JP2006244784A - Magnesium oxide particulate dispersion for forming dielectric layer protecting film of ac type plasma display panel - Google Patents
Magnesium oxide particulate dispersion for forming dielectric layer protecting film of ac type plasma display panel Download PDFInfo
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- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 title claims abstract description 112
- 239000000395 magnesium oxide Substances 0.000 title claims abstract description 111
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 239000006185 dispersion Substances 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 claims abstract description 25
- 238000002296 dynamic light scattering Methods 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000000576 coating method Methods 0.000 claims abstract description 9
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 6
- 239000011248 coating agent Substances 0.000 claims abstract description 4
- 239000010419 fine particle Substances 0.000 claims description 76
- 239000002245 particle Substances 0.000 claims description 22
- 230000001681 protective effect Effects 0.000 claims description 14
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 239000010408 film Substances 0.000 abstract description 39
- 239000010409 thin film Substances 0.000 abstract description 4
- 229910052799 carbon Inorganic materials 0.000 abstract 1
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 14
- 238000002834 transmittance Methods 0.000 description 14
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 13
- 239000011164 primary particle Substances 0.000 description 13
- 239000011521 glass Substances 0.000 description 11
- 239000000758 substrate Substances 0.000 description 11
- 239000011324 bead Substances 0.000 description 10
- 238000009826 distribution Methods 0.000 description 9
- 238000005259 measurement Methods 0.000 description 9
- 239000000203 mixture Substances 0.000 description 8
- 239000002612 dispersion medium Substances 0.000 description 6
- 239000011230 binding agent Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 238000004528 spin coating Methods 0.000 description 4
- 239000002562 thickening agent Substances 0.000 description 4
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- AKTIAGQCYPCKFX-FDGPNNRMSA-L magnesium;(z)-4-oxopent-2-en-2-olate Chemical compound [Mg+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O AKTIAGQCYPCKFX-FDGPNNRMSA-L 0.000 description 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical class OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 description 2
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 2
- -1 magnesium alkoxide Chemical class 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 description 2
- LNAZSHAWQACDHT-XIYTZBAFSA-N (2r,3r,4s,5r,6s)-4,5-dimethoxy-2-(methoxymethyl)-3-[(2s,3r,4s,5r,6r)-3,4,5-trimethoxy-6-(methoxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6r)-4,5,6-trimethoxy-2-(methoxymethyl)oxan-3-yl]oxyoxane Chemical compound CO[C@@H]1[C@@H](OC)[C@H](OC)[C@@H](COC)O[C@H]1O[C@H]1[C@H](OC)[C@@H](OC)[C@H](O[C@H]2[C@@H]([C@@H](OC)[C@H](OC)O[C@@H]2COC)OC)O[C@@H]1COC LNAZSHAWQACDHT-XIYTZBAFSA-N 0.000 description 1
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- 235000010944 ethyl methyl cellulose Nutrition 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000005243 fluidization Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000007646 gravure printing Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229940035429 isobutyl alcohol Drugs 0.000 description 1
- 150000002681 magnesium compounds Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 235000010981 methylcellulose Nutrition 0.000 description 1
- 229920003087 methylethyl cellulose Polymers 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N n-propyl alcohol Natural products CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
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Abstract
Description
本発明は、交流型プラズマディスプレイパネルの誘電体層保護膜形成用の酸化マグネシウム微粒子分散液に関する。本発明はまた、上記酸化マグネシウム微粒子分散液から形成された酸化マグネシウム膜が積層された交流型プラズマディスプレイパネル、及び交流型プラズマディスプレイパネルの誘電体層保護膜の製造方法にも関する。 The present invention relates to a magnesium oxide fine particle dispersion for forming a dielectric layer protective film of an AC type plasma display panel. The present invention also relates to an AC plasma display panel in which magnesium oxide films formed from the magnesium oxide fine particle dispersion are laminated, and a method for manufacturing a dielectric layer protective film of the AC plasma display panel.
交流型プラズマディスプレイパネル（以下、ＡＣ型ＰＤＰという）誘電体層の保護膜として、酸化マグネシウム薄膜が用いられている。ＰＤＰの誘電体層保護用の酸化マグネシウム薄膜の製造方法としては、電子ビーム蒸着法やスパッタ法などの物理的な方法が主流である。しかしながら、これらの製造方法では大規模な製造装置を用いて厳しい製造条件の管理が必要となる、また歩留まりが低いなどの問題がある。このため、酸化マグネシウム微粒子の分散液を誘電体層の上に塗布、乾燥（さらに必要に応じて、焼成）することによって酸化マグネシウム薄膜を形成する方法（塗布法）の研究が進められている。 A magnesium oxide thin film is used as a protective film for an AC plasma display panel (hereinafter referred to as AC type PDP) dielectric layer. As a manufacturing method of a magnesium oxide thin film for protecting a dielectric layer of a PDP, a physical method such as an electron beam evaporation method or a sputtering method is mainly used. However, these manufacturing methods have problems such as requiring management of strict manufacturing conditions using a large-scale manufacturing apparatus and low yield. For this reason, research on a method (coating method) for forming a magnesium oxide thin film by applying a dispersion of magnesium oxide fine particles on a dielectric layer and drying (further firing if necessary) is underway.
