JPH0432558A - Production of multilayered dielectric film - Google Patents
Production of multilayered dielectric filmInfo
- Publication number
- JPH0432558A JPH0432558A JP13947390A JP13947390A JPH0432558A JP H0432558 A JPH0432558 A JP H0432558A JP 13947390 A JP13947390 A JP 13947390A JP 13947390 A JP13947390 A JP 13947390A JP H0432558 A JPH0432558 A JP H0432558A
- Authority
- JP
- Japan
- Prior art keywords
- refractive index
- film
- dielectric multilayer
- multilayer film
- substrate
- 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.)
- Granted
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- 239000000758 substrate Substances 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000007789 gas Substances 0.000 claims abstract description 20
- 239000011261 inert gas Substances 0.000 claims abstract description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000001301 oxygen Substances 0.000 claims abstract description 12
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 12
- 238000001704 evaporation Methods 0.000 claims abstract description 11
- 230000008020 evaporation Effects 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims description 9
- 230000003287 optical effect Effects 0.000 abstract description 9
- 229910001635 magnesium fluoride Inorganic materials 0.000 abstract description 4
- 229910052984 zinc sulfide Inorganic materials 0.000 abstract description 4
- 230000006866 deterioration Effects 0.000 abstract description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 abstract 2
- 239000008246 gaseous mixture Substances 0.000 abstract 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 1
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- 238000007733 ion plating Methods 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 229910052950 sphalerite Inorganic materials 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 239000010408 film Substances 0.000 description 62
- 150000002500 ions Chemical class 0.000 description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 239000010409 thin film Substances 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 4
- 239000011521 glass Substances 0.000 description 3
- 238000010849 ion bombardment Methods 0.000 description 3
- 238000001771 vacuum deposition Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- 239000005083 Zinc sulfide Substances 0.000 description 2
- 239000003989 dielectric material Substances 0.000 description 2
- 238000010030 laminating Methods 0.000 description 2
- 238000003475 lamination Methods 0.000 description 2
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 2
- YIWGJFPJRAEKMK-UHFFFAOYSA-N 1-(2H-benzotriazol-5-yl)-3-methyl-8-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carbonyl]-1,3,8-triazaspiro[4.5]decane-2,4-dione Chemical compound CN1C(=O)N(c2ccc3n[nH]nc3c2)C2(CCN(CC2)C(=O)c2cnc(NCc3cccc(OC(F)(F)F)c3)nc2)C1=O YIWGJFPJRAEKMK-UHFFFAOYSA-N 0.000 description 1
- VCUFZILGIRCDQQ-KRWDZBQOSA-N N-[[(5S)-2-oxo-3-(2-oxo-3H-1,3-benzoxazol-6-yl)-1,3-oxazolidin-5-yl]methyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C1O[C@H](CN1C1=CC2=C(NC(O2)=O)C=C1)CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F VCUFZILGIRCDQQ-KRWDZBQOSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005422 blasting Methods 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 229910052743 krypton Inorganic materials 0.000 description 1
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
Landscapes
- Optical Elements Other Than Lenses (AREA)
- Optical Filters (AREA)
- Physical Vapour Deposition (AREA)
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野］
本発明は、反射鏡、帯域フィルターなどとして光学分野
にて一般的に使用される誘電体多層膜の製造法に関する
ものである。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a method for manufacturing a dielectric multilayer film commonly used in the optical field as a reflecting mirror, a bandpass filter, etc.
