JPWO2006129674A1 - 導電性マイエナイト型化合物の製造方法 - Google Patents
導電性マイエナイト型化合物の製造方法 Download PDFInfo
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- JPWO2006129674A1 JPWO2006129674A1 JP2007519014A JP2007519014A JPWO2006129674A1 JP WO2006129674 A1 JPWO2006129674 A1 JP WO2006129674A1 JP 2007519014 A JP2007519014 A JP 2007519014A JP 2007519014 A JP2007519014 A JP 2007519014A JP WO2006129674 A1 JPWO2006129674 A1 JP WO2006129674A1
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- 150000001875 compounds Chemical class 0.000 title claims abstract description 107
- 238000000034 method Methods 0.000 title claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 73
- 239000001301 oxygen Substances 0.000 claims abstract description 54
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 54
- 239000002243 precursor Substances 0.000 claims abstract description 51
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 43
- 238000004519 manufacturing process Methods 0.000 claims abstract description 23
- 239000011261 inert gas Substances 0.000 claims abstract description 4
- 239000013078 crystal Substances 0.000 claims description 32
- 239000000843 powder Substances 0.000 claims description 32
- 239000000203 mixture Substances 0.000 claims description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 229910052782 aluminium Inorganic materials 0.000 claims description 12
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- 238000006243 chemical reaction Methods 0.000 claims description 12
- 239000003638 chemical reducing agent Substances 0.000 claims description 10
- 229910052791 calcium Inorganic materials 0.000 claims description 9
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 229910052719 titanium Inorganic materials 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 4
- 229910052684 Cerium Inorganic materials 0.000 claims description 3
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 3
- 229910052693 Europium Inorganic materials 0.000 claims description 3
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 3
- 229910052779 Neodymium Inorganic materials 0.000 claims description 3
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 3
- 229910052772 Samarium Inorganic materials 0.000 claims description 3
- 229910052771 Terbium Inorganic materials 0.000 claims description 3
- 229910052788 barium Inorganic materials 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
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- 229910052748 manganese Inorganic materials 0.000 claims description 3
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- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
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- 238000005245 sintering Methods 0.000 claims description 2
- 230000007704 transition Effects 0.000 claims 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 7
- 239000002178 crystalline material Substances 0.000 abstract description 2
- 229910052593 corundum Inorganic materials 0.000 abstract 2
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 2
- 239000011575 calcium Substances 0.000 description 19
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 16
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- -1 oxygen ions Chemical class 0.000 description 13
- 238000002844 melting Methods 0.000 description 9
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- 239000002994 raw material Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 230000031700 light absorption Effects 0.000 description 6
