CN103243299A - AZO-zinc halide bilayer conductive film and preparation method - Google Patents

AZO-zinc halide bilayer conductive film and preparation method Download PDF

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CN103243299A
CN103243299A CN2012100302144A CN201210030214A CN103243299A CN 103243299 A CN103243299 A CN 103243299A CN 2012100302144 A CN2012100302144 A CN 2012100302144A CN 201210030214 A CN201210030214 A CN 201210030214A CN 103243299 A CN103243299 A CN 103243299A
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zinc halide
ceramic target
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conducting film
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CN103243299B (en
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周明杰
王平
陈吉星
黄辉
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Abstract

The invention belongs to the field of conductive films, and discloses an AZO-zinc halide bilayer conductive film and a preparation method thereof. The bilayer conductive film includes an AZO layer and a zinc halide layer; wherein the AZO layer includes 80-97 wt% of ZnO and 3-20 wt% of SnO2; and the halogen in the zinc halide layer is selected from the group consisting of F, Cl and Br. According to the invention, a magnetron sputtering apparatus is used for preparing the AZO-zinc halide bilayer conductive film. The AZO-zinc halide bilayer conductive film has a visible light transmittance of 85-90% in the wavelength range of 450-790 nm, a square resistance range of 20-90 omega/square, and a surface work function of 5.5-6.1 eV.

Description

Double-deck conducting film of AZO-zinc halide and preparation method thereof
Technical field
The present invention relates to the conductive film field, relate in particular to double-deck conducting film of a kind of AZO-zinc halide and preparation method thereof.
Background technology
The transparent conductive film electrode is the basic component of organic electroluminescence device (OLED), and the quality of its performance directly affects the luminous efficiency of entire device.Wherein, oxygen zinc-aluminium (AZO) is the most frequently used transparent conductive film material, has higher visible light transmittance rate and low resistivity.But improve the luminous efficiency of device, require the transparent conductive film anode to have higher surface work function.And the work function of AZO generally has only 4.5eV, through also reaching 4.7～5.1eV after the processing such as UV optical radiation or ozone, (be typically 5.7～6.3eV) and also have bigger energy level difference distance with the HOMO energy level of general organic luminous layer, cause the increase of current carrier injection barrier, hindering the raising of luminous efficiency.
Can improve the surface work function of conductive film by the method for aftertreatment, but because more process cause cost higher, and the lower result of efficient.And by the method that work function usually improves in some unit of mixing, certain restriction is arranged again in film: can influence the conductivity of film in a large number because mix, mixing does not reach the purpose that work function improves on a small quantity again.
Summary of the invention
One of problem to be solved by this invention is to provide a kind of AZO-zinc halide that not only can improve the conductive film surface work function but also can reduce cost double-deck conducting film.
A kind of AZO-zinc halide (ZnR 2) double-deck conducting film, comprise AZO layer and zinc halide layer; Wherein, in the AZO layer, in the AZO layer, ZnO quality percentage composition is 90～99.5%, Al 2O 3The quality percentage composition be 0.5～10%; Zinc halide (ZnR 3) in, R is halogen, is selected from F, Cl or Br.
Described AZO-ZnR 2Double-deck conducting film, preferred, in the AZO layer, ZnO quality percentage composition is 97%, Al 2O 3The quality percentage composition be 3%;
Described AZO-ZnR 2Double-deck conducting film, the thickness of described AZO layer is 50～300nm, the thickness of zinc halide layer is 0.5～3nm; Preferably, the thickness of described AZO layer is 150nm, and the thickness of zinc halide layer is 1nm.