特許文献１には、ＰＤＰの誘電体層保護膜形成用の酸化マグネシウム微粒子分散液として、酸化マグネシウム粉末分散液と、マグネシウムアルコキシド又はマグネシウムアセチルアセトネートを含むバインダ溶液とを混合して調製した分散液が開示されている。この特許文献１において、酸化マグネシウム粉末分散液は、平均粒子径が５ｎｍ〜５μｍ、好ましくは１０〜２００ｎｍの酸化マグネシウム微粒子と、アルコールを主成分とする溶媒又はアルコールとエチレングリコール誘導体との混合溶媒とエチレングリコール誘導体を主成分とする分散剤とを混合して調製されている。 Patent Document 1 discloses a dispersion prepared by mixing a magnesium oxide powder dispersion and a binder solution containing magnesium alkoxide or magnesium acetylacetonate as a magnesium oxide fine particle dispersion for forming a PDP dielectric layer protective film. Is disclosed. In this Patent Document 1, the magnesium oxide powder dispersion is composed of magnesium oxide fine particles having an average particle diameter of 5 nm to 5 μm, preferably 10 to 200 nm, a solvent containing alcohol as a main component, or a mixed solvent of alcohol and ethylene glycol derivative. It is prepared by mixing with a dispersant mainly composed of an ethylene glycol derivative.
特許文献２には、マグネシウムアセチルアセトナート、エタノールアミン、脂肪酸、有機溶剤からなる混合液に、酸化マグネシウム微粒子を分散させて調製した酸化マグネシウム微粒子分散液が開示されている。この特許文献２では、酸化マグネシウム微粒子は平均粒子径が１０ｎｍ以下の微粒子が好ましいとされている。
均一な厚さで、かつ透明性の高い酸化マグネシウム保護膜を塗布法により形成させるためには、分散液中の酸化マグネシウム微粒子の凝集が少ないこと、即ち酸化マグネシウム微粒子が一次粒子もしくはそれに近い形で分散されていることが望ましい。しかしながら、上記の特許文献には、酸化マグネシウム微粒子を用いて分散液を調製する旨の開示がされているものの、その酸化マグネシウム微粒子を一次粒子もしくはそれに近い形で分散させる方法についての具体的な開示がない。従って、微細な各粒子の相当部分が凝集体として分散されていると理解される。
本発明の目的は、均一な厚さで、かつ透明性の高い酸化マグネシウム保護膜を塗布法により形成させるのに有用な、酸化マグネシウム微粒子が一次粒子もしくはそれに近い形で分散されている酸化マグネシウム微粒子の分散液を提供することにある。
In order to form a magnesium oxide protective film having a uniform thickness and high transparency by a coating method, there is little aggregation of the magnesium oxide fine particles in the dispersion, that is, the magnesium oxide fine particles are in the form of primary particles or close to them. It is desirable to be distributed. However, although the above-mentioned patent document discloses that a dispersion liquid is prepared using magnesium oxide fine particles, a specific disclosure about a method of dispersing the magnesium oxide fine particles in primary particles or a form close thereto. There is no. Therefore, it is understood that a substantial part of each fine particle is dispersed as an aggregate.
An object of the present invention is to form magnesium oxide fine particles in which magnesium oxide fine particles are dispersed in primary particles or in a form close to them, which is useful for forming a magnesium oxide protective film having a uniform thickness and high transparency by a coating method. It is to provide a dispersion liquid.
本発明者は、酸化マグネシウム微粒子を分散させるための分散媒体の種類、そして分散媒体中に酸化マグネシウム微粒子を分散させるための分散化方法を選ぶことによって、平均一次粒子径が５〜１００ｎｍの範囲にある酸化マグネシウム微粒子を、一次粒子もしくはそれに近い小径の凝集粒子として分散させることができることを見い出した。そして、その微細な酸化マグネシウム微粒子が一次粒子もしくはそれに近い小径の凝集粒子として分散されている分散液を用いることにより、均一な厚さで、かつ透明性の高い酸化マグネシウム保護膜を塗布法により形成することができることを確認して、本発明に到達した。 The inventor chooses the type of dispersion medium for dispersing the magnesium oxide fine particles, and the dispersion method for dispersing the magnesium oxide fine particles in the dispersion medium, so that the average primary particle diameter is in the range of 5 to 100 nm. It has been found that certain magnesium oxide fine particles can be dispersed as primary particles or small-diameter aggregate particles close to the primary particles. Then, by using a dispersion in which the fine magnesium oxide fine particles are dispersed as primary particles or small-sized aggregate particles close to the primary particles, a magnesium oxide protective film having a uniform thickness and high transparency is formed by a coating method. After confirming that this can be done, the present invention has been reached.
