CN103590011B - A kind of magnetron sputtering prepares the device and method of AZO nesa coating - Google Patents

A kind of magnetron sputtering prepares the device and method of AZO nesa coating Download PDF

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CN103590011B
CN103590011B CN201310548414.3A CN201310548414A CN103590011B CN 103590011 B CN103590011 B CN 103590011B CN 201310548414 A CN201310548414 A CN 201310548414A CN 103590011 B CN103590011 B CN 103590011B
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tungsten filament
azo
solenoid
nesa coating
magnetron sputtering
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CN103590011A (en
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彭寿
王芸
马立云
崔介东
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China Triumph International Engineering Co Ltd
Bengbu Glass Industry Design and Research Institute
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China Triumph International Engineering Co Ltd
Bengbu Glass Industry Design and Research Institute
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Abstract

The present invention discloses the device and method that a kind of magnetron sputtering prepares AZO nesa coating, change the incorporation way in magnetic field in magnetron sputtering technique, the magnetic field orthogonal with electric field is introduced by a solenoid, the tungsten filament of external heating power supply, potential power source is also provided with in solenoid, tungsten filament is connected with the negative pole of potential power source, and be connected to copper earth plate, make the current potential of tungsten filament be negative, and form electric field between the vacuum chamber of ground connection.The thermionic movement locus controlling tungsten filament transmitting is longer, thus more effectively carries out ionization by collision with argon molecules; The negative pole of external source of the stainless steel-based end, guarantees that the stainless steel-based end is negative potential, can reduce surface potential barrier, and utilize field to cause effect and produce more electronics and argon molecules is collided, the ionization level of argon gas brings up to 70 ~ 80%.

