US20120263885A1 - Method for the manufacture of a reflective layer system for back surface mirrors - Google Patents

Method for the manufacture of a reflective layer system for back surface mirrors Download PDF

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Publication number
US20120263885A1
US20120263885A1 US13/444,298 US201213444298A US2012263885A1 US 20120263885 A1 US20120263885 A1 US 20120263885A1 US 201213444298 A US201213444298 A US 201213444298A US 2012263885 A1 US2012263885 A1 US 2012263885A1
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Prior art keywords
layer
substrate
reflective layer
reflective
manufacture
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US13/444,298
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English (en)
Inventor
Christoph Koeckert
Markus Berendt
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Von Ardenne Anlagentechnik GmbH
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Von Ardenne Anlagentechnik GmbH
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Assigned to VON ARDENNE ANLAGENTECHNIK GMBH reassignment VON ARDENNE ANLAGENTECHNIK GMBH ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: BERENDT, MARKUS, KOECKERT, CHRISTOPH
Publication of US20120263885A1 publication Critical patent/US20120263885A1/en
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    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/08—Mirrors
    • G02B5/0816—Multilayer mirrors, i.e. having two or more reflecting layers
    • G02B5/085—Multilayer mirrors, i.e. having two or more reflecting layers at least one of the reflecting layers comprising metal
    • G02B5/0858—Multilayer mirrors, i.e. having two or more reflecting layers at least one of the reflecting layers comprising metal the reflecting layers comprising a single metallic layer with one or more dielectric layers
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/10—Glass or silica
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F24—HEATING; RANGES; VENTILATING
    • F24S—SOLAR HEAT COLLECTORS; SOLAR HEAT SYSTEMS
    • F24S23/00—Arrangements for concentrating solar-rays for solar heat collectors
    • F24S23/70—Arrangements for concentrating solar-rays for solar heat collectors with reflectors
    • F24S23/82—Arrangements for concentrating solar-rays for solar heat collectors with reflectors characterised by the material or the construction of the reflector
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/08—Mirrors
    • G02B5/0816—Multilayer mirrors, i.e. having two or more reflecting layers
    • G02B5/085—Multilayer mirrors, i.e. having two or more reflecting layers at least one of the reflecting layers comprising metal
    • G02B5/0875—Multilayer mirrors, i.e. having two or more reflecting layers at least one of the reflecting layers comprising metal the reflecting layers comprising two or more metallic layers
    • 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
    • Y02E10/40—Solar thermal energy, e.g. solar towers

