JPH08146201A - Production of optical thin film - Google Patents
Production of optical thin filmInfo
- Publication number
- JPH08146201A JPH08146201A JP6289395A JP28939594A JPH08146201A JP H08146201 A JPH08146201 A JP H08146201A JP 6289395 A JP6289395 A JP 6289395A JP 28939594 A JP28939594 A JP 28939594A JP H08146201 A JPH08146201 A JP H08146201A
- Authority
- JP
- Japan
- Prior art keywords
- target
- film
- thin film
- single crystal
- optical thin
- 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
- 230000003287 optical effect Effects 0.000 title claims abstract description 15
- 239000010409 thin film Substances 0.000 title claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- 239000010408 film Substances 0.000 claims abstract description 53
- 238000000034 method Methods 0.000 claims abstract description 18
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims abstract description 16
- 239000007789 gas Substances 0.000 claims abstract description 13
- 239000011261 inert gas Substances 0.000 claims abstract description 5
- 238000005546 reactive sputtering Methods 0.000 claims abstract description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 4
- 239000001301 oxygen Substances 0.000 claims abstract description 4
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 14
- 239000000758 substrate Substances 0.000 abstract description 16
- 239000013078 crystal Substances 0.000 abstract description 3
- 230000003746 surface roughness Effects 0.000 abstract description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract 2
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- 238000010891 electric arc Methods 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 description 9
- 238000001755 magnetron sputter deposition Methods 0.000 description 7
- 238000004544 sputter deposition Methods 0.000 description 7
- 230000003595 spectral effect Effects 0.000 description 6
- 239000013077 target material Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000000149 argon plasma sintering Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000010419 fine particle Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000001552 radio frequency sputter deposition Methods 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 230000032900 absorption of visible light Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000009191 jumping Effects 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
Landscapes
- Surface Treatment Of Optical Elements (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、スパッタリング法によ
り光学薄膜を製造する方法に係り、特にＳｉＯ2 膜を形
成する光学薄膜の製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing an optical thin film by a sputtering method, and more particularly to a method for producing an optical thin film for forming a SiO 2 film.
【０００２】[0002]
【従来の技術】従来、反射防止膜やミラー、干渉フィル
ターなどの光学薄膜を光学部品に形成する場合、膜材料
を加熱して蒸発させ、それを基板に付着させる真空蒸着
法が主に使われてきた。しかし、近年になり、これら光
学薄膜においても、真空蒸着法と比較して自動化、省力
化、大面積基板への適用性などの点で有利なスパッタリ
ング法によるコーティングの要求が高まってきた。2. Description of the Related Art Conventionally, when forming an optical thin film such as an antireflection film, a mirror or an interference filter on an optical component, a vacuum evaporation method has been mainly used in which a film material is heated to evaporate and adhered to a substrate. Came. However, in recent years, even for these optical thin films, there is an increasing demand for coating by a sputtering method, which is advantageous in terms of automation, labor saving, applicability to a large area substrate, etc., as compared with the vacuum vapor deposition method.
【０００３】スパッタリング法に適した低屈折率物質と
してはＳｉＯ2 が多く用いられる。そして、一般に、Ｄ
Ｃスパッタリング法による方がＲＦスパッタリング法よ
りも、成膜速度が速い、基板の温度上昇が少ない、制御
性がよい、電源価格が安い等の利点があることが知られ
ており、ＤＣスパッタリング法を採用したいというニー
ズが大きい。ところが、Ｓｉターゲットを用いたＤＣス
パッタリング法によりＳｉＯ2 膜を形成しようとした場
合、上記のように成膜速度が速い等の利点はあるもの
の、アークが発生してターゲット材料表面の微粒子が跳
び出してしまい、外観上の問題がでやすい等の欠点があ
り、光学的用途に用いる薄膜の製造方法としては不向き
であった。SiO 2 is often used as a low refractive index material suitable for the sputtering method. And, in general, D
It is known that the C sputtering method has advantages over the RF sputtering method such as a faster film formation rate, less increase in substrate temperature, better controllability, and lower power supply cost. There is a great need to adopt it. However, if an attempt is made to form a SiO 2 film by a DC sputtering method using a Si target, an arc is generated and fine particles on the surface of the target material jump out although there are advantages such as a high film formation rate as described above. However, it is not suitable as a method for producing a thin film used for optical applications because it has drawbacks such as easy appearance problems.
