CN1064426A - The laser vapor phase method of making metal-powder and equipment thereof - Google Patents
The laser vapor phase method of making metal-powder and equipment thereof Download PDFInfo
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- CN1064426A CN1064426A CN 92102518 CN92102518A CN1064426A CN 1064426 A CN1064426 A CN 1064426A CN 92102518 CN92102518 CN 92102518 CN 92102518 A CN92102518 A CN 92102518A CN 1064426 A CN1064426 A CN 1064426A
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Abstract
The present invention proposes a kind of method and apparatus for preparing the spherical magnetic metal superfine powder of chain with the laser Gaseous pyrolysis.Contain the carbonyls of the ferromagnetic metal element of single or mixing in the raw material, laser causes pyrolytic reaction and the powder nucleating growth carries out in magnetic field.Magnetic field intensity is 20-300 Gausses, magnet be located at the reactor cavity inner nozzle over against the side.The spherical magnetic metal superfine powder of chain of the present invention's preparation has good magnetic property, is applicable to the magnetic recording material of high record density.
Description
The present invention relates to prepare the method and the equipment thereof of submicron particle, particularly prepare the method and apparatus of the spherical magnetic metal superfine powder of chain with the laser Gaseous pyrolysis.
Usually the laser vapor phase method of preparation superfine metal or metal compound powder is the metallic compound of easily gasification and causes pyrolytic reaction with the mixture of nonmetallic compound at laser and generate supersaturated vapor, becomes superfine powder through being condensed into nucleus growth.This laser vapor phase method easily makes epigranular, metal or metallic compound superfine powder that purity is high.
For example United States Patent (USP): US4558017 discloses laser pyrolysis and has prepared the metal silicide superfine powder; US4548798 discloses to use with quadrat method and has prepared the fire-resistant powder of oxide, and US4667753 discloses laser method and prepared the Fe/C Ultra-fine Particle Catalysts; US4468474 discloses laser method and has prepared the Fe/Sl/C Ultra-fine Particle Catalysts.But these methods all can only make spherical or be similar to spherical particulate, and spherical metal or metal compound powder can not satisfy anisotropic requirement, and the application that makes it aspect magnet material is subjected to certain restriction.
The equipment that general laser vapor phase method prepares metal or metallic compound superfine powder mainly is made of laser source system, reactor, raw material supplying system, powder capturing and collecting device and exhaust pump.Laser source system is made up of laser, laser condensing lens, and reactor is made up of cavity and nozzle, preceding light pipe, back light pipe; The raw material supplying system is made up of the head tank of carrier gas, sensitising agent, coaxial carrier gas source of the gas and flowmeter thereof and reaction raw materials and band heating.The past light pipe introducing reactor cavity after the laser beam line focus that laser produces, through after light pipe derive, interior carrier gas after metering with after sensitising agent mixes again with head tank in the be heated unstripped gas constitutive material gaseous mixture of gasification, material mixed gas sprays into from nozzle in the reactor cavity and intersects vertically with laser beam, under laser caused, material mixed gas generated supersaturated vapor by pyrolytic reaction; Being condensed into nucleus growth becomes ultrafine particle, under the carrier band of coaxial carrier gas, obtains superfine powder by the powder capturing and collecting device collection.Exhaust pump is operated reactor under negative pressure or positive pressure, and makes gas discharge reactor.
The present invention proposes a kind of laser Gaseous method and equipment thereof for preparing the spherical submicron particle of chain.The spherical submicron particle of chain is that the spherical or approximate spherical particle with magnetic dipole joins each other with opposite pole, and the total magnetic dipole moment that forms chain has the submicron particle of a fixed orientation.
The method that the present invention proposes is to adopt the raw material that contains the magnetic metal compound, cause pyrolytic reaction by laser, under the action of a magnetic field, the supersaturated vapor that pyrolytic reaction generates is condensed into nucleus growth becomes the spherical submicron particle of chain, it is except the advantage that has general laser vapor phase method and prepare superfine powder, also have good magnetic property, be applicable to the magnetic recording material of high record density.Because the method that the present invention proposes need be carried out in magnetic field, therefore the equipment that adopts is in the equipment reactor cavity that former laser vapor phase method uses; Nozzle over against the side establish a magnet, constitute by permanent magnet or dc coil, to form a magnetic field.
