JP6691133B2 - アルミナ焼結体及び光学素子用下地基板 - Google Patents
アルミナ焼結体及び光学素子用下地基板 Download PDFInfo
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- JP6691133B2 JP6691133B2 JP2017543545A JP2017543545A JP6691133B2 JP 6691133 B2 JP6691133 B2 JP 6691133B2 JP 2017543545 A JP2017543545 A JP 2017543545A JP 2017543545 A JP2017543545 A JP 2017543545A JP 6691133 B2 JP6691133 B2 JP 6691133B2
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- sintered body
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- alumina sintered
- alumina
- pores
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims description 139
- 239000000758 substrate Substances 0.000 title claims description 30
- 230000003287 optical effect Effects 0.000 title claims description 15
- 239000011148 porous material Substances 0.000 claims description 30
- 238000002834 transmittance Methods 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 26
- 239000013078 crystal Substances 0.000 claims description 24
- 238000005259 measurement Methods 0.000 claims description 9
- 230000000007 visual effect Effects 0.000 claims description 6
- 238000002441 X-ray diffraction Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 description 37
- 239000000843 powder Substances 0.000 description 37
- 238000010304 firing Methods 0.000 description 25
- 239000010410 layer Substances 0.000 description 18
- 238000005498 polishing Methods 0.000 description 13
- 239000000523 sample Substances 0.000 description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 238000001514 detection method Methods 0.000 description 8
- 239000002346 layers by function Substances 0.000 description 8
- 239000011777 magnesium Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 238000000465 moulding Methods 0.000 description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- 238000009616 inductively coupled plasma Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- 238000000005 dynamic secondary ion mass spectrometry Methods 0.000 description 5
- 238000005530 etching Methods 0.000 description 5
- 239000011261 inert gas Substances 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 238000004445 quantitative analysis Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000006061 abrasive grain Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 4
- 238000000992 sputter etching Methods 0.000 description 4
- 229910052717 sulfur Inorganic materials 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 3
- 238000000280 densification Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229910003460 diamond Inorganic materials 0.000 description 3
- 239000010432 diamond Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 3
- 239000000395 magnesium oxide Substances 0.000 description 3
- 239000011812 mixed powder Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- YIWUKEYIRIRTPP-UHFFFAOYSA-N 2-ethylhexan-1-ol Chemical compound CCCCC(CC)CO YIWUKEYIRIRTPP-UHFFFAOYSA-N 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 2
- 229910052692 Dysprosium Inorganic materials 0.000 description 2
