CN102330075A - Preparation method of ZnO-based transparent conductive film - Google Patents
Preparation method of ZnO-based transparent conductive film Download PDFInfo
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- CN102330075A CN102330075A CN201110286754A CN201110286754A CN102330075A CN 102330075 A CN102330075 A CN 102330075A CN 201110286754 A CN201110286754 A CN 201110286754A CN 201110286754 A CN201110286754 A CN 201110286754A CN 102330075 A CN102330075 A CN 102330075A
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Abstract
The invention provides a preparation method of a ZnO-based transparent conductive film by adopting a spraying pyrolysis method. The method provided by the invention comprises the following steps of: preparing a precursor solution composed of a Zn source and a doped ion source, wherein the concentration of Zn<2+> in the precursor solution is 0.01-5mol/L, the mol ratio of Zn<2+> to doped ion is 1: (0.01-0.3); adding acid and an organic solvent into the precursor solution, then atomizing the precursor solution, transporting the atomized solution into a film growth chamber by virtue of a carrier gas, and decomposing and depositing on the surface of a substrate with the temperature of 250-850 DEG C to generate the ZnO-based transparent conductive film. The method for preparing the ZnO-based transparent conductive film has low equipment and raw material cost, simple process and short production period, and the prepared product has low surface resistivity and high light transmittance.
Description
Technical field
The invention provides a kind of method for preparing the zno-based transparent conductive film, be specially a kind of method that adopts spray pyrolysis to prepare the zno-based transparent conductive film.
Background technology
Transparent conductive film is a kind of to visible transparent and have the film of excellent conductive capability, is mainly used in fields such as solar cell, liquid-crystal display, photodiode, laser diode and heat-insulating and energy-saving glass.Transparent conductive film mainly contains four big systems, and sheet metal conducting film, ITO transparent conductive film, FTO transparent conductive film and zno-based transparent conductive film (be mainly ZnO:Al, In, Ga).Wherein the sheet metal conducting film can only apply to the less demanding field of light transmission owing to light transmission is too poor; ITO transparent conductive film and FTO transparent conductive film have higher visible light transmissivity and specific conductivity simultaneously; But main element In and Sn in these two kinds of transparent conductive films are considerably less at the content of occurring in nature; Cost an arm and a leg, and stability is not high in hydrogen plasma.Therefore, the zno-based transparent conductive film that how research prepares that the raw material reserves are abundant, cheap, environmental friendliness, visible light transmissivity and electroconductibility can be compared with the ITO transparent conductive film mutually to the price of devices such as reduction liquid-crystal display, solar cell highly significant.
The preparation method of present zno-based transparent conductive film has multiple, mainly comprises magnetron sputtering method (MS), plasma enhanced chemical vapor deposition method (PECVD), sol-gel method (Sol-Gel) and spray pyrolysis (SP).Adopt the zno-based transparent conductive film representative value of magnetron sputtering method preparation to be: surface resistivity 10
-3～10
-4Ω cm, visible light average transmittances 80%～85%.Though the zno-based transparent conductive film of magnetron sputtering method preparation has higher visible light transmissivity and lower surface resistivity simultaneously, this equipment needs higher vacuum tightness, and maintenance of the equipment is complicated, and process step is many and utilization rate of raw materials is low.The characteristics that the plasma enhanced chemical vapor deposition method is the most outstanding are to be lowered into film temperature, in industry, be applied to the preparation of zno-based transparent conductive film, but this method need vacuum apparatus equally, and cost is higher.Sol-gel method is that a kind of technology is simple, can big area film forming and lower-cost method for manufacturing thin film.But since in the heat treatment process with the volatilization and the decomposition of organic solvent, the film density is not high, surface resistivity is bigger.Method is compared in the spray pyrolysis and above-mentioned three, and equipment and raw materials cost are lower, and technology is simple, with short production cycle, and is bigger but its shortcoming is the surface resistivity of film.
