CN111446042B - High-performance transparent conductive film and preparation method and application thereof - Google Patents
High-performance transparent conductive film and preparation method and application thereof Download PDFInfo
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- H—ELECTRICITY
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
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- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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- C23C14/28—Vacuum evaporation by wave energy or particle radiation
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Abstract
The invention belongs to the field of conductive film materials, and discloses a high-performance transparent conductive film, and a preparation method and application thereof. The preparation method comprises the following steps: and cleaning and drying the transparent substrate, and depositing the GZO conductive film at room temperature by using pulsed laser to obtain the high-performance transparent conductive film. The conductive film adopts GZO as a conductive film material, and is green and environment-friendly; moreover, a single-layer GZO film is adopted, so that the process is simple; and the preparation is carried out through pulsed laser deposition, annealing treatment is not needed, and the cost is effectively reduced. The obtained GZO conductive thin film has the advantages of high transmittance, low roughness and low resistance, and can be used for shielding electromagnetic devices and equipment, such as: a battle base hatch cover, a naval vessel porthole and the like.
Description
Technical Field
The invention belongs to the field of conductive film materials, and particularly relates to a high-performance transparent conductive film, and a preparation method and application thereof.
Background
Because many electromagnetic devices and equipment, especially military electromagnetic devices and equipment, transmit or reflect electromagnetic signals, their anti-interference and shielding capabilities become important indicators, such as fighters, also known as fighters, that is, military aircraft used to eliminate enemies and other flight-type air-raid weapons in the air. Since the interior of the cabin of a fighter plane is a cavity structure, each component is a large reflection source. After the external electromagnetic wave is emitted into the cabin, the external electromagnetic wave is easily reflected for multiple times and then is emitted out of the cabin for multiple times, a cavity reflection effect (similar to a corner reflector) is formed, and the radar reflection sectional area (RCS) of the fighter plane is greatly improved. And various devices in the cockpit can actively emit electromagnetic waves, and the electromagnetic waves not only have the signal characteristic of exposing the direction of the airplane, but also have the possibility of exposing the combat information of the fighter, thereby not only increasing the equivalent reflection area of the fighter, but also having the possibility of information leakage. For modern innovative combat fighters, the stealth effect is just needed, so plating a transparent conductive film with an RCS (radar cross section) reducing effect on a base cabin cover of the fighter becomes a necessity of the fighter.
The coating materials for the cabin of a fighter plane are mainly divided into two categories. One type adopts an Indium Tin Oxide (ITO) conductive film, the thickness of the ITO conductive film is 10-20 nm, the indium oxide accounts for 90%, and the tin oxide accounts for 10%. ITO Films prepared by Magnetron Sputtering are widely used because of their High Transmittance and low resistivity ([1] Bush KA, Bailie C D, Chen Y, et al. thermal and Environmental Stability of Semi-transmissive Perovskite solvent Cells for derived Enabled by a Solution-Processed Nano particulate Buffer Layer and dispersed ITO Electrode [ J ]. Advanced Materials,2016,28(20): 3937-. The other type adopts a metal film, particularly a gold film (Au film), which is directly plated by using a gold material, so that the cost is relatively lower than that of the ITO film, the process is not complicated by the ITO film, and the daily maintenance is simpler.
Patent No. CN101881850A discloses a display filter with electromagnetic radiation prevention and filtering functions and a display using the same. The electromagnetic shielding layer is of a 13-layer or 17-layer structure consisting of TiO/AZO or ITO or GZO/Cu/GZO or ITO or AZO repeatedly, wherein the GZO is 1.0-50nm in thickness. Patent No. CN108642473B discloses an infrared transparent window with electromagnetic shielding function and a preparation method thereof. The electromagnetic shielding layer is an oxide laminated film and comprises tin-doped indium oxide (ITO), aluminum-doped zinc oxide (AZO), gallium-doped indium oxide (GZO) and fluorine-doped tin oxide (FTO), and the total thickness of the electromagnetic shielding layer is 0.2-200 mu m. In the conductive film, the ITO film contains In which is a rare element and the In compound has high toxicity, so the ITO conductive film is expensive and not beneficial to environmental protection. In addition, the ITO film requires high temperature annealing to achieve good performance, which requires high requirements for the canopy glass substrate, further increasing cost. In the case of a metal film, the film is transparent and conductive within a certain thickness range, and has a lower resistivity than an ITO film, but when the film thickness is increased, the transmittance is significantly reduced, and it is difficult for a single metal film to satisfy both high transmittance and low resistance. In the patent, a multilayer structure is adopted, the thickness is thick, and the process is complex.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention mainly aims to provide a preparation method of a high-performance transparent conductive film.
