CN101722312B - Preparation method of zero-dimensional polyhedron Fe nano capsule - Google Patents
Preparation method of zero-dimensional polyhedron Fe nano capsule Download PDFInfo
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- CN101722312B CN101722312B CN200910220293A CN200910220293A CN101722312B CN 101722312 B CN101722312 B CN 101722312B CN 200910220293 A CN200910220293 A CN 200910220293A CN 200910220293 A CN200910220293 A CN 200910220293A CN 101722312 B CN101722312 B CN 101722312B
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Abstract
The invention relates to a magnetic nano material, in particular to a preparation method of a zero-dimensional polyhedron Fe nano capsule. The method is characterized by comprising the following steps of: under a non high vacuum condition, by using Fe-Al alloy as a raw material and an anode (the content of Al does not exceed 10 at percent of the total content of the anode Fe-Al alloy), and using metal tungsten as a cathode, putting the Fe-Al alloy on the anode, packaging equipment and vacuumizing to 0.1-3*10-2Pa; washing by using helium, and then charging a mixed gas of helium and hydrogen, wherein the hydrogen and the helium have a proportion relation that the volume ratio of H2:He is (0.2-0.6):1; after reaching a certain pressure, arcing with a high frequency, and then stopping arcing and settling; vacuumizing, and recharging Ar gas containing little oxygen to 1 atmospheric pressure; and after a sample is prepared, preparing nuclear shell Al2O3 coated polyhedron Fe nano capsules. The invention aims to provide a preparation method of the zero-dimensional polyhedron Fe nano capsule under a non high vacuum condition in specific to the defects in the application of a magnetic metal nano particles technology.
Description
Technical field:
The present invention relates to a kind of magnetic Nano material, specifically a kind of preparation method of zero-dimensional polyhedron Fe nano capsule.
Background technology:
The core-shell particles composite is as a kind of novel electromagnetic wave absorption functional material; Not only in military stealth technology field; And the noise jamming that reduces the microelectronics communication system, eliminate electromagnetic wave to the radiation of human body, administer field such as electromagnetic environmental pollution and all have significant application value; Have traditional material incomparable advantage, the research of its preparation and relevant electricity, magnetic, sound, microwave property is one of focus of paying close attention to of Chinese scholars always.
Core-shell material is meant that nuclear and shell are the materials that is interconnected through physics or chemical action by two kinds of different materials.Be wrapped in the outside shell of particle and can change and give characteristics such as particle light, electricity, magnetic, catalysis, improve its oxidation resistance.And has the core-shell particles of special construction; Compare with its bulk material and to have bigger specific area; Less density, and might form " black hole " to microwave electromagnetic field, be expected to obtain high performance Radar Stealth Materials; And then reach control its electromagnetic wave loss and Dispersion through the shell material that changes core-shell particles, reach the requirement of " thin, light, wide, strong ".Therefore, core-shell material is the focus content of microwave absorption area research.
Research shows that the absorbing property of material and the shape of material have confidential relation.The Magnaglo of bar-shaped, sheet, shape anisotropy such as fibrous is superior to the absorbing property of spherical Magnaglo.And present magnetic metal nano-powder absorbing material, it is spherical mostly powder granule is, and make anisotropic Magnaglo, some complicacy aspect the requiring of material chosen, technology, thereby do not see the report of polyhedron Fe nano particle as absorbing material.
Summary of the invention:
Goal of the invention: the objective of the invention is provides under a kind of non-high vacuum condition the preparation method of zero-dimensional polyhedron Fe nano capsule to the deficiency that exists in the nano metallic nickel granular material technical application.
Technical scheme: the present invention realizes through following technical scheme:
A kind of preparation method of zero-dimensional polyhedron Fe nano capsule is characterized in that: with the Fe-Al alloy be raw material as anode, with tungsten as negative electrode; Be put in the Fe-Al alloy on the water-cooled copper anode, packaged equipment is evacuated to 0.1～3 * 10
-2Pa uses helium purge, charges into the mist of helium and hydrogen again, and when pressure was 100～700Torr, the using plasma arc process began electric arc, and the adjustment arc current is 50-100A, and voltage is 30V～40V; Stop the arc sedimentation after 1～2 hour, stop behind the arc argon gas passivation more than 4 hours that contains a little oxygen charging into, sample preparation finishes; The Al that can obtain nucleocapsid structure at the sidewall and the top of reative cell
2O
3Coat polyhedron Fe Nano capsule, examine and be that α-Fe, shell are Al
2O
3
As the Fe-Al alloy of anode, wherein Al content is no more than the 10at% of anode Fe-Al alloy total amount, and the proportionate relationship that charges into hydrogen and helium is H
2: the He volume ratio is 0.2～0.6: 1.