Two of problem to be solved by this invention is to provide above-mentioned AZO-ZnR 2The preparation method of double-deck conducting film, this preparation method's step is as follows:
S1, take by weighing ZnO and Al 2O 3Powder after evenly mixing, 900～1300 ℃ of following sintering processes, makes the AZO ceramic target; Wherein, in the AZO ceramic target, ZnO quality percentage composition is 80～97%, Al 2O 3The quality percentage composition be 3～20%; And
With ZnR 2Powder places 600～950 ℃ of following sintering processes, makes the zinc halide ceramic target; Wherein, ZnR 2In the powder, R is halogen, is selected from F, Cl or Br;
S2, with among the step S1 AZO ceramic target, zinc halide ceramic target and substrate pack in the vacuum cavity of magnetron sputtering film device, and the vacuum tightness of vacuum cavity is arranged on 1.0 * 10 -3Pa～1.0 * 10 -5Between the Pa;
S3, adjustment magnetron sputtering plating processing parameter is: basic target spacing is 45～95mm, and magnetron sputtering operating pressure 0.2～4Pa, the flow of argon gas working gas are 10～35sccm, and underlayer temperature is 250 ℃～750 ℃, and sputtering power is 30～150W; Wherein, basic target spacing is 45～95mm, just refers to the vertical range of substrate and one of them target, and another target just waits and finishes after first, and the position of adjusting to first target place again just;
S4, sputter coating handle: sputter AZO ceramic target at first, and at substrate surface deposition AZO layer; Then sputter zinc halide ceramic target deposits ZnR at the AZO laminar surface 2Layer; After sputter coating is finished dealing with, make AZO-ZnR 2Double-deck conducting film.
Described AZO-ZnR 2The preparation method of double-deck conducting film, preferred:
Among the described step S1, in the AZO ceramic target, ZnO quality percentage composition is 97%, Al 2O 3The quality percentage composition be 3%; The sintering temperature of described AZO ceramic target preparation is 1250 ℃, and the sintering temperature of described zinc halide ceramic target preparation is 750 ℃;
Among the described step S2, the vacuum tightness of vacuum cavity is arranged on 5.0 * 10 -4Pa;
Among the described step S3, described basic target spacing is 60mm; Described magnetron sputtering operating pressure is 2.0Pa; The flow of described argon gas working gas is 25sccm; Described underlayer temperature is 500 ℃, and described sputtering power is 100W;
Among the described step S4, the thickness of described AZO layer is 50～300nm, and the thickness of zinc halide layer is 0.5～3nm; More preferably, the thickness of described AZO layer is 150nm, and the thickness of zinc halide layer is 1nm.
AZO-ZnR of the present invention 2Double-deck conducting film, at 450～790nm wavelength region visible light transmissivity 85%～90%, square resistance scope 20～90 Ω/, surface work function 5.5～6.1eV; The double-deck conducting film of AZO-zinc halide of the present invention can keep excellent conducting performance, and the work function of film is significantly improved; Use this film as the anode of OLED, its luminous efficiency is significantly improved.
Adopt magnetron sputtering equipment to prepare AZO-ZnR 2Double-deck conducting film, its preparation technology is simple, be easy to control.
Description of drawings
The AZO-ZnF that Fig. 1 makes for embodiment 1 2The transmitted spectrum of double-deck conducting film sample.
Embodiment
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in further detail.
Substrate among following each embodiment all adopts glass.
Embodiment 1
1, select for use purity to be respectively 99.99% ZnO and Al 2O 3(wherein, the total mass number of ZnO is 194g to powder, Al 2O 3Total mass number be 6g), after evenly mixing, at 1250 ℃ of following sintering, naturally cooling obtains AZO ceramic target sample, it is that 50mm, thickness are the AZO ceramic target of 2mm that the ceramic target sample is cut into diameter; And
Select for use purity to be respectively 99.99% ZnF 2Powder 150g, at 750 ℃ of following sintering, naturally cooling obtains ZnF 2The ceramic target sample, it is that 50mm, thickness are the ZnF of 2mm that the ceramic target sample is cut into diameter 2Ceramic target;
2, with AZO, ZnF 2Ceramic target is packed in the vacuum cavity of magnetron sputtering film device;
3, carry out oxygen plasma treatment successively with acetone, dehydrated alcohol and deionized water ultrasonic cleaning glass substrate, and to it, put into the vacuum cavity of magnetron sputtering film device after finishing; Wherein, the basic target spacing of target and glass is set at 60mm;
4, with mechanical pump and molecular pump the vacuum tightness of the vacuum cavity of magnetron sputtering film device is extracted into 5.0 * 10 -4Pa;
5, adjust the magnetron sputtering plating processing parameter: argon gas working gas flow is 25sccm; The magnetron sputtering operating pressure is 2.0Pa; Underlayer temperature is 500 ℃, and sputtering power is 100W;
6, then carry out plated film: at first, sputter AZO ceramic target is the TIO conducting film of 150nm at the glass substrate surface deposit thickness; Then, sputter ZnF 2Ceramic target is the ZnF of 1nm at AZO laminar surface deposit thickness 2Layer; Obtain AZO ZnF at last 2Double-deck conducting film, this conducting film is transparence; The piece resistance range 20 Ω/ of this conducting film, surface work function are 6.0eV.
