CN103121666B - Method for preparing Fe4-xMxN (M=Ni,Co) soft-magnetism powder with favorable electromagnetic properties - Google Patents
Method for preparing Fe4-xMxN (M=Ni,Co) soft-magnetism powder with favorable electromagnetic properties Download PDFInfo
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- CN103121666B CN103121666B CN201310042674.3A CN201310042674A CN103121666B CN 103121666 B CN103121666 B CN 103121666B CN 201310042674 A CN201310042674 A CN 201310042674A CN 103121666 B CN103121666 B CN 103121666B
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Abstract
The invention relates to a method for preparing Fe4-xMxN (M=Ni,Co) soft-magnetism powder with favorable electromagnetic properties, belonging to the field of new materials. According to the method, FeNi and FeCo alloy powders used as raw materials are nitridized in an NH3 and H2 atmosphere by a solid-gas reaction method. The heating process adopts a two-step method and comprises the following steps: eliminating residual stress generated in the raw material powder preparation process at high temperature, and enabling multiple phases in the raw material powder to form a single gamma phase at high temperature; and nitridizing at low temperature to obtain the Fe4-xMxN (M=Ni,Co) three-element iron nitrogen compound, wherein 0.01<=x<=3 in the Fe4-xNixN, and 0.01<=y<=0.4 in the Fe4-yCoyN. The product powder has the advantages of favorable particle dispersity (the average particle size is 5 mu m), high saturation magnetiation and low coercive force.
Description
Technical field
The present invention relates to one and prepare the 3rd element Ni, Co doped F e
4n material obtains Fe
4-xm
xthe method of N (M=Ni, Co) soft magnetism powder, belongs to field of new.
Background technology
In recent years, along with the development of electronics industry and wireless telecommunications, the electronic and electrical equipment of various numeral, high frequency as computer, mobile phone universal daily life rapidly, they while bringing convenience to people's life again to the electromagnetic wave of a large amount of different frequency of space radiation.Electromagnetic wave not only can to the healthy generation harm of people, can produce interference, can affect the normal use of electronic and electrical equipment between the electromagnetic wave of different frequency simultaneously.The electromagnetic pollution produced by electromagnetic wave has caused attention and the concern of people gradually.Fe
4owing to having excellent magnetic performance, (saturation magnetization is 190Am to N material
2/ kg), good chemical stability and higher mechanical strength and be supposed to become a kind of outstanding artificial electromagnetic medium.And Fe
4the resistivity of N material is little, and the problems such as skin depth is little, poor processability limit its practical application.
To Fe
4the 3rd element that adulterates in N material improves its soft magnet performance and a kind of effective approach of processing characteristics.3rd Elements Atom replaces Fe
4the Fe atom of the vertex position in N anti-perovskite structure will inevitably cause saturation magnetization M
sreduction, and the saturation magnetization M of the initial permeability of material and material
ssquare to be directly proportional.Choose for material after ensureing doping has higher magnetic conductivity doped chemical there is ferromagnetic transiting group metal elements Ni and Co.Current preparation Fe
4-xm
xthe method of N (M=Ni, Co) ternary iron nitride mainly contains following three kinds:
1, oxalates nitriding.First chemical coprecipitation process is used to obtain the oxalates powder containing Fe ion, Ni ion or Co ion.Then by the NH of this oxalate precursor at certain volume ratio
3and H
2mixed atmosphere in nitrogenize, the ratio of nitriding temperature metal ion shared by Ni ion and Co ion and determining.
2, mechanical alloying method.Before this at NH
3nitrogen Fe powder obtains Fe
2n powder, then by Fe
2n powder and high-purity Fe powder and want the metal powder of doped chemical to be put in high-energy ball milling tank according to certain stoichiometric proportion to be filled with inert gas high speed ball milling and to obtain Fe
4-xm
xn powder.
3, magnetron sputtering embrane method.Adopt the composition target of Fe target and Ni target (or Co target) as target, by Ni(or Co on control Fe target) amount change the content of Ni in film.Sputter the mist that atmosphere used is argon gas and nitrogen, changed the content of N in film by the dividing potential drop controlling nitrogen.
