In-situ nitride reinforced 3d printed nickel-based superalloy powder

Abstract

The application discloses in-situ nitride reinforced 3D printing nickel-based superalloy powder, and the sum of the mass percentages of components of the powder is 100% in mass percentage, and the powder comprises the following components: Co: 12-17%, Nb: 3-4%, Al: 4-6%, Ru: 0.3-3%, Ta: 1-2%, Y: 0.02-0.1%, La: 0.05-0.1%, Cr: 8-12%, Si: 0.2-1.5%, Re: 0.02-0.05%, B: 0.01-0.015%, and the balance is Ni. The powder is used for preparing a dispersion-strengthened nickel-based superalloy by in-situ generation of nitrides through 3D printing. The application prepares a new type of nickel-based superalloy powder suitable for 3D printing by reasonably designing the proportion of each alloy element, combining vacuum induction melting and atomization powder preparation technology. The nickel-based superalloy forming piece prepared by using in-situ generated Si3N4 strengthening second phase in the printing process has high density, good internal quality, few defects, excellent tensile strength and ductility, the tensile strength of the nickel-based superalloy at room temperature is up to 1.62 GPa at the highest, and the elongation is up to 16.8% at the highest.

Description

TECHNICAL FIELD

[0001] The present application belongs to the field of powder metallurgy, i.e. advanced manufacturing technology, and particularly relates to a kind of in-situ nitride reinforced 3D printing nickel-based superalloy powder. BACKGROUND

[0002] Nickel-based alloys have excellent comprehensive performance, such as high temperature resistance, corrosion resistance, fatigue resistance, wear resistance and high strength, and the maximum use temperature can reach 1100℃. Therefore, nickel-based alloys are widely used in aerospace, metallurgy, power and other fields.

[0003] Nickel-based superalloys are difficult to cut and have low forming freedom, so it is difficult to use traditional methods to prepare nickel-based superalloys. 3D printing is a near-net shaping technology based on the principle of layering and stacking. It breaks through the inherent limitations of traditional subtractive manufacturing methods, improves material utilization, and can be used to prepare dense solid parts. It has good applicability for materials that are difficult to process or have complex internal structures.

[0004] During 3D printing, there is a high temperature gradient and large thermal stress, which can easily cause microcracks, seriously affecting the performance and application of the product. To solve this problem, the substrate is usually preheated before printing or post-processing is performed after printing, but this increases the production cost. Some scholars consider using second-phase strengthened nickel-based superalloys, which are artificially added to the substrate or use a specific process to form highly dispersed second-phase particles in the substrate. However, in general, the preparation process of nickel-based superalloys with direct addition of secondary reinforcing phase to the substrate is complex, time-consuming and costly, and can easily form a rough structure, resulting in low ductility. Therefore, some scholars propose to use the advantages of 3D printing to generate second-phase particles in-situ during the forming process. However, precise control of in-situ generated second-phase particles cannot be achieved by simply changing the laser parameters of 3D printing, so the effect of second-phase strengthening cannot be well applied.

[0005] The patent with publication number CN114054775B discloses an aging strengthened nickel-based superalloy 3D printing process and a 3D printed part prepared thereby. The aging strengthened nickel-based superalloy 3D printing process includes the following steps: 3D printing of the aging strengthened nickel-based superalloy powder in a vacuum or protective atmosphere, the power of the 3D printing is 280-290W, and the scanning speed of the 3D printing is 920-965mm / s; the aging strengthened nickel-based superalloy powder is prepared by vacuum melting gas atomization. The 3D printing process generates second-phase particles in-situ during the forming process, but precise control of in-situ generated second-phase particles cannot be achieved by simply changing the laser parameters of 3D printing, so the effect of second-phase strengthening cannot be well applied. SUMMARY

[0006] The present application provides an in-situ nitride reinforced 3D printed nickel-based superalloy powder to solve the problems in the prior art.

[0007] The technical scheme adopted by the present application is:

[0008] An in-situ nitride reinforced 3D printed nickel-based superalloy powder, the sum of the mass percentages of the components of the powder is 100% by mass, comprising: Co: 12-17%, Nb: 3-4%, Al: 4-6%, Ru: 0.3-3%, Ta: 1-2%, Y: 0.02-0.1%, La: 0.05-0.1%, Cr: 8-12%, Si: 0.2-1.5%, Re: 0.02-0.05%, B: 0.01-0.015%, and the balance being Ni.