本発明は、炭素原子数３〜５の一価アルコール中に、酸化マグネシウム微粒子が０．０５〜２０質量％の範囲にて分散されてなり、動的光散乱法によって測定された酸化マグネシウム微粒子のＤ50が５〜１００ｎｍの範囲にある交流型プラズマディスプレイパネルの誘電体層保護膜形成用の酸化マグネシウム微粒子分散液にある。 The present invention relates to magnesium oxide fine particles measured by a dynamic light scattering method in which magnesium oxide fine particles are dispersed in a monohydric alcohol having 3 to 5 carbon atoms in a range of 0.05 to 20% by mass. D 50 is in the magnesium oxide fine particle dispersion for forming the dielectric layer protective film of the AC type plasma display panel in the range of 5 to 100 nm.
本発明の酸化マグネシウム微粒子分散液の好ましい態様は、以下の通りである。
（１）動的光散乱法によって測定された酸化マグネシウム微粒子のＤ50が５〜２０ｎｍの範囲にあり、Ｄ10／Ｄ90が０．４以上である。
（２）動的光散乱法によって測定された酸化マグネシウム微粒子のＤ50が４５〜９０ｎｍの範囲にあり、Ｄ10／Ｄ90が０．１以上である。
（３）一価アルコールが、イソプロピルアルコール又はブチルアルコール、もしくはこれら混合物である。
Preferred embodiments of the magnesium oxide fine particle dispersion of the present invention are as follows.
(1) The D 50 of the magnesium oxide fine particles measured by the dynamic light scattering method is in the range of 5 to 20 nm, and D 10 / D 90 is 0.4 or more.
(2) The D 50 of the magnesium oxide fine particles measured by the dynamic light scattering method is in the range of 45 to 90 nm, and D 10 / D 90 is 0.1 or more.
(3) The monohydric alcohol is isopropyl alcohol or butyl alcohol, or a mixture thereof.
本発明はまた、上記本発明の酸化マグネシウム微粒子分散液から形成された酸化マグネシウム膜が誘電体層の上に積層されている交流型プラズマディスプレイパネルにもある。 The present invention is also an AC plasma display panel in which a magnesium oxide film formed from the magnesium oxide fine particle dispersion of the present invention is laminated on a dielectric layer.
本発明はさらに、上記本発明の酸化マグネシウム微粒子分散液を、プラズマディスプレイパネルの誘電体層の上に塗布して、乾燥することからなる交流型プラズマディスプレイパネルの誘電体層保護膜の製造方法にもある。 The present invention further provides a method for producing a protective film for a dielectric layer of an alternating current plasma display panel, which comprises applying the magnesium oxide fine particle dispersion of the present invention onto a dielectric layer of a plasma display panel and drying the coating. There is also.
本発明の酸化マグネシウム微粒子分散液を用いることにより、ＡＣ型ＰＤＰの誘電体層の上に膜厚が均一で、かつ透明性が高い酸化マグネシウム保護膜を容易に形成することができる。 By using the magnesium oxide fine particle dispersion of the present invention, a magnesium oxide protective film having a uniform film thickness and high transparency can be easily formed on the dielectric layer of the AC type PDP.
本発明の酸化マグネシウム微粒子分散液は、炭素原子数３〜５の一価アルコール中に酸化マグネシウム微粒子を、分散液の全組成物の質量を基準として０．０５〜２０質量％の範囲、好ましくは１〜１５質量％の範囲にて含む。 The magnesium oxide fine particle dispersion of the present invention comprises magnesium oxide fine particles in a monohydric alcohol having 3 to 5 carbon atoms, preferably in the range of 0.05 to 20% by mass, preferably based on the mass of the total composition of the dispersion. In the range of 1 to 15% by mass.
本発明の分散液に含まれる酸化マグネシウム微粒子は、動的光散乱法によって測定されたＤ50（累積通過分布の５０％に相当する粒子径）が５〜１００ｎｍの範囲にある。酸化マグネシウム微粒子は、Ｄ10（累積通過分布の１０％に相当する粒子径）とＤ90（累積通過分布の９０％に相当する粒子径）との比（Ｄ10／Ｄ90）が０．１以上であることが好ましく、０．１５以上であることがより好ましく、０．４以上であることが特に好ましい。Ｄ10／Ｄ90は、粒子径の分布の拡がりを評価する指標の一つであり、１に近い方が分布の拡がりが狭いこと、すなわち粒子径の均一性が高いことを表す。 The magnesium oxide fine particles contained in the dispersion of the present invention have a D 50 (particle diameter corresponding to 50% of the cumulative passage distribution) measured by a dynamic light scattering method in the range of 5 to 100 nm. MgO particles, the ratio of D 10 and D 90 (particle diameter corresponding to 10% of the accumulated passage distribution) (particle diameter corresponding to 90% of the accumulated passage distribution) (D 10 / D 90) is 0.1 Preferably, it is preferably 0.15 or more, and more preferably 0.4 or more. D 10 / D 90 is one index for evaluating the spread of the particle size distribution, and the closer to 1, the narrower the spread of the distribution, that is, the higher the uniformity of the particle size.
