CN1743103A - Rear-earth nano granule and nano crystal material preparing method and apparatus - Google Patents
Rear-earth nano granule and nano crystal material preparing method and apparatus Download PDFInfo
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- CN1743103A CN1743103A CN 200510089080 CN200510089080A CN1743103A CN 1743103 A CN1743103 A CN 1743103A CN 200510089080 CN200510089080 CN 200510089080 CN 200510089080 A CN200510089080 A CN 200510089080A CN 1743103 A CN1743103 A CN 1743103A
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- 239000000463 material Substances 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000002159 nanocrystal Substances 0.000 title claims description 6
- 239000008187 granular material Substances 0.000 title abstract 7
- 238000005245 sintering Methods 0.000 claims abstract description 35
- 239000007789 gas Substances 0.000 claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 21
- 238000002360 preparation method Methods 0.000 claims abstract description 21
- 239000001307 helium Substances 0.000 claims abstract description 8
- 229910052734 helium Inorganic materials 0.000 claims abstract description 8
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000011261 inert gas Substances 0.000 claims abstract description 8
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 5
- 239000010937 tungsten Substances 0.000 claims abstract description 5
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 28
- 239000002105 nanoparticle Substances 0.000 claims description 25
- 238000000465 moulding Methods 0.000 claims description 14
- 238000005516 engineering process Methods 0.000 claims description 13
- 239000002245 particle Substances 0.000 claims description 13
- 230000005540 biological transmission Effects 0.000 claims description 11
- 238000000151 deposition Methods 0.000 claims description 9
- 230000008021 deposition Effects 0.000 claims description 9
- 238000007781 pre-processing Methods 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 239000011858 nanopowder Substances 0.000 claims description 7
- 150000002910 rare earth metals Chemical class 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 230000001681 protective effect Effects 0.000 claims description 6
- 241001080061 Talides Species 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 230000005291 magnetic effect Effects 0.000 claims description 3
- 239000002707 nanocrystalline material Substances 0.000 claims description 3
- 238000000137 annealing Methods 0.000 claims description 2
- 230000036316 preload Effects 0.000 claims description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 5
- 238000000746 purification Methods 0.000 abstract description 2
- 239000002178 crystalline material Substances 0.000 abstract 2
- 239000013049 sediment Substances 0.000 abstract 2
- 125000004122 cyclic group Chemical group 0.000 abstract 1
- 238000004321 preservation Methods 0.000 abstract 1
- -1 rare earths as anode Substances 0.000 abstract 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 229910052688 Gadolinium Inorganic materials 0.000 description 5
- 229910052772 Samarium Inorganic materials 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 5
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 5
- 238000005240 physical vapour deposition Methods 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000002490 spark plasma sintering Methods 0.000 description 3
- 229910052779 Neodymium Inorganic materials 0.000 description 2
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000009770 conventional sintering Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000005641 tunneling Effects 0.000 description 1
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Abstract
The invention relates to nano material preparation process which comprises granule and crystalline material making. The granule making process as follows: physical gas phase sediment, rare earths as anode, tungsten as cathode, then produce nanometer granule at the protection of helium, 50-400A, 10-50V, arcing time is 0.5-5 hours. The crystalline material making process as follow: place the granule into the pretreatment room with inert gases, which is preformed in a module, the pressure is 10-1000Mpa. discharge plasma sinter with the protection of inert gases, temperature is 200-500 deg.C, pressure is 30-1000Mpa, heat preservation time 0-10min, temperature-rising speed is 20-100 deg.C per minute. The equipment comprises gas phase sediment part, powder collecting machine, transfering machine, pretreating part, sintering and forming part. Each part has vacuum pump and inertia gases bottle, which are placed in glove box with inertia gases protection. The pretreatment and sintering part have the gas cyclic purification device. The diameter of granule is smaller than 100 nano meter and the material has high density, crystalline granule is fine.
Description
Technical field
The present invention relates to the preparation method and the equipment thereof of rare earth element nano particle and high density nano crystal block body material, belong to the nano material preparation technical field.
Background technology
In recent years, nano material has received extensive studies and concern because of it has the incomparable special performance of traditional material.Studies show that, the small-size effect that nano material had, surface interface effect, quantum size effect and quantum tunneling effect have determined this class material to have characteristics such as unusual mechanics, electricity, magnetics, calorifics, optics and chemism, thereby have great potential using value.
