CN113817935A - High-purity nickel-based high-temperature alloy and preparation method of spherical powder thereof - Google Patents

High-purity nickel-based high-temperature alloy and preparation method of spherical powder thereof Download PDF

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CN113817935A
CN113817935A CN202110949796.5A CN202110949796A CN113817935A CN 113817935 A CN113817935 A CN 113817935A CN 202110949796 A CN202110949796 A CN 202110949796A CN 113817935 A CN113817935 A CN 113817935A
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powder
purity
atomization
metal
smelting
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徐飞鹏
康凯
肖海波
范超
徐新浩
彭炜
张晓平
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Panxing New Alloy Material Changzhou Co ltd
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Panxing New Alloy Material Changzhou Co ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C19/00Alloys based on nickel or cobalt
    • C22C19/03Alloys based on nickel or cobalt based on nickel
    • C22C19/05Alloys based on nickel or cobalt based on nickel with chromium
    • C22C19/051Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
    • C22C19/056Alloys 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%
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
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    • B22F10/00Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/20Direct sintering or melting
    • B22F10/28Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/22Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
    • B22F3/225Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip by injection molding
    • BPERFORMING OPERATIONS; TRANSPORTING
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    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making 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
    • B22F9/082Making 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/14Making metallic powder or suspensions thereof using physical processes using electric discharge
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE 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
    • B33Y70/00Materials specially adapted for additive manufacturing
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • C22C1/023Alloys based on nickel
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C24/00Coating starting from inorganic powder
    • C23C24/08Coating starting from inorganic powder by application of heat or pressure and heat
    • C23C24/10Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
    • C23C24/103Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
    • C23C24/106Coating with metal alloys or metal elements only
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making 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
    • B22F9/082Making 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
    • B22F2009/0844Making 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making 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
    • B22F9/082Making 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
    • B22F2009/0896Making 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
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/25Process efficiency

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Abstract

The invention discloses a preparation method of high-purity nickel-based high-temperature alloy and spherical powder thereof, which comprises the steps of selecting high-purity metal ingredients, smelting in a vacuum induction suspension smelting furnace, realizing pure purification smelting by controlling parameters such as smelting vacuum degree, refining temperature, time and the like, and then pouring to obtain steel ingots to prepare bars; smelting and atomizing the bar material to prepare powder by EIGA and PREP technologies to obtain spherical metal powder; and classifying the spherical powder under the protection of inert gas by adopting vibration screening and airflow classification. The method effectively controls the content of non-metallic impurities through raw material smelting control, atomization process control and aftertreatment control, so that the powder chemical elements have extremely high purity, the high-purity high-temperature alloy spherical powder has the defects of difficult crack generation and the like in the subsequent laser additive printing and laser cladding processes, and the high-purity high-temperature alloy spherical powder has good binding force, high strength and good toughness and can be used for repairing high-end parts.

Description

High-purity nickel-based high-temperature alloy and preparation method of spherical powder thereof
Technical Field
The invention relates to the fields of laser cladding, additive manufacturing and high-end repair, in particular to a preparation method of spherical powder of a high-purity nickel-based superalloy.
Background
At present, the nickel-based superalloy manufacturing technology generally comprises the steps of performing induction melting on alloy raw materials, and then pouring the alloy raw materials into a die tube to prepare an alloy bar. The bar has many internal defects and more impurities, and also has the problem of loosening and dredging holes, and particularly, under the influence of various impurity elements such as C, P, S, Si, Mn, O, N, H and the like, the high-temperature processing performance and the comprehensive mechanical property of the bar are greatly influenced. In particular, oxygen and nitrogen, etc. which are harmful elements in the superalloy and are called residual gases, increase in the content of N causes both the high-temperature tensile strength and plasticity of the hot-corrosion-resistant superalloy to decrease, and the durability of the alloy to significantly decrease and the volatility to increase. Oxygen exists in the high-temperature alloy as trace impurity elements, and the oxygen mainly exists in a solid solution state and oxide inclusion. Oxygen present in solid solution has essentially no effect on the properties of the superalloy, but oxide inclusions are generally the initiation and propagation pathways for fatigue cracks. Therefore, it is important to control oxygen and nitrogen in the superalloy.
In the powder preparation stage, most of the traditional nickel-based high-temperature alloys adopt a vacuum induction melting VIGA method, the process adopts a melting crucible for bar material melting, after metal clear liquid is formed, the metal clear liquid is poured into a heat-preservation crucible, and under the condition of ensuring a certain superheat degree, the metal clear liquid is crushed by high-pressure gas through a guide pipe to form metal powder. The method can not ensure that a high-purity product is prepared, the molten metal can contact various basic oxide crucibles or refractory materials of other ceramic materials in the production process, and the non-metallic impurities can be washed into the metal powder by the molten metal in the atomization process to become the non-metallic impurities. Meanwhile, oxide impurities in the molten metal float on the upper layer after forming clear liquid, enter a tundish in the furnace pouring process to block a discharge spout, so that furnace blockage is caused, and the furnace forming rate is low; meanwhile, the high-temperature alloy powder prepared by gas atomization has the problems of high hollow powder rate, insufficient sphericity, cracking during final use, poor welding performance and the like.
Disclosure of Invention
The invention aims to solve the problems and provides a preparation method of a high-purity nickel-based high-temperature alloy and spherical powder thereof; the high-purity nickel-based high-temperature alloy prepared by the method has low impurity and few defects. The invention adopts a cold-wall suspension smelting mode, reduces the introduction of non-metallic impurities in the smelting stage, adopts EIGA and PREP technologies to prepare powder, has less powder hollow powder and high sphericity, performs post-treatment under the protection of argon, further controls the phenomenon of oxygen and nitrogen increase, and has lower product gas impurities.
The technical scheme of the invention is as follows:
the invention provides a high-purity nickel-based high-temperature alloy which comprises the following components in parts by weight: 0.005-0.015 part of C, 14.5-19 parts of Cr, 2.4-2.5 parts of Mo, 4-5.8 parts of Nb, 0.65-0.71 part of Ti, 1.4-1.5 parts of Al, 7-9.8 parts of Fe, 8.5-9 parts of Co, 0.8-1 part of W, 0.002-0.02 part of P, 50-61 parts of Ni, 0-0.0020 part of S, 0-0.05 part of Si, 0-0.002 part of Mg, 0-0.02 part of Mn, 0-0.05 part of Cu, 0-0.0009 part of O and 0-0.001 part of N; all of the elements are impurity elements, and the impurity content is required to be reduced. Especially oxygen and nitrogen as interstitial elements, the content is less than or equal to 10 ppm.
A preparation method of spherical powder of high-purity nickel-based superalloy comprises the following specific steps:
step 1: putting all the components into a vacuum induction suspension smelting furnace for alloy smelting, and pouring the alloy into an ingot mold pipe after the alloy smelting is finished to prepare an ingot;
step 2: processing the steel ingot to prepare a bar; the bending degree of the alloy bar is required to be less than 1 mm/bar.
And step 3: processing the bar into powder by adopting an EIGA gas atomization powder making furnace to obtain metal powder;
or step 3': and processing the bar into powder by using PREP plasma rotating electrode atomization powder manufacturing equipment to obtain metal powder.
Further, in the step 1, the diameter of the ingot mold tube is 40-70mm, and the length is 500-800 mm.
Furthermore, all the raw materials of the components in the step 1 are high-purity materials, including the purity of metal chromium is more than or equal to 99.9%, the purity of metal molybdenum is more than or equal to 99.9%, the purity of metal niobium is more than or equal to 99.9%, the purity of sponge titanium is more than or equal to 99.8%, the purity of aluminum is more than or equal to 99.9%, the purity of metal iron is more than or equal to 99.9%, the purity of metal cobalt is more than or equal to 99.9%, the purity of metal tungsten is more than or equal to 99.9%, the purity of metal nickel is more than or equal to 99.9%, and the purity of high-purity carbon particles is more than or equal to 99.7%; the vacuum degree is required to be less than 5Pa in the vacuum induction melting process, and the refining temperature is 1500-; the deoxidation capacity of carbon is improved by controlling the vacuum degree, the refining temperature and the refining time in the vacuum induction melting period, and the deoxidation and denitrification capacity of carbon under vacuum is enhanced along with the improvement of the vacuum degree.
Further, the step 2 specifically includes processing the steel ingot by using a lathe and a grinding machine to obtain a pre-alloy bar, and performing oil removal, chip removal and drying treatment on the pre-alloy bar.
Further, the step 3 specifically includes:
step 3-1, vacuumizing the EIGA gas atomization powder making furnace;
3-2, replacing the gas in the EIGA gas atomization powder making furnace by using inert gas;
and 3-3, smelting the bar by adopting an EIGA gas atomization powder making furnace to form metal liquid drops, then forming metal powder through atomization and solidification, and collecting the powder after the metal powder is cooled to room temperature.
Further, in step 3-1, vacuum is applied until the degree of vacuum is 1.0X 10-1Pa, the pressure rise rate is lower than 2 Pa/h; in the step 3-2, argon is adopted as inert gas, and the purity of the argon is 99.999 percent; 2-3 times of replacement; in step 3-3, the atomization parameters are set as follows: the atomization pressure is 3.0-5.0MPa, and the feeding speed is 30-80 mm/min; the smelting parameters are set as follows: the power is 20-30 Kw; the atomization adopts a free Laval supersonic atomization spray disk; the invention has high atomization efficiency and good product performance, the yield of the 15-53 mu m powder for selective laser additive manufacturing is more than 40 percent, and the powder fluidity is lower than 15 s.
Further, the step 3' specifically includes:
3-1', starting an electrode rotating motor of the PREP plasma rotating electrode atomization powder making equipment, and melting the bar by using a plasma gun to form metal droplets;
and 3-2', condensing the molten metal drops into spherical powder, and enabling the spherical powder to fall into a powder collecting system.
Further, in the step 3-1', the rotating speed of the bar is 10000-.
Further, in the powder making process of the step 3', inert protective gas is automatically charged and discharged, so that the inside of the PREP plasma rotating electrode atomization powder making equipment is always in a micro-positive pressure state, and the pressure range is 0.03-0.04 Ma.
Further, after step 3, the method further comprises: and 4, step 4: the metal powder is classified, and the classification comprises powder screening and powder airflow classification.
Further, powder screening and powder airflow classification are both carried out under the protection of high-purity 99.999% inert gas argon, namely, before operation, inert gas replacement treatment is respectively carried out on the rotary vibrating screen and the airflow classifier, and after 30min of replacement, the oxygen content in the equipment is lower than 10 ppm.
Further, explosion-proof treatment is carried out on a pneumatic feeding mode in the powder screening process, the pressure of the pneumatic feeding is 0.2-0.6MPa, the pendulum angle is 60-80 degrees, the ultrasonic mode is intermittent or continuous, and the powder is screened to obtain powder with the particle size section of +250 mu m, 150-250 mu m and 0-150 mu m; classifying the powder with the particle size of 0-150 μm by air flow, adjusting the frequency of a fan to be 30-50Hz, the feeding frequency to be 5-15Hz and the classification frequency to be 15-30Hz, classifying the powder into three sections of powder by screening and air flow classification through one-time feeding to obtain the powder with the particle size of 0-15 μm, 15-53 μm and 53-150 μm; the screening efficiency of the invention is more than 150kg/h, and the degree of automation is high; air flow classification, which is to classify the sieved particles to 0-150 μm to 0-15 μm, 15-53 μm and 53-150 μm. The graded particles with the diameter of 0-15 mu m can be used in the field of injection molding, the particles with the diameter of 15-53 mu m can be used in selective laser additive manufacturing, and the particles with the diameter of 53-150 mu m can be used in the fields of laser cladding and high-end repair.
The invention has the beneficial effects that:
according to the invention, high-purity metals such as Ni, Cr, Fe, Co and the like are selected as raw materials according to a proportion to be mixed to obtain a mixed alloy; through means such as raw material smelting control, atomization process control, aftertreatment control and the like, the content of non-metallic impurities such as C, P, S, Si, Mn, O, N, H and the like is effectively controlled, so that the powder chemical elements have extremely high purity, the high-purity high-temperature alloy is not easy to generate defects such as cracks in subsequent printing and laser cladding processes, the binding force is good, the strength is high, the toughness is good, and the high-temperature alloy can be used for additive manufacturing of complex high-temperature structural parts and repairing of high-end parts.
The invention adopts a vacuum induction suspension smelting mode to smelt the pre-alloy and the pre-alloy bar, which is beneficial to preparing the high-quality pre-alloy bar and controls impurity elements from source raw materials; the spherical powder for additive manufacturing is prepared by adopting an EIGA (enhanced inert gas) or PREP (pre-compaction press) technology, the production process is safer and more controllable, and the molten metal is not contacted with ceramics and refractory materials, so that foreign impurities are prevented from being introduced; under the state that powder is transported and the aftertreatment is all in inert gas protection, avoid transporting and introducing the xenogenesis impurity in the aftertreatment process, avoid the condition such as moisture absorption, oxidation to take place. The powder product prepared by the method has the advantages of uniform components, no segregation, low impurity content, good fluidity (less than 15s) and high apparent density (more than 4.9 g/cm)3)。
After the powder is subjected to laser cladding, no crack or fusion is found through fluorescence penetration detection, and the bonding force between the cladding layer and the base material is good, so that the powder is suitable for repairing high-end parts; after the powder is subjected to selective laser printing, the tensile strength at room temperature in the XYZ direction is greater than 1300MPa, the yield strength is greater than 1100MPa, the elongation after fracture is higher than 20%, and the room-temperature mechanical property is good. The tensile strength at high temperature of 650 ℃ is more than 1100MPa, the yield strength is more than 900MPa, the elongation is more than 22 percent, and the high-temperature mechanical property is good.
In the whole preparation process, the high-purity argon atmosphere is adopted to ensure atomization and grading, and the condition that oxygen absorption and nitrogen absorption occur in the atomization process of the molten metal to increase oxygen and nitrogen is more favorably ensured. Although the pressure rise rate of the atomizing furnace for production is less than 2Pa/h, the atomizing furnace is slightly pressurized in the atomizing process, so that certain mutual leakage between the argon in the furnace body and the air outside the furnace body still exists. Because the atomization and the smelting are carried out synchronously, the furnace body leaks to easily oxidize and nitrify the molten metal liquid, so that high-purity argon is selected, the water oxygen content in the argon is lower, and after the furnace body replacement is completed, a better protection effect is realized on the metal atomization process, so that the oxygen increase and the nitrogen increase of a product are controlled at a very low level. The same problem also occurs in the post-treatment process, the rotary vibrating screen, the airflow classifier and the glove box are not strictly vacuum equipment, but the powder product is micron-sized, has large surface area and is easy to generate the conditions of oxygen absorption, water absorption phenomenon to cause agglomeration or oxygen increase and the like, and the post-treatment by adopting high-purity 99.999 percent argon protection is favorable for controlling the powder performance.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
The above and other objects, features and advantages of the present invention will become more apparent by describing in more detail exemplary embodiments thereof with reference to the attached drawings, in which like reference numerals generally represent like parts throughout.
FIG. 1 is a schematic view of an ingot mould tube according to the invention.
FIG. 2 is a schematic diagram of the morphology of a PREP product according to the present invention.
FIG. 3 is a schematic representation of a pre-alloyed rod of the present invention.
Detailed Description
Preferred embodiments of the present invention will be described in more detail below with reference to the accompanying drawings. While the preferred embodiments of the present invention are shown in the drawings, it should be understood that the present invention may be embodied in various forms and should not be limited to the embodiments set forth herein.
Example 1
A high-purity nickel-based high-temperature alloy comprises the following components in parts by weight: 0.005 part of C, 14.5 parts of Cr, 2.4 parts of Mo, 4 parts of Nb, 0.65 part of Ti, 1.4 parts of Al, 7 parts of Fe, 8.5 parts of Co, 0.8 part of W, 0.002 part of P, 50 parts of Ni, 0.0020 part of S, 0.05 part of Si, 0.002 part of Mg, 0.02 part of Mn, 0.05 part of Cu, 0.0009 part of O and 0.001 part of N.
The preparation method of the high-purity nickel-based high-temperature alloy comprises the following steps:
step 1, preparing materials, wherein oxygen and nitrogen are used as interstitial elements, and the content of the oxygen and the nitrogen is less than or equal to 10 ppm; putting all the components into a vacuum induction suspension smelting furnace for alloy smelting, and pouring the components into an ingot mold pipe after the smelting is finished to prepare a steel ingot, wherein the diameter of the ingot mold pipe is 40-70mm, and the length of the ingot mold pipe is 500-800mm, as shown in figure 1;
step 2: processing the steel ingot by using a lathe and a grinding machine to obtain a pre-alloy bar, as shown in figure 3; carrying out oil removal, scrap removal and drying treatment on the prealloying bar;
and step 3: adopt EIGA gas atomization powder making stove to process the powder process to the rod, obtain metal powder, specifically include: step 3-1, vacuumizing the EIGA gas atomization powder making furnace until the vacuum degree is 1.0 multiplied by 10-1Pa, the pressure rise rate is lower than 2 Pa/h; 3-2, replacing the gas in the EIGA gas atomization powder making furnace by using inert gas; wherein, the inert gas adopts argon gas, and the purity of the argon gas is 99.999 percent; 2-3 times of replacement; step 3-3, adopting an EIGA gas atomization powder making furnace to smelt the bar to form metal liquid drops, and then carrying out atomization solidificationForming metal powder, and collecting the powder after the metal powder is cooled to room temperature; wherein, the atomization parameters are set as follows: the atomization pressure is 3.0-5.0MPa, and the feeding speed is 30-80 mm/min; the smelting parameters are set as follows: the power is 20-30 Kw; the atomization adopts a free Laval supersonic atomization spray disk, the atomization efficiency is high, the product performance is good, the yield of 15-53 mu m powder for selective laser additive manufacturing is more than 40%, and the powder fluidity is lower than 15 s;
and 4, step 4: classifying the metal powder, including powder screening and powder airflow classification;
powder screening and powder airflow classification are both carried out under the protection of high-purity 99.999% inert gas argon, namely, before operation, the rotary vibrating screen and the airflow classifier are respectively subjected to inert gas replacement treatment, and after 30min of replacement, the oxygen content in the equipment is lower than 10 ppm;
firstly, carrying out explosion-proof treatment on a pneumatic feeding mode in the powder screening process, wherein the pressure of the pneumatic feeding is 0.2-0.6MPa, the pendulum angle is 60-80 degrees, the ultrasonic mode is intermittent or continuous, and the particle size section of the powder obtained after the powder screening is +250 mu m, 150-250 mu m and 0-150 mu m; performing air flow classification on 0-150 mu m powder, adjusting the frequency of a fan to be 30-50Hz, the feeding frequency to be 5-15Hz and the classification frequency to be 15-30Hz, classifying the powder into three sections of powder by one-time feeding in the air flow classification of powder screening to obtain the powder with the particle size of 0-15 mu m, 15-53 mu m and 53-150 mu m, wherein the screening efficiency is more than 150kg/h and the degree of automation is high; the graded particles with the diameter of 0-15 mu m can be used in the field of injection molding, the particles with the diameter of 15-53 mu m can be used in selective laser additive manufacturing, and the particles with the diameter of 53-150 mu m can be used in the fields of laser cladding and high-end repair.
In the embodiment, high-purity metals such as Ni, Cr, Fe, Co and the like are selected as raw materials according to a proportion to be mixed to obtain a mixed alloy; through means such as raw material smelting control, atomization process control, aftertreatment control, the non-metallic impurity content has effectively been controlled for powdered chemical element has high purity, and high-purity superalloy is difficult for producing defects such as crackle in subsequent printing and laser cladding process, and the cohesion is good, and intensity is high, and toughness is good, can be used to the restoration of high-end part.
Example 2
According to the steps of the embodiment 1, wherein the step 3 adopts the step 3', the bar is processed and powdered by using a PREP plasma rotating electrode atomization powder manufacturing device, and metal powder is obtained, which specifically comprises the following steps:
3-1', starting an electrode rotating motor of the PREP plasma rotating electrode atomization powder making equipment, and melting the bar by using a plasma gun to form metal droplets; wherein the rotating speed of the bar is 10000-;
step 3-2', condensing the molten metal drops into spherical powder, and enabling the spherical powder to fall into a powder collecting system;
and 3 ', automatically charging and discharging inert protective gas in the powder making process in the step 3', so that the inside of the PREP plasma rotating electrode atomization powder making equipment is always in a micro-positive pressure state, and the pressure range is 0.03-0.04 Ma.
In the embodiment, the spherical powder for additive manufacturing is prepared by the PREP technology, the production process is safer and more controllable, and the molten metal is not in contact with ceramic and refractory materials, so that foreign impurities are prevented from being introduced; the powder product has the advantages of uniform components, no segregation, low impurity content, high sphericity, good fluidity (less than 15s) and high apparent density (more than 4.9g/cm 3).
Example 3
A high-purity nickel-based high-temperature alloy comprises the following components in parts by weight: 0.015 part of C, 19 parts of Cr, 2.5 parts of Mo, 5.8 parts of Nb, 0.71 part of Ti, 1.5 parts of Al, 9.8 parts of Fe, 9 parts of Co, 1 part of W, 0.02 part of P, 61 parts of Ni, 0.0020 part of S, 0.05 part of Si, 0.002 part of Mg, 0.02 part of Mn, 0.05 part of Cu, 0.0009 part of O and 0.001 part of N; the procedure was as in example 1.
Test example 1
The high-temperature alloy metal powders obtained in examples 1 to 3 of the present invention were subjected to index and performance tests, and the test results are shown in table 1:
TABLE 1 indices and Performance test results
Figure BDA0003217947250000091
In the embodiments 1, 2, and 3, after laser cladding of the finished powder, no crack is found and no fusion is found through fluorescence penetration detection, and the bonding force between the cladding layer and the substrate is good, so that the method is suitable for repairing high-end parts; after the powder is subjected to selective laser printing, the tensile strength at room temperature in the XYZ direction is greater than 1300MPa, the yield strength is greater than 1100MPa, the elongation after fracture is higher than 20%, and the room-temperature mechanical property is good. The tensile strength at high temperature of 650 ℃ is more than 1100MPa, the yield strength is more than 900MPa, the elongation is more than 22 percent, and the high-temperature mechanical property is good.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments.

Claims (10)

1. The high-purity nickel-based high-temperature alloy is characterized by comprising the following components in parts by weight:
0.005 to 0.015 part of C, 14.5 to 19 parts of Cr, 2.4 to 2.5 parts of Mo, 4 to 5.8 parts of Nb, 0.65 to 0.71 part of Ti, 1.4 to 1.5 parts of Al, 7 to 9.8 parts of Fe, 8.5 to 9 parts of Co, 0.8 to 1 part of W, 0.002 to 0.02 part of P, 50 to 61 parts of Ni, 0 to 0.0020 part of S, 0 to 0.05 part of Si, 0 to 0.002 part of Mg, 0 to 0.02 part of Mn, 0 to 0.05 part of Cu, 0 to 0.0009 part of O and 0 to 0.001 part of N.
2. A preparation method of spherical powder of high-purity nickel-based superalloy is characterized by comprising the following specific steps:
step 1: putting all the components into a vacuum induction suspension smelting furnace for alloy smelting, and pouring the alloy into an ingot mold pipe after the alloy smelting is finished to prepare an ingot;
step 2: processing the steel ingot to prepare a bar; the bending degree of the alloy bar is required to be less than 1 mm/bar.
And step 3: processing the bar into powder by adopting an EIGA gas atomization powder making furnace to obtain metal powder;
or step 3': and processing the bar into powder by using PREP plasma rotating electrode atomization powder manufacturing equipment to obtain metal powder.
