JPS6121505B2 - - Google Patents
Info
- Publication number
- JPS6121505B2 JPS6121505B2 JP7338780A JP7338780A JPS6121505B2 JP S6121505 B2 JPS6121505 B2 JP S6121505B2 JP 7338780 A JP7338780 A JP 7338780A JP 7338780 A JP7338780 A JP 7338780A JP S6121505 B2 JPS6121505 B2 JP S6121505B2
- Authority
- JP
- Japan
- Prior art keywords
- terbium
- yttrium
- scandium
- brightness
- oxide
- 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
Links
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 8
- 229910052727 yttrium Inorganic materials 0.000 description 10
- 229910052771 Terbium Inorganic materials 0.000 description 9
- 238000010304 firing Methods 0.000 description 9
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 9
- 229910052706 scandium Inorganic materials 0.000 description 8
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 8
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 8
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 6
- 230000005284 excitation Effects 0.000 description 6
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 229910003451 terbium oxide Inorganic materials 0.000 description 3
- SCRZPWWVSXWCMC-UHFFFAOYSA-N terbium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Tb+3].[Tb+3] SCRZPWWVSXWCMC-UHFFFAOYSA-N 0.000 description 3
- -1 terbium-yttrium scandium phosphor Chemical compound 0.000 description 3
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910052693 Europium Inorganic materials 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 239000005083 Zinc sulfide Substances 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 238000000295 emission spectrum Methods 0.000 description 2
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium oxide Chemical compound O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 229910052984 zinc sulfide Inorganic materials 0.000 description 2
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000004110 Zinc silicate Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000012190 activator Substances 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
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000001028 reflection method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 235000019352 zinc silicate Nutrition 0.000 description 1
- XSMMCTCMFDWXIX-UHFFFAOYSA-N zinc silicate Chemical compound [Zn+2].[O-][Si]([O-])=O XSMMCTCMFDWXIX-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Luminescent Compositions (AREA)
Description
この発明は電子線および紫外線で励起され、緑
色に発光するテルビウムふ活けい酸イツトリウム
スカンヂウム蛍光体に関するものである。
投写形テレビに用いられているブラウン管は高
い輝度を必要とするところから高電流密度で動作
される。したがつて蛍光面は色調が適当なこと、
電流一輝度特性（ガンマ特性）がよいことのほか
長時間の励起に対しても安定なことが要求され
る。
現在、青発光成分には硫化亜鉛：銀、緑発光成
分としてはけい酸イツトリウム：テルビウウ：赤
発光成分には酸化イツトリウム：ユーロピウムが
用いられている。このうち酸化イツトリワム：ユ
ーロピウムはほゞ満足できる特性を有している。
硫化亜鉛：銀はガンマ特性がやゝ悪いが現在のと
ころこれに替り得る色調、輝度を有するものが開
発されておらず止むを得ず使用されている。けい
酸イツトリウム：テルビウムはよく知られている
けい酸亜鉛：マンガンに比べ色純度はやゝ悪い
が、温度、ガンマ特性にすぐれている。たゞし白
色画面を構成する色配分比はＧ：Ｂ：Ｒそれぞれ
約70：10：20でありＧ成分により画面明るさが支
配されておりその輝度はなるべく高い方が望まし
い。
本発明は、けい酸イツトリウムの一部をスカン
ヂウムで置換することが輝度の改善に有効なこと
を見出し、その組成条件を定めたものである。
ふつう、けい酸イツトリウム：テルビウムは酸
化イツトリウム、酸化テルビウムおよび無水けい
酸の微粉末を混合し、1300℃以上、５容量％の水
素を含むチツ素雰囲気中で焼成して得られる。
焼成は要すれば２回以上行つても差支えない。
原料混合時少量のフツ化アンモンを添加すると、
そのフラツクス作用のため固体反応が進行し易い
ので焼成温度は約1200℃に下げる必要がある。合
成した蛍光体は軽くボールミルを行い篩を透して
使用するが、このときの平均粒径は比表面積径で
ほゞ３〜７ミクロンである。
このけい酸イツトリウムのイツトリウムの一部
を、同じ3b族のスカンヂウムにより置換すると
