JP2000321401A - Manufacture of optical article - Google Patents
Manufacture of optical articleInfo
- Publication number
- JP2000321401A JP2000321401A JP11131024A JP13102499A JP2000321401A JP 2000321401 A JP2000321401 A JP 2000321401A JP 11131024 A JP11131024 A JP 11131024A JP 13102499 A JP13102499 A JP 13102499A JP 2000321401 A JP2000321401 A JP 2000321401A
- Authority
- JP
- Japan
- Prior art keywords
- organic compound
- fiber
- fibrous material
- film
- optical article
- 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.)
- Pending
Links
Landscapes
- Surface Treatment Of Optical Elements (AREA)
- Physical Vapour Deposition (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、ＣＲＴ、ＬＣＤ、
ＰＤＰ、ＥＬなど各種ディスプレイまたは各種表示装置
の表示面や光学フィルター類、眼鏡レンズ、光学レン
ズ、照明用具、展示用のケースやショーウインドウ、絵
画の額、窓ガラスなどの光学物品、またはそれらを構成
するフィルムなどの光学物品に、有機化合物、特に防汚
剤や反射防止加工用の低屈折率膜を真空蒸着法などで付
与する光学物品の製造方法に関わる。TECHNICAL FIELD The present invention relates to a CRT, an LCD,
Display surfaces of various displays or various display devices such as PDPs and ELs, optical filters, spectacle lenses, optical lenses, lighting tools, display cases and show windows, picture frames, window glass, and other optical articles, or components thereof The present invention relates to a method for producing an optical article in which an organic compound, particularly an antifouling agent or a low-refractive-index film for antireflection processing is applied to an optical article such as a film to be formed by a vacuum deposition method or the like.
【０００２】[0002]
【従来の技術】防汚剤や低屈折率膜を光学物品に付与す
る方法として、溶液を用い、枚葉方式で行うディッピン
グ法、スピンコート法など、また連続方式で行うフィル
ムへのグラビアコート法、スリットダイコート法、リバ
ースコート法などのいわゆるウエットコート法が知られ
ている。2. Description of the Related Art As a method of applying an antifouling agent or a low refractive index film to an optical article, a dipping method or a spin coating method using a solution and a single-wafer method, or a gravure coating method on a film using a continuous method is used. So-called wet coating methods such as a slit die coating method and a reverse coating method are known.
【０００３】一方、真空蒸着法やスパッター法では、光
学物品に無機系の反射防止膜を付与した後に、同一装置
内で連続的に防汚剤を付与できるなどのため、いわゆる
ドライコート法の要求がある。On the other hand, in a vacuum evaporation method or a sputtering method, an antifouling agent can be continuously applied in the same apparatus after an inorganic antireflection film is applied to an optical article. There is.
【０００４】真空蒸着法で用いられている無機化合物と
比べ、一般に有機化合物は融点や沸点、昇華点が低い。
また、有機化合物は不純物を多く含んでいたり、分子量
分布を持つものがあり、沸点の分布を持ちやすい。さら
に、有機化合物は無機化合物に比べ、熱伝導性が低く、
真空蒸発の際の加熱が局所的になりやすいという欠点が
ある。In general, organic compounds have lower melting points, boiling points, and sublimation points than inorganic compounds used in vacuum deposition.
Some organic compounds contain a large amount of impurities or have a molecular weight distribution, and thus easily have a boiling point distribution. Furthermore, organic compounds have lower thermal conductivity than inorganic compounds,
There is a disadvantage that heating during vacuum evaporation tends to be localized.
【０００５】そのため、有機化合物を真空蒸発する場合
は、加熱コントロールが無機化合物と比べて難しく、局
所的な加熱による突沸現象（スプラッシュ）を起こしや
すい。光学物品の場合、スプラッシュによる蒸着面への
飛沫飛散は、たとえそれが微細なものであっても肉眼視
できるものは欠点であり、収率低下の大きな原因にな
る。[0005] Therefore, when the organic compound is vacuum-evaporated, the heating control is more difficult than the inorganic compound, and the bumping phenomenon (splash) due to local heating is liable to occur. In the case of an optical article, even if it is fine, even if it is fine, it is a defect, and the scattering of the splash on the deposition surface due to the splash is a major cause of a reduction in yield.
