JP2000034557A - Reflection enhancing film for near infrared rays and production of the same - Google Patents
Reflection enhancing film for near infrared rays and production of the sameInfo
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- JP2000034557A JP2000034557A JP10201475A JP20147598A JP2000034557A JP 2000034557 A JP2000034557 A JP 2000034557A JP 10201475 A JP10201475 A JP 10201475A JP 20147598 A JP20147598 A JP 20147598A JP 2000034557 A JP2000034557 A JP 2000034557A
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は近赤外線用反射鏡の
増反射膜およびその製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a reflective film for a near-infrared reflecting mirror and a method of manufacturing the same.
【０００２】[0002]
【従来の技術】発振波長１．０６μｍのＹＡＧレーザ用
反射鏡などの近赤外線用反射鏡は、ＢＫ−７ガラス（商
品名：硼珪クラウンガラス）や石英ガラスなどの基材の
表面に、必要によりＡｕ膜をコートした基板（反射鏡の
部材）上に、誘電体の多層膜（高屈折率材料の膜と低屈
折率材料の膜とを交互に積層した増反射コーティング
膜）をコーティングすることにより反射率を高めた構造
となっている。増反射コーティング膜は散乱損失および
吸収損失をできるだけ少なくする必要があり、低屈折率
材料としてはＳｉＯ2 が、高屈折率材料としてはＴｉＯ
2 、Ｔａ2 Ｏ5 又はＨｆＯ2 などが用いられている。従
来の近赤外線用反射鏡の膜構造の１例を図２に示すが、
ＢＫ−７ガラスや石英ガラスからなる基材１の表面にＴ
ｉＯ2 、Ｔａ2 Ｏ5 又はＨｆＯ2 などの高屈折率材料の
膜からなる高屈折率層３と、ＳｉＯ2 などの低屈折率材
料の膜からなる低屈折率層２とが交互に１５層以上積層
された構造となっており、反射率は９９．０％以上とな
っている。増反射膜はそれぞれの膜の界面での反射を利
用して反射率を高めている。従って界面が多いほど（膜
の層数が多いほど）高反射率となる。また、界面での反
射の大小は膜材料の屈折率の差で決まり、その差が大き
いほど反射率は大きくなる。従来多用されている低屈折
率膜材料であるＳｉＯ2 の屈折率は１．５、高屈折率膜
材料であるＴｉＯ2 、Ｔａ2 Ｏ5 およびＨｆＯ2 の屈折
率はそれぞれ２．２、２．１および１．９であり、９
９．０％以上の反射率を得るためには１５層以上、９
９．５％以上の反射率を達成するためには２１層以上が
必要とされている。2. Description of the Related Art A near-infrared reflecting mirror such as a reflecting mirror for a YAG laser having an oscillation wavelength of 1.06 .mu.m is required on the surface of a base material such as BK-7 glass (trade name: borosilicate crown glass) or quartz glass. Coating on a substrate (reflective mirror member) coated with an Au film by the method described above, a dielectric multilayer film (increased reflection coating film in which a film of a high refractive index material and a film of a low refractive index material are alternately laminated). The structure has a higher reflectivity. It is necessary to reduce scattering loss and absorption loss of the high reflection coating film as much as possible. SiO 2 is used as a low refractive index material, and TiO is used as a high refractive index material.
2 , Ta 2 O 5 or HfO 2 is used. FIG. 2 shows an example of a film structure of a conventional near-infrared reflecting mirror.
The surface of the substrate 1 made of BK-7 glass or quartz glass has T
Fifteen high-refractive-index layers 3 made of a film of a high-refractive-index material such as iO 2 , Ta 2 O 5, or HfO 2 and low-refractive-index layers 2 made of a film of a low-refractive index material such as SiO 2 are alternately formed. The structure is stacked as described above, and the reflectance is 99.0% or more. The reflection-enhancing film uses a reflection at the interface of each film to increase the reflectance. Therefore, the reflectance increases as the number of interfaces increases (the number of layers of the film increases). The magnitude of the reflection at the interface is determined by the difference in the refractive index of the film material. The greater the difference, the greater the reflectance. The refractive index of SiO 2 , which is a low-refractive-index film material which has been widely used, is 1.5, and the refractive indexes of TiO 2 , Ta 2 O 5, and HfO 2 which are high-refractive-index film materials are 2.2, 2. 1 and 1.9, 9
To obtain a reflectance of 9.0% or more, 15 layers or more, 9
To achieve a reflectivity of 9.5% or more, 21 layers or more are required.