輝度が改善されることが見出された。すなわち実
用的には通常0.12乃至0.17モルのテルビウムが付
活剤として、導入されているが、この量に対して
ほゞ1/3量のスカンヂウムを添加混合して焼成す
ることにより、約10％の輝度の上昇が得られる。
焼成条件は、スカンヂウムを添加することにより
特に変化させる必要はない。
以下実施例について述べる。
〔実施例 １〕
酸化イツトリウム Y2O3（Ｙとして）1.81モル
酸化テルビウム Tb4O7（Tbとして）0.14〃
酸化スカンヂウム Sc2O3（Scとして）0.05〃
無水けい酸 SiO2 1.00モル
いずれも99.99％以上の純度を有する原料微粉
末を秤量し、エチルアルコールを加えてボールミ
ルにて粉砕混合したのち過乾燥する。
これを高アルミナ質るつぼに充填し1470℃にて
３時間、５容量％の水素を含むチツ素中で保持し
た。焼成後の冷却中にも同様の還元雰囲気で行
う。
〔実施例 ２〕
酸化イツトリウム Y2O3（Ｙとして）1.84モル
酸化テルビウム Yb4O7（Tbとして）0.12
酸化スカンヂウム Sc2O3（Scとして）0.04
無水けい酸 SiO2 1.00
フツ化アンモンNH4Fを上記全量の２重量％こ
れを実施例〔１〕と同様の操作で混合する。ただ
し焼成条件は1250℃にて３時間が適当であつた。
なおこの場合はフラツクスの揮散を少なくする目
的でるつぼに蓋をして焼成した。
このようにして、得られた蛍光体を電子線によ
る励起で輝度を測定したところ以下に示す結果が
えられた。
This invention relates to a terbium-yttrium scandium phosphor that emits green light when excited by electron beams and ultraviolet rays. The cathode ray tubes used in projection televisions require high brightness and are therefore operated at high current densities. Therefore, the color tone of the fluorescent screen must be appropriate;
In addition to having good current-luminance characteristics (gamma characteristics), it is also required to be stable for long-term excitation. Currently, zinc sulfide and silver are used for the blue emitting component, yttrium silicate and terbium are used for the green emitting component, and yttrium oxide and europium are used for the red emitting component. Among these, yttriwaum oxide: europium has almost satisfactory properties.
Zinc sulfide: Silver has rather poor gamma characteristics, but at present no substitute for it with color tone and brightness has been developed, so its use is unavoidable. Yttrium silicate: Terbium has slightly lower color purity than the well-known zinc silicate: manganese, but it has excellent temperature and gamma characteristics. However, the color distribution ratio constituting a white screen is about 70:10:20 for G:B:R, respectively, and the screen brightness is controlled by the G component, and it is desirable that the brightness be as high as possible. The present invention is based on the discovery that replacing a portion of yttrium silicate with scandium is effective in improving brightness, and the compositional conditions thereof have been determined. Yttrium:Terbium silicate is usually obtained by mixing fine powders of yttrium oxide, terbium oxide, and silicic anhydride and firing the mixture at 1300° C. or higher in a nitrogen atmosphere containing 5% by volume of hydrogen. If necessary, firing may be performed two or more times.
When a small amount of ammonium fluoride is added when mixing raw materials,
Because of the flux action, the solid reaction progresses easily, so the firing temperature needs to be lowered to about 1200°C. The synthesized phosphor is lightly ball milled and passed through a sieve before use, and the average particle size at this time is approximately 3 to 7 microns in terms of specific surface area. It has been found that when part of the yttrium in this yttrium silicate is replaced with scandium, which also belongs to Group 3b, the brightness can be improved. In other words, in practice, normally 0.12 to 0.17 moles of terbium are introduced as an activator, but by adding and mixing approximately 1/3 of scandium to this amount and firing, approximately 10% An increase in brightness can be obtained.