Summary of the invention
The invention provides a kind of method for preparing the zno-based transparent conductive film, lower at equipment and raw materials cost, technology is simple, can the big area film forming, on the basis with short production cycle, prepared product transmission of visible light is high, surface resistivity is little.
Realize that the technical scheme that above-mentioned purpose of the present invention adopted is:
A kind of preparation method of zno-based transparent conductive film may further comprise the steps:
(1) precursor solution of preparation Zn source and dopant ion source formation, Zn in the precursor solution
2+Concentration be 0.01mol/L～5mol/L, Zn
2+With the mole proportioning of dopant ion be 1: 0.01～0.3, wherein dopant ion comprises Al at least
3+, In
3+, Ga
3+, Sn
4+And F
-In a kind of.
(2) in precursor solution, add acid and organic solvent; Make the pH value of precursor solution be adjusted to 1.50～6.00; And make Zn ion and dopant ion uniform mixing in the precursor solution; The acid that adds comprises that at least a kind of in acetic acid, oxalic acid, Hydrocerol A, Whitfield's ointment, xitix, nitric acid and the hydrochloric acid, the organic solvent of adding comprise a kind of in ethanol, methyl alcohol and the acetone at least;
(3) with the precursor solution atomizing that mixes; Solution after the atomizing is transported to thin film growth chamber through carrier gas; Be to decompose deposition on 250 ℃～850 ℃ the substrate surface to generate the zno-based transparent conductive film in temperature, substrate is monocrystalline silicon piece, silicate glass, silica glass, sapphire or silicon carbide plate;
Zn source in the step (1) comes from Zn (CH
3COO)
2Or Zn (NO
3)
2
Atomizing adopts pressurized air or ultrasonic atomizer to carry out in the step (3); Air, nitrogen or nitrogen hydrogen mixeding gas are adopted in carrier gas in the step (3); Substrate is selected sheet glass for use in the step (3), and the temperature of sheet glass is 420 ℃; Growth for Thin Film speed is 10nm/min～50nm/min in the step (3); As preferably, step (3) growth for Thin Film speed is 20nm/min.
In the step (3) transparent conductive film that makes is carried out anneal under rare gas element or weak reducing gas atmosphere, 200 ℃～550 ℃ of annealing temperatures, annealing time is 5min～120min; As preferably, in the step (3) with the transparent conductive film that makes at H
2With N
2Volume ratio be to carry out anneal under 1: 9 the atmosphere, annealing temperature is 400 ℃, annealing time is 20min.
The preparation method of zno-based transparent conductive film provided by the invention compared with prior art has some advantages: compare with magnetron sputtering method, the present invention can reduce the film preparation cost significantly, comprises raw materials cost and cost of equipment maintenance; Compare with plasma reinforced chemical vapour deposition, the film of the present invention's preparation has remarkable advantages aspect preparation cost, and technology is simpler; Compare with sol-gel method, this method thin film preparation process is simpler, and the cycle is short, and uniformity of film is better, and has higher visible light transmissivity and lower surface resistivity.Compare with existing spray pyrolysis, the prepared product surface resistivity of the present invention is lower.
Embodiment
The present invention is done bright in detail specifically below in conjunction with specific embodiment.