【０００３】[0003]
【発明が解決しようとする課題】前記従来技術において
は散乱損失および吸収損失の点では満足できるものの、
膜の層数を多くする必要があり、製造上問題がある。本
発明者は低屈折率材としてＳｉＯ2 よりも屈折率の小さ
いＹＦ3 やＹｂＦ3を用いた、透過部材又は反射部材か
らなる基材の表面に低屈折率材および高屈折率材からな
るコーティング膜を形成させた赤外線用光学部品を開発
し、提案している（特開平７−３３１４１２号公報）。
この公報には、ＡｕをコートしたＳｉ又はＣｕ基板上
に、低屈折率材であるＹＦ3 やＹｂＦ3 の膜と、高屈折
率材であるＺｎＳｅ又はＺｎＳの膜とを交互に積層した
増反射膜も開示されている。しかしながら、Ａｕをコー
トしたＳｉ又はＣｕ基板上に前記ＹＦ3 やＹｂＦ3のコ
ーティング膜を形成させた場合、膜の付着強度が低いと
いう問題があった。本発明はこのような従来技術の実状
に鑑み、少ない層数で高い反射率が得られ、しかも十分
な膜付着強度と耐環境性を備えた近赤外線用反射鏡の増
反射膜およびその製造方法を提供することを目的とす
る。In the above prior art, although the scattering loss and the absorption loss are satisfactory,
It is necessary to increase the number of layers of the film, and there is a problem in manufacturing. The present inventor uses YF 3 or YbF 3 having a lower refractive index than SiO 2 as a low-refractive-index material, and coats a surface made of a low-refractive-index material and a high-refractive-index material on the surface of a substrate made of a transmitting member or a reflecting member. An infrared optical component having a film formed thereon has been developed and proposed (Japanese Patent Application Laid-Open No. Hei 7-331412).
This publication discloses an enhanced reflection in which a film of YF 3 or YbF 3 as a low-refractive index material and a film of ZnSe or ZnS as a high-refractive index material are alternately laminated on a Si or Cu substrate coated with Au. A membrane is also disclosed. However, when the coating film of YF 3 or YbF 3 is formed on a Si or Cu substrate coated with Au, there is a problem that the adhesion strength of the film is low. The present invention has been made in view of the above circumstances of the prior art, and has a high reflectance with a small number of layers, and has a sufficient film adhesion strength and environmental resistance. The purpose is to provide.
【０００４】[0004]
【課題を解決するための手段】本発明は（１）Ｃｕ、Ｓ
ｉ、ＢＫ−７ガラス又は石英ガラスからなる基材の表面
にＣｒ、Ｔｉ又はＮｉ層を介してＡｕ膜をコートした基
板上にＺｎＳｅ又はＺｎＳよりなるバッファー層を設
け、その上にＹＦ3 、ＹｂＦ3 又はＤｙＦ3 のいずれか
１種よりなる低屈折率層とＺｎＳｅ又はＺｎＳよりなる
高屈折率層とを交互に形成させてなることを特徴とする
近赤外線用増反射膜、（２）前記低屈折率層と高屈折率
層の層数がそれぞれ３〜４層であることを特徴とする前
記（１）の近赤外線用増反射膜、および（３）Ｃｕ、Ｓ
ｉ、ＢＫ−７ガラス又は石英ガラスからなる基材の表面
にＣｒ、Ｔｉ又はＮｉ層を介してＡｕ膜をコートした基
板を１２０〜１８０℃に加熱し、該温度範囲に保持しな
がらＺｎＳｅ又はＺｎＳを蒸着させてバッファー層を形
成し、さらに前記温度範囲に維持しながらＹＦ3 、Ｙｂ
Ｆ3 又はＤｙＦ3 のいずれか１種とＺｎＳｅ又はＺｎＳ
とを交互に蒸着させ、ＹＦ3 、ＹｂＦ3 又はＤｙＦ3 の
いずれか１種よりなる低屈折率層とＺｎＳｅ又はＺｎＳ
よりなる高屈折率層とを交互に形成させることを特徴と
する近赤外線用増反射膜の製造方法である。The present invention provides (1) Cu, S
i, a buffer layer made of ZnSe or ZnS is provided on a substrate coated with an Au film via a Cr, Ti or Ni layer on the surface of a base material made of BK-7 glass or quartz glass, and YF 3 , YbF A high-refractive-index film for near-infrared light, wherein a low-refractive-index layer made of any one of 3 and DyF 3 and a high-refractive-index layer made of ZnSe or ZnS are alternately formed; The number of layers of the refractive index layer and the number of the high refractive index layers are each 3 to 4 layers, and the near-infrared enhanced reflective film of (1), and (3) Cu, S
i, a substrate in which a surface of a substrate made of BK-7 glass or quartz glass is coated with an Au film via a Cr, Ti, or Ni layer is heated to 120 to 180 ° C., and ZnSe or ZnS is maintained while maintaining the temperature range. Is deposited to form a buffer layer, and while maintaining the above temperature range, YF 3 , Yb
Any one of F 3 or DyF 3 and ZnSe or ZnS
Are alternately deposited, and a low refractive index layer made of any one of YF 3 , YbF 3 or DyF 3 and ZnSe or ZnS
And a high refractive index layer formed alternately.