The firing conditions do not need to be particularly changed by adding scandium. Examples will be described below. [Example 1] Yttrium oxide Y 2 O 3 (as Y) 1.81 mol Terbium oxide Tb 4 O 7 (as Tb) 0.14〃 Scandium oxide Sc 2 O 3 (as Sc) 0.05 〃 Silicic acid anhydride SiO 2 1.00 mol A raw material fine powder with a purity of 99.99% or more is weighed, ethyl alcohol is added, and the mixture is ground and mixed in a ball mill, followed by over-drying. This was filled into a high alumina crucible and held at 1470°C for 3 hours in a nitrogen atmosphere containing 5% by volume of hydrogen. Cooling after firing is also carried out in a similar reducing atmosphere. [Example 2] Yttrium oxide Y 2 O 3 (as Y) 1.84 mol Terbium oxide Yb 4 O 7 (as Tb) 0.12 Scandium oxide Sc 2 O 3 (as Sc) 0.04 Silicic acid anhydride SiO 2 1.00 Ammonium fluoride NH 4 2% by weight of F based on the above total amount was mixed in the same manner as in Example [1]. However, the firing conditions were appropriate at 1250°C for 3 hours.
In this case, the crucible was fired with a lid on to reduce volatilization of the flux. When the luminance of the thus obtained phosphor was measured by excitation with an electron beam, the following results were obtained.
【表】
励起条件：加速電圧30KV、電流密度10μＡ／
cm2、測定は粉末反射法とよばれる方法であり、粒
径による輝度の差を無視出来るよう試料塗布密度
は10mg／cm2とした。発光スペクトルはいずれも変
化なく第１図にしめすごとくであつた。
またスカンヂウム含有の差による結晶形の変化
をＸ線パターンで求めたが、これも著るしい差は
みられなかつた。
なお、254mm紫外線励起下でも明るく発光す
る。周知の如く試料間に粒径に依存する紫外線の
吸収率の差があり、これを補正するとほぼ同様な
輝度値をしめした。
第２図は本発明による蛍光体のと従来の蛍光体
ｂの電流−輝度特性を示している。
以上に述べたことについて考察すると、けい酸
イツトリウムのイツトリウムをテルビウムが置換
する場合、そのイオン半径の差を無視出来ない。
すなわち、Y3+0.893Åに対しTb3+0.923Åであり
当然結晶に“ひずみ”が生ずる。これに
Sc3+0.732Åを添加したとき体積的に補償されて
安定するものと考える。スカンヂウム量がテルビ
ウムの量の約1/3で効果のあることも、両者のイ
ツトリウムイオン半径に対する大きさの差に起因
するものであろう。
なお、テルビウムの量を0.12〜0.18モルとした
のは、実用的に充分輝度を示すためである。スカ
ンヂウム添加の効果が表１における如く、約10％
と僅かであるが、もとのけい酸イツトリウム：テ
ルビウム自体すでに非常に優れた特性を有してお
り、これを大きく向上させることは甚だ困難な問
題である。
しかしながら、実用的には少しでも輝度の高い
ものが望まれているのが現状であり、その効果は
充分認められる。なお、輝度差が明らかに認め得
られる判定の条件としては、前記したように、高
電圧、高電流の負荷により励起された場合であ
り、紫外線励起の場合は明確な差が見られないの
は、その励起負荷密度が低いことと、侵入電子に
よる結晶格子の振動作用が含まれていないことと
考える。
なお、実施例に示したように、合成条件の僅か
な差、すなわち、テルビウム、スカンヂウムの量
およびその比は、一般式Y2−ｘ−ｙ
ScxTbySiO5で表わされるものにおいて、ｘおよ
びｙのモル比がｘ＝ｙ／２〜４，ｙ＝0.12〜0.18
の組成が許容される。
また、焼成温度、時間および焼成雰囲気は、こ
の種けい光物質製造の通念として、それ程厳密な
ものではない。[Table] Excitation conditions: Acceleration voltage 30KV, current density 10μA/
cm 2 , was measured by a method called powder reflection method, and the sample coating density was set to 10 mg/cm 2 so that differences in brightness due to particle size could be ignored. The emission spectra were as shown in FIG. 1 without any change. In addition, changes in crystal form due to differences in scandium content were determined using X-ray patterns, but no significant differences were observed. Furthermore, it emits bright light even under 254mm ultraviolet excitation. As is well known, there is a difference in the ultraviolet absorption rate between the samples depending on the particle size, and when this is corrected, the brightness values are almost the same. FIG. 2 shows the current-luminance characteristics of the phosphor according to the present invention and the conventional phosphor b. Considering the above, when terbium replaces yttrium in yttrium silicate, the difference in ionic radius cannot be ignored.
