CN103448323B - Transparent conducting oxide film-plated glass and preparation method thereof - Google Patents
Transparent conducting oxide film-plated glass and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a piece of transparent conducting oxide film-plated glass. The transparent conducting oxide film-plated glass comprises a glass matrix, a shielding layer, and a transparent conducting oxide layer, wherein the above-mentioned components are successively laminated. Grain sizes of the oxide of the transparent conducting oxide layer are gradually reduced from one side approaching the shielding layer to one side far away from the shielding layer. Because of controlling of the grain size of the oxide of the transparent conducting oxide layer of the transparent conducting oxide film-plated glass, the grain size of one side approaching the shielding layer is large and the grain size of one side far away from the shielding layer is relatively small. The film layer structure of the transparent conducting oxide layer has the high scattering characteristic for the solar light form the long wave length to the short wave length, so that the transparent conducting oxide film-plated glass can absorb the solar light with the wide spectral region. In addition, the invention also provides a preparation method for the transparent conducting oxide film-plated glass.
Description
Technical field
The present invention relates to special glass preparation field, particularly relate to a kind of transparent conductive oxide coated glass and preparation method thereof.
Background technology
TCO (Transparent conducting oxide) glass, i.e. transparent conductive oxide coated glass, the conductive oxide evenly plating layer of transparent by the method for physics or plated film at surface of plate glass obtains.
Transparent conductive oxide coated glass serves as electrode before battery in silicon-based film solar cells, plays a part printing opacity and collected current.In silicon-based film solar cells, the light absorption of non-crystalline silicon mainly concentrates in visible ray (380nm ~ 780nm) scope, its battery structure is P, I, N tri-layers of amorphous silicon film composition, and wherein intrinsic amorphous silicon layer and I layer are the generation regions of photo-generated carrier.When solar irradiation is mapped to after amorphous silicon thin-film solar cell, the photon (corresponding specific wavelength of light) that energy is more than or equal to I layer non-crystalline silicon bandwidth is in the Electron absorption of valence band, photon gives electronics energy trasfer, transit to conduction band after electrons gain energy and form photo-generate electron-hole pair, this electron-hole pair does displacement respectively to P, n-quadrant under the built in field effect of PN junction, thus forms photogenerated current.Energy is then not enough to make electron transition in valence band to conduction band lower than the photon of I layer non-crystalline silicon bandwidth, therefore can not be absorbed by solar cell and waste.Be 300nm ~ 2500nm for its scope of solar spectral, the main concentrated area of its energy is visible region and near infrared region.
Relative to crystal silicon solar batteries, the generated output of thin-film solar cells is on the low side.The spectral region of the sunshine that can absorb of the transparent conductive oxide coated glass that traditional thin-film solar cells adopts is narrower, and its sunshine utilized mainly concentrates on visible region, and in the sunshine of near infrared region, energy major part is wasted.
Summary of the invention
Based on this, the problem that the spectral region of the sunshine that can absorb of the transparent conductive oxide coated glass adopted for traditional thin-film solar cells is narrower, be necessary to provide a kind of can the transparent conductive oxide coated glass and preparation method thereof of the wider sunshine of absorption spectrum ranges.
A kind of transparent conductive oxide coated glass, comprises the following structure stacked gradually:
Glass basis, screen layer and including transparent conducting oxide layer;
The crystallite dimension of the oxide of described including transparent conducting oxide layer diminishes near described screen layer side gradually to away from described screen layer side.
In one embodiment, the refractive index of described screen layer becomes large near described glass basis side gradually to away from described glass basis side, and the excursion of refractive index is 1.48 ~ 1.56.
In one embodiment, the material of described screen layer is SiO
2, the thickness of described screen layer is 30nm ~ 100nm.
In one embodiment, the material of described including transparent conducting oxide layer is SnO
2, the thickness of described including transparent conducting oxide layer is 500nm ~ 1200nm.
A preparation method for transparent conductive oxide coated glass, comprises the steps:
Glass basis is provided;
Described glass basis is heated to 500 DEG C ~ 650 DEG C, adopts aumospheric pressure cvd method, be carrier with inert gas respectively by monosilane and oxidant, be passed into described glass basis surface reaction and form screen layer;
Described glass basis is heated to 500 DEG C ~ 600 DEG C, by the Xi Yuan of prefabricated gasification, containing oxygen source, adulterant and stabilizing agent respectively with described inert gas for carrier, be passed into described glass basis surface and form including transparent conducting oxide layer on described screen layer, first high rear low by the temperature controlling described glass basis, control the described concentration proportioning containing oxygen source and Xi Yuan first big after small or control that described stabilizing agent adds first many after few, the crystallite dimension of the oxide of described including transparent conducting oxide layer is diminished near described screen layer side gradually to away from described screen layer side.
