JP4833899B2 - Zinc-containing magnesium oxide fired powder - Google Patents
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- JP4833899B2 JP4833899B2 JP2007085121A JP2007085121A JP4833899B2 JP 4833899 B2 JP4833899 B2 JP 4833899B2 JP 2007085121 A JP2007085121 A JP 2007085121A JP 2007085121 A JP2007085121 A JP 2007085121A JP 4833899 B2 JP4833899 B2 JP 4833899B2
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- 239000000843 powder Substances 0.000 title claims description 78
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 title claims description 56
- 239000000395 magnesium oxide Substances 0.000 title claims description 55
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 title claims description 55
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims description 43
- 229910052725 zinc Inorganic materials 0.000 title claims description 43
- 239000011701 zinc Substances 0.000 title claims description 43
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 24
- 239000010410 layer Substances 0.000 claims description 23
- 239000011241 protective layer Substances 0.000 claims description 13
- 238000010304 firing Methods 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 239000011787 zinc oxide Substances 0.000 claims description 9
- 239000007789 gas Substances 0.000 description 39
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 11
- 238000000034 method Methods 0.000 description 8
- 239000010408 film Substances 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 230000001771 impaired effect Effects 0.000 description 2
- 150000002681 magnesium compounds Chemical class 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
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- 150000003752 zinc compounds Chemical class 0.000 description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 2
- 238000004438 BET method Methods 0.000 description 1
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 description 1
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000007610 electrostatic coating method Methods 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 description 1
- 239000011654 magnesium acetate Substances 0.000 description 1
- 235000011285 magnesium acetate Nutrition 0.000 description 1
- 229940069446 magnesium acetate Drugs 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 229910052754 neon Inorganic materials 0.000 description 1
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- 239000004246 zinc acetate Substances 0.000 description 1
- 239000011667 zinc carbonate Substances 0.000 description 1
- 235000004416 zinc carbonate Nutrition 0.000 description 1
- 229910000010 zinc carbonate Inorganic materials 0.000 description 1
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 description 1
- 229940007718 zinc hydroxide Drugs 0.000 description 1
- 229910021511 zinc hydroxide Inorganic materials 0.000 description 1
- ZPEJZWGMHAKWNL-UHFFFAOYSA-L zinc;oxalate Chemical compound [Zn+2].[O-]C(=O)C([O-])=O ZPEJZWGMHAKWNL-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/02—Magnesia
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J11/00—Gas-filled discharge tubes with alternating current induction of the discharge, e.g. alternating current plasma display panels [AC-PDP]; Gas-filled discharge tubes without any main electrode inside the vessel; Gas-filled discharge tubes with at least one main electrode outside the vessel
- H01J11/20—Constructional details
- H01J11/34—Vessels, containers or parts thereof, e.g. substrates
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Plasma & Fusion (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Gas-Filled Discharge Tubes (AREA)
- Luminescent Compositions (AREA)
Description
本発明は、亜鉛を含有する酸化マグネシウム焼成物粉末に関する。 The present invention relates to a magnesium oxide fired powder containing zinc.
交流型プラズマディスプレイパネル（以下、ＡＣ型ＰＤＰともいう）は、一般に、画像表示面となる前面板と、放電ガスが充填された放電空間を挟んで対向配置された背面板とからなる。前面板は、前面ガラス基板、前面ガラスの上に形成された一対の放電電極、放電電極を被覆するように形成された誘電体層、そして誘電体層の表面に形成された誘電体保護層からなる。背面板は、背面ガラス基板、ガラス基板の上に形成されたアドレス電極、ガラス基板とアドレス電極とを被覆するように形成された、放電空間を区画するための隔壁、そして隔壁の表面に形成された赤、緑、青の蛍光体層からなる。 An AC type plasma display panel (hereinafter also referred to as AC type PDP) is generally composed of a front plate serving as an image display surface and a back plate disposed so as to face each other across a discharge space filled with a discharge gas. The front plate includes a front glass substrate, a pair of discharge electrodes formed on the front glass, a dielectric layer formed to cover the discharge electrodes, and a dielectric protective layer formed on the surface of the dielectric layer. Become. The back plate is formed on the back glass substrate, the address electrodes formed on the glass substrate, the barrier ribs for partitioning the discharge space formed to cover the glass substrate and the address electrodes, and the barrier rib surfaces. It consists of red, green and blue phosphor layers.