本発明の分散液に含まれる酸化マグネシウム微粒子は、動的光散乱法によって測定された酸化マグネシウム微粒子のＤ50が５〜２０ｎｍの範囲にあり、Ｄ10／Ｄ90が０．１以上（特に、０．４以上）であるか、動的光散乱法によって測定された酸化マグネシウム微粒子のＤ50が４５〜９０ｎｍの範囲にあり、Ｄ10／Ｄ90が０．１以上（特に、０．１５以上）であることが好ましい。 The magnesium oxide fine particles contained in the dispersion of the present invention have a D 50 of magnesium oxide fine particles measured by a dynamic light scattering method in the range of 5 to 20 nm and a D 10 / D 90 of 0.1 or more (in particular, 0.4 or higher) or D 50 of the magnesium oxide fine particles measured by the dynamic light scattering method is in the range of 45 to 90 nm, and D 10 / D 90 is 0.1 or higher (particularly 0.15 or higher). ) Is preferable.
酸化マグネシウム微粒子のＤ50が５〜２０ｎｍの範囲にある分散液は、透光性が高いという特徴がある。特に、分散媒体にブチルアルコールを用いると透光性が高くなる傾向にある。Ｄ50が５〜２０ｎｍの範囲にある酸化マグネシウム微粒子をブチルアルコールに分散させた分散液の波長７００ｎｍの光の透過率（測定：セル厚１０ｍｍ）は、酸化マグネシウム微粒子濃度が５質量％の分散液で６０％以上、酸化マグネシウム微粒子濃度が１質量％の分散液で９０％以上の値を示す。 A dispersion having a D 50 of magnesium oxide fine particles in the range of 5 to 20 nm is characterized by high translucency. In particular, when butyl alcohol is used as the dispersion medium, the translucency tends to increase. The light transmittance at a wavelength of 700 nm (measurement: cell thickness 10 mm) of a dispersion in which magnesium oxide fine particles having a D 50 in the range of 5 to 20 nm are dispersed in butyl alcohol is a dispersion having a magnesium oxide fine particle concentration of 5% by mass. And a dispersion having a magnesium oxide fine particle concentration of 1% by mass shows a value of 90% or more.
本発明の分散液において分散媒体として用いられる炭素原子数が３〜５の一価アルコールは、分岐を有していてもよい。一価アルコールとしては、プロピルアルコール、イソプロピルアルコール、ブチルアルコール、イソブチルアルコール、ｓｅｃ−ブチルアルコール、ｔｅｒｔ−ブチルアルコール、ペンチルアルコール、イソペンチルアルコールなどを用いることができる。これらは二種以上を併用してもよい。一価アルコールとして好ましいのは、イソプロピルアルコール及びブチルアルコール、そしてこれらの混合物である。 The monohydric alcohol having 3 to 5 carbon atoms used as a dispersion medium in the dispersion of the present invention may have a branch. As the monohydric alcohol, propyl alcohol, isopropyl alcohol, butyl alcohol, isobutyl alcohol, sec-butyl alcohol, tert-butyl alcohol, pentyl alcohol, isopentyl alcohol, and the like can be used. Two or more of these may be used in combination. Preferred as the monohydric alcohol are isopropyl alcohol and butyl alcohol, and mixtures thereof.
本発明の酸化マグネシウム微粒子分散液は、例えば、平均一次粒子径が５〜１００ｎｍの範囲にある酸化マグネシウム微粒子を、炭素原子数３〜５の一価アルコールに投入して得た混合物を、ビーズを用いた粉砕装置にて分散処理を行なうことからなる方法により製造することができる。 In the magnesium oxide fine particle dispersion of the present invention, for example, a mixture obtained by introducing magnesium oxide fine particles having an average primary particle diameter in the range of 5 to 100 nm into a monohydric alcohol having 3 to 5 carbon atoms is used as beads. It can be produced by a method comprising carrying out a dispersion treatment with the used pulverizer.
酸化マグネシウム微粒子としては、金属マグネシウム蒸気と酸素とを反応させる方法（気相酸化合成法）により製造した酸化マグネシウム微粒子を好適に用いることができる。気相酸化合成法により製造した酸化マグネシウム微粒子としては、宇部マテリアルズ（株）から販売されている１００Ａ（平均一次粒子径：１０ｎｍ）や５００Ａ（平均一次粒子径：５０ｎｍ）が知られている。酸化マグネシウム微粒子の平均一次粒子径は、電界放射型走査電子顕微鏡（ＦＥ−ＳＥＭ）を用いて測定することができる。 As the magnesium oxide fine particles, magnesium oxide fine particles produced by a method of reacting metal magnesium vapor and oxygen (gas phase oxidation synthesis method) can be suitably used. As magnesium oxide fine particles produced by the vapor phase oxidation synthesis method, 100A (average primary particle size: 10 nm) and 500A (average primary particle size: 50 nm) sold by Ube Materials Co., Ltd. are known. The average primary particle diameter of the magnesium oxide fine particles can be measured using a field emission scanning electron microscope (FE-SEM).