In one embodiment, described deposition is formed in the step of screen layer, low or to control the concentration proportioning of described oxidant and monosilane first big after small after first high by the temperature that controls described glass basis, make the refractive index of described screen layer become large near described glass basis side gradually to away from described glass basis side.
In one embodiment, formed in the step of described screen layer, according to molar percentage, the content of monosilane is 0.1% ~ 10%, and the content of oxidant is 10% ~ 50%.
In one embodiment, in the step of described formation including transparent conducting oxide layer, according to molar percentage, the content of Xi Yuan is 5% ~ 60%, and the content containing oxygen source is 10% ~ 80%, and the content of adulterant is 1% ~ 10%, and the content of stabilizing agent is 1% ~ 10%.
In one embodiment, described oxidant is oxygen, and described inert gas is nitrogen or argon gas.
In one embodiment, described Xi Yuan is at least one in butter of tin, monobutyl-tin-trichloride, dimethyltin chloride and tetramethyl tin;
Described adulterant is trifluoroacetic acid, hydrogen fluoride, at least one crossed in fluoroacetic acid and perfluor acetic acid;
Described is at least one in water and peroxide water containing oxygen source;
Described stabilizing agent is at least one in methyl alcohol, ethanol and hydrogen chloride.
Make it larger near screen layer side crystallite dimension by the crystallite dimension of the oxide controlling the including transparent conducting oxide layer of transparent conductive oxide coated glass, and it is relatively little away from screen layer side crystallite dimension, the film layer structure of this including transparent conducting oxide layer grows to long wavelength to sunshine from shortwave and all possesses higher scattering properties, thus makes transparent conductive oxide coated glass can the wider sunshine of absorption spectrum ranges.
Accompanying drawing explanation
Fig. 1 is the sectional view of the transparent conductive oxide coated glass of an embodiment;
Fig. 2 is the preparation flow figure of transparent conductive oxide coated glass as shown in Figure 1;
Fig. 3 is the electromicroscopic photograph of transparent conductive oxide coated glass near screen layer side transparent conductive oxide film layer of embodiment 1 preparation;
Fig. 4 is the electromicroscopic photograph of transparent conductive oxide coated glass away from screen layer side transparent conductive oxide film layer of embodiment 1 preparation.
Detailed description of the invention
For the ease of understanding the present invention, below with reference to relevant drawings, the present invention is described more fully.Preferred embodiment of the present invention is given in accompanying drawing.But the present invention can realize in many different forms, is not limited to embodiment described herein.On the contrary, provide the object of these embodiments be make the understanding of disclosure of the present invention more comprehensively thorough.
The transparent conductive oxide coated glass of an embodiment as shown in Figure 1, comprises the following structure stacked gradually: glass basis 10, screen layer 20 and including transparent conducting oxide layer 30.
The crystallite dimension of the oxide of including transparent conducting oxide layer 30 diminishes near screen layer 20 side gradually to away from screen layer 20 side.
Make it larger near screen layer 20 side crystallite dimension by the crystallite dimension of the oxide controlling the including transparent conducting oxide layer 30 of transparent conductive oxide coated glass, and it is relatively little away from screen layer 20 side crystallite dimension, the film layer structure of this including transparent conducting oxide layer 30 grows to long wavelength to sunshine from shortwave and all possesses higher scattering properties, thus makes transparent conductive oxide coated glass can the wider sunshine of absorption spectrum ranges.
Glass basis 10 can be the sodium calcium ordinary flat flint glass or low iron ultrawhite plate glass that 1mm ~ 5mm is thick.
The excursion of the refractive index of screen layer 20 is 1.48 ~ 1.56.
The material of screen layer 20 can be SiO
2, thickness can be 30nm ~ 100nm.Screen layer 20 can stop that the basic ion in glass basis spreads to including transparent conducting oxide layer 30.
In a preferred embodiment, the refractive index of screen layer 20 becomes large near glass basis 10 side gradually to away from glass basis 10 side.Thus make screen layer 20 form a damping layer, reduce the transmitting look of including transparent conducting oxide layer 30.
