CN111001807B - Method for regulating and controlling Nb-rich phase precipitation behavior in laser 3D printing nickel-based superalloy - Google Patents

Method for regulating and controlling Nb-rich phase precipitation behavior in laser 3D printing nickel-based superalloy Download PDF

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CN111001807B
CN111001807B CN201911410952.XA CN201911410952A CN111001807B CN 111001807 B CN111001807 B CN 111001807B CN 201911410952 A CN201911410952 A CN 201911410952A CN 111001807 B CN111001807 B CN 111001807B
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nickel
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肖辉
谢盼
宋立军
易黄懿
肖文甲
成满平
罗国云
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Hunan University
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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
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • 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
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/20—Direct sintering or melting
    • 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
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/30—Process control
    • B22F10/36—Process control of energy beam parameters
    • 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
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/30—Process control
    • B22F10/36—Process control of energy beam parameters
    • B22F10/368—Temperature or temperature gradient, e.g. temperature of the melt pool
    • 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
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/60—Treatment of workpieces or articles after build-up
    • B22F10/64—Treatment of workpieces or articles after build-up by thermal means
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • 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
    • B33Y10/00—Processes of additive manufacturing
    • 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
    • B33Y50/00—Data acquisition or data processing for additive manufacturing
    • B33Y50/02—Data acquisition or data processing for additive manufacturing for controlling or regulating additive manufacturing processes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/0433—Nickel- or cobalt-based alloys
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • B22F2003/248—Thermal after-treatment
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

Abstract

A method for regulating and controlling Nb-rich phase precipitation behavior in a laser 3D printing nickel-based superalloy, comprises the steps of firstly, preliminarily optimizing a laser 3D printing process window; obtaining instantaneous and fixed point temperature change curves by using a colorimetric pyrometer; extracting the average value Tmax of the peak temperature and the average value Tmin of the trough temperature in the instantaneous temperature curve of the molten pool, and calculating the average cooling rate xi of the temperature range between the solidus and the liquidus of the fixed point temperature curve; according to the conditions that Tmax is more than or equal to 1.4Tm and less than or equal to 1.8Tm, Tmin is more than or equal to 0.8Tm and less than or equal to 0.9Tm, and xi is more than or equal to 2.0 multiplied by 104Optimizing the technological parameters according to the principle of DEG C/s, and printing the formed sample under the optimized parameters to perform the following subsequent solid solution-aging heat treatment: and obtaining the nickel-based superalloy formed piece with the controlled Nb-rich phase. The method can effectively control the precipitation behavior of the Nb-rich phase in the laser 3D printing and subsequent heat treatment processes, and further improve the mechanical property of the nickel-based forming piece.