［従来技術］
反射鏡、帯域フィルターの誘電体多層膜は、高屈折率誘
電体物質の薄膜と低屈折率誘電体物質の薄膜とが基板上
に複数層交互に積層されてなるものであり、従来は、通
常、真空槽内に設置された蒸発源より高屈折率膜の材料
と低屈折率膜の材料を交互に蒸発させ、該真空槽内に保
持された基板上にそれらの材料を蒸着積層させ、誘電体
多層膜を形成する方法（真空蒸着法）により製造されて
きた。[Prior Art] A dielectric multilayer film for a reflecting mirror or a bandpass filter is formed by alternately laminating a plurality of thin films of a high refractive index dielectric material and thin films of a low refractive index dielectric material on a substrate. Conventionally, materials for high refractive index films and materials for low refractive index films are alternately evaporated from an evaporation source installed in a vacuum chamber, and these materials are deposited on a substrate held in the vacuum chamber. It has been manufactured by a method of stacking layers to form a dielectric multilayer film (vacuum evaporation method).
しかし、上記の真空蒸着法では、その実施に際して高度
の真空度が要求されるため、作業効率および条件の制御
等において不利があり、このため、真空槽内に導入され
た少量の不活性気体または反応性気体と不活性気体の混
合気体の存在下にて、該真空槽内に設置された蒸発源よ
り高屈折率膜の材料と低屈折率膜の材料を交互に蒸発さ
せ、該真空槽内に保持された基板上に誘電体多層膜を形
成させる方法が既に提案されている（特公昭４４−８２
７２号公報）。However, the above-mentioned vacuum evaporation method requires a high degree of vacuum for its implementation, which is disadvantageous in terms of work efficiency and control of conditions. In the presence of a mixed gas of a reactive gas and an inert gas, the material for the high refractive index film and the material for the low refractive index film are alternately evaporated from an evaporation source installed in the vacuum chamber. A method has already been proposed in which a dielectric multilayer film is formed on a substrate held by
Publication No. 72).
一方、上記の真空蒸着法に実施に際して、基板上に薄膜
が形成されつつあるときに、その膜面をイオン衝撃する
操作を行なう方法は、イオンブレーティング法と呼ばれ
、高密度の誘電体多層膜の製造に適していることから、
光学用途を考慮した誘電体多層膜の製造にも利用されて
いる。たとえば、特開平１−２２９２０２号公報には、
反射基板面に硫化亜鉛の薄膜とフッ化マグネシウムの薄
膜とをイオンブレーティング法を利用して交互に積層し
て高密度の多層膜からなる多層膜反射鏡を製造する方法
が開示されている。On the other hand, when carrying out the vacuum evaporation method described above, a method in which the film surface is bombarded with ions while a thin film is being formed on the substrate is called the ion blating method, and is used to form a high-density dielectric multilayer. Because it is suitable for manufacturing membranes,
It is also used in the production of dielectric multilayer films for optical applications. For example, in Japanese Patent Application Laid-Open No. 1-229202,
A method is disclosed for manufacturing a multilayer film reflecting mirror consisting of a high-density multilayer film by alternately laminating thin films of zinc sulfide and thin films of magnesium fluoride on the surface of a reflective substrate using an ion-blating method.
［本発明が解決しようとする問題点１
反射鏡、特に冷光鏡（コールドミラー）などの反射鏡の
誘電体多層膜は、近年では、その使用において３００℃
以上の高温となることがあるが、これまでに知られてい
る方法によって製造された誘電体多層膜は、耐熱性が充
分でないため、比較的短期間のうちに、光透過（あるい
は光反射）特性の顕著な変動が発生したり１Ｍ電体多暦
膜が基板から剥離するなどの劣化が発生しやすく、長期
間の連続使用には適していない、このような不充分な耐
熱性は、近年における誘電体多層膜の使用条件の過酷化
（更に高い温度になる条件下の長期間の連続使用）では
、特に改良すべき問題となる。[Problem 1 to be solved by the present invention In recent years, dielectric multilayer films of reflective mirrors, particularly cold mirrors, have been heated to temperatures of 300°C during use.
