JP4374114B2 - Phosphor production method - Google Patents
Phosphor production method Download PDFInfo
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- JP4374114B2 JP4374114B2 JP2000122883A JP2000122883A JP4374114B2 JP 4374114 B2 JP4374114 B2 JP 4374114B2 JP 2000122883 A JP2000122883 A JP 2000122883A JP 2000122883 A JP2000122883 A JP 2000122883A JP 4374114 B2 JP4374114 B2 JP 4374114B2
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- phosphoric acid
- phosphor
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- earth oxide
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Description
【０００１】
【発明の属する技術分野】
この発明は、蛍光体の製造方法に関し、特に、発光効率の向上した希土類正燐酸塩の蛍光体の製造方法に関するものである。
【０００２】
【従来の技術】
従来、希土類正燐酸塩を成分とする蛍光体として、テルビウム付活性燐酸ランタン・セリウム蛍光体が知られている。このテルビウム付活性燐酸ランタン・セリウム蛍光体は、紫外線励起によって、波長５４３ｎｍを発光ピークとする緑色光を発し、その発光スペクトルの幅は鋭く、線状である。
【０００３】
このため、テルビウム付活性燐酸ランタン・セリウム蛍光体は、青色、緑色、赤色の３色に発光する蛍光体を使用した３波長域発光形蛍光ランプの緑色成分として重要な実用性価値を持っている。すなわち、緑色光は、可視光領域の中間にあり人間の視感度が高いため、緑色蛍光体の発光効率が、３波長域発光形蛍光ランプの全光束に大きな影響を与える。したがって、テルビウム付活性燐酸ランタン・セリウム蛍光体の発光効率の向上が大いに望まれている。
【０００４】
ここで、先行技術文献（特公昭６３−５２０７７号）には、希土類酸化物の粉末を水に投入し攪拌してスラリーとした後、燐酸（Ｈ3 ＰＯ4 ）を注入して化学反応を起こさせ、化学反応の結果得られた希土類燐酸塩を焼成して蛍光体を製造する方法が記載されている。すなわち、図４に示すように、希土類酸化物を水に入れて攪拌したスラリーに対して、燐酸を注入していく方法が記載されている。ここで、スラリーとは、粉状の固体と流体の混合物をいう。
【０００５】
しかるに、この方法では、希土類酸化物を水に入れて攪拌したスラリーに対して、燐酸を注入し反応させる際、希土類酸化物と燐酸に未反応な部分ができるという問題点があった。したがって、その後、焼成して蛍光体を製造すると暗く、安定した高発光効率が得られないという問題点があった。
【０００６】
【発明が解決しようとする課題】
この発明は、上記した従来技術の問題点を除くためになされたものであって、その目的とするところは、従来の蛍光体製造方法よりも発光効率の高い蛍光体を製造することができる蛍光体の製造方法を得ることにある。
【０００７】
また、他の目的は、従来の蛍光体製造方法により製造された蛍光体よりも発光効率のばらつきの少ない蛍光体製造方法を得ることにある。
【０００８】
【課題を解決するための手段】
この発明に係る蛍光体製造方法は、共沈塩を焼成して希土類酸化物を生成する希土類酸化物生成工程と、上記希土類酸化物生成工程で生成した希土類酸化物を燐酸水溶液に入れて反応させる反応工程と、上記反応工程で生成された反応生成物を焼成する反応生成物焼成工程とを備えることを特徴とする。
【０００９】
また、上記希土類酸化物生成工程は、ランタン（Ｌａ）、テルビウム（Ｔｂ）、セリウム（Ｃｅ）の共沈塩を焼成して希土類酸化物を生成することを特徴とする。
【００１０】
すなわち、この発明に係る蛍光体製造方法によれば、高温になっても蒸発しにくい燐酸水溶液の中に希土類酸化物を少しずつ投入することで未反応な部分もなく反応させ粉末を作り焼成するので、従来の蛍光体製造方法で製造された蛍光体よりも安定して高い発光効率の蛍光体を製造できるものである。
【００１１】
【実施例】
実施例１．
以下、この発明に係る蛍光体製造方法の一実施例として、テルビウム付活性燐酸ランタン・セリウム蛍光体の製造方法を図１を参照しながら説明する。
【００１２】
酸化テルビウム（Ｔｂ4 Ｏ7 ）と酸化ランタン（Ｌａ2 Ｏ3 ）と炭酸セリウム（Ｃｅ2 ＣＯ3 ）を硝酸水溶液に溶解してできた希土類硝酸塩水溶液に、シュウ酸（ＨＯＣＯＣＯＯＨ・２Ｈ2 Ｏ）水溶液を攪拌しながら徐々に注入して希土類シュウ酸塩（共沈シュウ酸塩）の沈殿を生成した（共沈シュウ酸塩合成工程Ｓ１００）。
【００１３】
