CN1073483C - Nm gamma (iron, nickel) alloy powder and its making method and use - Google Patents

Abstract

The present invention relates to nanometer gamma-(Fe, Ni) alloy powder which belongs to the field of metal magnetic materials. The nanometer gamma-(Fe, Ni) alloy powder is composed of iron and nickel, the particle shape of the nanometer gamma-(Fe, Ni) alloy powder is aspherical, the phase structure of the nanometer gamma-(Fe, Ni) alloy powder is a gamma phase, and the granularity of the nanometer gamma-(Fe, Ni) alloy powder is from 10 to 50 nm. In a preparation method, iron pentacarbonyl liquid and nickel tetracarbonyl liquid are sufficiently mixed according to a certain proportion, are poured in a thermal decomposer, are thermally decomposed at 400 to 600 DEG C and are treated by a quick freezing technique by cold nitrogen gas, NH3 gas and liquid nitrogen. The alloy powder is capable of being applied to optical absorption materials, electromagnetic functional materials and antioxidation special materials, has the advantages of high purity, small granularity, high electromagnetic performance and moderate cost, and is capable of being produced industrially.

Description

Nano gamma- (iron, nickel) alloy powder and its production method

The present invention belongs to the field of magnetic metal material, and is suitable for making nano level gamma- (Fe, Ni) alloy powder.

The current methods for obtaining nanoscale powders are common chemical vapor deposition methods such as vapor phase: carrying out chemical reaction by utilizing gas phase to generate metal compound powder with the granularity of 100-1000 nm; precipitation by liquid phase method: through solution chemical reaction, particles are deposited, but the particles are fine and are generally in a micron order; an electrolytic method: adopting a rotating or vibrating electrode and electrolyzing a metal salt solution to obtain metal particles with the granularity being more than or equal to 500nm, and adopting a solid-phase gas reduction method: reducing with solid salt via gas to obtain metal particles with particle size of 10nm-50 μm; vapor phase method vapor evaporation method: the metal is evaporated and then agglutinated in the gas to obtain the particle size of 10-1000nm, and the like, and with the development of science and technology, a laser powder preparation method is also developed at present. The metal nanoparticles obtained by the powder preparation method always have the defects, such as the chemical vapor phase method can obtain finer particles and can be industrially produced, but the powder purity is not high enough; in addition, for example, the powder obtained by the liquid phase method can also be industrially produced, but the purity of the obtained product is not high enough; the powder property is worse by the solid-phase method; as for the laser method, the powder is expensive although it has good properties.

The invention provides a nano gamma- (Fe, Ni) alloy powder which has high purity, fine granularity, good oxidation resistance and high electromagnetic property and can be industrially produced, a preparation method and application thereof.

The invention relates to a nanometer gamma- (iron, nickel) alloy powder, which consists of iron and nickel, and comprises the following chemical compositions (weight percent): 20-80% of iron, and nickel: 80-20%, its characteristics are: its particle shape is non-spherical, phase structure is gamma phase, and its grain size is 10-50 nm.

The method for preparing the nano gamma- (Fe, Ni) alloy powder is obtained by a method for thermally decomposing carbonyl metal compounds, and comprises the following working procedures of material preparation, thermal decomposition and cooling: the method is characterized in that:

(1) preparing materials: 20-80% of iron pentacarbonyl liquid (weight percent) and 80-20% of nickel tetracarbonyl liquid (weight percent) are fully and uniformly mixed in a closed container;

(2) putting the fully mixed liquid into a thermal decomposer to carry out thermal decomposition at the temperature of 400-800 ℃; the reaction process can be carried out by the following formulaThe following steps are described:

(3) then, cold nitrogen and NH are introduced₃And carrying out quick cooling technical treatment on any one of gas and liquid nitrogen to obtain the gamma- (Fe, Ni) alloy powder.

The gamma- (Fe, Ni) alloy powder with different components can be respectively applied to optical absorption materials, electromagnetic functional materials, special anti-oxidation materials and the like, and the gamma- (Fe, Ni) alloy powder with different chemical components is obtained by controlling the proportioning content of iron pentacarbonyl and nickel tetracarbonyl, wherein the general proportion content of the iron pentacarbonyl is 20-80 percent and is matched with the nickel tetracarbonyl to be uniformly mixed and subjected to thermal decomposition to obtain the gamma- (Fe, Ni) alloy powder with different specifications so as to meet the requirements of various applications.

The gamma-phase structure Fe-Ni alloy particle of the invention is used for effectively preventing the oxidation of the nano magnetic particle, and in the prior published data report, the nano iron powder and the nano nickel powder both have thicker oxide films, but the invention does not have oxides and other impurities, which is a great characteristic of the invention. Because the problem of oxidation resistance of various nanoscale magnetic particles in application has not been solved, particularly, ferromagnetic particles such as nanoscale iron powder and nanoscale nickel powder are the difficulties in application.

The invention can not generate oxidation phenomenon in various application occasions, and has more application value that the phenomenon does not occur even after being stored for several years, thereby laying a foundation for developing the application of new materials.

In addition, the invention has high purity more than or equal to 99.9 percent, fine granularity, high electromagnetic performance, industrialized production and moderate cost.

FIG. 1 is a set of electron microscope bright field images and selected area electron diffraction patterns of the nano gamma- (Fe, Ni) alloy particles of the present invention, wherein A, B is the electron microscope bright field image of theparticles, and C is the selected area electron diffraction pattern of the particles.

FIG. 2 is a typical EPS spectrum for nano gamma- (Fe-Ni) alloy particles, where A is Fe-rich particles, B is Ni-rich particles, and C is the average composition, i.e., Fe: Ni content 44: 56.

