JP4684549B2 - Ferrite coated particulate manufacturing equipment - Google Patents
Ferrite coated particulate manufacturing equipment Download PDFInfo
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- JP4684549B2 JP4684549B2 JP2003411218A JP2003411218A JP4684549B2 JP 4684549 B2 JP4684549 B2 JP 4684549B2 JP 2003411218 A JP2003411218 A JP 2003411218A JP 2003411218 A JP2003411218 A JP 2003411218A JP 4684549 B2 JP4684549 B2 JP 4684549B2
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- 229910000859 α-Fe Inorganic materials 0.000 title claims description 69
- 238000004519 manufacturing process Methods 0.000 title claims description 18
- 239000013618 particulate matter Substances 0.000 claims description 37
- 238000006243 chemical reaction Methods 0.000 claims description 31
- 230000001590 oxidative effect Effects 0.000 claims description 28
- 238000007747 plating Methods 0.000 claims description 26
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 14
- 229910001448 ferrous ion Inorganic materials 0.000 claims description 14
- 239000007800 oxidant agent Substances 0.000 claims description 14
- 239000011236 particulate material Substances 0.000 claims description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 13
- 239000001301 oxygen Substances 0.000 claims description 13
- 229910052760 oxygen Inorganic materials 0.000 claims description 13
- 238000000576 coating method Methods 0.000 claims description 9
- 239000011248 coating agent Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 230000003647 oxidation Effects 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 3
- 239000000243 solution Substances 0.000 description 37
- 239000002245 particle Substances 0.000 description 26
- 101100298222 Caenorhabditis elegans pot-1 gene Proteins 0.000 description 12
- 238000000034 method Methods 0.000 description 10
- 239000000758 substrate Substances 0.000 description 9
- 239000000843 powder Substances 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 239000007864 aqueous solution Substances 0.000 description 5
- 239000012295 chemical reaction liquid Substances 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229920002678 cellulose Polymers 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910000000 metal hydroxide Inorganic materials 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000012860 organic pigment Substances 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920001059 synthetic polymer Polymers 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- -1 metal hydroxide ions Chemical class 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
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Description
本発明は、粒子状物に対するフェライト被覆方法及びそのためのフェライト製造装置とに関する。 The present invention relates to a ferrite coating method for particulate matter and a ferrite manufacturing apparatus therefor.
基体表面にフェライト膜を形成する方法としては、フェライト粒子状物とバインダとを混合した組成物を塗布する方法、またはスパッタ等の物理的な付着による方法等の種々の方法が提案されている。 As a method for forming a ferrite film on the surface of a substrate, various methods such as a method of applying a composition in which ferrite particulates and a binder are mixed, or a method of physical adhesion such as sputtering have been proposed.
これに対し、近年基体表面にフェライトの結晶を成長させる方法（以下、フェライトメッキ法）が提案された。 On the other hand, in recent years, a method of growing ferrite crystals on the substrate surface (hereinafter referred to as a ferrite plating method) has been proposed.
フェライトメッキとは、例えば、特許文献１に示されているように、固体表面に、金属イオンとして少なくとも第１鉄イオンを含む水溶液を接触させ、固体表面にＦｅ２＋またはこれと他の水酸化金属イオンを吸着させ、続いて吸着したＦｅ２＋を酸化させることにより、Ｆｅ３＋を得、これが水溶液中の水酸化金属イオンとの間でフェライト結晶化反応を起こし、これによって固体表面にフェライト膜を形成することをいう。 For example, as disclosed in Patent Document 1, ferrite plating is a method in which an aqueous solution containing at least ferrous ions as metal ions is brought into contact with a solid surface, and Fe 2+ or this and other metal hydroxides are brought into contact with the solid surface. Ions are adsorbed, and then the adsorbed Fe 2+ is oxidized to obtain Fe 3+ , which causes a ferrite crystallization reaction with metal hydroxide ions in an aqueous solution, thereby forming a ferrite film on the solid surface. To do.
フェライトメッキは、膜を形成しようとする固体が前述した水溶液に対して耐性があれは何でも良い。更に、水溶液を介した反応であるため、温度が比較的低温（常温〜水溶液の沸点以下）でスピネル型フェライト膜を形成できるという特徴がある。そのため、他のフェライト膜作製技術に比べて、固体の限定範囲が小さい。 The ferrite plating may be anything as long as the solid to form a film is resistant to the aqueous solution described above. Further, since the reaction is via an aqueous solution, the spinel ferrite film can be formed at a relatively low temperature (normal temperature to the boiling point of the aqueous solution). Therefore, the limited range of solids is small compared to other ferrite film manufacturing techniques.
