CN108160305B - 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 PDF

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CN108160305B
CN108160305B CN201810126300.2A CN201810126300A CN108160305B CN 108160305 B CN108160305 B CN 108160305B CN 201810126300 A CN201810126300 A CN 201810126300A CN 108160305 B CN108160305 B CN 108160305B
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powder
ware
atmosphere furnace
furnace
mixed
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CN108160305A (en
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吴伟辉
李湘勤
黄长征
李银
范文明
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Shaoguan University
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Shaoguan University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION 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
    • B03BSEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
    • B03B5/00Washing granular, powdered or lumpy materials; Wet separating
    • B03B5/28Washing granular, powdered or lumpy materials; Wet separating by sink-float separation
    • B03B5/30Washing granular, powdered or lumpy materials; Wet separating by sink-float separation using heavy liquids or suspensions
    • B03B5/44Application of particular media therefor
    • B03B5/442Application of particular media therefor composition of heavy media
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION 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
    • B03BSEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
    • B03B5/00Washing granular, powdered or lumpy materials; Wet separating
    • B03B5/28Washing granular, powdered or lumpy materials; Wet separating by sink-float separation
    • B03B5/30Washing granular, powdered or lumpy materials; Wet separating by sink-float separation using heavy liquids or suspensions
    • B03B5/44Application of particular media therefor
    • B03B5/447Application 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, for mixed-powder separating-purifying after 3D printing, process for separation and purification include: (1) it is preselected it is spherical, particle size distribution range is identical, maximum particle diameter less than 2 times of minimum grain sizes two or more metal powders as 3D printing material.(2) separating-purifying step: to mixed powder after 3D printing, first screening goes size in gumming to be greater 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 for being thermally formed setting density 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 easy, low in cost, purification purity is high.

Description

A kind of mixed metal powder separation method and atmosphere furnace used
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 furnace.
Background technique
The research of 3D printing (also known as increasing material manufacturing) 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 is melted in selective laser ) and electron beam selection region melt-shaping (Electron Beam Selective Melting-EBSM) skill Melting-SLM Art is the metal parts 3D printing technique of the great development prospect of two of them, uses metal powder and is used as molding raw material, Working principle is as follows: the metal powder material of needs is first preset to the shaped platform with accurate elevating function by powder supply mechanism, Then computer control laser beam (to SLM) or electron beam (to EBSM) are 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, melts powder movement in constituency, forms new entity synusia.So successively powder is preset, successively fusing accumulation, most Entire part prints at last.
After molding, it can be melted into the metal powder of design of part for powdering process end, for the data of saving, need 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 valence using both 3D printing techniques Value largely sees if there is suitable mixed metal powder separation and method of purification.
For mixed metal powder separate a kind of method be using metal magnetism and it is non magnetic separate, this side Method can only separate two kinds of magnetism with nonmagnetic mixed metal powder, be all non magnetic for mixed metal powder or be all magnetic The powder of property can not efficiently separate purification.
It is to realize separating-purifying using centrifugal force there are also a kind of method, mixed metal powder is placed in centrifuge, utilizes Density contrast between material carries out separating-purifying at different rates.But because of the metal powder granulates granularity that 3D printing uses (such as 15-53 microns) in a certain range, particle varies, and diameter is small, light-weight, and this method is also difficult to do It is purified to efficiently separating.
It is using sieve method separating-purifying there are also a kind of method.But this method requires two kinds of powder, and there are apparent particles Difference in size, this is difficult to accomplish in the metal parts 3D printing technique that molding thickness is only 20-100 microns;And it is 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, it is easy because liquid state molten pool and solid-state basis wetability are bad, by surface tension effects, Fracture winding balling-up, i.e. generation spheroidized particle, and these new particles are also to be made of bimetallic material.Therefore, these are seeped Enter bimetallic ingredient granules or cluster of grains into mixed metal powder, further increases the separating-purifying of mixed metal powder Difficulty.
Therefore, the mixed metal powder after currently how efficiently separating purification 3D printing, is SLM technology and EBSM technology Realize metal gradient material parts 3D printing one of 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 pure 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 When with different mass percents, alloy melting point is different, such as when the mass percent of bismuth is 20%, magnesium bismuth alloy density is 3.352 grams/cc, the temperature of alloy is controlled at 640 DEG C or more, can obtain the magnesium bismuth alloy of liquid infinitely dissolve;Bismuth Mass percent when being 60%, magnesium bismuth alloy density is 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 at 300 DEG C or more, can obtain the pure bismuth of liquid.
Therefore, the two makees components matching appropriate, 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 can be effectively reduced under the premise of hardly changing alloy melting point.
During metal gradient material parts 3D printing, when selection is spherical, metal powder with same particle size range End be used as moulding material, and the maximum particle diameter of powder particle be no more than 2 times of minimum grain sizes when, 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 greater 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, the length dimension in molten bath are much larger than powder particle partial size, and width dimensions are generally also several times bigger than powder particle partial size, high Degree size is arranged then bigger than powder particle partial 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 mention to remove these most newborn bimetal granules from mixed metal powder Chance is supplied.