【０００４】そこで、ターゲット材料の固体粒子の跳び
出しを防ぐ方法として、例えば、特公平４−６１３２８
号公報には、注型し、溶融状態から凝固した多結晶珪素
成形体をターゲットとし、ＤＣスパッタリング法により
ＳｉＯ2 膜を形成する方法が開示されている。Therefore, as a method for preventing the solid particles of the target material from jumping out, for example, Japanese Patent Publication No. 4-61328.
The publication discloses a method of forming a SiO 2 film by a DC sputtering method, using a polycrystalline silicon compact which is cast and solidified from a molten state as a target.
【０００５】[0005]
【発明が解決しようとする課題】しかし、上記公報記載
の従来技術では、ターゲット材料として多結晶のものを
用いているために、粒界が存在した。粒界には不純物が
析出しやすく、不純物はＳｉとスパッタ率が異なるため
に、ミクロに見れば粒界付近では不均一にスパッタされ
ており、ターゲット材料の表面粗さが大きくなってしま
う。そして、粒界付近に形成された尖端部に電圧が集中
することで、アークが発生しやすくなってしまう。ま
た、アークが発生しないまでもターゲット面内の均一性
が良くないために、形成される膜質の均一性も低くなっ
てしまうという問題点があった。さらに、上記従来技術
では、特殊なターゲット材料を用いるためにその設備が
必要になり、入手性に難があるとともに、またコストア
ップになりやすいという問題点もあった。However, in the prior art described in the above publication, grain boundaries exist because the target material is polycrystalline. Impurities tend to precipitate at the grain boundaries, and since the impurities have a different sputter rate from Si, microscopically, they are non-uniformly sputtered near the grain boundaries, and the surface roughness of the target material increases. Then, the voltage is concentrated on the tip portion formed near the grain boundary, so that the arc easily occurs. Further, even if the arc is not generated, the uniformity in the target surface is not good, so that there is a problem in that the uniformity of the quality of the formed film is reduced. Further, in the above-mentioned conventional technique, there is a problem that the equipment is required because a special target material is used, the availability is difficult, and the cost is easily increased.
【０００６】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、高品質な光学薄
膜として用いることのできるＳｉＯ2 膜をスパッタリン
グ法により生産性良く、低コストで製造することができ
る光学薄膜の製造方法を提供することを目的とする。The present invention has been made in view of the above-mentioned conventional problems. The invention according to claim 1 is a SiO 2 film which can be used as a high quality optical thin film and has a high productivity and a low productivity by a sputtering method. An object of the present invention is to provide a method for manufacturing an optical thin film that can be manufactured at low cost.
【０００７】請求項２に係る発明は、上記目的に加え、
アークの発生を確実に抑制し、より高品質なＳｉＯ2 膜
を形成することができる光学薄膜の製造方法を提供する
ことを目的とする。The invention according to claim 2 provides, in addition to the above objects,
An object of the present invention is to provide a method for producing an optical thin film capable of reliably suppressing generation of an arc and forming a higher quality SiO 2 film.
【０００８】[0008]
【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、光学薄膜を製造するにあた
り、単結晶Ｓｉターゲットを用いて、酸素を含むガスお
よび不活性ガスの少なくとも２種類のガスを導入した雰
囲気中で、直流電源に正電圧をパルス状に印加しなが
ら、反応性スパッタリング法によりＳｉＯ2 膜を形成す
ることとした。In order to solve the above-mentioned problems, the invention according to claim 1 uses a single crystal Si target to manufacture an optical thin film, and at least a gas containing oxygen and an inert gas are used. It was decided to form a SiO 2 film by the reactive sputtering method while applying a positive voltage in a pulse form to a DC power source in an atmosphere in which two kinds of gases were introduced.