また、特許文献２には、前述のフェライトメッキ膜を粒子状物に応用する提案がなされている。特許文献２によれば、金属イオンとして少なくとも第１鉄イオンと粒子状物を含む脱酸素溶液に酸化剤溶液を添加して、粒子状物表面にフェライト膜を生成することが提案されている。 Patent Document 2 proposes to apply the above-described ferrite plating film to a particulate material. According to Patent Document 2, it is proposed that an oxidant solution is added to a deoxygenated solution containing at least ferrous ions and particulate matter as metal ions to form a ferrite film on the particulate matter surface.
しがし、特許文献２において、粒子状物のフェライト被覆は単一の反応容器中で行われており、単一時間に多量の粒子状物をフェライト被覆することには問題がある。 However, in Patent Document 2, the ferrite coating of the particulate matter is performed in a single reaction vessel, and there is a problem in coating a large amount of the particulate matter in a single time.
フェライト被覆した粒子状物は、例えば、樹脂、金属、金属酸化物、有機顔料、セルロース、合成高分子材料、セラミックス等々種々考えられるが、量産化を考慮した場合には単一時間に多量の粒子物を効率良くフェライト被覆する必要がある。 There are various types of ferrite-coated particulate materials, such as resins, metals, metal oxides, organic pigments, cellulose, synthetic polymer materials, ceramics, etc., but considering mass production, a large amount of particles can be obtained in a single time. It is necessary to efficiently coat the object with ferrite.
更に、単一時間に多量のフェライト被覆粒子状物を得ようとした場合、粒子状物に対する均一なフェライト被覆膜を得るためには、少なくとも第一鉄イオンを含む反応液、少なくとも酸化剤もしくは少なくとも酸素を含んだ酸化媒体、及び粒子状物を効率よく撹伴しなければならない。
そこで、本発明の技術的課題は、粒子状物に対するフェライト被覆において、かかる従来の欠点を解消して、工業的な生産性を増し、均一に被覆されたフェライト被覆粒子物の製造装置を提供することにある。 Therefore, the technical problem of the present invention is to provide a manufacturing apparatus for uniformly coated ferrite-coated particles, which eliminates the conventional drawbacks in ferrite coating on particulates, increases industrial productivity. There is.
本発明者等は、種々検討の結果、少なくとも第一鉄イオンを含む反応液、少なくとも酸化剤、もしくは少なくとも酸素を含んだ酸化媒体を基体に接触させる機構、フェライト層で被覆される粒子状物が装置内部に連続しで供給、回収される機構、及び少なくとも第一鉄イオンを含む反応液、少なくとも酸化剤、もしくは少なくとも酸素を含んだ酸化媒体、及び粒子状物が超音波により攪拌される機構を備えたフェライト被覆粒子状物の製造装置によって、フェライト被覆粒子状物の工業的な生産性が向上し、また粒子状物がフェライトによって均一に被覆可能であることを見出した。 As a result of various studies, the present inventors have found that a reaction solution containing at least ferrous ions, a mechanism for bringing an oxidizing medium containing at least an oxidizing agent or at least oxygen into contact with a substrate, and a particulate matter coated with a ferrite layer A mechanism for continuously supplying and recovering the inside of the apparatus, and a mechanism for stirring the reaction liquid containing at least ferrous ions, the oxidizing medium containing at least an oxidizing agent, or at least oxygen, and the particulate matter by ultrasonic waves. It was found that the industrial productivity of the ferrite-coated particulate matter was improved by the ferrite-coated particulate production apparatus provided, and that the particulate matter could be uniformly coated with ferrite.
