JPH0790262A - Production of fluorescent material for electroluminescence element - Google Patents
Production of fluorescent material for electroluminescence elementInfo
- Publication number
- JPH0790262A JPH0790262A JP5239313A JP23931393A JPH0790262A JP H0790262 A JPH0790262 A JP H0790262A JP 5239313 A JP5239313 A JP 5239313A JP 23931393 A JP23931393 A JP 23931393A JP H0790262 A JPH0790262 A JP H0790262A
- Authority
- JP
- Japan
- Prior art keywords
- phosphor
- firing
- fluorescent
- fluorescent material
- activator
- 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.)
- Withdrawn
Links
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 239000000463 material Substances 0.000 title abstract description 7
- 238000005401 electroluminescence Methods 0.000 title abstract description 6
- 239000002245 particle Substances 0.000 claims abstract description 29
- 150000002681 magnesium compounds Chemical class 0.000 claims abstract description 8
- 150000001880 copper compounds Chemical class 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 239000005749 Copper compound Substances 0.000 claims abstract description 4
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims abstract 4
- 239000003795 chemical substances by application Substances 0.000 claims abstract 4
- 229910001629 magnesium chloride Inorganic materials 0.000 claims abstract 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 47
- 238000010304 firing Methods 0.000 claims description 28
- 239000011159 matrix material Substances 0.000 claims description 15
- 239000012190 activator Substances 0.000 claims description 10
- 239000005083 Zinc sulfide Substances 0.000 claims description 7
- 229910052984 zinc sulfide Inorganic materials 0.000 claims description 7
- 150000004820 halides Chemical class 0.000 claims description 5
- 239000007952 growth promoter Substances 0.000 claims description 4
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical group [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 claims description 2
- 125000005843 halogen group Chemical group 0.000 claims 1
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 abstract description 12
- 238000009826 distribution Methods 0.000 abstract description 10
- 229910052943 magnesium sulfate Inorganic materials 0.000 abstract description 6
- 235000019341 magnesium sulphate Nutrition 0.000 abstract description 6
- 239000006185 dispersion Substances 0.000 abstract description 5
- -1 halide compound Chemical class 0.000 abstract 3
- 230000003213 activating effect Effects 0.000 abstract 2
- 230000004907 flux Effects 0.000 description 15
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 239000011812 mixed powder Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 101100496858 Mus musculus Colec12 gene Proteins 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013039 cover film Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229920006122 polyamide resin Polymers 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Electroluminescent Light Sources (AREA)
- Luminescent Compositions (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、特に分散型電界発光素
子の発光層等に使用される蛍光体の製造方法に関するも
のである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a phosphor used in a light emitting layer of a dispersion type electroluminescent device.
【０００２】[0002]
【従来の技術】液晶ディスプレイパネルのバックライト
等に使用される有機分散型電界発光灯（以下、ＥＬパネ
ルと称す）を図２（ａ）（ｂ）を参照して以下に示す。
上記ＥＬパネル（１）は、背面電極（２）と反射絶縁層
（３）と発光層（４）と透明電極（５）とを順次、積層
して形成された電界発光素子（６）の上下にポリアミド
樹脂等の吸湿フィルム（７）を配置し、吸湿フィルム
（７）を含む電界発光素子（６）の全体をフッ素系樹脂
等からなる外皮フィルム（８）で気密に封止すると共
に、背面電極（２）及び透明電極（５）から外皮フィル
ム（８）の封止部位を通ってリード（９）（10）を導出
したものである。2. Description of the Related Art An organic dispersion type electroluminescent lamp (hereinafter referred to as an EL panel) used for a backlight of a liquid crystal display panel or the like is shown below with reference to FIGS.
