JPH11279537A - Aqueous dispersion of cerium oxide ultramicroparticle and its production - Google Patents
Aqueous dispersion of cerium oxide ultramicroparticle and its productionInfo
- Publication number
- JPH11279537A JPH11279537A JP10095158A JP9515898A JPH11279537A JP H11279537 A JPH11279537 A JP H11279537A JP 10095158 A JP10095158 A JP 10095158A JP 9515898 A JP9515898 A JP 9515898A JP H11279537 A JPH11279537 A JP H11279537A
- Authority
- JP
- Japan
- Prior art keywords
- cerium oxide
- aqueous dispersion
- weight
- cerium
- particles
- 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
Landscapes
- Surface Treatment Of Glass (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、研磨材として有用な酸
化セリウム超微粒子水分散体およびその製造方法に関す
る。The present invention relates to an aqueous dispersion of cerium oxide ultrafine particles useful as an abrasive and a method for producing the same.
【０００２】[0002]
【従来技術】酸化セリウム微粒子は、一般にガラスの研
磨材として用いられている。従来の酸化セリウム微粒子
からなる研磨材は、セリウムの水酸化物や炭酸塩を焼
成、粉砕、分級して製造されている。しかしながら、こ
のような製法による酸化セリウム微粒子は、５重量％水
分散体のＰＨが６程度であり、一般的に１μｍ前後の平
均粒径を有し、平均粒径が３００ｎｍ程度のものが最小
で、水分散体とした場合、高価な分散剤などを使用し
て、凝集や沈降を防いでいた。2. Description of the Related Art Cerium oxide fine particles are generally used as a polishing material for glass. Conventional abrasives comprising cerium oxide fine particles are produced by firing, pulverizing, and classifying cerium hydroxide or carbonate. However, cerium oxide fine particles produced by such a method have a pH of about 6 of a 5% by weight aqueous dispersion, generally have an average particle size of about 1 μm, and a particle having an average particle size of about 300 nm is the minimum. When an aqueous dispersion is used, an expensive dispersant or the like is used to prevent aggregation and sedimentation.
【０００３】最近、光学レンズやガラス製ハードディス
ク基板などで超精密研磨に使用する平均粒径がより小さ
な酸化セリウム超微粒子を使用し、酸性領域で安定な水
分散体が求められていた。Recently, there has been a demand for an aqueous dispersion that is stable in an acidic region by using ultrafine cerium oxide particles having a smaller average particle size for use in ultra-precision polishing of optical lenses and glass hard disk substrates.
【０００４】[0004]
【発明が解決しようとする課題】本発明は、分散剤を使
用しなくても安定で、極めて容易に製造できる酸化セリ
ウム超微粒子水分散体を提供することにある。SUMMARY OF THE INVENTION An object of the present invention is to provide an aqueous dispersion of ultrafine cerium oxide particles which is stable without using a dispersant and can be produced very easily.
【０００５】[0005]
【課題を解決するための手段】本発明は、 １．５重量％水分散体のＰＨが４．２〜５．３の範囲で
あり平均粒子径が５〜７０ｎｍ、好ましくは８〜３０ｎ
ｍの範囲である酸化セリウム超微粒子と、分散媒として
の水からなる酸化セリウム超微粒子水分散体。 ２．酸化セリウム超微粒子の含有量が１〜２５重量％、
好ましくは１０〜２０重量％であることを特徴とする請
求項１記載の酸化セリウム超微粒子水分散体。 ３．セリウム原料を直流アークプラズマ法によって加
熱、気化させ、そのセリウム蒸気を酸化、冷却すること
により、５重量％水分散体のＰＨが４．２〜５．３の範
囲であり平均粒子径が５〜７０ｎｍの範囲である酸化セ
リウム超微粒子を製造する工程と、分散媒としての水に
上記酸化セリウム超微粒子を分散させる工程と、からな
ることを特徴とする酸化セリウム超微粒子水分散体の製
造方法。 ４．酸化セリウム超微粒子の含有量が１〜２５重量％、
好ましくは１０〜２２重量％であることを特徴とする請
求項３記載の酸化セリウム超微粒子水分散体の製造方
法。にある。According to the present invention, a 1.5% by weight aqueous dispersion has a pH of 4.2 to 5.3 and an average particle diameter of 5 to 70 nm, preferably 8 to 30 n.
