CN106216705B - A kind of preparation method of 3D printing fine grained simple substance globular metallic powder - Google Patents

A kind of preparation method of 3D printing fine grained simple substance globular metallic powder Download PDF

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CN106216705B
CN106216705B CN201610832136.8A CN201610832136A CN106216705B CN 106216705 B CN106216705 B CN 106216705B CN 201610832136 A CN201610832136 A CN 201610832136A CN 106216705 B CN106216705 B CN 106216705B
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powder
metal
hydrogen
elemental metals
particle
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CN106216705A (en
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聂祚仁
张亚娟
宋晓艳
王海滨
刘雪梅
贺定勇
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Beijing University of Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/12—Making metallic powder or suspensions thereof using physical processes starting from gaseous material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06—Metallic powder characterised by the shape of the particles
    • B22F1/065—Spherical particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14—Treatment of metallic powder
    • B22F1/142—Thermal or thermo-mechanical treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14—Treatment of metallic powder
    • B22F1/148—Agglomerating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/026—Spray drying of solutions or suspensions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy

Abstract

A kind of preparation method the present invention relates to 3D printing with fine grained simple substance globular metallic powder, belongs to metal dust preparing technical field.The preparation method uses high pure metal bulk as raw material, in an inert atmosphere by arc evaporation, while is filled with hydrogen and controls the heat transfer of metal gas atom and activity to be allowed to cool deposition and obtain high purity elemental nano metal powder particle；Then agglomeration granulation is carried out to high purity elemental nano metal powder, obtains the micron order elemental metals powder of higher density；Finally micron order elemental metals powder after granulation is heat-treated, by degumming and densification consolidation, obtains the elemental metals powder particle that granularity, sphericity, mobility and oxygen content meet 3D printing requirement.This method is strong to the controllability of the sphericity of metallic particles, particle diameter distribution and oxygen content compared with other processes, and with the advantage that technique is simple and cost is low.

