JPH0437617A - Optical element forming die and its production - Google Patents
Optical element forming die and its productionInfo
- Publication number
- JPH0437617A JPH0437617A JP14162090A JP14162090A JPH0437617A JP H0437617 A JPH0437617 A JP H0437617A JP 14162090 A JP14162090 A JP 14162090A JP 14162090 A JP14162090 A JP 14162090A JP H0437617 A JPH0437617 A JP H0437617A
- Authority
- JP
- Japan
- Prior art keywords
- mold
- diamond
- film
- molding
- base material
- 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
- 230000003287 optical effect Effects 0.000 title claims abstract description 26
- 238000004519 manufacturing process Methods 0.000 title claims description 15
- 239000010432 diamond Substances 0.000 claims abstract description 197
- 229910003460 diamond Inorganic materials 0.000 claims abstract description 194
- 239000000463 material Substances 0.000 claims abstract description 71
- 239000011521 glass Substances 0.000 claims abstract description 58
- 239000013078 crystal Substances 0.000 claims abstract description 33
- 239000011248 coating agent Substances 0.000 claims abstract description 8
- 238000000576 coating method Methods 0.000 claims abstract description 8
- 238000000465 moulding Methods 0.000 claims description 68
- 238000000034 method Methods 0.000 claims description 26
- 238000005268 plasma chemical vapour deposition Methods 0.000 claims description 10
- 239000012071 phase Substances 0.000 claims description 4
- 239000012808 vapor phase Substances 0.000 claims description 3
- 238000004554 molding of glass Methods 0.000 claims 1
- 238000002156 mixing Methods 0.000 abstract description 2
- 238000005498 polishing Methods 0.000 description 88
- 239000000843 powder Substances 0.000 description 47
- 239000002245 particle Substances 0.000 description 46
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 42
- 239000007789 gas Substances 0.000 description 41
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 30
- 230000003746 surface roughness Effects 0.000 description 30
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 27
- 238000000151 deposition Methods 0.000 description 17
- 230000008021 deposition Effects 0.000 description 17
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 16
- 230000015572 biosynthetic process Effects 0.000 description 16
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 14
- 229910052802 copper Inorganic materials 0.000 description 14
- 239000010949 copper Substances 0.000 description 14
- 238000001237 Raman spectrum Methods 0.000 description 13
- 239000006061 abrasive grain Substances 0.000 description 13
- 229910003481 amorphous carbon Inorganic materials 0.000 description 13
- 238000002003 electron diffraction Methods 0.000 description 13
- 230000009477 glass transition Effects 0.000 description 13
- 238000010438 heat treatment Methods 0.000 description 13
- 125000004432 carbon atom Chemical group C* 0.000 description 11
- 238000000921 elemental analysis Methods 0.000 description 11
- 238000010884 ion-beam technique Methods 0.000 description 10
- 241000511976 Hoya Species 0.000 description 8
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 8
- 229910052742 iron Inorganic materials 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- 239000005304 optical glass Substances 0.000 description 5
- 239000002344 surface layer Substances 0.000 description 5
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 230000001133 acceleration Effects 0.000 description 4
- ORILYTVJVMAKLC-UHFFFAOYSA-N adamantane Chemical compound C1C(C2)CC3CC1CC2C3 ORILYTVJVMAKLC-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 125000004429 atom Chemical group 0.000 description 3
- 239000011195 cermet Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- 238000007740 vapor deposition Methods 0.000 description 3
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- -1 TaCTiC Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 229910002090 carbon oxide Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052754 neon Inorganic materials 0.000 description 2
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- FDPIMTJIUBPUKL-UHFFFAOYSA-N pentan-3-one Chemical compound CCC(=O)CC FDPIMTJIUBPUKL-UHFFFAOYSA-N 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000010583 slow cooling Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 1
- 235000014443 Pyrus communis Nutrition 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000011278 co-treatment Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000001659 ion-beam spectroscopy Methods 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
- 239000001272 nitrous oxide Substances 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 229930195734 saturated hydrocarbon Natural products 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 229930195735 unsaturated hydrocarbon Natural products 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B11/00—Pressing molten glass or performed glass reheated to equivalent low viscosity without blowing
- C03B11/06—Construction of plunger or mould
- C03B11/08—Construction of plunger or mould for making solid articles, e.g. lenses
- C03B11/084—Construction of plunger or mould for making solid articles, e.g. lenses material composition or material properties of press dies therefor
- C03B11/086—Construction of plunger or mould for making solid articles, e.g. lenses material composition or material properties of press dies therefor of coated dies
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B11/00—Pressing molten glass or performed glass reheated to equivalent low viscosity without blowing
- C03B11/06—Construction of plunger or mould
- C03B11/08—Construction of plunger or mould for making solid articles, e.g. lenses
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2215/00—Press-moulding glass
- C03B2215/02—Press-mould materials
- C03B2215/08—Coated press-mould dies
- C03B2215/14—Die top coat materials, e.g. materials for the glass-contacting layers
- C03B2215/24—Carbon, e.g. diamond, graphite, amorphous carbon
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Re-Forming, After-Treatment, Cutting And Transporting Of Glass Products (AREA)
- Chemical 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、レンズ、プリズム等のガラス製光学素子を、
ガラス素材のプレス成形により製造するのに使用される
型及びその製造方法に関するものである。[Detailed Description of the Invention] [Industrial Application Field] The present invention provides glass optical elements such as lenses and prisms,
The present invention relates to a mold used for manufacturing a glass material by press molding and a manufacturing method thereof.
[従来の技術]
研磨工程を必要としないでガラス素材のプレス成形によ
ってレンズを製造する技術は従来のレンズの製造に於て
必要とされた複雑な工程をな(し、簡単かつ安価にレン
ズを製造することを可能とし、近来、レンズのみならず
プリズムその他のガラス製光学素子の製造に使用される
ようになってきた。[Prior art] The technology of manufacturing lenses by press-molding glass materials without requiring a polishing process eliminates the complicated processes required in conventional lens manufacturing (and allows lenses to be manufactured easily and inexpensively). Recently, it has come to be used for manufacturing not only lenses but also prisms and other glass optical elements.
このようなガラスの光学素子のプレスに使用される型材
に要求される性質としては、硬さ、耐熱性、離型性、鏡
面加工性等に優れていることが挙げられる。従来、この
種の型材として金属やセラミックス及びそれらをコーテ
ィングしたものとして特開昭49−5112、特開昭5
2−45613、特開昭60−246230を初めとし
、数多くの提案がされている。しかし、これらの型及び
コーテイング材は、酸化し易い物質であったり、成形品
であるガラスとの融着やガラス面に曇りを生ずる等光学
ガラスの型材やコーテイング材として適当ではなかった
。Properties required of the mold material used for pressing such glass optical elements include excellent hardness, heat resistance, mold releasability, mirror workability, and the like. Conventionally, metals, ceramics, and coated materials of this type have been disclosed in Japanese Patent Application Laid-Open Nos. 49-5112 and 1973.
Many proposals have been made, including JP-A No. 2-45613 and JP-A No. 60-246230. However, these molds and coating materials are not suitable as mold materials or coating materials for optical glass because they are easily oxidized, fuse with the molded glass, or cause clouding on the glass surface.
[発明が解決しようとする課題]
これに対し、最近は上記の物質よりもガラスとの化学反
応が起こりにく(、酸化にも強く、大きな硬度を持つダ
イヤモンドをコーティングしたガラス成形用型(特開昭
61−183134.特開昭61−242922、特開
平1−301864)が提案されている。しかしながら
、ガラス成形用型のコーテイング材として勝れた性質を
持つダイヤモンド膜は、型母材との!着力が十分でない
場合が多く、室温からガラス成形温度の間で温度を変化
させると、型母材からダイヤモンド膜か浮きあがってき
たり、剥離してしまうことがし7ばしば生ずる。更に極
端な場合は、800℃〜1000℃でダイヤモンドを成
膜し、室温に戻しただけで型からダイヤモンド膜が浮き
上がり、剥離してしまうことさえある。これは、ダイヤ
モンドの線膨張係数が一般的な型母材物質のそれよりも
一桁小さいために生ずるものと考えられる。特開昭61
−183134及び特開昭61−242922に開示さ
れているイオンビームスパッタ法によるダイヤモンドも
例外ではなくアモルファス成分の少ない高品質のダイヤ
モンド膜であればあるほど型から剥離する場合が多い。[Problem to be solved by the invention] In contrast, recently, glass molding molds coated with diamond, which is resistant to oxidation and has high hardness, have been developed that are less likely to cause chemical reactions with glass than the above-mentioned substances (especially 183134/1983, 242922/1982, and 301864/1999). However, diamond film, which has excellent properties as a coating material for glass molding molds, has poor bonding with the mold base material. !In many cases, the adhesion strength is not sufficient, and when the temperature is changed between room temperature and glass molding temperature, the diamond film often lifts up or peels off from the mold base material. In some cases, diamond film is formed at 800°C to 1000°C, and the diamond film lifts from the mold and even peels off simply by returning it to room temperature.This is because the coefficient of linear expansion of diamond is This is thought to occur because it is one order of magnitude smaller than that of the base material. JP-A-61
Diamond produced by the ion beam sputtering method disclosed in JP-A-183134 and JP-A-61-242922 is no exception; a high-quality diamond film with less amorphous components is more likely to peel off from the mold.
また、ダイヤモンド、グラファイト及びアモルファス状
カーボンの3種類の物質から成るC昆合膜をコーティン
グした型(特開平1−301864)は、温度変化で剥
離することは稀であるが、成形を重ねるにしたがいアモ
ルファス状カーボンが摩耗し、ダイヤモンド結晶だけが
特異的に残り、最大面粗さ200人という面精度を保つ
ことができな(なるという欠点を有している。In addition, molds coated with a carbon film made of three types of materials: diamond, graphite, and amorphous carbon (Japanese Unexamined Patent Publication No. 1-301864) rarely peel off due to temperature changes, but as molding is repeated, The amorphous carbon wears away and only the diamond crystals remain, making it impossible to maintain the surface accuracy of a maximum surface roughness of 200 mm.
従って、本発明の第1の目的は、室温からガラス成形温
度の間での温度変化によっても型母材から浮きあがって
きたり剥離したりしない、密着性に優れたダイヤモンド
膜が被覆された成形用型及びその製造方法を提供するこ
とにある。Therefore, the first object of the present invention is to provide a molding device coated with a diamond film with excellent adhesion that does not lift or peel off from the mold base material even when the temperature changes between room temperature and glass molding temperature. The object of the present invention is to provide a mold and a method for manufacturing the same.
本発明の第2の目的は、酸化し難く、ガラスとの融着や
ガラス面に曇りを生じない、コーティング成形用型及び
その製造方法を提供することにある。A second object of the present invention is to provide a mold for coating molding that is resistant to oxidation and does not cause fusion with glass or clouding of the glass surface, and a method for manufacturing the same.
本発明の第3の目的は、硬さ、耐熱性、離型性、鏡面加
工性等に優れている成形用型及びその製造方法を提供す
ることにある。A third object of the present invention is to provide a mold that is excellent in hardness, heat resistance, mold releasability, mirror workability, etc., and a method for manufacturing the same.
[課題を解決するための手段及び作用]本発明は、以上
述べたようなダイヤモンド膜と型母材との密着力の弱さ
を解決するためになされたものであり、光学ガラス素子
の形状に対応するようにあらかじめ加工したガラス成形
用型の表層にダイヤモンド結晶を含有させ、この上にダ
イヤモンド月莫を堆積させている。[Means and effects for solving the problems] The present invention has been made to solve the above-mentioned weak adhesion between the diamond film and the mold base material, and it Diamond crystals are contained in the surface layer of a correspondingly processed glass mold, and diamond crystals are deposited on top of this.
すなわち、本発明は、ガラス製光学素子のプレス成形に
使用される型において、型母材の少なくとも成形面には
ダイヤモンド結晶が型母材表面に露出するように埋め込
まれており、かつ該ダイヤモンド結晶が埋め込まれを母
材表面には気相法によって堆積した多結晶ダイヤモンド
膜か被覆されていることを特徴とする、光学素子成形用
型、並びに、型母材の少なくとも成形面にはダイヤモン
ド結晶が型母材表面に露出するように埋め込まれている
型母材上に、気相法によって多結晶ダイヤモンド膜を被
覆することを特徴とする製造方法である。That is, the present invention provides a mold used for press-molding a glass optical element, in which diamond crystals are embedded in at least the molding surface of the mold base material so as to be exposed on the surface of the mold base material, and the diamond crystals are embedded in at least the molding surface of the mold base material, and A mold for molding an optical element is characterized in that the surface of the base material is coated with a polycrystalline diamond film deposited by a vapor phase method, and at least the molding surface of the mold base material has diamond crystals. This manufacturing method is characterized in that a polycrystalline diamond film is coated by a vapor phase method on a mold base material embedded so as to be exposed on the surface of the mold base material.
以下、本発明について詳述する。The present invention will be explained in detail below.
