JPH0862402A - Antireflection coating and manufacture thereof - Google Patents

Antireflection coating and manufacture thereof

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Publication number
JPH0862402A
JPH0862402A JP6224179A JP22417994A JPH0862402A JP H0862402 A JPH0862402 A JP H0862402A JP 6224179 A JP6224179 A JP 6224179A JP 22417994 A JP22417994 A JP 22417994A JP H0862402 A JPH0862402 A JP H0862402A
Authority
JP
Japan
Prior art keywords
target
refractive index
sio
fluoride
mixture
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.)
Withdrawn
Application number
JP6224179A
Other languages
Japanese (ja)
Inventor
Toshiaki Oimizu
利明 生水
Nobuyoshi Toyohara
延好 豊原
Takeshi Kawamata
健 川俣
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.)
Olympus Corp
Original Assignee
Olympus Optical Co Ltd
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 Olympus Optical Co Ltd filed Critical Olympus Optical Co Ltd
Priority to JP6224179A priority Critical patent/JPH0862402A/en
Publication of JPH0862402A publication Critical patent/JPH0862402A/en
Withdrawn legal-status Critical Current

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Abstract

PURPOSE: To form an antireflection coating having sufficient optical characteristics by constituting a target with a mixture of fluoride and SiO2 and by subjecting the target to sputtering. CONSTITUTION: A target is constituted with a mixture of fluoride, whose refractive index is lower than that of SiO2 and SiO2 , and the target is subjected to sputtering for forming an antireflection coating. As fluoride, CaF2 , LiF, SrF2 , Na3 AIF6 or Na5 Al3 F14 is preferable. The mixture in the target may be in a chemically bonded condition or in a merely mixed condition. The refractive index of the coating thus formed is approximately 1.36 to 1.43 that is lower than that of SiO2 , and even in a single layer, sufficient antireflective effect can be obtained. Even in the case where a polarized beam splitter or an edge filter is constituted, sufficient characteristics can be obtained with a fewer number of layers.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【産業上の利用分野】本発明は、光学部品に用いられる
反射防止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 an antireflection film used for optical parts and a method for manufacturing the same.

【0002】[0002]

【従来の技術】近年、基板を加熱することなく優れた膜
の密着性を得られることや、自動化の容易さといった利
点から、スパッタリング法による光学薄膜形成の技術が
注目されている。ところが、真空蒸着法の場合に低屈折
率材料として最も一般的に用いられているMgF2 は、
スパッタリングを行うことによりフッ素が解離し可視光
の吸収が生じるため、使用することができない。そのた
め、SiO2 あるいはSiO2 と他の物質との混合物を
用いることが検討されている。例えば、特開平2−96
701号公報には、低屈折率材料にSiO2 、SiO2
とアルミナ(Al2 3 )との混合物、またはSiO2
を主成分とする物質を用い、高屈折率材料にTiO2
Ta2 5 ,ZrO2 ,In2 3 ,SnO2 ,Nb2
5 もしくはYb2 3 またはこれらの混合物を用い
て、透明基板上に前記高屈折率材料と前記低屈折率材料
をスパッタリングにより交互に積層することにより反射
防止膜を得ることが開示されている。
2. Description of the Related Art In recent years, a technique for forming an optical thin film by a sputtering method has attracted attention because of its advantages such as excellent film adhesion without heating the substrate and easiness of automation. However, in the case of the vacuum deposition method, MgF 2 which is most commonly used as a low refractive index material is
Fluorine is dissociated by the sputtering and absorption of visible light occurs, so that it cannot be used. Therefore, it is considered to use SiO 2 or a mixture of SiO 2 and another substance. For example, JP-A-2-96
No. 701 discloses that low refractive index materials include SiO 2 and SiO 2.
Of alumina and alumina (Al 2 O 3 ) or SiO 2
Is used as a high refractive index material, and TiO 2 ,
Ta 2 O 5 , ZrO 2 , In 2 O 3 , SnO 2 , Nb 2
It is disclosed that an antireflection film is obtained by alternately stacking the high refractive index material and the low refractive index material on a transparent substrate by sputtering using O 5 or Yb 2 O 3 or a mixture thereof. .

