JP6263772B2 - 塩化セシウム型類似構造の酸化ストロンチウム結晶の製造方法 - Google Patents
塩化セシウム型類似構造の酸化ストロンチウム結晶の製造方法 Download PDFInfo
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- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 title claims description 278
- 239000013078 crystal Substances 0.000 title claims description 134
- 238000004519 manufacturing process Methods 0.000 title claims description 17
- AIYUHDOJVYHVIT-UHFFFAOYSA-M caesium chloride Chemical compound [Cl-].[Cs+] AIYUHDOJVYHVIT-UHFFFAOYSA-M 0.000 title description 61
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 71
- 238000000034 method Methods 0.000 claims description 34
- 150000003438 strontium compounds Chemical class 0.000 claims description 26
- 150000002736 metal compounds Chemical class 0.000 claims description 20
- 239000012298 atmosphere Substances 0.000 claims description 18
- 229910052693 Europium Inorganic materials 0.000 claims description 17
- 229910052712 strontium Inorganic materials 0.000 claims description 15
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims description 14
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 claims description 13
- 239000011812 mixed powder Substances 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 12
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 12
- 239000000395 magnesium oxide Substances 0.000 claims description 11
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 11
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 11
- -1 organic acid salts Chemical class 0.000 claims description 10
- 150000002178 europium compounds Chemical class 0.000 claims description 8
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 claims description 7
- 229910000018 strontium carbonate Inorganic materials 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- UUCCCPNEFXQJEL-UHFFFAOYSA-L strontium dihydroxide Chemical compound [OH-].[OH-].[Sr+2] UUCCCPNEFXQJEL-UHFFFAOYSA-L 0.000 claims description 6
- 229910001866 strontium hydroxide Inorganic materials 0.000 claims description 6
- 150000004649 carbonic acid derivatives Chemical class 0.000 claims description 4
- 150000004697 chelate complex Chemical class 0.000 claims description 4
- 239000013522 chelant Substances 0.000 claims description 3
- 150000004679 hydroxides Chemical class 0.000 claims description 3
- 150000002902 organometallic compounds Chemical class 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 2
- 239000007790 solid phase Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical group [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 57
- 238000002441 X-ray diffraction Methods 0.000 description 43
- 239000011780 sodium chloride Substances 0.000 description 25
- 150000002681 magnesium compounds Chemical class 0.000 description 18
- 230000005284 excitation Effects 0.000 description 16
- 239000000843 powder Substances 0.000 description 16
- 238000000295 emission spectrum Methods 0.000 description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 229910052751 metal Inorganic materials 0.000 description 12
- 239000002184 metal Substances 0.000 description 12
- 239000000243 solution Substances 0.000 description 11
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 10
- 229910052792 caesium Inorganic materials 0.000 description 10
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 10
- 239000000758 substrate Substances 0.000 description 10
- 238000010894 electron beam technology Methods 0.000 description 8
- 150000001875 compounds Chemical class 0.000 description 7
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 239000010408 film Substances 0.000 description 6
- 238000006722 reduction reaction Methods 0.000 description 6
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 239000001569 carbon dioxide Substances 0.000 description 5
- 229910002092 carbon dioxide Inorganic materials 0.000 description 5
- 230000008859 change Effects 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 150000002739 metals Chemical class 0.000 description 5
- 238000010298 pulverizing process Methods 0.000 description 5
- 230000009467 reduction Effects 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 150000001768 cations Chemical class 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 238000001694 spray drying Methods 0.000 description 4