The EL panel (1) comprises an electroluminescent device (6) formed by laminating a back electrode (2), a reflective insulating layer (3), a light emitting layer (4) and a transparent electrode (5) in this order. A hygroscopic film (7) such as a polyamide resin is arranged on the back surface, and the entire electroluminescent element (6) including the hygroscopic film (7) is hermetically sealed with an outer skin film (8) made of a fluororesin or the like, The leads (9) and (10) are led out from the electrode (2) and the transparent electrode (5) through the sealing portion of the outer cover film (8).
【０００３】上記発光層（４）は、図２（ｃ）に示すよ
うに、有機バインダ（11）に、銅で活性化した硫化亜鉛
（ＺｎＳ）等の蛍光体（12）を分散させることによって
形成され、有機バインダ（11）により反射絶縁層（３）
に接着されている。上記ＥＬパネル（１）では、リード
（９）（10）から背面電極（２）と透明電極（５）間に
高電圧を印加することによって、両電極（２）（５）間
に挟まれた発光層（４）の蛍光体（12）を発光させ、所
望の発光輝度で駆動させている。As shown in FIG. 2 (c), the light emitting layer (4) is formed by dispersing a phosphor (12) such as zinc sulfide (ZnS) activated by copper in an organic binder (11). Reflective insulation layer (3) formed by organic binder (11)
Is glued to. In the EL panel (1), the electrodes (2) and (5) were sandwiched between the electrodes (2) and (5) by applying a high voltage from the leads (9) and (10) between the back electrode (2) and the transparent electrode (5). The phosphor (12) of the light emitting layer (4) is caused to emit light and is driven at a desired emission brightness.
【０００４】上記蛍光体（12）は、一般的に粒状硫化亜
鉛（ＺｎＳ）を蛍光母体とし、それに銅化合物（ＣｕＳ
Ｏ4）からなる付活剤、及び塩化物（ＭｇＣｌ2、ＮａＣ
ｌ、ＳｒＣｌ2）からなる共付活剤兼用粒成長促進剤
（フラックス）を添加した混合粉末を焼成して得られ
る。そして、１〜３μｍ径の蛍光母体原料をフラックス
により２０〜３０μｍ径まで粒成長させて長寿命化を図
ると共に、銅と塩素を発光中心としてドーピングし、高
輝度化を図る。The above phosphor (12) is generally made of granular zinc sulfide (ZnS) as a phosphor matrix, and a copper compound (CuS) is added thereto.
O 4 ) activator and chlorides (MgCl 2 , NaC
It is obtained by firing a mixed powder to which a co-activator and grain growth promoter (flux) composed of SrCl 2 ) is added. Then, a fluorescent host material having a diameter of 1 to 3 μm is grain-grown with a flux to a diameter of 20 to 30 μm to prolong the life, and at the same time, copper and chlorine are doped as emission centers to achieve high brightness.
【０００５】そこで、上記蛍光体（１）を形成する際、
まずＺｎＳ（蛍光母体）１ｍｏｌに対してＣｕＳＯ
4（付活剤）を０．１〜０．２ｍｏｌ％添加して乾燥処
理する。次に、図２（ｄ）に示すように、ＭｇＣｌ2の
３ｍｏｌ％と、ＮａＣｌの３ｍｏｌ％と、ＳｒＣｌ2の
３ｍｏｌ％とを混合してなるフラックス（12a）を蛍光
母体（12b）の微粉末と共にルツボ（13）内に供給す
る。そして、ルツボ（13）内で上記混合粉末を１１５０
°Ｃで６時間、加熱して一次焼成すると、まずフラック
ス（12a）（融点７００°Ｃ）が溶融して液状となり、
ルツボ内の底部付近に溜まって逐次、蒸気となる。そこ
で、ルツボ内を攪拌すると、フラックス（12a）が分散
すると共に、その融液又は蒸気を介して蛍光母体粒子が
互いに溶融・結合し合って次第に粒径が大きく成長す
る。上記一次焼成後、水洗してフラックス分を除去し乾
燥させて中間蛍光体を形成すると、それをラバープレス
等にて静的に加圧する。次に、７００°Ｃで１時間、二
次焼成（アニール）し、更に、酸（ＨＣｌ）及びシアン
（ＫＣＮ）洗浄して蛍光体表面の余剰の銅化合物を除去
した後、水洗してシアン成分を除去し、乾燥させて分級
（ふるい分け）すると、所望の電界発光素子用蛍光体を
得る。Therefore, when forming the phosphor (1),
First, CuSO for 1 mol of ZnS (fluorescent matrix)
4 (Activator) is added in an amount of 0.1 to 0.2 mol% and dried. Next, as shown in FIG. 2D, a flux (12a) obtained by mixing 3 mol% of MgCl 2 , 3 mol% of NaCl, and 3 mol% of SrCl 2 is used as a fine powder of the phosphor matrix (12b). It is also supplied into the crucible (13). Then, in the crucible (13), 1150 the above-mentioned mixed powder.
