CN107116224A - A kind of preparation method of the mould powdered steels of 18Ni 300 for 3D printing technique - Google Patents

A kind of preparation method of the mould powdered steels of 18Ni 300 for 3D printing technique Download PDF

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Publication number
CN107116224A
CN107116224A CN201710274793.XA CN201710274793A CN107116224A CN 107116224 A CN107116224 A CN 107116224A CN 201710274793 A CN201710274793 A CN 201710274793A CN 107116224 A CN107116224 A CN 107116224A
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mould
printing technique
powder
preparation
steels
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吴文恒
吴凯琦
卢林
仲守亮
杨启云
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Shanghai Institute of Materials
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Shanghai Institute of Materials
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • 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
    • 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
    • B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
    • C22C38/105—Ferrous alloys, e.g. steel alloys containing cobalt containing Co and Ni
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0836—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with electric or magnetic field or induction
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0844—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid in controlled atmosphere
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0896—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid particle transport, separation: process and apparatus
    • 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

The invention discloses a kind of preparation method of the mould powdered steels of 18Ni 300 for 3D printing technique, this method uses vacuum melting aerosolization technology, the powder of different-grain diameter is matched with ultrasonic vibration, air current classifying method, by vacuum degassing technology, the mould powdered steels of 18Ni 300 suitable for different metal 3D printing technique are prepared.Compared with prior art, the mould powdered steels of 18Ni 300 prepared by the present invention have sphericity height, particle diameter distribution is uniform, oxygen content is low, the low performance characteristics of impurity content, performance requirement of the different 3D printing techniques to dusty material is met, the development of metal increases material manufacturing technology is promoted.

Description

A kind of preparation method of 18Ni-300 mould powdered steels for 3D printing technique
Technical field
The present invention relates to the preparation method of alloy powder, more particularly, to a kind of 18Ni-300 moulds for 3D printing technique Have the preparation method of powdered steel, belong to material increasing field.
Background technology
3D printing is a kind of using means such as laser or electron beams, according to three-dimensional modeling, is successively added under the control of the computer Plus the manufacturing technology of part is directly quickly precisely formed in accumulation material, also referred to as " increasing material manufacturing ".Increases material manufacturing technology need not be passed Cutter, fixture and the multi-step process of system, can rapidly and precisely be produced using three-dimensional design data in an equipment The part of arbitrarily complicated shape, compared to the traditional processing and common special processing technology that material removes (or deformation), increases material Manufacturing technology has high stock utilization.
Metal 3D printing technique, as forefront and most potential technology in whole 3D printing system, is advanced manufacture skill The important development direction of art.Metal 3D printing technique is divided into three classes according to the mode that adds of metal dust：
(1) selective laser smelting technology (Selective Laser Melting, SLM) is metal parts straight forming A kind of method, is the latest development of metal increases material manufacturing technology.Most basic thought of the technology based on rapid shaping, i.e., successively melt " increment " manufacture covered, has metal in the part of geometry in particular, forming process according to threedimensional model straight forming Powder is completely melt, produces metallurgical binding.SLM can produce the shape that can not be manufactured using traditional machining means Baroque metal parts, and manufacturing procedure is greatly reduced, shorten the process-cycle.It is currently used in SLM metal dust Material has titanium alloy, aluminium alloy, stainless steel, mould steel, nickel-base alloy etc..
(2) Engineered Net Shaping Aftertreatment (Laser Engineered Net Shaping, LENS) refers in substrate Selected metal cladding material is given in preset or synchronization on alloy surface, is then allowed to through laser treatment with substrate top layer simultaneously Fusing, and the superficial layer with base material in metallurgical binding is rapidly solidificated into, so as to significantly change the wear-resisting, resistance to of base material The process of the characteristic such as erosion, heat-resisting.
(3) electron beam melting technology (Electron Beam Melting, EBM) difference closely similar with SLM, most basic It is not that thermal source is different.EBM as thermal source, keeps part building course temperature in annealing temperature using electron beam, micro- to part Structure is seen to have a significant effect.