Definitions

  • the invention generally refers to a method for the manufacture of a reflective layer system for back surface mirrors, which is deposited on a substrate, and which comprises at least one reflective layer as well as at least one silicon oxide containing layer.
  • the invention refers in particular to a method for the manufacture of such a layer system for solar applications.
  • Reflective layer systems have always been used in many different areas of life; however they have become increasingly more important today, e.g. for mirrors that aid the solution concerning energy. While mirrors for common interior use, ‘only’ need to reflect the visible components of the light spectrum, they must reflect the entire spectrum of sun light for new solar applications, preferably, wavelengths within a range of approximately 300 to approximately 2500 nm.
  • a reflective layer system comprises a reflective layer or several reflective layers, which combined contribute to the desired high reflection.
  • this is mostly a combination of a silver and a copper layer, wherein the silver layer faces the incident light and the copper layer acts as a protective layer of the silver, however given the layer thickness of the silver does not contribute to the reflection.
  • other highly reflective materials may be considered such as aluminium, gold, silver, chrome, platinum or molybdenum.
  • Back surface mirrors are mirrors that have the reflective coating on the back surface of the substrate facing away from the incident light.
  • the quality of a reflective layer system is determined also by the value of its Total Solar Reflectivity (TSR); that is, its capacity to reflect solar radiation. This value is determined mainly by the reflection capacity of its coating in addition to the loss of absorption through the substrate itself.
  • TSR Total Solar Reflectivity
  • silver mainly as a reflective layer and a substrate particularly low in absorption and highly transparent, e.g. so called white glass or solar glass are used.
  • white glass or solar glass are used on the back surface.
  • the silver layer is then finished with a copper layer, which at the same time serves as an interface layer for a possible subsequent lacquer coating.
  • Such reflective layer systems on back surface mirrors can be described as follows. Subsequent to a suitable prior necessary processing, which can comprise the cutting into a required shape, the grinding of the edges of the substrate, their bending and/or tempering of the flat or already bended substrate and other steps, they are, if necessary, polished and washed again. Still wet, they are then activated through an adhesive-promoting tin chloride solution. Subsequently, the plate moves through coating stations one-by-one, where it is coated with silver in a wet-chemical manner, and directly following, coated with copper.
  • a suitable prior necessary processing which can comprise the cutting into a required shape, the grinding of the edges of the substrate, their bending and/or tempering of the flat or already bended substrate and other steps, they are, if necessary, polished and washed again. Still wet, they are then activated through an adhesive-promoting tin chloride solution. Subsequently, the plate moves through coating stations one-by-one, where it is coated with silver in
  • mirrors with a TSR of for instance 93%-94% and a solar glass thickness of 4 mm can be manufactured using the described method. This value is below the obtainable values which could be determined through simulation calculations using corresponding tabulated optical data for silver.
  • a reflective layer system frequently can comprise one, mostly several reflection-enhancing layers that consist of dielectric, low absorptive material.
  • double and multi-layered alternating layer systems on glass substrates which comprise at least one series of layers containing a dielectric layer with a high refractive index, which is facing the incident light, and a transparent dielectric layer with a low refractive index. Because of such a function, the alternating layer system is arranged on the incident light facing side of the reflective layer system.
  • Having a high refractive index in regards to solar applications means a material with a refractive index of greater than 2.0, and having a low refractive index means a refractive index of less than 1.8, preferably less than 1.65.
  • One object of the invention is to present a method for the manufacture of a reflective layer system through which a higher reflection can be achieved in a cost-effective way.
  • a method which makes use of known and tested wet-chemical methods for the deposition of the reflective layer or the reflective layers that have very good reflective characteristics, and which combines these layers with at least one dielectric, transparent and silicon oxide containing layer.
  • the latter in particular, is preferred as a component of the reflective layer system because of its chemical and mechanical resistance.
