CN108160305A - A kind of mixed metal powder separation method and atmosphere furnace used - Google Patents
A kind of mixed metal powder separation method and atmosphere furnace used Download PDFInfo
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- CN108160305A CN108160305A CN201810126300.2A CN201810126300A CN108160305A CN 108160305 A CN108160305 A CN 108160305A CN 201810126300 A CN201810126300 A CN 201810126300A CN 108160305 A CN108160305 A CN 108160305A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03B—SEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
- B03B5/00—Washing granular, powdered or lumpy materials; Wet separating
- B03B5/28—Washing granular, powdered or lumpy materials; Wet separating by sink-float separation
- B03B5/30—Washing granular, powdered or lumpy materials; Wet separating by sink-float separation using heavy liquids or suspensions
- B03B5/44—Application of particular media therefor
- B03B5/442—Application of particular media therefor composition of heavy media
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03B—SEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
- B03B5/00—Washing granular, powdered or lumpy materials; Wet separating
- B03B5/28—Washing granular, powdered or lumpy materials; Wet separating by sink-float separation
- B03B5/30—Washing granular, powdered or lumpy materials; Wet separating by sink-float separation using heavy liquids or suspensions
- B03B5/44—Application of particular media therefor
- B03B5/447—Application of particular media therefor recovery of heavy media
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Abstract
The present invention relates to a kind of mixed metal powder process for separation and purification and atmosphere furnaces used, include for mixed-powder separating-purifying, process for separation and purification after 3D printing:(1)Preselected spherical shape, particle size distribution range are identical, maximum particle diameter is less than the two or more metal powders of 2 times of minimum grain sizes as 3D printing material.(2)Separating-purifying step:To mixed powder after 3D printing, first screening goes size in gumming to be more than the particles of 2 times of minimum grain sizes;Then according to the component powders density of mixed powder, pure magnesium, the pure bismuth auxiliary material of selection appropriate mass percentage are calculated, is put into the magnesium bismuth alloy liquid that setting density is thermally formed in the atmosphere furnace of argon gas protection;Mixed powder is put into aluminium alloy and stirs and stands;The powder for floating on aluminium alloy top and be sunken to aluminium alloy lower part is fetched into different vessels respectively;Container is finally put into vacuum distillation furnace evaporative removal magnesium bismuth, obtains the metal powder through separating-purifying.Have the characteristics that simple and practicable, of low cost, purification purity is high.
Description
Technical field
The invention belongs to metal parts 3D printing technique fields, are related to a kind of mixed metal powder separation method and gas used
Atmosphere stove.
Background technology
3D printing(Also known as increasing material manufacturing)The research of technology just carries out like a raging fire, is directly had by 3D printing
The metal gradient material parts of functionally gradient material (FGM) ingredient are one of important research targets of 3D printing.
In the 3D printing Direct Manufacture Process of existing metal parts, selective laser fusing(Selective Laser
Melting-SLM)And electron beam selection region melt-shaping(Electron Beam Selective Melting-EBSM)Skill
Art is the metal parts 3D printing technique of the great development prospect of two of which, employs metal powder and is used as molding raw material,
Operation principle is as follows:The metal powder material of needs is first preset to the shaped platform with accurate elevating function by powdering mechanism,
Then computer control laser beam(To SLM)Or electron beam(To EBSM) it is spread in advance by part slice graph outline selective melting
If good metal powder, and an entity synusia of part is solidified out into, subsequent shaped platform declines a thickness, repeats above-mentioned
Powder is preset, powder action in fusing constituency, forms new entity synusia.So successively powder is preset, successively fusing accumulation, most
Entire part prints at last.
After molding, the metal powder of design of part can be melted into for powdering process end, for the data of saving, is needed pair
Powder is recycled.The Powder Recovery of single pure part is relatively easy to.But above-mentioned technology is being used, with two or more metals
When powder 3D printing goes out gradient material component, after printing, it is enclosed in around forming part and powder recovering device
Residual powder is the mixed metal powder that two or more metal powders mix, and such as not separating-purifying, will be caused great
Waste of material!Therefore, carry out whether the 3D printing of metal gradient material parts has business valency using both 3D printing techniques
Value largely sees if there is suitable mixed metal powder separation and method of purification.
A kind of method of separation for mixed metal powder is to be detached using the magnetism of metal with non magnetic, this side
Method can only detach two kinds of magnetism with nonmagnetic mixed metal powder, is all non magnetic for mixed metal powder or is all magnetic
The powder of property can not efficiently separate purification.
Also a kind of method is to realize separating-purifying using centrifugal force, and mixed metal powder is placed in centrifuge, is utilized
Density contrast between material carries out separating-purifying at different rates.But the because metal powder granulates granularity that 3D printing uses
In certain range(Such as 15-53 microns), particle varies, and diameter is small, light-weight, and this method also is difficult to do
It is purified to efficiently separating.
Also a kind of method is to use sieve method separating-purifying.But this method requires two kinds of powder, and there are apparent particles
Difference in size, this is difficult to accomplish in being molded thickness and being only 20-100 microns of metal parts 3D printing technique;It is and general
Screening plant, it is more difficult to pass through fine powder particles more than 300 mesh.
In addition, during metal gradient material parts 3D printing, since the powder in functionally gradient material (FGM) region is all two kinds of gold
Belong to the mixed-powder that is mixed into of powder, it therefore, can be by the portion near constituency when laser beam or electron-beam melting functionally gradient material (FGM) region
Powder particle is divided to sinter bimetallic component powders cluster of grains into.In addition, when laser beam or electron-beam melting functionally gradient material (FGM) region,
As general single material 3D printing process, easily because liquid state molten pool and solid-state basis wetability are bad, by surface tension effects,
Fracture winding balling-up, that is, generate spheroidized particle, and these new particles are also to be made of bimetallic material.Therefore, these are oozed
Enter bimetallic ingredient granules or cluster of grains into mixed metal powder, further increase the separating-purifying of mixed metal powder
Difficulty.
Therefore, the mixed metal powder after purification 3D printing currently how is efficiently separated, is SLM technologies and EBSM technologies
Realize one of metal gradient material parts 3D printing important technical difficult point in the urgent need to address.
It is not chemically reacted generally between metal material.In metal material, the fusing point of bismuth is 271.3 DEG C, and boiling point is
1560 DEG C, density is 9.8 grams/cc;The fusing point of magnesium is 650 DEG C, and boiling point is 1108 DEG C, and density is 1.74 grams/cube li
Rice.And two kinds of simple metal are harmless to environment and human body, are also readily available on the market.When the two presses different quality percentages
Than matching, the alloy that density is 1.74-9.8 grams/cc can be obtained.From magnesium bismuth alloy phasor it is found that when bismuth magnesium is adopted
During with different mass percents, alloy melting point is different, such as when the mass percent of bismuth is 20%, and magnesium bismuth alloy density is
3.352 grams/cc, control the temperature of alloy that can obtain the magnesium bismuth alloy of liquid infinitely dissolve at 640 DEG C or more;Bismuth
Mass percent be 60% when, magnesium bismuth alloy density be 6.576 grams/cc, control the temperature of alloy at 600 DEG C or more,
The magnesium bismuth alloy of liquid infinitely dissolve can be obtained;When the mass percent of bismuth is 100%, pure bismuth density is 9.8 grams/cube li
Rice, controls the temperature of alloy that can obtain the pure bismuth of liquid at 300 DEG C or more.
Therefore, the two makees appropriate components matching, can obtain the not high magnesium bismuth alloy of fusing point.Although two kinds of proof gold of magnesium bismuth
The boiling point of category is respectively 1108 DEG C and 1560 DEG C, but since melting point substance is hardly by effects of air pressure, boiling point by effects of air pressure very
Greatly, by vacuumizing, the boiling point of two kinds of metal components under the premise of hardly alloy melting point is changed, can effectively be reduced.
During metal gradient material parts 3D printing, when selection is spherical, metal powder with same particle size range
End is as moulding material, and when the maximum particle diameter of powder particle is no more than 2 times of minimum grain sizes, after 3D printing, because sintering into
In the bimetallic ingredient granules group that group is formed, usually several metallic particles are sintered the cluster of grains formed together, size
The overwhelming majority is more than 2 times of minimum grain sizes.In addition, the spheroidized particle that laser or electron-beam melting functionally gradient material (FGM) region are formed contain it is double
Metal component obtains the single component dusty material of high-purity for separating-purifying, also needs to remove this kind of particle, still, due to ball
Changing particle is formed by liquid state molten pool fracture winding, selective laser fusing or electron beam selection region melt-shaping 3D printing
Cheng Zhong, for the length dimension in molten bath much larger than powder particle grain size, width dimensions are generally also several times bigger than powder particle grain size, high
Degree size sets then bigger than powder particle grain size or is not much different depending on thickness, thus the spheroidized particle overwhelming majority compares starting powder
Grain diameter is several times big.The two rules are to remove these most newborn bimetal granules from mixed metal powder to carry
Chance is supplied.
