JP6840765B2 - 合成により製造された石英ガラスのディフューザー材料及びその全体又は一部を構成する成形体の製造方法 - Google Patents
合成により製造された石英ガラスのディフューザー材料及びその全体又は一部を構成する成形体の製造方法 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims description 98
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims description 85
- 238000000034 method Methods 0.000 title claims description 42
- 230000015572 biosynthetic process Effects 0.000 title claims description 10
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 238000003786 synthesis reaction Methods 0.000 title claims description 9
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- 229910004298 SiO 2 Inorganic materials 0.000 claims description 40
- 238000005245 sintering Methods 0.000 claims description 38
- 239000001257 hydrogen Substances 0.000 claims description 26
- 229910052739 hydrogen Inorganic materials 0.000 claims description 26
- 239000002245 particle Substances 0.000 claims description 25
- 238000010521 absorption reaction Methods 0.000 claims description 22
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 22
- 229910052754 neon Inorganic materials 0.000 claims description 21
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 21
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 20
- 239000007858 starting material Substances 0.000 claims description 20
- 239000002002 slurry Substances 0.000 claims description 17
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
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- 229910052782 aluminium Inorganic materials 0.000 description 3
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- 230000008859 change Effects 0.000 description 3
- 229910052804 chromium Inorganic materials 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
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- 229910052742 iron Inorganic materials 0.000 description 3
- 230000001788 irregular Effects 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 229910052748 manganese Inorganic materials 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
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- 229910052750 molybdenum Inorganic materials 0.000 description 3
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- 229910052708 sodium Inorganic materials 0.000 description 3
- 238000010561 standard procedure Methods 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- 229910052726 zirconium Inorganic materials 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910021486 amorphous silicon dioxide Inorganic materials 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
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- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
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- 239000012634 fragment Substances 0.000 description 2
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- 235000021384 green leafy vegetables Nutrition 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
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- 150000003377 silicon compounds Chemical class 0.000 description 2
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- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
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- 241000282341 Mustela putorius furo Species 0.000 description 1
- 238000003841 Raman measurement Methods 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 229910003902 SiCl 4 Inorganic materials 0.000 description 1
- 101710137710 Thioesterase 1/protease 1/lysophospholipase L1 Proteins 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/06—Glass compositions containing silica with more than 90% silica by weight, e.g. quartz
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
- C03B19/066—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction for the production of quartz or fused silica articles
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/14—Other methods of shaping glass by gas- or vapour- phase reaction processes
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B20/00—Processes specially adapted for the production of quartz or fused silica articles, not otherwise provided for
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C11/00—Multi-cellular glass ; Porous or hollow glass or glass particles
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C4/00—Compositions for glass with special properties
- C03C4/005—Compositions for glass with special properties for opaline glass
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/12—Other methods of shaping glass by liquid-phase reaction processes
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/06—Doped silica-based glasses