この得られた沈殿をろ過し乾燥した後（ろ過・乾燥工程Ｓ１０１）、１０００℃にて空気中１．５時間焼成して希土類酸化物を生成した（希土類酸化物生成工程Ｓ１０２）。
【００１４】
次に、溶液の溶質に対する重量パーセントで８５％の燐酸を４０℃の水で希釈して作った２７％濃度（重量パーセント）の燐酸水溶液１０ｋｇに対して上記希土類酸化物の粉末４．７ｋｇと炭酸リチウム（Ｌｉ2 ＣＯ3 ）０．０１９ｋｇの割合で攪拌しながら少しずつ投入して反応させた（反応工程Ｓ１０３）。この炭酸リチウムは、紫外線による蛍光劣化を防止するために添加するものである。また、反応中に触媒として３０％濃度（重量パーセント）の過酸化水素水（Ｈ2 Ｏ2 ）を上記２７％濃度（重量パーセント）の燐酸水溶液１０ｋｇに対して２．６ｋｇの割合で少量ずつ注入して反応を促進させる。反応終了後、スラリーを乾燥して粉末を得た。
【００１５】
こうして得られた粉末を、１２５０℃にて窒素と水素の混合気体中、１．５時間焼成し（反応生成物焼成工程Ｓ１０４）、冷却、粉砕して蛍光体を得た（冷却・粉砕工程Ｓ１０５）。
【００１６】
上述した本発明に係る蛍光体製造方法は、図２に示すように、燐酸水溶液に対して、希土類酸化物を投入することによって、燐酸と希土類酸化物とを反応させることを特徴としている。この発明の効果を検証するため、従来技術で記載した方法、すなわち、図４に示したように、希土類酸化物を水に入れて攪拌したスラリーに対して、燐酸を注入していく方法を用いた比較例の蛍光体を作った。
【００１７】
具体的に比較例は、希土類酸化物の粉末４．７ｋｇを６．８ｋｇの４０℃の水に加え、攪拌して分散させた後、８５％（重量パーセント）の燐酸を攪拌しながら少しずつ投入して反応させた。それ以外は、実施例１と同様にした。
【００１８】
このようにして、実施例及び比較例について各２０Ｌｏｔずつ蛍光体を製造し、その蛍光体を用いて４０ワット直管形蛍光ランプを作成した。
図３に、作成した４０ワット直管形蛍光ランプの点灯初期の全光束（明るさ）とＬｏｔ数の関係を示した。
図３において、横軸は、全光束を示したものであり単位は、ｌｍ（ルーメン）であり、縦軸は、Ｌｏｔ数を示したものである。図から明らかなように、本発明に係る蛍光体製造方法で製造した蛍光体を用いたランプの全光束（明るさ）の平均の方が、比較例の蛍光体を用いたランプの全光束（明るさ）の平均より大きいこと及びＬｏｔごとの全光束（明るさ）のばらつきが小さいことがわかる。
【００１９】
具体的には、本発明による蛍光体２０Ｌｏｔで作成した蛍光ランプの全光束の平均値は、５１００ｌｍ、明るさの標準偏差は、３２．７２であったのに対し、比較例による蛍光体２０Ｌｏｔで作成した蛍光ランプの全光束の平均値は、４９９１ｌｍ、明るさの標準偏差は、７５．７５であった。本発明による蛍光体による蛍光ランプの明るさは、比較例に比べて明るく、また、Ｌｏｔ毎の明るさのバラツキも少なく性能が安定している。
【００２０】
本実施例においては、希土類酸化物を得るために共沈シュウ酸塩を合成して用いたが、焼成して酸化物となる塩であれば、他の希土類共沈塩、例えば、共沈炭酸塩を合成して用いても同様の効果が得られる。
【００２１】
また、本実施例においては、ランプ製造時のベーキング工程や、ランプ点灯時の１８５ｎｍ紫外線による蛍光体の劣化を抑制する物質として、炭酸リチウムを用いたが、他の同様の効果を有する物質、例えば、ホウ酸リチウム、ホウ酸カリウム、ホウ酸セシウム、炭酸カリウムなどのアルカリ塩を用いた場合でも同様の効果が得られる。
【００２２】
また、本実施例においては、燐酸反応を促進する物質として過酸化水素水を用いたが、他の燐酸反応を促進する物質を用いるか、促進する物質なしの場合でも同様の効果が得られる。
【００２３】
また、本実施例においては、４０℃の水を用いたが、常温の水、又は反応時のスラリーの温度が燐酸の蒸発を起こさない範囲であれば、本実施例より高い温度の水を用いても同様の効果が得られる。すなわち、温度特性が良好である。
【００２４】
【発明の効果】
本発明に係る蛍光体製造方法は、共沈塩を焼成して希土類酸化物を生成する希土類酸化物生成工程と、上記希土類酸化物生成工程で生成した希土類酸化物を燐酸水溶液に入れて反応させる反応工程と、上記反応工程で生成された反応生成物を焼成する反応生成物焼成工程とを備えたので、従来の蛍光体製造方法よりも発光効率の高い蛍光体を製造することができる効果が得られる。
【００２５】
また、本発明に係る蛍光体製造方法によれば、従来の蛍光体製造方法により製造された蛍光体よりも発光効率のばらつきの少ない蛍光体を得ることができる効果が得られる。
【図面の簡単な説明】
【図１】 本発明に係る蛍光体製造方法のフローチャートを示した図である。
【図２】 燐酸水溶液に対して、希土類酸化物を投入することによって、燐酸と希土類酸化物とを反応させる様子を示した図である。
【図３】 本実施例による蛍光体を用いた蛍光ランプと比較例による蛍光体を用いた蛍光ランプの点灯初期の全光束（明るさ）とＬｏｔ数の関係を示した図である。
【図４】 希土類酸化物を水に入れて攪拌したスラリーに対して、燐酸を注入していく様子を示した図である。
【符号の説明】