[0009] Further, the powder is obtained by 3D printing in-situ to generate nitrides to obtain a dispersion strengthened nickel-based superalloy.

[0010] Further, the dispersion strengthened nickel-based superalloy preparation method comprises:

[0011] S1: Under vacuum conditions, prepare a metal powder according to the mass percentage;

[0012] S2: The prepared metal powder is subjected to melting and degassing treatment to obtain a melt;

[0013] S3: The obtained melt is subjected to gas atomization treatment to obtain a 3D printed nickel-based superalloy powder;

[0014] S4: Using the 3D printed nickel-based superalloy powder as raw material, a product is prepared by 3D printing.

[0015] Further, in step S2, the prepared metal powder is melted, and the prepared alloy powder is placed in a melting furnace, and when the vacuum degree of the furnace cavity is higher than 0.1 MPa, inert gas protection is filled.

[0016] Further, in step S2, the degassing treatment is carried out at a degassing temperature of 1500℃ for 8-10min.

[0017] Further, in step S3, the gas atomization treatment is carried out by introducing inert gas for atomization powdering, and the pressure in the furnace is 0.2-0.3 bar.

[0018] Further, in step S3, the powder after atomization powdering is placed in a drying box, the holding time is 16-20 hours, and the drying temperature is 70-90℃.

[0019] Further, the inert gas is high-purity argon with a purity of 99.99%.

[0020] Further, after atomization and powdering in the step S3, the powder with a particle size of 35-45 mu is obtained by screening.

[0021] Further, the device used in the 3D printing is a selective laser melting device, the control laser power is 280-320 W, the scanning speed is 800-1000 mm / s, the scanning interval is 0.08-0.12 mm, the layer thickness is 0.2-0.3 mm, and the rotation angle of adjacent layers is 67°.

[0022] Compared with the prior art, the beneficial effects of the present application are:

[0023] In the prepared nickel-based superalloy powder of the present application, the elements Nb, Ru, Ta, Y and La can improve the strength, hardness, wear resistance and high-temperature performance of the nickel-based alloy; the addition of the element Si enables the in-situ generation of fine reinforcing particles Si3N4 under heating conditions in the 3D printing process and in the nitrogen environment of the forming environment, the existence of the second phase reinforcing particles has a strong pinning effect on dislocations, grain boundaries and subgrain boundaries, thereby strengthening the alloy and especially improving the high-temperature performance of the material; the existence of the element Re acts as a catalyst to promote the heating reaction of Si and nitrogen, which is beneficial to the generation of the reinforcing particles Si3N4. Through the composition design of the 3D printed nickel-based superalloy, the tensile strength of the nickel-based superalloy at room temperature can be up to 1.62 GPa, and the elongation can be up to 16.8%.

[0024] By reasonably designing the proportions of various alloy elements, combining vacuum induction melting and argon gas atomization powdering technology, a new type of nickel-based superalloy powder suitable for 3D printing is prepared; under the premise of ensuring that the prepared powder has high sphericity, low oxygen content, good flowability and few satellite powders, the nickel-based superalloy forming piece prepared by using the in-situ generated Si3N4 strengthening second phase in the printing process has high density, good internal quality, few defects, excellent tensile strength and ductility, which meets the quality requirements of current nickel-based superalloys. BRIEF DESCRIPTION OF DRAWINGS

[0025] Figure 1 SEM image of Example 1 magnified 200 times;

[0026] Figure 2 SEM image of Example 1 magnified 500 times;

[0027] Figure 3 Metallographic image of the nickel-based superalloy sample prepared in Example 1;

[0028] Figure 4 Metallographic image of the nickel-based superalloy sample prepared in Example 2;

[0029] Figure 5 Metallograph of a nickel-based superalloy sample prepared for Example 3;

[0030] Figure 6 Metallograph of a nickel-based superalloy sample prepared for Example 4. DETAILED DESCRIPTION

[0031] In order to clearly illustrate the technical features of the present application, the following will describe the present application in detail with specific embodiments and in conjunction with the accompanying drawings. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present application. However, the present application can be practiced in other ways different from those described herein, and therefore the scope of protection of the present application is not limited by the specific embodiments disclosed below. Unless otherwise defined, all professional terms used herein have the same meaning as commonly understood by those skilled in the art. The professional terms used herein are only for the purpose of describing specific embodiments and are not intended to limit the scope of protection of the present application.