However, since dielectric multilayer films manufactured by methods known so far do not have sufficient heat resistance, light transmission (or light reflection) may occur in a relatively short period of time. In recent years, insufficient heat resistance has been developed, which tends to cause deterioration such as noticeable changes in characteristics and peeling of the 1M electric multilayer film from the substrate, making it unsuitable for long-term continuous use. This becomes a problem that should be improved especially when the dielectric multilayer film is used under harsh conditions (continuous use for a long period of time under conditions of even higher temperatures).
［発明の目的］
本発明は、耐熱性、すなわち高温使用における耐久性が
顕著に向上する誘電体多層膜の製造法を提供することを
、その目的とする。[Object of the Invention] An object of the present invention is to provide a method for manufacturing a dielectric multilayer film that has significantly improved heat resistance, that is, durability in high-temperature use.
［発明の内容］
本発明は、真空槽内に導入された少量の不活性気体また
は反応性気体と不活性気体の混合気体の存在下で、該真
空槽内に設置された蒸発源より高屈折率膜の材料と低屈
折率膜の材料を交互に蒸発させ、イオンブレーティング
法を利用して、該真空槽内に保持された基板上に誘電体
多層膜を形成させたのち、すぐに該誘電体多層膜を、酸
素もしくは酸素含有気体混合物の雰囲気中において、４
００℃以上、かつ誘電体多層膜の実際の使用時の温度よ
りも１０℃以上高い温度にて、熱処理を施すことからな
る誘電体多層膜の製造法にある。[Contents of the Invention] The present invention provides a method for achieving higher refraction than an evaporation source installed in the vacuum chamber in the presence of a small amount of inert gas or a mixed gas of a reactive gas and an inert gas introduced into the vacuum chamber. After the dielectric multilayer film is formed on the substrate held in the vacuum chamber by alternately evaporating the material for the high index film and the material for the low refractive index film using the ion blating method, the dielectric multilayer film is immediately evaporated. The dielectric multilayer film is heated for 4 hours in an atmosphere of oxygen or an oxygen-containing gas mixture.
The present invention provides a method for producing a dielectric multilayer film, which comprises performing heat treatment at a temperature of 00°C or higher and at least 10°C higher than the temperature at which the dielectric multilayer film is actually used.
［発明の構成］
本発明は、真空槽内に導入された少量の不活性気体また
は反応性気体と不活性気体の混合気体の存在下で、該真
空槽内に設置された蒸発源より高屈折率膜の材料と低屈
折率膜の材料を交互に蒸発させ、イオンブレーティング
法を利用して、該真空槽内に保持された基板上に誘電体
多層膜を特定の条件にて加熱処理することからなる耐熱
性が向上した誘電体多層膜の製造方法である。[Structure of the Invention] The present invention provides a method of increasing refractive index from an evaporation source installed in the vacuum chamber in the presence of a small amount of inert gas or a mixed gas of a reactive gas and an inert gas introduced into the vacuum chamber. The material for the index film and the material for the low refractive index film are alternately evaporated, and the dielectric multilayer film is heat-treated under specific conditions on the substrate held in the vacuum chamber using the ion blating method. This is a method for manufacturing a dielectric multilayer film with improved heat resistance.
本発明の誘電体多層膜の製造に用いられる高屈折率膜の
材料と低屈折率膜の材料とは、いずれも公知の誘電体多
層膜の製造に利用される材料から選ぶことができる。得
られる高屈折率膜の例としては、ＺｎＳ、Ｔｉ０ｚ 、
ＺｒＯ２，Ｔａ２０５があり、また低屈折率膜の例とし
てはＭｇＦ２．５ｉ０２ 、ＡｆＬ２０３がある。これ
らの高屈折率と屈折率膜とは種々の組合せにて利用され
る。そのような組合せの例としては、Ｚ ｎ Ｓ −Ｍ
ｇ Ｆ ２系、ＺｎＳ−３ｉＯ２系、Ｔ ｉ ０２−
ＭｇＦ２系、そしてＴａ２０５−３ ｉ ０２系を挙げ
ることができる。Both the material of the high refractive index film and the material of the low refractive index film used in the production of the dielectric multilayer film of the present invention can be selected from materials used in the production of known dielectric multilayer films. Examples of high refractive index films that can be obtained include ZnS, Ti0z,
Examples of low refractive index films include MgF2.5i02 and AfL203. These high refractive indexes and refractive index films are used in various combinations. An example of such a combination is Z n S −M
g F2-based, ZnS-3iO2-based, T i 02-
Mention may be made of MgF2 series and Ta205-3 i 02 series.