Said method is mainly used by people to study Fe in the lab
4-xm
xthe problems such as the different element of the crystal structure of N (M=Ni, Co) ternary nitride, Occupation, hyperfine magnetic field, homogeneity can shift, complicated process of preparation, is not easy to produce in enormous quantities, meanwhile, for Fe
4-xm
xthe research that N (M=Ni, Co) material is used for artificial electromagnetic medium aspect is few.
Summary of the invention
The invention provides one and prepare ternary iron nitride Fe
4-xm
xthe method of N (M=Ni, Co) soft magnetism powder, the features such as it is simple and easy to do that it has preparation technology, and product controllability is strong, this soft magnetism powder has excellent electromagnetic performance simultaneously, and can become a kind of outstanding artificial electromagnetic medium, tool has significant practical applications.
Fe
4-xm
xn (M=Ni, Co) soft magnetism raw powder's production technology is characterized in that comprising following step:
1. Fe is prepared
4-xm
xthe raw material that N (M=Ni, Co) soft magnetism powder adopts is FeNi, FeCo alloy powder, and this alloy powder can by carbonyl process, atomization, and mechanical alloying method or physical gas-phase deposite method obtain;
2. material powder is evenly laid in alumina crucible, crucible is put in after in vacuum tube furnace and vacuumizes process, pass into NH afterwards
3and H
2mist, then vacuum tube furnace is warmed up to a temperature a period of time;
3. control temperature in 1-2h from step 2. temperature drop to nitriding temperature, insulation a period of time, regulate NH simultaneously
3and H
2volume ratio control nitrogen atom concentration in boiler tube;
4. nitrogenize cools with stove after terminating, and drops to after uniform temperature take out powder sample until stove.
Preferred steps 1. in Raw FeNi alloy powder the scope of the atomic percent w of Ni be 0.25%≤w≤75%, in FeCo alloy powder, the scope of the atomic percent w of Co is 0.25%≤w≤10%;
Preferred steps 2. middle thermal creep stress is single γ phase for making adopted alloy under this temperature conditions, when raw material is FeNi alloyed powder, temperature range is in Fe-Ni binary phase diagraml shown in phase change line ABC(accompanying drawing 1) more than 10 DEG C-100 DEG C, when raw material is FeCo alloyed powder, temperature range is in Fe-Co binary phase diagraml shown in phase change line DE(accompanying drawing 2) more than 10 DEG C-100 DEG C, temperature retention time is 0.5h-2h.NH in mist
3volume fraction within the scope of 0-50%.
Preferred steps 3. middle nitriding temperature is in a temperature range of below the phase change line of selected alloy, when raw material is FeNi alloyed powder, nitriding temperature scope is that in Fe-Ni binary phase diagraml, phase change line ABC(accompanying drawing 1 is shown) 10 DEG C-300 DEG C below, when raw material is FeCo alloyed powder, nitriding temperature scope is that in Fe-Co binary phase diagraml, phase change line DE(accompanying drawing 2 is shown) 300 DEG C-500 DEG C below, temperature retention time is 3h-8h.NH in mist
3volume fraction within the scope of 50%-100%.
The preferred steps temperature that 4. middle sample is come out of the stove is less than 300 DEG C.
Technical scheme of the present invention is: with FeNi, FeCo alloy powder for raw material, adopts solid slope technology method at NH
3and H
2mixed atmosphere in nitrogenize, by the concentration regulating the throughput of two kinds of gases to control nitrogen-atoms in boiler tube.Heating process adopts two-step method, first at Fe-Ni, the single-phase phase change line to two phase in version (the ABC line in accompanying drawing 1 in Fe-Co binary phase diagraml, DE line in accompanying drawing 2) more than 10 DEG C-100 DEG C insulation a period of times, one is eliminate the residual stress produced in material powder preparation process, two is that make to exist in material powder heterogeneous at high temperature forms single γ phase, makes the homogenization of thing phase, NH in atmosphere in this process
3volume fraction within the scope of 0-50%.Nitrogenize at suitable nitridation reaction temperature again, concrete temperature range is below phase change line ABC 10 DEG C-300 DEG C in Fe-Ni binary phase diagraml, below phase change line DE 300 DEG C-500 DEG C in Fe-Co binary phase diagraml, this stage is the nitridation reaction stage, NH in atmosphere in this process
3volume fraction within the scope of 50%-100%.
