JP2006225240A - Magnesium oxide particulate-dispersed liquid - Google Patents
Magnesium oxide particulate-dispersed liquid Download PDFInfo
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本発明は、酸化マグネシウム微粒子分散液に関するものである。 The present invention relates to a magnesium oxide fine particle dispersion.
プラズマディスプレイパネル（以下、ＰＤＰという）の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 a dielectric layer of a plasma display panel (hereinafter referred to as PDP). 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. 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。
均一な厚さの酸化マグネシウム薄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、すなわ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小径の凝集粒子として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、均一な厚さの酸化マグネシウム薄膜を塗布法により形成させるのに有利な、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 thin film having a uniform thickness by a coating method, there is little aggregation of magnesium oxide fine particles in the dispersion, that is, the magnesium oxide fine particles are dispersed as primary particles or small-sized aggregate particles close to the primary particles. It is desirable. 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 provide a dispersion of magnesium oxide fine particles, in which magnesium oxide fine particles are dispersed as primary particles or small aggregated particles close to them, which is advantageous for forming a magnesium oxide thin film having a uniform thickness by a coating method. It is to provide.
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、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-sized aggregated particles close to the primary particles, and the present invention has been achieved.
本発明は、炭素原子数３〜５の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の範囲にある酸化マグネシウム微粒子分散液にある。 In the present invention, magnesium oxide fine particles are dispersed in an alcohol having 3 to 5 carbon atoms in a range of 0.05 to 20% by mass, and the D 50 of the magnesium oxide fine particles measured by a dynamic light scattering method is The magnesium oxide fine particle dispersion is 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（１−ブタノール）、もしくはこれらの混合物である。
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 (1-butanol), or a mixture thereof.
本発明の酸化マグネシウム微粒子分散液は、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と、炭素原子数３〜５の一価アルコールとを混合し、次いで、その混合物を平均粒子径が２０〜３００μｍの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。 The magnesium oxide fine particle dispersion of the present invention is prepared by mixing magnesium oxide fine particles having an average primary particle diameter in the range of 5 to 100 nm and monohydric alcohol having 3 to 5 carbon atoms, and then mixing the mixture with an average particle diameter. Can be produced by a method comprising a dispersion treatment in a pulverizer using beads having a diameter of 20 to 300 μm.
本発明の酸化マグネシウム微粒子分散液は、均一な厚さの酸化マグネシウム薄膜を塗布法により形成させるのに有利である。
また、本発明の製造方法を利用することにより、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酸化マグネシウム微粒子の分散液を工業的に有利に製造することができる。
The magnesium oxide fine particle dispersion of the present invention is advantageous for forming a magnesium oxide thin film having a uniform thickness by a coating method.
Further, by using the production method of the present invention, a dispersion of magnesium oxide fine particles in which magnesium oxide fine particles are dispersed as primary particles or small-diameter aggregate particles close thereto can be advantageously produced industrially.
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.
本発明の分散液は、酸化マグネシウム薄膜形成用の塗布液として有利に用いることができる。本発明の分散液を用いて形成した酸化マグネシウム薄膜は、膜厚の均一性が高い。特に、本発明の分散液を用いて形成した膜厚が５００ｎｍ〜２μｍの酸化マグネシウム薄膜は高い透明性を示すため、ＰＤＰの誘電体層の保護膜として有用である。本発明の分散液を用いて酸化マグネシウム薄膜を形成する方法としては、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。 The dispersion liquid of the present invention can be advantageously used as a coating liquid for forming a magnesium oxide thin film. The magnesium oxide thin film formed using the dispersion liquid of the present invention has high film thickness uniformity. In particular, a magnesium oxide thin film having a film thickness of 500 nm to 2 μm formed using the dispersion of the present invention exhibits high transparency and is useful as a protective film for a dielectric layer of PDP. Examples of the method for forming a magnesium oxide thin film using the dispersion of the present invention 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. .
本発明の分散液はまた、粉体や液体に容易に混合分散することができるため、食品、医薬あるいは化粧品のｐＨ調製剤、高分子安定剤、各種セラミックス材料の焼結助剤としても利用することができる。 Since the dispersion of the present invention can be easily mixed and dispersed in powders and liquids, it can also be used as a pH adjuster for food, medicine or cosmetics, a polymer stabilizer, and a sintering aid for various ceramic materials. be able to.
［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、イソプロピルアルコール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：１０５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Ｄ10、Ｄ50、Ｄ90の測定結果及びＤ10／Ｄ90を表１に示す。
[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 isopropyl 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: 105 minutes, to prepare a magnesium oxide fine particle dispersion. 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. The measurement results of D 10 , D 50 and D 90 and D 10 / D 90 are shown in Table 1.
