CN103268799A - Iron nitrogen boron nano-crystalline soft magnetic material and preparation method thereof - Google Patents

Iron nitrogen boron nano-crystalline soft magnetic material and preparation method thereof Download PDF

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CN103268799A
CN103268799A CN2013101581002A CN201310158100A CN103268799A CN 103268799 A CN103268799 A CN 103268799A CN 2013101581002 A CN2013101581002 A CN 2013101581002A CN 201310158100 A CN201310158100 A CN 201310158100A CN 103268799 A CN103268799 A CN 103268799A
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唐建成
卓海鸥
叶楠
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Nanchang University
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Nanchang University
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Abstract

The invention discloses an iron nitrogen boron nano-crystalline soft magnetic material and a preparation method thereof. The method includes the steps: (1) preparing master batches according to Fe92B8 alloying constituents, using vacuum melting for preparing alloy ingots, and then preparing Fe92B8 amorphous strips on a vacuum rapid-quenching furnace; (2) placing the Fe92B8 amorphous strips prepared in the step (1) into a tubular atmosphere furnace, and then performing nitriding in mixed gas which comprises, by volume fraction, 92% of NH3 and 8% of H2, for 30-90min at the temperature of 580-620 DEG C; (3) performing homogenizing annealing for 30-60min at the temperature of 580-620 DEG C; (4) cooling test samples in the step (3) to the room temperature by the aid of a water quenching method; and (5) subjecting the water-quenched samples in the step (4) to aging treatment for 1-2h at the temperature of 150-200 DEG C. The prepared soft magnetic material is excellent in performance, and resistivity, saturation magnetostriction rate, saturation magnetization, coercivity, initial permeability and relaxation frequency thereof are 246muomegacm, 2.52X10<-6>, 2.35T, 11.4A/m, 9.1X10<4> and 4.1X10<4>Hz respectively.

