CN106180737A - A kind of method preparing submicron metal - Google Patents
A kind of method preparing submicron metal Download PDFInfo
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- CN106180737A CN106180737A CN201610534026.3A CN201610534026A CN106180737A CN 106180737 A CN106180737 A CN 106180737A CN 201610534026 A CN201610534026 A CN 201610534026A CN 106180737 A CN106180737 A CN 106180737A
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- deoxidizing
- covering agent
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0844—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid in controlled atmosphere
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0848—Melting process before atomisation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/086—Cooling after atomisation
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Abstract
The present invention is a kind of method preparing submicron metal, belongs to field of material preparation.Concretely comprise the following steps: melting, be atomized, cool down, deposit, be dried and staged care.It is additionally included in smelting process the deoxidation treatment step arranged.The present invention increases deoxidizing covering agent in smelting process and reduces the degree of oxidation, can with the non-metallic inclusion in active adsorption melting liquid, tiny fire resisting material particle thus purify smelting liquid.And use Laval nozzle to increase the spouting velocity of atomization gas in atomization process, 2.5 5 times of supersonic laminar flow atomization air flows can be formed at 0.2 mpa, its laminar flow atomization air flow can effectively suppress the generation of superfine alloy agglomeration, the super-refinement of metal dust can be realized, the yield rate of superfines is greatly improved.
Description
Technical field
The present invention relates to field of material preparation, in particular to a kind of method preparing submicron metal.
Background technology
Submicron metal size is little, and specific surface area is big, has many with its metallic element prepared and is different from routine
The character of material, the most excellent mechanical property, special magnetic property, does and to obtain electrical conductivity and diffusibility, high reaction are lived
Property and catalysis activity.These special natures make super-fine metal powder powder material obtain more in fields such as Aero-Space, metallurgy, chemical industry
Carry out the most application.
At present, the method preparing submicron metal, mainly include ball-milling method, airflow milling comminuting method, plasma electric rotating
Pole method, physical-chemical process and gas atomization.
Wherein, gas atomization is one of main method producing superfine metal and alloy powder.Gas atomization basic
Principle is with high velocity air, liquid metal stream to be broken into droplet and be frozen into the process of powder.Current gas atomization,
It is all to use gas to be atomized, owing to the air injection equipment of present stage is direct injection body, to a certain extent at atomization step
The air-flow velocity making gas is low, thus causes the metal or alloy powder size prepared partially thick, will realize thinner powder system
Standby necessary supercharging, even if the yield rate of the powder size that supercharging is prepared is the highest in body.
Further, in prior art when smelting metal or alloy, the control for the degree of purity of metal or alloy cannot be done
To optimization, situation about so directly resulting in is exactly that the degree of purity of the submicron metal prepared does not reaches, containing more
Impurity.And the most traditional metallurgical technology to add coverture after smelting terminates on liquid level of solution be maximally effective a kind of skill
Art, but almost all of coverture is all to have added on the liquid level of solution to tundish after having smelted again, and many institute's weeks
Know that smelting itself is a process, and the generation of impurity also carries out central in smelting and produces, and work as in smelting process
Middle smelting liquid easily and refractory masses generation redox reaction, makes the Si in smelting liquid exceed standard and generates a large amount of Al2O3It is mingled with
Thing, causes melting liquid contaminated.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of submicron metal, atomization gas when can increase gas atomization
The spouting velocity of body, enables the fineness of the metal dust prepared to reach materials'use requirement；And by smelting
Journey is added novel deoxidizing covering agent, there is stronger deoxidation, desulfidation, on the one hand purified smelting liquid, on the other hand energy
Effectively the smelting liquid after purifying is carried out covering protection, prevent from smelting liquid secondary oxidation, add the purity smelting liquid, make to surpass
The purity of fine metal powder increases.
The present invention is achieved in that
A kind of method preparing submicron metal, it is characterised in that described in concretely comprise the following steps:
(1) use prefabricated smelting furnace that metal melts into solution, and after 8～14 minutes, addition deoxidation is covered after melting starts
Lid agent；
(2) utilize noble gas that solution is carried out atomization process, obtain molten drop；
(3) utilize cooling medium that described molten drop is cooled down, obtain metallic particles；
(4) carry out described metallic particles successively depositing, being dried and staged care.
