JP2007137695A - Magnesium oxide fine power dispersion and method for producing the same - Google Patents
Magnesium oxide fine power dispersion and method for producing the same Download PDFInfo
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- 239000006185 dispersion Substances 0.000 title claims abstract description 99
- 239000000395 magnesium oxide Substances 0.000 title claims abstract description 93
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 title claims abstract description 93
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 239000010419 fine particle Substances 0.000 claims abstract description 63
- 239000000843 powder Substances 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000003495 polar organic solvent Substances 0.000 claims abstract description 9
- 238000002296 dynamic light scattering Methods 0.000 claims abstract description 8
- 239000011164 primary particle Substances 0.000 claims description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 12
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052804 chromium Inorganic materials 0.000 claims description 6
- 239000011651 chromium Substances 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 6
- 229910052759 nickel Inorganic materials 0.000 claims description 6
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims 1
- 229910001928 zirconium oxide Inorganic materials 0.000 claims 1
- 239000010409 thin film Substances 0.000 abstract description 11
- 238000000576 coating method Methods 0.000 abstract description 6
- 239000002245 particle Substances 0.000 description 19
- 239000007788 liquid Substances 0.000 description 11
- 238000009826 distribution Methods 0.000 description 10
- 239000010408 film Substances 0.000 description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 8
- 238000011282 treatment Methods 0.000 description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 5
- 229910052726 zirconium Inorganic materials 0.000 description 5
- 150000001298 alcohols Chemical class 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 229910052749 magnesium Inorganic materials 0.000 description 4
- 239000011777 magnesium Substances 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical class OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 3
- 230000001186 cumulative effect Effects 0.000 description 3
- 150000002576 ketones Chemical class 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
- 238000005259 measurement Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 2
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000007789 gas Substances 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
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- FDPIMTJIUBPUKL-UHFFFAOYSA-N pentan-3-one Chemical compound CCC(=O)CC FDPIMTJIUBPUKL-UHFFFAOYSA-N 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000004528 spin coating Methods 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 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
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 238000010130 dispersion processing Methods 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- 239000012776 electronic material Substances 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
- 238000010304 firing Methods 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
- 238000007646 gravure printing Methods 0.000 description 1
- 229940035429 isobutyl alcohol Drugs 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
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- MSXVEPNJUHWQHW-UHFFFAOYSA-N tertiary amyl alcohol Natural products CCC(C)(C)O MSXVEPNJUHWQHW-UHFFFAOYSA-N 0.000 description 1
Abstract
Description
本発明は、酸化マグネシウム微粒子分散液及びその製造方法に関するものである。 The present invention relates to a magnesium oxide fine particle dispersion and a method for producing the same.
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には、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粉末分散液を調製し、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主成分とするバインダと、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添加剤とを混合してバインダ溶液を調製し、粉末分散液とバインダ溶液をペイントシェーカーやロールミルなどを用いて混合することによって調製することができるとされている。但し、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子径に関する記載はない。 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 size of 5 nm to 5 μm, preferably 10 to 200 nm, a solvent mainly containing alcohol, or a mixed solvent of alcohol and ethylene glycol derivative. And a dispersant mainly containing an ethylene glycol derivative to prepare a powder dispersion, a binder mainly containing magnesium alkoxide or magnesium acetylacetonate, a solvent mainly containing alcohol or alcohol and ethylene A binder solution is prepared by mixing a mixed solvent with a glycol derivative and an additive mainly composed of an ethylene glycol derivative, and then prepared by mixing the powder dispersion and the binder solution using a paint shaker or a roll mill. It is supposed to be possible. However, there is no description regarding the particle diameter of the magnesium oxide fine particles in the magnesium oxide fine particle dispersion.
