CN114525425A - MC type carbide reinforced nickel-based superalloy composite material, preparation method and application thereof - Google Patents
MC type carbide reinforced nickel-based superalloy composite material, preparation method and application thereof Download PDFInfo
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Abstract
An MC type carbide reinforced nickel-based high-temperature alloy composite material, a preparation method and an application thereof belong to the field of high-temperature alloy materials. The MC type carbide reinforced nickel-based high-temperature alloy composite material consists of an austenite matrix phase and a large amount of MC type carbide reinforced phases which are dispersed and distributed. Wherein, the MC type carbide reinforcing phase is induced and separated out by the added high melting point nano carbide ceramic particles. The preparation method comprises the following steps: 1) and ball-milling and mixing the high-melting-point carbide nano powder and the Ni micron powder, and wrapping the mixture by using a nickel foil to obtain a uniformly mixed powder bag. 2) And putting the powder packet and the nickel-based high-temperature alloy block material with the surface oxides and the greasy dirt removed into a crucible of a vacuum smelting furnace for smelting together, refining for 2-8 min under the condition of high superheat temperature of 1500-1550 ℃, cooling to 1400-1470 ℃, and casting into ingots to obtain the MC type carbide dispersion reinforced nickel-based high-temperature alloy composite material. The invention can solve the problems of low product strength and poor toughness of aerospace products under the high-superheat-degree pouring condition; the production cost is low, the process is simple, the equipment is not limited, and the method is suitable for industrial production.
Description
Technical Field
The invention belongs to the field of high-temperature alloy materials, and relates to an MC type carbide reinforced nickel-based high-temperature alloy composite material, a preparation method and an application thereof.
Background
The nickel-based casting high-temperature alloy for aerospace has a wide service temperature range, can be stably used at the temperature of-196-850 ℃ for a long time, has excellent low/high temperature strength, corrosion resistance, cold and hot workability, weldability, high-temperature creep resistance, high-temperature oxidation resistance and other excellent performances, and is one of the most used component materials in the aerospace manufacturing industry. With the continuous improvement of the demand of a liquid power system, the liquid oxygen kerosene rocket engine needs to burn a large amount of propellant in a short time, and the thrust, the specific impulse and the pressure of a combustion chamber are continuously increased. In order to overcome the severe service environment, the core components of the engine have increasingly complex structures, and the manufacturing difficulty coefficient is increased continuously. Under the development trend of 'large size, integration, precision and complicated structure' of aerospace product high-temperature alloy parts, high pouring temperature and high shell heat preservation temperature are needed for investment precision casting so as to facilitate mold filling. The slow cooling rate allows sufficient time for the grains and large-size skeletal carbides to grow. The tip of the large-size skeleton-shaped carbide becomes a local stress concentration point, so that the crack is easy to nucleate and expand, and the medium-low temperature mechanical property is comprehensively expressed as low.
In recent decades, the development of high-toughness nickel-based cast superalloy has been the focus of scientific research workers and has resulted in numerous results. The refiner for precision investment casting of the high-temperature alloy is mostly externally added with micron-sized particles, and the externally added nano-particles are used as the refiner for precision investment casting of the nickel-based high-temperature alloy in fewer reports. Representative examples are: potentilla knight-errant et al obtained a fine-grained ingot by introducing a preformed master alloy of W-Co-Cr-C into a superalloy (patent application No. CN110872652. A). The method needs electromagnetic stirring and rapid pouring, and as aerospace products are mostly complex structural parts, the pouring is usually carried out under the process of high pouring temperature and proper time heat preservation, the refiner can be melted, and the refining effect is limited. For complex structures, electromagnetic stirring may not even allow sufficient convection of the melt. Huangpoliten et al prepared TiC-enhanced nickel-based composite material (patent application No. CN106319288.B) by introducing micron-sized TiC-Ti-C preform and by in-situ reaction, however, the size and volume fraction of the enhanced phase of the in-situ generated nickel-based composite material were highly uncontrollable, and the raw material which did not react completely could be used as impurity, which seriously affects the performance of the nickel-based superalloy. Wangrui et al successfully prepared TiN-reinforced nickel-based composites [ Wangrui. Journal of Alloys and composites, 762(2018) 237-.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides an MC type carbide reinforced nickel-based high-temperature alloy composite material, and a preparation method and application thereof. The MC type carbide reinforced nickel-based high-temperature alloy composite material prepared by the method has the advantages of greatly improving the strength and the toughness, adopting an investment precision casting technology, having low cost, not needing to change the production process of the original aerospace product, and perfectly adapting to the industrial requirements of enterprises. And the high-melting point nano carbide ceramic particles become a precipitation substrate of the MC type carbide, so that the volume fraction of the MC type carbide is increased, the MC type carbide is dispersed and precipitated in a crystal boundary and a crystal interior, and the appearance is changed from a thick long chain shape to a fine particle shape. In addition, the high-melting-point nano ceramic particles and the induced and precipitated granular MC type carbide also serve as nucleating agents to refine grains, so that the plasticity is improved; the grain boundary and a large amount of granular carbides which are dispersed and distributed in the grain boundary can effectively prevent the nucleation and further expansion of cracks, help the matrix to transfer load, generate an Orowan effect and a load transfer effect, and increase the strength.
In order to achieve the purpose, the invention adopts the technical scheme that:
the MC type carbide reinforced nickel-base high-temperature alloy composite material consists of an austenite matrix phase and a large amount of MC type carbide reinforced phases which are dispersed. Wherein, the MC type carbide reinforcing phase is induced and separated out by adding high melting point nano carbide ceramic particles.
A preparation method of an MC type carbide reinforced nickel-based superalloy composite material comprises the following steps:
(1) placing a proper amount of high-melting-point carbide nano powder and Ni micron powder in a stainless steel ball milling tank according to the mass ratio of 1: 1.5-2, vacuumizing, and introducing argon to prevent the Ni powder from being oxidized in the ball milling process. And placing the stainless steel ball milling tank in a planetary ball mill for mechanical ball milling and mixing, setting the ball milling rotation speed to be 300-500 rpm/min, setting the ball milling time to be 30-60 min, and wrapping the mixed powder subjected to ball milling with nickel foil to obtain a mixed powder bag A. In the step, Ni micron powder is used as a carrier for adding carbide nano powder into the melt, so that the agglomeration of the nano powder is reduced.
(2) Blowing sand to remove an oxide layer on the nickel-based high-temperature alloy block, placing the nickel-based high-temperature alloy block and a casting mould in a drying furnace together, and drying the nickel-based high-temperature alloy block and the casting mould to remove oil stains on the surfaces of the alloy block and the casting mould, wherein the casting mould is dried and then subjected to heat preservation treatment. The drying temperature is 200 ℃, and the drying time is 4 h. The mass ratio of the mass of the nickel-based high-temperature alloy block to the mass of the mixed powder packet A is 100: 0.5-3.
(3) Placing the mixed powder packet A obtained in the step (1) at the bottom of a melting crucible of a vacuum induction melting furnace, placing the nickel-based high-temperature alloy lump material with the oxide layer and the surface oil stain removed in the step (2) at the upper part of the mixed powder packet A in the melting crucible, melting for 30-60 min at 1400-1500 ℃, and then refining for 2-8 min at the temperature of 1500-1550 ℃ and high superheat degree, wherein the refining aims to ensure that the melt is sufficiently convected under the action of induced current and the added solid nano carbide particles are uniformly distributed. And (3) cooling to 1400-1470 ℃, quickly pouring the cooled alloy into the dried and insulated casting mold in the step (2), and inducing a large amount of MC type carbide to be dispersed and separated out by solid nano carbide particles uniformly distributed in the melt in the solidification process to obtain the MC type carbide reinforced nickel-based high-temperature alloy composite ingot.
Further, the grain diameter of the high-melting-point carbide nano powder in the step (1) is 40-500 nm, the carbide type is one or more of carbide types contained in the nickel-based high-temperature alloy, such as TiC, MoC, NbC and the like, and the purity is more than or equal to 99.99%.
Further, the particle size distribution range of the Ni micro-rice powder in the step (1) is 40-70 μm, and the purity is more than or equal to 99.99%.
Further, the nickel-based superalloy in the step (2) is any one of the grades of nickel-based superalloys, such as K35, K4169, K4202 and the like.
Further, the MC type carbide component in the step (3) is (Ti, W, Mo, Nb, etc.) C, and the actual specific component is determined by the kind of the strong carbide forming element contained in the selected Ni-based superalloy.
Further, the gas atomization method can be flexibly selected according to specific metal alloys, for example, the EIGA method can be selected for titanium alloys, and the VIGA method can be selected for high-temperature alloys, stainless steel and aluminum alloys.
