JPWO2011142228A1 - β型サイアロンの製造方法、β型サイアロン及びその利用製品 - Google Patents
β型サイアロンの製造方法、β型サイアロン及びその利用製品 Download PDFInfo
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- JPWO2011142228A1 JPWO2011142228A1 JP2012514750A JP2012514750A JPWO2011142228A1 JP WO2011142228 A1 JPWO2011142228 A1 JP WO2011142228A1 JP 2012514750 A JP2012514750 A JP 2012514750A JP 2012514750 A JP2012514750 A JP 2012514750A JP WO2011142228 A1 JPWO2011142228 A1 JP WO2011142228A1
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- sialon
- raw material
- firing
- powder
- phosphor
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 56
- 239000002994 raw material Substances 0.000 claims abstract description 47
- 238000010304 firing Methods 0.000 claims abstract description 31
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 30
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 26
- 239000010439 graphite Substances 0.000 claims abstract description 26
- 229910052582 BN Inorganic materials 0.000 claims abstract description 21
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 13
- 150000001875 compounds Chemical class 0.000 claims abstract description 9
- 229910001873 dinitrogen Inorganic materials 0.000 claims abstract description 9
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 9
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 8
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims abstract description 8
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 8
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 7
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 33
- 238000000034 method Methods 0.000 claims description 14
- 229910001940 europium oxide Inorganic materials 0.000 claims description 4
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 claims description 4
- 239000000843 powder Substances 0.000 description 47
- 238000011049 filling Methods 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 238000010306 acid treatment Methods 0.000 description 7
- 239000002253 acid Substances 0.000 description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 238000010298 pulverizing process Methods 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 230000005284 excitation Effects 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000012300 argon atmosphere Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 229910018516 Al—O Inorganic materials 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 229910007991 Si-N Inorganic materials 0.000 description 1
- 229910006294 Si—N Inorganic materials 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000003303 reheating Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 1
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 1
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- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
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Abstract
Description
本発明のβ型サイアロンの製造方法は、酸化アルミニウム又は酸化ケイ素の少なくとも一つと、窒化ケイ素と、窒化アルミニウムと、光学活性元素化合物とを混合したβ型サイアロンの原料を、1820℃以上2200℃以下の温度で焼成する焼成工程を有するものであって、焼成工程を、複数の窒化ホウ素製の容器に充填されたβ型サイアロンの原料を窒素ガスと触れやすくなるように黒鉛ボックス内に配置し、黒鉛ボックスの上部を解放して窒素雰囲気下で行うことを特徴とする。
本発明のβ型サイアロンは、一般式:Si6−zAlzOzN8−zで示されるβ型サイアロンのホスト結晶に、発光中心としてEu,Mn,Sm,Ceから選択される1以上の元素が含有されたものである。とくに、Euを含有するものが、紫外線から可視光の幅広い波長域で励起されるため、好ましい。
