WO2006004021A1 - Light-storing compound and method for producing same - Google Patents

Light-storing compound and method for producing same Download PDF

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Publication number
WO2006004021A1
WO2006004021A1 PCT/JP2005/012134 JP2005012134W WO2006004021A1 WO 2006004021 A1 WO2006004021 A1 WO 2006004021A1 JP 2005012134 W JP2005012134 W JP 2005012134W WO 2006004021 A1 WO2006004021 A1 WO 2006004021A1
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Prior art keywords
compound
phosphorescent
oxide
light
storing
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PCT/JP2005/012134
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French (fr)
Japanese (ja)
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Yuji Ueno
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Media Com International Co., Ltd.
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Priority to JP2006528831A priority Critical patent/JPWO2006004021A1/en
Publication of WO2006004021A1 publication Critical patent/WO2006004021A1/en

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials

Definitions

  • the present invention relates to a phosphorescent compound and a method for producing the phosphorescent compound, and more particularly to a phosphorescent compound to which a luminance enhancer for improving the luminance and afterglow time of a phosphorescent oxide is added and a method for producing the same.
  • phosphorescent oxides When this energy storage oxide absorbs energy such as light, it stores the energy and emits light. Based on such a light emission phenomenon, phosphorescent materials are used as luminescent products such as luminescent sheets as advertising media and signs and display boards that emit light at night.
  • Patent Document 1 discloses an aluminate phosphorescent phosphor “MA1 O: XK-YL-ZPJ [provided that
  • M is a kind of metal selected from the group consisting of calcium, norlium, strontium, magnesium, and mixtures thereof;
  • X is an activator that also consists of Pylum, Y, and ⁇ are lanthanum series elements, and manganese, tin, and Bisumasuka group consisting force selected vehicles Katsusukezai;
  • kappa is 0.001 to 10, L at mole 0/0 for Micromax, the molar 0/0 0 ⁇ optimum 10 for Micromax, and ⁇ Represents 0 to 10 in terms of mol% with respect to soot.
  • the technology of the luminescent composite sheet using the above is disclosed.
  • Patent Document 1 Japanese Patent Laid-Open No. 10-114030
  • an object of the present invention is to provide a phosphorescent compound having improved luminance and afterglow time without increasing the amount of phosphorescent oxide used, and a method for producing the same.
  • Means for solving the problem [0006] As a result of intensive studies to solve the problem, the present inventor has found that a specific compound improves the luminous power of the phosphorescent oxide, and based on this knowledge, completes the present invention. It came.
  • the phosphorescent compound according to claim 1 of the present invention is obtained by adding to the phosphorescent oxide compound an additive that has both or either one of an ethylene glycol compound and a zinc oxide mixed compound. It is characterized by that.
  • a phosphorescent compound having improved luminance and afterglow time is provided.
  • the method for producing a phosphorescent compound according to claim 1 of the present invention is characterized in that the additive is added to the phosphorescent compound.
  • the blending ratio of the ethylene glycol compound and the acid-zinc mixed compound blended in the phosphorescent compound is 5% to 20%. It is characterized by.
  • the phosphorescent compound according to claim 3 of the present invention is characterized in that the phosphorescent oxide has 60% or more of an aluminate oxide having a hexagonal crystal structure.
  • the luminance is higher than that of the phosphorescent acid compound.
  • FIG. 1 is a characteristic comparison diagram of phosphorescent compounds according to the present invention and the prior art.
  • the additive compound absorbs light energy, particularly light energy in the ultraviolet region, and also has a function of converting it into heat energy. Therefore, the light energy can be emitted by the heat energy obtained.
  • the power that is, the emission luminance can be improved.
  • These compounds can be used in the form of liquids, granules, etc., but when forming a coating film using a coating solution, the powdery type is used for the coating solution properties (dispersibility and solubility) and coating. Preferred in terms of film properties (surface stickiness, coating smoothness).
  • the use ratio of the additive used in the present invention is preferably 5% to 20%.
  • the blending ratio is less than this range, the brightness of the phosphorescent compound cannot be improved, and if it is more than this range, the effect of improving the brightness just by adding it is not seen, which causes the brightness to decrease. Further, the yellowing degree of the coating film is increased and the appearance is deteriorated.
  • the phosphorescent oxide used in the present invention is a conventionally known phosphorescent pigment, for example, a pigment obtained from an acidic compound such as barium, strontium, calcium, that is, the following general formula (1):
  • M is at least one selected from the group consisting of calcium, strontium and barium forces
  • magnesium obtained by adding magnesium to the mother crystal oxide
  • an activator for the added acid oxide or the above-described mother crystal oxide or magnesium-added carbonate
  • activated phosphorescent oxide added with any of Pyum, dysprosium, or neodymium is cited. .
  • the additive may be added to the phosphorescent oxide.
  • the mixed solution is placed in an electric furnace heated to 600 degrees. Burns after about 3 minutes. Keep in the furnace for 20 minutes, then remove and cool.
  • the obtained phosphorescent compound was irradiated with a xenon lamp for 15 minutes for excitation, and the emission spectrum was examined.
  • the fluorescence spectrum 3 of the phosphorescent compound 1 according to the present invention is 1.5 times higher than that of the fluorescence spectrum 3 of the conventional phosphorescent compound 2 when the strontium key aluminate phosphorescent oxide is used alone. Improvement was confirmed.
  • a phosphorescent compound having improved luminance and afterglow time without increasing the amount of phosphorescent oxide used, and a method for producing the phosphorescent compound. It is preferably used for a luminescent sheet as a medium, or a luminescent product such as a signboard or a display board that emits light at night.