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には、酸化マグネシウム微粒子は平均粒子径が１０ｎｍ以下であることが好ましいとされており、さらに酸化マグネシウム微粒子は、例えば、ロールミル、ホモミキサー、ボールミル等の分散機器を用いて分散させることができる旨の記載がある。但し、この特許文献２にも、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子径に関する記載はない。
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、本発明者の検討によると、前記の特許文献１、２に記載されているような分散装置では、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分散液を製造することは難しいことが判明した。従って、前記の特許文献１、２に記載されている酸化マグネシウム微粒子分散液では、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及びその製造方法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, according to the study by the present inventor, in the dispersing apparatus as described in the above-mentioned Patent Documents 1 and 2, magnesium oxide fine particle dispersion in which magnesium oxide fine particles are dispersed as primary particles or small-sized aggregated particles close thereto. It has proven difficult to produce the liquid. Therefore, in the magnesium oxide fine particle dispersion described in Patent Documents 1 and 2, 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 the primary particles, which is advantageous for forming a magnesium oxide thin film having a uniform thickness by a coating method. It is in providing the manufacturing method.
本発明は、極性有機溶媒中に、酸化マグネシウム微粒子が分散液全体量に対して０．０５〜２０質量％の範囲となる量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５〜２０ｎｍの範囲にあり、Ｄ10／Ｄ90が０．３以上で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 a polar organic solvent in an amount ranging from 0.05 to 20% by mass with respect to the total amount of the dispersion, and measured by the dynamic light scattering method. The magnesium oxide fine particle dispersion has a D 50 of magnesium fine particles in the range of 5 to 20 nm and a D 10 / D 90 of 0.3 or more.
本発明の酸化マグネシウム微粒子分散液は、ジルコニウム、鉄、ニッケル、クロム及びアルミニウムをそれぞれ、分散液全体量に対して２０質量ｐｐｍ以上含むことがないことが好ましい。 The magnesium oxide fine particle dispersion of the present invention preferably does not contain 20 mass ppm or more of zirconium, iron, nickel, chromium and aluminum with respect to the total amount of the dispersion.
本発明はまた、平均一次粒子径が５〜２０ｎｍの範囲にある酸化マグネシウム微粒子からなる酸化マグネシウム粉末を、極性有機溶媒に分散させて分散液を調製する工程、そして該分散液に圧力を付与して分散液噴流を生成させ、次いで該分散液噴流を二以上に分岐させ、各分散液噴流を対向下に衝突させることにより分散液中の酸化マグネシウム粉末を崩壊させて微粒子の分散液とする工程を含む上記本発明の酸化マグネシウム微粒子分散液の製造方法にもある。 The present invention also includes a step of dispersing a magnesium oxide powder comprising magnesium oxide fine particles having an average primary particle diameter in the range of 5 to 20 nm in a polar organic solvent to prepare a dispersion, and applying pressure to the dispersion. A step of generating a dispersion liquid jet, then branching the dispersion liquid jet into two or more, and colliding each dispersion liquid jet against each other to collapse the magnesium oxide powder in the dispersion liquid to form a fine particle dispersion liquid There is also a method for producing a magnesium oxide fine particle dispersion of the present invention including the above.
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、極性有機溶媒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 contains magnesium oxide fine particles in a polar organic solvent in a range of 0.05 to 20% by mass, preferably in a range of 1 to 15% by mass, based on the mass of the total composition of the dispersion. Included.
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５〜２０ｎｍの範囲にあり、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０．３以上である。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。Ｄ10／Ｄ90は、０．３５以上であることがより好ましい。 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 the dynamic light scattering method in the range of 5 to 20 nm, and D 10 (cumulative). The ratio (D 10 / D 90 ) between D 90 (particle diameter corresponding to 10% of the passage distribution) and D 90 (particle diameter corresponding to 90% of the cumulative passage distribution) is 0.3 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. D 10 / D 90 is more preferably 0.35 or more.
本発明の分散液において用いられる極性有機溶媒の例としては、アルコール類及びケトン類を挙げることができる。アルコール類の例としては、メタノール、エタノール、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の一価アルコールを挙げることができる。ケトン類の例としては、アセトン、エチルメチルケトン、ジエチルケトンを挙げることができる。これらのアルコール類及びケトン類は、二種以上を併用してもよい。
極性有機溶媒は、炭素原子数が３〜５の一価アルコールであることが好ましく、特に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り、さらに好ましいのはブチルアルコールである。
Examples of the polar organic solvent used in the dispersion of the present invention include alcohols and ketones. Examples of alcohols include monohydric alcohols such as methanol, ethanol, propyl alcohol, isopropyl alcohol, butyl alcohol, isobutyl alcohol, sec-butyl alcohol, tert-butyl alcohol, pentyl alcohol, and isopentyl alcohol. Examples of ketones include acetone, ethyl methyl ketone, and diethyl ketone. Two or more of these alcohols and ketones may be used in combination.
