CN103147061B - Method for preparing amorphous transparent zinc oxide film - Google Patents
Method for preparing amorphous transparent zinc oxide film Download PDFInfo
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- CN103147061B CN103147061B CN201310092190.XA CN201310092190A CN103147061B CN 103147061 B CN103147061 B CN 103147061B CN 201310092190 A CN201310092190 A CN 201310092190A CN 103147061 B CN103147061 B CN 103147061B
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Abstract
The invention relates to the technology of a film, and discloses a method for preparing an amorphous transparent zinc oxide film. The method comprises the following steps of: on the basis of utilizing the surface of a substrate as a basal layer, coating a uniform metal zinc film layer on the basal layer, and carrying out thermal oxidation treatment on the metal zinc film in an air environment so as to obtain the zinc oxide film; and putting the prepared metal zinc film in a muffle, rising the temperature to 400-600 DEG C in 4-25 minutes in the air environment, and carrying out heat treatment on the metal zinc film so as to obtain the amorphous transparent zinc oxide film. According to the method, the amorphous transparent zinc oxide film can be prepared through adjusting the thermal oxidation rate and temperature of the metal zinc film.
Description
Technical field
The present invention relates to thin film technique, be specifically related to a kind of preparation method of zinc-oxide film.
Background technology
Broad stopband oxide semiconductor owing to having high permeability and good conductivity in visible-range, be widely used in the fields such as solar cell, flat-panel monitor, organic LED, low emissivity glass, transparent film transistor and flexible electronic device, its Commercial Prospect is very good., there is the defects such as a large amount of crystal boundaries, caused the problem of many device performance aspects in traditional semiconductor film.As device stability reduces, homogeneity is deteriorated, and I-V characteristic is changed significantly in time, and after stressed bending, performance is undergone mutation, and these all limit materials application field.Theoretical and experiment proves, noncrystalline membrane material is not owing to existing the defects such as crystal boundary, and prepared device has good homogeneity and good bending resistance etc.
Amorphous zinc oxide base semiconductor oxide compound, has following characteristics: (1) metallic zinc element obtains easily, low price; (2) the ITO electroconductibility of amorphous zinc oxide electroconductibility and crystalline state is close, and amorphous kenel structure is easy to etching; (3) comparatively ITO is mild for amorphous zinc oxide surface roughness, contributes to luminous efficiency and the life of photoelectric device; (4) amorphous zinc oxide is conducive to low temperature growth, can obtain well-behaved nesa coating on a flexible substrate; (5) after significantly bending, still retention is constant; (6) suitable doping effectively can improve conductive capability etc.This material is subject to the favor of numerous researchists, is to be applied in the semiconductor material that transparent flexible electron device is expected most at present.
A kind of method of non-crystalline state transparent oxide film is had, Chinese invention patent " method of forming amorphous transparent oxide film at low temperature ", the patent No.: ZL201010218263 in existing technology.The method has lot of advantages, but, still there are some essence not enough: 1) poor by the adhesive force of low temperature (273K) deposition acquisition, easily come off; 2) low temperature environment in membrane-film preparation process realizes difficulty, and cost is high, cannot prepare on a large scale.
Summary of the invention
The object of the invention is to, provide a kind of method preparing non-crystalline state zinc carbonate film, to solve the problem.
Technical problem solved by the invention can realize by the following technical solutions:
A kind of method preparing non-crystalline state zinc carbonate film, comprise a substrate, adopt substrate surface as stratum basale, it is characterized in that: plate one deck homogeneous metal zinc rete at stratum basale, metallic zinc film by thermal oxidative treatment, namely obtains zinc-oxide film in air ambient.The metallic zinc film prepared is placed in retort furnace, under air ambient, in 4-25 minute, temperature is risen to 400-600 degree Celsius, metallic zinc film is heat-treated, non-crystalline state zinc carbonate film can be obtained.The present invention can prepare non-crystalline state zinc carbonate film by regulating metallic zinc film thermal oxidation rate and temperature.Compared with prior art, advantage of the present invention and positively effect are: in air atmosphere, reach by the temperature and heat-up rate that regulate the thermooxidizing of metallic zinc the non-crystalline state and transparent object that realize zinc-oxide film, be widely used in the fields such as solar cell, flat-panel monitor, organic LED, low emissivity glass, transparent film transistor and flexible electronic device.
