CN107611188A - A kind of multilayer film transparent conducting glass preparation method with micro-structural - Google Patents
A kind of multilayer film transparent conducting glass preparation method with micro-structural Download PDFInfo
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- CN107611188A CN107611188A CN201710796298.5A CN201710796298A CN107611188A CN 107611188 A CN107611188 A CN 107611188A CN 201710796298 A CN201710796298 A CN 201710796298A CN 107611188 A CN107611188 A CN 107611188A
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- based film
- polystyrene sphere
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The present invention discloses a kind of multilayer film transparent conducting glass preparation method with micro-structural, comprises the following steps:S1, the zno-based film in the case where glass substrate surface sputters growth at room temperature;S2, using bar knife coating, prepare the polystyrene sphere mask layer of the discrete distribution of individual layer in lower zno-based film surface;S3, using rf magnetron sputtering technique, by the use of polystyrene sphere mask layer as mask, zno-based film in growth is sputtered at room temperature in lower zno-based film surface;The thickness of upper zno-based film is less than the diameter of polystyrene sphere;S4, pass through ethanol immersion treatment, remove the zno-based film above polystyrene sphere mask layer and polystyrene sphere mask layer, zno-based film surface is formed the ball hole of one group of discrete distribution, obtain the multilayer film transparent conducting glass that surface is in concavo-convex textured structure;This method can obtain high transmittance, low-resistance transparent conducting glass, and its surface micro-structure is controllable.
Description
Technical field
The present invention relates to transparent conducting glass preparing technical field, specifically a kind of multilayer film with micro-structural is transparent to lead
Electric method for glass preparation.
Background technology
Transparent conducting glass due to have concurrently the transparency and electric conductivity, and possess raw material be easy to get, be environment-friendly, chemically stable
The advantages that property is good, therefore in many fields, such as photoelectron detector, photovoltaic device, film(Photoelectricity)Transistor, liquid crystal display,
The all existing important application prospect of sensor, heat reflector etc..
And be a kind of high transmittance, low-resistivity functional glass with fine surface micro-structural photoelectric glass, it is that one kind can
Hope and obtain the novel inorganic nonmetallic materials of important application in thin-film solar cells, environment conscious material etc..
In the application of the window layer material of thin-film solar cells, compared to traditional zno-based photoelectric functional glass, have
Micro-structural zno-based photoelectric functional glass has higher transmitance and bigger mist degree, by increasing the sunken light ability of Window layer,
Light path of the sunshine in Window layer can be extended, so as to improve absorption of the device to sunshine, to improving its light conversion efficiency and steady
It is qualitative to play key effect.
The content of the invention
It is an object of the invention to provide a kind of multilayer film transparent conducting glass preparation method with micro-structural, this method
High transmittance, low-resistance transparent conducting glass can be obtained, and its surface micro-structure is controllable.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of multilayer film transparent conducting glass preparation method with micro-structural, comprises the following steps:
S1, using rf magnetron sputtering technique, the zno-based film in the case where glass substrate surface sputters growth at room temperature;
S2, using bar knife coating, prepare the polystyrene sphere mask layer of the discrete distribution of individual layer in lower zno-based film surface;
S3, using rf magnetron sputtering technique, by the use of polystyrene sphere mask layer as mask, in lower zno-based film surface
The upper zno-based film of sputtering growth at room temperature;The thickness of upper zno-based film is less than the diameter of polystyrene sphere;
S4, by ethanol immersion treatment, remove the ZnO above polystyrene sphere mask layer and polystyrene sphere mask layer
Base film, zno-based film surface is formed the ball hole of one group of discrete distribution, obtain the multilayer that surface is in concavo-convex textured structure
Film transparent conducting glass.
Further, the step S1 uses zno-based ceramic target, using Ar ions as sputter gas, radio-frequency power supply
Act on negative electrode, radio-frequency power supply sputtering power is 150~250W, operating pressure 0.2Pa, and target voltage is 62~87V, glass lined
The spacing of bottom and target is 70mm, and the thickness for obtaining lower zno-based film is 600 ± 50nm.
Further, the concentration of polystyrene sphere mask layer is 0.1~0.5%wt in the step S2, and polystyrene is small
Bulb diameter is 300~1000nm.
Further, the step S3 uses zno-based ceramic target, using Ar ions as sputter gas, radio-frequency power supply
Act on negative electrode, radio-frequency power supply sputtering power is 150~250W, operating pressure 0.2Pa, and target voltage is 62~87V, glass lined
The spacing of bottom and target is 70mm, and the thickness for obtaining zno-based film is 200 ± 50nm.
