JP2002363554A - Acid nitride phosphor activated with rare earth element - Google Patents
Acid nitride phosphor activated with rare earth elementInfo
- Publication number
- JP2002363554A JP2002363554A JP2001171831A JP2001171831A JP2002363554A JP 2002363554 A JP2002363554 A JP 2002363554A JP 2001171831 A JP2001171831 A JP 2001171831A JP 2001171831 A JP2001171831 A JP 2001171831A JP 2002363554 A JP2002363554 A JP 2002363554A
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- Japan
- Prior art keywords
- phosphor
- rare earth
- alpha sialon
- earth element
- activated
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Abstract
Description
【0001】[0001]
【発明の属する技術分野】この出願の発明は、希土類元
素を付活させた酸窒化物蛍光体に関するものである。さ
らに詳しくは、この出願の発明は、青色発光ダイオード
(青色LED)を光源とする白色発光ダイオード(白色LE
D)の高輝度化を可能とする、希土類元素を付活させた
酸窒化物蛍光体に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an oxynitride phosphor activated with a rare earth element. More specifically, the invention of this application relates to a white light emitting diode (white LE) using a blue light emitting diode (blue LED) as a light source.
The present invention relates to an oxynitride phosphor activated with a rare earth element, which makes it possible to increase the luminance of D).
【0002】[0002]
【従来の技術】ケイ酸塩、リン酸塩(たとえばアパタイ
トなど)、さらにアルミン酸塩を母体材料とし、これら
母体材料に遷移金属若しくは希土類金属を付活させた蛍
光体が、広く知られている。2. Description of the Related Art Phosphors in which silicates, phosphates (such as apatite), and aluminates are used as a base material and a transition metal or a rare earth metal is activated in the base material are widely known. .
【0003】一方、窒化物若しくは酸窒化物を母体材料
とした遷移金属若しくは希土類金属付活の蛍光体は、さ
ほど知られていない。窒化物蛍光体としては、たとえ
ば、ドイツ特許第789,890号公報にマンガン活性窒化ア
ルミニウムが、また、文献「Izv. Akad. Nauk SSSR, Ne
org. Master」17(8), 1431-5 (1981)に、希土類元素に
より活性化させたマグネシウム窒化ケイ素(MgSiN2)が
記載されている。最近では、歪んだウルツ型構造を有す
るZnSiN2にMnを付活させた赤色蛍光体(T. Endo et al.
「High pressure synthesis of"periodic compound" a
nd its optical and electrical properties」, In T.
Tsuruta, M. Doyama and Seno (Editors), New Functio
nality Materials, Volume C, Elsevier, Amsterdam, T
he Netherlands, pp. 107-112(1993))や、CaSiN2にEu
を付活させた赤色蛍光体(S. S. Lee et al. 「Photolu
minescence and Electroluminescence Characteristic
of CaSiN2:Eu」, Proc. SPIE-Int. Soc. Opt. Eng., 32
41, 75-83(1997))、さらに、Ba2Si5N8にEuを付活させ
た蛍光体などが報告されているのみである。On the other hand, a transition metal- or rare-earth metal-activated phosphor using nitride or oxynitride as a base material has not been known much. As the nitride phosphor, for example, manganese-activated aluminum nitride is disclosed in German Patent No. 789,890, and the literature “Izv. Akad. Nauk SSSR, Ne
org. Master ”17 (8), 1431-5 (1981) describes magnesium silicon nitride (MgSiN 2 ) activated by a rare earth element. Recently, a red phosphor obtained by activating Mn on ZnSiN 2 having a distorted wurtz-type structure (T. Endo et al.
"High pressure synthesis of" periodic compound "a
nd its optical and electrical properties '', In T.
Tsuruta, M. Doyama and Seno (Editors), New Functio
nality Materials, Volume C, Elsevier, Amsterdam, T
he Netherlands, pp. 107-112 (1993)) and CaSiN 2 with Eu.
Activated phosphor (SS Lee et al. “Photolu
minescence and Electroluminescence Characteristic
of CaSiN 2 : Eu ", Proc. SPIE-Int. Soc. Opt. Eng., 32
41, 75-83 (1997)), and only a phosphor in which Eu is activated in Ba 2 Si 5 N 8 is reported.
【0004】酸窒化物蛍光体については、ベータサイア
ロンを母体材料とする蛍光体(特開昭60-206889号公
報)をはじめ、ケイ酸塩鉱物やアパタイト構造を有する
Y-Si-O-N系複合酸窒化ケイ素にCeを付活させた蛍光体
(J. W. H. van Krevel et al. 「Long wavelength Ce
3+ emission in Y-Si-O-N materials」, J. Alloys and
Compounds, 268, 272-277(1998))や、ベータアルミナ
構造を有するBa1-xEuxAl11O1 6N蛍光体(H. Hintzen et
al. 「On the Existence of Europium Aluminum Oxynit
rides with a Magnetoplumbite or β-Alumina-Type St
ructure」, J. SolidState Chem., 142, 48-50(1999)、
及びS. R. Jansen et al. 「Eu-Doped BariumAluminum
Oxynitride with β-Alumina-Type Structure as New B
lue-EmittingPhosphor」, J. Electrochem. Soc., 146,
800-806(1999))が報告されている。最近では、オキシ
ナトライドガラスを母体材料とする蛍光体が提案されて
いるのみである(特願2000-030280)。For oxynitride phosphors, beta sia
Phosphors based on Ron (Japanese Patent Application Laid-Open No. 60-206889)
), Silicate minerals and apatite structure
Phosphor with Ce-activated Y-Si-O-N based composite silicon oxynitride
(J. W. H. van Krevel et al. “Long wavelength Ce
3+ emission in Y-Si-O-N materials ", J. Alloys and
Compounds, 268, 272-277 (1998)) and beta alumina
Ba with structure1-xEUxAl11O1 6N phosphor (H. Hintzen et
al. "On the Existence of Europium Aluminum Oxynit
rides with a Magnetoplumbite or β-Alumina-Type St
ructure ", J. SolidState Chem., 142, 48-50 (1999),
And S. R. Jansen et al. "Eu-Doped BariumAluminum
Oxynitride with β-Alumina-Type Structure as New B
lue-EmittingPhosphor ", J. Electrochem. Soc., 146,
800-806 (1999)). Recently, oxy
Phosphors based on natride glass have been proposed.
Only (Japanese Patent Application 2000-030280).
【0005】ところで、防災照明若しくは信号灯などの
信頼性が要求される分野、車載照明や液晶のバックライ
トのように小型軽量化が望まれる分野、また、駅の行き
先案内板などのように視認性が必要とされる分野などに
は、白色LEDが用いられてきている。この白色LEDの発光
色、すなわち白色光は、光の混色により得られものであ
り、発光源である波長450〜550nmのInGaN系の青色LEDが
発する青色光と、蛍光体が発する黄色光とが混合したも
のである。[0005] By the way, fields requiring reliability such as disaster prevention lighting or signal lights, fields where small size and light weight are desired such as on-board lighting and liquid crystal backlights, and visibility such as destination guide boards at stations are used. For example, white LEDs have been used in fields that require such devices. The emission color of this white LED, that is, white light, is obtained by mixing light, and blue light emitted by an InGaN-based blue LED having a wavelength of 450 to 550 nm, which is a light emitting source, and yellow light emitted by a phosphor are used. It is a mixture.
