JP4894244B2 - Phosphor paste for plasma display panel - Google Patents
Phosphor paste for plasma display panel Download PDFInfo
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- JP4894244B2 JP4894244B2 JP2005341756A JP2005341756A JP4894244B2 JP 4894244 B2 JP4894244 B2 JP 4894244B2 JP 2005341756 A JP2005341756 A JP 2005341756A JP 2005341756 A JP2005341756 A JP 2005341756A JP 4894244 B2 JP4894244 B2 JP 4894244B2
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Description
本発明は、プラズマディスプレイパネル用蛍光体ペーストに関するものである。 The present invention relates to a phosphor paste for a plasma display panel.
プラズマディスプレイパネル（以下ＰＤＰと略称する）を製造するためには、発光表示材料である蛍光体をセル内面に塗布する必要がある。このような蛍光体の塗布は、まず蛍光体粉体を有機バインダー樹脂で分散したペーストを製造し、これを隔壁セル内に吐出、もしくは印刷して行うのが一般的である。 In order to manufacture a plasma display panel (hereinafter abbreviated as PDP), it is necessary to apply a phosphor as a light emitting display material to the inner surface of the cell. In general, such a phosphor is applied by first producing a paste in which phosphor powder is dispersed with an organic binder resin, and discharging or printing the paste in a partition cell.
最終的に発光させるには、焼成により有機バインダー樹脂を燃焼、除去する必要があり、この際に有機物の痕跡があると発光の妨げとなるので、燃焼性の点においてはできる限り有機バインダー樹脂の含有量が少ないほうが好ましい。 In order to finally emit light, it is necessary to burn and remove the organic binder resin by firing. At this time, if there is a trace of organic matter, it will hinder light emission. A lower content is preferred.
しかしながら、有機バインダー樹脂の含有量を少なくすると蛍光体ペーストの粘度が低下し、ペースト中で蛍光体粉体が沈降してしまうという課題があった。 However, when the content of the organic binder resin is reduced, the viscosity of the phosphor paste decreases, and there is a problem that the phosphor powder settles in the paste.
また、蛍光体ペーストを印刷、塗布する際においてもペーストの粘度が低すぎると、取扱い性が著しく低下し、隔壁セル内へのペースト注入が不均一になってしまうという課題もあった。 In addition, when the phosphor paste is printed and applied, if the viscosity of the paste is too low, the handleability is remarkably lowered, and there is a problem that the paste is not uniformly injected into the partition walls.
このような課題の解決策として、例えば特許文献１に示すように、増粘剤を添加する方法が提案されているが、構造粘性が強くなって印刷、塗布性が低下するという問題があった。また使用する増粘剤の燃焼性に対しての懸念もあった。
本発明は、このような課題に鑑みなされたもので、燃焼性に懸念のある添加剤（増粘剤）を使用することなく、ペーストの沈降性や取扱い性を改善することを目的とする。 This invention is made | formed in view of such a subject, and it aims at improving the sedimentation property and handleability of a paste, without using the additive (thickener) which has concern about combustibility.
上記課題を解決するために本発明によるＰＤＰ用蛍光体ペーストは、以下の（１）〜（３）の条件を満たすことを特徴とする。
（１）温度２５℃でのせん断速度１００ｓ-1の時の粘度が、５〜３０Ｐａ・ｓの範囲
（２）温度２５℃でのせん断速度２００ｓ-1の時の粘度が、１〜２０Ｐａ・ｓの範囲
（３）温度２５℃でのせん断速度１０００ｓ-1の時の粘度が、０．１〜１Ｐａ・ｓの範囲
In order to solve the above problems, the phosphor paste for PDP according to the present invention satisfies the following conditions (1) to (3).
(1) Viscosity at a shear rate of 100 s −1 at 25 ° C. in the range of 5 to 30 Pa · s (2) Viscosity at a shear rate of 200 s −1 at a temperature of 25 ° C. of 1 to 20 Pa · s (3) The viscosity at a shear rate of 1000 s −1 at a temperature of 25 ° C. is in the range of 0.1 to 1 Pa · s.
本発明の蛍光体ペーストは、良好な燃焼性を持ちながら、優れた取扱い性を有するため、これを採用することで、ＰＤＰの信頼性や生産性を向上させることが可能となる。 Since the phosphor paste of the present invention has excellent combustibility while having good flammability, the use of this makes it possible to improve the reliability and productivity of the PDP.
