surpass with absolute ethyl alcohol
Sound cleans 2 times, and the glass substrate high pure nitrogen after cleaning dries up, and is placed in constant temperature and humidity storage bin standby.
4) arranging drying baker temperature is 100 DEG C, and wide-mouth muffle furnace is 420 DEG C.
5) take standby glass substrate to be placed on the vacuum suction pallet of sol evenning machine, sol evenning machine rotating speed is set and the time is：
Low speed 500rpm, time 5s；High speed 3000rpm, time 30s.Start sol evenning machine, the glass substrate surface of low speed rotation drips
Precursor sol after upper ageing.After High Rotation Speed terminates, take off the substrate scribbling precursor sol, put into the baking of 100 DEG C
It in case, under air atmosphere, is dried 10 minutes, be coated with subsequently in the Muffle furnace that the substrate of precursor colloids film puts into 420 DEG C,
It under air atmosphere, is heat-treated 15 minutes.For increase film thickness and raising film electric conductivity, will heat treatment after thin
Spin coating, drying, heat treatment 7 times are repeated in film surface, obtain AZO film.
6) the AZO film preparing spin coating is put in the Sample Room of magnetic control sputtering system, will enter with standard machinery pump
Specimen chamber is evacuated to 10Pa and keeps.It is brought rapidly up to 530 DEG C with the speed of 15 DEG C/min, insulation annealing 2h, with stove cooling.
7) recover, after room temperature, in Sample Room, to be passed through high-purity argon gas (also can be nitrogen), in 2-5Pa vacuum until Sample Room
Degree lower ionization starter, adjustment vacuum is to 1Pa subsequently, keeps AZO film at Ar+Film surface is cleaned 3 minutes under reverse sputtering.
(2) comparative example 1：Annealing preparation AZO film in air：
1)-5) step is with (one), and collosol and gel spin-coating method prepares AZO film on substrate.
6) the AZO film preparing spin coating is put in wide-mouth Muffle furnace, with the speed of 15 DEG C/min be brought rapidly up to
530 DEG C, insulation annealing 2h, with stove cooling.Obtain air makes annealing treatment the AZO transparent conductive film of preparation.
(3) comparative example 2：Protective atmosphere (N2Gas) under annealing preparation AZO film：
1)-5) step is with (one), and collosol and gel spin-coating method prepares AZO film on substrate.
6) the AZO film preparing spin coating is put in atmosphere furnace, is passed through N in atmosphere furnace2Gas, gas flow rate is
20sccm.It is brought rapidly up to 530 DEG C with the speed of 15 DEG C/min, insulation annealing 2h, with stove cooling.Obtain protective atmosphere (N2Gas)
The AZO transparent conductive film of lower annealing preparation.
Embodiment 2
1)-5) step prepares AZO film with (one) in embodiment 1, collosol and gel spin-coating method on substrate.
6) the AZO film preparing spin coating is put in the Sample Room of magnetic control sputtering system, will enter with standard machinery pump
Specimen chamber is evacuated to 1Pa and keeps.It is brought rapidly up to 530 DEG C with the speed of 15 DEG C/min, insulation annealing 2h, with stove cooling.
7) recover, after room temperature, in Sample Room, to be passed through high-purity argon gas until Sample Room, under 2-5Pa vacuum, ionize starter,
Adjustment vacuum is to 1Pa subsequently, keeps AZO film at Ar+Film surface is cleaned 3 minutes under reverse sputtering.
Embodiment 3
1)-5) step prepares AZO film with (one) in embodiment 1, collosol and gel spin-coating method on substrate.
6) the AZO film preparing spin coating is put in the Sample Room of magnetic control sputtering system, will enter with standard machinery pump
Specimen chamber is evacuated to 100Pa and keeps.It is brought rapidly up to 530 DEG C with the speed of 15 DEG C/min, insulation annealing 2h, with stove cooling.
7) recover, after room temperature, in Sample Room, to be passed through high-purity argon gas until Sample Room, under 2-5Pa vacuum, ionize starter,
Adjustment vacuum is to 1Pa subsequently, keeps AZO film at Ar+Film surface is cleaned 3 minutes under reverse sputtering.
Embodiment 4
1)-5) step prepares AZO film with (one) in embodiment 1, collosol and gel spin-coating method on substrate.