【0003】[0003]

【発明が解決しようとする課題】しかし、SiO2 の屈
折率は1.46程度であり、MgF2 (屈折率1.3
8)と比較して高いため、反射防止膜に用いる場合に、
単層のみでは充分な反射防止効果を得られない。そのた
め、2層以上の膜構成としなければ実用的な反射防止効
果を得られず、さらに、得られた反射防止効果も充分と
はいえない。また、偏光ビームスプリッターやエッジフ
ィルター等を構成する場合には、高屈折率と低屈折率と
の屈折率差が大きいほうが望ましいが、低屈折率として
SiO2 を使うと充分な特性を得られなかったり、層数
が増えてコストアップにつながる等の問題が生じる。
However, the refractive index of SiO 2 is about 1.46, and MgF 2 (refractive index 1.3
Since it is higher than that of 8), when used for an antireflection film,
A single layer alone cannot provide a sufficient antireflection effect. Therefore, a practical antireflection effect cannot be obtained unless the film structure has two or more layers, and the obtained antireflection effect is not sufficient. Further, when constructing a polarization beam splitter, an edge filter, or the like, it is desirable that the difference in refractive index between the high refractive index and the low refractive index is large, but if SiO2 is used as the low refractive index, sufficient characteristics may not be obtained. However, there is a problem that the number of layers increases and the cost increases.

【0004】本発明は、かかる従来の問題点に鑑みてな
されたもので、請求項1に係る発明は、充分な光学特性
を有する反射防止膜を製造するのに適した製造方法を提
供することを目的とする。請求項2に係る発明は、充分
な光学特性を有する反射防止膜を提供することを目的と
する。
The present invention has been made in view of the above conventional problems, and the invention according to claim 1 provides a manufacturing method suitable for manufacturing an antireflection film having sufficient optical characteristics. With the goal. An object of the invention according to claim 2 is to provide an antireflection film having sufficient optical characteristics.

【0005】[0005]

【課題を解決するための手段】上記課題を解決するため
に、請求項1に係る発明は、フッ化物とSiO2 との混
合物でターゲットを構成し、このターゲットをスパッタ
リングすることにより反射防止膜を形成することとし
た。請求項2に係る発明は、上記フッ化物がCaF2
LiF,SrF2 ,Na3AlF6 またはNa5 Al3
14からなり、請求項1記載の製造方法により成膜した
層を少なくとも1層設けた反射防止膜である。
In order to solve the above-mentioned problems, the invention according to claim 1 constitutes a target with a mixture of fluoride and SiO 2 and forms an antireflection film by sputtering this target. It was decided to form. In the invention according to claim 2, the fluoride is CaF 2 ,
LiF, SrF 2 , Na 3 AlF 6 or Na 5 Al 3
An antireflection film comprising F 14 and provided with at least one layer formed by the manufacturing method according to claim 1.

【0006】[0006]

【作用】SiO2 より屈折率の低いフッ化物(Ca
2 ,LiF,SrF2 ,Na3 AlF6 ,Na5 Al
3 14)にSiO2 を混合したターゲットをスパッタリ
ングすることにより、フッ素の解離が抑制され吸収の極
めて少ない膜を容易に得ることを、鋭意研究の結果、見
い出した。また、SiO2 の割合は、1重量%以上あれ
ば著しい効果が認められるが、特に制限するものではな
い。一方、SiO2 を加えることにより一般的に屈折率
は上昇してしまうため、必要量以上に混合するのは光学
特性の点からあまり望ましいことではない。なお、ター
ゲット中の混合物は化学的に結合した状態となっていて
も良いし、単なる混合状態でも良い。
[Function] Fluoride (Ca, which has a lower refractive index than SiO 2
F 2 , LiF, SrF 2 , Na 3 AlF 6 , Na 5 Al
As a result of earnest research, it has been found that a film in which fluorine dissociation is suppressed and absorption is extremely small can be easily obtained by sputtering a target in which 3 F 14 ) is mixed with SiO 2 . Further, if the proportion of SiO 2 is 1% by weight or more, a remarkable effect is recognized, but it is not particularly limited. On the other hand, since the refractive index is generally increased by adding SiO 2 , it is not desirable from the viewpoint of optical characteristics to mix more than necessary amount. The mixture in the target may be in a chemically bound state or may be a simple mixed state.