Description

A kind of preparation method of 3D printing fine grained simple substance globular metallic powder
Technical field
A kind of preparation method the present invention relates to 3D printing with fine grained simple substance globular metallic powder, belongs to metal dust system Standby technical field.
Background technology
It is all that 3D printing technique combines digital modeling techniques, Electromechanical Control technology, information technology, material science and chemistry etc. Multi-field cutting edge technology, applied to the field such as product prototype, mold manufacturing, bioengineering and medicine, jewelry-making, can replace Lift for conventional fine processing technology and largely the efficiency and measure of precision of making.However, 3D printing technical process The requirement of higher is proposed to metal powder material, such as requires particle size range to contain at 20-50 microns, with high sphericity and hypoxemia Amount etc..At present, domestic required fine grain globular metallic powder relies on import substantially, and due to the preparation process of powder, there are raw material It is the low bottleneck problem of utilization rate, expensive, this largely constrain the popularization of China's metal 3D printing technique with should With.
Existing metal dust technology of preparing mainly has：Mechanical attrition method, atomization, plasma rotating electrode process, physics Chemical method etc..Wherein, gas atomization is one of main method for preparing superfine metal and alloy powder, but one of its maximum Problem is exactly low yield, and the yield rate that the metal or alloy powder size prepared reaches less than 50 μm only has 30% or so；Ball Mill method is only used for fragile material, and usual oxygen content is higher and is unable to control powder particle pattern；Plasma rotating electrode process system Standby powder diameter is larger, is typically larger than 50 μm；Electrochemistry, reduction method cost are higher, and the solvent and reducing agent used has more Severe toxicity, and it is readily incorporated the impurity such as halogen, sulphur.CN201010219344.3 discloses a kind of ultra-fine and nano WC-Co composite powder Agglomerating prilling method, after carrying out agglomeration granulation to ultra-fine and nano WC-Co composite powder using this method, agglomerated particle can be direct For hot-spraying technique, ultra-fine and nanostructured the hard alloy coating with excellent comprehensive performance can be prepared, but for The requirement of 3D printing metal or alloy powder also has certain gap, needs on its basis further research.Therefore, it is urgent at present Demand low cost, high-purity, size tunable 3D printing metal or alloy powder preparation method.
The content of the invention
Above-mentioned limitation based on the prior art, the present invention provide a kind of 3D printing fine grained simple substance globular metallic powder Preparation method.For solving, 3D printing metal or alloy powder purity is low, particle diameter is uncontrollable and raw material availability is low, price The problems such as expensive.
Technical scheme is as follows：
The preparation method of a kind of 3D printing fine grained simple substance globular metallic powder, it is characterised in that the preparation method is adopted It is raw material with high pure metal bulk, in an inert atmosphere by arc evaporation, while it is former to be filled with hydrogen control metal gas The heat transfer and activity of son are allowed to cool deposition and obtain high purity elemental nano metal powder particle；Then high purity elemental metal is received Rice flour end carries out agglomeration granulation, obtains the micron order elemental metals powder of higher density；Finally to micron order elemental gold after granulation Belong to powder to be heat-treated, by degumming and densification consolidation, obtain granularity, sphericity, mobility and oxygen content and meet The elemental metals powder particle of 3D printing requirement, it specifically includes following steps：
(1) using high pure metal bulk as anode, tungsten is cathode, under inert gas and hydrogen environment, is made by discharging With high intensity electric arc evaporated metal generation gas atom is formed, the solid-state elemental metals that particle diameter is 20~80nm are formed after condensation and are received The component of rice grain, wherein metal block material is selected from Fe, Co, Ni or Zn, and inert gas and being passed through for hydrogen are sequentially：First take out true Sky, then passes to the argon gas progress starting the arc and starts to evaporate, be then passed through hydrogen again and carry out continuous evaporation；
(2) the elemental metals nano particle for preparing polyvinyl alcohol, polyethylene glycol and deionized water and step (1) is by certain Ratio, is combined preparation by ball milling and mechanical agitation and obtains stable suspension slurry, then done using closed cycle spray Dry equipment carries out agglomeration granulation, obtains 20~50 μm of spherical metallic particles, wherein dried medium is argon gas；Ball milling and machinery stir Mix and be combined, first carry out ball milling, then carry out mechanical agitation again；
(3) spherical metallic particles prepared using the tube furnace of argon gas protection to step (2) are heat-treated, the first stage Heat treatment temperature is 250~350 DEG C, 90~150min of soaking time；Second stage heat treatment temperature is Tm/ 2+80~Tm/2+ 180 DEG C, TmFor elemental metals fusing point, soaking time is 120~180min；Finally cool to room temperature with the furnace, obtain being suitable for 3D The fine grained simple substance globular metallic powder of printing demand；
Wherein, the pressure ratio that hydrogen and argon gas are filled with step (1) is 1：1~3, it is passed through argon gas to vacuum pressure and reaches 0.04~0.06MPa carries out the starting the arc, then passes to hydrogen to vacuum pressure and reaches 0.01~0.03MPa progress continuous evaporations；
The slurry ball-milling time is 40~80min in step (2), and rotating speed is 300~400r/min, and the mechanical agitation time is 20 ~40min, stir speed (S.S.) are 100~200r/min, ensure total time in 60~120min.
The technical characteristic and advantage of the present invention mainly has：(1) during the metal starting the arc is evaporated, hydrogen is filled with, in height The lower hydrogen of temperature can improve yield and control the activity of metal gas atom as heat-conducting medium, the mutually pure elemental gold of product Belong to nano-particle；(2) aaerosol solution slurry is prepared by original material of the mutually pure nano metal powder of thing.In the present invention, surely The preparation for determining distributed slurry has vital effect to the pattern and particle diameter distribution of prilling powder, is stirred using ball milling and machinery The mode being combined is mixed, the effect of first stage ball milling is to smash nanoparticle agglomerates body, organic binder bond and dispersant is existed The absorption of particle surface reaches balance, and using the relatively low mechanical agitation of energy, effect is discharged to be mingled with second stage in slurry Bubble simultaneously makes the macromolecular chain of organic additive connect to form uniform and stable tridimensional network；(3) spray drying is passed through Method is granulated prepared stable suspersion solution slurry, can obtain with good sphericity, low oxygen content and compared with The micron particles of high-compactness.In the present invention, drying tower is closed, and dried medium is inert gas, can effectively be controlled most Oxygen content in the metal powder granulates prepared eventually.(4) heat treatment process after being granulated, meets 3D printing requirement to final acquisition Metal dust it is extremely important.In the present invention, using stage heat treatment mode, the first stage effect of heat treatment is to make granulation During add organic binder bond volatilization；The effect of second stage heat treatment is that formation solid phase is glued between making metal powder granulates Knot, not only ensures with enough an interparticle bond strength and consistency, but also particle (or internal microstructure) does not occur and is quickly roughened It is or integral sintered.Parameter combination of the invention by regulating and controlling each processing step, can be prepared with excellent sphericity, Gao Liu Dynamic property, low oxygen content and average grain diameter and particle diameter distribution meet the pure simple substance metal dust of 3D printing requirement.Meanwhile this method with Other processes are compared, strong to the controllability of the sphericity of metallic particles, particle diameter distribution and oxygen content, and with technique letter Single advantage low with cost.