【0006】このような白色LEDに適当な蛍光体として
は、組成式:(Y,Gd)3(Al,Ga)5O12で示されるYAG系酸化
物にCeをドープした蛍光体が最もよく用いられている。
この蛍光体は、発光源である前記InGaN系の青色LEDチッ
プの表面に薄くコーティングされる。As a phosphor suitable for such a white LED, a phosphor obtained by doping Ce with a YAG-based oxide represented by a composition formula: (Y, Gd) 3 (Al, Ga) 5 O 12 is most preferable. Used.
This phosphor is thinly coated on the surface of the InGaN-based blue LED chip as a light emitting source.
【0007】[0007]
【発明が解決しようとする課題】しかしながら、酸化物
系蛍光体は、一般に、励起波長が400nmを超えると、ス
ペクトル強度が著しく減少するという欠点を有してい
る。したがって、InGaN系青色LEDのチップ表面にYAG系
酸化物からなる蛍光体をコーティングして得られる白色
LEDは、蛍光体であるYAG系酸化物の励起エネルギーと、
光源の青色LEDの励起エネルギーとが一致せず、励起エ
ネルギーが効率よく変換されないため、高輝度の白色LE
Dを作製することは難しいとされていた。However, oxide phosphors generally have the disadvantage that when the excitation wavelength exceeds 400 nm, the spectral intensity is significantly reduced. Therefore, the white surface obtained by coating the phosphor of YAG-based oxide on the chip surface of InGaN-based blue LED
LED has excitation energy of YAG-based oxide which is a phosphor,
Since the excitation energy of the blue LED of the light source does not match and the excitation energy is not efficiently converted, a high-brightness white LE
Making D was difficult.
【0008】この出願の発明は、以上の通りの事情に鑑
みてなされたものであり、青色発光ダイオード(青色LE
D)を光源とする白色発光ダイオード(白色LED)の高輝
度化を可能とする、希土類元素を付活させた酸窒化物蛍
光体を提供することを課題としている。[0008] The invention of this application has been made in view of the circumstances described above, and a blue light emitting diode (blue LE) has been developed.
It is an object of the present invention to provide a rare-earth-activated oxynitride phosphor capable of increasing the brightness of a white light-emitting diode (white LED) using D) as a light source.
【0009】[0009]
【課題を解決するための手段】この出願の発明の発明者
らは、発光の中心となる希土類元素の周りを囲む酸素原
子を窒素原子に置き換え、希土類元素の電子が、周りに
ある原子から受ける影響を緩和させることにより、従来
の酸化物系蛍光体が示す励起・発光ピークの位置が長波
長側に移行するとの技術的知見を得、この技術的知見に
基づき、オキシナイトライドガラスを母体材料に用い、
可視領域(≦500μm)にも及ぶ励起スペクトルを有する
蛍光体を前述の通り提案している(特願2000-030280
号)。Means for Solving the Problems The inventors of the present invention replace the oxygen atoms surrounding the rare earth element, which is the center of light emission, with nitrogen atoms and receive electrons of the rare earth element from the surrounding atoms. By mitigating the influence, we obtained technical knowledge that the position of the excitation / emission peak of the conventional oxide-based phosphor shifts to the longer wavelength side, and based on this technical knowledge, we made oxynitride glass a base material. Used for
As described above, a phosphor having an excitation spectrum extending to the visible region (≦ 500 μm) has been proposed (Japanese Patent Application No. 2000-030280).
issue).
【0010】そして、この出願の発明は、前記技術的知
見を基礎とし、また別の酸化物系蛍光体の存在について
鋭意検討した結果、オキシナイトライドガラスよりも窒
素含有率の高いアルファサイアロンを母体材料に用い、
母体材料であるアルファサイアロンに固溶する金属Me
(Meは、Ca、Mg、Y、又はLaとCeを除くランタニド金属
の一種若しくは二種以上)の一部若しくは全てが、発光
の中心となるランタニド金属Re1(Re1は、Ce、Pr、Eu、
Tb、Yb、又はErの一種若しくは二種以上)又は二種類の
ランタニド金属Re1及び共付活剤としてのRe2(Re2はD
y)で置換した結晶性の酸窒化物蛍光体が、高輝度の白
色LEDを可能とすることを見出し、この出願の発明を完
成させたのである。The invention of this application is based on the above technical knowledge, and as a result of intensive studies on the existence of another oxide-based phosphor, it was found that alpha sialon having a higher nitrogen content than oxynitride glass was used as a base material. Used for materials,
Metal Me dissolved in alpha sialon, the parent material
(Me is Ca, Mg, Y, or one or more of lanthanide metals except for La and Ce), part or all of which is a lanthanide metal Re1 (Re1 is Ce, Pr, Eu,
One or more of Tb, Yb, or Er) or two kinds of lanthanide metals Re1 and Re2 as a coactivator (Re2 is D
The inventors have found that the crystalline oxynitride phosphor substituted by y) enables a high-brightness white LED, and completed the invention of this application.
【0011】この出願の発明は、前述の課題を解決する
ものとして、一般式:MexSi12-(m+n )Al(m+n)OnN16-n:Re
1yRe2zで示され、アルファサイアロンに固溶する金属Me
(Meは、Ca、Mg、Y、又はLaとCeを除くランタニド金属
の一種若しくは二種以上)の一部若しくは全てが、発光
の中心となるランタニド金属Re1(Re1は、Ce、Pr、Eu、
Tb、Yb、又はErの一種若しくは二種以上)又は二種類の
ランタニド金属Re1及び共付活剤としてのRe2(Re2はD
y)で置換された蛍光体であることを特徴とする希土類
元素を付活させた酸窒化物蛍光体(請求項1)を提供す
る。The invention of this application solves the above-mentioned problems.
As a general formula: MexSi12- (m + n )Al(m + n)OnN16-n: Re
1yRe2zMetal Me dissolved in alpha sialon
(Me is Ca, Mg, Y, or lanthanide metals excluding La and Ce
Some or all of them) emit light
Lanthanide metal Re1 (Re1 is Ce, Pr, Eu,
One or more of Tb, Yb, or Er) or two
Lanthanide metal Re1 and Re2 as coactivator (Re2 is D
a rare earth element characterized by being a phosphor substituted with y)
Provided is an oxynitride phosphor activated by an element (Claim 1)
You.
【0012】またこの出願の発明は、金属Meが二価のと
き、0.6<m<3.0、かつ0≦n<1.5であること(請求項
2)、若しくは金属Meが三価のとき、0.9<m<4.5、か
つ0≦n<1.5であること一態様として提供する。Further, the invention of the present application is characterized in that when the metal Me is divalent, 0.6 <m <3.0 and 0 ≦ n <1.5 (claim 2), or when the metal Me is trivalent, 0.9 <m <3.0. It is provided as one embodiment that m <4.5 and 0 ≦ n <1.5.
【0013】さらにこの出願の発明は、以上の希土類元
素を付活させた酸窒化物蛍光体に関し、m=1.5、n=0.75
であり、組成式:MexSi9.75Al2.25O0.75N15.25:Re1yRe2
zにおいて、0.3<x+y<0.75、かつ0.01<y+z<0.7(た
だし、y>0.01、0.0≦z<0.1)であること(請求項
4)、さらに、0.3<x+y+z<1.5、0.01<y<0.7、かつ
0.0≦z<0.1であること(請求項5)を一態様として提
供する。Further, the invention of this application relates to an oxynitride phosphor activated with the above rare earth element, wherein m = 1.5 and n = 0.75.
And a composition formula: Me x Si 9.75 Al 2.25 O 0.75 N 15.25 : Re1 y Re2
In z , 0.3 <x + y <0.75 and 0.01 <y + z <0.7 (where y> 0.01, 0.0 ≦ z <0.1) (claim 4), and 0.3 <x + y + z <1.5, 0.01 <y <0.7, and
It is provided as an embodiment that 0.0 ≦ z <0.1 (claim 5).