型母材は成形する光学ガラスの形状に対応する形状に加
工されており、その材質として超硬合金、WC,SiC
,SiN、アルミナ、S i 02Z rO2サーメツ
ト、TaCTiC,Ni基合金、CO基合金が挙げられ
るが、このほかにも耐熱性に優れ、酸化に強く、成形時
の加圧に対して十分な硬度を持っている物質ならば用い
ることが可能である。ダイヤモンド結晶をこれらの型の
表層に導入する方法は、型の焼結体を合成するさいに型
表層部にダイヤモンド結晶を混入させても良いし、型形
成後に結晶のダイヤモンド砥粒を含有する溶液中で型を
超音波処理し、ダイヤモンドを型表面に埋め込んでも良
い。ただし、ダイヤモンド結晶を型表層に埋め込む方法
は、これらに限るものではなく、他のどのような方法で
もさしつかえない。The mold base material is processed into a shape that corresponds to the shape of the optical glass to be molded, and its materials include cemented carbide, WC, and SiC.
, SiN, alumina, SiO2ZrO2 cermet, TaCTiC, Ni-based alloy, and CO-based alloy, but there are also other materials that have excellent heat resistance, are resistant to oxidation, and have sufficient hardness to withstand pressure during molding. You can use any substance you have. Diamond crystals can be introduced into the surface layer of these molds by mixing diamond crystals into the surface layer of the mold when synthesizing the sintered body of the mold, or by adding diamond crystals to a solution containing crystal diamond abrasive grains after mold formation. The mold may be subjected to ultrasonic treatment inside the mold to embed diamonds into the mold surface. However, the method of embedding diamond crystals in the mold surface layer is not limited to these methods, and any other method may be used.
表層部に埋め込まれたダイヤモンド結晶は、それを核と
してダイヤモンド多結晶が成長できるように、第1図に
示すようにその一部が型母材1表面に露出している。こ
れらのダイヤモンド結晶は型母材とこの上に堆積される
ダイヤモト膜を強固に結び付ける役割をする。その露出
状態は、ダイヤモンド結晶の一部が表面より上に出でい
ても良いしく第1図のa)、型表面と同じ高さで出てい
ても良い(第1図のb)。ただし、表面よりその一部が
出るような埋め込まれ方の第1図の8の場合にはダイヤ
モンド結晶の体積の半分以上が型母材中に埋め込まれて
いることが望ましい。また、埋め込むべきダイヤモンド
結晶の平均粒径は型母材に悪影響を及ぼさない範囲あれ
ば、どのような大きさでもさしつかえないが、型母材表
層に出る部分は、堆積するダイヤモンド膜の平坦化や後
のダイヤモンド膜の研磨を容易にするためには1μm以
下であることが望ましい。又、ダイヤモンド膜を緻密に
堆積するために、ダイヤモンド結晶の表面密度はは0.
01個/μm2以上であることが望ましい。A portion of the diamond crystal embedded in the surface layer is exposed on the surface of the mold base material 1, as shown in FIG. 1, so that diamond polycrystals can grow using the diamond crystal as a nucleus. These diamond crystals serve to firmly connect the mold base material and the diamond film deposited thereon. The exposed state may be such that a part of the diamond crystal is exposed above the surface (a) in FIG. 1, or it may be exposed at the same height as the mold surface (b in FIG. 1). However, in the case of 8 in FIG. 1, where a portion of the diamond crystal is embedded above the surface, it is desirable that half or more of the volume of the diamond crystal be embedded in the mold base material. In addition, the average grain size of the diamond crystals to be embedded may be any size as long as it does not adversely affect the mold base material, but the portion that appears on the surface of the mold base material may flatten the deposited diamond film or In order to facilitate subsequent polishing of the diamond film, it is desirable that the thickness be 1 μm or less. In addition, in order to deposit a diamond film densely, the surface density of diamond crystals is set to 0.
01 pieces/μm2 or more is desirable.
上記型母材にコートする多結晶ダイヤモンド膜は、主と
してダイヤモンド結晶からなる。各結晶は、様々の格子
欠陥や(111)面の積層欠陥を含んでいるが基本構造
は立方晶ダイヤモンドである。ただし、2つの結晶がぶ
つがり合う境界には曲線状の、また、多数の結晶がぶつ
かり合う境界には多角柱のアモルファス炭素相が存在す
る。格子欠陥やアモルファス相には、炭素以外の元素が
含まれでいても良いが、これらの不純物原子の総量は、
原子数で01%以下であることが望ましい。これより不
純物原子の数が増えると、ダイヤモンド構造の不安定化
を招く。The polycrystalline diamond film coated on the mold base material is mainly composed of diamond crystals. Although each crystal contains various lattice defects and (111)-plane stacking faults, the basic structure is cubic diamond. However, a curved amorphous carbon phase exists at the boundary where two crystals collide, and a polygonal columnar amorphous carbon phase exists at the boundary where many crystals collide. Lattice defects and amorphous phase may contain elements other than carbon, but the total amount of these impurity atoms is
It is desirable that the number of atoms is 0.1% or less. If the number of impurity atoms increases beyond this, the diamond structure becomes unstable.
これらの多結晶ダイヤモンド膜の形成には、マイクロ波
プラズマCVD法、高周波プラズマCVD法、直流プラ
ズマCVD法、直流アーク塾プラズマCVD法、高層波
熱プラズマCVD法、燃焼炎、・去、軌フィラメント法
、電子アシストプラズマCV D法等既に公知の多結晶
ダイヤモンド膜の形成刃1去を用いる。These polycrystalline diamond films can be formed using microwave plasma CVD, high-frequency plasma CVD, DC plasma CVD, DC arc plasma CVD, high-wave thermal plasma CVD, combustion flame, orbital filament methods, etc. A known technique for forming a polycrystalline diamond film, such as electron-assisted plasma CVD method, is used.
これらの装置を用いて多結晶ダイヤモンド膜を形成する
さいには、後の研磨を容易にするために多結晶ダイヤモ
ンド膜の膜厚や膜質が可能な限り均一になるように成膜
中に型母材を回転させたり、平面運動をさせたりするこ
とが好ましい。When forming a polycrystalline diamond film using these devices, a mold matrix is used during film formation to make the thickness and quality of the polycrystalline diamond film as uniform as possible to facilitate subsequent polishing. It is preferable to rotate the material or make it move in a plane.
これらの装置を用いて多結晶ダイヤモンド膜を形成する
原料ガスには、炭素含有ガスを用いる。A carbon-containing gas is used as a raw material gas for forming a polycrystalline diamond film using these devices.
これに混合するガスとして、水素、酸素、ヘリウム、ネ
オン、アルゴン、キセノン等を用いる。炭素含有物とし
ては、メタン、エタン、プロパン、アダマンタン等の飽
和炭化水素類、ベンゼン、ナフタリン等の不飽和炭化水
素類及びこれらの水素原子を他の基で置換した物質、メ
タノール、エタノール等のアルコール類、−酸化炭素、
二酸化炭素等の酸化物、アセトアルデヒド、ホルムアル
デヒド等のアルデヒド類、ギ酸、酢酸等のカルボン酸類
、アセトン、ジエチルケトン等のケトン類、メチルエー
テル、エチルエーテル等のエーテル類を用いる。これら
の炭素含有物のうち室温でガスのものはそのままボンベ
より成膜室へ導入するが、室温で液体や固体のものはバ
ブリングや加熱してガス化してから成膜室へ導入する。Hydrogen, oxygen, helium, neon, argon, xenon, etc. are used as the gas to be mixed with this. Examples of carbon-containing substances include saturated hydrocarbons such as methane, ethane, propane, and adamantane, unsaturated hydrocarbons such as benzene and naphthalene, substances in which these hydrogen atoms have been replaced with other groups, and alcohols such as methanol and ethanol. -carbon oxide,
Oxides such as carbon dioxide, aldehydes such as acetaldehyde and formaldehyde, carboxylic acids such as formic acid and acetic acid, ketones such as acetone and diethyl ketone, and ethers such as methyl ether and ethyl ether are used. Among these carbon-containing substances, those that are gases at room temperature are directly introduced into the film forming chamber from a cylinder, but those that are liquid or solid at room temperature are gasified by bubbling or heating before being introduced into the film forming chamber.
又、上言己方法によって光学素子形成用型材の上にコー
ティングした多結晶ダイヤモンド膜の表面粗さが光学素
子成形用に適合しないほどに荒れている時には研磨を行
なう。研磨は、適当な溶媒に溶かしたダイヤモンド粉末
と金属板やダイヤモンド粉末を埋め込んだ金属板等を用
いて行なう。ダイヤモンド粉末を溶かず溶媒としては水
や研磨用の油を用いる。金属板には、銅、鉄、ニッケル
、コバルト、アルミニウム及びこれらの合金を用いるこ
とが可能である。金属板及び型をそれぞれ回転させなが
ら両者を接触させて多結晶ダイヤモンド膜を研磨する。Further, when the surface roughness of the polycrystalline diamond film coated on the mold material for forming an optical element by the above-mentioned method is too rough to be suitable for forming an optical element, polishing is performed. Polishing is performed using diamond powder dissolved in a suitable solvent and a metal plate or a metal plate embedded with diamond powder. Water or polishing oil is used as a solvent without dissolving the diamond powder. Copper, iron, nickel, cobalt, aluminum, and alloys thereof can be used for the metal plate. The polycrystalline diamond film is polished by bringing the metal plate and mold into contact while rotating them.
この際、多結晶ダイヤモンド膜の研磨速度を促進するた
めに金属板を加熱したり、研磨雰囲気ガスとして水素、
酸素、ヘリウム、ネオン、アルゴン、キセノン、窒素、
−酸化炭素、二酸化炭素、亜酸化窒素、二酸化窒素等を
用いても良い。以上、ダイヤモンド膜の研磨方法につい
て述べたが、研磨方法はこれに限るものではな(、他の
方法であっても良い。At this time, the metal plate is heated to accelerate the polishing speed of the polycrystalline diamond film, and hydrogen is used as the polishing atmosphere gas.
oxygen, helium, neon, argon, xenon, nitrogen,
- Carbon oxide, carbon dioxide, nitrous oxide, nitrogen dioxide, etc. may be used. Although the diamond film polishing method has been described above, the polishing method is not limited to this (other methods may also be used).
[実施例]
以下、実施例により本発明の光学ガラス成形用型の製造
方法とこれを用いて光学ガラス素子を形成した結果につ
いて述べる。[Example] Hereinafter, the method for manufacturing an optical glass mold of the present invention and the results of forming an optical glass element using the same will be described in Examples.
〈実施例1〉
第2図、第3図は本発明に係る光学素子成形用型の1つ
の実施態様を示すもので、図中、1(ま超硬合金を初め
とする耐熱性、耐圧性の型母材、2は該型母材のガラス
素材に接触する成形面に形成された多結晶ダイヤモンド
膜である。<Example 1> Figures 2 and 3 show one embodiment of the mold for molding an optical element according to the present invention. The mold base material 2 is a polycrystalline diamond film formed on the molding surface of the mold base material that comes into contact with the glass material.
第2図は光学素子のプレス成形前の状態を示し、第3図
は光学素子成形後の状態を示す。第2図に示すように、
型の間に置かれたガラス素材3をプレス成形することに
よって、第3図に示すようにレンズ等の光学素子4が形
成される。FIG. 2 shows the optical element before press molding, and FIG. 3 shows the optical element after molding. As shown in Figure 2,
By press-molding the glass material 3 placed between the molds, an optical element 4 such as a lens is formed as shown in FIG.
先ず、第4図のマイクロ波CVD装置を用い、表面層に
平均粒径5μmのダイヤモンド結晶を埋め込んだSil
N4m結体からなる直径35mm、曲率半径45mmの
凹状の型母材13を型ホルダ−15上に設置する。型表
面のダイヤモンド結晶密度は0.01/μm27表面に
出ているダイヤモンドの平均粒径は、SEM観察より0
.7μmである。型ホルダ−15の軸は、真空室11の
エアベアリング20を通って外側に設置されたモーター
21に繋っており、この機構により減圧下で型ホルダ−
15を回転させることができる。回転数は、1分間2回
転にした。First, using the microwave CVD apparatus shown in FIG.
A concave mold base material 13 made of N4m solid and having a diameter of 35 mm and a radius of curvature of 45 mm is placed on the mold holder 15. The diamond crystal density on the mold surface is 0.01/μm27 The average grain size of the diamonds on the surface is 0.01/μm from SEM observation.
.. It is 7 μm. The shaft of the mold holder 15 is connected to a motor 21 installed outside through an air bearing 20 in the vacuum chamber 11, and this mechanism rotates the mold holder under reduced pressure.
15 can be rotated. The number of revolutions was 2 revolutions per minute.
次に5真空室11内を不図示のメカニカルブスターボン
ブ、回転ポンプにより排気口12から排気して真空度を
2X10−3Torrに引上げる。これらポンプの最終
段は、これもまた不図示のガスの除外装置に繋り、成膵
用排ガスは入気中に排出される。原料ガスの導入口14
は、−本の場合もあるし一本以上で構成されている場合
もある。この原料ガスラインは不図示のマスフロー制御
系及びガスボンベに繋っており、1種類のガスを流すこ
とも2種類以上のガスを流すことも2種類以上のガスを
混合して流すことも可能である。Next, the inside of the vacuum chamber 11 is evacuated from the exhaust port 12 using a mechanical booster bomb (not shown) or a rotary pump to raise the degree of vacuum to 2×10 −3 Torr. The last stage of these pumps is connected to a gas exclusion device, also not shown, so that the adult pancreatic waste gas is discharged into the inlet air. Raw material gas inlet 14
may be - books or may consist of one or more books. This raw gas line is connected to a mass flow control system and gas cylinder (not shown), and it is possible to flow one type of gas, two or more types of gas, or a mixture of two or more types of gas. be.
