CN109360691A - A kind of preparation method of doped zinc oxide transparent conductive film - Google Patents
A kind of preparation method of doped zinc oxide transparent conductive film Download PDFInfo
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Abstract
The present invention relates to the preparation methods of a kind of graphene and aluminium co-doped zinc oxide transparent conductive thin film, it is characterized in that preparing graphene and aluminium co-doped zinc oxide transparent conductive thin film using sol-gal process, using zinc powder as the raw material of the reducing agent of graphene oxide and formation zinc oxide, the chemical composition of transparent conductive film are as follows: Zn1‑ xO1+zAlxCy, wherein x=0.02-0.1, y=0.05-0.25, z=0.05y-0.1y, preparation process include alumina sol preparation, the reduction of graphene oxide, the preparation of doping colloidal sol, hybrid film coating and hybrid film post-processing.The present invention uses dopant, crystal seed and dispersing agent of the nano alumina sol as hybrid film, improves the light transmittance and electric conductivity of doping film；Using the relatively low new stabilizer of boiling point, overcomes existing stabilizer and be difficult to volatilize, the deficiency for causing transparent conductive film light transmittance to reduce.
Description
Technical field
The present invention relates to a kind of preparation method of doped zinc oxide transparent conductive film, especially a kind of graphene and aluminium are total
The preparation method of doped zinc oxide transparent conductive film, belongs to new material and energy conservation and environmental protection.
Technical background
Transparent conductive film is the photoelectric material with optical transparence and electric conductivity, is supported on glass or transparent tree
It can be used as transparent electrode, the liquid crystal display electrode, gas sensors electrode, the antifog electricity of vehicle window of thin film solar cell on rouge material
Pole and catalysis material etc..Common transparent conductive film material includes indium oxide base (ITO), tin oxide base (FTO) and oxidation
Zinc-base (AZO) transparent conductive oxide film, low resistance precious metal material and grapheme material.
Not only there is aluminium-doped zinc oxide (AZO) transparent conductive oxide film lower resistivity and high optics to penetrate
Rate, and raw material is cheap and easy to get, non-toxic, and easily etching, stability are good, it is considered to be replace the best of indium oxide based conductive film
Candidate material has attracted large quantities of scientific research personnel to be engaged in technological improvement research.Researched and developed sputtering method, pulsed laser deposition,
A variety of AZO transparent conductive film preparation methods such as chemical vapour deposition technique, spray heating decomposition and sol-gel method, but it is thoroughly
Light rate and electric conductivity cannot still reach the technical indicator of ito thin film or FTO film.With the quick hair of graphene preparation technology
Exhibition, professional set about research by graphene and AZO Material cladding, to optimize its light transmission, conduction and catalysis.
The light transmittance of single-layer graphene is up to 97% or more, and for the light transmittance of 4 layers of graphene also up to 90%, electric conductivity is close golden
Belong to copper, there is rollable property and chemical stability, if the doped graphene in zinc oxide or Al-Doped ZnO, covalent bond
Graphene reduce the intergranular resistance of oxide, theoretically by the carrier concentration improved in doping zinc-oxide semiconductor and lead
Electrically, while the toughness for forming film is improved.For example, Chinese patent CN103922388A (2014-07-16) discloses a kind of graphite
Alkene/Al-Doped ZnO conducing composite material preparation method.Chinese patent CN108165956A (2018-06-15) is open a kind of
Add the preparation method of the AZO laminated film of graphene.
