CN101962722A - Method for preparing single-phase SmCo7 nanocrystalline alloy block material without doping elements - Google Patents
Method for preparing single-phase SmCo7 nanocrystalline alloy block material without doping elements Download PDFInfo
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- CN101962722A CN101962722A CN 201010515835 CN201010515835A CN101962722A CN 101962722 A CN101962722 A CN 101962722A CN 201010515835 CN201010515835 CN 201010515835 CN 201010515835 A CN201010515835 A CN 201010515835A CN 101962722 A CN101962722 A CN 101962722A
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Abstract
The invention discloses a method for preparing a single-phase SmCo7 nanocrystalline alloy block material without doping elements, which belongs to the technical field of nanometer materials and novel powder metallurgy. The method comprises the following steps of: mixing metals Sm and Co in the mass ratio of 26.7:73.3, and smelting the mixture to form SmCo7 alloy ingot casting base metal by using a vacuum induction smelting furnace; under the protection of argon gas, crushing the base metal alloy into powder, and placing the powder in a ball milling jar for ball milling to prepare allow powder with an amorphous structure; placing the amorphous alloy powder in a mould, and fast sintering the powder for forming by using spark plasma sintering technology to obtain the single-phase SmCo7 nanocrystalline alloy block material; and placing the single-phase SmCo7 nanocrystalline alloy block material which is obtained by the spark plasma sintering in a vacuum thermal treatment furnace for annealing. The single-phase SmCo7 nanocrystalline alloy prepared by the method has a uniform and fine organization and a pure grain boundary area without precipitated phases, and the method has a simple route, short flow and controllable technical parameters.
Description
Technical field
The present invention relates to a kind of single-phase SmCo of non-impurity-doped element
7The preparation method of nanometer crystal alloy block materials belongs to nano material and novel powder metallurgical technology field.
Background technology
Material with metastable structure has the not available property of many conventional stable state materials, has very wide application prospect in multiple military and civilian field.Generally speaking, metastable material all under extraordinary condition (as high pressure, microgravity, chilling, strong-electromagnetic field, gross distortion etc.) prepare, therefore, metastable material development direction also is that the investigator finds novel material, new phenomenon and the new key areas of using, and is one of the research focus in current new high-tech material in the world and modern technique field.
SmCo
7The type alloy is the most representative class material with metastable structure in the Sm-Co alloy system.The Curie temperature of Yin Qigao (Tc), saturation magnetization (Ms), anisotropy field (are Sm
2Co
171.2～1.4 times of class permanent magnet alloy) and lower HCJ temperature factor (0.10～-0.16%), make it to have excellent high-temperature magnetic energy, be one of preferred material of developing in recent years high temperature permanent magnetic material, receive the very big concern of international magneticsubstance research field.Yet owing to be subjected to the restriction of technology of preparing, people are to SmCo
7The research of type alloy mainly concentrates on by adding element and improves SmCo
7The stability of phase, optimize the multielement microstructure improving aspect such as magnetic property, and for the single-phase SmCo of binary
7The research report of alloy does not seldom still have the SmCo that is entirely for preparing non-impurity-doped element (promptly only containing two kinds of elements of Sm, Co) especially at present
7The research report of monophasic alloy block material.For this reason, we utilizing the nanoscale effect that the alloy metastable phase is carried out the previous work basis of stabilization treatment, research and develop out a kind of single-phase SmCo of non-impurity-doped element based on this study group
7The preparation method of bulk nanometer material, the preparation route of this technology has advantages such as technical process is short, controllability is strong, application potential is big, and can extend in the preparation of single-phase nano crystalline alloy block material of other metastable structure.
