Temperature-stable soft-magnetic powder

Patent metadata

Field	Value
Publication number	US-10373748-B2
Application number	US-201415034039-A
Country	US
Kind code	B2
Filing date	Nov 4, 2014
Priority date	Nov 6, 2013
Publication date	Aug 6, 2019
Grant date	Aug 6, 2019

Abstract

The invention further relates to a process of coating the soft-magnetic powder, the use of such soft-magnetic powder and an electronic component including such soft-magnetic powder.

First claim

The invention claimed is:

1. A soft-magnetic powder coated with a silicon based coating, wherein the silicon based coating comprises at least one of the following fluorine containing compositions:
a) a fluorine containing composition of formula (I)
Si 1-0,25a M1 a O 2-0,5b F b   (I)

wherein
a is in the range of 0.015 to 0.52,
b is in the range of 0.015 to 0.52,
M1 is H, K, Rb, Cs or NR 1 4 , wherein each R 1 is independently selected from the group
consisting of H, C 1-6 alkyl, phenyl and benzyl;
b) a fluorine containing composition of formula (II)
Si 1-0,75c M2 c O 2-0,5d F d   (II)

wherein
c is in the range of 0.005 to 0.17,
d is in the range of 0.015 to 0.52,
M2 is B or Al;
or
c) a fluorine containing composition of formula (III)
Si 1-1,25e P e O 2-0,5f F f   (III)

wherein
e is in the range of 0.003 to 0.10, and
f is in the range of 0.015 to 0.52.

2. The soft-magnetic powder of claim 1 , comprising at least one fluorine containing composition of formula (I), wherein M1 is H, Cs or NH 4 and at least one fluorine containing composition of formula (II), wherein M2 is B.

3. The soft-magnetic powder of claim 1 , wherein silicon based coating comprises between 0.1 to 5 wt.-% of the at least one fluorine containing composition of formula (I), (II) or (III).

4. The soft-magnetic powder of claim 1 , wherein the fluorine component of the fluorine containing composition is embedded within a SiO 2 -matrix and/or bonded to a surface of a SiO 2 -coating.

5. The soft-magnetic powder of claim 1 , wherein the silicon based coating has an average thickness of 2 to 100 nm.

6. A process for coating the soft-magnetic powder, the coating comprising at least one of the following fluorine containing compositions:
a) a fluorine containing composition of formula (I)
Si 1-0,25a M1 a O 2-0,5b F b   (I)

wherein
a is in the range of 0.015 to 0.52,
b is in the range of 0.015 to 0.52,
M1 is 1H, K, Rb, Cs or NR 1 4 , wherein each R 1 is independently selected from the group consisting of H, C 1-6 alkyl, phenyl and benzyl;
b) a fluorine containing composition of formula (II)
Si 1-0,75c M2 c O 2-0,5d F d   (II)

wherein
c is in the range of 0.005 to 0.17,
d is in the range of 0.015 to 0.52,
M2 is B or Al;
or
c) a fluorine containing composition of formula (III)
Si 1-1,25e P e O 2-0,5f F f   (III)

wherein
e is in the range of 0.003 to 0.10, and
f is in the range of 0.015 to 0.52
wherein the soft-magnetic powder is mixed with a silicon based solution containing a soluble fluorination agent (F).

7. The process of claim 6 , wherein the soft-magnetic powder is mixed with a silicon based solution and soluble fluorination agent (F) is added after at least partial treatment of the soft-magnetic powder with the silicon based solution.

8. The process of claim 6 , wherein the at least one soluble fluorination agent (F) is
(A) a salt of formula (IVa) or (IVb)
M1F  (IVa)

M2F 3   (IVb)

wherein
M1 is defined as in formula (I),
M2 is defined as in formula (II);
(B) a compound of formula (V)
(M3) 2 (SiF 6 )  (V)

wherein
M3 is H, Na, K, Rb, Cs or NR 1 4 , wherein R 1 is defined as in formula (I);
(C) a compound of formula (VI)
M3PF 6   (VI);

wherein
M3 is defined as in formula (V);
or
(D) a Lewis acid-Lewis base adduct, wherein the Lewis acid is M2F 3
with
M2 is defined as in formula (II).

9. The process of claim 8 , wherein the at least one Lewis acid-Lewis base adduct is selected from the group consisting of
(D1) an adduct of formula (VIIa)
L 1 •sM2F 3    (VIIa)