Graphene is mainly from graphene oxide reduction preparation, and graphite oxide has two-dimensional slice similar with graphene
Structure, the difference is that introducing a large amount of oxygen-containing group in its molecule, sheet surfaces are dispersed with hydroxyl and epoxy group, lamella side
Edge contains carboxyl and carbonyl, and electric conductivity is greatly reduced, it is necessary to remove oxygen-containing group by reduction reaction.Restoring method packet
Include thermal reduction, hydrothermal reduction method and chemical reduction method etc..The key of chemical reduction method is the selection of chemical reducing agent, Ji Yaokao
Consider its reducing power and price, also to consider Environmental Safety factor when application.The graphene oxide electronation of open report
Agent is more than 10 kinds existing, and organic reducing agent is mainly hydrated hydrazine and its derivative, vitamin C, reduced sugar and amino acid etc.；It is inorganic to go back
Former agent is mainly active metal, sodium borohydride, lithium aluminium hydride reduction, hydrogen, hydroiodic acid and sodium hydrosulfite etc..Chinese patent
CN106140130A (2016-11-23) discloses a kind of ZnO- redox graphene composite photo-catalyst, using zinc powder in alkalinity
Under the conditions of redox graphene, since the zinc oxide of formation is the coarse granule sediment of cohesion, rather than colloidal sol, it is impossible to be used in
Film application.It is multiple that Chinese patent CN105976941A (2016-09-28) discloses a kind of flexible aluminium-doped zinc oxide/graphene
The preparation process of condensation material will restore after graphene oxide film, then be coated with aluminum-doped zinc oxide films on it, technical process
It is more complicated, also without the openly light transmission of composite material film and conductive effect.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of doped zinc oxide transparent conductive film, it is characterised in that uses
Sol-gal process prepares graphene and aluminium co-doped zinc oxide transparent conductive thin film, using zinc powder as the reducing agent of graphene oxide
With the raw material for forming zinc oxide, the chemical composition of transparent conductive film are as follows: Zn1-xO1+zAlxCy , wherein x=0.02-0.1, y=
0.05-0.25, z=0.05y-0.1y, preparation process include alumina sol preparation, the reduction of graphene oxide, doping colloidal sol system
Standby, hybrid film coating and hybrid film post-processing.
Alumina sol preparation is the ethanol solution of aluminium isopropoxide to be added in the inorganic acid aqueous solution of 0.2mol/L,
Heating hydrolysis 4-6h at 60-80 DEG C, it is adsorbed slough inorganic acid after cooling with anion exchange resin, and forming pH is 4-6's
The nano aluminium oxide hydrosol, as the dopant, crystal seed and dispersing agent for preparing doping zinc-oxide colloidal sol, the inorganic acid is nitre
Acid, hydrochloric acid, sulfuric acid and phosphoric acid.
The in-situ reducing of graphene oxide is that nano oxygen is added in the graphene oxide of Hummers graphite oxide method preparation
Change and be ultrasonically treated 0.5-1 h in aluminum water colloidal sol, makes graphene oxide scattered adsorption in nano aluminium oxide hydrosol particle surface, so
Zinc oxide stabilizing agentof sol and organic solvent are added afterwards, by zinc powder batch reactions solution, controls raw material zinc powder, stabilizer, aluminium
The molar ratio of dopant and graphene oxide C are as follows: 1:0.2-0.6:0.02-0.1:0.05-0.25 keeps graphene oxide former
Expect that the oxygen-containing functional group in molecule restores removal, zinc powder is made to be oxidized to Zn under the alkaline condition of pH 8-102+, then hydrolyze
It forms graphene and aluminium codope ZnO nano colloidal sol, the zinc oxide stabilizing agentof sol is methylamine, acetylacetone,2,4-pentanedione and pyroracemic aldehyde
Etc. the compound that can form water soluble ligand with zinc ion, the complexing dissolution of stabilizer prevents to form Zn (OH)2
Precipitating.
Doping colloidal sol preparation be by reduction reaction liquid at 70-90 DEG C back flow reaction 4-6h, react raw material zinc powder completely
Dissolution makes graphene, aluminium oxide and zinc oxide nano-particle carry out hydro-thermal doping, uses organic solvent diluting after cooling, make to adulterate
Solids mass concentration is 5%-6% in colloidal sol, and the organic solvent is one of ethyl alcohol, isopropanol or tetrahydrofuran, passes through tune
Whole doping collosol concentration and organic solvent ratio therein can improve the filming performance of doping colloidal sol.
Hybrid film coating is to be applied using lifting, stick, be coated on solar cell glass matrix by the way of roller coating or spin coating
Hybrid collosol, be heating and curing 3-5min at 130-150 DEG C, and graphene and aluminium codope make gel film crystallization refinement, prevents
Zinc oxide crystal growth has also been blocked in the quick volatilization of the formation of bulky grain zinc oxide crystallization, organic solvent, after solvent volatilizees
Nanometer doped zinc oxide colloidal sol forms fine and close smooth hybrid film.
