JPS5919160B2 - Shigaibuhatsukokeikoutai - Google Patents

Shigaibuhatsukokeikoutai

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Publication number
JPS5919160B2
JPS5919160B2 JP15338775A JP15338775A JPS5919160B2 JP S5919160 B2 JPS5919160 B2 JP S5919160B2 JP 15338775 A JP15338775 A JP 15338775A JP 15338775 A JP15338775 A JP 15338775A JP S5919160 B2 JPS5919160 B2 JP S5919160B2
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JP
Japan
Prior art keywords
phosphor
output
initial
ultraviolet rays
emission
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.)
Expired
Application number
JP15338775A
Other languages
Japanese (ja)
Other versions
JPS5277888A (en
Inventor
一夫 成田
信之 津田
明 田屋
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Toshiba Corp
Original Assignee
Tokyo Shibaura Electric Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Tokyo Shibaura Electric Co Ltd filed Critical Tokyo Shibaura Electric Co Ltd
Priority to JP15338775A priority Critical patent/JPS5919160B2/en
Publication of JPS5277888A publication Critical patent/JPS5277888A/en
Publication of JPS5919160B2 publication Critical patent/JPS5919160B2/en
Expired legal-status Critical Current

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Description

【発明の詳細な説明】 〔発明の属する技術分野〕 この発明は253.7nm紫外線の刺激下で300nm
より短波長部に発光ピークを有し、且つ劣化の少い紫外
部発光螢光体に関する。
[Detailed Description of the Invention] [Technical Field to which the Invention Pertains] This invention relates to the use of ultraviolet rays of 300 nm under the stimulation of 253.7 nm ultraviolet rays.
The present invention relates to an ultraviolet-emitting phosphor that has an emission peak in a shorter wavelength region and is less likely to deteriorate.

〔発明の技術的背景およびその問題点〕[Technical background of the invention and its problems]

一般に、300mn付近の波長を有する紫外線は健康的
に好ましい作用を示すことが知られている。
Generally, it is known that ultraviolet rays having a wavelength of around 300 mn exhibit beneficial effects on health.

この目的にかなつた螢光体として310nmに発光ピー
クを有するタリウム付活オルソリン酸カリシウム((C
a、Zn)3(PO4)2:Ti)を挙げることができ
る。ところが最近になつて280nm付近の紫外線の方
が300nmより長波長の紫外線より大きな健康的作用
を有すると考えられるようになつた。
A phosphor suitable for this purpose is thallium-activated potassium orthophosphate ((C
a, Zn)3(PO4)2:Ti). However, recently it has come to be believed that ultraviolet rays around 280 nm have greater health effects than ultraviolet rays with wavelengths longer than 300 nm.

またこの波長領域の光は光化学反応の光源としても有用
であることが知られている。従来、この波長領域で発光
する螢光体として、米国特許2450548号に記載さ
れたフッ化セリウム(CeF3)およびこれとアルミニ
ウム(Al)、トリウ(Th)、ジルコニウム(Zr)
、ハフニウム(Hf)、希土類元素などのフッ化物との
固溶体が知られている。
It is also known that light in this wavelength range is useful as a light source for photochemical reactions. Conventionally, phosphors that emit light in this wavelength range include cerium fluoride (CeF3) described in U.S. Pat.
Solid solutions with fluorides such as , hafnium (Hf), and rare earth elements are known.