Advantage of the present invention is: be that raw material adopts two-step method to add hot preparation Fe with alloy powder
4-xm
xthe advantage of the technique of N (M=Ni, Co) soft magnetism powder is that doped chemical content is controlled, according to requirements more easily can regulate the ratio of each component in iron nitride, can improve the purity of ternary nitride in product.
Effect of the present invention is:
The invention provides one and prepare ternary iron nitride Fe
4-xm
xthe method of N (M=Ni, Co) soft magnetism powder, its main efficacy results has:
1, Fe is synthesized
4-xm
xn (M=Ni, Co) ternary iron nitride, wherein Fe
4-xni
xin N, the scope of x is 0.01≤x≤3, Fe
4-yco
yin N, the scope of y is 0.01≤y≤0.4.
2, the good dispersion of powder product particle, size is homogeneous, and average grain diameter is 5 μm.
3, the Fe prepared
4-xm
xn (M=Ni, Co) ternary iron nitride has excellent magnetic performance, high saturation magnetization and low coercivity.
Accompanying drawing explanation
Fig. 1: Fe-Ni binary alloy phase diagram;
Fig. 2: Fe-Co binary alloy phase diagram;
Fig. 3: the X ray diffracting spectrum of nitrogenize product in embodiment 1;
Fig. 4: the hysteresis curve figure of nitrogenize product in embodiment 1;
Fig. 5: the X ray diffracting spectrum of nitrogenize product in embodiment 2;
Fig. 6: the X ray diffracting spectrum of nitrogenize product in embodiment 5;
Fig. 7: the scanning electron microscopic picture of nitrogenize product in embodiment 5;
Fig. 8: the hysteresis curve figure of nitrogenize product in embodiment 5.
Detailed description of the invention
Below in conjunction with drawings and Examples, the invention will be further described, but the present invention is not limited to following examples.
Embodiment 1: raw material is FeNi alloy powder prepared by carbonyl process, atomic percent shared by Ni element is 0.25%, the powder sample taking 3g is put in alumina crucible, in vacuum tube furnace, adopt two-step method to heat, first rise to 860 DEG C with the heating rate of 10 DEG C/min, at 860 DEG C of insulation 30min.Only H is passed in this process
2, H
2throughput be 200ml/min.In 2h, temperature drops to 550 DEG C from 860 DEG C afterwards, at 550 DEG C of insulation 3h, only passes into NH in this process
3, NH
3throughput be 200ml/min.Afterwards with stove cooling, when temperature drops to below 300 DEG C, from boiler tube, take out sample.
Through XRD determining, nitrogenize generates Fe
3.99ni
0.01n phase, XRD collection of illustrative plates is as shown in Figure 3. and after nitrogenize, the particle diameter of powder particle is 5 μm.As shown in Figure 4, saturation magnetization is 182emu/g to the hysteresis curve recorded by vibrating specimen magnetometer, and coercivity is 17Oe.
Embodiment 2: raw material is FeNi alloy powder prepared by carbonyl process, atomic percent shared by Ni element is 5%, and the powder sample taking 4g is put in alumina crucible, adopts two-step method to heat in vacuum tube furnace, first rise to 900 DEG C with the heating rate of 10 DEG C/min, at 900 DEG C of insulation 1h.H is passed in this process
2and NH
3mist, H
2and NH
3volume ratio be 1:1.In 1.5h, temperature drops to 500 DEG C from 800 DEG C afterwards, at 500 DEG C of insulation 5h, passes into H in this process
2and NH
3mist, throughput is 200ml/min.Afterwards with stove cooling, when temperature drops to below 300 DEG C, from boiler tube, take out sample.
Through XRD determining, nitrogenize generates Fe
3.8ni
0.2n phase, XRD collection of illustrative plates as shown in Figure 5.After nitrogenize, the particle diameter of powder particle is 5 μm.The saturation magnetization being recorded product by vibrating specimen magnetometer is 177emu/g, and coercivity is 38Oe.
Embodiment 3: raw material is FeNi alloy powder prepared by carbonyl process, atomic percent shared by Ni element is 30%, and the powder sample taking 4g is put in alumina crucible, adopts two-step method to heat in vacuum tube furnace, first rise to 600 DEG C with the heating rate of 10 DEG C/min, at 600 DEG C of insulation 1h.H is passed in this process
2and NH
3mist, H
2and NH
3volume ratio be 2:1.In 1h, temperature drops to 400 DEG C from 600 DEG C afterwards, at 400 DEG C of insulations 5h, H in this process
2and NH
3mist, H
2and NH
3volume ratio be 1:2.Afterwards with stove cooling, when temperature drops to below 300 DEG C, from boiler tube, take out sample.