真空槽にて用いる不活性気体の例としては、アルゴン（
Ａｒ）、 クリプトン（Ｋ）、＋セノン（Ｘ ｅ ）を
挙げることができ、また不活性気体と混合して用いられ
る反応性気体の例としては酸素ガス（０２）を挙げるこ
とができる。An example of an inert gas used in a vacuum chamber is argon (
Ar), krypton (K), +senone (X e ), and oxygen gas (02) is an example of the reactive gas used in mixture with an inert gas.
上記の不活性気体もしくは不活性気体と反応性気体との
混合気体は、真空槽の中に、通常は、分圧０ 、４〜１
、４Ｘ １０−３ｍｍＨｇ（７）範囲を示すように導
入される。The above-mentioned inert gas or a mixture of an inert gas and a reactive gas is placed in a vacuum chamber at a partial pressure of 0.4 to 1.
, 4X 10-3 mmHg (7).
真空槽内に設置された蒸発源より高屈折率膜の材料と低
屈折率膜の材料を交互に蒸発させ、イオンブレーティン
グ法を利用して、該真空槽内に保持された基板上に誘電
体多層膜を形成する方法は既に知られており、公知の装
置にて公知の方法を利用して実施することができる。A high refractive index film material and a low refractive index film material are alternately evaporated from an evaporation source installed in a vacuum chamber, and a dielectric layer is formed on a substrate held in the vacuum chamber using the ion blating method. The method of forming a body multilayer film is already known, and can be carried out using a known method using a known apparatus.
ただし、本発明の誘電体多層膜の製造法においては、真
空槽内に設置された蒸発源より高屈折率膜の材料と低屈
折率の材料を交互に蒸発させて、基板上に誘電体多層膜
を形成させる際に、高周波励起イオンブレーティングを
利用することが好ましく、特に、基板の保持体を電極と
してＲＦ電力を印加することによりＲＦ放電を発生させ
、導入気体と蒸発蒸気のＲＦ放電により電離されたイオ
ンを用いて、上記のＲＦ放電によって基板表面に誘起さ
れた自己バイアス電圧の作用によって多層膜を形成する
操作を利用することイオン衝撃装置（特開昭６１−２３
３９５７号公報に記載）を用いることが好ましい。However, in the method for manufacturing a dielectric multilayer film of the present invention, a material for a high refractive index film and a material for a low refractive index film are alternately evaporated from an evaporation source installed in a vacuum chamber to form a dielectric multilayer film on a substrate. When forming a film, it is preferable to use high-frequency excited ion blating. In particular, RF discharge is generated by applying RF power using the substrate holder as an electrode, and the RF discharge of introduced gas and evaporated vapor is used. An ion bombardment device (JP-A-61-23
3957) is preferably used.
本発明においては、イオンブレーティングを利用した蒸
着操作により上記のように基板上に形成した誘電体多層
膜を、すぐに酸素もしくは酸素含有気体混合物の雰囲気
中において、４００℃以上、かつ誘電体多層膜の実際の
使用時の温度よりも１０℃以上高い温度にて、熱処理を
施すことを特徴とする。In the present invention, a dielectric multilayer film formed on a substrate as described above by a vapor deposition operation using ion blating is immediately exposed to a temperature of 400°C or higher in an atmosphere of oxygen or an oxygen-containing gas mixture. It is characterized in that the heat treatment is performed at a temperature that is 10°C or more higher than the temperature at which the membrane is actually used.