The beneficial effect of such scheme:
The invention provides the preparation method of a kind of superfine metal, specially one utilizes gas atomization ultra-fine to prepare
Metal dust.The present invention increases deoxidizing covering agent in smelting process and reduces the degree of oxidation, can be with active adsorption melting liquid
In non-metallic inclusion, tiny fire resisting material particle thus purify smelting liquid.Because being to add in smelting process in the present invention
The deoxidizing covering agent entered, adds unlike deoxidizing covering agent from prior art after smelting, and adds de-in prior art
Oxygen coverture is primarily to make will not mix in tundish and have oxygen and smelt liquid and will not aoxidize thus block head piece.But this
Invention be in smelting process add deoxidizing covering agent, the effect of do so can make exactly in whole smelting process all without
Being aoxidized, it is smelted in liquid will not mix the composition having oxygen, and the particle diameter of its final submicron metal is less than existing skill
Particle diameter in art, and sphericity is higher.The present invention uses Laval nozzle to increase atomization gas equally in atomization process
Spouting velocity, can form 2.5-5 times of supersonic laminar flow atomization air flow at 0.2 mpa, and its laminar flow atomization air flow can effectively suppress
The generation of superfine alloy agglomeration, it is possible to achieve the super-refinement of metal dust, is greatly improved the yield rate of superfines.This
What the bright setting by atomization jet angle improve submicron metal with the selection of cooling medium becomes sphericity.
Accompanying drawing explanation
In order to be illustrated more clearly that the technical scheme of the embodiment of the present invention, below by embodiment required use attached
Figure is briefly described, it will be appreciated that the following drawings illustrate only certain embodiments of the present invention, and it is right to be therefore not construed as
The restriction of scope, for those of ordinary skill in the art, on the premise of not paying creative work, it is also possible to according to this
A little accompanying drawings obtain other relevant accompanying drawings.
Fig. 1 is the scanning electron microscope microstructure figure of the superfine alloy powder of the embodiment of the present invention 1 preparation.
Detailed description of the invention
Below in conjunction with embodiment, embodiment of the present invention are described in detail, but those skilled in the art will
Understanding, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the present invention.In embodiment unreceipted specifically
Condition person, the condition advised according to normal condition or manufacturer is carried out.Agents useful for same or instrument unreceipted production firm person, be
Can be by the commercially available conventional products bought and obtain.
Preparation method below for the superfine metal of the embodiment of the present invention is specifically described:
Metal in the present invention includes metal simple-substance and alloy.
A kind of method preparing submicron metal, comprises the following steps:
Metal is placed in smelting furnace, melts as metallic solution at a temperature of 200 DEG C～2000 DEG C.200 DEG C～2000
DEG C substantially cover relatively conventional can the fusing point of the valuable metal carrying out melting, so in the specific embodiment of the invention
In-furnace temperature is set to 200 DEG C～2000 DEG C, but is not intended that the submicron metal preparation method of the present invention is not suitable for height
In 2000 DEG C with less than the situation of 200 DEG C.
When melting carries out 8～14 minutes, add quality be metal 2～8% deoxidizing covering agent to melting terminate after the most quiet
To 3～15 minutes, remove the scum silica frost of superjacent, obtain pure metallic solution.With add deoxidation after melting in prior art
Agent is compared, and the deoxidizer in the present invention adds in fusion process, and the topmost effect of deoxidizer of the prior art is
In order to make the head piece of tundish will not be blocked because of melting liquid oxidation.And the topmost effect of deoxidizer in the present invention is
Make in the middle of fusion process the melting liquid will not be oxidized and will not make in melting liquid containing minute bubbles thus affect fining metal powder
The molding at end.And be with the fusion process of different metal as standard about the selection of joining day, the metal that melting is fast adds
The time metal slow compared with melting is wanted early, and the most low-melting metal adds the time of deoxidizer will be early than melting point metals.In melting
Journey is added deoxidizer and makes melting liquid will not mix have minute bubbles, thus obtain the submicron metal that quality is high.
