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WO2015093082A1 - Procédé de production d'un élément en verre, et élément en verre - Google Patents

Procédé de production d'un élément en verre, et élément en verre Download PDF

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Publication number
WO2015093082A1
WO2015093082A1 PCT/JP2014/066023 JP2014066023W WO2015093082A1 WO 2015093082 A1 WO2015093082 A1 WO 2015093082A1 JP 2014066023 W JP2014066023 W JP 2014066023W WO 2015093082 A1 WO2015093082 A1 WO 2015093082A1
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WO
WIPO (PCT)
Prior art keywords
glass member
glass
etching
glass substrate
convex portion
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2014/066023
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English (en)
Japanese (ja)
Inventor
至崇 岡田
宮野　健次郎
正和 杉山
エフライン・エドアルド タマヨ・ルイス
渡辺　健太郎
拓也 星井
亮 玉置
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
University of Tokyo NUC
Original Assignee
University of Tokyo NUC
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by University of Tokyo NUC filed Critical University of Tokyo NUC
Publication of WO2015093082A1 publication Critical patent/WO2015093082A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
    • C03C23/0005—Other surface treatment of glass not in the form of fibres or filaments by irradiation
    • C03C23/006—Other surface treatment of glass not in the form of fibres or filaments by irradiation by plasma or corona discharge
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
    • G02B1/11—Anti-reflection coatings
    • G02B1/118—Anti-reflection coatings having sub-optical wavelength surface structures designed to provide an enhanced transmittance, e.g. moth-eye structures
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/20—Materials for coating a single layer on glass
    • C03C2217/28—Other inorganic materials
    • C03C2217/284—Halides
    • C03C2217/285—Fluorides
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/52—PV systems with concentrators