A cerium oxide ultrafine particle aqueous dispersion comprising cerium oxide ultrafine particles having a range of m and water as a dispersion medium. 2. The content of cerium oxide ultrafine particles is 1 to 25% by weight,
The cerium oxide ultrafine particle aqueous dispersion according to claim 1, wherein the content is preferably 10 to 20% by weight. 3. The cerium raw material is heated and vaporized by the direct current arc plasma method, and the cerium vapor is oxidized and cooled, whereby the pH of the 5% by weight aqueous dispersion is in the range of 4.2 to 5.3 and the average particle diameter is 5 to 5. A method for producing a cerium oxide ultrafine particle aqueous dispersion, comprising: a step of producing cerium oxide ultrafine particles having a diameter of 70 nm; and a step of dispersing the cerium oxide ultrafine particles in water as a dispersion medium. 4. The content of cerium oxide ultrafine particles is 1 to 25% by weight,
The method for producing a cerium oxide ultrafine particle aqueous dispersion according to claim 3, wherein the content is preferably 10 to 22% by weight. It is in.
【０００６】本発明において使用する酸化セリウム超微
粒子は、直流プラズマアーク法、プラズマジェット法、
高周波プラズマ法などのプラズマ法で製造できるが、直
流プラズマアーク法が生産性などの点から最も好まし
い。このプラズマ法で製造した酸化セリウム超微粒子の
水分散体が、高価な分散剤を用いなくても容易に製造で
きる理由は不明であるが、表面活性が強く酸化セリムウ
超微粒子が水に分散した時に、その表面に水酸基が吸着
され、その電荷によって凝集が妨げられるものと考えら
れる。The cerium oxide ultrafine particles used in the present invention can be obtained by a direct current plasma arc method, a plasma jet method,
Although it can be manufactured by a plasma method such as a high-frequency plasma method, a DC plasma arc method is most preferable in terms of productivity and the like. It is unknown why the aqueous dispersion of cerium oxide ultrafine particles produced by this plasma method can be easily produced without using an expensive dispersant, but the surface activity is strong when the cerium oxide ultrafine particles are dispersed in water. It is considered that a hydroxyl group is adsorbed on the surface, and the charge prevents the aggregation.
【０００７】本発明において使用する直流プラズマアー
ク法は、金属セリウム等のセリウム原料を消費アノード
電極とし、カソード電極からアルゴンガスのプラズマフ
レームを発生させ、前記セリウム原料を加熱、蒸発さ
せ、その金属セリウム蒸気を酸化、冷却するものであ
り、平均粒子径が５〜７０ｎｍの範囲である酸化セリウ
ム超微粒子を製造することができる。平均粒子径が５ｎ
ｍ未満のものは製造の効率が悪くなり、平均粒子径が７
０ｎｍを超えるものは粗大粒子が生成する可能性が大き
くなるので好ましくない。なお、平均粒子径の測定は、
比表面積法によって算出した。In the DC plasma arc method used in the present invention, a cerium raw material such as cerium metal is used as a consumed anode electrode, a plasma flame of argon gas is generated from a cathode electrode, and the cerium raw material is heated and evaporated, and the cerium raw material is evaporated. It oxidizes and cools the vapor, and can produce ultrafine cerium oxide particles having an average particle diameter in the range of 5 to 70 nm. Average particle size is 5n
If the average particle diameter is less than 7 m, the production efficiency becomes poor.
Those having a thickness exceeding 0 nm are not preferred because the possibility of formation of coarse particles increases. In addition, the measurement of the average particle diameter is as follows.
It was calculated by the specific surface area method.