Description

A kind of iron nitrogen boron nano crystal soft magnetic material and preparation method thereof
Technical field
The invention belongs to soft magnetic material and preparation field.
Background technology
The iron based nano crystal soft magnetic material becomes one of present soft magnetic material of studying the most popularly because having high saturation magnetization and high initial permeability.The microscopic structure of nano crystal soft magnetic material is made up of Fe-based amorphous matrix and the nano magnetic particle that is distributed in the noncrystal substrate.At present, study maximum iron based nano crystal soft magnetic materials and comprise Finemet (Fe-Si-B-Nb-Cu) alloy, Nanoperm (Fe-Zr-B-Cu) alloy and Hitperm ((Fe, Co)-Zr-B-Cu) alloy, in these alloys, the nano magnetic particle that is distributed in the noncrystal substrate is respectively α -Fe (Si), α -Fe and α -Fe (Co) particle.Improve saturation magnetization and resistivity and be and improve the effective method of iron based nano crystal material softer magnetic property.
α " Fe 16N 2Because the saturation magnetization that has up to 2.83T causes extensive concern. α " Fe 16N 2Preparation process comprise nitrogenize, martensite phase transformation and 3 steps of ordering pransition, nitrogenize is α The process of-Fe nitriding and homogenizing in nitriding atmosphere its objective is to be met α " Fe 16N 2The alloy that composition requires.The martensite phase transformation is satisfied α " Fe 16N 2The alloy fast quenching that composition requires obtains α '-Fe 8The martensitic process of N.Ordering pransition is α '-Fe 8N martensite obtains in the proper temperature timeliness α " Fe 16N 2Process.By control α -Fe nitrogenize, martensite phase transformation and ordering pransition process are prepared and are contained α " Fe 16N 2Film and block materials obtained paying close attention to widely with the soft magnet performance that improves material.
α " Fe 16N 2High saturation magnetization makes with the high resistivity that Yin Qi gap crystal structure mutually produces α " Fe 16N 2Tool application prospect widely in iron based nano crystal soft magnetism band.
Summary of the invention
The invention provides a kind of α " Fe 16N 2Nano particle is distributed in the Fe-N-B nano-crystal soft-magnetic band on the noncrystal substrate, and nano-crystalline Fe-N-B band is a kind of iron based nano crystal soft magnetic material that has excellent magnetic characteristics.The present invention also provides the preparation technology of this nano crystal soft magnetic material.
A kind of iron nitrogen boron nano crystal soft magnetic material of the present invention has following chemical molecular formula: Fe 92B 8
The step of preparation process that the present invention adopts is as follows:
(1) presses Fe 92B 8Alloying component configuration masterbatch adopts the method for vacuum melting to prepare alloy cast ingot, prepares Fe at vacuum quick quenching furnace then 92B 8Amorphous ribbon.
(2) nitrogenize: with prepared Fe in the step (1) 92B 8Amorphous ribbon places the tubular type atmosphere furnace to carry out nitrogenize, and nitrogenize is to be 92% NH in volume fraction 3With volume fraction be 8% H 2Mist in carry out, nitriding temperature is 580 ~ 620 ℃, nitridation time is 30 ~ 90min.
(3) homogenizing annealing: the temperature of homogenizing annealing is the same with nitriding temperature in the step (2), and the time is 30 ~ 60min.
(4) quench: the sample cool to room temperature of the method that adopts shrend after with homogenizing annealing in the step (3).
(5) Ageing Treatment: water-quenched sample in the step (4) is carried out Ageing Treatment at 150 ~ 200 ℃, and the time is 1 ~ 2h.
The nano-crystalline Fe of above-mentioned technology preparation 84.6N 7.8B 7.4Band is a kind of α " Fe 16N 2Nano particle is distributed in the nano-crystal soft-magnetic band on the noncrystal substrate, has utilized α " Fe 16N 2High magnetic moment and the nano particle of resistivity in nano crystal soft magnetic material Nanoperm, Finemet and the Hitperm α -Fe, α -Fe (Si) and α The advantage of-Fe (Co), nano-crystalline Fe 84.6N 7.8B 7.4Band becomes a kind of soft magnetic material of function admirable, and its resistivity, saturation magnetostriction rate, saturation magnetization, coercive force, initial permeability and relaxation frequency are respectively 246 μ ΩCm, 2.52 * 10 -6, 2.35T, 11.4A/m, 9.1 * 10 4With 4.1 * 10 4Hz.
Description of drawings
Fig. 1 is embodiment 2 X-ray diffraction spectrum of (b) after (a) and Ageing Treatment after the shrend.
Fig. 2 is amorphous Fe 92B 8Band and nano-crystalline Fe 84.6N 7.8B 7.4The magnetostriction curve of band.
Embodiment
The present invention will be described further by following examples, but protection scope of the present invention is not limited thereto.
Embodiment 1.