When heated at 6 ° C for 6 hours and fired for the first time, the flux (12a) (melting point 700 ° C) melts and becomes liquid.
It accumulates near the bottom of the crucible and becomes vapor sequentially. Then, when the inside of the crucible is stirred, the flux (12a) is dispersed, and the phosphor base particles are fused and bonded to each other through the melt or vapor, and the particle size gradually grows. After the primary firing, the flux is removed by washing with water and drying to form an intermediate phosphor, which is statically pressed by a rubber press or the like. Next, after secondary baking (annealing) at 700 ° C. for 1 hour, further washing with acid (HCl) and cyan (KCN) to remove excess copper compound on the surface of the phosphor, and then washing with water to prepare a cyan component. Are removed, dried, and classified (sieved) to obtain a desired phosphor for an electroluminescent device.
【０００６】[0006]
【発明が解決しようとする課題】解決しようとする課題
は、一次焼成時のフラックス量が蛍光母体１ｍｏｌに対
して１０ｍｏｌ％以下であるため、フラックス（12a）
が溶融すると、ルツボ内で蒸気になり、蛍光母体（12
b）の粒子を覆いつつ結合し合って粒成長し、フラッ ク
ス蒸気による固相反応が主体となる。フラックス蒸気が
存在している領域では、粒子が十分に成長する一方、フ
ラックス蒸気が不十分であると、粒子の未成長や不十分
な成長粒子も生じ、成長した粒子が不揃いになって粒度
分布が広くなり、輝度や寿命が低下したり、或いは収率
が低下し、又、粒形状が不安定になって電界が加わり難
くなるという不具合が生じる。又、固相反応によれば、
異なる結晶軸を持つ粒子が結合してそのまま粒成長し易
いため、それにより粒子の各結晶軸方向によって電界の
加わり方が異なり、蛍光母体（12b）として輝度が低下
す るという不具合もある。この場合、高温で長時間、
焼成すれば、粒子の各結晶軸方向が揃い易くなるが、焼
成条件を無闇に変えることは出来ず、実際上、実施不能
である。The problem to be solved is that the amount of flux during the primary firing is 10 mol% or less with respect to 1 mol of the phosphor matrix, so the flux (12a)
When melted, it becomes vapor in the crucible, and the phosphor matrix (12
The particles of b) are covered and bonded to each other to grow the particles, and the solid-phase reaction by the flux vapor is the main component. In the area where flux vapor is present, the particles grow sufficiently, but when the flux vapor is insufficient, ungrown particles or insufficiently grown particles also occur, and the grown particles become uneven and the particle size distribution Becomes wider, the brightness and life are reduced, the yield is reduced, and the grain shape becomes unstable, which makes it difficult to apply an electric field. Moreover, according to the solid phase reaction,
Since particles having different crystal axes are likely to be bonded and grow as they are, the way the electric field is applied differs depending on the crystal axis directions of the particles, and the brightness of the phosphor matrix (12b) decreases. In this case, at high temperature for a long time,
If firing is performed, the crystal axis directions of the particles are easily aligned, but firing conditions cannot be changed indiscriminately, which is practically impossible.
