CN107267929A - A kind of ZnO high transmittance high conductivity method for manufacturing thin film based on electron beam evaporation technique - Google Patents
A kind of ZnO high transmittance high conductivity method for manufacturing thin film based on electron beam evaporation technique Download PDFInfo
- Publication number
- CN107267929A CN107267929A CN201710598810.5A CN201710598810A CN107267929A CN 107267929 A CN107267929 A CN 107267929A CN 201710598810 A CN201710598810 A CN 201710598810A CN 107267929 A CN107267929 A CN 107267929A
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- electron beam
- beam evaporation
- bell jar
- glass
- cleaning
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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
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
- C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
-
- 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
Abstract
The invention discloses a kind of ZnO high transmittance high conductivity method for manufacturing thin film based on electron beam evaporation technique, comprise the following steps：Zinc oxide particles are placed in mould and pressurizeed, after the block for being pressed into densification, takes out, is placed in corundum box, is put into after 24h in sintering furnace, at a certain temperature sinter molding target；Open machine target is put into copper crucible, the quartz glass after cleaning-drying is caught in slide glass dish, the bell jar of electron beam evaporation platform is evacuated, it is filled with hydrogen or nitrogen cleaning bell jar, heated quartz sheet glass, uses beam bombardment target, and control evaporation rate.Film obtained by the present invention has very high stability, light transmission rate and electrical conductivity, and the used prices of raw materials are extremely cheap, meet the high transmission rate of transparent conductive film, high conductance, cheap basic demand.
Description
Technical field
The present invention relates to field of material preparation, and in particular to a kind of ZnO high transmittances based on electron beam evaporation technique are high
Electrical conductivity method for manufacturing thin film.
Background technology
Zinc oxide (ZnO) transparent conductive film is in field of photoelectric devices, acousto-optical device and acousto-optic modulator field and army
Thing purposes etc. application above have been obtained for being widely applied, existing preparation method mainly have chemical method, Chemical Physics method and
Physical method；Film transmitance prepared by chemical method is relatively low, and the film conductivity obtained by the preparation of the method for magnetron sputtering is not high,
Its process of the zinc-oxide film of reaction evaporation preparation is difficult to control very much, and unstable.
The content of the invention
To solve the above problems, the invention provides a kind of high conductance of ZnO high transmittances based on electron beam evaporation technique
Rate method for manufacturing thin film.
To achieve the above object, the technical scheme taken of the present invention is：
A kind of ZnO high transmittance high conductivity method for manufacturing thin film based on electron beam evaporation technique, comprises the following steps：
S1, by Zinc oxide powder (particle) be placed in mould pressurize, be pressed into densification block after, take out, be placed in stone
In English or corundum box, it is put into after 24h in sintering furnace, at a certain temperature sinter molding；
S2, opening machine bell jar, target is put into copper crucible, the quartz glass after cleaning-drying is caught in into slide glass
Disk, the bell jar of electron beam evaporation platform is evacuated, and is filled with hydrogen or nitrogen cleaning bell jar, and heated quartz sheet glass uses electronics
Beam bombards target, and controls evaporation rate.
Preferably, the quartz glass completes to be cleaned and dried by following steps：
The glass of certain size is taken, after two sides is cleaned up with detergent, successively with running water, deionized water rinsing, from
It is placed on after so drying on stainless steel hanger, is cleaned by ultrasonic 5 minutes with acetone ultrasonic cleaning 5 minutes, absolute ethyl alcohol successively, gone
Ionized water is cleaned by ultrasonic twice, 5 minutes every time, and washed glass then is put into oven drying, stand-by.
