JPH02215105A - Manufacture of magnetic fluid - Google Patents
Manufacture of magnetic fluidInfo
- Publication number
- JPH02215105A JPH02215105A JP1037199A JP3719989A JPH02215105A JP H02215105 A JPH02215105 A JP H02215105A JP 1037199 A JP1037199 A JP 1037199A JP 3719989 A JP3719989 A JP 3719989A JP H02215105 A JPH02215105 A JP H02215105A
- Authority
- JP
- Japan
- Prior art keywords
- magnetic material
- magnetic fluid
- oxide
- oxide magnetic
- magnetic
- 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
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/44—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids
- H01F1/445—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids the magnetic component being a compound, e.g. Fe3O4
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Lubricants (AREA)
- Soft Magnetic Materials (AREA)
Abstract
Description
【発明の詳細な説明】 〔発明の目的] (産業上の利用分野) 本発明は、磁性流体の製造方法の改良に関する。[Detailed description of the invention] [Purpose of the invention] (Industrial application field) The present invention relates to an improvement in a method for producing magnetic fluid.
(従来の技術)
液相中にコロイドサイズの強磁性微粉末(微粒子)を安
定分散させて成る磁性流体は、たとえば、磁気シール、
スピーカーのダンピング特性の改善、有用資源回収のた
めの比重差選別への応用などとして実用に洪されている
。すなわち、磁性流体を利用した磁気シールは、零リー
ケージであること、固体間の摩擦がないので摩耗を生じ
ないこと、シャフトの表面仕上と寸法公差に余裕のある
こと、発熱がないことなどから半導体製造用の蒸着装置
などに使用されている。また、磁性流体に磁界を印加す
るとその中に磁気勾配を生じ、密度分布を生じたのと同
じ効果が得られる。したがって、この密度分布の中に非
磁性体をおくと磁界の低い方向に浮力が生じるのを利用
し、有用資源を比重差選別することなどが知られている
。(Prior art) A magnetic fluid made by stably dispersing colloid-sized ferromagnetic fine powder (fine particles) in a liquid phase can be used, for example, as a magnetic seal,
It has been put to practical use in applications such as improving the damping characteristics of speakers and sorting out differences in specific gravity to recover useful resources. In other words, magnetic seals using magnetic fluids have zero leakage, do not cause wear because there is no friction between solid objects, have sufficient shaft surface finish and dimensional tolerances, and do not generate heat, making them suitable for semiconductors. Used in manufacturing vapor deposition equipment, etc. Furthermore, when a magnetic field is applied to a magnetic fluid, a magnetic gradient is generated therein, producing the same effect as creating a density distribution. Therefore, it is known that when a non-magnetic material is placed in this density distribution, buoyancy is generated in the direction of a lower magnetic field, which is used to select useful resources based on their specific gravity.
しかして、前記磁性流体は、通常次のようにして製造さ
れている。先ずボールミルに所要の強磁性微粉末(微粒
子)たとえば、Pe304 。The magnetic fluid is usually manufactured in the following manner. First, the ferromagnetic fine powder (fine particles) required for the ball mill, such as Pe304.
(Mn−Zn) Po204 、 (Nl−Zn)
Fe204などの強磁性酸化物粉末や強磁性金属もしく
は合金粉末、分散溶媒たとえば、エステル炭化水素、フ
ッ化炭化水素油や水、および末端にカルボキシル基、ス
ルホン基、アミノ基、スルホコハク酸基などの極性基を
有する界面活性剤たとえば、オレイン酸ソーダなどを装
入して長時間混合、粉砕して安定な分散系を成す磁性流
体を得ている。(Mn-Zn) Po204, (Nl-Zn)
Ferromagnetic oxide powder such as Fe204, ferromagnetic metal or alloy powder, dispersion solvent such as ester hydrocarbon, fluorinated hydrocarbon oil or water, polarity such as carboxyl group, sulfone group, amino group, sulfosuccinic acid group at the end A magnetic fluid having a group-containing surfactant such as sodium oleate is charged and mixed and pulverized for a long period of time to form a stable dispersion system.
