JP2006243567A - Infrared antireflection film - Google Patents
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- 239000000758 substrate Substances 0.000 claims abstract description 21
- 239000000126 substance Substances 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims description 17
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 claims description 4
- 230000003287 optical effect Effects 0.000 abstract description 12
- 238000003475 lamination Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 30
- 239000012788 optical film Substances 0.000 description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 230000035939 shock Effects 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000002834 transmittance Methods 0.000 description 4
- 230000003014 reinforcing effect Effects 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
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Abstract
Description
本発明は、赤外線領域の光学部材として用いられる赤外反射防止膜に関する。 The present invention relates to an infrared antireflection film used as an optical member in the infrared region.
従来から、Ｓｉ、ＺｎＳ、ＺｎＳｅなどの基板に、基板から数えて第１層目に中間屈折率のＳｉＯ、第２層目に高屈折率のＧｅ、第３層目に中間屈折率のＳｉＯ、第４層目に低屈折率のＭｇＦ2またはＭｇＦ2混合層を積層した赤外反射防止膜が知られている（例えば、特許文献１参照）。
しかしながら、このようなＭｇＦ2またはＭｇＦ2混合層を積層した赤外反射防止膜は、例えば５００℃程度の高熱処理を行なうと、肉眼では見えないが顕微鏡で観察できる膜割れ、膜剥がれが発生してしまう。 However, an infrared antireflection film in which such an MgF 2 or MgF 2 mixed layer is laminated, when subjected to a high heat treatment at about 500 ° C., causes film cracking and film peeling that cannot be seen with the naked eye but can be observed with a microscope. End up.
そこで、膜剥がれなどの原因として膜の密着力が弱いことが考えられるため、基板表面の改善を行ない、密着力を強化するために、成膜前にイオン銃によりイオン化した気体を基板に照射するイオンクリーニングを行なうことが考えられる。 Therefore, it is considered that the adhesion of the film is weak as a cause of film peeling, etc., so that the substrate surface is improved and the substrate is irradiated with ionized gas by an ion gun before film formation in order to improve the adhesion. It is conceivable to perform ion cleaning.
ところが、イオンクリーニングにより耐熱性を向上させようとしても、マイクロクラック（超微小なひび割れ）が発生してしまう。 However, even if the heat resistance is improved by ion cleaning, microcracks (ultra-fine cracks) are generated.
一般に、基板上に成膜した薄膜には、圧縮応力と引っ張り応力が生じる。これらの応力（ストレス）は成膜中に生じる薄膜の成長様式に依存した密度変化に伴って発生したり、基板と薄膜の熱膨張係数の違いにより発生したりする。 Generally, compressive stress and tensile stress are generated in a thin film formed on a substrate. These stresses (stresses) are generated with a density change depending on the growth mode of the thin film generated during film formation, or are generated due to a difference in thermal expansion coefficient between the substrate and the thin film.
上記ＭｇＦ2またはＭｇＦ2混合層を積層した赤外反射防止膜では、ＭｇＦ2の引っ張り応力が大きい。 In the infrared antireflection film in which the MgF 2 or MgF 2 mixed layer is laminated, the tensile stress of MgF 2 is large.
そのため、引っ張り応力が大きいＭｇＦ2の厚みが厚いことが原因しているものと考えられる。 Therefore, it is considered that the reason is that the thickness of MgF 2 having a large tensile stress is large.
そこで、本発明では、ＭｇＦ2またはＭｇＦ2混合層の厚みを薄くしても、光学特性を変化させず、高温環境下においてもマイクロクラック等が発生しない赤外反射防止膜を提供することを目的とする。 Accordingly, an object of the present invention is to provide an infrared antireflection film that does not change the optical characteristics even when the thickness of the MgF 2 or MgF 2 mixed layer is reduced and does not generate microcracks or the like even in a high temperature environment. And
上記課題を解決するため、請求項１に係る本発明は、Ｇｅ基板に中間屈折率物質と高屈折率物質を繰り返し積層し最外層にＭｇＦ2を積層した赤外反射防止膜において、中間屈折率物質と高屈折率物質の繰り返し積層膜を再度繰り返し積層しＭｇＦ2の厚みを薄くしたことを特徴とする。 In order to solve the above problems, the present invention according to claim 1 is an infrared antireflection film in which an intermediate refractive index substance and a high refractive index substance are repeatedly laminated on a Ge substrate, and MgF 2 is laminated on the outermost layer. It is characterized in that a repeated laminated film of a material and a high refractive index material is repeatedly laminated again to reduce the thickness of MgF 2 .