In present embodiment, the material of including transparent conducting oxide layer 30 can be SnO
2, thickness can be 500nm ~ 1200nm.SnO
2the sedimentation rate of the including transparent conducting oxide layer 30 of material controls by changing glass substrate temperature, type of feed and concentration and adding stabilizing agent.Pure SnO
2film is a kind of broad-band gap oxide semiconductor to visible transparent, and energy gap 3.7 ~ 4.0eV, has positive tetrahedron rutile structure.
In a preferred embodiment, the material of including transparent conducting oxide layer 30 can for mixing the SnO of fluorine
2.After doped with fluorine, SnO
2film has advantages such as sunshine permeability is good, resistivity is low, stable chemical performance.
The preparation method of the transparent conductive oxide coated glass of an embodiment as shown in Figure 2, comprises the steps:
S10, provide glass basis 10.
Glass basis 10 can be the sodium calcium ordinary flat flint glass or low iron ultrawhite plate glass that 1mm ~ 5mm is thick.
Glass basis 10 is cleaned up rear drying, can for the preparation of transparent conductive oxide coated glass.
S20, glass basis 10 is heated to 500 DEG C ~ 650 DEG C, adopts aumospheric pressure cvd method, be carrier with inert gas respectively by monosilane and oxidant, be passed into glass basis 10 surface reaction and form screen layer 20.
Aumospheric pressure cvd method (APCVD) is adopted in body of heater plated film district, be carrier with inert gas respectively by monosilane and oxidant, be passed into glass basis 10 surface that the S10 at 500 DEG C ~ 650 DEG C obtains and form that thickness is 30nm ~ 100nm, the scope of refractive index is the SiO of 1.48 ~ 1.56
2the screen layer 20 of material.
In a preferred embodiment, by controlling the temperature of glass basis 10, first high rear low or controlled oxidization agent and monosilane concentration proportioning is first big after small, the rate of film build of screen layer 20 is accelerated, thus the refractive index of the screen layer 20 obtained become large near glass basis 10 side gradually to away from glass basis 10 side.
In one embodiment, can form screen layer 20 at twice, second time rate of film build is fast comparatively for the first time.
The screen layer 20 of the silica material formed can not only stop that the basic ion in glass basis 10 spreads to including transparent conducting oxide layer 30, the scope simultaneously also forming refractive index due to the inconsistent of its rate of film build is the distribution between 1.48 ~ 1.56, provide a damping layer, the transmitting look of including transparent conducting oxide layer 30 can be reduced.
Monosilane (SiH
4) molecule has Si
+-H
-ionic species, can the adsorption of positive potential be had, thus can glass basis 10 surface produce current potential corrigendum molecule contribute to glass basis 10 surface potential corrigendum, at same glass substrate 10 temperature, change the reaction rate of monosilane, thus change SiO
2sedimentation rate.
In this step, according to molar percentage, the content of monosilane is 0.1% ~ 10%, and the content of oxidant is 10% ~ 50%.
In actual production process, by the molar percentage of monosilane and oxidant, calculating the volume ratio of monosilane and oxidant, can be generally 1:50 ~ 1:500.
Oxidant can be oxygen, and inert gas can be nitrogen or argon gas.
Inert gas serves as the vector gas of monosilane and oxidant on the one hand, is also plated film device isolation gas on the other hand.When concrete operations, monosilane and inert gas mixing, oxidant and inert gas mixing, separately have part inert gas to serve as plated film device isolation gas, three kinds of gases are in the mixing of glass basis 10 surface simultaneously.
S30, glass basis 10 is heated to 500 DEG C ~ 600 DEG C, be carrier respectively with inert gas by the Xi Yuan of prefabricated gasification, containing oxygen source, adulterant and stabilizing agent, be passed into glass basis 10 surface and form including transparent conducting oxide layer 30 on screen layer 20, low after first high by the temperature that controls glass basis 10, control concentration proportioning containing oxygen source and Xi Yuan first big after small or control that stabilizing agent adds first many after few, the crystallite dimension of the oxide of including transparent conducting oxide layer 30 is diminished near screen layer 20 side gradually to away from screen layer 30 side.
In this step, according to molar percentage, the content of Xi Yuan is 5% ~ 60%, and the content containing oxygen source is 10% ~ 80%, and the content of adulterant is 1% ~ 10%, and the content of stabilizing agent is 1% ~ 10%.