ガス導入口14より真空室11にCH4,H,をそれぞ
れ0,25.2005CCMの流量で混合して導入し、
プランジャー17、不図示の電源部に接続しているスリ
ースタブ18を調節して型の位置にプラズマを生成した
。なお、16は導波管である。2.45GHzのマイク
ロ波出力900W、圧力120Torr、型加勢なしの
条件下、80時間の堆積で50μmの膜が形成された。CH4 and H are mixed and introduced into the vacuum chamber 11 from the gas inlet 14 at a flow rate of 0 and 25.2005 CCM, respectively.
Plasma was generated at the position of the mold by adjusting the plunger 17 and the sleeve stub 18 connected to a power source (not shown). Note that 16 is a waveguide. A 50 μm film was formed in 80 hours of deposition under conditions of 2.45 GHz microwave power of 900 W, pressure of 120 Torr, and no mold support.
成膜中の型温度は850℃〜870°Cであった。表面
粗さはRmaxo、8μmであった。The mold temperature during film formation was 850°C to 870°C. The surface roughness was Rmaxo, 8 μm.
真空室から取りだした多結晶ダイヤモンド膜2をコート
した型1を第5図に示す研磨装置50内の型ホルダ−5
2に設置した。排気口57から研磨装置50内を3X1
0−3Torrまで排気した後、ガス導入口58から1
ト、素ガスを11005CCの流量で研磨装置50内に
導入した。平均粒径05μmのダイヤモンド粉末を含ん
だ鉄板51及び型ホルダ−52をエアベアリング53.
54及びモーター55.56を用いて500rpmで回
転させ1時間研磨した。鉄板の表面形状は直径70 m
m +球面半径45mの凸状にした。型表面粗さはR
max200人であった。The mold 1 coated with the polycrystalline diamond film 2 taken out from the vacuum chamber is placed in a mold holder 5 in the polishing device 50 shown in FIG.
It was installed on 2. 3X1 inside the polishing device 50 from the exhaust port 57
After exhausting to 0-3 Torr, from the gas inlet 58 to 1
First, raw gas was introduced into the polishing apparatus 50 at a flow rate of 11005 cc. An iron plate 51 containing diamond powder with an average particle size of 05 μm and a mold holder 52 are placed on an air bearing 53.
It was rotated at 500 rpm using a motor 54 and a motor 55, and polished for 1 hour. The surface shape of the iron plate is 70 m in diameter.
It was made into a convex shape with m + spherical radius of 45 m. The mold surface roughness is R
The maximum number of people was 200.
型上のダイヤモンド膜のラマンスペクトルを測定すると
、鋭い1333cm−’のピークのみが観測された。反
射電子線回折ではダイヤモンドのみが観測された。これ
らの結果より型上の膜は、ダイヤモンドからなることが
解った。又、膜中の元素分析では炭素原子以外の元素は
見出されなかった。When the Raman spectrum of the diamond film on the mold was measured, only a sharp peak at 1333 cm-' was observed. Only diamond was observed by reflection electron diffraction. From these results, it was found that the film on the mold was composed of diamond. Further, elemental analysis in the film did not find any elements other than carbon atoms.
次に、この型を用いてガラスレンズのプレス成形を行っ
た。成形装置を第6図に示す。102は成形装置、10
4は取入れ用置換室であり、106は成形室である。1
08は蒸着室で、110は取り出し用置換室である。1
12114.116はゲートバルブであり、118はレ
ールであり、120は該レール上を矢印へ方向に搬送せ
しめられるパレットである。124.138.140.
150はシリンダであり、126.152はバルブであ
る。128は成形室106内においてレール118に沿
って配列されているヒーターである。Next, a glass lens was press-molded using this mold. The molding apparatus is shown in FIG. 102 is a molding device, 10
4 is an intake replacement chamber, and 106 is a molding chamber. 1
08 is a deposition chamber, and 110 is a replacement chamber for extraction. 1
12114.116 is a gate valve, 118 is a rail, and 120 is a pallet that is transported on the rail in the direction of the arrow. 124.138.140.
150 is a cylinder, and 126.152 is a valve. 128 is a heater arranged along the rail 118 in the molding chamber 106.
成形室106内はパラレット搬送方向に沿って順に加熱
ゾーン106−1、ブレスゾーン106−2及び徐冷ゾ
ーン106−3とされている。プレスゾーン106−2
において、上記シリンダ138のロッド134の下端に
は成形用上型部材130が固定されており、上記シリン
ダ140のロッド136の上端には成形用下型部材13
2が固定されている。これら上型部材130及び下型部
材132は、上記第2図の本発明による型部材である。Inside the molding chamber 106, a heating zone 106-1, a press zone 106-2, and a slow cooling zone 106-3 are arranged in order along the pallet transport direction. Press zone 106-2
An upper mold member 130 for molding is fixed to the lower end of the rod 134 of the cylinder 138, and a lower mold member 13 for molding is fixed to the upper end of the rod 136 of the cylinder 140.
2 is fixed. These upper mold member 130 and lower mold member 132 are the mold members according to the present invention shown in FIG. 2 above.
蒸着室108内においては、蒸着物質146を収容した
容器142及び該容器を加熱するためのヒーター144
が配置されている。Inside the vapor deposition chamber 108, there is a container 142 containing a vapor deposition substance 146 and a heater 144 for heating the container.
is located.
軟化用、5p=586℃、ガラス転移、占Tg=485
℃の光学ガラス5F14 (ホーヤ製)を所定の形状に
加工して、成形のためのブランクを得た。For softening, 5p=586℃, glass transition, Tg=485
℃ optical glass 5F14 (manufactured by Hoya) was processed into a predetermined shape to obtain a blank for molding.
ガラスブランクをパレット120に置き、取り入れ置換
室104内の120−1の位置へ入れ、該位置のパレッ
トをシリンダ124のロッド122によりA方向に押し
てゲートバルブ112を越えて成形室106内の120
−2の位置へと搬送し、以下同様にして所定のタイミン
グで順次新たに取り入れ置換室104内にパレットを入
れ、このたびにパレットを成形室106内で120−2
−・・・・・・−120−8の位置へと順次搬送した。A glass blank is placed on the pallet 120 and put into the position 120-1 in the intake/displacement chamber 104, and the pallet at that position is pushed in the direction A by the rod 122 of the cylinder 124, past the gate valve 112 and placed at the position 120-1 in the molding chamber 106.
-2 position, and in the same manner, new pallets are sequentially introduced into the replacement chamber 104 at predetermined timing, and each time the pallet is transferred to the molding chamber 106 at 120-2.
It was sequentially conveyed to the position of -...-120-8.
この間に、加熱ゾーン106−1ではガラスブランクを
ヒーター128により徐々に加熱し、12’O−4の位
置で軟化点以上とした上で、ブレスゾーン106−2へ
と搬送し、ここでシリンダ138,140を動作させて
上型部材130及び下型部材132により10kg/c
m2の圧力で5分間プレスし、その後圧力を解除しガラ
ス転移点値下まで冷却し、その後シリンダ138,14
0を作動させて上型部材130及び下型部材132をガ
ラス成形品から離型した。During this time, in the heating zone 106-1, the glass blank is gradually heated by the heater 128, and after reaching the softening point or higher at the 12'O-4 position, it is transported to the breath zone 106-2, where it is heated to the cylinder 138. , 140 and the upper mold member 130 and lower mold member 132 produce 10 kg/c.
The cylinders 138, 14 are pressed for 5 minutes at a pressure of m2, then the pressure is released and the cylinders 138, 14 are cooled to below the glass transition point.
0 was activated to release the upper mold member 130 and the lower mold member 132 from the glass molded product.
該プレスに際しては、上記パレットが成形用銅型部材と
して利用された。然る後に、徐冷ゾーン106−3では
ガラス成形品を徐々に冷却した。During the pressing, the pallet was used as a molding copper mold member. After that, the glass molded product was gradually cooled in the slow cooling zone 106-3.
尚、成形室106内には窒素ガスを充満させた。Note that the molding chamber 106 was filled with nitrogen gas.
成形室106内に置いて120−8の位置に到達したパ
レットを、次の搬送ではゲートバルブ114を越久て蒸
着室108内の120−9の位置へと搬送し、続けてゲ
ートバルブ116を越えて取り出し置換室110内の1
20−10の位置へと搬送した。そして、次の搬送時に
はシリンダ150を作動させてロット148によりガラ
ス成形品を成形装置102外へ取り出した。The pallet that has been placed in the molding chamber 106 and has reached the position 120-8 is then transported past the gate valve 114 to the position 120-9 in the deposition chamber 108, and then continues past the gate valve 116. 1 in the extraction and replacement chamber 110
It was transported to the 20-10 position. Then, during the next conveyance, the cylinder 150 was operated and the glass molded product was taken out of the molding apparatus 102 by the lot 148.
このようにして連続5000回の成形を行なった結果を
途中経過と共に表1に示す。成形品の表面粗さ、可視光
の透過率は光学素子成形品として十分であり、型と成形
品との離形性にも問題がなかった。Table 1 shows the results of 5000 continuous moldings in this manner, along with the progress. The surface roughness and visible light transmittance of the molded product were sufficient for an optical element molded product, and there were no problems in the releasability between the mold and the molded product.
表1
〈比較例1〉
先ず、Si、N、からなる直径35mm、曲率半径45
mmの凹状の型をエタノール、アセトン中でこの順番に
10分ずつ超音波洗浄し大気中で十分乾燥させる。この
型を実施例1と同じ第4図のマイクロ波CVD装置の型
ホルダ−15上に設置する。回転数は、1分間2回転に
した。Table 1 <Comparative Example 1> First, a material made of Si and N with a diameter of 35 mm and a radius of curvature of 45
A concave mold of 1.0 mm in diameter was ultrasonically cleaned in ethanol and acetone for 10 minutes each in this order, and thoroughly dried in the atmosphere. This mold is placed on the mold holder 15 of the microwave CVD apparatus shown in FIG. 4, which is the same as in Example 1. The number of revolutions was 2 revolutions per minute.
次に、真空室11の真空度を2X10−”Torrまで
引き上げる。ガス導入口14より真空室11にCH4,
H2をそれぞれ0125.200SCCMの流量で混合
して導入し、型の位置にプラズマを生成した。2.45
GHzのマイクロ波出力9000W、圧力120Tor
r、型加熱なしの条件下、80時間の堆積で75μmの
膜が形成された。成膜中の型温度は850℃〜870℃
であった。Next, the degree of vacuum in the vacuum chamber 11 is raised to 2×10-” Torr. CH4,
H2 was mixed and introduced at a flow rate of 0.125.200 SCCM each to generate a plasma at the mold location. 2.45
GHz microwave output 9000W, pressure 120 Tor
r, a 75 μm film was formed after 80 hours of deposition under conditions without mold heating. Mold temperature during film formation is 850℃~870℃
Met.
更に同条件で型を4つの型を作成したところ、5つのう
ちの1つは成膜後、真空室11を窒素ガスでリークし、
型を取りだすと型表面からダイヤモンド膜が剥離してし
まった。Furthermore, when four molds were made under the same conditions, one of the five leaked nitrogen gas from the vacuum chamber 11 after the film was formed.
When the mold was removed, the diamond film peeled off from the mold surface.
〈比較例2〉
先ず、5L3N4からなる直径35mm、曲率半径45
mmの凹状の型を平均粒径2OLtmのダイヤモンド砥
粒で2時間研磨したのち、エタノール、アセトン中でこ
の順番に10分ずつ超音波洗浄し大気中で十分乾燥させ
た。この型の表面をSEMで観察すると、ダイヤモンド
砥粒が多数残存していた。ダイヤモンド砥粒は型材内に
埋め込まれているわけではな(、線状の傷や凹み部分を
中心に散在していた。ダイヤモンド砥粒の密度は、Q、
1/mm”であった。この型を実施例1と同じ第4図の
マイクロ波CVD装置の型ホルダ−15上に設置する。<Comparative Example 2> First, a material made of 5L3N4 with a diameter of 35 mm and a radius of curvature of 45
After polishing the concave mold with a diameter of 2 OLtm for 2 hours using diamond abrasive grains having an average particle size of 2 OLtm, the mold was ultrasonically cleaned in ethanol and acetone for 10 minutes each in this order, and thoroughly dried in the atmosphere. When the surface of this mold was observed using a SEM, it was found that many diamond abrasive grains remained. The diamond abrasive grains are not embedded in the mold material (they are scattered mainly in linear scratches and dents.The density of the diamond abrasive grains is Q,
1/mm''. This mold was placed on the mold holder 15 of the microwave CVD apparatus shown in FIG. 4, which is the same as in Example 1.
回転数は、1分間2回転にした。The number of revolutions was 2 revolutions per minute.
