CN105349970B - A kind of electric thin preparation method of excellent performance - Google Patents
A kind of electric thin preparation method of excellent performance Download PDFInfo
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- CN105349970B CN105349970B CN201510892350.8A CN201510892350A CN105349970B CN 105349970 B CN105349970 B CN 105349970B CN 201510892350 A CN201510892350 A CN 201510892350A CN 105349970 B CN105349970 B CN 105349970B
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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
-
- 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
- C23C18/1258—Spray pyrolysis
Abstract
The invention provides a kind of method of low temperature preparation zinc oxide electronic film, using spray heating decomposition, including prepares precursor liquid, thin film deposition steps, the precursor liquid is zinc ammonium [(Zn (NH3)4](OH)2Solution.The present invention, using spray pyrolysis, using removable heating platform as heating source, can prepare the excellent ZnO film of crystallographic property using the zinc ammonium salt solution of alkalescence as precursor liquid at 130 DEG C or so, with substrate is not hindered, low cost is pollution-free, the advantages that nontoxic, technique is simple, and energy large area is film-made.
Description
The application be for Application No. 201410034109.7, the applying date be on 01 24th, 2014, it is entitled
The divisional application of " a kind of method of low temperature preparation zinc oxide electronic film ".
Technical field
The present invention relates to the preparation method of the preparation method of film, more particularly to zinc-oxide film.
Background technology
Zinc-oxide film is a kind of multifunction electronic film, can be prepared into electrically conducting transparent by mixing the elements such as B, Al, In, Ga
Sull (TCO), there is extensive answer touching display, solar cell window, Low emissivity (Low-E) glass etc.
With.In the recent period, it has been found that undoped with ZnO film there is very important use in the cathode buffer layer of organic solar batteries
On the way, its photoelectric transformation efficiency (PCE) and service life can be improved.
Preparing ZnO film using ultrasonic spray pyrolysis has relevant report, and generally existing shortcoming mainly has：(1) depositing temperature
Height, (2) can not realize large area film forming, and (3) cost of material is high, and (4) raw material does harm to people and environmental toxic.Example：Patent
CN1707752 A, using tube furnace as heating source, the ZnO film of small area can only be prepared；Film deposition temperature height (500~800
DEG C), resistant to elevated temperatures inorganic material can only be used as substrate., can be in 130 DEG C or so systems and raw material decomposes temperature of the present invention is low
Standby ZnO film；Removable heating platform is employed as heating source, it is possible to achieve it is thin to prepare large area ZnO on flexible substrates
Film, adapts to volume to volume technique and large-scale production requires.Example again：Yoshino Kenji. Low-Temperature Growth
of ZnO Films by Spray Pyrolysi:Japan, Japanese Journal of Applied Physics, 50
(4), report using diethyl zinc and raw material within (2011), although preparing ZnO film in lower temperature (100 DEG C), raw material
Diethyl zinc strong toxicity, easy Fire explosion are expensive；Preparation technology is closer to chemical vapor transportation (CVD) method, process
Control relative complex, oxygen and vapor are controlled strict, therefore need to carried out under an inert atmosphere；In addition with fixed warm table
As heating source, it is difficult to realize that large area is film-made.
The content of the invention
It is an object of the invention to provide a kind of low temperature, the antivacuum method for preparing large-area zinc oxide electric thin.
The purpose of the present invention is realized by following measures：
A kind of preparation method of zinc oxide electronic film, comprises the following steps：
(1) precursor liquid is prepared
5~20g soluble zinc salts are dissolved in deionized water, certain density unsaturated solution is configured to, is placed in beaker.