Deoxidizing covering agent includes that the upper strata deoxidation accounting for deoxidizing covering agent gross mass 45%～80% covers by weight percentage
The middle level deoxidizing covering agent of agent, 10%～13% and lower floor's deoxidizing covering agent of 7%～45%；Its at the middle and upper levels deoxidizing covering agent press
Percentage by weight includes the SiO of 80%～89%2, 1%～the CaO of 8% and the inevitable impurity of surplus；Middle level deoxidation is covered
Lid agent includes the SiO of 2%～12% by weight percentage2, 2～the C of the MgO of the CaO of 10%, 65%～80%, 1%～4%
And the impurity of surplus；Lower floor's deoxidizing covering agent include by weight percentage CaO, 3%～13% of 55%～63% MgO,
The SiO of 1%～8%2With 20%～28% Al2O3.The present invention use deoxidizing covering agent be multilamellar deoxidizing covering agent, upper in
In the deoxidizing covering agent of lower three layers quality accounting most for upper strata deoxidizing covering agent, its work that deoxidizing covering agent plays at the middle and upper levels
With being isolation extraneous air.The quality accounting of lower floor's deoxidizing covering agent is taken second place, and wherein the effect of lower floor's deoxidizing covering agent is mainly
Contact with smelting liquid phase thus play the effect of isolation air and because directly contacting with the melting liquid phase of high heat, then lower floor
Deoxidizing covering agent to have resistant to elevated temperatures physical property, is added with Al in lower floor's deoxidizing covering agent2O3, thus enhance lower floor
High temperature resistant and the corrosion resistance of deoxidizing covering agent.What weight accounting was minimum is middle level deoxidizing covering agent, middle level deoxidizing covering agent because of
For neither contacting in extraneous air, liquid does not contacts with smelting liquid phase, mainly plays buffering and increases the effect in space.This
Deoxidizing covering agent in bright, can improve alloy molten solution mobile performance well, hence it is evident that reduces gas in alloy molten solution and contains with being mingled with
Amount；On the one hand having purified aluminium alloy, the deoxidation products on the other hand floated is relatively big due to specific surface area, can be effectively to purifying after
Aluminium alloy carry out covering protection, prevent aluminium alloy secondary oxidation；Make submicron metal oxygen content less than 100ppm.
The bottom pour ladle with the traffic flow via hole diameter of 12 kg/min as 5mm of the solution of gained after deoxidation is leak into nebulizer, enters
Row atomization, during atomization use argon as atomizing medium, employing convergent-divergent channel is shower nozzle, during atomization pressure medium be 0.2～
12MPa, medium spouting velocity is 380～600m/s, and spray angle is 13～18 °.Laval nozzle mini sprinkler of the present invention,
Just can form 2.5-5 times of supersonic laminar flow atomization air flow under the pressure of 0.2MPa, its laminar flow atomization air flow can effectively suppress super
The generation of thin alloy agglomeration, is greatly improved the yield rate of superfines with this；And the present invention uses high-purity argon gas conduct
Atomization source of the gas and cooling medium, thus can grain about processing machinery excellent performance, sphericity height, ultra low oxygen content, 0.1-10 μm
The metal or alloy powder of degree.In order to increase the one-tenth sphericity of submicron metal, the present invention is for the spray angle of convergent-divergent channel
Being defined, test proves that, spray angle can make the one-tenth sphericity of submicron metal the highest between 13～18 °.
The metallic solution drop of gained after atomization is placed in atomized water cooling medium and cools down, obtain fine metal
Grain, wherein the granularity of atomized water is 1～55 μm, and resistivity is 10～20 Ω mm2/ m, temperature is 0 DEG C～5 DEG C.The tool of cooling
Body method is: use convergent-divergent channel spray described cooling medium and make described cooling medium process, with atomization, the molten drop obtained
Contact.Cooling uses atomized water to be the most efficient cooling way, and under the effect of convergent-divergent channel, atomized water is with ultrasonic speed
Degree carries out spraying and contacts with the submicron metal after atomization, can make submicron metal the most near 60～70 DEG C with
Under temperature, make metal dust gas be difficult to reunite, it is simple to collect, steady quality, the added value of submicron metal is higher.And
And the granularity of atomized water is 1～55 μm, the least granularity can to plagiarize metal dust surface polish, again because
The speed of atomized water quickly, makes polishing more homogenization, so that the one-tenth sphericity of submicron metal increases.