【0014】さらにまたこの出願の発明は、請求項2、
4又は5に係る発明に関し、金属MeがCaであること(請
求項6)を一態様として提供する。以下、実施例を示し
つつ、この出願の発明の希土類元素を付活させた酸窒化
物蛍光体についてさらに詳しく説明する。Further, the invention of the present application is based on claim 2,
In the invention according to 4 or 5, the metal Me is Ca (claim 6) is provided as one embodiment. Hereinafter, the oxynitride phosphor activated with a rare earth element of the invention of the present application will be described in more detail with reference to examples.
【0015】[0015]
【発明の実施の形態】この出願の発明の希土類元素を付
活させた酸窒化物蛍光体は、前述の通り、一般式:MexS
i12-(m+n)Al(m+n)OnN16-n:Re1yRe2zで示され、アルファ
サイアロンに固溶する金属Me(Meは、Ca、Mg、Y、又はL
aとCeを除くランタニド金属の一種若しくは二種以上)
の一部若しくは全てが、発光の中心となるランタニド金
属Re1(Re1は、Ce、Pr、Eu、Tb、Yb、又はErの一種若し
くは二種以上)又は二種類のランタニド金属Re1及び共
付活剤としてのRe2(Re2はDy)で置換されている。BEST MODE FOR CARRYING OUT THE INVENTION The oxynitride phosphor activated with a rare earth element according to the invention of the present application has a general formula: Me x S, as described above.
i 12- (m + n) Al (m + n) O n N 16-n: Re1 indicated by y Re2 z, metal Me (Me is a solid solution in the alpha-SiAlON is, Ca, Mg, Y, or L
One or more lanthanide metals except a and Ce)
Lanthanide metal Re1 (Re1 is one or more of Ce, Pr, Eu, Tb, Yb, or Er) or two or more lanthanide metals Re1 and a coactivator, some or all of which are light emission centers (Re2 is Dy).
【0016】この出願の発明の希土類元素を付活させた
酸窒化物蛍光体において、金属Meは、(Si,Al)3(N,O)4の
4式量を含むアルファサイアロンの大きな単位胞3個当
たり最低1個から、単位胞1個当たり最高1個まで固溶
する。固溶限界は、一般に、金属Meが二価のとき、前述
の一般式において、0.6<m<3.0、かつ0≦n<1.5であ
り、金属Meが三価のとき、0.9<m<4.5、かつ0≦n<1.5
である。この範囲以外の領域では、アルファサイアロン
とならなくなる。In the oxynitride phosphor activated with a rare earth element of the invention of this application, the metal Me is a large unit cell of alpha sialon containing four formula quantities of (Si, Al) 3 (N, O) 4. Solid solution from at least 1 per 3 cells to at most 1 per unit cell. In general, the solid solubility limit is 0.6 <m <3.0 and 0 ≦ n <1.5 when the metal Me is divalent, and 0.9 <m <4.5 when the metal Me is trivalent. And 0 ≦ n <1.5
It is. In areas outside this range, it will not be alpha sialon.
【0017】このの金属Meの一部若しくは全てを置換
し、付活する、発光の中心となるランタニド金属Re1の
イオン間距離は、最低約5Åであり、これまでに知られ
ている蛍光体の3〜4Åよりはるかに大きい。このた
め、母体材料に含まれる発光の中心となるランタニド金
属の濃度が高いときに生じていた濃度消光による発光強
度の著しい低下を抑制することができると考えられる。The distance between the ions of the lanthanide metal Re1 which is the center of light emission, which replaces and activates a part or all of the metal Me, is at least about 5 °, and is the same as that of the known phosphor. Much larger than 3-4 °. Therefore, it is considered that a remarkable decrease in emission intensity due to concentration quenching, which occurred when the concentration of lanthanide metal, which is the center of light emission contained in the base material, was high.
【0018】また、この出願の発明の希土類元素を付活
させた酸窒化物蛍光体では、前記金属Meを発光の中心と
なるランタニド金属Re1の他に、共付活剤であるランタ
ニド金属Re2で置換することができるが、この共付活剤
としてのランタニド金属Re2の共付活効果は、二つ考え
られる。一つは増感作用であり、もう一つは、キャリア
ーのトラップ準位を新たに形成し、長残光の発現若しく
はその改善、さらに熱ルミネセンスを改善させるなどで
ある。このようなランタニド金属Re2の置換量は、共付
活剤であることから、一般に、前述の一般式において、
0.0≦z<0.1とするのが適当である。In the oxynitride phosphor activated with a rare earth element according to the invention of the present application, the metal Me is replaced by a lanthanide metal Re2 which is a co-activator, in addition to the lanthanide metal Re1 which is a center of light emission. Although it can be substituted, there are two possible co-activating effects of the lanthanide metal Re2 as this co-activating agent. One is a sensitizing effect, and the other is to newly form a trap level of a carrier, develop or improve long afterglow, and further improve thermoluminescence. Such a substitution amount of the lanthanide metal Re2 is a co-activator, and therefore, in general, in the aforementioned general formula,
It is appropriate that 0.0 ≦ z <0.1.
【0019】さらに、この出願の発明の希土類元素を付
活させた酸窒化物蛍光体は、前述の通り、アルファサイ
アロンを母体材料とするものであり、ベータサイアロン
を母体材料とする蛍光体とは、組成及び結晶構造におい
て本質的に異なる。Further, as described above, the oxynitride phosphor activated with a rare earth element according to the invention of the present application uses alpha sialon as a host material, and a phosphor using beta sialon as a host material. , Composition and crystal structure.
【0020】すなわち、ベータサイアロンは、一般式:
Si6-zAlzOzN8-z(0<z<4.2)で示され、ベータ型窒化
ケイ素の固溶体であり、Si位置の一部がAlで、また、N
位置の一部がOで置換されたものである。That is, beta sialon has the general formula:
Si 6-z Al z O z N 8-z (0 <z <4.2), a solid solution of beta-type silicon nitride, part of Si position is Al, and N
Some of the positions are replaced with O.
【0021】これに対し、アルファサイアロンは、一般
式:MexSi12-(m+n)Al(m+n)OnN16-nで示され、アルファ
型窒化ケイ素の固溶体であり、Si-N結合の一部がAl-N結
合で置換されるとともに、特定の金属Me(Meは、Ca、M
g、Y、又はLaとCeを除くランタニド金属の一種若しくは
二種以上)が、格子間に侵入、固溶したものである。On the other hand, alpha sialon is represented by the general formula: Me x Si 12- (m + n) Al (m + n) O n N 16-n and is a solid solution of alpha-type silicon nitride. -N bonds are partially replaced by Al-N bonds, and specific metals Me (Me is Ca, M
g, Y, or one or two or more lanthanide metals other than La and Ce) are interstitial and solid-dissolved.
【0022】このように両者では固溶状態が異なるた
め、ベータサイアロンは酸素含有率が高く、アルファサ
イアロンは窒素含有率が高くなっている。そして、ベー
タサイアロンを母体材料とし、発光の中心となるCe、P
r、Eu、Tb、Yb及びErの希土類酸化物の一種若しくは二
種以上を添加して合成した蛍光体は、ベータサイアロン
にはそれら金属が固溶しないため、ベータサイアロン粒
子間に希土類金属を含む化合物が生成した混合材料とな
る。As described above, since the solid solution states of the two are different, the beta sialon has a high oxygen content and the alpha sialon has a high nitrogen content. Then, using Beta Sialon as a base material, Ce, P
Phosphors synthesized by adding one or more of the rare earth oxides of r, Eu, Tb, Yb and Er contain rare earth metals between the beta sialon particles because those metals do not form a solid solution in beta sialon. The compound is a mixed material produced.