しかしながらこの種の従来の螢光体は効率の悪いもので
あつた。これらの問題点を解決するために、我々は、既
にCeF3を含む希土類フッ化物について、組成と焼成
条件を詳細に検討し、(Al、La、Ce)F3、(A
t、Y、Ce)F3、(La、Pr、Ce)F3、(Y
、La、Ce)F3、(At、Pr、Ce)F3などの
固溶体を600℃〜1000℃の還元性のない雰囲中で
少くとも5分間焼成して生成せしめることにより好適な
効率が得られる紫外部発光螢光体(特開昭48一717
87)を発明している。なおこの螢光体は(At、La
、Ce)F3、(La、Pr、Ce)F3、(Aι)
Pr、Ce)F3では約286nmに、また(Al、Y
、Ce)F3、(Y、La、Ce)F3では約295n
mに発光ピークを有する。また、この主発光ピークのほ
かに、約2000CWL−1長波長側に第2の発光ピー
クを有するので発光中心はΞ価セリウムイオ0 ン(C
e3f)である。しカルながら、これらの螢光体のうち
の一部はランプに被着して長時間点灯すると発光出力の
低下を示すことが判明した。たとえば(Aio、1La
O2Ce02)F3なる組成の螢光体を塗布したIOW
低圧水銀ランプを連続点灯■5 したところ、螢光出力
は100時間でほぼ半減した。〔発明の目的〕 この発明は上述した従来のものの不都合さを改良したも
ので、300nmより短波長の光を発光し、その発光効
率が良く、しかもその発光出力の低下の少ない紫外部発
光螢光体を提供することを目的とする。
However, conventional phosphors of this type have low efficiency. In order to solve these problems, we have already studied in detail the composition and firing conditions of rare earth fluorides containing CeF3, and have found that (Al, La, Ce)F3, (A
t, Y, Ce) F3, (La, Pr, Ce) F3, (Y
, La,Ce)F3, (At,Pr,Ce)F3, etc., by calcination for at least 5 minutes in a non-reducing atmosphere at 600°C to 1000°C to obtain a suitable efficiency. Ultraviolet light-emitting phosphor (Japanese Patent Application Laid-Open No. 48-717
87). Note that this phosphor is (At, La
,Ce)F3,(La,Pr,Ce)F3,(Aι)
Pr, Ce) F3 has a wavelength of about 286 nm, and (Al, Y
, Ce)F3, (Y, La, Ce)F3 is about 295n
It has an emission peak at m. In addition to this main emission peak, there is a second emission peak on the long wavelength side of about 2000 CWL-1, so the emission center is Ξ-valent cerium ion (C
e3f). However, it has been found that some of these phosphors adhere to lamps and show a decrease in luminous output when the lamps are left on for a long time. For example (Aio, 1La
IOW coated with phosphor of composition O2Ce02)F3
When a low-pressure mercury lamp was continuously lit ■5, the fluorescent output was reduced by almost half in 100 hours. [Object of the Invention] The present invention improves the disadvantages of the conventional products described above, and provides an ultraviolet-emitting fluorescent light that emits light with a wavelength shorter than 300 nm, has good luminous efficiency, and has little reduction in luminous output. The purpose is to provide the body.

〔発明の概要〕[Summary of the invention]

以下この発明について詳細に説明する。 This invention will be explained in detail below.

この発明による紫外部発光螢光体は(M1−x−YPr
xCey)F3(ただし、MはAt,YおよびLaのう
ち少なくとも一種であり、0.45≦x≦0.95,0
.05≦y≦0.55,0.85≦x+y≦1である。
The ultraviolet-emitting phosphor according to this invention is (M1-x-YPr
xCey) F3 (where M is at least one of At, Y and La, 0.45≦x≦0.95, 0
.. 05≦y≦0.55, 0.85≦x+y≦1.

)の組成比で表わされる混合物を温度600℃乃至10
00℃の還元性のない雰囲気中で少なくとも5分間焼成
することによつて得られるものである。〔発明の実施例
〕 次に、この発明による螢光体の組成範囲に於ける発光出
力およびその所定条件での時間経過に伴なう出力変化に
ついて、本発明の実施例である第4図乃至第6図に示し
て説明する。
) at a temperature of 600°C to 10°C.
It is obtained by firing for at least 5 minutes in a non-reducing atmosphere at 00°C. [Embodiments of the Invention] Next, the luminous output in the composition range of the phosphor according to the present invention and its change in output over time under predetermined conditions are shown in FIGS. 4 to 4 which are embodiments of the present invention. This will be explained with reference to FIG.