Summary of the invention
The object of the present invention is to provide a kind of single-phase SmCo of non-impurity-doped element
7The preparation method of nanometer crystal alloy block materials.At first with metal Sm and Co according to the mixed in molar ratio of 1:7, be smelted into SmCo with vacuum induction melting furnace
7Alloy cast ingot is as mother metal.Under argon shield, the mother metal alloy is broken into the powder of particle diameter less than 500 μ m, again powder is put into ball grinder and carry out ball milling, prepare the powdered alloy of non-crystal structure.Amorphous powdered alloy is put into mould, utilize existing discharge plasma sintering technique, obtain single-phase SmCo the moulding of powder Fast Sintering
7The nanometer crystal alloy block materials.The single-phase SmCo that discharge plasma sintering is prepared then
7The nanometer crystal alloy block materials is put into vacuum heat treatment furnace and is annealed, and obtains the single-phase SmCo of various grain sizes
7The nanometer crystal alloy block materials.
The single-phase SmCo of non-impurity-doped element provided by the invention
7The preparation method of nanometer crystal alloy block materials is characterized in that, specifically may further comprise the steps:
(1) will be cut into and put into mould after the metal Sm of fine strip shape and granular metal Co powder mix according to 26.7: 73.3 mass ratio and be pressed into block, it is SmCo that nominal composition is prepared in the copper crucible melting that block is put into cold wall magnetic levitation vortex induction stove
7Alloy cast ingot, alloy cast ingot is carried out more than 3 times remelting handles, obtaining nominal composition is SmCo
7Mother alloy ingot;
(2) mother alloy ingot is broken into powder particle less than 500 μ m, powder particle after the fragmentation is packed in the ball grinder according to 25: 1 ball material mass ratio, rotating speed during ball milling is 400～700r/min, 10～25 hours ball milling time, obtains the powdered alloy of complete non-crystal structure;
(3) under argon shield, pack into sintered-carbide die and pre-molding of the amorphous powder that ball milling is obtained; send into and carry out sintering densification in the discharging plasma sintering equipment; adopt following processing parameter: the final state sintering temperature is 580～680 ℃; sintering pressure is 550～800MPa; reach not to be incubated after the final state sintering temperature and directly be cooled to room temperature, obtain the single-phase SmCo of discharge plasma sintering
7The nanometer crystal alloy block;
(4) the single-phase SmCo that discharge plasma sintering is prepared
7The nanometer crystal alloy block is put into vacuum heat treatment furnace, makes vacuum tightness remain on 5 * 10
-3～2 * 10
-2Pa 300～600 ℃ of vacuum heat-preserving anneal of carrying out 10～50min, prepares the single-phase SmCo with various grain sizes at last
7The nanometer crystal alloy block materials.
In the step (1), by being pressed into the method for block mixture after fine strip shape Sm and the granular Co powder mixes, can utilize the Co powder that rare-earth Sm is covered, wraps up, avoid the oxidation of Sm on the one hand, can prevent the volatilization loss of Sm in the vacuum melting process on the other hand effectively, like this, can ensure that Sm and Co keep designed mol ratio.Alloy cast ingot being carried out remelting repeatedly handle, is in order to obtain the uniform mother alloy ingot of composition, during each remelting the top and bottom of ingot casting is overturn and puts into crucible again, to promote the homogenization of composition in the melting.In the step (2), ratio of grinding media to material and rotational speed of ball-mill can rationally be adjusted according to the needs of preparation efficiency, adopt bigger rotational speed of ball-mill can obtain the powdered alloy of non-crystal structure at short ball milling in the time.In the step (3), the optimization of sintering temperature and sintering pressure collocation can guarantee to prepare densification, single SmCo
7Thing phase, single-phase SmCo with different initial grain-sizes
7The nanometer crystal alloy block materials.In the step (4),, can obtain having different other single-phase SmCo of final state grain-size level by regulating annealing temperature and soaking time
7The nanometer crystal alloy block especially, can improve SmCo significantly
7The comprehensive magnetic property of alloy block material.