Under magnetic force or electric stirring effect, concentrated ammonia liquor is instilled, it is 7~8, Zn to control solution pH range2+Progressively it is converted into Zn (OH)2It is heavy
Form sediment；Vacuum filtration, precipitation is rinsed repeatedly with a large amount of deionized waters when filtering, removes acid ion (such as：CH3COO-、NO3 -、Cl-
Deng impurity), it is drying precipitated；Dried precipitation is weighed, deionized water is added and is disperseed with methyl alcohol mixed liquor, add ammoniacal liquor
Until precipitation dissolving, methanol volume：The volume sum of water and ammoniacal liquor is 1:2~5, it is 10~12 that pH, which is made, [(Zn (NH3)4]2+
Concentration is the transparent zinc ammonium salt solutions of 0.05~0.2mol/L as precursor liquid；
(2) thin film deposition
Substrate (slide, PET or PMMA) is placed in removable warm table, 130 DEG C~200 DEG C are heated to, in control panel
The walking manner of the upper removable warm table of setting；It is fixed by finer atomization nozzle (hereinafter referred to as nozzle), adjustment nozzle height away from
200~500mm of substrate；The control program of the removable heating platform of operation, removable heating platform press setting means automatically walk；
Access compressed air simultaneously opens nozzle；Take 30~100ml precursor liquid to be put into conical flask, peristaltic pump is accessed into nozzle, controlling stream
Measure as 0.5ml/min~5ml/min；By pressure control it is 1.5atm~5atm by pressure regulator valve, liquid is atomized through gas shock,
Film forming after substrate is sprayed on, deposition velocity is about 2nm/min~10nm/min；
(3) it is heat-treated
By the ZnO film of preparation and silicon to 200 DEG C~250 DEG C, 2h is incubated to improve its crystallinity；If as
TCO thin film use, by ZnO film and substrate as week reduction gas in tube-type atmosphere furnace, is passed through after, be evacuated to 10-3 Pa
~10-2Pa, 400 DEG C~800 DEG C are heated to, natural cooling after 2h are incubated, to improve electric conductivity.
The chemical reagent such as zinc acetate, zinc nitrate, zinc chloride used in the present invention are to analyze more than pure (AR).Institute of the present invention
Finer atomization nozzle material is stainless steel, and pin nozzle aperture footpath is 0.3mm~0.5mm.Warm table is may move used in the present invention to add
Hot device is cast aluminium heating plate, center and edge temperature difference ＜ ± 1 DEG C.
The present invention has the advantages that：
Organic solvent of the raw material of the present invention without organometallic complex and difficult volatilization, not only film deposition temperature is low,
And cost is low, preparation technology is simple, can be with large-scale promotion application.The present invention adopts using the zinc ammonium salt solution of alkalescence as precursor liquid
With spray pyrolysis, using removable heating platform as heating source, it is excellent crystallographic property can be prepared at 130 DEG C or so
The advantages that ZnO film, with substrate is not hindered, low cost, pollution-free, nontoxic, technique is simple, and energy large area is film-made.Technique
The range of choice of middle backing material is big, is restricted small, if using the organic film of flexibility as substrate, uses special transmission to fill
Put, it is possible to achieve volume to volume produces.
ZnO film main application prepared by the present invention be organic solar batteries cathode buffer layer, can improve it is organic too
Positive energy cell photoelectric conversion efficiency (PCE)；TCO thin film can also be also served as by doping.The obtained zinc-oxide film tool of the present invention
There is excellent performance, it is seen that mean transmissivity reaches more than 85%, surface roughness ＜ 10nm in optical range, and molten without remaining
Agent, impurity content is below 1%.ZnO film prepared by the present invention is the ZnO film of C axle preferrel orientations, and microscopic particles are averaged
Particle diameter about 10nm~20nm, uniformity are good.
Brief description of the drawings
The X-ray diffraction spectrum of ZnO film prepared by Fig. 1；
The Scanning Electron microphotograph of ZnO film prepared by Fig. 2.
Embodiment
The embodiment of the present invention is further described with reference to embodiment, therefore not limited the present invention
System is among described scope of embodiments.
