JPH07268318A - Fluorescent substance, its production and fluorescent lamp - Google Patents
Fluorescent substance, its production and fluorescent lampInfo
- Publication number
- JPH07268318A JPH07268318A JP6048994A JP6048994A JPH07268318A JP H07268318 A JPH07268318 A JP H07268318A JP 6048994 A JP6048994 A JP 6048994A JP 6048994 A JP6048994 A JP 6048994A JP H07268318 A JPH07268318 A JP H07268318A
- Authority
- JP
- Japan
- Prior art keywords
- phosphor
- infrared
- iron
- lithium aluminate
- particles
- 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- Withdrawn
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Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は蛍光体、蛍光体の製造方
法、および蛍光ランプに係り、さらに詳しくは、鉄付活
アルミン酸リチウム赤外発光蛍光体、この蛍光体の製造
方法、およびこの蛍光体を使用して構成した蛍光ランプ
に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a phosphor, a method of manufacturing the phosphor, and a fluorescent lamp, and more particularly, an iron-activated lithium aluminate infrared light emitting phosphor, a method of manufacturing the phosphor, and The present invention relates to a fluorescent lamp constructed by using a phosphor.
【０００２】[0002]
【従来の技術】周知のように、赤外発光型の蛍光ランプ
は、たとえばＯＣＲなどの文字読取り機器の光源、ある
いは植物の育成に有効な波長域の光を照射するための植
物育成用光源として実用されている。ところで、最近の
ＯＡ機器の技術革新は目覚ましく、激しい性能競争が展
開されており、前記ＯＣＲなどの文字読取り機器の光源
として使用されている赤外発光の蛍光ランプに対して
も、発光効率の向上および長寿命化などが強く望まれて
いる。また、この種の赤外発光蛍光ランプにおいては、
たとえば 254nmの紫外線で励起したときに赤外波長域に
発光し、その発光ピーク波長が 740nm付近にある一般
式、 ＬｉＡｌＯ2 ：Ｆｅ で示される鉄付活アルミン酸リチウム赤外発光蛍光体
を、紫外線励起による発光体として使用している。2. Description of the Related Art As is well known, an infrared emission type fluorescent lamp is used as a light source for a character reading device such as an OCR or a light source for cultivating plants for irradiating light in a wavelength range effective for growing plants. It is in practical use. By the way, recent technological innovation of OA equipment is remarkable, and fierce performance competition has been developed, and the luminous efficiency is improved even with respect to the infrared fluorescent lamp used as the light source of the character reading equipment such as the OCR. And longevity is strongly desired. In addition, in this type of infrared fluorescent lamp,
For example, when excited by an ultraviolet ray of 254 nm, it emits light in the infrared wavelength range, and its emission peak wavelength is around 740 nm. An iron-activated lithium aluminate infrared light emitting phosphor represented by LiAlO 2 : Fe It is used as a luminous body by excitation.
【０００３】しかしながら、前記鉄付活アルミン酸リチ
ウム赤外発光蛍光体は、吸湿性を有し化学的な安定性が
良好でないため、実用上、いろいろ不都合な問題があ
る。たとえば、蛍光体自体の吸湿性により長期保存過程
で、発光効率の低下を招来したり、点灯時に黒化を発生
し易いという問題がある。また、蛍光ランプの製造に当
たって、換言すると光透過性ガラス管内壁面に蛍光体層
を形成するため、前記鉄付活アルミン酸リチウム赤外発
光蛍光体粒子を、ＮＣバインダー（ニトロセルロースを
酢酸ブチルに溶解したもの）などに分散して調製した蛍
光体スラリーは、前記蛍光体の吸湿性によって、ゲル化
などの変成を起こして、所要の蛍光体層を形成し得ない
という事態を発生することもある。ここで、ゲル化など
の変成を起こした蛍光体スラリーは、再生して使用し得
ないので、結果的に破棄することになる。そして、その
変成を起こした蛍光体スラリーを、蛍光ランプの製造ラ
インで交換する処理作業を要することは、前記蛍光体が
高価であることと相俟って、製造コストの増大を招くこ
とになる。However, since the iron-activated lithium aluminate infrared light emitting phosphor has hygroscopicity and is not good in chemical stability, there are various problems in practical use. For example, there is a problem that the hygroscopicity of the phosphor itself causes a decrease in luminous efficiency in a long-term storage process, and blackening is likely to occur during lighting. In manufacturing the fluorescent lamp, in other words, in order to form a phosphor layer on the inner wall surface of the light-transmitting glass tube, the iron-activated lithium aluminate infrared light-emitting phosphor particles are mixed with NC binder (nitrocellulose dissolved in butyl acetate). In some cases, the phosphor slurry prepared by being dispersed in (for example) may undergo a transformation such as gelation due to the hygroscopicity of the phosphor, resulting in a situation in which the required phosphor layer cannot be formed. . Here, the phosphor slurry that has undergone modification such as gelation cannot be regenerated and used, and as a result is discarded. Further, the need for a processing operation for replacing the modified phosphor slurry with a fluorescent lamp manufacturing line, combined with the fact that the phosphor is expensive, will lead to an increase in manufacturing cost. .
【０００４】上記鉄付活アルミン酸リチウム赤外発光蛍
光体の吸湿性に起因する問題を解消するため、蛍光体粒
子表面を、重量比で 0.5〜10.0％のＡｌ2 Ｏ3 で被覆す
ることが提案されている（特開平 1−215885号公報）。In order to solve the problem caused by the hygroscopicity of the iron-activated lithium aluminate infrared light-emitting phosphor, the phosphor particle surface may be coated with 0.5 to 10.0% by weight of Al 2 O 3. It has been proposed (Japanese Patent Laid-Open No. 1-215885).