１ 燐酸水溶液、２ 希土類酸化物、３ 希土類酸化物スラリ−、Ｓ１０２ 希土類酸化物生成工程、Ｓ１０３ 反応工程、Ｓ１０４ 反応生成物焼成工程。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method for producing a phosphor, and more particularly, to a method for producing a rare-earth orthophosphate phosphor having improved luminous efficiency.
[0002]
[Prior art]
Conventionally, an active lanthanum phosphate cerium phosphate phosphor with terbium is known as a phosphor containing rare earth orthophosphate as a component. This activated lanthanum phosphate phosphor with terbium emits green light having an emission peak at a wavelength of 543 nm by ultraviolet excitation, and the emission spectrum has a sharp width and a linear shape.
[0003]
Therefore, the active lanthanum phosphate / cerium phosphor with terbium has an important practical value as a green component of a three-wavelength-range fluorescent lamp using phosphors that emit light in three colors of blue, green, and red. . That is, since green light is in the middle of the visible light region and has high human visibility, the luminous efficiency of the green phosphor has a great influence on the total luminous flux of the three-wavelength region-emitting fluorescent lamp. Therefore, improvement of the luminous efficiency of the terbium-attached activated lanthanum phosphate / cerium phosphor is highly desired.
[0004]
Here, in the prior art document (Japanese Patent Publication No. 63-52077), a rare earth oxide powder is put into water and stirred to form a slurry, and then phosphoric acid (H 3 PO 4 ) is injected to cause a chemical reaction. A phosphor is produced by firing rare earth phosphate obtained as a result of a chemical reaction. That is, as shown in FIG. 4, a method is described in which phosphoric acid is injected into a slurry obtained by stirring a rare earth oxide in water. Here, the slurry refers to a mixture of powdered solid and fluid.
[0005]
However, this method has a problem in that when a reaction is performed by injecting phosphoric acid into a slurry obtained by stirring a rare earth oxide in water, an unreacted portion is formed between the rare earth oxide and phosphoric acid. Therefore, after that, when the phosphor is manufactured by firing, there is a problem that it is dark and stable high luminous efficiency cannot be obtained.