The submicron metal obtained after cooling is sucked by vacuum collector and deposits, make submicron metal enter
Row is assembled.Deposition can make submicron metal to be diffused, better collection.
Being placed in tunnel dehydrator by post-depositional submicron metal and dry, drying mode is that infrared ray radiation is dried
Dry, drying temperature is preferably 100 DEG C～160 DEG C, obtains being dried submicron metal.The drying mode used in the present invention is excellent
Select tunnel dehydrator, because the submission of submicron metal is less, be not suitable for carrying out traditional drying pattern of hot-air seasoning.This
The airtight tunnel dehydrator of bright employing can produce the submicron metal surface after high temperature evaporate cooling by infrared ray radiation
On moisture make its be dried, it is fast that tunnel dehydrator has rate of drying, it is easy to the effect of collection.
The tiny submicron metal that will obtain after drying carries out staged care by different granularity requirements, both obtains.System
Having the situation that particle diameter differs in the submicron metal got ready, the screening means such as at this moment sieve carry out metal dust grain
The differentiation in footpath.
The present invention increases deoxidizing covering agent in smelting process and reduces the degree of oxidation, can be with in active adsorption melting liquid
Non-metallic inclusion, tiny fire resisting material particle thus purify smelting liquid.The deoxidizing covering agent added in smelting process, can
So that all without being aoxidized in whole smelting process, smelting will not mix in liquid has oxygen, its final submicron metal
Particle diameter less than particle diameter of the prior art, and sphericity is higher.Same use Laval nozzle increase in atomization process
The spouting velocity of atomization gas, can form 2.5-5 times of supersonic laminar flow atomization air flow at 0.2 mpa, its laminar flow atomization air flow energy
The effective generation suppressing superfine alloy agglomeration, it is achieved the super-refinement of metal dust, is greatly improved the finished product of superfines
Rate.
Below in conjunction with embodiment, the preparation method of the submicron metal of the present invention is described in further detail.
Embodiment one
A kind of method preparing ultra-fine pure tin powder, comprises the following steps:
(1) selecting metal is stannum simple substance, because stannum is amphoteric metal, so stannum is placed in acid smelting furnace or caustic fusion stove
The most all can, melt at a temperature of 250 DEG C as metallic tin solution；
(2) when melting carries out 8 minutes, deoxidizing covering agent to the melting adding quality is stannum 8% terminates rear quiet to 6 points
Clock, removes the scum silica frost of superjacent, obtains pure solution of tin, wherein deoxidizing covering agent include by weight percentage 55% upper
Layer deoxidizing covering agent, the middle level deoxidizing covering agent of 12% and lower floor's deoxidizing covering agent of 33%；Its at the middle and upper levels deoxidizing covering agent press
Percentage by weight includes the SiO of 85%2, the CaO of 7% and the inevitable impurity of surplus；Middle level deoxidizing covering agent includes 9%
SiO2, the CaO of 8%, the MgO of 78%, the C of 2% and the impurity of surplus；Described deoxidizing covering agent includes by weight percentage
The CaO of 60%, the MgO of 10%, the SiO of 5%2With 25% Al2O3；
(3) bottom pour ladle with the traffic flow via hole diameter of 12 kg/min as 5mm of the solution of gained after deoxidation is leak into atomization
Device, is atomized, and uses argon as atomizing medium during atomization, and employing convergent-divergent channel is shower nozzle, and during atomization, pressure medium is
6MPa, medium spouting velocity is the 420m/ second, and spray angle is 13 °；
(4) the solution of tin drop of gained will be placed in atomized water cooling medium and cool down after atomization, obtain tiny wet
Profit pure tin granule, the granularity of atomized water is 20 μm, and resistivity is 13 Ω mm2/m, and temperature is 1 DEG C；
(5) the tiny moistening pure tin granule obtained after cooling is deposited by vacuum collector suction, make pure tin
Granule is assembled；
(6) being placed in tunnel dehydrator by post-depositional pure tin granule and dry, drying mode is that infrared ray radiation is dried
Dry, drying temperature is 85 DEG C, obtains the pure tin granule being dried；
(7) the tiny pure tin granule that will obtain after drying carries out staged care by different granularity requirements, both obtains.