Definitions

  • the present invention relates to a method for producing a glass member and a glass member, and particularly to an optical member of a solar cell.
  • Solar cells are attracting attention as a source of clean electrical energy, and improvement in power generation efficiency is desired.
  • the light transmitted through the optical member is increased by suppressing reflection that occurs at the interface between the optical member such as the cover glass, the transparent electrode, and the homogenizer of the solar cell and the air.
  • a method for increasing the light applied to the cell has been studied.
  • a technique for changing the optical characteristics of the optical member for example, a technique for obtaining an antireflection effect by controlling the refractive index in a pseudo manner by forming a fine structure smaller than the wavelength of light on the surface of the optical member. has been proposed (for example, Patent Document 1).
  • Patent Document 1 discloses a method of obtaining a high antireflection performance by providing a two-dimensional uneven structure having a wavelength equal to or smaller than the minimum wavelength of light to be prevented from reflecting on a transparent substrate.
  • Patent Document 1 in order to form an antireflection structure, a resist is exposed by photolithography or electron beam lithography to produce a mask, and the surface of the glass substrate is etched using the mask. The manufacturing process of the antireflection structure is complicated.
  • a solar cell according to claim 7 of the present invention is characterized by using the glass member according to any one of claims 1 to 6.
  • the method for producing a glass member according to claim 8 of the present invention includes plasma etching the surface of a glass substrate containing one or more elements selected from alkali metals, alkaline earth metals, and rare earths using a fluorine-based gas.
  • the 1st process to be provided is provided, It is characterized by the above-mentioned.
  • the glass member according to claim 1 of the present invention includes a plurality of convex portions formed integrally with the base on at least one surface of the base formed of glass, and the convex portions include an alkali metal, an alkaline earth metal, and Since the tip portion has a fluoride layer containing one or more selected from rare earth fluorides, the optical characteristics change.
  • the solar battery according to claim 7 of the present invention can efficiently collect light in the solar battery cell due to a change in the characteristics of the optical member formed of glass. Therefore, power generation efficiency can be improved.
  • the method for producing a glass member according to claim 8 of the present invention includes plasma etching the surface of a glass substrate containing one or more elements selected from alkali metals, alkaline earth metals, and rare earths using a fluorine-based gas. Since the first layer is provided, a fluoride layer is formed on the surface of the glass substrate during the first step, the fluoride layer functions as a mask, and the portion covered by the mask remains without being etched. Thus, a convex portion having a fluoride layer at the tip end portion is formed. Therefore, it is possible to easily manufacture a glass member whose optical characteristics are changed only by a plasma etching process.
  • FIG. 5A is the transmittance
  • FIG. 7A glass members etching time of 20 minutes by CHF 3
  • FIG. 7B is a glass member etching time of 30 minutes by CHF 3
  • FIG. 7C is CHF 3 etching time by 40 minutes of the glass member (example 1 glass members) in FIG. 7D glass member etching time of 60 minutes by CHF 3
  • FIG. 7E is a cross-sectional SEM photograph of the glass member 80 minute etching time by CHF 3. It is a figure which shows the result of the composition analysis of the surface of the glass member of the Example by XPS
  • FIG. 8A is the analysis result of the glass substrate before the etching process of Example 1
  • the glass member after the etching process of Example 1 is the analysis result of the glass substrate before the etching process of Example 1
  • FIG. 9A is a view showing the analysis result of the composition of the glass member after the etching treatment of Example 1 by STEM-EDX
  • FIG. 9A is a cross-sectional TEM photograph of the glass member after the etching treatment
  • FIG. 9B is a region 1 shown in FIG.
  • FIG. 9C is a diagram showing the EDX analysis result of region 2 shown in FIG. 9A.
  • FIG. 10A is a diagram showing a composition analysis result of the glass member after the etching treatment of Example 1 by STEM-EDX
  • FIG. 10A is a diagram showing a composition analysis result of the glass member after the etching treatment of Example 1 by STEM-EDX
  • FIG. 10A is a diagram showing a composition analysis result of the glass member after the etching treatment of Example 1 by STEM-EDX
  • FIG. 10A is a diagram showing a composition analysis result of the glass member after the etching treatment of Example 1 by STEM-EDX
  • FIG. 10A is a diagram showing a composition analysis result of
  • FIG. 10A is a cross-sectional TEM photograph of the glass member after the etching treatment of Example 1
  • FIG. 10C is a diagram showing the F distribution
  • FIG. 10D is the Si distribution
  • FIG. 10E is the Ca distribution
