CN110184501B - ECY768 cobalt-based alloy powder and preparation method and application thereof - Google Patents
ECY768 cobalt-based alloy powder and preparation method and application thereof Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 86
- 229910000531 Co alloy Inorganic materials 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000002844 melting Methods 0.000 claims abstract description 43
- 230000008018 melting Effects 0.000 claims abstract description 43
- 238000004519 manufacturing process Methods 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000002245 particle Substances 0.000 claims abstract description 16
- 238000005516 engineering process Methods 0.000 claims abstract description 14
- 230000006698 induction Effects 0.000 claims description 41
- 229910045601 alloy Inorganic materials 0.000 claims description 34
- 239000000956 alloy Substances 0.000 claims description 34
- 238000012216 screening Methods 0.000 claims description 18
- 239000002994 raw material Substances 0.000 claims description 15
- 238000000889 atomisation Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 8
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- 239000000654 additive Substances 0.000 abstract description 6
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- 239000001301 oxygen Substances 0.000 abstract description 3
- 229910052760 oxygen Inorganic materials 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 description 21
- 239000002184 metal Substances 0.000 description 21
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 9
- 239000010936 titanium Substances 0.000 description 8
- 239000007789 gas Substances 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
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- 229910052786 argon Inorganic materials 0.000 description 3
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- 229910017052 cobalt Inorganic materials 0.000 description 3
- 239000010941 cobalt Substances 0.000 description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
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- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910000601 superalloy Inorganic materials 0.000 description 2
- 229910052715 tantalum Inorganic materials 0.000 description 2
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- 238000012356 Product development Methods 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910001566 austenite Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
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- 239000010935 stainless steel Substances 0.000 description 1
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- 238000012360 testing method Methods 0.000 description 1
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- 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
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
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- 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
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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- B33—ADDITIVE MANUFACTURING TECHNOLOGY
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- B33Y70/00—Materials specially adapted for additive manufacturing
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
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- B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
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- B22F9/00—Making metallic powder or suspensions thereof
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- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
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Abstract
The invention relates to the technical field of selective laser melting, in particular to ECY768 cobalt-based alloy powder and a preparation method and application thereof. The ECY768 cobalt-based alloy powder prepared by the method has high purity, low oxygen content, high sphericity, uniform particle size distribution (D95 is less than or equal to 53 mu m) and high apparent density (6.24 g/mm)3) The flowability is good (13s/50g), the use requirement of a selective laser melting technology can be met, the yield of fine powder of the ECY768 cobalt-based alloy powder prepared by the method is high, the powder with the particle size smaller than 50 mu m accounts for more than 80%, the recovered powder can be used for other additive manufacturing technologies, and the production cost and pollution are greatly reduced.
Description
Technical Field
The invention relates to the technical field of selective laser melting, in particular to ECY768 cobalt-based alloy powder and a preparation method and application thereof.
Background
Additive manufacturing is a rapid prototyping technology based on a part digital model and produced in a discrete-layering-overlaying mode by means of laser, plasma beams and the like, and is also called as a 3D printing technology. Compared with the traditional manufacturing method, the additive manufacturing has the characteristics of high overall material utilization rate, shortened product development and production period, capability of manufacturing parts with complex structures, free design according to mechanical property requirements and the like, and the more complex the workpiece is, the higher the processing cost is, so that the 3D printing has more advantages in the production process of the complex parts.
The selective laser melting technology is one of additive manufacturing technologies, and the principle is that a part 3D model is discretized into a series of ordered micron-sized thin layers along a certain direction through computer software, metal powder is melted layer by taking laser as an energy source, and geometric parts with specific geometric shapes are manufactured. The technology can be used for manufacturing composite structure parts which cannot be manufactured by the traditional manufacturing means, and solves the problems of long period, difficult processing and high cost in the production process of metal parts with complex structures. The metal powders that can be currently applied to the selective laser melting technology mainly include stainless steel, titanium-based alloys, nickel-based alloys, cobalt-based alloys, and the like.