放電ガスとしては、一般にＸｅ（キセノン）とＮｅ（ネオン）との混合ガスが利用されている。この混合ガスでは、Ｘｅが放電ガスであり、Ｎｅはバッファガスである。
誘電体保護層の形成材料には、ＡＣ型ＰＤＰの作動電圧を低減し、かつ放電空間に生成したプラズマから誘電体層を保護するために、二次電子放出係数が高く、耐スパッタ性に優れる酸化マグネシウムが広く利用されている。
As the discharge gas, a mixed gas of Xe (xenon) and Ne (neon) is generally used. In this mixed gas, Xe is a discharge gas and Ne is a buffer gas.
The material for forming the dielectric protective layer has a high secondary electron emission coefficient and excellent sputter resistance in order to reduce the operating voltage of the AC type PDP and protect the dielectric layer from the plasma generated in the discharge space. Magnesium oxide is widely used.
従来より、ＡＣ型ＰＤＰにおいては、発光特性の向上を目的として、誘電体保護層の放電空間側の表面に、放電ガスにより生成する紫外光によって励起されて、蛍光体層の蛍光体を励起し得る波長の紫外光を放出する紫外光放出層を設けて、放電ガスから放出される紫外光と、紫外光放出層から放出される紫外光とにより蛍光体層の蛍光体を励起させることにより、蛍光体層の発光効率を向上させることが検討されている。 Conventionally, in the AC type PDP, for the purpose of improving the light emission characteristics, the phosphor of the phosphor layer is excited on the surface of the dielectric protective layer on the discharge space side by the ultraviolet light generated by the discharge gas. By providing an ultraviolet light emitting layer that emits ultraviolet light of a wavelength to be obtained, by exciting the phosphor in the phosphor layer with ultraviolet light emitted from the discharge gas and ultraviolet light emitted from the ultraviolet light emitting layer, It has been studied to improve the luminous efficiency of the phosphor layer.
例えば、特許文献１には、マグネシウムが加熱されて発生される蒸気が気相酸化されることによって生成した、ＢＥＴ法によって測定した平均粒子径が５００オングストローム以上、好ましくは２０００オングストローム以上の気相法酸化マグネシウム単結晶体からなる紫外光放出層を、誘電体保護層の放電空間側の表面に形成したＡＣ型ＰＤＰが開示されている。そして、この紫外光放出層は２３０〜２５０ｎｍの範囲にピーク波長を有する紫外光を放出し、その波長の紫外光により蛍光体が励起されて発光することにより、ＰＤＰの輝度が増加することが開示されている。 For example, Patent Document 1 discloses a vapor phase method in which vapor generated by heating magnesium is vapor-phase oxidized, and an average particle size measured by the BET method is 500 angstroms or more, preferably 2000 angstroms or more. There is disclosed an AC type PDP in which an ultraviolet light emitting layer made of a magnesium oxide single crystal is formed on the surface of the dielectric protective layer on the discharge space side. This ultraviolet light emitting layer emits ultraviolet light having a peak wavelength in the range of 230 to 250 nm, and the phosphor is excited by the ultraviolet light of that wavelength to emit light, thereby increasing the brightness of the PDP. Has been.
一方、特許文献２には、酸化マグネシウムと酸化亜鉛とを混合・混練して調製した分散溶液を用いて製造したＰＤＰの誘電体層保護層（酸化マグネシウム膜）が開示されている。この特許文献２には、酸化亜鉛の添加効果として、放電開始電圧が低減する旨の記載がある。但し、得られた酸化マグネシウム薄膜が、ＰＤＰの放電ガスにて生成した紫外光により励起されることにより、紫外光を発光する旨の記載はない。
本発明の目的は、ＡＣ型ＰＤＰなどのガス放電発光装置の誘電体保護層の上に形成する紫外光放出層の材料として有用な、Ｘｅガスのガス放電により生成した紫外光により励起されると、波長２５０ｎｍ付近にピーク波長を有する紫外光を高い効率で放出する酸化マグネシウム粉末を提供することにある。 The object of the present invention is to be excited by ultraviolet light generated by gas discharge of Xe gas, which is useful as a material for an ultraviolet light emitting layer formed on a dielectric protective layer of a gas discharge light emitting device such as an AC type PDP. Another object of the present invention is to provide a magnesium oxide powder that emits ultraviolet light having a peak wavelength around 250 nm with high efficiency.
