CN103643211A - Novel AZO thin film preparation deposition process - Google Patents
Novel AZO thin film preparation deposition process Download PDFInfo
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- CN103643211A CN103643211A CN201310590537.3A CN201310590537A CN103643211A CN 103643211 A CN103643211 A CN 103643211A CN 201310590537 A CN201310590537 A CN 201310590537A CN 103643211 A CN103643211 A CN 103643211A
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Abstract
The present invention relates to a novel AZO thin film preparation process, which can be used for preparation of thin film solar energy window layers and preparation of transparent conductive layers in the flat panel display industry, wherein an AZO ceramic target is subjected to magnetron sputtering, and is characterized in that Al2O3 content is 1-3 at%, the balance is ZnO, and Fe content is less than 10 ppm. According to the AZO thin film preparation process controlling a pulse duty cycle and a pulse frequency of a direct current pulse power supply, the forward direction peak height and the reverse direction peak height of the output pulse, and the continuous times of the forward direction square wave and the reverse direction square wave in a pulse generator are adjusted, the pulse frequency of the output pulse square wave is adjusted, the detected voltage change on the target surface and the detected air pressure change of the sputtering are adopted, and simulation calculation adjustment is performed, such that the whole sputtering AZO process is stable, the arcing phenomenon can be avoided, and sputtering thin film performance reduction caused by sputtering anode disappearance can be avoided so as to obtain the transparent conductive thin film AZO with characteristics of high sputtering rate, high transmittance, high conductivity, high density and high haze.
Description
Technical field
The invention belongs to plated film industry about transparent conductive film TCO field, specially refer to a kind of novel preparation AZO thin film deposition processes, belong to and prepare transparent conductive film field.
Background technology
Nesa coating ITO is the class being most widely used in all transparent conductive materials.The film of preparing due to this material not only has very high transmitance in visible region, infrared also very high with near-infrared region transmitance, and the resistivity of film is lower, therefore both can show the plane electrode material that (FPD) and sun power are used as plane, also can be used for energy-conservation aspect, as glass surface etc., also can be used for vehicle glass and microwave oven.In this class material, that be most widely used at present is indium tin oxide transparent conductive semiconductor film ITO.But one of main component indium metal is rare metal in ITO, and in its smelting process, can cause the pollution of environment, therefore, from the angle of Save Resource Protect Environment, should replace ito thin film by the high performance AZO film of widespread use.
AZO coated glass, the i.e. resulting ZnO:Al transparent conductive film glass of doped with Al in ZnO system.AZO film conductivity after doping can increase substantially, resistivity can be reduced to 10-4 Ω cm, and AZO film stability in hydrogen plasma is better than ITO, AZO has the photoelectric characteristic that can compare favourably with ITO simultaneously, and AZO film is easy to prepare, element resource is abundanter, and nontoxic, be the best replacer of ito thin film, AZO film has obtained certain applications in flat-panel monitor and thin-film solar cells at present.
Vacuum sputtering technology can, by controlling technological temperature and vacuum atmosphere, be prepared square resistance scope at the AZO of 3-12 ohm film.But, in order to realize good microcosmic nanostructure, distribute and higher mist degree, need to control the coating process of AZO coated glass, especially need strictly to control technological temperature and vacuum atmosphere, this causes the AZO coated glass cost produced higher, surface nano-structure distributing homogeneity is poor, and this is unfavorable for the application of follow-up battery, thus we need be extensively, stable coating process on practical, production line.
Therefore, the present invention has developed a kind of technique of direct current pulse power source dutycycle of the AZO of control sputter, has reduced and has needed the accurately strict defect of controlling process gas atmosphere and temperature, obtains that a kind of resistivity is low, high permeability, the film that compactness is high.
Summary of the invention
In view of problems of the prior art as mentioned above, the present invention is a kind of novel preparation technology who develops on existing AZO coating process, can be applicable to a large amount of large-area manufacture AZO films, below for the present invention, is elaborated:
The technique of a kind of novel preparation AZO film provided by the invention, it is characterized in that, adopt magnetron sputtering AZO ceramic target, control the pulse duty factor of direct current pulse power source and the technique that pulse-repetition is prepared AZO film, in regulating impulse producer, the pulse forward of output and reverse peak height and the time length of Direct/Reverse square wave, and the pulse-repetition of the pulse square wave of regulation output, and lodge voltage change and the sputtering technology pressure variation that detects target material surface, analog calculation regulates, make its whole sputter AZO process stabilizing, avoid beating arc phenomenon, obtain high permeability, the transparent conductive film AZO of high conductivity.