【０００９】請求項２に係る発明は、請求項１に係る発
明において、単結晶Ｓｉターゲットの抵抗値が１０ｍΩ
・ｃｍ以下であることを特徴とする。The invention according to claim 2 is the invention according to claim 1, wherein the resistance value of the single crystal Si target is 10 mΩ.
・ Characteristics are below cm.
【００１０】[0010]
【作用】本発明ではターゲットとして単結晶のＳｉを用
いることとした。これは、半導体製造などに多量に使用
されているＳｉウェハと全く同じ製法、装置で作製する
ものであり、従来例に示したものと比較して低コストで
製造することが可能である。そのうえ、多結晶と違って
粒界が存在しないことから、従来例のようにターゲット
の表面粗さが大きくなることがない。このために、アー
クが発生しにくく、また、ターゲット面内の均一性に優
れ、その結果、大面積基板に成膜しても膜質の均一性が
高くなる。そして、反応性スパッタリングを行っている
際に直流電源に正電圧をパルス状に印加することで、タ
ーゲット表面に電荷が蓄積されにくく、アークが発生す
ることを防止する作用、効果を更に高めることができ
る。In the present invention, single crystal Si is used as the target. This is manufactured by the same manufacturing method and apparatus as a Si wafer which is used in a large amount in semiconductor manufacturing and the like, and can be manufactured at a lower cost than that shown in the conventional example. Moreover, unlike polycrystals, there are no grain boundaries, so that the surface roughness of the target does not increase as in the conventional example. For this reason, arc is less likely to occur, and the uniformity in the target surface is excellent. As a result, the uniformity of film quality is high even when a film is formed on a large area substrate. Then, by applying a positive voltage in a pulse form to the DC power supply during the reactive sputtering, it is possible to further enhance the action and the effect of preventing the electric charge from accumulating on the target surface and preventing the arc from being generated. it can.
【００１１】なお、Ｓｉターゲットを用いた反応性ＤＣ
マグネトロンスパッタリング法による場合、Ｓｉを酸化
させる必要があるため、酸素を含むガスを導入するのは
勿論であるが、さらに、成膜速度を向上させるために不
活性ガスを同時に導入するとよい。この方法によれば、
ＳｉＯ2 ターゲットを用いたＲＦスパッタリング法の場
合と比較して、成膜速度は５倍以上となり、生産性が大
幅に向上する。Reactive DC using a Si target
In the case of the magnetron sputtering method, since it is necessary to oxidize Si, it is needless to say that a gas containing oxygen is introduced, but further, an inert gas may be introduced at the same time in order to improve the film formation rate. According to this method
Compared with the case of the RF sputtering method using a SiO 2 target, the film formation rate is 5 times or more, and the productivity is significantly improved.
【００１２】なお、ターゲットとして使用する単結晶Ｓ
ｉの抵抗値が大きいと、直流電源に正電圧をパルス状に
印加しても電荷が蓄積されやすく、アークが発生して、
外観上の問題が生じるおそれがある。そこで、請求項２
に係る発明では、単結晶Ｓｉの抵抗値を１０ｍΩ・ｃｍ
以下とし、アークの発生を抑える作用を非常に大きくし
た。なお、このような抵抗値の単結晶Ｓｉターゲット
は、Ｂ（硼素）やＰ（リン）をドープすることで容易に
得ることができる。The single crystal S used as the target
If the resistance value of i is large, even if a positive voltage is applied to the DC power source in a pulsed manner, electric charge is likely to be accumulated and an arc occurs,
Appearance problems may occur. Therefore, claim 2
In the invention according to, the resistance value of single crystal Si is 10 mΩ · cm.
Below, the effect of suppressing the generation of arcs is greatly increased. The single crystal Si target having such a resistance value can be easily obtained by doping B (boron) or P (phosphorus).