次に、真空室11内の真空度を2xio−”r。Next, the degree of vacuum in the vacuum chamber 11 is set to 2xio-"r.
rrまで引き上げる。ガス導入口14より真空室11に
CH4H2をそれぞれ0.25.200SCCMの流量
で混合して導入し、型の位置にプラズマを生成した。2
.45GHzのマイクロ波出力9000W、圧力120
Torr、型加執なしの条件下、80時間の堆積で80
μmの膜が形成された。成膜中の型温度は850℃〜8
70℃であった。表面粗さはRmaxO,8μmであっ
た。Raise it to rr. CH4H2 was mixed and introduced into the vacuum chamber 11 from the gas inlet 14 at a flow rate of 0.25.200 SCCM, thereby generating plasma at the position of the mold. 2
.. 45GHz microwave output 9000W, pressure 120
Torr, 80 after 80 hours of deposition under conditions without mold addition.
A μm film was formed. The mold temperature during film formation is 850℃~8
The temperature was 70°C. The surface roughness was RmaxO, 8 μm.
真空室から取りだした多結晶ダイヤモンド膜2をコーテ
ィングした型1を第5図に示す研磨装置50内の型ホル
ダ−52に設置した。排気口57から研磨装置50内を
3X10−3Torrまで排気した後、ガス導入口58
から水素ガスを11005CCの流量で研磨装置50内
に導入した。平均粒径05μmのダイヤモンド粉末を含
んだ鉄板51及び型ホルダ−52をエアベアリング53
.54及びモータ〜55.56を用いて500rpmで
回転させ1時間研磨した。鉄板の表面形状は直径70m
m、球面半径45rr+rr+の凸状にした。型表面粗
さはRmax200人であった。The mold 1 coated with the polycrystalline diamond film 2 taken out from the vacuum chamber was placed in a mold holder 52 in a polishing apparatus 50 shown in FIG. After exhausting the inside of the polishing apparatus 50 to 3X10-3 Torr from the exhaust port 57, the gas inlet 58
Hydrogen gas was introduced into the polishing apparatus 50 at a flow rate of 11005 cc. An iron plate 51 containing diamond powder with an average particle size of 05 μm and a mold holder 52 are placed on an air bearing 53.
.. 54 and motor ~55.56 at 500 rpm for polishing for 1 hour. The surface shape of the iron plate is 70m in diameter.
m, and a convex shape with a spherical radius of 45rr+rr+. The mold surface roughness was Rmax 200.
電子線回折からこの膜はダイヤモンドと同定された。ま
た、ラマンスペクトルにはダイヤモンドの1330cm
−’のピークが観測された。This film was identified as diamond by electron diffraction. Also, the Raman spectrum shows 1330cm of diamond.
-' peak was observed.
次に、この型を用いて実施例1と全く同様に硝材に軟化
点5p=586℃、ガラス転移、申、 1” g =4
85℃の5F14を用いてガラスレンズのプレス成形を
行ったところ、256回目に型中心部のダイヤモンド膜
が剥離したので成形を中止した。Next, using this mold, the glass material was given a softening point of 5p = 586°C and a glass transition of 1" g = 4 in the same manner as in Example 1.
When a glass lens was press-molded using 5F14 at 85°C, the diamond film at the center of the mold peeled off at the 256th time, so the molding was discontinued.
く比較例3〉
先ず、513N4からなる直径35mm、曲率半径45
mmの凹状の型を平均粒径20 Ii、 mのダイヤモ
ンド砥粒を含むエタノール中で05時間超音波処理した
のち、エタノール、アセトン中でこの順番に10分ずつ
超音fj、洗浄し大気中で十分乾燥させる。SEMによ
る表面観察ではダイヤモンド砥粒密度は約0.0057
μm2であった。Comparative Example 3> First, a material made of 513N4 with a diameter of 35 mm and a radius of curvature of 45
A concave mold of 1 mm in diameter was subjected to ultrasonic treatment for 05 hours in ethanol containing diamond abrasive grains with an average particle diameter of 20 Ii, m, and then cleaned with ultrasonic fj for 10 minutes each in ethanol and acetone in this order, and then exposed to air in air. Dry thoroughly. Surface observation by SEM shows that the diamond abrasive grain density is approximately 0.0057.
It was μm2.
この型を図3のマイクロ波CVD装置の梨ホルダー15
上に設置する。回転数は]分子、u+ 2 g転にした
。This mold is used in the pear holder 15 of the microwave CVD apparatus shown in Fig. 3.
Place it on top. The number of rotations was set to ] numerator, u+2g rotation.
次に、真空室11内の真空度を2xlO−3T。Next, the degree of vacuum in the vacuum chamber 11 is set to 2xlO-3T.
rrまで引き上げる。ガス導入口14より真空室11に
CH,、H2をそれぞれ0.25.200SCCMの流
量で混合して導入し、型の位置にプラズマを生成した。Raise it to rr. A mixture of CH and H2 was introduced into the vacuum chamber 11 through the gas inlet 14 at a flow rate of 0.25.200 SCCM to generate plasma at the position of the mold.
2.45GHzのマイクロ波出力9000W、圧力12
0Torr、型加熱なしの条件下、80時間の堆積で8
0μmの膜が形成された。成膜中の型温度は850℃〜
870℃であった。表面粗さはRmaxo、8μmであ
った。2.45GHz microwave output 9000W, pressure 12
8 after 80 hours of deposition at 0 Torr and without mold heating.
A film of 0 μm was formed. Mold temperature during film formation is 850℃~
The temperature was 870°C. The surface roughness was Rmaxo, 8 μm.
真空室から取りだした多結晶ダイヤモンド膜2をコート
した型1を第5図に示す研磨装置50内の型ホルダ−5
2に設置した。排気口57がら研磨装置50内を3X1
0−3Torrまで排気した後、ガス導入口58から水
素ガスを11005CCの流量で研磨装置50内に導入
した。平均粒径0.5μmのダイヤモンド粉末を含んだ
鉄板51及び型ホルダ−52をエアベアリング53.5
4及びモーター55.56を用いて500rpmで回転
させ1時間研磨した。鉄板の表面形状は直径70mm、
球面半径45mmの凸状にした。研磨後の型表面粗さは
Rmax200人であった。The mold 1 coated with the polycrystalline diamond film 2 taken out from the vacuum chamber is placed in a mold holder 5 in the polishing device 50 shown in FIG.
It was installed on 2. 3X1 inside the polishing device 50 through the exhaust port 57
After exhausting to 0-3 Torr, hydrogen gas was introduced into the polishing apparatus 50 from the gas inlet 58 at a flow rate of 11005 cc. An iron plate 51 containing diamond powder with an average particle size of 0.5 μm and a mold holder 52 are placed on an air bearing 53.5.
4 and motor 55.56 at 500 rpm for polishing for 1 hour. The surface shape of the iron plate is 70mm in diameter.
It has a convex shape with a spherical radius of 45 mm. The mold surface roughness after polishing was Rmax 200.
型上のダイヤモンド膜のラマンスペクトルを測定すると
、鋭い1333cm”’のピークが観測された。反射電
子線回折ではダイヤモンドのみが観測された。これらの
結果より型上の膜は、ダイヤモンドからなることが解っ
た。When the Raman spectrum of the diamond film on the mold was measured, a sharp peak at 1333 cm'' was observed.Only diamond was observed in reflection electron diffraction.From these results, it was concluded that the film on the mold was composed of diamond. I understand.
次に、この型を用いて実施例1と全く同様に硝材に軟化
点5p=586℃、ガラス転移C!:1.Tg=485
℃の5F14を用いてガラスレンズのプレス成形を行っ
たところ、成形品の表面粗さやガラスとの離形性に問題
はなかったが、950回目に型中心部のダイヤモンド膜
が剥離したので成形を中止した。Next, using this mold, a glass material with a softening point of 5p=586°C and a glass transition of C! :1. Tg=485
When we press-molded a glass lens using 5F14 at ℃, there were no problems with the surface roughness of the molded product or the releasability from the glass, but the diamond film in the center of the mold peeled off at the 950th press, so we stopped molding. Canceled.
〈実施例2〉
先ず、SiCからなる直径25mm、曲率半径45mm
の凹状の型をエタノール、アセトン中でこの順番に10
分ずつ超音波洗浄し大気中で十分乾燥させる。型表面に
は填結時に型表面にダイヤモンド砥粒を表面密度0.1
/μm2で埋め込んだ。この型を実施例1と同じマイク
ロ波CVD装置の型ホルダ−15上に設置する。回転数
は、1分間1回転にした。<Example 2> First, a material made of SiC with a diameter of 25 mm and a radius of curvature of 45 mm
The concave mold was washed in ethanol and acetone in this order for 10 minutes.
Ultrasonic cleaning for minutes at a time and dry thoroughly in air. Diamond abrasive grains are applied to the mold surface at a surface density of 0.1 during filling.
/μm2. This mold is placed on the mold holder 15 of the same microwave CVD apparatus as in Example 1. The rotation speed was 1 rotation per minute.
次に、真空室11内の真空度を2X10−3T。Next, the degree of vacuum in the vacuum chamber 11 is set to 2X10-3T.
rrまで引き上げる。ガス導入口14より真空室11に
C2Ha 、H2をそれぞれ0.25.2003CCM
の流量で混合して導入し、プランジャー17、スリース
タブ18を調節して型の位置にプラズマを生成した。2
.45GHzのマイクロ波出力1000W、圧力90T
orr、型加熱なしの条件下、4時間の堆積で5μmの
膜が形成された。成膜中の型温度は880℃〜900″
Cであった。Raise it to rr. 0.25.2003 CCM of C2Ha and H2 are each introduced into the vacuum chamber 11 from the gas inlet 14.
The plunger 17 and the sleeve stub 18 were adjusted to generate plasma at the position of the mold. 2
.. 45GHz microwave output 1000W, pressure 90T
orr, a 5 μm film was formed in 4 hours of deposition under conditions without mold heating. Mold temperature during film formation is 880℃~900''
It was C.
真空室11から取りだした多結晶ダイヤモンド膜2をコ
ートした型lを実施例1と同じ研磨装置50内の型ホル
ダ−52に設置した。研磨装置50を3X10−3To
rrまで排気した後、ガス導入口58から酸素ガスを2
00SCCMの流量で研磨装置50内に導入した。平均
粒径10umのダイヤモンド粉末を含んだ銅板51及び
型ホルダ−52を60Orpmで回転させた。銅板の表
面形状は直径70mm 球面半径45mmの凸状にし
た。10時間研磨した後平均粒径10μmのダイヤモン
ド粉末を含んだ銅板51を平均粒径3μmのダイヤモン
ド粉末を含んだ銅板51に変えさらに2時間研磨した。The mold 1 coated with the polycrystalline diamond film 2 taken out from the vacuum chamber 11 was placed in the mold holder 52 in the same polishing device 50 as in Example 1. Polishing device 50 3X10-3To
After exhausting to rr, oxygen gas is introduced from the gas inlet 58 by 2
It was introduced into the polishing apparatus 50 at a flow rate of 00 SCCM. A copper plate 51 containing diamond powder with an average particle size of 10 um and a mold holder 52 were rotated at 60 rpm. The surface shape of the copper plate was a convex shape with a diameter of 70 mm and a spherical radius of 45 mm. After polishing for 10 hours, the copper plate 51 containing diamond powder with an average particle size of 10 μm was replaced with a copper plate 51 containing diamond powder with an average particle size of 3 μm, and polishing was continued for another 2 hours.
そして、最終研磨用の平均粒径0.5μmのダイヤモン
ド粉末を含んだ銅板51で更に1時間研磨した。型表面
の粗さはRmax210人であった。Then, polishing was performed for an additional hour using a copper plate 51 containing diamond powder with an average particle size of 0.5 μm for final polishing. The roughness of the mold surface was Rmax 210.
型上のダイヤモンド膜のラマンスペクトルを測定すると
、鋭い1333cm−’のピークが観測された。反射電
子線回折ではダイヤモンドのみが観測された。これらの
結果より型上の膜は、ダイヤモンドとからなることが解
った。又、膜中の元素分析では炭素原子以外の元素は見
出されなかった。When the Raman spectrum of the diamond film on the mold was measured, a sharp peak at 1333 cm-' was observed. Only diamond was observed by reflection electron diffraction. From these results, it was found that the film on the mold was composed of diamond. Further, elemental analysis in the film did not find any elements other than carbon atoms.
次に、この型を用いて実施例1と全く同様に硝材に軟化
点5p=586℃、ガラス転移点Tg=485℃の5F
14を用いてガラスレンズのプレス成形を行った。Next, using this mold, in exactly the same manner as in Example 1, 5F with a softening point of 5p = 586°C and a glass transition point of Tg = 485°C was prepared.
A glass lens was press-molded using No. 14.
このようにして連続5000回の成形を行なった結果を
途中経過と共に表2に示す。Table 2 shows the results of 5,000 continuous moldings in this manner, along with the progress.