Hybrid film post-processing is that the glass for covering hybrid film is heated 0.5-1h at 500-600 DEG C, keeps hydridization thin
Film is sintered on glass matrix, enters graphene and aluminium codope in zinc oxide lattice, and removes remaining organic matter ashing,
The thicknesses of layers for forming transparent conductive film glass is 400-1200nm, it is seen that light transmittance 84%-89%, square resistance are
10-20Ω/□。
Following reaction is carried out in the present invention during the in-situ reducing of graphene oxide: (1) in graphene oxide molecule
Oxygen-containing functional group is reduced, and improves the C/O ratio in graphene oxide raw molecule；(2) zinc powder being added is oxidized to simultaneously
Zn2+；(3) Zn2+Hydrolysis generates graphene and aluminium codope ZnO nano colloidal sol；(4) ZnO nanoparticle and stabilizer covalent bond
It forms stable ligand and has blocked Zn (OH)2Precipitating is formed.The relatively low new stabilizer of boiling point is used in the present invention, solidifying
It can volatilize completely during glue film drying, overcome conventional ethanol amines stabilizer and be difficult to volatilize, hold in last handling process
Easily charing is mingled with the defect for causing transparent conductive film light transmittance to reduce in the film.
Graphene oxide used in the present invention is prepared using Hummers graphite oxide method, specific embodiment are as follows:
Expanded graphite micro mist and the concentrated sulfuric acid are mixed, is stirred under the conditions of ice-water bath, NaNO is added into reaction vessel3 With
KMnO4, persistently stir 0.5 h.It then heats the mixture to 40 DEG C or so constant temperature and stirs 1 h, appropriate amount of deionized water is added,
Decomposing hydrogen dioxide solution remnants high oxidation state manganese is added after hydrolysis is stablized, is centrifugated sediment.With dilute hydrochloric acid and deionized water
Washing precipitate, until water phase, close to neutrality, centrifugation obtains graphene oxide.
Graphene oxide is a kind of important Graphene derivative, has two-dimensional slice structure similar with graphene.No
Be which introduce a large amount of oxygen-containing group, sheet surfaces are dispersed with hydroxyl and epoxy group, lamella edge contain carboxyl and
Carbonyl.It is introduced into the big pi bond after oxygen-containing group in graphene to be destroyed, mechanical property and electric property all decline, or even lose
Electric conductivity.But oxygen-containing group can be used as active reaction sites, and small molecule can be grafted to graphene oxide by chemical reaction
Surface, change the chemical composition and polarity of graphene oxide, the interlamellar spacing of graphene oxide made to become larger, Van der Waals force reduce,
More difficult generation aggregation, makes it in water and there are commonly dissolubilities in solvent to increase.By containing in graphene oxide molecule
Oxygen functional group is removed using modes such as electronation, hydrothermal reduction, thermal reduction and catalysis reduction, and can restore generation reduction-oxidation
Graphene, the electric conductivity of redox graphene and carbon-to-oxygen ratio relationship in its molecule are very big.
Using the carboxyl and carbonyl oxygen-containing functional group in zinc powder electronation removal graphene oxide in the present invention, make its C/
O ratio greatly improves, since zinc reducing power is weaker than under acid condition in neutral conditions, by the way of being heated to reflux, with
Zinc powder is set to react dissolution completely.The unreacted zinc powder of oxide coated by zinc is prevented by the way of stabilizer is added.
Experimental raw graphite powder, potassium permanganate, sulfuric acid, hydrogen peroxide, hydrochloric acid, zinc powder, methylamine, levulinic used in the present invention
Ketone, pyroracemic aldehyde, ethyl alcohol, isopropanol and tetrahydrofuran etc. are commercially available chemically pure reagent；Experiment glass is commercially available 1.0mm ultrawhite
Glass commodity, it is seen that light transmittance 91.6%.
The graphene oxide used in the present invention is to prepare in accordance with the following methods: 10g sodium nitrate and 20g graphite powder are added
Into the 500 mL concentrated sulfuric acids, then 60g potassium permanganate is added portionwise, 90 min is stirred to react at lower than 20 DEG C, at 35 DEG C
It is stirred to react 30 min.It is then added into 2800 mL deionized waters, adds the hydrogen peroxide that 200 mL mass concentrations are 3%
Decompose high oxidation state manganese.The bright yellow solution of formation is stood overnight.It is centrifugated the upper layer light liquid of oxidation solution, is with mass concentration
5% hydrochloric acid solution washs precipitating, until wash water, close to neutrality, yellow mercury oxide is dried in vacuo solid to get graphene oxide at 60 DEG C
Body 21g.