請求項２に係る本発明は、請求項１に記載の赤外反射防止膜において、中間屈折率物質をＧｅ、高屈折率物質をＳｉＯとしたことを特徴とする。 The present invention according to claim 2 is the infrared antireflection film according to claim 1, wherein the intermediate refractive index material is Ge and the high refractive index material is SiO.
請求項３に係る本発明は、Ｓｉ、ＺｎＳｅ、ＺｎＳのいずれか１つを基板とし、中間屈折率物質と高屈折率物質を繰り返し積層し最外層にＭｇＦ2を積層した赤外反射防止膜において、中間屈折率物質と高屈折率物質の繰り返し積層膜を再度繰り返し積層しＭｇＦ2の厚みを薄くしたことを特徴とする。 According to a third aspect of the present invention, there is provided an infrared antireflection film in which any one of Si, ZnSe, and ZnS is used as a substrate, an intermediate refractive index substance and a high refractive index substance are repeatedly laminated, and MgF 2 is laminated on the outermost layer. characterized by repeating the repeated stacked film of the intermediate-refractive index material and a high refractive index material again stacked and the thickness of MgF 2.
請求項４に係る本発明は、請求項３に記載の赤外反射防止膜において、中間屈折率物質をＧｅ、高屈折率物質をＳｉＯとしたことを特徴とする。 According to a fourth aspect of the present invention, in the infrared antireflection film according to the third aspect, the intermediate refractive index substance is Ge and the high refractive index substance is SiO.
本発明によれば、中間屈折率物質と高屈折率物質の繰り返し積層膜であるＧｅ−ＳｉＯを再度繰り返し積層し、ＭｇＦ2の厚みを薄くして、ＭｇＦ2の引っ張り応力（ストレス）を緩和し、光学特性を変化させず、高温環境下においても耐久性・耐熱性を向上させることができる。 According to the present invention, Ge—SiO, which is a repeated laminated film of an intermediate refractive index material and a high refractive index material, is repeatedly laminated again, the thickness of MgF 2 is reduced, and the tensile stress (stress) of MgF 2 is reduced. The durability and heat resistance can be improved even in a high temperature environment without changing the optical characteristics.
以下、図面を参照しつつ本発明の実施例を説明する。 Embodiments of the present invention will be described below with reference to the drawings.
〔実施例１〕
基板 Ｇｅ
第１層 Ｇｅ 光学膜厚 ０．２０λ0
第２層 ＳｉＯ 光学膜厚 ０．１０λ0
第３層 Ｇｅ 光学膜厚 ０．５０λ0
第４層 ＳｉＯ 光学膜厚 ０．３０λ0
第５層 Ｇｅ 光学膜厚 ０．２０λ0
第６層 ＳｉＯ 光学膜厚 ０．７０λ0
第７層 ＭｇＦ2 光学膜厚 ０．７０λ0
ただし、中心波長λ0＝３．５μｍである。
ここでＭｇＦ2の膜厚ｄを求めると、４ｎ・ｄ＝０．７０λ0
ｄ＝０．７０×３．５／４ｎ＝０．４５μｍ
（ただし、ＭｇＦ2の屈折率ｎは１．３７とする。）
なお、基板の材料としてはＧｅの他にＳｉ、ＺｎＳｅ、ＺｎＳを用いることができる。
[Example 1]
Substrate Ge
First layer Ge optical film thickness 0.20λ 0
Second layer SiO Optical film thickness 0.10λ 0
Third layer Ge optical film thickness 0.50λ 0
Fourth layer SiO Optical film thickness 0.30λ 0
5th layer Ge optical film thickness 0.20λ 0
Sixth layer SiO optical film thickness 0.70λ 0
7th layer MgF 2 optical film thickness 0.70λ 0
However, the center wavelength λ 0 = 3.5 μm.
Here, when the film thickness d of MgF 2 is determined, 4n · d = 0.70λ 0
d = 0.70 × 3.5 / 4n = 0.45 μm
(However, the refractive index n of MgF 2 is 1.37.)
As a substrate material, Si, ZnSe, or ZnS can be used in addition to Ge.