表2
〈実施例3〉
WCを主成分としTiC,TaCをバインダーとする直
径40mm、平板の型をエタノール、アセトン中でこの
順番に10分ずつ超音波洗浄し大気中で十分乾燥させる
。型表面にはダイヤモンド砥粒が0.05/μm2で埋
め込まれている。この型を実施例1と同じマイクロ波C
VD装置の型ホルダ−15上に設置する。回転数は、1
分間1回転にした。 次に、真空室11内の真空度を2
X10−3Torrまで引上げる。C2H50H(総量
200cc)をバブラーを通して気化し、ガス導入口1
4より真空室11に水素ガス(流量、2003CCM)
と共に導入し、プランジャー17、スリースタブ18を
調節して型の位置にプラズマを生成した。2.45GH
zのマイクロ波出力1000W、圧力90Torr、型
加熱なしの条件下、1時間の堆積で10umの膜が形成
された。成膜中の型温度は800°C〜820℃であっ
た。Table 2 <Example 3> A flat plate mold with a diameter of 40 mm containing WC as a main component and TiC and TaC as binders was ultrasonically cleaned in ethanol and acetone for 10 minutes each in this order and thoroughly dried in the atmosphere. Diamond abrasive grains are embedded in the mold surface at a density of 0.05/μm2. This mold was heated using the same microwave C as in Example 1.
Place it on the mold holder 15 of the VD device. The number of rotations is 1
The speed was set to 1 rotation per minute. Next, the degree of vacuum in the vacuum chamber 11 is set to 2.
Pull up to X10-3 Torr. C2H50H (total amount 200cc) is vaporized through a bubbler, and gas inlet 1 is
4 to vacuum chamber 11 (flow rate, 2003CCM)
The plunger 17 and sleeve stub 18 were adjusted to generate plasma at the position of the mold. 2.45GH
A film of 10 um was formed by deposition for 1 hour under the conditions of a microwave power of 1000 W, a pressure of 90 Torr, and no mold heating. The mold temperature during film formation was 800°C to 820°C.
真空室11から取りだした多結晶ダイヤモンド膜2をコ
ーティングした型1を実施例1と同じ研磨装置50内の
型ホルダ−52に設置した。研磨装置50を3X10−
3Torrまで排気した後、ガス導入口58からアルゴ
ンガスをIO3CCMの流量で研磨装置50内に導入し
た。平均粒径10μmのダイヤモンド粉末を含んだNi
151及び型ホルダ−52を600rpmで回転させた
。Ni板の表面形状は直径100mm、平板状にした。The mold 1 coated with the polycrystalline diamond film 2 taken out from the vacuum chamber 11 was placed in the mold holder 52 in the same polishing device 50 as in Example 1. The polishing device 50 is 3X10-
After exhausting to 3 Torr, argon gas was introduced into the polishing apparatus 50 from the gas inlet 58 at a flow rate of IO3CCM. Ni containing diamond powder with an average particle size of 10 μm
151 and mold holder 52 were rotated at 600 rpm. The surface shape of the Ni plate was a flat plate with a diameter of 100 mm.
10時間研磨した後平均粒径10LLmのダイヤモンド
粉末を含んだNi板51を平均粒径3μmのダイヤモン
ド粉末を含んだNl板51に変えさらに2時間研磨した
。そして、最終研磨用の平均粒径0.5μmのダイヤモ
ンド粉末を含んだNi板51で更に1時間研磨した。型
表面の粗さはRma x 200人であった。After polishing for 10 hours, the Ni plate 51 containing diamond powder with an average particle size of 10 LLm was replaced with an Nl plate 51 containing diamond powder with an average particle size of 3 μm, and polishing was continued for another 2 hours. Then, polishing was performed for an additional hour using a Ni plate 51 containing diamond powder with an average particle size of 0.5 μm for final polishing. The roughness of the mold surface was Rmax x 200.
型上のダイヤモンド膜のラマンスペクトルを測定すると
、鋭い1333cm−’のピークとブロードな1580
cm−’のピークが観測された。反射電子線回折ではダ
イヤモンドのみが観測された。When we measured the Raman spectrum of the diamond film on the mold, we found a sharp peak at 1333 cm-' and a broad peak at 1580 cm-'.
A peak of cm-' was observed. Only diamond was observed by reflection electron diffraction.
これらの結果より型上の膜は、ダイヤモンドとアモルフ
ァス状炭素からなることが解った。又、膜中の元素分析
では炭素原子以外の元素は見出されなかった。These results revealed that the film on the mold was composed of diamond and amorphous carbon. Further, elemental analysis in the film did not find any elements other than carbon atoms.
次に、この型を用いて実施例1と全く同様に硝材に軟化
点5p=650℃、ガラス転移点Tg二600℃のPS
K2 (ホーヤ製)を用いてガラスレンズのプレス成形
を行った。Next, using this mold, in exactly the same manner as in Example 1, a glass material was coated with PS having a softening point of 5p = 650°C and a glass transition point of Tg of 2600°C.
A glass lens was press-molded using K2 (manufactured by Hoya).
このようにして連続5000回の成形を行ない100回
毎に100個のガラス板をサンプリングして表面粗さを
測定したところ、5000回目の表面粗さの平均はRm
ax250μmであった。When molding was performed 5000 times in a row in this way and the surface roughness was measured by sampling 100 glass plates every 100 times, the average surface roughness at the 5000th time was Rm
The ax was 250 μm.
〈実施例4〉
WC90%、Co10%からなる直径40mm、平板の
型に平均粒径1μmのダイヤモンド砥粒を含んだエタノ
ール溶液中で20時間超音波洗浄した。この時用いたダ
イヤモンド砥粒の形状は球状ではなく多面体である。こ
の型を実施例1と同じマイクロ波CVD装置の型ホルダ
−15上に設置する。回転数は、1分間1回転にした。<Example 4> A flat plate mold with a diameter of 40 mm and made of 90% WC and 10% Co was ultrasonically cleaned for 20 hours in an ethanol solution containing diamond abrasive grains with an average grain size of 1 μm. The shape of the diamond abrasive grains used at this time was not spherical but polyhedral. This mold is placed on the mold holder 15 of the same microwave CVD apparatus as in Example 1. The rotation speed was 1 rotation per minute.
次に、真空室11内の真空度を2X10−”Torrま
で引上げる。アセトン(総量300cc)をバブラーを
通して気化し、ガス導入口14より真空室11に水素ガ
ス(流量、200SCCM)と共に導入し、プランジャ
ー17、スリースタブ18を調節して型の位置にプラズ
マを生成した。Next, the degree of vacuum in the vacuum chamber 11 is raised to 2X10-'' Torr. Acetone (total amount 300 cc) is vaporized through a bubbler and introduced into the vacuum chamber 11 from the gas inlet 14 together with hydrogen gas (flow rate, 200 SCCM). Plasma was generated at the position of the mold by adjusting the plunger 17 and sleeve stub 18.
2.45GHzのマイクロ、f1出力800W、圧力1
00Torr、型加熱なしの条件下、1時間の堆積で1
0μmの膜が形成された。成膜中の型温度は800℃〜
820℃であった。2.45GHz micro, f1 output 800W, pressure 1
1 after 1 hour of deposition at 00 Torr and without mold heating.
A film of 0 μm was formed. Mold temperature during film formation is 800℃~
The temperature was 820°C.
真空室11から取りだした多結晶ダイヤモンド膜2をコ
ートした型1を実施例1と同じ研磨装置50内の型ホル
ダ−52に設置した。研磨装置50内を3×10弓To
rrまで排気した後、ガス導入口58から水素ガスをI
O3CCMの流量で研磨装置50内に導入した。平均粒
径ioμmのダイヤモンド粉末を含んだCO板51及び
型ホルダ−52を600rpmで回転させた。Co板の
表面形状は直径100mm、平板状にした。The mold 1 coated with the polycrystalline diamond film 2 taken out from the vacuum chamber 11 was placed in the mold holder 52 in the same polishing device 50 as in Example 1. 3×10 bows inside the polishing device 50
After exhausting to rr, hydrogen gas is introduced from the gas inlet 58 to I
The flow rate of O3CCM was introduced into the polishing apparatus 50. The CO plate 51 and mold holder 52 containing diamond powder with an average particle diameter of io μm were rotated at 600 rpm. The surface shape of the Co plate was a flat plate with a diameter of 100 mm.
10時間研磨した後平均粒径10LLmのダイヤモンド
粉末を含んだCo板51を平均粒径3μmのダイヤモン
ド粉末を含んだCO板51に変えさらに2時間研磨した
。そして、最終研磨用の平均粒径05μmのダイヤモン
ド粉末を含んだCO板51で更に1時間研磨した。型表
面の粗さはRmax200人であった。After polishing for 10 hours, the Co plate 51 containing diamond powder with an average particle size of 10 LLm was replaced with a CO plate 51 containing diamond powder with an average particle size of 3 μm, and polishing was continued for another 2 hours. Then, polishing was performed for an additional hour using a CO plate 51 containing diamond powder with an average particle size of 05 μm for final polishing. The roughness of the mold surface was Rmax 200.
型上のダイヤモンド膜のラマンスペクトルを測定すると
、鋭い1333cm−’のピークとブロードな1580
cm−’のピークが観測された。反射電子線回折ではダ
イヤモンドのみが観測された。When we measured the Raman spectrum of the diamond film on the mold, we found a sharp peak at 1333 cm-' and a broad peak at 1580 cm-'.
A peak of cm-' was observed. Only diamond was observed by reflection electron diffraction.
これらの結果より型上の膜は、ダイヤモンドとアモルフ
ァス状炭素からなることが解った。又、膜中の元素分析
では炭素原子以外の元素は見出されなかった。These results revealed that the film on the mold was composed of diamond and amorphous carbon. Further, elemental analysis in the film did not find any elements other than carbon atoms.
次に、この型を用いて実施例1と全く同様に硝材に軟化
点5p=490℃、ガラス転移点Tg=465℃のFS
X2 (ホーヤ製)を用いてガラスレンズのプレス成形
を行った。Next, using this mold, in exactly the same manner as in Example 1, FS with a softening point of 5p = 490°C and a glass transition point of Tg = 465°C was applied to the glass material.
A glass lens was press-molded using X2 (manufactured by Hoya).
このようにして連続5000回の成形を行ない100回
毎に100個のガラス板をサンプリングして表面粗さを
測定したところ、5000回目の表面粗さの平均はRm
ax240μmであった。When molding was performed 5000 times in a row in this way and the surface roughness was measured by sampling 100 glass plates every 100 times, the average surface roughness at the 5000th time was Rm
The ax was 240 μm.
〈実施例5〉
アルミナからなる直径25mm、曲率半径45mmの凸
状の型を平均粒径1μmのダイヤモンド砥粒を含むエタ
ノール中で20時間超音波処理したのち、エタノール、
アセトン中でこの順番に10分ずつ超音波洗浄し大気中
で十分乾燥させる。この型を公知の直tLCV D装置
の型ホルダ−15上に設置する。<Example 5> A convex mold made of alumina with a diameter of 25 mm and a radius of curvature of 45 mm was subjected to ultrasonic treatment for 20 hours in ethanol containing diamond abrasive grains with an average particle size of 1 μm.
Ultrasonic cleaning was performed in acetone for 10 minutes each in this order, and then thoroughly dried in the air. This mold is placed on the mold holder 15 of a known direct LCV D apparatus.
次に、真空室11内の真空度を2xio−”r。Next, the degree of vacuum in the vacuum chamber 11 is set to 2xio-"r.
rrまで引上げる。エチルエーテル(総量250CC)
をバブラーを通して気化し、ガス導入口14より真空室
11に水素ガス(流量、200SCCM)と共に導入し
、直流3000V、電極間距離15mm、圧力]00T
orr、型加執なしの条件下、1時間の堆積で9μmの
膜か形成された。成膜中の型温度は820℃〜840℃
であった。Pull up to rr. Ethyl ether (total amount 250CC)
was vaporized through a bubbler and introduced into the vacuum chamber 11 from the gas inlet 14 along with hydrogen gas (flow rate, 200 SCCM), DC 3000 V, electrode distance 15 mm, pressure] 00 T.
orr, a 9 μm film was formed in 1 hour of deposition under conditions without mold addition. Mold temperature during film formation is 820℃~840℃
Met.
真空室11から取りだした多結晶ダイヤモンド膜2をコ
ートした型1を実施例1と同じ研磨装置50内の型ホル
ダ−52に設置した。研磨装置50内を3X10−”T
orrまで排気した後、ガス導入口58から水Tガスを
10 S CCMの流量で研磨装置50内に導入した。The mold 1 coated with the polycrystalline diamond film 2 taken out from the vacuum chamber 11 was placed in the mold holder 52 in the same polishing device 50 as in Example 1. 3X10-”T inside the polishing device 50
After exhausting the atmosphere to a level of 0.03 m, water T gas was introduced into the polishing apparatus 50 from the gas inlet 58 at a flow rate of 10 S CCM.