Invention content
In order to overcome the disadvantages mentioned above of the prior art, the present invention provides a kind of mixed metal powder separation method and gas used
Atmosphere stove, it can melt 3D printing or electron beam selection region melt-shaping 3D printing to metal gradient material parts selective laser
Mixed metal powder afterwards realizes separating-purifying, to improve the utilization rate of material and economize on resources, and with simple and practicable, cost
Cheap, the characteristics of purification purity is high.
The technical solution adopted by the present invention to solve the technical problems is:A kind of mixed metal powder separation method, packet
It is pre-processed before including a 3D printing, selects spherical, and particle size distribution range is identical, maximum particle diameter is less than 2 times of minimum grain sizes
Two or more metal powders are as metal gradient material parts 3D printing material.
To the mixed-powder after pretreated 3D printing, separating-purifying step is as follows:
(1)Size is more than the powder particle of 2 times of minimum grain sizes in screening removal mixed-powder;
(2)According to the component powders density of purification mixed metal powder to be separated, judgement institute detaches required to mixed metal powder
Liquid medium density, liquid medium density should be between two kinds of powder densities to be separated;
(3)Pure magnesia amount as needed for the calculating of formula d=a%*1.74+ (1-a%) * 9.8 forms the aluminium alloy of liquid medium density d
The mass percent of percentage a% and pure bismuth (1-a%), and by the mass percent calculated choose respectively purity for 99.99% with
On pure magnesium and pure bismuth metal auxiliary material, the total volume of two kinds of metal auxiliary materials should be greater than the mixed metal powder opisthosoma of purification to be separated
Product;
(4)Two kinds of simple metal auxiliary materials are added in atmosphere furnaces, are filled with more than 99.99% argon gas as protective gas, then by atmosphere
Stove is warming up to the suitable temperature less than component powders fusing point in mixed-powder, is completely melt two kinds of simple metal auxiliary materials, and appropriate
Stirring, makes two kinds of simple metal form the magnesium bismuth alloy liquid of infinitely dissolve in atmosphere furnace;
(5)Mixed metal powder is added in the magnesium bismuth alloy solution in atmosphere furnace, stirring after ten minutes, then stands a timing
Between, mixed-powder is made to be layered in aluminium alloy by density;
(6)The powder for floating on aluminium alloy top powder and be sunken to aluminium alloy lower part is taken out be placed in different vessels respectively, is held
Electric mixer is carried in device;
(7)After temperature is down to below room temperature in atmosphere furnace, container is taken out, is placed in vacuum distillation furnace;
(8)Control vacuum distillation furnace that there is suitable pressure, the pressure for making vacuum distillation furnace is 0.001-1Pa, then by temperature
Suitable temperature is heated to, which is higher than the boiling point of simple metal auxiliary material used under the pressure, but less than mixed metal powder
The fusing point of component powders, and held for some time, while metal powder is stirred by the electric mixer in container, make metal powder
Magnesium, the bismuth element of last surface adhesion fully evaporate, when on the condenser being vaporized through in vacuum distillation furnace in magnesium, bismuth element, into
Row magnesium bismuth steam condenses, and is recycled after solidification;
(9)After magnesium bismuth alloy on evaporating completely removal powder particle, when furnace temperature drops to room temperature, container is taken out, is at this moment held
The powder filled in device is exactly the powder after separating-purifying.
During the mixed metal powder more than two, remaining dystectic metal powder is evaporated through vacuum distillation furnace distillation
End repeats above-mentioned steps(2)-(9)Separating-purifying process, until the metal powder in powder containing only single component, you can complete
The separating-purifying of pairs of various metals mixed-powder.
In the step(8)In every time be evaporated in vacuo after condensation magnesium bismuth alloy, for save cost for the sake of, can not be right
Magnesium bismuth alloy carries out separating-purifying, but is reused directly for similarly meeting the magnesium bismuth alloy density after next remelting between two
The mixed metal powder separating-purifying of condition between kind powder density to be separated, at this moment can save step(3), and by step
(4)It is changed to:Magnesium bismuth alloy auxiliary material of the density of recycling between two kinds of powder densities to be separated is added in atmosphere furnace, auxiliary material
Total volume should be greater than the mixed metal powder volume of purification to be separated, be filled with more than 99.99% argon gas as protective gas,
Atmosphere furnace is warming up to suitable temperature again, two kinds of simple metal auxiliary materials is made to be completely melt, and suitably stir, two kinds of simple metal is made to exist
The magnesium bismuth alloy liquid of infinitely dissolve is formed in atmosphere furnace.
A kind of atmosphere furnace for mixed metal powder separation method, atmosphere furnace is by being placed on intermediate support plate is divided into
Furnace chamber and lower furnace chamber are provided with separation ware in upper furnace chamber, detach built-in electric heater on ware wall, can to material in separation ware into
Row heating;It is set in ware is detached there are one lateral active clapboard, active clapboard, which can move left and right, is separated into separation ware
Under disconnected two parts, play the role of isolation separation ware in material;Two-part separation ware is separated by active clapboard
Top and lower part are respectively provided with a leakage hole, and two leakage holes respectively realize the on and off of leakage hole by a sliding block;It detaches in ware
Top pushes agitating plate equipped with first, lower part pushes agitating plate equipped with second, is slided for detaching material stirring or leakage hole in ware
The passage of block or pushing for salvage stores;Two-chamber charging carriage, the chamber of left and right two of two-chamber charging carriage are equipped in lower furnace chamber
For loaded material.
The ware that detaches is square hollow structure, opened upper end, on support plate, the underface of sealing cover.
It is stayed on the support plate there are four hole, both sides hole is used for the connection of upper and lower protective gas, and intermediate holes is lets out
Leakage hole is let out for detaching in ware under material.
The active clapboard includes partition board, partition board push rod two parts, and partition board is with detaching that ware inner space is wide, length is slightly larger
In separation ware inner space length, partition board top surface is with detaching that leakage hole bottom on ware is tangent, bottom surface and second pushes agitating plate top
Face is tangent, and partition board push rod one end is connected with partition board, and the other end stretches out atmosphere furnace, in partition board with detaching ware contact position, partition board push rod
Refractory seals are designed with atmosphere furnace joint.
Two leakage hole, sliding block all with to detach ware inner space wide, two leakage holes respectively pass through a material guide groove and branch
Two leaks on board are respectively connected with leading to, and two sliding blocks are provided with high temperature resistant horizontal through corresponding guide groove with guide groove joint
Sealing.
Described first pushes agitating plate is made of scraper plate, plush copper, deflector hole, scraper plate push rod, five part of thrust pin.Scraper plate with
Separation ware inner space is wide, and the upper end is provided with multiple deflector holes for the material that circulates, and agitating plate movement is pushed to reduce
When the resistance from material.Scraper plate side is provided with for that will correspond to the plush copper that sliding block is pushed open, and plush copper is cylinder, plush copper cylinder
Face and scraper plate bottom surface are tangent, and length is pushed away from detaching ware inner wall joint place to corresponding to guide groove inner wall patch with by corresponding sliding block
Distance at conjunction is equal, and diameter is less than corresponding sliding block thickness.Scraper plate push rod one end is connected across separation ware top surface with scraper plate, another
End is reached outside atmosphere furnace shell, length need to ensure scraper plate can will corresponding sliding block from detach ware inner wall joint place push away to it is right
Guide groove inner wall joint place is answered, removable thrust pin is additionally provided with reaching the side outside atmosphere furnace shell, can make to mix the used time
Plush copper does not contact corresponding sliding block.The scraper plate push rod of agitating plate is pushed first and atmosphere furnace shell joint is equipped with refractory seals.
First when pushing agitating plate installation, must ensure that the top surface of scraper plate bottom surface and active clapboard fits, so that first pushes agitating plate
The salvage stores on active clapboard can be effectively removed.Described second pushes the shape of agitating plate, composition pushes agitating plate with first
Identical, only size and installation site are different, plush copper length with by corresponding sliding block from detach ware inner wall joint place elapse to
The distance of corresponding guide groove inner wall joint place is equal, and plush copper diameter is less than corresponding sliding block thickness, and scraper plate push rod one end, which passes through, to be divided
It is connected from ware inner wall with scraper plate, the other end is reached outside atmosphere furnace shell, and length need to ensure that scraper plate can be by corresponding sliding block from dividing
From ware inner wall joint place push away to corresponding guide groove inner wall joint place;In its scraper plate push rod with detaching ware inner wall joint, scraper plate
Push rod is designed with refractory seals with atmosphere furnace shell joint.Second push agitating plate installation when, must ensure scraper plate bottom surface with point
Fit from ware inner bottom surface so that second push agitating plate can effectively remove separation ware inner bottom surface on salvage stores.