In actual production process, by Xi Yuan, molar percentage containing oxygen source, adulterant and stabilizing agent, calculate Xi Yuan, volume ratio containing oxygen source, adulterant and stabilizing agent, can be generally, the volume ratio of Xi Yuan and adulterant is 1:1 ~ 20:1, volume ratio containing oxygen source and stabilizing agent is 1:50 ~ 1:500, Xi Yuan and the volume ratio containing oxygen source is 1:30 ~ 1:100.
Xi Yuan is at least one in butter of tin, monobutyl-tin-trichloride, dimethyltin chloride and tetramethyl tin.
Adulterant is trifluoroacetic acid, hydrogen fluoride, at least one crossed in fluoroacetic acid and perfluor acetic acid.
Containing at least one that oxygen source is in water and peroxide water.
Stabilizing agent is at least one in methyl alcohol, ethanol and hydrogen chloride.
In present embodiment, the material of including transparent conducting oxide layer 30 can be SnO
2, thickness can be 500nm ~ 1200nm.SnO
2the sedimentation rate of the including transparent conducting oxide layer 30 of material controls by changing glass substrate temperature, type of feed and concentration and adding stabilizing agent.Pure SnO
2film is a kind of broad-band gap oxide semiconductor to visible transparent, and energy gap 3.7 ~ 4.0eV, has positive tetrahedron rutile structure.
In a preferred embodiment, the material of including transparent conducting oxide layer 30 can for mixing the SnO of fluorine
2.After doped with fluorine, SnO
2film has advantages such as sunshine permeability is good, resistivity is low, stable chemical performance.
Including transparent conducting oxide layer 30 is deposited on screen layer 20, by control SnO
2the sedimentation rate of film controls the crystalline condition of including transparent conducting oxide layer 30, forms the crystallite dimension of oxide from close screen layer 20 side to the film layer structure diminished gradually away from screen layer 20 side.This structure can under the condition keeping including transparent conducting oxide layer 30 low-resistance high-transmittance rate, from shortwave, long wavelength is grown to sunshine and all possesses higher scattering properties, thus reflect including transparent conducting oxide layer 30 and all keep higher level at the haze value of sunshine scope.
It is below specific embodiment part.
Embodiment 1
In APCVD reaction chamber, be successively the conversion zone of 620 DEG C and 600 DEG C by space temperature by glass basis, the concentration of monosilane is respectively according to molar percentage 0.1% and 0.15%, oxygen concentration ratio is respectively according to molar percentage 10% and 15%, the screen layer that the obtained composite refractive index of deposition is 1.52, thickness is the silica membrane material of 55nm.
The glass basis depositing screen layer is introduced tin dioxide film deposit cavity, and successively by the deposition of three tin dioxide films, reaction condition is as following table:
Record the including transparent conducting oxide layer prepared, square resistance is 9 Ω/, and transmissivity reaches 80.2%.550nm single-point mist degree is 16.2%, 380nm ~ 780nm average haze is 15.5%.
As can be seen from Fig. 3 and Fig. 4, the crystallite dimension of the oxide of the transparent conductive oxide film layer of transparent conductive oxide coated glass prepared by the present embodiment is obviously being greater than away from screen layer side (in the diagram) near screen layer side (in Fig. 3).
Embodiment 2
In APCVD reaction chamber, be successively the conversion zone of 620 DEG C and 620 DEG C by space temperature by glass basis, the concentration of monosilane is respectively according to molar percentage 0.08% and 0.12%, oxygen concentration ratio is respectively according to molar percentage 15% and 20%, the screen layer that the obtained composite refractive index of deposition is 1.55, thickness is the silica material of 60nm.
The glass basis depositing screen layer is introduced tin dioxide film deposit cavity, and successively by the deposition of twice tin dioxide film, reaction condition is as following table:
Record the including transparent conducting oxide layer prepared, square resistance is 8.9 Ω/, and transmissivity reaches 80.8%.550nm single-point mist degree is 14.3%, 380nm ~ 780nm average haze is 12.9%.
Embodiment 3
In APCVD reaction chamber, be successively the conversion zone of 600 DEG C and 600 DEG C by space temperature by glass basis, the concentration of monosilane is respectively according to molar percentage 0.1% and 0.15%, oxygen concentration ratio is respectively according to molar percentage 10% and 15%, the screen layer that the obtained composite refractive index of deposition is 1.55, thickness is the silica material of 50nm.