An ECY768 co-based alloy is an austenitic high temperature alloy, and unlike other superalloys, a co-based superalloy is not strengthened by ordered precipitates that are strongly bonded to the matrix, but rather by an austenite fcc matrix that has been solution strengthened and a small amount of carbides distributed therein. As one of the high temperature alloys, the cobalt-based high temperature alloy is widely used in products such as space engines and industrial gas turbines due to its high strength, good thermal fatigue resistance and excellent corrosion resistance. The ECY768 performance processed by adopting traditional means such as casting and the like can meet the requirement of ASTM F75 casting standard, but most parts processed by using ECY768 cobalt-based high-temperature alloy have relatively complex mechanical structures, so that the traditional processing means such as casting and the like are difficult to meet the requirement, the cost of the parts is greatly increased, the development of the cobalt-based high-temperature alloy in the fields of aerospace, industrial turbines and the like is greatly limited, the problems can be effectively solved by the selective laser melting technology, the performance of the final parts is improved, and the progress and development of the final products are promoted.
In the prior art, ECY768 cobalt-based alloy powder is mainly subjected to simple screening to obtain powder with a proper particle size and is completely applied to selective laser melting, the problem that the density of the ECY768 cobalt-based alloy powder is poor is not solved, and finally the forming performance of the ECY768 cobalt-based alloy powder is poor and even parts cannot be formed. Therefore, how to obtain the ECY768 cobalt-based alloy powder with high density and proper particle size is the main direction of research.
Disclosure of Invention
The invention aims to provide a preparation method of ECY768 cobalt-based alloy powder, and the ECY768 cobalt-based alloy powder prepared by the preparation method can enable a formed piece to have higher density, and the formed piece has small deformation, high precision and good mechanical property.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of ECY768 cobalt-based alloy powder, which comprises the following steps:
mixing raw materials of an ECY768 cobalt-based alloy, and carrying out first vacuum induction smelting to obtain a master alloy bar;
sequentially carrying out second vacuum induction melting, atomization powder making and powder screening on the master alloy bar to obtain ECY768 cobalt-based alloy powder;
the ECY768 cobalt-based alloy comprises the following raw materials in percentage by mass:
co 51.69-57.85%, Cr 22.5-24.35%, Ni 9.0-11.0%, W6.5-7.5%, Ta 3.0-4.0%, C0.55-0.65%, Zr 0.25-0.45%, Ti 0.15-0.30%, Al 0.10-0.25% and B less than or equal to 0.01%.
Preferably, the temperature of the first vacuum induction melting is 1600-1650 ℃, and the vacuum degree is<1.33×10-2Pa。
Preferably, the first vacuum induction melting is carried out for three times, and the heat preservation time of each time is 15-20 min.
Preferably, the temperature of the second vacuum induction melting is 1650-1700 ℃, the heat preservation time is 15-20 min, and the vacuum degree<1.0×10-2Pa。
Preferably, the second vacuum induction melting is performed in a vacuum induction furnace;
and heating the middle drain ladle of the vacuum induction furnace to 1150-1250 ℃ during the second vacuum induction melting.
Preferably, the atomization pressure of the atomized powder is 2.0-3.5 MPa.
Preferably, the powder screening mode is ultrasonic vibration screening and air flow classification which are sequentially carried out;
the mesh number of the screen used for ultrasonic vibration screening is 300 meshes.
Preferably, the grain diameter of the ECY768 cobalt-based alloy powder is 15-53 mu m.
The invention also provides ECY768 cobalt-based alloy powder prepared by the preparation method in the technical scheme.
The invention also provides application of the ECY768 cobalt-based alloy powder in the technical scheme in the technical field of selective laser melting.
The invention provides a preparation method of ECY768 cobalt-based alloy powder, which comprises the following steps: mixing raw materials of an ECY768 cobalt-based alloy, and carrying out first vacuum induction smelting to obtain a master alloy bar; sequentially carrying out second vacuum induction melting, atomization powder making and powder screening on the master alloy bar to obtain ECY768 cobalt-based alloy powder; the ECY768 cobalt-based alloy comprises the following raw materials in percentage by mass: 51.69-57.85% of Co, 22.5-24.35% of Cr22, 9.0-11.0% of Ni, 6.5-7.5% of W, 3.0-4.0% of Ta3, 0.55-0.65% of C, 0.25-0.45% of Zr, 0.15-0.30% of Ti, 0.10-0.25% of Al and less than or equal to 0.01% of B. The ECY768 cobalt-based alloy powder prepared by the method has high purity, low oxygen content, high sphericity, uniform particle size distribution (D95 is less than or equal to 53 mu m) and high apparent density (6.24 g/mm)3) The flowability is good (13s/50g), the use requirement of a selective laser melting technology can be met, the yield of fine powder of the ECY768 cobalt-based alloy powder prepared by the method is high, the powder with the particle size smaller than 50 mu m accounts for more than 80%, the recovered powder can be used for other additive manufacturing technologies, and the production cost and pollution are greatly reduced.