Trolley inlet/outlet is equipped in the lower furnace chamber side, is set between trolley inlet/outlet and lower furnace chamber there are one ring packing
Pad.
The top of the atmosphere furnace be equipped with bell, set between bell and atmosphere furnace there are one annular bell gasket, stove
Lid is fixed on by the wing bolt at both ends in atmosphere furnace.
One and the powder hopper being connected in atmosphere furnace are additionally provided with above the bell, powder hopper lid is equipped at the top of powder hopper;Stove
Lid middle part is provided with bell powder-exhausting hole, connects with powder hopper outlet and realizes that powder hopper is connected with atmosphere furnace;It is set on the blanking direction of powder hopper
Powder hopper switch is equipped with, powder switch is preferably butterfly valve.
The bell top is additionally provided with that powder hopper top is made to keep the snorkel ventilated, upper part and powder hopper with atmosphere furnace
Connection, lower part is connect with bell venthole.
Described that intake valve is equipped in atmosphere furnace lower part, the powder hopper side of covering is equipped with air outlet valve, for passing in and out protective gas.
The refractory seals, all sealing material including mounting base and in mounting base, sealing material are preferably
Graphite packing.
A kind of application method of atmosphere furnace for mixed metal powder separation method is as follows using process:
(1)Bell is opened, the position that two sliding blocks are pushed into fit with detaching ware inner wall makes above and below separation ware at two leakage holes
In closed state;Trolley inlet/outlet is opened, two-chamber charging carriage is placed in lower furnace chamber, its two chamber of left and right is made to be located at two respectively
Immediately below leak, trolley inlet/outlet is closed;The scraper plate push rod and the partition board push rod of active clapboard for pushing agitating plate by two are outside
Draw, make two push agitating plate scrape plate face fit with detaching ware inner wall, the partition board of active clapboard with push agitating plate plush copper institute
Scraper plate face paste close;
(2)The pure magnesium metal auxiliary material of appropriate mass is chosen by precalculated proportioning and pure bismuth metal auxiliary material puts into separation ware
In, close bell;
(3)The powder switch in powder hopper is closed, opens powder hopper lid, the mixed-powder being sieving through described in addition is then shut off powder
Bucket cover;
(4)Intake valve and air outlet valve are opened, purity is filled with up to more than 99.99% argon gas, treats the quality percentage of oxygen at air outlet valve
After content is down to less than 0.05%, atmosphere furnace is warming up to less than ingredient powder in mixed-powder by detaching the electric heating tube in ware
The suitable temperature of last fusing point is completely melt two kinds of simple metal auxiliary materials.It is pushed two and thrust pin is loaded onto on agitating plate, then pushed
Two push agitating plate agitated liquid, and two kinds of simple metal is made to form the magnesium bismuth alloy liquid of infinitely dissolve in atmosphere furnace;
(5)The powder switch in powder hopper is opened, mixed metal powder is added in separation ware, is continuously stirred using agitating plate is pushed
10 minutes;
(6)Mixture is stood into certain time, mixed-powder is made to be layered in aluminium alloy by density;
(7)Active clapboard is pushed home into, separation ware is separated to open and is divided into two parts from intermediate liquid, material performance more than partition board
For metal powder in upper, liquid auxiliary materials under, detach ware internal partition below material show as metal powder under, liquid auxiliary materials
Upper;
(8)It removes two and pushes thrust pin on agitating plate, inwardly push two to push agitating plate to ware opposite side is detached, by two sliding blocks
It pushes open, so as to open two leakage mouths, subsequent two push stirring sheet reset, then active clapboard top material under corresponding guide groove through letting out
To the left chamber of two-chamber charging carriage, active clapboard lower part material under corresponding guide groove through letting out to the right chamber of two-chamber charging carriage;
(9)Agitating plate is pushed by two inwardly to push, and the material for detaching ware inner wall remnants is pushed at two leakage holes, makes separation ware
Interior material is collected into as much as possible on two-chamber charging carriage;
(10)The electric heating tube on separation ware is closed, when atmosphere furnace is cooled to room temperature, opens the trolley inlet/outlet in atmosphere furnace,
The draw ring on trolley is caught on hook, two-chamber charging carriage is pulled out into atmosphere furnace, for removing demagging bismuth in next step.
The magnesium bismuth alloy that the positive effect of the present invention is 1, is pre-processed, sieved by combining powder, different densities are configured is molten
The means such as liquid reduce the mixed metal powder after principle separating-purifying 3D printing, Ke Yishi based on law of buoyancy and decompression boiling point
Now the separating-purifying of most of mixed metal powder of the fusing point more than 700 DEG C, separation purity are high;2nd, pure magnesium, pure bismuth be on the market
Be easy to get, fusing point it is not high so that separating technology is easily manipulated, and magnesium, bismuth do not generate toxic action to environment or human body;3rd, it carries
Magnesium that pure procedure is used, bismuth metal auxiliary material can Reusability, process only uses electric energy, there's almost no physical deterioration, save
Cost;4th, it is not high because being related to temperature for the atmosphere furnace clever structure of mixed metal powder separation method, it is easy to build, and
It is few by being polluted between separated powder.
Description of the drawings
Fig. 1 is the atmosphere furnace structure diagram for mixed metal powder separation method.
Fig. 2 is the first structure diagram for pushing agitating plate.
Fig. 3 is active clapboard structure diagram.
In Fig. 1:1- two-chamber charging carriages, 2- intake valves, 3- atmosphere furnace shells, furnace chamber under 4-, 5- support plates, 501- first are logical
Stomata, the first leaks of 502-, the second ventholes of 503-, the upper furnace chambers of 6-, the first refractory seals of 7-, the first sliding blocks of 8-, 9- electricity
Heating tube, 10- separation wares, 11- bell gaskets, 12- bells, 1201- bell ventholes, the first powder of 13-, 14- ventilations
Pipe, 15- powder hoppers, 16- powder hopper lids, 17- mixed-powders, 18- air outlet valves, 19- powder hoppers switch, 20- magnesium bismuth alloy liquid, 1202- stoves
Lid powder-exhausting hole, 21- first push agitating plate, and the second refractory seals of 22-, 23- third refractory seals, 24- second, which is pushed, to be stirred
Mix plate, 25- active clapboards, the 4th refractory seals of 26-, the 5th refractory seals of 27-, the 6th refractory seals of 28-, 29- is small
Vehicle inlet/outlet, 30- trolleies disengaging door sealing, second of powder of 31-, 101- stirring motors, 102- trolley draw rings, 103- trolleies are right
Chamber, the second leaks of 504-, the second guide grooves of 32-, the 7th refractory seals of 33-, the second sliding blocks of 34-, the first guide grooves of 35-, 104-
Trolley left chamber, 105- agitating augers;
In Fig. 2:2101- scraper plates, 2102- plush coppers, 2103- deflector holes, 2104- scraper plate push rods, 2105- thrust pins;
In Fig. 3:2501- partition boards, 2502- partition board push rods.
Specific embodiment
The present invention is further described with reference to the accompanying drawings and embodiments.
A kind of mixed metal powder separation method, including a preprocessing process:Before 3D printing, spherical shape is selected,
And particle size distribution range is identical, maximum particle diameter is less than the two or more metal powders of 2 times of minimum grain sizes as more material metals zero
Part 3D printing material.
To the mixed-powder after pretreated 3D printing, separating-purifying step is as follows:
(1)Using screening plant, preferably magnetic suspension vibrating sieves, and with reference to the standard screen of suitable mesh number, removes ruler in mixed-powder
The very little powder particle for being more than 2 times of minimum grain sizes obtains purification mixed metal powder to be separated.
(2)According to the component powders density of purification mixed metal powder to be separated, judgement institute is required to mixed metal powder
The liquid medium density of separation, liquid medium density should be between two kinds of powder densities to be separated.
(3)Pure magnesium as needed for the calculating of formula d=a%*1.74+ (1-a%) * 9.8 forms the aluminium alloy of liquid medium density d
The mass percent of mass percent a% and pure bismuth (1-a%), and choose purity respectively by the mass percent calculated and be
More than 99.99% pure magnesium and pure bismuth metal auxiliary material, the total volume of two kinds of metal auxiliary materials should be greater than the mixed metal of purification to be separated
Powder volume.