【０００６】スプラッシュ対策として、特開平４−７２
０５５号公報や特開平５−２１５９０５号公報で、有機
化合物を多孔性セラミックや金属燒結体に含浸する方法
が提案されている。また、特開平６−３４０９６６号公
報では有機化合物を繊維状の導電性物質の塊に付着する
方法が提案されている。As a countermeasure against splash, Japanese Patent Application Laid-Open No. 4-72
No. 055 and JP-A-5-215905 propose a method of impregnating a porous ceramic or metal sintered body with an organic compound. Japanese Patent Application Laid-Open No. 6-340966 proposes a method of attaching an organic compound to a fibrous conductive substance mass.
【０００７】[0007]
【発明が解決しようとする課題】多孔性セラミックや金
属燒結体に含浸する方法は、含浸量がばらつきやすいこ
と、及び有機化合物による多孔内の汚れを完全に除去す
ることが難しく、従って高価な多孔性セラミックや金属
燒結体を使い捨てにする経済的不利がある。The method of impregnating a porous ceramic or metal sintered body involves a problem that the impregnation amount tends to vary, and it is difficult to completely remove dirt in the pores due to an organic compound. There is an economic disadvantage that disposable ceramic and metal sinters are disposable.
【０００８】また、有機化合物を繊維状の導電性物質の
塊に付着する方法は、有機化合物の粘度が高かったり、
溶媒に溶解しない場合は、繊維状の導電性物質の塊に満
遍なく付着することができない欠点を持つ。[0008] In addition, the method of attaching an organic compound to a fibrous mass of a conductive material involves a method in which the viscosity of the organic compound is high,
When it does not dissolve in a solvent, it has a disadvantage that it cannot be uniformly attached to a lump of fibrous conductive substance.
【０００９】本発明は、粘度が高い、あるいは溶媒への
溶解性の悪い有機化合物にも適用でき、抵抗加熱法や電
子ビーム加熱法など加熱法にかかわらず使用でき、且つ
安価で、スプラッシュを起こさない有機化合物を真空蒸
発などにより付与させることを特徴とした光学物品の製
造方法を提供することを目的とする。The present invention can be applied to an organic compound having a high viscosity or poor solubility in a solvent, can be used regardless of a heating method such as a resistance heating method or an electron beam heating method, is inexpensive, and has no splash. It is an object of the present invention to provide a method for producing an optical article, wherein an organic compound is provided by vacuum evaporation or the like.
【００１０】[0010]
【課題を解決するための手段】上記目的を達成するため
に、本発明は下記構成を有する。In order to achieve the above object, the present invention has the following constitution.
【００１１】「光学物品表面に有機化合物を被覆する光
学物品の製造方法において、蒸発源である有機化合物の
表面を、直接又は空隙を介して間接的に繊維状物で被覆
し、真空下で加熱することを特徴とする光学物品の製造
方法」。[0011] In a method for manufacturing an optical article in which the surface of an optical article is coated with an organic compound, the surface of the organic compound as an evaporation source is coated with a fibrous material directly or indirectly through a gap and heated under vacuum. A method for producing an optical article ".
【００１２】[0012]
【発明の実施の形態】以下に、真空蒸着法の場合を例に
とり、本発明を説明する。DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be described below by taking the case of a vacuum deposition method as an example.
【００１３】本発明が対象とする光学物品の基板は、Ｃ
ＲＴ、ＬＣＤ、ＰＤＰ、ＥＬなど各種ディスプレイ類の
画像面、各種計器類の表示面そのもの、それらへ貼付す
るなどにより直接装着する、あるいは組み込んだり、外
部装着する偏光板や光学フィルター類、眼鏡レンズ、光
学レンズ、照明用具、展示用のケースやショーウインド
ウ、絵画の額、窓ガラスなどの光学物品、またはそれを
構成するフィルムなどが含まれる。The substrate of the optical article to which the present invention is directed is C
Image planes of various displays such as RT, LCD, PDP, EL, display planes of various instruments, etc., directly attached or incorporated by attaching them to them, or externally attached polarizing plates and optical filters, eyeglass lenses, Examples include optical lenses, lighting tools, display cases and show windows, picture frames, optical articles such as window glasses, and films constituting them.
【００１４】これらの光学物品には、アクリル樹脂、ポ
リカーボネート樹脂、ポリスチレン樹脂、ポリウレタン
系樹脂、ポリ４−メチルペンテン−１樹脂、ジエチレン
グリコールビスアリルカーボネート樹脂、ポリエステル
樹脂、ポリエーテルサルホン樹脂などの樹脂類やガラス
などで作られるものが含まれる。These optical articles include resins such as acrylic resins, polycarbonate resins, polystyrene resins, polyurethane resins, poly-4-methylpentene-1 resins, diethylene glycol bisallyl carbonate resins, polyester resins, and polyether sulfone resins. And those made of glass.
