Process for production of magnetic thin film, magnetic thin film, and magnetic material

Patent metadata

Field	Value
Publication number	US-9886978-B2
Application number	US-201013378730-A
Country	US
Kind code	B2
Filing date	Jun 24, 2010
Priority date	Jun 24, 2009
Publication date	Feb 6, 2018
Grant date	Feb 6, 2018

Abstract

The present invention provides a process for production of a magnetic thin film which has insulation properties, serves as a permanent magnet, and has improved residual magnetization in comparison with prior arts, the magnetic thin film, and a magnetic material. When a magnetic thin film 3 is formed, an external magnetic field with a predetermined intensity is applied to a coating liquid containing magnetic particles containing epsilon-type iron-oxide-based compounds which have insulation properties and which serve as a permanent magnet, and the coating liquid is let cured in order to form the magnetic thin film 3 . Accordingly, the magnetic particles containing the epsilon-type iron-oxide-based compounds can be fixed while being oriented regularly in a magnetization direction. This realizes the process for production of the magnetic thin film 3 which has insulation properties and which serve as a permanent magnet, the magnetic thin film 3 , and a magnetic material 1.

First claim

The invention claimed is:

1. A process for production of a magnetic thin film, the process comprising:
producing a mixed solution by mixing a raw-material solution to which calcium ions as a shape control agent are added in the amount of equal to or smaller than 8 wt % with a neutralizer solution to which a neutralizer is added such that a precipitation reaction of ferric-hydroxide-based compound particles progresses in the mixed solution;
producing silica-coated ferric-hydroxide-based compound particles by adding silane compounds to the mixed solution;
producing thermally processed powders by separating the silica-coated ferric-hydroxide-based compound particles from the mixed solution and calcining the silica-coated ferric-hydroxide-based compound particles;
producing magnetic particles by adding the thermally processed powders to an aqueous solution such that silica coating the thermally processed powders is completely eliminated, the magnetic particles being formed of epsilon-type iron-oxide-based compounds, having insulation properties, and serving as a permanent magnet, each magnetic particle being in a rod-like shape having a long-axis size equal to or longer than 100 nm and an aspect ratio equal to or higher than 3.1 and providing a magnetic domain wall therein;
producing a magnetic material slurry having a ratio of an average particle diameter of the magnetic particles by a dynamic light scattering method to an observed average particle diameter of the magnetic particles by an observation through a transmission electron microscope equal to or less than five by purifying the aqueous solution, in which the magnetic particles are dispersed, with a pH adjustment and a solid content concentration adjustment without a dry process;
producing a coating liquid having a solution viscosity in a range from 170 cP to 1000 cP by mixing a polymer consisting of polyvinyl-alcohol aqueous solution or PEG aqueous solution with the magnetic material slurry;
coating a film-formation target with the coating liquid; and
curing the coating liquid coating the film-formation target while applying an external magnetic field with a predetermined intensity to the coating liquid and forming a magnetic thin film, wherein the external magnetic field is continuously applied during a time period until the coating liquid is dried and cured, and wherein
a ratio of residual magnetization M r relative to saturated magnetization M s of the magnetic thin film is equal to or greater than 0.78.

2. The process according to claim 1 , wherein the external magnetic field has an intensity equal to or greater than 2 T.

3. The process according to claim 1 , wherein
the magnetic particles dispersed in a solution of the coating liquid contain equal to or greater than 99 wt % of the epsilon-type iron-oxide-based compounds.

4. The process according to claim 1 , wherein the epsilon-type iron-oxide-based compounds are each at least one of the following: ∈-Fe 2 O 3 ; ∈-A x Fe 2-x O 3 (where A is an element other than Fe and 0<x<2); and ∈-B y C z Fe 2-y-z O 3 (where B and C are elements other than A and Fe and mutually different elements and 0<y<1 and 0<z<1).

5. A magnetic thin film comprising:
magnetic particles formed of epsilon-type iron-oxide-based compounds, the magnetic particles having insulation properties and serving as a permanent magnet, each magnetic particle being in a rod-like shape having a long-axis size equal to or longer than 100 nm and an aspect ratio equal to or higher than 3.1 and providing a magnetic domain wall therein; and
a polymer consisting of polyvinyl-alcohol or PEG, wherein

the magnetic particles are oriented in a predetermined direction in accordance with an external magnetic field applied when the magnetic thin film is formed, and a ratio of residual magnetization M r relative to saturated magnetization M s of the magnetic thin film is equal to or greater than 0.78.

6. The magnetic thin film according to claim 5 , wherein the magnetic particles containing equal to or greater than 99 wt % of the epsilon-type iron-oxide-based compounds are dispersed and arranged in the magnetic thin film and a thickness of the magnetic thin film is 10 μm or less and a haze is equal to or lower than 40%.

7. The magnetic thin film according to claim 5 , wherein the epsilon-type iron-oxide-based compounds are each at least one of the following: ∈-Fe 2 O 3 ; ∈-A x Fe 2-x O 3 (where A is an element other than Fe and 0<x<2); and ∈-B y C z Fe 2-y-z O 3 (where B and C are elements other than A and Fe and mutually different elements and 0<y<1 and 0<z<1).

8. A magnetic thin film comprising:
a predetermined area including magnetic particles formed of epsilon-type iron-oxide-based compounds, the magnetic particles having insulation properties and serving as a permanent magnet, each magnetic particle being in a rod-like shape having a long-axis size equal to or longer than 100 nm and an aspect ratio equal to or higher than 3.1 and providing a magnetic domain wall therein, and a polymer consisting of polyvinyl-alcohol or PEG; and
another area including the magnetic particles and the polymer, wherein
the magnetic particles in the predetermined area are oriented in a predetermined direction in accordance with an external magnetic field applied when the magnetic thin film is formed, and the magnetic particles in the other area are oriented in a direction different from the predetermined direction, and a ratio of residual magnetization M r relative to saturated magnetization M s of the magnetic thin film in the predetermined area is equal to or greater than 0.78.

9. The magnetic thin film according to claim 5 , wherein the magnetic thin film absorbs electromagnetic wave of a millimeter-wave range from 30 to 300 GHz.

10. A magnetic material comprising the magnetic thin film according to claim 5 on a film-formation target.

11. The magnetic thin film according to claim 5 , comprising a rod-like secondary particle formed of a plurality of the rod-like shaped magnetic particles bonded together with lengthwise directions aligned, the rod-like secondary particle being oriented in a predetermined direction in accordance with the external magnetic field.

Assignees

• Ohkoshi Shin Ichi
• Namai Asuka
• Takami Kazuyuki
• Tomita Koutaro
• Univ Tokyo
• Dowa Electronics Materials Co Ltd

Inventors

• Ohkoshi Shin Ichi
• Namai Asuka
• Takami Kazuyuki
• Tomita Koutaro

Classifications

• C01P2004/10

  extending in one dimension, e.g. needle-like · CPC title

• G11B5/845 Primary

  in a magnetic field · CPC title

• C01P2006/22

  Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability · CPC title

• H01F41/24

  from liquids · CPC title

• C01P2002/52

  containing elements as dopants · CPC title