The application of the MC type carbide reinforced nickel-based high-temperature alloy composite material is applied to the field of additive manufacturing. During the powdering process of the precast ingot containing the nano ceramic particles, the nano ceramic particles can regulate and control the solidification process of metal liquid drops, and formed micron spherical crystals are smaller and more uniform in components.
The invention has the following beneficial effects:
(1) the invention does not change the original production process of aerospace products, and the nickel-based casting high-temperature alloy with fine crystal grains and excellent medium-low temperature mechanical properties can be obtained only by putting the nano ceramic carbide particles and the nickel-based high-temperature alloy into a crucible for smelting during smelting and feeding.
(2) The nickel-base cast superalloy itself contains MC type carbide having (Ti, W, Mo, Nb..) C or the like as a component. Therefore, high melting point nano carbide particles such as TiC, MoC, NbC and the like are selected and introduced and cannot be used as impurities.
(3) The high-melting-point nano carbide particles can be used as a precipitation substrate of MC type carbide in the nickel-based high-temperature alloy to promote the precipitation of the MC type carbide, and the MC type carbide is dispersed in a crystal boundary and a crystal interior and is changed from a thick long chain shape into fine particles in appearance. A large amount of dispersed MC carbide can generate an orowan effect and a load transfer effect, and the strength is improved.
(4) The high-melting-point nano carbide ceramic particles and the MC type carbide which is induced and precipitated are used as solidification nucleating agents, so that the growth of columnar crystals during casting solidification and the abnormal growth of the crystal grains during solution aging treatment are inhibited, and the plasticity is increased.
(5) The nano ceramic particles can improve the grain size, the shape, the orientation and the mechanical property of a printed product in the printing process when being applied to the field of additive manufacturing.
Drawings
FIG. 1(a) is a phase diagram of MC type carbide gold inside a sample under comparative example conditions; FIG. 1(b) is a phase diagram of MC type carbide gold in the sample under the conditions of example 1;
FIG. 2(a) is an SEM image of MC type carbide inside a sample under comparative example conditions; FIG. 2(b) SEM image of MC type carbide inside the sample under the conditions of example 1, and FIGS. 2(c) and 2(d) are EDS energy spectra of the indicated positions of FIGS. 2(a) and 2(d), respectively;
FIG. 3 is a graph comparing the room temperature performance of investment precision castings prepared under the conditions of comparative example and example 1;
FIG. 4 is an SEM image of spherical powder for additive manufacturing prepared by an aerosolization process of an MC/K4202 nickel-base superalloy composite material prepared under the conditions of example 1;
FIG. 5 is a graph comparing the room temperature performance of comparative example and the MC/K4202 nickel-base superalloy composite spherical powder printed additive manufactured part of FIG. 3.
Detailed Description
The present invention will be described in detail with reference to specific examples. To assist the skilled person in further understanding the invention. The technical parameters related to the present invention are only an optimal value, and are not limited to specific values in the embodiments, and a person skilled in the art can make several modifications without departing from the core of the present invention, but all of them fall within the protection scope of the present invention.
Comparative example:
the MC type carbide reinforced nickel-base high temperature alloy composite material has no added nanometer carbide ceramic powder and the nickel-base high temperature alloy K4202 as example and includes the following steps:
(1) placing 400g of Ni micron powder in a stainless steel ball milling tank, vacuumizing, and introducing argon to prevent the Ni micron powder from being oxidized in the ball milling process. And placing the stainless steel ball milling tank in a planetary ball mill for mechanical ball milling and mixing, setting the ball milling rotation speed to be 450rpm/min and the ball milling time to be 50min, and wrapping the mixed powder subjected to ball milling by nickel foil to obtain the Ni powder bag.
(2) Weighing 20kg of K4202 nickel-based high-temperature alloy lump material, blowing sand to remove an oxide layer, and placing the lump material and a casting mold in a drying furnace together to remove greasy dirt on the surface of the lump material and the casting mold, wherein the drying temperature is 200 ℃, and the drying time is 4 hours.
(3) Placing the Ni powder bag weighed in the step (1) at the bottom of a melting crucible of a vacuum induction melting furnace, placing the nickel-based superalloy block material with the oxide layer and the surface oil stain removed in the step (2) at the upper part of the Ni powder bag in the melting crucible, melting at 1500 ℃ for 60min, and refining at 1520 ℃ and high superheat degree for 5min, so that the melt is sufficiently convected under the action of induction current to promote the uniform distribution of the added solid nano carbide particles. And (3) cooling to 1450 ℃, and quickly pouring the alloy into the casting mold dried and insulated in the step (2) to obtain the K4202 nickel-based high-temperature alloy cast ingot.