【００１５】また、光学物品の形状としては、平面形状
かフィルム状である場合が、真空蒸着の操作性、均質性
から好ましい。The shape of the optical article is preferably a flat shape or a film shape from the viewpoint of the operability and uniformity of vacuum deposition.
【００１６】中でも、光学物品の表面が、反射防止膜や
赤外線の遮蔽膜や電磁波の遮蔽膜のような無機質膜によ
って被覆され、その最外層が金、銀、アルミニウムなど
の金属膜、酸化ケイ素、酸化チタン、酸化ジルコニウ
ム、酸化スズ、酸化インジュウム、炭化珪素、窒化ケイ
素のような無機質膜である場合、特に本発明は好ましく
適用される。その理由は後述するように、表面が無機質
膜である方が蒸着される有機化合物と光学物品との間の
密着性を向上しやすいためである。無機質膜が特に酸化
ケイ素である場合、有機化合物との密着性を有利に高め
ることができるため、本発明に好適である。In particular, the surface of the optical article is coated with an inorganic film such as an antireflection film, an infrared shielding film, or an electromagnetic wave shielding film, and the outermost layer is a metal film such as gold, silver, or aluminum, silicon oxide, or the like. The present invention is particularly preferably applied to an inorganic film such as titanium oxide, zirconium oxide, tin oxide, indium oxide, silicon carbide, and silicon nitride. The reason is that, as will be described later, when the surface is an inorganic film, the adhesiveness between the organic compound to be deposited and the optical article is easily improved. In the case where the inorganic film is particularly silicon oxide, the adhesion to an organic compound can be advantageously increased, which is suitable for the present invention.
【００１７】本発明に用いる有機化学物質は、熱に比較
的安定であり、真空下で蒸発可能な性質を持ち、且つ蒸
着後の基板表面で被膜を形成し得るものであれば、いず
れの有機化合物でも本発明を適用できるが、用途的には
撥水、撥油性機能を持つ防汚剤や反射防止膜としての低
屈折率膜になり得るものが特に好ましい。The organic chemical substance used in the present invention is relatively stable to heat, has the property of being able to evaporate under vacuum, and is capable of forming a film on the substrate surface after vapor deposition. Although the present invention can be applied to a compound, a compound which can be used as an antifouling agent having a water repellent or oil repellent function or a low refractive index film as an antireflection film is particularly preferable.
【００１８】撥水、撥油性機能を持つ防汚剤や反射防止
膜としての低屈折率膜を形成し得る有機化合物の中で、
熱に比較的安定であり、蒸発可能な性質を持ち、且つ蒸
着後の基板表面で被膜を形成し得るものとして、分子内
にフッ素原子を含むものが挙げられる。また、上記した
ように、基板特に無機質膜、なかでも酸化ケイ素膜との
密着性を向上するために、該有機化合物はシラン系化合
物あるいはシラザン系化合物であることが好ましい。中
でも、シラノール基を形成し得る加水分解性に関して２
官能性以上、好ましくは３官能性以上である場合、無機
質膜あるいは酸化ケイ素膜への密着性を高くしやすい。Among organic compounds capable of forming a low-refractive-index film as an antifouling agent having a water-repellent and oil-repellent function and an antireflection film,
As a material which is relatively stable to heat, has an evaporable property, and can form a film on a substrate surface after vapor deposition, a material containing a fluorine atom in a molecule can be mentioned. Further, as described above, the organic compound is preferably a silane-based compound or a silazane-based compound in order to improve the adhesion to a substrate, particularly an inorganic film, especially a silicon oxide film. Above all, regarding hydrolyzability capable of forming a silanol group, 2
When the functionality is not less than the functionality, and preferably not less than the functionality, the adhesion to the inorganic film or the silicon oxide film is easily increased.
【００１９】本発明に適用される有機化合物の代表例を
下記する。Representative examples of the organic compound applied to the present invention are described below.
【００２０】ハロゲン化シラン類として、トリメチルク
ロロシラン、ジメチルジクロロシラン、ジエチルジクロ
ロシラン、メチル−３，３，３−トリフルオロプロピル
ジクロロシランなど。Examples of the halogenated silanes include trimethylchlorosilane, dimethyldichlorosilane, diethyldichlorosilane, and methyl-3,3,3-trifluoropropyldichlorosilane.
