JPH11228123A - Spherical amorphous mullite based fine particle and its production and its utilization - Google Patents
Spherical amorphous mullite based fine particle and its production and its utilizationInfo
- Publication number
- JPH11228123A JPH11228123A JP5125798A JP5125798A JPH11228123A JP H11228123 A JPH11228123 A JP H11228123A JP 5125798 A JP5125798 A JP 5125798A JP 5125798 A JP5125798 A JP 5125798A JP H11228123 A JPH11228123 A JP H11228123A
- Authority
- JP
- Japan
- Prior art keywords
- based fine
- fine particles
- spherical amorphous
- mullite
- amorphous mullite
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、電子写真用トナー
の外添剤、蛍光灯の内面コーティング用、研磨材、充填
剤などに有用な透明性の良好な球状の非晶質ムライト系
微粒子およびその製造方法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to spherical amorphous mullite fine particles having good transparency useful as an external additive for electrophotographic toner, an inner coating of a fluorescent lamp, an abrasive, a filler and the like. The present invention relates to the manufacturing method.
【０００２】[0002]
【従来の技術】ムライトは、一般式３Ａｌ2 ０3 ・２Ｓ
ｉＯ2 で表される針状の結晶で、耐熱性があり、熱膨張
率が小さいので、高温用エンジニアリングセラミック、
電子基板材料、触媒担体として期待さている。このムラ
イトの製造方法としては、アルミナゾルとシリカゾルの
混合ゾルをゲル化した後、焼成する方法（ゾル・ゲル
法）、アルミニウムアルコキシドとケイ素アルコキシド
を混合し、加水分解した後、脱水、乾燥、焼成する方法
（アルコキシド法）、シリカとアルミナ原料を電解炉に
より溶融したものを粉砕する方法、アルミナゾルとシリ
カゾルの分散液を火炎温度が１０００〜１７００℃の雰
囲気中に分散液の噴霧液滴粒径が１５０μｍ以下で噴
霧、焼成し球状粉末を得る方法（特開平５−１０５４１
９号公報）などがある。 2. Description of the Related Art Mullite has a general formula of 3Al 2 O 3 .2S
A needle-shaped crystal represented by iO 2, which has heat resistance and a low coefficient of thermal expansion.
It is expected as an electronic substrate material and a catalyst carrier. As a method for producing this mullite, a mixed sol of alumina sol and silica sol is gelled and then calcined (sol-gel method), aluminum alkoxide and silicon alkoxide are mixed, hydrolyzed, dehydrated, dried and calcined. Method (alkoxide method), a method in which silica and alumina raw materials are melted by an electrolytic furnace and pulverized, and a dispersion liquid of alumina sol and silica sol is sprayed in an atmosphere having a flame temperature of 1000 to 1700 ° C., and the droplet diameter of the spray liquid is 150 μm. A method of obtaining a spherical powder by spraying and baking below (JP-A-5-10541)
No. 9).
【０００３】[0003]
【発明が解決しようとする課題】しかしながら、透明性
が良く平均粒子径が数１０ｎｍ位の極めて小さな球状の
非晶質ムライト系微粒子を効率よく得る方法は無かっ
た。そこで、本発明の目的は、上記の球状の非晶質ムラ
イト系微粒子を容易に製造し、この微粒子を電子写真用
トナーの外添剤や蛍光灯の内面コーティング用として提
供することにある。However, there has been no method for efficiently obtaining extremely small spherical amorphous mullite-based fine particles having good transparency and an average particle diameter of about several tens of nanometers. Accordingly, an object of the present invention is to easily produce the above-mentioned spherical amorphous mullite-based fine particles, and to provide the fine particles as an external additive for an electrophotographic toner or an inner surface coating of a fluorescent lamp.
【０００４】[0004]
【課題を解決するための手段】アルミニウム・ケイ素合
金としては、球状の非晶質ムライト系微粒子を構成する
酸化アルミニウムと酸化ケイ素の組成比が得られるよう
に合金の組成比を調製する。Means for Solving the Problems The composition ratio of the aluminum-silicon alloy is adjusted so that the composition ratio of aluminum oxide and silicon oxide constituting the spherical amorphous mullite fine particles can be obtained.