The glass basis depositing screen layer is introduced tin dioxide film deposit cavity, and successively by the deposition of four tin dioxide films, reaction condition is as following table:
Record the including transparent conducting oxide layer prepared, square resistance is 8.5 Ω/, and transmissivity reaches 80.6%.550nm single-point mist degree is 17.9%, 380nm ~ 780nm average haze is 16.1%.
The above embodiment only have expressed one or more embodiments of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. a transparent conductive oxide coated glass, is characterized in that, comprises the following structure stacked gradually:
Glass basis, screen layer and including transparent conducting oxide layer;
The crystallite dimension of the oxide of described including transparent conducting oxide layer diminishes near described screen layer side gradually to away from described screen layer side.
2. transparent conductive oxide coated glass according to claim 1, is characterized in that, the refractive index of described screen layer becomes large near described glass basis side gradually to away from described glass basis side, and the excursion of refractive index is 1.48 ~ 1.56.
3. transparent conductive oxide coated glass according to claim 1, is characterized in that, the material of described screen layer is SiO
2, the thickness of described screen layer is 30nm ~ 100nm.
4. transparent conductive oxide coated glass according to claim 1, is characterized in that, the material of described including transparent conducting oxide layer is SnO
2, the thickness of described including transparent conducting oxide layer is 500nm ~ 1200nm.
5. a preparation method for transparent conductive oxide coated glass, is characterized in that, comprises the steps:
Glass basis is provided;
Described glass basis is heated to 500 DEG C ~ 650 DEG C, adopts aumospheric pressure cvd method, be carrier with inert gas respectively by monosilane and oxidant, be passed into described glass basis surface reaction and form screen layer;
Described glass basis is heated to 500 DEG C ~ 600 DEG C, by the Xi Yuan of prefabricated gasification, containing oxygen source, adulterant and stabilizing agent respectively with described inert gas for carrier, be passed into described glass basis surface and form including transparent conducting oxide layer on described screen layer, first high rear low by the temperature controlling described glass basis, control the described concentration proportioning containing oxygen source and Xi Yuan first big after small or control that described stabilizing agent adds first many after few, the crystallite dimension of the oxide of described including transparent conducting oxide layer is diminished near described screen layer side gradually to away from described screen layer side.
6. the preparation method of transparent conductive oxide coated glass according to claim 5, it is characterized in that, described deposition is formed in the step of screen layer, low or to control the concentration proportioning of described oxidant and monosilane first big after small after first high by the temperature that controls described glass basis, make the refractive index of described screen layer become large near described glass basis side gradually to away from described glass basis side.
7. the preparation method of transparent conductive oxide coated glass according to claim 5, is characterized in that, is formed in the step of described screen layer, and according to molar percentage, the content of monosilane is 0.1% ~ 10%, and the content of oxidant is 10% ~ 50%.
8. the preparation method of transparent conductive oxide coated glass according to claim 5, it is characterized in that, in the step of described formation including transparent conducting oxide layer, according to molar percentage, the content of Xi Yuan is 5% ~ 60%, content containing oxygen source is 10% ~ 80%, and the content of adulterant is 1% ~ 10%, and the content of stabilizing agent is 1% ~ 10%.
9. the preparation method of transparent conductive oxide coated glass according to claim 5, is characterized in that, described oxidant is oxygen, and described inert gas is nitrogen or argon gas.
10. the preparation method of transparent conductive oxide coated glass according to claim 5, is characterized in that, described Xi Yuan is at least one in butter of tin, monobutyl-tin-trichloride, dimethyltin chloride and tetramethyl tin;
Described adulterant is trifluoroacetic acid, hydrogen fluoride, at least one crossed in fluoroacetic acid and perfluor acetic acid;
Described is at least one in water and peroxide water containing oxygen source;
Described stabilizing agent is at least one in methyl alcohol, ethanol and hydrogen chloride.
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| GB0915376D0 (en) * | 2009-09-03 | 2009-10-07 | Isis Innovation | Transparent conducting oxides |
| US20120107554A1 (en) * | 2010-10-29 | 2012-05-03 | Pfaff Gary L | TCO Coating and Coated Substrate for High Temperature Applications |
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Effective date of registration: 20160505 Address after: Jingtou town 511600 Guangdong city of Qingyuan province Fogang County Industrial Park eight Jinling Jinling Road No. 1 Patentee after: QINGYUAN CSG NEW ENERGY-SAVING MATERIALS CO., LTD. Address before: Six industrial intersection, Shekou Industrial Zone, Shenzhen, Guangdong, Nanshan District 518047, China Patentee before: CSG Holding Co., Ltd. |