即ち、本発明によれば、粒子状物を供給し、前記粒子状物の表面をフェライトめっき膜で被覆し、表面が前記フェライトめっき膜で被覆された粒子状物を回収するこれらの操作を連続的に行うフェライト被覆粒子状物の製造装置であって、前記製造装置は少なくとも第一鉄イオンを含む反応液、少なくとも酸化剤もしくは少なくとも酸素を含んだ酸化媒体を流下、噴霧、もしくは液滴の滴下によって前記反応液及び前記酸化媒体を前記粒子状物に接触させて当該粒子状物と直接反応させて、前記粒子状物の表面をフェライトめっき膜で被覆する機構と、前記反応液、前記酸化媒体、及び粒子状物を超音波により攪拌し、前記粒子状物の表面を均一にフェライトめっき膜で被覆するための攪拌手段とを備えることを特徴とするフェライト被覆粒子状物の製造装置が得られる。 That is, according to the present invention, these operations of supplying particulate matter, covering the surface of the particulate matter with a ferrite plating film, and recovering the particulate matter whose surface is covered with the ferrite plating film are continuously performed. an apparatus for producing a manner performing ferrite-coated particulates, the reaction solution producing apparatus comprising at least ferrous ions, flowing down the oxidizing medium containing at least an oxidant or at least oxygen, spraying or dripping of droplets, wherein the reaction solution and the oxidizing medium is contacted with said particulate material is reacted directly with the particulate material by a mechanism for coating the surface of the particulate matter in the ferrite plating film, the reaction solution, the oxidizing medium , and particulate was stirred by ultrasonic, ferrite coated particles, wherein the obtaining Bei and stirring means for coating with uniform ferrite-plated film surface of the particulate material Jo of manufacturing device can be obtained.
本発明によれば、少なくとも第一鉄イオンを含む反応液、少なくとも酸化剤、もしくは少なくとも酸素を含んだ酸化媒体を基体に接触させる機構、及びフェライト層で被覆される粒子状物が装置内部に連続しで供給、回収される機構を備えることによって、工業的な生産性を向上したフェライト被覆粒子状物の製造装置が得られる。 According to the present invention, a reaction solution containing at least ferrous ions, a mechanism for bringing an oxidizing medium containing at least an oxidizing agent or at least oxygen into contact with a substrate, and particulate matter coated with a ferrite layer are continuously provided inside the apparatus. By providing the mechanism that is supplied and recovered, an apparatus for producing a ferrite-coated particulate matter with improved industrial productivity can be obtained.
また、本発明によれば、少なくとも第一鉄イオンを含む反応液、少なくとも酸化剤、もしくは少なくとも酸素を含んだ酸化媒体を基体に接触させる機構、フェライト層で被覆される粒子状物が装置内部に連続しで供給、回収される機構、及び少なくとも第一鉄イオンを含む反応液、少なくとも酸化剤、もしくは少なくとも酸素を含んだ酸化媒体及び粒子状物が超音波により攪拌される機構を備えたフェライト被覆粒子状物の製造装置によって、表面がフェライトで均一に覆われたフェライト被覆粒子状物が得られる。以上により、本発明の工業的な利用価値は大である。 Further, according to the present invention, the reaction solution containing at least ferrous ions, the mechanism for contacting at least the oxidizing agent or the oxidizing medium containing at least oxygen with the substrate, and the particulate matter coated with the ferrite layer are placed inside the apparatus. Ferrite coating with a mechanism that continuously supplies and recovers, and a mechanism in which a reaction solution containing at least ferrous ions, at least an oxidizing agent, or an oxidizing medium containing at least oxygen and particulate matter are agitated by ultrasonic waves. By the particulate material manufacturing apparatus, a ferrite-coated particulate material whose surface is uniformly covered with ferrite is obtained. As described above, the industrial utility value of the present invention is great.
まず、本発明を更に詳しく説明する。 First, the present invention will be described in more detail.
本発明のフェライト被覆粒子状物の製造装置では、少なくとも第１鉄イオンを含む反応液、少なくとも酸化剤、もしくは、少なくとも酸素を含んだ酸化媒体を基体に接触させる機構、及びフェライト層で被覆される粒子状物が装置内部に連続しで供給、回収される機構を備えることによって、工業的な生産性を向上させるものである。 In the apparatus for producing a ferrite-coated particulate matter according to the present invention, the reaction liquid containing at least ferrous ions, the mechanism for bringing the oxidizing medium containing at least an oxidizing agent or at least oxygen into contact with the substrate, and the ferrite layer are coated. Industrial productivity is improved by providing a mechanism in which particulate matter is continuously supplied and recovered inside the apparatus.