【０００５】上記のアルミニウム・ケイ素合金を直流ア
ークプラズマ法によって加熱、気化させ、その蒸気を酸
化、冷却し、平均粒子径が１０ｎｍ〜７０ｎｍである球
状の非晶質ムライト系微粒子を製造方法することができ
る。The above-mentioned aluminum / silicon alloy is heated and vaporized by a DC arc plasma method, and the vapor is oxidized and cooled to produce spherical amorphous mullite fine particles having an average particle diameter of 10 nm to 70 nm. Can be.
【０００６】上記によって製造された透明性の良好な平
均粒子径が１０ｎｍ〜７０ｎｍである球状の非晶質ムラ
イト系微粒子は、電子写真用トナーの外添剤、蛍光灯の
内面コーティング用、研磨剤などの用途に使用すること
ができる。外添剤に使用する場合、トリメチルクロルシ
ラン、ヘキサメチルジシラザンなどのシランカップリン
グ剤やシリコーンオイルで表面処理を施すのが好まし
い。コーティング用や研磨剤として使用する場合、水あ
るいは有機溶剤に分散させて使用することができる。分
散方法としては、超音波ミル、ディスクミル、ビーズミ
ルなどの粉砕機を用いて調製することができる。[0006] The spherical amorphous mullite fine particles having good transparency and an average particle diameter of 10 nm to 70 nm produced as described above are used as an external additive for toner for electrophotography, an inner coating for fluorescent lamps, and an abrasive. It can be used for such purposes. When used as an external additive, it is preferable to perform a surface treatment with a silane coupling agent such as trimethylchlorosilane or hexamethyldisilazane or silicone oil. When used as a coating or as an abrasive, they can be used after being dispersed in water or an organic solvent. The dispersing method can be prepared using a pulverizer such as an ultrasonic mill, a disc mill, and a bead mill.
【０００７】[0007]
【実施例】〔球状の非晶質ムライト系微粒子の製造〕製
造装置にアルミニウム７５モル％、ケイ素２５モル％か
らなるアルミニウム・ケイ素合金の長尺体を設置し、こ
れを消費アノード電極とし、カソード電極を中央に配し
たトーチを前記合金の長尺体の先端に向かう対向位置に
設け、トーチ内に供給されるアルゴンガスで酸化性雰囲
気からカソード電極を保護すると共に、上記の電極間に
電圧を印加してアーク放電させると、アルゴンガスのプ
ラズマフレームが発生し、前記合金を加熱、蒸発させ
る。その蒸気を酸化、冷却することにより、Ａｌ2 ０3
が７４重量％、ＳｉＯ2 が２６重量％の組成を持ち、平
均粒子径が３０ｎｍである球状のムライト系微粒子を製
造した。また、上記消費アノード電極であるアルミニウ
ム・ケイ素合金の長尺体の消費分を順次供給することに
より、連続して球状のムライト系微粒子の製造が可能で
ある。上記のムライト系微粒子の結晶形態を解析するた
め、Ｘ線回析法を用いて測定したところＸ線回析スペク
トルチャートに明確なピークが存在せず非晶質ムライト
系微粒子であることが分かった。[Example] [Production of spherical amorphous mullite-based fine particles] A long body of an aluminum-silicon alloy composed of 75 mol% of aluminum and 25 mol% of silicon was installed in a production apparatus, and this was used as a consumed anode electrode. A torch with an electrode disposed in the center is provided at a position facing the tip of the long body of the alloy, and the cathode electrode is protected from an oxidizing atmosphere by argon gas supplied into the torch, and a voltage is applied between the electrodes. When the arc discharge is applied, a plasma flame of argon gas is generated, and the alloy is heated and evaporated. By oxidizing and cooling the vapor, Al 2 O 3
Of 74% by weight and 26% by weight of SiO 2 , and spherical mullite fine particles having an average particle size of 30 nm were produced. Further, by sequentially supplying the consumption of the long body of the aluminum-silicon alloy as the above-mentioned consumed anode electrode, it is possible to continuously produce spherical mullite-based fine particles. In order to analyze the crystal morphology of the mullite-based fine particles described above, it was determined by using an X-ray diffraction method that there was no clear peak in the X-ray diffraction spectrum chart and the amorphous mullite-based fine particles were found. .