酸化マグネシウム微粒子の分散処理に用いるビーズ（ボールともいう）は、平均粒子径が２０〜３００μｍの範囲、好ましくは２０〜１５０μｍの範囲、特に好ましくは２０〜１００μｍの範囲にある。ビーズの材料としては、酸化ジルコニウムなどの公知のセラミックス材料が挙げられる。 The beads (also called balls) used for the dispersion treatment of the magnesium oxide fine particles have an average particle diameter in the range of 20 to 300 μm, preferably in the range of 20 to 150 μm, particularly preferably in the range of 20 to 100 μm. Examples of the material for the beads include known ceramic materials such as zirconium oxide.
粉砕装置としては、転動ミル（回転ミル）、振動ミル、揺動ミル（ロッキングミル）、遊星ミル、ＣＦミル（遠心流動化ミル）、アニュラーミル（転動攪拌ミル）などのミル容器を駆動することによってビーズにエネルギーを伝達するビーズミル、ミル容器内に充填したビーズをミル容器中に挿入されている攪拌機にて攪拌することによってビーズにエネルギーを伝達する攪拌ミルが挙げられる。これらの中で好ましいのは、揺動ミル及び攪拌ミルである。 As the grinding device, it drives mill containers such as rolling mill (rotating mill), vibration mill, rocking mill (rocking mill), planetary mill, CF mill (centrifugal fluidization mill), annular mill (rolling stirring mill), etc. Examples thereof include a bead mill that transmits energy to the beads and a stirring mill that transmits energy to the beads by stirring the beads filled in the mill container with a stirrer inserted in the mill container. Among these, a rocking mill and a stirring mill are preferable.
本発明の酸化マグネシウム微粒子分散液は、塗布後の酸化マグネシウム粒子同士の密着性あるいは酸化マグネシウム粒子と誘電体層との密着性を高めるために、バインダを添加してもよい。バインダの例としては、マグネシウムアルコキシド、マグネシウムアセチルアセトネートなどの加熱により酸化マグネシウムを生成するマグネシウム化合物を挙げることができる。バインダの添加量は、分散液の全組成物の質量を基準として０．０５〜１０質量％の範囲、好ましくは１〜５質量％の範囲である。 In the magnesium oxide fine particle dispersion of the present invention, a binder may be added in order to improve the adhesion between the magnesium oxide particles after coating or the adhesion between the magnesium oxide particles and the dielectric layer. Examples of the binder include magnesium compounds that generate magnesium oxide by heating, such as magnesium alkoxide and magnesium acetylacetonate. The addition amount of the binder is in the range of 0.05 to 10% by mass, preferably in the range of 1 to 5% by mass, based on the mass of the total composition of the dispersion.
本発明の酸化マグネシウム微粒子分散液はさらに、増粘剤を添加してもよい。増粘剤の例としては、ポリエチレングリコール、ポリプロピレングリコール、メチルセルロース、エチルセルロースを挙げることができる。増粘剤の添加量は、分散液の全組成物の質量を基準として０．０５〜１０質量％の範囲、好ましくは１〜５質量％の範囲である。 A thickener may be further added to the magnesium oxide fine particle dispersion of the present invention. Examples of thickeners include polyethylene glycol, polypropylene glycol, methyl cellulose, and ethyl cellulose. The addition amount of the thickener is in the range of 0.05 to 10% by mass, preferably in the range of 1 to 5% by mass, based on the mass of the total composition of the dispersion.
上記バインダ及び増粘剤の添加は、酸化マグネシウム微粒子の分散処理を行なった後に行なうことが好ましい。 The binder and the thickener are preferably added after the dispersion treatment of the magnesium oxide fine particles.
本発明の酸化マグネシウム微粒子分散液を、ＡＣ型ＰＤＰの誘電体層の上に塗布して、乾燥することによりＡＣ型ＰＤＰの酸化マグネシウム保護膜を形成することができる。塗布法としては、スピンコート法、スプレーコート法、スクリーン印刷法、グラビア印刷法、ディップ法、ドクタブレード法等の公知の方法を挙げることができる。乾燥温度は、一般に５０〜２００℃の範囲である。乾燥後の酸化マグネシウム膜は、３００〜７００℃の温度で焼成することが好ましい。乾燥及び焼成は大気中で行なうことが好ましい。 The magnesium oxide fine particle dispersion of the present invention is applied on the dielectric layer of the AC type PDP and dried to form a magnesium oxide protective film of the AC type PDP. Examples of the coating method include known methods such as a spin coating method, a spray coating method, a screen printing method, a gravure printing method, a dip method, and a doctor blade method. The drying temperature is generally in the range of 50 to 200 ° C. The dried magnesium oxide film is preferably fired at a temperature of 300 to 700 ° C. Drying and firing are preferably performed in the air.