なおこの発明による螢光体の組成範囲以外については、
比較例として、第1図乃至第53図に示し、さらに、第
4図乃至第6図内に併記した。第1図乃至第6図内は各
組成をモル%で示した三元図、各螢光体の組成に於ける
初期発光出力を、各図内での最も高いものに対する比較
値(パーセント(%))として示し、さらに各螢光体の
組成について、その螢光体に185nmの波長の紫外線
を6時間照射し、その照射後の発光出力を、その螢光体
の初期出力に対する比較値(パーセント(%))ととし
て〔 〕内に示した。
Regarding other than the composition range of the phosphor according to this invention,
Comparative examples are shown in FIGS. 1 to 53, and are also shown in FIGS. 4 to 6. Figures 1 to 6 are ternary diagrams showing each composition in mol%, and the initial luminous output for each phosphor composition is compared to the highest one in each figure (percentage). )), and for the composition of each phosphor, the phosphor is irradiated with ultraviolet light with a wavelength of 185 nm for 6 hours, and the luminous output after irradiation is expressed as a comparative value (percentage) with respect to the initial output of the phosphor. (%)) is shown in [ ].

たとえば、第1図中のLaF,7Oモル%、CeF32
Oモル%、AtF3lOモル%の点に示した82〔32
.0〕は、LaF,5Oモル%、Ce2Oモル%、At
F,3Oモルの点の螢光体に対し、その初期発光出力が
82%であり、185nm波長の紫外線を6時間照射し
た後の発光出力が初期発光出力に対して32.0%に低
下したことを表わす。第1図乃至第6図内で示された螢
光体仄その各組成比で調製された混合物を800℃の温
度の空気中雰囲気で30分間焼成して製造したものであ
る。
For example, LaF, 7O mol%, CeF32 in Figure 1
82 [32
.. 0] are LaF, 5O mol%, Ce2O mol%, At
The initial luminescence output of the point phosphor containing 30 moles of F was 82%, and after 6 hours of irradiation with ultraviolet light with a wavelength of 185 nm, the luminescence output decreased to 32.0% of the initial luminescence output. represents something. The fluorescent materials shown in FIGS. 1 to 6 were prepared by firing a mixture of the phosphors in each composition ratio in an air atmosphere at a temperature of 800 DEG C. for 30 minutes.

なお、図内の〔 〕で示した発光出力の変化は、光源と
して石英の外管を用いた低圧水銀灯を使用し、空気によ
る紫外線の吸収を避けるため真空中で各螢光体に照射し
て調べた値である。比較例 1第1図に(At,La,
Ce)F3螢光体の比較例を示す。
The changes in luminous output shown in parentheses in the figure were obtained by using a low-pressure mercury lamp with a quartz outer tube as the light source, and irradiating each phosphor in a vacuum to avoid absorption of ultraviolet rays by the air. This is the value we investigated. Comparative Example 1 In Figure 1 (At, La,
A comparative example of Ce) F3 phosphor is shown.

La,At,Ceの3成分より成る螢光体では、185
nmの紫外線が照射されると、その発光出力は初期の値
に対して32.0%乃至57.1%に低下する。比較例
2 第2図に、(At,Y,Ce)F3螢光体の比較例を示
す。
In a phosphor composed of three components, La, At, and Ce, 185
When irradiated with nanometer ultraviolet rays, the luminous output decreases to 32.0% to 57.1% of the initial value. Comparative Example 2 FIG. 2 shows a comparative example of (At, Y, Ce)F3 phosphor.

同図に示すような(At,Y,Ce)F3螢光体であつ
てもその発光出力の変化は大く、最高のものでも44.
9%以下に低下する。
Even with the (At, Y, Ce) F3 phosphor shown in the figure, the luminous output varies greatly, and the highest one is 44.
It decreases to 9% or less.

比較例 3 (Y,La,Ca)F遭光体の比較例を第3図に示す。Comparative example 3 A comparative example of (Y, La, Ca) F photodetector is shown in FIG.

