CN104923797A - Preparation method of Incone1625 nickel base alloy powder for selective laser melting technology - Google Patents

Preparation method of Incone1625 nickel base alloy powder for selective laser melting technology Download PDF

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CN104923797A
CN104923797A CN201510210563.8A CN201510210563A CN104923797A CN 104923797 A CN104923797 A CN 104923797A CN 201510210563 A CN201510210563 A CN 201510210563A CN 104923797 A CN104923797 A CN 104923797A
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inconel625
alloy powder
selective laser
powder
alloy
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CN104923797B (en
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吴文恒
杨启云
仲守亮
曹冲
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Shanghai Inst. of Materials
Zhongtian Material Supplementary Manufacturing Co., Ltd.
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SHANGHAI INST OF MATERIALS
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Abstract

The invention relates to a preparation method of Incone1625 nickel base alloy powder for a selective laser melting technology. The method combines a vacuum electrode induction smelting technology with an ultrasonic tight coupling atomization technology, applies methods of ultrasonic vibration separation and airflow classification, and matches powder with different particle sizes to prepare the Incone1625 nickel base alloy powder suitable for the selective laser melting technology. Compared with the prior art, the Incone1625 nickel base alloy powder, prepared by the method, has such performance characteristics as high sphericility, uniform particle size distribution, low oxygen content and low impurity content, satisfies the performance requirements of the selective laser melting technology on powder materials, and promotes the development of a metal material increase manufacturing technology.

Description

For the preparation method of the Inconel625 Co-based alloy powder of selective laser smelting technology
Technical field
The present invention relates to a kind of preparation method of Co-based alloy powder, especially relate to a kind of preparation method of the Inconel625 Co-based alloy powder for selective laser smelting technology, belong to and increase material manufacture field.
Background technology
Increasing material manufacture is that one utilizes the means such as laser or electron beam, according to three-dimensional modeling, successively adds under the control of the computer and piles up the manufacturing technology that material directly accurately forms part fast, also claim " 3D printing ".Increase material manufacturing technology and do not need traditional cutter, fixture and multi-step process, utilize three-dimensional design data can produce the part of any complicated shape fast and accurately on an equipment, remove the tradition processing of (or distortion) and common special processing technology compared to material, increasing material manufacturing technology has high stock utilization.
Selective laser smelting technology (Selective Laser Melting, SLM) is a kind of method of metal parts straight forming, is the latest development that metal increases material manufacturing technology.This technology is based on the basic thought of rapid shaping, i.e. " increment " manufacture of successively cladding, have the part of geometry in particular according to threedimensional model straight forming, in forming process, metal dust melts completely, produces metallurgical binding.SLM can produce and adopt traditional machined means cannot the metal parts of produced shape and structure complexity, and greatly reduces manufacturing procedure, shortens the process-cycle.The current metal powder material for SLM has titanium alloy, aluminium alloy, stainless steel, mould steel, nickel-base alloy etc.
Inconel625 nickel-base alloy is a kind of typical solution strengthening type ni-base wrought superalloy, the high-load of its chromium, molybdenum is to numerous corrosive medium, from high oxidation environment to general corrosion environment, all there is high resistance pitting, cracking resistance becomes corrosive power, show remarkable corrosion resistance characteristic, be widely used in the industries such as Aero-Space, defence and military, chemical industry., there is macro-components segregation and the low shortcoming of stock utilization respectively, and adopt SLM technique, can effectively overcome above-mentioned shortcoming in the Inconel625 nickel-base alloy part adopting casting and the traditional handicraft such as forging to manufacture.Inconel625 Co-based alloy powder for SLM has the powder characteristics being different from prior powder metallurgy, not only require that powder purity is high, oxygen content is low, also require that powder sphericity is high, even particle size distribution, and good mobility and apparent density.