(発明が解決しようとする課題)
しかし、上記磁性流体の製造方法においては、次のよう
な不都合がある。すなわち、磁性流体の主要部を成す強
磁性粉末乃至微粒子の製造と、磁性流体の調製(製造)
とが別々の工程としてなされている。つまり、強磁性酸
化物粉末を予め製造しておくこと、前記製造し、用意(
貯蔵)しておいた強磁性酸化物粉末を所要の溶媒に分散
させるため、所要の界面活性剤を加えボールミルなどを
用い長時間攪拌混合することの不連続な2段階方式を採
っている。このため製造設備や製造操作面で繁雑さがあ
るばかりでなく、製造コストも割高になると言う間通が
ある。すなわち、前記強磁性酸化物粉末などは凝集し易
いため界面活性剤で処理しても分散性が悪く、安定な分
散系とするには比較的長時間の攪拌混合を要することに
なる。(Problems to be Solved by the Invention) However, the above method for producing magnetic fluid has the following disadvantages. That is, the production of ferromagnetic powder or fine particles that form the main part of the magnetic fluid, and the preparation (manufacturing) of the magnetic fluid.
and are done as separate processes. In other words, the ferromagnetic oxide powder must be manufactured in advance, and the ferromagnetic oxide powder must be manufactured and prepared (
In order to disperse the stored ferromagnetic oxide powder in the required solvent, a discontinuous two-step method is adopted in which the required surfactant is added and the mixture is stirred and mixed for a long time using a ball mill or the like. For this reason, there is a consensus that not only is the manufacturing equipment and manufacturing operations complicated, but the manufacturing costs are also relatively high. That is, since the ferromagnetic oxide powder and the like tend to aggregate, they have poor dispersibility even when treated with a surfactant, and a relatively long period of stirring and mixing is required to form a stable dispersion system.
本発明はこのような従来の事情に対処してなされたもの
で、容易にかつ、比較的低コストで所要の磁性流体を製
造しうる方法を提供することを目的とする。The present invention has been made in response to these conventional circumstances, and it is an object of the present invention to provide a method of manufacturing a required magnetic fluid easily and at relatively low cost.
[発明の構成]
(課題を解決するための手段)
本発明の磁性流体の製造方法は、酸化物磁性体の基本成
分およびガラス形成成分を含む原料混合物を加熱溶融さ
せた後、急冷して非晶質体とする工程と、この非晶質体
を形成される酸化物磁性体の結晶化温度より80℃高い
温度を超えない範囲で熱処理を施し酸化物磁性体の結晶
を析出させる工程と、この熱処理を施された焼結体を微
粉砕し、希酸によってガラス形成成分を溶解除去して酸
化物磁性体の結晶を洗い出す工程と、この洗い出した結
晶に界面活性剤を吸着させ乾燥後、油類と攪拌混合する
工程とを具備することを特徴とする。[Structure of the Invention] (Means for Solving the Problems) The method for producing a magnetic fluid of the present invention involves heating and melting a raw material mixture containing a basic component of an oxide magnetic material and a glass-forming component, and then rapidly cooling it to make it non-stick. a step of forming a crystalline body; a step of precipitating crystals of the oxide magnetic substance by heat-treating the amorphous body at a temperature not exceeding 80° C. higher than the crystallization temperature of the oxide magnetic substance to be formed; The heat-treated sintered body is finely pulverized, the glass-forming components are dissolved and removed with dilute acid, and the crystals of the oxide magnetic material are washed out. After drying, the washed out crystals are adsorbed with a surfactant. It is characterized by comprising a step of stirring and mixing with oil.
(作 用)
本発明の磁性流体の製造方法は、いわゆるガラス結晶化
法による強磁性粉末の製造に連続して、得られた強磁性
粉末の界面活性剤処理1分散用溶媒への攪拌1分散が行
われる。つまり、所要の強磁性粉末の製造および磁性流
体の調製(製造)が一連の操作として行われ、かつ強磁
性粉末は粉末乃至粒子が個々の状態で界面活性剤処理さ
れることにより、凝集した形を呈していないため、容易
に安定した分散系を形成し得るので、製造上の繁雑さや
コストの低減を容易に図り得る。(Function) The method for producing a magnetic fluid of the present invention involves the following steps: 1) treating the obtained ferromagnetic powder with a surfactant; 1) stirring in a dispersing solvent; will be held. In other words, the production of the required ferromagnetic powder and the preparation (manufacturing) of the magnetic fluid are performed as a series of operations, and the ferromagnetic powder is produced in an aggregated form by treating each individual powder or particle with a surfactant. Therefore, it is possible to easily form a stable dispersion system, thereby easily reducing manufacturing complexity and cost.
(実施例)
以下本発明の詳細な説明する。先ず酸化物に換算してZ
nO:15so1%、MnO:22*o1%、Fe2O
3:3g101%、B 203 :25101%となる
よう1こ、ZnO。(Example) The present invention will be described in detail below. First, in terms of oxide, Z
nO: 15so1%, MnO: 22*o1%, Fe2O
3: 3g 101%, B 203: 1 oz. ZnO so that the ratio is 25101%.
