CN111962023B - 一种光谱选择性反射膜及其制备方法 - Google Patents

一种光谱选择性反射膜及其制备方法 Download PDF

Info

Publication number
CN111962023B
CN111962023B CN202010855565.3A CN202010855565A CN111962023B CN 111962023 B CN111962023 B CN 111962023B CN 202010855565 A CN202010855565 A CN 202010855565A CN 111962023 B CN111962023 B CN 111962023B
Authority
CN
China
Prior art keywords
layer
film
infrared
visible light
gas
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.)
Active
Application number
CN202010855565.3A
Other languages
English (en)
Other versions
CN111962023A (zh
Inventor
王成龙
王锐东
李东锴
王天鹏
王良璧
马军
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.)
Lanzhou Jiaotong University
Original Assignee
Lanzhou Jiaotong University
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 Lanzhou Jiaotong University filed Critical Lanzhou Jiaotong University
Priority to CN202010855565.3A priority Critical patent/CN111962023B/zh
Publication of CN111962023A publication Critical patent/CN111962023A/zh
Application granted granted Critical
Publication of CN111962023B publication Critical patent/CN111962023B/zh
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • 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
    • C23C14/08—Oxides
    • C23C14/081—Oxides of aluminium, magnesium or beryllium
    • 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
    • C23C14/0021—Reactive sputtering or evaporation
    • 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
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive sputtering
    • 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
    • C23C14/08—Oxides
    • 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
    • C23C14/08—Oxides
    • C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • 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
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/34—Nitrides
    • C23C16/345—Silicon nitride
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
    • C23C16/511—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges using microwave discharges
    • 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
    • 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

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Sustainable Development (AREA)
  • Sustainable Energy (AREA)
  • Thermal Sciences (AREA)
  • Combustion & Propulsion (AREA)
  • General Engineering & Computer Science (AREA)
  • Plasma & Fusion (AREA)
  • Surface Treatment Of Glass (AREA)
  • Surface Treatment Of Optical Elements (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

本发明是一种光谱选择性反射膜及其制备方法，由缓冲层、红外反射层、可见光的减反射层构成；缓冲层构成物质为硬质Al2O3或Si3N4中的一种；红外反射层构成物质为AZO或Si3N4或ITO中的一种；所述可见光的减反射层构成物质为硬质SiO2或Si3N4中的一种。在透光性基材一面上依次制作缓冲层、红外反射层，在红外反射层之上、透光性基材另一面分别制作可见光的减反射层，或在透光性基材一面上依次制作红外反射层、缓冲层，在缓冲层之上、透光性基材另一面分别制作可见光的减反射层。该薄膜用于线性菲涅尔式聚光器的玻璃盖板表面，可以增加太阳光热能的利用率，提高了光学效率，有效的降低了热损失，为该***的运行提供了极大的支持。