- 229910052691 Erbium Inorganic materials 0.000 description 2
- 229910052693 Europium Inorganic materials 0.000 description 2
- 229910052688 Gadolinium Inorganic materials 0.000 description 2
- 229910052689 Holmium Inorganic materials 0.000 description 2
- 229910052765 Lutetium Inorganic materials 0.000 description 2
- 229910052779 Neodymium Inorganic materials 0.000 description 2
- 229910052777 Praseodymium Inorganic materials 0.000 description 2
- 229910052772 Samarium Inorganic materials 0.000 description 2
- 229910052771 Terbium Inorganic materials 0.000 description 2
- 229910052775 Thulium Inorganic materials 0.000 description 2
- 229910052769 Ytterbium Inorganic materials 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000000538 analytical sample Substances 0.000 description 2
- 229910052787 antimony Inorganic materials 0.000 description 2
- 229910052785 arsenic Inorganic materials 0.000 description 2
- 229910052790 beryllium Inorganic materials 0.000 description 2
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 229910052794 bromium Inorganic materials 0.000 description 2
- 229910052793 cadmium Inorganic materials 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000002612 dispersion medium Substances 0.000 description 2
- 238000004993 emission spectroscopy Methods 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 229910052732 germanium Inorganic materials 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- 229910052741 iridium Inorganic materials 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910052746 lanthanum Inorganic materials 0.000 description 2
- 229910052745 lead Inorganic materials 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- 230000002093 peripheral effect Effects 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 229910052703 rhodium Inorganic materials 0.000 description 2
- 229910052701 rubidium Inorganic materials 0.000 description 2
- 229910052707 ruthenium Inorganic materials 0.000 description 2
- 229910052711 selenium Inorganic materials 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 238000007569 slipcasting Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229910052712 strontium Inorganic materials 0.000 description 2
- 229910052715 tantalum Inorganic materials 0.000 description 2
- 229910052718 tin Inorganic materials 0.000 description 2
- XQQWBPOEMYKKBY-UHFFFAOYSA-H trimagnesium;dicarbonate;dihydroxide Chemical compound [OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[O-]C([O-])=O.[O-]C([O-])=O XQQWBPOEMYKKBY-UHFFFAOYSA-H 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- 229910016569 AlF 3 Inorganic materials 0.000 description 1
- 229920002799 BoPET Polymers 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000282994 Cervidae Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- PRXRUNOAOLTIEF-ADSICKODSA-N Sorbitan trioleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](OC(=O)CCCCCCC\C=C/CCCCCCCC)[C@H]1OC[C@H](O)[C@H]1OC(=O)CCCCCCC\C=C/CCCCCCCC PRXRUNOAOLTIEF-ADSICKODSA-N 0.000 description 1