さらに、詳しく述べると、本発明のフェライト被覆粒子状物の製造装置では、第一鉄イオンを含む反応液、少なくとも酸化剤、少なとも酸素を含んだ酸化媒体を基体に接触させる機構、フェライト層で被覆される粒子状物が装置内部に連続して供給、回収される機構、及び少なくとも第一鉄イオンを含む反応液、少なくとも酸化剤、もしくは、少なくとも酸素を含んだ酸化媒体、及び粒子状物が超音波により攪拌される機構を備えることによって、表面がフェライトで均一に覆われたフェライト被覆粒子状物を得るものである。 More specifically, in the ferrite coated particulate matter manufacturing apparatus of the present invention, a reaction solution containing ferrous ions, a mechanism for contacting an oxidizing medium containing at least an oxidizing agent and at least oxygen, and a substrate, a ferrite layer A mechanism for continuously supplying and recovering the particulate matter to be coated inside the apparatus, and a reaction solution containing at least ferrous ions, an oxidizing medium containing at least an oxidizing agent, or an oxidizing medium containing at least oxygen, and a particulate matter. By providing a mechanism that is stirred by ultrasonic waves, a ferrite-coated particulate material whose surface is uniformly covered with ferrite is obtained.
次に、本発明のフェライト被覆粒子状物の製造装置を図を用いて更に詳細に説明する。 Next, the apparatus for producing a ferrite-coated particulate material according to the present invention will be described in more detail with reference to the drawings.
図１は本発明のフェライトメッキ膜製造装置の概略構成を示す図である。図１においては、メッキポット（容器）１内部が見えるように、メッキポット１を仮想線で示してある。メッキポット１の中心には、中心シャフト２が配置されている。中心シャフト２には、螺旋状の回転羽３が固定されており、中心シャフト２が回転するとメッキポット１内部で回転羽３も同時に回転する。これらは、供給及び回収が連続的におこなわれる機構を構成する。
FIG. 1 is a diagram showing a schematic configuration of a ferrite plating film manufacturing apparatus of the present invention. In FIG. 1, the plating pot 1 is indicated by a virtual line so that the inside of the plating pot (container) 1 can be seen. A central shaft 2 is disposed at the center of the plating pot 1. A spiral rotating
粒子状物は供給口４から供給され、回転羽３が回転することで、ポット内部を順次排出口５へ攪拌されながら送られる。メッキポット１には、少なくとも第１鉄イオンを含む反応液、少なくとも酸化剤もしくは少なくとも酸素を含んだ酸化媒体をポット内部へ供給する少なくとも酸化剤、少なとも酸素を含んだ酸化媒体を基体に接触させる機構としての供給ノズル６，７が配置され、ポット内部を攪拌されながら送られる粒子状物に反応液、酸化媒体を適宜供給することで、粒子状物の表面にフェライト層が形成される。これらは基体に流下して接触させる構成であるが、噴霧や液滴の滴下であっても良いことは勿論である。更に、粒子状物、反応液、酸化媒体は、攪拌手段である超音波ホーン８によって均一に攪拌される。尚、超音波ホーンの設置位置、本数は必要に応じて適宜調整することが出来る。
Particulate matter is supplied from the
それでは、本発明の製造の具体例を述べる。 Then, the specific example of manufacture of this invention is described.
（例）
純水１リットル（以下、Ｌと示す）に対して、ＦｅＣｌ２・４Ｈ２Ｏを１０ｇ、ＮｉＣｌ２・６Ｈ２Ｏを２．３９ｇ、ＺｎＣｌ２を０．２７ｇそれぞれ溶解した反応液を作製した。別の溶液として、純水１Ｌに対してＮａＮＯ２を２ｇ溶解した酸化液を作製した。
(Example)
1 liter of pure water (hereinafter, referred to as L) with respect to prepare FeCl 2 · 4H 2 O and 10g, NiCl 2 · 6H 2 O and 2.39 g, the reaction solution obtained by dissolving ZnCl 2 0.27 g respectively. As another solution, an oxidizing solution in which 2 g of NaNO 2 was dissolved in 1 L of pure water was prepared.
これらの溶液を用いて、図１に示したような装置を用いてフェライト膜を作製した。フェライト膜の作製は、以下の手順で行った。 Using these solutions, a ferrite film was produced using an apparatus as shown in FIG. The ferrite film was produced according to the following procedure.