上記の操作における「すぐに」とは、通常は２４時間以
内を意味し、好ましくは１２時間以内であり、さらに好
ましくは６時間以内である。すなわち、イオンブレーテ
ィングを利用した蒸着操作により基板上に形成した誘電
体多層膜は、そのまま長時間放置すると、多層膜と基板
との間の剥離が発生しやすく、−旦剥離が発生した製品
は、これを加熱処理しても、発生した剥離はそのまま残
ってしまう、また、剥離が発生しない場合でも、長時間
経過後の熱処理は、本願発明の目的においては何ら有効
でない。"Immediately" in the above operation usually means within 24 hours, preferably within 12 hours, and more preferably within 6 hours. In other words, if a dielectric multilayer film formed on a substrate by a vapor deposition operation using ion blating is left as it is for a long time, peeling between the multilayer film and the substrate is likely to occur. Even if this is heat-treated, the peeling that has occurred remains as is.Also, even if no peeling occurs, heat treatment after a long period of time is not effective at all for the purpose of the present invention.
本発明において、誘電体多層膜の熱処理は、酸素または
酸素含有気体混合物の雰囲気中において４００℃以上、
かつ誘電体多層膜の実際の使用時の温度よりも１０℃以
上高い温度にて実施する。In the present invention, the dielectric multilayer film is heat-treated at 400°C or higher in an atmosphere of oxygen or an oxygen-containing gas mixture.
The test is carried out at a temperature that is 10° C. or more higher than the temperature at which the dielectric multilayer film is actually used.
酸素含有気体混合物としては、空気のような、酸素と窒
素（不活性気体）の混合物が用いられるが、酸素と他の
気体との組合せであってもよい。As the oxygen-containing gas mixture, a mixture of oxygen and nitrogen (an inert gas) is used, such as air, but a combination of oxygen and other gases may also be used.
加熱温度は、４００℃以上（好ましくは４１０℃以上）
であり、かつ通常では６００℃以下、好ましくは５９０
℃以下である。ただし、この加熱温度は、誘導体多層膜
製品の実際の使用に際しての想定到達温度より１０℃以
上高い必要がある。Heating temperature is 400°C or higher (preferably 410°C or higher)
and usually below 600°C, preferably 590°C
below ℃. However, this heating temperature needs to be 10° C. or more higher than the expected temperature when the dielectric multilayer film product is actually used.
好ましくは、想定到達温度より２０℃以上高い温度であ
り、さらに想定到達温度より５０℃以上高い温度が特に
好ましい。Preferably, the temperature is 20°C or more higher than the expected temperature to reach, and particularly preferably 50°C or more higher than the expected temperature to reach.
上記の加熱処理は、通常１０分〜５時間の範囲内の時間
をかけて行なわれる。この加熱処理時間は、３０分〜３
時間の範囲にあることが特に好ましい。The above heat treatment is usually carried out over a period of time ranging from 10 minutes to 5 hours. This heat treatment time is 30 minutes to 3
Particularly preferred is a range of hours.
［発明の効果］
本発明の製造法により得られる誘電体多層膜は、基板と
の密着性が良いのみではなく、耐熱性が顕著に高く、大
気中の長期間の実際の使用に際しても光学特性の劣化が
少なく、また誘電体多層膜と基板との間の剥離も発生し
にくい。[Effects of the Invention] The dielectric multilayer film obtained by the manufacturing method of the present invention not only has good adhesion to the substrate, but also has significantly high heat resistance, and has excellent optical properties even when actually used in the atmosphere for a long time. The deterioration of the dielectric multilayer film and the substrate is less likely to occur, and peeling between the dielectric multilayer film and the substrate is less likely to occur.
［実施例と比較例］
硫化亜鉛とフッ化マグネシウムとからなる誘電体多層膜
を、下記の条件により製造した。[Example and Comparative Example] A dielectric multilayer film made of zinc sulfide and magnesium fluoride was manufactured under the following conditions.