The AZO-ZnF that Fig. 1 makes for embodiment 1 2The transmitted spectrum of double-deck conducting film sample; The test of use ultraviolet-visible pectrophotometer, the test wavelength is 300～900nm; As can be known, film has good through performance at visible-range among Fig. 1, is outstanding transparent conductive film material.
Embodiment 2
1, select for use purity to be respectively 99.99% ZnO and Al 2O 3(wherein, the total mass number of ZnO is 180g to powder, Al 2O 3Total mass number be 20g), after evenly mixing, at 900 ℃ of following sintering, naturally cooling obtains AZO ceramic target sample, it is that 50mm, thickness are the AZO ceramic target of 2mm that the ceramic target sample is cut into diameter; And
Select for use purity to be respectively 99.99% ZnF 2Powder 150g, at 600 ℃ of following sintering, naturally cooling obtains ZnF 2The ceramic target sample, it is that 50mm, thickness are the ZnF of 2mm that the ceramic target sample is cut into diameter 2Ceramic target;
2, with AZO, ZnF 2Ceramic target is packed in the vacuum cavity of magnetron sputtering film device;
3, carry out oxygen plasma treatment successively with acetone, dehydrated alcohol and deionized water ultrasonic cleaning glass substrate, and to it, put into the vacuum cavity of magnetron sputtering film device after finishing; Wherein, the basic target spacing of target and glass is set at 45mm;
4, with mechanical pump and molecular pump the vacuum tightness of the vacuum cavity of magnetron sputtering film device is extracted into 1.0 * 10 -3Pa;
5, adjust the magnetron sputtering plating processing parameter: argon gas working gas flow is 10sccm; The magnetron sputtering operating pressure is 0.2Pa; Underlayer temperature is 250 ℃, and sputtering power is 150W;
6, then carry out plated film: at first, sputter AZO ceramic target is the TIO conducting film of 50mm at the glass substrate surface deposit thickness; Then, sputter ZnF 2Ceramic target is the ZnF of 3nm at AZO laminar surface deposit thickness 2Layer; Obtain AZO-ZnF at last 2Double-deck conducting film, this conducting film is transparence; The piece resistance range 90 Ω/ of this conducting film, surface work function are 6.1eV.
Embodiment 3
1, select for use purity to be respectively 99.99% ZnO and Al 2O 3(wherein, the total mass number of ZnO is 199g to powder, Al 2O 3Total mass number be 1g), after evenly mixing, at 1300 ℃ of following sintering, naturally cooling obtains AZO ceramic target sample, it is that 50mm, thickness are the AZO ceramic target of 2mm that the ceramic target sample is cut into diameter; And
Select for use purity to be respectively 99.99% ZnF 2Powder 150g, at 950 ℃ of following sintering, naturally cooling obtains ZnF 2The ceramic target sample, it is that 50mm, thickness are the ZnF of 2mm that the ceramic target sample is cut into diameter 2Ceramic target;
2, with AZO, ZnF 2Ceramic target is packed in the vacuum cavity of magnetron sputtering film device;
3, carry out oxygen plasma treatment successively with acetone, dehydrated alcohol and deionized water ultrasonic cleaning glass substrate, and to it, put into the vacuum cavity of magnetron sputtering film device after finishing; Wherein, the basic target spacing of target and glass is set at 95mm;
4, with mechanical pump and molecular pump the vacuum tightness of the vacuum cavity of magnetron sputtering film device is extracted into 1.0 * 10 -5Pa;
5, adjust the magnetron sputtering plating processing parameter: argon gas working gas flow is 35sccm; The magnetron sputtering operating pressure is 4.0Pa; Underlayer temperature is 750 ℃, and sputtering power is 30W;
6, then carry out plated film: at first, sputter AZO ceramic target is the TIO conducting film of 300mm at the glass substrate surface deposit thickness; Then, sputter ZnF 2Ceramic target is the ZnF of 0.5nm at AZO laminar surface deposit thickness 2Layer; Obtain AZO-ZnF at last 2Double-deck conducting film, this conducting film is transparence; The piece resistance range 20 Ω/ of this conducting film, surface work function are 5.5eV.