【０００５】[0005]
【発明が解決しようとする課題】前記鉄付活アルミン酸
リチウム赤外発光蛍光体表面を、重量比で 0.5〜10.0％
のＡｌ2 Ｏ3 で被覆することにより、前記吸湿性に基づ
く発光効率の低下の問題、蛍光体スラリー保存時におけ
るゲル化などの変成の問題など、ある程度解消・改善し
得るが、なお、実用上十分とはいえない。すなわち、蛍
光ランプとしたときの発光効率（もしくは明るさ）は未
だ十分といえない。また、調製後ある期間経過した蛍光
体スラリーで蛍光体層を形成したとき、その蛍光ランプ
の発光効率（もしくは明るさ）は大幅に低下しており、
加えて点灯時に黒化を発生し易い傾向が依然として認め
られる。そして、このような問題、たとえば発光効率
（もしくは明るさ）の僅かな向上、点灯時における黒化
の全面的な発生解消の問題は、たとえばＯＣＲなどの文
字読取り機器などの光源として用いた場合、文字読取り
機器などの機能向上もしくは信頼性向上などを図る上
で、重要な因子を成すことから、多くの関心が払われ、
かつ注力されているのが実状である。The iron-activated lithium aluminate infrared light emitting phosphor surface is 0.5 to 10.0% by weight ratio.
By coating with Al 2 O 3 of the above, it is possible to solve or improve to some extent the problems of the decrease in luminous efficiency due to the hygroscopicity and the problems of transformation such as gelation during storage of the phosphor slurry, but in practical use Not enough. That is, the luminous efficiency (or brightness) of the fluorescent lamp is still insufficient. In addition, when a phosphor layer is formed from a phosphor slurry that has passed a certain period after preparation, the luminous efficiency (or brightness) of the fluorescent lamp is significantly reduced,
In addition, the tendency that blackening is likely to occur during lighting is still recognized. Then, such problems, for example, a slight improvement in luminous efficiency (or brightness) and the complete elimination of blackening at the time of lighting, when used as a light source of a character reading device such as OCR, Much attention has been paid because it is an important factor in improving the functions of character reading devices or improving reliability.
And it is the actual situation that is being focused.
【０００６】本発明は上記事情に対処してなされたもの
で、発光効率の高く、かつ安定性が良好な赤外発光蛍光
体、この蛍光体の製造方法、および高発光効率で、安定
性も良好な赤外発光型の蛍光ランプの提供を目的とす
る。The present invention has been made in view of the above circumstances, and an infrared-emitting phosphor having high luminous efficiency and good stability, a method for producing this phosphor, and high luminous efficiency and stability. An object of the present invention is to provide a good infrared-emitting fluorescent lamp.
【０００７】[0007]
【課題を解決するための手段】本発明に係る蛍光体は、
紫外線で励起したときに赤外波長域に発光し、その発光
ピーク波長が 740nm付近にある一般式、 ＬｉＡｌＯ2 ：Ｆｅ で示される鉄付活アルミン酸リチウム赤外発光蛍光体粒
子であって、前記鉄付活アルミン酸リチウム赤外発光蛍
光体粒子は、その粒子表面にＭｇＯ，ＣａＯ，ＳｒＯ，
ＢａＯおよびＹ2 Ｏ3 から成る群れから選ばれた少なく
とも１種の金属酸化物微粒子を重量比で0.01〜 1.0％付
着させて成ることを特徴とする。 本発明に係る蛍光体
の製造方法は、紫外線で励起したときに赤外波長域に発
光し、その発光ピーク波長が 740nm付近にある一般式、 ＬｉＡｌＯ2 ：Ｆｅ で示される鉄付活アルミン酸リチウム赤外発光蛍光体粒
子を、Ｍｇ，Ｃａ，Ｓｒ，ＢａおよびＹから成る群れか
ら選ばれた少なくとも１種の金属アルコキシド化合物の
溶液ないし分散液にて表面処理した後、蛍光体粒子表面
に付着した金属アルコキシド化合物を分解させ、金属酸
化物微粒子を析出・被着させる工程を具備することを特
徴とする。さらに、本発明に係る蛍光ランプは、水銀お
よび希ガスを含む封入ガスが充填された光透過性ガラス
管と、前記光透過性ガラス管内壁面に設けられた蛍光体
粒子を含む蛍光体層と、前記封入ガス中で陽光柱放電を
維持するための手段とを具備する低圧水銀蒸気放電型の
蛍光ランプにおいて、前記蛍光体層は、紫外線で励起し
たときに赤外波長域に発光し、かつ発光ピーク波長が 7
40nm付近にある粒子表面に、ＭｇＯ，ＣａＯ，ＳｒＯ，
ＢａＯおよびＹ2 Ｏ3 から成る群れから選ばれた少なく
とも１種の金属酸化物微粒子を重量比で0.01〜 1.0％付
着した一般式、 ＬｉＡｌＯ2 ：Ｆｅ で示される鉄付活アルミン酸リチウム赤外発光蛍光体粒
子を含有していることを特徴とする。The phosphor according to the present invention comprises:
When excited by ultraviolet light, it emits light in the infrared wavelength region, and its emission peak wavelength is around 740 nm. A general formula, LiAlO 2 : Fe, which is an iron-activated lithium aluminate infrared light-emitting phosphor particle, wherein: The iron-activated lithium aluminate infrared light emitting phosphor particles have MgO, CaO, SrO,
It is characterized in that at least one kind of metal oxide fine particles selected from the group consisting of BaO and Y 2 O 3 is deposited in an amount of 0.01 to 1.0% by weight. The method for producing a phosphor according to the present invention emits light in the infrared wavelength region when excited by ultraviolet rays, and has a general formula in which the emission peak wavelength is around 740 nm: LiAlO 2 : Fe Iron activated lithium aluminate The infrared-emitting phosphor particles were surface-treated with a solution or dispersion of at least one metal alkoxide compound selected from the group consisting of Mg, Ca, Sr, Ba and Y, and then adhered to the surface of the phosphor particles. The method is characterized by comprising a step of decomposing the metal alkoxide compound and depositing and depositing metal oxide fine particles. Furthermore, the fluorescent lamp according to the present invention, a light-transmissive glass tube filled with a filling gas containing mercury and a rare gas, and a phosphor layer containing phosphor particles provided on the inner wall surface of the light-transmissive glass tube, In a low-pressure mercury vapor discharge type fluorescent lamp comprising means for maintaining a positive column discharge in the enclosed gas, the phosphor layer emits light in an infrared wavelength region when excited by ultraviolet rays, and emits light. Peak wavelength is 7
On the particle surface near 40 nm, MgO, CaO, SrO,
Iron-activated lithium aluminate infrared emission represented by the general formula LiAlO 2 : Fe, in which 0.01 to 1.0% by weight of at least one kind of metal oxide fine particles selected from the group consisting of BaO and Y 2 O 3 is attached. It is characterized by containing phosphor particles.