That is, Y 3+ is 0.893 Å while Tb 3+ is 0.923 Å, which naturally causes “strain” in the crystal. to this
It is assumed that when 0.732 Å of Sc 3+ is added, it is volumetrically compensated and stabilized. The fact that the amount of scandium is effective at about 1/3 of the amount of terbium is also probably due to the difference in size with respect to the radius of the yttrium ions. The reason why the amount of terbium is set to 0.12 to 0.18 mol is to provide sufficient brightness for practical use. As shown in Table 1, the effect of scandium addition is approximately 10%.
However, the original yttrium/terbium silicate itself already has very excellent properties, and it is an extremely difficult problem to significantly improve these properties. However, for practical purposes, it is currently desired to have as high a luminance as possible, and its effects are well recognized. As mentioned above, the condition for determining that a brightness difference can be clearly recognized is when excited by a high voltage and high current load, and in the case of ultraviolet excitation, no clear difference can be seen. This is thought to be due to the low excitation load density and the fact that the crystal lattice vibration effect due to intruding electrons is not included. As shown in the examples, slight differences in the synthesis conditions, i.e., the amounts of terbium and scandium and their ratio, are determined by the general formula Y 2 -x-y
In what is represented by ScxTbySiO 5 , the molar ratio of x and y is x=y/2~4, y=0.12~0.18
Compositions of are permissible. Furthermore, the firing temperature, time and firing atmosphere are not so strict as is generally accepted in the production of this type of fluorescent material.
第１図は本発明にかゝる蛍光体の発光スペクト
ルを示す図、第２図は本発明による蛍光体と従来
の蛍光体の電流輝度特性を示す特性図である。
FIG. 1 is a diagram showing the emission spectrum of the phosphor according to the present invention, and FIG. 2 is a characteristic diagram showing the current luminance characteristics of the phosphor according to the present invention and the conventional phosphor.
Claims (1)
され、ｘおよびｙのモル比が、 ｘ＝ｙ／２〜４ ｙ＝0.12〜0.18 の組成であることを特徴とする蛍光体。[Claims] 1 It is represented by the general formula Y 2 -x-y Scx Tby SiO 5 and characterized in that the molar ratio of x and y is x=y/2-4 y=0.12-0.18. phosphor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7338780A JPS56167783A (en) | 1980-05-28 | 1980-05-28 | Fluorescent substance |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7338780A JPS56167783A (en) | 1980-05-28 | 1980-05-28 | Fluorescent substance |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS56167783A JPS56167783A (en) | 1981-12-23 |
| JPS6121505B2 true JPS6121505B2 (en) | 1986-05-27 |
Family
ID=13516724
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7338780A Granted JPS56167783A (en) | 1980-05-28 | 1980-05-28 | Fluorescent substance |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS56167783A (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0331738B1 (en) * | 1987-08-10 | 1996-11-27 | Mitsubishi Denki Kabushiki Kaisha | Green light emitting rare gas discharge lamp |
| JP3872472B2 (en) | 2003-11-12 | 2007-01-24 | 日亜化学工業株式会社 | Green light emitting yttrium silicate phosphor for projection tube and projection tube using the same |
| JP4272973B2 (en) | 2003-11-13 | 2009-06-03 | Ｎｅｃライティング株式会社 | Vacuum ultraviolet light excited green phosphor material and light emitting device using the same |
| JP4679180B2 (en) * | 2005-03-01 | 2011-04-27 | Ｎｅｃライティング株式会社 | Red vacuum ultraviolet excited phosphor and light emitting device using the same |
| JP4890777B2 (en) * | 2005-03-29 | 2012-03-07 | Ｎｅｃライティング株式会社 | Vacuum ultraviolet light-excited phosphor and light emitting device using the same |
| JP4927352B2 (en) | 2005-05-31 | 2012-05-09 | 株式会社 日立ディスプレイズ | Image display device |
| CN102191053B (en) * | 2010-03-01 | 2013-07-24 | 海洋王照明科技股份有限公司 | Preparation method of silicate luminescent material and silicate luminescent material prepared by same |
-
1980
- 1980-05-28 JP JP7338780A patent/JPS56167783A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS56167783A (en) | 1981-12-23 |
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