Summary of the invention
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 furnace, 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 has simple and easy, cost Feature cheap, 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, steps are as follows for separating-purifying:
(1) powder particle of the size greater than 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, determine institute required to mixed metal powder Isolated liquid medium density, liquid medium density should be between two kinds of powder densities to be separated;
(3) pure magnesium needed for the aluminium alloy of liquid medium density d is formed by the calculating of formula d=a%*1.74+ (1-a%) * 9.8 The mass percent (1-a%) of mass percent a% and pure bismuth, and choose purity respectively by mass percent calculated and be 99.99% or more 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 pure metal auxiliary materials are added in atmosphere furnaces, are filled with 99.99% or more argon gas as protective gas, then general Atmosphere furnace is warming up to the suitable temperature lower than component powders fusing point in mixed-powder, is completely melt two kinds of pure metal auxiliary materials, and Appropriate stirring, makes two kinds of pure 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 is layered mixed-powder in aluminium alloy by density;
(6) aluminium alloy top powder will be floated on and is sunken to the powder of aluminium alloy lower part and takes out be placed in different vessels respectively In, electric mixer is had in container;
(7) after temperature is down to room temperature or less in atmosphere furnace, container is taken out, is placed in vacuum distillation furnace;
(8) control vacuum distillation furnace has suitable pressure, makes the pressure 0.001-1Pa of vacuum distillation furnace, then will Temperature is heated to suitable temperature, which is higher than the boiling point of pure metal auxiliary material used under the pressure, but is lower than mixed metal powder The fusing point of the component powders at end, and held for some time, while metal powder is stirred by the electric mixer in container, make gold Magnesium, the bismuth element for belonging to powder surface adhesion sufficiently evaporate, and are vaporized through on the condenser in vacuum distillation furnace in magnesium, bismuth element When, the condensation of magnesium bismuth steam is carried out, is recycled after solidification;
(9) after the 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.
When 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, it can be complete The separating-purifying of pairs of various metals mixed-powder.
The magnesium bismuth alloy of condensation after being evaporated in vacuo every time in the step (8) can not be right for the sake of saving cost 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 powder density kind 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 being 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 99.99% or more argon gas as protective gas, Atmosphere furnace is warming up to suitable temperature again, is completely melt two kinds of pure metal auxiliary materials, and suitably stir, two kinds of pure 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, separate built-in electric heater on ware wall, can to material in separation ware into Row heating;The active clapboard of a transverse direction is equipped in separation ware, 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 pass through the on and off that a sliding block realizes leakage hole;It separates in ware Top pushes agitating plate equipped with first, lower part is equipped with second and pushes agitating plate, sliding for separating 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 separation ware is square hollow structure, and opened upper end is located on support plate, the underface of sealing cover.
It is stayed on the support plate there are four hole, two sides hole is used for the connection of upper and lower protective gas, and intermediate two holes are to let out Leak hole is let out under material for separating in ware.
The active clapboard includes partition, partition push rod two parts, partition with separate that ware inner space is wide, length is slightly larger In separation ware inner space length, partition top surface with separate that leakage hole bottom on ware is tangent, bottom surface and second pushes agitating plate top Face is tangent, and partition push rod one end and partition are connected, and the other end stretches out atmosphere furnace, partition with separate ware contact position, partition push rod Refractory seals are designed with atmosphere furnace joint.
Two leakage hole, sliding block all with to separate ware inner space wide, two leakage holes respectively pass through a material guide groove and branch Two leaks on board are respectively connected with logical, and two sliding blocks are provided with high temperature resistant with guide groove joint horizontal through corresponding guide groove 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 materials that circulate, and pushes agitating plate movement to reduce When the resistance from material.Scraper plate side is provided with the plush copper pushed open for that will correspond to sliding block, and plush copper is cylindrical, plush copper cylinder Face and scraper plate bottom surface are tangent, length with by corresponding sliding block from separate ware inner wall joint place push away to corresponding guide groove inner wall patch Being equidistant at conjunction, diameter are less than corresponding sliding block thickness.Scraper plate push rod one end is connected across separation ware top surface and scraper plate, another End reaches outside atmosphere furnace shell, length need to guarantee scraper plate can will corresponding sliding block from separate 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 for pushing agitating plate first and atmosphere furnace shell joint are equipped with refractory seals. First when pushing agitating plate installation, must guarantee 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, which 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 separate ware inner wall joint place elapse to Corresponding guide groove inner wall joint place is equidistant, and plush copper diameter is less than corresponding sliding block thickness, and scraper plate push rod one end, which passes through, to be divided Be connected from ware inner wall and scraper plate, the other end reaches outside atmosphere furnace shell, length need to guarantee scraper plate can will corresponding sliding block from point From ware inner wall joint place push away to corresponding guide groove inner wall joint place;Its scraper plate push rod with separate ware inner wall joint, scraper plate Push rod and atmosphere furnace shell joint are designed with refractory seals.Second push agitating plate installation when, must guarantee 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.
It is equipped with trolley inlet/outlet in the lower furnace chamber side, a ring packing is equipped between trolley inlet/outlet and lower furnace chamber Pad.
The top of the atmosphere furnace is equipped with bell, and an annular bell gasket, furnace are equipped between bell and atmosphere furnace Lid is fixed in atmosphere furnace by the wing bolt at both ends.
The powder hopper for being additionally provided with one above the bell and being connected in atmosphere furnace, powder hopper top are equipped with powder hopper lid;Furnace Lid middle part is provided with bell powder-exhausting hole, connects with powder hopper outlet and realizes that powder hopper is connected to atmosphere furnace;It is set on the blanking direction of powder hopper It is equipped with powder hopper switch, powder switch is preferably butterfly valve.
The bell top is additionally provided with for making powder hopper top and atmosphere furnace keep the snorkel of ventilation, upper part and powder hopper Connection, lower part is connect with bell venthole.
