CN103570254B - Conductive glass, its preparation method and application - Google Patents
Conductive glass, its preparation method and application Download PDFInfo
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- CN103570254B CN103570254B CN201210272588.7A CN201210272588A CN103570254B CN 103570254 B CN103570254 B CN 103570254B CN 201210272588 A CN201210272588 A CN 201210272588A CN 103570254 B CN103570254 B CN 103570254B
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Abstract
The present invention is applicable to special glass field, provides a kind of conductive glass, its preparation method and application.This conductive glass comprises mutually stacked glass substrate layers, sodium ion blocking layer and conductive film layer, it is characterized in that, also comprises antireflection layer, and this antireflection layer is laminated on this conductive film layer.Conductive glass of the present invention, by increasing one deck antireflection layer on conducting film, this antireflection layer forms three layers of antireflection film system together with conductive film layer and sodium ion blocking layer, realizes the remarkable lifting of this conductive glass to visible light transmissivity.Conductive glass preparation method of the present invention, simple to operate, with low cost, productivity effect is high, is very suitable for suitability for industrialized production.
Description
Technical field
The invention belongs to special glass field, particularly relate to a kind of conductive glass, its preparation method and application.
Background technology
At present, transparent conductive oxide film has and mixes fluorine SnO
2film (FTO), mix aluminium ZnO film (AZO) and In
2o
3: Sn (ITO) film etc.Compared with the above two, ito thin film is under equal specific conductivity, and have that rete is thin, visible light transmissivity is high and the advantage such as Color Neutral, therefore it is quite extensive in the application of the field such as liquid-crystal display and illumination.But due in ito thin film, In material is few at nature reserves, harmful in preparation process, and the nucleidic mass of Sn and In is comparatively large, easily penetrates into substrate interior in film process, poison substrate material, especially in liquid crystal display device, contamination phenomenon is serious.Therefore, the substitute products finding a kind of ito thin film are necessary.
ZnO-based transparent conductive film has starting material and is easy to get, low price, and nontoxic and easier than the ITO advantage such as to etch, has the photoelectric characteristic comparable with ITO simultaneously.At present, one of ZnO-TCO film function film being considered to great exploitation potential for its, becomes the study hotspot that may substitute ito thin film.When nesa coating layer thickness is more than 0.1 μm, the repeatedly interference in rete will produce visible color, and the increase of thicknesses of layers can cause the raising of reflectivity and aberration, therefore will realize the industrial application of ZnO-TCO film, must improve these problems.
Summary of the invention
In view of this, the invention provides a kind of conductive glass, in solution prior art, ZnO-TCO conductive glass transmittance is not high, and aberration is large, the technical problem of unstable properties.
The present invention is achieved in that
A kind of conductive glass, comprise mutually stacked glass substrate layers, sodium ion blocking layer and conductive film layer, also comprise antireflection layer, this antireflection layer is laminated on this conductive film layer.
And,
Preparation method planted by above-mentioned conductive glass, comprises the steps:
This glass substrate layers is provided;
On this glass substrate layers, sodium ion blocking layer is formed by magnetron sputtering;
On this sodium ion blocking layer, conductive film layer is formed by magnetron sputtering;
On this conductive film layer, form antireflection layer by magnetron sputtering, obtain conductive glass.
The present invention further provides the application of above-mentioned conductive glass in solar cell, touch-screen, liquid crystal display device or illuminating device.
Conductive glass of the present invention, by increasing one deck antireflection layer on conducting film, this antireflection layer forms three layers of antireflection film system together with conductive film layer and sodium ion blocking layer, realizes the remarkable lifting of this conductive glass to visible light transmissivity.