Abstract

Disclosed is a light-storing compound having improved luminance and afterglow time without increasing the amount of light-storing oxide used therein. Also disclosed is a method for producing such a light-storing compound. The light-storing compound is characterized in that it is obtained by adding a compound composed of one or both of an ethylene glycol compound and a zinc oxide mixed compound to a light-storing oxide. Preferably, the blending ratio of the ethylene glycol compound and zinc oxide mixed compound is from 5% to 20% and the light-storing oxide contains 60% or more of an aluminate oxide having a hexagonal structure.

Description

明 細 書  Specification
蓄光化合物及びその製造法  Phosphorescent compound and production method thereof
技術分野  Technical field
[0001] 本発明は、蓄光化合物及びその製造法に係り、蓄光酸化物の輝度と残光時間を向 上させる輝度向上剤を添加した蓄光化合物及びその製造方法に関するものである。 背景技術  TECHNICAL FIELD [0001] The present invention relates to a phosphorescent compound and a method for producing the phosphorescent compound, and more particularly to a phosphorescent compound to which a luminance enhancer for improving the luminance and afterglow time of a phosphorescent oxide is added and a method for producing the same. Background art
[0002] 従来、蓄光酸ィ匕物については各種のものが知られている。この蓄光酸化物は、これ に光等のエネルギーを吸収させると、そのエネルギーを貯蔵し、発光を生じるもので ある。蓄光体は、このような発光現象に基づいて、広告媒体としての発光性シートや、 夜中に発光する看板や表示板等の発光性製品として利用されている。  Conventionally, various types of phosphorescent oxides are known. When this energy storage oxide absorbs energy such as light, it stores the energy and emits light. Based on such a light emission phenomenon, phosphorescent materials are used as luminescent products such as luminescent sheets as advertising media and signs and display boards that emit light at night.
[0003] 例えば特許文献 1には、アルミン酸塩蓄光性蛍光体「MA1 O :XK-YL-ZPJ [但し  [0003] For example, Patent Document 1 discloses an aluminate phosphorescent phosphor “MA1 O: XK-YL-ZPJ [provided that
2 4  twenty four
、 Mは、カルシウム、ノ リウム、ストロンチウム、マグネシウム、及びこれらの混合物から 成る群から選択された一種の金属; Xは、ユウ口ピウムカも成る賦活剤; Y、及び Ζは、 ランタン系列元素、及びマンガン、スズ、並びにビスマスカ 成る群力 選択された賦 活助剤； Κは、 Μに対するモル0 /0で 0. 001乃至 10、 Lは、 Μに対するモル0 /0で 0乃 至 10、そして Ρは、 Μに対するモル％で 0乃至 10を表す。 ]を用いた発光性複合シー トの技術が開示されている。 , M is a kind of metal selected from the group consisting of calcium, norlium, strontium, magnesium, and mixtures thereof; X is an activator that also consists of Pylum, Y, and Ζ are lanthanum series elements, and manganese, tin, and Bisumasuka group consisting force selected vehicles Katsusukezai; kappa is 0.001 to 10, L at mole 0/0 for Micromax, the molar 0/0 0乃optimum 10 for Micromax, and Ρ Represents 0 to 10 in terms of mol% with respect to soot. The technology of the luminescent composite sheet using the above is disclosed.
特許文献 1：特開平 10— 114030号公報  Patent Document 1: Japanese Patent Laid-Open No. 10-114030
[0004] このような発光性製品においては、その輝度 (発光輝度）は高い方が望ましいことは 明らかであり、その蓄光酸化物を多量用いることにより、その輝度を向上させることは 可能であるが、この場合には、その蓄光酸ィ匕物は高価なものであることから、製品コ ストが高くなると 、う問題を生じた。 [0004] In such luminescent products, it is clear that higher luminance (emission luminance) is desirable, and it is possible to improve the luminance by using a large amount of the phosphorescent oxide. In this case, since the phosphoric acid oxide is expensive, a problem arises when the product cost increases.