Described to be equipped with intake valve 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 sealing material that the refractory seals all include mounting base and are mounted in mounting base, sealing material are preferably Graphite packing.
A kind of application method of the atmosphere furnace for mixed metal powder separation method, the use process is as follows:
(1) bell is opened, two sliding blocks are pushed into make to separate ware two leakages up and down with the position for separating ware inner wall and fitting Mouth is in close state;Trolley inlet/outlet is opened, two-chamber charging carriage is placed in lower furnace chamber, its two chamber of left and right is located at Immediately below two leaks, trolley inlet/outlet is closed;The partition push rod of the scraper plate push rod and active clapboard that push agitating plate for two Be pulled outwardly, make two push agitating plate scrape plate face with separate ware inner wall fit, the partition of active clapboard with to push agitating plate convex Scraper plate face paste where head is closed;
(2) it by precalculated proportion chooses the pure magnesium metal auxiliary material of appropriate mass and pure bismuth metal auxiliary material is put into point From in ware, bell is closed;
(3) the powder switch in powder hopper is closed, powder hopper lid is opened, the mixed-powder being sieving through is added, then closes Close powder hopper lid;
(4) intake valve and air outlet valve are opened, quality of the purity up to 99.99% or more argon gas, to oxygen at air outlet valve is filled with After percentage composition is down to 0.05% or less, by separation ware in electric heating tube by atmosphere furnace be warming up to lower than in mixed-powder at The suitable temperature for dividing melting point, is completely melt two kinds of pure metal auxiliary materials.It is pushed two and loads onto thrust pin on agitating plate, then It pushes two to push agitating plate stirring liquid, two kinds of pure 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, it is continuous using agitating plate is pushed Stirring 10 minutes;
(6) mixture is stood into certain time, is layered mixed-powder in aluminium alloy by density;
(7) it is pushed home into active clapboard, separation ware is separated from intermediate fluid zone and is divided into two parts, material more than partition Metal powder is shown as in upper, liquid auxiliary materials under, separation ware internal partition material below shows as metal powder under, liquid Auxiliary material is upper;
(8) two are removed and pushes thrust pin on agitating plate, inwardly pushes two to push agitating plate to the separation ware other side, by two Sliding block is pushed open, to open two leakage mouths, subsequent two push stirring sheet reset, then active clapboard top material is through corresponding guide groove Under let 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 side of two-chamber charging carriage Chamber;
(9) agitating plate is pushed by two inwardly to push, the material for separating ware inner wall remnants is pushed at two leakage holes, is made point It is collected on two-chamber charging carriage as much as possible from material in ware;
(10) close separation ware on electric heating tube, when atmosphere furnace is cooled to room temperature, open atmosphere furnace on trolley into It gos out, catches on the pull ring on trolley with hook, two-chamber charging carriage is pulled out into atmosphere furnace, for removing demagging bismuth in next step.
The positive effect of the present invention is 1, molten by combining powder pretreatment, screening, the magnesium bismuth alloy of configuration different densities The means such as liquid reduce the mixed metal powder after the 3D printing of principle separating-purifying, 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 greater than 700 DEG C, separation purity are high;2, 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;3, it mentions 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;4, not high because being related to temperature for the atmosphere furnace clever structure of mixed metal powder separation method, it is easy to construct, and It is few by being polluted between separated powder.
Detailed description of the invention
Fig. 1 is the atmosphere furnace structural schematic diagram for mixed metal powder separation method.
Fig. 2 is the first structural schematic diagram for pushing agitating plate.
Fig. 3 is active clapboard structural schematic diagram.
In Fig. 1: 1- two-chamber charging carriage, 2- intake valve, 3- atmosphere furnace shell, furnace chamber under 4-, 5- support plate, 501- first are logical Stomata, the first leak of 502-, the second venthole of 503-, the upper furnace chamber of 6-, the first refractory seals of 7-, the first sliding block of 8-, 9- electricity Heating tube, 10- separate ware, 11- bell gasket, 12- bell, 1201- bell venthole, the first powder of 13-, 14- ventilation Pipe, 15- powder hopper, 16- powder hopper lid, 17- mixed-powder, 18- air outlet valve, 19- powder hopper switch, 20- magnesium bismuth alloy liquid, 1202- furnace 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 clapboard, 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- trolley pass in and out door sealing, second of powder of 31-, 101- stirring motor, 102- trolley pull ring, the 103- trolley right side Chamber, the second leak of 504-, the second guide groove of 32-, the 7th refractory seals of 33-, the second sliding block of 34-, the first guide groove of 35-, 104- Trolley left chamber, 105- agitating auger;
In Fig. 2: 2101- scraper plate, 2102- plush copper, 2103- deflector hole, 2104- scraper plate push rod, 2105- thrust pin;
In Fig. 3: 2501- partition, 2502- partition push rod.
Specific embodiment
The present invention is further described with reference to the accompanying drawings and embodiments.
A kind of mixed metal powder separation method a comprising preprocessing process: before 3D printing, selecting spherical shape, And particle size distribution range is identical, maximum particle diameter less than 2 times of minimum grain sizes two or more metal powders as more material metals zero Part 3D printing material.
To the mixed-powder after pretreated 3D printing, steps are as follows for separating-purifying:
(1) screening plant is used, preferably magnetic suspension vibrating sieves, and in conjunction with the standard screen of suitable mesh number, removes mixed-powder Middle size is greater than the powder particle of 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, determine institute required to mixed metal powder Isolated liquid medium density, liquid medium density should be between two kinds of powder densities to be separated.