The method that the present invention proposes, contain the ferromagnetic metal carbonyls in the raw material, because iron, cobalt, ferronickel magnetic metal carbonyls easily produce thermal decomposition under laser causes, and metallic particles is magnetized produce magnetic dipole and end to end, therefore easily form the higher submicron particle of the spherical purity of chain.The magnetic field intensity of the spherical magnetic powder of preparation chain is generally in 20-300 Gauss.The variation of the particle diameter of powder is identical with general laser vapor phase method, the influence of factors such as Stimulated Light power density, spot diameter, material mixed gas flow velocity, reaction pressure.
Fig. 1 is an equipment schematic diagram of the present invention.
Fig. 2 is equipment one an illustration intention of the present invention.
The present invention by the laser that laser instrument 1 produces, is introduced the cavity 3 of reactors as shown in Figure 1 by front light pipe 2 after the line focus, through after light pipe 4 derive. In cavity 3, be provided with magnet 5, magnet 5 be located at nozzle 6 over against the side; Iron, cobalt, ferronickel magnetic metal carbonyls single or that mix are contained in the position vertical with laser beam in the raw material 7. Interior carrier gas 8 is introduced in the head tank 10 after metering mixes with sensitising agent 9, raw material 7 is heated after the gasification in head tank and interior carrier gas 8 and sensitising agent constitutive material gaseous mixture, sprayed in the reactor cavity 3 by nozzle, the flow of material mixed gas depends on the flow of interior carrier gas 8 and sensitising agent 9 and the heating-up temperature of head tank. Material mixed gas produces pyrolytic reaction in laser beam, under magnetic fields, and the powder nucleating growth, form the spherical superfine powder of chain, discharged from cavity 3 pumping by exhaust pump 11, under the carrier band of coaxial carrier gas 13, powder is being confined to an orientation, pass through magnetic field center in spreading between few strip area, thereby can not be deposited on the magnet wall, powder is collected in powder collector 12 with air-flow, and reacting gas is discharged by exhaust pump 11, the reaction pressure of reactor is negative pressure or malleation, is controlled by exhaust pump. Magnet 5 also can be as shown in FIG. 2 except consisting of the magnetic field for coil passes to DC current as shown in FIG. 1, and magnet 5 is permanent magnet, is shaped as cylindrical shape. The present invention is suitable for preparing in a large number the spherical ultra-fine magnetic metal powder of chain.
Embodiment 1:
With ferromagnetic metal carbonyls Fe(CO)
5Be raw material, sulphur hexafluoride SF
6Be sensitising agent, adopt 150WCWCO
2Laser, laser power density are 4500WCM
-2, interior carrier gas is Ar, flow is 0.03Lmln
-1, the sensitising agent flow is 0.005Lmln
-1Coaxial carrier gas is Ar, and flow velocity is 0.3Lmln
-1; The temperature of material mixed gas is 40 ℃, and the diameter of nozzle is 2mm; Magnetic field intensity is chosen in 20-300 Gauss scope.As shown in Figure 1, reactor cavity 3 is filled behind the forevacuum with inert gas, the steam supply valve of carrier 8, reaction raw materials 7 and sensitising agent 9 in opening, treat steady air current after, adjust exhaust pump 11 and set reaction pressures; Head tank 10 and nozzle 6 by heater heats to 60 ℃, are injected in the reactor cavity 3 with laser beam respectively, meet SF with material mixed gas from nozzle 6 ejections
6Absorb luminous energy and give Fe(CO with energy delivery) through molecular collision
5, cause Fe(CO)
5Decompose, generate the supersaturated vapor of Fe atom, and the cohesion nucleation, under the carrier band of coaxial carrier gas 13, be magnetized by magnet 5, form the spherical powder of chain, be pumped into powder capturing and collecting device 12 by exhaust pump 11 and collect, powder collector 12 is displaced downwardly in the anaerobic glove box at sealing state and takes out iron powder.What obtain with transmission electron microscope observing is the spherical ultra-fine magnetic powder of chain.When magnetic field intensity is respectively 300,120, during 20 Gausses, it is as shown in the table for the ultra-fine magnetic iron powder magnetic result who obtains.
Embodiment 2:
By the condition that embodiment 1 is given, reaction raw materials changes Fe(CO into)
5With acetylene C
2H
2Gaseous mixture, make that the Fe/C mol ratio is 10 in the reaction raw materials gaseous mixture: 0.5-10: 10.Can make Fe
xC
YThe spherical magnetic powder of bianry alloy chain.