The mobility of powder is all for one of key performance of dusty material of 3D printing technique, preferable powder stream Dynamic property be conducive to improve SLM, EBM during powdering uniformity and LENS during powder feeding stability, 3D can not only be improved and beaten Dimensional accuracy, the surface quality of drip molding are printed, the density and structural homogenity of drip molding can be also improved, part is greatly reduced Process time.
The granule-morphology of powder directly determines the mobility of powder, and powder its pattern prepared with different atomization methods is It is different.Common granule-morphology has：Spherical, dendriform, needle-like, granular, sheet etc., apply in general to 3D printing technique is ball Shape powder.The higher powder of particle sphericity is due to good fluidity, and even relatively fine powder, course of conveying is also more suitable Profit, the relatively low powder of phase counter particles sphericity, poor fluidity, causes powdering uneven or powder feeding is not smooth, finally influences 3D The forming quality of printout.Further, since aspherical powder Surface and internal structure is loose, therefore the 3D printing of aspherical powder There is certain gas hole defect inside drip molding, and the drip molding internal porosity of spherical powder seldom even without.
Although the good fluidity of the high powder of particle sphericity, spheric granules bulk density is small, space is big so that shaping The relative density of part is small, and tangent two-by-two between spheric granules, influences forming quality.So in the reality of spherical particle powder In use, needing according to different 3D printing techniques, grain size proportion, mixing are carried out to powder, to realize the excellent of variable grain Change combination, improve forming quality.
18Ni-300 mould steel is, as matrix, intermetallic compound to be produced during timeliness using carbon-free (or micro- carbon) martensite The unimach of precipitation-hardening.Different from traditional high strength steel, 18Ni-300 mould steel does not lean on carbon, and by intermetallic compound Disperse educt strengthen.Therefore with following characteristic：1. high tenacity and excellent cold and hot working performance；2. corrosion resistance Good, corrosion rate in an atmosphere is only the half of general low-alloy steel, to the drag of corrosive solution than low-alloy steel more It is excellent；3. simple Technology for Heating Processing, is hardly deformed during timeliness；4. welding performance is good, is not in weld crack, is heated The hardening of influence part is small, and postwelding aging temp is low.
At present, the main preparation methods of metal dust are gas atomizations, and its general principle is with high velocity air that liquid is golden Category stream is broken into droplet and is rapidly solidificated into the process of powder, because powder prepared by gas atomization has high purity, oxygen Content is low, powder size is controllable, production cost is low and the advantages of high sphericity, is particular enable to meet 3D printing technique for gold Belong to the requirement of powder property, it has also become the main development direction of high-performance and special alloy powder technology of preparing.
18Ni-300 moulds powdered steel for 3D printing technique has the powder being different from required for prior powder metallurgy Characteristic, high-purity, low oxygen content that conventional powder must possess are not required nothing more than, while also requiring powder sphericity height, granularity point Cloth optimizes, and with good mobility and apparent density.Due to sensitive, the existing atomization to impurity component of 18Ni-300 mould steel Often there is the phenomenon that impurity is more, sphericity is not high in powder prepared by method, have a strong impact on the 3D printing forming property of powder, Accordingly, it would be desirable to a kind of preparation method for the 18Ni-300 mould powdered steels that can be used in 3D technology.
The content of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide one kind is used for 3D printing skill The preparation method of the 18Ni-300 mould powdered steels of art.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of preparation method of 18Ni-300 mould powdered steels for 3D printing technique, comprises the following steps：
(1) alloy melting：Melting is carried out in vaccum sensitive stove to 18Ni-300 mould steel raw materials, alloy melt is obtained；
(2) powder by atomization：Inert gas is filled with body of heater with vacuum breaker, when furnace pressure reaches tiny structure, is opened Air exhauster, and alloy melt poured into middle bottom pour ladle, opens material leakage valve, small opening of the alloy melt through middle bottom pour ladle bottom freely to Lower inflow gas atomization stove, high velocity inert gas stream is impacted by close coupled type circumferential weld nozzle to alloy melt, makes its powder Fine droplets are broken into, 18Ni-300 mould powdered steels are obtained after to be cooled, solidification, 18Ni-300 mould powdered steels drop to atomization Tower bottom is cooled down, powder collection device is brought into by gas；
(3) powder sieving：By 18Ni-300 moulds powdered steel made from step (2) according to different metal 3D printing technique pair The requirement of powder diameter is sieved, is classified；
(4) vacuum outgas：The 18Ni-300 moulds powdered steel matched dress boat is placed in vacuum degassing furnace, in certain vacuum A period of time is incubated under degree and certain temperature, the 18Ni-300 mould powdered steels for 3D printing technique are finally made.