- C03B2201/07—Impurity concentration specified
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/06—Doped silica-based glasses
- C03B2201/20—Doped silica-based glasses doped with non-metals other than boron or fluorine
- C03B2201/21—Doped silica-based glasses doped with non-metals other than boron or fluorine doped with molecular hydrogen
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/06—Doped silica-based glasses
- C03B2201/20—Doped silica-based glasses doped with non-metals other than boron or fluorine
- C03B2201/23—Doped silica-based glasses doped with non-metals other than boron or fluorine doped with hydroxyl groups
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2201/00—Glass compositions
- C03C2201/06—Doped silica-based glasses
- C03C2201/20—Doped silica-based glasses containing non-metals other than boron or halide
- C03C2201/21—Doped silica-based glasses containing non-metals other than boron or halide containing molecular hydrogen
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2201/00—Glass compositions
- C03C2201/06—Doped silica-based glasses
- C03C2201/20—Doped silica-based glasses containing non-metals other than boron or halide
- C03C2201/23—Doped silica-based glasses containing non-metals other than boron or halide containing hydroxyl groups
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2201/00—Glass compositions
- C03C2201/80—Glass compositions containing bubbles or microbubbles, e.g. opaque quartz glass
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2203/00—Production processes
- C03C2203/50—After-treatment
- C03C2203/52—Heat-treatment
- C03C2203/54—Heat-treatment in a dopant containing atmosphere
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- Manufacturing & Machinery (AREA)
- Geochemistry & Mineralogy (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Dispersion Chemistry (AREA)
- Glass Compositions (AREA)
- Optical Elements Other Than Lenses (AREA)
- Glass Melting And Manufacturing (AREA)
- Compositions Of Oxide Ceramics (AREA)
Description
「スペクトラロン」は、反射率が99%より高い平坦な分光プロファイル、及び、赤外からおよそ300nmの波長までの幅広い波長域にわたってのランベルト反射の挙動を示す。
(a)少なくとも200wt.ppmのヒドロキシル基含有量を有する合成により製造された透明石英ガラスの出発材料を粉砕し、SiO2グレインを得る工程と、
(b)前記分散液中の前記SiO2グレインを前記分散液と、大部分が10μm未満の大きさである、SiO2粉末粒子との前記スラリーを形成するように湿式摩砕する工程と、
(c)前記スラリーを前記SiO2粉末粒子の前記グリーン体に成形する工程。
450wt.ppmのヒドロキシル基含有量の透明石英ガラスの円筒が、SiCl4の火炎加水分解により標準的な方法で製造される。200−2500nmの波長域での透過率及び反射率の値は、両面が研磨された合成石英ガラスからなる測定試料を、分光器(Perkin Elmer Lamda900/950)を使用する方法により決定した。
顆粒状の破砕された出発材料の調製のために、合成石英ガラスの石英ガラス円筒はミル加工され、グレインサイズが250μmと650μmの間であるアモルファス石英ガラス断片2の粒度分が、ふるい分けにより抽出される。
スラリー5は市販のダイキャスト機械のダイに投入され、多孔質プラスチック膜を通して脱水され、多孔質グリーン体6が形成される。グリーン体6は、380nmの外径及び40nmの厚さを有するプレート形状を有する。
グリーン体6を焼結するために、上記グリーン体は、1395℃の加熱温度まで、1時間以内で、空気中、焼結炉内で加熱され、1時間その温度で維持される。冷却は、1000℃の炉温度まで1℃/minの冷却ランプで、続けて、閉じた状態の炉で、非制御方式で、行われる。
ディフューザー材料/成形体8は、450wt.ppmのヒドロキシル基含有量であり、3×1017分子/cm3の水素の平均充填量であり、2.145g/cm3の密度である気密性の密閉気孔の不透明な石英ガラスからなる。プレート径は80mmであり、プレート厚さは5mmである。
Claims (11)
- 化学的純度が少なくとも99.9%SiO2であり、クリストバライト含有量が1%以下であり、密度が2.0から2.18g/cm3の範囲であり、空孔を含んでいる石英ガラスのディフューザー材料であって、
前記空孔の少なくとも80%は、最大空孔寸法が20μm未満であり、
(1)前記石英ガラスは合成石英ガラスであり、
(2)前記石英ガラスはヒドロキシル基含有量が200wt.ppmを超える範囲であり、
(3)前記石英ガラスは、10 17 分子/cm 3 から10 19 分子/cm 3 の範囲の濃度で水素を含むことを特徴とするディフューザー材料。 - 前記空孔の体積が0.9〜5%の範囲であり、好ましくは2.5%より大きいことを特徴とする請求項1に記載のディフューザー材料。
- 前記空孔の少なくとも80%は、最大空孔寸法が10μm未満であることを特徴とする請求項1又は請求項2に記載のディフューザー材料。
- 5cmの測定長さにわたって均一に分布し、1cm3の試料体積を有する5つの密度測定試料が、0.01g/cm3未満の密度範囲を有するという意味で、前記密度の分布が均質であることを特徴とする請求項1から請求項3のいずれか一項に記載のディフューザー材料。
- 前記空孔がネオンを含むことを特徴とする請求項1から請求項4のいずれか一項に記載のディフューザー材料。
- 前記石英ガラスはヒドロキシル基含有量が450+/−50wt.ppmであることを特徴とする請求項1から請求項5のいずれか一項に記載のディフューザー材料。
- 請求項1から請求項6のいずれか一項に記載の前記合成により製造されたディフューザー材料の少なくとも一部を構成する成形体を製造する方法であって、グリーン体が分散液と純度が少なくとも99.9%SiO2 のSiO2粉末粒子とを含むスラリーから製造され、前記グリーン体が前記ディフューザー材料への焼結により処理され、以下の方法ステップ:
(a)珪素を含む出発物質の火炎加水分解を含む合成プロセスに基づいて、合成により製造された透明石英ガラスの出発材料を製造し、前記出発材料は200wt.ppmを超えるヒドロキシル基含有量を有し、前記出発材料は200nmの波長での透過係数k200が5×10 −3 cm −1 未満である工程と、
(b)前記出発材料を粉砕し、SiO 2 グレインとする工程と、
(c)前記分散液中の前記SiO2グレインを前記分散液と、大部分が10μm未満の大きさである、SiO2粉末粒子との前記スラリーを形成するように湿式摩砕する工程と、
(d)前記スラリーを前記SiO2粉末粒子の前記グリーン体に成形する工程と、
(e)前記グリーン体を、前記ディフューザー材料を形成するように、1400℃未満の温度で焼結する工程と、
(f)水素とともに前記ディフューザー材料を充填する工程であって、水素を含む雰囲気中で少なくとも1bar及び500℃未満の温度での処理を含む工程と
を含むことを特徴とする方法。 - 焼結中に分解する成分を前記スラリーに加えることを特徴とする請求項7に記載の方法。
- 焼結はネオンを含む雰囲気中で行われることを特徴とする請求項7又は請求項8に記載の方法。
- 前記出発材料は1064nmの波長での吸収係数が10ppm/cm以下であり、946nmでの吸収係数が2000ppm/cm以下であることを特徴とする請求項7から請求項9のいずれか一項に記載の方法。
- 請求項1から請求項6のいずれか一項に記載のディフューザー材料からなる成形体であって、分光及び宇宙応用でのディフューザー、デンシトメーター標準、リモートセンシングターゲット、レーザーの共振器及びレーザーの反射器、積分球又は光源のクラッド材として使用するための成形体。
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