Embodiment 1
Present embodiment adopts preferred processing condition, adopts In (NO
3)
3The aqueous solution and Zn (CH
3COO)
2Aqueous solution configuration precursor solution, Zn in the precursor solution
2+Concentration is 0.1mol/L, Zn
2+And In
3+The mole proportioning be 1: 0.0225.Add ethanol and Glacial acetic acid min. 99.5, make the pH value of precursor solution be adjusted to 4.91, and mix.Open temperature regulating device, heating silicate glass substrate to 420 ℃, temperature-stable is at 420 ± 10 ℃.Treat the stable back unlatching of underlayer temperature atomisation unit; The precursor solution for preparing is atomized into small droplets under hyperacoustic concussion effect; Be transported to thin film growth chamber through air; And on the surface of substrate, decompose deposition generation zno-based transparent conductive film, the growth for Thin Film rate-controlling is about 20nm/min.Turn off atomisation unit and temperature regulating device behind the growth 25min clock, taking-up gets final product behind the film sample furnace cooling.The thickness of the zno-based transparent conductive film that makes in the present embodiment is approximately 500nm, and the surface resistivity that four point probe records this sample is 1.93 * 10
-2Ω cm.With the transparent conductive film that makes at H
2With N
2Volume ratio be to carry out anneal under 1: 9 the atmosphere, annealing temperature is 400 ℃, annealing time is 20min.Annealing back surface resistivity is 3.5 * 10
-3Ω cm, average transmittance is 93.78% in 400nm～850nm wavelength region.
Atomisation unit also can adopt Compressed Air Nebulizer in the present embodiment; Carrier gas also can be adopted nitrogen or nitrogen hydrogen mixeding gas in the present embodiment; Substrate can also be selected monocrystalline silicon piece, silica glass, sapphire or silicon carbide plate for use in this enforcement.
Embodiment 2
Adopt In (NO
3)
3The aqueous solution and Zn (NO
3)
2Aqueous solution configuration precursor solution, Zn in the precursor solution
2+Concentration is 3mol/L, Zn
2+And In
3+The mole proportioning be 1: 0.03.Add methyl alcohol and nitric acid, make the pH value of precursor solution be adjusted to 2.35, and mix.Open temperature regulating device, heating silica glass substrate to 400 ℃, temperature-stable is at 400 ± 10 ℃.Treat the stable back unlatching of underlayer temperature atomisation unit; The precursor solution for preparing is atomized into small droplets under hyperacoustic concussion effect; Be transported to thin film growth chamber through air; And on the surface of substrate, decompose deposition generation zno-based transparent conductive film, the growth for Thin Film rate-controlling is about 30nm/min.Turn off atomisation unit and temperature regulating device behind the growth 17min clock, taking-up gets final product behind the film sample furnace cooling.The thickness of the zno-based transparent conductive film that makes in the present embodiment is approximately 500nm, and the surface resistivity that four point probe records this sample is 2.8 * 10
-1Ω cm.With the transparent conductive film that makes at H
2With N
2Volume ratio be to carry out anneal under 1: 9 the atmosphere, annealing temperature is 400 ℃, annealing time is 20min.Annealing back surface resistivity is 6.2 * 10
-3Ω cm, average transmittance is 92.24% in 400nm～850nm wavelength region.
Atomisation unit also can adopt Compressed Air Nebulizer in the present embodiment; Carrier gas also can be adopted nitrogen or nitrogen hydrogen mixeding gas in the present embodiment; Substrate can also be selected monocrystalline silicon piece, silicate glass, sapphire or silicon carbide plate for use in this enforcement
Embodiment 3
Adopt Sn (NO
3)
3The aqueous solution and Zn (CH
3COO)
2Aqueous solution configuration precursor solution, Zn in the precursor solution
2+Concentration is 0.1mol/L, Zn
2+And Sn
4+The mole proportioning be 1: 0.1.Add acetone, ethanol, Hydrocerol A, Whitfield's ointment and hydrochloric acid, make the pH value of precursor solution be adjusted to 2.93, and mix.Open temperature regulating device, heating silicate glass substrate to 320 ℃, temperature-stable is at 320 ± 10 ℃.Treat the stable back unlatching of underlayer temperature atomisation unit; The precursor solution for preparing is atomized into small droplets under hyperacoustic concussion effect; Be transported to thin film growth chamber through air; And on the surface of substrate, decompose deposition generation zno-based transparent conductive film, the growth for Thin Film rate-controlling is about 15nm/min.Turn off atomisation unit and temperature regulating device behind the growth 33min clock, taking-up gets final product behind the film sample furnace cooling.The thickness of the zno-based transparent conductive film that makes in the present embodiment is approximately 500nm, and the surface resistivity that four point probe records this sample is 6.37 * 10
-2Ω cm.With the transparent conductive film that makes at H
2With N
2Volume ratio be to carry out anneal under 1: 9 the atmosphere, annealing temperature is 400 ℃, annealing time is 30min.Annealing back surface resistivity is 5 * 10
-3Ω cm, average transmittance is 93.54% in 400nm～850nm wavelength region.