(4)Two kinds of simple metal auxiliary materials are added in atmosphere furnaces, are filled with more than 99.99% argon gas as protective gas, then general
Atmosphere furnace is warming up to the suitable temperature less than component powders fusing point in mixed-powder, is completely melt two kinds of simple metal auxiliary materials, and
Appropriate stirring, makes two kinds of simple metal form the magnesium bismuth alloy liquid of infinitely dissolve in atmosphere furnace.
(5)Mixed metal powder is added in the magnesium bismuth alloy solution in atmosphere furnace, stirring after ten minutes, then is stood certain
Time makes mixed-powder be layered in aluminium alloy by density.
(6)Aluminium alloy top powder will be floated on and be sunken to the powder of aluminium alloy lower part under the protective atmosphere protection of atmosphere furnace
It is fetched into respectively in different containers, container carries electric mixer.
(7)Then after atmosphere furnace is cooled to room temperature, container is taken out, is placed in vacuum distillation furnace.
(8)Control vacuum distillation furnace that there is suitable pressure, the pressure for making vacuum distillation furnace is 0.001-1Pa, then will
Temperature is heated to suitable temperature, which is higher than the boiling point of simple metal auxiliary material used under the pressure, but less than mixed metal powder
The fusing point of the component powders at end, and kept the temperature, soaking time passes through the electric mixing in container depending on metal powder amount
Device stirring metal powder is mixed, magnesium, bismuth element that metal powder surface adheres to is made fully to evaporate, is vaporized through very in magnesium, bismuth element
When on the condenser in empty retort, the condensation of magnesium bismuth steam is carried out, is recycled after solidification.
(9)After magnesium bismuth alloy on evaporating completely removal powder particle, when furnace temperature drops to room temperature, container is taken out, this
When container in the powder that is filled be exactly powder after separating-purifying.
During the mixed metal powder more than two, remaining dystectic metal powder is evaporated through vacuum distillation furnace distillation
End repeats above-mentioned steps(2)-(9)Separating-purifying process, until the metal powder in powder containing only single component, you can complete
The separating-purifying of pairs of various metals mixed-powder.
In the step(8)In every time be evaporated in vacuo after condensation magnesium bismuth alloy, for save cost for the sake of, can not be right
Magnesium bismuth alloy carries out separating-purifying, but is reused directly for similarly meeting the magnesium bismuth alloy density after next remelting between two
The mixed metal powder separating-purifying of condition between kind powder density to be separated, at this moment can save step(3), and by step
(4)It is changed to:Magnesium bismuth alloy auxiliary material of the density of recycling between two kinds of powder densities to be separated is added in atmosphere furnace, auxiliary material
Total volume should be greater than the mixed metal powder volume of purification to be separated, be filled with more than 99.99% argon gas as protective gas,
Atmosphere furnace is warming up to suitable temperature again, two kinds of simple metal auxiliary materials is made to be completely melt, and suitably stir, two kinds of simple metal is made to exist
The magnesium bismuth alloy liquid of infinitely dissolve is formed in atmosphere furnace.
Referring to Fig. 1-Fig. 3, a kind of atmosphere furnace for mixed metal powder separation method, atmosphere furnace is by being placed in intermediate branch
Board 5 is divided into upper furnace chamber 6 and lower furnace chamber 4, and separation ware 10 is provided in upper furnace chamber 6, detaches interior setting electrical heating on 10 wall of ware
Pipe 9 can heat material in separation ware 10;Set in ware 10 is detached there are one lateral active clapboard 25, activity every
Plate 25 can be moved left and right is separated into disconnected two parts up and down by separation ware 10, plays the work of material in isolation separation ware 10
With;The top of two-part separation ware is separated by active clapboard 10 and lower part is respectively provided with a leakage hole, upper leakage hole passes through
First sliding block 8 realizes the on and off of upper leakage hole, and lower leakage hole realizes the on and off of upper leakage hole by the second sliding block 34;Separation
10 internal upper part of ware pushes agitating plate 21 equipped with first, lower part pushes agitating plate 24 equipped with second, is stirred for detaching material in ware 10
It mixes or the passage of sliding block or salvage stores pushes;Two-chamber charging carriage 1, a left side for two-chamber charging carriage 1 are equipped in lower furnace chamber 4
Chamber 104 and right chamber 103 are respectively used to load the top material being separated by active clapboard 25 in separation ware 10 and lower part material.
The ware 10 that detaches is square hollow structure, opened upper end, on support plate 5, the underface of bell 12.
It is stayed on the support plate 5 there are four hole, the first venthole 501, the second venthole 503 are used for upper and lower protective gas
Connection;Intermediate holes is respectively the first leak 502 and the second leak 504, be respectively used to separate in ware 10 by activity every
It is let out under top material and lower part material that plate 25 is separated into.
The active clapboard 25 includes partition board 2501,2502 two parts of partition board push rod, and partition board 2501 is with detaching inside ware 10
Space is wide, length is slightly larger than separation 10 inner space length of ware, and 2501 top surface of partition board is with detaching leakage hole bottom phase on ware 10
Cut, that bottom surface with second pushes 24 top surface of agitating plate is tangent, 2502 one end of partition board push rod is connected with partition board 2501, and the other end stretches out gas
Outside atmosphere furnace shell 3, in partition board 2501 with detaching 10 contact position of ware equipped with the second refractory seals 22, partition board push rod 2502 and atmosphere furnace
3 joint of shell is designed with the 5th refractory seals 27.
Two leakage hole, the first sliding block 8, the second sliding block 34 all with to detach 10 inner space of ware wide, upper leakage hole leads to
It crosses the first guide groove 35 with the first leak 502 on support plate 5 to be connected, lower leakage hole passes through the second guide groove 32 and support plate 5
On the second leak 504 be connected, the first sliding block 8 is led horizontal through the first guide groove 35, the second sliding block 34 horizontal through second
Slot 32.First sliding block 8 and 35 joint of the first guide groove are provided with the first refractory seals 7, the second sliding block 34 and the second guide groove 32
Joint is provided with the 7th refractory seals 33.
Described first pushes agitating plate 21 by scraper plate 2101, plush copper 2102, deflector hole 2103, scraper plate push rod 2104, thrust
2,105 5 part of pin forms.Scraper plate 2101 is wide with detaching 10 inner space of ware, and the upper end is provided with multiple for the material that circulates
Deflector hole 2103, with reduce push agitating plate movement when the resistance from material.2101 side of scraper plate is provided with to slide
The plush copper 2102 that block is pushed open, plush copper 2102 is cylinder, and 2102 cylindrical surface of plush copper and 2101 bottom surface of scraper plate are tangent, and length is with inciting somebody to action
First sliding block 8 is pushed away from detaching 10 inner wall joint place of ware to equal with the distance of 35 inner wall joint place of the first guide groove, and diameter is small
In 8 thickness of the first sliding block.2104 side of scraper plate push rod is connected across separation 10 top surface of ware and scraper plate 2101, and opposite side reaches gas
Outside atmosphere furnace shell 3, length need to ensure that scraper plate 2101 can push away the first sliding block 8 to first from detaching 10 inner wall joint place of ware
35 inner wall joint place of guide groove is additionally provided with 2105 mounting hole of thrust pin reaching the side outside atmosphere furnace shell 3, can install thrust
Pin 2105, can make to mix used time plush copper 2102 and not contact the first sliding block 8.In the scraper plate push rod 2104 that first pushes agitating plate 21
The 4th refractory seals 26 are equipped with 3 joint of atmosphere furnace shell.Thrust pin 2105 first push agitating plate 21 for stir divide
From being loaded onto during material in ware 10, removed when for pushing leakage hole in the first sliding block 8 opening open or when pushing salvage stores.First
When pushing the installation of agitating plate 21, it must ensure that 2101 bottom surface of scraper plate and the top surface of active clapboard 25 fit, to guarantee effectively to go
Except the salvage stores on active clapboard 25.
Described second shape for pushing agitating plate 24 forms that push agitating plate 21 with first identical, only size and installation position
Put difference, plush copper length is pasted with by the second sliding block 34 from pushing away to 32 inner wall of the second guide groove with detaching 10 inner wall joint place of ware
Distance at conjunction is equal, and diameter is less than 34 thickness of the second sliding block.Its scraper plate push rod side passes through separation 10 inner wall of ware to consolidate with scraper plate
Even, opposite side reached outside atmosphere furnace shell 3, length need to ensure second push agitating plate 24 can be by the second sliding block 34 from detaching
10 inner wall joint place of ware push away to 32 inner wall joint place of the second guide groove.It is set in its scraper plate push rod with detaching 10 inner wall joint of ware
There are third refractory seals 23;The 6th refractory seals 28 are equipped in its scraper plate push rod and 3 joint of atmosphere furnace shell.Its thrust pin
Agitating plate 24 is pushed second for being loaded onto when being sirred and separated material in ware 10, is leaked for pushing open under the second sliding block 34 is opened
It is removed during mouth or when pushing salvage stores.Second push agitating plate 24 install when, must ensure scraper plate bottom surface with detaching inside ware 10
Bottom surface fits, and the salvage stores detached in 10 inner bottom surface of ware can be effectively removed by pushing agitating plate 24 with guarantee second.