【０００８】次に、本発明の酸化セリウム超微粒子水分
散体の製造方法について述べる。本発明の酸化セリウム
超微粒子水分散体は、上記によって製造された酸化セリ
ウム超微粒子を、分散媒としての水に加え、種々の方法
によって分散させることによって得られる。分散方法と
しては、超音波ミル、サンドミル、ディスクミル等の粉
砕機を用いて調整することができる。水分散体の酸化セ
リウムの含有量は１〜２５重量％、好ましくは１０〜２
２重量％である。２５重量％を超えると分散時に粘度が
高くなり研磨用としては好ましくなく、１重量％以下だ
と濃度当たりの処理コストが高くなり好ましくない。ま
た、使用する用途に応じて水分散体の濃度を薄めて使用
することも可能である。Next, a method for producing the cerium oxide ultrafine particle aqueous dispersion of the present invention will be described. The aqueous dispersion of cerium oxide ultrafine particles of the present invention is obtained by adding the cerium oxide ultrafine particles produced as described above to water as a dispersion medium and dispersing the same by various methods. The dispersion method can be adjusted using a pulverizer such as an ultrasonic mill, a sand mill, and a disk mill. The content of cerium oxide in the aqueous dispersion is 1 to 25% by weight, preferably 10 to 2%.
2% by weight. If it exceeds 25% by weight, the viscosity at the time of dispersion increases, which is not preferable for polishing. If it is 1% by weight or less, the processing cost per concentration becomes undesirably high. Further, it is also possible to use the aqueous dispersion at a reduced concentration according to the intended use.
【０００９】[0009]
【実施例】製造装置に原料としての金属セリウムの棒状
物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金属セリウムの棒状物の先
端に対向位置に設ける。トーチ内にアルゴンガスを供給
することによりカソード電極を酸化性雰囲気から保護す
ると共に、上記電極間に電圧を印加しアーク放電させる
と、アルゴンガスのプラズマフレームが発生し、発生し
たプラズマフレームにより金属セリウムを加熱、蒸発さ
せる。その蒸気を酸化、冷却することにより球状及び角
形状の混ざった平均粒径が２０ｎｍの酸化セリウム超微
粒子を製造した。この酸化セリウム超微粒子をイオン交
換水に５重量％入れ超音波ミルで処理して得られた水分
散体のＰＨは、４．２であった。一方、純水に酸化セリ
ウム超微粒子を２０重量％入れ、超音波ミルで１時間処
理し、上澄部分を分取した。この分取した水分散体は、
酸化セリウム含有量が約１８重量％であり、放置しても
凝集や沈殿が殆どなかった。なお、純水を適宜補充し少
し撹拌処理することにより酸化セリウム含有量の異なる
各種水分散体を得ることができた。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS A rod made of cerium metal as a raw material is installed in a manufacturing apparatus, and this rod is used as a consumed anode electrode. The cathode electrode is protected from the oxidizing atmosphere by supplying argon gas into the torch, and when a voltage is applied between the electrodes to cause arc discharge, a plasma frame of argon gas is generated. Is heated and evaporated. The vapor was oxidized and cooled to produce ultrafine cerium oxide particles having an average particle diameter of 20 nm in which spherical and angular shapes were mixed. The pH of the aqueous dispersion obtained by adding 5% by weight of the cerium oxide ultrafine particles to ion-exchanged water and treating with an ultrasonic mill was 4.2. Separately, 20% by weight of ultrafine cerium oxide particles were added to pure water, and the mixture was treated with an ultrasonic mill for 1 hour, and the supernatant was collected. This separated aqueous dispersion is
The cerium oxide content was about 18% by weight, and there was almost no agglomeration or precipitation even after standing. In addition, various water dispersions having different cerium oxide contents could be obtained by appropriately supplementing pure water and performing a little stirring treatment.
【００１０】[0010]
【発明の効果】本発明によれば、凝集や沈殿が殆どない
酸化セリウム超微粒子の水分散体を効率よく製造でき、
水を補充することによって使用濃度の水分散体を簡単に
作ることができる。本発明の酸化セリウム超微粒子は、
表面活性が強く、分散剤を用いなくても容易に水分散体
を得ることができる。According to the present invention, it is possible to efficiently produce an aqueous dispersion of cerium oxide ultrafine particles with little aggregation or precipitation,
By replenishing the water, an aqueous dispersion of the working concentration can be easily made. Cerium oxide ultrafine particles of the present invention,
The surface activity is strong, and an aqueous dispersion can be easily obtained without using a dispersant.