Wherein metallic tin powder average particle size is that the pure tin powder of 9.4 μm, wherein granularity less than 9 accounts for the 56.7% of gross mass,
Sphericity reaches 98%, and oxygen content is 75ppm.
Embodiment two
A kind of method preparing ultra-fine fine silver powder, comprises the following steps:
(1) melting, because silver is alkalinous metal, it is possible to be placed in by silver in caustic fusion stove, the temperature of 1000 DEG C
Under melt as silver metal solution；
(2) deoxidation: when melting carries out 11 minutes, add quality be silver 10% deoxidizing covering agent terminate to melting after
Quiet to 10 minutes, removing the scum silica frost of superjacent, obtain pure silver-colored solution, wherein deoxidizing covering agent includes by weight percentage
The upper strata deoxidizing covering agent of 55%, the middle level deoxidizing covering agent of 12% and lower floor's deoxidizing covering agent of 33%；Its deoxidation at the middle and upper levels
Coverture includes the SiO of 85% by weight percentage2, the CaO of 7% and the inevitable impurity of surplus；Middle level deoxidation covers
Agent includes the SiO of 8%2, the CaO of 7%, the MgO of 77%, the C of 3% and the impurity of surplus；Described deoxidizing covering agent is by weight
Percentage ratio includes CaO, the MgO of 10%, the SiO of 5% of 60%2With 25% Al2O3；
(3) atomization: the bottom pour ladle with the traffic flow via hole diameter of 12 kg/min as 5mm of the solution of gained after deoxidation is leak into
Nebulizer, is atomized, and uses argon as atomizing medium during atomization, and employing convergent-divergent channel is shower nozzle, pressure medium during atomization
For 5.7MPa, medium spouting velocity is the 400m/ second, and spray angle is 13 °；
(4) the tiny alloy liquid droplet of gained after atomization being placed in granularity 35 μm, resistivity is 15 Ω/m2, temperature is 5 DEG C
Low-temperature atomizing high purity water in cool down, obtain tiny ferro-silicium granule；
(5) deposition: the tiny moistening fine silver granules obtained after cooling is sucked by vacuum collector and deposits, make
Fine silver granules is assembled；
(6) drying: be placed in tunnel dehydrator by post-depositional fine silver granules and dry, drying mode is that infrared ray shines
Penetrating drying, drying temperature is 85 DEG C, obtains the fine silver granules being dried；
(7) classification: the tiny fine silver granules obtained after drying carries out staged care by different granularity requirements, both
?.
Gained powder, mean diameter is 6.3 μm, and granularity accounts for the 73% of gross mass less than the fine silver powder of 6 μm, and sphericity reaches
96%, oxygen content 80ppm.