Embodiment 3:
In the reaction raw materials gaseous mixture, stop sensitising agent SF
6, increase silane SiH
4, other condition is identical with enforcement 1.The Fe/Si mol ratio is 10 in the material mixed gas: 0.5-10: 20, can make Fe
xSi
YThe spherical magnetic powder of bianry alloy chain.
Embodiment 4:
Raw material Fe(CO among the embodiment 1 to embodiment 3)
5The middle Co(CO that increases)
4And Ni(CO)
4The molar content sum of Fe, Co, three kinds of elements of Ni is 100% in the raw material, and the molar content of Fe is 0-100%, and the molar content of Co is 0-100%, the molar percentage of Ni is 0-100%, then contains Fe, Co, Ni carbonyls single or that mix in the raw material.Can make the spherical powder of chain of monobasic metal, binary, ternary or multicomponent alloy.
Claims (4)
1, a kind of laser Gaseous pyrolysis prepares the method for superfine powder, raw material contains the metallic compound of easy gasification, raw material and interior carrier gas, sensitising agent constitutive material gaseous mixture spray in the reactor cavity from nozzle, cause pyrolytic reaction by laser and make submicron particle, it is characterized in that containing in the raw material ferromagnetic metal carbonyls single or that mix, pyrolytic reaction and powder nucleating growth carry out in magnetic field, and the powder that makes is the spherical ultra-fine magnetic metal powder of chain.
2, method according to claim 1 is characterized in that, magnetic field intensity is 20-300 Gauss.
3, a kind of laser Gaseous pyrolysis equipment of preparing submicron particle is made of laser source system, reactor, raw material supplying system, powder capturing and collecting device and exhaust pump, reactor is made up of cavity, nozzle, preceding light pipe and back light pipe, it is characterized in that the reactor cavity inner nozzle over against just being provided with a magnet.
4,, it is characterized in that magnet is made of cylindrical permanent-magnet iron or dc coil according to the equipment of claim 3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92102518 CN1021889C (en) | 1992-04-20 | 1992-04-20 | Laser gas phase method for making metal-powder and equipment thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92102518 CN1021889C (en) | 1992-04-20 | 1992-04-20 | Laser gas phase method for making metal-powder and equipment thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1064426A true CN1064426A (en) | 1992-09-16 |
| CN1021889C CN1021889C (en) | 1993-08-25 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 92102518 Expired - Lifetime CN1021889C (en) | 1992-04-20 | 1992-04-20 | Laser gas phase method for making metal-powder and equipment thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1058920C (en) * | 1994-08-15 | 2000-11-29 | 中国科学院金属研究所 | Technology for preparing room temp. austenitic iron submicron-sized particles |
| CN1058921C (en) * | 1994-08-15 | 2000-11-29 | 中国科学院金属研究所 | Lasser gas-phase synthesis of gamma ferric oxide nanometer micropowder |
| CN101056698B (en) * | 2004-11-09 | 2010-12-01 | 法国原子能委员会 | System and method for continuous flow production of nanometric or sub-micrometric powders by the action of a pyrolytic laser |
| CN107418295A (en) * | 2010-06-29 | 2017-12-01 | 纳克公司 | Silicon/germanium nanoparticle inks, laser pyrolysis reactor and correlation technique for synthesizing nano-particle |
| CN107570696A (en) * | 2017-07-10 | 2018-01-12 | 向勇 | Metal dust mixing arrangement and its method, high flux metal alloy preparation system |
-
1992
- 1992-04-20 CN CN 92102518 patent/CN1021889C/en not_active Expired - Lifetime
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1058920C (en) * | 1994-08-15 | 2000-11-29 | 中国科学院金属研究所 | Technology for preparing room temp. austenitic iron submicron-sized particles |
| CN1058921C (en) * | 1994-08-15 | 2000-11-29 | 中国科学院金属研究所 | Lasser gas-phase synthesis of gamma ferric oxide nanometer micropowder |
| CN101056698B (en) * | 2004-11-09 | 2010-12-01 | 法国原子能委员会 | System and method for continuous flow production of nanometric or sub-micrometric powders by the action of a pyrolytic laser |
| CN107418295A (en) * | 2010-06-29 | 2017-12-01 | 纳克公司 | Silicon/germanium nanoparticle inks, laser pyrolysis reactor and correlation technique for synthesizing nano-particle |
| CN107570696A (en) * | 2017-07-10 | 2018-01-12 | 向勇 | Metal dust mixing arrangement and its method, high flux metal alloy preparation system |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1021889C (en) | 1993-08-25 |
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