6) the AZO film preparing spin coating is put in the Sample Room of magnetic control sputtering system, will enter with standard machinery pump
Specimen chamber is evacuated to 10Pa and keeps.It is brought rapidly up to 530 DEG C with the speed of 15 DEG C/min, insulation annealing 2h, with stove cooling.
7) recover, after room temperature, in Sample Room, to be passed through high-purity argon gas until Sample Room, under 2-5Pa vacuum, ionize starter,
Adjustment vacuum is to 1Pa subsequently, keeps AZO film at Ar+Film surface is cleaned 15 minutes under reverse sputtering.
Embodiment 5
1)-5) step prepares AZO film with (one) in embodiment 1, collosol and gel spin-coating method on substrate.
6) the AZO film preparing spin coating is put in the Sample Room of magnetic control sputtering system, will enter with standard machinery pump
Specimen chamber is evacuated to 10Pa and keeps.It is brought rapidly up to 530 DEG C with the speed of 15 DEG C/min, insulation annealing 2h, with stove cooling.
7) recover, after room temperature, in Sample Room, to be passed through high-purity argon gas until Sample Room, under 2-5Pa vacuum, ionize starter,
Adjustment vacuum is to 1Pa subsequently, keeps AZO film at Ar+Film surface is cleaned 10 minutes under reverse sputtering.
Embodiment 6 sample detection
1st, resistivity measurement
AZO film is as a kind of transparent conductive film material, and its most important performance is the size of resistivity.Use Hall
Effect instrument testing example the 1st, embodiment the 2nd, embodiment the 3rd, comparative example 1 and the AZO film of comparative example 2 preparation, each embodiment and right
The resistivity value of ratio such as accompanying drawing 1.In air, AZO film (comparative example 1) resistivity of annealing is about 10 Ω cm.Nitrogen
The AZO film (comparative example 2) of the lower annealing preparation of protection, its resistivity is about 0.2 Ω cm, thin compared with the AZO of annealing in air
Film resistance rate is much lower, the AZO film (embodiment 3) of annealing under even below 100Pa vacuum.The AZO of embodiment 1 preparation
Film (annealing vacuum is 10Pa), its resistivity is about (0.0025) Ω cm；(annealing is true for the AZO film of embodiment 2 preparation
Reciprocal of duty cycle is 1Pa), its resistivity is about (0.00411) Ω cm, true in showing well below the AZO film of annealing in air
Under reciprocal of duty cycle, annealing can obtain the fabulous AZO transparent conductive film of electric conductivity.
2nd, transmissivity
As a kind of transparent conductive film material, another important indicator of AZO film is the transmissivity to visible ray.Figure
2a and Fig. 2 b is embodiment the 1st, embodiment the 3rd, embodiment 4 and the transmissivity of AZO film of comparative example 1 preparation.From Fig. 2 a, real
Executing example the 1st, embodiment 3 and the AZO film of comparative example 1 preparation being very high to the transmissivity of visible ray, its average transmittance is more than 90%.
Additionally, under 10Pa vacuum the AZO film (embodiment 1) of preparation, it is to the cut-off transmission peak wavelength ratio of visible ray in air
The AZO film (comparative example 1) of annealing preparation is short, shows that the annealing of middle vacuum is reducing AZO film resiativity, can also improve simultaneously
Its to visible ray pass through ability.Equally, Fig. 2 b displays that the surface backwash through certain time for the AZO film cleans, and it is to can
See that the cut-off transmission peak wavelength of light is shorter than the AZO film (comparative example 1) of preparation of annealing in air, it is seen that backwash is clear through surface
Washing, the ability that passes through to visible ray for the film obtains lifting again.
3rd, surface topography
When transparent conductive film is used as the electrode of solar cell, it is desirable to transparent conductive film (TCO) surface has one
Fixed ups and downs suede structure, this surface texture can promote reflection, refraction and the scattering of incident sunshine, thus will
Incident sunshine is distributed to all angles, effectively strengthens the capture to incident sunshine for the light absorbing material in solar cell, light
The increase absorbing can increase the short circuit current of solar cell, finally realizes the raising of solar cell photoelectric conversion efficiency.Fig. 3
Surface topography SEM figure for comparative example 1 and the AZO film of embodiment 5 preparation.AZO film can be clearly seen from Fig. 3
Surface backwash through 10min cleans, and a large amount of ups and downs suede structure occurs in film surface, it is contemplated that the present invention can be very big
The resistivity of reduction AZO film, promote film simultaneously and ability passed through to visible ray, this makes AZO film at photoelectric device
The application in field has possessed splendid competitiveness.