On form, nano material mainly comprises nano-particle material and has the block materials of nanometer crystal microstructure.With regard to range of application and application prospect, the latter has bigger advantage.At present, carried out a large amount of work about the research and the industrialization aspect of nano powder preparation.People adopt several different methods such as inert-gas condensation method, plasma (orifice) gas phase synthesi, sol-gel processing, hydro-thermal method or the like to synthesize multiple metal and ZnO, TiO such as Fe, Co, Ni
2, ZrO
2Etc. multiple compound nano-particle material.And the general preparation method of bulk nanometer material has sever Plastic Deformation, smelting solidification method, powder metallurgy sintered method etc., and these methods all have significant limitation, can not prepare the brilliant material of the following high density nano of 100nm.Discharge plasma sintering technique (Spark Plasma Sintering, be called for short SPS) have the heating rate height (1000 ℃/min), sintering (the sintered heat insulating time only needs 3-5 minute), technical characterstic such as sintering temperature is low, sintering mechanism is special fast.Though discharge plasma sintering technique also is used to prepare nanocrystalline material, stand-alone type SPS can not be used for the preparation of easy oxidation, high activity material.Therefore, the preparation of rare earth element nano particle and bulk nanometer material but exists very big difficulty, the rarely seen report of research work.Particularly, there are two difficult points in preparation rare earth element nano particle and bulk nanometer material: first, for rare earth element, its nano particle all has very strong activity, therefore very easy oxidation adopts common treatment technology and equipment to be difficult to guarantee that material is not oxidized in processing procedure.The second, because nano grain surface can be big, grain growth is rapid, adopts conventional sintering technology to be easy to grow up to more than 100 nanometers.Therefore, the technology of preparing of at present relevant rare earth element nano particle and bulk nanometer material has become the subject matter that this class material of restriction further enlarges application.
Summary of the invention
The objective of the invention is the problem that exists in above-mentioned rare earth element nano particle and the bulk nanometer material technology of preparing, the in-situ preparing technology of a kind of rare earth element nano particle and high density nano crystal block body material is provided.
A kind of preparation method of rare earth nanometer particle is characterized in that, may further comprise the steps:
With physical gas phase deposition technology rare earths material is prepared into Powdered nano particle; be higher than the high-purity rare-earth element of 99.5wt% as anode with purity; tungsten is as negative electrode; under the protective atmosphere of helium; select electric current 50-400A; arc voltage 10-50V became nano particle with feedstock production in arcing time 0.5-5 hour.
The brilliant preparation methods of a kind of rare earth element nano is characterized in that, may further comprise the steps:
Step 1: utilize physical gas phase deposition technology, the high-purity rare-earth element that is higher than 99.5wt% with purity is as anode, and tungsten is as negative electrode, under the protective atmosphere of helium, select electric current 50-400A, arc voltage 10-50V became nano particle with feedstock production in arcing time 0.5-5 hour;
Step 2: above-mentioned powder particle is inserted the pretreatment chamber of inert gas shielding, with nano powder pack into Talide mould or graphite jig and pre-molding, preload pressure scope 10-1000Mpa;
Step 3: after the precompressed under inert gas shielding; utilize discharge plasma sintering technique that the pressed compact sintering is synthesized bulk nanometer material, sintering temperature is controlled at 200-500 ℃, and sintering pressure is 30-1000Mpa; the sintered heat insulating time is 0-10min, and the sintering heating rate is 20-100 ℃/min.
Rare earth element nano particle provided by the invention: uniform granularity, particle diameter are less than 100 nanometers, and the granularity of the powder of different embodiment preparations sees Table 1.The concrete pattern of particle is shown in accompanying drawing 2,3,4.
Rare earth element nano crystal block body material provided by the invention: material has very high density (reaching more than 99% of solid density).Material microstructure crystal grain is tiny, even, and grain size is less than 100 nanometers (as shown in Figure 5).Simultaneously, X-ray diffraction shows that material has good single phase property, does not have oxide (as shown in Figure 6).
Preparation method's device therefor of a kind of rare earth nanometer particle provided by the invention and nanocrystalline material, it is characterized in that, comprise Material Physics vapour deposition part 1 successively, the nanometer powder that has the nanometer powder collection container captures mechanism 2, the nanometer powder transmission mechanism 3 that has the special-purpose machinery transmission mechanism, nano-powder particles preprocessing part 4, bulk nanometer material sinter molding part 5 (as shown in Figure 1), each part mentioned above includes vavuum pump that is used to vacuumize and the gas cylinder that feeds inert atmosphere protection, wherein capture mechanism 2, transmission mechanism 3, preprocessing part 4, sinter molding part 5 is inserted in the glove box that is filled with inert protective atmosphere; Nano-powder particles preprocessing part 4 and sinter molding part 5 have the gas circulation purifier; At nanometer powder preprocessing part 4 the magnetic field orientating device is arranged, annealing device, powder moulding mold, hydraulic means and ball mill device.