【００１３】[0013]
［実施例１］本実施例では、ガラス基板上に２層の反射
防止膜を形成した例を示す。まず、ＢＫ系のガラス基板
を真空槽にセットし、１×１０-4Ｐａまで排気した後、
それぞれ分圧が１．９Ｐａ、０．１ＰａのＡｒガス、Ｏ
2 ガスを真空槽に導入した。基板側から第１層目は、Ｔ
ｉターゲットを用いて、投入電力を５００Ｗとし、通常
の反応性ＤＣマグネトロンスパッタリング法によりＴｉ
Ｏ2 膜を成膜した。[Embodiment 1] This embodiment shows an example in which a two-layer antireflection film is formed on a glass substrate. First, set a BK-based glass substrate in a vacuum chamber, evacuate to 1 × 10 −4 Pa, and then
Ar gas with partial pressures of 1.9 Pa and 0.1 Pa, respectively, O
Two gases were introduced into the vacuum chamber. The first layer from the substrate side is T
Using an i target, the input power was set to 500 W, and Ti was formed by the usual reactive DC magnetron sputtering method.
An O 2 film was formed.
【００１４】第２層目は、Ｂをドープして抵抗値を約５
ｍΩ・ｃｍとした単結晶Ｓｉからなるターゲットを用い
た。直流電源から、図１のような波形の電圧、すなわ
ち、パルスの間隔が５μｓｅｃであり、パルスが正に反
転している時間が０．５μｓｅｃ以上１μｓｅｃ以下で
あるような電圧をターゲットに供給した。投入電力１ｋ
Ｗとし、反応性ＤＣマグネトロンスパッタリング法によ
りＳｉＯ2 膜を形成した。このとき、アークの発生は全
く見られなかった。The second layer is doped with B to have a resistance value of about 5
A target made of single crystal Si having mΩ · cm was used. A voltage having a waveform as shown in FIG. 1, that is, a voltage having a pulse interval of 5 μsec and a positive inversion time of the pulse of 0.5 μsec or more and 1 μsec or less was supplied from the DC power source to the target. Input power 1k
A W 2 film was formed by reactive DC magnetron sputtering. At this time, no arc was observed.
【００１５】それぞれの成膜条件、膜厚、成膜時間等を
表１に、分光反射率を図２に示す。反射率は５３０ｎｍ
で１．５％以下と十分な反射防止特性が得られた。成膜
時間は２層あわせてわずか５０秒であり、極めて生産性
が良かった。また、成膜中にアークの発生がないため
に、ターゲット材料表面の微粒子が跳び出して膜にパー
ティクルとして付着することがなく、その結果、外観上
の問題や可視光の散乱、吸収等の問題も生じなかった。
また、基板内での分光反射率は一定で、屈折率の均一性
が高いことも確認できた。なお、Ａｒガス、Ｏ2 ガスに
加えて、Ｈ2 ガスやＨｅガスを０．１Ｐａ程度導入する
と、プラズマが活性化され、膜と基板との密着性が向上
する。Table 1 shows the film forming conditions, film thickness, film forming time and the like, and FIG. 2 shows the spectral reflectance. Reflectance 530nm
Of 1.5% or less, a sufficient antireflection property was obtained. The film formation time for the two layers was only 50 seconds, and the productivity was extremely good. Further, since no arc is generated during film formation, fine particles on the surface of the target material do not jump out and adhere to the film as particles. As a result, there are problems such as appearance problems and visible light scattering and absorption. Also did not occur.
It was also confirmed that the spectral reflectance within the substrate was constant and the refractive index was highly uniform. If H 2 gas or He gas of about 0.1 Pa is introduced in addition to Ar gas and O 2 gas, plasma is activated and adhesion between the film and the substrate is improved.
【００１６】[0016]
【表１】 [Table 1]
【００１７】［実施例２］実施例１の単結晶Ｓｉからな
るターゲットに代えて、Ｂのドープ量が少なく、抵抗値
が１０、５０、３００ｍΩ・ｃｍの３種のターゲットを
用意し、実施例１と同様の条件にてＳｉＯ2 膜を形成し
た。Example 2 In place of the target made of single crystal Si of Example 1, three types of targets having a small B doping amount and resistance values of 10, 50 and 300 mΩ · cm were prepared. A SiO 2 film was formed under the same conditions as in 1.