［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.
［実施例２］
実施例１において、分散媒体をブチルアルコールとし、分散処理の条件を、処理時間：１３５分間とした以外は、実施例１と同様にし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、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前記の方法により測定した。そのＤ10、Ｄ50、Ｄ90の測定結果及びＤ10／Ｄ90を表１に示す。
[Example 2]
A magnesium oxide fine particle dispersion was prepared in the same manner as in Example 1 except that in Example 1, the dispersion medium was butyl alcohol, and the conditions for the dispersion treatment were treatment time: 135 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 method described above. The measurement results of D 10 , D 50 and D 90 and D 10 / D 90 are shown in Table 1.
［実施例３］
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、イソプロピルアルコール９５質量部に投入して混合物を得た。次いで、その混合物を、ロッキングミル（ミル容器の容量：１００ｍＬ、ＲＭ−０１、（株）セイワ技研製）を用いて、ビーズ：平均粒子径１００μｍ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：５０体積％、ミル容器の振動速度：５００ｒｐｍ、処理時間：６０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中の酸化マグネシウム微粒子の粒度分布を前記の方法により測定した。そのＤ10、Ｄ50、Ｄ90の測定結果及びＤ10／Ｄ90を表１に示す。
[Example 3]
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 isopropyl alcohol to obtain a mixture. Subsequently, the mixture was used for rocking mill (capacity of mill container: 100 mL, RM-01, manufactured by Seiwa Giken Co., Ltd.), beads: beads made of zirconium oxide having an average particle diameter of 100 μm, and bead filling ratio in the mill container. : Dispersion treatment was performed under the conditions of 50 volume%, mill container vibration speed: 500 rpm, treatment time: 60 minutes to prepare a magnesium oxide fine particle dispersion.
The particle size distribution of the magnesium oxide fine particles in the obtained magnesium oxide fine particle dispersion was measured by the method described above. The measurement results of D 10 , D 50 and D 90 and D 10 / D 90 are shown in Table 1.
［実施例４］
実施例１において、分散媒体をブチルアルコールとし、分散処理の条件を、処理時間：１２０分間とした以外は、実施例１と同様にし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中の酸化マグネシウム微粒子の粒度分布を前記の方法により測定した。そのＤ10、Ｄ50、Ｄ90の測定結果及びＤ10／Ｄ90を表１に示す。
[Example 4]
In Example 1, a magnesium oxide fine particle dispersion was prepared in the same manner as in Example 1 except that the dispersion medium was butyl alcohol and the conditions for the dispersion treatment were treatment time: 120 minutes.
The particle size distribution of the magnesium oxide fine particles in the obtained magnesium oxide fine particle dispersion was measured by the method described above. The measurement results of D 10 , D 50 and D 90 and D 10 / D 90 are shown in Table 1.
［実施例５］
実施例１において、酸化マグネシウム微粒子を平均一次粒子径が５０ｎｍの酸化マグネシウム微粒子（５００Ａ、宇部マテリアルズ（株）製）とし、分散処理の条件を、攪拌機の周速：１４／秒、処理時間：１０５分間とした以外は、実施例１と同様にし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中の酸化マグネシウム微粒子の粒度分布を前記の方法により測定した。そのＤ10、Ｄ50、Ｄ90の測定結果及びＤ10／Ｄ90を表１に示す。
[Example 5]
In Example 1, the magnesium oxide fine particles are magnesium oxide fine particles having an average primary particle diameter of 50 nm (500A, manufactured by Ube Materials Co., Ltd.), and the dispersion treatment conditions are as follows: peripheral speed of stirrer: 14 / second, treatment time: A magnesium oxide fine particle dispersion was prepared in the same manner as in Example 1 except that the duration was 105 minutes.
The particle size distribution of the magnesium oxide fine particles in the obtained magnesium oxide fine particle dispersion was measured by the method described above. The measurement results of D 10 , D 50 and D 90 and D 10 / D 90 are shown in Table 1.