粒子状物は平均粒径１００μｍのカルボニルＦｅ粒子とし、内容積１Ｌのメッキポット１に連続して供給した。Ｆｅ粒子を供給するメッキポット１内部の温度は９０℃で一定に保ち、またポット１内には、窒素ガスを１．５Ｌ／ｍｉｎで供給しで非酸化性雰囲気を得た。 The particulate matter was carbonyl Fe particles having an average particle diameter of 100 μm, and was continuously supplied to the plating pot 1 having an internal volume of 1 L. The temperature inside the plating pot 1 for supplying Fe particles was kept constant at 90 ° C., and nitrogen gas was supplied into the pot 1 at 1.5 L / min to obtain a non-oxidizing atmosphere.
反応液、酸化液の流量は１０ｍＬ／ｍｉｎに調整し、Ｆｅ粒子に連続的に供給し、更に反応液、酸化液、Ｆｅ粒子は超音波ホーンから供給される超音波によって攪拌した。 The flow rates of the reaction solution and the oxidizing solution were adjusted to 10 mL / min, and were continuously supplied to the Fe particles. The reaction solution, the oxidizing solution, and the Fe particles were further stirred by ultrasonic waves supplied from an ultrasonic horn.
Ｆｅ粒子は、メッキポット１内に１時間滞留するように回転羽３の回転数を調整した。
The rotational speed of the
得られたＦｅ粉末は、黒褐色を呈しており、得られた量は７ｋｇであった。 The obtained Fe powder had a dark brown color, and the amount obtained was 7 kg.
（比較例１）
純水１Ｌに対しでＦｅＣｌ２・４Ｈ２Ｏを１０ｇ、ＮｉＣｌ２・６Ｈ２Ｏを２．３９ｇ、ＺｎＣ１２を０．２７ｇそれぞれ溶解した反応液を作製した。別の溶液として、純粋１Ｌに対して、ＮａＮＯ２を２ｇ溶解した酸化液を作製した。
(Comparative Example 1)
A reaction solution was prepared by dissolving 10 g of FeCl 2 .4H 2 O, 2.39 g of NiCl 2 .6H 2 O, and 0.27 g of ZnC 1 2 per 1 L of pure water. As another solution, an oxidation solution in which 2 g of NaNO 2 was dissolved in 1 L of pure was prepared.
粒子状物は、平均粒径１００μｍのカルボニルＦｅ粒子とし、反応容器中の純水１Ｌに十分均一に分散可能な量を投入した。また、反応容器中の純水は、予め窒素ガスにより脱酸素を行った。 The particulate matter was carbonyl Fe particles having an average particle diameter of 100 μm, and an amount capable of being dispersed sufficiently uniformly in 1 L of pure water in the reaction vessel was added. The pure water in the reaction vessel was previously deoxygenated with nitrogen gas.
反応液、酸化液の流量は１０ｍＬ／ｍｉｎに調整し、反応容器内に連続的に供給した。その間、反応液中のｐＨはアンモニア水を適宜供給することで６〜８に保った。また、反応容器内の温度は９０℃で一体に保った。反応時間は１時間とした。得られたＦｅ粉末は黒褐色を呈しており、得られた量は５０ｇであった。 The flow rates of the reaction solution and the oxidizing solution were adjusted to 10 mL / min and continuously supplied into the reaction vessel. Meanwhile, the pH in the reaction solution was kept at 6 to 8 by appropriately supplying ammonia water. The temperature in the reaction vessel was kept at 90 ° C. integrally. The reaction time was 1 hour. The obtained Fe powder had a blackish brown color, and the amount obtained was 50 g.
（比較例２）
純水１Ｌに対して、ＦｅＣｌ２・４Ｈ２Ｏを１０ｇ、ＮｉＣｌ２・６Ｈ２Ｏを２．３９ｇ、ＺｎＣ１２を０．２７ｇそれそれ溶解した反応液を作製した。別の溶液としで、鈍水１Ｌに対しでＮａＮＯ２を２ｇ溶解した酸化液を作製した。
(Comparative Example 2)
A reaction liquid was prepared by dissolving 10 g of FeCl 2 .4H 2 O, 2.39 g of NiCl 2 .6H 2 O, and 0.27 g of ZnC 1 2 per 1 L of pure water. As another solution, an oxidizing solution in which 2 g of NaNO 2 was dissolved in 1 L of blunt water was prepared.