【００１８】投入電力が１ｋＷの場合、抵抗値が１０ｍ
Ω・ｃｍのもののみ全くアークは発生しなかったが、他
の２種のターゲットでは多少アークが発生した。しか
し、投入電力を６００Ｗに下げた場合、抵抗値が５０お
よび３００ｍΩ・ｃｍのものでもアークは発生しなかっ
た。また、この条件で成膜した場合、外観上の問題や可
視光の散乱、吸収等の問題は生じなかった。When the input power is 1 kW, the resistance value is 10 m
No arc was generated at all for Ω · cm, but some arcs were generated for the other two types of targets. However, when the applied power was lowered to 600 W, no arc was generated even when the resistance values were 50 and 300 mΩ · cm. In addition, when the film was formed under these conditions, there were no problems in appearance and problems such as scattering and absorption of visible light.
【００１９】［実施例３］本実施例では、プラスチック
基板上にミラーを設けた例を示す。まず、ポリカーボネ
ート製の基板を真空槽にセットし、３×１０-4Ｐａまで
排気した。基板側から第１層目は、分圧が０．１Ｐａの
Ａｒガスを真空槽に導入し、Ａｌターゲットを用いて、
投入電力を１．５ｋＷとし、通常のＤＣマグネトロンス
パッタリング法によりＡｌ膜を形成した。[Embodiment 3] This embodiment shows an example in which a mirror is provided on a plastic substrate. First, a polycarbonate substrate was set in a vacuum chamber and evacuated to 3 × 10 −4 Pa. For the first layer from the substrate side, Ar gas having a partial pressure of 0.1 Pa was introduced into a vacuum chamber, and an Al target was used to
The applied power was set to 1.5 kW, and the Al film was formed by the usual DC magnetron sputtering method.
【００２０】第２層目は、Ｐをドープして抵抗値を約３
ｍΩ・ｃｍとした単結晶Ｓｉからなるターゲットを用い
た。直流電源から、図３のような波形の電圧、すなわ
ち、パルスの間隔が３μｓｅｃであり、パルスが瞬間的
に正に反転し、その後１．５μｓｅｃの間に元の負電圧
に復帰するような鋸歯状の電圧をターゲットに供給し
た。投入電力７００Ｗとし、反応性ＤＣマグネトロンス
パッタリング法によりＳｉＯ2 膜を形成した。このと
き、アークの発生は全く見られなかった。The second layer is doped with P to have a resistance value of about 3
A target made of single crystal Si having mΩ · cm was used. A voltage having a waveform as shown in FIG. 3, that is, a sawtooth having a pulse interval of 3 μsec from the DC power supply, the pulse momentarily inverted to positive, and then returning to the original negative voltage within 1.5 μsec. Voltage was applied to the target. An input power of 700 W was used to form a SiO 2 film by the reactive DC magnetron sputtering method. At this time, no arc was observed.
【００２１】それぞれの成膜条件、膜厚、成膜時間等を
表２に示す。成膜時間は２層あわせて１４秒であり、極
めて生産性が良かった。また、外観上の問題や可視光の
散乱、吸収等の問題も生じなかった。４５゜入射光の反
射率を図４に示す。図４から判るように、可視域全域で
８９％以上と高い反射率を得ることができた。Table 2 shows the film forming conditions, film thickness, film forming time and the like. The film formation time for the two layers was 14 seconds, and the productivity was extremely good. In addition, there were no problems in appearance and problems such as visible light scattering and absorption. The reflectance of 45 ° incident light is shown in FIG. As can be seen from FIG. 4, a high reflectance of 89% or more could be obtained in the entire visible region.
【００２２】[0022]
【表２】 [Table 2]
【００２３】［実施例４］本実施例では、ＢＫ系の光学
ガラス基板上に４層の反射防止膜を形成した例を示す。
基板側から第１層目は、Ｔａターゲットを用いて、投入
電力を７００Ｗとし、通常の反応性ＤＣマグネトロンス
パッタリング法によりＴａ2 Ｏ5 膜を形成した。[Embodiment 4] In this embodiment, an example in which four layers of antireflection films are formed on a BK type optical glass substrate is shown.
A Ta 2 O 5 film was formed on the first layer from the substrate side by using a Ta target with an input power of 700 W and an ordinary reactive DC magnetron sputtering method.