【０００７】[0007]
【課題を解決するための手段】本発明は、蛍光母体に付
活剤と共付活剤兼用粒成長促進剤とを添加した混合物を
高温で一次焼成し、蛍光母体粒子を所定径に成長させて
中間蛍光体を得た後、それを二次焼成して蛍光体を形成
するにあたり、上記一次焼成時及び／又は二次焼成時に
ハロゲン化物以外のマグネシウム化合物を蛍光母体１ｍ
ｏｌに対し０．１〜１０ｍｏｌ％添加することを特徴と
する。According to the present invention, a mixture of an activator and a co-activator / granular growth accelerator added to a phosphor matrix is primarily fired at a high temperature to grow the phosphor matrix particles to a predetermined diameter. In order to form a phosphor by secondarily firing the intermediate phosphor after obtaining the intermediate phosphor, a magnesium compound other than a halide is added to the phosphor host 1 m during the above-mentioned primary firing and / or second firing.
It is characterized in that 0.1 to 10 mol% is added to ol.
【０００８】[0008]
【作用】上記技術的手段によれば、蛍光母体の粒成長反
応の際、マグネシウム化合物の添加により未成長粒子の
発生が消滅し、粒径及び形状が揃って安定化する。According to the above technical means, during the grain growth reaction of the phosphor matrix, the addition of the magnesium compound eliminates the generation of ungrown grains and stabilizes the grain size and shape.
【０００９】[0009]
【実施例】本発明に係る電界発光素子用蛍光体の製造方
法の実施例を図１（ａ）（ｂ）を参照して以下に説明す
る。本発明の特徴は、２段焼成により電界発光素子用蛍
光体を形成するにあたり、一次焼成時及び／又は二次焼
成時にフラックス用ハロゲン化物以外のマグネシウム化
合物、例えばＭｇＳＯ4（硫酸マグネシウム）を蛍光母
体１ｍｏｌに対し０．１〜１０ｍｏｌ％添加することで
ある。上記フラックスとしては、アルカリ金属やアルカ
リ土類金属のハロゲン化物を複数種類、選択的に使用す
れば良い。EXAMPLE An example of a method for manufacturing a phosphor for an electroluminescent device according to the present invention will be described below with reference to FIGS. 1 (a) and 1 (b). The feature of the present invention is that when a phosphor for an electroluminescent device is formed by two-step firing, a magnesium compound other than a halide for a flux, for example, MgSO 4 (magnesium sulfate) is used as a phosphor host during primary firing and / or secondary firing. That is, 0.1 to 10 mol% is added to 1 mol. As the above-mentioned flux, plural kinds of halides of alkali metals or alkaline earth metals may be selectively used.
【００１０】上記手段に基づき本発明を説明する。まず
ＺｎＳ（蛍光母体）の１ｍｏｌに対してＣｕＳＯ4（付
活剤）を０．１〜０．２ｍｏｌ％添加して乾燥処理し、
且つ、ＭｇＳＯ4を０．１〜１０ｍｏｌ％添加して湿式
又は乾式により混合する。次に、図２（ｄ）と同様に、
ＭｇＣｌ2１０ｍｏｌ％及びＮａＣｌ１ｍｏｌ％を混合
してなるフラックス（共付活剤兼用粒成長促進剤）（12
a）を硫酸マグネシウム添加の蛍光母体（12b）の微粉末
と共にルツボ（13）内に供給する。そして、ルツボ（1
3）内で上記混合粉末を１１００°Ｃで３時間、大気雰
囲気中で加熱及び攪拌して一次焼成する。上記一次焼成
後、水洗して残留フラックス分を除去し、１２０°Ｃで
１２時間、加熱して乾燥させ、中間蛍光体を形成する
と、それをボールミル等により動的に加圧して外力を加
える。次に、７５０°Ｃで３時間、アニール（二次焼
成）した後、酸（ＨＣｌ）及びシアン（ＫＣＮ）洗浄す
る。そして、１２０°Ｃで１２時間、加熱して乾燥さ
せ、分級して所望の電界発光素子用蛍光体を得る。The present invention will be described based on the above means. First, CuSO 4 (activator) was added in an amount of 0.1 to 0.2 mol% with respect to 1 mol of ZnS (fluorescent matrix), followed by drying treatment.