Brief description of the drawings
The thing phase test map of nano metal powder prepared by Fig. 1 a- Fig. 1 c present invention；Wherein a is nanometer in embodiment 1 The thing phase test map of cobalt powder, b are the thing phase test map of nanometer iron powder in embodiment 2, and c is nano-nickel powder in embodiment 3 Determinand vaseline parcel (is prevented from aoxidizing) by thing phase test map wherein before test.
Microstructure, crystal structure and the particle diameter distribution of nano metal powder prepared by Fig. 2 a- Fig. 2 c present invention；Wherein a For the high power transmission electron microscope shape appearance figure of nano-cobalt powder in embodiment 1, b is the selective electron diffraction collection of illustrative plates of nanometer iron powder particle with standing The calibration result of square crystal structure, c are the particle diameter distribution statistical result of nano-nickel powder particle.
The thing phase test map of 3D printing micron-size spherical metal dust prepared by Fig. 3 a- Fig. 3 c present invention；Wherein a is The thing phase test map of cobalt powder in embodiment 1, b are the thing phase test map of iron powder in embodiment 2, and c is nickel powder in embodiment 3 Thing phase test map.
The microstructure and particle diameter distribution of 3D printing metal powder granulates prepared by Fig. 4 a- Fig. 4 c present invention；Wherein a is The high power shape appearance figure of single metal cobalt granule in embodiment 1, b be embodiment 2 in iron granule scanning electron microscope shape appearance figure, c For the particle diameter distribution statistical result of metallic nickel powder particle in embodiment 3.
Embodiment
With reference to embodiment, the present invention will be further described, but the present invention is not limited to following embodiments.
1 embodiment of the present invention 1 of table, apply the spherical of metallic cobalt, iron and nickel by powder particle that example 2 and embodiment 3 are prepared Degree, mobility and Density Detection result.
Embodiment 1, using raw material high-purity cobalt bulk (purity 99.99wt%) as anode, tungsten is cathode, first vacuumizes and is passed through Argon gas to vacuum pressure reaches 0.04MPa, forms high intensity electric arc by discharge process, hydrogen is passed through after the completion of the starting the arc to vacuum Pressure reaches 0.03MPa, condenses to form the high-purity cobalt nano-particle of solid-state by evaporated metal gas atom, its thing phase test map Such as Fig. 1 a, microstructure such as Fig. 2 a；Using existing patented technology (granted patent number 201010219344.3), by cobalt nano-particle Mixed with polyvinyl alcohol, polyethylene glycol and deionized water, then ball milling 60min, then mechanical agitation 20min, obtain uniform and stable Suspension slurry, utilize closed cycle spray drying equipment to carry out agglomeration granulation, obtain 20~50 μm of spherical cobalt granule；Adopt The tube furnace protected with argon gas is heat-treated the cobalt dust after granulation, and first stage heat treatment temperature is 250 DEG C, during insulation Between 150min；Second stage heat treatment temperature is 915 DEG C, soaking time 120min；Finally cool to room temperature with the furnace, obtain simultaneous Have high compactness and the fine grained micron-size spherical cobalt dust of mobility.The cobalt powder thing phase test map such as Fig. 3 a being prepared, The high power pattern of single metal cobalt granule such as Fig. 4 a, its sphericity, apparent density, mobility and measurement of oxygen content the results are shown in Table 1.
Embodiment 2, using raw material high purity iron bulk (purity 99.99wt%) as anode, be first passed through argon gas to vacuum pressure Reach 0.05MPa, high intensity electric arc is formed by discharge process, hydrogen to vacuum pressure is passed through after the completion of the starting the arc and is reached 0.02MPa, condenses to form the high-purity iron nano-particle of solid-state by evaporated metal gas atom, its thing phase test map such as Fig. 1 b, The crystal face calibration result of selective electron diffraction collection of illustrative plates and cubic crystal structure such as Fig. 2 b；Utilize existing patented technology (granted patent Number 201010219344.3), iron nano-particle is mixed with polyvinyl alcohol, polyethylene glycol and deionized water, ball milling 70min, then Mechanical agitation 30min obtains uniform and stable suspension slurry, carries out agglomeration granulation using closed cycle spray drying equipment, obtains Obtain 20~50 μm of spherical iron particles；The tube furnace protected using argon gas is heat-treated the iron powder after granulation, the first rank Section heat treatment temperature is 300 DEG C, soaking time 120min；Second stage heat treatment temperature is 920 DEG C, and soaking time is 150min；Finally cool to room temperature with the furnace, obtain having concurrently the fine grained micron-size spherical iron powder of high compactness and mobility.System Standby obtained iron powder thing phase test map such as Fig. 3 b, scanning electron microscope pattern such as Fig. 4 b of iron granule, its sphericity, pine fill close Degree, mobility and measurement of oxygen content the results are shown in Table 1.
Embodiment 3, using raw material high purity nickel bulk (purity 99.99wt%) as anode, be first passed through argon gas to vacuum pressure Reach 0.06MPa, high intensity electric arc is formed by discharge process, hydrogen to vacuum pressure is passed through after the completion of the starting the arc and is reached 0.01MPa, condenses to form the high-purity nano nickel particles of solid-state by evaporated metal gas atom, its thing phase test map such as Fig. 1 c, The particle diameter distribution statistical result of nano nickel powder particle such as Fig. 2 c；Utilize existing patented technology (granted patent number 201010219344.3), nano nickel particles are mixed with polyvinyl alcohol, polyethylene glycol and deionized water, then ball milling 80min, Mechanical agitation 40min obtains uniform and stable suspension slurry again, and agglomeration granulation is carried out using closed cycle spray drying equipment, Obtain 20~50 μm of spherical nickel particle；The tube furnace protected using argon gas is heat-treated the nickel by powder after granulation, and first Phase heat treatment temperature is 350 DEG C, soaking time 90min；Second stage heat treatment temperature is 810 DEG C, and soaking time is 180min；Finally cool to room temperature with the furnace, obtain having high compactness and the fine grained micron-size spherical nickel by powder of mobility concurrently.System Standby obtained nickel powder thing phase test map such as Fig. 3 c, particle diameter distribution statistical result such as Fig. 4 c of particle, its sphericity, pine fill close Degree, mobility and measurement of oxygen content the results are shown in Table 1.
The physical parameter for the metal dust that 1 embodiment of the present invention 1 of table, embodiment 2 and embodiment 3 are prepared