The polar organic solvent is preferably a monohydric alcohol having 3 to 5 carbon atoms, particularly preferably isopropyl alcohol and butyl alcohol, and a mixture thereof, and more preferably butyl alcohol.
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５〜２０ｎｍの範囲にある酸化マグネシウム微粒子からなる酸化マグネシウム粉末を、極性有機溶媒に分散させて分散液を調製する工程、そして該分散液に圧力を付与して分散液噴流を生成させ、次いで該分散液噴流を二以上に分岐させ、各分散液噴流を対向下に衝突させることにより分散液中の酸化マグネシウム粉末を崩壊させて微粒子の分散液とする衝突分散処理工程を含む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 comprises a step of preparing a dispersion by dispersing magnesium oxide powder composed of magnesium oxide fine particles having an average primary particle diameter in the range of 5 to 20 nm in a polar organic solvent, and the dispersion Pressure is applied to generate a dispersion jet, then the dispersion jet is branched into two or more, and each dispersion jet collides under the opposite direction to collapse the magnesium oxide powder in the dispersion, thereby It can be produced by a method including a collision dispersion treatment step as a dispersion.
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）により製造された平均一次粒子が２０ｎｍ以下の酸化マグネシウム粉末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された平均一次粒子径が２０ｎｍ以下の酸化マグネシウム粉末としては、宇部マテリアルズ（株）製の１００Ａ（平均一次粒子径：１０ｎｍ）が知られている。酸化マグネシウム粉末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 powder having an average primary particle size of 20 nm or less produced by a method of reacting metal magnesium vapor with oxygen (gas phase oxidation synthesis method) can be suitably used. As a magnesium oxide powder having an average primary particle diameter of 20 nm or less manufactured by a gas phase oxidation synthesis method, 100A (average primary particle diameter: 10 nm) manufactured by Ube Materials Co., Ltd. is known. The average primary particle diameter of the magnesium oxide powder can be measured using a field emission scanning electron microscope (FE-SEM).
衝突分散処理工程においては、酸化マグネシウム粉末の分散液に圧力を付与して分散液噴流を生成させ、次いで該分散液噴流を二以上、好ましくは二つに分岐させ、各分散液を対向下に衝突させる。分散液噴流の圧力は、１００〜２５０ＭＰａの範囲にあることが好ましく、１３０〜２３０ＭＰａの範囲にあることが特に好ましい。 In the collision dispersion treatment step, pressure is applied to the dispersion of the magnesium oxide powder to generate a dispersion jet, and then the dispersion jet is branched into two or more, preferably two, and each dispersion is placed under the facing. Collide. The pressure of the dispersion jet is preferably in the range of 100 to 250 MPa, and particularly preferably in the range of 130 to 230 MPa.
衝突分散処理工程は、複数回行なってもよい。衝突分散処理工程の回数は、１〜１０００回の範囲にあることが好ましい。
衝突分散処理工程において用いる衝突装置の例としては、吉田機械工業（株）から販売されているナノマイザーシステムを挙げることができる。
The collision dispersion processing step may be performed a plurality of times. The number of collision dispersion treatment steps is preferably in the range of 1 to 1000 times.
As an example of the collision device used in the collision dispersion treatment process, a nanomizer system sold by Yoshida Machine Industry Co., Ltd. can be cited.