【０００５】[0005]
【発明の実施の態様】本発明の近赤外線用増反射膜はＣ
ｕ、Ｓｉ、ＢＫ−７ガラス又は石英ガラスからなる基材
の表面にＡｕ膜の付着力を向上させるためのＣｒ、Ｔｉ
又はＮｉ層を介してＡｕ膜をコーティングしたものを基
板とし、この上にＹＦ3 、ＹｂＦ3 又はＤｙＦ3 のいず
れか１種よりなる低屈折率層とＺｎＳｅ又はＺｎＳより
なる高屈折率層とを交互に形成させて反射率を向上させ
ている。さらに本発明の近赤外線用増反射膜において
は、前記低屈折率層と高屈折率層とが交互に形成された
増反射コーティング膜と前記基板との間に、厚さ６０〜
８０ｎｍのＺｎＳｅ又はＺｎＳよりなるバッファー層が
設けられている点が最大の特徴である。このバッファー
層を設けることにより、基板と増反射コーティング膜と
の付着力が向上する。通常、バッファー層を設けると光
学的特性（反射率）が低下するが、本発明においては、
バッファー層の材料としてＺｎＳｅ又はＺｎＳを使用
し、上記のような厚み範囲とすることにより光学的特性
の低下を抑え、付着力を向上させている。バッファー層
の厚みが上記範囲を外れるとバッファー層としての効果
が小さくなり、膜が剥離しやすくなる。DESCRIPTION OF THE PREFERRED EMBODIMENTS The near-infrared reflective film of the present invention is C
Cr, Ti for improving the adhesion of an Au film to the surface of a substrate made of u, Si, BK-7 glass or quartz glass
Alternatively, a substrate coated with an Au film via a Ni layer is used as a substrate, and a low-refractive-index layer made of any one of YF 3 , YbF 3 and DyF 3 and a high-refractive-index layer made of ZnSe or ZnS are formed thereon. They are alternately formed to improve the reflectance. Further, in the near-infrared enhanced reflective film of the present invention, between the substrate and the enhanced reflective coating film in which the low-refractive index layer and the high-refractive index layer are alternately formed, a thickness of 60 to
The most significant feature is that a buffer layer made of ZnSe or ZnS of 80 nm is provided. By providing this buffer layer, the adhesion between the substrate and the enhanced reflection coating film is improved. Usually, when a buffer layer is provided, the optical characteristics (reflectance) decrease, but in the present invention,
By using ZnSe or ZnS as the material of the buffer layer and setting the thickness range as described above, a decrease in optical characteristics is suppressed, and the adhesive force is improved. When the thickness of the buffer layer is out of the above range, the effect as the buffer layer is reduced, and the film is easily peeled.
【０００６】低屈折率膜材料であるＹＦ3 、ＹｂＦ3 お
よびＤｙＦ3 の屈折率はいずれも１．３８であり、高屈
折率膜材料であるＺｎＳｅおよびＺｎＳの屈折率はそれ
ぞれ２．５および２．３である。そのため従来使用され
ている低屈折率膜材料であるＳｉＯ2 と高屈折率膜材料
であるＴｉＯ2 、Ｔａ2 Ｏ5 又はＨｆＯ2 との組み合わ
せの場合に比較して屈折率差が大きいので、少ない層数
の増反射コーティング膜で高反射率が得られ、低屈折率
層と高屈折率層がそれぞれ３層の合計６層で９９．０％
以上、それぞれ４層の合計８層とすることで９９．５％
以上の高反射率を得ることができる。各低屈折率層及び
高屈折率層の厚みは対象とする近赤外線の波長及び入射
角によって異なるが、波長λ、膜材料の屈折率がｎで光
が垂直に入射する場合には、それぞれの層の厚みがほぼ
λ／（４・ｎ）となるようにする。例えば、波長１０６
２ｎｍのＹＡＧレーザで、レーザ光線の入射角が４５°
であり、低屈折率膜材料としてＹｂＦ3 、高屈折率膜材
料としてＺｎＳｅを使用する場合、低屈折率層及び高屈
折率層の厚みはそれぞれ２０９ｎｍ及び１１１ｎｍとす
ればよい。The refractive indices of the low refractive index film materials YF 3 , YbF 3 and DyF 3 are 1.38, and the refractive indices of the high refractive index film materials ZnSe and ZnS are 2.5 and 2 respectively. .3. Therefore, the difference in the refractive index is larger than that of the combination of the conventionally used low-refractive-index film material SiO 2 and the high-refractive-index film material TiO 2 , Ta 2 O 5, or HfO 2 , so that the difference is small. High reflectivity is obtained with the number of layers of the high-reflection coating film, and 99.0% of a total of 6 low-refractive-index layers and 3 high-refractive-index layers.
As described above, 99.5% is achieved by making each of the four layers a total of eight layers.
The above high reflectance can be obtained. Although the thickness of each low-refractive-index layer and high-refractive-index layer differs depending on the wavelength and incident angle of the near-infrared ray to be targeted, when the wavelength is λ, the refractive index of the film material is n and light is incident vertically, the respective The thickness of the layer is set to be approximately λ / (4 · n). For example, the wavelength 106
2nm YAG laser, incident angle of laser beam is 45 °
When using YbF 3 as the low-refractive-index film material and ZnSe as the high-refractive-index film material, the thicknesses of the low-refractive-index layer and the high-refractive-index layer may be 209 nm and 111 nm, respectively.