本発明の酸化マグネシウム微粒子分散液を用いて形成するＡＣ型ＰＤＰの酸化マグネシウム保護膜の膜厚は、５００ｎｍ〜２μｍの範囲にあることが好ましい。 The film thickness of the magnesium oxide protective film of the AC type PDP formed using the magnesium oxide fine particle dispersion of the present invention is preferably in the range of 500 nm to 2 μm.
［実施例１］
平均一次粒子径が１０ｎｍの酸化マグネシウム微粒子（１００Ａ、宇部マテリアルズ（株）製）５質量部を、ブチルアルコール９５質量部に投入して混合物を得た。次いで、その混合物を、攪拌ミル（攪拌機付きミル容器の容量：１７０ｍＬ、ウルトラアペックスミルＵＡＭ０１５、寿工業（株）製）を用いて、ビーズ：平均粒子径３０μｍの酸化ジルコニウム製ビーズ、ミル容器内のビーズ充填率：６０体積％、攪拌機の周速：８．０ｍ／秒、処理時間：１３５分の条件にて分散処理を行なって、酸化マグネシウム微粒子分散液を調製した。得られた酸化マグネシウム微粒子分散液の波長７００ｎｍの光の透過率を、セル厚１０ｍｍの条件で測定したことろ、６３％であった。
得られた酸化マグネシウム微粒子分散液中の酸化マグネシウム微粒子の粒度分布を動的光散乱法によって下記の条件にて測定した。その結果、Ｄ10は６．６ｎｍ、Ｄ50は８．５ｎｍ、Ｄ90は１３．４ｎｍ、であり、Ｄ10／Ｄ90は０．４９であった。
[Example 1]
5 parts by mass of magnesium oxide fine particles (100A, manufactured by Ube Materials Co., Ltd.) having an average primary particle diameter of 10 nm were added to 95 parts by mass of butyl alcohol to obtain a mixture. Then, the mixture was mixed with beads: beads of zirconium oxide having an average particle size of 30 μm, using a stirring mill (capacity of mill container with stirrer: 170 mL, Ultra Apex Mill UAM015, manufactured by Kotobuki Industries Co., Ltd.) Dispersion treatment was performed under the conditions of bead filling ratio: 60% by volume, stirrer peripheral speed: 8.0 m / second, treatment time: 135 minutes, and a magnesium oxide fine particle dispersion was prepared. The transmittance of light having a wavelength of 700 nm of the obtained magnesium oxide fine particle dispersion was measured under the condition of a cell thickness of 10 mm, and was 63%.
The particle size distribution of the magnesium oxide fine particles in the obtained magnesium oxide fine particle dispersion was measured by the dynamic light scattering method under the following conditions. As a result, D 10 is 6.6 nm, D 50 is 8.5 nm, D 90 is 13.4nm,, D 10 / D 90 was 0.49.
［粒度分布の測定条件］
酸化マグネシウム微粒子分散液を、酸化マグネシウム微粒子の濃度が３〜４質量％となるように分散媒体にて希釈し、超音波ホモジナイザー（Ｓ−１５０Ｄ、ブランソン製）にて、パワー強度８の条件で１分間分散処理を行なう。得られた希釈分散液中の酸化マグネシウム微粒子の粒度分布を、動的光散乱式粒度分析計（マイクロトラックＵＰＡ１５０、日機装製）を用いて、半導体レーザ（＋３Ｂ）波長：７８０ｎｍ、３ｍＷの条件にて測定する。測定は５回行い、その平均値を算出する。
[Measurement conditions of particle size distribution]
The magnesium oxide fine particle dispersion is diluted with a dispersion medium so that the concentration of the magnesium oxide fine particles is 3 to 4% by mass, and is 1 with an ultrasonic homogenizer (S-150D, manufactured by Branson) at a power intensity of 8 conditions. Disperse for a minute. Using a dynamic light scattering particle size analyzer (Microtrac UPA150, manufactured by Nikkiso), the particle size distribution of the magnesium oxide fine particles in the obtained diluted dispersion was measured under the conditions of a semiconductor laser (+ 3B) wavelength: 780 nm, 3 mW. taking measurement. The measurement is performed 5 times, and the average value is calculated.