【０００８】上記発明は、一般式、ＬｉＡｌＯ2 ：Ｆｅ
で示される鉄付活アルミン酸リチウム赤外発光蛍光体粒
子について、詳細に調査，実験，検討を進めた結果、Ｍ
ｇＯ，ＣａＯ，ＳｒＯ，ＢａＯおよびＹ2 Ｏ3 の少なく
ともいずれか１種の金属酸化物微粒子を重量比で0.01〜
1.0％（より好ましくは 0.1〜 1.0％）、蛍光体粒子表
面に付着させたとき、 (a)蛍光体粒子の耐水性が大幅に
改善（吸水性の低減・解消）されること、 (b)蛍光体ス
ラリーとしての長期保存も可能となること、さらに (c)
発光効率も大幅に向上することを見出し、この知見に基
づいて達成したものである。なお、前記金属酸化物中Ｍ
ｇＯ，Ｙ2 Ｏ3 が特に好ましい。The above invention is based on the general formula LiAlO 2 : Fe
As a result of detailed investigations, experiments, and studies on the iron-activated lithium aluminate infrared light-emitting phosphor particles shown by
The weight ratio of at least one kind of metal oxide fine particles of gO, CaO, SrO, BaO and Y 2 O 3 is 0.01 to.
1.0% (more preferably 0.1 to 1.0%), when attached to the surface of the phosphor particles, (a) the water resistance of the phosphor particles is significantly improved (reduction / elimination of water absorption), (b) Long-term storage as a phosphor slurry is also possible, and (c)
The inventors have found that the luminous efficiency is significantly improved, and have achieved this based on this finding. In addition, M in the metal oxide
gO, Y 2 O 3 is particularly preferred.
【０００９】本発明において、蛍光体粒子表面に付着さ
せた金属酸化物微粒子が、重量比で0.01未満では、前記
のような作用・効果が認められないし、重量比で 1.0％
を超えると反って発光効率の低下などが認められるの
で、前記範囲内で常に選択する必要がある。つまり、こ
れらの金属酸化物微粒子の付着比率は、鉄付活アルミン
酸リチウム赤外発光蛍光体の発光効率の向上、および化
学的安定性の向上に大きく関与している。そして、蛍光
体に対する金属酸化物微粒子の付着量が、重量比で0.01
未満では、蛍光体に対する保護膜としての効果が低く、
化学的安定性の向上も十分に図り得ないし、逆に、 1.0
％を超えると遮光現象が起こって発光効率の低下を招来
したり、形成する蛍光体層の膜肌不良が発生し易い傾向
が認められるからである。In the present invention, when the weight ratio of the metal oxide fine particles adhered to the surface of the phosphor particles is less than 0.01, the above-described action and effect are not observed, and the weight ratio is 1.0%.
If the value exceeds the range, the luminous efficiency is lowered, so that it is necessary to always select within the above range. That is, the attachment ratio of these metal oxide fine particles has a great influence on the improvement of the luminous efficiency and the chemical stability of the iron-activated lithium aluminate infrared light emitting phosphor. And, the adhesion amount of the metal oxide fine particles to the phosphor is 0.01 by weight ratio.
If less than, the effect as a protective film for the phosphor is low,
The chemical stability cannot be improved sufficiently, on the contrary, 1.0
This is because if it exceeds%, a light-shielding phenomenon occurs to cause a decrease in luminous efficiency, and a film surface defect of the formed phosphor layer tends to occur.
【００１０】本発明において、蛍光体粒子表面に対する
金属酸化物微粒子の付着は、たとえば所要量の前記金属
酸化物微粒子の分散液に、所要量の蛍光体粒子を分散混
合させてから、濾取・乾燥後焼成処理を施すか、あるい
は前記金属のアルコキシド化合物を所要量含む溶液中
に、所要量の蛍光体粒子を分散させ、表面にアルコキシ
ド化合物を含む膜を形成させてから、濾取・乾燥後焼成
処理を施すことによって付着し得る。ここで、付着させ
る金属酸化物微粒子は、少なくとも50重量％が粒子径
0.1〜 1μm の範囲内にあることが望ましく、さらに、
蛍光体粒子表面に対する金属酸化物微粒子の付着状態
は、ほぼ一様な薄い膜状（もしくは層状）が好ましい
が、島状ないし斑点状であっても差支えない。In the present invention, the metal oxide fine particles are adhered to the surface of the phosphor particles by, for example, dispersing and mixing the required amount of the phosphor particles in a required amount of the dispersion liquid of the metal oxide fine particles, and then filtering and After baking after drying, or by dispersing the required amount of phosphor particles in a solution containing the required amount of the metal alkoxide compound, to form a film containing the alkoxide compound on the surface, after filtration and drying It can be attached by applying a baking treatment. Here, at least 50% by weight of the metal oxide fine particles to be adhered has a particle diameter.
It is desirable to be in the range of 0.1 to 1 μm.
The adhered state of the metal oxide fine particles on the surface of the phosphor particles is preferably a substantially uniform thin film (or layer), but may be island-shaped or spot-shaped.
【００１１】本発明に係る蛍光体の製造方法において、
使用するＭｇ，Ｃａ，Ｓｒ，Ｂａ，Ｙなどのアルコキシ
ド化合物としては、たとえばＭｇ（ＯＣ2 Ｈ5 ）2 、Ｂ
ａ（ＯＣ2 Ｈ5 ）2 、Ｙ（ＯＣ2 Ｈ5 ）3 、Ｍｇ（ＯＣ
3 Ｈ7 ）2 などが例示され、これらは１種もしくは２種
以上の混合系で用いることもでき、さらにアルコキシド
化合物の使用量は、熱分解して生成するＭｇＯ，Ｙ2 Ｏ
3 の付着量を考慮して選択することになる。In the method for producing a phosphor according to the present invention,
Examples of the alkoxide compound such as Mg, Ca, Sr, Ba and Y used include Mg (OC 2 H 5 ) 2 and B.
a (OC 2 H 5 ) 2 , Y (OC 2 H 5 ) 3 , Mg (OC
3 H 7 ) 2 and the like, and these can be used alone or in a mixture of two or more kinds. Further, the amount of the alkoxide compound used is MgO, Y 2 O produced by thermal decomposition.