本発明者は、酸化マグネシウム源粉末と酸化亜鉛源粉末とを焼成後の亜鉛含有量が０．１〜３０質量％となるように混合して、好ましくは８５０℃以上の温度で、特に１０分以上焼成することにより得られた亜鉛含有酸化マグネシウム焼成物粉末は、Ｘｅガスのガス放電により生成した紫外光に励起されて波長２５０ｎｍ付近（波長２３０〜２６０ｎｍの範囲）にピーク波長を有する紫外光を高い効率で放出することを見出し、本発明を完成した。 The inventor mixed the magnesium oxide source powder and the zinc oxide source powder so that the zinc content after firing would be 0.1 to 30% by mass, preferably at a temperature of 850 ° C. or more, particularly for 10 minutes. The zinc-containing magnesium oxide fired powder obtained by firing as described above is excited by ultraviolet light generated by gas discharge of Xe gas and emits ultraviolet light having a peak wavelength in the vicinity of a wavelength of 250 nm (wavelength range of 230 to 260 nm). The present invention was completed by finding that it can be released with high efficiency.
従って、本発明は、亜鉛を０．１〜３０質量％の範囲にて含有し、Ｘｅガスのガス放電により生成した紫外光に励起されて波長２３０〜２６０ｎｍの範囲にピーク波長を有する紫外光を放出する亜鉛含有酸化マグネシウム焼成物粉末にある。 Therefore, the present invention contains ultraviolet light containing zinc in a range of 0.1 to 30% by mass and having a peak wavelength in the range of 230 to 260 nm when excited by ultraviolet light generated by gas discharge of Xe gas. It is in the zinc-containing magnesium oxide fired powder to be released .
上記本発明の亜鉛含有酸化マグネシウム焼成物粉末の好ましい態様は次の通りである。（１）亜鉛含有量が０．５〜７質量％の範囲にある。
（２）酸化マグネシウム源粉末と酸化亜鉛源粉末との粉末混合物を、８５０℃以上、特に９００〜１５００℃の範囲の温度で焼成することにより得られたものである。
（３）上記の粉末混合物の焼成時間が１０分以上である。
（４）交流型プラズマディスプレイパネルの誘電体保護層の放電空間側の表面に形成される紫外光放出層の製造用である。
Preferred embodiments of the zinc-containing magnesium oxide fired powder of the present invention are as follows. ( 1 ) The zinc content is in the range of 0.5 to 7% by mass.
( 2 ) It is obtained by firing a powder mixture of a magnesium oxide source powder and a zinc oxide source powder at a temperature in the range of 850 ° C. or higher, particularly 900 to 1500 ° C.
( 3 ) The firing time of the powder mixture is 10 minutes or more.
( 4 ) For manufacturing an ultraviolet light emitting layer formed on the surface of the dielectric protective layer of the AC type plasma display panel on the discharge space side.
本発明はまた、亜鉛を０．１〜３０質量％の範囲にて含有する、交流型プラズマディスプレイパネルの誘電体保護層の放電空間側の表面に形成される紫外光放出層の製造用である亜鉛含有酸化マグネシウム焼成物粉末にもある。 The present invention is also for producing an ultraviolet light emitting layer formed on the surface of the dielectric protective layer of the AC type plasma display panel on the discharge space side, containing zinc in the range of 0.1 to 30% by mass. There are also zinc-containing magnesium oxide fired powders .
本発明はまた、上記本発明の亜鉛含有酸化マグネシウム焼成物粉末から製造された、交流型プラズマディスプレイパネルの誘電体保護層の放電空間側の表面に形成される紫外光放出層にもある。 The present invention also resides in an ultraviolet light emitting layer formed on the surface of the dielectric protective layer of the AC type plasma display panel on the discharge space side, produced from the zinc-containing sintered magnesium oxide powder of the present invention.