(3) pure magnesium needed for the aluminium alloy of liquid medium density d is formed by the calculating of formula d=a%*1.74+ (1-a%) * 9.8 The mass percent (1-a%) of mass percent a% and pure bismuth, and choose purity respectively by mass percent calculated and be 99.99% or more 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 pure metal auxiliary materials are added in atmosphere furnaces, are filled with 99.99% or more argon gas as protective gas, then general Atmosphere furnace is warming up to the suitable temperature lower than component powders fusing point in mixed-powder, is completely melt two kinds of pure metal auxiliary materials, and Appropriate stirring, makes two kinds of pure 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 is layered mixed-powder in aluminium alloy by density.
(6) aluminium alloy top powder will be floated on and is sunken to the powder of aluminium alloy lower part under the protective atmosphere protection of atmosphere furnace It is fetched into different containers respectively, container has electric mixer.
(7) then container is taken out, is placed in vacuum distillation furnace after atmosphere furnace is cooled to room temperature.
(8) control vacuum distillation furnace has suitable pressure, makes the pressure 0.001-1Pa of vacuum distillation furnace, then will Temperature is heated to suitable temperature, which is higher than the boiling point of pure metal auxiliary material used under the pressure, but is lower 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, the magnesium for adhering to metal powder surface, bismuth element are sufficiently evaporated, be 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 the 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.
When 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, it can be complete The separating-purifying of pairs of various metals mixed-powder.
The magnesium bismuth alloy of condensation after being evaporated in vacuo every time in the step (8) can not be right for the sake of saving cost 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 powder density kind 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 being 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 99.99% or more argon gas as protective gas, Atmosphere furnace is warming up to suitable temperature again, is completely melt two kinds of pure metal auxiliary materials, and suitably stir, two kinds of pure metal is made to exist The magnesium bismuth alloy liquid of infinitely dissolve is formed in atmosphere furnace.
Referring to figures 1-3, 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, separates interior setting electric heating on 10 wall of ware Pipe 9 can heat material in separation ware 10;Separation ware 10 in be equipped with a transverse direction active clapboard 25, activity every Plate 25, which can be moved left and right, is separated into disconnected two parts up and down for 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 is equipped with second and pushes agitating plate 24, stirs for separating 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 and lower part material being separated into separation ware 10 by active clapboard 25.
The separation ware 10 is square hollow structure, and opened upper end is located 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 two holes are 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 include partition 2501,2502 two parts of partition push rod, partition 2501 with separate inside ware 10 Space is wide, length is slightly larger than separation 10 inner space length of ware, 2501 top surface of partition with separate 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 push rod and partition 2501 are connected, and the other end stretches out gas Outside atmosphere furnace shell 3, the second refractory seals 22, partition push rod 2502 and atmosphere furnace are equipped with 10 contact position of ware is separated in partition 2501 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 separate 10 inner space of ware wide, upper leakage hole is logical It crosses the first guide groove 35 to be connected with the first leak 502 on support plate 5, 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 composition.Scraper plate 2101 with to separate 10 inner space of ware wide, the upper end is provided with multiple for the material that circulates Deflector hole 2103, with reduce push agitating plate it is mobile when the resistance from material.2101 side of scraper plate is provided with for that will slide The plush copper 2102 that block is pushed open, plush copper 2102 is cylindrical, and 2102 cylindrical surface of plush copper and 2101 bottom surface of scraper plate are tangent, length and general For first sliding block 8 from being equidistant with separating ware 10 inner wall joint place and push away to 35 inner wall joint place of the first guide groove, 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 the other side reaches gas Outside atmosphere furnace shell 3, length need to guarantee scraper plate 2101 can by the first sliding block 8 from separate 10 inner wall joint place of ware and push away to first 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 when material in ware 10, for pushing open when the first sliding block 8 opens upper leakage hole or being removed when pushing salvage stores.First When pushing the installation of agitating plate 21, it must guarantee 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 push agitating plate 24 shape, constitute that push agitating plate 21 with first identical, only size and installation position Set difference, plush copper length with by the second sliding block 34 from pasting with separating 10 inner wall joint place of ware and push away to 32 inner wall of the second guide groove Being equidistant at conjunction, 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 and scraper plate is solid Even, the other side reaches outside atmosphere furnace shell 3, length need to guarantee second push agitating plate 24 can by the second sliding block 34 from separate 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 10 inner wall joint of ware is separated 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 for loading onto when being sirred and separated material in ware 10 second, is leaked for pushing open under the second sliding block 34 is opened It removes when mouth or when pushing salvage stores.Second push agitating plate 24 install when, must guarantee scraper plate bottom surface with separate inside ware 10 Bottom surface fits, and the salvage stores separated 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 is equipped with trolley inlet/outlet 29, and an annular is equipped between trolley inlet/outlet 29 and lower furnace chamber 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 screw.
The two-chamber charging carriage 1 is equipped with trolley pull ring 102, for taking out two-chamber charging carriage 1 from atmosphere furnace; It is additionally provided with stirring motor 101 and agitating auger 105, is used to stir material in two-chamber charging carriage when subsequent vacuum distillation.