Atomisation unit also can adopt Compressed Air Nebulizer in the present embodiment; Carrier gas also can be adopted nitrogen or nitrogen hydrogen mixeding gas in the present embodiment; Substrate can also be selected monocrystalline silicon piece, silica glass, sapphire or silicon carbide plate for use in this enforcement.
Embodiment 4
Adopt Al (NO
3)
3The aqueous solution and Zn (CH
3COO)
2Aqueous solution configuration precursor solution, Zn in the precursor solution
2+Concentration is 0.5mol/L, Zn
2+And Al
3+The mole proportioning be 1: 0.08.Add ethanol, xitix and oxalic acid, make the pH value of precursor solution be adjusted to 5.26, and mix.Open temperature regulating device, heating silicate glass substrate to 320 ℃, temperature-stable is at 320 ± 10 ℃.Treat the stable back unlatching of underlayer temperature atomisation unit; The precursor solution for preparing is atomized into small droplets under hyperacoustic concussion effect; Be transported to thin film growth chamber through air; And on the surface of substrate, decompose deposition generation zno-based transparent conductive film, the growth for Thin Film rate-controlling is about 20nm/min.Turn off atomisation unit and temperature regulating device behind the growth 25min clock, taking-up gets final product behind the film sample furnace cooling.The thickness of the zno-based transparent conductive film that makes in the present embodiment is approximately 500nm, and the surface resistivity that four point probe records this sample is 9.8 * 10
-2Ω cm.With the transparent conductive film that makes at H
2With N
2Volume ratio be to carry out anneal under 1: 8 the atmosphere, annealing temperature is 300 ℃, annealing time is 40min.Annealing back surface resistivity is 7.5 * 10
-3Ω cm, average transmittance is 90.58% in 400nm～850nm wavelength region.
Atomisation unit also can adopt Compressed Air Nebulizer in the present embodiment; Carrier gas also can be adopted nitrogen or nitrogen hydrogen mixeding gas in the present embodiment; Substrate can also be selected monocrystalline silicon piece, silica glass, sapphire or silicon carbide plate for use in this enforcement.
Embodiment 5
Adopt the identical experimental procedure of embodiment 1, different is that dopant ion is In
3+And Al
3+Hybrid ionic, the mole proportioning be Zn
2+: In
3+: Al
3+=1: 0.02: 0.01, prepared the zno-based transparent conductive film that thickness is approximately 500nm, when unannealed the surface resistivity of sample is 2.1 * 10
-2Ω cm, with the transparent conductive film that makes at H
2With N
2Volume ratio be to carry out anneal under 1: 8 the atmosphere, annealing temperature is 500 ℃, annealing time is 20min.Annealing back surface resistivity is 3.6 * 10
-3Ω cm, average transmittance is 90.58% in 400nm～850nm wavelength region.
Embodiment 6
Adopt the identical experimental procedure of embodiment 1, different is that dopant ion is Ga
3+And F
-Hybrid ionic, Zn in the precursor solution
2+Concentration be 1.5mol/L, the mole proportioning be Zn
2+: Ga
3+: F
-=1: 0.02: 0.01, prepared the zno-based transparent conductive film that thickness is approximately 500nm, when unannealed the surface resistivity of sample is 7.40 * 10
-2Ω cm, with the transparent conductive film that makes at H
2With N
2Volume ratio be to carry out anneal under 1: 9 the atmosphere, annealing temperature is 400 ℃, annealing time is 20min.Annealing back surface resistivity is 6.83 * 10
-3Ω cm, average transmittance is 91.37% in 400nm～850nm wavelength region.