FIG. 3 is γ - (Fe)₈₀,Ni₂₀) The centimeter wave radar of the alloy powder has the absorption characteristic.

FIG. 4 is γ - (Fe)₈₀,Ni₂₀) The millimeter wave radar absorption characteristic of the alloy powder.

Example (b):

example one

In the application of electromagnetic field, high magnetic permeability occasion requires high Fe% content in alloy, controls Fe (CO)₅And Ni (CO)₄The mixing ratio is 80: 20 (wt%): if in the field of special anticorrosive materialThe domain development application requires higher content of N and controls Fe (CO)₅And Ni (CO)₄In a mixing ratio of 20: 80 wt.%, in the general case Fe (CO) is controlled₅And Ni (CO)₄The mixing ratio of (B)/(B) being 44: 56), the bright field electron microscope image and the selected area electron diffraction pattern are shown in FIG. 1, and the typical EDS spectrum of carbonyl Fe-Ni particles is shown in FIG. 2.

Example two

Development and application in optical characteristics

Control of Fe (CO)₅And Ni (CO)₄In a mixing ratio of 44: 56 of nano gamma- (Fe)₄₄Ni₅₆) Application of the alloy powder:

1, for the component gamma- (Fe)₄₄Ni₅₆) The result of the test of the alloy powder in the ultraviolet light wave band shows that the alloy powder has excellent ultraviolet light absorption characteristic, shown in table 1, so that the alloy powder can be used for developing ultraviolet-resistant materials.

For the gamma- (Fe) of the species₄₄Ni₅₆) The results of the near-infrared and far-infrared band tests of the alloy powder show that the alloy powder has excellent absorption effects shown in tables 2 and 3, so that the infrared absorption material can be developed.

EXAMPLE III

Development and application in magnetic property

Controlling the mixing ratio of the carbonyl iron and the carbonyl nickel to be 80: 20₈₀,Ni₂₀) The application of the alloy powder is that the alloy powder has high magnetic permeability so that:

1, the test result also has good absorption effect on the centimeter wave, as shown in figure 3, so that the centimeter wave resistant radar material can be developed.

2, the millimeter wave test result has good absorption effect, as shown in figure 4, so that the millimeter wave radar resistant material can be developed, and the millimeter wave radar resistant material can be particularly used as an electromagnetic smoke screen material.

Example four

Application in electronic industry

Control of Fe (CO)₅And Ni (CO)₄In a mixing ratio of 60: 40 of nano gamma- (Fe)₆₀,Ni₄₀) Application of the alloy powder.

The alloy powder has high magnetic response, coercive force quality factor and remanence, so that new materials, such as high-quality video tapes, induction cores, loudspeakers, high-strength magnetic electronic materials, new magnetic materials and the like can be developed in the electronic industry.

TABLE 1 nanometer gamma- (Fe)₄₄-Ni₅₆) Ultraviolet absorption characteristics of alloy powder

Wavelength (nm)	Sample 1#	Sample 2#	Sample 3#
				400	98.1	98.5	98.6
390	97.8	98.1	79.7
				380	97.8	98.2	98.5
370	97.7	97.6	98.0
				360	97.8	97.5	98.2
350	97.0	97.4	98.1
				340	97.4	97.6	97.2
330	97.5	97.1	97.1
				320	97.2	97.0	97.4
310	97.3	97.2	97.5
				300	97.2	97.2	97.5
290	97.1	97.0	97.8
				280	97.5	97.3	97.2
270	96.0	97.4	97.1
				260	96.2	97.5	96.8
250	96.1	96.8	96.6
				240	96.0	96.6	95.7
230	95.8	96.5	95.8
				220	95.2	96.4	94.8
210	95.5	95.8	95.2
				200	95.4	95.3	95.1

TABLE 2 nanometer gamma- (Fe)₄₄-Ni₅₆) Near infrared absorption characteristics of alloy powder

Wavelength (mum)	Sample 1#	Sample 2#
			3.0	95.5	95.4
2.8	95.5	95.8
			2.6	95.6	95.7
2.4	96.1	95.8
			2.2	95.8	96.1
2.0	95.7	96.2
			1.8	96.1	96.0
1.6	95.8	96.7
			1.4	96.2	96.5
1.2	95.7	96.3
			1.0	95.8	96.1
0.8	95.4	95.8

TABLE 3 TABLE 1 nm γ - (Fe)₄₄-Ni₅₆) Far infrared absorption characteristic of alloy powder

Wavelength (mum)	Sample 1#	Sample 2#
			20	97.5	96.5
18	96.8	96.8
			16	96.4	96.2
14	96.7	96.8
			12	95.8	96.5
10	96.0	97.2
			8	96.2	96.7
6	96.0	96.8

Claims (2)

1. A nanometer gamma- (iron, nickel) alloy powder is composed of iron and nickel, and the chemical composition (weight percent) is as follows: 20-80% of iron, and nickel: 80-20%, its characterized in that: its particle shape is non-spherical, phase structure is gamma phase, and its grain size is 10-50 nm.

2. A method for manufacturing nano-scale gamma- (iron, nickel) alloy powder comprises the working procedures of batching, thermal decomposition and cooling, and is characterized in that:

(1) preparing materials: 20-80% of iron pentacarbonyl liquid (weight percent) and 80-20% of nickel tetracarbonyl liquid (weight percent) are fully and uniformly mixed in a closed container;

(2) putting the fully mixed liquid into a thermal decomposer to carry out thermal decomposition at the temperature of 400-800 ℃;

(3) then, cold nitrogen and NH are introduced₃And carrying out quick cooling technical treatment on any one of gas and liquid nitrogen to obtain the gamma- (Fe, Ni) alloy powder.

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