【０００８】〔トナーの製造〕磁性酸化鉄１００重量
部、ポリエステル樹脂（ガラス転移点Ｔｇ：６０℃）１
００重量部、ワックス（離形剤）３重量部および鉄アゾ
錯体（荷電制御材）１重量部からなるトナー組成物を溶
融混練し、冷却後、微粉砕し分級することにより平均粒
径１０μｍの磁性トナー原料を得た。この磁性トナー原
料に対し、ヘキサメチルシラザンで疎水化処理した上記
の球状の非晶質ムライト系微粒子１重量％を外添剤とし
て添加してヘンシェルミキサーで混合し、さらにハイブ
リダイザー（奈良機械製作所製）により、トナー表面に
固定化し磁性トナーを得た。従来のシリカ系の外添剤に
比べて、疎水化処理に使用したシランカップリング剤が
少量でも流動性が良好で、湿度環境の変化に対する安定
性も良好であった。[Production of Toner] 100 parts by weight of magnetic iron oxide, polyester resin (glass transition point Tg: 60 ° C.) 1
A toner composition comprising 00 parts by weight, 3 parts by weight of a wax (release agent) and 1 part by weight of an iron azo complex (charge control material) is melt-kneaded, cooled, pulverized and classified to obtain an average particle diameter of 10 μm. A magnetic toner raw material was obtained. To the magnetic toner raw material, 1% by weight of the above-mentioned spherical amorphous mullite-based fine particles hydrophobized with hexamethylsilazane was added as an external additive, mixed with a Henschel mixer, and further mixed with a hybridizer (manufactured by Nara Machinery Co., Ltd.). ) To obtain a magnetic toner fixed on the toner surface. Compared with a conventional silica-based external additive, even a small amount of the silane coupling agent used in the hydrophobizing treatment showed good fluidity and good stability against changes in the humidity environment.
【０００９】〔蛍光灯用スラリーの製造方法〕水に上記
の球状の非晶質ムライト系微粒子２０重量％を配合し、
超音波ミルによってスラリーを製造した。このスラリー
に必要に応じてポリビニルアルコールなどの増粘剤を添
加し、蛍光灯のガラスバルブの内面に塗布、乾燥、焼き
付けして被膜層を設けた。この被覆層はガラスバルブの
アルカリ成分の遮蔽効果があり、紫外線の反射性や可視
光線に対する透明性が良好なので蛍光灯の明るさや寿命
が改善されるという効果がある。[Method of Manufacturing Slurry for Fluorescent Lamp] 20% by weight of the above-mentioned spherical amorphous mullite fine particles are mixed with water,
The slurry was produced by an ultrasonic mill. If necessary, a thickener such as polyvinyl alcohol was added to the slurry, and the slurry was applied to the inner surface of a glass bulb of a fluorescent lamp, dried and baked to form a coating layer. This coating layer has an effect of shielding the alkali component of the glass bulb, and has an effect of improving the brightness and the life of the fluorescent lamp because of its good reflectivity of ultraviolet light and transparency to visible light.