Through XRD determining, nitrogenize generates Fe
2.8ni
1.2n phase, after nitrogenize, the particle diameter of powder particle is 5 μm.
Embodiment 4: raw material is FeNi alloy powder prepared by carbonyl process, atomic percent shared by Ni element is 40%, and the powder sample taking 4g is put in alumina crucible, adopts two-step method to heat in vacuum tube furnace, first rise to 500 DEG C with the heating rate of 10 DEG C/min, at 500 DEG C of insulation 2h.H is passed in this process
2and NH
3mist, H
2and NH
3volume ratio be 4:3.In 1.5h, temperature drops to 350 DEG C from 500 DEG C afterwards, at 350 DEG C of insulation 6h, passes into H in this process
2and NH
3mist, throughput is 200ml/min.Afterwards with stove cooling, when temperature drops to below 300 DEG C, from boiler tube, take out sample.
Through XRD determining, nitrogenize generates Fe
2.4ni
1.6n phase, after nitrogenize, the particle diameter of powder particle is 5 μm.The saturation magnetization being recorded product by vibrating specimen magnetometer is 100emu/g, and coercivity is 10Oe.
Embodiment 5: raw material is FeNi alloy powder prepared by carbonyl process, atomic percent shared by Ni element is 75%, and the powder sample taking 3g is put in alumina crucible, adopts two-step method to heat in vacuum tube furnace, first rise to 600 DEG C with the heating rate of 10 DEG C/min, at 600 DEG C of insulation 1h.Only H is passed in this process
2, H
2throughput be 200ml/min.In 1h, temperature drops to 450 DEG C from 600 DEG C afterwards, at 450 DEG C of insulation 8h, only passes into NH in this process
3, NH
3throughput be 200ml/min.Afterwards with stove cooling, when temperature drops to below 300 DEG C, from boiler tube, take out sample.
Through XRD determining, nitrogenize generates FeNi
3n phase, XRD collection of illustrative plates as shown in Figure 6.After nitrogenize, the microscopic appearance of powder particle as shown in Figure 7, and average grain diameter is 5 μm.This Magnaglo saturation magnetization be 72.7emu/g, coercivity is 29.5Oe, and hysteresis curve is as shown in Figure 8.
Embodiment 6: raw material is FeCo alloy powder, atomic percent shared by Co element is 10%, and the powder sample taking 3g is put in alumina crucible, adopts two-step method to heat in vacuum tube furnace, first rise to 930 DEG C with the heating rate of 10 DEG C/min, at 930 DEG C of insulation 0.5h.H is passed in this process
2and NH
3, H
2and NH
3volume ratio be 5:3.In 1h, temperature drops to 620 DEG C from 930 DEG C afterwards, at 620 DEG C of insulation 5h, passes into NH in this process
3and H
2mist, H
2and NH
3volume ratio be 3:5.Afterwards with stove cooling, when temperature drops to below 300 DEG C, from boiler tube, take out sample.
Through XRD determining, nitrogenize generates Fe
3.6co
0.4n phase, after nitrogenize, the particle diameter of powder particle is 5 μm, this Magnaglo saturation magnetization be 159emu/g.
Embodiment 7: raw material is FeCo alloy powder, atomic percent shared by Co element is 5%, the powder sample taking 3g is put in alumina crucible, in vacuum tube furnace, adopt two-step method to heat, first rise to 950 DEG C with the heating rate of 10 DEG C/min, at 950 DEG C of insulation 2h, in this process, only pass into H
2, H
2throughput be 200ml/min.In 1.5h, temperature drops to 500 DEG C from 950 DEG C afterwards, at 500 DEG C of insulation 3h, passes into NH in this process
3and H
2mist, H
2and NH
3volume ratio be 1:1.Afterwards with stove cooling, when temperature drops to below 300 DEG C, from boiler tube, take out sample.
Through XRD determining, nitrogenize generates Fe
3.8co
0.2n phase, after nitrogenize, the particle diameter of powder particle is 5 μm, this Magnaglo saturation magnetization be 172emu/g.