In a better embodiment of the present invention, described preparation AZO film, adopts magnetic control sputtering device, and this device comprises: transmission system, negative electrode, power supply, process gas, pump group, heating system, measuring system; For transparent conductive film AZO deposition equipment therefor.
In another better embodiment of the present invention, described sputtering technology flow process is first to use vacuum pump cavity to be evacuated to certain vacuum tightness, and base vacuum is evacuated to 5x10
-4below Pa, control moisture dividing potential drop lower than 4% of base vacuum, this need to use the metering facilitys such as high-low pressure vacuumometer in measuring system; Reuse transmission system substrate is sent to sputter cavity, below equipment, is furnished with driving motor, motor driven gear, gear driven belt, belt drives roller, roller relies on frictional force to drive substrate to transmit forward, in the process of transmission, heating system is started working, and can select the mode of resistance wire or infrared lamp to heat substrate, be heated to 100-300 ℃, but require the temperature homogeneity of whole substrate in ± 5 ℃; Secondly board transport, to sputter cavity, passes into Ar/O
2mix and Ar process gas, blending ratio is O
2: Ar is between 1%-20%, and adjusting process pressure is controlled between 0.1-1Pa; Finally by direct current pulse power source, power, by process gas ionization, then bombard AZO target and realize on target AZO deposition of material to the process of substrate.
In another better embodiment of the present invention, in described AZO ceramic target, Al in target
2o
3content between 1%-3%, other compositions are ZnO, wherein the content of Fe is lower than 10ppm.
In another better embodiment of the present invention, described target is the little target of plane, can is planar rectangular, rotating cylindrical target.
In another better embodiment of the present invention, described negative electrode is static magnetic field negative electrode or removable magnetic field cathode.
In another better embodiment of the present invention, described magnetic control sputtering device is various small-scale test type magnetic control board platforms, produces horizontal board or produce vertical board etc.
In another better embodiment of the present invention, described sputter ceramic target AZO, negative electrode adopts the negative electrode of high-intensity magnetic field, during magneticstrength between 600GS-1300GS.
In another better embodiment of the present invention, described magnetron sputtering ceramic target AZO, power acquisition direct current pulse power source used, dutycycle, the pulse-repetition of the pulse of power supply are adjustable, and variable range is between 10%-60%.Output waveform is square wave.
In another better embodiment of the present invention, the pulse duty factor of described control direct current pulse power source and pulse-repetition are prepared the technique of AZO film, in regulating impulse producer, the pulse forward of output and reverse peak height and the time length of Direct/Reverse square wave, and the pulse-repetition of the pulse square wave of regulation output, and lodge voltage change and the sputtering technology pressure variation that detects target material surface, analog calculation regulates.
In another better embodiment of the present invention, during described magnetron sputtering ceramic target AZO, Sputtering power density 50W/m-15KW/m.
In another better embodiment of the present invention, during described magnetron sputtering ceramic target AZO, the temperature of base plate heating is 100 ℃-300 ℃.
In another better embodiment of the present invention, described base plate heating, adopts infrared lamp type of heating or Resistant heating mode, and requires the temperature non of big area heated substrates to be less than ± 5 ℃.
In another better embodiment of the present invention, during described magnetron sputtering ceramic target AZO, sputtering target cardinal distance (target material surface is to the distance of substrate) is between 70-100mm.
In another better embodiment of the present invention, during described magnetron sputtering ceramic target AZO, the base vacuum of sputter need to be evacuated to 5x10
-4below Pa, control the dividing potential drop of moisture lower than 4% of base vacuum.
In another better embodiment of the present invention, described sputtering technology gas, adopts Ar and O
2, purity is all higher than 99.999%.General O2 adopts mixed gas, Ar/O
2mixed gas, blending ratio is O
2: Ar is between 1%-20%.Adopt the air pressure ratio that mixed gas is convenient to technique precisely to regulate.