【０００７】本発明の近赤外線用増反射膜の膜構造の１
例を図１に示す。この例ではＣｕ、Ｓｉ、ＢＫ−７ガラ
ス又は石英ガラスからなる基材１の表面にＣｒ層５を介
してＡｕ膜６をコートした基板上に、ＺｎＳｅ又はＺｎ
Ｓのバッファー層７を設け、その上にＹＦ3 、ＹｂＦ3
又はＤｙＦ3 からなる低屈折率層２とＺｎＳｅ又はＺｎ
Ｓからなる高屈折率層３とが交互に各４層、合計８層積
層された構造となっている。[0007] One of the film structures of the near-infrared enhanced reflection film of the present invention
An example is shown in FIG. In this example, ZnSe or ZnSe is deposited on a substrate in which an Au film 6 is coated on the surface of a substrate 1 made of Cu, Si, BK-7 glass or quartz glass with a Cr layer 5 interposed therebetween.
An S buffer layer 7 is provided, and YF 3 , YbF 3
Or, the low refractive index layer 2 made of DyF 3 and ZnSe or Zn
It has a structure in which high refractive index layers 3 made of S are alternately stacked in four layers, each of which is a total of eight layers.
【０００８】本発明の近赤外線用増反射膜は例えば次の
ようにして製造することができる。Ｃｕ、Ｓｉ、ＢＫ−
７ガラス又は石英ガラスからなる基材の表面にＣｒ、Ｔ
ｉ又はＮｉ層を介してＡｕ膜をコートした基板を、図３
に示す構成の真空蒸着装置の真空チャンバ１１内に入
れ、高真空に排気しヒータ１２により１２０〜１８０℃
に加熱し、同温度範囲に保持しながらＺｎＳｅ又はＺｎ
Ｓを蒸着させて厚さ６０〜８０ｎｍのバッファー層を形
成させる。このバッファー層の上に、さらに前記温度範
囲に維持しながら低屈折率膜材料であるＹＦ3 、ＹｂＦ
3 又はＤｙＦ3のいずれか１種と高屈折率膜材料である
ＺｎＳｅ又はＺｎＳとを交互に蒸着させ、低屈折率層と
高屈折率層とを交互に形成させる。各膜材料は電子ビー
ム蒸発源（ＥＢ蒸発源）１４から基板１３に蒸着され
る。図３中の１５はシャッターである。真空蒸着の際の
基板温度が１２０℃未満では膜の付着強度が十分でな
く、また１８０℃を超えると付着強度が低下するほか、
膜の表面に荒れが発生する。The near-infrared reflective film of the present invention can be manufactured, for example, as follows. Cu, Si, BK-
7 Cr or T on the surface of a substrate made of glass or quartz glass
A substrate coated with an Au film via an i or Ni layer is shown in FIG.
Into a vacuum chamber 11 of a vacuum evaporation apparatus having the structure shown in FIG.
While maintaining the same temperature range, ZnSe or Zn
S is deposited to form a buffer layer having a thickness of 60 to 80 nm. On this buffer layer, while maintaining the above temperature range, YF 3 , YbF
Either 3 or DyF 3 and ZnSe or ZnS, which is a high-refractive-index film material, are alternately deposited to form a low-refractive-index layer and a high-refractive-index layer alternately. Each film material is deposited on the substrate 13 from an electron beam evaporation source (EB evaporation source) 14. Reference numeral 15 in FIG. 3 denotes a shutter. If the substrate temperature during vacuum deposition is lower than 120 ° C., the adhesive strength of the film is not sufficient, and if it exceeds 180 ° C., the adhesive strength is reduced,
Roughness occurs on the surface of the film.
【０００９】本発明の近赤外線用増反射膜は波長８５０
〜２５００ｎｍの近赤外線に対し高い反射率を示し、膜
の付着性及び耐環境性に優れた増反射膜であり、ＹＡＧ
レーザ用反射鏡の増反射膜などの用途に有用なものであ
る。The near-infrared enhanced reflection film of the present invention has a wavelength of 850.
YAG is a high-reflection film that exhibits high reflectance to near-infrared rays of up to 2500 nm and is excellent in film adhesion and environmental resistance.
It is useful for applications such as a reflection-enhancing film of a laser reflecting mirror.