Conductive glass preparation method of the present invention, simple to operate, with low cost, productivity effect is high, is very suitable for suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is embodiment of the present invention conductive glass structure iron;
Fig. 2 is comparative example conductive glass structure iron;
Fig. 3 is the embodiment of the present invention and comparative example transmitance correlation curve.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Refer to Fig. 1, Fig. 1 reality embodiment of the present invention conductive glass structure, this conductive glass comprise stack gradually glass substrate layers 1, sodium ion blocking layer 2 and conductive film layer 3, also comprise antireflection layer 4, this is anti-reflection 4 folds on this conductive film layer 3 layer by layer.Concrete, this sodium ion blocking layer 2 is laminated on this glass substrate layers 1, this conductive film layer 3 is laminated on this sodium ion blocking layer 2, and this antireflection layer 4 is laminated in (antireflection layer 4 is laminated in the surface relative with sodium ion blocking layer 2 of this conductive film layer 3) on this conductive film layer 3.
Embodiment of the present invention conductive glass, by setting up one deck antireflection layer on conductive film layer, this antireflection layer can form three layers of antireflection film system together with this conductive film layer, sodium ion blocking layer, there is destructive interference at four bed interface places of conductive glass in incident light, thus realizes conductive glass and greatly increase in the transmitance of visible region; Especially in conjunction with the thickness of above-mentioned each layer, the occurrence degree of this destructive interference is promoted further, conductive glass is strengthened further in the transmitance of visible ray.Through higher, reflected colour and will more close to muted color through look, color value just has very large decline.
The thickness of this glass substrate layers is preferably 1mm-5mm, and the material of this glass substrate layers is preferably the ultra-white float glass basic unit of iron ion content lower than 200PPM, and it is greater than 90% in visible ray section transmitance.This glass substrate layers can also select other conventional materials in this area.
The thickness on this sodium ion blocking layer is 50 ~ 90 nanometers, and material is preferably SiN
xo
y(0.7<x<1.2,0.25<y<1) compound, its specific refractory power in visible ray section is 1.6 ~ 1.8.This sodium ion blocking layer effectively can stop that the sodium ion in glass substrate layers infiltrates in conductive film layer, prevent sodium ion from damaging conductive film layer, this sodium ion blocking layer can effective enhanced film system (sodium ion blocking layer, conductive film layer and the antireflection layer) sticking power on glass substrate layers simultaneously.This sodium ion blocking layer forms the antireflection film system of three layers together with conductive film layer and antireflection layer, greatly can strengthen the transmittance of conductive glass in visible ray section.Other conventional material can also to be selected in this area in sodium ion blocking layer.
The thickness of this conductive film layer is 200 ~ 400 nanometers, material can make Zinc oxide film (ZnO film), doped with at least one element in B, Al, Ge in this Zinc oxide film, it can be such as at least one in the glass such as BZO, AZO, GZO or GAZO, in B, Al, Ge, the content of at least one element in ZnO conductive layer 3 gross weight is preferably greater than 0.25%, is less than or equal to 5%.This conductive film layer can also be ITO, FTO etc.
This antireflection layer is the low refractive index dielectric layer of conductive glass, and its specific refractory power in visible ray section is 1.35 ~ 1.5, and its thickness is 30 ~ 90 nanometers, and the material of this antireflection layer can be SiO
2film, magnesium fluoride film or other there are other anti-reflection films of low absorptivity and optical extinction coefficient k ≈ 0 in visible-range.The increase of this antireflection layer, can not impact the conductivity of conductive glass or affect small, but this antireflection layer can form the low absorption antireflection film system of three layers with aforesaid sodium ion blocking layer together with conductive film layer, conductive glass can be greatly reduced to visible light reflectance, improve the transmitance of conductive glass in visible ray section; And can effectively regulate conductive glass color, be conductive glass through look close to middle look, reach the requirement of industrial application.
The embodiment of the present invention provides the preparation method of above-mentioned conductive glass further, comprises the steps:
Step S01, provides stratum basale:
This glass substrate layers is provided;
Step S02, prepares sodium ion blocking layer:
On this glass substrate layers, sodium ion blocking layer is formed by magnetron sputtering;
Step S03, prepares conductive film layer:
On this sodium ion blocking layer, conductive film layer is formed by magnetron sputtering;
Step S04, prepares antireflection layer:
On this conductive film layer, form antireflection layer by magnetron sputtering, obtain conductive glass.