Drawings
FIG. 1 is a particle size distribution diagram of an ECY768 Co-based alloy powder prepared in example 1;
FIG. 2 is a morphology of ECY768 cobalt-based alloy powder prepared in example 1;
fig. 3 is a plot of a laser melt-formed sample using selected regions of the ECY768 cobalt-based alloy powder prepared in example 2.
Detailed Description
The invention provides a preparation method of ECY768 cobalt-based alloy powder, which comprises the following steps:
mixing raw materials of an ECY768 cobalt-based alloy, and carrying out first vacuum induction smelting to obtain a master alloy bar;
sequentially carrying out second vacuum induction melting, atomization powder making and powder screening on the master alloy bar to obtain ECY768 cobalt-based alloy powder;
the ECY768 cobalt-based alloy comprises the following raw materials in percentage by mass:
co 51.69-57.85%, Cr 22.5-24.35%, Ni 9.0-11.0%, W6.5-7.5%, Ta 3.0-4.0%, C0.55-0.65%, Zr 0.25-0.45%, Ti 0.15-0.30%, Al 0.10-0.25% and B less than or equal to 0.01%.
In the present invention, all the raw material components are commercially available products well known to those skilled in the art unless otherwise specified.
Mixing raw materials of an ECY768 cobalt-based alloy, and carrying out first vacuum induction smelting to obtain a master alloy bar; in the invention, the raw material of the ECY768 cobalt-based alloy comprises the following components in percentage by mass: 51.69-57.85% of Co, 22.5-24.35% of Cr, 9.0-11.0% of Ni, 6.5-7.5% of W, 3.0-4.0% of Ta, 0.55-0.65% of C, 0.25-0.45% of Zr, 0.15-0.30% of Ti, 0.10-0.25% of Al and less than or equal to 0.01% of B; more preferably comprises the following components: 53.5-55% of Co, 23-24% of Cr, 9.5-10.5% of Ni, 6.8-7.2% of W, 3.2-3.6% of Ta, 0.58-0.62% of C, 0.3-0.4% of Zr, 0.2-0.25% of Ti, 0.15-0.2% of Al and less than or equal to 0.01% of B. In the present invention, the raw material of the ECY768 cobalt-based alloy is preferably a simple metal corresponding to the above-described metal element. In the invention, the loss of each component in the first vacuum induction smelting process is ignored, namely the raw material of the ECY768 cobalt-based alloy is considered to be the same as the component of the prepared master alloy bar. The present invention does not require any particular mixing, and the mixing may be carried out by mixing procedures well known to those skilled in the art.
In the invention, the temperature of the first vacuum induction melting is preferably 1600-1650 ℃, more preferably 1610-1640 ℃, and most preferably 1620-1630 ℃; the degree of vacuum is preferably<1.33×10-2Pa, more preferably<1.0×10-2Pa. The first vacuum induction melting is preferably carried out three times, and the heat preservation time of each time is preferably 15-20 min, and more preferably 16-18 min.
In the present invention, the first vacuum induction melting is preferably performed in a vacuum induction melting furnace.
After the first vacuum induction melting is finished, the obtained alloy crude product is preferably cut and polished; the present invention does not have any particular limitation on the cutting and grinding, and the cutting or grinding may be performed by a process well known to those skilled in the art. In the present invention, the polishing is intended to remove an oxide layer in the crude alloy.
After obtaining a master alloy bar, sequentially carrying out second vacuum induction melting, atomization powder preparation and powder screening on the master alloy bar to obtain ECY768 cobalt-based alloy powder; in the invention, the temperature of the second vacuum induction melting is preferably 1650-1700 ℃, more preferably 1660-1690 ℃, most preferably 1670-1680 ℃, and the heat preservation time is preferably 15-30 min, more preferably 20-25 min; the degree of vacuum is preferably<1.0×10-2Pa. In the present invention, the second vacuum induction melting is performed in a vacuum induction furnace; and heating the temperature of a middle tundish of the vacuum induction furnace to 1150-1250 ℃ during the second vacuum induction melting, and more preferably 1180-1220 ℃.