Embodiment 7
Adopt the spray pyrolysis of prior art to prepare the zno-based transparent conductive film in the present embodiment, the Zn source is a zinc acetate, and dopant ion is In
3+, prepared the zno-based transparent conductive film that thickness is approximately 500nm.The surface resistivity of sample is 58.9 * 10 when unannealed
-2Ω cm is at H
2With N
2Volume ratio be to carry out anneal under 1: 9 the atmosphere, annealing temperature is 400 ℃, annealing time is 20min.Annealing back surface resistivity is 1.77 * 10
-2Ω cm, average transmittance is 93.56% in 400nm～850nm wavelength region.
Embodiment 7 and embodiment 1～6 are compared, find to adopt the surface resistivity of the prepared zno-based transparent conductive film of technology of the present invention that great reduction has been arranged with respect to prior art, thereby make performance of products excellent more.
Claims (9)
1. the preparation method of a zno-based transparent conductive film may further comprise the steps:
(1) precursor solution of preparation Zn source and dopant ion source formation, Zn in the precursor solution
2+Concentration be 0.01mol/L～5mol/L, Zn
2+With the mole proportioning of dopant ion be 1: 0.01～0.3, wherein dopant ion comprises Al at least
3+, In
3+, Ga
3+, Sn
4+And F
-In a kind of;
(2) in precursor solution, add acid and organic solvent; Make the pH value of precursor solution be adjusted to 1.50～6.00 and make Zn ion and the dopant ion uniform mixing in the precursor solution; The acid that adds comprises that at least a kind of in acetic acid, oxalic acid, Hydrocerol A, Whitfield's ointment, xitix, nitric acid and the hydrochloric acid, the organic solvent of adding comprise a kind of in ethanol, methyl alcohol and the acetone at least;
(3) with the precursor solution atomizing that mixes; Solution after the atomizing is transported to thin film growth chamber through carrier gas; Be to decompose deposition on 250 ℃～850 ℃ the substrate surface to generate the zno-based transparent conductive film in temperature, substrate is monocrystalline silicon piece, silicate glass, silica glass, sapphire or silicon carbide plate.
2. the preparation method of zno-based transparent conductive film according to claim 1 is characterized in that: the Zn source in the step (1) comes from Zn (CH
3COO)
2Or Zn (NO
3)
2
3. the preparation method of zno-based transparent conductive film according to claim 1 is characterized in that: atomizing adopts pressurized air or ultrasonic atomizer to carry out in the step (3).
4. the preparation method of zno-based transparent conductive film according to claim 1 is characterized in that: air, nitrogen or nitrogen hydrogen mixeding gas are adopted in carrier gas in the step (3).
5. the preparation method of zno-based transparent conductive film according to claim 1 is characterized in that: substrate is selected sheet glass for use in the step (3), and the temperature of sheet glass is 420 ℃.
6. the preparation method of zno-based transparent conductive film according to claim 1 is characterized in that: growth for Thin Film speed is 10nm/min～50nm/min in the step (3).
7. the preparation method of zno-based transparent conductive film according to claim 6 is characterized in that: step (3) growth for Thin Film speed is 20nm/min.
8. the preparation method of zno-based transparent conductive film according to claim 1; It is characterized in that: in the step (3) transparent conductive film that makes is carried out anneal under rare gas element or weak reducing gas atmosphere; 200 ℃～550 ℃ of annealing temperatures, annealing time is 5min～120min.