[0032] Example 1

[0033] An embodiment provided by the present application is a kind of in-situ nitride reinforced 3D printing nickel-based superalloy powder, the specific chemical composition is Co: 15%, Nb: 3%, Al: 5%, Ru: 0.4%, Ta: 2%, Y: 0.08%, La: 0.06%, Cr: 9%, Si: 1%, Re: 0.03%, B: 0.01%, and the balance is Ni.

[0034] S1: under vacuum conditions, prepare metal powder according to the mass percentage;

[0035] S2: raw material smelting: add the prepared metal powder into the smelting furnace for vacuum smelting, the smelting temperature is 1500℃; when the vacuum degree of the furnace cavity is higher than 0.1MPa, inert gas protection is filled, and the degassing time is 9min;

[0036] S3: atomization powder, the obtained melt is introduced into the atomization furnace for gas atomization treatment, a ring hole conical nozzle is used for gas atomization treatment, the diameter is 3.5mm; the spray gas cone angle is 55°, the atomization temperature is above 400℃ of the liquidus temperature; the spray speed of gas atomization treatment is controlled at 3.7kg / min; the pressure in the gas atomization furnace is controlled at 0.25bar; the pressure of high-pressure atomization medium is controlled at 4.5MPa; powder screening: the above pre-alloyed metal powder is subjected to mesh screening treatment to obtain metal powder with a particle size range of 35μm-45μm. Heat preservation and drying: the screened powder is placed in a drying box, the heat preservation time is 18 hours, and the drying temperature is 80℃

[0037] S4: taking the 3D printing nickel-based superalloy powder as raw material, a product is prepared by 3D printing. The laser parameters for 3D printing of the above powder are: the preheating temperature of the printing substrate is 150℃; the laser scanning power is 280W; the laser scanning speed is 800mm / s; the scanning interval is 0.10mm; and the interlayer thickness is 0.3mm.

[0038] Reference Figures 1-3 As shown in the figure, the tensile strength of the zero-component part is measured to be 1620MPa, and the elongation is 16.7%.

[0039] Example 2

[0040] An embodiment provided by the application: an in-situ nitride reinforced 3D printing nickel-based superalloy powder, the prepared metal powder has the following chemical composition in terms of mass percentage: Co: 15%, Nb: 1.5%, Al: 5%, Ru: 0.4%, Ta: 2%, Y: 0.08%, La: 0.06%, Cr: 9%, Si: 1%, Re: 0.03%, B: 0.01%, and the balance is Ni.

[0041] S1: preparing the metal powder according to the mass percentage under vacuum conditions;

[0042] S2: raw material smelting: the prepared metal powder is added into a smelting furnace for vacuum smelting, the smelting temperature is 1500℃; when the vacuum degree of the furnace cavity is higher than 0.1MPa, inert gas protection is filled, and the degassing time is 9min;

[0043] S3: atomization powder preparation, the obtained melt is introduced into an atomization furnace for gas atomization treatment, a ring-hole conical nozzle is used for the gas atomization treatment, the diameter of the nozzle is 3.5mm; the spray gas cone angle is 55°, the atomization temperature is 400℃ above the liquidus temperature; the spraying speed of the gas atomization treatment is controlled to be 3.7kg / min; the pressure in the gas atomization furnace is controlled to be 0.25bar; the pressure of the high-pressure atomization medium is controlled to be 4.5MPa; powder screening: the above pre-alloyed metal powder is subjected to mesh screening treatment to obtain metal powder with a particle size range of 35μm-45μm. Heat preservation and drying: the screened powder is placed in a drying box, the heat preservation time is 18 hours, and the drying temperature is 80℃.

[0044] S4: taking the 3D printing nickel-based superalloy powder as raw material, a product is prepared by 3D printing. The laser parameters for 3D printing of the above powder are: the preheating temperature of the printing substrate is 150℃; the laser scanning power is 280W; the laser scanning speed is 800mm / s; the scanning interval is 0.10mm; and the interlayer thickness is 0.3mm.

[0045] Reference Figure 4The tensile strength of the measured component is 1470 MPa, and the elongation is 14.8%.

[0046] Example 3

[0047] An embodiment provided by the application is a 3D printing nickel-based superalloy powder in-situ nitride reinforced, which is consistent with the conditions of Example 1, except that the metal powder is prepared, and the specific chemical composition is Co: 15%, Nb: 3%, Al: 5%, Ru: 0.2%, Ta: 2%, Y: 0.08%, La: 0.06%, Cr: 9%, Si: 1%, Re: 0.03%, B: 0.01% in terms of mass percentage, and the balance is Ni.