発明の開示  Disclosure of the invention
発明が解決しょうとする課題  Problems to be solved by the invention
[0005] 従って本発明は、蓄光酸ィ匕物の使用量を増加させることなぐその輝度及び残光時 間を向上させた蓄光化合物及びその製造方法を提供することをその課題とする。 課題を解決するための手段 [0006] 本発明者は、課題を解決するために鋭意研究を重ねた結果、特定の化合物が、蓄 光酸化物の発光力を向上することを見出し、この知見に基づき本発明を完成するに 至った。 [0005] Accordingly, an object of the present invention is to provide a phosphorescent compound having improved luminance and afterglow time without increasing the amount of phosphorescent oxide used, and a method for producing the same. Means for solving the problem [0006] As a result of intensive studies to solve the problem, the present inventor has found that a specific compound improves the luminous power of the phosphorescent oxide, and based on this knowledge, completes the present invention. It came.
[0007] 即ち、本発明の請求項 1による蓄光化合物は、エチレングリコール系化合物及び酸 化亜鉛混合ィ匕合物の双方又はいずれか一方力もなる添加物を蓄光酸ィ匕物に付与し てなることを特徴とする。  [0007] That is, the phosphorescent compound according to claim 1 of the present invention is obtained by adding to the phosphorescent oxide compound an additive that has both or either one of an ethylene glycol compound and a zinc oxide mixed compound. It is characterized by that.
このようにして輝度および残光時間が向上した蓄光化合物が提供される。 また、本発明の請求項 1による蓄光化合物の製造方法は、蓄光化合物に前記添加 物を添加することを特徴とする。  In this way, a phosphorescent compound having improved luminance and afterglow time is provided. The method for producing a phosphorescent compound according to claim 1 of the present invention is characterized in that the additive is added to the phosphorescent compound.
[0008] さらに、本発明の請求項 2による蓄光化合物は、前記蓄光化合物中に配合したェ チレングリコール系化合物及び酸ィ匕亜鉛混合ィ匕合物の配合割合が 5%から 20%で あることを特徴とする。 [0008] Further, in the phosphorescent compound according to claim 2 of the present invention, the blending ratio of the ethylene glycol compound and the acid-zinc mixed compound blended in the phosphorescent compound is 5% to 20%. It is characterized by.
[0009] さらにまた、本発明の請求項 3による蓄光化合物は、前記蓄光酸化物が六方晶系 構造であるアルミン酸系酸化物を 60%以上有することを特徴とする。  [0009] Further, the phosphorescent compound according to claim 3 of the present invention is characterized in that the phosphorescent oxide has 60% or more of an aluminate oxide having a hexagonal crystal structure.
発明の効果  The invention's effect
[0010] 本発明によれば、蓄光酸ィ匕物にエチレングリコール系化合物及び/又は酸ィ匕亜鉛 混合ィ匕合物を添加し製造することにより、蓄光酸ィ匕物のもつ輝度よりも高い輝度と長 [0010] According to the present invention, by adding an ethylene glycol compound and / or an acid-zinc mixed compound to the phosphorescent acid compound, the luminance is higher than that of the phosphorescent acid compound. Luminance and length
V、残光時間を得ることができる。 V, afterglow time can be obtained.
図面の簡単な説明  Brief Description of Drawings
[0011] [図 1]本発明と従来技術による蓄光化合物の特性比較図である。  FIG. 1 is a characteristic comparison diagram of phosphorescent compounds according to the present invention and the prior art.
符号の説明  Explanation of symbols
[0012] 1 本発明による蓄光化合物の輝度特性  [0012] 1 Luminance characteristics of phosphorescent compounds according to the present invention