In the invention, the atomization milling is preferably carried out in a vacuum induction gas atomization furnace, and the specific process of the atomization milling is preferably as follows: and opening a material leaking valve, enabling the molten metal to flow to the atomizing furnace through a leakage hole at the bottom of the middle leakage ladle (the middle leakage ladle heated to 1150-1250 ℃), in the atomizing furnace, under the impact of high-purity argon gas flow, the molten metal is broken into tiny metal droplets, the metal droplets are cooled and solidified into ECY768 cobalt-based alloy powder in the falling process of the metal droplets, and the metal droplets are carried into a powder collecting device by gas at the bottom of the atomizing furnace.
In the present invention, the atomization pressure (pressure in the furnace of the aerosol furnace) of the atomized powder is preferably 2.0 to 3.5MPa, and more preferably 2.5 to 3.0 MPa.
In the invention, the powder screening is preferably performed by ultrasonic vibration screening and air flow classification which are sequentially performed; the mesh number of the screen used for ultrasonic vibration screening is preferably 300 meshes, so that the particle size of the powder obtained after screening is less than 53 mu m; the gas stream classification according to the invention is not subject to any particular limitation, and is carried out using procedures known to those skilled in the art and which ensure that powders having a particle size of less than 15 μm can be removed.
The invention also provides ECY768 cobalt-based alloy powder prepared by the preparation method in the technical scheme. In the invention, the grain diameter of the ECY768 cobalt-based alloy powder is preferably 15-53 μm.
The invention also provides application of the ECY768 cobalt-based alloy powder in the technical scheme in the technical field of selective laser melting.
The ECY768 co-based alloy powder provided by the present invention and the preparation method and application thereof will be described in detail with reference to the following examples, but they should not be construed as limiting the scope of the present invention.
Example 1
According to the mass ratio of Cr to 23.09 percent, Ni to 9.0 percent, W to 6.75 percent, Ta to 3.02 percent, C to 0.65 percent, Zr to 0.26 percent, Ti to 0.18 percent, Al to 0.15 percent and Co to Bal, the raw materials are mixed, and first vacuum induction melting is carried out at 1600 ℃ (the vacuum degree is 1 multiplied by 10)-2Pa) for 3 times, keeping the temperature for 15min each time, cutting and polishing to obtain a master alloy bar;
subjecting the master alloy bar to a second vacuum induction melting (6.0 × 10)-3Pa, 1650 ℃, 20min), heating the middle drain ladle to 1220 ℃, opening a material leakage valve, leading the molten metal to flow to the atomizing furnace through a leakage hole at the bottom of the middle drain ladle, leading the pressure in the atomizing furnace to be 2.5MPa, and flushing high-purity argon flowUnder impact, the molten metal is broken into tiny metal droplets, the metal droplets are cooled and solidified into ECY768 cobalt-based alloy powder in the falling process of the metal droplets, the ECY768 cobalt-based alloy powder is taken into a powder collecting device by gas at the bottom of an aerosol furnace, and ultrasonic vibration screening (300 meshes) and airflow classification are carried out to obtain the ECY768 cobalt-based alloy powder with the particle size of 15-53 mu m.