Embodiment 1
A kind of method that cold nebulization thermal decomposition prepares ZnO electric thins, step are as follows：
(1) precursor liquid is prepared
11g zinc acetates are dissolved in deionized water, 1mol/L zinc acetate solution is configured to, is placed in beaker, in magnetic force or electricity
Under dynamic stirring action, concentrated ammonia liquor is instilled, it is 8, Zn to control solution PH2+Progressively it is converted into Zn (OH)2Precipitation, vacuum filtration, while taking out
Filter side is rinsed repeatedly with a large amount of deionized waters, removes unnecessary anion (CH3COO-、NO3 -、Cl-Deng impurity), dry, weigh 5g
Sediment, 30ml deionized waters and 10ml methanol are added, add 10ml ammoniacal liquor, precipitation dissolving, it is 11 to form pH, [(Zn (NH3)4
]2+Concentration is the transparent zinc ammonium salt solutions of 0.1mol/L as precursor liquid.
(2) thin film deposition
Glass fiber reinforcement PET (polyethylene terephthalate) substrate is placed in removable warm table, is heated to
130 DEG C, the motion mode of moveable platform is controlled, walking speed is 50mm/s, and the domain of walk is 200mm × 200mm.Adjustment spray
Mouth and substrate distance are 300mm, access compressed air and open nozzle, take 50ml precursor liquid to be put into conical flask, by peristaltic pump
Conical flask and nozzle are accessed, the control of forerunner's flow quantity is 1ml/min, by pressure control is 3atm by pressure regulator valve, liquid is through gas
Impact atomization is flowed, is sprayed on substrate, sedimentation time 100min.
(3) it is heat-treated
By the ZnO film of preparation and silicon to 200 DEG C, natural cooling after 2h is incubated.
The ZnO film for C axle preferrel orientations of preparation is can be seen that from the X-ray diffraction spectrum in Fig. 1, Fig. 2 is made
The SEM photograph of standby ZnO film, shows average grain diameter about 10nm~20nm of the ZnO film microscopic particles, and uniformity is good.
Embodiment 2
A kind of method that cold nebulization thermal decomposition prepares ZnO electric thins, with embodiment 1, wherein：
In (1) step, the raw material that precursor liquid is prepared uses zinc nitrate, and 25ml deionized waters and 15ml first are added in sediment
Alcohol.
In (2) step, substrate heating temperature is 150 DEG C.
In (3) step, the ZnO film and silicon of preparation are incubated natural cooling after 2h to 250 DEG C.
Obtained ZnO film：Mean transmissivity reaches more than 85%, surface roughness ＜ 10nm in visible-range, and not
Containing residual solvent, impurity content is below 1%, C axle preferrel orientations, average grain diameter about 10nm~20nm of microscopic particles, uniformity
It is good.
Embodiment 3
A kind of method that cold nebulization thermal decomposition prepares ZnO electric thins, with embodiment 1, wherein：
In (2) step, adjustment nozzle and substrate distance are 200mm, take 30ml precursor liquid to be put into conical flask, by peristaltic pump
Nozzle is accessed, the control of forerunner's flow quantity is 0.5ml/min, by pressure control is 2atm by pressure regulator valve, sedimentation time is
30min。
Obtained ZnO film：Mean transmissivity reaches more than 85%, surface roughness ＜ 10nm in visible-range, and not
Containing residual solvent, impurity content is below 1%, C axle preferrel orientations, average grain diameter about 10nm~20nm of microscopic particles, uniformity
It is good.
Embodiment 4
A kind of method that cold nebulization thermal decomposition prepares ZnO electric thins, with embodiment 1, wherein：
In (1) step, the raw material that precursor liquid is prepared uses zinc acetate solution, and it is 10 that pH, which is made, [(Zn (NH3)4]2+Concentration
It is zinc ammonium salt solution transparent 0.05mol/L as precursor liquid.