本発明の発光装置は、上述のβ型サイアロンで形成される蛍光体と、発光光源とを備えて構成されている。この発光装置を用いて、350nm以上500nm以下の波長を含有している紫外光や可視光を励起源として、β型サイアロンに照射する。照射によって、β型サイアロンが520nm以上550nm以下の範囲の波長にピークを持つ高い発光強度を有する光を発し、これにより本発明の発光装置は高い発光強度を有する。発光装置の励起源としては、紫外LED、青色LED、蛍光体ランプの単体又はこれらの組み合わせがある。また、β型サイアロン蛍光体と、赤色発光蛍光体や青色発光蛍光体とを組み合わせることによって、発光色を白色や他の波長の色とすることができる。
α型窒化ケイ素粉末(電気化学工業社製NP−400グレード、酸素含有量0.96質量%)95.4質量%、窒化アルミニウム粉末(トクヤマ社製Fグレード、酸素含有量0.9質量%)3.1質量%、酸化アルミニウム粉末(大明化学社製TM−DARグレード)0.7質量%、及び酸化ユーロピウム粉末(信越化学工業社製RUグレード)0.8質量%を配合し、原料混合物1kgを得た。
<焼成工程>
上記のようにして得た原料粉末を、内寸で直径8cm×高さ8cmの蓋付きの円筒型窒化ホウ素製容器(電気化学工業社製N−1グレード)9個に各容器当たり100g充填し、内寸で51cm×31cm×高さ20cmの上蓋付き黒鉛ボックス内部に壁に沿って容器を配置した(原料充填率=0.9%)。カーボンヒーターの電気炉で0.9MPaの加圧窒素雰囲気中、2000℃で10時間の加熱処理を行った後、得られた粉末を室温まで徐冷した。得られた焼成物は、緩く凝集した塊状であり、清浄なゴム手袋を着用した人の手で軽度の解砕を行った。軽度の解砕をした原料を、目開き150μmの篩を通し、45gの合成粉末を得た。
原料充填率0.9%=((9×100)/3.2)/(51×31×20)
原料を充填した円筒型窒化ホウ素製の容器14個を、黒鉛ボックス内部に5個を3列に配置した。ただし、1列のみ4個とした(原料充填率=1.4%)。他は、実験例1の焼成工程と同じ条件で処理を行い、蛍光体粉末を得た。
黒鉛ボックスの上蓋を開け、実験例2と同じ個数の容器、焼成工程及び条件で処理を行い、蛍光体粉末を得た。
原料を充填した円筒型窒化ホウ素製の容器を19個とし、黒鉛ボックス内部に3列×5列に配置し(原料充填率=1.9%)、更に4個の容器を黒鉛ボックスの壁に沿って上段に配置するよう変更し、実験例1の焼成工程と同じ条件で処理を行い、蛍光体粉末を得た。
原料を充填した円筒型窒化ホウ素製の容器30個を、黒鉛ボックス内部に5個を3列、上下2段に配置する(原料充填率=3.0%)よう変更し、実験例1の焼成工程と同じ処理工程及び条件で処理を行い、蛍光体粉末を得た。
蛍光体粉末を10mm×10mm×45mmの2面透明石英セルに入れ、50回タッピングした後、セルの方向を180度変え、更に50回タッピングした。その蛍光体粉末の入ったセルを上記装置の試料室内にあるセルフォルダーに取り付けた。このセルに、発光光源(Xeランプ)から所定の波長に分光した単色光を導入した。この単色光を励起源として、蛍光体試料に照射し、分光光度計を用いて試料の発光強度を測定した。
本実施例での単色光は、波長455nmの青色光を用いた。
発光強度は、YAG:Ce(化成オプトニクス社製P46Y3)の発光強度を100%とした相対ピーク強度(%)で表した
原料充填率が低くなるほど炭素濃度が低くなっていた。特に原料充填率が2%以下であると、炭素濃度が200ppm以下であり好ましい。
また、上下2段に容器を配置する場合は、黒鉛ボックスの壁に沿って容器を配置することが好ましい。
さらに、Eu含有β型サイアロン用原料粉末を入れた窒化ホウ素製の容器を投入する黒鉛ボックスの蓋を開いた状態で焼成すると炭素含量が低減していた。
表1、表2及び図1より、合成粉末に含まれる炭素濃度を低減することで発光強度が向上していた。炭素濃度が200ppm以下であれば、YAG:Ceより高い発光強度となっていた。
実験例1で得られた合成粉末を超音速ジェット粉砕機(日本ニューマチック工業社製PJM−80SP)により解砕して粉末を得た。図2に、得られた粉砕粉末の走査型電子顕微鏡像(SEM像)を示す。粉砕粉末の粒径の制御は、粉砕機の粉砕室への試料供給速度と粉砕エアー圧力により行った。
粉砕後の粉末15gを、直径40mm×高さ45mmの蓋付きの円筒型窒化ホウ素製の容器(電気化学工業社製N−1グレード)に充填し、カーボンヒーターの電気炉で大気圧アルゴン雰囲気中、1450℃で8時間の加熱処理を行った。得られた粉末には焼成を伴う収縮はなく、加熱前とほとんど同じ性状であり、目開き45μmの篩を全て通過した。
加熱処理後の粉末を50%フッ化水素酸と70%硝酸の1:1混酸中で処理した。処理中に懸濁液は深緑色から鮮やかな緑色に変化した。その後、水洗及び乾燥してβ型サイアロンの粉末を得た。
得られたβ型サイアロンの粉末に対し、湿式沈降法により、微粉除去処理を行った。まず、蛍光体粉末を分散剤としてヘキサメタ燐酸ナトリウムを添加した水溶液中に分散した後、容器に移し、静置した後、上澄み液を除去する操作を、上澄み液が透明になるまで繰り返した。その後、沈殿物をろ過し、分散剤を除去するために十分に水洗し、乾燥を行い微粉除去したβ型サイアロンの粉末を得た(実験例5)。
比較例1に記載の合成粉末を、実験例5と同じ処理工程及び条件で処理を行い、β型サイアロンの粉末を得た。粉砕工程、加熱処理工程、酸処理工程及び分級工程を含む製造方法により、β型サイアロンの粉末を製造した(比較例2)。
Claims (7)
- 酸化アルミニウム又は酸化ケイ素の少なくとも一つと、窒化ケイ素と、窒化アルミニウムと、光学活性元素化合物とを混合したβ型サイアロンの原料を、1820℃以上2200℃以下の温度で焼成する焼成工程を有するβ型サイアロンの製造方法であって、焼成工程が、複数の窒化ホウ素製の容器に充填されたβ型サイアロンの原料を窒素ガスと触れやすくなるように黒鉛ボックス内に配置し窒素雰囲気下で焼成する工程である、β型サイアロンの製造方法。
- 酸化アルミニウム又は酸化ケイ素の少なくとも一つと、窒化ケイ素と、窒化アルミニウムと、光学活性元素化合物とを混合したβ型サイアロンの原料を、1820℃以上2200℃以下の温度で焼成する焼成工程を有するβ型サイアロンの製造方法であって、焼成工程が、複数の窒化ホウ素製の容器に充填されたβ型サイアロンの原料を窒素ガスと触れやすくなるように黒鉛ボックス内に配置し、黒鉛ボックスの上部を解放して窒素雰囲気下で焼成する工程である、β型サイアロンの製造方法。
- 複数の窒化ホウ素製の容器に充填されたβ型サイアロンの原料の総容積が黒鉛ボックスの内容積に対して2%である、請求項1又は2記載のβ型サイアロンの製造方法。
- 前記光学活性元素化合物が、酸化ユーロピウムである、請求項1又は2記載のβ型サイアロンの製造方法。
- 一般式:Si6−zAlzOzN8−zで示され、Euを含有するβ型サイアロンであって、炭素濃度が200ppm以下である、β型サイアロン。
- 請求項5に記載のβ型サイアロンを用いた蛍光体。
- 請求項6記載の蛍光体と、発光光源とを有する発光装置。
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