In step S01, this glass substrate layers is identical with aforesaid, does not repeat to set forth at this.
In step S02, this sodium ion blocking layer preparation method is magnetron sputtering method, and with high-purity Si target for sputtering target material, purity is 99.9%, with high-purity Ar, O
2and N
2the mixed gas of gas is working gas (purity of three kinds of gases is 99.999%), on this glass substrate layers, and sputtering sedimentation sodium ion blocking layer.During sputtering, the base vacuum of magnetron sputtering equipment is lower than 3.0E-6mbar, and underlayer temperature is 50 ~ 200 DEG C, and sputtering pressure is 1 ~ 6 × 10
-3mbar, Ar, O during sputtering
2and N
2the flow control of gas is: Ar gas accounts for about 20%, O of total tolerance
2/ N
2between 1:4 and 3:2., the walking speed of glass substrate is 1.4m/s.
Sodium ion stratum basale prepared in this step S02 is identical with aforesaid, does not repeat to set forth at this.
In step S03, this conductive film layer preparation method is magnetron sputtering method, with ZnO and doped element target (doping can be at least one element in B, Al, Ge, such as, Al
2o
3) ceramic target is sputtering target material, wherein the weight percent of doped element target is 0.25 ~ 5%, with high-purity Ar gas (or helium etc.) for sputter gas, and depositing electrically conductive rete on sodium ion blocking layer.Underlayer temperature during deposition is 250 ~ 320 DEG C, sputtering pressure is 1 ~ 6 × 10
-3mbar, Ar airshed is 200sccm, and the walking speed of glass substrate is 1.4m/s.Or on conductive film layer, prepare FTO film or ito film with reference to existing method.In this step S03, preparation-obtained conductive film layer is identical with aforementioned, does not repeat to set forth at this.
In step S04, on this conductive film layer, form antireflection layer by the method for sputtering, with high-purity Si target for sputtering target material, purity is 99.9%, with high-purity Ar and O
2mixed gas is working gas, and purity is more than 99.9%, and conductive film layer deposits SiO
2antireflection layer; Or underlayer temperature during deposition is 0 DEG C, and sputtering power is 14kw, and sputtering pressure is 1 ~ 6 × 10
-3mbar, Ar and O
2airshed ratio is respectively 50 ~ 150 and 40 ~ 110sccm.The preparation technology of magnesium fluoride with reference to existing method, such as, chemical solution method.
Embodiment of the present invention conductive glass preparation method, simple to operate, with low cost, productivity effect is high, is very suitable for suitability for industrialized production.Embodiment of the present invention conductive glass preparation method; ZnO-TCO glass basis is coated with one deck low refractive index dielectric layer; three layers of antireflection film system are formed together with sodium ion blocking layer and ZnO layer; available protecting ZnO layer can not only do not destroyed by the sodium ion in glass-base, and significantly can reduce visible reflectance.This ZnO-TCO glass properties is excellent, and visible light transmissivity can reach more than 90%, and can more effectively adjustable colors, make this ZnO-TCO glass through look close to neutral, reach the requirement of industrial application.This preparation method's process stabilizing, with low cost, continuously adjustabe, be applicable to big area industrial production.
The embodiment of the present invention provides the application of above-mentioned conductive glass in solar cell, touch-screen, liquid crystal display device or illuminating device further.This illuminating device is organic illumination device (OED) particularly.
Below in conjunction with specific embodiment, above-mentioned conductive glass and preparation method thereof is described in detail.
Embodiment 1
Embodiment of the present invention conductive glass, its structure as shown in Figure 1, comprises mutually stacked glass substrate layers 1, material is that wherein x is 1.2, y to SiNxOy(is 1) the sodium ion blocking layer 2 of compound, material for mixing Al zinc oxide conductive film layer 3, also comprise material SiO
2antireflection layer 4, this antireflection layer 4 is laminated on this conductive film layer 3, and wherein, glass substrate layers 1 thickness is 2mm, sodium ion blocking layer 2 thickness be 75nm, ZnO conductive film layer 3 thickness is 290nm, SiO
2anti-reflection film 4 thickness is 30nm.