2 従来の蓄光化合物の輝度特性  2 Luminance characteristics of conventional phosphorescent compounds
3 蛍光スペクトル (励起光照射後 10秒）  3 Fluorescence spectrum (10 seconds after irradiation with excitation light)
4 最高輝度の経時減衰特性  4 Maximum luminance decay with time
発明を実施するための最良の形態  BEST MODE FOR CARRYING OUT THE INVENTION
[0013] 本発明においては、蓄光酸ィ匕物の輝度向上対策として、酸ィ匕物の欠損としての自 由端酸素基の動きを抑制するために、エチレングリコール系化合物及び Z又は酸ィ匕 亜鉛混合化合物を添加する。 [0013] In the present invention, as a measure for improving the brightness of phosphorescent oxides, self In order to suppress the movement of the oxygen radical group, an ethylene glycol compound and Z or a zinc oxide mixed compound are added.
この場合の添加ィ匕合物は、光エネルギー、特に紫外線領域の光エネルギーを吸収 し、熱エネルギーに変換する作用も有するので、光エネルギー力 得られる熱ェネル ギ一により蓄光酸ィ匕物の発光力、すなわち、発光輝度を向上することができるように なる。  In this case, the additive compound absorbs light energy, particularly light energy in the ultraviolet region, and also has a function of converting it into heat energy. Therefore, the light energy can be emitted by the heat energy obtained. The power, that is, the emission luminance can be improved.
これらの化合物は、液状、顆粒等の形態のものも使用できるが、塗工液を用いて塗 膜を形成する場合、粉末状のものが、塗工液物性 (分散性及び溶解性)や塗膜の性 状 (表面のベタツキ性、塗膜の平滑性)の面で好まし 、。  These compounds can be used in the form of liquids, granules, etc., but when forming a coating film using a coating solution, the powdery type is used for the coating solution properties (dispersibility and solubility) and coating. Preferred in terms of film properties (surface stickiness, coating smoothness).
[0014] 本発明で用いる添加物の使用割合は、 5%から 20%で配合することが好ましい。 [0014] The use ratio of the additive used in the present invention is preferably 5% to 20%.
この範囲より配合割合が少ないと、蓄光化合物の輝度を向上することができないし 、この範囲より多いと、添加しただけの輝度向上効果が見られず、力えって輝度が低 下する原因となるし、さらに塗膜の黄変度が上がり、外観を悪化させるものとなる。  If the blending ratio is less than this range, the brightness of the phosphorescent compound cannot be improved, and if it is more than this range, the effect of improving the brightness just by adding it is not seen, which causes the brightness to decrease. Further, the yellowing degree of the coating film is increased and the appearance is deteriorated.
[0015] 本発明で用いる蓄光酸ィ匕物としては、従来公知の蓄光顔料、例えば、バリウム、スト ロンチウム、カルシウムなどの酸ィ匕物で得られる顔料、即ち、下記一般式（1)： [0015] The phosphorescent oxide used in the present invention is a conventionally known phosphorescent pigment, for example, a pigment obtained from an acidic compound such as barium, strontium, calcium, that is, the following general formula (1):
MA1 0 · · · (1)  MA1 0 · · · (1)
2 4  twenty four
(式中、 Mはカルシウム、ストロンチウム及びバリウム力もなる群より選択された少なくと も 1つからなる）で表わされる母結晶酸ィ匕物、前記母結晶酸ィ匕物にマグネシウムを添 カロしたマグネシウム添加酸ィ匕物、又は、前記母結晶酸ィ匕物もしくはマグネシウム添カロ 酸化物に対して賦活剤として、ユウ口ピウム、ジスプロシウム、ネオジムのいずれかを 添加した賦活蓄光酸化物、などが挙げられる。  (Wherein M is at least one selected from the group consisting of calcium, strontium and barium forces), and magnesium obtained by adding magnesium to the mother crystal oxide As an activator for the added acid oxide, or the above-described mother crystal oxide or magnesium-added carbonate, activated phosphorescent oxide added with any of Pyum, dysprosium, or neodymium is cited. .