9. the preparation method of zno-based transparent conductive film according to claim 8 is characterized in that: in the step (3) with the transparent conductive film that makes at H
2With N
2Volume ratio be to carry out anneal under 1: 9 the atmosphere, annealing temperature is 400 ℃, annealing time is 20min.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103590022A (en) * | 2013-11-27 | 2014-02-19 | 昆明理工大学 | Method for making film through ultrasonic atomization-microwave pyrolysis |
| CN103757613A (en) * | 2014-01-24 | 2014-04-30 | 重庆文理学院 | Method for preparing zinc oxide electronic film at low temperature |
| CN103803809A (en) * | 2014-02-22 | 2014-05-21 | 蚌埠玻璃工业设计研究院 | Method for producing zinc oxide-based transparent conductive coating glass |
| 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 |
| CN111293230A (en) * | 2018-12-10 | 2020-06-16 | 广东聚华印刷显示技术有限公司 | Thin film packaging layer and preparation method thereof, and preparation method of display panel |
| CN112133638A (en) * | 2020-04-28 | 2020-12-25 | 北京环境特性研究所 | Method for controlling film forming thickness of ZnO film based on precursor solution and application thereof |
| CN113066900A (en) * | 2021-03-24 | 2021-07-02 | 河北北方学院 | Preparation method of low-cost ZnO transparent conductive film |
| CN114892158A (en) * | 2022-03-25 | 2022-08-12 | 温州安能科技有限公司 | Method for plating corrosion-resistant low-resistance nano film on surface of aluminum alloy |
| TWI790667B (en) * | 2021-07-01 | 2023-01-21 | 國立中山大學 | Method for forming oxide-based thin film and semiconductor device including oxide-based thin film |
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| CN103590022A (en) * | 2013-11-27 | 2014-02-19 | 昆明理工大学 | Method for making film through ultrasonic atomization-microwave pyrolysis |
| CN105349970B (en) * | 2014-01-24 | 2017-12-05 | 重庆文理学院 | A kind of electric thin preparation method of excellent performance |
| CN105506584B (en) * | 2014-01-24 | 2018-04-13 | 重庆文理学院 | A kind of preparation method of electric thin |
| CN103757613B (en) * | 2014-01-24 | 2015-12-30 | 重庆文理学院 | A kind of method of low-temperature growth zinc oxide electronic film |
| CN105349970A (en) * | 2014-01-24 | 2016-02-24 | 重庆文理学院 | Method for preparing electronic film excellent in performance |
| CN105506584A (en) * | 2014-01-24 | 2016-04-20 | 重庆文理学院 | Preparation method of electronic thin film |
| CN103757613A (en) * | 2014-01-24 | 2014-04-30 | 重庆文理学院 | Method for preparing zinc oxide electronic film at low temperature |
| CN103803809A (en) * | 2014-02-22 | 2014-05-21 | 蚌埠玻璃工业设计研究院 | Method for producing zinc oxide-based transparent conductive coating glass |
| 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 |
| CN111293230A (en) * | 2018-12-10 | 2020-06-16 | 广东聚华印刷显示技术有限公司 | Thin film packaging layer and preparation method thereof, and preparation method of display panel |
| CN112133638A (en) * | 2020-04-28 | 2020-12-25 | 北京环境特性研究所 | Method for controlling film forming thickness of ZnO film based on precursor solution and application thereof |
| CN113066900A (en) * | 2021-03-24 | 2021-07-02 | 河北北方学院 | Preparation method of low-cost ZnO transparent conductive film |
| CN113066900B (en) * | 2021-03-24 | 2022-03-18 | 河北北方学院 | Preparation method of low-cost ZnO transparent conductive film |
| TWI790667B (en) * | 2021-07-01 | 2023-01-21 | 國立中山大學 | Method for forming oxide-based thin film and semiconductor device including oxide-based thin film |
| CN114892158A (en) * | 2022-03-25 | 2022-08-12 | 温州安能科技有限公司 | Method for plating corrosion-resistant low-resistance nano film on surface of aluminum alloy |
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Application publication date: 20120125 |