MnO,Fez O! 、)l s Bo3をそれぞ
れ所定量秤量し、これらを混合して原料成分を調製した
。MnO, Fez O! , )l s Bo3 were each weighed in predetermined amounts and mixed to prepare raw material components.
次いで、この混合物を白金ルツボに収容し、高周波誘導
加熱ヒータを用いて1400℃の温度で加熱溶融し、こ
の溶融物を水冷高速双ロール上で圧延急冷して40〜5
0μm厚のフレーク状の非晶質体を作成した。引き続き
、前記非晶質体を一定速度で昇温の後、750℃で5h
熱処理を行いフェライトの結晶を析出させた。しかる後
、この熱処理物をブラウンクラッシャーなどにより粉砕
し、さらにボールミルにより湿式粉砕を行った。次に、
得られた微粉末を加熱しながらかつ、超音波を加え酢酸
溶液にて処理してガラス形成物質のB2O3相を溶解除
去し、この酸処理後繰返して熱水により洗浄を施して、
Mn−Zn系微粒子(微粉末)スラリーを得た。上記に
よって得たMn−Zn系微粒子スラリーにオレイン酸ソ
ーダ水溶液を添加し、超音波を加えて前記Mn−Zn系
微粒子スラリーにオレイン酸ソーダを吸着させた。しか
る後、遠心分離機にかけ脱水し、乾燥させてから、これ
をケロシン(有機溶媒)に加えデイシルバー(攪拌機)
を用い攪拌を施して、Mn−Zn系微粒子が安定分散し
た磁性流体を得た。 なお、上記では、強磁性酸化物粉
末乃至微粒子として、Mn−Zn系フェライトを用いた
が、これに限られるものでなくたとえば−1Ni−Zn
系フェライト、Ba系フェライト、Pe203などであ
ってもよい。また、ガラス結晶化法で析出させた強磁性
酸化物粉末乃至微粒子に吸着させる界面活性剤も、オレ
イン酸ソーダに限られるものでなく磁性流体の製造に使
用されているものは、いずれも使用し得る。さらに、強
磁性酸化物粉末乃至微粒子を分散させる溶媒も、前記ケ
ロシンに限らず他の有機溶媒や水などであってもよい。Next, this mixture was placed in a platinum crucible, heated and melted at a temperature of 1400°C using a high-frequency induction heater, and this melt was rapidly cooled by rolling on water-cooled high-speed twin rolls to a temperature of 40 to 50°C.
A flaky amorphous material with a thickness of 0 μm was prepared. Subsequently, the temperature of the amorphous body was raised at a constant rate, and then heated at 750°C for 5 hours.
Heat treatment was performed to precipitate ferrite crystals. Thereafter, this heat-treated product was pulverized using a brown crusher or the like, and further subjected to wet pulverization using a ball mill. next,
While heating the obtained fine powder, applying ultrasonic waves and treating it with an acetic acid solution to dissolve and remove the B2O3 phase of the glass-forming substance, and after this acid treatment, the powder was repeatedly washed with hot water,
A slurry of Mn-Zn based fine particles (fine powder) was obtained. An aqueous solution of sodium oleate was added to the Mn--Zn-based fine particle slurry obtained above, and ultrasonic waves were applied to cause the sodium oleate to be adsorbed onto the Mn--Zn-based fine particle slurry. After that, it is dehydrated by centrifugation, dried, and then added to kerosene (organic solvent) and Daysilver (stirrer).
A magnetic fluid in which Mn--Zn-based fine particles were stably dispersed was obtained by stirring. In the above, Mn-Zn ferrite was used as the ferromagnetic oxide powder or fine particles, but it is not limited to this, and for example -1Ni-Zn
It may be a Ba-based ferrite, a Ba-based ferrite, Pe203, or the like. Furthermore, the surfactant to be adsorbed to the ferromagnetic oxide powder or fine particles precipitated by the glass crystallization method is not limited to sodium oleate, but any surfactant used in the production of magnetic fluids may be used. obtain. Furthermore, the solvent in which the ferromagnetic oxide powder or fine particles are dispersed is not limited to the above-mentioned kerosene, but may be other organic solvents, water, or the like.
つまり、調製した磁性流体の用途(使用目的)などによ
り、強磁性粉末、界面活性剤8分散溶媒などは適宜選択
することができる。In other words, the ferromagnetic powder, surfactant 8 dispersion solvent, etc. can be appropriately selected depending on the intended use of the prepared magnetic fluid.