In step (1), vacuum is ＜ 1 × 10 in vaccum sensitive stove-1Pa, when 18Ni-300 mould steel material temperatures are reached At 1400~1450 DEG C, 18Ni-300 mould steel raw materials start fusing.
In step (1), after 18Ni-300 mould steel raw materials are completely melt, control alloy melt temperature is 1600~1700 DEG C, and continue 15~20min of insulation.
In step (1), 18Ni-300 mould steel material composition composition meets following requirement by percentage to the quality： Ni18.0%~19.0%, Co8.5%~9.5%, Mo4.6%~5.2%, Ti0.5%~0.8%, C≤0.03%, Mn≤ 0.1%, P≤0.01%, S≤0.01%.
In step (2), described tiny structure is 90-100KPa, preferably 99.4KPa.
In step (2), temperature control is at 1100~1200 DEG C in described middle bottom pour ladle.
In step (2), described inert gas is that the atomizing pressure in high-purity argon gas or high pure nitrogen, gas atomization stove is 3.5MPa。
In step (2), described close coupled type circumferential weld nozzle circumferential weld area is in 25~38mm2Between.
In step (3), requirement of the different metal 3D printing technique to powder size is respectively：
Selective laser melting process：15~53 μm；Engineered Net Shaping Aftertreatment：45~150 μm；Electron beam melting skill Art：45~106 μm.
In step (4), per boat, dress powder is highly less than 15mm.
In step (4), 18Ni-300 mould powdered steels are 1.3 × 10﹣ 2Under Pa vacuum, successively at 400~600 DEG C and 700 2~5h is incubated respectively at~900 DEG C.
Using 18Ni-300 moulds powdered steel made from above-mentioned preparation method, available for a variety of 3D printing techniques.
The method that conventional metal dust improves, improved its mobility is addition dispersant, makes rubbing between powder particle Wipe and reduce, so as to play the effect for improving powder flowbility.But require powder for the 18Ni-300 moulds powdered steel of 3D printing The impurity content at end can undoubtedly mix more impurity elements in very low level, addition dispersant, and 3D printing shaping is caused Adverse effect.The method that powder particle sphericity is improved in powder atomization production is the size for increasing atomization cylinder, improves alloy The degree of superheat of drop, but the above method can cause production technology unstable, production cost increase, be unfavorable for 3D printing technique Popularization and application.
The present invention prepares 18Ni-300 mould comminuted steel shots using the combination of process for vacuum induction smelting and vacuum degassing technology End.Wherein, vacuum induction melting (Vacuum Induction Melting, VIM) is that one kind utilizes electromagnetism under vacuum Inductive heating principle carrys out the smithcraft processing procedure of smelting metal.Vortex flow can be produced during electromagnetic induction, makes metal molten. This processing procedure can be used to improve the purity of alloy, drop low-alloyed oxygen content.Vacuum outgas (Vacuum Degassing) refer to by Metal dust is placed in vacuum environment, at a certain temperature, the method for discharging the gas on powder gap or surface.Very Empty degassing process can improve the mobility of powder, because powder particle particle diameter is smaller, surface can be bigger, also easier Adsorbed gas, the gas of absorption can be further exacerbated by the adhesion of powder, reunion.The present invention is prepared according to optimum grain-diameter ratio range 18Ni-300 mould powdered steels in powder particle particle diameter it is smaller, mobility and 3D printing formability to powder have certain Influence, if to improve the mobility of 3D printing metal dust, Fruit storage is a kind of effective post-processing technology.