また、基板と第１層との間に密着強化層を設けてもよい。この密着強化層としては、Ａｌ2Ｏ3、Ｙ2Ｏ3、Ｔｉ2Ｏ3、ＴｉＯ、ＴｉＯ2のいずれであってもよい。なお、密着強化層は、３００ｎｍ以下の厚みである。
〔比較例１〕
実施例１と比較するために下記の比較例（従来例）１を示す。
基板 Ｇｅ
第１層 ＺｎＳ 光学膜厚 ０．４０λ0
第２層 Ｇｅ 光学膜厚 １．１５λ0
第３層 ＺｅＳ 光学膜厚 ３．０６λ0
第４層 ＭｇＦ2 光学膜厚 ３．１０λ0
ただし、中心波長λ0＝１．０μｍである。
ここで、ＭｇＦ2の膜厚ｄを求めると、４ｎｄ＝３．１０λ0
ｄ＝３．１０×１．０／４ｎ＝０．５７μｍ
（ただし、ＭｇＦ2の屈折率ｎは１．３７とする。）
この比較例１のＭｇＦ2の膜厚と実施例１のＭｇＦ2の膜厚との比を計算すると、０．４５／０．５７＝０．７９
となる。
Further, an adhesion reinforcing layer may be provided between the substrate and the first layer. The adhesion reinforcing layer may be any of Al 2 O 3 , Y 2 O 3 , Ti 2 O 3 , TiO, and TiO 2 . The adhesion reinforcing layer has a thickness of 300 nm or less.
[Comparative Example 1]
For comparison with Example 1, the following Comparative Example (Conventional Example) 1 is shown.
Substrate Ge
First layer ZnS optical film thickness 0.40λ 0
Second layer Ge optical film thickness 1.15λ 0
Third layer ZeS optical film thickness 3.06λ 0
Fourth layer MgF 2 optical film thickness 3.10λ 0
However, the center wavelength λ 0 = 1.0 μm.
Here, when the film thickness d of MgF 2 is obtained, 4nd = 3.10λ 0
d = 3.10 × 1.0 / 4n = 0.57 μm
(However, the refractive index n of MgF 2 is 1.37.)
When calculating the ratio of the thickness of the MgF 2 of Comparative Example 1 and MgF 2 having a film thickness of Example 1, 0.45 / 0.57 = 0.79
It becomes.
よって、実施例１のもののＭｇＦ2の膜厚は比較例１のもののＭｇＦ2の膜厚に対して約２割膜厚を減少させることができる。 Therefore, MgF 2 having a film thickness of those of Example 1 can be reduced from about 2 WarimakuAtsu for a film thickness of MgF 2 of that of Comparative Example 1.
また、実施例１と比較例１の各々の透過率（反射率）を表わすと、［図１］のようになり、９５％以上の透過率（５％以下の反射率）を示し、光学特性が変化していないことがわかる。 Further, the transmittance (reflectance) of Example 1 and Comparative Example 1 is expressed as shown in FIG. 1, showing a transmittance of 95% or more (reflectance of 5% or less), and optical characteristics. It can be seen that has not changed.
詳述すると、図１に示す通り、光学特性は、２.６〜６.０μｍの波長域で透過率が９５％以上であり、十分な光学特性を満足することがわかる。 More specifically, as shown in FIG. 1, it can be seen that the optical characteristics have a transmittance of 95% or more in the wavelength range of 2.6 to 6.0 μm and satisfy the sufficient optical characteristics.
次に、耐久性を測定する耐熱試験１、耐熱試験２、熱衝撃試験、耐水性試験を行なった。 Next, a heat resistance test 1, a heat resistance test 2, a thermal shock test, and a water resistance test for measuring durability were performed.