［実施例１］
イオンブレーティング装置：
特開昭６１−２３３９５７号公報に記載のイオン衝撃装
置を使用
高周波型カニ３００Ｗ
導入気体：アルゴン
真空槽内圧力＋８ＸＬＯ−’ｍｍＨｇ
基板：硬質ガラス（１２０℃）
積層膜数＝２２層
加熱雰囲気：空気（大気中）
加熱温度：４２０℃
加熱開始時期：積層終了後２時間後
加熱時間＝１時間
［比較例１］
イオンブレーティング装置：
特開昭６１−２３３９５７号公報に記載のイオン衝撃装
置を使用
高周波型カニ３００Ｗ
導入気体：アルゴン
真空槽内圧カニ ８ Ｘ １０−’ｍｍＨｇ基板：硬質
ガラス（１２０℃）
積層膜数＝２２層
加熱処理：無
［比較例２］
通常の真空蒸着装置を使用
導入気体：アルゴン
真空槽内圧カニ ８ Ｘ ｌ Ｏ−’ｍｍＨｇ基板：硬
質ガラス（１２０℃）
積層膜数＝２２層
加熱雰囲気：空気（大気中）
加熱温度＝４２０℃
加熱開始時期：積層終了後２時間後
加熱時間＝１時間
［誘導体多層膜の評価］
（１）光学特性変動
上記加熱処理後の実施例１と比較例２の誘電体多層膜に
おいて発生した光学特性の変動を調べた。この光学特性
の変動は、２０％透過率点の波長移動量（Δ入）と波長
５００ｎｍ点の透過率（Δｔ）を測定することにより評
価した。その結果を第１表に示す。[Example 1] Ion blasting device: Using the ion bombardment device described in JP-A No. 61-233957 High frequency type Crab 300W Introduced gas: Argon vacuum chamber pressure + 8XLO-'mmHg Substrate: Hard glass (120°C) Number of laminated films = 22 layers Heating atmosphere: Air (in the atmosphere) Heating temperature: 420°C Heating start time: 2 hours after completion of lamination Heating time = 1 hour [Comparative Example 1] Ion blating device: JP-A-61-233957 Using the ion bombardment device described in the publication.High frequency type crab 300W Introduced gas: Argon vacuum chamber internal pressure Crab 8 x 10-'mmHg Substrate: Hard glass (120°C) Number of laminated films = 22 layers Heat treatment: None [Comparative Example 2 ] Use ordinary vacuum evaporation equipment Introduced gas: Argon vacuum chamber internal pressure 8 X l O-'mmHg Substrate: Hard glass (120°C) Number of laminated films = 22 layers Heating atmosphere: Air (in the atmosphere) Heating temperature = 420°C Heating start time: 2 hours after completion of lamination Heating time = 1 hour [Evaluation of dielectric multilayer film] (1) Optical property variation Optical properties that occurred in the dielectric multilayer film of Example 1 and Comparative Example 2 after the above heat treatment We investigated the changes in This variation in optical properties was evaluated by measuring the amount of wavelength shift (Δin) at the 20% transmittance point and the transmittance (Δt) at the wavelength 500 nm point. The results are shown in Table 1.
第１表
Δλ （ｎ ｍ ）
Δ ｔ （％）
実施例１ ９ １
比較例２ １５ ２
実施例１と比較例１．２の誘電体多層膜の各々をについ
て大気中、４００℃、８４時間の強制加熱試験を行なっ
た。この強制加熱試験後の各誘電体多層膜において発生
した光学特性の変動を上記と同じ方法により調べた。そ
の結果を第２表に示す。Table 1 Δλ (n m ) Δ t (%) Example 1 9 1 Comparative Example 2 15 2 Each of the dielectric multilayer films of Example 1 and Comparative Example 1.2 was exposed to air at 400°C for 84 hours. A forced heating test was conducted. After this forced heating test, the variations in optical properties that occurred in each dielectric multilayer film were investigated using the same method as above. The results are shown in Table 2.