[0048] Reference Figure 5 The tensile strength of the measured component is 1530 MPa, and the elongation is 15.3%.

[0049] Example 4

[0050] An embodiment provided by the application is a 3D printing nickel-based superalloy powder in-situ nitride reinforced, which is consistent with the conditions of Example 1, except that the metal powder is prepared, and the specific chemical composition is Co: 15%, Nb: 3%, Al: 5%, Ru: 0.4%, Ta: 0.5%, Y: 0.08%, La: 0.06%, Cr: 9%, Si: 1%, Re: 0.03%, B: 0.01% in terms of mass percentage, and the balance is Ni.

[0051] Reference Figure 6 The tensile strength of the measured component is 1528 MPa, and the elongation is 15.2%.

[0052] Example 5

[0053] An embodiment provided by the application is a 3D printing nickel-based superalloy powder in-situ nitride reinforced, which is consistent with the conditions of Example 1, except that the metal powder is prepared, and the specific chemical composition is Co: 15%, Nb: 3%, Al: 5%, Ru: 0.4%, Ta: 2%, Y: 0.01%, La: 0.06%, Cr: 9%, Si: 1%, Re: 0.03%, B: 0.01% in terms of mass percentage, and the balance is Ni.

[0054] The tensile strength of the measured component is 1600 MPa, and the elongation is 16.3%.

[0055] Example 6

[0056] An embodiment provided by the application is a 3D printing in-situ nitride reinforced nickel-based superalloy powder, wherein the metal powder is prepared according to the following chemical composition: Co: 15%, Nb: 3%, Al: 5%, Ru: 0.4%, Ta: 2%, Y: 0.08%, La: 0.06%, Cr: 9%, Si: 0.6%, Re: 0.03%, B: 0.01%, and the balance is Ni.

[0057] The tensile strength of the zero-component part is 1603 MPa, and the elongation is 16.4%.

[0058] Example 7

[0059] An embodiment provided by the application is a 3D printing in-situ nitride reinforced nickel-based superalloy powder, wherein the metal powder is prepared according to the following chemical composition: Co: 15%, Nb: 3%, Al: 5%, Ru: 0.4%, Ta: 2%, Y: 0.08%, La: 0.06%, Cr: 9%, Si: 0.6%, Re: 0.03%, B: 0.01%, and the balance is Ni.

[0060] The tensile strength of the zero-component part is 1603 MPa, and the elongation is 16.4%.

[0061] Example 8

[0062] An embodiment provided by the application is a 3D printing in-situ nitride reinforced nickel-based superalloy powder, wherein the metal powder is prepared according to the following chemical composition: Co: 15%, Nb: 3%, Al: 5%, Ru: 0.4%, Ta: 2%, Y: 0.08%, La: 0.06%, Cr: 9%, Si: 0.6%, Re: 0.03%, B: 0.01%, and the balance is Ni.

[0063] The tensile strength of the zero-component part is 1603 MPa, and the elongation is 16.4%.

[0064] Example 9

[0065] An embodiment provided by the application is a 3D printing in-situ nitride reinforced nickel-based superalloy powder, wherein the metal powder is prepared according to the following chemical composition: Co: 15%, Nb: 3%, Al: 5%, Ru: 0.4%, Ta: 2%, Y: 0.08%, La: 0.06%, Cr: 9%, Si: 0.6%, Re: 0.03%, B: 0.01%, and the balance is Ni.

[0066] The tensile strength of the part is 1453 MPa, and the elongation is 15.1%.

[0067] Example 10

[0068] An embodiment provided by the application is a 3D printing in-situ nitride reinforced nickel-based superalloy powder, other conditions are the same as those in Example 1, and the difference is that the metal powder is prepared, and the specific chemical composition is Co: 15%, Nb: 3%, Al: 5%, Ru: 0.4%, Ta: 2%, Y: 0.08%, La: 0.06%, Cr: 9%, Si: 0.2%, Re: 0.03%, B: 0.01%, and the balance is Ni.

[0069] The tensile strength of the part is 1397 MPa, and the elongation is 14.3%.