Embodiment 8: raw material is FeCo alloy powder, and the percentage shared by Co element is 0.25%, the powder sample taking 4g is put in alumina crucible, in vacuum tube furnace, adopt two-step method to heat, first rise to 1020 DEG C with the heating rate of 10 DEG C/min, at 1020 DEG C of insulation 1h, in this process, pass into H
2and NH
3mist, H
2and NH
3volume ratio be 1:1.In 2h, temperature drops to 420 DEG C from 1020 DEG C afterwards, at 420 DEG C of insulation 8h, only passes into NH in this process
3, NH
3throughput be 200ml/min.Afterwards with stove cooling, when temperature drops to below 300 DEG C, from boiler tube, take out sample.
Through XRD determining, nitrogenize generates Fe
3.99co
0.01n phase, after nitrogenize, the particle diameter of powder particle is 5 μm.This Magnaglo saturation magnetization be 181emu/g.
Claims (1)
1. a preparation method for ternary iron nitride, this ternary iron nitride chemical formula is Fe
4-xm
xn, M are Ni or Co element, this ternary iron nitride by FeNi or FeCo alloy powder at NH
3and H
2atmosphere in adopt two-step method to add tropical resources to obtain, wherein Fe
4-xni
xin N, the scope of x is 0.01≤x≤3, Fe
4-yco
yin N, the scope of y is 0.01≤y≤0.4;
It is characterized in that concrete steps are:
1. in raw material FeNi alloy powder, the scope of the atomic percent w of Ni is 0.25%≤w≤75%, in FeCo alloy powder, the scope of the atomic percent w of Co is 0.25%≤w≤10%, this alloy powder by carbonyl process, atomization, mechanical alloying method or physical gas-phase deposite method obtain;
2. material powder is evenly laid in alumina crucible, crucible is put in after in vacuum tube furnace and vacuumizes process, pass into NH afterwards
3and H
2mist, wherein NH
3volume fraction within the scope of 0-50%, then vacuum tube furnace is made to be heated to a temperature 0.5h-2h, when raw material is FeNi alloyed powder, this temperature range is in Fe-Ni binary phase diagraml more than phase change line 10 DEG C-100 DEG C, and when raw material is FeCo alloyed powder, this temperature range is in Fe-Co binary phase diagraml more than phase change line 10 DEG C-100 DEG C;
3. control temperature in 1-2h from step 2. temperature drop to nitriding temperature, when raw material is FeNi alloyed powder, nitriding temperature scope is in Fe-Ni binary phase diagraml below phase change line 10 DEG C-300 DEG C, when raw material is FeCo alloyed powder, nitriding temperature scope is in Fe-Co binary phase diagraml below phase change line 300 DEG C-500 DEG C, under nitriding temperature, be incubated 3h-8h, the atmosphere in this process is NH
3and H
2mist, wherein NH
3volume fraction within the scope of 50%-100%;
4. nitrogenize cools with stove after terminating, and drops to after below 300 DEG C take out powder sample until stove.
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|---|---|---|---|---|
| CN1229767A (en) * | 1998-12-19 | 1999-09-29 | 吉林大学 | Method for preparing iron nitrogen Nm alloy and iron nitrogen-boron nitride nm composite material |
| CN1326200A (en) * | 2000-05-29 | 2001-12-12 | 大同特殊钢株式会社 | Isotropic powdery magnetic material, preparation thereof and resin binded magnet |
| CN101513995A (en) * | 2009-04-01 | 2009-08-26 | 武汉工程大学 | Method for preparing boron nitride nano-tube |
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| JP5822188B2 (en) * | 2010-09-24 | 2015-11-24 | 戸田工業株式会社 | Ferromagnetic particle powder and production method thereof, anisotropic magnet and bonded magnet |
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|---|---|---|---|---|
| CN1229767A (en) * | 1998-12-19 | 1999-09-29 | 吉林大学 | Method for preparing iron nitrogen Nm alloy and iron nitrogen-boron nitride nm composite material |
| CN1326200A (en) * | 2000-05-29 | 2001-12-12 | 大同特殊钢株式会社 | Isotropic powdery magnetic material, preparation thereof and resin binded magnet |
| CN101513995A (en) * | 2009-04-01 | 2009-08-26 | 武汉工程大学 | Method for preparing boron nitride nano-tube |
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