Iron-based oxide magnetic powder and method for producing same

Patent metadata

Field	Value
Publication number	US-2021300779-A1
Application number	US-201916979241-A
Country	US
Kind code	A1
Filing date	Mar 26, 2019
Priority date	Mar 29, 2018
Publication date	Sep 30, 2021
Grant date	—

Abstract

[Problem] To provide a method for producing iron based oxide magnetic powder that has a narrow particle size distribution and a small content of fine particles that do not contribute to the magnetic recording characteristics, and consequently has a narrow coercive force distribution and is suitable for the enhancement of the recording density of the magnetic recording medium. [Solution] ε-Type iron based oxide magnetic powder is obtained by a wet method, then a tetraalkylammonium salt as a surface modifier is added to a slurry containing the magnetic powder to make a concentration of 0.009 mol/kg or more and 1.0 mol/kg or less, and simultaneously to make pH of 11 or more and 14 or less, and the slurry is subjected to a dispersion treatment and then classified, so as to provide iron based oxide magnetic powder having a narrow particle size distribution and a narrow coercive force distribution.

First claim

1 . Iron based oxide magnetic powder comprising particles of an ε-iron oxide having an average particle diameter measured with a transmission electron microscope of 8 nm or more and 30 nm or less and a coefficient of variation of the particle diameter of 30% or less, and having a value of I L /I H defined below of 0.55 or less,
wherein I H represents an intensity of a peak that appears on a high magnetic field side in a differential B-H curve obtained by numerical differentiation of a B-H curve obtained by measuring under conditions of an applied magnetic field of 3,979 kA/m (50 kOe), an M measurement range of 0.005 A·m 2 (5 emu), an applied magnetic field change rate of 13 (kA/m·s), a time constant of 0.03 sec, and a wait time of 0.8 sec, and I L represents an intensity of an intercept of the ordinate at zero magnetic field in the differential B-H curve.

2 . Iron based oxide magnetic powder comprising particles of an ε-iron oxide having Fe sites, a part of which is substituted by other metal elements, having an average particle diameter measured with a transmission electron microscope of 8 nm or more and 30 nm or less and a coefficient of variation of the particle diameter of 30% or less, and having a value of I L /I H defined below of 0.55 or less,
wherein I H represents an intensity of a peak that appears on a high magnetic field side in a differential B-H curve obtained by numerical differentiation of a B-H curve obtained by measuring under conditions of an applied magnetic field of 1,035 kA/m (13 kOe), an M measurement range of 0.005 A·m 2 (5 emu), an applied magnetic field change rate of 15 (kA/m·s), a time constant of 0.03 sec, and a wait time of 0.1 sec, and I L represents an intensity of an intercept of the ordinate at zero magnetic field in the differential B-H curve.

3 . The iron based oxide magnetic powder according to claim 2 , wherein the metal elements substituting a par a part of the Fe sites are one kind or two or more kinds of Ga, Co, and Ti.

4 . The iron based oxide magnetic powder according to claim 1 , wherein the iron based oxide magnetic powder has a squareness ratio SQ of 0.54 or more.

5 . A method for producing iron based oxide magnetic powder, comprising:
preparing a slurry containing particles of an ε-iron oxide or an ε-iron oxide having Fe sites, a part of which is substituted d by other metal elements, having an average particle diameter measured with a transmission electron microscope of 5 nm or more and 100 nm or less and a coefficient of variation of the particle diameter of 70% or less; adding a quaternary ammonium salt as a surface modifier to the slurry to make a concentration of 0.009 mol/kg or more and 1.0 mol/kg or less, and simultaneously to make pH of 11 or more and 14 or less; subjecting the surface modifier-containing slurry to a dispersion treatment to provide an ε-iron oxide-dispersed slurry or a slurry having an ε-iron oxide having Fe sites, a part of which is substituted by other metal elements, dispersed therein; and classifying the ε-iron oxide-dispersed slurry or the slurry having an ε-iron oxide having Fe sites, a part of which is substituted by other metal elements, dispersed therein.

6 . The method for producing iron based oxide magnetic powder according to claim 5 , wherein the quaternary ammonium salt is a tetraalkylammonium salt.

7 . The method for producing iron based oxide magnetic powder according to claim 5 , wherein the quaternary ammonium salt is a tetraalkylammonium hydroxide.

8 . The method for producing iron based oxide magnetic powder according to claim 5 , wherein in the ε-iron oxide-dispersed slurry or the slurry having an ε-iron oxide having Fe sites, a part of which is substituted by other metal elements, dispersed therein, particles of the ε-iron oxide or the ε-iron oxide having Fe sites, a part of which is substituted by other metal elements, have an average secondary particle diameter measured with a dynamic light scattering particle size measurement device of 65 nm or less.

9 . The method for producing iron based oxide magnetic powder according to claim 5 , wherein the slurry containing particles of the ε-iron oxide or the ε-iron oxide having Fe sites, a part of which is substituted by other metal elements, has a conductivity of 15 mS/m or less.

10 . The method for producing iron based oxide magnetic powder according to claim 5 , wherein the classifying step includes subjecting the ε-iron oxide-dispersed slurry or the slurry having an ε-iron oxide having Fe sites, a part of which is substituted by other metal elements, dispersed therein to a centrifugal separator, and then removing a supernatant.

11 . The method for producing iron based oxide magnetic powder according to claim 10 , wherein in the classifying step, the centrifugal acceleration in subjecting to the centrifugal separator is 40,000 G or more.

Assignees

• Dowa Electronics Materials Co Ltd
• Univ Tokyo

Inventors

• Ohkoshi Shin-Ichi
• Namai Asuka
• Sakane Kenji
• Kawahito Tetsuya

Classifications

• C01P2006/42

  Magnetic properties · CPC title

• H01F1/11

  in the form of particles {(for magnetic record carriers G11B5/70626)} · CPC title

• C01P2004/04

  obtained by TEM, STEM, STM or AFM · CPC title

• C01P2004/64

  Nanometer sized, i.e. from 1-100 nanometer · CPC title

• C01G49/0018

  Mixed oxides or hydroxides, (C01G49/0009 takes precedence) · CPC title