Take by weighing straight iron powder 644g, boron powder 11g adopts the method for vacuum melting to prepare Fe 92B 8Alloy cast ingot, the Fe of the method preparation of usefulness single roller rapid quenching then 92B 8The thick 20 μ m of amorphous ribbon, wide 10mm is at NH 3(volume fraction is 92%) and H 2Carry out nitrogenize in the mist of (volume fraction is 8%), nitriding temperature is 600 ℃, and nitridation time is 30min.Then at 600 ℃ of following homogenizing annealing 30min.The sample cool to room temperature of the method that adopts shrend after with homogenizing annealing.Subsequently, at 150 ℃ water-quenched sample is carried out Ageing Treatment, the time is 120min.The gap phase composition of the nanocrystalline band that obtains is α -Fe+ α " Fe 16N 2
Embodiment 2.
Take by weighing straight iron powder 644g, boron powder 11g adopts the method for vacuum melting to prepare Fe 92B 8Alloy cast ingot adopts the Fe of the method preparation of single roller rapid quenching then 92B 8The thick 20 μ m of amorphous ribbon, wide 10mm is at NH 3(volume fraction is 92%) and H 2Carry out nitrogenize in the mist of (volume fraction is 8%), nitriding temperature is 600 ℃, and nitridation time is 45min.Then at 600 ℃ of following homogenizing annealing 30min.The sample cool to room temperature of the method that adopts shrend after with homogenizing annealing.Subsequently, at 150 ℃ water-quenched sample is carried out Ageing Treatment, the time is 120min.Sample after the shrend and the X-ray diffraction spectrum after the Ageing Treatment see accompanying drawing 1 (a) and (b) respectively.The nano-crystalline Fe that obtains 84.6N 7.8B 7.4The gap phase composition of band is α " Fe 16N 2, crystallite dimension is 18nm, and its magnetostriction curve is seen accompanying drawing 2, and the resistivity of this nanocrystalline band, saturation magnetostriction rate, saturation magnetization, coercive force, initial permeability and relaxation frequency are respectively 246 μ ΩCm, 2.52 * 10 -6, 2.35T, 11.4A/m, 9.1 * 10 4With 4.1 * 10 4Hz.
Embodiment 3.
Take by weighing straight iron powder 644g, boron powder 11g adopts the method for vacuum melting to prepare Fe 92B 8Alloy cast ingot adopts the Fe of the method preparation of single roller rapid quenching then 92B 8The thick 20 μ m of amorphous ribbon, wide 10mm is at NH 3(volume fraction is 92%) and H 2Carry out nitrogenize in the mist of (volume fraction is 8%), nitriding temperature is 600 ℃, and nitridation time is 90min.Then at 600 ℃ of following homogenizing annealing 30min.The sample cool to room temperature of the method that adopts shrend after with homogenizing annealing.Subsequently, at 150 ℃ water-quenched sample is carried out Ageing Treatment, the time is 120min.The gap phase composition of the nanocrystalline band that obtains is α " Fe 16N 2+ Fe 4N.
Embodiment 4.
Take by weighing straight iron powder 644g, boron powder 11g adopts the method for vacuum melting to prepare Fe 92B 8Alloy cast ingot adopts the Fe of the method preparation of single roller rapid quenching then 92B 8The thick 20 μ m of amorphous ribbon, wide 10mm is at NH 3(volume fraction is 92%) and H 2Carry out nitrogenize in the mist of (volume fraction is 8%), nitriding temperature is 620 oC, nitridation time are 30min.Then 620 oHomogenizing annealing 30min under the C.The sample cool to room temperature of the method that adopts shrend after with homogenizing annealing.Subsequently, 150 oThe water-quenched sample of C carries out Ageing Treatment, and the time is 120min.The gap phase composition of the nanocrystalline band that obtains is α -Fe+ α " Fe 16N 2
Embodiment 5.
Take by weighing straight iron powder 644g, boron powder 11g adopts the method for vacuum melting to prepare Fe 92B 8Alloy cast ingot adopts the Fe of the method preparation of single roller rapid quenching then 92B 8The thick 20 μ m of amorphous ribbon, wide 10mm is at NH 3(volume fraction is 92%) and H 2Carry out nitrogenize in the mist of (volume fraction is 8%), nitriding temperature is 620 ℃, and nitridation time is 45min.Then at 620 ℃ of following homogenizing annealing 30min.The sample cool to room temperature of the method that adopts shrend after with homogenizing annealing.Subsequently, at 150 ℃ water-quenched sample is carried out Ageing Treatment, the time is 120min.The gap phase composition of the nanocrystalline band that obtains is α " Fe 16N 2, crystallite dimension is 31nm.
Embodiment 6.
Take by weighing straight iron powder 644g, boron powder 11g adopts the method for vacuum melting to prepare Fe 92B 8Alloy cast ingot adopts the Fe of the method preparation of single roller rapid quenching then 92B 8The thick 20 μ m of amorphous ribbon, wide 10mm is at NH 3(volume fraction is 92%) and H 2Carry out nitrogenize in the mist of (volume fraction is 8%), nitriding temperature is 620 ℃, and nitridation time is 90min.Then at 620 ℃ of following homogenizing annealing 30min.The sample cool to room temperature of the method that adopts shrend after with homogenizing annealing.Subsequently, at 150 ℃ water-quenched sample is carried out Ageing Treatment, the time is 120min.The gap phase composition of the nanocrystalline band that obtains is α " Fe 16N 2+ Fe 4N.
Table 1 is the crystallite dimension of nitriding temperature, nitridation time, nitrogen content, phase composition and the nano particle of nanocrystalline band.
Table 1