Also, 0.1 to 10 mol% of MgSO 4 is added and mixed by a wet or dry method. Next, as in FIG. 2 (d),
Flux consisting of MgCl 2 10 mol% and NaCl 1 mol% (co-activator and grain growth promoter) (12
(a) is supplied into the crucible (13) together with fine powder of the fluorescent substance (12b) containing magnesium sulfate. And the crucible (1
In 3), the mixed powder is heated and stirred in an air atmosphere at 1100 ° C. for 3 hours for primary firing. After the above primary firing, the residual flux is removed by washing with water, and after heating and drying at 120 ° C. for 12 hours to form an intermediate phosphor, it is dynamically pressed by a ball mill or the like to apply an external force. Next, after annealing (secondary baking) at 750 ° C. for 3 hours, acid (HCl) and cyan (KCN) cleaning is performed. Then, it is heated at 120 ° C. for 12 hours, dried, and classified to obtain a desired phosphor for an electroluminescence device.
【００１１】上記実施例によれば、一次焼成時の蛍光母
体（12b）の粒成長反応の際、硫酸マグネシウムを添加
することにより未成長や不足成長粒子の発生が消滅し、
粒径及び形状が揃って安定化する。又、一次焼成後に外
力を加えることにより中間蛍光体粒子の内部に歪みが生
じ、更に、二次焼成によって粒子内で均一に分散してい
た銅が移動して歪みの部分に集まり、粒子内に導電層が
生じ（偏析）、発光中心（銅、塩素）が効率良く電界発
光する。この時、粒径及び形状が均一に揃っているた
め、外力を加える際、粒子に一個ずつ均等に応力が加わ
って上記歪みが均等に形成され、輝度向上に寄与する。According to the above-mentioned embodiment, during the grain growth reaction of the phosphor matrix (12b) during the primary firing, the addition of magnesium sulfate eliminates the generation of ungrown or undergrown grains,
The particle size and shape are uniform and stable. Further, by applying an external force after the primary firing, distortion occurs inside the intermediate phosphor particles, and further, the copper that has been uniformly dispersed in the particles is moved by the secondary firing and gathers in the distorted portion, A conductive layer is formed (segregation), and the luminescent centers (copper and chlorine) efficiently perform electroluminescence. At this time, since the particle size and the shape are uniform, when the external force is applied, the stress is evenly applied to the particles one by one, and the strain is uniformly formed, which contributes to the improvement of the brightness.
【００１２】ここで、図１（ａ）に示す粒度分布測定グ
ラフによれば、本発明の硫酸マグネシウム添加時におけ
る粒度分布図（Ａ）（破線）は、従来の硫酸マグネシウ
ム未添加時における粒度分布図（Ｂ）（実線）に比べて
先鋭になり、分布が狭くなることが知られる。又、図１
（ｂ）に示す輝度測定グラフによれば、本発明実施例に
おいて輝度は、従来よりも１０〜２５％向上することが
知られる。Here, according to the particle size distribution measurement graph shown in FIG. 1 (a), the particle size distribution diagram (A) (broken line) when magnesium sulfate of the present invention is added shows the particle size distribution when magnesium sulfate is not added in the conventional case. It is known that the distribution becomes sharper and the distribution becomes narrower than that in the diagram (B) (solid line). Moreover, FIG.
According to the luminance measurement graph shown in (b), it is known that the luminance in the example of the present invention is improved by 10 to 25% as compared with the conventional case.