Description

一种光谱选择性反射膜及其制备方法
技术领域
本发明属于太阳能光热光谱选择性膜技术领域，尤其属于光谱选择性反射膜线性菲涅尔式聚光集热领域。
背景技术
低辐射（Low emissivity，Low-E薄膜）薄膜是一种对波长范围2.5μm~40μm红外线有较高反射比，对可见光区具有高透射比的薄膜。根据膜系结构的不同，目前低辐射薄膜主要分为两大类体系：一类是以未掺杂或掺杂的宽禁带半导体为主的透明导电氧化物薄膜（TCO）；另一类是以电介质/金属/电介质等“三明治”多层结构为主的复合薄膜。以电介质/金属/电介质（D/M/D）为主的具有“三明治”结构的多层复合薄膜己成为目前世界上最为广泛使用的低辐射薄膜之一，与TCO薄膜相比，具有更加优异的低辐射特性。其基本结构如图1所示。其中金属层为功能层，采用Au、Ag、Al、Cu等，主要以Ag最为常见。Ag暴露于空气中，容易受到腐蚀。因此，银膜两侧必须添加介质层起保护作用。与玻璃基体接触的介质层作为金属层与玻璃之间的过渡层以增强两者之间的附着力。与空气接触的介质层（覆盖膜）主要用于保护金属层。金属基低辐射玻璃可以分为单银和双银（三银）低辐射膜系。与单银膜系结构相比，双银膜系结构在远红外区域具有更高的反射比，但其透过率比普通的单银膜系低。目前常用的典型Low-E玻璃的辐射率如表1所示。
Figure DEST_PATH_IMAGE001
Low-E膜层结构中，起红外高反射（低热发射比）作用的是金属Ag层，且Ag层越厚，则红外反射率越高，发射比越低（~0.1），同时，可见光的透过率也越低（约60%）。现有的工艺制备的Low-E膜层用作对可见光透过率要求不高的建筑节能玻璃是合适的，但是在一些对可见光透过率要求较高（＞85%）的领域，例如可见光窗口，应用将受到限制。研究人员通过利用铝掺杂氧化锌（AZO）和锡掺杂氧化铟（ITO）双层膜（AZO/ITO）替代银膜实现Low-E膜性能，实验条件下AZO/ITO的发射率0.07、平均可见光透过率为80%。结果验证了通过铝掺杂氧化锌（AZO）和锡掺杂氧化铟（ITO）替代Ag膜是解决现有工艺制备薄膜的可见光透过率较低的一种技术手段。但该可见光透过率仍然较低。
发明内容
本发明为了解决上述现有技术存在的问题，本发明提供了一种光谱选择性反射膜。同时提出其制备方法。
本发明的技术方案是：一种光谱选择性反射膜，由缓冲层、红外反射层、可见光的减反射层构成；所述缓冲层构成物质为硬质Al2O3或Si3N4中的一种；所述红外反射层构成物质为Al：ZnO或Si3N4或ITO中的一种；所述可见光的减反射层构成物质为硬质SiO2或Si3N4中的一种。
上述光谱选择性反射膜的制备方法：在透光性基材一面上依次制作缓冲层、红外反射层，在红外反射层之上、透光性基材另一面分别制作可见光的减反射层，或在透光性基材一面上依次制作红外反射层、缓冲层，在缓冲层之上、透光性基材另一面分别制作可见光的减反射层。
所述透光性基材为高硼硅玻璃。
优选的是：缓冲层构成物质为硬质Al2O3，红外反射层构成物质为AZO，可见光的减反射层构成物质为硬质SiO2。
其中硬质Al2O3的制备方法为：真空蒸发热氧化法，以纯度为99.99%的铝片为蒸发原料，经过去离子水清洗后放置于热蒸发干锅内，在本底真空为1×10-4Pa～4×10-4Pa的条件下通过热蒸发在玻璃基底上沉积一层厚度为30-50nm的铝膜；在真空蒸发室体内通入氧气，真空度为100-500Pa，关闭抽真空***，通过电偶加热的方式将室体内温度升高到500℃，保持7-9 h，在玻璃基体表面生成可见光透过率超过95%的氧化铝膜；
AZO（氧化锌掺铝，ZnO中掺杂2wt% Al2O3）薄膜的制备方法采用磁控溅射，制备过程为将AZO靶材放置在靶材基座上，调节Ar气流量，使压强为 0.3×10-2Pa～0.8×10-2Pa；调节溅射功率为100 W，控制溅射时间为20 min，得到所需要的AZO薄膜作为红外高反射（低辐射膜系）介质层，红外反射率＞91%，红外辐射率＜0.1；
硬质SiO2的制备方法为：采用中频磁控溅射镀膜方法制备，采用99.99%的多晶硅作为靶材，将本底真空抽到1×10-4Pa～9×10-4Pa后，通入Ar气与氧气，气体流量比为2:1，靶电压维持在300-400V，沉积厚度为80-100nm。
优选的是：缓冲层构成物质为Si3N4，红外反射层构成物质为ITO，可见光的减反射层构成物质为硬质SiO2。
其中Si3N4的制备方法：微波增强化学气相沉积(PECVD)，采用体积分数为5%的SiH4（Ar：SiH4=19:1）和高纯N2作为气源，其中氮气通入到放电室参与微波等离子体放电，气体流量为10-80 sccm，硅烷气体通入等离子体下游区域，气体流量为5-50 sccm，与N离子作用在基体上沉积形成Si3N4，沉积过程中温度为基体温度为350℃，微波功率为500-700W，氮化硅薄膜的粗糙度为1.3-1.5nm，制成的薄膜，厚度50-300nm，折射率在2.0；