4 side of lower furnace chamber be equipped with trolley inlet/outlet 29, set between trolley inlet/outlet 29 and lower furnace chamber there are one annular
Gasket 30, gasket material is using heat-resisting materials such as ceramic fiber mats;Trolley inlet/outlet 29, Gask-O-Seal 30 are in gas
During atmosphere furnaceman makees, it is fixed on lower furnace chamber using butterfly-type screw.
The two-chamber charging carriage 1 is equipped with trolley draw ring 102, for two-chamber charging carriage 1 to be taken out from atmosphere furnace;
Stirring motor 101 and agitating auger 105 are additionally provided with, material in stirring two-chamber charging carriage during for being subsequently evaporated in vacuo.
The top of the atmosphere furnace be equipped with bell 12, set between bell 12 and atmosphere furnace there are one annular bell gasket
11, the material of bell gasket 11 is made of heat-resisting materials such as ceramic fibre mats, the wing bolt that bell 12 passes through both ends
It is fixed in atmosphere furnace.
The bell 12 is additionally provided with one and the powder hopper 15 being connected in atmosphere furnace above, and 15 top of powder hopper is equipped with powder hopper
Lid 16, powder hopper lid 16 can be used screw and be fixed in powder hopper 15;12 middle part of bell is provided with bell powder-exhausting hole 1202, with powder hopper 15
Outlet, which connects, realizes that powder hopper 15 is connected with atmosphere furnace;Powder hopper switch 19, powder switch 19 are provided on the blanking direction of powder hopper 15
Preferably butterfly valve, for controlling the mixed-powder blanking in powder hopper 15.
12 top of bell is additionally provided with that 15 top of powder hopper is made to keep the snorkel 14 ventilated, upper part with atmosphere furnace
It is connected with powder hopper 15, lower part is connect with bell venthole 1201, realizes that powder hopper top keeps logical at any time with atmosphere furnace
Gas.
Described that intake valve 2 is equipped in atmosphere furnace lower part, gas is protected in 16 top of powder hopper lid equipped with air outlet valve 18 for passing in and out
Body.
First refractory seals 7, the second refractory seals 22, third refractory seals 23, the 4th refractory seals
26th, the 5th refractory seals 27, the 6th refractory seals 28, the 7th refractory seals 33, all including mounting base and mounted on peace
The sealing material in seat is filled, sealing material is preferably graphite packing.
A kind of application method of atmosphere furnace for mixed metal powder separation method is as follows using process:
(1)Bell 12 is opened, the position that the first sliding block 8 and the second sliding block 34 are pushed into fit with detaching 10 inner wall of ware makes point
From ware about 10 two leakage holes be closed;Trolley inlet/outlet 29 is opened, two-chamber charging carriage 1 is placed in lower furnace chamber 4
It is interior, make its two chamber of left and right respectively immediately below two leaks of support plate 5, close trolley inlet/outlet 29;Two are pushed and is stirred
Mix the scraper plate push rod of plate, active clapboard push rod 2502 is pulled outwardly, the plate face of scraping for pushing agitating plate is made to be affixed with detaching 10 inner wall of ware
It closes, partition board 2501 is closed with the scraper plate face paste where pushing agitating plate plush copper;
(2)The pure magnesium metal auxiliary material of appropriate mass is chosen by precalculated proportioning and the pure bismuth metal auxiliary material of appropriate mass is thrown
Enter into separation ware 10.
(3)Bell 12 is closed, the powder hopper switch 19 in powder hopper 15 is closed, opens powder hopper lid 16, be sieving through described in addition
Mixed-powder 17, be then shut off powder hopper lid 16.
(4)Intake valve 2 and air outlet valve 18 are opened, purity is filled with up to more than 99.99% argon gas, treats oxygen at air outlet valve 18
Mass percentage be down to less than 0.05% after, atmosphere furnace is warming up to by suitable temperature by the electric heating tube 9 detached in ware 10
Degree, is completely melt two kinds of simple metal auxiliary materials.Agitating plate 21 is pushed first and second is pushed and is loaded onto thrust pin on agitating plate 24,
Then two are pushed and pushes agitating plate agitated liquid, two kinds of simple metal is made to form the magnesium bismuth alloy of infinitely dissolve in atmosphere furnace
Liquid.
(5)The powder hopper switch 19 in powder hopper 15 is opened, mixed metal powder 17 is added in separation ware 10, using first
It pushes agitating plate 21 and second pushes agitating plate 24 and continuously stir 10 minutes.
(6)Mixture is stood into certain time, mixed-powder is made to be layered in aluminium alloy by density.
(7)Active clapboard 25 is pushed home into, separation ware 10 is separated to open and is divided into two parts from intermediate liquid, is detached in ware 10
The material of more than 25 active clapboard shows as metal powder in upper, liquid auxiliary materials under, and active clapboard is below 25 in separation ware 10
Material show as metal powder under, liquid auxiliary materials are upper.
(8)It removes first to push agitating plate 21 and second push thrust pin on agitating plate 24, inwardly pushes two to push and stirs
Plate is mixed to the opposite side for detaching ware 10, makes first to push agitating plate 21 and second push agitating plate 24 and the opposite side that detaches ware 10
Inner wall fits, and respectively pushes the first sliding block 8 and the second sliding block 34 open, and so as to open two leakage mouths, subsequent two push agitating plate
It resets, then detaches in ware 10 25 top material of active clapboard through being let out under corresponding first guide groove 35 to a left side for two-chamber charging carriage 1
Chamber 104, detach ware 10 in 25 lower part material of active clapboard through being let out under corresponding second guide groove 32 to the right chamber of two-chamber charging carriage 1
103。
(9)By first push agitating plate 21 and second push agitating plate 24 inwardly push, will separation 10 inner wall of ware, bottom,
And active clapboard about 25 the material of two surface residuals push at two leakage holes, make to share material in ware 10 as much as possible
It is collected on two-chamber charging carriage 1.
(10)The electric heating tube 9 on separation ware 10 is closed, when atmosphere furnace is fully cooled to room temperature, is opened in atmosphere furnace
Trolley inlet/outlet 29, the trolley draw ring 102 on two-chamber charging carriage 1 is caught on hook, and two-chamber charging carriage 1 is pulled out atmosphere
Stove, for subsequently removing demagging bismuth.
The magnesium bismuth alloy that the positive effect of the present invention is 1, is pre-processed, sieved by combining powder, different densities are configured is molten
The means such as liquid reduce the mixed metal powder after principle separating-purifying 3D printing, Ke Yishi based on law of buoyancy and decompression boiling point
Now the separating-purifying of most of mixed metal powder of the fusing point more than 700 DEG C, separation purity are high;2nd, pure magnesium, pure bismuth be on the market
Be easy to get, fusing point it is not high so that separating technology is easily manipulated, and magnesium, bismuth do not generate toxic action to environment or human body;3rd, it carries
Magnesium that pure procedure is used, bismuth metal auxiliary material can Reusability, process only uses electric energy, there's almost no physical deterioration, save
Cost;4th, it is not high because being related to temperature for the atmosphere furnace clever structure of mixed metal powder separation method, it is easy to build, and
It is few by being polluted between separated powder.
Embodiment one:
The spherical 316L stainless steel powders that particle size range is 28-53 microns are selected before 3D printing(Density:7.98 gram/cc)
With the spherical Ti6Al4V Titanium Powders that particle size range is 28-53 microns(Density:4.4 gram/cc)Two kinds of metal powders are made
For 3D printing material, completing the remaining mixed-powder process for separation and purification after 3D printing is:
(1)Selection mesh number is 270 the polished standard screens(Corresponding mesh size is 50 microns), it is fixed on magnetic suspension vibrating sieve, and
Remaining mixed-powder is poured into be sieved, then it is a small number of during 3D printing to be sintered bimetallic that is pockets of, being difficult to separating-purifying
Multicomponent metallic cluster of grains, the size overwhelming majority are more than 56 microns, and the diameter of spheroidized particle is also most to be more than starting powder
Several times of particle, therefore, these substances overwhelming majority will be left in standard screen, then are purification to be separated by the powder of standard screen
Mixed-powder 17.