Another object of the present invention is to provide a high-performance transparent conductive film prepared by the above method.
It is still another object of the present invention to provide the use of the above high performance transparent conductive film in shielding of electromagnetic devices or equipment.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a high-performance transparent conductive film comprises the following preparation steps:
and cleaning and drying the transparent substrate, and depositing the GZO conductive film at room temperature by using pulsed laser to obtain the high-performance transparent conductive film.
Further, the transparent substrate refers to an alkali-free glass substrate.
Further, the cleaning is ultrasonic cleaning with deionized water and isopropanol in sequence; the drying is drying at the temperature of 75-85 ℃.
Further, the conditions of the pulsed laser deposition are as follows: the distance from the target to the substrate is 7.5cm, the pulse energy is 450mJ, the frequency is 5Hz, the oxygen content is 0Pa, and the number of deposition pulses is 1500-3000.
Further, the thickness of the GZO conductive film is 40-80 nm.
Further, the GZO is comprised of 2 wt.% Ga2O3And 98 wt.% ZnO.
A high-performance transparent conductive film is prepared by the method.
The high-performance transparent conductive film is applied to shielding of electromagnetic devices or equipment.
The preparation method and the obtained product have the following advantages and beneficial effects:
(1) according to the invention, GZO is adopted as a conductive film material, and compared with ITO, the conductive film material does not contain In element, and the remaining Ga, Zn and O are nontoxic, so that the conductive film material conforms to the development trend of environmental protection.
(2) The single-layer GZO film is adopted, the thickness is small (40-80 nm), and the process is simple.
(3) The invention adopts the pulse laser deposition system to prepare the transparent conductive film, has simple operation and high repeatability, completes the preparation of the whole device at room temperature without annealing, and effectively reduces the cost.
(4) The GZO conductive film prepared by the invention can be used for shielding electromagnetic devices and equipment, such as: the battle base hatch cover, naval vessel porthole and the like have the advantages of high transmittance, low roughness and low resistance.
Drawings
FIG. 1 is an XRR test and fitting graph of GZO conductive thin films with different thicknesses obtained in examples 1-4;
FIG. 2 is a graph showing the results of density and roughness of the GZO conductive films of different thicknesses obtained in examples 1-4;
FIG. 3 is a graph showing the transmission spectra of GZO thin films of different thicknesses obtained in examples 1 to 4 in the visible light range (380 to 780 nm);
FIG. 4 is a graph showing the results of the average light transmittance, sheet resistance, resistivity and quality factor of the GZO thin films of different thicknesses obtained in examples 1 to 4;
FIG. 5 is an XRD spectrum of a GZO thin film obtained in example 3.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
Example 1
(1) Cleaning a substrate: arranging 1cm by 1cm alkali-free glass substrates on a film developing frame, putting the film developing frame into a large beaker, and respectively and sequentially ultrasonically cleaning the film developing frame for 15min by using deionized water and isopropanol.
(2) Drying the substrate: and (3) putting the cleaned glass substrate into an oven, and drying at 75-85 ℃.
(3) And (2) depositing the GZO conductive film at room temperature by adopting a pulse laser deposition system, wherein the material is a GZO (2 wt% Ga2O3,98 wt% ZnO) target, the distance from the target to the substrate is 7.5cm, the pulse energy is 450mJ, the frequency is 5Hz, the oxygen content is 0Pa, and the number of deposition pulses is 1500, so that the high-performance transparent conductive film is obtained.
Example 2
(1) Cleaning a substrate: arranging 1cm by 1cm alkali-free glass substrates on a film developing frame, putting the film developing frame into a large beaker, and respectively and sequentially ultrasonically cleaning the film developing frame for 15min by using deionized water and isopropanol.
(2) Drying the substrate: and (3) putting the cleaned glass substrate into an oven, and drying at 75-85 ℃.