- 239000010936 titanium Substances 0.000 description 6
- 150000001450 anions Chemical class 0.000 description 5
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- 238000010521 absorption reaction Methods 0.000 description 4
- 238000000862 absorption spectrum Methods 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- 229910052691 Erbium Inorganic materials 0.000 description 2
- 229910052689 Holmium Inorganic materials 0.000 description 2
- 235000019738 Limestone Nutrition 0.000 description 2
- 239000005084 Strontium aluminate Substances 0.000 description 2
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- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 2
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- 235000011116 calcium hydroxide Nutrition 0.000 description 2
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- 229910001882 dioxygen Inorganic materials 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
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- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 238000003303 reheating Methods 0.000 description 2
- 239000011435 rock Substances 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910052712 strontium Inorganic materials 0.000 description 2
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- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 229910052774 Proactinium Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical group [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000002419 bulk glass Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- VAWSWDPVUFTPQO-UHFFFAOYSA-N calcium strontium Chemical compound [Ca].[Sr] VAWSWDPVUFTPQO-UHFFFAOYSA-N 0.000 description 1
- XFWJKVMFIVXPKK-UHFFFAOYSA-N calcium;oxido(oxo)alumane Chemical class [Ca+2].[O-][Al]=O.[O-][Al]=O XFWJKVMFIVXPKK-UHFFFAOYSA-N 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
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- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- FNWBQFMGIFLWII-UHFFFAOYSA-N strontium aluminate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Al+3].[Sr+2].[Sr+2] FNWBQFMGIFLWII-UHFFFAOYSA-N 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000004857 zone melting Methods 0.000 description 1
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Abstract
Description
前駆体を熱処理する工程を含む導電性マイエナイト型化合物の製造方法であって、
前記前駆体は、CaとAlとを含有し、酸化物換算した、(CaO:Al2O3)のモル比が(12.6:6.4)〜(11.7:7.3)であり、CaOとAl2O3との合計が50モル%以上である、ガラス質又は結晶質であり、
前記熱処理は、熱処理温度Tが600〜1415℃で、かつ、酸素分圧PO2が、Pa単位で、
PO2≦105×exp[{−7.9×104/(T+273)}+14.4]
で表される範囲である不活性ガス又は真空雰囲気中に前記前駆体を保持する熱処理である、ことを特徴とする導電性マイエナイト型化合物の製造方法を提供する。
また本発明において、前記前駆体は、粉末、粉末をプレス成形したプレス成型体、又は粉末を成形したプレス成型体を焼結した焼結体としてもよく、板状としてもよい。
本発明はさらに、前述の製造方法により製造された、導電率が100S/cm超である導電性マイエナイト型化合物を提供する。
(1)代表組成が12CaO・7Al2O3である絶縁性マイエナイト型化合物、
(2)この結晶格子の骨格と骨格により形成されるケージ構造が保持される範囲で、骨格又はケージ中の陽イオン又は陰イオンの一部又はすべてが置換された同型化合物(以下、代表組成が12CaO・7Al2O3である、絶縁性あるいは導電性のマイエナイト型化合物、その陽イオン又は陰イオンが置換された同型化合物を、単にC12A7化合物という)、
(3)前記C12A7化合物と同等の組成を有するガラス、
(4)前記C12A7化合物に相当する組成で混合された、マイエナイト型化合物以外の結晶構造を持つ混合酸化物、単成分の酸化物、炭酸化物及び水酸化物、などの粉末の混合物(以下単に、混合原料という)。
(1)C12A7化合物の骨格の一部又はすべての陽イオンが置換されたストロンチウムアルミネートSr12Al14O33や、CaとSrの混合比が任意に変化された混晶であるカルシウムストロンチウムアルミネートCa12−xSrXAl14O33、
(2)シリコン置換型マイエナイトであるCa12Al10Si4O35、
(3)ケージ中のフリー酸素がOH−、F−、S2−、Cl−などの陰イオンによって置換された、たとえばCa12Al14O32:2OH−又はCa12Al14O32:2F−、
(4)陽イオンと陰イオンがともに置換された、たとえばワダライトCa12Al10Si4O32:6Cl−。