これらの溶液を用いて、図１に示したような装置を用いでフェライト膜を作製した。 Using these solutions, a ferrite film was produced using an apparatus as shown in FIG.
フェライト膜の作製は、以下の手順で行った。 The ferrite film was produced according to the following procedure.
粒子状物は平均粒径１００μｍのカルボニルＦｅ粒子とし、内容積１Ｌのメッキポット１に連続して、供給した。Ｆｅ粒子を供給するメッキポット１内部の温度は９０℃で一定に保ち、またメッキポット１内には窒素がスを１．５Ｌ／ｍｉｎで供給しで非酸化性雰囲気を得た。 The particulate matter was carbonyl Fe particles having an average particle size of 100 μm, and was continuously supplied to the plating pot 1 having an internal volume of 1 L. The temperature inside the plating pot 1 for supplying Fe particles was kept constant at 90 ° C., and nitrogen was supplied into the plating pot 1 at 1.5 L / min to obtain a non-oxidizing atmosphere.
反応液、酸化成の流量は１０ｍＬ／ｍｉｎに調整し、Ｆｅ粒子に連続的に供給した。 The flow rate of the reaction solution and oxidation was adjusted to 10 mL / min and continuously supplied to the Fe particles.
Ｆｅ粒子はメッキポット１内に１時間滞留するように回転羽３の回転数を調整した。
The rotational speed of the
得られたＦｅ粉末は、黒褐色を呈しでおり、得られた量は７ｋｇであった。 The obtained Fe powder had a blackish brown color, and the amount obtained was 7 kg.
下記表１に、本発明例、比較例１においで１時間フェライト被覆処理を施した後のＦｅ粉末の収量を示した。 Table 1 below shows the yield of Fe powder after the ferrite coating treatment for 1 hour in the inventive example and the comparative example 1.
上記表１から分かるように、本発明例においでフェライト被覆Ｆｅ粉末の収量は１４０倍に増加している。即ち、本発明例においで工業的な生産性を向上したフェライト被覆粒子状物の製造装置が得られた。 As can be seen from Table 1 above, the yield of the ferrite-coated Fe powder is increased 140 times in the examples of the present invention. That is, in the present invention example, an apparatus for producing ferrite-coated particulate matter with improved industrial productivity was obtained.
図２は本発明例に示したように超音波によって反応液、酸化液、Ｆｅ粒子を攪拌した場合のフェライト被覆Ｆｅ粒子の概略断面図を図３に本発明例と同じ設備を用いで超音波による攪拌を行わなかった場合のフェライト被覆Ｆｅ粒子の概略断面図である。 FIG. 2 is a schematic cross-sectional view of ferrite-coated Fe particles when the reaction solution, oxidizing solution, and Fe particles are stirred by ultrasonic waves as shown in the present invention example. FIG. It is a schematic sectional drawing of the ferrite covering Fe particle at the time of not performing stirring by.
図２及び図３から分かるように、反応液、酸化液、Ｆｅ粒子を超音波によって、攪拌することによって、表面が均一にフェライトで被覆されたＦｅ粒子が得られた。 As can be seen from FIGS. 2 and 3, the reaction solution, the oxidizing solution, and the Fe particles were agitated by ultrasonic waves to obtain Fe particles whose surfaces were uniformly coated with ferrite.
フェライト被覆粒子状物は、本発明例以外の金属扮末でも同様の効果が得られる。また、金属粉末以外の樹脂、金属酸化物、有機顔料、セルロース、合成高分子材料、セラミックス及び繊維状粒子、扁平状粒子においても同様の効果が得られる。 The same effect can be obtained with the ferrite-coated particulate matter even with a metal powder other than the example of the present invention. Similar effects can also be obtained with resins other than metal powders, metal oxides, organic pigments, cellulose, synthetic polymer materials, ceramics, fibrous particles, and flat particles.
本発明に係るフェライト被膜製造装置は、磁気記録媒体、光磁気記録媒体、磁気ヘッド、磁気光学素子、マイクロ波素子、磁歪素子、磁気音響素子用のフェライト被覆粒子状物の製造に適用できる。 The ferrite film production apparatus according to the present invention can be applied to the production of ferrite-coated particulates for magnetic recording media, magneto-optical recording media, magnetic heads, magneto-optical elements, microwave elements, magnetostrictive elements, and magnetoacoustic elements.