Advantage and effect: prepare Al with arc plasma process
2O
3Coat Fe polyhedron Nano capsule, synthetic polyhedron nucleocapsid structure Fe/Al
2O
3Nano wave-absorbing material utilizes differences such as polyhedron Fe, Al element fusing point, saturated vapour pressure, realizes the preparation of zero-dimensional polyhedron Fe nano capsule under the non-high vacuum condition.(so-called zero-dimensional polyhedron Nano capsule; The three-dimensional dimension that is meant material all is nano level; But it is shaped as polyhedral nucleocapsid structure material) the more important thing is and utilize its strong shape anisotropy and magnetocrystalline anisotropy and pass through control nucleocapsid ratio; Realize impedance matching, improve its microwave and absorb, prepare absorptivity height, coating is thin, absorption band is wide, in light weight, high temperature resistant, anticorrosive and cost is low microwave absorbing material.Be equipped with Al with the plasma-arc legal system
2O
3Coat polyhedron Fe Nano capsule, Nano capsule Al
2O
3Coat polyhedron Fe and have good electromagnetic performance and anticorrosive, oxidation resistance.
Concrete advantage is following:
1, a kind of simple to operate, cheap, good reproducibility, the non-high vacuum condition preparation method of preparation polyhedron Fe Nano capsule down is provided;
2, can prepare and have magnetocrystalline anisotropy and shape anisotropy Al
2O
3Coat polyhedron Fe nano particle, the Fe (Al of this method preparation
2O
3) Nano capsule purity is high, productive rate is big, cost is low, simple to operate, generated time weak point.Therefore be the high-quality Fe (Al of a kind of acquisition
2O
3) preparation method of Nano capsule.
3, prepared Fe (Al
2O
3) granular size is adjustable, good dispersion, uniform particles.Has very big using value aspect the exploitation high-performance wave-absorbing material.
Description of drawings:
Fig. 1 is Al
2O
3Coat the X-Ray diffraction pattern of polyhedron Fe Nano capsule;
Fig. 2 is Al
2O
3Coat the pattern and the high resolution electron microscopy photo of polyhedron Fe Nano capsule;
Fig. 3 is Al
2O
3Coat polyhedron Fe Nano capsule XPS photoelectron collection of illustrative plates;
Fig. 4 is Al
2O
3Relation between complex dielectric permittivity, complex permeability and the frequency of coating polyhedron Fe Nano capsule/paraffin;
Fig. 5 is Al
2O
3Coat the reflection loss of polyhedron Fe Nano capsule/paraffin and the relation between the frequency.
The specific embodiment:
The present invention provides under a kind of non-high vacuum condition, and the preparation method of zero-dimensional polyhedron Fe nano capsule is equipped with Al with the plasma-arc legal system
2O
3Coat polyhedron Fe Nano capsule.The present invention be achieved in that with the Fe-Al alloy be raw material as anode, as negative electrode, be placed on the Fe-Al alloy on the anode packaged equipment with tungsten; Vacuumize, use helium purge, charge into the mist of helium and hydrogen again, reach certain pressure; Beginning electric arc stops the arc sedimentation afterwards, vacuumizes; Charge into Ar gas to one atmospheric pressure that contains small amount of oxygen again, sample preparation finishes, and prepares the Al of nucleocapsid
2O
3Coat polyhedron Fe Nano capsule.