It will be selected in consideration of the adhesion amount of 3 .
【００１２】[0012]
【作用】本発明においては、耐水性など化学的安定性が
劣り、このため十分な発光効率や長期保存性などに問題
があった一般式、ＬｉＡｌＯ2 ：Ｆｅで示される鉄付活
アルミン酸リチウム赤外発光蛍光体粒子表面に、Ｍｇ
Ｏ，ＣａＯ，ＳｒＯ，ＢａＯおよびＹ2 Ｏ3 の少なくと
もいずれか１種の金属酸化物微粒子を重量比で0.01〜
1.0％付着させたことによって、蛍光体粒子の耐水性が
大幅に改善（吸水性の低減・解消）され、長期保存にお
ける特性の経時変化も低減されるとともに、発光層を形
成したときすぐれた発光効率を呈する。In the present invention, iron-activated lithium aluminate represented by the general formula LiAlO 2 : Fe, which has poor chemical stability such as water resistance and therefore has problems with sufficient luminous efficiency and long-term storage stability. Mg on the surface of the infrared-emitting phosphor particles
O-, CaO-, SrO-, BaO- and Y 2 O 3 at least one kind of metal oxide fine particles is contained in a weight ratio of 0.01-
The 1.0% adhesion significantly improves the water resistance of the phosphor particles (reduces / eliminates water absorption), reduces the change in properties over time during long-term storage, and provides excellent light emission when the light emitting layer is formed. Exhibit efficiency.
【００１３】また、本発明の製造方法において、蛍光体
粒子表面に付着する金属酸化物微粒子源として、金属の
アルコキシド化合物を用いることにより、より緻密で薄
い付着層（膜）を形成し得るので、発光効率および特性
の経時変化など、さらに改善実・向上される。ここで、
金属アルコキシド化合物の分散液（もしくは溶媒）とし
ては、水や有機溶媒をしようし得るが、エタノールが最
も好ましい。Further, in the production method of the present invention, since a metal alkoxide compound is used as the source of the metal oxide fine particles adhered to the surface of the phosphor particles, a denser and thinner adhesion layer (film) can be formed. Further improvements and improvements such as changes in luminous efficiency and characteristics over time. here,
Water or an organic solvent may be used as the dispersion liquid (or solvent) of the metal alkoxide compound, but ethanol is most preferable.
【００１４】さらに、本発明の蛍光ランプにおいては、
前記のごとく、蛍光体粒子の耐水性改善（吸水性の低減
・解消）、特性の経時変化も低減・防止、すぐれた発光
効率を呈する発光層の形成可能など、大幅に各種の特性
が改善・向上した鉄付活アルミン酸リチウム赤外発光蛍
光体を含む形の発光層を形成しているので、赤外発光効
率が大幅に改善された光源として機能する。Further, in the fluorescent lamp of the present invention,
As mentioned above, various characteristics are greatly improved, such as improving the water resistance of phosphor particles (reducing / eliminating water absorption), reducing / preventing changes in characteristics over time, and forming a light-emitting layer exhibiting excellent luminous efficiency. Since the light emitting layer is formed so as to include the improved iron-activated lithium aluminate infrared light emitting phosphor, it functions as a light source with a significantly improved infrared light emission efficiency.
【００１５】[0015]
【実施例】以下図１および図２を参照して本発明の実施
例を説明する。Embodiments of the present invention will be described below with reference to FIGS.
【００１６】実施例１ 先ず、原材料として、たとえばγ−アルミナ（Ａｌ源）
200g、炭酸リチウム（Ｌｉ源）170g、および塩化第二鉄
六水塩（Ｆｅ源）100gをそれぞれ秤量し、これらを十分
に混合した。その後、前記混合物をアルミナ製るつぼ
（もしくは石英製るつぼ）に収容し、 900〜1200℃で 3
〜 7時間焼成してから、その焼成物（焼成体）を粉砕
し、純水でよく洗浄した。次いで、前記洗浄した粉体に
乾燥処理を施して、主波長が 254nnの紫外線で励起した
とき 740nmに発光ピークを有するスペクトル分布を示す
蛍光体粉末を得た。この蛍光体粉末について、前記条件
で焼成，粉砕処理を 1〜 2回繰り返して、一般式、Ｌｉ
ＡｌＯ2 ：Ｆｅで示される鉄付活アルミン酸リチウム赤
外発光蛍光体（粒子）を得た。Example 1 First, as a raw material, for example, γ-alumina (Al source)
200 g, 170 g of lithium carbonate (Li source), and 100 g of ferric chloride hexahydrate (Fe source) were weighed and mixed sufficiently. Then, the mixture is placed in an alumina crucible (or a quartz crucible) and heated at 900-1200 ℃.
After firing for ~ 7 hours, the fired product (fired body) was crushed and thoroughly washed with pure water. Then, the washed powder was dried to obtain a phosphor powder having a spectral distribution having an emission peak at 740 nm when excited by ultraviolet rays having a main wavelength of 254 nn. The phosphor powder was fired and crushed once or twice under the above conditions to obtain the general formula, Li
An iron-activated lithium aluminate infrared light-emitting phosphor (particles) represented by AlO 2 : Fe was obtained.