同図の結果からも明らかなように、(Y,La,Ce)
F3螢光体であつても、185nmの紫外線が照射され
ると最も変化率の少ないものでも発光出力は初期値の4
5.2%に低下する。以上のように比較例で示した螢光
体に対し、本発明のPrを含む螢光体は、第4図乃至第
6図に示すように、ある特定範囲では初期の発光出力が
比較的高く、なおかつ、185nmの紫外線が照射され
てもその発光出力が大きく低下しない。
As is clear from the results in the same figure, (Y, La, Ce)
Even with F3 phosphors, when irradiated with 185 nm ultraviolet rays, even the one with the smallest rate of change will lose its initial value of 4.
This decreases to 5.2%. In contrast to the phosphors shown in the comparative examples above, the Pr-containing phosphors of the present invention have a relatively high initial light output in a certain range, as shown in FIGS. 4 to 6. Moreover, even when irradiated with 185 nm ultraviolet rays, the light emission output does not decrease significantly.

実施例 1(Pr,Ce)F3、螢光体の製法の1実施
例を示す。
Example 1 An example of the method for manufacturing (Pr,Ce)F3, a phosphor is shown.

以上の原料を乳鉢中でよく混合、粉砕してプタ,ツキル
ツボに入れ、800℃空気中で30分間焼成した。
The above raw materials were thoroughly mixed in a mortar, pulverized, placed in a pot and fired in air at 800°C for 30 minutes.

このようにして得られた螢光体は、第7図に示すように
、約285nmに発光ピークを有する発光スペクトルを
生じた。また真空中で この螢光体の粉体に185nm
紫外線を6時間照射した後の発光出力は初期値の74.
2%であつた。また、(La,Pr,Ce)F,螢光体
の組成比を変えたときの特性(発光出力と劣化率)を第
4図に示す。同図から明らかなように(La,Pr,C
e)F,螢光体、(Lal−x−YPrxCey)F,
(ただし、0.45≦x<E>0.95,0.05≦y
≦0.55,0.85≦x+y≦1)の範囲で、185
nmの紫外線を照射してもその発光出力は、最大に変化
するものでも初期値の68,3%にしか低下せず、良い
ものでは74.2%にしか低下せず、しかも初期の発光
効率の良いものであつた。
The phosphor thus obtained produced an emission spectrum having an emission peak at about 285 nm, as shown in FIG. In addition, in a vacuum, this phosphor powder was exposed to 185 nm.
After irradiating with ultraviolet rays for 6 hours, the luminous output was 74.
It was 2%. Further, FIG. 4 shows the characteristics (emission output and deterioration rate) when the composition ratio of (La, Pr, Ce) F and the phosphor is changed. As is clear from the figure (La, Pr, C
e) F, fluorophore, (Lal-x-YPrxCey)F,
(However, 0.45≦x<E>0.95, 0.05≦y
185 in the range of ≦0.55, 0.85≦x+y≦1)
Even when irradiated with nanometer ultraviolet rays, the luminous output only decreases to 68.3% of the initial value even in the case where the maximum change occurs, and only 74.2% in the good one, and furthermore, the luminous efficiency decreases from the initial value. It was a good one.

実施例 2 (At,Pr,Ce)F3螢光体の製法の1実施例を示
す。
Example 2 An example of a method for manufacturing an (At, Pr, Ce) F3 phosphor is shown.

しじR3u,J!LgS,V●υリ ζ 5以上の原料
により実施例1と同じ方法で製造した螢光体は約286
nmに発光ピークを有し、実施例1と同条件で185n
m照射試験を行つたところ、照射後の発光出力は初期値
の69.8%であつた。
Shiji R3u, J! The phosphor produced by the same method as in Example 1 using raw materials with LgS, V●υliζ 5 or more was about 286
It has an emission peak at 185 nm under the same conditions as Example 1.
When an irradiation test was conducted, the luminescence output after irradiation was 69.8% of the initial value.

また、その初期値は実施例1の螢光体より約6%高かつ
た。さらに、(At,Pr,Ce)F3螢光体の組成比
を変えたときの特性(発光出力と劣化率)を第5図に示
す。
Further, its initial value was about 6% higher than that of the phosphor of Example 1. Further, FIG. 5 shows the characteristics (emission output and deterioration rate) when the composition ratio of the (At,Pr,Ce)F3 phosphor is changed.