Further, the glass substrate for preparing upper zno-based film is immersed ethanol immersion by the step S4 at room temperature
Handle, the zno-based film above polystyrene sphere mask layer and polystyrene sphere mask layer.
The beneficial effects of the invention are as follows:Using rf magnetron sputtering technique, plasma density, film can be effectively improved
Photoelectric properties are more preferable;Using the polystyrene sphere of the discrete distribution of individual layer as micro-structural mask, polystyrene sphere is as micro-
The mask of structure can be adjusted to its diameter, concentration as needed so that the surface micro-structure of zno-based film is controllable, simultaneously
The mist degree of zno-based film is adjusted, obtaining surface has micro-structural, high transmittance, the multilayer film transparent conducting glass of low-resistivity.
Brief description of the drawings
The present invention is further described with reference to the accompanying drawings and examples:
Fig. 1 is step S1 of the present invention schematic diagram;
Fig. 2 is step S2 of the present invention schematic diagram;
Fig. 3 is step S3 of the present invention schematic diagram;
Fig. 4 is step S4 of the present invention schematic diagram.
Embodiment
Embodiment one
The present invention provides a kind of multilayer film transparent conducting glass preparation method with micro-structural, comprises the following steps:
S1, as shown in figure 1, using rf magnetron sputtering technique, zno-based is thin under sputtering growth at room temperature on the surface of glass substrate 1
Film 2;
Specially:Soda-lime-silica glass using thickness as 1.1mm is glass substrate 1, and glass substrate 1 is placed in into magnetron sputtering chamber
Interior, using zno-based ceramic target, the Ar gas for being passed through 30sccm keeps room temperature as sputter gas, preparation temperature;Zno-based ceramics
The spacing of target and glass substrate is preferably 70mm;
During magnetron sputtering, negative electrode is acted on using radio-frequency power supply, radio-frequency power supply sputtering power is 200W, target voltage 80V, is worked
Pressure is 0.2Pa;Pre-sputtering is first carried out to glass substrate, sputtering time 20min, it is 600nm's that then sputtering, which grows thickness,
Lower zno-based film 2;
S2, with reference to shown in Fig. 2, using bar knife coating, the polyphenyl second of the discrete distribution of individual layer is prepared on the lower surface of zno-based film 2
Alkene bead mask layer 3;
Specially:Using bar is scratched, using 0.5% wt polystyrene sphere solution as blade coating solution, the μ of bar thickness specification 20
M, obtain polystyrene sphere mask layer by layer 3, polystyrene sphere diameter 300nm;
S3, with reference to shown in Fig. 3, using rf magnetron sputtering technique, by the use of polystyrene sphere mask layer 3 as mask, under
The surface of zno-based film 2 sputters the upper zno-based film 4 of growth at room temperature;The thickness of upper zno-based film 4 is less than polystyrene sphere
Diameter;
Specially:Negative electrode is acted on using radio-frequency power supply, radio-frequency power supply sputtering power is 150W, target voltage 62V, operating pressure
For 0.2Pa;Pre-sputtering, sputtering time 8min are first carried out, then sputtering grows the upper zno-based film 4 that thickness is 200nm;
S4, with reference to shown in Fig. 4, by ethanol immersion treatment, remove polystyrene sphere mask layer 3 and polystyrene sphere covered
Zno-based film above film layer, the surface of zno-based film 4 is formed the ball hole 5 of one group of discrete distribution, obtain surface in bumps
The multilayer film transparent conducting glass of textured structure.
Specially:The glass substrate for preparing upper zno-based film is immersed to the ethanol immersion treatment of 95% concentration at room temperature
180 minutes.
The multilayer film transparent conducting glass that the present embodiment is obtained carries out thickness test, mist degree test, transmitance survey respectively
Examination, resistivity measurement and XRD are tested, and thickness be 600~800nm, mist degree 12.1%, it is seen that and light mean transmissivity is 87.9%,
Resistivity is 1.6*10-3Ω cm, XRD spectrum show that zno-based film occurs weaker diffraction maximum in 2 θ=34.4 °, and corresponding hexagonal is fine
Zinc ore ZnO structures(002)Diffraction maximum.