【００２４】第２層目は、Ｂをドープして抵抗値を約２
ｍΩ・ｃｍとした単結晶Ｓｉからなるターゲットを用い
た。直流電源から供給する電圧に、１３．５６ＭＨｚの
高周波電源から供給する電圧を重畳させることで、図５
のような波形の電圧をターゲットに供給した。直流電源
から５００Ｗ、高周波電源から１００Ｗの電力を投入
し、反応性マグネトロンスパッタリング法によりＳｉＯ
2 膜を形成した。このとき、アークの発生は全く見られ
なかった。以下、第１および第２層と同様にして、第３
および第４層を形成した。The second layer is doped with B and has a resistance value of about 2
A target made of single crystal Si having mΩ · cm was used. By superimposing the voltage supplied from the 13.56 MHz high frequency power supply on the voltage supplied from the DC power supply,
A voltage having a waveform as shown in FIG. Power of 500 W from a DC power supply and 100 W from a high frequency power supply was applied, and SiO was formed by a reactive magnetron sputtering method.
Two films were formed. At this time, no arc was observed. Hereinafter, in the same manner as the first and second layers, the third
And a fourth layer was formed.
【００２５】それぞれの成膜条件、膜厚、成膜時間等を
表３に、分光反射率を図６に示す。本実施例では、分光
反射率特性は可視域全域で１％以下であり、実施例１よ
り大幅に優れたものとなった。また、層数、膜厚が増え
た分だけ成膜時間が長くなるはずであるが、不活性ガス
としてＫｒを使用したので、成膜速度が速くなり、生産
性が著しく下がることはなかった。さらに、外観上の問
題や可視光の散乱、吸収等の問題は生じなかった。Table 3 shows the film forming conditions, film thickness, film forming time and the like, and FIG. 6 shows the spectral reflectance. In this example, the spectral reflectance characteristic was 1% or less in the entire visible region, which was significantly superior to that in Example 1. Further, although the film formation time should be lengthened by the increase in the number of layers and the film thickness, since Kr was used as the inert gas, the film formation speed was increased and the productivity was not significantly reduced. Furthermore, there were no problems in appearance, visible light scattering and absorption.
【００２６】[0026]
【表３】 [Table 3]
【００２７】[0027]
【発明の効果】以上のように、請求項１に係る発明によ
れば、単結晶Ｓｉターゲットを用いているので、低コス
トで容易に入手可能であり、また、ターゲット面内の均
一性に優れているため、大面積基板に成膜しても膜質の
均一性が高く保たれ、また、単結晶であることから、粒
界が存在しないので、アークが発生しにくく、さらに直
流電源に正電圧をパルス状に印加しながら、反応性スパ
ッタリング法によりＳｉＯ2 膜を形成することとしたの
で、より一層アークを防止する効果が高く、外観上に問
題のない高品質のＳｉＯ2 膜を生産性良く、低コストで
製造することができる。また、請求項２に係る発明によ
れば、上記効果に加え、単結晶Ｓｉターゲットの抵抗値
を１０ｍΩ・ｃｍ以下としたので、更にアークを防止す
る効果が高められ、より高品質なＳｉＯ2 膜を形成する
ことができる。As described above, according to the invention of claim 1, since the single crystal Si target is used, it can be easily obtained at a low cost, and the uniformity in the target plane is excellent. Therefore, even if a film is formed on a large area substrate, the uniformity of the film quality is kept high, and since it is a single crystal, there are no grain boundaries, so arcing does not easily occur, and a positive voltage is applied to the DC power supply. Since it was decided to form the SiO 2 film by the reactive sputtering method while applying in a pulsed manner, the effect of preventing the arc is even higher, and a high-quality SiO 2 film with no problem in appearance is produced with good productivity. Can be manufactured at low cost. According to the invention of claim 2, in addition to the above effects, the resistance value of the single crystal Si target is set to 10 mΩ · cm or less, so that the effect of preventing arc is further enhanced, and a higher quality SiO 2 film is obtained. Can be formed.
