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)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP14162090A Pending JPH0437617A (en) | 1990-06-01 | 1990-06-01 | Optical element forming die and its production |
Country Status (1)
| Country | Link |
|---|---|
| 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 |
-
1990
- 1990-06-01 JP JP14162090A patent/JPH0437617A/en active Pending
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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