The present invention can have unusual phase stability mutually according to Sm-Co alloy system some alloy things under nanoscale that we discover, thereby the technological line that utilizes high-energy ball milling and discharge plasma sintering to combine produces the special pathway of the nanometer crystal alloy in the certain size scope by amorphous powdered alloy generation crystallization, but prepares the single-phase SmCo of stable existence
7The nanometer crystal alloy block materials.Past people all is that the method by doped metallic elements (as Cu, Zr, Ti etc.) obtains to have SmCo
7Type thing phase (TbCu
7N-type waferN structure) pseudobinary alloy, and the alloy of the present invention's preparation does not contain any doped element, has complete single S mCo
7The thing phase.Wherein, utilize stove melting of cold wall magnetic levitation vortex induction and remelting to handle the nominal composition that obtains and be SmCo
7Alloy cast ingot, its thing phase composite is not SmCo
7Phase, but by Sm
2Co
17And SmCo
5Two phase composites, wherein Sm
2Co
17Be principal phase.In mechanical milling process, the mother alloy that is made of mutually two kinds of things is transformed into the powdered alloy with complete non-crystal structure.When amorphous powdered alloy is carried out discharge plasma sintering, the good Sm-Co powdered alloy of electroconductibility utilize pulsed current by the time joule heating effect that produces make powder particle be warmed up to comparatively high temps rapidly, amorphous powder is in sintering densification, the crystallization forming core takes place, the forming core mode belongs to instantaneous saturated forming core, produces single S mCo thus
7Thing phase nucleus, nucleus develops into the crystal of nanoscale, continues to grow up to contacting with each other again, and forms the polycrystalline bulk material that is full of spatial nanocrystal tissue.Therefore, through the complete crystallization and the densification of amorphous alloy powder, finally prepare fine and close SmCo
7The single-phase nano crystalline alloy block material.Compare with existing other powder metallurgy technology, in the discharge plasma sintering, coming from the concurrent joule heating effect of multiple spot causes powder particle to heat up rapidly, simultaneously can cause the quickening transmission mechanism of multiple solid phase atom, thereby significantly quicken the crystallization process of amorphous powder and improved the densification rate of powder.Simultaneously, the high sintering pressure that applies in sintering process can quicken the sintering densification process on the one hand, reduces sintering temperature and shortens sintering time, thereby effectively control the alligatoring of nanocrystal; On the other hand, because sintering time is short and sintering temperature is lower, can control the right ordering of the contained Co-Co dumbbell of crystallization and densification process interalloy effectively, this helps obtaining the SmCo of metastable structure very much
7Phase.The single-phase SmCo that discharge plasma sintering is obtained
7The nanometer crystal alloy block is annealed, and on the one hand, can make high-pressure sinter cause the SmCo that is preparing
7The internal stress that exists in the nanometer crystal alloy block is relaxed, and can improve the atomic arrangement order degree of nanocrystalline boundary region in the alloy system by the atom short-range diffusion, thereby helps obtaining good magnetic property; On the other hand, suitable anneal can make nanocrystal that growing up of suitable degree taken place, and makes average grain size reach optimum range, utilizes the nonlinear relationship of magnetic coercive force and nanocrystalline grain size, obtains best comprehensive magnetic property.In a word, the single-phase SmCo that utilizes the present invention to prepare
7The nanometer crystal alloy block can reach complete densification, its nanocrystal homogeneous microstructure is tiny, the regional pure no precipitated phase of crystal boundary, and the operational path of this method is simple, flow process short, the controllability of technical parameter is strong, can extend to fully in the preparation of other metastable structure materials with regard to its technological adaptability.
Description of drawings
Nominal composition is SmCo among Fig. 1 embodiment 1
7Mother alloy ingot and the single-phase SmCo of discharge plasma sintering preparation
7The X ray diffracting spectrum of nanometer crystal alloy block.
The single-phase SmCo of discharge plasma sintering preparation among Fig. 2 embodiment 1
7The transmission electron microscope bright field image (a) of nanometer crystal alloy block and corresponding selected area electron diffraction spectrum (b).
Among Fig. 3 embodiment 1 through the single-phase SmCo behind 300 ℃, 50min anneal
7The X ray diffracting spectrum of nanometer crystal alloy block.