【0023】これに対し、アルファサイアロンが母体材
料であると、その結晶構造に金属Me(Meは、Ca、Mg、
Y、又はLaとCeを除くランタニド金属の一種若しくは二
種以上)を取り込み、固溶させ、また、発光の中心とな
るCe、Pr、Eu、Tb、Yb及びErの希土類元素が、その金属
Meと置換するため、アルファサイアロン構造の単一相か
ら構成される酸窒化物蛍光体が得られる。On the other hand, when Alpha Sialon is the base material, the crystal structure of the metal Me (Me is Ca, Mg,
Y, or one or more lanthanide metals other than La and Ce) are taken in and dissolved, and rare earth elements such as Ce, Pr, Eu, Tb, Yb and Er, which are the center of light emission,
By substituting with Me, an oxynitride phosphor composed of a single phase having an alpha sialon structure is obtained.
【0024】したがって、母体材料をベータサイアロン
とするか、あるいはアルファサイアロンとするかにより
得られる蛍光体は、組成及び結晶構造において全く異な
り、これは蛍光体の発光特性に反映される。Therefore, the phosphors obtained depending on whether the base material is beta sialon or alpha sialon are completely different in composition and crystal structure, and this is reflected in the emission characteristics of the phosphor.
【0025】すなわち、ベータサイアロンを母体材料と
する場合、前述の特開昭60-206889号公報の実施例33〜3
5に記載されているようなベータサイアロンにEr酸化物
を添加し合成した蛍光体の有する発光色は、青色(410
〜440nm)であるが、この出願の発明の希土類元素を付
活させた酸窒化物蛍光体は、後述する実施例1及び図2
に示したように、同じErの付活により発光色は、橙色か
ら赤色(570〜590nm)である。この現象から、アルファ
サイアロンの結晶構造中にErが取り込まれることによ
り、結晶を構成する窒素原子の影響をErが受け、酸化物
を母体材料とする蛍光体では実現が非常に難しいとされ
る光源の長波長化が、容易に起こるものと推察される。That is, when beta sialon is used as a base material, Examples 33 to 3 of JP-A-60-206889 described above are used.
The emission color of the phosphor synthesized by adding Er oxide to beta sialon as described in 5 is blue (410
440 nm). The oxynitride phosphor activated with a rare earth element of the invention of this application is described in Example 1 and FIG.
As shown in (2), the emission color changes from orange to red (570 to 590 nm) due to the same activation of Er. From this phenomenon, Er is incorporated into the crystal structure of alpha sialon, which is affected by the nitrogen atoms that make up the crystal, making it extremely difficult to achieve with phosphors based on oxides. It is presumed that the longer wavelengths easily occur.
【0026】また、母体材料がアルファサイアロンであ
ることから、この出願の発明の希土類元素を付活させた
酸窒化物蛍光体は、母体材料のアルファサイアロンの長
所をも兼ね備える。Since the base material is alpha sialon, the oxynitride phosphor activated with a rare earth element according to the invention of the present application also has the advantages of alpha sialon as the base material.
【0027】すなわち、アルファサイアロンは、熱及び
機械的性質に優れ、励起エネルギーが失われる原因とな
る熱的緩和現象を抑えることができ、したがって、この
出願の発明の希土類元素を付活させた酸窒化物蛍光体
は、温度上昇にともなう発光強度の減少率が小さくな
る。このため、使用可能な温度域は、これまでの蛍光体
に比べ広くなる。That is, alpha sialon has excellent thermal and mechanical properties and can suppress the thermal relaxation phenomenon that causes the loss of excitation energy. Therefore, the acid activated with a rare earth element according to the invention of the present application can be suppressed. In the nitride phosphor, the rate of decrease in emission intensity with increasing temperature decreases. Therefore, the usable temperature range is wider than that of the conventional phosphor.
【0028】また、アルファサイアロンは、化学的安定
性にも優れ、したがって、耐光性に優れる蛍光体とな
る。そして、この出願の発明の希土類元素を付活させた
酸窒化物蛍光体は、組成式中のO/N比、金属Meを置換す
るランタニド金属Re1の種類の選択、及び共付活剤とし
てのランタニド金属Re2の有無により、紫外線からX線、
さらには電子線によって励起可能となる。Alpha Sialon is also a phosphor excellent in chemical stability and therefore in light resistance. The oxynitride phosphor activated by the rare earth element of the invention of the present application has an O / N ratio in the composition formula, selection of the type of the lanthanide metal Re1 that replaces the metal Me, and a coactivator. Depending on the presence or absence of lanthanide metal Re2, from ultraviolet to X-ray,
Further, it can be excited by an electron beam.
【0029】特に、この出願の発明の希土類元素を付活
させた酸窒化物蛍光体の中で、m=1.5、n=0.75であり、
組成式:MexSi9.75Al2.25O0.75N15.25:Re1yRe2zにおい
て、0.3<x+y<0.75、かつ0.01<y+z<0.7(ただし、y
>0.01、0.0≦z<0.1)、若しくは0.3<x+y+z<1.5、0.
01<y<0.7、かつ0.0≦z<0.1の条件を満たし、金属Me
がCaであるものは、特に発光特性に優れ、紫外−可視光
励起蛍光体のみならず、電子線励起蛍光体にも応用が期
待される。In particular, among the oxynitride phosphors in which the rare earth element is activated according to the invention of the present application, m = 1.5 and n = 0.75;
Composition formula: Me x Si 9.75 Al 2.25 O 0.75 N 15.25 : Re1 y Re2 z , 0.3 <x + y <0.75 and 0.01 <y + z <0.7 (where y
> 0.01, 0.0 ≦ z <0.1), or 0.3 <x + y + z <1.5, 0.
01 <y <0.7 and 0.0 ≦ z <0.1
Is particularly excellent in luminescent properties, and is expected to be applied not only to ultraviolet-visible light excited phosphors but also to electron beam excited phosphors.
【0030】このように、この出願の発明の希土類元素
を付活させた酸窒化物蛍光体は、白色LEDの作製に特に
有効であり、光源となるInGaN系青色LEDに適した蛍光体
である。As described above, the oxynitride phosphor activated with a rare earth element of the invention of this application is particularly effective for producing a white LED, and is a phosphor suitable for an InGaN blue LED as a light source. .