【００１７】一方、金属酸化物微粒子（微粉末）とし
て、ＭｇＯ，ＣａＯ，ＳｒＯ，ＢａＯ，Ｙ2 Ｏ3 ，Ｓｉ
Ｏ2 ，Ａｌ2 Ｏ3 ，ＺｎＯ，ＴｉＯ2 もしくはＴａ2 Ｏ
5 の微粒子（平均粒径 0.1〜 1μm ）をそれぞれ用意し
た。そして、これら金属酸化物微粒子を0.5g秤量し、そ
れぞれ水中に分散して10種類の分散液を調製し、これら
の分散液に、前記の鉄付活アルミン酸リチウム赤外発光
蛍光体（粒子）100gをそれぞれ加え、十分に攪拌・混合
した後、濾過，乾燥した。その後、 300〜 400℃で 1〜
4時間ベーキングしてから、篩別して蛍光体粒子表面
に、それぞれ対応する金属酸化物微粒子が付着した蛍光
体粒子を得た。これらの蛍光体粒子をそれぞれ分析した
ところ、蛍光体粒子表面の金属酸化物微粒子付着量は、
いずれも重量比で 0.5％であり、また主波長が 254nnの
紫外線で励起したときの発光スペクトル分布は、図１に
示すごとくであった。On the other hand, as metal oxide fine particles (fine powder), MgO, CaO, SrO, BaO, Y 2 O 3 and Si are used.
O 2 , Al 2 O 3 , ZnO, TiO 2 or Ta 2 O
Five fine particles (average particle size 0.1 to 1 μm) were prepared. Then, 0.5 g of these metal oxide fine particles were weighed, and each was dispersed in water to prepare 10 types of dispersion liquids, and these iron-activated lithium aluminate infrared light emitting phosphors (particles) were prepared. 100 g of each was added, thoroughly stirred and mixed, filtered, and dried. After that, 1 ~ at 300 ~ 400 ℃
After baking for 4 hours, it was sieved to obtain phosphor particles in which the corresponding metal oxide fine particles were attached to the surface of the phosphor particles. When each of these phosphor particles was analyzed, the amount of metal oxide fine particles deposited on the phosphor particle surface was
Each of them had a weight ratio of 0.5%, and the emission spectrum distribution when excited by ultraviolet rays having a dominant wavelength of 254nn was as shown in FIG.
【００１８】上記製造（調製）した各種の蛍光体粒子10
0g当たり、ニトロセルロースを酢酸ブチルに溶解して成
るバインダー（ＮＣバインダー） 100ccを添加し、十分
に攪拌，混合して、蛍光体スラリーをそれぞれ調製し
た。次いで、これらの蛍光体スラリーを２分し、一方の
蛍光体スラリーを、直管型のガラス管内壁面に塗布し、
乾燥後、バインダーを除去するベーキング工程、放電電
極（フィラメント型）の装着工程、排気工程を経てか
ら、水銀および封入ガスの封入，封止、さらにエージン
グ工程などを経て、 350Ｗ／ｍ2 の放射密度を有する管
径28mm，管長 600mmの直管型の蛍光ランプ（たとえばＦ
Ｌ２０ＳＳ）をそれぞれ作成した。図２はこのようにし
て、構成された蛍光ランプの要部を断面的に示したもの
で、１はガラス管、２はガラス管１の内壁面に塗布・形
成された蛍光体層（発光層）、３はガラス管１端部に封
着された放電電極、４は口金部である。これら製造した
各蛍光ランプについて、点灯を行いの発光の明るさを相
対表かする一方、 100時間点灯過程での黒化発生の有無
をみた結果を表−１に示す。なお、発光の明るさは、金
属酸化物微粒子を付着しない蛍光体で、蛍光体層を形成
した外は同一構成の蛍光ランプを基準とした。Various phosphor particles 10 produced (prepared) as described above
100 cc of a binder (NC binder) prepared by dissolving nitrocellulose in butyl acetate was added per 0 g, and the mixture was sufficiently stirred and mixed to prepare phosphor slurries. Next, these phosphor slurries are divided into two, and one of the phosphor slurries is applied to the inner wall surface of the straight tube type glass tube,
After drying, baking process to remove the binder, mounting process of the discharge electrode (filament type), exhaust process, and then sealing and sealing of mercury and sealed gas, and further aging process, radiation density of 350 W / m 2 Straight tube type fluorescent lamp with a tube diameter of 28 mm and a tube length of 600 mm (for example, F
L20SS) was prepared respectively. FIG. 2 is a cross-sectional view of the main part of the thus constructed fluorescent lamp, in which 1 is a glass tube and 2 is a phosphor layer (light emitting layer) applied / formed on the inner wall surface of the glass tube 1. ) 3 is a discharge electrode sealed to the end of the glass tube 1 and 4 is a base. For each of the manufactured fluorescent lamps, the brightness of the light emission after being lit is shown in a relative table, and the results of whether or not blackening occurred during the 100-hour lighting process are shown in Table-1. In addition, the brightness of the light emission was based on a fluorescent lamp having the same structure except that the fluorescent substance layer was not formed and a fluorescent substance layer was not formed.
【００１９】また、前記２分した残りの蛍光体スラリー
を１ケ月放置，保存した後、上記と同様な工程を採っ
て、それぞれ蛍光ランプを作成し、前記の場合と同様の
条件で発光の明るさ、黒化発生の有無を調べた結果を表
−１に併せて示す。Further, after the remaining phosphor slurry which has been divided into two parts is left for one month and stored, the same steps as described above are taken to make fluorescent lamps respectively, and the brightness of light emission is the same as the above case. Now, Table 1 also shows the results of examining the presence or absence of blackening.
【００２０】[0020]
【表１】 表−１から分かるように、本発明に係る鉄付活アルミン
酸リチウム赤外発光蛍光体（実施例）の場合は、従来例
を含む比較例の場合に比べて、蛍光体スラリー調製後す
ぐ作成した蛍光ランプでは、明るさが10〜25％改善され
ており、また１ケ月放置，保存後作成した蛍光ランプで
は、明るさが比較例では半減しているのに対して、僅か
5％低減している程度であり、さらに黒化発生も認めら
れず、安定性もすぐれていることが確認された。[Table 1] As can be seen from Table-1, in the case of the iron-activated lithium aluminate infrared light-emitting phosphor according to the present invention (Example), compared to the case of the comparative example including the conventional example, it was prepared immediately after the phosphor slurry was prepared. The brightness of the fluorescent lamp improved by 10 to 25%, and the brightness of the fluorescent lamp created after storage for one month after storage was reduced to half in the comparative example,
It was confirmed that it was reduced by 5%, blackening was not observed, and stability was excellent.