The top of the atmosphere furnace is equipped with bell 12, and an annular bell gasket is equipped between bell 12 and atmosphere furnace 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 be additionally provided with one above with the powder hopper 15 that is connected in atmosphere furnace, equipped with powder hopper at the top of powder hopper 15 Lid 16, powder hopper lid 16 can be used screw and be fixed in powder hopper 15;Bell powder-exhausting hole 1202 is provided in the middle part of bell 12, with powder hopper 15 Outlet, which connects, realizes that powder hopper 15 is connected to 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 for making 15 top of powder hopper and atmosphere furnace keep the snorkel 14 of ventilation, upper part It is connected to powder hopper 15, lower part is connect with bell venthole 1201, realizes that powder hopper top and atmosphere furnace keep logical at any time Gas.
It is described to be equipped with intake valve 2 in atmosphere furnace lower part, air outlet valve 18 is housed above powder hopper lid 16, for passing in and out protection gas Body.
First refractory seals 7, the second refractory seals 22, third refractory seals 23, the 4th refractory seals 26, the 5th refractory seals 27, the 6th refractory seals 28, the 7th refractory seals 33 all include mounting base and are mounted on peace The sealing material in seat is filled, sealing material is preferably graphite packing.
A kind of application method of the atmosphere furnace for mixed metal powder separation method, the use process is as follows:
(1) open bell 12, by the first sliding block 8 and the second sliding block 34 be pushed into the position that separates 10 inner wall of ware and fit, It is in close state separation about 10 two leakage holes of ware;Trolley inlet/outlet 29 is opened, two-chamber charging carriage 1 is placed in lower furnace It in room 4, is located at its two chamber of left and right immediately below two leaks of support plate 5, closes trolley inlet/outlet 29;Two are pushed Scraper plate push rod, the active clapboard push rod 2502 of agitating plate are pulled outwardly, make to push agitating plate scrape plate face with separate 10 inner wall phase of ware Fitting, partition 2501 and the scraper plate face paste where pushing agitating plate plush copper are closed;
(2) auxiliary by the pure magnesium metal auxiliary material of precalculated proportion selection appropriate mass and the pure bismuth metal of appropriate mass Material is put 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, described be sieving through is added Mixed-powder 17, be then shut off powder hopper lid 16.
(4) intake valve 2 and air outlet valve 18 are opened, is filled with purity up to 99.99% or more argon gas, to oxygen at air outlet valve 18 Mass percentage be down to 0.05% or less after, by separation ware 10 in electric heating tube 9 atmosphere furnace is warming up to suitable temperature Degree, is completely melt two kinds of pure metal auxiliary materials.Agitating plate 21 is pushed first and second is pushed and is loaded onto thrust pin on agitating plate 24, Then it pushes two to push agitating plate stirring liquid, two kinds of pure 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, is layered mixed-powder in aluminium alloy by density.
(7) it is pushed home into active clapboard 25, separation ware 10 is separated from intermediate fluid zone and is divided into two parts, is separated in ware 10 The material of 25 or more active clapboard shows as metal powder in upper, liquid auxiliary materials under, separates 25 or less active clapboard in 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 other side for separating ware 10, makes first to push agitating plate 21 and second push agitating plate 24 and the other side that separates ware 10 Inner wall fits, and respectively pushes the first sliding block 8 and the second sliding block 34 open, to open two leakage mouths, subsequent two push agitating plate It resets, then separates in ware 10 25 top material of active clapboard through letting out under corresponding first guide groove 35 to a left side for two-chamber charging carriage 1 Chamber 104, separate ware 10 in 25 lower part material of active clapboard through letting 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 separate 10 inner wall of ware, bottom, And the material of 25 upper and lower surfaces of active clapboard remnants is pushed at two leakage holes, make share ware 10 in material as much as possible It is collected on two-chamber charging carriage 1.
(10) 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 catches on the trolley pull ring 102 on two-chamber charging carriage 1 with hook, and two-chamber charging carriage 1 is pulled out atmosphere Furnace removes demagging bismuth for subsequent.
The positive effect of the present invention is 1, molten by combining powder pretreatment, screening, the magnesium bismuth alloy of configuration different densities The means such as liquid reduce the mixed metal powder after the 3D printing of principle separating-purifying, 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 greater than 700 DEG C, separation purity are high;2, 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;3, it mentions 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;4, not high because being related to temperature for the atmosphere furnace clever structure of mixed metal powder separation method, it is easy to construct, and It is few by being polluted between separated powder.
Embodiment one:
It is 28-53 microns of spherical 316L stainless steel powder (density: 7.98 grams/cube that particle size range is selected before 3D printing Centimetre) and particle size range be 28-53 microns two kinds of metals of spherical Ti6Al4V Titanium Powder (density: 4.4 grams/cc) As 3D printing material, the remaining mixed-powder process for separation and purification after completing 3D printing is powder:
(1) selecting mesh number is 270 the polished standard screens (corresponding mesh size is 50 microns), is fixed on magnetic suspension vibrating sieve On, and pour into remaining mixed-powder and sieved, then it is a small number of during 3D printing to be sintered pair that be pockets of, being difficult to separating-purifying Metal component metallic particles group, the size overwhelming majority are greater than 56 microns, and the diameter of spheroidized particle is also most greater than original Several times of powder particle, therefore, these substances overwhelming majority will be left in standard screen, then are to be separated by the powder of standard screen The mixed-powder 17 of purification.
(2) bell 12 is opened, the first sliding block 8 and the second sliding block 34 are pushed into and separate 10 inner wall joint place of ware, makes to separate About 10 two leakage holes of ware are in close state;Trolley inlet/outlet 29 is opened, two-chamber charging carriage 1 is placed in lower furnace chamber 4, It is located at its two chamber of left and right immediately below two leaks of support plate 5, closes 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 with separate 10 inner wall of ware fit, every Plate 2501 is closed with the scraper plate face paste where pushing agitating plate plush copper.