まず、本発明によるＰＤＰ用蛍光体ペーストは、少なくとも蛍光体粉末、有機バインダー樹脂および有機溶剤を構成成分とする蛍光体ペーストであり、以下の（１）〜（３）の条件を満たすことを特徴とする。
（１）温度２５℃でのせん断速度１００ｓ-1の時の粘度が、５〜３０Ｐａ・ｓの範囲
（２）温度２５℃でのせん断速度２００ｓ-1の時の粘度が、１〜２０Ｐａ・ｓの範囲
（３）温度２５℃でのせん断速度１０００ｓ-1の時の粘度が、０．１〜１Ｐａ・ｓの範囲
また、上記条件に加えて、温度２５℃でのせん断速度１ｓ-1の時の粘度が、３０〜６０Ｐａ・ｓの範囲であるのが望ましく、さらに蛍光体ペースト中の蛍光体粉末の含有量は、３０〜６０％（重量比）であり、また蛍光体ペースト中の有機バインダー樹脂の含有量は、１〜２０％（重量比）であるのが望ましい。
First, the phosphor paste for PDP according to the present invention is a phosphor paste containing at least phosphor powder, an organic binder resin, and an organic solvent as constituents, and satisfies the following conditions (1) to (3): And
(1) Viscosity at a shear rate of 100 s −1 at 25 ° C. in the range of 5 to 30 Pa · s (2) Viscosity at a shear rate of 200 s −1 at a temperature of 25 ° C. of 1 to 20 Pa · s (3) The viscosity at a shear rate of 1000 s −1 at a temperature of 25 ° C. is in the range of 0.1 to 1 Pa · s. In addition to the above conditions, at a shear rate of 1 s −1 at a temperature of 25 ° C. The viscosity of is preferably in the range of 30 to 60 Pa · s, and the phosphor powder content in the phosphor paste is 30 to 60% (weight ratio), and the organic binder in the phosphor paste The resin content is desirably 1 to 20% (weight ratio).
また、本発明の蛍光体ペーストの構成成分である蛍光体粉末は、波長２００ｎｍ以下、例えば１４７ｎｍの真空紫外線励起下で効率的に発光し得る蛍光体であることが好ましい。なかでも、［（Ｙ，Ｇｄ，Ｅｕ）ＢＯ3］、［（Ｚｎ，Ｍｎ）2ＳｉＯ4］、［（Ｂａ，Ｅｕ）ＭｇＡｌ10Ｏ17］は発光効率、色合いともに良好であるため特に好ましいが、蛍光体ペーストとしては、少なくともこれらのうちの１種類を含有していればよく、上記３種類に限定されるものではない。 Further, the phosphor powder that is a constituent component of the phosphor paste of the present invention is preferably a phosphor that can emit light efficiently under vacuum ultraviolet light excitation with a wavelength of 200 nm or less, for example, 147 nm. Among these, [(Y, Gd, Eu) BO 3 ], [(Zn, Mn) 2 SiO 4 ], and [(Ba, Eu) MgAl 10 O 17 ] are particularly preferable because of their good luminous efficiency and color. The phosphor paste only needs to contain at least one of these, and is not limited to the above three types.
また、有機バインダー樹脂は、平均分子量の異なった２種類の混合物で、それぞれの重量平均分子量が５０，０００〜１５０，０００の範囲および１５０，０００〜２５０，０００の範囲であることが好ましい。なかでも、７０，０００〜１００，０００の範囲および１７０，０００〜２００，０００の範囲の樹脂の組み合わせは、ペーストとしての取扱い性が優れているため、好ましい。 In addition, the organic binder resin is a mixture of two types having different average molecular weights, and each weight average molecular weight is preferably in the range of 50,000 to 150,000 and in the range of 150,000 to 250,000. Especially, since the combination of resin of the range of 70,000-100,000 and the range of 170,000-200,000 is excellent in the handleability as a paste, it is preferable.
さらに、本発明の蛍光体ペーストの構成成分である有機溶剤は、沸点が１００℃〜３００℃のもので、バインダー及び蛍光体粉体成分と分離しないものであれば特に制限はなく、アルコール系、エーテル系、エステル系のものが好ましい。例えば、テルピネオール（沸点２１７℃）、ベンジルアルコール（沸点２０５℃）、Ｎ−メチルピロリドン（沸点２０２℃）、ジエチレングリコールモノブチルエーテル（沸点２３１℃）、トリエチレングリコールモノメチルエーテル（沸点２４５℃）、トリエチレングリコールジメチルエーテル（沸点２１６℃）等は作業性に優れていて好ましい。 Furthermore, the organic solvent that is a constituent of the phosphor paste of the present invention has a boiling point of 100 ° C. to 300 ° C., and is not particularly limited as long as it does not separate from the binder and the phosphor powder component. Ether type and ester type are preferable. For example, terpineol (boiling point 217 ° C.), benzyl alcohol (boiling point 205 ° C.), N-methylpyrrolidone (boiling point 202 ° C.), diethylene glycol monobutyl ether (boiling point 231 ° C.), triethylene glycol monomethyl ether (boiling point 245 ° C.), triethylene glycol Dimethyl ether (boiling point 216 ° C.) or the like is preferable because of its excellent workability.