【００２１】実施例２ 実施例１の場合と同様にして製造した鉄付活アルミン酸
リチウム赤外発光蛍光体粒子、および平均粒径の異なる
ＭｇＯ，Ｙ2 Ｏ3 の微粒子をそれぞれ６種類用意した。
なお、前記金属酸化物微粒子の平均粒径は、電子顕微鏡
写真から目視で計算した値である。Example 2 Six kinds of iron-activated lithium aluminate infrared light emitting phosphor particles produced in the same manner as in Example 1 and fine particles of MgO and Y 2 O 3 having different average particle sizes were prepared. .
The average particle size of the metal oxide fine particles is a value visually calculated from an electron micrograph.
【００２２】次いで、前記実施例１の場合と同様にし
て、鉄付活アルミン酸リチウム赤外発光蛍光体粒子100g
当たり、ＭｇＯもしくはＹ2 Ｏ3 の微粒子を1.0gとして
処理し、蛍光体粒子表面にＭｇＯもしくはＹ2 Ｏ3 の微
粒子が重量比で1.0 ％付着した鉄付活アルミン酸リチウ
ム赤外発光蛍光体粒子を得た。Then, in the same manner as in Example 1, 100 g of iron-activated lithium aluminate infrared light emitting phosphor particles
Therefore, 1.0 g of MgO or Y 2 O 3 fine particles was treated, and iron-activated lithium aluminate infrared light-emitting phosphor particles with 1.0% by weight of MgO or Y 2 O 3 fine particles adhered to the surface of the phosphor particles. Got
【００２３】前記金属酸化物微粒子を付着した蛍光体粒
子を、実施例１の場合と同様の条件で、それぞれ蛍光体
スラリーを調製し、この蛍光体スラリーを２分して、そ
れぞれ直管型の蛍光ランプを作成して、明るさや黒化発
生の有無を評価した結果を表−２に示した。Phosphor particles to which the above-mentioned metal oxide fine particles are attached are prepared into phosphor slurry under the same conditions as in Example 1, and the phosphor slurry is divided into two parts, each of which has a straight tube shape. Table 2 shows the results of evaluating the brightness and the presence / absence of blackening by making a fluorescent lamp.
【００２４】[0024]
【表２】 表−２から分かるように、所定量のＭｇＯもしくはＹ2
Ｏ3 の微粒子を鉄付活アルミン酸リチウム赤外発光蛍光
体粒子面に付着させて成る鉄付活アルミン酸リチウム赤
外発光蛍光体は、付着したＭｇＯもしくはＹ2 Ｏ3 の微
粒子の平均粒径が 0.1〜 1.0μm のとき、特に好まし
く、この範囲内では、初期蛍光体スラリーで形成した蛍
光体層の明るさ特性が20〜25％向上しており、１ケ月放
置後形成した蛍光体層の明るさ特性の低下も僅か過ぎ
ず、また黒化発生の有無でも良好な特性を示した。つま
り、付着微粒子は、平均粒径が 0.1〜 1.0μm が好まし
い。[Table 2] As can be seen from Table-2, a certain amount of MgO or Y 2
The iron-activated lithium aluminate infrared light emitting phosphor obtained by adhering fine particles of O 3 on the particle surface of the iron-activated lithium aluminate infrared light-emitting phosphor has an average particle diameter of the attached MgO or Y 2 O 3 fine particles. Is 0.1 to 1.0 μm, it is particularly preferable. Within this range, the brightness characteristics of the phosphor layer formed by the initial phosphor slurry are improved by 20 to 25%, and the phosphor layer formed after leaving for 1 month is The decrease in brightness characteristics was not too slight, and good characteristics were shown with or without blackening. That is, the adhered fine particles preferably have an average particle size of 0.1 to 1.0 μm.
【００２５】実施例３ 実施例１の場合と同様にして製造した鉄付活アルミン酸
リチウム赤外発光蛍光体粒子、およびＭｇ（ＯＣ
2 Ｈ5 ）2 、Ｍｇ（ＯＣ3 Ｈ7 ）2 、Ｙ（ＯＣ2 Ｈ5）
3 、Ｂａ（ＯＣ2 Ｈ5 ）2 をそれぞれ用意した。次い
で、前記各金属アルコキシド化合物を所要量秤取し、エ
タノール中に分散・溶液化して、エタノール分散液中
に、前記蛍光体粒子の所要量を添加して、十分に攪拌，
混合した。なお、前記金属アルコキシド化合物の秤取
（秤量）に当たっては、分解して金属酸化物化したとき
の量を考慮して行われ、鉄付活アルミン酸リチウム赤外
発光蛍光体粒子100g当たり、重量比で 0.5％のたとえば
ＭｇＯ微粒子を付着する場合、Ｍｇ（ＯＣ2 Ｈ5 ）2 を
1.4g秤取（秤量）すればよい。Example 3 Iron-activated lithium aluminate infrared light emitting phosphor particles produced in the same manner as in Example 1, and Mg (OC)
2 H 5 ) 2 , Mg (OC 3 H 7 ) 2 , Y (OC 2 H 5 )
3 and Ba (OC 2 H 5 ) 2 were prepared. Next, the required amount of each metal alkoxide compound was weighed, dispersed and made into a solution in ethanol, and the required amount of the phosphor particles was added to the ethanol dispersion, and the mixture was sufficiently stirred,
Mixed. Incidentally, in the weighing (weighing) of the metal alkoxide compound, it is performed in consideration of the amount when the metal oxide is decomposed to form a metal oxide, and 100 g of iron-activated lithium aluminate infrared light emitting phosphor particles is used in a weight ratio. For example, if 0.5% of MgO particles are attached, Mg (OC 2 H 5 ) 2
1.4g Weigh (weigh).