Preferably, the step S1 specifically includes following steps：
S11, Zinc oxide particles are filled to a diameter of 2.5cm, deep 4cm mould is vibrated slightly, and a cleaning is poured into after filling
In container, a small amount of polyvinyl alcohol (- [CH2CH (OH)] n-) is added, mould is loaded after stirring, is then pressurizeed, works as pressure
Stop pressurization when 31MPa, obtain fine and close block；
S12, the fine and close block taking-up by gained, are put into corundum box and cover.Sample box is put into sintering after 24h
Heated in stove, flat-temperature zone temperature is 50 DEG C, 100 DEG C, 250 DEG C, 400 DEG C, 600 DEG C, 800 DEG C, 1000 DEG C, 1100 DEG C.
Preferably, the step S2 specifically includes following steps：
S21, the bell jar for opening electron beam evaporation platform, are caught in slide glass dish by the quartz glass after cleaning-drying, will prepare
Target be put into copper crucible, closed bell jar and locked opens mechanical pump and low vacuum valve, when vacuum reaches 10-1Pa's
When, low vacuum valve is closed, and hydrogen or nitrogen are filled with to 0.1MPa (cleaning bell jar) into bell jar；Low vacuum valve is opened, when
Vacuum reaches 10 again-1When Pa, the mechanical pump gas road control valve of switching to the system of taking out；Turbomolecular pump is opened, opens high
Vacuum valve, treats that vacuum reaches 4 × 10-4When Pa, start quartz glass heater and rotary drive mechanism, in quartzy glass
When glass temperature reaches 425 DEG C, and vacuum reaches 4 × 10 again-3When Pa, open filament power supply opens 6000 volts of high pressures,
Slow regulation filament voltage simultaneously observes the position that electron beam is beaten on target, while adjusting magnetic field changes landing of beam to suitable position
Put；
S22, opening THICKNESS GAUGE FOR THE MEASUREMENT OF THIN FOILS and baffle plate, observation calibrator indicate numerical value, when film thickness reaches certain thickness,
High pressure is closed, filament voltage is closed, is then shut off calibrator, heater, rotary drive mechanism, high vacuum valve, turbo-molecular
Pump and mechanical pump, take out after machine cooling, produce.
The invention has the advantages that：
Using the method for electron beam evaporation, the film of gained has very high stability, light transmission rate and electrical conductivity；Made
The prices of raw materials are extremely cheap, such as every gram of oxide powder and zinc is less than 0.1 yuan, if every gram of mass purchase is less than 0.01 yuan；
Therefore the transparent conductive film prepared with this technique has more price advantage.Quartz glass has extremely strong resisting temperature change energy
Power, the high grade of transparency for having wide spectrum, growing zinc oxide film is highly useful on this glass.
Brief description of the drawings
Fig. 1 is the heating-up time corresponding to each flat-temperature zone temperature in the embodiment of the present invention and constant temperature time schematic diagram.
Fig. 2 is the Transmissivity measurement curve in the embodiment of the present invention.
Embodiment
In order that objects and advantages of the present invention are more clearly understood, the present invention is carried out with reference to embodiments further
Describe in detail.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to limit this hair
It is bright.
Embodiment
The embodiments of the invention provide a kind of ZnO high transmittance high conductivity film preparations based on electron beam evaporation technique
Method, comprises the following steps：
S1, glass cleaning process
The glass of certain size is placed on the bracket of rinse bath, sponged down glass two with cleanser+liquid detergent
Face, after cleaning up, is rinsed with running water, then with deionized water rinsing and is spontaneously dried；Glass is placed on stainless steel hanger
On with acetone be cleaned by ultrasonic 5 minutes, then with absolute ethyl alcohol ultrasound 5 minutes；It is cleaned by ultrasonic twice with deionized water, 5 minutes every time.
Washed glass is put into oven drying stand-by.
S2, ZnO target material preparation technology
ZnO powder is filled into diameter 2.5cm, deep 4cm mould, and vibrated slightly.Poured into after filling in a cleaning container,
Add a small amount of polyvinyl alcohol (- [CH2CH (OH)] n-) and stir, mould is loaded after stirring, is then pressurizeed, works as pressure
Stop pressurization when 31MPa.The sample suppressed is taken out, is put into corundum box and covers.Sample box is put into after 24h
Heated in sintering furnace, take out stand-by after cooling.Flat-temperature zone temperature is 50 DEG C, 100 DEG C, 250 DEG C, 400 DEG C, 600 DEG C, 800 DEG C,
1000℃、1100℃；Their corresponding heating-up times and constant temperature time are as shown in Figure 1.