In (2) step, nozzle is 200mm with substrate distance, and the control of forerunner's flow quantity is 0.5ml/min,
After the completion of (3) step, sample is taken out after being incubated 2h.
Obtained ZnO film：Mean transmissivity reaches more than 85%, surface roughness ＜ 10nm in visible-range, and not
Containing residual solvent, impurity content is below 1%, C axle preferrel orientations, average grain diameter about 10nm~20nm of microscopic particles, uniformity
It is good.
Embodiment 5
A kind of method that cold nebulization thermal decomposition prepares ZnO electric thins, with embodiment 1, wherein：
In (1) step, the raw material that precursor liquid is prepared uses zinc chloride, is made into 0.5mol/L liquor zinci chloridi, and pH is made
For 12, [(Zn (NH3)4]2+Concentration is the transparent zinc ammonium salt solutions of 0.2mol/L as precursor liquid.
In (2) step, substrate heating temperature is 200 DEG C.
After the completion of (2) step, natural cooling after 2h is incubated.
Obtained ZnO film：Mean transmissivity reaches more than 85%, surface roughness ＜ 10nm in visible-range, and not
Containing residual solvent, impurity content is below 1%, C axle preferrel orientations, average grain diameter about 10nm~20nm of microscopic particles, uniformity
It is good.
Embodiment 6
A kind of method that cold nebulization thermal decomposition prepares ZnO electric thins, wherein：(1) step is the same as embodiment 1, (2) step
With (3) step with embodiment 4.
After (3) the end of the step, P3HT is sequentially depositing in sample coating one side by spraying process:PCBM、PEDOT:PSS and silver
Electrode, it is assembled into polymer thin-film solar cell (PSC).
Obtained ZnO film：Mean transmissivity reaches more than 85%, surface roughness ＜ 10nm in visible-range, and not
Containing residual solvent, impurity content is below 1%, C axle preferrel orientations, average grain diameter about 10nm~20nm of microscopic particles, uniformity
It is good.
The polymer thin-film solar cell of assembling：Open-circuit voltage VOCFor：0.63V, short circuit current JSCFor：8.6mA/cm2,
PCE is：3.3%.
Embodiment 7
A kind of cold nebulization thermal decomposition prepares ZnO:The method of B electric thins, with embodiment 1, wherein：
In (1) step, ammonium borate (NH is added in the precursor liquid of such as method of embodiment 1 configuration4B5O8) so that in solution
B/Zn=3at%。
In (2) step, using quartz glass as substrate, substrate heating temperature is 200 DEG C.
In (3) step, by ZnO film and substrate as in tube-type atmosphere furnace, H is passed through2Volume content is that 5%, Ar volumes contain
After measuring the mixed gas for 95%, 10 are evacuated to-3, 600 DEG C are heated to, is incubated natural cooling after 2h.