It can ensure the ratio of spherical powder particle more than 90% by the method for the present invention, so that the powder of preparation End can be completely used for 3D printing technique, and an innovative point of preparation method of the present invention is to combine different 3D printing techniques spies Point, by method of the powder of preparation by vibrosieve, air current classifying, is respectively used to different metal 3D printing techniques, significantly The utilization rate of powder is improved, the problem of conventional 3D printing metal dust utilization rate is too low is solved, reduces production cost, Achieve obvious economic benefit.
In summary, compared with prior art, the present invention has advantages below and beneficial effect：
1st, the 18Ni-300 mould steel impurity content of powder that prepared by the present invention is low, and particle diameter distribution is uniform, and powder particle is spherical Degree is high, and average spherical degree >=0.80, powder flowbility is good (≤18s/50g), apparent density height (>=4.0g/cm3), beaten by 3D Obtained drip molding even tissue, densification are printed, dimensional accuracy is high, good mechanical performance.
2nd, the present invention is directed to requirement of the different metal 3D printing technique to powder diameter, passes through the side such as screening, air current classifying Method, prepares the 18Ni-300 mould powdered steels suitable for a variety of 3D printing techniques；Vacuum degassing technology is used simultaneously, is effectively carried The high mobility of 18Ni-300 mould powdered steels.
Brief description of the drawings
Fig. 1 is 18Ni-300 mould steel powder particle shape appearance figure made from embodiment 1；
Fig. 2 is 18Ni-300 mould steel powder particle shape appearance figure made from embodiment 2；
Fig. 3 is 18Ni-300 mould steel powder particle shape appearance figure made from embodiment 3.
Embodiment
A kind of preparation method of 18Ni-300 mould powdered steels for 3D printing technique, comprises the following steps：
(1) alloy melting：Melting is carried out in vaccum sensitive stove to 18Ni-300 mould steel raw materials, alloy melt is obtained, Vacuum is ＜ 1 × 10 in vaccum sensitive stove-1Pa, when 18Ni-300 mould steel material temperatures reach 1400~1450 DEG C, 18Ni-300 mould steel raw materials start fusing, after 18Ni-300 mould steel raw materials are completely melt, control alloy melt temperature exists 1600~1700 DEG C, and continue insulation 15~20min, 18Ni-300 mould steel material composition composition meet by percentage to the quality It is following to require：Ni18.0%~19.0%, Co8.5%~9.5%, Mo4.6%~5.2%, Ti0.5%~0.8%, C≤ 0.03%, Mn≤0.1%, P≤0.01%, S≤0.01%.
(2) powder by atomization：Inert gas is filled with body of heater with vacuum breaker, when furnace pressure reaches 90-100KPa, is opened Air exhauster is opened, and alloy melt is poured into temperature control in middle bottom pour ladle, middle bottom pour ladle and, at 1100~1200 DEG C, opens material leakage Valve, small opening of the alloy melt through middle bottom pour ladle bottom freely flows downwardly into gas atomization stove, high velocity inert gas circulation tension coupling Box-like circumferential weld nozzle, close coupled type circumferential weld nozzle circumferential weld area is in 25~38mm2Between, alloy melt is impacted, inertia Gas is that the atomizing pressure in high-purity argon gas or high pure nitrogen, gas atomization stove is 3.5MPa, it is ground into fine droplets, treats 18Ni-300 mould powdered steels are obtained after cooling, solidification, 18Ni-300 mould powdered steels drop to atomizing cooling tower bottom, by gas Body brings powder collection device into；
(3) powder sieving：By 18Ni-300 moulds powdered steel made from step (2) according to different metal 3D printing technique pair The requirement of powder diameter is sieved, is classified, and requirement of the different metal 3D printing technique to powder size is respectively：Precinct laser Smelting technology：15~53 μm；Engineered Net Shaping Aftertreatment：45~150 μm；Electron beam melting technology：45~106 μm；
(4) vacuum outgas：The 18Ni-300 moulds powdered steel matched dress boat is placed in vacuum degassing furnace, dress powder is high per boat Degree is less than 15mm, and 18Ni-300 mould powdered steels are 1.3 × 10﹣ 2Under Pa vacuum, successively in 400~600 DEG C and 700~900 DEG C It is lower to be incubated 2~5h respectively, the 18Ni-300 mould powdered steels for 3D printing technique are finally made.