以下、具体的実施例により本発明をさらに詳しく説明する。以下の実施例は例示の目的で提供され、本発明を限定するものではない。 Hereinafter, the present invention will be described in more detail with reference to specific examples. The following examples are provided for purposes of illustration and are not intended to limit the invention.
（蛍光体ペーストの調整）
重量平均分子量の主ピークが７４，０００であるエチルセルロースを、ベンジルアルコールに溶解し、２０％（重量）濃度の溶液を作製し、有機バインダー樹脂Ａのストック溶液とした。
(Adjustment of phosphor paste)
Ethyl cellulose having a main peak of weight average molecular weight of 74,000 was dissolved in benzyl alcohol to prepare a 20% (weight) concentration solution as a stock solution of organic binder resin A.
また、重量平均分子量の主ピークが１９０，０００であるエチルセルロースを、ベンジルアルコールに溶解し、２０％（重量）濃度の溶液を作製し、有機バインダー樹脂Ｂのストック溶液とした。 Further, ethyl cellulose having a main peak of weight average molecular weight of 190,000 was dissolved in benzyl alcohol to prepare a 20% (weight) concentration solution, which was used as a stock solution of organic binder resin B.
上記有機バインダー樹脂Ａのストック溶液３９．７ｇと、有機バインダー樹脂Ｂのストック溶液１０．６ｇとを混合（樹脂Ａ／樹脂Ｂ＝１５／４）し、これに４９．７ｇの赤色蛍光体粉末［（Ｙ，Ｇｄ，Ｅｕ）ＢＯ3］を投入し、一様に分散するまでステンレスヘラを用いて約５分間撹拌し、予備混練した。予備混練後のペーストを３本ロールミルを用いて本混練（ロールギャップなし、２回混練）し、およそ９０ｇの赤色蛍光体ペーストを得た。 39.7 g of the organic binder resin A stock solution and 10.6 g of the organic binder resin B stock solution were mixed (resin A / resin B = 15/4), and 49.7 g of red phosphor powder [ (Y, Gd, Eu) BO 3 ] was added, and the mixture was stirred for about 5 minutes using a stainless spatula until uniformly dispersed, and pre-kneaded. The pre-kneaded paste was main-kneaded (no roll gap, twice kneaded) using a three-roll mill to obtain about 90 g of a red phosphor paste.
緑色蛍光体粉末［（Ｚｎ，Ｍｎ）2ＳｉＯ4］、及び青色蛍光体粉末［（Ｂａ，Ｅｕ）ＭｇＡｌ10Ｏ17］についても、上記赤色蛍光体粉末の場合と同様にペースト混練を行い、それぞれおよそ９０ｇの蛍光体ペーストを得た。 For green phosphor powder [(Zn, Mn) 2 SiO 4 ] and blue phosphor powder [(Ba, Eu) MgAl 10 O 17 ], paste kneading was performed in the same manner as in the case of the red phosphor powder, Approximately 90 g of phosphor paste was obtained.
また、比較用として有機バインダー樹脂Ａのみを用いて、上記と同様に赤色蛍光体ペーストを作製した。 For comparison, a red phosphor paste was prepared in the same manner as described above using only the organic binder resin A.
（蛍光体ペーストの粘度測定）
上記で作製した４種類の蛍光体ペーストについて、それぞれの粘度特性を測定した。測定には、ハーケ社製ストレスレオメータＲＳ−１５０を用い、せん断速度がそれぞれ、１ｓ-1、１０ｓ-1、１００ｓ-1、２００ｓ-1、１０００ｓ-1の時の粘度を測定した。結果を（表１）に示す。なお、粘性係数はせん断速度１ｓ-1の時の粘度である。
(Measurement of viscosity of phosphor paste)
The viscosity characteristics of each of the four types of phosphor pastes prepared above were measured. For the measurement, using a Haake Co. stress rheometer RS-0.99, shear rate, respectively, 1s -1, 10s -1, 100s -1, 200s -1, the viscosity was measured at a 1000 s -1. The results are shown in (Table 1). The viscosity coefficient is a viscosity at a shear rate of 1 s- 1 .
（蛍光体ペーストの燃焼分析）
上記比較用以外の３種類のペーストについて、室温→５２０℃（３０分）、５２０℃到達後１０分間保持の昇温条件で熱分析を行い、重量減少割合を測定した。測定前のペースト重量に対する燃焼残分の重量比を（表１）に示す。
(Combustion analysis of phosphor paste)
For the three types of pastes other than those for comparison, room temperature → 520 ° C. (30 minutes), thermal analysis was performed under the temperature rising condition of holding for 10 minutes after reaching 520 ° C., and the weight loss ratio was measured. The weight ratio of the combustion residue to the paste weight before measurement is shown in (Table 1).