ITO的制备方法：射频磁控溅射法制备ITO薄膜，高纯Ar作为工作气体，高纯O2作为反应气体，靶材为ITO（In2O3和SnO2质量分数比为9:1）氧化物陶瓷靶，纯度为99.99%，本底真空度为4.0×10-4Pa，镀膜时的基底温度为200℃，射频功率为130-150W，溅射时真空室体内压力位1-2Pa，氩气与氧气气体流量比为99:1，溅射ITO薄膜1-1.5μm；红外反射率＞91%，红外辐射率＜0.1；
硬质SiO2的制备方法为：采用中频磁控溅射镀膜方法制备，采用99.99%的多晶硅作为靶材，将本底真空抽到1×10-4Pa～9×10-4Pa后，通入Ar气与氧气，气体流量比为2:1，靶电压维持在300-400V，沉积厚度为80-100nm。
本发明的有益效果是：缓冲层、红外反射层、可见光的减反射层相互协调、共同作用，当太阳光直射到玻璃表面时，一部分光发生反射，另一部分光透过玻璃表面，光谱选择性反射膜的厚度介于280nm~2.5μm之间，在该厚度下，可见光透过率达到90%以上，从而保证了光的高透过率，同时对＞2.5μm的红外光具有高反射率和低的红外热发射比（~0.1）。如将该薄膜用于线性菲涅尔式聚光器开口处的玻璃盖板表面，可以增加太阳光热能的利用率，提高了光学效率，有效的降低了热损失。
附图说明
图1是低辐射玻璃基本结构；
图2是实施例1结构示意图；
图3是实施例2结构示意图。
具体实施方式
实施例1
光谱选择性反射膜，缓冲层构成物质为硬质Al2O3，红外反射层构成物质AZO，可见光的减反射层构成物质为硬质SiO2，
硬质Al2O3的制备方法为：真空蒸发热氧化法，以纯度为99.99%的铝片为蒸发原料，经过去离子水清洗后放置于热蒸发干锅内，在本底真空约为3×10-4Pa的条件下通过热蒸发在玻璃基底上沉积一层厚度为30-50nm的铝膜；在真空蒸发室体内通入氧气，真空度为350Pa，关闭抽真空***，通过电偶加热的方式将室体内温度升高到500℃，保持8 h，在玻璃基体表面生成可见光透过率超过95%的氧化铝膜；
AZO（氧化锌掺铝，ZnO中掺杂2wt% Al2O3）薄膜的制备方法采用磁控溅射，制备过程为将AZO靶材放置在靶材基座上，调节Ar气流量，使压强为 0.5×10-2Pa；调节溅射功率为100 W，控制溅射时间为20 min，得到所需要的AZO薄膜作为红外高反射（低辐射膜系）介质层，红外反射率为91%，红外辐射率0.09；
硬质SiO2的制备方法为：采用中频磁控溅射镀膜方法制备，采用99.99%的多晶硅作为靶材，将本底真空抽到3×10-4Pa后，通入Ar气与氧气，气体流量比为2:1，靶电压维持在350V，沉积厚度为90nm。
经测试，该光谱选择性反射膜的红外反射率为91%，可见光透过率为90%。
实施例2
光谱选择性反射膜，缓冲层构成物质为Si3N4，红外反射层构成物质为ITO，可见光的减反射层构成物质为硬质SiO2，
其中Si3N4的制备方法：微波增强化学气相沉积（PECVD），采用体积分数为5%的SiH4（Ar：SiH4=19:1）和高纯N2作为气源，其中氮气通入到放电室参与微波等离子体放电，气体流量为10-80 sccm，硅烷气体通入等离子体下游区域，气体流量为5-50 sccm，与N离子作用在基体上沉积形成Si3N4，沉积过程中温度为基体温度为350℃，微波功率为600W，氮化硅薄膜的粗糙度为1.3-1.5nm，制成的薄膜，厚度200nm，折射率在2.0；
ITO的制备方法：射频磁控溅射法制备ITO薄膜，高纯Ar作为工作气体，高纯O2作为反应气体，靶材为ITO（In2O3和SnO2质量分数比为9:1）氧化物陶瓷靶，纯度为99.99%，本底真空度为4.0×10-4Pa，镀膜时的基底温度为200℃，射频功率为150W，溅射时真空室体内压力位1.5Pa，氩气与氧气气体流量比为99:1，溅射ITO薄膜1.3μm；红外反射率90%，红外辐射率0.1；
硬质SiO2的制备方法为：采用中频磁控溅射镀膜方法制备，采用99.99%的多晶硅作为靶材，将本底真空抽到3×10-4Pa后，通入Ar气与氧气，气体流量比为2:1，靶电压维持在350V，沉积厚度为100nm。
经测试，该光谱选择性反射膜的红外反射率为90%，可见光透过率为91%。
由以上方法制得的介质能够使缓冲层、红外反射层、可见光的减反射层相互协调、共同作用，当太阳光直射到玻璃表面时，极少部分可见光光发生反射，绝大部分可见光透过玻璃表面，光谱选择性反射膜的厚度介于280nm~2.5μm之间，在该厚度下，光的透过率达到90%以上，中红外波段反射率达到90%，从而保证了光的高透过率。