【0031】[0031]
【実施例】希土類元素を付活させた酸窒化物蛍光体を、
ホットプレス装置を用い、20MPaの加圧下、1700℃、1at
mの窒素雰囲気中で1時間反応させて、以下に示す八つの
原料粉末を作製した。この原料の出発原料として用いた
化学試薬のモル比も以下の通りとした。 Ca-アルファサイアロン(Ca0.75Si9.75Al2.25N15.25O
0.75) 窒化ケイ素(Si3N4):窒化アルミニウム(AlN):酸化カル
シウム(CaO)=13:9:3 Eu-アルファサイアロン(Eu0.5Si9.75Al2.25N15.25O
0.75) 窒化ケイ素(Si3N4):窒化アルミニウム(AlN):酸化ユー
ロピウム(Eu2O3)=13:9:1 Pr-アルファサイアロン(Pr0.5Si9.75Al2.25N15.25O
0.75) 窒化ケイ素(Si3N4):窒化アルミニウム(AlN):酸化プラ
セオジム(Pr6O11)=30:27:1 Tb-アルファサイアロン(Tb0.5Si9.75Al2.25N15.25O
0.75) 窒化ケイ素(Si3N4):窒化アルミニウム(AlN):酸化テル
ビウム(Tb4O7)=26:18:1 Dy-アルファサイアロン(Dy0.5Si9.75Al2.25N15.25O
0.75) 窒化ケイ素(Si3N4):窒化アルミニウム(AlN):酸化ディ
スプロシウム(Dy2O3)=13:9:1 Y-アルファサイアロン(Y0.5Si9.75Al2.25N15.25O
0.75) 窒化ケイ素(Si3N4):窒化アルミニウム(AlN):酸化ディ
スプロシウム(Dy2O3)=13:9:1 Yb-アルファサイアロン(Yb0.5Si9.75Al2.25N15.25O
0.75) 窒化ケイ素(Si3N4):窒化アルミニウム(AlN):酸化イッ
テルビウム(Yb2O3)=13:9:1 Er-アルファサイアロン(Er0.5Si9.75Al2.25N15.25O
0.75) 窒化ケイ素(Si3N4):窒化アルミニウム(AlN):酸化エル
ビウム(Er2O3)=13:9:1 (実施例1)Eu2+イオンの付活量を変化させたCa-アル
ファサイアロン蛍光体を、上記及びの原料粉末を用
いて七種類作製した。作製条件は、原料粉末を以下のモ
ル比に混合し、ホットプレス装置を用い、20MPaの加圧
下、1700℃、1atmの窒素雰囲気中で1時間反応させた。 [1] Ca(0%Eu)-アルファサイアロン蛍光体(Ca0.75Si9.75
Al2.25N15.25O0.75) Ca-アルファサイアロンのみを原料とした。 [2] Ca(5%Eu)-アルファサイアロン蛍光体(Ca0.71Eu
0.025Si9.75Al2.25N15.25O0. 75) Ca-アルファサイアロン: Eu-アルファサイアロン
=95:5 [3] Ca(10%Eu)-アルファサイアロン蛍光体(Ca0.68Eu
0.05Si9.75Al2.25N15.25O0. 75) Ca-アルファサイアロン: Eu-アルファサイアロン
=90:10 [4] Ca(20%Eu)-アルファサイアロン蛍光体(Ca0.60Eu
0.10Si9.75Al2.25N15.25O0. 75) Ca-アルファサイアロン: Eu-アルファサイアロン
=80:20 [5] Ca(30%Eu)-アルファサイアロン蛍光体(Ca0.53Eu
0.15Si9.75Al2.25N15.25O0. 75) Ca-アルファサイアロン: Eu-アルファサイアロン
=70:30 [6] Ca(50%Eu)-アルファサイアロン蛍光体(Ca0.38Eu
0.25Si9.75Al2.25N15.25O0. 75) Ca-アルファサイアロン: Eu-アルファサイアロン
=50:50 [7] Ca(70%Eu)-アルファサイアロン蛍光体(Ca0.23Eu
0.35Si9.75Al2.25N15.25O0. 75) Ca-アルファサイアロン: Eu-アルファサイアロン
=30:70 図1は、これら[1]〜[7]の蛍光体の赤色発光に関するス
ペクトルを示したチャートである。EXAMPLE An oxynitride phosphor activated with a rare earth element was
Using a hot press machine, under pressure of 20MPa, 1700 ℃, 1at
m for 1 hour in a nitrogen atmosphere.
Raw material powder was produced. Used as starting material for this material
The molar ratios of the chemical reagents were also as follows. Ca-Alpha Sialon (Ca0.75Si9.75Al2.25N15.25O
0.75) Silicon nitride (SiThreeNFour): Aluminum nitride (AlN): Calcium oxide
Cium (CaO) = 13: 9: 3 Eu-alpha sialon (Eu0.5Si9.75Al2.25N15.25O
0.75) Silicon nitride (SiThreeNFour): Aluminum nitride (AlN): Oxide oxide
Lopium (EuTwoOThree) = 13: 9: 1 Pr-alpha sialon (Pr0.5Si9.75Al2.25N15.25O
0.75) Silicon nitride (SiThreeNFour): Aluminum nitride (AlN): Oxide plastic
Theodymium (Pr6O11) = 30: 27: 1 Tb-alpha sialon (Tb0.5Si9.75Al2.25N15.25O
0.75) Silicon nitride (SiThreeNFour): Aluminum nitride (AlN): Ter oxide
Bium (TbFourO7) = 26: 18: 1 Dy-Alpha Sialon (Dy0.5Si9.75Al2.25N15.25O
0.75) Silicon nitride (SiThreeNFour): Aluminum nitride (AlN): Dioxide
Sprosium (DyTwoOThree) = 13: 9: 1 Y-Alpha Sialon (Y0.5Si9.75Al2.25N15.25O
0.75) Silicon nitride (SiThreeNFour): Aluminum nitride (AlN): Dioxide
Sprosium (DyTwoOThree) = 13: 9: 1 Yb-alpha sialon (Yb0.5Si9.75Al2.25N15.25O
0.75) Silicon nitride (SiThreeNFour): Aluminum nitride (AlN): Oxide oxide
Terbium (YbTwoOThree) = 13: 9: 1 Er-Alpha Sialon (Er0.5Si9.75Al2.25N15.25O
0.75) Silicon nitride (SiThreeNFour): Aluminum nitride (AlN): Oxide oxide
Bium (ErTwoOThree) = 13: 9: 1 (Example 1) Eu2+Ca-Al with different ion activation amount
Phasialon phosphor is used as raw material powder
And made seven kinds. The production conditions were as follows:
And pressurized to 20MPa using a hot press
The reaction was carried out at 1700 ° C. for 1 hour in a nitrogen atmosphere of 1 atm. [1] Ca (0% Eu) -alpha sialon phosphor (Ca0.75Si9.75
Al2.25N15.25O0.75) Only Ca-alpha sialon was used as a raw material. [2] Ca (5% Eu) -alpha sialon phosphor (Ca0.71EU
0.025Si9.75Al2.25N15.25O0. 75) Ca-Alpha Sialon: Eu-Alpha Sialon
= 95: 5 [3] Ca (10% Eu) -alpha sialon phosphor (Ca0.68EU
0.05Si9.75Al2.25N15.25O0. 75) Ca-Alpha Sialon: Eu-Alpha Sialon
= 90: 10 [4] Ca (20% Eu) -alpha sialon phosphor (Ca0.60EU
0.10Si9.75Al2.25N15.25O0. 75) Ca-Alpha Sialon: Eu-Alpha Sialon
= 80: 20 [5] Ca (30% Eu) -alpha sialon phosphor (Ca0.53EU
0.15Si9.75Al2.25N15.25O0. 75) Ca-Alpha Sialon: Eu-Alpha Sialon
= 70: 30 [6] Ca (50% Eu) -alpha sialon phosphor (Ca0.38EU
0.25Si9.75Al2.25N15.25O0. 75) Ca-Alpha Sialon: Eu-Alpha Sialon
= 50: 50 [7] Ca (70% Eu) -alpha sialon phosphor (Ca0.23EU
0.35Si9.75Al2.25N15.25O0. 75) Ca-Alpha Sialon: Eu-Alpha Sialon
= 30:70 Figure 1 shows the red emission of these phosphors [1] to [7].
It is a chart showing a spectrum.