また、Si又はGeは、生成された導電性マイエナイト型化合物中のAlの位置を置換させて含有させてもよく、この場合、ドーピング効果により該結晶に包接される電子密度を増大させる効果がある。ドーピング効果を得るためには、好ましくは6モル%以上とされる。Si、Ge又はBの含有量が過多では溶融温度が再び上昇する。また、Si又はGeの含有量が過多ではドーピング効果が得られなくなる。そのため、Si、Ge又はBの含有量は好ましくは17モル%以下とされる。
PO2≦105×exp[{−7.9×104/(T+273)}+14.4](1)
で表される範囲である不活性ガス又は真空雰囲気中に前記前駆体を保持しておこなわれる。すなわち、横軸を熱処理温度、縦軸を熱処理雰囲気中の酸素分圧PO2として(1)式をプロットした図3のグラフにおいて、ハッチングをかけた領域の熱処理温度及び酸素分圧PO2の条件で熱処理がおこなわれる。
本発明では、フリー酸素を電子に置換することにより、マイエナイト型化合物に導電性を付与するが、この置換反応は、バルクから表面へのフリー酸素イオンの移動と、表面における、フリー酸素の引き抜き反応を経由する。マイエナイト型化合物の代表組成である、C12A7化合物について、次の酸化反応、Ca12Al14O32:2e-+1/2O2=Ca12Al14O32:O2--ΔGC12A7を仮定すれば、雰囲気の酸素分圧が、概略、PO2=(1/K)=exp(ΔGo/RT)以下のときは、K<1であって、表面での引き抜き反応が進行する。酸素分圧が前記の値を超えると、高温状態においては、導電性マイエナイト化合物が雰囲気中の酸素を取り込んで、ケージ中の電子がフリー酸素イオンに置換される反応が進行するため、作製されるマイエナイト型化合物の導電性が低下する。
酸化物換算したCaO:Al2O3のモル比が12:7となるように炭酸カルシウムと酸化アルミニウムとを調合し、大気雰囲気下、1300℃で6時間保持したのち室温まで冷却して、得られた焼結物を粉砕して、粒子径50μmの粉末を得た。得られた粉末(以下粉末Aという)は白色の絶縁体であって、X線回折によるとマイエナイト型構造をもつC12A7化合物であった。
熱処理温度を1000℃、1100℃、及び1200℃とした以外は例1と同様に、カーボンによる酸素の吸収により低酸素分圧に保たれた雰囲気中で、結晶粉末試料(A)を熱処理して、それぞれ例2〜4の熱処理物を得た。熱処理時の酸素分圧PO2は、例2、3ではそれぞれ10−14Pa、10−13.5Paで、(1)式の関係を満足しなかった。例4では10−13Paであって、(1)式の関係を満足した。
粉末Aをプレス成形して、縦×横×高さが約2cm×2cm×1cmの成型体とし、金属アルミニウムと一緒に蓋付きアルミナ容器に入れ、ロータリーポンプで真空引きした真空炉中で1300℃まで昇温させ10時間保持する熱処理をおこなった。熱処理中の容器内は、容器に一緒に入れたアルミニウムによる酸素の吸収により酸素分圧が10−21Paと低酸素分圧であり、(1)式を満足する条件の雰囲気であった。
アーク放電溶融法により、(59.69CaO−32.21Al2O3−5.01SiO2−0.33Fe2O3−1.79TiO2−0.96MgO)なる組成の1cm角の立方体形状のバルクガラスを作製した。これを前駆体として、例1と同様にして(1)式を満足する条件下で熱処理をおこなった。熱処理後の試料は緑色で、X線回折によりマイエナイト型構造のピークを持つことが確認された。光吸収スペクトルより求めたキャリア密度は2.5×1019/cm3であり、導電性を有していた。以上により、導電性マイエナイト型化合物が得られたことが確認された。
帯域溶融法により作製したC12A7単結晶体を加工して、厚み0.5mm、1cm角の板状試料を2枚作成した。それぞれの板状のC12A7単結晶体を、金属Tiと一緒にシリカガラス管に入れ、ロータリーポンプで真空引きしたのち封止して、電気炉中で、それぞれ700℃で12時間、1000℃で120時間保持する熱処理をおこなった。熱処理中の容器内の雰囲気は、容器に一緒に入れた金属Tiによる酸素の吸収により、酸素分圧が、700℃においては10−33Pa、1000℃においては10−22Paの低酸素分圧であり、ともに(1)式の関係を満足する。
なお、2005年5月30日に出願された日本特許出願2005−157882号の明細書、特許請求の範囲、図面及び要約書の全内容をここに引用し、本発明の明細書の開示として、取り入れるものである。
Claims (11)
- 前駆体を熱処理する工程を含む導電性マイエナイト型化合物の製造方法であって、
前記前駆体は、
CaとAlとを含有し、酸化物換算した、CaO:Al2O3のモル比が12.6:6.4〜11.7:7.3であり、かつCaOとAl2O3との合計が50モル%以上である、ガラス質又は結晶質であり、
前記熱処理は、
熱処理温度Tが600〜1415℃で、かつ、酸素分圧PO2が、Pa単位で、
PO2≦105×exp[{−7.9×104/(T+273)}+14.4]
で表される範囲である不活性ガス又は真空雰囲気中に前記前駆体を保持する熱処理である、
ことを特徴とする導電性マイエナイト型化合物の製造方法。 - 前記結晶質の前駆体が、12CaO・7Al2O3なる組成を有し三次元的に連結されたケージから構成される結晶構造を持つマイエナイト型化合物、又はマイエナイト型化合物のCa及びAlの一部が他の元素で置換された同型化合物である請求項1に記載の導電性マイエナイト型化合物の製造方法。
- 前記前駆体が含有するCaの一部又はすべてが、同じ原子数のSrで置換されている請求項1又は2に記載の導電性マイエナイト型化合物の製造方法。
- 前記前駆体が含有するAlの一部が、同じ原子数のSi又はGeで置換されている請求項1又は2に記載の導電性マイエナイト型化合物の製造方法。
- 前記前駆体が、Si、Ge及びBからなる群から選ばれる少なくとも1種を酸化物換算した合計で0〜17モル%;Li、Na及びKからなる群から選ばれる少なくとも1種を酸化物換算した合計で0〜5モル%;Mg及びBaからなる群から選ばれる少なくとも1種を酸化物換算した合計で0〜10モル%;(Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm及びYbからなる群から選ばれる少なくとも1種の希土類元素)、及び(Ti、V、Cr、Mn、Fe、Co、Ni及びCuからなる群から選ばれる少なくとも1種の遷移金属元素あるいは典型金属元素)からなる群から選ばれる少なくとも1種を酸化物換算した合計で0〜8モル%;を含有する請求項1〜4のいずれか1項に記載の導電性マイエナイト型化合物の製造方法。
- 前記前駆体がガラス質であって、前記熱処理工程の前に950〜1415℃に加熱する工程を含んでいるか、又は、前記熱処理工程の熱処理温度Tが950〜1415℃である請求項1、3、4又は5に記載の導電性マイエナイト型化合物の製造方法。
- 前記前駆体が、マイエナイト型化合物以外の結晶構造をもつ結晶質であって、前記熱処理工程の前に1000〜1415℃に加熱する工程を含んでいるか、又は、前記熱処理工程の熱処理温度Tが1000〜1415℃である請求項1、3、4又は5に記載の導電性マイエナイト型化合物の製造方法。
- 前記前駆体が、粉末、粉末をプレス成形したプレス成型体、又は粉末を成形したプレス成型体を焼結した焼結体である請求項1〜7のいずれか1項に記載の導電性マイエナイト型化合物の製造方法。
- 前記前駆体が、板状である請求項1〜7のいずれか1項に記載の導電性マイエナイト型化合物の製造方法。
- 前記前駆体を、炭素、Al及びTiからなる群から選ばれるいずれかの還元剤とともに容器中に密閉した雰囲気中で熱処理がおこなわれる請求項1〜7のいずれか1項に記載の導電性マイエナイト型化合物の製造方法。
- 導電率が100S/cm超である、請求項1〜10のいずれか1項に記載の製造方法で製造された導電性マイエナイト型化合物。
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