Claims (10)
1. the method preparing high-performance AZO transparent conductive film, it is characterised in that comprise the following steps：
1) preparation of precursor sol：
Dissolving in a solvent two acetate hydrate zinc, the molar concentration making zinc ion is 0.2-1mol/L, under the conditions of 25-40 DEG C
It after stirring is extremely dissolved, in solution, is sequentially added into stabilizer and nine water aluminum nitrates, in molar ratio, Al3+:Zn2+=0.01-0.05:
1, by mixed solution, in the water-bath of 70-80 DEG C, constant temperature stirs 3-4h, and gained mixed solution is at room temperature aged 20-24h, obtains
Precursor sol；
2) preparation of AZO film：
By step 1) precursor sol that obtains, use spin-coating method to prepare AZO gel film on substrate, the AZO obtaining is coagulated
Glue film in atmosphere, is dried 5-15 minute under the conditions of 90-110 DEG C；Then in atmosphere, heat treatment under the conditions of 400-450 DEG C
10-20 minute, obtains AZO film；
3) annealing of AZO film and Ar+Backwash cleans：
By step 2) the AZO film that obtains, put in the Sample Room of magnetic control sputtering system, be 1-300Pa in vacuum, 400-
Make annealing treatment 2-3h under the conditions of 600 DEG C, after Sample Room naturally cools to room temperature, in Sample Room, be passed through backwash purge gas, 1Pa
Lower backwash cleans.
2. in accordance with the method for claim 1, it is characterised in that：Step 1) in, described solvent is EGME or second
Glycol ether.
3. in accordance with the method for claim 1, it is characterised in that：Step 1) in, described stabilizer is MEA.
4. in accordance with the method for claim 3, it is characterised in that：Step 1) in, in molar ratio, MEA：Zn2+=1:1.
5. in accordance with the method for claim 1, it is characterised in that：Step 2) in, described substrate is glass, quartz or silicon
Piece.
6. in accordance with the method for claim 1, it is characterised in that：Step 2) in, described spin-coating method technological parameter is：Rotating speed
3000rpm, spin-coating time 30s.
7. in accordance with the method for claim 1, it is characterised in that：Step 2) repeat 7-10 time, obtain certain thickness AZO thin
Film.
8. in accordance with the method for claim 1, it is characterised in that：Step 3) in, vacuum is 1-100Pa, and annealing temperature is
400-600℃.
9. in accordance with the method for claim 1, it is characterised in that：Step 3) in, described backwash purge gas is Ar gas or N2
Gas.
10. in accordance with the method for claim 1, it is characterised in that：Step 3) in, backwash scavenging period is 2-20min.
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| CN107507660A (en) * | 2017-08-14 | 2017-12-22 | 高崇光 | A kind of method that short annealing prepares nesa coating |
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| CN107507660A (en) * | 2017-08-14 | 2017-12-22 | 高崇光 | A kind of method that short annealing prepares nesa coating |
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| CN107689272A (en) * | 2017-08-25 | 2018-02-13 | 南昌航空大学 | One species graphene carbonitride Modification on Al adulterates the preparation method of ZnO transparent conductive thin film |
| CN107689272B (en) * | 2017-08-25 | 2019-02-05 | 南昌航空大学 | The preparation method of one type graphene carbonitride Modification on Al doping ZnO transparent conductive thin film |
| CN107723688A (en) * | 2017-10-24 | 2018-02-23 | 河南理工大学 | It is prepared by one kind（002）The method of the AZO transparent conductive film of orientation |
| CN108165956A (en) * | 2017-12-29 | 2018-06-15 | 中建材蚌埠玻璃工业设计研究院有限公司 | A kind of preparation method for the AZO laminated films for adding graphene |
| CN115938647A (en) * | 2022-12-02 | 2023-04-07 | 宁波碳源新材料科技有限公司 | Silver nanowire/aluminum-doped zinc oxide composite flexible transparent conductive film with ultrahigh adhesion and preparation method thereof |
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