Claims (4)
３の範囲であり平均粒子径が５〜７０ｎｍの範囲である
酸化セリウム超微粒子と、分散媒としての水からなる酸
化セリウム超微粒子水分散体。1. A 5% by weight aqueous dispersion having a pH of 4.2 to 5.
3. A cerium oxide ultrafine particle aqueous dispersion comprising cerium oxide ultrafine particles having a range of 3 and an average particle diameter of 5 to 70 nm, and water as a dispersion medium.
５重量％、好ましくは１０〜２２重量％であることを特
徴とする請求項１記載の酸化セリウム超微粒子水分散
体。2. The content of ultrafine cerium oxide particles is 1 to 2
The cerium oxide ultrafine particle aqueous dispersion according to claim 1, wherein the aqueous dispersion is 5% by weight, preferably 10 to 22% by weight.
よって加熱、気化させ、そのセリウム蒸気を酸化、冷却
することにより、５重量％水分散体のＰＨが４．２〜
５．３の範囲であり平均粒子径が５〜７０ｎｍの範囲で
ある酸化セリウム超微粒子を製造する工程と、 分散媒としての水に上記酸化セリウム超微粒子を分散さ
せる工程と、 からなることを特徴とする酸化セリウム超微粒子水分散
体の製造方法。3. The cerium raw material is heated and vaporized by a direct current arc plasma method, and the cerium vapor is oxidized and cooled, whereby the pH of the 5% by weight aqueous dispersion is 4.2 to 4.2.
A step of producing cerium oxide ultrafine particles having a range of 5.3 and an average particle diameter of 5 to 70 nm, and a step of dispersing the cerium oxide ultrafine particles in water as a dispersion medium. For producing an aqueous dispersion of ultrafine cerium oxide particles.
５重量％、好ましくは１０〜２２重量％であることを特
徴とする請求項３記載の酸化セリウム超微粒子水分散体
の製造方法。4. The content of ultrafine cerium oxide particles is 1 to 2
The method for producing a cerium oxide ultrafine particle aqueous dispersion according to claim 3, wherein the amount is 5% by weight, preferably 10 to 22% by weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10095158A JPH11279537A (en) | 1998-03-25 | 1998-03-25 | Aqueous dispersion of cerium oxide ultramicroparticle and its production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10095158A JPH11279537A (en) | 1998-03-25 | 1998-03-25 | Aqueous dispersion of cerium oxide ultramicroparticle and its production |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH11279537A true JPH11279537A (en) | 1999-10-12 |
Family
ID=14129985
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10095158A Pending JPH11279537A (en) | 1998-03-25 | 1998-03-25 | Aqueous dispersion of cerium oxide ultramicroparticle and its production |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH11279537A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007100093A1 (en) * | 2006-03-03 | 2007-09-07 | Hitachi Chemical Co., Ltd. | Metal oxide particle, polishing material containing same, substrate polishing method using such polishing material, and method for manufacturing semiconductor device |
| JP2011051851A (en) * | 2009-09-03 | 2011-03-17 | Hitachi Chem Co Ltd | Rare earth fluoride fine particle dispersion, method for producing the dispersion, method for producing rare earth fluoride thin film using the dispersion, method for producing polymer compound/rare earth fluoride composite film using the dispersion, and rare earth sintered magnet using the dispersion |
-
1998
- 1998-03-25 JP JP10095158A patent/JPH11279537A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007100093A1 (en) * | 2006-03-03 | 2007-09-07 | Hitachi Chemical Co., Ltd. | Metal oxide particle, polishing material containing same, substrate polishing method using such polishing material, and method for manufacturing semiconductor device |
| JP2011051851A (en) * | 2009-09-03 | 2011-03-17 | Hitachi Chem Co Ltd | Rare earth fluoride fine particle dispersion, method for producing the dispersion, method for producing rare earth fluoride thin film using the dispersion, method for producing polymer compound/rare earth fluoride composite film using the dispersion, and rare earth sintered magnet using the dispersion |
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