【００１０】[0010]
【発明の効果】本発明の方法によれば、透明性の良好な
球状の非晶質ムライト系微粒子を効率よく工業的に製造
することができる。本発明の方法によって得られた透明
性の良好な球状の非晶質ムライト系微粒子は、着色剤含
有樹脂粒子を含有する電子写真用トナーの外添剤とし
て、或いは蛍光灯のガラスバルブと蛍光体層との間に形
成される金属酸化物被膜として利用される他、研磨材、
充填剤などに有用である。According to the method of the present invention, spherical amorphous mullite fine particles having good transparency can be efficiently and industrially produced. The spherical amorphous mullite-based fine particles having good transparency obtained by the method of the present invention can be used as an external additive for an electrophotographic toner containing colorant-containing resin particles, or a glass bulb of a fluorescent lamp and a phosphor. In addition to being used as a metal oxide film formed between layers, abrasives,
Useful for fillers and the like.
Claims (4)
2 が２０〜５０重量％の組成を持ち、平均粒子径が１０
ｎｍ〜７０ｎｍである球状の非晶質ムライト系微粒子。1. An Al 2 O 3 content of 50 to 80% by weight, SiO 2
2 has a composition of 20 to 50% by weight and an average particle size of 10
Spherical amorphous mullite-based fine particles having a diameter of from 70 nm to 70 nm.
プラズマ法によって加熱、気化させ、その蒸気を酸化、
冷却することを特徴とする請求項１記載の球状の非晶質
ムライト系微粒子の製造方法。2. An aluminum / silicon alloy is heated and vaporized by a DC arc plasma method, and the vapor is oxidized.
The method for producing spherical amorphous mullite-based fine particles according to claim 1, wherein cooling is performed.
用トナーの外添剤に用いられることを特徴とする請求項
１記載の球状の非晶質ムライト系微粒子。3. The spherical amorphous mullite-based fine particles according to claim 1, which is used as an external additive for an electrophotographic toner containing colorant-containing resin particles.
に形成される金属酸化物被膜層に用いられることを特徴
とする請求項１記載の球状の非晶質ムライト系微粒子。4. The spherical amorphous mullite-based fine particles according to claim 1, which is used for a metal oxide coating layer formed between a glass bulb of a fluorescent lamp and a phosphor layer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5125798A JPH11228123A (en) | 1998-02-18 | 1998-02-18 | Spherical amorphous mullite based fine particle and its production and its utilization |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5125798A JPH11228123A (en) | 1998-02-18 | 1998-02-18 | Spherical amorphous mullite based fine particle and its production and its utilization |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH11228123A true JPH11228123A (en) | 1999-08-24 |
Family
ID=12881905
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5125798A Pending JPH11228123A (en) | 1998-02-18 | 1998-02-18 | Spherical amorphous mullite based fine particle and its production and its utilization |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH11228123A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001139935A (en) * | 1999-11-12 | 2001-05-22 | Cheil Ind Co Ltd | Composition for polishing |
| JP2010249902A (en) * | 2009-04-13 | 2010-11-04 | Seiko Epson Corp | Toner, image forming method, and image forming apparatus |
| JP2010249909A (en) * | 2009-04-13 | 2010-11-04 | Seiko Epson Corp | Toner, method for manufacturing toner, and image forming apparatus using the same |
| WO2021124772A1 (en) * | 2019-12-20 | 2021-06-24 | Jsr株式会社 | Composition for chemical mechanical polishing, method for chemical mechanical polishing, and method for manufacturing chemical mechanical polishing particles |
-
1998
- 1998-02-18 JP JP5125798A patent/JPH11228123A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001139935A (en) * | 1999-11-12 | 2001-05-22 | Cheil Ind Co Ltd | Composition for polishing |
| KR20010046395A (en) * | 1999-11-12 | 2001-06-15 | 안복현 | Composition for cmp polishing |
| JP2010249902A (en) * | 2009-04-13 | 2010-11-04 | Seiko Epson Corp | Toner, image forming method, and image forming apparatus |
| JP2010249909A (en) * | 2009-04-13 | 2010-11-04 | Seiko Epson Corp | Toner, method for manufacturing toner, and image forming apparatus using the same |
| WO2021124772A1 (en) * | 2019-12-20 | 2021-06-24 | Jsr株式会社 | Composition for chemical mechanical polishing, method for chemical mechanical polishing, and method for manufacturing chemical mechanical polishing particles |
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