第２表
Δ入（ｎｍ） Δｔ（％）
実施例１ １０ ４
比較例１ ４６ ３５
比較例２ ３０ ２９
以上の結果から明らかなように、本発明に従いイオンブ
レーティング法を利用し、かつ多層膜形成後すぐに高温
加熱処理を行なって製造した誘電体多層膜は、その後の
過酷な加熱試験によっても光学特性の変動が少ない、す
なわち、実用上においての耐久性が顕著に向上している
。Table 2 ΔInput (nm) Δt (%) Example 1 10 4 Comparative Example 1 46 35 Comparative Example 2 30 29 As is clear from the above results, the ion blating method was used according to the present invention, and the multilayer film Dielectric multilayer films manufactured by performing high-temperature heat treatment immediately after formation exhibit little variation in optical properties even after subsequent severe heating tests, that is, their durability in practical use is significantly improved.
Claims (1)
性気体と不活性気体の混合気体の存在下で、該真空槽内
に設置された蒸発源より高屈折率膜の材料と低屈折率膜
の材料を交互に蒸発させ、イオンブレーティング法を利
用して、該真空槽内に保持された基板上に誘電体多層膜
を形成させたのち、すぐに該誘電体多層膜を、酸素もし
くは酸素含有気体混合物の雰囲気中において、４００℃
以上、かつ誘電体多層膜の実際の使用時の温度よりも１
０℃以上高い温度にて、熱処理を施すことからなる誘電
体多層膜の製造法。1. In the presence of a small amount of inert gas or a mixture of reactive gas and inert gas introduced into the vacuum chamber, the material of the high refractive index film and the low refractive index film are removed from the evaporation source installed in the vacuum chamber. After the dielectric multilayer film is formed on the substrate held in the vacuum chamber by alternately evaporating the materials and using the ion blating method, the dielectric multilayer film is immediately exposed to oxygen or 400°C in an atmosphere containing a gas mixture
above, and 1 higher than the temperature during actual use of the dielectric multilayer film.
A method for producing a dielectric multilayer film, which comprises performing heat treatment at a temperature higher than 0°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2139473A JP2902729B2 (en) | 1990-05-29 | 1990-05-29 | Manufacturing method of dielectric multilayer film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2139473A JP2902729B2 (en) | 1990-05-29 | 1990-05-29 | Manufacturing method of dielectric multilayer film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0432558A true JPH0432558A (en) | 1992-02-04 |
| JP2902729B2 JP2902729B2 (en) | 1999-06-07 |
Family
ID=15246065
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2139473A Expired - Lifetime JP2902729B2 (en) | 1990-05-29 | 1990-05-29 | Manufacturing method of dielectric multilayer film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2902729B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0772330A (en) * | 1993-05-26 | 1995-03-17 | Litton Syst Inc | Mirror for reflecting light having selected frequency and formation thereof |
| WO2020129558A1 (en) * | 2018-12-21 | 2020-06-25 | コニカミノルタ株式会社 | Dielectric multilayer film, method for producing same and optical member using same |
-
1990
- 1990-05-29 JP JP2139473A patent/JP2902729B2/en not_active Expired - Lifetime
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0772330A (en) * | 1993-05-26 | 1995-03-17 | Litton Syst Inc | Mirror for reflecting light having selected frequency and formation thereof |
| WO2020129558A1 (en) * | 2018-12-21 | 2020-06-25 | コニカミノルタ株式会社 | Dielectric multilayer film, method for producing same and optical member using same |
| JPWO2020129558A1 (en) * | 2018-12-21 | 2021-11-04 | コニカミノルタ株式会社 | Dielectric multilayer film, its manufacturing method, and optical members using it |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2902729B2 (en) | 1999-06-07 |
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