上記の衝突分散処理により得られた酸化マグネシウム微粒子分散液は、微粒子分散のための衝突分散が、分散液の金属壁への衝突によるものではなく、分散液同士の衝突により行われるため、重金属の混入が少ない。ジルコニウム、鉄、ニッケル、クロム及びアルミニウムについては、それぞれ全体量に対して２０質量ｐｐｍ以上含むことがない高純度の酸化マグネシウム微粒子分散液を製造することができる。 In the magnesium oxide fine particle dispersion obtained by the above-described collision dispersion treatment, collision dispersion for fine particle dispersion is not caused by collision of the dispersion against the metal wall, but by collision between the dispersions. There is little contamination. About zirconium, iron, nickel, chromium, and aluminum, it is possible to produce a high-purity magnesium oxide fine particle dispersion that does not contain 20 mass ppm or more of the total amount.
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させ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原料及び焼結助剤としても利用することができる。また、ジルコニウム、鉄、ニッケル、クロム及びアルミニウムの混入量の少ない高純度の本発明の酸化マグネシウム微粒子分散液は、電子材料、医薬品原料、飲食料品の添加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 food, pharmaceutical or cosmetic pH adjuster, polymer stabilizer, raw materials for various ceramic materials and sintering aids. Can be used. In addition, the high-purity magnesium oxide fine particle dispersion of the present invention having a small amount of zirconium, iron, nickel, chromium, and aluminum can be used as an additive for electronic materials, pharmaceutical raw materials, and food and drink products.
［実施例１］
平均一次粒子径が１０ｎｍの酸化マグネシウム粉末（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質量部に投入して濃度５質量％の酸化マグネシウム粉末分散液を得た。この酸化マグネシウム粉末分散液を、ナノマイザーシステム（ＮＭ２、吉田機械工業（株）製、ノズル径：１５０μｍ×１７０μｍ）を用いて、分散液噴流の圧力２００Ｍｐａ、衝突分散処理回数１００回の条件にて、酸化マグネシウム粉末を崩壊させて酸化マグネシウム微粒子分散液を製造した。
[Example 1]
5 parts by mass of magnesium oxide powder (100A, Ube Materials Co., Ltd.) having an average primary particle size of 10 nm was added to 95 parts by mass of butyl alcohol to obtain a magnesium oxide powder dispersion having a concentration of 5% by mass. This magnesium oxide powder dispersion was subjected to a dispersion jet pressure of 200 Mpa and a collision dispersion treatment count of 100 using a nanomizer system (NM2, manufactured by Yoshida Machine Industry Co., Ltd., nozzle diameter: 150 μm × 170 μm). Then, the magnesium oxide powder was disintegrated to produce a magnesium oxide fine particle dispersion.
得られた酸化マグネシウム微粒子分散液中のジルコニウム、鉄、ニッケル、クロム及びアルミニウムを定量したところ、ジルコニウム６質量ｐｐｍ、鉄１．８質量ｐｐｍ、ニッケル１．０質量ｐｐｍ、クロム４．０質量ｐｐｍ及びアルミニウム２．０質量ｐｐｍであった。 When zirconium, iron, nickel, chromium and aluminum in the obtained magnesium oxide fine particle dispersion were quantified, zirconium 6 mass ppm, iron 1.8 mass ppm, nickel 1.0 mass ppm, chromium 4.0 mass ppm and It was 2.0 mass ppm of aluminum.
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１１．３ｎｍ、Ｄ50は１４．２ｎｍ、Ｄ90は２９．１ｎｍであり、Ｄ10／Ｄ90は０．３９であった。 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 11.3 nm, D 50 is 14.2 nm, D 90 is 29.1nm, D 10 / D 90 was 0.39.
［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) under the condition of power intensity of 8. 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の膜厚と波長６００ｎｍの光の透光率をガラス基板の中心、中心から右端に１５ｍｍ、中心から左端に１５ｍｍの位置にて測定した。その結果を表１に示す。 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. A magnesium oxide film is prepared by dropping 1 g of a magnesium oxide fine particle dispersion on the center of a 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 thickness of the formed magnesium oxide film and the transmittance of light having a wavelength of 600 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. The results are shown in Table 1.
表１
────────────────────────────────────────
中心から右端 中心 中心から左端
に１５ｍｍ に１５ｍｍ
────────────────────────────────────────
膜厚（μｍ） １．９３ ２．０８ ２．０５
透光率（％） ９５．１ ９６．４ ９８．４
────────────────────────────────────────
Table 1
────────────────────────────────────────
Center to right edge Center Center to left edge
15mm to 15mm
────────────────────────────────────────
Film thickness (μm) 1.93 2.08 2.05
Light transmittance (%) 95.1 96.4 98.4
────────────────────────────────────────
表１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 1, 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.