At present, the main preparation methods of metal dust is aerosolization method, its general principle is, with high velocity air, liquid metal stream is broken into droplet and the process of rapid solidification powdered, because aerosolization legal system is standby, powder has high purity, oxygen content is low, powder size is controlled, production cost is low and sphericity advantages of higher, the requirement of SLM technology for metal dust performance can be met especially, become the main development direction of high-performance and special alloy powder preparation technology.
Vacuum electrode induction melting technology is a kind of novel process grown up on the basis of vacuum aerosolization technology.It has, and material is not oxidizable, metal dust cooling changes degree comparatively advantages of higher fast and automatically.The cardinal principle of this technology is as consutrode using prealloy rod, induction melting is carried out when not using melting kettle, induction melting is carried out by being reduced in a toroidal inductor with certain speed by the metal electrode of slow circumvolve, electrode drop freely falls into gas atomizing nozzle system, utilizes indifferent gas to be atomized.This technology great advantage is that of avoiding the nonmetallic inclusion that traditional crucible for smelting technique is mixed, and substantially increases by the degree of purity of smelting metal, reduces the degree of oxidation of metal bath.
Ultrasonic close coupling atomization technique is that one carries out structure optimization to close-coupled nozzle, makes the muzzle velocity of air-flow exceed the velocity of sound, and increases the mass flowrate of metal, thus obtain high velocity air under less atomizing pressure, define ultrasonic close coupling atomization technique.The feature of powder prepared by this atomization technique is that attritive powder recovery rate is high, particle diameter is little, narrow particle size distribution, and higher cooling velocity is conducive to the production of microcrystallizing alloy or amorphous powdered alloy.From current development, ultrasonic close coupling atomization technique represents the new developing direction of metal dust atomization technique, can be widely used in the production of the superfine alloy powders such as fine stainless steel, ferrous alloy, nickel-base alloy, magnetic material.
Inconel625 Co-based alloy powder for selective laser smelting technology prepared by prior art, only simply sieves powder, is directly used in SLM former after obtaining the suitable powder of particle size range.But the powder of same particle size range, different grain size proportioning, its laser fusion formability differs greatly; Just there will be " reunion " phenomenon when powder reaches more than 80 μm, cause paving powder mobility not smooth.The present invention prepare Ni-base Superalloy Powder, its average grain diameter is less than paving powder accumulation horizon thickness, by weight accurate proportioning is carried out to the powder of different grain size rank, the powder bed of high-compactness is formed after ensureing paving powder, in selective laser fusing forming process, " splashing " phenomenon does not occur, and forming part distortion is little, precision is high, and performance can meet instructions for use.According to the feature of powder sieving technique, preparation method of the present invention is applying vibration screening+air current classifying method innovatively, not only increases powder sieving efficiency, can also ensure higher screening effect.
In sum, compared with prior art, the present invention has the following advantages and beneficial effect:
1, the present invention is directed to selective laser smelting technology feature, in conjunction with different powder preparation technology, preparation Inconel625 Co-based alloy powder high purity, impurity and oxygen content is low, particle sphericity is high, the powder mixture ratio relation of even particle size distribution, different-grain diameter rank is suitable, there is good mobility and higher apparent density, meet and be suitable for the particular/special requirement of selective laser smelting technology for powder property.
2, in the Inconel625 Co-based alloy powder that prepared by the present invention, the recovery rate of fine powder is high, wherein the powder yield of particle diameter≤60 μm is higher than 40%, the Inconel625 Co-based alloy powder remaining >=60 μm can be used for laser melting and coating technique and traditional powder metallurgy product, greatly reduce production cost, also there is preparation process and pollute little, operating automation degree advantages of higher.
Summary of the invention
Object of the present invention is exactly provide a kind of preparation method of the Inconel625 Co-based alloy powder for selective laser smelting technology to overcome defect that above-mentioned prior art exists, and the powder that preparation method of the present invention obtains has the performance characteristics such as sphericity is high, even particle size distribution, oxygen content are low, impurity content is extremely low, laser sintering (SLS) is stable.