Embodiment 4
1, select for use purity to be respectively 99.99% ZnO and Al 2O 3(wherein, the total mass number of ZnO is 194g to powder, Al 2O 3Total mass number be 6g), after evenly mixing, at 1250 ℃ of following sintering, naturally cooling obtains AZO ceramic target sample, it is that 50mm, thickness are the AZO ceramic target of 2mm that the ceramic target sample is cut into diameter; And
Select for use purity to be respectively 99.99% ZnCl 2Powder 150g, at 750 ℃ of following sintering, naturally cooling obtains ZnCl 2The ceramic target sample, it is that 50mm, thickness are the ZnCl of 2mm that the ceramic target sample is cut into diameter 2Ceramic target;
2, with AZO, ZnCl 2Ceramic target is packed in the vacuum cavity of magnetron sputtering film device;
3, carry out oxygen plasma treatment successively with acetone, dehydrated alcohol and deionized water ultrasonic cleaning glass substrate, and to it, put into the vacuum cavity of magnetron sputtering film device after finishing; Wherein, the basic target spacing of target and glass is set at 60mm;
4, with mechanical pump and molecular pump the vacuum tightness of the vacuum cavity of magnetron sputtering film device is extracted into 5.0 * 10 -4Pa;
5, adjust the magnetron sputtering plating processing parameter: argon gas working gas flow is 25sccm; The magnetron sputtering operating pressure is 2.0Pa; Underlayer temperature is 500 ℃, and sputtering power is 100W;
6, then carry out plated film: at first, sputter AZO ceramic target is the TIO conducting film of 150nm at the glass substrate surface deposit thickness; Then, sputter ZnCl 2Ceramic target is the ZnCl of 1nm at AZO laminar surface deposit thickness 2Layer; Obtain AZO-ZnCl at last 2Double-deck conducting film, this conducting film is transparence; The piece resistance range 25 Ω/ of this conducting film, surface work function are 6.0eV.
Embodiment 5
1, select for use purity to be respectively 99.99% ZnO and Al 2O 3(wherein, the total mass number of ZnO is 180g to powder, Al 2O 3Total mass number be 20g), after evenly mixing, at 900 ℃ of following sintering, naturally cooling obtains AZO ceramic target sample, it is that 50mm, thickness are the AZO ceramic target of 2mm that the ceramic target sample is cut into diameter; And
Select for use purity to be respectively 99.99% ZnCl 2Powder 150g, at 600 ℃ of following sintering, naturally cooling obtains ZnCl 2The ceramic target sample, it is that 50mm, thickness are the ZnCl of 2mm that the ceramic target sample is cut into diameter 2Ceramic target;
2, with AZO, ZnCl 2Ceramic target is packed in the vacuum cavity of magnetron sputtering film device;
3, carry out oxygen plasma treatment successively with acetone, dehydrated alcohol and deionized water ultrasonic cleaning glass substrate, and to it, put into the vacuum cavity of magnetron sputtering film device after finishing; Wherein, the basic target spacing of target and glass is set at 45mm;
4, with mechanical pump and molecular pump the vacuum tightness of the vacuum cavity of magnetron sputtering film device is extracted into 1.0 * 10 -3Pa;
5, adjust the magnetron sputtering plating processing parameter: argon gas working gas flow is 10sccm; The magnetron sputtering operating pressure is 0.2Pa; Underlayer temperature is 250 ℃, and sputtering power is 150W;
6, then carry out plated film: at first, sputter AZO ceramic target is the TIO conducting film of 50mm at the glass substrate surface deposit thickness; Then, sputter ZnCl 2Ceramic target is the ZnCl of 3nm at AZO laminar surface deposit thickness 2Layer; Obtain AZO-ZnCl at last 2Double-deck conducting film, this conducting film is transparence; The piece resistance range 70 Ω/ of this conducting film, surface work function are 6.1eV.