本発明の亜鉛含有酸化マグネシウム焼成物粉末は、Ｘｅガスのガス放電により生成した紫外光に励起されて波長２５０ｎｍ付近（波長２３０〜２６０ｎｍの範囲）にピーク波長を有する紫外光を高い効率で放出する。このため、本発明の亜鉛含有酸化マグネシウム焼成物粉末から製造された酸化マグネシウム膜を、ＡＣ型ＰＤＰや蛍光体ランプ等のガス放電発光装置の放電空間内に配置することにより、放電空間内に放出される紫外光の光量を増加させることができ、ガス放電発光装置から放出される可視光の量を増加させることが可能になる。本発明の亜鉛含有酸化マグネシウム焼成物粉末から製造された酸化マグネシウム膜は、ＡＣ型ＰＤＰのガス誘電体保護層の表面に形成される紫外光放出層として、特に有用である。 The zinc-containing magnesium oxide fired powder of the present invention is excited by ultraviolet light generated by gas discharge of Xe gas and emits ultraviolet light having a peak wavelength in the vicinity of a wavelength of 250 nm (wavelength range of 230 to 260 nm) with high efficiency. . For this reason, the magnesium oxide film manufactured from the zinc-containing sintered magnesium oxide powder of the present invention is disposed in the discharge space of a gas discharge light-emitting device such as an AC type PDP or a phosphor lamp, thereby releasing into the discharge space. The amount of ultraviolet light emitted can be increased, and the amount of visible light emitted from the gas discharge light emitting device can be increased. The magnesium oxide film produced from the zinc-containing magnesium oxide fired powder of the present invention is particularly useful as an ultraviolet light emitting layer formed on the surface of the gas dielectric protective layer of the AC type PDP.
本発明の亜鉛含有酸化マグネシウム焼成物粉末は、亜鉛を０．１〜３０質量％、好ましくは０．５〜７質量％、更に好ましくは１〜６質量％の範囲にて含有する。本発明の亜鉛含有酸化マグネシウム焼成物粉末は、ＢＥＴ比表面積が０．１〜３０ｍ2／ｇの範囲にあることが好ましく、０．２〜１２ｍ2／ｇの範囲にあることが特に好ましい。 The zinc-containing magnesium oxide fired powder of the present invention contains zinc in the range of 0.1 to 30% by mass, preferably 0.5 to 7% by mass, and more preferably 1 to 6% by mass. Zinc-containing magnesium oxide calcined powder of the present invention preferably has BET specific surface area in the range of 0.1~30m 2 / g, and particularly preferably in the range of 0.2~12m 2 / g.
本発明の亜鉛含有酸化マグネシウム焼成物粉末は、酸化マグネシウム源粉末と酸化亜鉛源粉末とを混合して、粉末混合物を得て、次いで該粉末混合物を焼成することにより得ることができる。粉末混合物の焼成温度は、好ましくは８５０℃以上、より好ましくは９００〜１５００℃、更に好ましくは１０００〜１５００℃の範囲である。焼成時間は、好ましくは１０分以上、より好ましくは１０分〜２時間、更に好ましくは２０分〜２時間の範囲である。粉末混合物の焼成は、例えば、常圧下、昇温速度１００〜５００℃／時間の条件で、上記の焼成温度にまで昇温し、次いで上記の焼成時間焼成した後、降温速度１００〜５００℃／時間の条件で、室温まで冷却することにより行なうことができる。焼成雰囲気は大気下であればよい。 The zinc-containing magnesium oxide fired powder of the present invention can be obtained by mixing a magnesium oxide source powder and a zinc oxide source powder to obtain a powder mixture, and then firing the powder mixture. The firing temperature of the powder mixture is preferably 850 ° C. or higher, more preferably 900-1500 ° C., and still more preferably 1000-1500 ° C. The firing time is preferably 10 minutes or more, more preferably 10 minutes to 2 hours, and still more preferably 20 minutes to 2 hours. For example, the powder mixture is baked under the conditions of normal pressure and a temperature increase rate of 100 to 500 ° C./hour. It can carry out by cooling to room temperature on condition of time. The firing atmosphere may be in the air.