【００２１】アルコキシシラン類として、トリメチルエ
トキシシラン、ジメチルジメトキシシラン、３，３，３
−トリフルオロプロピルトリメトキシシランなど。As alkoxysilanes, trimethylethoxysilane, dimethyldimethoxysilane, 3,3,3
-Trifluoropropyltrimethoxysilane and the like.
【００２２】アミノシラン類として、３、３、３−トリ
フルオロプロピルトリアミノシラン、２−（パーフルオ
ロプロピル）エチルトリアミノシラン、２−（パーフル
オロオクチル）エチルトリアミノシランなど。Examples of the aminosilanes include 3,3,3-trifluoropropyltriaminosilane, 2- (perfluoropropyl) ethyltriaminosilane, and 2- (perfluorooctyl) ethyltriaminosilane.
【００２３】シラザン類として、ヘキサメチルジシラザ
ン、１，１，３，３，５，５，７，７−オクチルメチル
シクロテトラシラザンなど。Examples of the silazane include hexamethyldisilazane, 1,1,3,3,5,5,7,7-octylmethylcyclotetrasilazane.
【００２４】これらの有機化合物は、単独または混合し
て用いられるが、最も好ましい使用方法は、真空蒸着前
の段階で事前部分加水分解処理し、少なくともその一部
をシロキサン結合させて分子量を高めたもの、場合によ
ってはゲル状物にしたものを本発明に適用すると、防汚
性能や基板との密着性、表面硬度の高いものが得られや
すい。These organic compounds are used singly or as a mixture. The most preferred method of use is to preliminarily partially hydrolyze at a stage before vacuum deposition, and at least a part thereof is siloxane-bonded to increase the molecular weight. When a material, or a gel material in some cases, is applied to the present invention, a material having high antifouling performance, adhesion to a substrate, and high surface hardness is easily obtained.
【００２５】中でも、下記構造を持つ有機化合物Ｉ、I
I、III、IVに示すような、分子内にパーフルオロポリエ
ーテル構造を持つ、例えば分子量１０００〜５００００
程度の比較的大きな化合物は、防汚性能としての指紋拭
き取り性が上記化合物と比較して格段に優れるが、極め
て高粘度である。また、その部分加水分解物は固体に近
い難溶解性のゲル状物であるため、多孔性セラミックや
金属燒結体へ含浸したり、繊維状の導電性物質の塊に付
着することが難しく、本発明に好ましく適用される。 有機化合物ＩAmong them, organic compounds I and I having the following structures
Having a perfluoropolyether structure in the molecule as shown in I, III, IV, for example, a molecular weight of 1,000 to 50,000
A relatively large compound has a very high fingerprint wiping property as an antifouling property as compared with the above compound, but has an extremely high viscosity. In addition, since the partial hydrolyzate is a hardly soluble gel-like substance close to a solid, it is difficult to impregnate porous ceramics and metal sintered bodies or adhere to fibrous conductive material lump. It is preferably applied to the invention. Organic compound I
【００２６】[0026]
【化１】 Embedded image
【００２７】（式中、Ｒｆは炭素数１〜１０の直鎖状あ
るいは分岐状のパーフルオロ基あるいはハイドロパーフ
ルオロ基、Ｘはフッ素原子、ヨウ素原子、臭素原子、塩
素原子あるいは水素原子、Ｙは水素原子または炭素数１
〜１０の低級アルキル基、Ｚはフッ素原子あるいは炭素
数１〜１６の直鎖状あるいは分岐状のパーフルオロ基あ
るいはハイドロパーフルオロ基、Ｒ1は水酸基あるいは
加水分解可能な基、加水分解可能な基としてはハロゲ
ン、−ＯＲ、−ＯＣＯＲ、−ＯＣ（Ｒ）＝Ｃ（Ｒ） 2、
−ＯＮ＝Ｃ（Ｒ）2が、より好ましくは−ＯＣＨ3，−Ｏ
Ｃ2Ｈ5，−Ｃｌが挙げられる。Ｒ2は一価の有機基、a,
b,c,dはそれぞれ０〜２００の整数であって、１≦a+b+c
+d≦２００である。ｅは０または１、ｌは０〜３の整
数、ｍは１〜１０の整数、ｎは０〜２の整数を表す。） 有機化合物II(Wherein, Rf is a straight chain having 1 to 10 carbon atoms)
Or branched perfluoro group or hydroperf
X is a fluorine atom, iodine atom, bromine atom, salt
An element atom or a hydrogen atom, and Y is a hydrogen atom or a carbon atom of 1
A lower alkyl group of 10 to 10, Z is a fluorine atom or carbon
A linear or branched perfluoro group of
Or a hydroperfluoro group, R1Is a hydroxyl group or
Hydrolyzable groups, as the hydrolyzable group
, -OR, -OCOR, -OC (R) = C (R) Two,
-ON = C (R)TwoBut more preferably -OCHThree, -O