Object of the present invention can be achieved through the following technical solutions:
For a preparation method for the Inconel625 Co-based alloy powder of selective laser smelting technology, comprise the following steps:
(1) alloy smelting: Inconel625 nickel-base alloy raw material is added vacuum induction furnace smelting, obtained Inconel625 nickel-base alloy bar after smelting;
(2) bar processing: cylindrical bar Inconel625 nickel-base alloy bar being processed into band cone angle;
(3) powder by atomization: vacuum electrode induction melting is carried out to the Inconel625 nickel-base alloy bar of completion of processing, cone angle surface, bar lower end is fused into liquid state under the heating of induction coil, control the decrease speed of bar, ensure that bar lower end forms continual and steady alloy liquid droplet, under the impact of the supersonic atomization medium that molten metal drop ejects at close-coupled nozzle, atomization forms fine droplets, drop in flight course by being rapidly solidificated into Inconel625 Co-based alloy powder under the cooling of atomizing medium, powder drops to atomizing cooling tower conical lower portion, brought in powder collection device by air-flow,
(4) proportioning is sieved: divide carrying out ultrasonic vibrating screen after the Inconel625 Co-based alloy powder cooling of collecting after atomization, remove the particle of particle diameter >=60 μm, then air current classifying is carried out to the particle that residue particle diameter is 0 ~ 60 μm, account for 10 ~ 20% according to particle diameter 0 ~ 15 μm, particle diameter 15 ~ 30 μm accounts for 20 ~ 50%, 30 ~ 45 μm and account for 20 ~ 50%, 45 ~ 60 μm of part by weight relations accounting for 10 ~ 20% and carry out proportioning, finally obtain the Inconel625 Co-based alloy powder being applicable to selective laser smelting technology.
In step (1), described Inconel625 nickel-base alloy raw alloy component ratio is: Ni: >=58%, Cr:20 ~ 23%, Mo:8 ~ 10%, Nb:3.15 ~ 4.15%, Fe :≤5%, Al :≤0.4%, Ti :≤0.4%, Mn :≤0.5%, Si :≤0.5%, C :≤0.1%, P :≤0.015%, S :≤0.015%.
In step (1), smelting temperature controls at 1400 ~ 1600 DEG C.
In step (2), described angle of taper is 75 ~ 90 °.Cone angle is processed as 75 ~ 90 ° can ensure the melting rate that bar is stable, and the length of bar and diameter can adjust according to the size of the structure of the pay-off of atomizing furnace and induction coil.The recyclable raw material being used as alloy smelting of waste cut materials after processing, to improve the utilization rate of material.
When carrying out vacuum electrode induction melting in step (3), the decrease speed of Inconel625 nickel-base alloy bar will control according to the burn-off rate of bar, and as preferred embodiment, the decrease speed of bar controls at 10 ~ 50mm/min.
In step (3), the nozzle exit pressure of close-coupled nozzle is 1.0 ~ 5.0MPa.
Atomizing medium described in step (3) adopts high-purity argon gas or high pure nitrogen.
In step (4), the gas medium of air current classifying adopts nitrogen or argon gas, carries out vacuum packaging to the Inconel625 Co-based alloy powder after classification, proportioning, prevents the powder prepared from making moist, being oxidized.
Conventional Inconel625 Co-based alloy powder atomization technique many employings crucible+middle bottom pour ladle melting, a certain amount of nonmetallic inclusion can be mixed in obtained powder, this impurity is mainly derived from crucible refractory material and middle bottom pour ladle, impurity can reduce the mobility of powder, affect the smooth degree of selective laser fusing forming process middle berth powder, the microstructure of SLM formation of parts and mechanical property are also had a negative impact simultaneously.Preparation method of the present invention using Inconel625 nickel-base alloy bar as consutrode, directly carry out induction melting, greatly reduce the introducing of nonmetallic inclusion, avoid because impurity mixes the adverse effect caused selective laser melt-forming process and final part performance.