Description

A kind of magnetron sputtering prepares the device and method of AZO nesa coating
Technical field
The present invention relates to transparent conductive film preparing technical field, particularly a kind of device and method adopting AZO Thin Films Made by Magnetron Sputtering.
Background technology
In recent years, the transparent conductive film of zinc oxide (ZnO) base has attracted a lot of attentions, and typical purposes comprises, thin-film solar cells, flat pannel display, flexible electronic product etc.The doped element improving ZnO electroconductibility has many, but what mix aluminium is one of the most promising.The method can preparing aluminium-doped zinc oxide (AZO) film is a lot, comprises chemical Vapor deposition process (CVD), physical vaporous deposition (PVD), sol-gel method, spraying method etc.The merits and demerits of various method differs.Due to the success in preparing at electron devices such as semiconductor integrated circuit, magnetically controlled sputter method is hopeful one of the extensive industry production method for AZO most.So the AZO film prepared for magnetron sputtering both at home and abroad gives considerable concern.
The preparation method that ionization level is higher, electroconductibility and the transmitance of the AZO film of acquisition are better.And in existing magnetron sputtering technique, just going out electronics by emission of cathode, the ionization level of argon gas only has about 30%, relatively low, needs to improve further and improve to the utilization ratio of argon gas and the photoelectric properties of target bombardment effect and prepared AZO film.
Summary of the invention
For the problem that in existing magnetron sputtering technique, argon gas ionization level is lower, film forming photoelectric properties are to be improved, the object of the present invention is to provide a kind of device and method that can significantly improve argon gas ionization level, while realizing high speed deposition transparent conductive film, obtain excellent photoelectric properties.
The object of the invention is to be achieved by the following technical programs, a kind of magnetron sputtering prepares the device of AZO nesa coating, comprise vacuum chamber 1, gas flow controller 14, vacuum pump group 15, underboarding 4 is provided with in vacuum chamber 1, substrate heater 5, AZO target 8, the stainless steel-based end 9 and insulcrete 10, it is characterized in that, solenoid 2 is provided with in described vacuum chamber 1, the external coil power 3 of solenoid 2, described underboarding 4, AZO target 8, the stainless steel-based end 9 and insulcrete 10 are all arranged in described solenoid 2, external heating power supply 11 is also provided with in described solenoid 2, the tungsten filament 6 of potential power source 12, tungsten filament 6 is connected with the negative pole of potential power source 12, and be connected to copper earth plate 16, the current potential of tungsten filament 6 is made to be negative, and form electric field between the vacuum chamber 1 of ground connection.
Further, the described stainless steel-based end 9, connects the negative pole of substrate power supply 13 by wire and is connected with copper earth plate 16, and the current potential at the stainless steel-based end 9 is negative.
Further, be provided with tungsten filament support 7 in vacuum chamber 1, tungsten filament 6 is arranged on tungsten filament support 7.
Further, the number of turn of described solenoid is 50 ~ 80 circles.
Further, described tungsten filament is arranged at 3 ~ 5cm place above AZO target.
Utilize said apparatus to prepare the method for AZO nesa coating, it is characterized in that,
The composition mass ratio of AZO target is, ZnO:Al 2o 3=98%:2%, substrate heating temperature is 200 DEG C, is 200sccm by the flow of gas flow-control argon gas, utilizes vacuum pump Controlling Technology air pressure to be 5 ~ 10Pa;
The voltage of adjustment substrate power supply is 600 ~ 800V, makes the stainless steel-based end utilize field emission effect to produce electron emission around, and collision argon molecules makes it ionization, realizes glow discharge;
The voltage control regulating heating power supply is 20 ~ 30A by the electric current of tungsten filament; The voltage of adjustment coil power, controlling by the electric current of solenoid is 60 ~ 90A, and tungsten filament generates heat backward surrounding electron emission, constantly collides, ionize out argon ion with the argon molecules of operation interval;
Under above processing parameter condition, sputtering time 30 minutes, prepares AZO transparent conductive film, and its resistivity is 4.7 ~ 5.2 × 10 -4ohm. centimetre, the average transmittances in visible wavelength is 86.8%.
Compared with prior art, the present invention changes the incorporation way in magnetic field in magnetron sputtering technique, introduce the magnetic field orthogonal with electric field by a solenoid, the thermionic movement locus controlling tungsten filament transmitting is longer, thus more effectively carries out ionization by collision with argon molecules; The negative pole of external source of the stainless steel-based end, guarantee that the stainless steel-based end is negative potential, reduce surface potential barrier, utilize field to cause effect and produce more electronics and argon molecules is collided, the ionization level of argon gas brings up to 70 ~ 80%, adopt the present invention to deposit the AZO transparent conductive film obtained, resistivity is 4.7 ~ 5.2 ~ × 10 -4ohm. centimetre, the transmitance in visible wavelength is 86 ~ 88%, the AZO transparent conductive film that prior art is produced, and resistivity is 2 ~ 3 × 10 -4ohm. centimetre, the transmitance in visible wavelength is 84 ~ 86%.
accompanying drawing explanationfig. 1 is the device schematic diagram that the present invention proposes.
Embodiment
As shown in Figure 1, a kind of magnetron sputtering provided by the invention prepares the device of AZO nesa coating, comprise vacuum chamber 1, gas flow controller 14, vacuum pump group 15, underboarding 4 is provided with in vacuum chamber 1, substrate heater 5, AZO target 8, the stainless steel-based end 9 and insulcrete 10, solenoid 2 is also provided with in vacuum chamber 1, the external coil power 3 of solenoid 2, the number of turn of solenoid is 50 ~ 80 circles, underboarding 4, AZO target 8, the stainless steel-based end 9 and insulcrete 10 are all arranged in solenoid 2, tungsten filament 6 is also provided with in solenoid 2, tungsten filament is arranged at 3 ~ 5cm place above AZO target 8, the external heating power supply 11 of tungsten filament 6 and potential power source 12, tungsten filament 6 is connected with the negative pole of potential power source 12, and be connected to copper earth plate 16, the current potential of tungsten filament 6 is made to be negative, and form electric field between the vacuum chamber 1 of ground connection, to control the motion of tungsten filament electron emission.Be provided with tungsten filament support 7 in vacuum chamber 1, tungsten filament 6 is arranged on tungsten filament support 7, and the stainless steel-based end 9 connects the negative pole of substrate power supply 13 by wire and is connected with copper earth plate 16, makes the current potential at the stainless steel-based end 9 be negative.This device introduces the magnetic field orthogonal with electric field by solenoid, and the thermionic movement locus controlling tungsten filament transmitting is longer, more effectively carries out ionization by collision with argon molecules; Simultaneously the current potential at the stainless steel-based end be negative, utilizes field to cause effect generation electron emission, produces more electronics and argon molecules is collided, the ionization level of raising argon gas.
Provide the embodiment that the apparatus and method adopting the present invention to propose prepare AZO nesa coating below.
Embodiment 1:
The flow utilizing flow control system to control argon gas is 200sccm, vacuum pump group Controlling Technology air pressure is utilized to be 5Pa, the voltage of power supply of the stainless steel-based end 13 is 750V, control by the electric current of tungsten filament to be 25A by regulating the voltage swing of tungsten filament heating power supply 11, be 80A by the voltage control of regulating winding power supply 3 by the electric current of solenoid 2, the number of turn of solenoid 2 is 60 circles, and substrate heating temperature is 200 DEG C, and the composition of AZO target is: ZnO:Al 2o 3=98%:2%(wt.%).Under above processing parameter condition, sputtering time 30 minutes, prepares AZO film, and its resistivity is 5 × 10 -4ohm. centimetre, the average transmittances in visible wavelength is 86%.
Embodiment 2:
The flow utilizing flow control system to control argon gas is 200sccm, vacuum pump group Controlling Technology air pressure is utilized to be 10Pa, the voltage of power supply of the stainless steel-based end 13 is 800V, control by the electric current of tungsten filament to be 30A by regulating the voltage swing of tungsten filament heating power supply 11, be 90A by the voltage control of regulating winding power supply 3 by the electric current of solenoid 2, the number of turn of solenoid 2 is 70 circles, and substrate heating temperature is 200 DEG C, and the composition of AZO target is: ZnO:Al 2o 3=98%:2%(wt.%).Under above processing parameter condition, sputtering time 30 minutes, prepares AZO film, and its resistivity is 4.7 × 10 -4ohm. centimetre, the average transmittances in visible wavelength is 86.8%.
Embodiment 3:
The flow utilizing flow control system to control argon gas is 200sccm, vacuum pump group Controlling Technology air pressure is utilized to be 8Pa, the voltage of power supply of the stainless steel-based end 13 is 600V, control by the electric current of tungsten filament to be 20A by regulating the voltage swing of tungsten filament heating power supply 11, be 60A by the voltage control of regulating winding power supply 3 by the electric current of solenoid 2, the number of turn of solenoid 2 is 80 circles, and substrate heating temperature is 200 DEG C, and the composition of AZO target is: ZnO:Al 2o 3=98%:2% (wt.%).Under above processing parameter condition, sputtering time 30 minutes, prepares AZO film, and its resistivity is 4.7 × 10 -4ohm. centimetre, the average transmittances in visible wavelength is 87.5%.
The above is only preferred embodiment of the present invention, not does any pro forma restriction to the present invention; Any those of ordinary skill in the art, do not departing under technical solution of the present invention ambit, the Method and Technology content of above-mentioned announcement all can be utilized to make many possible variations and modification to technical solution of the present invention, or be revised as the Equivalent embodiments of equivalent variations.Therefore, every content not departing from technical solution of the present invention, according to technical spirit of the present invention to any simple modification made for any of the above embodiments, equivalent replacement, equivalence change and modification, all still belongs in the scope of technical solution of the present invention protection.