Embodiment 6
1, select for use purity to be respectively 99.99% ZnO and Al 2O 3(wherein, the total mass number of ZnO is 199g to powder, Al 2O 3Total mass number be 1g), after evenly mixing, at 1300 ℃ of following sintering, naturally cooling obtains AZO ceramic target sample, it is that 50mm, thickness are the AZO ceramic target of 2mm that the ceramic target sample is cut into diameter; And
Select for use purity to be respectively 99.99% ZnCl 2Powder 150g, at 950 ℃ of following sintering, naturally cooling obtains ZnCl 2The ceramic target sample, it is that 50mm, thickness are the ZnCl of 2mm that the ceramic target sample is cut into diameter 2Ceramic target;
2, with AZO, ZnCl 2Ceramic target is packed in the vacuum cavity of magnetron sputtering film device;
3, carry out oxygen plasma treatment successively with acetone, dehydrated alcohol and deionized water ultrasonic cleaning glass substrate, and to it, put into the vacuum cavity of magnetron sputtering film device after finishing; Wherein, the basic target spacing of target and glass is set at 95mm;
4, with mechanical pump and molecular pump the vacuum tightness of the vacuum cavity of magnetron sputtering film device is extracted into 1.0 * 10 -5Pa;
5, adjust the magnetron sputtering plating processing parameter: argon gas working gas flow is 35sccm; The magnetron sputtering operating pressure is 4.0Pa; Underlayer temperature is 750 ℃, and sputtering power is 30W;
6, then carry out plated film: at first, sputter AZO ceramic target is the TIO conducting film of 300mm at the glass substrate surface deposit thickness; Then, sputter ZnCl 2Ceramic target is the ZnCl of 0.5nm at AZO laminar surface deposit thickness 2Layer; Obtain AZO-ZnCl at last 2Double-deck conducting film, this conducting film is transparence; The piece resistance range 20 Ω/ of this conducting film, surface work function are 5.6eV.
Embodiment 7
1, select for use purity to be respectively 99.99% ZnO and Al 2O 3(wherein, the total mass number of ZnO is 194g to powder, Al 2O 3Total mass number be 6g), after evenly mixing, at 1250 ℃ of following sintering, naturally cooling obtains AZO ceramic target sample, it is that 50mm, thickness are the AZO ceramic target of 2mm that the ceramic target sample is cut into diameter; And
Select for use purity to be respectively 99.99% ZnBr 2Powder 150g, at 750 ℃ of following sintering, naturally cooling obtains ZnBr 2The ceramic target sample, it is that 50mm, thickness are the ZnBr of 2mm that the ceramic target sample is cut into diameter 2Ceramic target;
2, with AZO, ZnBr 2Ceramic target is packed in the vacuum cavity of magnetron sputtering film device;
3, carry out oxygen plasma treatment successively with acetone, dehydrated alcohol and deionized water ultrasonic cleaning glass substrate, and to it, put into the vacuum cavity of magnetron sputtering film device after finishing; Wherein, the basic target spacing of target and glass is set at 60mm;
4, with mechanical pump and molecular pump the vacuum tightness of the vacuum cavity of magnetron sputtering film device is extracted into 5.0 * 10 -4Pa;
5, adjust the magnetron sputtering plating processing parameter: argon gas working gas flow is 25sccm; The magnetron sputtering operating pressure is 2.0Pa; Underlayer temperature is 500 ℃, and sputtering power is 100W;
6, then carry out plated film: at first, sputter AZO ceramic target is the TIO conducting film of 150nm at the glass substrate surface deposit thickness; Then, sputter ZnBr 2Ceramic target is the ZnBr of 1nm at AZO laminar surface deposit thickness 2Layer; Obtain AZO-ZnBr at last 2Double-deck conducting film, this conducting film is transparence; The piece resistance range 25 Ω/ of this conducting film, surface work function are 5.9eV.