[0016] 本発明により前記蓄光酸化物の輝度を向上させるには、前記添加物を蓄光酸化物 に添加すればよい。ただし、添加の効果を高めるためには、蓄光酸化物の構造を高 温安定相である六方晶系の密な篕構造にして自由端酸素基を少なくしておくことが 望ましい。 In order to improve the luminance of the phosphorescent oxide according to the present invention, the additive may be added to the phosphorescent oxide. However, in order to enhance the effect of the addition, it is desirable to make the structure of the phosphorescent oxide a hexagonal dense cage structure, which is a high temperature stable phase, and to reduce the number of free end oxygen groups.
[0017] 次に図 1を参照して、本発明を実施例によりさらに詳細に説明する。  Next, referring to FIG. 1, the present invention will be described in more detail by way of examples.
[0018] ストロンチウムケィ素アルミン酸蓄光酸化物 85重量0 /0、エチレングリコール 10重量 %、酸化亜鉛 5重量％を混合し、その総量 50gを尿素 20gと混ぜ、水 lOOccに溶解し 溶液とする。 [0018] Strontium Kei-containing aluminate phosphorescent oxide 85 weight 0/0, ethylene glycol 10 wt%, zinc oxide 5 wt% were mixed, mix the total 50g with urea 20g, was dissolved in water lOOcc Make a solution.
600度に加熱した電気炉内に前記混合溶液を配置する。約 3分後に燃焼する。 20 分間炉内に維持した後取り出し放冷する。  The mixed solution is placed in an electric furnace heated to 600 degrees. Burns after about 3 minutes. Keep in the furnace for 20 minutes, then remove and cool.
[0019] 得られた蓄光化合物をキセノンランプで 15分間照射して励起後、発光スペクトルを 調べた。 [0019] The obtained phosphorescent compound was irradiated with a xenon lamp for 15 minutes for excitation, and the emission spectrum was examined.
本発明による蓄光化合物 1の蛍光スペクトル 3は、前記ストロンチウムケィ素アルミン 酸蓄光酸化物が単独の場合、即ち従来の蓄光化合物 2の蛍光スペクトル 3と比較す ると、 1. 5倍以上の輝度の向上が確認された。  The fluorescence spectrum 3 of the phosphorescent compound 1 according to the present invention is 1.5 times higher than that of the fluorescence spectrum 3 of the conventional phosphorescent compound 2 when the strontium key aluminate phosphorescent oxide is used alone. Improvement was confirmed.
[0020] さらに、最高輝度の経時減衰特性 4を比較すると、当初最高輝度の半分の輝度に 到達する時間は 1. 2倍となった。 [0020] Further, when comparing the decay characteristic 4 of the maximum brightness with time, the time to reach half the initial maximum brightness was 1.2 times.
また、ストロンチウムケィ素アルミン酸の構造をエックス線回折で調べたところ、単斜 方晶に比べ六方晶が多ぐ回折ピークから予測して半定量的には 80%以上六方晶 と解釈でき、六方晶系の密な篕構造が添加物の効果を高めていることが裏付けられ た。  In addition, when the structure of strontium key aluminate was examined by X-ray diffraction, it was predicted from the diffraction peaks that had more hexagonal crystals than monoclinic crystals, and could be interpreted semi-quantitatively as more than 80% hexagonal. It was confirmed that the dense structure of the system enhances the effect of the additive.
産業上の利用可能性  Industrial applicability
[0021] 本発明によれば、蓄光酸化物の使用量を増加させることなぐその輝度及び残光時 間を向上させた蓄光化合物及びその製造方法を提供できるので、本発明による蓄光 化合物は、広告媒体としての発光性シートや、夜中に発光する看板や表示板等の発 光性製品に用いると好適である。 [0021] According to the present invention, it is possible to provide a phosphorescent compound having improved luminance and afterglow time without increasing the amount of phosphorescent oxide used, and a method for producing the phosphorescent compound. It is preferably used for a luminescent sheet as a medium, or a luminescent product such as a signboard or a display board that emits light at night.