【0032】いずれの蛍光体の励起スペクトルにも、28
0nmと400〜450nmに広いピークが認められる。この二つ
のピークは、Eu2+イオンが付活される割合が50%まで、
付活量の増加にともないピーク強度の増大が見られる。
一方、付活量が50%を超えると、濃度消光によるピーク
強度の減少が起こるが、それでも付活量が30%のときよ
りピーク強度は依然として高い。The excitation spectrum of any of the phosphors has 28
Wide peaks are observed at 0 nm and 400 to 450 nm. These two peaks show that the rate at which Eu 2+ ions are activated is up to 50%.
The peak intensity increases as the activation amount increases.
On the other hand, when the activation amount exceeds 50%, the peak intensity decreases due to concentration quenching, but the peak intensity is still higher than when the activation amount is 30%.
【0033】励起スペクトルに現れた二つのピークの
内、280nmのピークは、母体材料Ca-アルファサイアロン
が励起されたピークに帰属し、400〜450nmのピークは、
Eu-(N又はO)の電荷移動吸収帯に帰属する。後者のEu-
(N,O)の電荷移動吸収帯に帰属するピークは、Eu2+イオ
ンの付活量の増加にともない長波長側にシフトしている
ことから、InGaN系青色LEDの励起光(450〜550nm)として
利用可能である。Of the two peaks appearing in the excitation spectrum, the peak at 280 nm belongs to the peak at which the base material Ca-alpha sialon is excited, and the peak at 400 to 450 nm is
It belongs to the charge transfer absorption band of Eu- (N or O). Eu- of the latter
Since the peak attributed to the charge transfer absorption band of (N, O) shifts to the longer wavelength side as the activation amount of Eu 2+ ions increases, the excitation light (450 to 550 nm ) Is available.
【0034】図2は、Eu2+イオンの付活量を変化させた
Ca-アルファサイアロン蛍光体の発光スペクトルを示し
たチャートである。観測されたピークは一つであり、こ
のピークは、Eu2+イオンの付活量の増加にしたがって56
0nmから590nmに連続的にシフトした。この発光スペクト
ルにおいても、図1に示した励起スペクトルと同様に、
ピークの最大強度は、Eu2+イオンの付活量が50%のとき
観測され、付活量が50%を超えると、濃度消光によるピ
ーク強度の減少が起こるが、それでも付活量が30%のと
きよりピーク強度は依然として高い。FIG. 2 shows that the activation amount of Eu 2+ ion was changed.
5 is a chart showing an emission spectrum of a Ca-alpha sialon phosphor. Only one peak was observed, and this peak increased as the activation amount of Eu 2+ ion increased.
Shifted continuously from 0 nm to 590 nm. Also in this emission spectrum, similarly to the excitation spectrum shown in FIG.
The peak maximum intensity is observed when the activation amount of Eu 2+ ions is 50%, and when the activation amount exceeds 50%, the peak intensity decreases due to concentration quenching, but the activation amount is still 30% The peak intensity is still higher than at the time.
【0035】なお、以上のCa-アルファサイアロン蛍光
体がEu2+イオン付活量を有するのは、前述の通り、付活
したEu2+イオン間の距離が約5Åも離れていることによ
るものである。 (実施例2)原料粉末を、 Ca-アルファサイアロン:
Pr-アルファサイアロン=50:50のモル比に混合し、
この混合粉末をホットプレス装置を用いて20MPaの加圧
下、1700℃、1atmの窒素雰囲気中で1時間反応させてPr
3+イオンを付活させたCa-アルファサイアロン蛍光体(Ca
0.38Pr0.25Si9.75Al2.25N15.25O0.75)を合成した。[0035] The above Ca- of alpha-SiAlON phosphor having a Eu 2+ ions activated amount, as described above, due to the distance between activated the Eu 2+ ions is approximately 5Å also away It is. (Example 2) Raw material powder was prepared using Ca-alpha sialon:
Pr-alpha sialon = 50:50 molar ratio,
This mixed powder was reacted for 1 hour in a nitrogen atmosphere at 1700 ° C. and 1 atm under a pressure of 20 MPa using a hot press apparatus to obtain Pr.
3+ ion activated Ca-alpha sialon phosphor (Ca
0.38 Pr 0.25 Si 9.75 Al 2.25 N 15.25 O 0.75 ) was synthesized.
【0036】図3(a)(b)は、各々、Pr3+イオンを付活さ
せたCa-アルファサイアロン蛍光体の励起スペクトル、
発光スペクトルを示したチャートである。励起スペクト
ルには、263nmに広いピークと、460nm付近にPr3+イオン
のf-f遷移に基づく輝線ピークが観測された。発光ピー
クには、450〜750nmにPr3+イオンのf-f遷移に基づく輝
線ピークが観測された。 (実施例3)原料粉末を、 Ca-アルファサイアロン:
Tb-アルファサイアロン=50:50のモル比に混合し、
この混合粉末をホットプレス装置を用いて20MPaの加圧
下、1700℃、1atmの窒素雰囲気中で1時間反応させてTb
3+イオンを付活させたCa-アルファサイアロン蛍光体(Ca
0.38Tb0.25Si9.75Al2.25N15.25O0.75)を合成した。FIGS. 3 (a) and 3 (b) show an excitation spectrum of a Ca-alpha sialon phosphor activated with Pr 3+ ions, respectively.
5 is a chart showing an emission spectrum. In the excitation spectrum, a broad peak at 263 nm and a bright line peak near 460 nm based on the ff transition of Pr 3+ ions were observed. In the emission peak, a bright line peak based on the ff transition of Pr 3+ ions was observed at 450 to 750 nm. (Example 3) A raw material powder was prepared using Ca-alpha sialon:
Tb-alpha sialon = 50:50 molar ratio,
This mixed powder was reacted for 1 hour in a nitrogen atmosphere at 1700 ° C. and 1 atm under a pressure of 20 MPa using a hot press apparatus to obtain Tb.
3+ ion activated Ca-alpha sialon phosphor (Ca
0.38 Tb 0.25 Si 9.75 Al 2.25 N 15.25 O 0.75 ) was synthesized.
【0037】図4(a)(b)は、各々、Tb3+イオンを付活さ
せたCa-アルファサイアロン蛍光体の励起スペクトル、
発光スペクトルを示したチャートである。励起スペクト
ルには、263nmに広いピークが認められた。発光ピーク
には、470〜650nmにTbr3+イオンのf-f遷移に基づく輝線
ピークが観測された。この輝線ピークは、550nmにおい
て最大であり、緑色発光として観測される。 (実施例4)原料粉末を、 Ca-アルファサイアロン:
Eu-アルファサイアロン: Dy-アルファサイアロン
=50:40:10のモル比に混合し、この混合粉末をホット
プレス装置を用いて20MPaの加圧下、1700℃、1atmの窒
素雰囲気中で1時間反応させてEu3+イオンを付活させたC
a-アルファサイアロン蛍光体にさらにDy3+を共付活させ
た蛍光体(Ca0.38Eu0.20Dy0.05Si9.75Al2.25N
15.25O0.75)を合成した。4 (a) and 4 (b) show the excitation spectrum of the Ca-alpha sialon phosphor activated with Tb 3+ ion, respectively.