Claims (1)

1. a kind of 3D printing preparation method of fine grained simple substance globular metallic powder, it is characterised in that the preparation method uses High pure metal bulk is raw material, in an inert atmosphere by arc evaporation, while is filled with hydrogen control metal gas atom Heat transfer and activity be allowed to cool deposition and obtain high purity elemental nano metal powder particle；Then to high purity elemental metal nano Powder carries out agglomeration granulation, obtains the micron order elemental metals powder of higher density；Finally to micron order elemental metals after granulation Powder is heat-treated, and by degumming and densification consolidation, is obtained granularity, sphericity, mobility and oxygen content and is met 3D Desired elemental metals powder particle is printed, it specifically includes following steps：
(1) using high pure metal bulk as anode, tungsten is cathode, under inert gas and hydrogen environment, passes through discharge process shape Gas atom is generated into high intensity electric arc evaporated metal, the solid-state elemental metals nanometer that particle diameter is 20~80nm is formed after condensation Grain, the wherein component of metal block material are selected from Fe, Co, Ni or Zn, and inert gas and being passed through for hydrogen are sequentially：First vacuumize, so After be passed through argon gas carry out the starting the arc start to evaporate, be then passed through again hydrogen carry out continuous evaporation；
(2) by elemental metals nano particle prepared by polyvinyl alcohol, polyethylene glycol and deionized water and step (1) by certain ratio Example, is combined preparation by ball milling and mechanical agitation and obtains stable suspension slurry, then dried using closed cycle spray Equipment carries out agglomeration granulation, obtains 20~50 μm of spherical metallic particles, wherein dried medium is argon gas；Ball milling and mechanical agitation It is combined, first carries out ball milling, then carries out mechanical agitation again；
(3) spherical metallic particles prepared using the tube furnace of argon gas protection to step (2) are heat-treated, at first stage heat It is 250~350 DEG C to manage temperature, 90~150min of soaking time；Second stage heat treatment temperature is Tm/ 2+80~Tm/ 2+180 DEG C, TmFor elemental metals fusing point, soaking time is 120~180min；Finally cool to room temperature with the furnace, obtain needing suitable for 3D printing The fine grained simple substance globular metallic powder asked；
Wherein, the pressure ratio that hydrogen and argon gas are filled with step (1) is 1：1~3, be passed through argon gas to vacuum pressure reach 0.04~ 0.06MPa carries out the starting the arc, then passes to hydrogen to vacuum pressure and reaches 0.01~0.03MPa progress continuous evaporations；
The slurry ball-milling time is 40~80min in step (2), and rotating speed is 300~400r/min, the mechanical agitation time for 20~ 40min, stir speed (S.S.) are 100~200r/min, ensure total time in 60~120min.
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