- 239000004147 Sorbitan trioleate Substances 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229960000391 sorbitan trioleate Drugs 0.000 description 1
- 235000019337 sorbitan trioleate Nutrition 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
- C04B35/111—Fine ceramics
- C04B35/115—Translucent or transparent products
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/638—Removal thereof
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- C04B35/64—Burning or sintering processes
- C04B35/645—Pressure sintering
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
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Description
T2=(1-R)(T1/(1-R))^(t2/t1)
1.アルミナ焼結体の作製
(1)粉末混合、テープ成形
市販の板状アルミナ粉末(YFA10030、キンセイマテック製、平均粒径10μm、平均厚み0.35μm、アスペクト比29)0.9質量部と、微細なアルミナ粉末(TM−DAR、平均粒径0.1μm、大明化学製)99.1質量部とを混合し、混合アルミナ粉末とした。板状アルミナ粉末と微細なアルミナ粉末との質量比をT:(100−T)で表すとT=0.9である。この混合アルミナ粉末100質量部に対し、酸化マグネシウム(500A、宇部マテリアルズ製)0.0125質量部(125質量ppm)と、バインダーとしてポリビニルブチラール(品番BM−2、積水化学工業製)7.8質量部と、可塑剤としてジ(2−エチルヘキシル)フタレート(黒金化成製)3.9質量部と、分散剤としてトリオレイン酸ソルビタン(レオドールSP−O30、花王製)2質量部と、分散媒として2−エチルヘキサノールとを加えて混合した。分散媒の量は、スラリー粘度が20000cPとなるように調整した。このようにして調製されたスラリーを、ドクターブレード法によってPETフィルムの上に乾燥後の厚さが20μmとなるようにシート状に成形した。得られたテープを直径50.8mm(2インチ)の円形に切断した後150枚積層し、厚さ10mmのAl板の上に載置した後、パッケージに入れて内部を真空にすることで真空パックとした。この真空パックを85℃の温水中で100kgf/cm2の圧力にて静水圧プレスを行い、円板状の成形体を得た。
得られた成形体を脱脂炉中に配置し、600℃で10時間の条件で脱脂を行った。得られた脱脂体を黒鉛製の型を用い、ホットプレスにて窒素中、焼成温度(最高到達温度)1975℃で4時間、面圧200kgf/cm2の条件で焼成し、アルミナ焼結体を得た。なお、焼成温度から降温する際に1200℃までプレス圧を維持し、1200℃未満の温度域ではプレス圧をゼロに開放した。
得られたアルミナ焼結体の板面に対しダイヤモンド砥粒を用いて表裏両面を鏡面研磨して厚さ0.5mmとし、研磨した焼結体(試料)をアセトン、エタノール、イオン交換水の順でそれぞれ10分間洗浄し、c面配向度、直線透過率、密度(気孔有無観察)用の試料を得た。
(1)c面配向度の算出
得られたアルミナ焼結体の配向度を確認するため、XRDによりc面配向度を測定した。鏡面研磨後のアルミナ焼結体に対し、その研磨面に対してXRD装置(リガク製、RINT−TTR III)を用いてX線を照射したときの2θ=20〜70°の範囲でXRDプロファイルを測定した。具体的には、CuKα線を用いて電圧50kV、電流300mAという条件で測定した。c面配向度は、ロットゲーリング法によって算出した。具体的には、前出の式により算出した。実験例1のアルミナ焼結体のc面配向度は100%であった。
アルミナ焼結体の板面(c面配向度測定と同じ面)に対し、図7のようにX線源と検出器を連動させてスキャンし、得られたカーブの半値幅(XRC・FWHM)を測定した。このように2θ(検出器と入射X線とのなす角度)の値をその回折ピーク位置に固定し、ω(試料基板面と入射X線とのなす角度)のみ走査する測定方法をロッキングカーブ測定とよぶ。装置はリガク製、RINT−TTR IIIを用い、CuKα線を用いて電圧50kV、電流300mAという条件でωの走査範囲を3.8°〜38.8°とした。実験例1のアルミナ焼結体のXRC・FWHMは3.2°であった。
(3−1)Fの定量分析
鏡面研磨後のアルミナ焼結体をD−SIMS(CAMECA製IMS−6f)にて分析した。測定条件は下記のとおりとした。
・一次イオン種:Cs+
・一次イオン加速エネルギー:14〜15eV
・二次イオン極性:Negative
・電荷補償:E−gun
・スパッタサイクル:100〜500サイクル
200−300スパッタサイクル間の平均値をF量として用いた。定量分析の際は分析試料と同組成(AlO)の濃度既知の標準試料を分析試料と同条件で測定し、相対感度係数を求めて定量を行った。その結果、焼結体中のF量は検出限界(0.1質量ppm)以下であった。
(3−2)Mgの定量分析
アルミナ焼結体を純度99.9%のアルミナ乳鉢で粉砕した後、JISR1649に準拠した加圧硫酸分解法にて板状アルミナ粉末を溶解し、ICP(誘導結合プラズマ)発光分析装置(日立ハイテクサイエンス製 PS3520UV−DD)にて定量分析した。実験例1のアルミナ焼結体のMg量は64質量ppm検出された。
(3−3)その他の元素の定量分析
C,S:炭素・硫黄分析装置(LECO製 CS844)を用いて燃焼(高周波加熱)−赤外線吸収法にて分析した。
N:酸素・窒素分析装置(堀場製作所製 EMGA−650W)を用いて、不活性ガス融解−熱伝導度法にて分析した。
H:水素分析装置(堀場製作所製 EMGA−921)にて不活性ガス融解−非分散型赤外線吸収法にて分析した。
上記以外の不純物元素(主にSi,Fe,Ti,Na,Ca,Mg,K,P,V,Cr,Mn,Co,Ni,Cu,Zn,Y,Zr,Pb,Bi,Li,Be,B,Cl,Sc,Ga,Ge,As,Se,Br,Rb,Sr,Nb,Mo,Ru,Rh,Pd,Ag,Cd,In,Sn,Sb,Te,Cs,Ba,Hf,Ta,W,Ir,Pt,Au,Hg,La,Ce,Pr,Nd,Sm,Eu,Gd,Tb,Dy,Ho,Er,Tm,Yb,Lu):JISR1649に準拠した加圧硫酸分解法にて板状アルミナ粉末を溶解し、ICP(誘導結合プラズマ)発光分析装置(日立ハイテクサイエンス製 PS3520UV−DD)にて分析した。