Obtained TCO thin film：Mean transmissivity reaches more than 85% in visible-range, surface roughness ＜ 10nm, current-carrying
Sub- concentration is：1.4×1022/cm3, resistivity is：3.3×10-3Ω·cm。
Claims (1)
1. a kind of method that cold nebulization thermal decomposition prepares zinc oxide electronic film, it is characterised in that step is as follows：
(1) precursor liquid is prepared
11g zinc acetates are dissolved in deionized water, 1mol/L zinc acetate solution is configured to, is placed in beaker, in magnetic force or electric mixing
Mix under effect, instill concentrated ammonia liquor, it is 8, Zn to control pH value of solution2+Progressively it is converted into Zn (OH)2Precipitation, vacuum filtration, when filtering
Rinsed repeatedly with deionized water, remove unnecessary anion, dried, weigh 5g sediments, add 30mL deionized waters and 10mL
Methanol, 10mL ammoniacal liquor is added, precipitation dissolving, it is 11 to form pH, [(Zn (NH3)4]2+Concentration is that the transparent zinc ammoniums of 0.1mol/L are molten
Liquid is as precursor liquid；
(2) thin film deposition
Glass fiber reinforcement PET (polyethylene terephthalate) substrate is placed in removable warm table, is heated to 130 DEG C,
The motion mode of moveable platform is controlled, walking speed is 50mm/s, and the domain of walk is 200mm × 200mm；Adjust nozzle and lining
Bottom distance is 200mm, accesses compressed air and opens nozzle, take 30mL precursor liquid to be put into conical flask, peristaltic pump is accessed and bored
Shape bottle and nozzle, the control of forerunner's flow quantity is 0.5mL/min, by pressure control is 2atm by pressure regulator valve, liquid rushes through air-flow
Atomization is hit, is sprayed on substrate, sedimentation time 30min；
(3) it is heat-treated
By the ZnO film of preparation and silicon to 200 DEG C, natural cooling after 2h is incubated.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510892350.8A CN105349970B (en) | 2014-01-24 | 2014-01-24 | A kind of electric thin preparation method of excellent performance |
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| CN201410034109.7A CN103757613B (en) | 2014-01-24 | 2014-01-24 | A kind of method of low-temperature growth zinc oxide electronic film |
| CN201510892350.8A CN105349970B (en) | 2014-01-24 | 2014-01-24 | A kind of electric thin preparation method of excellent performance |
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| CN201410034109.7A Active CN103757613B (en) | 2014-01-24 | 2014-01-24 | A kind of method of low-temperature growth zinc oxide electronic film |
| CN201510892469.5A Active CN105506584B (en) | 2014-01-24 | 2014-01-24 | A kind of preparation method of electric thin |
| CN201510892350.8A Active CN105349970B (en) | 2014-01-24 | 2014-01-24 | A kind of electric thin preparation method of excellent performance |
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| CN201410034109.7A Active CN103757613B (en) | 2014-01-24 | 2014-01-24 | A kind of method of low-temperature growth zinc oxide electronic film |
| CN201510892469.5A Active CN105506584B (en) | 2014-01-24 | 2014-01-24 | A kind of preparation method of electric thin |
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| CN106000705B (en) * | 2016-07-12 | 2018-11-06 | 河北大学 | A kind of full-automatic Pulse Spraying device and spraying method being used to prepare film |
| CN107699870B (en) * | 2017-09-18 | 2020-01-21 | 中山大学 | Method for preparing film in supergravity chemical deposition tube and system required by same |
| CN108091414B (en) * | 2017-12-13 | 2020-05-15 | 浙江海洋大学 | Silver nanowire composite transparent conductive film and preparation thereof |
| CN110590181A (en) * | 2018-06-12 | 2019-12-20 | 兰州大学 | Preparation method of ZnO film and application of ZnO film in ultraviolet sensor |
| CN111239203B (en) * | 2018-11-29 | 2022-05-17 | 中国科学院大连化学物理研究所 | Preparation method of copper oxide film |
| CN109752431B (en) * | 2018-12-29 | 2021-07-30 | 海南大学 | Method for preparing microelectrode by spray drying method |
| CN114182235B (en) * | 2020-09-14 | 2023-09-29 | 北京环境特性研究所 | Method for establishing gas balance flow field in growth chamber |
| CN112939580B (en) * | 2021-01-29 | 2022-07-01 | 广西碧清源环保投资有限公司 | Preparation method of ceramic filtering membrane |
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- 2014-01-24 CN CN201410034109.7A patent/CN103757613B/en active Active
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Also Published As
| Publication number | Publication date |
|---|---|
| CN103757613A (en) | 2014-04-30 |
| CN105506584B (en) | 2018-04-13 |
| CN105506584A (en) | 2016-04-20 |
| CN105483656B (en) | 2018-03-06 |
| CN105483656A (en) | 2016-04-13 |
| CN105349970A (en) | 2016-02-24 |
| CN103757613B (en) | 2015-12-30 |
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