During thermal oxidative treatment, thermooxidizing heat-up rate is 4-25 minute.The oxidation temperature range of metallic zinc film is 400-600 degree Celsius.Described substrate is quartz, glass, crystal or silicon chip.
As a kind of preferred version, under room temperature, adopt Magnetron reactive sputtering, the metallic zinc of experiment employing 99.99% is as cathode target, and anode is connected with vacuum chamber.Be contained in substrate chuck by the substrate after ultrasonic cleaning, shifting board is placed between substrate chuck and target; Vacuumize after shutting each air valve, until vacuum tightness reaches 2 × more than 10-4Pa; Pass into appropriate argon gas; Regulate high threshold to required operating air pressure; Open direct supply build-up of luminance pre-sputtering number minute; Rotating substrate fixture, removes shifting board, starts deposit film.
The metallic zinc film deposited is placed in retort furnace, under air ambient, in 5 minutes, temperature is risen to 400 degree, film is heat-treated, non-crystalline state zinc carbonate film can be obtained.
As another kind of preferred version, under room temperature, adopt Magnetron reactive sputtering, the metallic zinc of experiment employing 99.99% is as cathode target, and anode is connected with vacuum chamber.Be contained in substrate chuck by the substrate after ultrasonic cleaning, shifting board is placed between substrate chuck and target; Vacuumize after shutting each air valve, until vacuum tightness reaches 2 × more than 10-4Pa; Pass into appropriate argon gas; Regulate high threshold to required operating air pressure; Open direct supply build-up of luminance pre-sputtering number minute; Rotating substrate fixture, removes shifting board, starts deposit film.
By the metallic zinc film that deposited as in retort furnace, under air ambient, in 10 minutes, temperature is risen to 500 degree, film is heat-treated, non-crystalline state zinc carbonate film can be obtained.
As another kind of preferred version, under room temperature, adopt Magnetron reactive sputtering, the metallic zinc of experiment employing 99.99% is as cathode target, and anode is connected with vacuum chamber.Be contained in substrate chuck by the substrate after ultrasonic cleaning, shifting board is placed between substrate chuck and target; Vacuumize after shutting each air valve, until vacuum tightness reaches 2 × more than 10-4Pa; Pass into appropriate argon gas; Regulate high threshold to required operating air pressure; Open direct supply build-up of luminance pre-sputtering number minute; Rotating substrate fixture, removes shifting board, starts deposit film.
By the metallic zinc film that deposited as in retort furnace, under air ambient, in 20 minutes, temperature is risen to 600 degree, film is heat-treated, non-crystalline state zinc carbonate film can be obtained.
Beneficial effect: the invention provides a kind of method preparing non-crystalline state zinc carbonate film, not only preparation technology is simple, and cost is low, and realizes the adjustment of structural and optical properties of zinc-oxide film by thermal treatment temp and speed.Non-crystalline state zinc carbonate film of the present invention is a kind of brand-new photoelectric function thin films material preparation method designed based on transparent flexible electron device.
Accompanying drawing explanation
Fig. 1 is non-crystalline state zinc carbonate film preparation principle schematic;
Fig. 2 is the X-ray diffraction spectrogram of zinc-oxide film prepared by the present invention;
Fig. 3 is the optical transmittance graphic representation of zinc-oxide film prepared by the present invention.
Embodiment
The technique means realized to make the present invention, creation characteristic, reaching object and effect is easy to understand, setting forth the present invention further below in conjunction with accompanying drawing.
With reference to Fig. 1, Fig. 2 and Fig. 3, a kind of method preparing non-crystalline state zinc carbonate film, comprises a substrate, adopt substrate surface as stratum basale, plate one deck homogeneous metal zinc rete at stratum basale, metallic zinc film by thermal oxidative treatment, namely obtains zinc-oxide film in air ambient.The metallic zinc film prepared is placed in retort furnace, under air ambient, in 4-25 minute, temperature is risen to 400-600 degree Celsius, metallic zinc film is heat-treated, non-crystalline state zinc carbonate film can be obtained.The present invention can prepare non-crystalline state zinc carbonate film by regulating metallic zinc film thermal oxidation rate and temperature.Compared with prior art, advantage of the present invention and positively effect are: in air atmosphere, reach by the temperature and heat-up rate that regulate the thermooxidizing of metallic zinc the non-crystalline state and transparent object that realize zinc-oxide film, be widely used in the fields such as solar cell, flat-panel monitor, organic LED, low emissivity glass, transparent film transistor and flexible electronic device.