In preparation method of the present invention, another innovative point of atomization flow process is, while adopting vacuum electrode induction melting technology, combine ultrasonic close coupling atomization technique, make argon gas obtain supersonic airstream under less atomizing pressure, alloy liquid droplet, under powerful gas shock effect, not only easily forms more tiny drop, and the inter-adhesive probability forming " satellite ball " particle together of drop reduces greatly, ensures that particle has very high sphericity.Because cooling velocity is fast, the Inconel625 Co-based alloy powder granularity obtained after solidifying is more even, tiny, substantially increases atomization rates simultaneously, reduces the production cost of atomization.
Accompanying drawing explanation
Fig. 1 is structural representation after the processing of Inconel625 nickel-base alloy bar;
Fig. 2 is the grain size distribution of the Inconel625 Co-based alloy powder particle that embodiment 1 obtains;
Fig. 3 is the shape appearance figure of the Inconel625 Co-based alloy powder particle that embodiment 1 obtains;
Fig. 4 is the shape appearance figure of the Inconel625 Co-based alloy powder particle that embodiment 2 obtains;
Fig. 5 is the shape appearance figure of the Inconel625 Co-based alloy powder particle that embodiment 3 obtains.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Embodiment 1
For the preparation method of the Inconel625 Co-based alloy powder of selective laser smelting technology, comprise the following steps:
(1) smelt: Inconel625 nickel-base alloy raw material is added vacuum induction furnace smelting, and smelting temperature controls at 1450 DEG C, obtained Inconel625 nickel-base alloy bar after smelting, alloying component ratio is: Ni:62%, Cr:22%, Mo:9%, Nb:4.0%, Fe:2.5%, Al :≤0.4%, Ti :≤0.4%, Mn :≤0.5%, Si :≤0.5%, C :≤0.1%, P :≤0.015%, S :≤0.015%;
(2) process: cylindrical bar Inconel625 nickel-base alloy bar being processed into band cone angle according to Fig. 1 structure, angle of taper is 80 °;
(3) be atomized: vacuum electrode induction melting is carried out to the Inconel625 nickel-base alloy bar after processing, the decrease speed of bar controls at 20mm/min, after fusing the supersonic airstream that the molten drop of drippage ejects at close-coupled nozzle impact under, atomization forms fine droplets, atomization gas adopts high-purity argon gas, atomization air pressure 3.0MPa, drop is rapidly solidificated into Inconel625 Co-based alloy powder under the cooling of inert gas;
(4) sieve: divide carrying out ultrasonic vibrating screen after the Inconel625 Co-based alloy powder cooling of collecting after atomization, remove the particle of particle diameter >=60 μm, then air current classifying is carried out to the particle that residue particle diameter is 0 ~ 60 μm, account for 20% according to particle diameter 0 ~ 15 μm, particle diameter 15 ~ 30 μm accounts for 30%, 30 ~ 45 μm and account for 30%, 45 ~ 60 μm of part by weight relations accounting for 20% and carry out proportioning, finally obtain the Inconel625 Co-based alloy powder for selective laser smelting technology.
As shown in Figure 2, pattern as shown in Figure 3 for the Inconel625 Co-based alloy powder particle size distribution that the present embodiment prepares.Oxygen content is 0.04% after testing, average grain diameter 35.79 μm, sphericity 0.81, apparent density 4.473g/cm3, it is shaping that powder carries out part SLM on EOS M280 equipment, and in paving powder process, powder flowbility is good, process is without " nodularization " phenomenon, little, the uniform texture of part deformation that selective laser fusing is shaped, the maximum tensile strength can more than 750MPa, can meet the instructions for use of part.