Embodiment 1
With the Fe-Al alloy be raw material as anode, with tungsten as negative electrode.Be placed on the Fe-Al alloy on the anode, the Al atomic percent is 10% of an anode total amount, and the Fe atomic percent is 90% of an anode total amount, and packaged equipment is evacuated to 0.1 * 10
-2Pa with helium purge twice, charges into the mist of helium and hydrogen, H again
2: the He volume ratio is 0.3: 1, and when reaching pressure and being 500Torr, the using plasma arc process begins electric arc, and the adjustment arc current is 50-100A, and voltage is 30V～35V.Stop the arc sedimentation after 1 hour, be evacuated down to 10
-2Torr charges into and contains a spot of argon gas to an atmospheric pressure, passivation 4 hours, and sample preparation finishes, and prepares the Al of nucleocapsid
2O
3Coat polyhedron Fe Nano capsule structure, examine and be that α-Fe, shell are Al
2O
3
With the Fe-Al alloy be raw material as anode, with tungsten as negative electrode.Be placed on the Fe-Al alloy on the anode, the Al atomic percent is 8% of an anode total amount, and the Fe atomic percent is 92% of an anode total amount, and packaged equipment is evacuated to 1 * 10
-2Pa with helium purge twice, charges into the mist of helium and hydrogen, H again
2: the He volume ratio is 0.5: 1, and when reaching pressure and being 600Torr, the using plasma arc process begins electric arc, and arc current is 50-100A, and voltage is 35V～40V.Stop the arc sedimentation after 1 hour, be evacuated down to 10
-2Torr charges into argon gas to an atmospheric pressure again, passivation 6 hours, and sample preparation finishes, and prepares the Al of nucleocapsid
2O
3Coat polyhedron Fe Nano capsule structure, examine and be that α-Fe, shell are Al
2O
3
Embodiment 3
With the Fe-Al alloy be raw material as anode, with tungsten as negative electrode.Be placed on the Fe-Al alloy on the anode, the Al atomic percent is 5% of an anode total amount, and the Fe atomic percent is 95% of an anode total amount, and packaged equipment is evacuated to 3 * 10
-2Pa with helium purge twice, charges into the mist of helium and hydrogen, H again
2: the He volume ratio is 0.5: 1, and when reaching pressure and being 700Torr, the using plasma arc process begins electric arc, and arc current is 50-100A, and voltage is 35V～40V.Stop the arc sedimentation after 1 hour, be evacuated down to 10
-2Torr charges into argon gas to an atmospheric pressure again, passivation 8 hours, and sample preparation finishes, and prepares the Al of nucleocapsid
2O
3Coat polyhedron Fe Nano capsule structure, examine and be that α-Fe, shell are Al
2O
3
Theoretical explanation: the present invention be with the Fe-Al alloy be raw material as anode, the introducing of a small amount of Al atom uses the plasma arc method to prepare Al
2O
3Coat polyhedron Fe Nano capsule, and the Fe particle can keep its crystal habit, and (according to existing reported in literature, Fe is only in high vacuum 10
-4More than the Pa, under high-purity Fe condition, the condensation of Fe atom just can keep crystal habit when forming solid).Because the chemism of Al atom is higher than metal Fe; Characteristics such as the low and two kinds of metal electronegativity differences of fusing point, saturated vapor pressure ratio Fe are little, two kinds of metals by arc evaporation after, utilize the difference of two kinds of above-mentioned property differences of metal, condensation order; The Al atom provides the space environment of a high-purity, high vacuum when being frozen into solid particle for the Fe atom after evaporating; Keep its distinctive crystal habit when therefore the Fe atom is frozen into solid particle, the Al atomic deposition is on the surface of Fe subsequently, and Al is prepared in passivation
2O
3Coat polyhedron Fe Nano capsule, and the bigger Al of hardness
2O
3Help keeping the crystal habit of Fe.
In the preparation process, control anode A l atomic percent is no more than the 10at% of Fe-Al alloy total amount, otherwise is prone to form Fe behind the arc evaporation
xAl
yAlloy in case form alloy, when the Fe atomic cohesion becomes solid, can not keep its crystal habit.Should control the content of hydrogen in the mist in addition.The content of hydrogen is high, though can improve the powder productive rate, starting the arc difficulty, through multiple comparison test, the optimum volume ratio of hydrogen and helium is controlled at 0.2～0.6: 1.