(3) pure magnesium, pure bismuth metal auxiliary material 4:6 in mass ratio are equipped with, the magnesium of outfit, bismuth mixed metal auxiliary material is put into gas In separation ware 10 in atmosphere furnace.
(4) the powder hopper switch 19 in powder hopper 15 is closed, the powder hopper lid 16 in powder hopper 15 is opened, the mixed powder that need to be separated is added 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, it is filled with mass percentage drop of the purity up to 99.99% or more argon gas, to 18 exit oxygen at air outlet valve To after 0.05% or less, 700 DEG C are warming up to by ware 10 is separated by the heating tube 9 in separation ware 10, keeps two kinds of pure metal auxiliary materials complete Running down.First push agitating plate 21 and second push agitating plate 24 push rod end load onto thrust pin, then push two push away Agitating plate stirring liquid is scraped, two kinds of pure 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 push agitating plate 21 and second push the reset of agitating plate 24, and mixture is stood 20 minutes or more, makes to mix Powder is closed to be layered in aluminium alloy by density.
(8) it is pushed home into active clapboard 25, separation ware 10 is separated from intermediate fluid zone and is divided into two parts, is separated in ware 10 The material of 25 or more active clapboard shows as metal powder in upper, liquid auxiliary materials under, separates 25 or less active clapboard in 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 other side for separating ware 10, makes first to push agitating plate 21 and second push agitating plate 24 and the other side that separates ware 10 Inner wall fits, and respectively pushes the first sliding block 8 and the second sliding block 34 open, to open two leakage mouths, subsequent two push agitating plate It resets, then separates in ware 10 25 top material of active clapboard through letting out under corresponding first guide groove 35 to a left side for two-chamber charging carriage 1 Chamber 104, separate ware 10 in 25 lower part material of active clapboard through letting out under corresponding second guide groove 32 to the right chamber of two-chamber charging carriage 1 103。
(10) 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 catches on the trolley pull ring 102 on two-chamber charging carriage 1 with hook, and two-chamber charging carriage 1 is pulled out atmosphere furnace, Demagging bismuth is removed for subsequent.
(11) two-chamber charging carriage 1 is put into vacuum distillation furnace.Controlling vacuum distillation furnace has suitable pressure, generally Ground can make the pressure 0.001-1Pa of vacuum distillation furnace.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 powder, generally view vacuum Retort pressure value value within the scope of 500-690 DEG C.And keep the temperature arrive the suitable time, make metal powder surface adhere to magnesium, Bismuth element sufficiently evaporates, while starting the stirring motor 101 on double-chamber unit trolley 2, so that agitating auger 105 is stirred material, adds Liquid evaporation on fast metal powder granulates.When magnesium, bismuth element are vaporized through on the condenser in vacuum distillation furnace, magnesium is carried out The condensation of bismuth steam, recycles after solidification.
(12) after the 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 Powder after separating-purifying, right Metal powder in chamber 103 is the 316L stainless steel powder after separating-purifying.
Embodiment two:
Ti6AlV4 Titanium Powder (density: 4.4 grams/cc), Inconel718 high temperature nickel is selected to close before 3D printing Three kinds of bronze (density: 8.24 grams/cc), fine silver powder (density: 10.5 grams/cc) metal powders are as forming material Material, the particle size range of three kinds of powder is all 38-75 microns, and pattern is all spherical.Remaining mixed-powder after then completing 3D printing Process for separation and purification is:
(1) selecting mesh number is 200 the polished standard screens (corresponding mesh size is 75 microns), is fixed on magnetic suspension vibrating sieve On, and pour into remaining mixed-powder and sieved.Because 3D printing process minority is sintered double gold that are pockets of, being difficult to separating-purifying Belong to multicomponent metallic cluster of grains, the size overwhelming majority is greater than 76 microns, and the diameter of spheroidized particle is also most to be greater than original powder Several times of last particle, therefore, these substances overwhelming majority will be left in standard screen, then are to be separated mention by the powder of standard screen Pure mixed-powder 17.
(2) bell 12 is opened, the first sliding block 8 and the second sliding block 34 are pushed into and separate 10 inner wall joint place of ware, makes to separate About 10 two leakage holes of ware are in close state;Trolley inlet/outlet 29 is opened, two-chamber charging carriage 1 is placed in lower furnace chamber 4, It is located at its two chamber of left and right immediately below two leaks of support plate 5, closes 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 with separate 10 inner wall of ware fit, 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, the mixed powder that need to be separated is added 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, it is filled with mass percentage drop of the purity up to 99.99% or more argon gas, to 18 exit oxygen at air outlet valve To after 0.05% or less, 350 DEG C are warming up to by ware 10 is separated by the heating tube 9 in separation ware 10, keeps 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 push agitating plate 21 and second push the reset of agitating plate 24, and mixture is stood 20 minutes or more, makes to mix Powder is closed to be layered in aluminium alloy by density.