平均粒径10umのダイヤモンド粉末を含んだFe板5
1及び型ホルダ−52を60Orpmで回転させた。F
e扱の表面形状は直径70mmの凹状にした。10時間
研磨した後平均粒径10umのダイヤモンド粉末を含ん
だFe板51を平均粒径3μmのダイヤモンド粉末を含
んだFe板51に変えさらに2時間研磨した。そして、
R終研磨用の平均粒径0.5μmのダイヤモンド粉末を
含んだFe板51で更に1時間′6升磨した。型表面の
粗さはRmax220人であった。Fe plate 5 containing diamond powder with an average particle size of 10 um
1 and mold holder 52 were rotated at 60 rpm. F
The surface shape of the e-treated material was a concave shape with a diameter of 70 mm. After polishing for 10 hours, the Fe plate 51 containing diamond powder with an average particle size of 10 μm was replaced with an Fe plate 51 containing diamond powder with an average particle size of 3 μm, and polishing was continued for another 2 hours. and,
Polishing was further performed for 1 hour using an Fe plate 51 containing diamond powder with an average particle size of 0.5 μm for R final polishing. The roughness of the mold surface was Rmax 220.
型上のダイヤモンド膜のラマンスペクトルを測定すると
、鋭い1333cm−’のピークとブロードな1580
cm−’のピークが観測された。反射電子線回折ではダ
イヤモンドのみが観測された。When we measured the Raman spectrum of the diamond film on the mold, we found a sharp peak at 1333 cm-' and a broad peak at 1580 cm-'.
A peak of cm-' was observed. Only diamond was observed by reflection electron diffraction.
これらの結果より型上の膜は、ダイヤモンドとアモルフ
ァス状炭素からなることが解った。又、膜中の元素分析
では炭素原子以外の元素は見出されなかった。These results revealed that the film on the mold was composed of diamond and amorphous carbon. Further, elemental analysis in the film did not find any elements other than carbon atoms.
次に、この型を用いて実施例1と全く同様に硝材に軟化
点5p=630″C,ガラス転移点Tg=565℃のB
K7 (ホーヤ製)を用いてガラスレンズのプレス成形
を行った。Next, using this mold, in exactly the same manner as in Example 1, a glass material with a softening point of 5p=630''C and a glass transition point of Tg=565°C was prepared.
A glass lens was press-molded using K7 (manufactured by Hoya).
このようにして連続5000回の成形を行ない100回
毎に100個のガラスレンズをサンプリングして表面粗
さを測定したところ、5000回目の表面粗さの平均は
Rmax255μmであった。In this way, molding was performed 5000 times in a row, and 100 glass lenses were sampled every 100 times to measure the surface roughness, and the average surface roughness at the 5000th time was Rmax 255 μm.
〈実施例6〉
S、O2からなる直径35mm、曲率半径45mmの凸
状の型をエタノール、アセトン中でこの順番に10分ず
つ超音波洗浄し大気中で十分乾燥させる。 この型には
平均粒径200人のダイヤモンド粉末が密度10/μm
3で含まれている。<Example 6> A convex mold made of S and O2 and having a diameter of 35 mm and a radius of curvature of 45 mm was ultrasonically cleaned in ethanol and acetone for 10 minutes each in this order and thoroughly dried in the atmosphere. This mold contains diamond powder with an average particle size of 200 and a density of 10/μm.
Included in 3.
この型を公知の13.65MHzの高周波CVD装置の
型ホルダ−15上に設置する。次に、真空室11の真空
度を2xlO−3Torrまで引上げる。アセトアルデ
ヒド(総量200cc)をバブラーを通して気化し、ガ
ス導入口14より真空室11に水素ガス(流量、200
3CCM)と共に導入し、高周波出力800W、電極間
距離15mm、圧力30Torr、型加熱なしの条件下
、1時間の堆積で8μmの膜が形成された6成膜中の型
温度は850℃〜870°Cであった。This mold is placed on a mold holder 15 of a known 13.65 MHz high frequency CVD apparatus. Next, the degree of vacuum in the vacuum chamber 11 is raised to 2xlO-3 Torr. Acetaldehyde (total amount 200 cc) is vaporized through a bubbler, and hydrogen gas (flow rate, 200 cc) is introduced into the vacuum chamber 11 from the gas inlet 14.
A film of 8 μm was formed in 1 hour of deposition under conditions of high frequency output of 800 W, electrode distance of 15 mm, pressure of 30 Torr, and no mold heating. 6 The mold temperature during film formation was 850°C to 870°. It was C.
真空室11から取りだした多結晶ダイヤモンド膜2をコ
ートした型1を実施例1の研磨装置50の真空室を除い
た装置の型ホルダ−52に設置した。平均粒径10μm
のダイヤモンド粉末を含んだ水溶液をFe板51上に流
しながらFe板51及び型ホルダ−52を600 r
pmで回転させた。Fe板の表面形状は直径90mm、
曲率半径45mmの凹状にした。10時間研磨した後平
均粒径10μmのダイヤモンド粉末を含んだFe板を平
均粒径3μmのダイヤモンド粉末を含んだFe板に変え
さらに2時間研磨した。そして、最終研磨用の平均粒径
0.5μmのダイヤモンド粉末を含んだ水溶液をFe板
51上に流しながら、更に1時間研磨した。型表面の粗
さはRmax280人であった。The mold 1 coated with the polycrystalline diamond film 2 taken out from the vacuum chamber 11 was placed in the mold holder 52 of the polishing apparatus 50 of Example 1 except for the vacuum chamber. Average particle size 10μm
While pouring an aqueous solution containing diamond powder onto the Fe plate 51, the Fe plate 51 and mold holder 52 were heated at 600 r.
Rotated at pm. The surface shape of the Fe plate is 90 mm in diameter,
It was made into a concave shape with a radius of curvature of 45 mm. After polishing for 10 hours, the Fe plate containing diamond powder with an average particle size of 10 μm was replaced with an Fe plate containing diamond powder with an average particle size of 3 μm, and polishing was continued for another 2 hours. Then, while flowing an aqueous solution containing diamond powder with an average particle size of 0.5 μm for final polishing onto the Fe plate 51, polishing was further performed for 1 hour. The roughness of the mold surface was Rmax 280.
型上のダイヤモンド膜のラマンスペクトルを測定すると
、鋭い1333cm−’のピークとブロードな1580
cm−’のピークが観測された。反射電子線回折ではダ
イヤモンドのみが観測された。When we measured the Raman spectrum of the diamond film on the mold, we found a sharp peak at 1333 cm-' and a broad peak at 1580 cm-'.
A peak of cm-' was observed. Only diamond was observed by reflection electron diffraction.
これらの結果より型上の膜は、ダイヤモンドとアモルフ
ァス状炭素からなることが解った。又、膜中の元素分析
では炭素原子以外の元素は見出されなかった。These results revealed that the film on the mold was composed of diamond and amorphous carbon. Further, elemental analysis in the film did not find any elements other than carbon atoms.
次に、この型を用いて実施例1と全く同様に硝材に軟化
点5p=595℃、ガラス転移点Tg=525℃のに7
(ホーヤ製)を用いてガラスレンズのプレス成形を行っ
た。Next, using this mold, a glass material with a softening point of 5p=595°C and a glass transition point of Tg=525°C was prepared in the same manner as in Example 1.
(manufactured by Hoya) to press mold a glass lens.
このようにして連続5000回の成形を行ない100回
毎に100個のガラスレンズをサンプリングして表面粗
さを測定したところ、5000回目の表面粗さの平均は
Rmax300μmであった。In this way, molding was performed 5000 times in a row, and 100 glass lenses were sampled every 100 times to measure the surface roughness, and the average surface roughness at the 5000th time was Rmax 300 μm.
〈実施例7〉
Z r Ozからなる直径35mm、曲率半径45mm
の凹上の型をイオンビーム装置に投石し、加速電圧10
00VのArイオンビームでダイヤモンド多結晶体のタ
ーゲットを20時間スパッタし、Z r OR型表面に
ダイヤモンドクラスターを埋め込んだ後、公知の13.
65MHzの高周波CVD装置の型ホルダ−15上に設
置する。次に、真空室11内の真空度を2X10−”T
orrまで引上げる。酢酸(総量200cc)をバブラ
ーを通して気化し、ガス導入口14より真空室11に水
素ガス(流量、200SCCM)と共に導入し、高周波
出力900W、電極間距離15mm、圧力30Torr
、型加熱なしの条件下、1M間の堆積で5μmの膜が形
成された。成膜中の型温度は840℃〜860℃であっ
た。<Example 7> Made of Z r Oz, diameter 35 mm, radius of curvature 45 mm
A concave mold is thrown into an ion beam device, and an acceleration voltage of 10
After sputtering a polycrystalline diamond target for 20 hours with a 00V Ar ion beam and embedding diamond clusters in the Z r OR type surface, the well-known method 13.
It is installed on the mold holder 15 of a 65 MHz high frequency CVD device. Next, the degree of vacuum in the vacuum chamber 11 is set to 2X10-”T.
Raise it to orr. Acetic acid (total amount 200 cc) was vaporized through a bubbler and introduced into the vacuum chamber 11 from the gas inlet 14 along with hydrogen gas (flow rate, 200 SCCM), high frequency output 900 W, interelectrode distance 15 mm, pressure 30 Torr.
, a 5 μm film was formed by deposition for 1M under conditions without mold heating. The mold temperature during film formation was 840°C to 860°C.
真空室11から取りだした多結晶ダイヤモンド膜2をコ
ートした型1を実施例6と同じ装置の型ホルダ−52に
設置した。平均粒径10μmのダイヤモンド粉末を含ん
だ研磨油液を銅板51上に流しながら銅板51及び型ホ
ルダ−52を60Orpmで回転させた。銅板の表面形
状は直径90mm、曲率半径45mmの凸状にした。1
0時間研磨した後平均粒径10μmのダイヤモンド粉末
を含んだ銅板を平均粒径3μmのダイヤモンド粉末を含
んだ銅板に変えさらに2時間研磨した。そして、最終研
磨用の平均粒径0.5μmのダイヤモンド粉末を含んだ
研磨油液を銅板51上に流しながら更に1時間研磨した
。型表面の粗さはRmax250人であった。The mold 1 coated with the polycrystalline diamond film 2 taken out from the vacuum chamber 11 was placed in the mold holder 52 of the same device as in Example 6. The copper plate 51 and mold holder 52 were rotated at 60 rpm while flowing a polishing oil containing diamond powder with an average particle size of 10 μm onto the copper plate 51. The surface shape of the copper plate was a convex shape with a diameter of 90 mm and a radius of curvature of 45 mm. 1
After polishing for 0 hours, the copper plate containing diamond powder with an average particle size of 10 μm was replaced with a copper plate containing diamond powder with an average particle size of 3 μm, and polishing was continued for another 2 hours. Then, the copper plate 51 was polished for another hour while a polishing oil containing diamond powder having an average particle size of 0.5 μm for final polishing was poured onto the copper plate 51. The roughness of the mold surface was Rmax 250.
型上のダイヤモンド膜のラマンスペクトルを測定すると
、鋭い1333cm−’のピークとブロードな1580
cm−’のピークが観測された。反射電子線回折ではダ
イヤモンドのみが観測された。When we measured the Raman spectrum of the diamond film on the mold, we found a sharp peak at 1333 cm-' and a broad peak at 1580 cm-'.
A peak of cm-' was observed. Only diamond was observed by reflection electron diffraction.
これらの結果より型上の膜は、ダイヤモンドとアモルフ
ァス状炭素からなることが解った。又、膜中の元素分析
では炭素原子以外の元素は見出されなかった。These results revealed that the film on the mold was composed of diamond and amorphous carbon. Further, elemental analysis in the film did not find any elements other than carbon atoms.
次に、この型を用いて実施例1と全く同様に硝材に軟化
点5p=700℃、ガラス転移点Tg=655℃のSK
5 (ホーヤ製)を用いてガラスレンズのプレス成形を
行った。Next, using this mold, in exactly the same manner as in Example 1, SK with a softening point of 5p = 700°C and a glass transition point of Tg = 655°C was prepared.
5 (manufactured by Hoya) to press mold a glass lens.
このようにして連続5000回の成形を行ない100回
毎に100個のガラスレンズをサンプリングして表面粗
さを測定したところ、5000回目の表面粗さの平均は
Rmax270人であった。Molding was performed 5,000 times in a row in this manner, and 100 glass lenses were sampled every 100 times to measure the surface roughness, and the average surface roughness at the 5,000th time was Rmax 270.
〈比較例4〉
実施例7でZrO□型上にダイヤモンド多結晶体ターゲ
ットをスパッタする時間を30分にしたほかは実施例7
と同様にして型を作成した。真空室11から型を取りだ
すとダイヤモンド膜が型から浮きあっがでいる部分が2
か所あったので成形は行なわなかった。<Comparative Example 4> Example 7 except that the sputtering time of the diamond polycrystalline target on the ZrO□ type was changed to 30 minutes.
A mold was created in the same way. When the mold is removed from the vacuum chamber 11, the part where the diamond film is lifted from the mold is 2.
Since there were some spots, no molding was performed.
〈実施例8〉
TaCからなる直径35mm、曲率半径45mmの凹状
の型をイオンビーム装置に設置し、加速電圧1000■
のArイオンビームでダイヤモンド多結晶体のターゲッ
トを20時間スパッタし、TaC型表面にダイヤモンド
クラスターを埋め込んだ後、公知の熱フィラメント法装
置の型ホルダ−15上に設置する。次に、真空室11内
の真空度を2X10−”Torrまで引上げる。水素、
メタンをそれぞれ200.0.5SCCMの流量、ガス
導入口14より真空室+1に導入し、フィラメント温度
2100℃、電極間距離15mm、圧力30Torrの
条件下、5時間の堆積で4μmの膜が形成された。成膜
中の型iFA度は840”C〜860℃であった。<Example 8> A concave mold made of TaC with a diameter of 35 mm and a radius of curvature of 45 mm was installed in an ion beam device, and an accelerating voltage of 1000 mm was installed.