上記の酸化マグネシウム微粒子分散液を用いて、ガラス基板（サイズ：縦４０ｍｍ×横４０ｍｍ×厚さ０．５ｍｍ）上にスピンコート法により酸化マグネシウム膜を形成した。酸化マグネシウム膜は、酸化マグネシウム微粒子分散液１ｇをガラス基板の中心に滴下した後、ガラス基板をその中心を軸として１０００ｒｐｍの回転速度で６０秒、２０００ｒｐｍの回転速度で２０秒、３０００ｒｐｍの回転速度で２０秒の順で回転させる操作を５回行なった後、１２０℃の温度で１時間乾燥し、次いで５００℃の温度で１時間焼成して形成した。形成した酸化マグネシウム膜について、ガラス基板の中心から右端に１５ｍｍ、中心から右端に５ｍｍ、中心から左端に５ｍｍ、中心から左端に１５ｍｍの位置にて膜厚と波長５５０ｎｍの光の透過率とを測定した。膜厚は、反射分光膜厚計を用いて測定した。透過率は、分光光度計（ＵＶ−２５５０、（株）島津製作所製、光源：ハロゲンランプ）を用いて測定した。膜厚と透過率の測定結果とをそれぞれ表１に示す。 Using the magnesium oxide fine particle dispersion, a magnesium oxide film was formed on a glass substrate (size: length 40 mm × width 40 mm × thickness 0.5 mm) by spin coating. The magnesium oxide film is prepared by dropping 1 g of a magnesium oxide fine particle dispersion on the center of the glass substrate, and then rotating the glass substrate at the rotation speed of 1000 rpm for 60 seconds, the rotation speed of 2000 rpm for 20 seconds, and the rotation speed of 3000 rpm. The operation of rotating in the order of 20 seconds was performed 5 times, followed by drying at a temperature of 120 ° C. for 1 hour and then baking at a temperature of 500 ° C. for 1 hour. For the formed magnesium oxide film, the film thickness and light transmittance at a wavelength of 550 nm are measured at a position 15 mm from the center of the glass substrate to the right end, 5 mm from the center to the right end, 5 mm from the center to the left end, and 15 mm from the center to the left end. did. The film thickness was measured using a reflection spectral film thickness meter. The transmittance was measured using a spectrophotometer (UV-2550, manufactured by Shimadzu Corporation, light source: halogen lamp). Table 1 shows the film thickness and the measurement result of the transmittance.
表１
────────────────────────────────────────
中心から右端 中心から右端 中心から左端 中心から左端
に１５ｍｍ に５ｍｍ に５ｍｍ に１５ｍｍ
────────────────────────────────────────
膜厚 １６４３ｎｍ １５６１ｎｍ １５６１ｎｍ １５３９ｎｍ
────────────────────────────────────────
波長５５０ｎｍの
光の透過率 ９８％以上 ９８％以上 ９８％以上 ９８％以上
────────────────────────────────────────
Table 1
────────────────────────────────────────
Center to right edge Center to right edge Center to left edge Center to left edge
15mm to 5mm to 5mm to 15mm
────────────────────────────────────────
Film thickness 1643nm 1561nm 1561nm 1539nm
────────────────────────────────────────
Transmittance of light with a wavelength of 550 nm 98% or more 98% or more 98% or more 98% or more ──────────────────────────────── ─────────
［実施例２］
前記実施例１にて調製した酸化マグネシウム微粒子分散液をブチルアルコールで希釈して、酸化マグネシウム微粒子の濃度を２質量％に調整した。この希釈分散液を用いて、ガラス基板（サイズ：縦４０ｍｍ×横４０ｍｍ×厚さ０．５ｍｍ）上にスピンコート法により酸化マグネシウム膜を形成した。酸化マグネシウム膜は、希釈分散液１ｇをガラス基板の中心に滴下した後、ガラス基板をその中心を軸として５００ｒｐｍの回転速度で２００秒、１５００ｒｐｍの回転速度で６０秒、３０００ｒｐｍの回転速度で６０秒の順で回転させる操作を１０回行なった後、１２０℃の温度で１時間乾燥し、次いで５００℃の温度で１時間焼成して形成した。形成した酸化マグネシウム膜について、ガラス基板の中心、中心から右端に１５ｍｍ、中心から左端に１５ｍｍの位置にて膜厚と波長５５０ｎｍの光の透過率とを測定した。膜厚の測定には、（株）菱化システム製のマイクロマップ５５７Ｎを用いた。透過率の測定には、分光光度計（ＵＶ−２５５０、（株）島津製作所製、光源：ハロゲンランプ）を用いた。膜厚と透過率の測定結果とをそれぞれ表２に示す。
[Example 2]
The magnesium oxide fine particle dispersion prepared in Example 1 was diluted with butyl alcohol to adjust the concentration of the magnesium oxide fine particles to 2% by mass. Using this diluted dispersion, a magnesium oxide film was formed on a glass substrate (size: length 40 mm × width 40 mm × thickness 0.5 mm) by spin coating. For the magnesium oxide film, 1 g of the diluted dispersion is dropped onto the center of the glass substrate, and then the glass substrate is used as the axis for 200 seconds at a rotation speed of 500 rpm, 60 seconds at a rotation speed of 1500 rpm, and 60 seconds at a rotation speed of 3000 rpm. After rotating 10 times in this order, it was dried at 120 ° C. for 1 hour, and then fired at 500 ° C. for 1 hour to form. With respect to the formed magnesium oxide film, the film thickness and the transmittance of light having a wavelength of 550 nm were measured at the center of the glass substrate, 15 mm from the center to the right end and 15 mm from the center to the left end. For measurement of the film thickness, Micromap 557N manufactured by Ryoka System Co., Ltd. was used. A spectrophotometer (UV-2550, manufactured by Shimadzu Corporation, light source: halogen lamp) was used for the measurement of transmittance. Table 2 shows the film thickness and the measurement results of transmittance.