(8) it is pushed home into active clapboard 25, separation ware 10 is separated from intermediate fluid zone and is divided into two parts, is separated in ware 10 The material of 25 or more active clapboard shows as Ti6AlV4 titanium alloy+Inconel718 high temperature nickel alloy mixed-powder in upper, liquid Auxiliary material separates the material below of active clapboard 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 other side for separating ware 10, makes first to push agitating plate 21 and second push agitating plate 24 and the other side that separates ware 10 Inner wall fits, and respectively pushes the first sliding block 8 and the second sliding block 34 open, to open two leakage mouths, subsequent two push agitating plate It resets, then separates in ware 10 25 top material of active clapboard through letting out under corresponding first guide groove 35 to a left side for two-chamber charging carriage 1 Chamber 104, separate ware 10 in 25 lower part material of active clapboard through letting out under corresponding second guide groove 32 to the right chamber of two-chamber charging carriage 1 103。
(10) 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 catches on the trolley pull ring 102 on two-chamber charging carriage 1 with hook, and two-chamber charging carriage 1 is pulled out atmosphere furnace, Demagging bismuth is removed for subsequent.
(11) two-chamber charging carriage 1 is put into vacuum distillation furnace.Controlling vacuum distillation furnace has suitable pressure, generally Ground can make the pressure 0.001-1Pa of vacuum distillation furnace.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 lower than mixed metal powder, the general vacuum distillation furnace pressure value that regards exist Value within the scope of 500-690 DEG C.And keep the temperature and arrive the suitable time, the bismuth element for adhering to metal powder surface sufficiently evaporates, together Stirring motor 101 on Shi Qidong double-chamber unit trolley 2 makes agitating auger 105 stir material, accelerates on metal powder granulates Liquid evaporation.When bismuth element is vaporized through on the condenser in vacuum distillation furnace, the condensation of bismuth steam is carried out, benefit is recycled after solidification With.
(12) after the 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 be separating-purifying after Ti6AlV4 titanium alloy+ Inconel718 high temperature nickel alloy mixed-powder, 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 powder still needs 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, cleaned the liquid or particle of its surface adhesion, then use one technology of embodiment, can separating-purifying, respectively obtain titanium Alloyed powder Ti6AlV4 and Inconel718 alloy powder.To complete the separating-purifying of the metal powder mixed to three kinds of ingredients.
It is different from other mixed metal process for separation and purification, by combining powder pretreatment, screening, configure different densities The means such as magnesium bismuth alloy solution reduce the mixed metal powder after the 3D printing of principle separating-purifying based on law of buoyancy and decompression boiling point The separating-purifying of mixed metal powder of most of fusing point greater than 700 DEG C may be implemented in end, has 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 construct, 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, it is other it is any without departing from the spirit and principles of the present invention made by change, modification, substitution, combination, letter Change, should be equivalent substitute mode, be included within the 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 less than 2 times of minimum grain sizes two or more metal powders as metal gradient material Part 3D printing material;
To the mixed-powder after pretreated 3D printing, steps are as follows for separating-purifying:
(1) powder particle of the size greater than 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, determine institute required to mixed metal powder separation Liquid medium density, liquid medium density should be between two kinds of powder densities to be separated;
(3) pure magnesia amount needed for the aluminium alloy of liquid medium density d is formed by the calculating of formula d=a%*1.74+ (1-a%) * 9.8 The mass percent (1-a%) of percentage a% and pure bismuth, and by mass percent calculated choose respectively purity be 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 pure metal auxiliary materials are added in atmosphere furnaces, are filled with 99.99% or more argon gas as protective gas, then by atmosphere Furnace is warming up to the suitable temperature lower than component powders fusing point in mixed-powder, is completely melt two kinds of pure metal auxiliary materials, and appropriate Stirring, makes two kinds of pure 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, it is layered mixed-powder in aluminium alloy by density;
(6) aluminium alloy top powder will be floated on and is sunken to the powder of aluminium alloy lower part and takes out be placed in different vessels respectively, held Electric mixer is had in device;
(7) after temperature is down to room temperature or less in atmosphere furnace, container is taken out, is placed in vacuum distillation furnace;
(8) control vacuum distillation furnace has suitable pressure, makes the pressure 0.001-1Pa of vacuum distillation furnace, then by temperature It is heated to suitable temperature, which is higher than the boiling point of pure metal auxiliary material used under the pressure, but lower 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 sufficiently evaporate, when magnesium, bismuth element are vaporized through on the condenser in vacuum distillation furnace, into The condensation of row magnesium bismuth steam, recycles after solidification;
(9) after the 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, can be completed the separating-purifying to various metals mixed-powder.
3. mixed metal powder separation method as described in claim 1, it is characterised in that: each vacuum in the step (8) The magnesium bismuth alloy of condensation after distillation can not carry out separating-purifying to magnesium bismuth alloy for the sake of saving cost, but in next time It is reused directly for similarly meeting the mixed of 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 be saved step (3), and step (4) is changed to: by the density of recycling between two kinds wait divide 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 99.99% or more is warming up to suitable temperature as protective gas, then by atmosphere furnace, makes two kinds Pure metal auxiliary material is completely melt, and is suitably stirred, and two kinds of pure 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, separate in-built electrical on ware wall and add Heat pipe can heat material in separation ware;The active clapboard of a transverse direction is equipped in separation ware, 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 respectively pass through a sliding block and realize The on and off of leakage hole;Two leakage hole, sliding block all with to separate ware inner space wide, two leakage holes respectively pass through a guide groove with Two leaks on support plate are respectively connected with logical, and two sliding blocks are provided with resistance to height with guide groove joint horizontal through corresponding guide groove Temperature sealing;Separation ware internal upper part pushes agitating plate equipped with first, lower part is equipped with second and pushes agitating plate, for separating 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;It is equipped with trolley inlet/outlet in lower furnace chamber side, between trolley inlet/outlet and lower furnace chamber Equipped with a Gask-O-Seal.