  • their optical characteristics can be adjusted very easily via the deposition procedure and/or their proportion of reactive gas if the deposition takes place using PVD, preferably using sputtering, so that the substrate or an already on the substrate deposited stack of layers of several transparent layers is covered through the use of a silicon oxide containing layer for the dielectric, transparent layer by a material, which has the preferred optical, chemical and mechanical characteristics comparable to the characteristics of the glass substrate.
  • a silicon oxide containing layer as an under-layer proves itself as advantageous, as it presents a cover layer, which can serve temporarily as a preliminary product that is coated using PVD, and as it enables the transfer out of vacuum for further coating.
  • a preliminary product is manufactured, which is very flexibly applicable in regard to further processing, so that the following procedural steps are largely disconnected from prior steps.
  • the covering of the uncoated or coated substrate with a silicon oxide containing layer permits the subsequent wet-chemical deposition, under normal pressure, of differently structured reflective layers or layer systems as it is known from the direct coating of substrates.
  • a subsequently wet-chemically deposited silver containing reflective layer has good adhesive characteristics in contrast to silver layers deposited using PVD.
  • the method according to the invention permits that both the second and first, in a vacuum conducted, portions of the method can largely be varied and optimized separately.
  • the variation refers, in particular, in this case to the amount and order of the individual layers or optional pre-treatments, e.g. the materials used, the addition of adhesive-promoting layers in several necessary or beneficial locations, or a preferred order of the transparent, dielectric layers.
  • the optimization refers, in particular, to the procedural parameters, so that beneficial or pre-defined characteristics can be adjusted. For instance, it is known that the refractive index of the silicon oxide can be manipulated via the oxygen and nitrogen levels or via the regulation of the procedure.
  • the method according to the invention permits an intermediate storage between both basic stages of the method.
  • various pre-treatments of the preliminary product can take place prior to and/or following the outward transfer from the vacuum of the preliminary product.
  • the known chemical activation of the preliminary product can be used prior to the wet-chemical deposition, e.g. using a tin chloride solution or another suitable solution for a subsequent deposition of the silver.
  • the silicon oxide containing layer can be coated with an adhesive layer using PVD methods. Only a small thickness of such an adhesive layer within a range of 5 mn is necessary.
  • a silicon oxide containing layer has the advantage that this layer can be part of a reflection-enhancing, transparent alternating layer system, which comprises, according to one embodiment of the invention, at least one dielectric layer with a high refractive index facing the incident light and the silicon oxide containing layer as a layer with a low refractive index. Also, other sequences of an alternating layer system with a silicon oxide containing layer as a finishing layer are possible.
  • the associated drawing presents an embodiment of a reflective layer system of a back surface mirror.
  • the reflective layer system according to the FIGURE comprises a substrate S, which faces the incident light.
  • the incident light is represented by three arrows.
  • the substrate S all common materials can be used, e.g. glass or plastic, also flexible materials.
  • the following layers are deposited one-by-one through magnetron sputtering without any further pre-treatments in a vacuum and of the following thicknesses:
  • the deposition of these four layers takes place always through magnetron sputtering.
  • the adhesive-promoting layers HS are manufactured either from a ceramic target with or without an additional inlet of oxygen in DC or MF mode, or from a metallic target in a fully reactive mode with an inlet of oxygen in MF mode.
  • the sputtering process is operated in an oxidic mode.
  • particular intensive plasma combined with small sputtering rates is realized.
  • carbonaceous contaminations which usually have a negative effect on the adhesiveness, are oxidized to gaseous CO 2 , which can be evacuated via the vacuum pump.
  • the dielectric, transparent layer with a high refractive index of the alternating layer system WS consistent with this embodiment consists of TiO 2 or of comparably well adhering material, the first adhesive-promoting layer HS can be omitted.
  • the layers of the alternating layer system WS are deposited in one embodiment of the method in a reactive MF mode.
  • the dielectric layer with a high refractive index is deposited from a metallic target in a fully reactive MF mode with an inlet of oxygen.
  • it can also be deposited from a ceramic target with a small, additional inlet of oxygen in MF mode.
  • the sputtering process can be, on the one hand, operated in an oxidic mode.
  • the sputtering process can be operated within the transitional range between oxidic and metallic range in a so called transition mode in a controlled manner. This range is characteristic of no or low absorption at significantly higher coating rates through a suitable choice of an operating point in comparison to the oxidic mode.