得られたアルミナ焼結体の任意の断面をダイヤモンド砥粒を用いて予備研磨した後、クロスセクションポリッシャ(CP)(日本電子製、IB−09010CP)で研磨した。CPはイオンミリングの範疇に属する。CPを用いたのは、研磨面に脱粒が生じないからである。得られた断面を走査型電子顕微鏡(日本電子製、JSM−6390)にて撮影した。観察する倍率は、具体的には、縦92.5μm×横124.0μmの視野を倍率1000倍で撮影した写真を、縦4枚分、横3枚分連続的な写真(縦370.0μm×横372.0μm)となるように並べ、目視により直径0.2〜1.0μmの気孔の数をカウントした。倍率を1000倍とすることでより微細な気孔を目視で判別することが可能となる。実験例1のアルミナ焼結体で確認された気孔数は7個であった。なお、気孔の直径は、気孔の外周上の2定点の距離が最大となる長さとした。
鏡面研磨後のアルミナ焼結体を、純度99.5質量%の高純度アルミナ製のさや(容積750cm3)に入れ、大気中で1550℃で45分間、サーマルエッチング処理を行った。本サーマルエッチング処理を行うことにより、粒内部と粒界部でエッチングレートが異なるために粒界を鮮明に観察できるようになる。そのサーマルエッチング処理を行った面の画像を走査型電子顕微鏡(日本電子製、JSM−6390)にて撮影した。視野範囲は、次のようにして設定した。すなわち、得られた画像上に長方形を配置してその対角線を引いた場合に、いずれの対角線も10個から30個の粒子と交わるように長方形のサイズを設定し、その長方形を視野範囲に設定した。そして、その長方形の2本の対角線と交わる全ての粒子に対し、個々の粒子の内側の線分の長さを平均したものに1.5を乗じた値を板面の平均粒径とした。実験例1のアルミナ焼結体の平均粒径(結晶粒径)は44μmであった。
得られたアルミナ焼結体を、10mm×10mmの大きさに切り出し、φ68mmの金属製定盤の最外周部に90°おきに4個固定し、SiC研磨紙上で、金属製定盤と研磨治具の荷重のみ(合わせて1314g)をかけた状態で#800で10分、#1200で5分ラップ研磨(予備研磨)した。その後、セラミック定盤上でダイヤモンド砥粒を用いたラップ研磨を行った。ラップ研磨は、砥粒サイズ1μmで30分、その後、砥粒サイズ0.5μmで2時間行った。研磨後の10mm×10mm×0.5mm厚の試料をアセトン、エタノール、イオン交換水の順でそれぞれ3分間洗浄した後、分光光度計(Perkin Elmer製、Lambda900)を用いて波長300〜1000nmにおける直線透過率を測定した。実験例1のアルミナ焼結体の波長300〜1000nmにおける直線透過率は60.4%以上であった。
実験例2〜13は、実験例1に準じて、表1に示すアルミナ焼結体の製造条件でアルミナ焼結体を作製した。具体的には、実験例2,3は、焼成温度をそれぞれ1900℃,1850℃とした以外は、実験例1と同様にしてアルミナ焼結体を作製した。実験例4〜7,9〜12は、T(混合アルミナ粉末中の板状アルミナ粉末の質量%)を表1に示す値とした以外は、実験例1と同様にしてアルミナ焼結体を作製した。実験例8は、焼成温度1975℃で2時間、面圧1886kgf/cm2の条件でHIP焼成してアルミナ焼結体を得た。HIP焼成においては、1975℃のキープ終了後、1200℃までは面圧1000kgf/cm2以上の高圧を保った状態で降温した。実験例13は、Tを2とし焼成温度を1800℃としたこと以外は、実験例1と同様にしてアルミナ焼結体を作製した。これらのアルミナ焼結体につき、上記2.(1)〜(5)の特性を求めた。その結果を表1に示した。
実験例14〜22は、実験例1に準じて、表1に示すアルミナ焼結体の製造条件でアルミナ焼結体を作製した。
実験例1〜11,14〜19のアルミナ焼結体は、いずれも、c面配向度が5%以上、XRC半値幅が15.0°以下、F含有量が検出限界以下、結晶粒径が15〜200μm、直径0.2〜1.0μmの気孔の数が25個以下であった。これらの実験例で得られたアルミナ焼結体の厚みを0.5mmとしたときの波長300nm〜1000nmにおける直線透過率は50%以上であり、直線透過率が高く、透明性に優れていた。このように優れた透明性が得られた理由は定かではないが、c面配向度、XRC半値幅、F含有量、結晶粒径及び直径0.2〜1.0μmの気孔の数がそれぞれ適正な値であったことが複合的に寄与した結果であろうと考えられる。
Claims (10)
- X線を照射したときの2θ=20°〜70°の範囲におけるX線回折プロファイルを用いてロットゲーリング法により求めたc面配向度が5%以上かつロッキングカーブ測定におけるXRC半値幅が15.0°以下であり、
D−SIMSで測定したときのF含有量が0.99質量ppm未満であり、
結晶粒径が15〜200μmであり、
縦370.0μm×横372.0μmの視野を倍率1000倍で撮影した写真を目視したときの直径0.2μm〜1.0μmの気孔の数が25個以下である、
アルミナ焼結体。 - 前記F含有量が0.1質量ppm以下である、
請求項1に記載のアルミナ焼結体。 - 前記結晶粒径が20〜200μmである、
請求項1又は2に記載のアルミナ焼結体。 - 前記気孔の数が15個以下である、
請求項1〜3のいずれか1項に記載のアルミナ焼結体。 - 前記F含有量が0.1質量ppm以下であり、
前記結晶粒径が20〜200μmであり、
前記気孔の数が10個以下である、
請求項1に記載のアルミナ焼結体。 - 前記c面配向度が60%以上かつ前記XRC半値幅が5.0°以下であり、
前記結晶粒径が40〜95μmであり、
前記気孔の数が7個以下である、
請求項5に記載のアルミナ焼結体。 - 前記結晶粒径が45〜95μmであり、
前記気孔の数が5個以下である、
請求項6に記載のアルミナ焼結体。 - 前記c面配向度が96%以上かつ前記XRC半値幅が2.6°以下であり、
前記気孔の数が3個以下である、
請求項7に記載のアルミナ焼結体。 - 0.5mm厚の前記アルミナ焼結体の300〜1000nmにおける直線透過率が78%以上である、
請求項1〜8のいずれか1項に記載のアルミナ焼結体。 - 請求項1〜9のいずれか1項に記載のアルミナ焼結体からなる光学素子用下地基板。
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EP2305621B1 (en) * | 2009-09-09 | 2015-04-22 | NGK Insulators, Ltd. | Translucent polycrystalline sintered body, method for producing the same, and arc tube for high-intensity discharge lamp |
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