In another better embodiment of the present invention, during described magnetron sputtering ceramic target AZO, sputtering technology pressure is controlled between 0.1-1Pa, wherein O
2content account between the 0.1%-5% of this vacuum tightness.
The technique of described a kind of novel preparation AZO film, is characterized in that, the thickness of described sputter AZO transparent conductive film is between 500nm-1.5 μ m.
In another better embodiment of the present invention, described magnetron sputtering ceramic target AZO, detecting voltage change and the sputtering technology pressure variation of target material surface, is by power supply self monitoring electric power output voltage variation and vacuum pressure measuring apparatus monitoring process atmospheric pressures, to change respectively.
Described vacuum pressure measuring apparatus, is characterized in that: described vacuum pressure measuring apparatus is ionization vacuum meter, resistance vacuum gauge, electric capacity vacuumometer.
Described analog calculation, it is characterized in that: according to the fluctuation of monitoring process pressure constantly of vacuum pressure measuring apparatus, in associating, monitor constantly electric power output voltage in the fluctuation of target material surface, by simulation calculation module, calculate, dutycycle and the frequency of pulse wave that regulates conversely the surge generator output of power supply, reaches sputtering technology stable.
Described substrate, is characterized in that: substrate adopts stainless steel, glass, polyimide (PI) etc., and its size does not limit.
The stability that AZO plated film preparation technology of the present invention has had, can prepare low square resistance, high permeability, high densification, higher mist degree, the AZO transparent conductive film being evenly distributed.
Accompanying drawing explanation
Accompanying drawing 2 is AZO condition of surface SEM figure of the embodiment of the present invention;
Accompanying drawing 3 is test patterns of the AZO film transmitance of the embodiment of the present invention.
Embodiment
Below in conjunction with drawings and Examples, the present invention is done to concrete explaination.
Its preparation process of a kind of novel preparation AZO film provided by the invention, comprising:
Adopt magnetron sputtering AZO ceramic target, control the pulse duty factor of direct current pulse power source and the technique that pulse-repetition is prepared AZO film, in regulating impulse producer, the pulse forward of output and reverse peak height and the time length of Direct/Reverse square wave, and the pulse-repetition of the pulse square wave of regulation output, and lodge voltage change and the sputtering technology pressure variation that detects target material surface, analog calculation regulates, and makes its whole sputter AZO process stabilizing, avoids the transparent conductive film AZO that beats arc phenomenon, obtain high permeability, high conductivity.As shown in fig. 1, wherein 1 is glass to its structure, and 2 is AZO film;
Described preparation AZO film, adopts magnetic control sputtering device, and this device comprises: transmission system, negative electrode, power supply, process gas, pump group, heating system, measuring system; For transparent conductive film AZO deposition equipment therefor.
Described sputtering technology flow process is first to use vacuum pump cavity to be evacuated to certain vacuum tightness, and base vacuum is evacuated to 5x10
-4below Pa, control moisture dividing potential drop lower than 4% of base vacuum, this need to use the metering facilitys such as high-low pressure vacuumometer in measuring system; Reuse transmission system substrate is sent to sputter cavity, below equipment, is furnished with driving motor, motor driven gear, gear driven belt, belt drives roller, roller relies on frictional force to drive substrate to transmit forward, in the process of transmission, heating system is started working, and can select the mode of resistance wire or infrared lamp to heat substrate, be heated to 100-300 ℃, but require the temperature homogeneity of whole substrate in ± 5 ℃; Secondly board transport, to sputter cavity, passes into Ar/O
2mix and Ar process gas, blending ratio is O
2: Ar is between 1%-20%, and adjusting process pressure is controlled between 0.1-1Pa; Finally by direct current pulse power source, power, by process gas ionization, then bombard AZO target and realize on target AZO deposition of material to the process of substrate.
In described AZO ceramic target, Al in target
2o
3content between 1%-3%, other compositions are ZnO, wherein the content of Fe is lower than 10ppm.
Described target is the little target of plane, can is planar rectangular, rotating cylindrical target.
Described negative electrode is static magnetic field negative electrode or removable magnetic field cathode.
Described magnetic control sputtering device is various small-scale test type magnetic control board platforms, produces horizontal board or produce vertical board etc.