5 is a chart showing an emission spectrum. A broad peak was observed at 263 nm in the excitation spectrum. In the emission peak, a bright line peak based on the ff transition of Tbr 3+ ion was observed at 470 to 650 nm . This emission line peak is maximum at 550 nm and is observed as green emission. (Example 4) A raw material powder was prepared using Ca-alpha sialon:
Eu-alpha sialon: Dy-alpha sialon = 50: 40: 10 was mixed in a molar ratio, and this mixed powder was reacted for 1 hour in a nitrogen atmosphere of 1700 ° C. and 1 atm under a pressure of 20 MPa using a hot press apparatus. Activated Eu 3+ ion
a-alpha sialon phosphor further activated with Dy 3+ (Ca 0.38 Eu 0.20 Dy 0.05 Si 9.75 Al 2.25 N
15.25 O 0.75 ) was synthesized.
【0038】図5(a)(b)は、各々、Eu2+イオンとDy3+イ
オンをともに付活させたCa-アルファサイアロン蛍光体
の励起スペクトル、発光スペクトルを示したチャートで
ある。FIGS. 5A and 5B are charts respectively showing the excitation spectrum and the emission spectrum of the Ca-alpha sialon phosphor activated with both Eu 2+ ions and Dy 3+ ions.
【0039】励起スペクトルには、290nmと450nmに広い
ピークが二つ認められた。この二つのピークの内、290n
mのピークは、母体材料のCa-アルファサイアロンが励起
されたピークに帰属し、450nmのピークは、Eu-(N,O)の
電荷移動吸収帯に帰属する。発光ピークに観測されるピ
ークは、一つであり、このピークは、Eu2+イオンのd-f
遷移に基づいている。 (実施例5)原料粉末を、 Y-アルファサイアロン:
Eu-アルファサイアロン=95:5のモル比に混合し、
この混合粉末をホットプレス装置を用いて20MPaの加圧
下、1700℃、1atmの窒素雰囲気中で1時間反応させてEu
3+イオンを付活させたY-アルファサイアロン蛍光体(Y
0.38Eu0.02Si9.75Al2.25N15.25O0.75)を合成した。In the excitation spectrum, two broad peaks were observed at 290 nm and 450 nm. 290n of these two peaks
The peak at m belongs to the peak where the Ca-alpha sialon of the base material is excited, and the peak at 450 nm belongs to the charge transfer absorption band of Eu- (N, O). There is one peak observed in the emission peak, and this peak is the df of the Eu 2+ ion.
Based on transitions. (Example 5) A raw material powder was prepared using Y-alpha Sialon:
Eu-Alpha Sialon = 95: 5 molar ratio,
This mixed powder was reacted at 1700 ° C. under a nitrogen atmosphere of 1 atm under a pressure of 20 MPa using a hot press apparatus for 1 hour to obtain Eu.
3+ ion activated Y-alpha sialon phosphor (Y
0.38 Eu 0.02 Si 9.75 Al 2.25 N 15.25 O 0.75 ) was synthesized.
【0040】図6(a)(b)は、各々、Eu2+イオンを付活さ
せたY-アルファサイアロン蛍光体の励起スペクトル、発
光スペクトルを示したチャートである。励起スペクトル
には、310nmと410nmに広いピークが二つ認められた。発
光ピークには、570nmにピークが観測され、このピーク
は、Eu2+イオンのd-f遷移に基づいている。 (実施例6)前記のYb2+アルファサイアロン(Yb0.5Si
9.75Al2.25N15.25O0.75)をそのまま蛍光体とした。FIGS. 6A and 6B are charts showing an excitation spectrum and an emission spectrum of a Y-alpha sialon phosphor activated with Eu 2+ ions, respectively. In the excitation spectrum, two broad peaks were observed at 310 nm and 410 nm. A peak is observed at 570 nm in the emission peak, and this peak is based on the df transition of the Eu 2+ ion. (Example 6) The above-mentioned Yb 2+ alpha sialon (Yb 0.5 Si
9.75 Al 2.25 N 15.25 O 0.75 ) was used as it is as a phosphor.
【0041】図7(a)(b)は、各々、Yb2+アルファサイア
ロン蛍光体の励起スペクトル、発光スペクトルを示した
チャートである。励起スペクトルには、約240nmに広い
ピークが観測された。発光ピークには、510nmにピーク
が観測され、このピークは、Yb2+イオンのd-f遷移に基
づいている。 (実施例7)前記のEr-アルファサイアロン(Er0.5Si
9.75Al2.25N15.25O0.75) をそのまま蛍光体とした。FIGS. 7A and 7B are charts showing an excitation spectrum and an emission spectrum of the Yb 2+ alpha sialon phosphor, respectively. A broad peak was observed at about 240 nm in the excitation spectrum. The emission peak has a peak at 510 nm, which is based on the df transition of the Yb 2+ ion. (Example 7) The above-mentioned Er-alpha sialon (Er 0.5 Si
9.75 Al 2.25 N 15.25 O 0.75 ) was used as the phosphor.
【0042】図8(a)(b)は、各々、Er3+アルファサイア
ロン蛍光体の励起スペクトル、発光スペクトルを示した
チャートである。励起スペクトルには、263nmに広いピ
ークと、400nm付近にEr3+イオンのf-f遷移に基づく輝線
ピークが観測された。発光ピークには、500〜600nmにEr
3+イオンのf-f遷移に基づく輝線ピークが観測された。FIGS. 8A and 8B are charts showing the excitation spectrum and the emission spectrum of the Er 3+ alpha sialon phosphor, respectively. In the excitation spectrum, a broad peak at 263 nm and a bright line peak near 400 nm based on the ff transition of Er 3+ ion were observed. The emission peak has an Er at 500-600 nm.
A bright line peak based on the ff transition of the 3+ ion was observed.
【0043】もちろん、この出願の発明は、以上の実施
形態及び実施例によって限定されるものではない。原料
の調製、モル比、作製条件などの細部については様々な
態様が可能であることは言うまでもない。Of course, the invention of this application is not limited by the above embodiments and examples. It goes without saying that various aspects are possible for details such as preparation of raw materials, molar ratios, and preparation conditions.
【0044】[0044]
【発明の効果】以上詳しく説明した通り、この出願の発
明の希土類元素を付活させた酸窒化物蛍光体は、その励
起スペクトルの位置が、従来の酸化物蛍光体と比較して
長波長側にシフトし、吸収ピークが、青色LEDが発する
発光(450〜500nm)に重なる。このため、この出願の発明
により、青色LEDを光源とする白色LEDの高輝度化を可能
とする、希土類元素を付活させた酸窒化物蛍光体が提供
される。As described above in detail, the oxynitride phosphor activated with a rare earth element according to the invention of the present application has the excitation spectrum position on the longer wavelength side as compared with the conventional oxide phosphor. , And the absorption peak overlaps the emission (450-500 nm) emitted by the blue LED. Therefore, according to the invention of this application, an oxynitride phosphor activated with a rare earth element and capable of increasing the brightness of a white LED using a blue LED as a light source is provided.
【0045】また、この出願の発明の希土類元素を付活
させた酸窒化物蛍光体は、母体材料がアルファサイアロ
ンであるため、熱及び機械的性質、さらに化学的安定性
に優れる。したがって、この出願の発明により、厳しい
環境下においても安定に動作可能な、すなわち耐光性に
優れた、希土類元素を付活させた酸窒化物蛍光体が提供
される。The oxynitride phosphor activated with a rare earth element according to the invention of this application is excellent in thermal and mechanical properties and chemical stability since the base material is alpha sialon. Therefore, according to the invention of this application, an oxynitride phosphor activated with a rare earth element, which can operate stably even in a severe environment, that is, has excellent light resistance is provided.
【図1】Eu2+イオンの付活量を変化させたCa-アルファ
サイアロン蛍光体の赤色発光に関する励起スペクトルを
示したチャートである。FIG. 1 is a chart showing an excitation spectrum relating to red emission of a Ca-alpha sialon phosphor in which the activation amount of Eu 2+ ion is changed.
