Iron-based oxide magnetic powder and production method therefor

Patent metadata

Field	Value
Publication number	US-2022081319-A1
Application number	US-202017419346-A
Country	US
Kind code	A1
Filing date	Feb 4, 2020
Priority date	Feb 5, 2019
Publication date	Mar 17, 2022
Grant date	—

Abstract

An iron-based oxide magnetic powder has good thermal stability and a small change in coercive force even in a high-temperature environment and is one composed of particles of ε-iron oxide in which Fe sites are partially substituted by another metal element. A production method for such an iron-based oxide magnetic powder includes allowing a phosphorus-containing ion to coexist when a precipitate of an iron hydroxide containing a substituent metal element produced by neutralizing an acidic aqueous solution containing a trivalent iron ion and an ion of a metal that partially substitutes Fe sites is coated with silicon oxide using a silane compound.

First claim

1 . An iron-based oxide magnetic powder, comprising particles of ε-iron oxide in which Fe sites are partially substituted by another metal element, wherein when coercive forces Hc as measured at a maximum applied magnetic field of 1193 kA/m and a measurement temperature of 25° C., 60° C., and 90° C. are represented by Hc 25 , Hc 60 , and Hc 90 , respectively, the absolute values of ΔHc 60 and ΔHc 90 defined by the following formula (1) and formula (2) are both 0.15 or less:
Δ Hc 60 =( Hc 60 −Hc 25 )/ Hc 25   (1); and

Δ Hc 90 =( Hc 90 −Hc 25 )/ Hc 25   (2).

2 . The iron-based oxide magnetic powder according to claim 1 , wherein the metal element that partially substitutes the Fe sites is Ti, Co, and one type selected from Ga and Al.

3 . A production method for an iron-based oxide magnetic powder composed of particles of ε-iron oxide in which Fe sites are partially substituted by another metal element, comprising:
a neutralization step of neutralizing an acidic aqueous solution containing a trivalent iron ion, an ion of a metal that partially substitutes the Fe sites, and a phosphorus-containing ion in which the molar ratio (P/Si) of the amount of phosphorus contained in the phosphorus-containing ion to the amount of Si of a silane compound to be added in the following coating step is 0.0001 or more and 0.01 or less with an alkali aqueous solution, thereby obtaining a slurry of a precipitate of an iron hydroxide containing a substituent metal element;
a coating step of adding a silane compound in which the molar ratio (Si/(Fe+M)) of the amount of Si of the silane compound to the sum (Fe+M) of the amount of the iron ion and the amount of the substituent metal ion contained in a raw material solution is 0.50 or more and 10 or less to the slurry containing the precipitate of the iron hydroxide containing the substituent metal element, thereby coating the precipitate of the iron hydroxide containing the substituent metal element with a hydrolysate of the silane compound in the presence of the phosphorus-containing ion;
a recovery step of recovering the precipitate of the iron hydroxide containing the substituent metal element coated with the hydrolysate of the silane compound by solid-liquid separation;
a heating step of heating the recovered precipitate of the iron hydroxide containing the substituent metal element coated with the hydrolysate of the silane compound, thereby obtaining an iron oxide powder containing the substituent metal element coated with silicon oxide; and
a dissolution step of dissolving the silicon oxide coating by immersing the iron oxide powder containing the substituent metal element coated with silicon oxide obtained by the heating step in an alkali aqueous solution, thereby obtaining the iron oxide powder containing the substituent metal element.

4 . A production method for an iron-based oxide magnetic powder composed of particles of ε-iron oxide in which Fe sites are partially substituted by another metal element, comprising:
a neutralization step of neutralizing an acidic aqueous solution containing a trivalent iron ion and an ion of a metal that partially substitutes the Fe sites with an alkali aqueous solution, thereby obtaining a slurry of a precipitate of an iron hydroxide containing a substituent metal element;
a coating step of adding a silane compound in which the molar ratio (Si/(Fe+M)) of the amount of Si of a silane compound to the sum (Fe+M) of the amount of the iron ion and the amount of the substituent metal ion contained in a raw material solution is 0.50 or more and 10 or less, and a phosphorus-containing ion in which the molar ratio (P/Si) of the amount of phosphorus contained in the phosphorus-containing ion to the amount of Si of the silane compound is 0.0001 or more and 0.01 or less to the slurry containing the precipitate of the iron hydroxide containing the substituent metal element, thereby coating the precipitate of the iron hydroxide containing the substituent metal element with a hydrolysate of the silane compound in the presence of the phosphorus-containing ion;
a recovery step of recovering the precipitate of the iron hydroxide containing the substituent metal element coated with the hydrolysate of the silane compound by solid-liquid separation;
an oxidation step of heating the recovered precipitate of the iron hydroxide containing the substituent metal element coated with the hydrolysate of the silane compound, thereby obtaining an iron oxide powder containing the substituent metal element coated with silicon oxide; and
a dissolution step of dissolving the silicon oxide coating by immersing the iron oxide powder containing the substituent metal element coated with silicon oxide obtained by the oxidation step in an alkali aqueous solution, thereby obtaining the iron oxide powder containing the substituent metal element.

5 . The production method for an iron-based oxide magnetic powder according to claim 3 , wherein the metal element that partially substitutes the Fe sites is Ti, Co, and one type selected from Ga and Al.

6 . The production method for an iron-based oxide magnetic powder according to claim 3 , wherein the phosphorus-containing ion is one or more types selected from a phosphate ion, a phosphite ion, and a hypophosphite ion.

Assignees

• Dowa Electronics Materials Co Ltd
• Univ Tokyo

Inventors

• Ohkoshi Shin-Ichi
• Namai Asuka
• YOSHIKIYO Marie
• Kodama Daisuke
• Obata Shiho
• Gotoh Masahiro

Classifications

• H01F1/11

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

• C01G49/0018 Primary

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

• C01P2002/72

  by d-values or two theta-values, e.g. as X-ray diagram · CPC title

• C01P2004/64

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

• C01G49/06 Primary

  Ferric oxide [Fe2O3] · CPC title