【００１３】尚、上記マグネシウム化合物としては、硫
酸マグネシウムの他、酸化マグネシウムや硝酸マグネシ
ウム等も好適である。又、一次焼成時に代えて二次焼成
時にマグネシウム化合物を所定量添加しても同様の効果
を得ることが出来、又、一次及び二次焼成時の両方に添
加しても良い。この場合、各焼成時の添加量をやや減ら
し、その総量を単独の添加量に適合させれば良い。As the above magnesium compound, magnesium oxide, magnesium oxide, magnesium nitrate and the like are also suitable. The same effect can be obtained by adding a predetermined amount of the magnesium compound during the secondary firing instead of during the primary firing, or may be added during both the primary and secondary firings. In this case, the addition amount at each firing may be slightly reduced, and the total amount may be adapted to the individual addition amount.
【００１４】[0014]
【発明の効果】本発明によれば、２段焼成して電界発光
素子用蛍光体を形成する際、一次焼成時及び／又は二次
焼成時にハロゲン化物以外のマグネシウム化合物を蛍光
母体１ｍｏｌに対し０．１〜１０ｍｏｌ％添加したか
ら、蛍光母体の粒成長反応において粒径及び形状が均一
に揃い、輝度向上及び長寿命化を図ることが出来、又、
粒度分布が狭くなって収率が向上する。EFFECTS OF THE INVENTION According to the present invention, when a phosphor for an electroluminescent device is formed by two-step firing, magnesium compounds other than halides are added to 1 mole of the fluorescent host during primary firing and / or secondary firing. Since 1 to 10 mol% is added, the grain size and shape are uniformly aligned in the grain growth reaction of the phosphor matrix, and it is possible to improve the brightness and prolong the life.
The particle size distribution is narrowed and the yield is improved.
【図１】（ａ）は本発明に係る電界発光素子用蛍光体の
製造方法による粒度分布グラフである。（ｂ）は本発明
に係る電界発光素子用蛍光体の製造方法による電力に対
する輝度分布グラフである。FIG. 1A is a particle size distribution graph according to a method for manufacturing a phosphor for an electroluminescent device according to the present invention. (B) is a luminance distribution graph with respect to electric power according to the method for manufacturing a phosphor for an electroluminescent device according to the present invention.
【図２】（ａ）は有機分散型電界発光灯の一例を示す側
断面図である。（ｂ）は有機分散型電界発光灯の一例を
示す平面図である。（ｃ）は発光層の部分側断面図であ
る。（ｄ）は従来の電界発光素子用蛍光体の製造方法の
実施例の一工程を示すルツボの側断面図である。FIG. 2A is a side sectional view showing an example of an organic dispersion type electroluminescent lamp. (B) is a top view which shows an example of an organic dispersion type electroluminescent lamp. (C) is a partial side sectional view of a light emitting layer. FIG. 3D is a side sectional view of the crucible showing a step of an example of a conventional method for manufacturing a phosphor for an electroluminescence device.
12a 粒成長促進剤 12b 蛍光母体 12a Grain growth promoter 12b Fluorescent matrix
Claims (3)
促進剤とを添加した混合物を高温で一次焼成し、蛍光母
体粒子を所定径に成長させて中間蛍光体を得た後、それ
を二次焼成して蛍光体を形成するにあたり、上記一次焼
成時及び／又は二次焼成時にハロゲン化物以外のマグネ
シウム化合物を蛍光母体１ｍｏｌに対し０．１〜１０ｍ
ｏｌ％添加することを特徴とする電界発光素子用蛍光体
の製造方法。1. A mixture obtained by adding an activator and a co-activator / granular growth accelerating agent to a phosphor matrix is primarily fired at a high temperature to grow the phosphor matrix particles to a predetermined diameter to obtain an intermediate phosphor. When the second firing is performed to form a phosphor, a magnesium compound other than a halide is used in the first firing and / or the second firing in an amount of 0.1 to 10 m with respect to 1 mol of the phosphor host.
A method for producing a phosphor for an electroluminescent device, characterized in that the phosphor is added in an amount of ol%.