Embodiment three
A kind of method preparing ultra-fine ferrum silicon soft magnetic powder, comprises the following steps:
(1) ferrum and silicon mixture (wherein silicone content be 5.7wt.%, Fe are surplus) are placed in acid smelting furnace or alkalescence
In any stove of smelting furnace, melt as metallic solution at a temperature of 1600 DEG C；
(2) when melting carries out 14 minutes, add quality be Fe and Si mixture gross mass 8% deoxidizing covering agent extremely
Melting terminates latter quiet to 15 minutes, removes the scum silica frost of superjacent, obtains pure ferro-silicium solution, wherein deoxidizing covering agent
Include that lower floor's deoxidation of the upper strata deoxidizing covering agent of 55%, the middle level deoxidizing covering agent of 12% and 33% covers by weight percentage
Agent；Its at the middle and upper levels deoxidizing covering agent include by weight percentage 85% SiO2, the CaO of 7% and surplus the most miscellaneous
Matter；Middle level deoxidizing covering agent includes the SiO of 6%2, the CaO of 8%, the MgO of 77%, the C of 3% and the impurity of surplus；Described de-
Oxygen coverture includes CaO, the MgO of 10%, the SiO of 5% of 60% by weight percentage2With 25% Al2O3；
(3) bottom pour ladle with the traffic flow via hole diameter of 12 kg/min as 5mm of the solution of gained after deoxidation is leak into atomization
Device, is atomized, and uses argon as atomizing medium during atomization, and employing convergent-divergent channel is shower nozzle, and during atomization, pressure medium is
12MPa, medium spouting velocity is the 570m/ second, and spray angle is 15 °；
(4) the tiny alloy liquid droplet of gained after atomization being placed in granularity 50 μm, resistivity is 16 Ω mm2/ m, temperature is 0
DEG C low-temperature atomizing high purity water in cool down, obtain tiny ferro-silicium granule；
(5) will obtain after cooling tiny moistening go out ferro-silicium granule sucked by vacuum collector and deposit,
Fine silver granules is made to assemble；
(6) being placed in tunnel dehydrator by post-depositional fine silver granules and dry, drying mode is that infrared ray radiation is dried
Dry, drying temperature is 110 DEG C, obtains the fine silver granules being dried；
(7) the tiny fine silver granules that will obtain after drying carries out staged care by different granularity requirements, both obtains.
The powder average particle size of gained is 10.2 μm, and wherein the ferrum silicon soft magnetic powder below granularity 10 μm accounts for gross mass
61.7%, sphericity reaches 95%, and oxygen content is 90ppm.
Comparative example 1
This comparative example be using melting complete interpolation deoxidizing covering agent as difference technical scheme and the present invention in melting
During add deoxidizing covering agent compare.
A kind of method preparing ultra-fine pure tin powder, comprises the following steps:
(1) metallic tin is melted as metallic tin solution at a temperature of 250 DEG C；
(2) in the metallic tin solution that step (1) obtains, add the deoxidizing covering agent of quality is stannum 8%, stir 15 points
Clock, stands 5 minutes, removes the scum silica frost above tin liquor, be so repeated 3 times；
(3) bottom pour ladle with the traffic flow via hole diameter of 12 kg/min as 5mm of the solution of gained after deoxidation is leak into atomization
Device, is atomized, and uses argon as atomizing medium during atomization, and employing convergent-divergent channel is shower nozzle, and during atomization, pressure medium is
6MPa, medium spouting velocity is the 420m/ second, and spray angle is 13 °；
(4) after being atomized, the solution of tin drop of gained is placed in mist helium cooling medium and cools down, and obtains tiny moistening
Pure tin granule；
(5) the tiny moistening pure tin granule obtained after cooling is deposited by vacuum collector suction, make pure tin
Granule is assembled；
(6) being placed in tunnel dehydrator by post-depositional pure tin granule and dry, drying mode is that infrared ray radiation is dried
Dry, drying temperature is 85 DEG C, obtains the pure tin granule being dried；
(7) the tiny pure tin granule that will obtain after drying carries out staged care by different granularity requirements, both obtains.
Gained submicron metal, mean diameter is that the pure tin powder of below 10.7 μm, wherein granularity 10 μm accounts for gross mass
47.31%, sphericity reaches 95%, oxygen content 185ppm.
The method of deoxidation used in comparative example 1 is for adding deoxidizing covering agent after melting terminates, and the effect of generation is
For embodiment 1, mean diameter is bigger than the particle diameter of embodiment 1 due to the proportion adding bubble.Sphericity is former because of bubble
Being irregular form because making the submicron metal of part, sphericity is lower than embodiment 1.And oxygen content is because tying in melting
Shu Houjia makes melting liquid partial oxidation thus adds the oxygen content in melting liquid, makes oxygen content be higher than embodiment 1.
There is reduction metal dust particle diameter from the above it can be seen that add deoxidizing covering agent in smelting process, improve sphericity, fall
The effect of low oxygen content.