Experiment conclusion: can know the Al of the nucleocapsid that obtains through the foregoing description by Fig. 1
2O
3Coat polyhedron Fe Nano capsule structure, carry out the X-Ray atlas analysis and can know, the sample after the electric arc preparation has only α-Fe phase; Can know by Fig. 2, in above-mentioned sample, get a part of sample and be placed in the alcohol, supersonic oscillations 10 minutes; Drop on the little grid of Cu with tweezers; Send on the JEOL2010 high resolution electron microscopy pattern and the structure of observing it at last to, be core-shell structure, examine and be α-Fe; And be hexagon and quadrangle, can judge it is the projection of α-Fe granatohedron.Fig. 3 is the XPS photoelectron spectrogram of sample; Interior illustration is Al2p, the Fe2p high-resolution XPS photoelectron spectrogram that the surface is about 1nm; Can know 45.6wt%O according to semi-quantitative analysis; Al50.9wt%, Fe5.5wt% (not calculating the content that pollutes C in the XPS test process), the surperficial main component that can judge prepared sample from this figure is Al
2O
3, can confirm that its shell is Al
2O
3, kernel is α-Fe.Can judge that from the electromagnetic property research of Fig. 4, Fig. 5 made sample has good electro-magnetic wave absorption performance.
The experiment proof: with the Fe-Al alloy is that raw material is as anode; With tungsten as negative electrode; Under plasma-arc method condition, evaporation Fe-Al alloy, the chemism of utilizing Al atom characteristics such as high and fusing point, saturated vapor pressure ratio Fe are low than metal Fe, two kinds of metal electronegativity differences are little; The space environment of a high-purity, high vacuum is provided when being frozen into solid particle for the Fe atom after the evaporation; Therefore to be frozen into solid particle be to keep its distinctive crystal habit to the Fe atom, and the Al atomic deposition is on the surface of Fe, and Al is prepared in passivation
2O
3Coat polyhedron Fe Nano capsule, and have good electromagnetic performance and anticorrosive, oxidation resistance.
Claims (1)
1. the preparation method of a zero-dimensional polyhedron Fe nano capsule is characterized in that: with the Fe-Al alloy be raw material as anode, with tungsten as negative electrode; Be put in the Fe-Al alloy on the water-cooled copper anode, packaged equipment is evacuated to 0.1～3 * 10
-2Pa uses helium purge, charges into the mist of helium and hydrogen again, when pressure is 500～700Torr, and the starting the arc of using plasma arc process high frequency, the adjustment arc current is 50-100A, voltage is 30V～40V, stops the arc sedimentation after 1～2 hour; Stop charging into behind the arc argon gas passivation more than 4 hours that contains a little oxygen, sample preparation finishes again; The Al that can obtain nucleocapsid structure at the sidewall and the top of reative cell
2O
3Coat polyhedron Fe Nano capsule, examine and be that α-Fe, shell are Al
2O
3
As the Fe-Al alloy of anode, wherein the Al atomic percent is 10% of an anode total amount;
The proportionate relationship that charges into helium and hydrogen is H
2: the He volume ratio is 0.2～0.6: 1.
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| CN200910220293A CN101722312B (en) | 2009-12-01 | 2009-12-01 | Preparation method of zero-dimensional polyhedron Fe nano capsule |
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| CN101722312B true CN101722312B (en) | 2012-09-26 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106180740B (en) * | 2015-05-27 | 2019-02-12 | 中国科学院金属研究所 | Co, Ni, FeCo, GdCo5Nano capsule primary reconstruction nano chain and its preparation |
| CN105127414B (en) * | 2015-09-29 | 2017-05-31 | 安徽工业大学 | A kind of preparation method of core shell structure silver nickel coat nano-powder material |
| CN105127437B (en) * | 2015-09-29 | 2017-04-05 | 安徽工业大学 | A kind of preparation method of nucleocapsid structure silver iron clad nano-powder material |
| CN113233444B (en) * | 2021-04-27 | 2022-11-08 | 中国科学院金属研究所 | Loaded with Ni 3 Multilayer graphite lamellar structure of Fe @ C nanocapsule and having N-doped defects |
-
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Non-Patent Citations (2)
| Title |
|---|
| G.M. Shi et al..Al2O3/Fe2O3 composite-coated polyhedral Fe nanoparticles prepared by arc discharge.《Journal of Alloys and Compounds》.2004,第384卷296–299. * |
| 孙维民等.直流电弧等离子体法制备纳米粒子实验装置研究.《大学物理实验》.2009,第22卷(第2期),42-45. * |
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