[0006]
[Problems to be solved by the invention]
The present invention has been made to eliminate the above-mentioned problems of the prior art, and an object of the present invention is to provide a phosphor capable of producing a phosphor having higher luminous efficiency than the conventional phosphor production method. The object is to obtain a manufacturing method of the body.
[0007]
Another object is to obtain a phosphor manufacturing method with less variation in luminous efficiency than phosphors manufactured by a conventional phosphor manufacturing method.
[0008]
[Means for Solving the Problems]
In the phosphor manufacturing method according to the present invention, a rare earth oxide production step of firing a coprecipitated salt to produce a rare earth oxide, and reacting the rare earth oxide produced in the rare earth oxide production step in a phosphoric acid aqueous solution. It comprises a reaction step and a reaction product baking step of baking the reaction product generated in the reaction step.
[0009]
The rare earth oxide production step is characterized in that a rare earth oxide is produced by firing a coprecipitated salt of lanthanum (La), terbium (Tb), and cerium (Ce).
[0010]
That is, according to the phosphor manufacturing method according to the present invention, a rare earth oxide is gradually added into a phosphoric acid aqueous solution that does not easily evaporate even at a high temperature, thereby causing a reaction without an unreacted portion to produce a powder and firing it. Therefore, it is possible to manufacture a phosphor with higher luminous efficiency more stably than the phosphor manufactured by the conventional phosphor manufacturing method.
[0011]
【Example】
Example 1.
Hereinafter, as an embodiment of the phosphor manufacturing method according to the present invention, a method for manufacturing a terbium-attached active lanthanum phosphate / cerium phosphor will be described with reference to FIG.
[0012]
An aqueous solution of oxalic acid (HOCOCOOH · 2H 2 O) is added to a rare earth nitrate aqueous solution obtained by dissolving terbium oxide (Tb 4 O 7 ), lanthanum oxide (La 2 O 3 ) and cerium carbonate (Ce 2 CO 3 ) in an aqueous nitric acid solution. Was gradually poured while stirring to form a precipitate of rare earth oxalate (coprecipitated oxalate) (coprecipitate oxalate synthesis step S100).
[0013]
The obtained precipitate was filtered and dried (filtration / drying step S101), and then fired in air at 1000 ° C. for 1.5 hours to generate a rare earth oxide (rare earth oxide generation step S102).
[0014]
Next, 4.7 kg of the rare earth oxide powder and carbonic acid are added to 10 kg of a 27% phosphoric acid aqueous solution prepared by diluting 85% phosphoric acid by weight with respect to the solute of the solution with 40 ° C. water. Lithium (Li 2 CO 3 ) was added and reacted little by little at a rate of 0.019 kg (reaction step S103). This lithium carbonate is added in order to prevent fluorescence deterioration due to ultraviolet rays. Further, during the reaction, 30% concentration (weight percent) of hydrogen peroxide (H 2 O 2 ) is injected as a catalyst at a rate of 2.6 kg with respect to 10 kg of the 27% concentration (weight percent) phosphoric acid aqueous solution. To promote the reaction. After completion of the reaction, the slurry was dried to obtain a powder.
[0015]
The powder thus obtained was fired at 1250 ° C. in a mixed gas of nitrogen and hydrogen for 1.5 hours (reaction product firing step S104), cooled and ground to obtain a phosphor (cooling / ground step S105). ).
[0016]
The phosphor manufacturing method according to the present invention described above is characterized in that phosphoric acid and the rare earth oxide are reacted by introducing the rare earth oxide into the phosphoric acid aqueous solution, as shown in FIG. In order to verify the effect of the present invention, the method described in the prior art, that is, the method in which phosphoric acid is injected into the slurry obtained by stirring the rare earth oxide in water as shown in FIG. The phosphor of the comparative example was made.
[0017]
Specifically, in the comparative example, 4.7 kg of rare earth oxide powder was added to 6.8 kg of 40 ° C. water and dispersed by stirring, and then 85% (weight percent) phosphoric acid was added little by little while stirring. And reacted. Otherwise, the same procedure as in Example 1 was performed.
[0018]
In this manner, phosphors of 20 lots were manufactured for each of the examples and comparative examples, and 40 watt straight tube fluorescent lamps were produced using the phosphors.