During thermal oxidative treatment, thermooxidizing heat-up rate is 4-25 minute.The oxidation temperature range of metallic zinc film is 400-600 degree Celsius.Substrate is quartz, glass, crystal or silicon chip.
Specific embodiment 1, under room temperature, adopts Magnetron reactive sputtering, and the metallic zinc of experiment employing 99.99% is as cathode target, and anode is connected with vacuum chamber.Be contained in substrate chuck by the substrate after ultrasonic cleaning, shifting board is placed between substrate chuck and target; Vacuumize after shutting each air valve, until vacuum tightness reaches 2 × more than 10-4Pa; Pass into appropriate argon gas; Regulate high threshold to required operating air pressure; Open direct supply build-up of luminance pre-sputtering number minute; Rotating substrate fixture, removes shifting board, starts deposit film.
The metallic zinc film deposited is placed in retort furnace, under air ambient, in 5 minutes, temperature is risen to 400 degree, film is heat-treated, non-crystalline state zinc carbonate film can be obtained.
Specific embodiment 2, under room temperature, adopts Magnetron reactive sputtering, and the metallic zinc of experiment employing 99.99% is as cathode target, and anode is connected with vacuum chamber.Be contained in substrate chuck by the substrate after ultrasonic cleaning, shifting board is placed between substrate chuck and target; Vacuumize after shutting each air valve, until vacuum tightness reaches 2 × more than 10-4Pa; Pass into appropriate argon gas; Regulate high threshold to required operating air pressure; Open direct supply build-up of luminance pre-sputtering number minute; Rotating substrate fixture, removes shifting board, starts deposit film.
By the metallic zinc film that deposited as in retort furnace, under air ambient, in 10 minutes, temperature is risen to 500 degree, film is heat-treated, non-crystalline state zinc carbonate film can be obtained.
Specific embodiment 3, under room temperature, adopts Magnetron reactive sputtering, and the metallic zinc of experiment employing 99.99% is as cathode target, and anode is connected with vacuum chamber.Be contained in substrate chuck by the substrate after ultrasonic cleaning, shifting board is placed between substrate chuck and target; Vacuumize after shutting each air valve, until vacuum tightness reaches 2 × more than 10-4Pa; Pass into appropriate argon gas; Regulate high threshold to required operating air pressure; Open direct supply build-up of luminance pre-sputtering number minute; Rotating substrate fixture, removes shifting board, starts deposit film.
By the metallic zinc film that deposited as in retort furnace, under air ambient, in 20 minutes, temperature is risen to 600 degree, film is heat-treated, non-crystalline state zinc carbonate film can be obtained.
More than show and describe ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (3)
1. prepare the method for non-crystalline state zinc carbonate film for one kind, comprise a substrate, described substrate is quartz or silicon chip, adopt substrate surface as stratum basale, plate one deck homogeneous metal zinc film at stratum basale, the metallic zinc film prepared is placed in retort furnace, under air ambient, thermal oxidative treatment is carried out to metallic zinc film, namely obtains non-crystalline state zinc carbonate film;
Concrete operations are as follows:
Under room temperature, adopt Magnetron reactive sputtering, the metallic zinc of experiment employing 99.99% is as cathode target, and anode is connected with vacuum chamber;
Be contained in substrate chuck by the substrate after ultrasonic cleaning, shifting board is placed between substrate chuck and target; Vacuumize after shutting each air valve, until vacuum tightness reaches 2 × 10
-4more than Pa;
Pass into appropriate argon gas;
Regulate high threshold to required operating air pressure;
Open direct supply build-up of luminance pre-sputtering number minute;
Rotating substrate fixture, removes shifting board, starts metal refining zinc film;
The metallic zinc film deposited is placed in retort furnace, under air ambient, in 5 minutes, temperature is risen to 400 degrees Celsius, thermal oxidative treatment is carried out to metallic zinc film, namely obtain non-crystalline state zinc carbonate film.