CTwoHFive, -Cl. RTwoIs a monovalent organic group, a,
b, c, d are each an integer of 0 to 200, and 1 ≦ a + b + c
+ d ≦ 200. e is 0 or 1, l is an integer of 0 to 3
The number, m represents an integer of 1 to 10, and n represents an integer of 0 to 2. ) Organic compounds II
【００２８】[0028]
【化２】 Embedded image
【００２９】（式中、Ｘは水素原子またはヨウ素原子、
Ｙは水素原子または炭素数１〜１０の低級アルキル基、
Ｒ1は水酸基あるいは加水分解可能な基である。ａは１
〜１００の整数、ｌは０〜３の整数、ｍは１〜１０の整
数、ｎは０〜２の整数を表す。Ｒ2は一価の有機基を表
す。） 有機化合物IIIWherein X is a hydrogen atom or an iodine atom;
Y is a hydrogen atom or a lower alkyl group having 1 to 10 carbon atoms,
R 1 is a hydroxyl group or a hydrolyzable group. a is 1
An integer of 100, l is an integer of 0-3, m is an integer of 1-10, and n is an integer of 0-2. R 2 represents a monovalent organic group. ) Organic compounds III
【００３０】[0030]
【化３】 Embedded image
【００３１】有機化合物IV (EtO)3SiCH2CH2CH2NHCOOCH2(CF2CF2O)p(CF2O)qCH2 OCON
HCH2CH3CH2Si(OEt)3 （式中、ｐ、ｑは１〜１００の整数を表す。）本発明で
使用する繊維状物は、上記有機化合物の蒸発温度におい
て、熱分解等による放出ガスや蒸発物質が無いか、有っ
ても少ないことが要求される。そのため、無機系繊維で
あるか、耐熱性の有機系繊維であることが好ましい。Organic compound IV (EtO) 3 SiCH 2 CH 2 CH 2 NHCOOCH 2 (CF 2 CF 2 O) p (CF 2 O) q CH 2 OCON
HCH 2 CH 3 CH 2 Si ( OEt) 3 ( wherein, p, q is an integer of 1 to 100.) Fibrous material used in the present invention, in the evaporation temperature of the organic compound, by thermal decomposition It is required that there be no or little if any emitted gas or evaporating substance. Therefore, it is preferable to use inorganic fibers or heat-resistant organic fibers.
【００３２】本発明に好ましく適用できる繊維状物の具
体例として、金属繊維、セラミックス繊維、ガラス繊
維、ロックウール、アスベスト繊維、炭素繊維、ポリイ
ミド繊維、芳香族ポリアミド繊維などを挙げることがで
きる。このうち、耐熱性及び放出ガスの少なさ、熱伝導
性の良さから、無機系繊維の金属繊維、セラミックス繊
維、ガラス繊維、ロックウール、アスベスト繊維、炭素
繊維が特に好ましく使用される。Specific examples of the fibrous material preferably applicable to the present invention include metal fibers, ceramic fibers, glass fibers, rock wool, asbestos fibers, carbon fibers, polyimide fibers, and aromatic polyamide fibers. Among these, metal fibers of inorganic fibers, ceramic fibers, glass fibers, rock wool, asbestos fibers, and carbon fibers are particularly preferably used because of their excellent heat resistance, small amount of released gas, and good thermal conductivity.
【００３３】本発明における上記繊維状物は、蒸発源で
ある有機化合物を直接あるいは間接的に覆い、有機化合
物に対する熱伝導体になるとともに、有機化合物の蒸気
に対するフィルターとなって、スプラッシュ飛沫を捕捉
し、そこで再蒸発させる役割をになっている。このた
め、繊維径０．５〜５００μｍであることが好ましく、
さらには１〜４００μｍの繊維集合体を主体にするもの
であることが好ましい。繊維径が０．５μｍ未満では繊
維の酸化安定性などが不安定である可能性があり、一方
５００μｍを越えるとスプラッシュ飛沫の捕捉性能が低
下する傾向がある。In the present invention, the fibrous material directly or indirectly covers the organic compound as an evaporation source, serves as a heat conductor for the organic compound, and serves as a filter for the vapor of the organic compound, thereby catching splash droplets. And then re-evaporate. For this reason, the fiber diameter is preferably 0.5 to 500 μm,
Further, it is preferable that the main body is a fiber aggregate of 1 to 400 μm. If the fiber diameter is less than 0.5 μm, the oxidative stability of the fiber may be unstable, while if it exceeds 500 μm, the performance of catching splash droplets tends to decrease.