The discharging plasma sintering equipment that is used in this equipment prepare the physical vapour deposition (PVD) part of nanometer powder and be used for the bulk nanometer material sintering all belongs to present common apparatus.But present equipment all belongs to stand-alone type, can't prepare to resemble this class of rare earth element and be easy to oxidation, active high material.And this equipment couples together capture, the transmission mechanism of these two capital equipments by nanometer powder, and is provided with the device that is used for powder pre-treating.A complete set of equipment is all inserted glove box simultaneously.Equipment pours means such as inert gas and gas circulation purification by vacuumizing, and has realized the oxygen free operation environment effectively, thereby realized the function that the rare earth element material prepares from the powder to the bulk nanometer.
Description of drawings
Fig. 1 is the structural representation of present device.
Among the figure: 1-physical vapour deposition (PVD) part; 2-captures mechanism; The 3-transmission mechanism; The 4-preprocessing part; 5-sinter molding part.
Fig. 2 is the shape appearance figure (transmission electron microscope photo) that adopts the rear earth element nd nano particle (embodiment 1) of original position physical gas phase deposition technology preparation.
Fig. 3 is the shape appearance figure (transmission electron microscope photo) that adopts the rare-earth element gadolinium nano particle (embodiment 2) of original position physical gas phase deposition technology preparation.
Fig. 4 is the shape appearance figure (transmission electron microscope photo) that adopts the rare earth element samarium nano particle (embodiment 3) of original position physical gas phase deposition technology preparation.
Fig. 5 is the crystal grain micro-organization chart (high explanation transmission electron microscope photo) of bulk nanometer material (embodiment 2) that adopts the rare-earth element gadolinium of discharge plasma sintering technique preparation.
Fig. 6 is the X-ray diffractogram of bulk nanometer material (embodiment 3) that adopts the rare earth samarium element of this equipment preparation.
The specific embodiment
Example 1, be that the high-purity neodymium of 99.5wt% is put into Pvd equipment, under helium atmosphere, select arc current 400A purity, arc voltage 50V, arcing time became feedstock production in 5 hours the nano particle of rear earth element nd.With the nano particle of above-mentioned neodymium at pretreatment chamber's powder of high-purity argon gas protection pack into graphite jig and pre-molding.Pressure 10MPa.Utilize discharge plasma sintering technique to be sintered into block materials on green compact.Concrete sintering process parameter is: sintering temperature is 500 ℃, and sintering pressure is 30MPa, and the sintered heat insulating time is 10min, and the sintering heating rate is 20 ℃/min.
Example 2, be that the high-purity gadolinium of 99.8wt% is put into Pvd equipment, under helium atmosphere, select arc current 200A purity, arc voltage 35V, arcing time became feedstock production in 2 hours the nano particle of rare-earth element gadolinium.With the nano particle of above-mentioned gadolinium at pretreatment chamber's powder of high-purity argon gas protection pack into Talide mould and pre-molding.Pressure 500MPa.Utilize discharge plasma sintering technique to be sintered into block materials on green compact.Concrete sintering process parameter is: sintering temperature is 300 ℃, and sintering pressure is 100MPa, and the sintered heat insulating time is 2min, and the sintering heating rate is 40 ℃/min.
Example 3, be that the high-purity samarium of 99.6wt% is put into Pvd equipment, under helium atmosphere, select arc current 50A purity, arc voltage 10V, arcing time became feedstock production in 0.5 hour the nano particle of rare earth element samarium.With the nano particle of above-mentioned samarium at pretreatment chamber's powder of high-purity argon gas protection pack into Talide mould and pre-molding.Pressure 1000MPa.Utilize discharge plasma sintering technique to be sintered into block materials on green compact.Concrete sintering process parameter is: sintering temperature is 200 ℃, and sintering pressure is 1000MPa, and the sintered heat insulating time is 0min, and the sintering heating rate is 100 ℃/min.
Invention for apparatus point of the present invention does not lie in the structure of each several part, and its general thought is described in summary of the invention, repeats no more.
Table 1
Claims (3)
1, a kind of preparation method of rare earth nanometer particle is characterized in that, may further comprise the steps:
With physical gas phase deposition technology rare earths material is prepared into Powdered nano particle; be higher than the high-purity rare-earth element of 99.5wt% as anode with purity; tungsten is as negative electrode; under the protective atmosphere of helium; select electric current 50-400A; arc voltage 10-50V became nano particle with feedstock production in arcing time 0.5-5 hour.