【００１０】[0010]
【実施例】以下実施例により本発明をさらに具体的に説
明する。 （実施例１）Ｃｕの表面にＣｒ層を介してＡｕ膜をコー
トした基板の表面に、表１に示す膜構成のバッファー層
と低屈折率層および高屈折率層を形成させた試料を作製
した。また、比較のためバッファー層を設けない試料を
作製した。、得られた近赤外線用増反射膜の試料１〜１
５について反射率及び付着強度の測定と外観観察を行っ
た。なお、バッファー層の厚みは６２ｎｍ、各低屈折率
層（ＹｂＦ3 、ＹＦ3又はＤｙＦ3 ）の厚みは２０９ｎ
ｍ、高屈折率層の厚みはＺｎＳｅは１１１ｎｍ、ＺｎＳ
は１１４ｎｍとした。蒸着時の基板温度および測定、観
察結果を表１に示す。表１において、反射率は分光光度
計により波長１．０６μｍの近赤外線の反射率を測定
し、付着強度はセロハンテープを貼り付けてゆっくりと
剥がすテープテストにより、膜剥離が発生しないものを
○、膜剥離が発生したものを×とした。外観は目視によ
り表面が鏡面状態であるものを○、表面がざらついて白
色に見えるものを×とした。また、水を張った超音波洗
浄機に入れて超音波を作用させる耐環境性（耐水性）試
験を行い、１０分間の処理で変化のないものを○、膜の
表面が白く荒れるか、あるいは剥離したものを×とし
た。さらに、得られた本発明の試料（Ｎｏ．１、５、
９、１３、１４、１５）について反射スペクトル（入射
角４５°）を測定した結果を図４〜図９に示す。The present invention will be described more specifically with reference to the following examples. (Example 1) A sample in which a buffer layer, a low refractive index layer, and a high refractive index layer having a film configuration shown in Table 1 were formed on the surface of a substrate in which a Cu film was coated with an Au film via a Cr layer. did. For comparison, a sample without a buffer layer was prepared. Samples 1 to 1 of the obtained near-infrared enhanced reflection film
For No. 5, the reflectance and the adhesion strength were measured and the appearance was observed. The thickness of the buffer layer was 62 nm, and the thickness of each low refractive index layer (YbF 3 , YF 3 or DyF 3 ) was 209 n.
m, the thickness of the high refractive index layer is 111 nm for ZnSe,
Was 114 nm. Table 1 shows the substrate temperature at the time of vapor deposition and the measurement and observation results. In Table 1, the reflectance was measured by a spectrophotometer to measure the reflectance of near-infrared light having a wavelength of 1.06 μm. The sample where film peeling occurred was evaluated as x. The appearance was evaluated as ○ when the surface was specular, and × when the surface was rough and white. In addition, an environment resistance (water resistance) test in which ultrasonic waves are applied in an ultrasonic cleaning machine filled with water and subjected to an ultrasonic test is performed. What peeled was set to x. Furthermore, the obtained samples of the present invention (Nos. 1, 5,
9, 13, 14, 15) are shown in FIG. 4 to FIG. 9 showing the results of measuring the reflection spectrum (incident angle: 45 °).
【００１１】[0011]
【表１】 [Table 1]
【００１２】表１の結果から、低屈折率層および高屈折
率層をそれぞれ３層としたものでは、低屈折率層および
高屈折率層からなる増反射コーティング膜と基板との間
にバッファー層を設け、基板温度１６０℃でコーティン
グ膜の蒸着を行った試料Ｎｏ．１および５は反射率が９
９．０％以上で外観、付着強度、耐環境性（耐水性）と
もに良好な結果を示した。しかしながら、同様にバッフ
ァー層を設けたものであっても、蒸着の際の基板温度が
１００℃と低い試料Ｎｏ．２および６では反射率が９
９．０％以上で外観も良好であったが、付着強度が低
く、耐環境性が悪くなり、蒸着の際の基板温度が２００
℃と高い試料Ｎｏ．３および７では反射率および付着強
度が低下し、外観及び耐環境性も悪くなっていることが
わかる。また、バッファー層を設けなかった試料Ｎｏ．
４および８では、基板温度が１６０℃であっても良好な
付着強度が得られないことがわかる。From the results shown in Table 1, when the low-refractive index layer and the high-refractive index layer are each composed of three layers, the buffer layer is provided between the substrate and the high reflection coating film composed of the low and high refractive index layers. And the sample No. in which a coating film was deposited at a substrate temperature of 160 ° C. 1 and 5 have a reflectivity of 9
At 9.0% or more, good results were exhibited in all of the appearance, adhesion strength and environmental resistance (water resistance). However, even in the case where the buffer layer was similarly provided, the sample No. in which the substrate temperature at the time of vapor deposition was as low as 100 ° C. At 2 and 6, the reflectivity is 9
The appearance was good at 9.0% or more, but the adhesion strength was low, the environmental resistance was poor, and the substrate temperature during evaporation was 200%.
° C and sample No. It can be seen that in the cases of Nos. 3 and 7, the reflectance and the adhesive strength were reduced, and the appearance and the environmental resistance were also poor. In addition, the sample No.
4 and 8, it can be seen that good adhesion strength cannot be obtained even when the substrate temperature is 160 ° C.