表２
────────────────────────────────────────
中心から右端 ガラス基板の中心 中心から左端
に１５ｍｍ に１５ｍｍ
────────────────────────────────────────
膜厚 ５０１ｎｍ ５００ｎｍ ５０２ｎｍ
────────────────────────────────────────
波長５５０ｎｍの
光の透過率 ９８％以上 ９８％以上 ９８％以上
────────────────────────────────────────
Table 2
────────────────────────────────────────
Center to right edge Center of glass substrate Left edge from center
15mm to 15mm
────────────────────────────────────────
Film thickness 501nm 500nm 502nm
────────────────────────────────────────
Light transmittance of 550 nm wavelength 98% or more 98% or more 98% or more ─────────────────────────────────── ──────
［実施例３］
実施例１において、分散媒体をイソプロピルアルコールとし、分散処理の条件を、処理時間：１０５分間とした以外は、実施例１と同様にして濃度５質量％の酸化マグネシウム微粒子分散液を調製した。得られた酸化マグネシウム微粒子分散液の波長７００ｎｍの光の透過率を、セル厚１０ｍｍの条件で測定したことろ、４０％であった。得られた酸化マグネシウム微粒子分散液中の酸化マグネシウム微粒子の粒度分布を動的光散乱法により前記の条件で測定した。その結果、Ｄ10は９．０ｎｍ、Ｄ50は１１．６ｎｍ、Ｄ90は１７．０ｎｍ、であり、Ｄ10／Ｄ90は０．５３であった。
上記の酸化マグネシウム微粒子分散液を、イソプロピルアルコールで希釈して、酸化マグネシウム微粒子の濃度を２質量％に調整した。この希釈分散液を用いて、スピンコートの実施回数を５回とする以外は、実施例２と同様にして酸化マグネシウム膜を形成した。形成した酸化マグネシウム膜について、ガラス基板の中心、中心から右端に１５ｍｍ、中心から左端に１５ｍｍの位置にて膜厚と波長５５０ｎｍの光の透過率とを実施例２と同様に測定した。膜厚と透過率の測定結果とをそれぞれ表３に示す。
[Example 3]
In Example 1, a magnesium oxide fine particle dispersion having a concentration of 5% by mass was prepared in the same manner as in Example 1 except that the dispersion medium was isopropyl alcohol and the conditions for the dispersion treatment were treatment time: 105 minutes. The transmittance of light having a wavelength of 700 nm of the obtained magnesium oxide fine particle dispersion was measured under the condition of a cell thickness of 10 mm, and was 40%. The particle size distribution of the magnesium oxide fine particles in the obtained magnesium oxide fine particle dispersion was measured by the dynamic light scattering method under the above conditions. As a result, D 10 is 9.0 nm, D 50 is 11.6 nm, D 90 is 17.0nm,, D 10 / D 90 was 0.53.
The magnesium oxide fine particle dispersion was diluted with isopropyl alcohol to adjust the concentration of the magnesium oxide fine particles to 2% by mass. Using this diluted dispersion, a magnesium oxide film was formed in the same manner as in Example 2 except that the number of times of spin coating was changed to 5. About the formed magnesium oxide film, the film thickness and the light transmittance at a wavelength of 550 nm were measured in the same manner as in Example 2 at the center of the glass substrate, 15 mm from the center to the right end and 15 mm from the center to the left end. Table 3 shows the film thickness and the measurement result of transmittance.
表３
────────────────────────────────────────
中心から右端 ガラス基板の中心 中心から左端
に１５ｍｍ に１５ｍｍ
────────────────────────────────────────
膜厚 ５７８ｎｍ ５６８ｎｍ ５６４ｎｍ
────────────────────────────────────────
波長５５０ｎｍの
光の透過率 ９８％以上 ９８％以上 ９８％以上
────────────────────────────────────────
Table 3
────────────────────────────────────────
Center to right edge Center of glass substrate Left edge from center
15mm to 15mm
────────────────────────────────────────
Film thickness 578nm 568nm 564nm
────────────────────────────────────────
Light transmittance of 550 nm wavelength 98% or more 98% or more 98% or more ─────────────────────────────────── ──────
実施例１〜３の結果から明らかなように、本発明の酸化マグネシウム微粒子分散液を用いることにより、均一な厚さで、かつ透光性の高い酸化マグネシウム膜を形成することができることが分かる。 As is apparent from the results of Examples 1 to 3, it can be seen that a magnesium oxide film having a uniform thickness and high translucency can be formed by using the magnesium oxide fine particle dispersion of the present invention.
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| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
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| LAPS | Cancellation because of no payment of annual fees |