Among Fig. 4 embodiment 1 through the single-phase SmCo behind 300 ℃, 50min anneal
7The transmission electron microscope bright field image (a) of nanometer crystal alloy block, the high-resolution-ration transmission electric-lens bright field image (c) that corresponding selected area electron diffraction spectrum (b) and regional area amplify.
Among Fig. 5 embodiment 2 through the single-phase SmCo behind 600 ℃, 10min anneal
7The X ray diffracting spectrum of nanometer crystal alloy block.
Among Fig. 6 embodiment 2 through the single-phase SmCo behind 600 ℃, 10min anneal
7The transmission electron microscope bright field image of nanometer crystal alloy block.
Among Fig. 7 embodiment 3 through the single-phase SmCo behind 500 ℃, 30min anneal
7The X ray diffracting spectrum of nanometer crystal alloy block.
Among Fig. 8 embodiment 3 through the single-phase SmCo behind 500 ℃, 30min anneal
7The transmission electron microscope bright field image of nanometer crystal alloy block.
Embodiment
The purity of raw material Sm and Co is 99.99% among all embodiment, is provided by Beijing Non-Fervoous Metal Inst..
Embodiment 1
(1) will be cut into and put into mould after the metal Sm of fine strip shape and granular metal Co powder mix according to 26.7: 73.3 mass ratio and be pressed into block, it is SmCo that nominal composition is prepared in the copper crucible melting that block is put into cold wall magnetic levitation vortex induction stove
7Alloy cast ingot, alloy cast ingot is carried out more than 3 times remelting handles, obtaining nominal composition is SmCo
7Mother alloy ingot;
(2) mother alloy ingot is broken into powder particle less than 500 μ m, powder particle after the fragmentation is packed in the ball grinder according to 25: 1 ball material mass ratio, rotating speed during ball milling is 400r/min, 25 hours ball milling time, obtains the powdered alloy of complete non-crystal structure;
(3) under argon shield, pack into sintered-carbide die and pre-molding of the amorphous powder that ball milling is obtained; send into and carry out sintering densification in the discharging plasma sintering equipment; adopt following processing parameter: the final state sintering temperature is 580 ℃; sintering pressure is 800MPa; reach not to be incubated after the final state sintering temperature and directly be cooled to room temperature, obtain the single-phase SmCo of discharge plasma sintering
7The nanometer crystal alloy block;
(4) the single-phase SmCo that will obtain from step (3)
7The nanometer crystal alloy block is put into vacuum heat treatment furnace, and its vacuum tightness is better than 8 * 10
-3Pa carries out 50min vacuum heat-preserving anneal at 300 ℃, cools to room temperature then with the furnace, and preparing average grain size is the single-phase SmCo of 28nm
7The nanometer crystal alloy block.
Nominal composition is SmCo among the embodiment 1
7The material phase analysis of mother alloy ingot see Fig. 1 (a), by Sm
2Co
17And SmCo
5Two kinds of things constitute mutually, wherein Sm
2Co
17Be principal phase; The single-phase SmCo of discharge plasma sintering preparation
7The material phase analysis of nanometer crystal alloy block is seen Fig. 1 (b), only by single-phase SmCo
7Constitute.The single-phase SmCo of discharge plasma sintering preparation
7Displaing micro tissue topography of nanometer crystal alloy block (transmission electron microscope bright field image) and material phase analysis (selected area electron diffraction spectrum) are seen Fig. 2, measure to show that average grain size is 20nm, has single-phase SmCo
7Structure.Through the single-phase SmCo behind 300 ℃, 50min anneal
7The material phase analysis of nanometer crystal alloy block is seen Fig. 3, only by single-phase SmCo
7Constitute.Through the single-phase SmCo behind 300 ℃, 50min anneal
7The displaing micro tissue topography of nanometer crystal alloy block (transmission electron microscope bright field image), material phase analysis (selected area electron diffraction spectrum) and regional area intensified image (high-resolution-ration transmission electric-lens picture) are seen Fig. 4, show that average grain size is 28nm, has single-phase SmCo
7Structure.