- ANPHGBOOSHEYIV-UHFFFAOYSA-N [Sr].[Eu] Chemical compound [Sr].[Eu] ANPHGBOOSHEYIV-UHFFFAOYSA-N 0.000 description 3
- 230000001133 acceleration Effects 0.000 description 3
- 239000003086 colorant Substances 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 229910001427 strontium ion Inorganic materials 0.000 description 3
- 239000000126 substance Substances 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
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- WTZCACCGYNWMDU-UHFFFAOYSA-K [NH4+].[Eu+3].C(CN(CC(=O)[O-])CC(=O)[O-])N(CC(=O)[O-])CC(=O)[O-] Chemical compound [NH4+].[Eu+3].C(CN(CC(=O)[O-])CC(=O)[O-])N(CC(=O)[O-])CC(=O)[O-] WTZCACCGYNWMDU-UHFFFAOYSA-K 0.000 description 2
- IQAPJLRHHAYONM-UHFFFAOYSA-L [NH4+].[NH4+].[Sr+2].C(CN(CC(=O)[O-])CC(=O)[O-])N(CC(=O)[O-])CC(=O)[O-] Chemical compound [NH4+].[NH4+].[Sr+2].C(CN(CC(=O)[O-])CC(=O)[O-])N(CC(=O)[O-])CC(=O)[O-] IQAPJLRHHAYONM-UHFFFAOYSA-L 0.000 description 2
- 150000004645 aluminates Chemical class 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 229910001940 europium oxide Inorganic materials 0.000 description 1
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 239000010437 gem Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- ORPJQHHQRCLVIC-UHFFFAOYSA-N magnesium;propan-2-olate Chemical compound CC(C)O[Mg]OC(C)C ORPJQHHQRCLVIC-UHFFFAOYSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- OHULXNKDWPTSBI-UHFFFAOYSA-N strontium;propan-2-olate Chemical compound [Sr+2].CC(C)[O-].CC(C)[O-] OHULXNKDWPTSBI-UHFFFAOYSA-N 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 230000005068 transpiration Effects 0.000 description 1
- HPNURIVGONRLQI-UHFFFAOYSA-K trifluoroeuropium Chemical compound F[Eu](F)F HPNURIVGONRLQI-UHFFFAOYSA-K 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/7729—Chalcogenides
- C09K11/7731—Chalcogenides with alkaline earth metals
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- 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
Description
酸化ストロンチウム(高純度化学社製,98%)を乳鉢で十分に粉砕し、その粉末5mgをエタノールに分散し、10mm×10mmの(110)配向の酸化マグネシウム基板上に滴下して乾燥した後、Ar+H2(3%)の気流中、1500℃で24時間還元処理することにより、酸化物を作製した。
酸化ストロンチウム(高純度化学社製,98%)を乳鉢で十分に粉砕し、その粉末5mgをエタノールに分散し、10mm×10mmの(100)配向の酸化マグネシウム基板上に滴下して乾燥した後、Ar+H2(3%)の気流中、1500℃で24時間還元処理することにより、酸化物を作製した。
実施例2の酸化ストロンチウムを炭酸ストロンチウム(和光純薬社製,99%)に代えた以外は実施例1の条件で酸化物を作製した。
200mL容のビーカーにエチレンジアミン四酢酸ストロンチウム二アンモニウム塩水溶液(Sr:6.5wt%)192.24gを入れ、さらにエチレンジアミン四酢酸ユウロピウムアンモニウム塩(Eu:31.1wt%)1.51gを加えて完全に溶解し、無色透明のストロンチウム−EDTAとユウロピウム−EDTAの混合溶液を得た。この溶液を、噴霧乾燥法によって乾燥温度160℃で粉末化することにより、(Sr,Eu)−EDTA錯体粉末を得た。この錯体粉末を、大気開放型の電気炉により800℃で3時間仮焼して有機物を熱分解除去し、ストロンチウムとユウロピウムからなる焼成粉末を得た。この焼成粉末5mgをエタノールに分散し、10mm×10mmの(110)配向の酸化マグネシウム基板上に滴下して乾燥した後、Ar+H2(3%)の気流中、1500℃で24時間還元処理することにより、蛍光体膜を作製した。
200mL容のビーカーにエチレンジアミン四酢酸ストロンチウム二アンモニウム塩水溶液(Sr:6.5wt%)192.24gを入れ、さらにエチレンジアミン四酢酸ユウロピウムアンモニウム塩(Eu:31.1wt%)1.51gを加えて完全に溶解し、無色透明のストロンチウム−EDTAとユウロピウム−EDTAの混合溶液を得た。この溶液を、噴霧乾燥法によって乾燥温度160℃で粉末化することにより、(Sr,Eu)−EDTA錯体粉末を得た。この錯体粉末を、大気開放型の電気炉により800℃で3時間仮焼して有機物を熱分解除去し、ストロンチウムとユウロピウムからなる焼成粉末を得た。この焼成粉末5mgをエタノールに分散し、10mm×10mmの(100)配向の酸化マグネシウム基板上に滴下して乾燥した後、Ar+H2(3%)の気流中、1500℃で24時間還元処理することにより、蛍光体を作製した。なお、EDTA溶液を用いた噴霧乾燥法により、非常に再現性良く良好な蛍光体を作製することができた。
塩化ナトリウム型構造を有する酸化ストロンチウム(高純度化学社製,98%)と酸化ユウロピウム(高純度化学社製,98%)を機械混合して得られた粉末5mgをエタノールに分散し、10mm×10mmの(110)配向の酸化マグネシウム基板上に滴下して乾燥した後、Ar+H2(3%)の気流中、1500℃で24時間還元処理することにより、蛍光体膜を作製した。
Claims (7)
- 正方晶または斜方晶を主体とする酸化ストロンチウム結晶を製造するための方法であって、
ストロンチウムのキレート錯体、有機酸塩、有機金属化合物、酸化物、水酸化物、炭酸塩から選択されるストロンチウム化合物と、酸化マグネシウムとを固相で接触させながら、還元雰囲気中、1200℃以上、1600℃以下で加熱処理する工程を含むことを特徴とする製造方法。 - ストロンチウム化合物と酸化マグネシウムに加え、さらに、ユウロピウムのキレート錯体、有機酸塩、有機金属化合物、酸化物、水酸化物、炭酸塩から選択されるユウロピウム化合物を接触させながら還元雰囲気中で加熱処理する請求項1に記載の製造方法。
- ストロンチウム化合物およびユウロピウム化合物を含む溶液から混合粉体を調製し、酸化マグネシウムと接触させる請求項2に記載の製造方法。
- 上記ストロンチウム化合物として、酸化ストロンチウム、水酸化ストロンチウムおよび炭酸ストロンチウムからなる群から選ばれる少なくとも一種を用いる請求項1〜3のいずれかに記載の製造方法。
- 一般組成式(Sr1-xEux)O[0<x≦0.5]で表され、且つ、正方晶または斜方晶を主体とする結晶を含むことを特徴とする酸化ストロンチウム系青色蛍光体。
- 上記一般組成式中、0.001≦x≦0.3である請求項5に記載の酸化ストロンチウム系青色蛍光体。
- 発光中心波長が450nm以上、485nm未満である請求項5または6に記載の酸化ストロンチウム系青色蛍光体。
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PCT/JP2012/055432 WO2012121161A1 (ja) | 2011-03-04 | 2012-03-02 | 塩化セシウム型類似構造の酸化ストロンチウム結晶の製造方法 |
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JP3268760B2 (ja) * | 1998-08-18 | 2002-03-25 | 株式会社リード | 高輝度アルミン酸ストロンチウム蓄光体 |
WO2005090513A1 (ja) * | 2004-03-19 | 2005-09-29 | Chubu Chelest Co., Ltd. | アルミン酸塩系蛍光体およびその製法 |
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