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1：
The 18Ni-300 mould powdered steels for SLM technologies are prepared using following steps：
(1) alloy remelting：50kg 18Ni-300 mould steel raw material is added into vacuum induction melting, alloying component is Ni18.6%, Co8.9%, Mo4.8%, Ti0.6%, C0.003%, Mn0.06%, P0.002%, S0.001%.Smelting furnace is true Reciprocal of duty cycle 7.2 × 10-2Pa, fusion temperature is 1420 DEG C, after raw material is completely melt, control smelting temperature is in (1620 ± 20) DEG C scope It is interior, and 20min is incubated, while middle bottom pour ladle is heated into 1140 DEG C；
(2) powder by atomization：Inert gas is filled with body of heater with vacuum breaker, when furnace pressure reaches 99.4KPa, is opened Air exhauster, middle bottom pour ladle is poured into by alloy melt, opens material leakage valve, and small opening of the alloy melt through middle bottom pour ladle bottom is freely downward Inflow gas atomizing furnace, the circumferential weld area of spray disk is 25mm2, the atomizing pressure in gas atomization stove is 3.5MPa, in high-purity argon Under the percussion of air-flow, alloy melt is ground into fine droplets, and 18Ni-300 mould powdered steels, powder are obtained after cooling, solidification End drops to atomizing cooling tower bottom, and powder collection device is brought into by gas；
(3) powder sieving：By 18Ni-300 mould powdered steels made from step (2) according to selective laser melting process (SLM) requirement (15~53 μm) to powder diameter is sieved, is classified.
(4) vacuum outgas：Step (3) is classified to obtained 18Ni-300 moulds powdered steel dress boat and is placed in vacuum degassing furnace, Per boat, dress powder is highly less than 15mm, 6 boats is put per stove, 1.3 × 10﹣ 2Under Pa vacuum, protected respectively at 400 DEG C and 700 DEG C successively Warm 4.5h.
The 18Ni-300 mould steel powder particle patterns that the present embodiment is prepared are as shown in figure 1, the μ of average grain diameter 34.74 M, sphericity 0.95, mobility 15.2s/50g, apparent density 4.21g/cm3, powder carries out part in EOS M280 equipment SLM is molded, and powder flowbility is good during powdering, and formation of parts deforms small, uniform texture, and mechanical property meets part Use requirement.
Embodiment 2
The 18Ni-300 mould powdered steels for LENS technologies are prepared using following steps：
(1) alloy melting：50kg 18Ni-300 mould steel raw material is added into vacuum induction melting, alloying component is Ni18.8%, Co8.7%, Mo4.9%, Ti0.6%, C0.002%, Mn0.03%, P0.005%, S0.003%.Fusion temperature For 1430 DEG C, vacuum is 8.1 × 10 in vaccum sensitive stove-2Pa, fusion temperature is 1410 DEG C, after raw material is completely melt, control Smelting temperature is incubated 20min in the range of (1640 ± 20) DEG C, while middle bottom pour ladle is heated into 1120 DEG C；
(2) powder by atomization：Inert gas is filled with body of heater with vacuum breaker, when furnace pressure reaches 90KPa, unlatching is taken out Blower fan, middle bottom pour ladle is poured into by alloy melt, opens material leakage valve, small opening of the alloy melt through middle bottom pour ladle bottom is freely to dirty Enter gas atomization stove, the circumferential weld area of spray disk is 30mm2, the atomizing pressure in gas atomization stove is 3.5MPa, in high-purity argon gas Under the percussion of stream, alloy melt is ground into fine droplets, and 18Ni-300 mould powdered steels, powder are obtained after cooling, solidification Atomizing cooling tower bottom is dropped to, powder collection device is brought into by gas；
(3) powder sieving：By 18Ni-300 mould powdered steels made from step (2) according to Engineered Net Shaping Aftertreatment (LENS) (45~150 μm) of requirement carries out ultrasonic screening, air current classifying, and the high ball for metal 3D printing technique is finally made Shape degree 18Ni-300 mould powdered steels.