【0007】以上のような方法により形成した膜の屈折
率は、混合物の添加量や成膜条件にもよるが、おおよそ
1.36から1.43程度とSiO2 に比べて低い。し
たがって、単層のみでも充分な反射防止効果を得ること
ができ、また、偏光ビームスプリッターやエッジフィル
ター等を構成する場合にも少ない層数で充分な特性を得
ることができる。
The refractive index of the film formed by the above method is about 1.36 to 1.43, which is lower than that of SiO 2 , though it depends on the amount of the mixture added and the film forming conditions. Therefore, a sufficient antireflection effect can be obtained even with only a single layer, and sufficient characteristics can be obtained with a small number of layers even when configuring a polarization beam splitter, an edge filter, or the like.

【0008】[0008]

【実施例】【Example】

[実施例1]屈折率1.75のガラス基板を真空槽にセ
ットし、2×10-4Paまで排気した後、分圧が0.3
PaのArガスを真空槽に導入した。基板加熱は行わ
ず、ターゲットは、LiFとSiO2 を重量比で8:2
に混合したものを使用した。高周波マグネトロンスパッ
タリング法を用い、投入電力100Wとして表1の膜厚
で成膜を行い、反射防止膜を得た。
Example 1 A glass substrate having a refractive index of 1.75 was set in a vacuum chamber and evacuated to 2 × 10 −4 Pa, and then a partial pressure was 0.3.
Ar gas of Pa was introduced into the vacuum chamber. The substrate was not heated, and the target was LiF and SiO 2 in a weight ratio of 8: 2.
The mixture was used. The high frequency magnetron sputtering method was used to form films with the film thicknesses shown in Table 1 at an input power of 100 W to obtain antireflection films.

【0009】[0009]

【表1】 [Table 1]

【0010】本実施例による反射防止膜の分光特性を図
1に示す。本実施例の反射防止膜は、図1に示すよう
に、波長400〜700nmで反射率が2%以下、特に
520nmで0.5%以下と充分に低く、単層で充分な
反射防止効果が得られ、また、可視域400〜700n
mでの吸収もなかった。
The spectral characteristics of the antireflection film according to this embodiment are shown in FIG. As shown in FIG. 1, the antireflection film of this example has a sufficiently low reflectance of 2% or less at a wavelength of 400 to 700 nm, particularly 0.5% or less at 520 nm, and has a sufficient antireflection effect in a single layer. Obtained and visible range 400-700n
There was no absorption at m.

【0011】[実施例2]アクリル樹脂基板(PMM
A)を真空槽にセットし、7×10-3Paまで排気した
後、分圧が1.5PaのArガスと、分圧が1PaのO
2 ガスを真空槽に導入した。基板加熱は行わず、ターゲ
ットは、CaF2 とSiO2 とをそれぞれ粉砕した後、
80:1の重量比で混合し焼結したものを低屈折率材料
として使用し、高屈折率材料としてWO3 を使用した。
それぞれ100Wの高周波マグネトロンスパッタリング
法にて表2の膜厚で成膜を行い、反射防止膜を得た。
Example 2 Acrylic resin substrate (PMM
A) was set in a vacuum chamber and evacuated to 7 × 10 −3 Pa, then Ar gas with a partial pressure of 1.5 Pa and O with a partial pressure of 1 Pa.
Two gases were introduced into the vacuum chamber. The substrate was not heated, the target was crushed CaF 2 and SiO 2 respectively,
What was mixed and sintered at a weight ratio of 80: 1 was used as a low refractive index material, and WO 3 was used as a high refractive index material.
Films having the film thicknesses shown in Table 2 were formed by a 100 W high-frequency magnetron sputtering method to obtain antireflection films.

【0012】[0012]

【表2】 [Table 2]

【0013】本実施例による反射防止膜の分光特性を図
2に示す。本実施例の反射防止膜は、波長400〜70
0nmで反射率0.8%、平均反射率0.3%以下の優
れた反射防止効果が得られた。また、実施例1と同様
に、吸収は全くみられなかった。
The spectral characteristics of the antireflection film according to this embodiment are shown in FIG. The antireflection film of this example has a wavelength of 400 to 70.
An excellent antireflection effect with a reflectance of 0% at 0 nm and an average reflectance of 0.3% or less was obtained. Also, as in Example 1, no absorption was observed.