(2)Bell 12 is opened, the first sliding block 8 and the second sliding block 34 are pushed into, with detaching 10 inner wall joint place of ware, to make separation
Ware about 10 two leakage holes be closed;Trolley inlet/outlet 29 is opened, two-chamber charging carriage 1 is placed in lower furnace chamber 4,
Make its two chamber of left and right respectively immediately below two leaks of support plate 5, close trolley inlet/outlet 29;Agitating plate is pushed by two
Scraper plate push rod, active clapboard push rod 2502 be pulled outwardly, make to push agitating plate scrape plate face fit with detaching 10 inner wall of ware, every
Plate 2501 is closed with the scraper plate face paste where pushing agitating plate plush copper.
(3)By pure magnesium, pure bismuth metal auxiliary material in mass ratio 4:6 are equipped with, and the magnesium of outfit, bismuth mixed metal auxiliary material are put into gas
In separation ware 10 in atmosphere stove.
(4)The powder hopper switch 19 in powder hopper 15 is closed, the powder hopper lid 16 in powder hopper 15 is opened, adds in the mixed powder that need to be detached
End is then shut off the powder hopper lid 16 of powder hopper 15.
(5)Bell 12 is pressed tightly against at the top of atmosphere furnace by wing bolt and bell gasket 11, opens intake valve 2
And air outlet valve 18, purity is filled with up to more than 99.99% argon gas, treats the mass percentage drop of 18 exit oxygen at air outlet valve
To after less than 0.05%, 700 DEG C are warming up to by ware 10 is detached by detaching the heating tube 9 in ware 10, makes two kinds of simple metal auxiliary materials complete
Running down.Agitating plate 21 is pushed first and the second push rod end for pushing agitating plate 24 loads onto thrust pin, and then pushing two pushes away
Agitating plate agitated liquid is scraped, two kinds of simple metal is made to form the magnesium bismuth alloy liquid of infinitely dissolve in atmosphere furnace.
(6)The powder hopper switch 19 in powder hopper 15 is opened, mixed metal powder 17 is added in separation ware 10, pushes first to push away
It scrapes agitating plate 21 and second pushes agitating plate 24 and continuously stir 10 minutes.
(7)First pushes agitating plate 21 and second pushes agitating plate 24 and reset, and mixture is stood 20 minutes or more, makes to mix
Powder is closed to be layered in aluminium alloy by density.
(8)Active clapboard 25 is pushed home into, separation ware 10 is separated to open and is divided into two parts from intermediate liquid, is detached in ware 10
The material of more than 25 active clapboard shows as metal powder in upper, liquid auxiliary materials under, and active clapboard is below 25 in separation ware 10
Material show as metal powder under, liquid auxiliary materials are upper.
(9)It removes first to push agitating plate 21 and second push thrust pin on agitating plate 24, inwardly pushes two to push and stirs
Plate is mixed to the opposite side for detaching ware 10, makes first to push agitating plate 21 and second push agitating plate 24 and the opposite side that detaches ware 10
Inner wall fits, and respectively pushes the first sliding block 8 and the second sliding block 34 open, and so as to open two leakage mouths, subsequent two push agitating plate
It resets, then detaches in ware 10 25 top material of active clapboard through being let out under corresponding first guide groove 35 to a left side for two-chamber charging carriage 1
Chamber 104, detach ware 10 in 25 lower part material of active clapboard through being let out under corresponding second guide groove 32 to the right chamber of two-chamber charging carriage 1
103。
(10)The heating tube 9 on separation ware 10 is closed, when atmosphere furnace is fully cooled to room temperature, is opened small in atmosphere furnace
Vehicle inlet/outlet 29, the trolley draw ring 102 on two-chamber charging carriage 1 is caught on hook, and two-chamber charging carriage 1 is pulled out atmosphere furnace,
For subsequently removing demagging bismuth.
(11)Two-chamber charging carriage 1 is put into vacuum distillation furnace.Control vacuum distillation furnace that there is suitable pressure, generally
Ground, the pressure that can make vacuum distillation furnace are 0.001-1Pa.Then in-furnace temperature is heated to suitable temperature, which is higher than should
The boiling point of magnesium and bismuth under pressure, but far below 316L powder of stainless steel and the fusing point of Ti6Al4V titanium alloy powders, generally regarding vacuum
Retort pressure value value in the range of 500-690 DEG C.And keep the temperature to the suitable time, make magnesium that metal powder surface adheres to,
Bismuth element fully evaporates, while starts the stirring motor 101 on double-chamber unit trolley 2, and agitating auger 105 is made to stir material, is added
Liquid evaporation on fast metal powder granulates.When on the condenser being vaporized through in vacuum distillation furnace in magnesium, bismuth element, magnesium is carried out
Bismuth steam condenses, and is recycled after solidification.
(12)After magnesium bismuth alloy on evaporating completely removal powder particle, when furnace temperature drops to room temperature, two-chamber dress is taken out
Trolley 1 is carried, at this moment the metal powder in 1 left chamber 104 of two-chamber charging carriage is the Ti6Al4V Titanium Powders after separating-purifying, right
Metal powder in chamber 103 is the 316L stainless steel powders after separating-purifying.
Embodiment two:
Ti6AlV4 Titanium Powders are selected before 3D printing(Density:4.4 gram/cc), Inconel718 high temperature nickel alloy powder
(Density:8.24 gram/cc), fine silver powder(Density:10.5 grams/cc)Three kinds of metal powders as moulding material,
The particle size range of three kinds of powder is all 38-75 microns, and pattern is all spherical.Then complete the separation of the remaining mixed-powder after 3D printing
Method of purification is:
(1)Selection mesh number is 200 the polished standard screens(Corresponding mesh size is 75 microns), it is fixed on magnetic suspension vibrating sieve, and
Remaining mixed-powder is poured into be sieved.Because 3D printing process minority be sintered bimetallic that is pockets of, being difficult to separating-purifying into
Parting metal particles group, the size overwhelming majority are more than 76 microns, and the diameter of spheroidized particle is also most to be more than starting powder
Several times of grain, therefore, these substances overwhelming majority will be left in standard screen, then is purification to be separated by the powder of standard screen
Mixed-powder 17.
(2)Bell 12 is opened, the first sliding block 8 and the second sliding block 34 are pushed into, with detaching 10 inner wall joint place of ware, to make separation
Ware about 10 two leakage holes be closed;Trolley inlet/outlet 29 is opened, two-chamber charging carriage 1 is placed in lower furnace chamber 4,
Make its two chamber of left and right respectively immediately below two leaks of support plate 5, close trolley inlet/outlet 29;Agitating plate is pushed by two
Scraper plate push rod, active clapboard push rod 2502 be pulled outwardly, make to push agitating plate scrape plate face fit with detaching 10 inner wall of ware, every
Plate 2501 is closed with the scraper plate face paste where pushing agitating plate plush copper.
(3)Bell 12 is opened, pure bismuth metal auxiliary material is put into the separation ware 10 in atmosphere furnace.
(4)The powder hopper switch 19 in powder hopper 15 is closed, the powder hopper lid 16 of powder hopper 15 is opened, adds in the mixed powder that need to be detached
End is then shut off the powder hopper lid 16 of powder hopper 15.
(5)Bell 12 is pressed tightly against at the top of atmosphere furnace by wing bolt and bell gasket 11, opens intake valve 2
And air outlet valve 18, purity is filled with up to more than 99.99% argon gas, treats the mass percentage drop of 18 exit oxygen at air outlet valve
To after less than 0.05%, 350 DEG C are warming up to by ware 10 is detached by detaching the heating tube 9 in ware 10, makes pure bismuth auxiliary material completely molten
Change.
(6)The powder hopper switch 19 in powder hopper 15 is opened, mixed metal powder 17 is added in separation ware 10, pushes first to push away
It scrapes agitating plate 21 and second pushes agitating plate 24 and continuously stir 10 minutes.
(7)First pushes agitating plate 21 and second pushes agitating plate 24 and reset, and mixture is stood 20 minutes or more, makes to mix
Powder is closed to be layered in aluminium alloy by density.
(8)Active clapboard 25 is pushed home into, separation ware 10 is separated to open and is divided into two parts from intermediate liquid, is detached in ware 10
The material of more than 25 active clapboard shows as Ti6AlV4 titanium alloy+Inconel718 high temperature nickel alloys mixed-powders in upper, liquid
Auxiliary material detaches material of the active clapboard below 25 in ware 10 and shows as fine silver powder under, liquid auxiliary materials are upper under.