Claims (2)

1. an iron nitrogen boron nano crystal soft magnetic material is characterized in that having following chemical molecular formula: Fe 92B 8
2. the preparation method of the described iron nitrogen of claim 1 boron nano crystal soft magnetic material is characterized in that as follows:
(1) presses Fe 92B 8Alloying component configuration masterbatch adopts the method for vacuum melting to prepare alloy cast ingot, prepares Fe at vacuum quick quenching furnace then 92B 8Amorphous ribbon;
(2) with prepared Fe in the step (1) 92B 8Amorphous ribbon places the tubular type atmosphere furnace to carry out nitrogenize, and nitrogenize is to be 92% NH in volume fraction 3With volume fraction be 8% H 2Mist in carry out, nitriding temperature is 580 ~ 620 ℃, nitridation time is 30 ~ 90min;
Homogenizing annealing 30 ~ 60min under (3) 580 ~ 620 ℃ of conditions;
(4) the sample cool to room temperature of the method that adopts shrend after with homogenizing annealing in the step (3);
(5) water-quenched sample in the step (4) is carried out Ageing Treatment at 150 ~ 200 ℃, the time is 1 ~ 2h.
CN2013101581002A 2013-05-02 2013-05-02 Iron nitrogen boron nano-crystalline soft magnetic material and preparation method thereof Pending CN103268799A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105499561A (en) * 2015-12-09 2016-04-20 西南交通大学 Preparing method of magnetic carbon nano tubes
CN106165027A (en) * 2014-03-28 2016-11-23 明尼苏达大学董事会 Comprise the iron nitride magnetic material of the nano-particle of coating
CN107919201A (en) * 2013-02-07 2018-04-17 明尼苏达大学董事会 Nitrided iron permanent magnet and the technology for forming nitrided iron permanent magnet
WO2023132141A1 (en) * 2022-01-06 2023-07-13 株式会社日立製作所 Soft magnetic iron alloy plate, and iron core and rotating electric machine utilizing said soft magnetic iron alloy plate
WO2023195226A1 (en) * 2022-04-06 2023-10-12 株式会社日立製作所 Soft magnetic iron alloy plate, production method for said soft magnetic iron alloy plate, and iron core and rotary electrical machine using said soft magnetic iron alloy plate

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JPH04293701A (en) * 1991-03-22 1992-10-19 Mitsubishi Materials Corp Production of soft magnetic powder having high saturation magnetic flux density

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Title
邰忠智: "纳米晶Fe-N-B 软磁条带的制备", 《中国有色金属学报》, vol. 20, no. 4, 30 April 2010 (2010-04-30) *

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107919201A (en) * 2013-02-07 2018-04-17 明尼苏达大学董事会 Nitrided iron permanent magnet and the technology for forming nitrided iron permanent magnet
US10692635B2 (en) 2013-02-07 2020-06-23 Regents Of The University Of Minnesota Iron nitride permanent magnet and technique for forming iron nitride permanent magnet
US11217371B2 (en) 2013-02-07 2022-01-04 Regents Of The University Of Minnesota Iron nitride permanent magnet and technique for forming iron nitride permanent magnet
CN106165027A (en) * 2014-03-28 2016-11-23 明尼苏达大学董事会 Comprise the iron nitride magnetic material of the nano-particle of coating
EP3123484A4 (en) * 2014-03-28 2017-06-14 Regents of the University of Minnesota Iron nitride magnetic material including coated nanoparticles
US11195644B2 (en) 2014-03-28 2021-12-07 Regents Of The University Of Minnesota Iron nitride magnetic material including coated nanoparticles
CN105499561A (en) * 2015-12-09 2016-04-20 西南交通大学 Preparing method of magnetic carbon nano tubes
WO2023132141A1 (en) * 2022-01-06 2023-07-13 株式会社日立製作所 Soft magnetic iron alloy plate, and iron core and rotating electric machine utilizing said soft magnetic iron alloy plate
WO2023195226A1 (en) * 2022-04-06 2023-10-12 株式会社日立製作所 Soft magnetic iron alloy plate, production method for said soft magnetic iron alloy plate, and iron core and rotary electrical machine using said soft magnetic iron alloy plate

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Application publication date: 20130828