FIG. 3 shows the relationship between the total luminous flux (brightness) and the number of lots in the initial lighting of the 40 watt straight tube fluorescent lamp.
In FIG. 3, the horizontal axis indicates the total luminous flux, the unit is lm (lumen), and the vertical axis indicates the number of lots. As is apparent from the figure, the average of the total luminous flux (brightness) of the lamp using the phosphor manufactured by the phosphor manufacturing method according to the present invention is the total luminous flux of the lamp using the phosphor of the comparative example ( It can be seen that the brightness is larger than the average and the variation of the total luminous flux (brightness) for each lot is small.
[0019]
Specifically, the average value of the total luminous flux of the fluorescent lamp made with the phosphor 20Lt according to the present invention was 5100 lm, and the standard deviation of the brightness was 32.72, whereas the average value of the phosphor 20Lt according to the comparative example was The average value of the total luminous flux of the produced fluorescent lamp was 4991 lm, and the standard deviation of brightness was 75.75. The brightness of the fluorescent lamp by the phosphor according to the present invention is brighter than that of the comparative example, and there is little variation in brightness from lot to lot, and the performance is stable.
[0020]
In this example, a coprecipitated oxalate was synthesized and used to obtain a rare earth oxide. However, other rare earth coprecipitated salts such as coprecipitated carbonic acid can be used as long as they are calcined to form oxides. The same effect can be obtained even if a salt is synthesized.
[0021]
In this example, lithium carbonate was used as a substance that suppresses phosphor deterioration due to 185 nm ultraviolet rays when the lamp is baked or when the lamp is lit, but a substance having other similar effects, for example, The same effect can be obtained even when an alkali salt such as lithium borate, potassium borate, cesium borate, or potassium carbonate is used.
[0022]
In this embodiment, hydrogen peroxide is used as the substance that promotes the phosphoric acid reaction. However, the same effect can be obtained even when another substance that promotes the phosphoric acid reaction is used or when no substance that promotes the phosphoric acid reaction is used.
[0023]
In this example, 40 ° C. water was used, but water at room temperature or water having a temperature higher than that of this example was used as long as the temperature of the slurry during the reaction did not cause phosphoric acid evaporation. However, the same effect can be obtained. That is, the temperature characteristics are good.
[0024]
【The invention's effect】
The phosphor manufacturing method according to the present invention includes a rare earth oxide production step of firing a coprecipitate salt to produce a rare earth oxide, and a reaction of the rare earth oxide produced in the rare earth oxide production step in a phosphoric acid aqueous solution. Since the reaction step and the reaction product baking step of baking the reaction product generated in the reaction step are provided, the effect of being able to manufacture a phosphor with higher luminous efficiency than the conventional phosphor manufacturing method is provided. can get.
[0025]
In addition, according to the phosphor manufacturing method according to the present invention, it is possible to obtain a phosphor with less variation in light emission efficiency than phosphors manufactured by the conventional phosphor manufacturing method.
[Brief description of the drawings]
FIG. 1 is a view showing a flowchart of a phosphor manufacturing method according to the present invention.
FIG. 2 is a diagram showing a state in which phosphoric acid and rare earth oxide are reacted by adding rare earth oxide to phosphoric acid aqueous solution.
FIG. 3 is a graph showing the relationship between the total luminous flux (brightness) and the number of lots at the beginning of lighting of the fluorescent lamp using the phosphor according to the present example and the fluorescent lamp using the phosphor according to the comparative example.
FIG. 4 is a view showing a state in which phosphoric acid is injected into a slurry obtained by stirring rare earth oxide in water.
[Explanation of symbols]
1 Phosphoric acid aqueous solution, 2 rare earth oxide, 3 rare earth oxide slurry, S102 rare earth oxide production step, S103 reaction step, S104 reaction product firing step.
Claims (3)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000122883A JP4374114B2 (en) | 2000-04-24 | 2000-04-24 | Phosphor production method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000122883A JP4374114B2 (en) | 2000-04-24 | 2000-04-24 | Phosphor production method |
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|---|---|
| JP2001303041A JP2001303041A (en) | 2001-10-31 |
| JP4374114B2 true JP4374114B2 (en) | 2009-12-02 |
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| JP2000122883A Expired - Fee Related JP4374114B2 (en) | 2000-04-24 | 2000-04-24 | Phosphor production method |
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