酸化マグネシウム源粉末としては、酸化マグネシウム粉末、及び加熱により酸化マグネシウム粉末に転化するマグネシウム化合物粉末を用いることができる。加熱により酸化マグネシウム粉末に転化するマグネシウム化合物粉末の例としては、水酸化マグネシウム粉末、塩基性炭酸マグネシウム粉末、硝酸マグネシウム粉末及び酢酸マグネシウム粉末が挙げられる。酸化マグネシウム源粉末は、酸化マグネシウム粉末であることが好ましく、酸化マグネシウム粉末としては、気相合成酸化法により製造された酸化マグネシウム粉末であることが好ましい。気相合成酸化法とは、金属マグネシウム蒸気と酸素含有気体とを気相で接触させて、金属マグネシウムを酸化して酸化マグネシウム粉末を製造する方法である。 As the magnesium oxide source powder, magnesium oxide powder and magnesium compound powder that is converted to magnesium oxide powder by heating can be used. Examples of the magnesium compound powder that is converted to magnesium oxide powder by heating include magnesium hydroxide powder, basic magnesium carbonate powder, magnesium nitrate powder, and magnesium acetate powder. The magnesium oxide source powder is preferably a magnesium oxide powder, and the magnesium oxide powder is preferably a magnesium oxide powder produced by a gas phase synthetic oxidation method. The gas phase synthetic oxidation method is a method of producing magnesium oxide powder by contacting metal magnesium vapor and an oxygen-containing gas in a gas phase to oxidize the metal magnesium.
酸化マグネシウム源粉末の純度は、９９．９５質量％以上であることが好ましい。酸化マグネシウム源粉末は、ＢＥＴ比表面積が５〜１５０ｍ2／ｇ、特に７〜５０ｍ2／ｇの範囲にあることが好ましい。なお、酸化マグネシウム源粉末の粒子径は、本発明の効果を損なわない限り特に制限されない。 The purity of the magnesium oxide source powder is preferably 99.95% by mass or more. The magnesium oxide source powder preferably has a BET specific surface area of 5 to 150 m 2 / g, particularly 7 to 50 m 2 / g. The particle diameter of the magnesium oxide source powder is not particularly limited as long as the effects of the present invention are not impaired.
酸化亜鉛源粉末としては、酸化亜鉛粉末、及び加熱により酸化亜鉛粉末に転化する亜鉛化合物粉末を用いることができる。加熱により酸化亜鉛粉末に転化する亜鉛化合物粉末の例としては、水酸化亜鉛粉末、炭酸亜鉛粉末、硝酸亜鉛粉末、酢酸亜鉛粉末及びシュウ酸亜鉛粉末が挙げられる。酸化亜鉛源粉末は、酸化亜鉛粉末であることが好ましい。酸化亜鉛源粉末の純度は９９．０質量％以上であることが好ましく、粒子径は、本発明の効果を損なわない限り特に制限されない。 As the zinc oxide source powder, zinc oxide powder and zinc compound powder that is converted into zinc oxide powder by heating can be used. Examples of zinc compound powders that are converted to zinc oxide powder by heating include zinc hydroxide powder, zinc carbonate powder, zinc nitrate powder, zinc acetate powder, and zinc oxalate powder. The zinc oxide source powder is preferably zinc oxide powder. The purity of the zinc oxide source powder is preferably 99.0% by mass or more, and the particle diameter is not particularly limited as long as the effect of the present invention is not impaired.
本発明の亜鉛含有酸化マグネシウム焼成物粉末は、Ｘｅガスのガス放電により生成した紫外光に励起されて波長２５０ｎｍ付近の紫外光（２３０〜２６０ｎｍの範囲にピーク波長を有する紫外光）を高い効率で放出する。また、ＡＣ型ＰＤＰや蛍光体ランプ等のガス放電発光装置に使用される蛍光体材料は、前記特許文献１に記載されているように波長２５０ｎｍ付近の紫外光に励起されて可視光を放出することが知られている。このため、本発明の亜鉛含有酸化マグネシウム焼成物粉末から製造された酸化マグネシウム膜を、ＡＣ型ＰＤＰや蛍光体ランプ等のＸｅガスを放電ガスに用いたガス放電発光装置の放電空間内、特に誘電体保護層の放電空間側の表面に配置すると、Ｘｅガスのガス放電により放電空間内に放出される紫外光の光量を増加させることができ、その結果、ガス放電発光装置から放出される可視光の量を増加させることが可能になる。従って、本発明の亜鉛含有酸化マグネシウム焼成物粉末は、ＡＣ型ＰＤＰの誘電体保護層の放電空間側の表面に形成される紫外光放出層の製造用として特に有用である。 The zinc-containing magnesium oxide fired powder of the present invention is excited by ultraviolet light generated by gas discharge of Xe gas, and emits ultraviolet light having a wavelength near 250 nm (ultraviolet light having a peak wavelength in the range of 230 to 260 nm) with high efficiency. discharge. Further, as described in Patent Document 1, phosphor materials used in gas discharge light emitting devices such as AC type PDPs and phosphor lamps emit visible light when excited by ultraviolet light having a wavelength of around 250 nm. It is known. For this reason, the magnesium oxide film manufactured from the zinc-containing magnesium oxide fired powder of the present invention is used in the discharge space of a gas discharge light-emitting device using Xe gas such as an AC type PDP or a phosphor lamp as a discharge gas, particularly a dielectric. When arranged on the surface of the body protection layer on the discharge space side, the amount of ultraviolet light emitted into the discharge space by the gas discharge of Xe gas can be increased, and as a result, visible light emitted from the gas discharge light-emitting device The amount of can be increased. Therefore, the zinc-containing magnesium oxide fired powder of the present invention is particularly useful for producing an ultraviolet light emitting layer formed on the surface of the dielectric protective layer of the AC type PDP on the discharge space side.