Described sputter ceramic target AZO, negative electrode adopts the negative electrode of high-intensity magnetic field, during magneticstrength between 600GS-1300GS.
Described magnetron sputtering ceramic target AZO, power acquisition direct current pulse power source used, dutycycle, the pulse-repetition of the pulse of power supply are adjustable, and variable range is between 10%-60%.Output waveform is square wave.
The pulse duty factor of described control direct current pulse power source and pulse-repetition are prepared the technique of AZO film, in regulating impulse producer, the pulse forward of output and reverse peak height and the time length of Direct/Reverse square wave, and the pulse-repetition of the pulse square wave of regulation output, and lodge voltage change and the sputtering technology pressure variation that detects target material surface, analog calculation regulates.
During described magnetron sputtering ceramic target AZO, Sputtering power density 50W/m-15KW/m.
During described magnetron sputtering ceramic target AZO, the temperature of base plate heating is 100 ℃-300 ℃.
Described base plate heating, adopts infrared lamp type of heating or Resistant heating mode, and requires the temperature non of big area heated substrates to be less than ± 5 ℃.
During described magnetron sputtering ceramic target AZO, sputtering target cardinal distance (target material surface is to the distance of substrate) is between 70-100mm.
During described magnetron sputtering ceramic target AZO, the base vacuum of sputter need to be evacuated to 5x10
-4below Pa, control the dividing potential drop of moisture lower than 4% of base vacuum.
Described sputtering technology gas, adopts Ar and O
2, purity is all higher than 99.999%.General O2 adopts mixed gas, Ar/O
2mixed gas, blending ratio is O
2: Ar is between 1%-20%.Adopt the air pressure ratio that mixed gas is convenient to technique precisely to regulate.
During described magnetron sputtering ceramic target AZO, sputtering technology pressure is controlled between 0.1-1Pa, wherein O
2content account between the 0.1%-5% of this vacuum tightness.
The thickness of described sputter AZO transparent conductive film is between 500nm-1.5 μ m.
Described magnetron sputtering ceramic target AZO, voltage change and the sputtering technology pressure variation of detection target material surface, be by power supply self monitoring electric power output voltage variation and vacuum pressure measuring apparatus monitoring process atmospheric pressures, to change respectively.
Described vacuum pressure measuring apparatus is ionization vacuum meter, resistance vacuum gauge, electric capacity vacuumometer.
Described analog calculation, it is characterized in that: according to the fluctuation of monitoring process pressure constantly of vacuum pressure measuring apparatus, in associating, monitor constantly electric power output voltage in the fluctuation of target material surface, by simulation calculation module, calculate, dutycycle and the frequency of pulse wave that regulates conversely the surge generator output of power supply, reaches sputtering technology stable.
The sputter flow speed of substrate is between 0.2m/s-0.6m/s.
Described substrate, is characterized in that: substrate adopts stainless steel, glass, polyimide (PI) etc., and its size does not limit.
Case 3 is implemented: magnetron sputtering vacuum cavity base vacuum is evacuated to 5x10-4Pa, substrate adopts glass substrate, sputter transmission speed is 0.28m/s, passes into Ar:300sccm, O2:2sccm, adjusting process pressure is 0.40Pa, shielding power supply power is 7KW, and the Duty ratio control of pulse is at 23:2, and frequency is 200KHz, the Heating temperature of substrate is 205 degrees Celsius, and the thickness of sputter AZO film is between 800-820nm.
The test of employing spectrophotometer, test wavelength scope is between 350nm-1300nm, the transmitance of testing film and substrate.
Adopt four point probe testing film square resistance.
| Sample number into spectrum | Process pressure | Substrate temperature | Thicknesses of layers | | Square resistance | |
| 1 | 0.32 | 205℃ | 861nm | 97.2% | 3.1Ω/□ | |
| 2 | 0.36 | 202℃ | 853nm | 98.8% | 3.2Ω/□ | |
| 3 | 0.40 | 208℃ | 821nm | 98.6% | 3.0Ω/□ |
Above specific embodiments of the invention are described in detail, but this example is only as example, the present invention is not limited to specific embodiment described above, to those skilled in the art, any equivalent modifications that the present invention is carried out and alternative also all among category of the present invention, therefore,, not departing from the scope of the present invention done equalization conversion and revising, all should contain within the scope of the invention.