2. prepare the method for non-crystalline state zinc carbonate film for one kind, comprise a substrate, described substrate is quartz or silicon chip, adopt substrate surface as stratum basale, plate one deck homogeneous metal zinc film at stratum basale, the metallic zinc film prepared is placed in retort furnace, under air ambient, thermal oxidative treatment is carried out to metallic zinc film, namely obtains non-crystalline state zinc carbonate film;
Concrete operations are as follows:
Under room temperature, adopt Magnetron reactive sputtering, the metallic zinc of experiment employing 99.99% is as cathode target, and anode is connected with vacuum chamber;
Be contained in substrate chuck by the substrate after ultrasonic cleaning, shifting board is placed between substrate chuck and target;
Vacuumize after shutting each air valve, until vacuum tightness reaches 2 × 10
-4more than Pa;
Pass into appropriate argon gas;
Regulate high threshold to required operating air pressure;
Open direct supply build-up of luminance pre-sputtering number minute;
Rotating substrate fixture, removes shifting board, starts metal refining zinc film;
The metallic zinc film deposited is placed in retort furnace, under air ambient, in 10 minutes, temperature is risen to 500 degrees Celsius, metallic zinc film is heat-treated, namely obtain non-crystalline state zinc carbonate film.
3. prepare the method for non-crystalline state zinc carbonate film for one kind, comprise a substrate, described substrate is quartz or silicon chip, adopt substrate surface as stratum basale, plate one deck homogeneous metal zinc film at stratum basale, the metallic zinc film prepared is placed in retort furnace, under air ambient, thermal oxidative treatment is carried out to metallic zinc film, namely obtains non-crystalline state zinc carbonate film;
Concrete operations are as follows:
Under room temperature, adopt Magnetron reactive sputtering, the metallic zinc of experiment employing 99.99% is as cathode target, and anode is connected with vacuum chamber;
Be contained in substrate chuck by the substrate after ultrasonic cleaning, shifting board is placed between substrate chuck and target;
Vacuumize after shutting each air valve, until vacuum tightness reaches 2 × 10
-4more than Pa;
Pass into appropriate argon gas;
Regulate high threshold to required operating air pressure;
Open direct supply build-up of luminance pre-sputtering number minute;
Rotating substrate fixture, removes shifting board, starts metal refining zinc film;
The metallic zinc film deposited is placed in retort furnace, under air ambient, in 20 minutes, temperature is risen to 600 degrees Celsius, thermal oxidative treatment is carried out to metallic zinc film, namely obtain non-crystalline state zinc carbonate film.
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| CN201310092190.XA CN103147061B (en) | 2013-03-21 | 2013-03-21 | Method for preparing amorphous transparent zinc oxide film |
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| CN103343327A (en) * | 2013-07-01 | 2013-10-09 | 上海理工大学 | Method for preparing amorphous transparent zinc oxide film |
| CN110867382A (en) * | 2019-11-22 | 2020-03-06 | 广西民族大学 | Preparation method of zinc oxide film material with micro-nano structure |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101748366A (en) * | 2010-01-11 | 2010-06-23 | 国家纳米科学中心 | Ultra-fine grain metal membrane or ultra-fine grain alloy membrane and preparation method thereof |
| CN101805892A (en) * | 2010-04-02 | 2010-08-18 | 上海工程技术大学 | Method for preparing zinc oxide films |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101748366A (en) * | 2010-01-11 | 2010-06-23 | 国家纳米科学中心 | Ultra-fine grain metal membrane or ultra-fine grain alloy membrane and preparation method thereof |
| CN101805892A (en) * | 2010-04-02 | 2010-08-18 | 上海工程技术大学 | Method for preparing zinc oxide films |
Non-Patent Citations (3)
| Title |
|---|
| coating technology》.2004,第198卷319-323. * |
| Z.W.Li,etal..Zinc oxide films by thermal oxidation of zinc thin films.《Surface& * |
| 磁控溅射及直接氧化法制备氧化锌薄膜及其结构与性质;杨跃;《中国优秀硕士学位论文全文数据库 基础科学辑》;20111231(第14期);A005-222 * |
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