【００３４】真空蒸着に際し、蒸発源である有機化合物
は通常、保持容器（るつぼとも言う）に収納する。保持
容器の形状を特に限定しないが、クヌーセン型、末広ノ
ズル型、直筒型、末広筒型、ボート型などがあり、これ
らの容器は少なくとも一方が開放している。保持容器の
種類は、蒸発物質、蒸発速度などによって適宜選択す
る。また、保持容器の材料についても、銅、タングステ
ン、タンタルなどの金属製のものやアルミナのようなセ
ラミックス製のものがあり、用途によって適宜選択す
る。At the time of vacuum deposition, an organic compound as an evaporation source is usually stored in a holding container (also called a crucible). Although the shape of the holding container is not particularly limited, there are a Knudsen type, a divergent nozzle type, a straight cylinder type, a divergent cylinder type, a boat type and the like, and at least one of these vessels is open. The type of the holding container is appropriately selected depending on the evaporating substance, the evaporating speed, and the like. Also, the material of the holding container may be a metal material such as copper, tungsten or tantalum, or a ceramic material such as alumina, and is appropriately selected depending on the application.
【００３５】上記保持容器へ、蒸発源として有機化合物
を直接、あるいは繊維状物に付着した状態で、あるいは
多孔体に吸収した状態などで収納したあと、上記繊維状
物で該有機化合物を直接又は空隙を介して間接的に被覆
する。有機化合物に対する均一な熱伝導とスプラッシュ
飛沫の捕捉性能の両面から、実質的に露出部分の無いよ
う全面的に被覆するのが好ましい。After the organic compound is stored in the holding container directly or as a source of evaporation, in a state of being attached to a fibrous material, or in a state of being absorbed in a porous material, the organic compound is directly or indirectly absorbed by the fibrous material. Coating indirectly through voids. From the viewpoint of both uniform heat conduction to the organic compound and the performance of capturing splash droplets, it is preferable to cover the entire surface substantially without any exposed portion.
【００３６】例えば、クヌーセン型や末広ノズル型の保
持容器では、器壁部分から中央部にかけ有機化合物の全
面にわたり満遍なく繊維状物を充填する。充填による繊
維状物と有機化合物との接触の程度、あるいは非接触の
程度を一概に指定できないが、一般論として、なるべく
均一に接触しているか、逆に全く接触していないかのど
ちらかにすることが好ましい。場合によっては、これら
の保持容器のノズル部分のみに繊維状物を充填する方法
があり、繊維状物の使用量を減らすことができる。For example, in the case of a Knudsen-type or divergent nozzle-type holding vessel, the fibrous material is uniformly filled over the entire surface of the organic compound from the vessel wall to the center. The degree of contact between the fibrous material and the organic compound due to filling or the degree of non-contact cannot be specified unconditionally, but in general terms, either the contact is as uniform as possible or the contact is not at all Is preferred. In some cases, there is a method of filling only the nozzle portion of these holding containers with a fibrous material, and the amount of fibrous material used can be reduced.
【００３７】また、直筒型、末広筒型の保持容器の場合
は、繊維状物を充填しやすいことから、有機化合物の表
面に密接するように繊維状物を全面的に満遍なく均一に
充填するのが好ましい。なお、繊維状物の充填量（ある
いは充填層の厚さ）は、蒸着膜の性能、品質、経済性な
どから決めるべきものである。In the case of a straight or divergent holding container, it is easy to fill the fibrous material. Therefore, the fibrous material should be filled evenly and uniformly so as to be in close contact with the surface of the organic compound. Is preferred. The filling amount of the fibrous material (or the thickness of the filling layer) should be determined based on the performance, quality, economy and the like of the deposited film.
【００３８】本発明は、真空蒸着法、イオンプレーティ
ング法、反応性蒸着法など熱蒸発技術を使用して有機化
合物の被膜を形成するＰＶＤ、ＣＶＤ法に好適に使用で
きる。The present invention can be suitably used for PVD and CVD methods for forming a film of an organic compound using a thermal evaporation technique such as a vacuum evaporation method, an ion plating method, and a reactive evaporation method.