The light transmittance of graphene and aluminium co-doped zinc oxide transparent conductive thin film glass is measured with spectrophotometric in the present invention
It is tried to calculate in the transmitance of 400-760nm visible-range；Four probe sheet resistances of the square resistance of transparent conductive film glass
Measurement examination.
The beneficial effects of the present invention are embodied in:
(1) chemical reducing agent and transparent conductive film main component of graphene oxide, reducing are used as simultaneously using zinc powder
Learn the consumption of reducing agent；
(2) dopant, crystal seed and dispersing agent of the nano alumina sol as hybrid film are used, the saturating of doping film is improved
Light rate and electric conductivity；
(3) the relatively low new stabilizer of boiling point is used, existing stabilizer is overcome and is difficult to volatilize, lead to transparent conductive film
The defect that light transmittance reduces.
Specific embodiment
Embodiment 1
Aluminium isopropoxide powder 4.1g(0.02mol) is dissolved in 50mL dehydrated alcohol, the hydrochloric acid of 100mL0.2mol/L is then added
In aqueous solution, 10g anion exchange resin adsorption desalination acid, filtering point is added in the heating hydrolysis 4-6h at 60-80 DEG C after cooling
From anion exchange resin, the nano aluminium oxide hydrosol that pH is 4-6 is obtained.
Graphene oxide 1.0g(0.05mol) is added in the nano aluminium oxide hydrosol, 0.5-1 h is ultrasonically treated, makes oxygen
Then acetylacetone,2,4-pentanedione stabilizer 50g(0.5mol is added in nano aluminium oxide hydrosol particle surface in graphite alkene scattered adsorption)
With dehydrated alcohol 500mL, 66 g(1.0mol of zinc powder) is added portionwise in reaction solution, the back flow reaction 4-6h at 70-90 DEG C,
So that raw material zinc powder is reacted dissolution completely, so that graphene, aluminium oxide and zinc oxide nano-particle is carried out hydro-thermal doping, obtain graphene
With aluminium codope ZnO nano colloidal sol, is diluted after cooling with dehydrated alcohol 1000mL, make to adulterate solids mass concentration in colloidal sol
5%-6%。
Solar cell glass cleaning is clean, it is cut into the square of 100mm ╳ 100mm, is coated with hybrid collosol with stick coating method
1-2 times, be heating and curing 3-5min at 130-150 DEG C, and nanometer doped zinc oxide colloidal sol forms fine and close smooth after solvent volatilization
Hybrid film.0.5-1h further is heated at 500-600 DEG C, makes hybrid film sintering on glass matrix, forms transparent lead
The thicknesses of layers of conductive film glass is 400nm, it is seen that light transmittance 89%, square resistance are 20 Ω/.
Embodiment 2
Aluminium isopropoxide powder 20.5g(0.1mol) is dissolved in 200mL dehydrated alcohol, the nitre of 100mL0.2mol/L is then added
In aqueous acid, the heating hydrolysis 4-6h at 60-80 DEG C is added 10g anion exchange resin and adsorbs denitrated acid, filtering after cooling
Anion exchange resin is separated, the nano aluminium oxide hydrosol that pH is 4-6 is obtained.
Graphene oxide 5.0g(0.25mol) is added in the nano aluminium oxide hydrosol, 0.5-1 h is ultrasonically treated, makes oxygen
Then pyroracemic aldehyde stabilizer 36g(0.5mol is added in nano aluminium oxide hydrosol particle surface in graphite alkene scattered adsorption) and
66 g(1.0mol of zinc powder) is added portionwise in reaction solution tetrahydrofuran 500mL, and back flow reaction 4-6h, makes at 70-90 DEG C
Raw material zinc powder reacts dissolution completely, and graphene, aluminium oxide and zinc oxide nano-particle is made to carry out hydro-thermal doping, obtain graphene and
Aluminium codope ZnO nano colloidal sol is diluted with dehydrated alcohol 1000mL after cooling, makes to adulterate solids mass concentration in colloidal sol
5%-6%。
Solar cell glass cleaning is clean, it is cut into the square of 100mm ╳ 100mm, is coated with hybrid collosol with stick coating method
1-2 times, be heating and curing 3-5min at 130-150 DEG C, and nanometer doped zinc oxide colloidal sol forms fine and close smooth after solvent volatilization
Hybrid film.0.5-1h further is heated at 500-600 DEG C, makes hybrid film sintering on glass matrix, forms transparent lead
The thicknesses of layers of conductive film glass is 1200nm, it is seen that light transmittance 84%, square resistance are 10 Ω/.