すなわち、耐熱試験１では、−８０度〜５５０度の温度サイクルを２回繰り返した。耐熱試験２では、液体窒素温度まで急冷した。また、１４０度で１００時間加熱処理した。熱衝撃試験では、蒸着した基板に熱衝撃を加えた。耐水性試験では、１６〜３２度の蒸留水（純水）に２４時間浸した。このような耐久試験を行なっても、劣化することがなかった。
〔実施例２〕
基板 Ｇｅ
第１層 Ｇｅ 光学膜厚 ０．２９λ0
第２層 ＳｉＯ 光学膜厚 ０．１４λ0
第３層 Ｇｅ 光学膜厚 ０．７１λ0
第４層 ＳｉＯ 光学膜厚 ０．４３λ0
第５層 Ｇｅ 光学膜厚 ０．２９λ0
第６層 ＳｉＯ 光学膜厚 １．００λ0
第７層 ＭｇＦ2 光学膜厚 １．００λ0
ただし、中心波長λ0＝２．４５μｍである。
That is, in the heat resistance test 1, a temperature cycle of −80 degrees to 550 degrees was repeated twice. In the heat resistance test 2, it was rapidly cooled to the liquid nitrogen temperature. Moreover, it heat-processed at 140 degree | times for 100 hours. In the thermal shock test, a thermal shock was applied to the deposited substrate. In the water resistance test, the sample was immersed in distilled water (pure water) at 16 to 32 degrees for 24 hours. Even when such an endurance test was performed, there was no deterioration.
[Example 2]
Substrate Ge
First layer Ge optical film thickness 0.29λ 0
Second layer SiO Optical film thickness 0.14λ 0
Third layer Ge optical film thickness 0.71λ 0
Fourth layer SiO optical film thickness 0.43λ 0
5th layer Ge optical film thickness 0.29λ 0
Sixth layer SiO optical film thickness 1.00λ 0
7th layer MgF 2 optical film thickness 1.00λ 0
However, the center wavelength λ 0 = 2.45 μm.
ここで、ＭｇＦ2の膜厚を求めると、屈折率ｎ＝１．３７を考慮し、
ｄ＝λ0／４ｎ＝４４５．１３ｎｍ
なお、光学膜厚として、下記の幅を採用することもできる。
第１層 0.01λ0≦4nd≦10.0λ0
第２層 0.71λ0≦4nd≦1.64λ0
第３層 0.50λ0≦4nd≦1.18λ0
第４層 0.84λ0≦4nd≦1.27λ0
第５層 0.86λ0≦4nd≦0.13λ0
第６層 0.75λ0≦4nd≦1.15λ0
第７層 0.70λ0≦4nd≦1.40λ0
〔比較例２〕
実施例２と比較するために下記の比較例（従来例）２を示す。
基板 Ｇｅ
第１層 ＺｎＳ 光学膜厚 ０．１３λ0
第２層 Ｇｅ 光学膜厚 ０．３７λ0
第３層 ＺｅＳ 光学膜厚 １．００λ0
第４層 ＭｇＦ2 光学膜厚 １．００λ0
ただし、中心波長λ0＝３．１０μｍである。
ここで、ＭｇＦ2の膜厚を求めると、
ｄ＝λ0／４ｎ＝５６３．２３ｎｍ
この実施例２の場合でも、従来に比べて約２割膜厚を減少させることができる。光学特性をグラフにすると図２に示すとおりである。
Here, when the film thickness of MgF 2 is obtained, the refractive index n = 1.37 is considered,
d = λ 0 /4n=445.13 nm
In addition, the following width | variety is also employable as an optical film thickness.
1st layer 0.01λ 0 ≦ 4nd ≦ 10.0λ 0
Second layer 0.71λ 0 ≦ 4nd ≦ 1.64λ 0
3rd layer 0.50λ 0 ≦ 4nd ≦ 1.18λ 0
4th layer 0.84λ 0 ≦ 4nd ≦ 1.27λ 0
5th layer 0.86λ 0 ≦ 4nd ≦ 0.13λ 0
6th layer 0.75λ 0 ≦ 4nd ≦ 1.15λ 0
7th layer 0.70λ 0 ≦ 4nd ≦ 1.40λ 0
[Comparative Example 2]
In order to compare with Example 2, the following comparative example (conventional example) 2 is shown.
Substrate Ge
First layer ZnS optical film thickness 0.13λ 0
Second layer Ge optical film thickness 0.37λ 0
Third layer ZeS optical film thickness 1.00λ 0
Fourth layer MgF 2 optical film thickness 1.00λ 0
However, the center wavelength λ 0 = 3.10 μm.
Here, when the film thickness of MgF 2 is obtained,
d = λ 0 /4n=563.23 nm
Even in the case of Example 2, the film thickness can be reduced by about 20% compared to the conventional case. The optical characteristics are shown in a graph in FIG.
この実施例２の場合も、実施例１と同様に光学特性は、２.６〜６.０μｍの波長域で透過率が９５％以上であり、十分な光学特性を満足することがわかる。 In the case of Example 2, as in Example 1, the optical characteristics have a transmittance of 95% or more in the wavelength range of 2.6 to 6.0 μm, and it can be seen that sufficient optical characteristics are satisfied.