【００３９】蒸発時の加熱方法として、ハロゲンランプ
法、シーズヒータ法、抵抗加熱法、電子線ビーム法、プ
ラズマ電子線ビーム法、誘導加熱法などがあるが、本発
明ではいずれの方法でも用いることが可能である。ま
た、蒸発は１０-6〜１０Ｐａ、さらには１０-4〜１Ｐａ
程度の減圧下で行うことが好ましい。As a heating method at the time of evaporation, there are a halogen lamp method, a sheath heater method, a resistance heating method, an electron beam method, a plasma electron beam method, an induction heating method, and the like. Is possible. Further, the evaporation is 10 -6 to 10 Pa, and furthermore, 10 -4 to 1 Pa
It is preferable to perform the reaction under a reduced pressure.
【００４０】なお、本発明の光学物品は、有機化合物の
被膜を形成する際、被膜の性能、品質などに従い、室温
から光学物品の耐熱温度または有機化合物の耐熱温度ま
での任意の温度を取りうるものである。When forming a coating of an organic compound, the optical article of the present invention can take any temperature from room temperature to the heat resistant temperature of the optical article or the organic compound according to the performance and quality of the coating. Things.
【００４１】[0041]
【実施例】本発明について、実施例を用いて具体的に説
明するが、本発明はこれらに限定されるものではない。 実施例１ 厚さ２ｍｍのＰＭＭＡ基板約４００ｃｍ2に、真空蒸着
法により基板側から外へ向かい、ＳｉＯ２／ＺｒＯ２／
ＳｉＯ２／ＺｒＯ２／ＳｉＯ２の順に多層反射防止膜を
積層し、防汚剤を真空蒸着する基板とした。EXAMPLES The present invention will be specifically described with reference to examples, but the present invention is not limited to these examples. Example 1 On a PMMA substrate having a thickness of 2 mm of about 400 cm 2 , SiO2 / ZrO2 /
A multilayer antireflection film was laminated in the order of SiO2 / ZrO2 / SiO2 to obtain a substrate on which an antifouling agent was vacuum-deposited.
【００４２】下記構造Ｖに示される防汚剤を、内径３ｃ
ｍ、深さ１．５ｃｍの銅製ハースへ０．２ｇ秤取し、そ
の上へ繊維径約２０μｍのスチールウール（”ボンスタ
ー”＃００００、日本スチールウール社）１．０ｇを満
遍なく防汚剤に接するように、開口部全面へ充填して蒸
発源とした。 構造Ｖ (EtO)3SiCH2CH2CH2NHCOOCH2(CF2CF2O)p(CF2O)qCH2 OCON
HCH2CH3CH2Si(OEt)3 （数平均分子量４５００ ｐ／ｑ≒１） 真空蒸着装置ＢＭＣ−７００（シンクロン社製）に上記
基板と蒸発源をセットした。２．５×１０-3Ｐａまで減
圧してから、電子ビーム法で加熱して防汚剤を基板に真
空蒸着した。An antifouling agent represented by the following structure V was used with an inner diameter 3c
0.2 g is weighed into a copper hearth having a depth of 1.5 cm and a depth of 1.5 cm, and 1.0 g of steel wool ("Bonstar"# 0000, Nippon Steel Wool Co., Ltd.) having a fiber diameter of about 20 μm is evenly contacted with the antifouling agent. Thus, the entire surface of the opening was filled to form an evaporation source. Structure V (EtO) 3 SiCH 2 CH 2 CH 2 NHCOOCH 2 (CF 2 CF 2 O) p (CF 2 O) q CH 2 OCON
HCH 2 CH 3 CH 2 Si (OEt) 3 (number average molecular weight 4500 p / q ≒ 1) The substrate and the evaporation source were set in a vacuum evaporation apparatus BMC-700 (manufactured by SYNCHRON). After reducing the pressure to 2.5 × 10 −3 Pa, the substrate was heated by an electron beam method, and the antifouling agent was vacuum-deposited on the substrate.
【００４３】得られた防汚膜にはブツが見られず、高い
指紋拭き取り性能を示した。 実施例２ 上記実施例において、スチールウールの代わりに繊維径
約７μｍの炭素繊維の繊維集合体を０．３ｇ用いる以外
は実施例１と同じにして、防汚剤を真空蒸着した。The obtained antifouling film was free of bumps and showed high fingerprint wiping performance. Example 2 An antifouling agent was vacuum deposited in the same manner as in Example 1 except that 0.3 g of a carbon fiber fiber aggregate having a fiber diameter of about 7 μm was used instead of steel wool.