Embodiment 8
1, select for use purity to be respectively 99.99% ZnO and Al 2O 3(wherein, the total mass number of ZnO is 180g to powder, Al 2O 3Total mass number be 20g), after evenly mixing, at 900 ℃ of following sintering, naturally cooling obtains AZO ceramic target sample, it is that 50mm, thickness are the AZO ceramic target of 2mm that the ceramic target sample is cut into diameter; And
Select for use purity to be respectively 99.99% ZnBr 2Powder 150g, at 600 ℃ of following sintering, naturally cooling obtains ZnBr 2The ceramic target sample, it is that 50mm, thickness are the ZnBr of 2mm that the ceramic target sample is cut into diameter 2Ceramic target;
2, with AZO, ZnBr 2Ceramic target is packed in the vacuum cavity of magnetron sputtering film device;
3, carry out oxygen plasma treatment successively with acetone, dehydrated alcohol and deionized water ultrasonic cleaning glass substrate, and to it, put into the vacuum cavity of magnetron sputtering film device after finishing; Wherein, the basic target spacing of target and glass is set at 45mm;
4, with mechanical pump and molecular pump the vacuum tightness of the vacuum cavity of magnetron sputtering film device is extracted into 1.0 * 10 -3Pa;
5, adjust the magnetron sputtering plating processing parameter: argon gas working gas flow is 10sccm; The magnetron sputtering operating pressure is 0.2Pa; Underlayer temperature is 250 ℃, and sputtering power is 150W;
6, then carry out plated film: at first, sputter AZO ceramic target is the TIO conducting film of 50mm at the glass substrate surface deposit thickness; Then, sputter ZnBr 23Ceramic target is the ZnBr of 3nm at AZO laminar surface deposit thickness 2Layer; Obtain AZO-ZnBr at last 2Double-deck conducting film, this conducting film is transparence; The piece resistance range 88 Ω/ of this conducting film, surface work function are 6.0eV.
Embodiment 9
1, select for use purity to be respectively 99.99% ZnO and Al 2O 3(wherein, the total mass number of ZnO is 199g to powder, Al 2O 3Total mass number be 1g), after evenly mixing, at 1300 ℃ of following sintering, naturally cooling obtains AZO ceramic target sample, it is that 50mm, thickness are the AZO ceramic target of 2mm that the ceramic target sample is cut into diameter; And
Select for use purity to be respectively 99.99% ZnBr 2Powder 150g, at 950 ℃ of following sintering, naturally cooling obtains ZnBr 2The ceramic target sample, it is that 50mm, thickness are the ZnBr of 2mm that the ceramic target sample is cut into diameter 2Ceramic target;
2, with AZO, ZnBr 2Ceramic target is packed in the vacuum cavity of magnetron sputtering film device;
3, carry out oxygen plasma treatment successively with acetone, dehydrated alcohol and deionized water ultrasonic cleaning glass substrate, and to it, put into the vacuum cavity of magnetron sputtering film device after finishing; Wherein, the basic target spacing of target and glass is set at 95mm;
4, with mechanical pump and molecular pump the vacuum tightness of the vacuum cavity of magnetron sputtering film device is extracted into 1.0 * 10 -5Pa;
5, adjust the magnetron sputtering plating processing parameter: argon gas working gas flow is 35sccm; The magnetron sputtering operating pressure is 4.0Pa; Underlayer temperature is 750 ℃, and sputtering power is 30W;
6, then carry out plated film: at first, sputter AZO ceramic target is the TIO conducting film of 300mm at the glass substrate surface deposit thickness; Then, sputter ZnBr 2Ceramic target is the ZnBr of 0.5nm at AZO laminar surface deposit thickness 2Layer; Obtain AZO-ZnBr at last 2Double-deck conducting film, this conducting film is transparence; The piece resistance range 20 Ω/ of this conducting film, surface work function are 5.8eV.
Should be understood that above-mentioned statement at preferred embodiment of the present invention is comparatively detailed, can not therefore think the restriction to scope of patent protection of the present invention, scope of patent protection of the present invention should be as the criterion with claims.

Claims (10)

1. the double-deck conducting film of AZO-zinc halide is characterized in that this bilayer conducting film comprises AZO layer and zinc halide layer; Wherein, in the AZO layer, ZnO quality percentage composition is 90～99.5%, Al 2O 3The quality percentage composition be 0.5～10%; Halogen in the zinc halide is selected from F, Cl or Br.
2. the double-deck conducting film of AZO-zinc halide according to claim 1 is characterized in that in the AZO layer, ZnO quality percentage composition is 97%, Al 2O 3The quality percentage composition be 3%.
3. the double-deck conducting film of AZO-zinc halide according to claim 1 and 2 is characterized in that the thickness of described AZO layer is 50～300nm, and the thickness of zinc halide layer is 0.5～3nm.
4. the double-deck conducting film of AZO-zinc halide according to claim 3 is characterized in that the thickness of described AZO layer is 150nm, and the thickness of zinc halide layer is 1nm.
5. the preparation method of the double-deck conducting film of an AZO-zinc halide is characterized in that this preparation method's step is as follows:
S1, take by weighing ZnO and Al 2O 3Powder after evenly mixing, 900～1300 ℃ of following sintering processes, makes the AZO ceramic target; Wherein, in the AZO ceramic target, ZnO quality percentage composition is 80～97%, Al 2O 3The quality percentage composition be 3～20%; And
The zinc halide powder is placed 600～950 ℃ of following sintering processes, make the zinc halide ceramic target; Wherein, the halogen in the zinc halide is selected from F, Cl or Br;
S2, with among the step S1 AZO ceramic target, zinc halide ceramic target and substrate pack in the vacuum cavity of magnetron sputtering film device, and the vacuum tightness of vacuum cavity is arranged on 1.0 * 10 -3Pa～1.0 * 10 -5Between the Pa;
S3, adjustment magnetron sputtering plating processing parameter is: basic target spacing is 45～95mm, and magnetron sputtering operating pressure 0.2～4Pa, the flow of argon gas working gas are 10～35sccm, and underlayer temperature is 250 ℃～750 ℃, and sputtering power is 30～150W;
S4, sputter coating handle: sputter AZO ceramic target at first, and at substrate surface deposition AZO layer; Then sputter zinc halide ceramic target deposits the zinc halide layer at the AZO laminar surface; After sputter coating is finished dealing with, make the double-deck conducting film of AZO-zinc halide.
6. the preparation method of the double-deck conducting film of AZO-zinc halide according to claim 5 is characterized in that among the described step S1, in the AZO ceramic target, ZnO quality percentage composition is 97%, Al 2O 3The quality percentage composition be 3%; The sintering temperature of described AZO ceramic target preparation is 1250 ℃, and the sintering temperature of described zinc halide ceramic target preparation is 750 ℃.
7. the preparation method of the double-deck conducting film of AZO-zinc halide according to claim 5 is characterized in that among the described step S2, the vacuum tightness of vacuum cavity is arranged on 5.0 * 10 -4Pa.
8. the preparation method of the double-deck conducting film of AZO-zinc halide according to claim 5 is characterized in that among the described step S3, described basic target spacing is 60mm; Described magnetron sputtering operating pressure is 2.0Pa; The flow of described argon gas working gas is 25sccm; Described underlayer temperature is 500 ℃, and described sputtering power is 100W.
9. the preparation method of the double-deck conducting film of AZO-zinc halide according to claim 5 is characterized in that among the described step S4, the thickness of described AZO layer is 50～300nm, and the thickness of zinc halide layer is 0.5～3nm.
10. the preparation method of the double-deck conducting film of AZO-zinc halide according to claim 9 is characterized in that among the described step S4, the thickness of described AZO layer is 150nm, and the thickness of zinc halide layer is 1nm.
CN201210030214.4A 2012-02-10 2012-02-10 AZO-zinc halide bilayer conductive film and preparation method thereof Expired - Fee Related CN103243299B (en)

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KR100859148B1 (en) * 2007-03-23 2008-09-19 희성금속 주식회사 High flatness transparent conductive thin films and its manufacturing method
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