Embodiment 2
For the preparation method of the Inconel625 Co-based alloy powder of selective laser smelting technology, comprise the following steps:
(1) smelt: Inconel625 nickel-base alloy raw material is added vacuum induction furnace smelting, and smelting temperature controls at 1500 DEG C, obtained Inconel625 nickel-base alloy bar after smelting, described alloying component ratio is: Ni:62%, Cr:22%, Mo:9%, Nb:3.6%, Fe:3.5%, Al :≤0.4%, Ti :≤0.4%, Mn :≤0.5%, Si :≤0.5%, C :≤0.1%, P :≤0.015%, S :≤0.015%;
(2) process: cylindrical bar Inconel625 nickel-base alloy bar being processed into band cone angle according to accompanying drawing 1, angle of taper is 75 °;
(3) be atomized: vacuum electrode induction melting is carried out to the Inconel625 nickel-base alloy bar after processing, the decrease speed of bar controls at 30mm/min, the supersonic gas that after fusing, the molten drop of drippage ejects at close-coupled nozzle flows down, atomization forms fine droplets, atomization gas adopts high-purity argon gas, atomization air pressure 4.0MPa, drop is rapidly solidificated into Inconel625 Co-based alloy powder under the cooling of inert gas;
(4) sieve: divide carrying out ultrasonic vibrating screen after the Inconel625 Co-based alloy powder cooling of collecting after atomization, remove the particle of particle diameter >=60 μm, then air current classifying is carried out to the particle that residue particle diameter is 0 ~ 60 μm, account for 15% according to particle diameter 0 ~ 15 μm, particle diameter 15 ~ 30 μm accounts for 35%, 30 ~ 45 μm and account for 25%, 45 ~ 60 μm of part by weight relations accounting for 15% and carry out proportioning, finally obtain the Inconel625 Co-based alloy powder being applicable to selective laser smelting technology.
The Inconel625 Co-based alloy powder granule-morphology that the present embodiment prepares as shown in Figure 4, oxygen content is 0.02% after testing, average grain diameter 30.52 μm, sphericity 0.87, apparent density 4.308g/cm3, it is shaping that powder carries out part SLM on Renishaw AM250 equipment, and powder conveying uniform, without splash phenomena, the part pore-free that selective laser fusing is shaped, the defect such as loose, dimensional accuracy is high, and the maximum tensile strength can more than 820MPa, can meet the instructions for use of part.
Embodiment 3
For the preparation method of the Inconel625 Co-based alloy powder of selective laser smelting technology, comprise the following steps:
(1) smelt: Inconel625 nickel-base alloy raw material is added vacuum induction furnace smelting, and smelting temperature controls at 1550 DEG C, smelt obtained Inconel625 nickel-base alloy bar, described alloying component ratio is: Ni:62%, Cr:22%, Mo:9%, Nb:3.2%, Fe:4.5%, Al :≤0.4%, Ti :≤0.4%, Mn :≤0.5%, Si :≤0.5%, C :≤0.1%, P :≤0.015%, S :≤0.015%;
(2) process: cylindrical bar Inconel625 nickel-base alloy bar being processed into band cone angle according to accompanying drawing 1, angle of taper is 90 °;
(3) be atomized: vacuum electrode induction melting is carried out to the Inconel625 nickel-base alloy bar after processing, the decrease speed of bar controls at 40mm/min, the supersonic gas that after fusing, the molten drop of drippage ejects at close-coupled nozzle flows down, atomization forms fine droplets, atomization gas adopts high-purity argon gas, atomization air pressure 4.3MPa, molten drop is rapidly solidificated into Inconel625 Co-based alloy powder under the cooling of inert gas;
(4) sieve: divide carrying out ultrasonic vibrating screen after the Inconel625 Co-based alloy powder cooling of collecting after atomization, remove the particle of particle diameter >=60 μm, then air current classifying is carried out to the particle that residue particle diameter is 0 ~ 60 μm, account for 10% according to particle diameter 0 ~ 15 μm, particle diameter 15 ~ 30 μm accounts for 40%, 30 ~ 45 μm and account for 40%, 45 ~ 60 μm of part by weight relations accounting for 10% and carry out proportioning, finally obtain the Inconel625 Co-based alloy powder being applicable to selective laser smelting technology.