（蛍光体ペーストの印刷、塗布性評価）
上記４種類のペーストについて、孔径１００μｍの穴が開けられた口金を用いて、４７０ｋＰａの圧力でガラス基板（２０×２０ｃｍ）上に吐出した。
(Printing of phosphor paste, evaluation of applicability)
About the said 4 types of paste, it discharged on the glass substrate (20 * 20 cm) with the pressure of 470 kPa using the nozzle | cap | die with which the hole diameter of 100 micrometers was opened.
ペーストの吐出と同時に、ガラス基板を４０ｍｍ／秒の速さで移動させ、線状に塗布されたペーストの、塗布量のムラ、塗布の抜けを観察した。 Simultaneously with the discharge of the paste, the glass substrate was moved at a speed of 40 mm / second, and unevenness in the coating amount and missing of the coating of the paste applied in a linear form were observed.
塗布ムラ、塗布抜けの有無を（表１）に示す。 The presence or absence of coating unevenness and missing coating is shown in Table 1.
以上のように本発明の蛍光体ペーストは、良好な燃焼性を持ちながら、優れた取扱い性を有するため、これを採用することで、ＰＤＰの信頼性や生産性を向上させることが可能となる。 As described above, since the phosphor paste of the present invention has excellent handling properties while having good flammability, the use of this makes it possible to improve the reliability and productivity of the PDP. .
Claims (5)
（１）温度２５℃でのせん断速度１ｓ −１ の時の粘度が、３０〜６０Ｐａ・ｓの範囲
（２）温度２５℃でのせん断速度１００ｓ−１の時の粘度が、５〜３０Ｐａ・ｓの範囲
（３）温度２５℃でのせん断速度２００ｓ−１の時の粘度が、１〜２０Ｐａ・ｓの範囲
（４）温度２５℃でのせん断速度１０００ｓ−１の時の粘度が、０．１〜１Ｐａ・ｓの範囲 In the phosphor paste for a plasma display panel having at least a phosphor powder, an organic binder resin, and an organic solvent as constituent components, the organic binder resin is composed of two types of organic binder resin A and organic binder resin B, and the organic The weight average molecular weight of the binder resin A is in the range of 50,000 to 150,000, the weight average molecular weight of the organic binder resin B is in the range of 150,000 to 250,000, and the following (1) to (4) A phosphor paste for a plasma display panel characterized by satisfying the following conditions.
(1) The viscosity at a shear rate of 1 s −1 at a temperature of 25 ° C. is in the range of 30 to 60 Pa · s.
(2) Viscosity at a shear rate of 100 s −1 at a temperature of 25 ° C. is in the range of 5 to 30 Pa · s.
(3) Viscosity at a shear rate of 200 s −1 at a temperature of 25 ° C. is in the range of 1 to 20 Pa · s.
(4) The viscosity at a shear rate of 1000 s −1 at a temperature of 25 ° C. is in the range of 0.1 to 1 Pa · s.
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| JP2005341756A JP4894244B2 (en) | 2005-11-28 | 2005-11-28 | Phosphor paste for plasma display panel |
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| JP2005341756A JP4894244B2 (en) | 2005-11-28 | 2005-11-28 | Phosphor paste for plasma display panel |
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| JP4894244B2 true JP4894244B2 (en) | 2012-03-14 |
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| JP2009167241A (en) * | 2008-01-11 | 2009-07-30 | Toray Ind Inc | Phosphor paste and manufacturing method of plasma display panel using the same |
| EP2752898A4 (en) | 2011-10-07 | 2015-09-09 | Konica Minolta Inc | Phosphor dispersion liquid, and production method for led device using same |
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| JP2001294850A (en) * | 2000-04-17 | 2001-10-23 | Matsushita Electric Ind Co Ltd | Fluorescent substance paste and plasma display panel using the same |
| JP2002150937A (en) * | 2000-11-07 | 2002-05-24 | Matsushita Electric Ind Co Ltd | Fluorescent substance paste |
| JP4281432B2 (en) * | 2002-06-27 | 2009-06-17 | パナソニック株式会社 | Method for manufacturing plasma display panel |
| KR20070043151A (en) * | 2005-10-20 | 2007-04-25 | 삼성전기주식회사 | Dispersant with silane head and phosphor paste compositions comprising the same |
| KR20070043142A (en) * | 2005-10-20 | 2007-04-25 | 삼성전기주식회사 | Thiol dispersant and sulfide phosphor paste composition comprising the same |
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