Claims (1)

1.一种提高红外反射率的光谱选择性反射膜，其特征是：由缓冲层、红外反射层、可见光的减反射层构成；
缓冲层构成物质为Si3N4，红外反射层构成物质为ITO，可见光的减反射层构成物质为硬质SiO2；
在透光性基材一面上依次制作缓冲层、红外反射层，在红外反射层之上、透光性基材另一面分别制作可见光的减反射层，或在透光性基材一面上依次制作红外反射层、缓冲层，在缓冲层之上、透光性基材另一面分别制作可见光的减反射层；
所述透光性基材为高硼硅玻璃；
Si3N4的制备方法：微波增强化学气相沉积，采用体积分数为5%的SiH4和高纯N2作为气源，其中氮气通入到放电室参与微波等离子体放电，气体流量为10-80 sccm，硅烷气体通入等离子体下游区域，气体流量为5-50 sccm，与N离子作用在基体上沉积形成Si3N4，沉积过程中温度为基体温度为350℃，微波功率为500-700W，氮化硅薄膜的粗糙度为1.3-1.5nm，制成的薄膜，厚度50-300nm，折射率在2.0；
ITO的制备方法：射频磁控溅射法制备ITO薄膜，高纯Ar作为工作气体，高纯O2作为反应气体，靶材为ITO氧化物陶瓷靶，纯度为99.99%，本底真空度为4.0×10-4 Pa，镀膜时的基底温度为200℃，射频功率为130-150W，溅射时真空室体内压力位1-2Pa，氩气与氧气气体流量比为99:1，溅射ITO薄膜1-1.5μm；红外反射率＞90%，红外辐射率＜0.1；
硬质SiO2的制备方法为：采用中频磁控溅射镀膜方法制备，采用99.99%的多晶硅作为靶材，将本底真空抽到1×10-4 Pa～9×10-4 Pa后，通入Ar气与氧气，气体流量比为2:1，靶电压维持在300-400V，沉积厚度为80-100nm。
CN202010855565.3A 2020-08-24 2020-08-24 一种光谱选择性反射膜及其制备方法 Active CN111962023B (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010855565.3A CN111962023B (zh) 2020-08-24 2020-08-24 一种光谱选择性反射膜及其制备方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010855565.3A CN111962023B (zh) 2020-08-24 2020-08-24 一种光谱选择性反射膜及其制备方法