Embodiment two
The present invention provides a kind of multilayer film transparent conducting glass preparation method with micro-structural, comprises the following steps:
S1, as shown in figure 1, using rf magnetron sputtering technique, zno-based is thin under sputtering growth at room temperature on the surface of glass substrate 1
Film 2;
Specially:Soda-lime-silica glass using thickness as 1.1mm is glass substrate 1, and glass substrate 1 is placed in into magnetron sputtering chamber
Interior, using zno-based ceramic target, the Ar gas for being passed through 30sccm keeps room temperature as sputter gas, preparation temperature;Zno-based ceramics
The spacing of target and substrate is preferably 70mm;
During magnetron sputtering, negative electrode is acted on using radio-frequency power supply, radio-frequency power supply sputtering power is 250W, target voltage 87V, is worked
Pressure is 0.2Pa;Pre-sputtering is first carried out to glass substrate, sputtering time 15min, it is 600nm's that then sputtering, which grows thickness,
Lower zno-based film 2;
S2, with reference to shown in Fig. 2, using bar knife coating, the polyphenyl second of the discrete distribution of individual layer is prepared on the lower surface of zno-based film 2
Alkene bead mask layer 3;
Specially:Using bar is scratched, using 0.5% wt polystyrene sphere solution as blade coating solution, the μ of bar thickness specification 20
M, obtain polystyrene sphere mask layer by layer 3, polystyrene sphere diameter 500nm;
S3, with reference to shown in Fig. 3, using rf magnetron sputtering technique, by the use of polystyrene sphere mask layer 3 as mask, under
The surface of zno-based film 2 sputters the upper zno-based film 4 of growth at room temperature;The thickness of upper zno-based film 4 is less than polystyrene sphere
Diameter;
Specially:Negative electrode is acted on using radio-frequency power supply, radio-frequency power supply sputtering power is 250W, target voltage 87V, operating pressure
For 0.2Pa;Pre-sputtering, sputtering time 5min are first carried out, then sputtering grows the upper zno-based film 4 that thickness is 200nm;
S4, with reference to shown in Fig. 4, by ethanol immersion treatment, remove polystyrene sphere mask layer 3 and polystyrene sphere covered
Zno-based film above film layer, the surface of zno-based film 4 is formed the ball hole 5 of one group of discrete distribution, obtain surface in bumps
The multilayer film transparent conducting glass of textured structure.
Specially:The glass substrate for preparing upper zno-based film is immersed to the ethanol immersion treatment of 95% concentration at room temperature
180 minutes.
The multilayer film transparent conducting glass that the present embodiment is obtained carries out thickness test, mist degree test, transmitance survey respectively
Examination, resistivity measurement and XRD are tested, and thickness be 600~800nm, mist degree 16.3%, it is seen that and light mean transmissivity is 86.7%,
Resistivity is 5.9*10-4Ω cm, XRD spectrum shows that zno-based film nearby more apparent diffraction maximum occurs in 2 θ=34.4 °, corresponding
Hexagonal wurtzite ZnO structures(002)Diffraction maximum.
Embodiment three
The present invention provides a kind of multilayer film transparent conducting glass preparation method with micro-structural, comprises the following steps:
S1, as shown in figure 1, using rf magnetron sputtering technique, zno-based is thin under sputtering growth at room temperature on the surface of glass substrate 1
Film 2;
Specially:Soda-lime-silica glass using thickness as 1.1mm is glass substrate 1, and glass substrate 1 is placed in into magnetron sputtering chamber
Interior, using zno-based ceramic target, the Ar gas for being passed through 30sccm keeps room temperature as sputter gas, preparation temperature;Zno-based ceramics
The spacing of target and substrate is preferably 70mm;
During magnetron sputtering, negative electrode is acted on using radio-frequency power supply, radio-frequency power supply sputtering power is 250W, target voltage 87V, is worked
Pressure is 0.2Pa;Pre-sputtering is first carried out to glass substrate, sputtering time 15min, it is 600nm's that then sputtering, which grows thickness,
Lower zno-based film 2;
S2, with reference to shown in Fig. 2, using bar knife coating, the polyphenyl second of the discrete distribution of individual layer is prepared on the lower surface of zno-based film 2
Alkene bead mask layer 3;
Specially:Using bar is scratched, using 0.5% wt polystyrene sphere solution as blade coating solution, the μ of bar thickness specification 20
M, obtain polystyrene sphere mask layer by layer 3, polystyrene sphere diameter 1000nm;
S3, with reference to shown in Fig. 3, using rf magnetron sputtering technique, by the use of polystyrene sphere mask layer 3 as mask, under
The surface of zno-based film 2 sputters the upper zno-based film 4 of growth at room temperature;The thickness of upper zno-based film 4 is less than polystyrene sphere
Diameter;
Specially:Negative electrode is acted on using radio-frequency power supply, radio-frequency power supply sputtering power is 250W, target voltage 87V, operating pressure
For 0.2Pa;Leading pre-sputtering, sputtering time 5min, then sputtering grow the upper zno-based film 4 that thickness is 200nm;
S4, with reference to shown in Fig. 4, by ethanol immersion treatment, remove polystyrene sphere mask layer 3 and polystyrene sphere covered
Zno-based film above film layer, the surface of zno-based film 4 is formed the ball hole 5 of one group of discrete distribution, obtain surface in bumps
The multilayer film transparent conducting glass of textured structure.
Specially:The glass substrate for preparing upper zno-based film is immersed to the ethanol immersion treatment of 95% concentration at room temperature
180 minutes.
The multilayer film transparent conducting glass that the present embodiment is obtained carries out thickness test, mist degree test, transmitance survey respectively
Examination, resistivity measurement and XRD are tested, and thickness be 600~800nm, mist degree 21.5%, it is seen that and light mean transmissivity is 89.7%,
Resistivity is 4.8*10-4Ω cm, XRD spectrum show that zno-based film stronger diffraction maximum nearby occurs in 2 θ=34.4 °, correspond to six
Angle buergerite ZnO structures(002)Diffraction maximum.
The above described is only a preferred embodiment of the present invention, any formal limitation not is made to the present invention;Appoint
What those skilled in the art, without departing from the scope of the technical proposal of the invention, all using the side of the disclosure above
Method and technology contents make many possible changes and modifications to technical solution of the present invention, or are revised as the equivalent reality of equivalent variations
Apply example.Therefore, every content without departing from technical solution of the present invention, the technical spirit according to the present invention are done to above example
Any simple modification, equivalent substitution, equivalence changes and modification, still fall within the range of technical solution of the present invention protects.
Claims (5)
1. a kind of multilayer film transparent conducting glass preparation method with micro-structural, it is characterised in that comprise the following steps:
S1, using rf magnetron sputtering technique, the zno-based film in the case where glass substrate surface sputters growth at room temperature;
S2, using bar knife coating, prepare the polystyrene sphere mask layer of the discrete distribution of individual layer in lower zno-based film surface;
S3, using rf magnetron sputtering technique, by the use of polystyrene sphere mask layer as mask, in lower zno-based film surface
The upper zno-based film of sputtering growth at room temperature;The thickness of upper zno-based film is less than the diameter of polystyrene sphere;
S4, by ethanol immersion treatment, remove the ZnO above polystyrene sphere mask layer and polystyrene sphere mask layer
Base film, zno-based film surface is formed the ball hole of one group of discrete distribution, obtain the multilayer that surface is in concavo-convex textured structure
Film transparent conducting glass.
2. a kind of multilayer film transparent conducting glass preparation method with micro-structural according to claim 1, its feature exist
In the step S1 uses zno-based ceramic target, and using Ar ions as sputter gas, radio-frequency power supply acts on negative electrode, radio frequency
Power supply sputtering power is 150~250W, and operating pressure 0.2Pa, target voltage is 62~87V, glass substrate and target spacing
For 70mm, the thickness for obtaining lower zno-based film is 600 ± 50nm.
3. a kind of multilayer film transparent conducting glass preparation method with micro-structural according to claim 1 or 2, its feature
It is, the concentration of polystyrene sphere mask layer is 0.1~0.5%wt in the step S2, polystyrene sphere a diameter of 300
~1000nm.
4. a kind of multilayer film transparent conducting glass preparation method with micro-structural according to claim 1 or 2, its feature
It is, the step S3 uses zno-based ceramic target, acts on negative electrode as sputter gas, radio-frequency power supply using Ar ions, penetrates
Frequency power sputtering power is 150~250W, and operating pressure 0.2Pa, target voltage is 62~87V, between glass substrate and target
Away from for 70mm, the thickness for obtaining zno-based film is 200 ± 50nm.
5. a kind of multilayer film transparent conducting glass preparation method with micro-structural according to claim 1 or 2, its feature
It is, the glass substrate for preparing upper zno-based film is immersed ethanol immersion treatment, polystyrene by the step S4 at room temperature
Zno-based film above bead mask layer and polystyrene sphere mask layer.
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CN109659375A (en) * | 2019-01-31 | 2019-04-19 | 中建材蚌埠玻璃工业设计研究院有限公司 | A kind of preparation method of biomimetic features hollow Nano silicon dioxide granule antireflective film |
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CN103367479A (en) * | 2013-07-03 | 2013-10-23 | 惠州市易晖太阳能科技有限公司 | Conducting substrate of flexible solar cell texture and preparation method thereof |
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CN102254961A (en) * | 2011-05-28 | 2011-11-23 | 惠州市易晖太阳能科技有限公司 | Conductive suede glass special for solar cells, and preparation method and application thereof |
CN103367479A (en) * | 2013-07-03 | 2013-10-23 | 惠州市易晖太阳能科技有限公司 | Conducting substrate of flexible solar cell texture and preparation method thereof |
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