また、同様に、耐久性を測定する耐熱試験１、耐熱試験２、熱衝撃試験、耐水性試験を行なった。 Similarly, a heat resistance test 1, a heat resistance test 2, a thermal shock test, and a water resistance test for measuring durability were performed.
すなわち、耐熱試験１では、−８０度〜５５０度の温度サイクルを２回繰り返した。耐熱試験２では、液体窒素温度まで急冷した。また、１４０度で１００時間加熱処理した。熱衝撃試験では、蒸着した基板に熱衝撃を加えた。耐水性試験では、１６〜３２度の蒸留水（純水）に２４時間浸した。このような耐久試験を行なっても、劣化することがなかった。 That is, in the heat resistance test 1, a temperature cycle of −80 degrees to 550 degrees was repeated twice. In the heat resistance test 2, it was rapidly cooled to the liquid nitrogen temperature. Moreover, it heat-processed at 140 degree | times for 100 hours. In the thermal shock test, a thermal shock was applied to the deposited substrate. In the water resistance test, the sample was immersed in distilled water (pure water) at 16 to 32 degrees for 24 hours. Even when such an endurance test was performed, there was no deterioration.
なお、本発明では、基板の片面に赤外反射防止膜を蒸着したが、これに限定されず、両面に蒸着しても良い。両面に蒸着することにより、ＭｇＦ2の引っ張り応力（ストレス）が両面で相殺され、膜の劣化を防止し、耐久性・耐熱性を更に向上させることができる。 In the present invention, the infrared antireflection film is vapor-deposited on one side of the substrate. However, the present invention is not limited to this, and it may be vapor-deposited on both sides. By vapor-depositing on both sides, the tensile stress (stress) of MgF 2 is canceled on both sides, the film can be prevented from being deteriorated, and the durability and heat resistance can be further improved.
Claims (4)
中間屈折率物質と高屈折率物質の繰り返し積層膜を再度繰り返し積層しＭｇＦ2の厚みを薄くしたことを特徴とする赤外反射防止膜。 In an infrared antireflection film in which an intermediate refractive index substance and a high refractive index substance are repeatedly laminated on a Ge substrate and MgF 2 is laminated on the outermost layer
An infrared antireflection film, wherein an intermediate refractive index material and a high refractive index material are repeatedly stacked again to reduce the thickness of MgF 2 .
中間屈折率物質をＧｅ、高屈折率物質をＳｉＯとしたことを特徴とする赤外反射防止膜。 The infrared antireflection film according to claim 1,
An infrared antireflection film characterized in that the intermediate refractive index material is Ge and the high refractive index material is SiO.
中間屈折率物質と高屈折率物質を繰り返し積層し最外層にＭｇＦ2を積層した赤外反射防止膜において、
中間屈折率物質と高屈折率物質の繰り返し積層膜を再度繰り返し積層しＭｇＦ2の厚みを薄くしたことを特徴とする赤外反射防止膜。 One of Si, ZnSe, and ZnS is used as a substrate,
In the infrared antireflection film in which an intermediate refractive index substance and a high refractive index substance are repeatedly laminated and MgF 2 is laminated on the outermost layer,
An infrared antireflection film, wherein an intermediate refractive index material and a high refractive index material are repeatedly stacked again to reduce the thickness of MgF 2 .
中間屈折率物質をＧｅ、高屈折率物質をＳｉＯとしたことを特徴とする赤外反射防止膜。 In the infrared antireflection film according to claim 3,
An infrared antireflection film characterized in that the intermediate refractive index material is Ge and the high refractive index material is SiO.
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| JPH08114701A (en) * | 1994-10-14 | 1996-05-07 | Topcon Corp | Infrared antireflection film |
| JPH11281801A (en) * | 1998-03-27 | 1999-10-15 | Minolta Co Ltd | Infrared reflection preventive film |
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| JPH08114701A (en) * | 1994-10-14 | 1996-05-07 | Topcon Corp | Infrared antireflection film |
| JPH11281801A (en) * | 1998-03-27 | 1999-10-15 | Minolta Co Ltd | Infrared reflection preventive film |
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| JPWO2017195603A1 (en) * | 2016-05-13 | 2018-08-23 | 三菱電機株式会社 | Optical components and laser processing machines |
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