【００１３】また、低屈折率層および高屈折率層をそれ
ぞれ４層としたものでは、バッファー層を設け、基板温
度１６０℃でコーティング膜の蒸着を行った試料Ｎｏ．
９、１３、１４及び１５は反射率が９９．５％以上で外
観、付着強度、耐環境性ともに良好な結果を示した。し
かしながら、同様にバッファー層を設けたものであって
も、蒸着の際の基板温度が１００℃と低い試料Ｎｏ．１
０では反射率が９９．５％以上で外観も良好であった
が、付着強度が低く、耐環境性が悪化し、蒸着の際の基
板温度が２００℃と高い試料Ｎｏ．１１では反射率およ
び付着強度が低下し、外観及び耐環境性も悪くなってい
ることがわかる。また、バッファー層を設けなかった試
料Ｎｏ．１２では、基板温度が１６０℃であっても良好
な付着強度は得られなかった。In the case where the low refractive index layer and the high refractive index layer each have four layers, the buffer layer was provided and the coating film was deposited at a substrate temperature of 160 ° C.
9, 13, 14 and 15 had a reflectance of 99.5% or more, and showed good results in appearance, adhesion strength and environmental resistance. However, even in the case where the buffer layer was similarly provided, the sample No. in which the substrate temperature at the time of vapor deposition was as low as 100 ° C. 1
In Sample No. 0, the reflectance was 99.5% or more and the appearance was good, but the adhesion strength was low, the environmental resistance was deteriorated, and the substrate temperature at the time of vapor deposition was as high as 200 ° C. In the case of No. 11, it can be seen that the reflectance and the adhesion strength are reduced, and the appearance and environmental resistance are also deteriorated. In addition, the sample No. In No. 12, good adhesion strength could not be obtained even when the substrate temperature was 160 ° C.
【００１４】（実施例２）実施例１で得た試料９と従来
品（石英ガラス基板にＳｉＯ2 ／ＴｉＯ2 の膜組成で層
数は２０層、反射率９９．５％以上）を使用して耐光強
度試験を行った。試験はＹＡＧレーザ光（波長１０６２
ｎｍ）をレンズで集光し、集光位置に試料をセットして
レーザ光を１秒間照射し、損傷の有無を目視及び顕微鏡
で観察することによって行った。レーザ光照射位置での
ビーム径は１〜１．４ｍｍ（楕円）、入射角は４５°と
した。最大出力である１．５ｋＷのレーザ光を照射（照
射されるエネルギー密度は１３５ｋＷ／ｃｍ2 ）した結
果、試料９及び従来品ともに損傷は発生しなかった。通
常の使用条件で照射されるレーザ光のエネルギー密度は
最大でも数ｋＷ／ｃｍ 2 であることから、本発明に係る
増反射膜は十分な耐光性を有していることがわかる。(Example 2) Sample 9 obtained in Example 1 and a conventional sample 9
Product (quartz glass substrate with SiOTwo/ TiOTwoLayer with film composition
Number is 20 layers, reflectivity is 99.5% or more)
Degree test. The test was performed using a YAG laser beam (wavelength 1062).
nm) with a lens, set the sample at the focusing position
Irradiate laser light for 1 second, visually inspect for damage and microscope
By observing at At the laser beam irradiation position
The beam diameter is 1 to 1.4 mm (ellipse) and the incident angle is 45 °
did. Irradiate 1.5 kW laser beam which is the maximum output
The energy density emitted is 135 kW / cmTwo)
As a result, no damage occurred in both Sample 9 and the conventional product. Through
The energy density of the laser beam irradiated under normal use conditions is
At most several kW / cm TwoTherefore, according to the present invention,
It can be seen that the enhanced reflection film has sufficient light resistance.
【００１５】[0015]
【発明の効果】本発明の近赤外線用増反射膜は層数が少
なく製造が容易で、しかも高い反射率を有しており、さ
らに膜の付着力が高く耐環境性に優れたものである。ま
た、本発明の製造方法によれば前記近赤外線用増反射膜
を容易に製造することができる。The near-infrared enhanced reflection film of the present invention has a small number of layers, is easy to manufacture, has a high reflectance, and has a high adhesion of the film and excellent environmental resistance. . Further, according to the manufacturing method of the present invention, the near-infrared enhanced reflection film can be easily manufactured.
【図１】本発明の近赤外線用増反射膜の膜構造の１例を
示す断面図。FIG. 1 is a cross-sectional view showing one example of a film structure of a near-infrared enhanced reflection film of the present invention.
【図２】従来技術による近赤外線用増反射膜の膜構造の
１例を示す断面図。FIG. 2 is a cross-sectional view showing an example of a film structure of a near-infrared enhanced reflection film according to a conventional technique.
【図３】本発明の近赤外線用増反射膜を製造するための
真空蒸着装置の構成を模式的に示す図。FIG. 3 is a diagram schematically showing a configuration of a vacuum evaporation apparatus for manufacturing the near-infrared enhanced reflection film of the present invention.
【図４】実施例１で作製した試料１の反射スペクトルを
示す図。FIG. 4 is a diagram showing a reflection spectrum of Sample 1 manufactured in Example 1.
【図５】実施例１で作製した試料５の反射スペクトルを
示す図。FIG. 5 is a diagram showing a reflection spectrum of Sample 5 manufactured in Example 1.
【図６】実施例１で作製した試料９の反射スペクトルを
示す図。FIG. 6 is a diagram showing a reflection spectrum of Sample 9 manufactured in Example 1.