【図１】実施例１で印加した電圧の波形を示す波形図で
ある。FIG. 1 is a waveform diagram showing a waveform of a voltage applied in Example 1.
【図２】実施例１で得た反射防止膜の分光反射率を示す
グラフである。2 is a graph showing the spectral reflectance of the antireflection film obtained in Example 1. FIG.
【図３】実施例３で印加した電圧の波形を示す波形図で
ある。FIG. 3 is a waveform diagram showing a waveform of a voltage applied in Example 3.
【図４】実施例３で得たミラーの４５゜入射光の反射率
を示すグラフである。FIG. 4 is a graph showing the reflectance of 45 ° incident light on the mirror obtained in Example 3;
【図５】実施例４で印加した電圧の波形を示す波形図で
ある。5 is a waveform diagram showing a waveform of a voltage applied in Example 4. FIG.
【図６】実施例４で得た反射防止膜の分光反射率を示す
グラフである。FIG. 6 is a graph showing the spectral reflectance of the antireflection film obtained in Example 4.
Claims (2)
含むガスおよび不活性ガスの少なくとも２種類のガスを
導入した雰囲気中で、直流電源に正電圧をパルス状に印
加しながら、反応性スパッタリング法によりＳｉＯ2 膜
を形成することを特徴とする光学薄膜の製造方法。1. Reactive sputtering while applying a positive voltage to a DC power source in a pulsed manner in an atmosphere in which at least two kinds of gas containing oxygen and an inert gas are introduced using a single crystal Si target. A method for producing an optical thin film, which comprises forming a SiO 2 film by a method.
Ω・ｃｍ以下であることを特徴とする請求項１記載の光
学薄膜の製造方法。2. The resistance value of a single crystal Si target is 10 m.
The method for producing an optical thin film according to claim 1, wherein it is Ω · cm or less.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28939594A JP3506782B2 (en) | 1994-11-24 | 1994-11-24 | Manufacturing method of optical thin film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28939594A JP3506782B2 (en) | 1994-11-24 | 1994-11-24 | Manufacturing method of optical thin film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH08146201A true JPH08146201A (en) | 1996-06-07 |
| JP3506782B2 JP3506782B2 (en) | 2004-03-15 |
Family
ID=17742674
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP28939594A Expired - Fee Related JP3506782B2 (en) | 1994-11-24 | 1994-11-24 | Manufacturing method of optical thin film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3506782B2 (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001094660A3 (en) * | 2000-06-02 | 2002-05-30 | Honeywell Int Inc | Sputtering target |
| US6569270B2 (en) | 1997-07-11 | 2003-05-27 | Honeywell International Inc. | Process for producing a metal article |
| US6723187B2 (en) | 1999-12-16 | 2004-04-20 | Honeywell International Inc. | Methods of fabricating articles and sputtering targets |
| US7101447B2 (en) | 2000-02-02 | 2006-09-05 | Honeywell International Inc. | Tantalum sputtering target with fine grains and uniform texture and method of manufacture |
| US7517417B2 (en) | 2000-02-02 | 2009-04-14 | Honeywell International Inc. | Tantalum PVD component producing methods |
-
1994
- 1994-11-24 JP JP28939594A patent/JP3506782B2/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6569270B2 (en) | 1997-07-11 | 2003-05-27 | Honeywell International Inc. | Process for producing a metal article |
| US6723187B2 (en) | 1999-12-16 | 2004-04-20 | Honeywell International Inc. | Methods of fabricating articles and sputtering targets |
| US6878250B1 (en) | 1999-12-16 | 2005-04-12 | Honeywell International Inc. | Sputtering targets formed from cast materials |
| US7101447B2 (en) | 2000-02-02 | 2006-09-05 | Honeywell International Inc. | Tantalum sputtering target with fine grains and uniform texture and method of manufacture |
| US7517417B2 (en) | 2000-02-02 | 2009-04-14 | Honeywell International Inc. | Tantalum PVD component producing methods |
| WO2001094660A3 (en) * | 2000-06-02 | 2002-05-30 | Honeywell Int Inc | Sputtering target |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3506782B2 (en) | 2004-03-15 |
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