FIG. 1 is a particle size distribution diagram of ECY768 Co-based alloy powder prepared in example 1, and it can be seen that the average particle size of the ECY768 Co-based alloy powder is 34.6 μm;
FIG. 2 is a morphology graph of ECY768 cobalt-based alloy powder prepared in example 1, and as can be seen, the morphology graph of ECY768 cobalt-based alloy powder prepared in example 1 is a sphere with regular morphology;
according to the GB/T35022-2018 standard, the flowability and the apparent density of the ECY768 cobalt-based alloy powder are tested, and the test result shows that the flowability is 13s/50g, and the apparent density is 6.24g/mm3。
Example 2
According to the mass ratio of Cr to 23.09 percent, Ni to 9.0 percent, W to 6.75 percent, Ta to 3.02 percent, C to 0.65 percent, Zr to 0.26 percent, Ti to 0.18 percent, Al to 0.15 percent and Co to Bal, the raw materials are mixed, and first vacuum induction melting is carried out at 1600 ℃ (the vacuum degree is 1 multiplied by 10)-2Pa) for 3 times, keeping the temperature for 15min each time, cutting and polishing to obtain a master alloy bar;
subjecting the master alloy bar to a second vacuum induction melting (7.0 × 10)-3Pa, 1670 ℃ and 20min), heating the middle drain ladle to 1200 ℃, opening a material leaking valve, enabling the metal liquid to flow to the atomizing furnace through a drain hole at the bottom of the middle drain ladle, enabling the pressure in the atomizing furnace to be 2.7MPa, under the impact of high-purity argon gas flow, breaking the metal liquid to form tiny metal droplets, cooling and solidifying the metal droplets into ECY768 cobalt-based alloy powder in the falling process of the metal droplets, introducing the gas into a powder collecting device at the bottom of the atomizing furnace, carrying out ultrasonic vibration screening (300 meshes) and air flow classification to obtain ECY768 cobalt-based alloy powder with the particle size of 15-53 mu m,
the ECY768 cobalt-based alloy powder is put on a Pro X200 deviceSelective laser melting forming is carried out, powder is smoothly laid in the selective laser melting forming process, the formed part has high density (more than 99.95 percent) and the hardness can reach 360HV0.2The above.
Fig. 3 is a sample of the ECY768 co-based alloy powder prepared in example 2, which was formed by selective laser melting, and it can be seen that the sample of the ECY768 co-based alloy powder prepared in example 2, which was formed by selective laser melting, can be formed with good surface quality.
As can be seen from the above examples, the ECY768 cobalt-based alloy powder prepared by the preparation method provided by the invention has the advantages of high purity, low oxygen content, high sphericity, uniform particle size distribution (D95 is less than or equal to 53 mu m) and high apparent density (6.24 g/mm)3) The flowability is good (13s/50g), the use requirement of a selective laser melting technology can be met, the yield of fine powder of the ECY768 cobalt-based alloy powder prepared by the method is high, the powder with the particle size smaller than 50 mu m accounts for more than 80%, the recovered powder can be used for other additive manufacturing technologies, and the production cost and pollution are greatly reduced.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (5)
1. A preparation method of ECY768 cobalt-based alloy powder is characterized by comprising the following steps:
mixing raw materials of an ECY768 cobalt-based alloy, and carrying out first vacuum induction smelting to obtain a master alloy bar;
sequentially carrying out second vacuum induction melting, atomization powder making and powder screening on the master alloy bar to obtain ECY768 cobalt-based alloy powder;
the ECY768 cobalt-based alloy comprises the following raw materials in percentage by mass:
51.69-57.85% of Co, 22.5-24.35% of Cr, 9.0-11.0% of Ni, 6.5-7.5% of W, 3.0-4.0% of Ta, 0.55-0.65% of C, 0.25-0.45% of Zr, 0.15-0.30% of Ti, 0.10-0.25% of Al and less than or equal to 0.01% of B;
the temperature of the first vacuum induction melting is 1600-1650 ℃, and the vacuum degree of the first vacuum induction melting is<1.33×10-2Pa；
The first vacuum induction melting comprises three times, and the heat preservation time of each time is 15-20 min;
the temperature of the second vacuum induction melting is 1650-1700 ℃, the heat preservation time is 15-20 min, and the vacuum degree<1.0×10-2Pa；
The second vacuum induction melting is carried out in a vacuum induction furnace;
heating the middle drain ladle of the vacuum induction furnace to 1150-1250 ℃ during the second vacuum induction smelting;
the powder screening mode is air flow classification and ultrasonic vibration screening which are sequentially carried out;
the mesh number of the screen used for ultrasonic vibration screening is 300 meshes.
2. The method of claim 1, wherein the atomized powder is prepared at an atomization pressure of 2.0 to 3.5 MPa.
3. The method according to claim 1, wherein the ECY768 Co-based alloy powder has a particle size of 15 to 53 μm.
4. ECY768 cobalt-based alloy powder produced by the production method according to any one of claims 1 to 3.
5. Use of the ECY768 Co-based alloy powder of claim 4 in the field of selective laser melting technology.
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