［実施例２］
ナノマイザーシステムによる酸化マグネシウム粉末分散液の衝突分散処理の回数を１０回とする以外は実施例１と同様にして微粒子分散液を製造した。
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１１．７ｎｍ、Ｄ50は１５．１ｎｍ、Ｄ90は２８．２ｎｍであり、Ｄ10／Ｄ90は０．４１であった。
[Example 2]
A fine particle dispersion was produced in the same manner as in Example 1 except that the number of collision dispersion treatments of the magnesium oxide powder dispersion by the nanomizer system was 10.
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 11.7 nm, D 50 is 15.1nm, D 90 is 28.2nm, D 10 / D 90 was 0.41.
［実施例３］
ナノマイザーシステムによる酸化マグネシウム粉末分散液の衝突分散処理の回数を５００回とする以外は実施例１と同様にして微粒子分散液を製造した。
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１１．５ｎｍ、Ｄ50は１５．１ｎｍ、Ｄ90は２７．１ｎｍであり、Ｄ10／Ｄ90は０．４２であった。
[Example 3]
A fine particle dispersion was produced in the same manner as in Example 1 except that the number of collision dispersion treatments of the magnesium oxide powder dispersion by the nanomizer system was 500 times.
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 11.5 nm, D 50 is 15.1nm, D 90 is 27.1nm, D 10 / D 90 was 0.42.
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| JP2012096951A (en) * | 2010-11-01 | 2012-05-24 | Ryukoku Univ | Method of manufacturing magnesium oxide thin film |
| JP2015010025A (en) * | 2013-07-01 | 2015-01-19 | 宇部マテリアルズ株式会社 | Alkaline earth metal compound fine particle dispersion and method for producing the same |
| 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 |
| JP2017069376A (en) * | 2015-09-30 | 2017-04-06 | 宇部興産株式会社 | Solar cell module and manufacturing method therefor |
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| JP2006225240A (en) * | 2005-02-21 | 2006-08-31 | Ube Material Industries Ltd | Magnesium oxide particulate-dispersed liquid |
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| JPH02160658A (en) * | 1988-12-13 | 1990-06-20 | Mitsubishi Mining & Cement Co Ltd | Method for granulating magnesium oxide raw material for forming |
| JP2006225240A (en) * | 2005-02-21 | 2006-08-31 | Ube Material Industries Ltd | Magnesium oxide particulate-dispersed liquid |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2012096951A (en) * | 2010-11-01 | 2012-05-24 | Ryukoku Univ | Method of manufacturing magnesium oxide thin film |
| JP2015010025A (en) * | 2013-07-01 | 2015-01-19 | 宇部マテリアルズ株式会社 | Alkaline earth metal compound fine particle dispersion and method for producing the same |
| 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 |
| CN106163988A (en) * | 2014-03-24 | 2016-11-23 | 宇部材料工业株式会社 | The sub-dispersion liquid of magnesium oxide particle and manufacture method thereof |
| KR20160136395A (en) | 2014-03-24 | 2016-11-29 | 우베 마테리알즈 가부시키가이샤 | Fine magnesium oxide particle dispersion liquid and method for producing same |
| JPWO2015146875A1 (en) * | 2014-03-24 | 2017-04-13 | 宇部マテリアルズ株式会社 | Magnesium oxide fine particle dispersion and method for producing the same |
| US10030150B2 (en) | 2014-03-24 | 2018-07-24 | Ube Material Industries, Ltd. | Fine magnesium oxide particle dispersion liquid and method for producing same |
| KR102275613B1 (en) * | 2014-03-24 | 2021-07-09 | 우베 마테리알즈 가부시키가이샤 | Fine magnesium oxide particle dispersion liquid and method for producing same |
| JP2017069376A (en) * | 2015-09-30 | 2017-04-06 | 宇部興産株式会社 | Solar cell module and manufacturing method therefor |
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