【0014】本実施例によれば、ターゲットとしてCa
2 とSiO2 とを混合したものを用いたため、フッ素
の解離を抑えることができ、吸収のない膜を容易に得る
ことができた。また、膜のテープ剥離試験を行ったが密
着性に関しても何ら問題はなかった。SiO2 と混合す
るフッ化物としてSrF2 を用いても同様の効果が得ら
れた。
According to this embodiment, Ca is used as a target.
Since a mixture of F 2 and SiO 2 was used, dissociation of fluorine could be suppressed and a film without absorption could be easily obtained. Further, a tape peeling test of the film was conducted, but there was no problem with the adhesion. The same effect was obtained by using SrF 2 as the fluoride mixed with SiO 2 .

【0015】[実施例3]ポリカーボネート樹脂基板
(PC)を真空槽にセットし、5×10-3Torrまで
排気した後、分圧が0.2PaのNeガスを真空槽に導
入した。ターゲットは、Na3 AlF6 とSiO2 をそ
れぞれ粉砕した後、9:1の重量比で混合し焼結したも
のを低屈折率材料として使用し、高屈折率材料としてZ
rO2 を使用した。それぞれ100Wの高周波スパッタ
リング法にて表3の膜厚で成膜を行い、反射防止膜を得
た。
Example 3 A polycarbonate resin substrate (PC) was set in a vacuum chamber and evacuated to 5 × 10 −3 Torr, and then Ne gas having a partial pressure of 0.2 Pa was introduced into the vacuum chamber. The target was crushed Na 3 AlF 6 and SiO 2 , respectively, mixed at a weight ratio of 9: 1 and sintered, and used as a low refractive index material, and as a high refractive index material Z.
rO 2 was used. Films having the film thicknesses shown in Table 3 were formed by a high-frequency sputtering method of 100 W to obtain antireflection films.

【0016】[0016]

【表3】 [Table 3]

【0017】本実施例の反射防止膜は、図3に示すよう
に、波長420〜700nmで反射率1%以下、平均反
射率0.3%以下の優れた分光特性を有していた。本実
施例によれば、ターゲットとしてNa3 AlF6 とSi
2 とを混合したものを用いたため、実施例2と同様
に、吸収のない膜を容易に得ることができた。また、混
合物の屈折率が実施例2よりも低いため、わずかながら
より低い屈折率を得ることができた。なお、SiO2
混合するフッ化物としてNa5 Al314を用いても同
様の効果が得られた。
As shown in FIG. 3, the antireflection film of this example had excellent spectral characteristics with a reflectance of 1% or less and an average reflectance of 0.3% or less at a wavelength of 420 to 700 nm. According to this embodiment, Na 3 AlF 6 and Si are used as targets.
Since a mixture of O 2 was used, a film without absorption could be easily obtained as in Example 2. Moreover, since the refractive index of the mixture was lower than that of Example 2, a slightly lower refractive index could be obtained. The same effect was obtained even when Na 5 Al 3 F 14 was used as the fluoride mixed with SiO 2 .

【0018】[比較例1]ポリカーボネート樹脂基板
(PC)を真空槽にセットし、2×10-4Paまで排気
した後、分圧が0.3PaのArガスを真空槽に導入し
た。基板加熱は行わず、低屈折率材料にはSiO2 、高
屈折率材料にはZrO2 のターゲットを用いて、それぞ
れ100Wの高周波マグネトロンスパッタリング法にて
表4の膜厚で成膜を行い、反射防止膜を得た。
Comparative Example 1 A polycarbonate resin substrate (PC) was set in a vacuum chamber and evacuated to 2 × 10 -4 Pa, and then Ar gas having a partial pressure of 0.3 Pa was introduced into the vacuum chamber. The substrate was not heated, SiO 2 was used as the low-refractive index material, and ZrO 2 was used as the high-refractive index material. The prevention film was obtained.