に外力を加えた後、二次焼成することを特徴とする請求
項１記載の電界発光素子用蛍光体の製造方法。2. The method for producing a phosphor for an electroluminescent device according to claim 1, wherein an external force is statically or dynamically applied to the intermediate phosphor after the primary firing, and then the secondary firing is performed.
物、そして粒成長促進剤は塩化マグネシウムを含むハロ
ゲン化物であることを特徴とする請求項１及び２記載の
電界発光素子用蛍光体の製造方法。3. The phosphor for an electroluminescent device according to claim 1, wherein the phosphor base is zinc sulfide, the activator is a copper compound, and the grain growth promoter is a halide containing magnesium chloride. Manufacturing method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5239313A JPH0790262A (en) | 1993-09-27 | 1993-09-27 | Production of fluorescent material for electroluminescence element |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5239313A JPH0790262A (en) | 1993-09-27 | 1993-09-27 | Production of fluorescent material for electroluminescence element |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0790262A true JPH0790262A (en) | 1995-04-04 |
Family
ID=17042861
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5239313A Withdrawn JPH0790262A (en) | 1993-09-27 | 1993-09-27 | Production of fluorescent material for electroluminescence element |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0790262A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100295401B1 (en) * | 1997-10-28 | 2001-11-05 | 가네꼬 히사시 | Fluorescent material manufacturing method |
| JP2002173676A (en) * | 2000-12-07 | 2002-06-21 | Toshiba Corp | High-lifetime electroluminescent phosphor and electroluminescent device using the same |
| JP2006008855A (en) * | 2004-06-25 | 2006-01-12 | Nemoto & Co Ltd | Red light emitting phosphor and method for producing the same |
| US7135130B2 (en) | 2003-02-12 | 2006-11-14 | Nemoto & Co. Ltd. | Electroluminescent phosphor and its production method |
| WO2008062693A1 (en) * | 2006-11-21 | 2008-05-29 | Kuraray Luminas Co., Ltd. | Process for producing phosphor precursor |
| JP2008251487A (en) * | 2007-03-30 | 2008-10-16 | Tdk Corp | Light-emitting element |
| WO2010114156A1 (en) * | 2009-03-31 | 2010-10-07 | Fujifilm Corporation | Dispersion-type electroluminescence device |
-
1993
- 1993-09-27 JP JP5239313A patent/JPH0790262A/en not_active Withdrawn
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100295401B1 (en) * | 1997-10-28 | 2001-11-05 | 가네꼬 히사시 | Fluorescent material manufacturing method |
| JP2002173676A (en) * | 2000-12-07 | 2002-06-21 | Toshiba Corp | High-lifetime electroluminescent phosphor and electroluminescent device using the same |
| US7135130B2 (en) | 2003-02-12 | 2006-11-14 | Nemoto & Co. Ltd. | Electroluminescent phosphor and its production method |
| JP2006008855A (en) * | 2004-06-25 | 2006-01-12 | Nemoto & Co Ltd | Red light emitting phosphor and method for producing the same |
| WO2008062693A1 (en) * | 2006-11-21 | 2008-05-29 | Kuraray Luminas Co., Ltd. | Process for producing phosphor precursor |
| JP5300490B2 (en) * | 2006-11-21 | 2013-09-25 | 株式会社クラレ | Method for producing phosphor precursor |
| JP2008251487A (en) * | 2007-03-30 | 2008-10-16 | Tdk Corp | Light-emitting element |
| WO2010114156A1 (en) * | 2009-03-31 | 2010-10-07 | Fujifilm Corporation | Dispersion-type electroluminescence device |
| JP2010257961A (en) * | 2009-03-31 | 2010-11-11 | Fujifilm Corp | Dispersive electroluminescence device |
| US8558447B2 (en) | 2009-03-31 | 2013-10-15 | Fujifilm Corporation | Dispersion-type electroluminescence device |
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