Claims

請求の範囲 The scope of the claims
[1] 蓄光酸化物と、エチレングリコール系化合物及び酸化亜鉛混合化合物の双方又は 何れか一方とからなることを特徴とする蓄光化合物及びその製造方法。  [1] A phosphorescent compound and a method for producing the phosphorescent compound, comprising the phosphorescent oxide and / or one or both of an ethylene glycol compound and a zinc oxide mixed compound.
[2] 前記蓄光化合物中に配合したエチレングリコール系化合物及び酸化亜鉛混合ィ匕 合物の配合割合が 5%から 20%であることを特徴とする請求項 1に記載の蓄光化合 物及びその製造方法。  [2] The phosphorescent compound according to claim 1, wherein the blending ratio of the ethylene glycol compound and the zinc oxide mixed compound blended in the phosphorescent compound is 5% to 20%. Method.
[3] 前記蓄光酸ィ匕物が六方晶系構造であるアルミン酸系酸ィ匕物を 60%以上有すること を特徴とする請求項 1又は 2に記載の蓄光化合物及びその製造方法。  [3] The phosphorescent compound according to claim 1 or 2, wherein the phosphorescent oxide has 60% or more of an aluminate-based oxide having a hexagonal structure.
PCT/JP2005/012134 2004-06-30 2005-06-30 Light-storing compound and method for producing same WO2006004021A1 (en)

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JPH11140438A (en) * 1997-11-07 1999-05-25 Nippon Chem Ind Co Ltd Luminous fluorescent substance
JPH11140439A (en) * 1997-11-07 1999-05-25 Nippon Chem Ind Co Ltd Luminous fluorescent substance
JP2000034480A (en) * 1998-05-13 2000-02-02 Ohara Inc Phosphorescent phosphor
JPH11322308A (en) * 1998-05-18 1999-11-24 Kasei Optonix Co Ltd Production of compound metal oxide
JP2000212557A (en) * 1999-01-28 2000-08-02 Ohara Inc Luminous phosphor
JP2000282032A (en) * 1999-03-30 2000-10-10 Taiheiyo Keizai Kaihatsu:Kk Luminous fluophor composition

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