(3) And (2) depositing the GZO conductive film at room temperature by adopting a pulse laser deposition system, wherein the material is a GZO (2 wt% Ga2O3,98 wt% ZnO) target, the distance from the target to the substrate is 7.5cm, the pulse energy is 450mJ, the frequency is 5Hz, the oxygen content is 0Pa, and the number of deposition pulses is 2250, so that the high-performance transparent conductive film is obtained.
Example 3
(1) Cleaning a substrate: arranging 1cm by 1cm alkali-free glass substrates on a film developing frame, putting the film developing frame into a large beaker, and respectively and sequentially ultrasonically cleaning the film developing frame for 15min by using deionized water and isopropanol.
(2) Drying the substrate: and (3) putting the cleaned glass substrate into an oven, and drying at 75-85 ℃.
(3) And (2) depositing the GZO conductive film at room temperature by adopting a pulse laser deposition system, wherein the material is a GZO (2 wt% Ga2O3,98 wt% ZnO) target, the distance from the target to the substrate is 7.5cm, the pulse energy is 450mJ, the frequency is 5Hz, the oxygen content is 0Pa, and the number of deposition pulses is 3000, so that the high-performance transparent conductive film is obtained.
Example 4
(1) Cleaning a substrate: arranging 1cm by 1cm alkali-free glass substrates on a film developing frame, putting the film developing frame into a large beaker, and respectively and sequentially ultrasonically cleaning the film developing frame for 15min by using deionized water and isopropanol.
(2) Drying the substrate: and (3) putting the cleaned glass substrate into an oven, and drying at 75-85 ℃.
(3) And (2) depositing the GZO conductive film at room temperature by adopting a pulse laser deposition system, wherein the material is a GZO (2 wt% Ga2O3,98 wt% ZnO) target, the distance from the target to the substrate is 7.5cm, the pulse energy is 450mJ, the frequency is 5Hz, the oxygen content is 0Pa, and the number of deposition pulses is 3500, so that the high-performance transparent conductive film is obtained.
In particular, in order to realize the semiconductor-to-conductor conversion of the GZO material, oxygen (oxygen content 0Pa) does not need to be introduced during the deposition process of the above embodiment, the thin film is in a crystalline state, and the conductivity of the thin film can be effectively improved when the thin film preferentially grows along the c axis.
And (3) carrying out performance test on the conductive film:
table 1 shows the thickness, density and roughness of the GZO conductive films obtained in examples 1 to 4; FIG. 1 is an XRR test and a fitting curve of GZO conductive thin films with different thicknesses obtained in examples 1-4; FIG. 2 shows the density and roughness of the GZO conductive films of different thicknesses obtained in examples 1-4.
TABLE 1 thickness, density and roughness of GZO conductive films obtained in examples 1 to 4
From the above experimental results, the invention successfully prepares a GZO transparent conductive film, the film density increases with the increase of the film thickness, and the film density of the embodiments 1-4 is 5.5 +/-0.2 g/cm3Thus, the obtained film has good compactness. The roughness of the film is increased along with the increase of the thickness of the film, and the roughness of the films in examples 1 to 3 is less than 1.5nm, which shows that the roughness of the films in examples 1 to 3 is small and the performance is excellent, and the roughness of the film is obviously increased when the thickness of the film is increased to 96.28nm in example 4.
Table 2 shows the photoelectric properties of the GZO conductive films obtained in examples 1-4, including the average light transmittance, sheet resistance, resistivity and quality factor in the visible light range (380-780 nm); FIG. 3 is a transmission spectrum of GZO thin films with different thicknesses obtained in examples 1 to 4 in a visible light range (380 to 780 nm); FIG. 4 shows the average light transmittance, sheet resistance, resistivity and quality factor of the GZO thin films of different thicknesses obtained in examples 1-4. FIG. 5 is an XRD spectrum of a GZO thin film obtained in example 3.