Embodiment 2
(1) will be cut into and put into mould after the metal Sm of fine strip shape and granular metal Co powder mix according to 26.7: 73.3 mass ratio and be pressed into block, it is SmCo that nominal composition is prepared in the copper crucible melting that block is put into cold wall magnetic levitation vortex induction stove
7Alloy cast ingot, alloy cast ingot is carried out more than 3 times remelting handles, obtaining nominal composition is SmCo
7Mother alloy ingot;
(2) mother alloy ingot is broken into powder particle less than 500 μ m, powder particle after the fragmentation is packed in the ball grinder according to 25: 1 ball material mass ratio, rotating speed during ball milling is 700r/min, 10 hours ball milling time, obtains the powdered alloy of complete non-crystal structure;
(3) under argon shield, pack into sintered-carbide die and pre-molding of the amorphous powder that ball milling is obtained; send into and carry out sintering densification in the discharging plasma sintering equipment; adopt following processing parameter: the final state sintering temperature is 680 ℃; sintering pressure is 550MPa; reach not to be incubated after the final state sintering temperature and directly be cooled to room temperature, obtain the single-phase SmCo of discharge plasma sintering
7The nanometer crystal alloy block;
(4) the single-phase SmCo that will obtain from step (3)
7The nanometer crystal alloy block is put into vacuum heat treatment furnace, and its vacuum tightness is better than 2 * 10
-2Pa carries out 10min vacuum heat-preserving anneal at 600 ℃, cools to room temperature then with the furnace, and preparing average grain size is the single-phase SmCo of 35nm
7The nanometer crystal alloy block.
The single-phase SmCo for preparing by discharge plasma sintering among the embodiment 2
7The nanometer crystal alloy block is through the single-phase SmCo behind 600 ℃, 10min anneal
7The material phase analysis of nanometer crystal alloy block is seen Fig. 5, only by single-phase SmCo
7Constitute.Through the single-phase SmCo behind 600 ℃, 10min anneal
7Fig. 6 sees in the displaing micro tissue topography of nanometer crystal alloy block (transmission electron microscope bright field image), shows that average grain size is 35nm, has single-phase SmCo
7Structure.
Embodiment 3
(1) will be cut into and put into mould after the metal Sm of fine strip shape and granular metal Co powder mix according to 26.7: 73.3 mass ratio and be pressed into block, it is SmCo that nominal composition is prepared in the copper crucible melting that block is put into cold wall magnetic levitation vortex induction stove
7Alloy cast ingot, alloy cast ingot is carried out more than 3 times remelting handles, obtaining nominal composition is SmCo
7Mother alloy ingot;
(2) mother alloy ingot is broken into powder particle less than 500 μ m, powder particle after the fragmentation is packed in the ball grinder according to 25: 1 ball material mass ratio, rotating speed during ball milling is 500r/min, 20 hours ball milling time, obtains the powdered alloy of complete non-crystal structure;
(3) under argon shield, pack into sintered-carbide die and pre-molding of the amorphous powder that ball milling is obtained; send into and carry out sintering densification in the discharging plasma sintering equipment; adopt following processing parameter: the final state sintering temperature is 600 ℃; sintering pressure is 700MPa; reach not to be incubated after the final state sintering temperature and directly be cooled to room temperature, obtain the single-phase SmCo of discharge plasma sintering
7The nanometer crystal alloy block;
(4) the single-phase SmCo that will obtain from step (3)
7The nanometer crystal alloy block is put into vacuum heat treatment furnace, and its vacuum tightness is better than 1 * 10
-2Pa carries out 30min vacuum heat-preserving anneal at 500 ℃, cools to room temperature then with the furnace, and preparing average grain size is the single-phase SmCo of 30nm
7The nanometer crystal alloy block.