(4) vacuum outgas：Step (3) is classified to obtained 18Ni-300 moulds powdered steel dress boat and is placed in vacuum degassing furnace, Per boat, dress powder is highly less than 15mm, 1.3 × 10﹣ 2Under Pa vacuum, 3.5h is incubated respectively at 500 DEG C and 800 DEG C successively.
The 18Ni-300 mould powdered steels that the present embodiment is prepared, 105.2 μm of average grain diameter, sphericity 0.91, flowing Property 12s/50g, apparent density 4.75g/cm3, powder carries out part LENS shapings in LSF-IVC equipment, powder paving send it is uniform, The part dense structure of shaping, deformation are small.
Embodiment 3：
The 18Ni-300 mould powdered steels for EBM technologies are prepared using following steps：
(1) alloy remelting：50kg 18Ni-300 mould steel raw material is added into vacuum induction melting, alloying component is Ni18.4%, Co8.8%, Mo4.7%, Ti0.7%, C0.002%, Mn0.03%, P0.004%, S0.002%.Smelting furnace is true Reciprocal of duty cycle 8.8 × 10-2Pa, fusion temperature is 1435 DEG C, after raw material is completely melt, control smelting temperature is in (1640 ± 20) DEG C scope It is interior, 20min is incubated, while middle bottom pour ladle is heated into 1180 DEG C；
(2) powder by atomization：Inert gas is filled with body of heater with vacuum breaker, when furnace pressure reaches 100KPa, is opened Air exhauster, middle bottom pour ladle is poured into by alloy melt, opens material leakage valve, and small opening of the alloy melt through middle bottom pour ladle bottom is freely downward Inflow gas atomizing furnace, the circumferential weld area of spray disk is 38mm2, the atomizing pressure in gas atomization stove is 3.5MPa, in high-purity argon Under the percussion of air-flow, alloy melt is ground into fine droplets, and 18Ni-300 mould powdered steels, powder are obtained after cooling, solidification End drops to atomizing cooling tower bottom, and powder collection device is brought into by gas；
(3) powder sieving：By 18Ni-300 moulds powdered steel made from step (2) according to electron beam cladding technology (EBM) Requirement (45~100 μm) to powder diameter is sieved, is classified.
(4) vacuum outgas：Step (3) is classified to obtained 18Ni-300 moulds powdered steel dress boat and is placed in vacuum degassing furnace, Per boat, dress powder is highly less than 15mm, 1.3 × 10﹣ 2Under Pa vacuum, 2.5h is incubated respectively at 600 DEG C and 900 DEG C successively.
18Ni-300 mould steel powder particle patterns that the present embodiment is prepared as shown in figure 3,70.3 μm of average grain diameter, Sphericity 0.95, mobility 14.1s/50g, apparent density 4.51g/cm3, powder carries out part EBM in Arcam Q20 equipment Shaping, powder paving is sent uniformly, and the part dense structure of shaping, deformation are small.
The above-mentioned description to embodiment is understood that for ease of those skilled in the art and using invention. Person skilled in the art obviously can easily make various modifications to these embodiments, and described herein general Principle is applied in other embodiment without passing through performing creative labour.Therefore, the invention is not restricted to above-described embodiment, ability Field technique personnel are according to the announcement of the present invention, and not departing from improvement and modification that scope made all should be the present invention's Within protection domain.