本発明方法において、急速冷却で得た非晶質体の熱処理
を、得られる強磁性酸化物粉末乃至微粒子の結晶化温度
よりも80℃を超えない温度範囲としたのは、これより
高温になると結晶化が進み、所要の強磁性酸化物粉末乃
至微粒子が得難くなるからである。In the method of the present invention, the heat treatment of the amorphous material obtained by rapid cooling is performed within a temperature range that does not exceed 80°C than the crystallization temperature of the resulting ferromagnetic oxide powder or fine particles. This is because crystallization progresses, making it difficult to obtain the required ferromagnetic oxide powder or fine particles.
[発明の効果]
上記本発明方法によれば、ガラス結晶化法による強磁性
酸化物粉末の製造過程で、つまり、非晶質体の粉砕、酸
処理、得られた強磁性粉末の水洗に引き続いて界面活性
剤処理が施される。かくして強磁性酸化物粉末表面には
前記界面活性剤が吸着保持されているため、強磁性酸化
物粉末(粒子)間の凝集は全面的に抑制もしくは防止さ
れる。したがって、この強磁性酸化物粉末(粒子)を分
散溶媒に、分散させて所要の磁性流体を調製する過程で
も容易に均一な分散系を形成し得る。すなわち、比較的
短時間の混合攪拌操作で安定した分散系を成す磁性流体
が容易に得られる。かくして本発明は製造操作などが簡
易で、混合攪拌操作も短時間で足り比較的低コストで製
造し得ることから、実用的な製造方法と言える。[Effects of the Invention] According to the method of the present invention, in the process of producing ferromagnetic oxide powder by the glass crystallization method, that is, after crushing the amorphous material, acid treatment, and washing the obtained ferromagnetic powder with water, Then, a surfactant treatment is performed. Since the surfactant is adsorbed and retained on the surface of the ferromagnetic oxide powder, aggregation between the ferromagnetic oxide powders (particles) is completely suppressed or prevented. Therefore, even in the process of preparing a desired magnetic fluid by dispersing this ferromagnetic oxide powder (particles) in a dispersion solvent, a uniform dispersion system can be easily formed. That is, a magnetic fluid forming a stable dispersion system can be easily obtained by a relatively short mixing and stirring operation. Thus, the present invention can be said to be a practical manufacturing method because the manufacturing operations are simple, the mixing and stirring operations can be performed in a short time, and the manufacturing process can be performed at relatively low cost.
出願人 東芝硝子株式会社 代理人 弁理士 須 山 佐 − (ばか1名)Applicant: Toshiba Glass Corporation Agent Patent Attorney Suyama Sa (1 idiot)
Claims (1)
原料混合物を加熱溶融させた後、急冷して非晶質体とす
る工程と、 この非晶質体を形成される酸化物磁性体の結晶化温度よ
り80℃高い温度を超えない範囲で熱処理を施し酸化物
磁性体の結晶を析出させる工程と、この熱処理を施され
た焼結体を微粉砕し、希酸によってガラス形成成分を溶
解除去して酸化物磁性体の結晶を洗い出す工程と、 この洗い出した結晶に界面活性剤を吸着させ乾燥後、分
散溶媒と攪拌混合する工程とを具備することを特徴とす
る磁性流体の製造方法。[Claims] A step of heating and melting a raw material mixture containing a basic component of an oxide magnetic material and a glass-forming component and then rapidly cooling it to form an amorphous body; A step of precipitating crystals of the oxide magnetic material by heat treatment at a temperature not exceeding 80°C higher than the crystallization temperature of the oxide magnetic material, and a step of finely pulverizing the heat-treated sintered body and pulverizing it with dilute acid. A magnetic material characterized by comprising a step of dissolving and removing glass-forming components and washing out crystals of the oxide magnetic material, and a step of adsorbing a surfactant to the washed out crystals, drying them, and then stirring and mixing them with a dispersion solvent. Fluid manufacturing method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1037199A JPH02215105A (en) | 1989-02-15 | 1989-02-15 | Manufacture of magnetic fluid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1037199A JPH02215105A (en) | 1989-02-15 | 1989-02-15 | Manufacture of magnetic fluid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH02215105A true JPH02215105A (en) | 1990-08-28 |
Family
ID=12490907
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1037199A Pending JPH02215105A (en) | 1989-02-15 | 1989-02-15 | Manufacture of magnetic fluid |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02215105A (en) |
-
1989
- 1989-02-15 JP JP1037199A patent/JPH02215105A/en active Pending
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