A polycrystalline diamond target was sputtered for 20 hours using an Ar ion beam to embed diamond clusters in the surface of the TaC mold, and then placed on a mold holder 15 of a known hot filament method apparatus. Next, the degree of vacuum in the vacuum chamber 11 is raised to 2×10-” Torr.Hydrogen,
Methane was introduced into the vacuum chamber +1 through the gas inlet 14 at a flow rate of 200.0.5 SCCM, and a 4 μm film was formed in 5 hours of deposition under conditions of filament temperature of 2100°C, interelectrode distance of 15 mm, and pressure of 30 Torr. Ta. The type iFA degree during film formation was 840''C to 860C.
真空室11から取りだした多結晶ダイヤモンド膜2をコ
ートした型1を実施例1と同じ研磨装置50内の型ホル
ダ−52に設置した。研磨装置50を3XIO−3To
rrまで排気した後、ガス導入口58から水素ガスを1
1005CCの流量で研磨装置50内に導入した。平均
粒径10μmのダイヤモンド粉末を含んだCo板51及
び型ホルダ−52を600rpmで回転させた。この時
ヒーター59.60を用いCo扱を900℃に加熱した
。Co板の表面形状は直径80mm、曲率半径45mm
の5平板状にした。5時間研磨した後平均粒径lOμm
のダイヤモンド粉末を含んたCo板51を平均粒径3μ
mのダイヤモンド粉末を含んだCO板51に変えさらに
05時間研磨した。そして、最終研磨用の平均粒径0.
5μmのダイヤモンド粉末を含んだCo板51で更に0
.5時間研磨した。型表面の粗さはRmax180人で
あった。The mold 1 coated with the polycrystalline diamond film 2 taken out from the vacuum chamber 11 was placed in the mold holder 52 in the same polishing device 50 as in Example 1. The polishing device 50 is 3XIO-3To
After exhausting to rr, 1 hydrogen gas is introduced from the gas inlet 58.
It was introduced into the polishing apparatus 50 at a flow rate of 1005 cc. The Co plate 51 containing diamond powder with an average particle size of 10 μm and the mold holder 52 were rotated at 600 rpm. At this time, the Co treatment was heated to 900° C. using a heater 59.60. The surface shape of the Co plate is 80 mm in diameter and 45 mm in radius of curvature.
5 flat plate shape. Average grain size after polishing for 5 hours: 10 μm
Co plate 51 containing diamond powder with an average particle size of 3μ
The plate was replaced with a CO plate 51 containing diamond powder of m and polished for an additional 0.5 hours. Then, the average particle size for final polishing is 0.
Furthermore, the Co plate 51 containing 5 μm diamond powder
.. Polished for 5 hours. The roughness of the mold surface was Rmax 180.
型上のダイヤモンド膜のラマンスペクトルを測定すると
、鋭い1333cm−’のピークとプロトな1580c
m−’のピークが観測された。反射電子線回折ではダイ
ヤモンドのみが観測された。When we measured the Raman spectrum of the diamond film on the mold, we found a sharp peak at 1333cm-' and a proto-1580c peak.
A peak of m-' was observed. Only diamond was observed by reflection electron diffraction.
これらの結果より型上の膜は、ダイヤモンドとアモルフ
ァス状炭素からなることが解った。又、膜中の元素分析
では炭素原子以外の元素は見出されなかった。These results revealed that the film on the mold was composed of diamond and amorphous carbon. Further, elemental analysis in the film did not find any elements other than carbon atoms.
次に、この型を用いて実施例1と全(同様に硝材に軟化
点5p=680℃、ガラス転移点Tg=640’CのL
aF2O(ホーヤ製)を用いてガラスレンズのプレス成
形を行った。Next, using this mold, we applied a glass material to L having a softening point of 5p = 680°C and a glass transition point of Tg = 640'C.
A glass lens was press-molded using aF2O (manufactured by Hoya).
このようにして連続5000回の成形を行ない100回
毎に100個のガラスレンズをサンプリングして表面粗
さを測定したところ、5000回目の表面粗さの平均は
Rmax200μmであった。In this way, molding was performed 5000 times in a row, and 100 glass lenses were sampled every 100 times to measure the surface roughness, and the average surface roughness at the 5000th time was Rmax 200 μm.
〈実施例9〉
サーメットからなる直径5mmの平板の型をイオンビー
ム装置に設置し、加速電圧1000VのArイオンビー
ムでダイヤモンド多結晶体のターゲットを20時間スパ
ッタし、サーメット型表面にダイヤモンドクラスターを
埋め込んだ後、公知の電子アシストプラズマ装置の型ボ
ルダ−15上に設置する。次に、真空室11内の真空度
を2×10−”Torrまで引上げる。<Example 9> A flat plate mold made of cermet with a diameter of 5 mm was placed in an ion beam device, and a polycrystalline diamond target was sputtered for 20 hours using an Ar ion beam with an acceleration voltage of 1000 V to embed diamond clusters on the surface of the cermet mold. After that, it is placed on a mold boulder 15 of a known electronically assisted plasma device. Next, the degree of vacuum in the vacuum chamber 11 is raised to 2×10 −” Torr.
アダマンクンを加熱昇華し、ガス導入口14より真空室
11に導入する。流量2003CCMで水素を流し、フ
ィラメント温度2100″C,電極間距離15mm、基
板バイアス−200V、圧力130Torrの条件下、
1時間の堆積で14μmの膜が形成された。成膜中の型
温度は900℃〜910℃であった。Adamanthus is sublimated by heating and introduced into the vacuum chamber 11 through the gas inlet 14. Hydrogen was flowed at a flow rate of 2003 CCM, the filament temperature was 2100''C, the distance between the electrodes was 15 mm, the substrate bias was -200 V, and the pressure was 130 Torr.
A 14 μm film was formed after 1 hour of deposition. The mold temperature during film formation was 900°C to 910°C.
真空室11から取りだした多結晶ダイヤモンド膜2をコ
ートした型1を実施例1と同じ研磨装置50内の型ホル
ダ−52に設置した。研磨装置50内を3X10−3T
orrまで排気した後、ガス導入口58から水素ガスを
11005ccの流量で研磨装置50内に導入した。平
均粒径10μmのダイヤモンド粉末を含んだFe板51
及び型ホルダ−52を600rpmで回転させた。The mold 1 coated with the polycrystalline diamond film 2 taken out from the vacuum chamber 11 was placed in the mold holder 52 in the same polishing device 50 as in Example 1. 3X10-3T inside the polishing device 50
After exhausting the atmosphere to 11005 cc, hydrogen gas was introduced into the polishing apparatus 50 from the gas inlet 58 at a flow rate of 11005 cc. Fe plate 51 containing diamond powder with an average particle size of 10 μm
And the mold holder 52 was rotated at 600 rpm.
この時ヒーター59.60を用いFe板51を950℃
に加熱した。Fe板の表面形状は直径80mmの平板状
にした。5時間研磨した後平均粒径10μmのダイヤモ
ンド粉末を含んだFe板51を平均粒径3μmのダイヤ
モンド粉末を含んだFe板51に変えさらに2時間研磨
した。そし。At this time, the Fe plate 51 was heated to 950°C using a heater 59.60.
heated to. The surface shape of the Fe plate was a flat plate with a diameter of 80 mm. After polishing for 5 hours, the Fe plate 51 containing diamond powder with an average particle size of 10 μm was replaced with an Fe plate 51 containing diamond powder with an average particle size of 3 μm, and polishing was continued for another 2 hours. stop.
て、最終研磨用の平均粒径05μmのダイヤモンド粉末
を含んだFe板51で更に1時間研磨した。型表面の粗
さはRmax 190人であった。Then, polishing was performed for an additional hour using an Fe plate 51 containing diamond powder with an average particle size of 05 μm for final polishing. The roughness of the mold surface was Rmax 190.
型上のダイヤモンド膜のラマンスペクトルを測定すると
、鋭い1333cm−’のピークとブロードな1580
cm−’のピークが観1Illjされた。反射電子線回
折ではダイヤモンドのみがし測された。When we measured the Raman spectrum of the diamond film on the mold, we found a sharp peak at 1333 cm-' and a broad peak at 1580 cm-'.
A peak at cm-' was observed. Only diamonds were detected by reflection electron diffraction.
これらの結果より型上の膜は、ダイヤモンドとアモルフ
ァス状炭素からなることが解った。又、膜中の元素分析
では炭素原子以外の元素は見出されなかった。These results revealed that the film on the mold was composed of diamond and amorphous carbon. Further, elemental analysis in the film did not find any elements other than carbon atoms.
次に、この型を用いて実施例1と全く同様に硝材に軟化
点5p=470℃、ガラス転移点Tg420”CのKF
6 (ホーヤ製)を用いてガラスレンズのプレス成形を
行った。Next, using this mold, in exactly the same manner as in Example 1, KF having a softening point of 5p=470°C and a glass transition point of Tg of 420"C was prepared.
6 (manufactured by Hoya) to press mold a glass lens.
このようにして連続5000回の成形を行ない100回
毎に100個のガラスレンズをサンプリングして表面粗
さを測定したところ、5000回目の表面粗さの平均は
Rmax215μmであった。In this way, molding was performed 5000 times in a row, and 100 glass lenses were sampled every 100 times to measure the surface roughness, and the average surface roughness at the 5000th time was Rmax 215 μm.
〈実施例10>
SiCm結体からなる直径5mmの平板の型をイオンビ
ーム装置に設置し、加速電圧1000VのArイオンビ
ームで多結晶ダイヤモンドのターゲットを20時間スパ
ッタし、SiC型表面にダイヤモンドクラスターを埋め
込んだ後、この型を公知の電子アシストプラズマ装置の
型ホルダ−15上に設置する。次に、真空室11内の真
空度を2X10−’Torrまで引上げる。<Example 10> A flat plate mold with a diameter of 5 mm made of SiCm solids was placed in an ion beam device, and a polycrystalline diamond target was sputtered for 20 hours using an Ar ion beam with an acceleration voltage of 1000 V to form diamond clusters on the surface of the SiC mold. After embedding, the mold is placed on a mold holder 15 of a known electronically assisted plasma device. Next, the degree of vacuum in the vacuum chamber 11 is raised to 2×10 −′ Torr.
アダマンタンを加熱昇華し、ガス導入口14より真空室
11に導入する。流量200 S CCMで水素を流し
、フィラメント温度2100℃、電極間距離15mm、
基板バイアス−200V、圧力130Torrの条件下
、1時間の堆積で14μmの膜が形成された。成膜中の
型温度は900℃〜910℃であった。Adamantane is sublimated by heating and introduced into the vacuum chamber 11 through the gas inlet 14. Hydrogen was flowed at a flow rate of 200 S CCM, the filament temperature was 2100°C, the distance between the electrodes was 15 mm,
A 14 μm film was formed by deposition for 1 hour under conditions of a substrate bias of −200 V and a pressure of 130 Torr. The mold temperature during film formation was 900°C to 910°C.
真空室11から取りだした多結晶ダイヤモンド膜2をコ
ートした型lを実施例1と同じ研磨装置50内の型ホル
ダ−52に設置した。研磨装置50内を3xlO−”T
orrまで排気した後、ガス導入口58から水素ガスを
11005ccの流量で研磨装置50内に導入した。平
均粒(710g mのダイヤモンド粉末を含んだFe板
51及び型ホルダ−52を600rpmで回転させた。The mold 1 coated with the polycrystalline diamond film 2 taken out from the vacuum chamber 11 was placed in the mold holder 52 in the same polishing device 50 as in Example 1. 3xlO-”T inside the polishing device 50
After exhausting the atmosphere to 11005 cc, hydrogen gas was introduced into the polishing apparatus 50 from the gas inlet 58 at a flow rate of 11005 cc. The Fe plate 51 and mold holder 52 containing average grains (710 g m of diamond powder) were rotated at 600 rpm.
この時ヒーター59,60を用いFe板51を950℃
に加熱した。Fe板の表面形状は直径80mmの平板状
にした。5時間研磨した後平均粒径10μmのダイヤモ
ンド粉末を含んだFe板51を平均粒径3μmのダイヤ
モンド粉末を含んだFe板51に変えさらに2時間研磨
した。そして、最終研磨用の平均粒径0.5μmのダイ
ヤモンド粉末を含んだFe板51で更に1時間研磨した
。型表面の粗さはRmax190人であった。At this time, heaters 59 and 60 are used to heat the Fe plate 51 to 950°C.
heated to. The surface shape of the Fe plate was a flat plate with a diameter of 80 mm. After polishing for 5 hours, the Fe plate 51 containing diamond powder with an average particle size of 10 μm was replaced with an Fe plate 51 containing diamond powder with an average particle size of 3 μm, and polishing was continued for another 2 hours. Then, polishing was performed for an additional hour using an Fe plate 51 containing diamond powder with an average particle size of 0.5 μm for final polishing. The roughness of the mold surface was Rmax 190.