(9)It removes first to push agitating plate 21 and second push thrust pin on agitating plate 24, inwardly pushes two to push and stirs
Plate is mixed to the opposite side for detaching ware 10, makes first to push agitating plate 21 and second push agitating plate 24 and the opposite side that detaches ware 10
Inner wall fits, and respectively pushes the first sliding block 8 and the second sliding block 34 open, and so as to open two leakage mouths, subsequent two push agitating plate
It resets, then detaches in ware 10 25 top material of active clapboard through being let out under corresponding first guide groove 35 to a left side for two-chamber charging carriage 1
Chamber 104, detach ware 10 in 25 lower part material of active clapboard through being let out under corresponding second guide groove 32 to the right chamber of two-chamber charging carriage 1
103。
(10)The heating tube 9 on separation ware 10 is closed, when atmosphere furnace is fully cooled to room temperature, is opened small in atmosphere furnace
Vehicle inlet/outlet 29, the trolley draw ring 102 on two-chamber charging carriage 1 is caught on hook, and two-chamber charging carriage 1 is pulled out atmosphere furnace,
For subsequently removing demagging bismuth.
(11)Two-chamber charging carriage 1 is put into vacuum distillation furnace.Control vacuum distillation furnace that there is suitable pressure, generally
Ground, the pressure that can make vacuum distillation furnace are 0.001-1Pa.Then in-furnace temperature is heated to suitable temperature, which is higher than should
The boiling point of pure bismuth under pressure, but the fusing point of the component powders less than mixed metal powder, generally exist regarding vacuum distillation furnace pressure value
Value in the range of 500-690 DEG C.And keep the temperature the bismuth element for the suitable time adhering to, metal powder surface and fully evaporate, together
Stirring motor 101 on Shi Qidong double-chamber units trolley 2 makes agitating auger 105 stir material, accelerates on metal powder granulates
Liquid evaporation.When on the condenser being vaporized through in vacuum distillation furnace in bismuth element, bismuth steam condensation is carried out, profit is recycled after solidification
With.
(12)After magnesium bismuth alloy on evaporating completely removal powder particle, when furnace temperature drops to room temperature, two-chamber dress is taken out
Carry trolley 1, at this moment the metal powder in 1 left chamber 104 of two-chamber charging carriage for the Ti6AlV4 titanium alloys after separating-purifying+
Inconel718 high temperature nickel alloy mixed-powders, the metal powder in right chamber 103 are the fine silver powder after separating-purifying.
In this way, the fine silver powder in 1 right chamber of two-chamber charging carriage has been purified, but the Titanium Powder in right chamber
Ti6AlV4+Inconel718 mixed metal powders still need to further separating-purifying.
At this moment can first will separation ware, guide groove, active clapboard, first push agitating plate, second push agitating plate and be heated to 680
DEG C, the liquid or particle of its surface adhesion are cleaned, then using one technology of embodiment, you can separating-purifying respectively obtains titanium
Alloyed powder Ti6AlV4 and Inconel718 alloy powder.So as to complete the separating-purifying of the metal powder to three kinds of ingredient mixing.
It is different from other mixed metal process for separation and purification, it pre-processed by combining powder, sieve, different densities is configured
The means such as magnesium bismuth alloy solution reduce the mixed metal powder after principle separating-purifying 3D printing based on law of buoyancy and decompression boiling point
End can realize the separating-purifying of mixed metal powder of most of fusing point more than 700 DEG C, have separation purity height, operation letter
The features such as single and at low cost.Also there is clever structure for the atmosphere furnace of mixed metal powder separation method simultaneously, be easy to build,
And the advantages that few is polluted between separated powder.
Above-mentioned two embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, letter
Change, should be equivalent substitute mode, be included within protection scope of the present invention.
Claims (10)
1. a kind of mixed metal powder separation method, it is characterised in that:Including being pre-processed before a 3D printing, select it is spherical,
And particle size distribution range is identical, maximum particle diameter is less than the two or more metal powders of 2 times of minimum grain sizes as metal gradient material
Part 3D printing material;
To the mixed-powder after pretreated 3D printing, separating-purifying step is as follows:
(1)Size is more than the powder particle of 2 times of minimum grain sizes in screening removal mixed-powder;
(2)According to the component powders density of purification mixed metal powder to be separated, judgement institute detaches required to mixed metal powder
Liquid medium density, liquid medium density should be between two kinds of powder densities to be separated;
(3)Pure magnesia amount as needed for the calculating of formula d=a%*1.74+ (1-a%) * 9.8 forms the aluminium alloy of liquid medium density d
The mass percent of percentage a% and pure bismuth (1-a%), and by the mass percent calculated choose respectively purity for 99.99% with
On pure magnesium and pure bismuth metal auxiliary material, the total volume of two kinds of metal auxiliary materials should be greater than the mixed metal powder opisthosoma of purification to be separated
Product;
(4)Two kinds of simple metal auxiliary materials are added in atmosphere furnaces, are filled with more than 99.99% argon gas as protective gas, then by atmosphere
Stove is warming up to the suitable temperature less than component powders fusing point in mixed-powder, is completely melt two kinds of simple metal auxiliary materials, and appropriate
Stirring, makes two kinds of simple metal form the magnesium bismuth alloy liquid of infinitely dissolve in atmosphere furnace;
(5)Mixed metal powder is added in the magnesium bismuth alloy solution in atmosphere furnace, stirring after ten minutes, then stands a timing
Between, mixed-powder is made to be layered in aluminium alloy by density;
(6)The powder for floating on aluminium alloy top powder and be sunken to aluminium alloy lower part is taken out be placed in different vessels respectively, is held
Electric mixer is carried in device;
(7)After temperature is down to below room temperature in atmosphere furnace, container is taken out, is placed in vacuum distillation furnace;
(8)Control vacuum distillation furnace that there is suitable pressure, the pressure for making vacuum distillation furnace is 0.001-1Pa, then by temperature
Suitable temperature is heated to, which is higher than the boiling point of simple metal auxiliary material used under the pressure, but less than mixed metal powder
The fusing point of component powders, and held for some time, while metal powder is stirred by the electric mixer in container, make metal powder
Magnesium, the bismuth element of last surface adhesion fully evaporate, when on the condenser being vaporized through in vacuum distillation furnace in magnesium, bismuth element, into
Row magnesium bismuth steam condenses, and is recycled after solidification;
(9)After magnesium bismuth alloy on evaporating completely removal powder particle, when furnace temperature drops to room temperature, container is taken out, is at this moment held
The powder filled in device is exactly the powder after separating-purifying.
2. mixed metal powder separation method as described in claim 1, it is characterised in that:The mixed metal powder more than two
When, remaining dystectic metal powder is evaporated through vacuum distillation furnace distillation, repeats above-mentioned steps(2)-(9)Separating-purifying mistake
Journey, until the metal powder in powder containing only single component, you can complete the separating-purifying to various metals mixed-powder.
3. mixed metal powder separation method as described in claim 1, it is characterised in that:In the step(8)In each vacuum
The magnesium bismuth alloy of condensation after distillation for the sake of saving cost, can not carry out separating-purifying to magnesium bismuth alloy, but in next time
It is reused directly for similarly meeting the mixed of the condition of the magnesium bismuth alloy density between two kinds of powder densities to be separated after remelting
Metal powder separating-purifying is closed, at this moment can save step(3), and by step(4)It is changed to:The density of recycling is treated between two kinds point
It is added in atmosphere furnace from the magnesium bismuth alloy auxiliary material between powder density, the total volume of auxiliary material should be greater than the mixing gold of purification to be separated
Belong to powder volume, the argon gas for being filled with more than 99.99% is warming up to suitable temperature as protective gas, then by atmosphere furnace, makes two kinds
Simple metal auxiliary material is completely melt, and is suitably stirred, and two kinds of simple metal is made to form the magnesium bismuth alloy liquid of infinitely dissolve in atmosphere furnace.
4. a kind of atmosphere furnace for mixed metal powder separation method as described in claim 1, it is characterised in that:Atmosphere furnace by
It is placed in intermediate support plate and is divided into upper furnace chamber and lower furnace chamber, separation ware is provided in upper furnace chamber, detach in-built electrical on ware wall and add
Heat pipe can heat material in separation ware;It is set in ware is detached there are one lateral active clapboard, active clapboard can
It moves left and right and separation ware is separated into disconnected two parts up and down, play the role of material in isolation separation ware;By activity every
Plate is separated into the top of two-part separation ware and lower part is respectively provided with a leakage hole, and two leakage holes are respectively realized by a sliding block
The on and off of leakage hole;Two leakage hole, sliding block all with to detach ware inner space wide, two leakage holes respectively by a guide groove with
Two leaks on support plate are respectively connected with leading to, and two sliding blocks are provided with resistance to height horizontal through corresponding guide groove with guide groove joint
Temperature sealing;Ware internal upper part pushes agitating plate equipped with first, lower part pushes agitating plate equipped with second for separation, for detaching material in ware
Stirring or the passage of leakage hole sliding block or pushing for salvage stores;Two-chamber charging carriage is equipped in lower furnace chamber, two-chamber loads small
The chamber of left and right two of vehicle is used for loaded material;Trolley inlet/outlet is equipped in lower furnace chamber side, between trolley inlet/outlet and lower furnace chamber
If there are one Gask-O-Seals.