１ メッキポット
２ 中心シャフト
３ 回転羽
４ 供給口
５ 排出口
６，７ 供給ノズル
８ 超音波ホーン
９，１０ Ｆｅ粉末断面
１１，１２ 被覆フェライト断面
１０１ フェライトメッキ膜製造装置
DESCRIPTION OF SYMBOLS 1 Plating pot 2
Claims (1)
前記製造装置は少なくとも第一鉄イオンを含む反応液、少なくとも酸化剤もしくは少なくとも酸素を含んだ酸化媒体を流下、噴霧、もしくは液滴の滴下によって前記反応液及び前記酸化媒体を前記粒子状物に接触させて当該粒子状物と直接反応させて、前記粒子状物の表面をフェライトめっき膜で被覆する機構と、
前記反応液、前記酸化媒体、及び粒子状物を超音波により攪拌し、前記粒子状物の表面を均一にフェライトめっき膜で被覆するための攪拌手段とを備える
ことを特徴とするフェライト被覆粒子状物の製造装置。 A ferrite-coated particulate material that supplies the particulate material, coats the surface of the particulate material with a ferrite plating film, and continuously collects the particulate material whose surface is coated with the ferrite plating film . Manufacturing equipment,
The manufacturing apparatus contacts the reaction solution and the oxidation medium with the particulate matter by flowing, spraying, or dropping droplets of a reaction solution containing at least ferrous ions, an oxidation medium containing at least an oxidizing agent or at least oxygen. A mechanism for directly reacting with the particulate matter and covering the surface of the particulate matter with a ferrite plating film ;
The reaction solution, and wherein said oxidizing medium, and the particulate was agitated ultrasonically obtain Bei and stirring means for coating with uniform ferrite-plated film surface of the particulate material <br/> that Manufacturing equipment for ferrite coated particulates.
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|---|---|---|---|---|
| JPH06231957A (en) * | 1992-08-31 | 1994-08-19 | Nippon Paint Co Ltd | Particle coated with ferrite and its manufacture |
| JPH07118864A (en) * | 1993-10-22 | 1995-05-09 | C Uyemura & Co Ltd | Electroless plating method and electroless plating device for particle |
| JPH07267627A (en) * | 1994-03-24 | 1995-10-17 | Katayama Chem Works Co Ltd | Ferromagnetism-coated porous silica fine powder and its use |
| JPH07320916A (en) * | 1994-05-26 | 1995-12-08 | Japan Synthetic Rubber Co Ltd | Method of manufacturing magnetic particle |
| JP2000128544A (en) * | 1998-10-28 | 2000-05-09 | Nittetsu Mining Co Ltd | Film-coated powder and its production |
| JP2002121421A (en) * | 2000-10-13 | 2002-04-23 | Sekisui Chem Co Ltd | Method for producing metal oxide-covered particle, and metal oxide-covered particle |
| JP2002121679A (en) * | 2000-10-13 | 2002-04-26 | Mitsuboshi Belting Ltd | Method for manufacturing conductive bead |
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2003
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06231957A (en) * | 1992-08-31 | 1994-08-19 | Nippon Paint Co Ltd | Particle coated with ferrite and its manufacture |
| JPH07118864A (en) * | 1993-10-22 | 1995-05-09 | C Uyemura & Co Ltd | Electroless plating method and electroless plating device for particle |
| JPH07267627A (en) * | 1994-03-24 | 1995-10-17 | Katayama Chem Works Co Ltd | Ferromagnetism-coated porous silica fine powder and its use |
| JPH07320916A (en) * | 1994-05-26 | 1995-12-08 | Japan Synthetic Rubber Co Ltd | Method of manufacturing magnetic particle |
| JP2000128544A (en) * | 1998-10-28 | 2000-05-09 | Nittetsu Mining Co Ltd | Film-coated powder and its production |
| JP2002121421A (en) * | 2000-10-13 | 2002-04-23 | Sekisui Chem Co Ltd | Method for producing metal oxide-covered particle, and metal oxide-covered particle |
| JP2002121679A (en) * | 2000-10-13 | 2002-04-26 | Mitsuboshi Belting Ltd | Method for manufacturing conductive bead |
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