型上のダイヤモンド膜のラマンスペクトルを泪1;定す
ると、鋭い1333cm−’のピークとプロトな158
0cm−’のピークが観測された。反射電子線回折では
ダイヤモンドのみがEイリ(;された。The Raman spectrum of the diamond film on the mold is determined to have a sharp peak at 1333 cm-' and a proto-158 cm peak.
A peak at 0 cm-' was observed. In backscattered electron diffraction, only diamond was E-irradiated.
これらの結果より型上の膜は、ダイヤモンドとアモルフ
ァス状炭素からなることが解った。又、膜中の元素分析
では炭素原子以外の元素は見出きれなかった。These results revealed that the film on the mold was composed of diamond and amorphous carbon. Furthermore, elemental analysis in the film did not reveal any elements other than carbon atoms.
次に、この型を用いて実施例1と全く同様に硝材に軟化
点5p=470℃、ガラス転移点Tg=420℃のKF
6を用いてガラスレンズのプレス成形を行った。Next, using this mold, in exactly the same manner as in Example 1, KF having a softening point of 5p = 470°C and a glass transition point of Tg = 420°C was applied to the glass material.
A glass lens was press-molded using No. 6.
このようにして連続5000回の成形を行ない100回
毎に100個のガラスレンズをサンプリングして表面粗
さを測定したところ、5000回目の表面粗さの平均は
Rmax215μmであった。In this way, molding was performed 5000 times in a row, and 100 glass lenses were sampled every 100 times to measure the surface roughness, and the average surface roughness at the 5000th time was Rmax 215 μm.
〈実施例11〉
WC填結体からなる直径5mmの平板の型をイオンビー
ム装置に設置し、加速電圧1000VのArイオンビー
ムで多結晶ダイヤモンドのタゲットを20時間スパッタ
し、WC型表面にダイヤモンドクラスターを埋め込んだ
後、この型を公知の熱フィラメント装置の型ホルダ−1
5上に設置する。次に、真空室11内の真空度を2×1
O−3Torrまで引上げる。 ガス導入口14より水
素、メタンをそれぞれ200,0.55CCMの流量で
真空室11に導入する。フィラメント温度2100℃、
電極間距離15mm、圧力130Torrの条件下、1
時間の堆積で10μmの膜が形成された。成膜中の型温
度は880℃〜890℃であった。<Example 11> A flat plate mold with a diameter of 5 mm made of WC packed bodies was placed in an ion beam device, and a polycrystalline diamond target was sputtered for 20 hours using an Ar ion beam with an acceleration voltage of 1000 V to form diamond clusters on the surface of the WC mold. After embedding the mold, the mold is placed in mold holder 1 of a known hot filament device.
5. Install on top. Next, the degree of vacuum in the vacuum chamber 11 is set to 2×1.
Raise the temperature to O-3 Torr. Hydrogen and methane are introduced into the vacuum chamber 11 through the gas inlet 14 at flow rates of 200 and 0.55 CCM, respectively. Filament temperature 2100℃,
Under conditions of 15 mm distance between electrodes and 130 Torr pressure, 1
A 10 μm film was formed with time deposition. The mold temperature during film formation was 880°C to 890°C.
真空室11から取りだした多結晶ダイヤモンド膜2をコ
ートした型1を実施例1と同じ研磨装置50内の型ホル
ダ−52に設置した。研磨装置50内を3X10−”T
orrまで排気した後、ガス導入口58から水素ガスを
11005CCの流量で研磨装置50内に導入した。平
均粒径10μmのダイヤモンド粉末を含んだFe板51
及び型ホルダ−52を600rpmで回転させた。The mold 1 coated with the polycrystalline diamond film 2 taken out from the vacuum chamber 11 was placed in the mold holder 52 in the same polishing device 50 as in Example 1. 3X10-”T inside the polishing device 50
After exhausting the atmosphere to a level of 1000 cc, hydrogen gas was introduced into the polishing apparatus 50 from the gas inlet 58 at a flow rate of 11005 cc. Fe plate 51 containing diamond powder with an average particle size of 10 μm
And the mold holder 52 was rotated at 600 rpm.
この時ヒーター59.60を用いFe板51を950℃
に加熱した。Fe板の表面形状は直径80mmの平板状
にした。5時間研磨した後平均粒径10μmのダイヤモ
ンド粉末を含んだFe板51を平均粒径3μmのダイヤ
モンド粉末を含んだFe板51に変えさらに2時間研磨
した。そして、最終研磨用の平均粒径0.5μmのダイ
ヤモンド粉末を含んだFe板51で更に1時間研磨した
。型表面の事且さはRmax200人であった。At this time, the Fe plate 51 was heated to 950°C using a heater 59.60.
heated to. The surface shape of the Fe plate was a flat plate with a diameter of 80 mm. After polishing for 5 hours, the Fe plate 51 containing diamond powder with an average particle size of 10 μm was replaced with an Fe plate 51 containing diamond powder with an average particle size of 3 μm, and polishing was continued for another 2 hours. Then, polishing was performed for an additional hour using an Fe plate 51 containing diamond powder with an average particle size of 0.5 μm for final polishing. The surface roughness of the mold was Rmax 200 people.
型上のダイヤモンド月0のラマンスペクトルを渭j定す
ると、鋭い1333cm−’のピークとブロードな15
80cm−’のピークが観測された。反射電子線回折で
はダイヤモンドのみが観測された。When we determine the Raman spectrum of the diamond moon 0 on the mold, we find a sharp peak at 1333 cm-' and a broad peak at 15 cm.
A peak at 80 cm-' was observed. Only diamond was observed by reflection electron diffraction.
これらの結果よりを上の膜は、ダイヤモンドとアモルフ
ァス状炭素からなることが解った。又、膜中の元素分析
では炭素原子以外の元素は見比されなかった。These results revealed that the above film was composed of diamond and amorphous carbon. Further, elemental analysis in the film did not reveal any elements other than carbon atoms.
次に、この型を用いて実施例1と全く同様に硝Hに軟化
r!″5p=470°C,ガラス転fg 、#、 ’i
−g420″CのKF6を用いてガラスレンズのプレス
成形を行った。Next, using this mold, soften r! ``5p=470°C, glass rotation fg, #, 'i
- A glass lens was press-molded using KF6 of g420″C.
このようにして連続5000回の成形を行ない100回
毎に100個のガラスレンズをサンプリングして表面粗
さを測定したところ、5000回目の表面粗さの平均は
Rmax220umであった。In this way, molding was performed 5000 times in a row, and 100 glass lenses were sampled every 100 times to measure the surface roughness, and the average surface roughness at the 5000th time was Rmax 220 um.
[発明の効果]
以上説明してきた様にダイヤモンド砥粒を散在させた型
にダイヤモンド膜をコートすることによって得られる本
発明の光学素子形成用型は、ダイヤモンド膜が型表面か
ら剥離することが少なく成形の熱サイクルに対して非常
に安定でありかつ光学素子形成に十分な表面粗さをもち
、多数回の成形にも膜剥れや硬度の低下を伴うことがな
く、光学素子成形用型として十分なものとなった。[Effects of the Invention] As explained above, the mold for forming an optical element of the present invention, which is obtained by coating a diamond film on a mold in which diamond abrasive grains are scattered, has less chance of the diamond film peeling off from the mold surface. It is extremely stable against thermal cycles of molding, has a surface roughness sufficient for forming optical elements, and can be used as a mold for molding optical elements without peeling or decreasing hardness even after multiple moldings. It was enough.
第1図は型表面におけるダイヤモンド粒子の存在形態の
模式図、第2図及び第3図は本発明に関わる光学素子の
成形用型の一態様を示す断面図で、第2図はプレス成形
前の状態、第3図はプレス成形後の状態を示す。第4図
は型母材の表面に多結晶ダイヤモンド膜を被覆するマイ
クロ波CVD法装置である。第5図は研磨装置である。
第6区は光学素子成形用型を使用するレンズの成形装置
を示す断面図である。
1、型の母材 2:被覆材
3ニガラス素材 4・成形されたレンズ12:排
気口
14.ガス導入口
16:導波管
18・スリースタブ
51:金属板
11:真空室
13:型母材
15:型ホルダ
17:ブランジャ
50:研磨装置
52:型ホルダ−
53: 54 :エアベアリング
55 : 56 :モータ
57:排気口
59.60:ヒーター
102:成形装置
104:取入れ用置換室
106:成形室
108:蒸着室
110:取り出し用置換室
112.114.116:ゲートバルブ118:レール
120・パレット122:ロッド 12
4 シリンダ126:バルブ 128:ヒーター
130、上型 132.下型
58 ガス導入口
第
図
図
第3図
134.136:ロッド
138.140ニジリンダ
142:容器
146:蒸着物質
150ニジリンダ
148:ロット
144:ヒーター
152・バルブFIG. 1 is a schematic diagram of the form of diamond particles present on the mold surface, FIGS. 2 and 3 are cross-sectional views showing one embodiment of the mold for molding an optical element related to the present invention, and FIG. 2 is a diagram before press molding. Figure 3 shows the state after press molding. FIG. 4 shows a microwave CVD method apparatus for coating the surface of a mold base material with a polycrystalline diamond film. FIG. 5 shows a polishing device. Section 6 is a sectional view showing a lens molding apparatus using an optical element mold. 1. Base material of the mold 2: Covering material 3 Glass material 4. Molded lens 12: Exhaust port 14. Gas inlet 16: Waveguide 18/Sleeve stub 51: Metal plate 11: Vacuum chamber 13: Mold base material 15: Mold holder 17: Plunger 50: Polishing device 52: Mold holder 53: 54: Air bearing 55: 56 : Motor 57: Exhaust port 59.60: Heater 102: Molding device 104: Intake replacement chamber 106: Molding chamber 108: Deposition chamber 110: Removal replacement chamber 112.114.116: Gate valve 118: Rail 120/Pallet 122 :Rod 12
4 Cylinder 126: Valve 128: Heater 130, upper mold 132. Lower mold 58 Gas inlet Figure 3 Figure 3 134.136: Rod 138.140 Niji cylinder 142: Container 146: Vapor deposition material 150 Niji cylinder 148: Lot 144: Heater 152/Valve
Claims (5)
おいて、型母材の少なくとも成形面にはダイヤモンド結
晶が型母材表面に露出するように埋め込まれており、か
つ該ダイヤモンド結晶が埋め込まれ型母材表面には多結
晶ダイヤモンド膜が被覆されていることを特徴とする、
光学素子成形用型。(1) In a mold used for press molding a glass optical element, diamond crystals are embedded in at least the molding surface of the mold base material so as to be exposed on the surface of the mold base material, and the diamond crystals are embedded in at least the molding surface of the mold base material, and The mold base material surface is coated with a polycrystalline diamond film,
Mold for molding optical elements.
.01/μm^2以上であることを特徴とする、請求項
1記載の光学素子成形用型。(2) The surface density of diamond crystals on the mold base material surface is 0
.. 2. The mold for molding an optical element according to claim 1, wherein the molding die has a diameter of 01/μm^2 or more.
製造方法において、少なくとも成形面にはダイヤモンド
結晶が型母材表面に露出するように埋め込まれている型
母材上に、気相法によって多結晶ダイヤモンド膜を被覆
することを特徴とする、光学素子成形用型の製造方法。(3) In the manufacturing method of a mold used for press molding of glass optical elements, a vapor phase method is used on a mold base material in which diamond crystals are embedded at least on the molding surface so as to be exposed on the mold base material surface. A method for manufacturing a mold for molding an optical element, the method comprising: coating a polycrystalline diamond film with a polycrystalline diamond film.
ラズマCVD法、直流プラズマCVD法、熱フィラメン
ト法または電子アシストプラズマCVD法である、請求
項3記載の光学素子成形用型の製造方法。(4) The method for manufacturing a mold for molding an optical element according to claim 3, wherein the gas phase method is a microwave plasma CVD method, a high-frequency plasma CVD method, a direct current plasma CVD method, a hot filament method, or an electron-assisted plasma CVD method.
.01/μm^2以上であることを特徴とする、請求項
3または4記載の光学素子成形用型の製造方法。(5) The surface density of diamond crystals on the surface of the mold base material is 0.
.. 5. The method for manufacturing a mold for molding an optical element according to claim 3, wherein the molding die is 01/μm^2 or more.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP14162090A JPH0437617A (en) | 1990-06-01 | 1990-06-01 | Optical element forming die and its production |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP14162090A JPH0437617A (en) | 1990-06-01 | 1990-06-01 | Optical element forming die and its production |
Publications (1)
Publication Number | Publication Date |
---|---|
JPH0437617A true JPH0437617A (en) | 1992-02-07 |
Family
ID=15296280
Family Applications (1)
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JP14162090A Pending JPH0437617A (en) | 1990-06-01 | 1990-06-01 | Optical element forming die and its production |
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Country | Link |
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JP (1) | JPH0437617A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2009023132A (en) * | 2007-07-18 | 2009-02-05 | Tomei Diamond Co Ltd | Nano-imprinting stamper, and method for producing the same |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2009023132A (en) * | 2007-07-18 | 2009-02-05 | Tomei Diamond Co Ltd | Nano-imprinting stamper, and method for producing the same |
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