【0019】[0019]

【表4】 [Table 4]

【0020】本比較例による反射防止膜の分光特性を図
4に示す。本比較例においては、上記実施例と同様に、
可視域の波長400〜700nmでの吸収はみられない
ものの、波長430〜700nmで反射率1%以下、平
均反射率0.7%以下と反射率が高めであり、充分な反
射防止効果が得られているとは言い難い。
The spectral characteristics of the antireflection film according to this comparative example are shown in FIG. In this comparative example, as in the above example,
Absorption at wavelengths of 400 to 700 nm in the visible region is not observed, but reflectance is high at 1% or less and average reflectance of 0.7% or less at wavelengths of 430 to 700 nm, and sufficient antireflection effect is obtained. It is hard to say that it is being done.

【0021】[0021]

【発明の効果】以上のように、請求項1に係る発明によ
れば、フッ化物にSiO2 を混合したターゲットを用い
たので、基板を加熱せずに充分な密着性を確保すること
ができ、自動化が容易であるなどの利点を持つスパッタ
リング法により、可視光の吸収の少ない低反射率の反射
防止膜を容易に得ることができる。請求項2に係る発明
によれば、SiO2 より屈折率の低いフッ化物を用いる
ことで、低屈折率材料としてSiO2 のみを用いた反射
防止膜に比べて光学性能が高くなる。
As described above, according to the invention of claim 1, since the target in which the fluoride is mixed with SiO 2 is used, it is possible to secure sufficient adhesion without heating the substrate. By the sputtering method, which has advantages such as easy automation, it is possible to easily obtain an antireflection film having a low reflectance and a low absorption of visible light. According to the second aspect of the present invention, by using the fluoride having a lower refractive index than SiO 2 , the optical performance becomes higher than that of the antireflection film using only SiO 2 as the low refractive index material.

【図面の簡単な説明】[Brief description of drawings]

【図1】実施例1の反射防止膜の分光特性を示すグラフ
である。
FIG. 1 is a graph showing spectral characteristics of an antireflection film of Example 1.

【図2】実施例2の反射防止膜の分光特性を示すグラフ
である。
FIG. 2 is a graph showing the spectral characteristics of the antireflection film of Example 2.

【図3】実施例3の反射防止膜の分光特性を示すグラフ
である。
3 is a graph showing the spectral characteristics of the antireflection film of Example 3. FIG.

【図4】比較例1の反射防止膜の分光特性を示すグラフ
である。
FIG. 4 is a graph showing the spectral characteristics of the antireflection film of Comparative Example 1.

Claims (2)

【特許請求の範囲】[Claims] 【請求項1】 フッ化物とSiO2 との混合物でターゲ
ットを構成し、このターゲットをスパッタリングするこ
とにより形成することを特徴とする反射防止膜の製造方
法。
1. A method for producing an antireflection film, which comprises forming a target with a mixture of a fluoride and SiO 2, and forming the target by sputtering.
【請求項2】 上記フッ化物はCaF2 ,LiF,Sr
2 ,Na3 AlF6 またはNa5 Al3 14からな
り、請求項1記載の製造方法により成膜した層を少なく
とも1層設けたことを特徴とする反射防止膜。
2. The fluoride is CaF 2 , LiF, Sr.
An antireflection film comprising at least one layer formed of F 2 , Na 3 AlF 6 or Na 5 Al 3 F 14 and formed by the manufacturing method according to claim 1.
JP6224179A 1994-08-25 1994-08-25 Antireflection coating and manufacture thereof Withdrawn JPH0862402A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP6224179A JPH0862402A (en) 1994-08-25 1994-08-25 Antireflection coating and manufacture thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP6224179A JPH0862402A (en) 1994-08-25 1994-08-25 Antireflection coating and manufacture thereof

Publications (1)

Publication Number Publication Date
JPH0862402A true JPH0862402A (en) 1996-03-08

Family

ID=16809769

Family Applications (1)

Application Number Title Priority Date Filing Date
JP6224179A Withdrawn JPH0862402A (en) 1994-08-25 1994-08-25 Antireflection coating and manufacture thereof

Country Status (1)

Country Link
JP (1) JPH0862402A (en)

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Date Code Title Description
A300 Withdrawal of application because of no request for examination

Free format text: JAPANESE INTERMEDIATE CODE: A300

Effective date: 20011106