Embodiment of the present invention conductive glass its preparation method is as follows:
After getting former of 2mm ultra-clear glasses cutting edging, after cleaning machine cleans and dries up, enter magnetron sputtering coater plated film;
With high-purity Si target for sputtering target material, purity is 99.9%, with high-purity Ar, O
2and N
2the mixed gas of gas is working gas (purity of three kinds of gases is 99.999%), glass substrate layers 1 deposits sodium ion blocking layer 2, during sputtering, the base vacuum of magnetron sputtering equipment is lower than 3.0E-6mbar, underlayer temperature when sodium ion blocking layer 2 deposits is 200 DEG C, sputtering power is 25kw, and sputtering pressure is 3.0E-3mbar, Ar, O during sputtering
2and N
2the flow of gas is respectively 100,70 and 100sccm, and the walking speed of glass substrate is 1.4m/s;
With ZnO:Al
2o
3ceramic target is sputtering target material, wherein component Al
2o
3weight percent be 1%, with high-purity Ar gas for sputter gas, sodium ion blocking layer 2 deposits ZnO conductive film layer 3.Underlayer temperature during deposition is 320 DEG C, and sputtering power is 90kw, and sputtering pressure is 5.0E-3mbar, Ar airshed is 200sccm, and the walking speed of glass substrate is 1.4m/s;
With high-purity Si target for sputtering target material, with Ar and O
2mixed gas is working gas, and ZnO conductive film layer 3 deposits SiO2 anti-reflection film.Underlayer temperature during deposition is 180 DEG C, and sputtering power is 14kw, and sputtering pressure is 2.5E-3mbar, Ar and O
2airshed is respectively 100 and 80sccm, and glass substrate walking speed is 1.4m/s, obtains conductive glass.
Embodiment 2
Embodiment of the present invention conductive glass, its structure as shown in Figure 1, comprise mutually stacked glass substrate layers 1, material be that wherein x is 0.7, y to SiNxOy(is 0.25) the sodium ion blocking layer 2 of compound, material for mixing Al zinc oxide conductive film layer 3, also comprise material SiO
2antireflection layer 4, this antireflection layer 4 is laminated on this conductive film layer 3, and wherein, glass substrate layers 1 thickness is 2mm, sodium ion blocking layer 2 thickness be 75nm, ZnO conductive film layer 3 thickness be 290nm, SiO2 anti-reflection film 4 thickness is 70nm.
Embodiment of the present invention conductive glass its preparation method is as follows:
The preparation technology of sodium ion blocking layer 2 and ZnO conductive film layer 3 is with reference to embodiment 1;
With high-purity Si target for sputtering target material, with Ar and O
2mixed gas is working gas, and ZnO conductive film 3 deposits SiO
2anti-reflection film.Underlayer temperature during deposition is 180 DEG C, and sputtering power is 26kw, and sputtering pressure is 2.8E-3mbar, Ar and O
2airshed is respectively 110 and 90sccm, and glass substrate walking speed is 1.4m/s, obtains conductive glass.
Reference example 1
This comparative example traditional Z nO-TCO glass, its structure as shown in Figure 2, comprises ultra-clear glasses substrate 1, SiNxOy compound film 2, mixes Al zinc oxide conducting film 3.Wherein, ultra-clear glasses substrate 1 thickness is 2mm, SiNxOy compound rete 2 thickness be 75nm, ZnO conducting film 3 thickness is 290nm.The preparation of traditional Z nO-TCO glass is except lacking SiO
2outside medium layer 4, all the other processing condition are completely identical with embodiment 1.