3. The method for preparing spherical powder of high purity Ni-based superalloy as claimed in claim 2, wherein in step 1, the ingot mold tube has a diameter of 40-70mm and a length of 500-800 mm; all the raw materials are high-purity materials, including metal chromium with the purity of more than or equal to 99.9 percent, metal molybdenum with the purity of more than or equal to 99.9 percent, metal niobium with the purity of more than or equal to 99.9 percent, sponge titanium with the purity of more than or equal to 99.8 percent, aluminum with the purity of more than or equal to 99.9 percent, metal iron with the purity of more than or equal to 99.9 percent, metal cobalt with the purity of more than or equal to 99.9 percent, metal tungsten with the purity of more than or equal to 99.9 percent, metal nickel with the purity of more than or equal to 99.9 percent, and high-purity carbon particles with the purity of more than or equal to 99.7 percent; the vacuum degree is required to be less than 5Pa in the vacuum induction melting process, and the refining temperature is 1500-; the deoxidation and denitrification capabilities of the carbon under vacuum are enhanced along with the improvement of the vacuum degree by controlling the vacuum degree, the refining temperature and the refining time in the vacuum induction melting period;
and 2, specifically, processing the steel ingot by using a lathe and a grinding machine to obtain a pre-alloy bar, and performing oil removal, scrap removal and drying treatment on the pre-alloy bar.
4. The method for preparing spherical powder of high purity nickel-base superalloy according to claim 2, wherein step 3 specifically comprises:
step 3-1, vacuumizing the EIGA gas atomization powder making furnace;
3-2, replacing the gas in the EIGA gas atomization powder making furnace by using inert gas;
and 3-3, smelting the bar by adopting an EIGA gas atomization powder making furnace to form metal liquid drops, then forming metal powder through atomization and solidification, and collecting the powder after the metal powder is cooled to room temperature.
5. The high purity nickel-base superalloy sphere of claim 4A process for producing a shaped powder, characterized in that, in step 3-1, a vacuum is applied to a degree of vacuum of 1.0X 10-1Pa, the pressure rise rate of the atomization furnace is lower than 2 Pa/h; in the step 3-2, argon is adopted as inert gas, and the purity of the argon is 99.999 percent; 2-3 times of replacement; in step 3-3, the atomization parameters are set as follows: the atomization pressure is 3.0-5.0MPa, and the feeding speed is 30-80 mm/min; the smelting parameters are set as follows: the power is 20-30 Kw; the atomization adopts a free Laval supersonic atomization spray disk, the atomization efficiency is high, and the product performance is good.
6. The method for preparing spherical powder of high purity nickel-base superalloy according to claim 2, wherein step 3' comprises:
3-1', starting an electrode rotating motor of the PREP plasma rotating electrode atomization powder making equipment, and melting the bar by using a plasma gun to form metal droplets;
and 3-2', condensing the molten metal drops into spherical powder, and enabling the spherical powder to fall into a powder collecting system.
7. The method for preparing spherical powder of high purity Ni-based superalloy as claimed in claim 6, wherein in step 3-1', the rotation speed of the rod is 10000-.
8. The method for preparing spherical powder of high-purity nickel-base superalloy according to claim 6, wherein inert shielding gas is automatically charged and discharged during the milling process in step 3', so that the inside of the powder milling device with the PREP plasma rotating electrode atomization is always in a micro-positive pressure state, and the pressure range is 0.03-0.04 MPa.
9. The method for preparing spherical powder of high purity nickel-base superalloy according to claim 2, further comprising, after step 3: and 4, step 4: the metal powder is classified, and the classification comprises powder screening and powder airflow classification.
10. The method for preparing spherical powder of high-purity nickel-base superalloy according to claim 9, wherein powder sieving and powder air flow classification are both performed under the protection of argon gas, which is inert gas with high purity of 99.999%, that is, before operation, inert gas replacement treatment is performed on the rotary vibrating sieve and the air flow classifier respectively, and after 30min of replacement, the oxygen content in the equipment is lower than 10 ppm;
explosion-proof treatment is carried out on the pneumatic feeding mode in the powder screening process, the pressure of the pneumatic feeding is 0.2-0.6MPa, the pendulum angle is 60-80 degrees, the ultrasonic mode is intermittent or continuous, and the particle size section of the powder obtained after the powder screening is +250 mu m, 150-250 mu m and 0-150 mu m; and (3) carrying out air flow classification on the powder with the particle size of 0-150 microns, adjusting the frequency of a fan to be 30-50Hz, the feeding frequency to be 5-15Hz and the classification frequency to be 15-30Hz, and classifying the powder into three sections of powder by one-time feeding through powder screening and air flow classification to obtain the powder with the particle size of 0-15 microns, 15-53 microns and 53-150 microns.
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