2, a kind of rare-earth nano-crystal preparation methods is characterized in that, may further comprise the steps:
Step 1: utilize physical gas phase deposition technology, the high-purity rare-earth element that is higher than 99.5wt% with purity is as anode, and tungsten is as negative electrode, under the protective atmosphere of helium, select electric current 50-400A, arc voltage 10-50V became nano particle with feedstock production in arcing time 0.5-5 hour;
Step 2: above-mentioned powder particle is inserted the pretreatment chamber of inert gas shielding, with nano powder pack into Talide mould or graphite jig and pre-molding, preload pressure scope 10-1000Mpa;
Step 3: after the precompressed under inert gas shielding; utilize discharge plasma sintering technique that the pressed compact sintering is synthesized bulk nanometer material, sintering temperature is controlled at 200-500 ℃, and sintering pressure is 30-1000Mpa; the sintered heat insulating time is 0-10min, and the sintering heating rate is 20-100 ℃/min.
3, preparation method's device therefor of rare earth nanometer particle according to claim 1 and 2 and nanocrystalline material, it is characterized in that, comprise Material Physics vapour deposition part (1) successively, the nanometer powder that has the nanometer powder collection container captures mechanism (2), the nanometer powder transmission mechanism (3) that has the special-purpose machinery transmission mechanism, nano-powder particles preprocessing part (4), bulk nanometer material sinter molding part (5), each part mentioned above includes vavuum pump that is used to vacuumize and the gas cylinder that feeds inert atmosphere protection, wherein capture mechanism (2), transmission mechanism (3), preprocessing part (4), sinter molding part (5) is inserted in the glove box that is filled with inert protective atmosphere; Nano-powder particles preprocessing part (4) and sinter molding part (5) have the gas circulation purifier; At nanometer powder preprocessing part (4) the magnetic field orientating device is arranged, annealing device, powder moulding mold, hydraulic means and ball mill device.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100394518C (en) * | 2006-08-04 | 2008-06-11 | 北京工业大学 | Method for preparing high coercive force sintering rare-earth-iron-p permanent magnetic material |
| CN102699334A (en) * | 2012-06-04 | 2012-10-03 | 北京工业大学 | Preparation method of nanocrystal lithium-rich single-phase Li-Si compound block material |
| CN103157802A (en) * | 2011-12-09 | 2013-06-19 | 沈阳工业大学 | Equipment and method for rapid-situ-packaging rare earth nanometer powder arc process preparation |
| CN103273069A (en) * | 2013-05-29 | 2013-09-04 | 北京工业大学 | Preparation method for high-purity superfine nanocrystalline lutetium block material |
| CN104923790A (en) * | 2014-11-25 | 2015-09-23 | 安泰科技股份有限公司 | Gadolinium block material and preparation method thereof |
| CN107552805A (en) * | 2017-09-07 | 2018-01-09 | 北京工业大学 | A kind of preparation method of composition and the regulatable samarium cobalt compound nano particle of granularity |
-
2005
- 2005-08-05 CN CN 200510089080 patent/CN1743103A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100394518C (en) * | 2006-08-04 | 2008-06-11 | 北京工业大学 | Method for preparing high coercive force sintering rare-earth-iron-p permanent magnetic material |
| CN103157802A (en) * | 2011-12-09 | 2013-06-19 | 沈阳工业大学 | Equipment and method for rapid-situ-packaging rare earth nanometer powder arc process preparation |
| CN103157802B (en) * | 2011-12-09 | 2015-04-15 | 沈阳工业大学 | Equipment and method for rapid-situ-packaging rare earth nanometer powder arc process preparation |
| CN102699334A (en) * | 2012-06-04 | 2012-10-03 | 北京工业大学 | Preparation method of nanocrystal lithium-rich single-phase Li-Si compound block material |
| CN102699334B (en) * | 2012-06-04 | 2013-12-04 | 北京工业大学 | Preparation method of nanocrystal lithium-rich single-phase Li-Si compound block material |
| CN103273069A (en) * | 2013-05-29 | 2013-09-04 | 北京工业大学 | Preparation method for high-purity superfine nanocrystalline lutetium block material |
| CN103273069B (en) * | 2013-05-29 | 2015-08-26 | 北京工业大学 | A kind of preparation method of high-purity superfine nanocrystalline lutetium block material |
| CN104923790A (en) * | 2014-11-25 | 2015-09-23 | 安泰科技股份有限公司 | Gadolinium block material and preparation method thereof |
| CN107552805A (en) * | 2017-09-07 | 2018-01-09 | 北京工业大学 | A kind of preparation method of composition and the regulatable samarium cobalt compound nano particle of granularity |
| CN107552805B (en) * | 2017-09-07 | 2020-04-03 | 北京工业大学 | Preparation method of samarium cobalt compound nanoparticles with adjustable components and particle sizes |
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