  • the dielectric SiO 2 -layer with a low refractive index is deposited either from the metallic target in fully reactive MF mode with an inlet of oxygen, or in voltage regulated transition mode.
  • the operating point of the sputtering process is here adjusted using the voltage of the process and arranged above the inlet of oxygen. In this way, significantly higher coating rates are obtained at a smaller partial pressure of the oxygen than in the fully reactive oxidic mode.
  • the alternating layer system is complemented by a further thin adhesive-promoting layer HS, which is deposited from the ceramic target without or with only a small, additional inlet of oxygen in DC or MF mode.
  • the layer created in this way serves as an adhesive-promoting layer between the dielectric SiO 2 and the reflective layer R that is to be deposited subsequently. It is not necessary that this layer has a closed surface. It can be understood as a so called seed layer. For this reason, very small layer thicknesses are sufficient in this case. They are usually below 5 nm, preferably smaller than 1 nm.
  • the coated substrate is transferred out of the vacuum subsequently, and using a wet-chemical method, the following layers are deposited one-by-one:
  • the light incidence takes place in the Figure through the substrate S, so that the metallic, reflective layer R is facing the light incidence in comparison to the metallic, reflective functional layer F.
  • the layer system according to the Figure is coated on the side facing away from the incident light with a lacquer, which, in the embodiment, has three lacquer layers L 1 , L 2 , L 3 , outside the vacuum system, and subsequently is dried. Alternatively, individual lacquer layers or other lacquer systems are possible too.
  • a pre-treated surface O of the substrate is produced through the deposition of the first adhesive-promoting layer HS.
  • a pre-treatment of the surface of the substrate S that is to be coated can take place alternatively also through a direct current (DC) or medium frequency (MF) glow discharge, which mostly is ignited in a rarefied gas atmosphere, that can contain Ar, O 2 , N2, CDA (Compressed Dry Air) or any combination of these, at a pressure of 2-5 ⁇ 10 ⁇ 2 .
  • DC direct current
  • MF medium frequency
  • the first adhesive-promoting layer HS or a pre-treatment can also be omitted, so that the silicon oxide containing layer or the alternating layer system as described in the above embodiment are directly deposited on the substrate S. This is possible, for instance if the first layer that is to be deposited on the substrate S of the alternating layer system WS is made of titanium oxide or a comparably well adhering material.
  • the second adhesive-promoting layer HS is optional as the silicon oxide containing layer SiOS that is to finish the alternating layer system WS has a good mechanical and chemical resistance, and thus, is suitable for the subsequent outward transfer and further treatment of the substrate taking place in atmospheric conditions.
  • the adhesive-promoting layer HS can be omitted in this reflective layer system.
  • a chemical activation of the surface of the silicon oxide containing layer SiOS through the known method using a solution acting as an adhesive agent, e.g. tin chloride, can take place as it is known from purely wet-chemically executed methods.
  • the ZAO adhesive-promoting layer HS can be omitted also in this reflective layer system, in this case the first adhesive-promoting layer HS.
  • the materials used for the reflective layer R and the reflective, functional layer F can deviate from the silver or copper as stated in this case.
  • other metals can be used such as aluminium, gold, platinum or an alloy, which contains at least one of the mentioned metals.
  • the mentioned metals all have a comparably high, in particular, solar reflection, if necessary for certain wavelengths such as for gold and platinum, and thus, are suitable for the reflective layer system.
  • the metallic, reflective functional layer F materials such as copper, nickel, chrome, stainless steel, silicon, tin, zinc or an alloy, which contains at least one of the mentioned metals, are considered. Through these materials, the reflective characteristics can be combined with mechanical and/or chemical protection.
  • dielectric layer with a high refractive index of the alternating layer system various materials can be used, e.g. also niobium oxide (Nb 2 O 5 ).
  • the adhesive-promoting layer HS other materials can be used as an alternative, e.g. materials made of a group of oxides comprising ZnOx, SiOx, SnOx, TiOx or ZrOx, wherein x ⁇ 2.
  • mirrors can be manufactured with a TSR according to ISO 9050:2003 of up to 95% using the layer system according to the invention, e.g. according to the above embodiments and the method of its manufacture for instance with a solar glass thickness of 4 mm.
US13/444,298 2011-04-15 2012-04-11 Method for the manufacture of a reflective layer system for back surface mirrors Abandoned US20120263885A1 (en)