Publications (2)

Publication Number Publication Date
CN111962023A CN111962023A (zh) 2020-11-20
CN111962023B true CN111962023B (zh) 2022-09-20

Family

ID=73390750

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010855565.3A Active CN111962023B (zh) 2020-08-24 2020-08-24 一种光谱选择性反射膜及其制备方法

Country Status (1)

Country Link
CN (1) CN111962023B (zh)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112626453B (zh) * 2020-12-15 2022-10-04 武汉正源高理光学有限公司 一种铝加铬薄膜及其制备方法和应用
CN113403583B (zh) * 2021-06-18 2023-02-07 陕西科技大学 一种柔性光热吸收材料及其制备方法和应用
CN115707260A (zh) * 2021-08-04 2023-02-17 隆基绿能科技股份有限公司 一种钙钛矿电池及光伏组件
CN115231834A (zh) * 2022-07-05 2022-10-25 中南大学 一种内外侧辐射特性双向调控的辐射制冷玻璃设计方法

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103884122A (zh) * 2012-12-21 2014-06-25 中国建筑材料科学研究总院 一种太阳能光热转换集热器透明热镜及其制备方法

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI230798B (en) * 2004-02-19 2005-04-11 Univ Nat Formosa Flexible plastic substrate for optical display and producing process

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103884122A (zh) * 2012-12-21 2014-06-25 中国建筑材料科学研究总院 一种太阳能光热转换集热器透明热镜及其制备方法

Also Published As

Publication number Publication date
CN111962023A (zh) 2020-11-20

Similar Documents

Publication Publication Date Title
CN111962023B (zh) 一种光谱选择性反射膜及其制备方法
WO2019214037A1 (zh) 一种曲面镀膜板及其制备方法和一种太阳能组件
CN108516699B (zh) 一种低辐射镀膜玻璃
CN103864315B (zh) 一种银钛复合功能层低辐射节能玻璃及其制备方法
CN102683433B (zh) 带有双面减反射膜的薄膜太阳能电池用导电玻璃及其制备方法
CN112194383A (zh) 一种低辐射玻璃及其制备方法
CN112071930A (zh) 光伏建筑一体化用蓝色盖板玻璃及其制备方法
CN109457219B (zh) 一种中低温太阳光谱选择性吸收涂层及其制备方法
CN102336529A (zh) 高透可钢化低辐射玻璃及其制造方法
CN102683436B (zh) 一种薄膜太阳能电池用导电玻璃及其制备方法
Xu et al. Optical optimization and thermal stability of SiN/Ag/SiN based transparent heat reflecting coatings
CN102683435B (zh) 薄膜太阳能电池用导电玻璃及其制备方法
CN103137717A (zh) 铜掺杂氧化锡透明导电薄膜及其制备方法
CN217868650U (zh) 一种单银层htle玻璃
CN1948201A (zh) 热稳定低辐射复合膜玻璃及其生产工艺
CN111393038A (zh) 一种中透低反灰色双银低辐射镀膜玻璃及制备方法
CN116394610A (zh) 一种柔性透明辐射制冷窗材料
CN108468033B (zh) 一种耐高温太阳能选择性吸收涂层及其制备方法
CN110128027B (zh) 一种多级渐变式自发调温的复合涂层及其制备方法
CN104034072B (zh) 太阳光谱选择性吸收涂层及其制备方法以及应用
CN102683434B (zh) 带有单面减反射膜的薄膜太阳能电池用导电玻璃及其制备方法
CN210030460U (zh) 一种可后续加工含铜双银低辐射镀膜玻璃
CN212476547U (zh) 一种中透低反灰色双银低辐射镀膜玻璃
CN111204987B (zh) 一种玻璃型热控涂层及其制备方法
CN114086121A (zh) 一种高性能辐射制冷无机多层膜

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant