CN106623959A - Preparation method of Waspalloy spherical powder for additive manufacturing - Google Patents

Preparation method of Waspalloy spherical powder for additive manufacturing Download PDF

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Publication number
CN106623959A
CN106623959A CN201611174420.7A CN201611174420A CN106623959A CN 106623959 A CN106623959 A CN 106623959A CN 201611174420 A CN201611174420 A CN 201611174420A CN 106623959 A CN106623959 A CN 106623959A
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waspalloy
powder
alloy
preparation
spherical
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赵霄昊
王�琦
张梅
徐伟
王庆相
梁书锦
张平祥
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XI'AN OUZHONG MATERIAL TECHNOLOGY Co Ltd
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XI'AN OUZHONG MATERIAL TECHNOLOGY Co Ltd
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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
    • B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
    • 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
    • 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
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
    • C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
    • C22C19/055—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 20% but less than 30%
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
    • C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
    • C22C19/056—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 10% but less than 20%

Abstract

A preparation method of Waspalloy spherical powder for additive manufacturing includes the steps of conducting alloy component compounding according to AMS 5706 standards and subjecting master ingots to vacuum melting twice; producing the master ingots into alloy electrode bars by means of forging and machining; subjecting an atomizing unit to pre-vacuum-pumping treatment, and feeding the atomizing unit with mixed inert protective gas; feeding the electrode bars into an atomizing chamber by a feeding system, heating electrode bar end faces by a plasma torch, preparing metal liquid droplets under the centrifugal action of a rotating electrode, and making the metal liquid droplets form spherical metal powder by flash setting; using a powder collecting device comprising an electrostatic separation component for removing inclusions of the spherical metal powder and collecting purified powder. The preparation method has the advantages of high production efficiency, high batch stability and high -270-mesh powder yield and can be used for easily preparing the Waspalloy spherical powder high in purity, sphericity and fluidity.

Description

A kind of increasing material manufacturing preparation method of Waspalloy spherical powders
Technical field
The invention belongs to metal and alloy powder preparing technical field, more particularly to a kind of increasing material manufacturing Waspalloy The preparation method of spherical powder.
Background technology
Waspalloy alloys are a kind of precipitation strength type high temperature alloys that element is need to strengthen based on Cr, Co, Mo, 650 Below DEG C, Waspalloy alloys have the performances such as resistance to lasting, antifatigue, anti-oxidant and resisting chloride ion penetration stress corrosion cracking (SCC), the conjunction Gold is mainly used in the structure members such as gas-turbine unit, nuclear-plant, aerospace engine and nuclear reactor.
In recent years, with laser powdering（SLM）, laser powder feeding（DED）, electron beam powdering（EBM）Deng metal increasing material manufacturing The continuous development of technology, Waspalloy from traditional forging high-temperature alloy be gradually developed to new powder metallurgy superalloy from And alloy property, expanded application scope are improved, market increases year by year the demand of metal dust.Using increases material manufacturing technology system Standby Waspalloy alloy components, are not only easy to obtain that microstructure is uniform, crystal grain is tiny, complex geometry parts, and And stock utilization can be significantly improved, it is prevented effectively from the high-power forging equipment and precision die for manufacturing and designing costliness.
At present, the production method of spherical powder mainly has inert gas atomizer method, radio frequency plasma spheroidizing of powder to process Method and plasma atomization etc..Wherein, gas atomization is to melt foundry alloy, high pressure, the height for recycling atomizer to produce Fast inert gas flow impact metallic solution forms droplet, and after Jing false sets obtain alloy powder.Gas atomization technique one Aspect has the advantages that production efficiency height, powder size wide scope, sphericity are preferable etc. and is easily achieved large-scale production, another Easily there is the powder such as hollow powder and satellite powder proportion are higher, powder flowbility is poor, degree of purity is limited in aspect powder product Last mass defect, therefore gas atomization is not suitable for the high Waspalloy alloy powders of large-scale production alloying level.Radio frequency Plasma atomization carries out secondary fusion to aspherical powder and using surface tension and high-temperature with irregular alloyed powder as raw material Molten drop is condensed into spheric granules by gradient.Powder prepared by the method has sphericity height, any surface finish, impurity content low excellent Point, but the technique exist low production efficiency, twice powder cycle length processed, equipment operation and maintenance cost it is high the shortcomings of.Plasma Atomization realizes that foundry alloy melting and powder by atomization are synchronously completed using superhigh temperature beam-plasma, and the mesh powder of gained powder -270 is received Yield is high, powder high purity.But Waspalloy metal wire material of the technique with diameter less than 5mm causes raw material as raw material Production difficulty and purchase cost significantly improve.
Therefore, it is extensive, the inexpensive production that solves the problems, such as super clean, high-quality Waspalloy alloy spherical powder, Other Waspalloy alloy powders preparation technology institute produced problem, the present invention is avoided to propose a kind of using plasma rotation The method that electrode method prepares Waspalloy alloy spherical powder.
The content of the invention
To overcome above-mentioned the deficiencies in the prior art, it is an object of the invention to provide a kind of adopt plasma rotating electrode process system The method of standby Waspalloy alloy spherical powder, solves lacking for above-mentioned Waspalloy alloy sphericals powder technology of preparing presence Point, and a kind of preparation of the Waspalloy alloy spherical powder that good fluidity, high purity, particle diameter are tiny, sphericity is high is provided Method, for meeting the market demand of various metals increases material manufacturing technology.
The present invention with meet the chemical composition of standard AMS 5706 requirement Waspalloy alloy bar materials as raw material, by sending Bar is sent into forvacuum and is filled with the spray chamber of high purity inert gas protection by material system；Using high-temperature plasma arc by height The cylindrical alloy bar of speed rotation progressively melts, and puddle is got rid of under the action of the centrifugal force molten drop, and drop is lazy Property gaseous environment in cooling and solidifying be spherical powder, Jing container bottoms enter rewinding tank.
For achieving the above object, the technical solution used in the present invention is：A kind of increasing material manufacturing Waspalloy spherical powders Preparation method, it is characterised in that comprise the following steps：
1）Dispensing is carried out according to composition needed for the alloy of standard AMS 5706 and obtains founding raw material, carry out a vacuum induction melting, The surface scale of melting once is removed, secondary vacuum consumable remelting is carried out, relative density is obtained more than 85% Waspalloy foundry alloy secondary smelting ingot shape blanks；
2）By step 1）Waspalloy foundry alloy secondary smelting ingot shape blank forgings obtain Waspalloy alloy bar materials, Jing Guoche Bed and precise NC lathe obtain meeting the Waspalloy alloys electricity of plasma rotating electrode process requirement after being machined Pole rod；
3）Waspalloy alloy electrode rods are placed in atomization plant, a whole set of powder manufacturing apparatus forvacuum is processed, be filled with lazy Property protective gas；
4）Atomization plant is opened, Waspalloy alloy electrode plane rod ends is heated using plasma torch so as to melt, in atomization Interior carries out centrifugal atomizing powder；
5）Super clean Waspalloy alloy spherical powder is obtained by powder collection device, powder size between 15-200 μm, Sieve on request and vacuum bulk packing after powder is cooled down completely.
The founding raw material includes following components：It is by weight percentage, the Cr of 18-21%, the Co of 12-15%, 3.5- The Ti of the Al of 5.0% Mo, 1.2-1.6%, 2.75--3.25%；Trace element C≤0.1%, Fe≤2%, Mn≤0.1%, S≤ 0.015%, P≤0.015%, Si≤0.15%, Cu≤0.1%, the B of 0.003-0.010%, the Zr of 0.020-0.080%, remaining is Ni。
Step 1）Described vacuum induction melting and the vacuum of vacuum consumable remelting is not less than 1 × 10-1 Pa.
Described Waspalloy alloy bar materials consistency is more than 99%, a diameter of without casting flaws such as obvious loose, shrinkage cavities 10-90mm, length is 100-900mm, and surface roughness Ra is not more than 3.2 μm.
The forvacuum process step includes：Vacuumized using the pump housing, treated that equipment vacuum degree reaches 1 × 10-3 Pa-10×10-3During Pa, the mixed inert protective gas of argon gas and helium composition is filled with, the pressure in equipment is 0.1 × 105-3 ×105Pa, the mass percent of atmosphere oxygen content is less than 0.01%.
The step 4）In spray chamber inner wall smooth, surface roughness be less than 1.6 μm.
The Waspalloy alloy electrodes rod rotating speed is 10000-30000 rev/min, and Waspalloy alloy electrode rods enter It is 1-10 mm/seconds to amount, between plasma gun power 100-400 kW.
The step 5）Waspalloy alloy sphericals powder collect process carry out under an inert atmosphere, treat Waspalloy Alloy spherical powder is sealed after cooling down completely and accesses electrostatic and goes to be mingled with equipment.
The step 5）Spherical metal powder screening and vacuum bulk packing carry out under inert gas shielding, inertia Gas is the mixed gas that argon gas and helium are constituted.
The beneficial effects of the present invention is：
1) using the plasma arc melting technology of non-diverting formula, realize that Waspalloy alloys are quick, pure fusing, be not used molten Change crucible, effectively reduce the introducing of impurity element.Using electrode bar progressively amount of feeding control technology, different batches are ensure that Powder quality stability and uniformity, it is easy to extensive repeatability production.
2) using ultracentrifugation atomization technique, the production efficiency and -270 mesh of Waspalloy alloy powders is significantly improved Powder yield, has the advantages that sphericity is high, impurity content is low, good fluidity, and effectively reduces satellite powder and hollow powder Formed, improve powder product rate, be particularly suitable as the raw material of metal increasing material manufacturing and heat and other static pressuring processes.
3) using argon gas and the mixed inert protective gas of helium, metal dust oxygen content can be effectively reduced, improves gold Category powder freezing rate, reduces the microscopic segregation of metal dust chemical composition, it is ensured that spherical metal powder chemical composition uniformity.
Description of the drawings
Fig. 1 is the equipment schematic diagram of PREP legal system powder of the present invention.
Wherein, 1 is inert protective gas spray chamber；2 is that electrode bar installs room；3 is the collection that electrostatic separation and powder are collected Into device；4 is plasma rotation negative electrode；5 is electrode bar feed system.
Fig. 2 is Waspalloy alloy spherical powder low power SEM microscopic appearance figures prepared by the present invention.
Fig. 3 is Waspalloy alloy spherical powder high power SEM microscopic appearance figures prepared by the present invention.
Fig. 4 is Waspalloy alloy spherical powder high power metallurgical microstructrue figures prepared by the present invention.
Specific embodiment
The present invention is described in further detail with reference to specific embodiments and the drawings.
Embodiment 1：A kind of increasing material manufacturing preparation method of Waspalloy spherical powders, comprises the following steps：
Adopt the mass percent of essential element for：Cr-18.3%, Co-12.5%, Mo-3.8%, Al-1.2%, Ti-2.8%, Fe-0.5%, Mn-0.03%, S-0.007%, P-0.006%, Si-0.08%, Cu-0.03%, B-0.004%, Zr-0.03%, C- 0.003%, Ni- surplus is balanced, and raw material is placed in the vaccum sensitive stove that vacuum is 0.1 Pa carries out melting once；Remove one The surface scale of secondary melting, carries out secondary vacuum consumable remelting, and vacuum is that to obtain relative density be 95% to 0.05 Pa Waspalloy foundry alloy secondary smelting ingot shape blanks；
The Waspalloy alloy bar materials that consistency is 99.6%, and Jing lathes and precise NC lathe are obtained by isothermal open die forging Be machined into a diameter of 75mm, length for 850mm Waspalloy alloy electrode rods；
Waspalloy alloy electrode rods are placed in into electrode bar to install in room 2, and it is true to taking out in inert protective gas spray chamber 1 Sky, treats that equipment vacuum degree reaches 1 × 10-3Argon, helium mixed inert gas are filled with during Pa, in equipment inert gas pressure be 0.3 × 105Pa；
Open atomization plant and prepare spherical powder, the plasma torch for rotating negative electrode 4 and the generation of electrode bar 5 using plasma adds Hot Waspalloy alloy electrodes plane rod end so as to melt, in inert protective gas spray chamber 1 centrifugal atomizing powder is carried out, electricity Pole rod rotating speed is 15000 revs/min, and the electrode bar amount of feeding is 1mm/s；
Gained super clean Waspalloy alloy sphericals powder removed by electrostatic separation part and received into powder after nonmetal inclusion Collection tank 3, sieves on request and vacuum bulk packing after powder is cooled down completely.
Jing test analysis understand that Waspalloy alloy sphericals powder average particle size is 95 μm, and wherein D10 is 68 microns, D50 is 95 microns, and D90 is 124 microns. oxygen content in power is 500 ppm, and inclusion content is less than 10/kg, Waspalloy Alloy powder good sphericity, surface smoothness is high, substantially eliminates satellite powder and hollow powder phenomenon, and Fig. 2 show gained powder Secondary electron image.
Embodiment 2：The preparation of Waspalloy alloy spherical powder
Adopt the quality proportioning of essential element for：Cr-19.8%, Co-13.5%, Mo-4.4%, Al-1.4%, Ti-2.98%, Fe- 1.3%, Mn-0.6%, S-0.011%, P-0.0010%, Si-0.12%, Cu-0.07%, B-0.007%, Zr-0.05%, C-0.006%, Ni- surpluses are balanced, and raw material is placed in the vaccum sensitive stove that vacuum is 0.05 Pa carries out melting once；Remove melting once Surface scale, carry out secondary vacuum consumable remelting, vacuum obtains the Waspalloy that relative density is 91% for 0.01Pa Foundry alloy secondary smelting ingot shape blank；
By Waspalloy foundry alloy secondary smelting ingot shape blanks, it is 99.5% to obtain consistency by isothermal open die forging Waspalloy alloy bar materials, and a diameter of 85mm is processed into, length is the Waspalloy alloy electrode rods of 500mm；
Alloy electrode is placed in into electrode bar to install in room 2, and to vacuumizing in inert protective gas spray chamber 1, treats equipment vacuum Degree reaches 3 × 10-3Argon, helium mixed inert gas are filled with during Pa, inert gas pressure is 1.8 × 10 in equipment5Pa；
Open atomization plant and prepare spherical powder, the plasma torch for rotating negative electrode 4 and the generation of electrode bar 5 using plasma adds Hot Waspalloy alloy electrodes plane rod end so as to which end face melts, in inert protective gas spray chamber 1 centrifugal atomizing system is carried out Powder, Waspalloy alloy electrode rods rotating speed is 22000 revs/min, and the electrode bar amount of feeding is 3mm/s；
Gained super clean Waspalloy alloy sphericals powder removed by electrostatic separation part and received into powder after nonmetal inclusion Collection tank 3, sieves on request and vacuum bulk packing after super clean Waspalloy alloy spherical powder is cooled down completely.
Jing test analysis understand that Waspalloy alloy sphericals powder average particle size is 59 μm, and wherein D10 is 34 microns, D50 is 59 microns, and D90 is 78 microns.Oxygen content in power is 600 ppm, and inclusion content is less than 10/kg, Waspalloy Alloy powder good sphericity, surface smoothness is high, satellite powder and hollow powder phenomenon is substantially eliminated, shown in Fig. 3.
Embodiment 3
Adopt the quality proportioning of essential element for：Cr-20.7%, Co-14.9%, Mo-4.7%, Al-1.6%, Ti-3.16%, Fe- 1.8%, Mn-0.9%, S-0.015%, P-0.0013%, Si-0.14%, Cu-0.10%, B-0.009%, Zr-0.08%, C-0.009%, Ni- surpluses are balanced, and raw material is placed in the vaccum sensitive stove that vacuum is 0.05 Pa carries out melting once；Remove melting once Surface scale, carry out secondary vacuum consumable remelting, vacuum obtains the Waspalloy that relative density is 91% for 0.01Pa Foundry alloy secondary smelting ingot shape blank；
By Waspalloy foundry alloy secondary smelting ingot shape blanks, it is 99.5% to obtain consistency by isothermal open die forging Waspalloy alloy bar materials, and a diameter of 10mm is processed into, length is the Waspalloy alloy electrode rods of 100mm；
Alloy electrode is placed in into electrode bar to install in room 2, and to vacuumizing in inert protective gas spray chamber 1, treats equipment vacuum Degree reaches 9 × 10-3Argon, helium mixed inert gas are filled with during Pa, inert gas pressure is 2.6 × 10 in equipment5Pa；
Open atomization plant and prepare spherical powder, the plasma torch for rotating negative electrode 4 and the generation of electrode bar 5 using plasma adds Hot Waspalloy alloy electrodes plane rod end so as to which end face melts, in inert protective gas spray chamber 1 centrifugal atomizing system is carried out Powder, Waspalloy alloy electrode rods rotating speed is 30000 revs/min, and the electrode bar amount of feeding is 3mm/s；
Gained super clean Waspalloy alloy sphericals powder removed by electrostatic separation part and received into powder after nonmetal inclusion Collection tank 3, sieves on request and vacuum bulk packing after super clean Waspalloy alloy spherical powder is cooled down completely.

Claims (9)

1. a kind of increasing material manufacturing preparation method of Waspalloy spherical powders, it is characterised in that comprise the following steps：
1）Dispensing is carried out according to composition needed for the alloy of standard AMS 5706 and obtains founding raw material, carry out a vacuum induction melting, The surface scale of melting once is removed, secondary vacuum consumable remelting is carried out, relative density is obtained more than 85% Waspalloy foundry alloy secondary smelting ingot shape blanks；
2）By step 1）Waspalloy foundry alloy secondary smelting ingot shape blank forgings obtain Waspalloy alloy bar materials, Jing Guoji Tool is processed, and obtains meeting the Waspalloy alloy electrode rods of plasma rotating electrode process requirement；
3）Waspalloy alloy electrode rods are placed in atomization plant, a whole set of powder manufacturing apparatus forvacuum is processed, be filled with lazy Property protective gas；
4）Atomization plant is opened, Waspalloy alloy electrode plane rod ends is heated using plasma torch so as to melt, in atomization Interior carries out centrifugal atomizing powder；
5）Super clean Waspalloy alloy spherical powder is obtained by powder collection device, powder size between 15-200 μm, Sieve on request and vacuum bulk packing after powder is cooled down completely.
2. a kind of increasing material manufacturing according to claim 1 preparation method of Waspalloy spherical powders, its feature exists In the founding raw material includes following components：It is by weight percentage, the Cr of 18-21%, the Co of 12-15%, 3.5-5.0%'s The Ti of the Al of Mo, 1.2-1.6%, 2.75--3.25%；Trace element C≤0.1%, Fe≤2%, Mn≤0.1%, S≤0.015%, P≤ 0.015%, Si≤0.15%, Cu≤0.1%, the B of 0.003-0.010%, the Zr of 0.020-0.080%, remaining is Ni.
3. a kind of increasing material manufacturing according to claim 1 preparation method of Waspalloy spherical powders, its feature exists In step 1）Described vacuum induction melting and the vacuum of vacuum consumable remelting is not less than 1 × 10-1 Pa。
4. a kind of increasing material manufacturing according to claim 1 preparation method of Waspalloy spherical powders, its feature exists In described Waspalloy alloy bar materials consistency is more than 99%, without the casting flaws such as obvious loose, shrinkage cavity, a diameter of 10- 90mm, length is 100-900mm, and surface roughness Ra is not more than 3.2 μm.
5. a kind of increasing material manufacturing according to claim 1 preparation method of Waspalloy spherical powders, its feature exists In the forvacuum process step includes：Vacuumized using the pump housing, treated that equipment vacuum degree reaches 1 × 10-3 Pa-10 During × 10-3Pa, the mixed inert protective gas of argon gas and helium composition is filled with, the pressure in equipment is 0.1 × 105-3 × 105 Pa, the mass percent of atmosphere oxygen content is less than 0.01%.
6. a kind of increasing material manufacturing according to claim 1 preparation method of Waspalloy spherical powders, its feature exists In the spray chamber inner wall smooth, surface roughness is less than 1.6 μm.
7. a kind of increasing material manufacturing according to claim 1 preparation method of Waspalloy spherical powders, its feature exists In the Waspalloy alloy electrodes rod rotating speed is 10000-30000 rev/min, the Waspalloy alloy electrode rod amount of feeding For 1-10 mm/seconds, between plasma gun power 100-400 kW.
8. a kind of increasing material manufacturing according to claim 1 preparation method of Waspalloy spherical powders, its feature exists In the step 5）Waspalloy alloy sphericals powder collect process carry out under an inert atmosphere, treat Waspalloy alloys Spherical powder is sealed after cooling down completely and accesses electrostatic and goes to be mingled with equipment.
9. a kind of increasing material manufacturing according to claim 1 preparation method of Waspalloy spherical powders, its feature exists In the step 5）Spherical metal powder screening and vacuum bulk packing carry out under inert gas shielding, inert gas For the mixed gas that argon gas and helium are constituted.
CN201611174420.7A 2016-12-19 2016-12-19 Preparation method of Waspalloy spherical powder for additive manufacturing Pending CN106623959A (en)

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