[0070] Example 11

[0071] An embodiment provided by the application is a 3D printing in-situ nitride reinforced nickel-based superalloy powder, other conditions are the same as those in Example 1, and the difference is that the metal powder is prepared, and the specific chemical composition is Co: 15%, Nb: 3%, Al: 5%, Ru: 0.4%, Ta: 2%, Y: 0.08%, La: 0.06%, Cr: 9%, Si: 1%, Re: 0.01%, B: 0.01%, and the balance is Ni.

[0072] The tensile strength of the part is 1615 MPa, and the elongation is 16.5%.

[0073] The application provides a 3D printing in-situ nitride reinforced nickel-based superalloy powder, in the prepared nickel-based superalloy powder, the elements Nb, Ru, Ta, Y and La can improve the strength, hardness, wear resistance and high-temperature performance of the nickel-based alloy; the addition of the element Si enables the element Si to react with nitrogen in the forming environment under heating conditions during the 3D printing process, thereby in-situ generating dispersed fine reinforcing particles Si3N4, the existence of the second-phase reinforcing particles has a strong pinning effect on dislocations, grain boundaries and subgrain boundaries, so that the alloy is strengthened, and in particular, the high-temperature performance of the material is improved; the existence of the element Re plays a role of a catalyst, promotes the heating reaction of Si and nitrogen, and is beneficial to the generation of the reinforcing particles Si3N4. Through the component design of the 3D printing nickel-based superalloy, the tensile strength of the nickel-based superalloy at room temperature can be up to 1.62 GPa at the highest, and the elongation can be up to 16.8% at the highest.

[0074] It is apparent for a person skilled in the art that the present application is not limited to the details of the above-described exemplary embodiments, but that it can be implemented in other concrete forms without departing from the spirit or essential characteristics of the application. Therefore, the embodiments should be considered in all respects as illustrative and not restrictive, the scope of the application being defined by the appended claims rather than the above description, and all changes coming within the meaning and range of equivalency of the claims are therefore intended to be embraced therein, no reference signs in the claims being regarded as limiting the claim in which they are used.

Claims

1. A dispersion-strengthened nickel-based superalloy, characterized in that, The sum of the mass percentages of the components of the powder is 100% by mass, and includes: Co: 15%, Nb: 3%, Al: 5%, Ru: 0.4%, Ta: 2%, Y: 0.01-0.08%, La: 0.01-0.06%, Cr: 9%, Si: 1%, Re: 0.01-0.03%, B: 0.01%, and the balance being Ni; The dispersion-strengthened nickel-based superalloy is in-situ generated by 3D printing of nitrides, and the preparation steps include: S1: under vacuum conditions, the metal powder is prepared according to the mass percentages; S2: raw material smelting: the prepared metal powder is added into a smelting furnace for vacuum smelting, the smelting temperature is 1500 DEG C; when the vacuum degree of the furnace cavity is higher than 0.1 MPa, inert gas protection is filled, and the melt is obtained by degassing, and the degassing time is 9 min; S3: atomization powdering: the obtained melt is introduced into an atomization furnace for gas atomization treatment, a ring-hole conical nozzle is used for the gas atomization treatment, the diameter is 3.5 mm; the spray gas cone angle is 55 DEG, the atomization temperature is above 400 DEG C of the liquidus temperature; the spraying speed of the gas atomization treatment is controlled at 3.7 kg / min; the pressure in the gas atomization furnace is controlled at 0.25 bar; the pressure of the high-pressure atomization medium is controlled at 4.5 MPa; and screening treatment obtains the metal powder with a particle size range of 35-45 μm; S4: the 3D printed nickel-based superalloy powder is used as raw material to prepare a product by 3D printing, and the laser parameters for 3D printing of the above powder are as follows: the preheating temperature of the printing substrate is 150 DEG C; the laser scanning power is 280 W; the laser scanning speed is 800 mm / s; the scanning interval is 0.10 mm; and the layer thickness is 0.3 mm.

2. The dispersion-strengthened nickel-based superalloy of claim 1, wherein, The degassing treatment in step S2 has a degassing temperature of 1500 DEG C and a degassing time of 8-10 min.

3. The dispersion-strengthened nickel-based superalloy of claim 1, wherein, After the powder prepared in step S3 is placed in a drying box, the holding time is 16-20 hours, and the drying temperature is 70-90 DEG C.

4. The dispersion-strengthened nickel-based superalloy of claim 1, wherein, The inert gas is high-purity argon with a purity of 99.99%.

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