Comparative example two
This comparative example is to use common cooling medium and the present invention to use atomized water to contrast.
A kind of method preparing ultra-fine fine silver powder, comprises the following steps:
(1) because silver is alkalinous metal, it is possible to silver is placed in caustic fusion stove, melted at a temperature of 1000 DEG C
For silver metal solution；
(2) when melting carries out 11 minutes, add quality be silver 10% deoxidizing covering agent to melting terminate after the most quiet extremely
10 minutes, remove the scum silica frost of superjacent, obtain pure silver-colored solution；
(3) bottom pour ladle with the traffic flow via hole diameter of 12 kg/min as 5mm of the solution of gained after deoxidation is leak into atomization
Device, is atomized, and uses argon as atomizing medium during atomization, and employing convergent-divergent channel is shower nozzle, and during atomization, pressure medium is
5.7MPa, medium spouting velocity is the 400m/ second, and spray angle is 13 °；
(4) after being atomized, the silver-colored solution droplets of gained is placed in water and cools down, and obtains tiny fine silver granules；
(5) the tiny fine silver granules obtained after cooling is deposited by vacuum collector suction, make fine silver granules
Assemble；
(6) drying: be placed in tunnel dehydrator by post-depositional fine silver granules and dry, drying mode is that infrared ray shines
Penetrating drying, drying temperature is 85 DEG C, obtains the fine silver granules being dried；
(7) classification: the tiny fine silver granules obtained after drying carries out staged care by different granularity requirements, both
?.
Gained submicron metal, mean diameter is that the pure tin powder of below 7.8 μm, wherein granularity 7 μm accounts for gross mass
72.4%, sphericity reaches 92%, oxygen content 75ppm.
The cooling medium used in comparative example two is conventional water, and the effect of generation is for embodiment two, averagely
Particle diameter than being big in embodiment two, sphericity embodiment to be far below two.And oxygen content is because both make in fusion process
Method the same, then be not changed in.
Comparative example three
This comparative example is that the convergent-divergent channel using common atomizing nozzle and the present invention to use contrasts.
A kind of method preparing ultra-fine ferrum silicon soft magnetic powder, comprises the following steps:
(1) ferrum and silicon mixture (wherein silicone content be 5.7wt.%, Fe are surplus) are placed in acid smelting furnace or alkalescence
In any stove of smelting furnace, melt as metallic solution at a temperature of 1600 DEG C；
(2) when melting carries out 14 minutes, add quality be Fe and Si mixture gross mass 8% deoxidizing covering agent extremely
Melting terminates latter quiet to 15 minutes, removes the scum silica frost of superjacent, obtains pure ferro-silicium solution；
(3) bottom pour ladle with the traffic flow via hole diameter of 12 kg/min as 5mm of the solution of gained after deoxidation is leak into atomization
Device, is atomized, and uses argon as atomizing medium during atomization, and during atomization, pressure medium is 12MPa, and medium spouting velocity is
The 143m/ second, spray angle is 15 °:
(4) the tiny alloy liquid droplet of gained after atomization being placed in granularity 50 μm, resistivity is 16 Ω mm2/m, and temperature is
The low-temperature atomizing high purity water of 0 ° cools down, obtains tiny ferro-silicium granule；
(5) will obtain after cooling tiny moistening go out ferro-silicium granule sucked by vacuum collector and deposit,
Fine silver granules is made to assemble；
(6) being placed in tunnel dehydrator by post-depositional fine silver granules and dry, drying mode is that infrared ray radiation is dried
Dry, drying temperature is 110 DEG C, obtains the fine silver granules being dried；
(7) the tiny fine silver granules that will obtain after drying carries out staged care by different granularity requirements, both obtains.
Gained submicron metal, mean diameter is that the pure tin powder of below 15.7 μm, wherein granularity 15 μm accounts for gross mass
46.4%, sphericity reaches 81%, oxygen content 75ppm.