The Inconel625 Co-based alloy powder granule-morphology that the present embodiment prepares as shown in Figure 5, oxygen content is 0.01% after testing, average grain diameter 28.32 μm, sphericity 0.92, apparent density 4.253g/cm3, it is shaping that powder carries out part SLM on SLMsolutions 280HL equipment, powder conveying is smooth, the part dense structure that selective laser fusing is shaped, be out of shape little, the maximum tensile strength can more than 910MPa, can meet the instructions for use of part.
Above-mentioned is can understand and use invention for ease of those skilled in the art to the description of embodiment.Person skilled in the art obviously easily can make various amendment to these embodiments, and General Principle described herein is applied in other embodiments and need not through performing creative labour.Therefore, the invention is not restricted to above-described embodiment, those skilled in the art, according to announcement of the present invention, do not depart from improvement that scope makes and amendment all should within protection scope of the present invention.

Claims (8)

1., for a preparation method for the Inconel625 Co-based alloy powder of selective laser smelting technology, it is characterized in that, comprise the following steps:
(1) alloy smelting: Inconel625 nickel-base alloy raw material is added vacuum induction furnace smelting, obtained Inconel625 nickel-base alloy bar after smelting;
(2) bar processing: cylindrical bar Inconel625 nickel-base alloy bar being processed into band cone angle;
(3) powder by atomization: vacuum electrode induction melting is carried out to the Inconel625 nickel-base alloy bar of completion of processing, under the impact of the supersonic atomization medium that molten metal drop ejects at close-coupled nozzle, atomization formed fine droplets, drop in flight course by being rapidly solidificated into Inconel625 Co-based alloy powder under the cooling of atomizing medium;
(4) proportioning is sieved: divide carrying out ultrasonic vibrating screen after the Inconel625 Co-based alloy powder cooling of collecting after atomization, remove the particle of particle diameter >=60 μm, then air current classifying is carried out to the particle that residue particle diameter is 0 ~ 60 μm, account for 10 ~ 20% according to particle diameter 0 ~ 15 μm, particle diameter 15 ~ 30 μm accounts for 20 ~ 50%, 30 ~ 45 μm and account for 20 ~ 50%, 45 ~ 60 μm of part by weight relations accounting for 10 ~ 20% and carry out proportioning, finally obtain the Inconel625 Co-based alloy powder being applicable to selective laser smelting technology.
2. the preparation method of a kind of Inconel625 Co-based alloy powder for selective laser smelting technology according to claim 1, it is characterized in that, in step (1), described Inconel625 nickel-base alloy raw alloy component ratio is: Ni: >=58%, Cr:20 ~ 23%, Mo:8 ~ 10%, Nb:3.15 ~ 4.15%, Fe :≤5%, Al :≤0.4%, Ti :≤0.4%, Mn :≤0.5%, Si :≤0.5%, C :≤0.1%, P :≤0.015%, S :≤0.015%.
3. the preparation method of a kind of Inconel625 Co-based alloy powder for selective laser smelting technology according to claim 1, is characterized in that, in step (1), smelting temperature controls at 1400 ~ 1600 DEG C.
4. the preparation method of a kind of Inconel625 Co-based alloy powder for selective laser smelting technology according to claim 1, is characterized in that, in step (2), described angle of taper is 75 ~ 90 °.
5. the preparation method of a kind of Inconel625 Co-based alloy powder for selective laser smelting technology according to claim 1, it is characterized in that, when carrying out vacuum electrode induction melting in step (3), the decrease speed of bar controls at 10 ~ 50mm/min.
6. the preparation method of a kind of Inconel625 Co-based alloy powder for selective laser smelting technology according to claim 1, is characterized in that, in step (3), the nozzle exit pressure of close-coupled nozzle is 1.0 ~ 5.0MPa.
7. the preparation method of a kind of Inconel625 Co-based alloy powder for selective laser smelting technology according to claim 1, is characterized in that, the atomizing medium described in step (3) adopts high-purity argon gas or high pure nitrogen.
8. the preparation method of a kind of Inconel625 Co-based alloy powder for selective laser smelting technology according to claim 1, is characterized in that, in step (4), the gas medium of air current classifying adopts nitrogen or argon gas.
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