【００２６】上記攪拌，混合から蛍光体粒子を濾取した
後、 300〜 500℃で、 1〜 4時間ベーキングを行って、
粒子表面に対応する金属酸化物微粒子が膜状に付着した
鉄付活アルミン酸リチウム赤外発光蛍光体粒子を得た。
また、この金属酸化物微粒子が膜状に付着した鉄付活ア
ルミン酸リチウム赤外発光蛍光体粒子について、電子顕
微鏡写真で観察したところ、金属酸化物微粒子の分散液
から付着させた場合よりも、緻密できれいな金属酸化物
微粒子層を付着（被覆）し得ることが確認された。After filtering the phosphor particles from the above stirring and mixing, baking is carried out at 300 to 500 ° C. for 1 to 4 hours,
Iron activated lithium aluminate infrared light emitting phosphor particles having metal oxide fine particles corresponding to the particle surfaces attached in a film form were obtained.
Further, with respect to the iron-activated lithium aluminate infrared light emitting phosphor particles in which the metal oxide fine particles are adhered in a film shape, when observed by an electron micrograph, as compared with the case where the metal oxide fine particles are adhered from a dispersion liquid, It was confirmed that a dense and clean metal oxide fine particle layer can be adhered (coated).
【００２７】前記金属酸化物微粒子を付着した各種の蛍
光体粒子を、実施例１の場合と同様の条件で、それぞれ
蛍光体スラリーを調製し、この蛍光体スラリーを２分し
て、それぞれ直管型の蛍光ランプを作成して、明るさや
黒化発生の有無を評価した結果を表−３に示した。A phosphor slurry was prepared for each of the various phosphor particles having the metal oxide fine particles adhered thereto under the same conditions as in Example 1, and the phosphor slurry was divided into two and straight pipes were respectively prepared. Table 3 shows the results of evaluating the brightness and the presence / absence of occurrence of blackening by making a type fluorescent lamp.
【００２８】[0028]
【表３】 表−３から分かるように、ＭｇＯ，ＢａＯもしくはＹ2
Ｏ3 の微粒子を、アルコキシド化合物を素材として鉄付
活アルミン酸リチウム赤外発光蛍光体粒子面に所要量付
着させて成る鉄付活アルミン酸リチウム赤外発光蛍光体
は、初期蛍光体スラリーで形成した蛍光体層の明るさ特
性などに比べて、１ケ月放置後形成した蛍光体層の明る
さ特性など遜色もなく、発行効率および安定性ともすぐ
れた特性を呈する。また、前記金属酸化物微粒子の付着
量が、重量比で0.01〜 1.0％のとき有効であり、さらに
Ｍｇ（ＯＣ2 Ｈ5 ）2 、およびＹ（ＯＣ2 Ｈ5 ）3 を素
材とした場合が有効であった。[Table 3] As can be seen from Table-3, MgO, BaO or Y 2
The iron-activated lithium aluminate infrared light emitting phosphor formed by adhering a required amount of fine particles of O 3 on the surface of the iron-activated lithium aluminate infrared light emitting phosphor particle using an alkoxide compound is formed by an initial phosphor slurry. Compared with the brightness characteristics of the phosphor layer described above, the brightness characteristics of the phosphor layer formed after being left for one month are comparable to those of the phosphor layer, and exhibit excellent emission efficiency and stability. Further, it is effective when the amount of the metal oxide fine particles adhered is 0.01 to 1.0% by weight ratio, and further, Mg (OC 2 H 5 ) 2 and Y (OC 2 H 5 ) 3 are used as materials. It was effective.
【００２９】なお、本発明は上記実施例に例示したもの
に限定されず、本発明の趣旨を逸脱しない範囲で、いろ
いろの変形を採ることも可能である。たとえば蛍光ラン
プの構成は、前記直管型の蛍光ランプＦＬ２０ＳＳ以外
の品種、あるいは他の発色蛍光体との混合系で蛍光体層
を形成する蛍光ランプなどであってもよい。The present invention is not limited to the ones illustrated in the above embodiments, and various modifications can be made without departing from the spirit of the present invention. For example, the configuration of the fluorescent lamp may be a type other than the straight tube type fluorescent lamp FL20SS, or a fluorescent lamp in which a phosphor layer is formed by a mixed system with another color-producing phosphor.
【００３０】[0030]
【発明の効果】以上説明したように、本発明に係る赤外
発光の鉄付活アルミン酸リチウム赤外発光蛍光体は、安
定的に高い発光効率を呈するとともに、化学的にも安定
性がすぐれており、スラリー状態で長期間の保存・管理
も可能となる。また、前記赤外発光の鉄付活アルミン酸
リチウム赤外発光蛍光体は、付着する金属酸化物微粒子
の生成源（素材）として、金属アルコキシド化合物を用
いることにより、容易に高品質のものを製造し得る。さ
らに、前記赤外発光の鉄付活アルミン酸リチウム赤外発
光蛍光体を、蛍光ランプの発光層とした場合は、前記す
ぐれた発光効率に伴い赤外領域での発光において、従来
の蛍光ランプに比べて大幅な改善・効果が認められる発
光源として機能する。つまり、本発明は、たとえばＯＣ
ＲなどＯＡ機器類、もしくは植物育成用など、赤外領域
の発光が要求される光源分野において、コスト面などか
らも多くの利点をもたらすものといえる。INDUSTRIAL APPLICABILITY As described above, the infrared-emitting iron-activated lithium aluminate infrared light-emitting phosphor according to the present invention stably exhibits high luminous efficiency and is chemically stable. Therefore, it can be stored and managed in a slurry state for a long period of time. Moreover, the iron-activated lithium aluminate infrared light-emitting phosphor for infrared light emission can be easily produced in high quality by using a metal alkoxide compound as a generation source (material) of the adhered metal oxide fine particles. You can Furthermore, when the iron-activated lithium aluminate infrared light emitting phosphor for infrared light emission is used as a light emitting layer of a fluorescent lamp, it is possible to obtain a conventional fluorescent lamp in light emission in the infrared region due to the excellent light emission efficiency. It functions as a light-emitting source that is significantly improved and effective. That is, the present invention, for example, OC
It can be said that it brings many advantages in terms of cost in the field of light sources that require light emission in the infrared region, such as OA equipment such as R, or for growing plants.
【図１】本発明に係る赤外発光の鉄付活アルミン酸リチ
ウム蛍光体の 254nm紫外線励起による発光スペクトルの
分布図。FIG. 1 is a distribution chart of an emission spectrum of an iron-activated lithium aluminate phosphor for infrared emission according to the present invention when excited by 254 nm ultraviolet light.