The single-phase SmCo for preparing by discharge plasma sintering among the embodiment 3
7The nanometer crystal alloy block is through the single-phase SmCo behind 500 ℃, 30min anneal
7The material phase analysis of nanometer crystal alloy block is seen Fig. 7, only by single-phase SmCo
7Constitute.Through the single-phase SmCo behind 500 ℃, 30min anneal
7Fig. 8 sees in the displaing micro tissue topography of nanometer crystal alloy block (transmission electron microscope bright field image), shows that average grain size is 30nm, has single-phase SmCo
7Structure.
Claims (1)
1. the single-phase SmCo of a non-impurity-doped element
7The preparation method of nanometer crystal alloy block materials is characterized in that, may further comprise the steps:
(1) put into mould after the metal Sm of fine strip shape and granular metal Co are mixed according to 26.7: 73.3 mass ratio and be pressed into block, it is SmCo that nominal composition is prepared in the copper crucible melting that block is put into cold wall magnetic levitation vortex induction stove
7Alloy cast ingot, alloy cast ingot is carried out more than 3 times remelting handles, obtaining nominal composition is SmCo
7Mother alloy ingot;
(2) mother alloy ingot is broken into powder particle less than 500 μ m, powder particle after the fragmentation is packed in the ball grinder according to 25: 1 ball material mass ratio, rotating speed during ball milling is 400～700r/min, 10～25 hours ball milling time, obtains the powdered alloy of complete non-crystal structure;
(3) under argon shield, pack into sintered-carbide die and pre-molding of the amorphous powder that ball milling is obtained; send into and carry out sintering densification in the discharging plasma sintering equipment; adopt following processing parameter: the final state sintering temperature is 580～680 ℃; sintering pressure is 550～800MPa; reach not to be incubated after the final state sintering temperature and directly be cooled to room temperature, obtain the single-phase SmCo of discharge plasma sintering
7The nanometer crystal alloy block;
(4) the single-phase SmCo that discharge plasma sintering is prepared
7The nanometer crystal alloy block is put into vacuum heat treatment furnace, makes vacuum tightness remain on 5 * 10
-3～2 * 10
-2Pa 300～600 ℃ of vacuum heat-preserving anneal of carrying out 10～50min, prepares the single-phase SmCo with various grain sizes at last
7The nanometer crystal alloy block materials.
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Cited By (5)
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|---|---|---|---|---|
| CN102140598A (en) * | 2011-03-07 | 2011-08-03 | 北京工业大学 | Preparation method of super high coercivity and low-Co type Sm-Co nanocrystalline alloy |
| CN107557634A (en) * | 2017-08-07 | 2018-01-09 | 中南大学 | A kind of SmCo rare-earth magnetic nanoporous alloy and preparation method thereof |
| CN108060319A (en) * | 2018-01-11 | 2018-05-22 | 谢石华 | A kind of efficiently pure aluminum alloy ring protects refining agent and its manufacturing method |
| CN108130442A (en) * | 2018-01-11 | 2018-06-08 | 谢石华 | A kind of smokeless aluminium alloy environmental protection refining agent of no sodium and its manufacturing method |
| CN114701723A (en) * | 2022-03-24 | 2022-07-05 | 徐亲成 | Vehicle-mounted passive vacuum insulation box suitable for long-time and long-distance transportation |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102140598A (en) * | 2011-03-07 | 2011-08-03 | 北京工业大学 | Preparation method of super high coercivity and low-Co type Sm-Co nanocrystalline alloy |
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| CN107557634A (en) * | 2017-08-07 | 2018-01-09 | 中南大学 | A kind of SmCo rare-earth magnetic nanoporous alloy and preparation method thereof |
| CN108060319A (en) * | 2018-01-11 | 2018-05-22 | 谢石华 | A kind of efficiently pure aluminum alloy ring protects refining agent and its manufacturing method |
| CN108130442A (en) * | 2018-01-11 | 2018-06-08 | 谢石华 | A kind of smokeless aluminium alloy environmental protection refining agent of no sodium and its manufacturing method |
| CN114701723A (en) * | 2022-03-24 | 2022-07-05 | 徐亲成 | Vehicle-mounted passive vacuum insulation box suitable for long-time and long-distance transportation |
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