Claims (11)
1. the technique of a novel preparation AZO film, it is characterized in that, adopt magnetron sputtering AZO ceramic target, control the pulse duty factor of direct current pulse power source and the technique that pulse-repetition is prepared AZO film, in regulating impulse producer, the pulse forward of output and reverse peak height and the time length of Direct/Reverse square wave, and the pulse-repetition of the pulse square wave of regulation output, and by the voltage change and the sputtering technology pressure variation that detect target material surface, analog calculation regulates, make its whole sputter AZO process stabilizing, avoid beating arc phenomenon, obtain high permeability, the transparent conductive film AZO of high conductivity,
Described AZO ceramic target, is characterized in that: Al
2o
3content be between 1at%-3at%, surplus is ZnO, wherein the content of Fe is lower than 10ppm.
2. technique according to claim 2, is characterized in that: described AZO ceramic target is plane small circular, planar rectangular or rotating cylindrical target.
3. technique according to claim 1, is characterized in that: during described magnetron sputtering, negative electrode adopts the negative electrode of high-intensity magnetic field, and magneticstrength is between 600GS-1300GS.
4. technique according to claim 1, it is characterized in that: power acquisition direct current pulse power source during described magnetron sputtering, dutycycle, the pulse-repetition of the pulse of power supply are adjustable, and variable range is between 10%-60%, output waveform is square wave, and sputtering power is according to practical situation adjustment.
5. technique according to claim 1, is characterized in that: during described magnetron sputtering, target material surface to the distance of substrate between 70-100mm.
6. technique according to claim 1, is characterized in that: the base vacuum of sputter need to be evacuated to 5 * 10
-4below Pa, control the dividing potential drop of moisture lower than 4% of base vacuum, adopting Ar, O2 is process gas, and process pressure is controlled between 0.1-1Pa, and in its sputter cavity, the content of O2 accounts between the 0.1%-5% of this vacuum tightness.
7. technique according to claim 7, is characterized in that: described process gas adopts Ar and O
2or Ar/O2 and Ar sputter, its purity is all higher than 99.999%, described mixed gas Ar/O
2, refer to the gas cylinder gas of purchase or just these two kinds of gases mixed according to a certain percentage before technique is used gas, as a kind of gas, pass into technique sputter, blending ratio is O
2: Ar is between 1%-20%.
8. technique according to claim 1, is characterized in that: during described magnetron sputtering, the temperature of base plate heating is 100 ℃-300 ℃.
9. technique according to claim 9, is characterized in that: base plate heating mode is Resistant heating or infrared lamp optical radiation heating, requires the temperature homogeneity of heating to be ± 5 ℃.
10. technique according to claim 1, is characterized in that: the thickness of described transparent conductive film AZO is between 500nm-1.5 μ m.
11. techniques according to claim 1, is characterized in that: the voltage change of described detection target material surface and sputtering technology pressure variation are by power supply self monitoring electric power output voltage variation and vacuum pressure measuring apparatus monitoring process atmospheric pressures, to change respectively.
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| CN108950501A (en) * | 2018-07-15 | 2018-12-07 | 天津大学 | A kind of preparation method of high light transmission ZAO conductive film |
| CN112038481A (en) * | 2020-09-01 | 2020-12-04 | 武汉大学 | Heavy rare earth doped ZnO columnar crystal preferred orientation piezoelectric film material and preparation method thereof |
| CN115125488A (en) * | 2022-07-08 | 2022-09-30 | 成都市精鹰光电技术有限责任公司 | Thermosensitive film prepared based on frequency mixing pulse reaction magnetron sputtering |
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| CN112038481B (en) * | 2020-09-01 | 2023-09-22 | 武汉大学 | Heavy rare earth doped ZnO columnar crystal preferred orientation piezoelectric film material and preparation method thereof |
| CN115125488A (en) * | 2022-07-08 | 2022-09-30 | 成都市精鹰光电技术有限责任公司 | Thermosensitive film prepared based on frequency mixing pulse reaction magnetron sputtering |
| CN115125488B (en) * | 2022-07-08 | 2023-11-03 | 成都市精鹰光电技术有限责任公司 | Thermosensitive film prepared based on mixed pulse reaction magnetron sputtering |
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Application publication date: 20140319 |