The atomizing nozzle used in comparative example three is common jet pipe, and its spouting velocity produced is little, then to metal powder
The kinetic energy of the shock at end is the least, is difficult to intend metal dust, easily produces the generation of the agglomeration of metal dust, and it is average
Particle diameter is significantly larger than particle diameter in embodiment three, and the sphericity in sphericity embodiment to be far below three, because fusion process
Consistent with the fusion process of embodiment three, then both oxygen contents indistinction.
Although illustrate and describing the present invention with specific embodiment, but it will be appreciated that without departing substantially from the present invention's
May be made that in the case of spirit and scope many other change and amendment.It is, therefore, intended that in the following claims
Including all such changes and modifications belonged in the scope of the invention.
Claims (10)
1. the method preparing submicron metal, it is characterised in that described in concretely comprise the following steps:
(1) use prefabricated smelting furnace that metal melts into solution, and after melting starts, after 8～14 minutes, add deoxidation covering
Agent；
(2) utilize noble gas that solution is carried out atomization process, obtain molten drop；
(3) utilize cooling medium that described molten drop is cooled down, obtain metallic particles；
(4) carry out described metallic particles successively depositing, being dried and staged care.
A kind of method preparing submicron metal the most according to claim 1, it is characterised in that in described step (1),
Also include:
Melting stands 3～15 minutes after terminating, and removes the scum silica frost of superjacent；The quality of described deoxidizing covering agent accounts for metal quality
2%～8%.
A kind of method preparing submicron metal the most according to claim 2, it is characterised in that described deoxidizing covering agent
For multilamellar deoxidizing covering agent, described multilamellar deoxidizing covering agent includes the upper strata deoxidizing covering agent of 45wt%～80wt%, 10wt%
～the middle level deoxidizing covering agent of 13wt% and lower floor's deoxidizing covering agent of 7wt%～45wt%；Described upper strata deoxidizing covering agent exists
The liquation overlying contact solution of melting；Described middle level deoxidizing covering agent is positioned on lower floor's deoxidizing covering agent；The deoxidation of described upper strata is covered
Lid agent is positioned on the coverture of middle level.
A kind of method preparing submicron metal the most according to claim 3, it is characterised in that the deoxidation of described upper strata is covered
Lid agent includes the SiO of 80wt%～89wt% by weight percentage2, the CaO of 1wt%～8wt% and surplus inevitable
Impurity；Described middle level deoxidizing covering agent includes inorganic non-metallic hollow bead；Described lower floor deoxidizing covering agent is by weight percentage
The SiO of MgO, 1wt%～8wt% including CaO, 3wt%～13wt% of 55wt%～63wt%2With 20wt%～28wt%
Al2O3。
A kind of method preparing submicron metal the most according to claim 4, it is characterised in that described inorganic non-metallic
Hollow bead includes 2%～12%SiO by weight percentage2, 2～10%CaO, 65%～80%MgO, 1%～4%C and
The impurity of surplus.
A kind of method preparing submicron metal the most according to claim 1, it is characterised in that process in described atomization
In step, described noble gas is argon, and when atomization processes, the pressure of argon is 0.2～12MPa, and medium spouting velocity is 380
～600m/s, spray angle is 13～18 °.
A kind of method preparing submicron metal the most according to claim 1, it is characterised in that at described cooling step
In, described cooling medium is one or more in steam, mist nitrogen, mist argon, mist helium, and the concrete grammar of cooling is: uses and draws
The Wa Er pipe described cooling medium of ejection the molten drop making described cooling medium obtain with atomization process contact.
A kind of method preparing submicron metal the most according to claim 7, it is characterised in that described steam is mist
Change water；The granularity of described atomized water is 1～55 μm, and resistivity is 10～20 Ω mm2/m, and temperature is 0 DEG C～5 DEG C.
A kind of method preparing submicron metal the most according to claim 1, it is characterised in that described smelting furnace includes
Acid smelting furnace and caustic fusion stove, described acid smelting furnace is for the melting of acid metal, and described caustic fusion stove is used for alkali
The melting of property metal；It is both provided with refractory masses in described acid smelting furnace and caustic fusion furnace body.
A kind of method preparing submicron metal the most according to claim 9, it is characterised in that described refractory material
Layer is the low calcium fire-resistant mud layer of silver hydrochlorate.
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