(4) The K4202 nickel-based superalloy ingot is converted into superalloy spherical powder for additive manufacturing through a gas atomization method. Specifically, EIGA electrode induction melting gas atomization method is adopted to prepare metal-based composite powder, and an atomization chamber and a smelting chamber are vacuumized to 10 degrees-3Pa, introducing argon to reach micro-positive pressure, wherein the pressure of the smelting chamber is slightly higher than that of the atomizing chamber, the technological parameters of the atomizing pressure is 3.8MPa, the smelting power is 18kW, the gas atomizing temperature is 40 ℃, the superheat degree is 230 ℃, and the high-temperature alloy spherical powder is prepared.
Example 1:
an MC type carbide reinforced nickel-based high temperature alloy composite material and a preparation method thereof, taking TiC with the grain diameter of 40nm, taking K4202 nickel-based high temperature alloy as an example, the preparation method comprises the following steps:
(1) 200g of 40nm TiC powder and 400g of Ni micron powder are placed in a stainless steel ball milling tank, argon is introduced after vacuumizing, and oxidation of the Ni micron powder in the ball milling process is prevented. And placing the stainless steel ball milling tank in a planetary ball mill for mechanical ball milling and mixing, setting the ball milling rotation speed to be 450rpm/min and the ball milling time to be 50min, and wrapping the mixed powder subjected to ball milling by nickel foil to obtain the TiC-Ni mixed powder bag.
(2) Weighing 20kg of K4202 nickel-based high-temperature alloy lump material, blowing sand to remove an oxide layer, and placing the lump material and a casting mold in a drying furnace together to remove greasy dirt on the surface of the lump material and the casting mold, wherein the drying temperature is 200 ℃, and the drying time is 4 hours.
(3) Placing the TiC-Ni mixed powder bag weighed in the step (1) at the bottom of a melting crucible of a vacuum induction melting furnace, placing the nickel-based high-temperature alloy lump material with the oxide layer and the surface oil stain removed in the step (2) at the upper part of the TiC-Ni mixed powder bag in the melting crucible, melting for 60min at 1500 ℃, and then refining for 5min under the condition of high superheat temperature of 1520 ℃, so that the melt is fully convected under the action of induced current to promote the uniform distribution of the added solid nano carbide particles. And (3) cooling to 1450 ℃, and quickly pouring the mixture into the casting mold which is dried and insulated in the step (2), so as to obtain the composite material cast ingot.
(4) And converting the composite material ingot into metal alloy composite powder reinforced by nano ceramic particles by an air atomization method. Specifically, EIGA electrode induction melting gas atomization method is adopted to prepare metal-based composite powder, and an atomization chamber and a smelting chamber are vacuumized to 10 degrees-3Pa, introducing argon to reach micro-positive pressure, wherein the pressure of the smelting chamber is slightly higher than that of the atomizing chamber, the technological parameters of the atomizing pressure is 3.8MPa, the smelting power is 18kW, the gas atomizing temperature is 40 ℃, and the superheat degree is 230 ℃, so as to prepare the metal-based composite powder.
Example 2:
an MC type carbide reinforced nickel-based high-temperature alloy composite material and a preparation method thereof, wherein MoC with the grain diameter of 500nm is taken as an example, K35 nickel-based high-temperature alloy is taken as the nickel-based high-temperature alloy, and the preparation method comprises the following steps:
(1) 40g of 500nm MoC powder and 60gNi micron powder are placed in a stainless steel ball milling tank, argon is introduced after vacuum pumping, and oxidation of the Ni micron powder in the ball milling process is prevented. And placing the stainless steel ball milling tank in a planetary ball mill for mechanical ball milling and mixing, setting the ball milling rotation speed at 300rpm/min and the ball milling time at 60min, and wrapping the mixed powder subjected to ball milling by using nickel foil to obtain the MoC-Ni mixed powder bag.
(2) Weighing 20kg of K35 nickel-based superalloy lump material, blowing sand to remove an oxide layer, and placing the lump material and a casting mold in a drying furnace together to remove greasy dirt on the surfaces of the lump material and the casting mold, wherein the drying temperature is 200 ℃, and the drying time is 4 hours.