Performance test:
Four point probe is utilized to survey the conductive glass square resistance of the embodiment of the present invention 1,2, with the visible light transmissivity of the spectrophotometric measurement embodiment of the present invention 1,2 conductive glass and reflection and through look, specific performance index is as shown in table 1, and transmitance correlation curve as shown in Figure 2.
As can be seen from the data of upper table, compared with comparative example conductive glass, the conductive glass of the embodiment of the present invention has larger increase on visible light transmissivity, reflectivity declines larger, meanwhile, the conductivity of embodiment of the present invention conductive glass does not have because of the increase of antireflection layer and significantly declines.
As can be seen from Figure 3, with reference example 1
*compare, the embodiment of the present invention 1 and embodiment 2 have in the transmitance of whole visible ray section and promote by a relatively large margin, particularly short-wave band transmitance promote more obvious, serve good antireflective effect.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. a conductive glass, comprise stack gradually glass substrate layers, sodium ion blocking layer and conductive film layer, be characterised in that, also comprise antireflection layer, described antireflection layer is laminated on described conductive film layer;
Wherein, described substrate of glass layer thickness is 2mm, and described sodium ion blocking layer is the SiN of thickness 75nm
1.2o layer, described conductive film layer is the ZnO layer of thickness 290nm, and described antireflection layer is the SiO of thickness 30nm
2layer; Or described substrate of glass layer thickness is 2mm, described sodium ion blocking layer is the SiN of thickness 75nm
0.7o
0.25layer, described conductive film layer is the ZnO layer of thickness 290nm, and described antireflection layer is the SiO of thickness 70nm
2layer.
2. conductive glass as claimed in claim 1, it is characterized in that, the visible ray specific refractory power of described antireflection layer is 1.35 ~ 1.5.
3. conductive glass as claimed in claim 1, it is characterized in that, the visible ray specific refractory power on described sodium ion blocking layer is 1.6 ~ 1.8.
4. the conductive glass preparation method as described in any one of claims 1 to 3, comprises the steps:
Described glass substrate layers is provided;
On described glass substrate layers, sodium ion blocking layer is formed by magnetron sputtering;
On described sodium ion blocking layer, conductive film layer is formed by magnetron sputtering;
On described conductive film layer, form antireflection layer by magnetron sputtering, obtain conductive glass.
5. the application of the conductive glass as described in any one of claims 1 to 3 in solar cell, touch-screen, liquid crystal display device or illuminating device.
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| CN104602375A (en) * | 2014-12-17 | 2015-05-06 | 内蒙古坤瑞玻璃工贸有限公司 | Thermal sensitive ceramic electrically heated glass and preparation method thereof |
| CN104635991B (en) | 2015-03-11 | 2019-01-11 | 合肥鑫晟光电科技有限公司 | A kind of shadow eliminating structure, touch screen and preparation method thereof |
| CN104860549A (en) * | 2015-04-20 | 2015-08-26 | 安徽立光电子材料股份有限公司 | Electric heating conductive glass and manufacturing method thereof |
| CN104951133A (en) * | 2015-06-18 | 2015-09-30 | 无锡启晖光电科技有限公司 | Touch screen anti-reflection anti-fouling membrane |
| CN106746710A (en) * | 2017-01-18 | 2017-05-31 | 陆开云 | A kind of manufacture method of electro-conductive glass |
| CN115583803B (en) * | 2022-11-08 | 2024-05-17 | 宁波海燕新材料有限公司 | AZO transparent conductive film and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0994081A1 (en) * | 1998-10-13 | 2000-04-19 | Glaverbel | Solar control coated glass |
| CN202782020U (en) * | 2012-07-31 | 2013-03-13 | 信义光伏产业(安徽)控股有限公司 | Conductive glass |
-
2012
- 2012-07-31 CN CN201210272588.7A patent/CN103570254B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0994081A1 (en) * | 1998-10-13 | 2000-04-19 | Glaverbel | Solar control coated glass |
| CN202782020U (en) * | 2012-07-31 | 2013-03-13 | 信义光伏产业(安徽)控股有限公司 | Conductive glass |
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