Description

Method for regulating and controlling Nb-rich phase precipitation behavior in laser 3D printing nickel-based superalloy
Technical Field
The invention relates to the field of laser material processing, in particular to a method for regulating and controlling the precipitation behavior of a Nb-rich phase in a laser 3D printing nickel-based superalloy.
Background
The nickel-based high-temperature alloy is widely applied to the fields of aviation, aerospace and energy sources due to good high-temperature mechanical property, oxidation resistance and corrosion resistance, such as the manufacture of steam turbines and critical parts of aircraft engines. The Nb-rich Ni-based high-temperature alloy such as Inconel 718 or Inconel 625, and the like, takes Nb as a main alloying element, and is strengthened mainly by a delta-Ni 3Nb phase, a gamma '-Ni 3Nb phase and a gamma' -Ni3(Al, Ti) phase.
Laser 3D printing technology is a revolutionary technology for layer-by-layer fabrication of near net-shape parts, and has gained increasing popularity in recent years in fabricating or repairing nickel-base superalloy parts. Coaxial powder fed laser 3D printing techniques typically utilize a high power laser to melt and deposit metal powder onto a substrate in a continuous wave mode, and then produce parts layer by layer. Continuous laser 3D printing has high cooling rate, high temperature gradient and rapid solidification characteristics. Segregation of Nb elements and formation of brittle Laves phases are generally caused during solidification of the molten pool. However, segregation of Nb elements and formation of brittle Laves phases reduces the mechanical properties of the shaped articles, such as tensile plasticity. In addition, precipitation of γ "-Ni 3Nb and γ' -Ni3(Al, Ti) strengthening phases is suppressed due to rapid cooling of the molten pool, thereby reducing the strength and hardness of the sample. Therefore, it is important to optimize the microstructure to improve the mechanical properties of nickel-base superalloy forms.
Generally, precipitation strengthened nickel-base superalloys involve 3 Nb-rich phases during the subsequent heat treatment of the laser 3D printer: the Laves phase formed during solidification; a delta-Ni 3Nb phase precipitated during solution treatment and a gamma' -Ni3Nb strengthening phase precipitated during aging. The morphology, distribution and number of these phases determine the final mechanical properties of the shaped article. Therefore, effective control of the above Nb-containing phase is required.
The method provided by the invention can effectively control the 3 Nb-rich phases and improve the mechanical properties of the material.
Disclosure of Invention
The invention aims to provide a method for regulating and controlling the precipitation behavior of an Nb-rich phase in a laser 3D printing nickel-based superalloy.
A method for regulating and controlling Nb-rich phase precipitation behavior in a laser 3D printing nickel-based superalloy comprises the following steps:
a method for regulating and controlling Nb-rich phase precipitation behavior in laser 3D printing nickel-based superalloy is characterized by comprising the following steps:
the method comprises the following steps: performing preliminary optimization on the laser 3D printing process parameters to obtain the preliminary optimized process parameters: the laser waveform is a square wave, the diameter of a laser spot is 0.5-2.0 mm, the peak power of the laser is 600-1000W, the repetition frequency is 5-100 Hz, the duty ratio is 0.45-0.9, the defocusing amount is-2.0 mm, and the scanning speed is 6-12 mm/s;
step two: two colorimetric pyrometers are adopted to record instantaneous temperature change of the center of a molten pool and fixed point temperature change experienced by a middle position point of a single deposition layer respectively to obtain an instantaneous and fixed point temperature change curve; extracting the peak temperature of the instantaneous temperature change curve of the molten pool, calculating a peak temperature average Tmax and a trough temperature average Tmin, performing derivation on the temperature drop part on the right side of the fixed point temperature change curve, and calculating an average value xi of the derivative, namely obtaining the average cooling rate xi of the molten pool;
step three: according to the conditions that Tmax is more than or equal to 1.4Tm and less than or equal to 1.8Tm, Tmin is more than or equal to 0.8Tm and less than or equal to 0.9Tm, and xi is more than or equal to 2.0 multiplied by 104Optimizing technological parameters such as the diameter of a laser spot, the peak power of the laser, the repetition frequency, the duty ratio, the defocusing amount, the scanning speed, the powder feeding amount and the like according to the principle of DEG C/s, wherein Tm is the melting point of the nickel-based alloy;
step four: obtaining an optimized process window: the laser waveform is square wave, the diameter of a laser spot is 0.8-1.5 mm, the peak power of the laser is 600-800W, the repetition frequency is 5-20 Hz, the duty ratio is 0.45-0.8, the defocusing amount is-2.0 mm, the scanning speed is 6-10 mm/s, and the powder feeding amount is 9-14 g/min;
step five: performing laser 3D printing according to the optimized process parameters obtained in the step four, and performing subsequent solid solution-aging heat treatment on the formed sample: 980 ℃/1 h/air cooling, 720 ℃/8 h/furnace cooling to 620 ℃, 620 ℃/8 h/air cooling to room temperature, and obtaining the Nb-rich phase controlled nickel-based superalloy forming piece.
In the second step, the emissivity of the colorimetric pyrometer is set to be 1.15, and the included angle between the colorimetric pyrometer and the horizontal plane is 70oThe spot size is 1mm, and the single data acquisition time is 1 ms.
The nickel-based superalloy is Nb-containing precipitation strengthening nickel-based superalloy or Nb-containing solid solution strengthening nickel-based superalloy.
The method can effectively control the precipitation behavior of the Nb-rich phase in the laser 3D printing and subsequent heat treatment processes, realize effective regulation and control of the Nb-containing phase, and further improve the mechanical property of the nickel-based forming piece.
Drawings
FIG. 1 is a scanning electron microscope image of a nickel-based alloy laser 3D printing sample obtained by the invention;
FIG. 2 is a scanning electron microscope image of a nickel-based alloy laser 3D printing sample obtained by a conventional method.
Detailed Description
Example 1
A method for regulating and controlling Nb-rich phase precipitation behavior in a laser 3D printing nickel-based superalloy comprises the following steps:
the method comprises the following steps: performing preliminary optimization on the laser 3D printing process parameters to obtain the preliminary optimized process parameters: the laser waveform is a square wave, the diameter of a laser spot is 0.5-2.0 mm, the peak power of the laser is 600-1000W, the repetition frequency is 5-100 Hz, the duty ratio is 0.45-0.9, the defocusing amount is-2.0 mm, and the scanning speed is 6-12 mm/s;
step two: two colorimetric pyrometers are adopted to record instantaneous temperature change of the center of a molten pool and fixed point temperature change experienced by a middle position point of a single deposition layer respectively to obtain an instantaneous and fixed point temperature change curve; extracting the peak temperature of the instantaneous temperature change curve of the molten pool, calculating a peak temperature average Tmax and a trough temperature average Tmin, performing derivation on the temperature drop part on the right side of the fixed point temperature change curve, and calculating an average value xi of the derivative, namely obtaining the average cooling rate xi of the molten pool;
step three: according to the conditions that Tmax is more than or equal to 1.4Tm and less than or equal to 1.8Tm, Tmin is more than or equal to 0.8Tm and less than or equal to 0.9Tm, and xi is more than or equal to 2.0 multiplied by 104Principle pair of DEG C/sOptimizing technological parameters such as laser spot diameter, laser peak power, repetition frequency, duty ratio, defocusing amount, scanning speed, powder feeding amount and the like, wherein Tm is the melting point of the nickel-based alloy;
step four: obtaining an optimized process window: the laser waveform is square wave, the diameter of a laser spot is 0.8-1.5 mm, the peak power of the laser is 600-800W, the repetition frequency is 5-20 Hz, the duty ratio is 0.45-0.8, the defocusing amount is-2.0 mm, the scanning speed is 6-10 mm/s, and the powder feeding amount is 9-14 g/min;
step five: performing laser 3D printing according to the optimized process parameters obtained in the step four, and performing subsequent solid solution-aging heat treatment on the formed sample: and (3) 980 ℃/1 h/air cooling, 720 ℃/8 h/furnace cooling to 620 ℃, 620 ℃/8 h air cooling to room temperature, and obtaining the Nb-rich phase controlled nickel-based superalloy forming piece.
Fig. 1 is a microstructure diagram of a nickel-based superalloy laser 3D printed sample. FIG. 1a is a scanning electron micrograph showing that the microstructure mainly consists of a Laves phase and a deta phase which are discretely distributed; FIG. 1b is a transmission electron micrograph taken under the [011] crystallographic band axis, from which it can be seen that a large amount of Nb-rich strengthening phases are precipitated in the matrix, which is consistent with the diffraction pattern results in the lower left corner of FIG. 1 b.
FIG. 2 is a microstructure diagram of a nickel-based superalloy laser 3D printed sample obtained by a conventional method. FIG. 2a is a scanning electron microscope image, from which it can be seen that the microstructure mainly consists of a Laves phase and a coarse deta phase, and the Laves phase and the deta phase are in a chain-like distribution; FIG. 2b is a transmission electron micrograph taken under the [011] ribbon axis, from which it can be seen that only a small amount of Nb-rich strengthening phase precipitates in the matrix, which is consistent with the diffraction pattern at the bottom left corner of FIG. 2 b.