S3, zinc-oxide film preparation technology
The bell jar of electron beam evaporation platform is opened, the quartz glass after cleaning-drying slide glass dish is caught in, by the target prepared
Material is put into copper crucible, closed bell jar and locked, unlatching mechanical pump and low vacuum valve, when vacuum reaches 10-1When Pa,
Low vacuum valve is closed, and is filled with into bell jar hydrogen or nitrogen cleaning bell jar；Low vacuum valve is opened, when vacuum reaches again
10-1When Pa, the mechanical pump gas road control valve of switching to the system of taking out；Turbomolecular pump is opened, high vacuum valve is opened, treats vacuum
Reach 4 × 10-4When Pa, start heater and rotary drive mechanism, when sample temperature reaches 425 DEG C, vacuum is again
It is secondary to reach 4 × 10-3When Pa, open filament power supply opens 6000 volts of high pressures, and slow regulation filament voltage simultaneously observes electron beam
The position on target is beaten, while adjusting magnetic field changes landing of beam to correct position；THICKNESS GAUGE FOR THE MEASUREMENT OF THIN FOILS is opened, baffle plate is opened,
Observe calibrator and indicate numerical value, when film thickness reaches 100nm or so (or certain thickness), close high pressure, close filament
Voltage, closes calibrator, closes substrate glass heating power supply, closes rotary sample driving power supply；High vacuum valve is closed, whirlpool is closed
Molecular pump is taken turns, mechanical pump is closed.Sample is taken out after machine cooling, transmitance is measured, square resistance is measured, preparation is finished.Through
Rate experiment curv is shown in that its electrical conductivity of Fig. 2 is about 1 × 104In Siemens/rice, figure, start wavelength is 200.0nm, terminates wavelength and is
1100.0nm, scanning accuracy is 0.1nm, and slit width is 1.8nm.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (4)
1. a kind of ZnO high transmittance high conductivity method for manufacturing thin film based on electron beam evaporation technique, it is characterised in that including
Following steps：
S1, by Zinc oxide powder be placed in mould pressurize, be pressed into densification block after, take out, be placed in corundum box, 24h
After be put into sintering furnace, sinter molding at a certain temperature；
S2, opening machine, target is put into copper crucible, the quartz glass after cleaning-drying is caught in into slide glass dish, by electronics
The bell jar of beam evaporation platform is evacuated, and is filled with hydrogen or nitrogen cleaning bell jar, and heated quartz sheet glass uses beam bombardment target
Material, and control evaporation rate.
2. a kind of ZnO high transmittance high conductivity film preparation side based on electron beam evaporation technique as claimed in claim 1
Method, it is characterised in that the quartz glass completes to be cleaned and dried by following steps：
The glass of certain size is taken, after two sides is cleaned up with detergent, successively with running water, deionized water rinsing, is done naturally
It is placed on after dry on stainless steel hanger, is cleaned by ultrasonic 5 minutes, absolute ethyl alcohol ultrasonic cleaning 5 minutes, deionization with acetone successively
Water is cleaned by ultrasonic twice, 5 minutes every time, and washed glass then is put into oven drying, stand-by.
3. a kind of ZnO high transmittance high conductivity film preparation side based on electron beam evaporation technique as claimed in claim 1
Method, it is characterised in that the step S1 specifically includes following steps：
S11, Zinc oxide particles (powder) are filled to a diameter of 2.5cm, deep 4cm mould vibrates slightly, and it is clear to pour into one after filling
In clean container, a small amount of polyvinyl alcohol is added, mould is loaded after stirring, is then pressurizeed, is stopped when pressure is in 31MPa
Pressurization, obtains fine and close block；
S12, the fine and close block taking-up by gained, are put into quartz or corundum box and cover.Sample box is put into burning after 24h
Heated in freezing of a furnace, flat-temperature zone temperature is 50 DEG C, 100 DEG C, 250 DEG C, 400 DEG C, 600 DEG C, 800 DEG C, 1000 DEG C, 1100 DEG C.