なお、本発明の亜鉛含有酸化マグネシウム焼成物粉末は、スプレー法や静電塗布法などの公知の方法を用いることにより酸化マグネシウム膜とすることができ、その粒子径は本発明の効果を損なわない範囲であれば特に制限されない。 The zinc-containing magnesium oxide fired powder of the present invention can be formed into a magnesium oxide film by using a known method such as a spray method or an electrostatic coating method, and the particle size does not impair the effects of the present invention. If it is a range, it will not restrict | limit in particular.
［実験例１］
（焼成物Ｎｏ．１〜Ｎｏ．１０の製造）
気相合成酸化法により製造された酸化マグネシウム粉末（２０００Ａ、宇部マテリアルズ（株）製、純度：９９．９８質量％、ＢＥＴ比表面積：８．７ｍ2／ｇ）と酸化亜鉛粉末（純度：９９．９９質量％）とを下記表１に示す量にて混合して、粉末混合物を得た。得られた粉末混合物を容量２５ｍＬのアルミナ坩堝に投入し、アルミナ坩堝に蓋をして電気炉に入れ、２４０℃／時間の昇温速度で炉内温度を１２００℃まで上昇させ、次いで該温度で３０分間加熱焼成した。その後、炉内温度を２４０℃／時間の降温速度で室温まで冷却した。そして、電気炉からアルミナ坩堝を取り出して、粉末混合物の焼成物Ｎｏ．１〜Ｎｏ．１０を得た。
[Experimental Example 1]
(Production of fired products No. 1 to No. 10)
Magnesium oxide powder (2000A, manufactured by Ube Materials Co., Ltd., purity: 99.98% by mass, BET specific surface area: 8.7 m 2 / g) and zinc oxide powder (purity: 99) produced by the gas phase synthetic oxidation method .99 mass%) was mixed in the amounts shown in Table 1 below to obtain a powder mixture. The obtained powder mixture is put into an alumina crucible having a capacity of 25 mL, the alumina crucible is covered and placed in an electric furnace, and the furnace temperature is increased to 1200 ° C. at a temperature rising rate of 240 ° C./hour. Bake for 30 minutes. Thereafter, the furnace temperature was cooled to room temperature at a temperature lowering rate of 240 ° C./hour. Then, the alumina crucible was taken out from the electric furnace, and the powder mixture fired product No. 1-No. 10 was obtained.
表１
────────────────────────────────────────
酸化マグネシウム粉末量（ｇ） 酸化亜鉛粉末量（ｇ）
────────────────────────────────────────
焼成物Ｎｏ．１ ５．０ ０
焼成物Ｎｏ．２ ５．０ ０．０１
焼成物Ｎｏ．３ ５．０ ０．０５
焼成物Ｎｏ．４ ５．０ ０．１０
焼成物Ｎｏ．５ ５．０ ０．２０
焼成物Ｎｏ．６ ５．０ ０．５０
焼成物Ｎｏ．７ ５．０ １．００
焼成物Ｎｏ．８ ４．０ ２．００
焼成物Ｎｏ．９ ３．０ ３．００
焼成物Ｎｏ．１０ ２．０ ４．００
────────────────────────────────────────
Table 1
────────────────────────────────────────
Magnesium oxide powder amount (g) Zinc oxide powder amount (g)
────────────────────────────────────────
Baked product No. 1 5.0 0
Baked product No. 2 5.0 0.01
Baked product No. 3 5.0 0.05
Baked product No. 4 5.0 0.10
Baked product No. 5 5.0 0.20
Baked product No. 6 5.0 0.50
Baked product No. 7 5.0 1.00
Baked product No. 8 4.0 2.00
Baked product No. 9 3.0 3.00
Baked product No. 10 2.0 4.00
────────────────────────────────────────
得られた焼成物Ｎｏ．１〜Ｎｏ．１０について、ＢＥＴ比表面積、亜鉛含有量、及び紫外光発光強度を測定した。その結果を表２に示す。なお、亜鉛含有量及び紫外光発光強度は以下の方法により測定した。 The obtained fired product No. 1-No. For No. 10, the BET specific surface area, zinc content, and ultraviolet light emission intensity were measured. The results are shown in Table 2. The zinc content and ultraviolet light emission intensity were measured by the following methods.