TABLE 2 photoelectric characteristics of the GZO conductive films obtained in examples 1 to 4
| Examples | Average light transmittance | Square resistance (omega/□) | Resistivity (omega. m) | Quality factor phiTC(Ω-1) |
| 1 | 87.98％ | 352.8 | 1.51×10-5 | 2.49×10-3 |
| 2 | 81.57％ | 225.2 | 1.48×10-5 | 3.62×10-3 |
| 3 | 76.77％ | 179.6 | 1.45×10-5 | 4.28×10-3 |
| 4 | 72.55％ | 301.13 | 2.90×10-5 | 2.41×10-3 |
From the experimental results, the invention successfully prepares the GZO conductive film and has excellent photoelectric characteristics. The transmittance of the film is reduced along with the increase of the thickness of the film, the light transmittance of the films obtained in examples 1 to 3 is more than 75 percent, and the GZO films obtained in examples 1 to 3 have high light transmittance; the film of example 4 had a low light transmission of 72.55%. With the increase of the thickness of the film, the resistivity of the film is firstly reduced and then increased, which shows that the conductivity of the film is firstly improved and then reduced, and the conductivity of the film is not obviously reduced when the thickness of the film is increased from about 40nm to about 80 nm; as the film thickness continues to increase to 96.28nm, the film conductivity decreases significantly because the film roughness increases significantly with increasing thickness, thereby impeding carrier transport. The film quality factor is an important index for measuring the performance of the transparent conductive film, and as the thickness of the film increases, the film quality factor increases first and then decreases, which indicates that the performance of the transparent conductive film increases first and then decreases, and example 3 is the preferred optimal condition. Fig. 5 is an XRD pattern of the GZO thin film obtained in example 3, which shows that the thin film preferentially grows along the c-axis and the grain boundary scattering is small, thereby improving the conductivity of the thin film.
Therefore, the high-performance transparent conductive film is successfully prepared from the GZO material, is non-toxic and environment-friendly, and is prepared by a pulse laser deposition method without an annealing step, so that the cost is effectively reduced.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (4)
1. A preparation method of a high-performance transparent conductive film is characterized by comprising the following preparation steps:
cleaning and drying the transparent substrate, and depositing a GZO conductive film at room temperature by using pulsed laser to obtain a high-performance transparent conductive film;
the transparent substrate is an alkali-free glass substrate;
the conditions of the pulsed laser deposition are as follows: the distance from the target to the substrate is 7.5cm, the pulse energy is 450mJ, the frequency is 5Hz, the oxygen content is 0Pa, and the number of deposition pulses is 1500-3000;
the thickness of the GZO conductive film is 40-80 nm;
the GZO is composed of 2 wt.% Ga2O3And 98 wt.% ZnO.
2. The method for preparing a high-performance transparent conductive film according to claim 1, wherein: the cleaning is ultrasonic cleaning by using deionized water and isopropanol respectively; the drying is drying at the temperature of 75-85 ℃.
3. A high-performance transparent conductive film is characterized in that: prepared by the method of any one of claims 1 to 2.
4. Use of a high performance transparent conductive film according to claim 3 in shielding of electromagnetic devices or equipment.
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Citations (3)
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|---|---|---|---|---|
| CN101221935A (en) * | 2007-01-10 | 2008-07-16 | 日东电工株式会社 | Transparent conductive film and method for producing the same |
| CN101403094A (en) * | 2008-10-28 | 2009-04-08 | 浙江大学 | Method for growth of type n ZnMgO Ga semiconductor film on flexible substrate |
| CN102965621A (en) * | 2012-11-08 | 2013-03-13 | 广州有色金属研究院 | Preparation method of ZnO transparent conductive film |
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| JP5432501B2 (en) * | 2008-05-13 | 2014-03-05 | 日東電工株式会社 | Transparent conductive film and method for producing the same |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101221935A (en) * | 2007-01-10 | 2008-07-16 | 日东电工株式会社 | Transparent conductive film and method for producing the same |
| CN101403094A (en) * | 2008-10-28 | 2009-04-08 | 浙江大学 | Method for growth of type n ZnMgO Ga semiconductor film on flexible substrate |
| CN102965621A (en) * | 2012-11-08 | 2013-03-13 | 广州有色金属研究院 | Preparation method of ZnO transparent conductive film |
Non-Patent Citations (2)
| Title |
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| Roughness evolution in Ga doped ZnO films deposited by pulsed laser deposition;Yun-yan Liu;《Thin Solid Films》;20110224;第519卷(第16期);第5444-5449页 * |
| 脉冲激光沉积法制备低阻掺镓氧化锌薄膜及其光电性能;莫观孔;《中国激光》;20190618;第212-218页 * |
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