wherein
M2 is defined as in formula (II);
L 1 is R 2 —O—R 3 or NR 4 R 5 R 6 ;
s is a number in the range of 0.5 to 1.0;
R 2 , R 3 are independently from each other selected from the group consisting of H; C 1-6 alkyl, optionally substituted with halogen or hydroxy; C 3-8 cycloalkyl, optionally substituted with halogen, hydroxy, C 1-6 alkyl, C 1-6 haloalkyl, C 1-6 hydroxyalkyl, C 2-6 alkenyl, C 1-6 alkoxy or C 2-6 alkenoxy; phenyl, optionally substituted with halogen, C 1-6 alkyl, C 1-6 haloalkyl, C 1-6 hydroxyalkyl, C 2-6 alkenyl, C 1-6 alkoxy or C 2-6 alkenoxy; and benzyl, optionally substituted with halogen, C 1-6 alkyl, C 1-6 haloalkyl, C 1-6 hydroxyalkyl, C 2-6 alkenyl, C 1-6 alkoxy or C 2-6 alkenoxy;
or R 2 , R 3 form, together with the oxygen atom they are bonded to, a 3-8-membered ring;
R 4 , R 5 , R 6 are independently from each other selected from the group consisting of H; C 1-6 alkyl, optionally substituted with halogen or hydroxyl; phenyl, optionally substituted with halogen, C 1-6 alkyl, C 1-6 haloalkyl, C 1-6 hydroxyalkyl, C 2-6 alkenyl, C 1-6 alkoxy or C 2-6 alkenoxy; and benzyl, optionally substituted with halogen, C 1-6 alkyl, C 1-6 haloalkyl, C 1-6 hydroxyalkyl, C 2-6 alkenyl, C 1-6 alkoxy or C 2-6 alkenoxy;
or two of R 4 , R 5 , R 6 form, together with the nitrogen atom they are bonded to, a 3-8-membered ring;
(D2) an adduct of formula (VIIb)

wherein
each M2 is independently as defined in formula (II);
t is a number in the range of 0.8 to 2;
G is a single bond or a linking group selected from the group consisting of C 1-6 alkyl, optionally substituted with halogen, hydroxy, C 1-6 alkoxy or C 2-6 alkenoxy; C 2-6 alkenyl, optionally substituted with halogen, hydroxy, C 2-6 alkenyl, C 1-6 alkoxy or C 2-6 alkenoxy; C 3-8 cycloalkyl, optionally substituted with halogen, hydroxy, C 1-6 alkyl, C 1-6 haloalkyl, C 1-6 hydroxyalkyl, C 2-6 alkenyl, C 1-6 alkoxy or C 2-6 alkenoxy; C 4-8 cycloalkenyl, optionally substituted with halogen, hydroxy, C 1-6 alkyl, C 1-6 haloalkyl, C 1-6 hydroxyalkyl, C 2-6 alkenyl, C 1-6 alkoxy or C 2-6 alkenoxy; and C 6-14 aryl, optionally substituted with halogen, hydroxy, C 1-6 alkyl, C 1-6 haloalkyl, C 1-6 hydroxyalkyl, C 2-6 alkenyl, C 1-6 alkoxy or C 2-6 alkenoxy; m and n are independently from each other 0, 1, 2, 3, or 4, under the proviso that m+n≠0, when G is a single bond;
each L 2 is independently selected from the group consisting of NR 7 R 8 and OR 9 , wherein
R 7 , R 8 are independently from each other selected from the group consisting of H, C 1-6 alkyl, optionally substituted with halogen, hydroxy, C 2-6 alkenyl, C 1-6 alkoxy or C 2-6 alkenoxy; phenyl, optionally substituted with halogen, hydroxy, C 1-6 alkyl, C 1-6 haloalkyl, C 1-6 hydroxyalkyl, C 2-6 alkenyl, C 1-6 alkoxy or C 2-6 alkenoxy; and benzyl, optionally substituted with halogen, hydroxy, C 1-6 alkyl, C 1-6 haloalkyl, C 4-6 hydroxyalkyl, C 2-6 alkenyl, C 1-6 alkoxy or C 2-6 alkenoxy;
or R 7 , R 8 form, together with the nitrogen atom they are bonded to, a 3-8-membered ring;
R 9 is selected from the group consisting of H; C 1-6 alkyl; phenyl, optionally substituted with halogen, hydroxy, C 1-6 alkyl, C 1-6 haloalkyl, C 1-6 hydroxyalkyl, C 2-6 alkenyl, C 1-6 alkoxy or C 2-6 alkenoxy; and benzyl, optionally substituted with halogen, hydroxy, C 1-6 alkyl, C 1-6 haloalkyl, C 1-6 hydroxyalkyl, C 2-6 alkenyl, C 1-6 alkoxy or C 2-6 alkenoxy;
and
(D3) an adduct of formula (VIIc)

wherein
each M2 is independently as defined in formula (II);
each L 2 is independently as defined in formula (VIIb);
u is a number in the range of 0.8 to 3.0;
G 1 , G 2

Assignees

• Basf Se

Inventors

• Pagano Sandro
• Hwang Jae Hyung
• Liebscher Ralf
• Prechtl Frank
• Koch Oliver
• Watzenberger Otto
• Klock Volker

Classifications

• C23C30/00

  Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process (C23C26/00, C23C28/00 take precedence) · CPC title

• H01F41/0246

  Manufacturing of magnetic circuits by moulding or by pressing powder (magnetic cores made by moulding or by pressing powder H01F27/255; soft magnetic particles H01F1/20, H01F1/36) · CPC title

• C01B35/06

  Boron halogen compounds · CPC title

• H01F1/36

  in the form of particles {(H01F1/346, H01F1/348 and H01F1/38 take precedence)} · CPC title

• H01F1/26 Primary

  by macromolecular organic substances · CPC title