【００４４】得られた防汚膜にはブツが見られず、高い
指紋拭き取り性能を示した。 比較例１ 実施例１において、スチールウールを用いずに防汚剤を
真空蒸着したところ、防汚膜に０．１ｍｍ前後のブツが
１個／ｃｍ2 程度発生した。The obtained antifouling film had no bumps and showed high fingerprint wiping performance. Comparative Example 1 In Example 1, when the antifouling agent was vacuum-deposited without using steel wool, spots of about 0.1 mm / cm 2 were generated on the antifouling film.
【００４５】[0045]
Claims (3)
物品の製造方法において、蒸発源である有機化合物の表
面を、直接又は空隙を介して間接的に繊維状物で被覆
し、真空下で加熱することを特徴とする光学物品の製造
方法。In a method for producing an optical article, wherein an organic compound is coated on the surface of an optical article, the surface of the organic compound, which is an evaporation source, is coated with a fibrous material directly or indirectly through a void, and the resultant is coated under vacuum. A method for producing an optical article, comprising heating.
の無機繊維の繊維集合体を主体とすることを特徴とする
請求項１記載の光学物品の製造方法。2. The fibrous material has a fiber diameter of 0.5 to 500 μm.
The method for producing an optical article according to claim 1, wherein a fiber aggregate of the inorganic fiber is mainly used.
ている保持容器に収まり、その表面が直接又は空隙を介
して間接的に繊維状物で全面的に被覆されていることを
特徴とする請求項１または２記載の光学物品の製造方
法。3. The method according to claim 1, wherein the organic compound is contained in a holding container having at least one open, and the surface thereof is directly or indirectly covered with a fibrous material through a void. A method for producing an optical article according to claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11131024A JP2000321401A (en) | 1999-05-12 | 1999-05-12 | Manufacture of optical article |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11131024A JP2000321401A (en) | 1999-05-12 | 1999-05-12 | Manufacture of optical article |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2000321401A true JP2000321401A (en) | 2000-11-24 |
Family
ID=15048234
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP11131024A Pending JP2000321401A (en) | 1999-05-12 | 1999-05-12 | Manufacture of optical article |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2000321401A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001281412A (en) * | 2000-03-31 | 2001-10-10 | Nissha Printing Co Ltd | Antireflection member and method for producing the same |
| JP2007155802A (en) * | 2005-11-30 | 2007-06-21 | Hoya Corp | Method for producing thin film and optical member |
| WO2009028389A1 (en) * | 2007-08-28 | 2009-03-05 | Hoya Corporation | Evaporation source, process for producing optical member, and optical member |
| WO2009101986A1 (en) * | 2008-02-12 | 2009-08-20 | Fujifilm Corporation | Fluorine-containing polyfunctional silicon compound and method for producing fluorine-containing polyfunctional silicon compound |
| JP2016011460A (en) * | 2014-06-02 | 2016-01-21 | キヤノンオプトロン株式会社 | Evaporation source and vapor deposition method using the same |
-
1999
- 1999-05-12 JP JP11131024A patent/JP2000321401A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001281412A (en) * | 2000-03-31 | 2001-10-10 | Nissha Printing Co Ltd | Antireflection member and method for producing the same |
| JP2007155802A (en) * | 2005-11-30 | 2007-06-21 | Hoya Corp | Method for producing thin film and optical member |
| WO2009028389A1 (en) * | 2007-08-28 | 2009-03-05 | Hoya Corporation | Evaporation source, process for producing optical member, and optical member |
| WO2009101986A1 (en) * | 2008-02-12 | 2009-08-20 | Fujifilm Corporation | Fluorine-containing polyfunctional silicon compound and method for producing fluorine-containing polyfunctional silicon compound |
| JP5286289B2 (en) * | 2008-02-12 | 2013-09-11 | 富士フイルム株式会社 | Fluorine-containing polyfunctional silicon compound and method for producing fluorine-containing polyfunctional silicon compound |
| US8541533B2 (en) | 2008-02-12 | 2013-09-24 | Fujifilm Corporation | Fluorine-containing polyfunctional silicon compound and method for producing fluorine-containing polyfunctional silicon compound |
| JP2016011460A (en) * | 2014-06-02 | 2016-01-21 | キヤノンオプトロン株式会社 | Evaporation source and vapor deposition method using the same |
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