【図２】本発明に係る蛍光ランプの要部構成例を示す断
面図。FIG. 2 is a sectional view showing a configuration example of a main part of a fluorescent lamp according to the present invention.
１…ガラス管 ２…蛍光体層（発光層） ３…放電
電極 ４…口金部1 ... Glass tube 2 ... Phosphor layer (light emitting layer) 3 ... Discharge electrode 4 ... Base part
Claims (3)
光し、その発光ピーク波長が 740nm付近にある一般式、 ＬｉＡｌＯ2 ：Ｆｅ で示される鉄付活アルミン酸リチウム赤外発光蛍光体粒
子であって、 前記鉄付活アルミン酸リチウム赤外発光蛍光体粒子は、
その粒子表面にＭｇＯ，ＣａＯ，ＳｒＯ，ＢａＯおよび
Ｙ2 Ｏ3 から成る群れから選ばれた少なくとも１種の金
属酸化物微粒子を重量比で0.01〜 1.0％付着させて成る
ことを特徴とする蛍光体。1. An iron-activated lithium aluminate infrared light-emitting phosphor particle represented by the general formula: LiAlO 2 : Fe, which emits light in the infrared wavelength range when excited by ultraviolet rays and has a peak emission wavelength near 740 nm. That is, the iron-activated lithium aluminate infrared light emitting phosphor particles,
A phosphor characterized by comprising 0.01 to 1.0% by weight of at least one kind of metal oxide fine particles selected from the group consisting of MgO, CaO, SrO, BaO and Y 2 O 3 deposited on the surface of the particles. .
光し、その発光ピーク波長が 740nm付近にある一般式、 ＬｉＡｌＯ2 ：Ｆｅ で示される鉄付活アルミン酸リチウム赤外発光蛍光体粒
子を、Ｍｇ，Ｃａ，Ｓｒ，ＢａおよびＹから成る群れか
ら選ばれた少なくとも１種の金属アルコキシド化合物の
溶液ないし分散液にて表面処理した後、蛍光体粒子表面
に付着した金属アルコキシド化合物を分解させ、金属酸
化物微粒子を析出・被着させる工程を具備することを特
徴とする蛍光体の製造方法。2. An iron-activated lithium aluminate infrared light-emitting phosphor particle represented by the general formula: LiAlO 2 : Fe, which emits light in the infrared wavelength region when excited by ultraviolet light and has a light emission peak wavelength near 740 nm. Is surface-treated with a solution or dispersion of at least one metal alkoxide compound selected from the group consisting of Mg, Ca, Sr, Ba and Y, and then the metal alkoxide compound attached to the surface of the phosphor particles is decomposed. A method for producing a phosphor, comprising a step of depositing and depositing metal oxide fine particles.
された光透過性ガラス管と、前記光透過性ガラス管内壁
面に設けられた蛍光体粒子を含む蛍光体層と、前記封入
ガス中で陽光柱放電を維持するための手段とを具備する
低圧水銀蒸気放電型の蛍光ランプにおいて、 前記蛍光体層は、紫外線で励起したときに赤外波長域に
発光し、かつ発光ピーク波長が 740nm付近にある粒子表
面に、ＭｇＯ，ＣａＯ，ＳｒＯ，ＢａＯおよびＹ2 Ｏ3
から成る群れから選ばれた少なくとも１種の金属酸化物
微粒子を重量比で0.01〜 1.0％付着した一般式、 ＬｉＡｌＯ2 ：Ｆｅ で示される鉄付活アルミン酸リチウム赤外発光蛍光体粒
子を含有していることを特徴とする蛍光ランプ。3. A light-transmitting glass tube filled with a filling gas containing mercury and a rare gas, a phosphor layer containing phosphor particles provided on the inner wall surface of the light-transmitting glass tube, and the filling gas in the filling gas. In a low-pressure mercury vapor discharge type fluorescent lamp comprising means for maintaining positive column discharge, the phosphor layer emits in an infrared wavelength region when excited by ultraviolet rays, and an emission peak wavelength is around 740 nm. , MgO, CaO, SrO, BaO and Y 2 O 3
Containing at least one kind of metal oxide fine particles selected from the group consisting of 0.01 to 1.0% by weight of the general formula, iron-activated lithium aluminate infrared light emitting phosphor particles represented by LiAlO 2 : Fe Fluorescent lamp characterized by having.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6048994A JPH07268318A (en) | 1994-03-30 | 1994-03-30 | Fluorescent substance, its production and fluorescent lamp |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6048994A JPH07268318A (en) | 1994-03-30 | 1994-03-30 | Fluorescent substance, its production and fluorescent lamp |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH07268318A true JPH07268318A (en) | 1995-10-17 |
Family
ID=13143753
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP6048994A Withdrawn JPH07268318A (en) | 1994-03-30 | 1994-03-30 | Fluorescent substance, its production and fluorescent lamp |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH07268318A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11263971A (en) * | 1998-03-19 | 1999-09-28 | Nichia Chem Ind Ltd | Iron-activated lithium aluminate fluorescent substance and its fluorescent lamp |
| US6290874B1 (en) * | 1999-01-16 | 2001-09-18 | U.S. Philips Corporation | Display screen comprising a metal oxide-containing phosphor composition |
| CN115109582A (en) * | 2022-06-09 | 2022-09-27 | 合肥工业大学智能制造技术研究院 | Red light-near infrared light LED device and application thereof |
-
1994
- 1994-03-30 JP JP6048994A patent/JPH07268318A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11263971A (en) * | 1998-03-19 | 1999-09-28 | Nichia Chem Ind Ltd | Iron-activated lithium aluminate fluorescent substance and its fluorescent lamp |
| US6290874B1 (en) * | 1999-01-16 | 2001-09-18 | U.S. Philips Corporation | Display screen comprising a metal oxide-containing phosphor composition |
| CN115109582A (en) * | 2022-06-09 | 2022-09-27 | 合肥工业大学智能制造技术研究院 | Red light-near infrared light LED device and application thereof |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A300 | Withdrawal of application because of no request for examination |
Free format text: JAPANESE INTERMEDIATE CODE: A300 Effective date: 20010605 |