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Application Number Priority Date Filing Date Title
DE102011007500.3 2011-04-15
DE102011007500 2011-04-15
DE102011080961.9 2011-08-15
DE102011080961A DE102011080961A1 (de) 2011-04-15 2011-08-15 Verfahren zur Herstellung eines Reflexionsschichtsystems für Rückseitenspiegel

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20170165513A1 (en) * 2014-02-13 2017-06-15 Zhejiang Geely Autombile Research Institute Co., Ltd Thermal management and automatic fire-extinguishing system of vehicle battery
JP2020510596A (ja) * 2017-03-01 2020-04-09 ガーディアン・グラス・エルエルシーＧｕａｒｄｉａｎ Ｇｌａｓｓ， Ｌｌｃ 銀系赤外線（ＩＲ）反射層を保護するための銀ドープ保護層を有する（低放射率）ｌｏｗ−Ｅコーティングを有するコーティングされた物品、及びその製造方法
US20220380896A1 (en) * 2021-05-27 2022-12-01 Tokyo Electron Limited Semiconductor process surface monitoring

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102019219177A1 (de) * 2019-12-09 2021-06-10 Carl Zeiss Smt Gmbh Optisches Element mit einer Schutzbeschichtung, Verfahren zu dessen Herstellung und optische Anordnung

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US5757564A (en) * 1994-01-10 1998-05-26 Pilkington Glass Limited Coatings on glass
US20010031365A1 (en) * 1999-05-20 2001-10-18 Charles Anderson Transparent substrate with an antireflection, low-emissivity or solar-protection coating
US20020187350A1 (en) * 2001-01-29 2002-12-12 Honeywell International Inc. Robust highly reflective optical construction
US20090233106A1 (en) * 2008-03-11 2009-09-17 Ppg Industries Ohio, Inc. Reflective article and method of making a reflective article
US20100200413A1 (en) * 2009-02-11 2010-08-12 United Solar Ovonic Llc Solution deposition method and apparatus with partiphobic substrate orientation
US20100271694A1 (en) * 2007-11-22 2010-10-28 Pilkington Group Limited Solar mirror
US20110070417A1 (en) * 2008-03-18 2011-03-24 Saint-Gobain Glass France Substrate provided with a stack having thermal properties

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US7067195B2 (en) * 2002-04-29 2006-06-27 Cardinal Cg Company Coatings having low emissivity and low solar reflectance
DE102006024524A1 (de) * 2006-05-23 2007-12-06 Von Ardenne Anlagentechnik Gmbh Infrarotstrahlung reflektierendes, transparentes Schichtsystem
DE102006037909A1 (de) * 2006-08-11 2008-02-14 Von Ardenne Anlagentechnik Gmbh Temperbares, Infrarotstrahlung reflektierendes Schichtsystem und Verfahren zu seiner Herstellung

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US5757564A (en) * 1994-01-10 1998-05-26 Pilkington Glass Limited Coatings on glass
US20010031365A1 (en) * 1999-05-20 2001-10-18 Charles Anderson Transparent substrate with an antireflection, low-emissivity or solar-protection coating
US20020187350A1 (en) * 2001-01-29 2002-12-12 Honeywell International Inc. Robust highly reflective optical construction
US20100271694A1 (en) * 2007-11-22 2010-10-28 Pilkington Group Limited Solar mirror
US20090233106A1 (en) * 2008-03-11 2009-09-17 Ppg Industries Ohio, Inc. Reflective article and method of making a reflective article
US20110070417A1 (en) * 2008-03-18 2011-03-24 Saint-Gobain Glass France Substrate provided with a stack having thermal properties
US20100200413A1 (en) * 2009-02-11 2010-08-12 United Solar Ovonic Llc Solution deposition method and apparatus with partiphobic substrate orientation

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20170165513A1 (en) * 2014-02-13 2017-06-15 Zhejiang Geely Autombile Research Institute Co., Ltd Thermal management and automatic fire-extinguishing system of vehicle battery
US10035032B2 (en) * 2014-02-13 2018-07-31 Zhejiang Geely Automobile Research Institute Co., Ltd. Thermal management and automatic fire-extinguishing system of vehicle battery
JP2020510596A (ja) * 2017-03-01 2020-04-09 ガーディアン・グラス・エルエルシーＧｕａｒｄｉａｎ Ｇｌａｓｓ， Ｌｌｃ 銀系赤外線（ＩＲ）反射層を保護するための銀ドープ保護層を有する（低放射率）ｌｏｗ−Ｅコーティングを有するコーティングされた物品、及びその製造方法
JP7022142B2 (ja) 2017-03-01 2022-02-17 ガーディアン・グラス・エルエルシー 銀系赤外線（ＩＲ）反射層を保護するための銀ドープ保護層を有する（低放射率）ｌｏｗ－Ｅコーティングを有するコーティングされた物品、及びその製造方法
US20220380896A1 (en) * 2021-05-27 2022-12-01 Tokyo Electron Limited Semiconductor process surface monitoring

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ES2404782B1 (es) 2014-08-08
ES2404782A1 (es) 2013-05-28
DE102011080961A1 (de) 2012-10-18

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