同図から明らかなように(At,Pr,Ce)F3螢光
体であつてもその範囲が(Atl−x−YPrxCey
)・F3(ただし、0.45≦X≦0.95,0.05
≦y≦0.55,0.85≦x+y≦1)であれば、1
85nmの紫外線の照射で発光出力低下が最大のもので
も初期値の62.3%であり最少のものでは74.2%
にしか低下しない。
As is clear from the figure, even if it is an (At, Pr, Ce) F3 fluorophore, its range is (Atl-x-YPrxCey
)・F3 (However, 0.45≦X≦0.95, 0.05
1 if ≦y≦0.55, 0.85≦x+y≦1)
When irradiated with 85 nm ultraviolet light, the maximum reduction in luminous output is 62.3% of the initial value, and the minimum is 74.2%.
It only decreases.

しかもその範囲の螢光体の初期発光出力は充分なものが
得られる。実施例 3(Y,Pr,Ce)F3螢光体の
製法の1実施例を示す。
Moreover, sufficient initial light emission output of the phosphor within this range can be obtained. Example 3 An example of a method for manufacturing a (Y, Pr, Ce) F3 phosphor is shown.

しV/L3Vl易8〜−一 以上の原料を混合して実施例1と同じ方法で製造した螢
光体は、第8図に示すように、約295nmに発光ピー
クを有する発光スペクトルを生じた。
The phosphor produced in the same manner as in Example 1 by mixing one or more raw materials produced an emission spectrum with an emission peak at about 295 nm, as shown in Figure 8. .

また実施例1と同じ条件で185nm照射試験を行つた
ところ、照射後の発光出力は初期値の71.0(!)で
あつた。さらに(Y,Pr,Ce)F3螢光体の組成比
を変えたときの特性(発光出力と劣化率)を第6図に示
す。
Further, when a 185 nm irradiation test was conducted under the same conditions as in Example 1, the light emission output after irradiation was the initial value of 71.0 (!). Further, FIG. 6 shows the characteristics (emission output and deterioration rate) when the composition ratio of the (Y,Pr,Ce)F3 phosphor is changed.

同図に示したように、(Y,Pr,Ce)F3螢光体で
あつても、その範囲が(Y1−x−YPrxCey)F
3(ただし、0.45≦x≦0.95,0,05≦y≦
0.55,0.85≦x+y≦1)であれば、185n
mの紫外線照射に対して初期値の68.0〜74.3%
にしか低下しない。
As shown in the figure, even if it is a (Y,Pr,Ce)F3 phosphor, its range is (Y1-x-YPrxCey)F
3 (However, 0.45≦x≦0.95, 0.05≦y≦
0.55, 0.85≦x+y≦1), then 185n
68.0-74.3% of the initial value for UV irradiation of m
It only decreases.

そして初期発光出力は十分なものである。なお、上記組
成の螢光体を製造する場合、その焼成温度が600℃乃
至1000℃以外であつては発光強度が弱く、さらにそ
の焼成条件は非還元性雰囲気中でなければ所望の発光出
力が得られず、その焼成時間は5分間以上の焼成が必要
であり、5分間未満であつては実用で5きる発光出力を
有する螢光体は得られない。
And the initial light emission output is sufficient. In addition, when manufacturing a phosphor having the above composition, the luminescence intensity will be weak if the firing temperature is other than 600°C to 1000°C, and the desired luminous output may not be achieved unless the firing conditions are in a non-reducing atmosphere. However, the firing time is 5 minutes or more, and if the firing time is less than 5 minutes, a phosphor with a practical luminous output cannot be obtained.