表１
────────────────────────────────────────
Ｄ10 Ｄ50 Ｄ90 Ｄ10／Ｄ90
（ｎｍ） （ｎｍ） （ｎｍ） （−）
────────────────────────────────────────
実施例１ ９．０ １１．６ １７．０ ０．５３
実施例２ ６．６ ８．５ １３．４ ０．４９
実施例３ ８．０ １０．１ １６．４ ０．４９
実施例４ ７．６ ８．９ １４．９ ０．５１
実施例５ ３４．７ ５３．９ １８９．２ ０．１８
────────────────────────────────────────
注）平均一次粒子径は、ＦＥ−ＳＥＭにて測定した値。
Table 1
────────────────────────────────────────
D 10 D 50 D 90 D 10 / D 90
(Nm) (nm) (nm) (-)
────────────────────────────────────────
Example 1 9.0 11.6 17.0 0.53
Example 2 6.6 8.5 13.4 0.49
Example 3 8.0 10.1 16.4 0.49
Example 4 7.6 8.9 14.9 0.51
Example 5 34.7 53.9 189.2 0.18
────────────────────────────────────────
Note) The average primary particle diameter is a value measured by FE-SEM.
［実施例６］
実施例２にて調製した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回行なって形成した。形成した酸化マグネシウム膜厚を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の位置にて反射分光膜厚計を用いて測定した。その結果を表２に示す。
[Example 6]
Using the magnesium oxide fine particle dispersion prepared in Example 2, 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. It was formed by performing the operation of rotating in the order of 20 seconds 5 times. The formed magnesium oxide film thickness was measured using a reflection spectral film thickness meter at a position of 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. The results are shown in Table 2.
表２
────────────────────────────────────────
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
────────────────────────────────────────
酸化マグネシウム膜
の膜厚（ｎｍ） １６４３ １５６１ １５６１ １５３９
────────────────────────────────────────
Table 2
────────────────────────────────────────
Center to right edge Center to right edge Center to left edge Center to left edge
15mm to 5mm to 5mm to 15mm
────────────────────────────────────────
Magnesium oxide film thickness (nm) 1643 1561 1561 1539
────────────────────────────────────────
表２に示すように、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、均一な厚さの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 shown in Table 2, it can be seen that a magnesium oxide film having a uniform thickness can be formed by using the magnesium oxide fine particle dispersion of the present invention.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007137695A (en) * | 2005-11-15 | 2007-06-07 | Ube Material Industries Ltd | Magnesium oxide fine power dispersion and method for producing the same |
| JP2010015699A (en) * | 2008-07-01 | 2010-01-21 | Panasonic Corp | Method of manufacturing plasma display panel, and method of manufacturing metal oxide paste for plasma display panel |
| WO2011007638A1 (en) * | 2009-07-14 | 2011-01-20 | 堺化学工業株式会社 | Magnesium oxide particles, method for producing same, heat dissipating filler, resin composition, heat dissipating grease, and heat dissipating coating composition |
| WO2012043564A1 (en) * | 2010-09-28 | 2012-04-05 | タテホ化学工業株式会社 | Magnesium hydroxide microparticles, magnexium oxide microparticles, and method for producing each |
| JP2014114178A (en) * | 2012-12-07 | 2014-06-26 | Ube Material Industries Ltd | Magnesium oxide fine particle fluid dispersion |
| WO2015146875A1 (en) * | 2014-03-24 | 2015-10-01 | 宇部マテリアルズ株式会社 | Fine magnesium oxide particle dispersion liquid and method for producing same |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58191759A (en) * | 1982-05-06 | 1983-11-09 | Shin Nippon Kagaku Kogyo Co Ltd | Magnesia for coating and its composition |
| JPH11157832A (en) * | 1997-11-28 | 1999-06-15 | Tsuchiya Co Ltd | Coating liquid for forming transparent magnesium oxide coating film |
| JP2000129161A (en) * | 1998-10-21 | 2000-05-09 | Mitsubishi Materials Corp | Coating solution for fpd protecting film and its preparation |
| JP2006173129A (en) * | 2004-12-16 | 2006-06-29 | Lg Electronics Inc | Dispersion solvent and manufacturing method of same |
-
2005
- 2005-02-21 JP JP2005044766A patent/JP4849807B2/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58191759A (en) * | 1982-05-06 | 1983-11-09 | Shin Nippon Kagaku Kogyo Co Ltd | Magnesia for coating and its composition |
| JPH11157832A (en) * | 1997-11-28 | 1999-06-15 | Tsuchiya Co Ltd | Coating liquid for forming transparent magnesium oxide coating film |
| JP2000129161A (en) * | 1998-10-21 | 2000-05-09 | Mitsubishi Materials Corp | Coating solution for fpd protecting film and its preparation |
| JP2006173129A (en) * | 2004-12-16 | 2006-06-29 | Lg Electronics Inc | Dispersion solvent and manufacturing method of same |
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| JP2011020870A (en) * | 2009-07-14 | 2011-02-03 | Sakai Chem Ind Co Ltd | Magnesium oxide particle, method for producing the same, heat dissipating filler, resin composition, heat dissipating grease, and heat dissipating coating composition |
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