5. it to be used for the atmosphere furnace of mixed metal powder separation method as claimed in claim 4, it is characterised in that:It is described separation ware be
Square hollow structure, opened upper end, on support plate, the underface of sealing cover;Hole there are four being stayed on support plate, both sides
Hole is used for the connection of upper and lower protective gas, and intermediate holes is leak, is let out under material for detaching in ware.
6. it to be used for the atmosphere furnace of mixed metal powder separation method as claimed in claim 4, it is characterised in that:The active clapboard
Including partition board, partition board push rod two parts, partition board is with detaching that ware inner space is wide, length is long slightly larger than ware inner space is detached
Degree, partition board top surface and detaches that leakage hole bottom on ware is tangent, bottom surface pushes tangent, partition board push rod one end of stirring plate top surface with second
It is connected with partition board, the other end stretches out atmosphere furnace, is designed in partition board with detaching ware contact position, partition board push rod and atmosphere furnace joint
Refractory seals.
7. the atmosphere furnace of mixed metal powder separation method to be used for as described in claim 4 or 6, it is characterised in that:High temperature resistant is close
Package includes mounting base and the sealing material in mounting base, and sealing material is preferably graphite packing.
8. it to be used for the atmosphere furnace of mixed metal powder separation method as claimed in claim 4, it is characterised in that:Described first pushes
Agitating plate is made of scraper plate, plush copper, deflector hole, scraper plate push rod, five part of thrust pin;Scraper plate is wide with detaching ware inner space,
The upper end is provided with multiple deflector holes for the material that circulates, the resistance from material when pushing agitating plate movement to reduce;It scrapes
Plate side is provided with for that will correspond to the plush copper that sliding block is pushed open, and plush copper is cylinder, and plush copper cylindrical surface and scraper plate bottom surface are tangent,
Length is pushed away from detaching ware inner wall joint place to, diameter equal with the distance of corresponding guide groove inner wall joint place with by corresponding sliding block
Less than corresponding sliding block thickness, scraper plate push rod one end is connected across separation ware top surface with scraper plate, and the other end is reached outside atmosphere furnace shell,
Its length need to ensure scraper plate can will corresponding sliding block from detach ware inner wall joint place push away to corresponding guide groove inner wall joint place,
It reaches the side outside atmosphere furnace shell and is additionally provided with removable thrust pin, can make to mix used time plush copper and do not contact corresponding sliding block;
The scraper plate push rod of agitating plate is pushed first and atmosphere furnace shell joint is equipped with refractory seals;First pushes agitating plate installation
When, it must ensure that the top surface of scraper plate bottom surface and active clapboard fits, so that first pushes agitating plate and can effectively remove active clapboard
On salvage stores;Described second shape for pushing agitating plate forms that push agitating plate with first identical, only size and installation position
Difference is put, plush copper length is elapsed from detaching ware inner wall joint place to corresponding to guide groove inner wall joint place with by corresponding sliding block
Apart from equal, plush copper diameter is less than corresponding sliding block thickness, and scraper plate push rod one end passes through separation ware inner wall to be connected with scraper plate, separately
One end is reached outside atmosphere furnace shell, length need to ensure scraper plate can will corresponding sliding block from detach ware inner wall joint place push away to
Corresponding guide groove inner wall joint place;In its scraper plate push rod with detaching ware inner wall joint, scraper plate push rod and atmosphere furnace shell joint all
Equipped with refractory seals;Second push agitating plate installation when, must ensure scraper plate bottom surface fit with detaching ware inner bottom surface so that
Second, which pushes agitating plate, can effectively remove the salvage stores detached in ware inner bottom surface.
9. it to be used for the atmosphere furnace of mixed metal powder separation method as claimed in claim 4, it is characterised in that:The atmosphere furnace
Top is equipped with bell, is set between bell and atmosphere furnace there are one the bell gasket of annular, the wing bolt that bell passes through both ends
It is fixed in atmosphere furnace;One and the powder hopper being connected in atmosphere furnace are additionally provided with above bell, powder hopper lid is equipped at the top of powder hopper;Stove
Lid middle part is provided with bell powder-exhausting hole, connects with powder hopper outlet and realizes that powder hopper is connected with atmosphere furnace;It is set on the blanking direction of powder hopper
Powder hopper switch is equipped with, powder switch is preferably butterfly valve;The bell top is additionally provided with that powder hopper top is made to keep with atmosphere furnace
The snorkel of ventilation, upper part are connected with powder hopper, and lower part is connect with bell venthole;The atmosphere furnace lower part is equipped with intake valve,
The powder hopper side of covering is equipped with air outlet valve, for passing in and out protective gas.
10. a kind of as claimed in claim 4 for the application method of the atmosphere furnace of mixed metal powder separation method, feature exists
In using process as follows:
(1)Bell is opened, the position that two sliding blocks are pushed into fit with detaching ware inner wall makes above and below separation ware at two leakage holes
In closed state;Trolley inlet/outlet is opened, two-chamber charging carriage is placed in lower furnace chamber, its two chamber of left and right is made to be located at two respectively
Immediately below leak, trolley inlet/outlet is closed;The scraper plate push rod and the partition board push rod of active clapboard for pushing agitating plate by two are outside
Draw, make two push agitating plate scrape plate face fit with detaching ware inner wall, the partition board of active clapboard with push agitating plate plush copper institute
Scraper plate face paste close;
(2)The pure magnesium metal auxiliary material of appropriate mass is chosen by precalculated proportioning and pure bismuth metal auxiliary material puts into separation ware
In, close bell;
(3)The powder switch in powder hopper is closed, opens powder hopper lid, the mixed-powder being sieving through described in addition is then shut off powder
Bucket cover;
(4)Intake valve and air outlet valve are opened, purity is filled with up to more than 99.99% argon gas, treats the quality percentage of oxygen at air outlet valve
After content is down to less than 0.05%, atmosphere furnace is warming up to less than ingredient powder in mixed-powder by detaching the electric heating tube in ware
The suitable temperature of last fusing point is completely melt two kinds of simple metal auxiliary materials;It is pushed two and thrust pin is loaded onto on agitating plate, then pushed
Two push agitating plate agitated liquid, and two kinds of simple metal is made to form the magnesium bismuth alloy liquid of infinitely dissolve in atmosphere furnace;
(5)The powder switch in powder hopper is opened, mixed metal powder is added in separation ware, is continuously stirred using agitating plate is pushed
10 minutes;
(6)Mixture is stood into certain time, mixed-powder is made to be layered in aluminium alloy by density;
(7)Active clapboard is pushed home into, separation ware is separated to open and is divided into two parts from intermediate liquid, material performance more than partition board
For metal powder in upper, liquid auxiliary materials under, detach ware internal partition below material show as metal powder under, liquid auxiliary materials
Upper;
(8)It removes two and pushes thrust pin on agitating plate, inwardly push two to push agitating plate to ware opposite side is detached, by two sliding blocks
It pushes open, so as to open two leakage mouths, subsequent two push stirring sheet reset, then active clapboard top material under corresponding guide groove through letting out
To the left chamber of two-chamber charging carriage, active clapboard lower part material under corresponding guide groove through letting out to the right chamber of two-chamber charging carriage;
(9)Agitating plate is pushed by two inwardly to push, and the material for detaching ware inner wall remnants is pushed at two leakage holes, makes separation ware
Interior material is collected into as much as possible on two-chamber charging carriage;
(10)The electric heating tube on separation ware is closed, when atmosphere furnace is cooled to room temperature, opens the trolley disengaging in atmosphere furnace
Door, the draw ring on trolley is caught on hook, two-chamber charging carriage is pulled out atmosphere furnace, for removing demagging bismuth in next step.
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CN110863108A (en) * | 2019-10-28 | 2020-03-06 | 中南大学 | Method for recovering platinum group metal in waste catalyst by melt extraction and vacuum distillation |
CN116735306A (en) * | 2023-05-19 | 2023-09-12 | 生态环境部南京环境科学研究所 | Device for screening out ferro-manganese nodules with various particle size sections from surface soil large sample |
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CN116735306B (en) * | 2023-05-19 | 2024-05-03 | 生态环境部南京环境科学研究所 | Device for screening out ferro-manganese nodules with various particle size sections from surface soil large sample |
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