  • FIG. 10F is a diagram showing the results of EDX analysis showing the Na distribution. It is a photograph which shows the result of the evaluation experiment of the characteristic with respect to the water of the glass member of Example 1
  • FIG. 11A is the experimental result about the glass substrate before an etching process
  • FIG. 11B is about the glass member after the etching process of Example 1.
  • the glass member 1 of the first embodiment includes a base 2 and a plurality of convex portions 3 formed on at least one surface of the base 2. Is provided.
  • the substrate 2 is made of glass, and the shape thereof can be any shape such as a plate shape, a lens shape having a curved surface, and a spherical shape.
  • the convex portion 3 has a columnar shape and is formed integrally with the base body 2.
  • the convex part 3 has a diameter of 50 to 150 nm and a length from the surface of the base 2 to the tip of the convex part 3 of 300 to 500 nm. That is, the convex portion 3 has an aspect ratio of 2 to 10 represented by a value obtained by dividing the length from the surface of the base 2 to the tip of the convex portion 3 by the length of the diameter of the convex portion 3. It has a high shape.
  • Such protrusions 3 are irregularly arranged on the surface of the base 2 with an interval of 5 to 30 nm.
  • the glass member 1 may be provided with the convex part 3 which has the above characteristics only on one surface, and may be provided also on the other surface.
  • the convex part 3 has a fluoride layer 4 mainly composed of a fluoride of one element selected from Na and Li which are alkali metals at the tip part.
  • the fluoride layer 4 is formed integrally with the convex portion 3 as a part of the convex portion 3.
  • CHF 3 was flowed into the chamber at a flow rate of 75 sccm to maintain the pressure in the chamber at 2 Pa. Subsequently, plasma was generated in the chamber with a high frequency output of 800 W, and the surface of the glass substrate A was reactive plasma etched for 40 minutes to produce a glass member etched with CHF 3 .
  • Example 1 after etching with CHF 3 , the inside of the chamber was evacuated, and O 2 gas was allowed to flow into the chamber at a flow rate of 50 sccm to maintain the pressure in the chamber at 4 Pa. Subsequently, plasma was generated in the chamber at a high frequency output of 200 W, and the surface of the glass substrate was reactive plasma etched for 10 minutes. Thus, a glass member that was etched with CHF 3 and O 2 (hereinafter referred to as an etching process) was produced.
  • an etching process a glass member that was etched with CHF 3 and O 2
  • the glass member after the etching treatment was immersed in the above-described ultrapure water, subjected to ultrasonic cleaning for 5 minutes, naturally dried at room temperature, and a glass member subjected to a water washing treatment was produced.
  • a glass member was also prepared by performing the etching process on the back surface of the glass member after the etching process.
  • the glass member was also washed with water after the etching treatment.
  • Example 1 As described above, in Example 1, four types of glass members were produced: a glass member etched with CHF 3 , a glass member after etching treatment, a glass member subjected to water washing treatment, and a glass member subjected to etching treatment on both sides. did.
  • Example 2 a glass substrate made of SCHOTT (D263 (registered trademark), hereinafter referred to as glass substrate B) having the same size as the glass substrate A and having the composition shown in Table 1 was used as the glass substrate.
  • the glass member of 2 embodiment was produced.
  • a glass member etched with CHF 3 and a glass member after the etching treatment were produced under the same manufacturing conditions as in Example 1.
  • FIG. 3 shows the transmittance of light of each wavelength in the glass member of Example 1.
  • the horizontal axis represents the wavelength of light
  • the vertical axis represents the light transmittance.
  • glass substrate is the measurement result of glass substrate A
  • after CHF 3 etching is the glass member etched with CHF 3
  • after O 2 etching is the measurement result of the glass member after etching treatment
  • After washing represents the measurement result of the glass member subjected to the washing treatment
  • Double-side treatment represents the measurement result of the glass member subjected to the etching treatment on both sides.
  • the light transmittance of the glass member etched with CHF 3 is higher than that of the glass substrate A except for light having a wavelength close to 400 nm. Therefore, it was confirmed that a glass member with improved light transmittance could be produced only by plasma etching.
  • the glass member after the etching treatment has improved transmittance of light having a wavelength close to 400 nm. This is because the carbide adhering to the surface of the glass substrate was oxidized by O 2 and removed from the surface of the glass substrate A. As a result, the light transmittance of the glass member of Example 1 was improved over the entire measured wavelength region as compared with the glass substrate A. Therefore, it was confirmed that a glass member with further improved light transmittance could be produced by etching with O 2 .