【図７】実施例１で作製した試料１３の反射スペクトル
を示す図。FIG. 7 shows a reflection spectrum of Sample 13 manufactured in Example 1.
【図８】実施例１で作製した試料１４の反射スペクトル
を示す図。FIG. 8 is a diagram showing a reflection spectrum of Sample 14 manufactured in Example 1.
【図９】実施例１で作製した試料１５の反射スペクトル
を示す図。9 shows a reflection spectrum of Sample 15 manufactured in Example 1. FIG.
１ 基材 ２ 低屈折率層 ３ 高屈折率層 ５
クロム層 ６ Ａｕ層 ７ バッファー層 １１ 真空チャン
バ １２ ヒータ １３ 基板 １４ ＥＢ蒸着源
１５ シャッターReference Signs List 1 base material 2 low refractive index layer 3 high refractive index layer 5
Chromium layer 6 Au layer 7 Buffer layer 11 Vacuum chamber 12 Heater 13 Substrate 14 EB evaporation source
15 Shutter
───────────────────────────────────────────────────── フロントページの続き Ｆターム(参考） 4F100 AA02D AA02E AA05E AA09D AA09E AB11A AB12B AB13B AB16B AB17A AB25C AG00A AT00A BA05 BA07 BA10A BA10E BA13 BA44 EG002 EH112 EH66D EH662 EJ422 JD10 JK06 JK11D JL00 JM02C JN06 JN18E 4K029 AA02 AA09 BA05 BA07 BA12 BA17 BA41 BA42 BA51 BB02 BC07 BD09 CA01 DB03 DB05 DB21 EA08 JA02 ──────────────────────────────────────────────────続 き Continued on the front page F term (reference) 4F100 AA02D AA02E AA05E AA09D AA09E AB11A AB12B AB13B AB16B AB17A AB25C AG00A AT00A BA05 BA07 BA10A BA10E BA13 BA44 EG002 EH112 EH66D EH662 EJ422 JD10 JKN JA10 JK10 BA17 BA41 BA42 BA51 BB02 BC07 BD09 CA01 DB03 DB05 DB21 EA08 JA02
Claims (3)
ラスからなる基材の表面にＣｒ、Ｔｉ又はＮｉ層を介し
てＡｕ膜をコートした基板上にＺｎＳｅ又はＺｎＳより
なるバッファー層を設け、その上にＹＦ3 、ＹｂＦ3 又
はＤｙＦ3 のいずれか１種よりなる低屈折率層とＺｎＳ
ｅ又はＺｎＳよりなる高屈折率層とを交互に形成させて
なることを特徴とする近赤外線用増反射膜。A buffer layer made of ZnSe or ZnS is provided on a substrate in which an Au film is coated on a surface of a substrate made of Cu, Si, BK-7 glass or quartz glass with a Cr, Ti or Ni layer interposed therebetween, A low-refractive-index layer made of any one of YF 3 , YbF 3 and DyF 3 and a ZnS
A high-reflection film for near-infrared rays, wherein high-refractive-index layers made of e or ZnS are alternately formed.
れぞれ３〜４層であることを特徴とする請求項１に記載
の近赤外線用増反射膜。2. The near-infrared enhanced reflection film according to claim 1, wherein the number of the low-refractive-index layers and the number of the high-refractive-index layers are three to four, respectively.
ラスからなる基材の表面にＣｒ、Ｔｉ又はＮｉ層を介し
てＡｕ膜をコートした基板を１２０〜１８０℃に加熱
し、該温度範囲に保持しながらＺｎＳｅ又はＺｎＳを蒸
着させてバッファー層を形成し、さらに前記温度範囲に
維持しながらＹＦ3 、ＹｂＦ3 又はＤｙＦ3 のいずれか
１種とＺｎＳｅ又はＺｎＳとを交互に蒸着させ、Ｙ
Ｆ3 、ＹｂＦ 3 又はＤｙＦ3 のいずれか１種よりなる低
屈折率層とＺｎＳｅ又はＺｎＳよりなる高屈折率層とを
交互に形成させることを特徴とする近赤外線用増反射膜
の製造方法。3. Cu, Si, BK-7 glass or quartz glass
A Cr, Ti or Ni layer is interposed on the surface of
The Au-coated substrate to 120-180 ° C
Then, while maintaining the temperature range, ZnSe or ZnS is vaporized.
To form a buffer layer, and
YF while maintainingThree, YbFThreeOr DyFThreeAny of
One kind and ZnSe or ZnS are alternately deposited, and Y
FThree, YbF ThreeOr DyFThreeLow consisting of any one of
A refractive index layer and a high refractive index layer made of ZnSe or ZnS.