4. a kind of ZnO high transmittance high conductivity film preparation side based on electron beam evaporation technique as claimed in claim 1
Method, it is characterised in that the step S2 specifically includes following steps：
S21, the bell jar for opening electron beam evaporation platform, are caught in slide glass dish, by the target prepared by the quartz glass after cleaning-drying
Material is put into copper crucible, closed bell jar door and locked, unlatching mechanical pump and low vacuum valve, when vacuum reaches 10-1Pa when
Wait, close low vacuum valve, and hydrogen or nitrogen are filled with to 0.1MPa (cleaning bell jar) into bell jar；Low vacuum valve is opened, is taken seriously
Reciprocal of duty cycle reaches 10 again-1When Pa, the mechanical pump gas road control valve of switching to the system of taking out；Open turbomolecular pump and high vacuum
Valve, treats that vacuum reaches 4 × 10-4When Pa, start lining heat and rotary drive mechanism, in the temperature of quartz glass plate
When degree reaches 425 DEG C, and vacuum reaches 4 × 10 again-3When Pa, open filament power supply opens 6000 volts of high pressures, slowly
Regulation filament voltage simultaneously observes the position that electron beam is beaten on target, while adjusting magnetic field changes landing of beam to suitable position
Put；
S22, opening THICKNESS GAUGE FOR THE MEASUREMENT OF THIN FOILS and baffle plate, observation calibrator indicate numerical value, when film thickness reaches certain thickness, close
High pressure, close filament voltage, be then shut off calibrator, heater, rotary drive mechanism, high vacuum valve, turbomolecular pump and
Mechanical pump, takes out after machine cooling, produces.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710598810.5A CN107267929A (en) | 2017-07-21 | 2017-07-21 | A kind of ZnO high transmittance high conductivity method for manufacturing thin film based on electron beam evaporation technique |
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| CN201710598810.5A CN107267929A (en) | 2017-07-21 | 2017-07-21 | A kind of ZnO high transmittance high conductivity method for manufacturing thin film based on electron beam evaporation technique |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108642444A (en) * | 2018-05-16 | 2018-10-12 | 太原理工大学 | A kind of preparation method of the zinc oxide of high transparency luminescence generated by light-polyethylene composite coating |
| CN115094388A (en) * | 2022-07-08 | 2022-09-23 | 广东信大科技有限公司 | Heating pipe coating method and rose gold pipe and gold pipe prepared by same |
| CN116102239A (en) * | 2022-12-30 | 2023-05-12 | 江苏弘扬石英制品有限公司 | Film coating process and preparation method of quartz large-caliber diffusion furnace tube for single crystal |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108642444A (en) * | 2018-05-16 | 2018-10-12 | 太原理工大学 | A kind of preparation method of the zinc oxide of high transparency luminescence generated by light-polyethylene composite coating |
| CN108642444B (en) * | 2018-05-16 | 2020-05-01 | 太原理工大学 | Preparation method of high-transparency photoluminescent zinc oxide-polyethylene composite coating |
| CN115094388A (en) * | 2022-07-08 | 2022-09-23 | 广东信大科技有限公司 | Heating pipe coating method and rose gold pipe and gold pipe prepared by same |
| CN115094388B (en) * | 2022-07-08 | 2024-02-09 | 广东信大科技有限公司 | Heating pipe coating method and rose gold pipe prepared by heating pipe coating method |
| CN116102239A (en) * | 2022-12-30 | 2023-05-12 | 江苏弘扬石英制品有限公司 | Film coating process and preparation method of quartz large-caliber diffusion furnace tube for single crystal |
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Application publication date: 20171020 |