〔発明の効果〕〔Effect of the invention〕

以上述べたように、この発明による螢光体は、その組成
範囲が(M1−x−YPrxCey)F3(ただし、M
=At,YおよびLaのうち少なくとも一種、0.45
≦x≦0.95,0.05≦y≦0.55,0.85≦
x+y≦1)で所定の処理を施したものであれば、18
5nmの紫外線の照射に対する発光出力の低下が少なく
、さらに初期の発光出力も充分ある憂れたものである。
As described above, the phosphor according to the present invention has a composition range of (M1-x-YPrxCey)F3 (However, M
=At least one of At, Y and La, 0.45
≦x≦0.95, 0.05≦y≦0.55, 0.85≦
x + y ≦ 1) and has been subjected to prescribed processing, 18
It is a matter of concern that there is little decrease in luminous output upon irradiation with 5 nm ultraviolet rays, and that the initial luminous output is also sufficient.

すなわち本発明による代表的な螢光体と従来の螢光体に
ついて、それらの初期発光出力、劣化率(185nm紫
外線6時間照射後の発光出力の初期出力に対する百分率
(%))、および劣化後の発光出力を示すと第1表のよ
うになる。
Specifically, for the typical phosphor according to the present invention and the conventional phosphor, their initial luminous output, deterioration rate (percentage (%) of luminous output to the initial output after irradiation with 185 nm ultraviolet rays for 6 hours), and the Table 1 shows the light emission output.

゛5 故に第1表から明らかのように1〜3で示す螢光体は本
発明の螢光体より初期出力の高いものでぁる力(劣化率
が大きいため劣化後の発光出力はほマ50以下(相対値
)である。
5 Therefore, as is clear from Table 1, the phosphors shown in numbers 1 to 3 have a higher initial output than the phosphor of the present invention. 50 or less (relative value).

これに対し本発明による4〜6で示す螢光体は75〜8
6に達し、明らかにすぐれていることがわかる。゛図面
の簡単な説明 第1図乃至第6図は各螢光体の各組成比に於ける発光出
力の特性を示す三元図であつて第4図乃至第6図は本発
明の実施例を示す図であり、第7図および第8図はこの
発明の実施例による発光スベクトルを示す特性図である
On the other hand, the phosphors shown by numbers 4 to 6 according to the present invention are 75 to 8
It reached 6, which shows that it is clearly superior.゛Brief explanation of the drawings Figures 1 to 6 are ternary diagrams showing the characteristics of light emission output at each composition ratio of each phosphor, and Figures 4 to 6 show examples of the present invention. FIG. 7 and FIG. 8 are characteristic diagrams showing the emission vector according to the embodiment of the present invention.

Claims (1)

【特許請求の範囲】 1 (M_1−x−yPrxCey)F_3(ただし、
MはAl、YおよびLaのうち少なくとも一種であり、
0.45≦x≦0.95、0.05≦y≦0.55、0
.85≦x+y≦1である。 )で表わされる組成の混合物を温度600℃乃至100
0℃の非還元性雰囲気中で少なくとも5分間焼成してな
ることを特徴とする紫外部発光螢光体。
[Claims] 1 (M_1-x-yPrxCey)F_3 (However,
M is at least one of Al, Y and La,
0.45≦x≦0.95, 0.05≦y≦0.55, 0
.. 85≦x+y≦1. ) at a temperature of 600°C to 100°C.
An ultraviolet-emitting phosphor characterized in that it is formed by firing in a non-reducing atmosphere at 0°C for at least 5 minutes.
JP15338775A 1975-12-24 1975-12-24 Shigaibuhatsukokeikoutai Expired JPS5919160B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP15338775A JPS5919160B2 (en) 1975-12-24 1975-12-24 Shigaibuhatsukokeikoutai

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP15338775A JPS5919160B2 (en) 1975-12-24 1975-12-24 Shigaibuhatsukokeikoutai

Publications (2)

Publication Number Publication Date
JPS5277888A JPS5277888A (en) 1977-06-30
JPS5919160B2 true JPS5919160B2 (en) 1984-05-02

Family

ID=15561357

Family Applications (1)

Application Number Title Priority Date Filing Date
JP15338775A Expired JPS5919160B2 (en) 1975-12-24 1975-12-24 Shigaibuhatsukokeikoutai

Country Status (1)

Country Link
JP (1) JPS5919160B2 (en)

Also Published As

Publication number Publication date
JPS5277888A (en) 1977-06-30

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