  • the light transmittance of the glass member subjected to the water washing treatment is higher in the entire wavelength region measured than the glass member after the etching treatment. This is because impurities and the like attached to the surface of the glass member are removed by washing with water. Thus, the light transmittance can be improved by washing the glass member with water.
  • the light transmittance of the glass member subjected to the etching treatment on both surfaces is measured in comparison with the glass member after the etching treatment and the glass member subjected to the water washing treatment, that is, the glass member subjected to the etching treatment only on one side.
  • the transmittance is high over the entire wavelength range and close to 99%.
  • the light transmittance of the glass member can be further improved by etching both surfaces of the glass member.
  • FIG. 6A is an AFM image showing the surface shape of the glass substrate A
  • FIG. 6B is an AFM image showing the surface shape of the glass member after the etching process of Example 1.
  • FIG. The white line shown in the figure is an index indicating a length of 1 ⁇ m.
  • index shown by the lower part in a figure is an parameter
  • FIG. 7A is CHF 3 by etching time 20 minutes the glass member
  • Figure 7B is CHF 3 by etching time of 30 minutes the glass member
  • Fig. 7C etching time of 40 minutes after the etching treatment of the glass member (Example 1 glass member)
  • Fig. 7D glass member 60 minutes the etching time by CHF 3 shows a cross-sectional SEM photograph of 80 minutes the glass member.
  • the convex portion of the glass member after the etching process of Example 1 has a diameter of about 50 to 150 nm, and the length from the surface of the base of the glass member to the tip of the convex portion.
  • FIG. 8B shows the analysis result of the glass member after the etching process of Example 2 and the analysis result of the glass substrate B.
  • Si2p, Si2s, and O1s peaks were observed, and other small NaKLL peaks were observed. Since no other large peak is observed, it can be seen that the surface of the glass substrate B mainly contains Si and O, and then contains a large amount of Na. Therefore, Si mainly bonds with O, and the surface of the glass substrate B mainly contains silicon oxide.
  • a concentrating solar cell includes, for example, a condensing unit composed of a Fresnel lens, a homogenizer for homogenizing sunlight collected by the condensing unit, and a solar cell. Etc.
  • the sunlight condensed by the condensing part is irradiated and homogenized by a homogenizer provided on the solar cell, and the uniformed sunlight is irradiated to the solar cell. Generate electromotive force.
  • the concentrating solar cell which used the glass member for the homogenizer was produced, and the characteristic of the said solar cell was evaluated.
  • a glass substrate made by Dr. Optics (LIBA2000) having almost the same composition as the glass substrate A is etched under the same conditions as in Example 1 to produce a glass member, and the glass member is used as a homogenizer.
  • a concentrating solar cell hereinafter referred to as solar cell SOE2
  • the light receiving surface of the homogenizer was etched.
  • the produced homogenizer is substantially hemispherical, and the light receiving surface is a curved surface.
  • the prepared concentrating solar cell is installed outdoors, shorts when sunlight is irradiated to the condensing type solar cell current density J SC and the power generation efficiency Eff. And the characteristics of the solar cell were evaluated. Power generation efficiency Eff and the short-circuit current density J SC. Measured twice at different times.
  • a concentrating solar cell (hereinafter referred to as solar cell Ref.) Using the glass substrate before the etching treatment as a homogenizer was produced, and its characteristics were similarly evaluated.
  • the present invention is not limited to the above-described embodiment, and can be appropriately changed within the scope of the gist of the present invention.
  • conditions for plasma etching with a fluorine-based gas, conditions for plasma etching with O 2 , a glass substrate cleaning method, a glass member water washing method, a glass member water repellent treatment method, and the like can be changed as appropriate.
  • the present invention is not limited to this, and the glass member etched with CHF 3 is used.
  • the water repellent treatment may be applied to the glass member subjected to the water washing treatment and the glass member subjected to the etching treatment on both surfaces.
  • the case where a glass member produced by etching a glass substrate having the same composition as that of the glass substrate A under the same conditions as in the embodiment 1 is used as a homogenizer has been described.
  • a glass member produced by etching the glass substrate with CHF 3 may be used, and the homogenizer may be washed with water.
  • the surface from which light is emitted from the homogenizer may be etched.
  • the shape of the homogenizer can be appropriately changed.
  • the light receiving surface may be a flat surface.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Optics & Photonics (AREA)
  • Plasma & Fusion (AREA)
  • Toxicology (AREA)
  • General Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Surface Treatment Of Glass (AREA)
  • Photovoltaic Devices (AREA)
  • Surface Treatment Of Optical Elements (AREA)