Highly reflective film for near infrared rays characterized by being formed alternately
Manufacturing method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10201475A JP2000034557A (en) | 1998-07-16 | 1998-07-16 | Reflection enhancing film for near infrared rays and production of the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10201475A JP2000034557A (en) | 1998-07-16 | 1998-07-16 | Reflection enhancing film for near infrared rays and production of the same |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2000034557A true JP2000034557A (en) | 2000-02-02 |
Family
ID=16441704
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10201475A Pending JP2000034557A (en) | 1998-07-16 | 1998-07-16 | Reflection enhancing film for near infrared rays and production of the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2000034557A (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002072343A1 (en) * | 2001-03-08 | 2002-09-19 | Shin-Etsu Handotai Co., Ltd. | Heat reflecting material and heating device using the material |
| WO2005003618A1 (en) * | 2003-07-04 | 2005-01-13 | Matsushita Electric Industrial Co., Ltd. | Vacuum thermal insulation material and equipment using the same |
| JP2008542082A (en) * | 2005-06-09 | 2008-11-27 | バイエル・マテリアルサイエンス・アクチェンゲゼルシャフト | Flame-resistant coated molded polycarbonate articles |
| KR101146619B1 (en) * | 2010-11-22 | 2012-05-14 | 한국전광(주) | High reflection mirror for simultaneously satisfying visible ray and infrared ray region |
| CN102941710A (en) * | 2012-11-14 | 2013-02-27 | 江苏欧邦塑胶有限公司 | Safe heat insulation glass |
| CN102950830A (en) * | 2012-11-14 | 2013-03-06 | 江苏欧邦塑胶有限公司 | Heat insulation film |
| CN103668067A (en) * | 2013-12-09 | 2014-03-26 | 西南技术物理研究所 | Preparation method of wide-angle multiband infrared high-reflective film system |
| KR101766392B1 (en) | 2017-03-29 | 2017-08-09 | (주) 유남옵틱스 | Reflective mirror and Method for manufacturing the same |
| CN115491638A (en) * | 2022-08-31 | 2022-12-20 | 中国电子科技集团公司第十一研究所 | Preparation method of broad-spectrum back anti-reflection film for detector chip |
| CN117512527A (en) * | 2023-11-10 | 2024-02-06 | 星际光(上海)实业有限公司 | Dielectric film reflector and preparation process thereof |
-
1998
- 1998-07-16 JP JP10201475A patent/JP2000034557A/en active Pending
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002072343A1 (en) * | 2001-03-08 | 2002-09-19 | Shin-Etsu Handotai Co., Ltd. | Heat reflecting material and heating device using the material |
| US6815645B2 (en) | 2001-03-08 | 2004-11-09 | Shin-Etsu Handotai Co., Ltd. | Heat reflecting material and heating device using the material |
| WO2005003618A1 (en) * | 2003-07-04 | 2005-01-13 | Matsushita Electric Industrial Co., Ltd. | Vacuum thermal insulation material and equipment using the same |
| EP1643180A1 (en) * | 2003-07-04 | 2006-04-05 | Matsushita Electric Industrial Co., Ltd. | Vacuum thermal insulation material and equipment using the same |
| CN1309991C (en) * | 2003-07-04 | 2007-04-11 | 松下电器产业株式会社 | Vacuum heat insulating material and machine using the same vacuum heat insulation material |
| US7485352B2 (en) | 2003-07-04 | 2009-02-03 | Panasonic Corporation | Vacuum heat insulator and apparatus using the same |
| EP1643180A4 (en) * | 2003-07-04 | 2010-08-25 | Panasonic Corp | Vacuum thermal insulation material and equipment using the same |
| JP2008542082A (en) * | 2005-06-09 | 2008-11-27 | バイエル・マテリアルサイエンス・アクチェンゲゼルシャフト | Flame-resistant coated molded polycarbonate articles |
| KR101146619B1 (en) * | 2010-11-22 | 2012-05-14 | 한국전광(주) | High reflection mirror for simultaneously satisfying visible ray and infrared ray region |
| CN102941710A (en) * | 2012-11-14 | 2013-02-27 | 江苏欧邦塑胶有限公司 | Safe heat insulation glass |
| CN102950830A (en) * | 2012-11-14 | 2013-03-06 | 江苏欧邦塑胶有限公司 | Heat insulation film |
| CN103668067A (en) * | 2013-12-09 | 2014-03-26 | 西南技术物理研究所 | Preparation method of wide-angle multiband infrared high-reflective film system |
| CN103668067B (en) * | 2013-12-09 | 2016-01-13 | 西南技术物理研究所 | The preparation method of the infrared highly reflecting films system of wide-angle multiband |
| KR101766392B1 (en) | 2017-03-29 | 2017-08-09 | (주) 유남옵틱스 | Reflective mirror and Method for manufacturing the same |
| CN115491638A (en) * | 2022-08-31 | 2022-12-20 | 中国电子科技集团公司第十一研究所 | Preparation method of broad-spectrum back anti-reflection film for detector chip |
| CN115491638B (en) * | 2022-08-31 | 2024-03-19 | 中国电子科技集团公司第十一研究所 | Preparation method of wide-spectrum back antireflection film for detector chip |
| CN117512527A (en) * | 2023-11-10 | 2024-02-06 | 星际光(上海)实业有限公司 | Dielectric film reflector and preparation process thereof |
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