5. being used for the atmosphere furnace of mixed metal powder separation method as claimed in claim 4, it is characterised in that: the separation ware is Square hollow structure, opened upper end are located on support plate, the underface of sealing cover;Hole there are four being stayed on support plate, two sides Hole is used for the connection of upper and lower protective gas, and intermediate two holes are leak, lets out under material for separating in ware.
6. being 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, partition push rod two parts, partition with separate that ware inner space is wide, length is long slightly larger than ware inner space is separated Degree, partition top surface with separate that leakage hole bottom on ware is tangent, bottom surface pushes with second tangent, partition push rod one end of stirring plate top surface It is connected with partition, the other end stretches out atmosphere furnace, is designed in partition with ware contact position, partition push rod and atmosphere furnace joint is separated Refractory seals.
7. being used for the atmosphere furnace of mixed metal powder separation method as described in claim 4 or 6, it is characterised in that: high temperature resistant is close The sealing material that package includes mounting base and is mounted in mounting base, sealing material are graphite packing.
8. being 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 with to separate ware inner space wide, 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 the plush copper pushed open for that will correspond to sliding block, and plush copper is cylindrical, and plush copper cylindrical surface and scraper plate bottom surface are tangent, Length with by corresponding sliding block from being equidistant with separating ware inner wall joint place and push away to corresponding guide groove inner wall joint place, diameter Less than corresponding sliding block thickness, scraper plate push rod one end is connected across separation ware top surface and scraper plate, and the other end reaches outside atmosphere furnace shell, Its length need to guarantee scraper plate can will corresponding sliding block from separate 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 for pushing agitating plate first and atmosphere furnace shell joint are equipped with refractory seals;First pushes agitating plate installation When, it must guarantee 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 push agitating plate shape, constitute that push agitating plate with first identical, only size and installation position Set difference, plush copper length with by corresponding sliding block from separate ware inner wall joint place elapse to corresponding guide groove inner wall joint place It is equidistant, plush copper diameter is less than corresponding sliding block thickness, and scraper plate push rod one end passes through separation ware inner wall and scraper plate is connected, separately One end reaches outside atmosphere furnace shell, length need to guarantee scraper plate can will corresponding sliding block from separate ware inner wall joint place push away to Corresponding guide groove inner wall joint place;Its scraper plate push rod with separate 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 guarantee scraper plate bottom surface fit with ware inner bottom surface is separated so that Second, which pushes agitating plate, can effectively remove the salvage stores separated in ware inner bottom surface.
9. being 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, and an annular bell gasket, the wing bolt that bell passes through both ends are equipped between bell and atmosphere furnace It is fixed in atmosphere furnace;The powder hopper for being additionally provided with one above bell and being connected in atmosphere furnace, powder hopper top are equipped with powder hopper lid;Furnace Lid middle part is provided with bell powder-exhausting hole, connects with powder hopper outlet and realizes that powder hopper is connected to atmosphere furnace;It is set on the blanking direction of powder hopper It is equipped with powder hopper switch, powder switch is butterfly valve;The bell top is additionally provided with for making powder hopper top and atmosphere furnace keep ventilating Snorkel, upper part is connected to powder hopper, and lower part is connect with bell venthole;The atmosphere furnace lower part is equipped with intake valve, powder hopper The side of covering is equipped with air outlet valve, for passing in and out protective gas.
10. a kind of application method for the atmosphere furnace of mixed metal powder separation method, feature as claimed in claim 4 exist In use process is as follows:
(1) open bell, by two sliding blocks be pushed into the position that separates ware inner wall and fit, make to separate ware up and down 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 Immediately below leak, trolley inlet/outlet is closed;The partition push rod of the scraper plate push rod and active clapboard that push agitating plate for two is outside Draw, make two push agitating plate scrape plate face with separate ware inner wall fit, the partition 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 proportion and pure bismuth metal auxiliary material puts into separation ware In, close bell;
(3) the powder switch in powder hopper is closed, powder hopper lid is opened, the mixed-powder being sieving through is added, is then shut off powder Bucket cover;
(4) intake valve and air outlet valve are opened, quality percentage of the purity up to 99.99% or more argon gas, to oxygen at air outlet valve is filled with After content is down to 0.05% or less, atmosphere furnace is warming up to lower than ingredient powder in mixed-powder by the electric heating tube in separation ware The suitable temperature of last fusing point is completely melt two kinds of pure metal auxiliary materials;It is pushed two and loads onto thrust pin on agitating plate, then pushed Two push agitating plate stirring liquid, and two kinds of pure 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, is layered mixed-powder in aluminium alloy by density;
(7) it is pushed home into active clapboard, separation ware is separated from intermediate fluid zone and is divided into two parts, material performance more than partition For metal powder in upper, liquid auxiliary materials under, separation ware internal partition material below show as metal powder under, liquid auxiliary materials Upper;
(8) two are removed and pushes thrust pin on agitating plate, inwardly pushes two to push agitating plate to the separation ware other side, by two sliding blocks It pushes open, 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, the material for separating ware inner wall remnants is pushed at two leakage holes, make to separate ware Interior material is collected into as much as possible on two-chamber charging carriage;
(10) electric heating tube on separation ware is closed, when atmosphere furnace is cooled to room temperature, opens the trolley disengaging in atmosphere furnace Door, catches on the pull ring on trolley with hook, two-chamber charging carriage is pulled out atmosphere furnace, for removing demagging bismuth in next step.
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