Abstract

La présente invention concerne : un procédé de production d'un élément en verre, grâce auquel il devient possible de produire facilement un élément en verre dont il est possible de faire varier les propriétés optiques ; et un élément en verre. Le procédé de production d'un élément en verre (1) selon la présente invention comprend une première étape de mise en œuvre d'une gravure au plasma de la surface d'un matériau de base en verre, qui contient au moins un élément sélectionné parmi un métal alcalin, un métal alcalino-terreux et une terre rare, avec un gaz contenant du fluor. Selon le procédé, une couche de fluorure (4) est formée sur la surface du matériau de base en verre durant la première étape, la couche de fluorure (4) sert de masque, et une partie couverte par le masque reste non gravée et forme une partie convexe (3), la couche de fluorure (4) étant formée à son extrémité. Par conséquent, il devient possible de produire facilement l'élément en verre (1), dont il est possible de faire varier les propriétés optiques, uniquement au moyen d'un traitement de gravure au plasma.
PCT/JP2014/066023 2013-12-18 2014-06-17 Procédé de production d'un élément en verre, et élément en verre Ceased WO2015093082A1 (fr)

Applications Claiming Priority (2)

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JP2013-260712 2013-12-18
JP2013260712A JP2015117147A (ja) 2013-12-18 2013-12-18 ガラス部材の製造方法及びガラス部材

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Publication number Priority date Publication date Assignee Title
WO2019159554A1 (fr) * 2018-02-13 2019-08-22 住友電気工業株式会社 Module photovoltaïque à concentrateur et dispositif photovoltaïque à concentrateur
WO2022185557A1 (fr) * 2021-03-05 2022-09-09 ナルックス株式会社 Procédé pour la fabrication d'une fine structure de surface irrégulière sur un substrat en verre

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WO2010007956A1 (fr) * 2008-07-17 2010-01-21 旭硝子株式会社 Substrat hydrophobe et son procédé de fabrication
WO2010128673A1 (fr) * 2009-05-07 2010-11-11 日本電気硝子株式会社 Substrat de verre et son procédé de production
WO2011004844A1 (fr) * 2009-07-08 2011-01-13 日本電気硝子株式会社 Plaque de verre
JP2011174001A (ja) * 2010-02-25 2011-09-08 Kazufumi Ogawa 撥水離水防汚処理液およびそれを用いた撥水離水性防汚膜とその製造方法およびそれらを用いた製品
WO2012141310A1 (fr) * 2011-04-15 2012-10-18 旭硝子株式会社 Procédé de fabrication d'un substrat de verre traité en surface
WO2012141311A1 (fr) * 2011-04-15 2012-10-18 旭硝子株式会社 Substrat de verre antireflet
JP2013087043A (ja) * 2011-10-21 2013-05-13 Mitsubishi Electric Corp 基板処理装置とその方法、および薄膜太陽電池
WO2013171846A1 (fr) * 2012-05-15 2013-11-21 三菱電機株式会社 Procédé de fabrication d'un substrat en verre et procédé de fabrication d'une batterie solaire en couche mince

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US8040607B2 (en) * 2008-04-25 2011-10-18 Jds Uniphase Corporation Surface-relief diffraction grating
JP5424154B2 (ja) * 2010-04-28 2014-02-26 公立大学法人大阪府立大学 光学部品
JP5071563B2 (ja) * 2011-01-19 2012-11-14 ソニー株式会社 透明導電性素子、入力装置、および表示装置

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2010007956A1 (fr) * 2008-07-17 2010-01-21 旭硝子株式会社 Substrat hydrophobe et son procédé de fabrication
WO2010128673A1 (fr) * 2009-05-07 2010-11-11 日本電気硝子株式会社 Substrat de verre et son procédé de production
WO2011004844A1 (fr) * 2009-07-08 2011-01-13 日本電気硝子株式会社 Plaque de verre
JP2011174001A (ja) * 2010-02-25 2011-09-08 Kazufumi Ogawa 撥水離水防汚処理液およびそれを用いた撥水離水性防汚膜とその製造方法およびそれらを用いた製品
WO2012141310A1 (fr) * 2011-04-15 2012-10-18 旭硝子株式会社 Procédé de fabrication d'un substrat de verre traité en surface
WO2012141311A1 (fr) * 2011-04-15 2012-10-18 旭硝子株式会社 Substrat de verre antireflet
JP2013087043A (ja) * 2011-10-21 2013-05-13 Mitsubishi Electric Corp 基板処理装置とその方法、および薄膜太陽電池
WO2013171846A1 (fr) * 2012-05-15 2013-11-21 三菱電機株式会社 Procédé de fabrication d'un substrat en verre et procédé de fabrication d'une batterie solaire en couche mince

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