Claims (6)
1. a kind of preparation method of doped zinc oxide transparent conductive film, it is characterised in that prepare graphene using sol-gal process
With aluminium co-doped zinc oxide transparent conductive thin film, using zinc powder as the reducing agent of graphene oxide and formed zinc oxide raw material,
The chemical composition of transparent conductive film are as follows: Zn1-xO1+zAlxCy , wherein x=0.02-0.1, y=0.05-0.25, z=0.05y-
0.1y, preparation process include alumina sol preparation, graphene oxide reduction, doping colloidal sol preparation, hybrid film coating and
Hybrid film post-processing.
2. the preparation method of doped zinc oxide transparent conductive film according to claim 1, it is characterised in that aluminium oxide is molten
Glue preparation is the ethanol solution of aluminium isopropoxide to be added in the inorganic acid aqueous solution of 0.2mol/L, and hydrolysis is heated at 60-80 DEG C
It is adsorbed with anion exchange resin after cooling and sloughs inorganic acid by 4-6h, forms the nano aluminium oxide hydrosol that pH is 4-6,
As the dopant, crystal seed and dispersing agent for preparing doping zinc-oxide colloidal sol, the inorganic acid is nitric acid, hydrochloric acid, sulfuric acid and phosphorus
Acid.
3. the preparation method of doped zinc oxide transparent conductive film according to claim 1, it is characterised in that graphite oxide
The in-situ reducing of alkene is that ultrasound in the nano aluminium oxide hydrosol is added in the graphene oxide of Hummers graphite oxide method preparation
0.5-1 h is handled, makes graphene oxide scattered adsorption in nano aluminium oxide hydrosol particle surface, stabilizing agentof sol is then added
And organic solvent, by zinc powder batch reactions solution, C in control raw material zinc powder, stabilizer, aluminium dopants and graphene oxide
Molar ratio are as follows: 1:0.2-0.6:0.02-0.1:0.05-0.25 makes the oxygen-containing functional group in graphene oxide raw molecule
Reduction removal, makes zinc powder be oxidized to Zn under the alkaline condition of pH 8-102+, then hydrolyze to form graphene and aluminium codope
ZnO nano colloidal sol, the zinc oxide stabilizing agentof sol are methylamine, acetylacetone,2,4-pentanedione and pyroracemic aldehyde.
4. the preparation method of doped zinc oxide transparent conductive film according to claim 1, it is characterised in that doping colloidal sol
Preparation be by reduction reaction liquid at 70-90 DEG C back flow reaction 4-6h, so that raw material zinc powder is reacted dissolution completely, make graphene, oxygen
Change aluminium and zinc oxide nano-particle carries out hydro-thermal doping, uses organic solvent diluting after cooling, make the matter for adulterating solids in colloidal sol
Amount concentration is 5%-6%, and the organic solvent is one of ethyl alcohol, isopropanol or tetrahydrofuran.
5. the preparation method of doped zinc oxide transparent conductive film according to claim 1, it is characterised in that hybrid film
Coating is to be applied using lifting, stick, be coated with hybrid collosol on solar cell glass matrix by the way of roller coating or spin coating, in 130-
Be heating and curing 3-5min at 150 DEG C, and nanometer doped zinc oxide colloidal sol forms fine and close smooth hybrid film after solvent volatilization.
6. the preparation method of doped zinc oxide transparent conductive film according to claim 1, it is characterised in that hybrid film
Post-processing is that the glass for covering hybrid film is heated 0.5-1h at 500-600 DEG C, forms the film of transparent conductive film glass
Layer is with a thickness of 400-1200nm, it is seen that light transmittance 84%-89%, square resistance are 10-20 Ω/.
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| CN112259770A (en) * | 2020-10-21 | 2021-01-22 | 贵州梅岭电源有限公司 | Anti-degradation enhanced proton exchange membrane and preparation method thereof |
| CN114656165A (en) * | 2022-03-24 | 2022-06-24 | 中建材玻璃新材料研究院集团有限公司 | Glass dustproof coating and preparation method thereof |
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