［亜鉛含有量］
焼成物を塩酸に溶解させて調製した溶液中の亜鉛量をＩＣＰ発光分析により測定する。
[Zinc content]
The amount of zinc in a solution prepared by dissolving the fired product in hydrochloric acid is measured by ICP emission analysis.
［紫外光発光強度］
焼成物にＸｅガスのガス放電により生成した紫外光を照射して、焼成物から放出された紫外光スペクトルを測定し、波長２５０ｎｍ付近（波長２３０〜２６０ｎｍの範囲）の最大ピーク値を紫外光発光強度として求める。なお、表２の値は、焼成物Ｎｏ．９の紫外光発光強度を１００とした相対値である。
[Ultraviolet light emission intensity]
The fired product is irradiated with ultraviolet light generated by gas discharge of Xe gas, the ultraviolet light spectrum emitted from the fired product is measured, and the maximum peak value in the vicinity of a wavelength of 250 nm (wavelength range of 230 to 260 nm) is emitted as ultraviolet light. Calculate as strength. The values in Table 2 indicate the fired product No. This is a relative value with the ultraviolet light emission intensity of 9 as 100.
表２
────────────────────────────────────────
ＢＥＴ比表面積 亜鉛含有量 紫外光発光強度
（ｍ2／ｇ） （質量％） （−）
────────────────────────────────────────
焼成物Ｎｏ．１ ５．０３ 検出されず 発光せず
焼成物Ｎｏ．２ ４．８８ ０．１４ １３６
焼成物Ｎｏ．３ ４．８３ ０．６４ ６６４
焼成物Ｎｏ．４ ４．７６ １．４ １０３１
焼成物Ｎｏ．５ ４．６７ ３．３ １７９０
焼成物Ｎｏ．６ ４．３８ ６．３ ９６６
焼成物Ｎｏ．７ ４．１３ １０．０ １９２
焼成物Ｎｏ．８ ３．２４ ２６．８ １４０
焼成物Ｎｏ．９ ２．０３ ４０．２ １００
焼成物Ｎｏ．１０ １．１４ ５３．６ １６
────────────────────────────────────────
Table 2
────────────────────────────────────────
BET specific surface area Zinc content Ultraviolet light emission intensity
(M 2 / g) (mass%) (−)
────────────────────────────────────────
Baked product No. 1 5.03 Not detected No light emitted. 2 4.88 0.14 136
Baked product No. 3 4.83 0.64 664
Baked product No. 4 4.76 1.4 1031
Baked product No. 5 4.67 3.3 1790
Baked product No. 6 4.38 6.3 966
Baked product No. 7 4.13 10.0 192
Baked product No. 8 3.24 26.8 140
Baked product No. 9 2.03 40.2 100
Baked product No. 10 1.14 53.6 16
────────────────────────────────────────
表２に示した結果から明らかなように、亜鉛含有量が０．１質量％以上の亜鉛含有酸化マグネシウム焼成物粉末（焼成物Ｎｏ．２〜Ｎｏ．８）は、Ｘｅガスの放電ガスにより生成した紫外光に励起されると波長２５０ｎｍ付近の紫外光を高い効率で放出することがわかる。 As is clear from the results shown in Table 2, zinc-containing magnesium oxide fired powders (baked products No. 2 to No. 8) having a zinc content of 0.1% by mass or more are generated by a discharge gas of Xe gas. It can be seen that when excited by ultraviolet light, ultraviolet light having a wavelength of about 250 nm is emitted with high efficiency.
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