【図2】Eu2+イオンの付活量を変化させたCa-アルファ
サイアロン蛍光体の発光スペクトルを示したチャートで
ある。FIG. 2 is a chart showing an emission spectrum of a Ca-alpha sialon phosphor in which the activation amount of Eu 2+ ion is changed.
【図3】(a)(b)は、各々、Pr3+イオンを付活させたCa-
アルファサイアロン蛍光体の励起スペクトル、発光スペ
クトルを示したチャートである。[FIG. 3] (a) and (b) show Ca− activated Pr 3+ ions, respectively.
3 is a chart showing an excitation spectrum and an emission spectrum of an alpha sialon phosphor.
【図4】(a)(b)は、各々、Tb3+イオンを付活させたCa-
アルファサイアロン蛍光体の励起スペクトル、発光スペ
クトルを示したチャートである。FIGS. 4 (a) and 4 (b) show Ca− activated with Tb 3+ ions, respectively.
3 is a chart showing an excitation spectrum and an emission spectrum of an alpha sialon phosphor.
【図5】(a)(b)は、各々、Eu2+イオンとDy3+イオンをと
もに付活させたCa-アルファサイアロン蛍光体の励起ス
ペクトル、発光スペクトルを示したチャートである。FIGS. 5A and 5B are charts showing an excitation spectrum and an emission spectrum of a Ca-alpha sialon phosphor activated with both Eu 2+ ions and Dy 3+ ions, respectively.
【図6】(a)(b)は、各々、Eu2+イオンを付活させたY-ア
ルファサイアロン蛍光体の励起スペクトル、発光スペク
トルを示したチャートである。FIGS. 6A and 6B are charts showing an excitation spectrum and an emission spectrum of a Y-alpha sialon phosphor activated with Eu 2+ ions, respectively.
【図7】(a)(b)は、各々、Yb2+アルファサイアロン蛍光
体の励起スペクトル、発光スペクトルを示したチャート
である。FIGS. 7A and 7B are charts respectively showing an excitation spectrum and an emission spectrum of a Yb 2+ alpha sialon phosphor.
【図8】(a)(b)は、各々、Er3+アルファサイアロン蛍光
体の励起スペクトル、発光スペクトルを示したチャート
である。FIGS. 8A and 8B are charts showing an excitation spectrum and an emission spectrum of an Er 3+ alpha sialon phosphor, respectively.
───────────────────────────────────────────────────── フロントページの続き Fターム(参考) 4G001 BA06 BA07 BA08 BA09 BA52 BB06 BB07 BB08 BB09 BB52 BC42 BC46 BD31 BE02 4H001 CA04 XA07 XA08 XA12 XA13 XA14 XA20 XA39 XA59 XA60 XA61 XA62 XA63 XA64 XA65 XA66 XA67 XA68 XA69 XA70 XA71 YA58 YA59 YA63 YA65 YA68 YA70 ──────────────────────────────────────────────────続 き Continued on the front page F-term (reference) 4G001 BA06 BA07 BA08 BA09 BA52 BB06 BB07 BB08 BB09 BB52 BC42 BC46 BD31 BE02 4H001 CA04 XA07 XA08 XA12 XA13 XA14 XA20 XA39 XA59 XA60 XA61 XA62 XA63 XA64 XA65 XA64 XA65 XA65 XA65 XA65 XA65 XA64 XA65 XA65 XA65 YA59 YA63 YA65 YA68 YA70
Claims (6)
Re1yRe2zで示され、アルファサイアロンに固溶する金属
Me(Meは、Ca、Mg、Y、又はLaとCeを除くランタニド金
属の一種若しくは二種以上)の一部若しくは全てが、発
光の中心となるランタニド金属Re1(Re1は、Ce、Pr、E
u、Tb、Yb、又はErの一種若しくは二種以上)又は二種
類のランタニド金属Re1及び共付活剤としてのRe2(Re2
はDy)で置換された蛍光体であることを特徴とする希土
類元素を付活させた酸窒化物蛍光体。[Claim 1] General formula: Me x Si 12- (m + n) Al (m + n) O n N 16-n :
Re1 y Re2 z , metal dissolved in alpha sialon
Some or all of Me (Me is Ca, Mg, Y, or one or more of lanthanide metals except La and Ce) is a lanthanide metal Re1 (Re1 is Ce, Pr, E
u, Tb, Yb, or Er) or two or more lanthanide metals Re1 and Re2 as a co-activator (Re2
Is an oxynitride phosphor activated with a rare earth element, wherein the phosphor is substituted with Dy).
つ0≦n<1.5である請求項1記載の希土類元素を付活さ
せた酸窒化物蛍光体。2. The oxynitride phosphor activated with a rare earth element according to claim 1, wherein when the metal Me is divalent, 0.6 <m <3.0 and 0 ≦ n <1.5.
つ0≦n<1.5である請求項1記載の希土類元素を付活さ
せた酸窒化物蛍光体。3. The oxynitride phosphor activated with a rare earth element according to claim 1, wherein 0.9 <m <4.5 and 0 ≦ n <1.5 when the metal Me is trivalent.
9.75Al2.25O0.75N15.2 5:Re1yRe2zにおいて、0.3<x+y<
0.75、かつ0.01<y+z<0.7(ただし、y>0.01、0.0≦z
<0.1)である請求項1乃至3いずれかに記載の希土類
元素を付活させた酸窒化物蛍光体。4. m = 1.5, n = 0.75, and the composition formula: MexSi
9.75Al2.25O0.75N15.2 Five: Re1yRe2z, 0.3 <x + y <
0.75, and 0.01 <y + z <0.7 (where y> 0.01, 0.0 ≦ z
The rare earth element according to any one of claims 1 to 3, which is <0.1).
An oxynitride phosphor activated with elements.
0.0≦z<0.1である請求項4記載の希土類元素を付活さ
せた酸窒化物蛍光体。5. The method according to claim 1, wherein 0.3 <x + y + z <1.5, 0.01 <y <0.7, and
5. The oxynitride phosphor activated with a rare earth element according to claim 4, wherein 0.0 ≦ z <0.1.
ずれかに記載の希土類元素を付活させた酸窒化物蛍光
体。6. The oxynitride phosphor activated with a rare earth element according to claim 2, wherein the metal Me is Ca.
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JP2001171831A JP3668770B2 (en) | 2001-06-07 | 2001-06-07 | Oxynitride phosphor activated with rare earth elements |
US10/162,614 US6632379B2 (en) | 2001-06-07 | 2002-06-06 | Oxynitride phosphor activated by a rare earth element, and sialon type phosphor |
AT02012727T ATE508177T1 (en) | 2001-06-07 | 2002-06-07 | ACTIVATED RARE EARTH ELEMENT OXYNITRIDE PHOSPHORUS AND SIALON PHOSPHORUS |
DE60239910T DE60239910D1 (en) | 2001-06-07 | 2002-06-07 | Activated rare earth element oxynitride phosphorus and sialon phosphorus |
EP08012606A EP2017323A3 (en) | 2001-06-07 | 2002-06-07 | Oxynitride phosphor activated by a rare earth element, and sialon type phosphor |
EP02012727A EP1264873B1 (en) | 2001-06-07 | 2002-06-07 | Oxynitride phosphor activated by a rare earth element, and sialon type phosphor |
US10/408,233 US6776927B2 (en) | 2001-06-07 | 2003-04-08 | Oxynitride phosphor activated by a rare earth element, and sialon type phosphor |
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