Claims (10)

1. the preparation method of a kind of 18Ni-300 mould powdered steels for 3D printing technique, it is characterised in that including following step Suddenly：
(1) alloy melting：Melting is carried out in vaccum sensitive stove to 18Ni-300 mould steel raw materials, alloy melt is obtained；
(2) powder by atomization：Inert gas is filled with body of heater with vacuum breaker, when furnace pressure reaches tiny structure, exhausting is opened Machine, and alloy melt is poured into middle bottom pour ladle, small opening of the alloy melt through middle bottom pour ladle bottom freely flows downwardly into gas atomization Stove, high velocity inert gas stream impacts to alloy melt by close coupled type circumferential weld nozzle, it is ground into fine droplets, 18Ni-300 mould powdered steels are obtained after to be cooled, solidification；
(3) powder sieving：By 18Ni-300 moulds powdered steel made from step (2) according to different metal 3D printing technique to powder The requirement of particle diameter is sieved, is classified；
(4) vacuum outgas：The 18Ni-300 moulds powdered steel matched dress boat is placed in vacuum degassing furnace, in certain vacuum degree and A period of time is incubated under certain temperature, the 18Ni-300 mould powdered steels for 3D printing technique are finally made.
2. a kind of preparation method of 18Ni-300 mould powdered steels for 3D printing technique according to claim 1, its It is characterised by, in step (1), vacuum is ＜ 1 × 10 in vaccum sensitive stove-1Pa, when 18Ni-300 mould steel material temperatures reach During to 1400~1450 DEG C, 18Ni-300 mould steel raw materials start fusing.
3. a kind of preparation method of 18Ni-300 mould powdered steels for 3D printing technique according to claim 1, its Be characterised by, in step (1), after 18Ni-300 mould steel raw materials are completely melt, control alloy melt temperature 1600~ 1700 DEG C, and continue 15~20min of insulation.
4. a kind of preparation method of 18Ni-300 mould powdered steels for 3D printing technique according to claim 1, its It is characterised by, in step (1), 18Ni-300 mould steel material composition composition meets following requirement by percentage to the quality： Ni18.0%~19.0%, Co8.5%~9.5%, Mo4.6%~5.2%, Ti0.5%~0.8%, C≤0.03%, Mn≤ 0.1%, P≤0.01%, S≤0.01%.
5. a kind of preparation method of 18Ni-300 mould powdered steels for 3D printing technique according to claim 1, its It is characterised by, in step (2), temperature control is at 1100~1200 DEG C in described middle bottom pour ladle.
6. a kind of preparation method of 18Ni-300 mould powdered steels for 3D printing technique according to claim 1, its It is characterised by, in step (2), described inert gas is the atomizing pressure in high-purity argon gas or high pure nitrogen, gas atomization stove For 3.5MPa.
7. a kind of preparation method of 18Ni-300 mould powdered steels for 3D printing technique according to claim 1, its It is characterised by, in step (2), described close coupled type circumferential weld nozzle circumferential weld area is in 25~38mm2Between.
8. a kind of preparation method of 18Ni-300 mould powdered steels for 3D printing technique according to claim 1, its It is characterised by, in step (3), requirement of the different metal 3D printing technique to powder size is respectively：
Selective laser melting process：15~53 μm；Engineered Net Shaping Aftertreatment：45~150 μm；Electron beam melting technology： 45~106 μm.
9. a kind of preparation method of 18Ni-300 mould powdered steels for 3D printing technique according to claim 1, its It is characterised by, in step (4), per boat, dress powder is highly less than 15mm.
10. a kind of preparation method of 18Ni-300 mould powdered steels for 3D printing technique according to claim 1, its It is characterised by, in step (4), 18Ni-300 mould powdered steels are 1.3 × 10﹣ 2Under Pa vacuum, successively at 400~600 DEG C and 700 2~5h is incubated respectively at~900 DEG C.
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CN113894293A (en) * 2021-10-08 2022-01-07 江苏省特种设备安全监督检验研究院 Method for preparing graphene composite 18Ni-300 antifriction metal material based on SLM technology
CN114682784A (en) * 2022-03-31 2022-07-01 钢铁研究总院有限公司 Low-cost powder preparation method and printing method of 1900 MPa-grade ultrahigh-strength steel for SLM
CN114682784B (en) * 2022-03-31 2023-11-28 钢铁研究总院有限公司 Low-cost powder preparation method and printing method of 1900 MPa-level ultrahigh-strength steel for SLM
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Application publication date: 20170901