# US 12,002,609 B2 · Temperature-stable soft-magnetic powder

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- Number: US 12,002,609 B2
- Document ID: US12002609B2
- Status: Granted
- Kind: B2
- Application number: 17/259,368
- Filed: 2019-07-09
- Published: 2021-09-23
- Granted: 2024-06-04
- Earliest claimed: 2018-07-11
- Assignees: BASF SE
- Applicants: BASF SE
- Inventors: Rene Koenig; Rastko Joksimovic; Ingo Muenster; Volker Klock; Jae Hyung Hwang; Moritz Ehrenstein; Eike Hupe; Joachim Nilges; Ralf Liebscher; Christoffer Kieburg
- Web page: https://patentgrep.com/patent/US12002609B2

## CPC

- H01F 1/33: mixtures of metallic and non-metallic particles; metallic particles having oxide skin
- B22F 1/16: Metallic particles coated with a non-metal (coated with lubricating or binding agents or with organic material B22F1/10)
- C22C 33/02: by powder metallurgy
- H01F 1/147: Alloys characterised by their composition {(treatment thereof for enhancing their electromagnetic properties C21D8/12)}
- H01F 1/24: the particles being insulated
- B22F 1/10: Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F 1/102: Metallic powder coated with organic material
- B22F 3/02: Compacting only
- B22F 3/225: {by injection molding}
- B22F 5/00: Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
- B22F 2998/10: Processes characterised by the sequence of their steps
- B22F 2999/00: Aspects linked to processes or compositions used in powder metallurgy
- C22C 2202/02: Magnetic
- H01F 1/26: by macromolecular organic substances
- H01F: MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- B22F: WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER (making alloys by powder metallurgy C22C); APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- C22C: ALLOYS (treatment of alloys C21D, C22F)

## Abstract

A soft-magnetic powder coated with a silicon-based coating, wherein the silicon-based coating comprises at least one fluorine containing composition of formula (I), Si1-0.75cMcO2-0.5cFd (I), wherein c is in the range of 0.01 to 0.5, d is in the range of 0.04 to 2, and M is B or Al.

## Claims

### Claim 1

A process for coating a soft-magnetic powder, the coating comprising at least one fluorine containing composition containing a composition of formula (I):
1.Si1-0.75cMcO2-0.5cFd (I)
wherein
c is in the range of 0.01 to 0.5,
d is in the range of 0.04 to 2, and
M is B or Al,
wherein the soft-magnetic powder is mixed with a silicon-based solution containing at least one soluble fluorination agent, wherein the at least one soluble fluorination agent is a compound of formula (II)
[Q][MF4] (II)
wherein
M is B or Al; and
Q is a cationic group selected from H+, Na+, K+, Rb+, Cs+ or [NR14]+, wherein R1 is independently selected from the group consisting of —H, —C1-12-alkyl, —C2-12-alkenyl, and —C6-18-aryl, each of which may be substituted with at least one group represented by the formula —OR2, wherein R2 is independently selected from —H, —C1-12-alkyl, —C2-12-alkenyl, and —C1-18-aryl.

### Claim 2 (depends on 1)

The process as claimed in claim 1, wherein the soft-magnetic powder is mixed with a silicon-based solution and the at least one soluble fluorination agent is added after at least partial treatment of the soft-magnetic powder with the silicon-based solution.

### Claim 3 (depends on 1)

The process as claimed in claim 1, wherein the at least one soluble fluorination agent is a compound of formula (II)
[Q][MF4] (II)
wherein
M is selected from B, and
Q is cationic group selected from H+ or [NR14]+,
wherein R1 is independently selected from the group consisting of —H, —C1-12-alkyl, —C2-12-alkenyl, and —C6-18-aryl, each of which may be substituted with at least one group represented by the formula —OR2, wherein R2 is independently selected from —H, —C1-12-alkyl, —C2-12-alkenyl, and —C1-18-aryl.

### Claim 4 (depends on 1)

The process as claimed in claim 1, wherein the soluble fluorination agent is selected from the group consisting of HBF4, [NH4][BF4], and [(R4—OR3)x—NH3-x][BF4],
wherein
R3 represents a group of the formula —(CnH2n+p)—;
n is an integer from 1 to 6,
p is an integer selected from 0 and −2,
R4 is selected from —H or —(CmH2m+q)—CH3,
m is an integer from 0 to 6,
q is an integer selected from 0 and −2,
with the proviso that when m=0 then q=0, and
x is an integer selected from 1 to 3.

### Claim 5 (depends on 1)

The process as claimed in claim 1, wherein the soluble fluorination agent has a solubility in ethanol at 0° C. of at least 15 wt.-%.

### Claim 6 (depends on 1)

The process as claimed in claim 1, wherein the soluble fluorination agent is added during treatment with the silicon-based solution or immediately after the treatment with the silicon-based solution.

### Claim 7 (depends on 1)

The process as claimed in claim 1, wherein 0.1 to 10 mmol of fluorination agent per kg of soft-magnetic powder is added to the silicon-based solution.

### Claim 8 (depends on 1)

The process as claimed in claim 1, wherein the silicon-based solution contains a silicon alkoxide, which is added in one or more steps to the reaction mixture.

### Claim 9

A soft-magnetic powder coated with a silicon-based coating, wherein the silicon-based coating comprises at least one fluorine containing composition of formula (I):
Si1.075-cMcO2-0.5cFd (I)
wherein
c is in the range of 0.01 to 0.5,
d is in the range of 0.04 to 2,
the index c and the index d have the following relation: d=4c and
M is B or Al,
wherein the silicon-based coating comprises between greater than 5 to 45 wt.-% of the at least one fluorine containing composition of formula (I).

### Claim 10 (depends on 9)

The soft-magnetic powder as claimed in claim 9, comprising at least one fluorine containing composition of formula (I), wherein M is B.

### Claim 11 (depends on 9)

The soft-magnetic powder as claimed in claim 9, wherein the silicon-based coating comprises 20 to 35 wt.-%, of the at least one fluorine containing composition of formula (I).

### Claim 12 (depends on 9)

The soft-magnetic powder as claimed in claim 9, wherein the fluorine component of the fluorine containing composition is embedded within a SiO2-matrix and/or bonded to a surface of a SiO2-coating.

### Claim 13 (depends on 9)

The soft-magnetic powder as claimed in claim 9, wherein the silicon-based coating has an average thickness of 2 to 100 nm.

### Claim 14 (depends on 9)

The soft-magnetic powder of as claimed in claim 9, wherein the soft magnetic powder comprises 0.1 to 10 wt.-% of the silicon based coating based on the total weight of the soft magnetic powder.

### Claim 15 (depends on 9)

An electronic component comprising the soft-magnetic powder as claimed in claim 9.