Claims (3)

1. A method for regulating and controlling Nb-rich phase precipitation behavior in laser 3D printing nickel-based superalloy is characterized by comprising the following steps:
the method comprises the following steps: performing preliminary optimization on the laser 3D printing process parameters to obtain the preliminary optimized process parameters: the laser waveform is a square wave, the diameter of a laser spot is 0.5-2.0 mm, the peak power of the laser is 600-1000W, the repetition frequency is 5-100 Hz, the duty ratio is 0.45-0.9, the defocusing amount is-2.0 mm, and the scanning speed is 6-12 mm/s;
step two: two colorimetric pyrometers are adopted to record instantaneous temperature change of the center of a molten pool and fixed point temperature change experienced by a middle position point of a single deposition layer respectively to obtain an instantaneous and fixed point temperature change curve; extracting the peak temperature of the instantaneous temperature change curve of the molten pool, calculating a peak temperature average Tmax and a trough temperature average Tmin, performing derivation on the temperature drop part on the right side of the fixed point temperature change curve, and calculating an average value xi of the derivative, namely obtaining the average cooling rate xi of the molten pool;
step three: according to the conditions that Tmax is more than or equal to 1.4Tm and less than or equal to 1.8Tm, Tmin is more than or equal to 0.8Tm and less than or equal to 0.9Tm, and xi is more than or equal to 2.0 multiplied by 104Optimizing technological parameters of the laser spot diameter, the laser peak power, the repetition frequency, the duty ratio, the defocusing amount, the scanning speed and the powder feeding amount according to the principle of DEG C/s, wherein Tm is the melting point of the nickel-based alloy;
step four: obtaining an optimized process window: the laser waveform is square wave, the diameter of a laser spot is 0.8-1.5 mm, the peak power of the laser is 600-800W, the repetition frequency is 5-20 Hz, the duty ratio is 0.45-0.8, the defocusing amount is-2.0 mm, the scanning speed is 6-10 mm/s, and the powder feeding amount is 9-14 g/min;
step five: performing laser 3D printing according to the optimized process parameters obtained in the step four, and performing subsequent solid solution-aging heat treatment on the formed sample: and (3) 980 ℃/1 h/air cooling, 720 ℃/8 h/furnace cooling to 620 ℃, 620 ℃/8 h air cooling to room temperature, and obtaining the Nb-rich phase controlled nickel-based superalloy forming piece.
2. The method for regulating and controlling the Nb-rich phase precipitation behavior in the laser 3D printing nickel-based superalloy according to claim 1, wherein the Nb-rich phase precipitation behavior comprises the following steps: in the second step, the emissivity of the colorimetric pyrometer is set to be 1.15, and the included angle between the colorimetric pyrometer and the horizontal plane is 70oThe spot size is 1mm, and the single data acquisition time is 1 ms.
3. The method for regulating and controlling the Nb-rich phase precipitation behavior in the laser 3D printing nickel-based superalloy according to claim 1, wherein the Nb-rich phase precipitation behavior comprises the following steps: the nickel-based superalloy is Nb-containing precipitation strengthening nickel-based superalloy or Nb-containing solid solution strengthening nickel-based superalloy.
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