Claims (6)

1. a magnetron sputtering prepares the device of AZO nesa coating, comprise vacuum chamber (1), gas flow controller (14), vacuum pump group (15), underboarding (4) is provided with in vacuum chamber (1), substrate heater (5), AZO target (8), the stainless steel-based end (9) and insulcrete (10), it is characterized in that, solenoid (2) is provided with in described vacuum chamber (1), solenoid (2) external coil power (3), described underboarding (4), AZO target (8), the stainless steel-based end (9) and insulcrete (10) are all arranged in described solenoid (2), external heating power supply (11) is also provided with in described solenoid (2), the tungsten filament (6) of potential power source (12), tungsten filament (6) is connected with the negative pole of potential power source (12), and be connected to copper earth plate (16), the current potential of tungsten filament (6) is made to be negative, and the vacuum chamber of ground connection forms electric field between (1).
2. a kind of magnetron sputtering according to claim 1 prepares the device of AZO nesa coating, it is characterized in that, the described stainless steel-based end (9) connects the negative pole of substrate power supply (13) by wire and is connected with copper earth plate (16), and the current potential of the stainless steel-based end (9) is negative.
3. a kind of magnetron sputtering according to claim 1 prepares the device of AZO nesa coating, it is characterized in that, is provided with tungsten filament support (7) in vacuum chamber (1), and tungsten filament (6) is arranged on tungsten filament support (7).
4. a kind of magnetron sputtering according to claim 1 prepares the device of AZO nesa coating, it is characterized in that, the number of turn of described solenoid is 50 ~ 80 circles.
5. a kind of magnetron sputtering according to claim 1 prepares the device of AZO nesa coating, it is characterized in that, described tungsten filament is arranged at 3 ~ 5cm place above AZO target.
6. utilize the arbitrary described device of claim 1-5 to prepare the method for AZO nesa coating, it is characterized in that,
The composition mass ratio of AZO target is, ZnO:Al 2o 3=98%:2%, substrate heating temperature is 200 DEG C, is 200sccm by the flow of gas flow-control argon gas, utilizes vacuum pump Controlling Technology air pressure to be 5 ~ 10Pa;
The voltage of adjustment substrate power supply is 600 ~ 800V, makes the stainless steel-based end utilize field emission effect to produce electron emission around, and collision argon molecules makes it ionization, realizes glow discharge;
The voltage control regulating heating power supply is 20 ~ 30A by the electric current of tungsten filament; The voltage of adjustment coil power, controlling by the electric current of solenoid is 60 ~ 90A, and tungsten filament generates heat backward surrounding electron emission, constantly collides, ionize out argon ion with the argon molecules of operation interval;
Under above processing parameter condition, sputtering time 30 minutes, prepares AZO nesa coating, and its resistivity is 4.7 ~ 5.2 × 10 -4ohmcm, the average transmittances in visible wavelength is 86.8%.
CN201310548414.3A 2013-11-08 2013-11-08 A kind of magnetron sputtering prepares the device and method of AZO nesa coating Active CN103590011B (en)

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CN201850306U (en) * 2010-08-17 2011-06-01 中国人民解放军第四军医大学 Mini type plasma film coating device for stomatological department
CN102863156A (en) * 2012-09-21 2013-01-09 蚌埠玻璃工业设计研究院 Preparation method of textured AZO (aluminum-doped zinc oxide) transparent conductive film
CN203582960U (en) * 2013-11-08 2014-05-07 蚌埠玻璃工业设计研究院 Magnetron sputtering device for preparing AZO transparent conductive film

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