(3) And (2) placing the MoC-Ni mixed powder bag weighed in the step (1) at the bottom of a melting crucible of a vacuum induction melting furnace, placing the nickel-based high-temperature alloy lump material with the oxide layer and the surface oil stain removed in the step (2) at the upper part of the MoC-Ni mixed powder bag in the melting crucible, melting for 45min at 1530 ℃, and then refining for 8min at 1500 ℃ and high superheat degree, so that the melt is fully convected under the action of induced current, and the added solid nano carbide particles are promoted to be uniformly distributed. And (3) cooling to 1400 ℃, and quickly pouring the mixture into the casting mold which is dried and insulated in the step (2).
Example 3:
an MC type carbide reinforced nickel-based high-temperature alloy composite material, a preparation method and an application thereof, NbC with the grain diameter of 500nm is taken, and K4169 nickel-based high-temperature alloy is taken as an example of the nickel-based high-temperature alloy, and the preparation method comprises the following steps:
(1) 100g of 500nm NbC powder and 180gNi micron powder are placed in a stainless steel ball milling tank, argon is introduced after vacuum pumping, and oxidation of the Ni micron powder in the ball milling process is prevented. And placing the stainless steel ball milling tank in a planetary ball mill for mechanical ball milling and mixing, setting the ball milling rotation speed at 500rpm/min and the ball milling time at 30min, and wrapping the mixed powder subjected to ball milling by using nickel foil to obtain the NbC-Ni mixed powder bag.
(2) Weighing 20kg of K4169 nickel-based superalloy lump material, blowing sand to remove an oxide layer, and placing the lump material and a casting mold in a drying furnace together to remove greasy dirt on the surfaces of the lump material and the casting mold, wherein the drying temperature is 200 ℃, and the drying time is 4 hours.
(3) Placing the NbC-Ni mixed powder bag weighed in the step (1) at the bottom of a melting crucible of a vacuum induction melting furnace, placing the nickel-based high-temperature alloy block material with the oxide layer and the surface oil stain removed in the step (2) at the upper part of the NbC-Ni mixed powder bag in the melting crucible, melting for 30min at 1550 ℃, and then refining for 2min at the high superheat temperature of 1550 ℃, so that the melt is fully convected under the action of induced current to promote the uniform distribution of the added solid nano carbide particles. And (3) cooling to 1470 ℃ and pouring into the dried and insulated casting mould in the step (2).
The results of the comparative and example show that: fig. 1(a) and 1(b) show that after high-melting-point nano carbide ceramic particles are introduced into the nickel-base superalloy, precipitated carbides are changed into fine particles from original long-strip skeletons, and the volume fraction is increased. FIGS. 2(a) and 2(b) show that the carbides precipitated in the comparative example and the example 1 are MC type carbides in the K4202 nickel-base superalloy; the results in fig. 3 show that the room temperature strength, yield strength and elongation are all improved for example 1 over the comparative example. The MC type carbide reinforced nickel-based high-temperature alloy composite material prepared by the method can also be used for an air atomization method to prepare the MC type carbide containing nickel-based high-temperature alloy composite material spherical powder, and the powder morphology is shown in figure 4. Figure 5 shows that room temperature strength, yield strength and elongation of parts printed with this powder are also improved. Example 1 has found application in investment casting of certain hot end components of aerospace products and additive manufacturing of the hot end components.
The above-mentioned embodiments only express the embodiments of the present invention, but not should be understood as the limitation of the scope of the invention patent, it should be noted that, for those skilled in the art, many variations and modifications can be made without departing from the concept of the present invention, and these all fall into the protection scope of the present invention.
Claims (7)
1. A preparation method of MC type carbide reinforced nickel-based high-temperature alloy composite material is characterized in that the MC type carbide reinforced nickel-based high-temperature alloy composite material consists of an austenite matrix phase and a large amount of dispersed MC type carbide reinforced phases, and the preparation method comprises the following steps:
(1) mechanically ball-milling and mixing the high-melting-point nano carbide powder and the Ni micro-rice powder according to the mass ratio of 1: 1.5-2, and wrapping by using nickel foil to obtain a mixed powder packet A;
(2) blowing sand to remove an oxide layer on the nickel-based high-temperature alloy block, placing the nickel-based high-temperature alloy block and a casting mould in a drying furnace together, and drying the nickel-based high-temperature alloy block and the casting mould to remove oil stains on the surfaces of the alloy block and the casting mould, wherein the casting mould is dried and then subjected to heat preservation treatment; the mass ratio of the mass of the nickel-based high-temperature alloy block to the mass of the mixed powder packet A is 100: 0.5-3;
(3) placing the mixed powder packet A obtained in the step (1) at the bottom of a melting crucible of a vacuum induction melting furnace, placing the nickel-based high-temperature alloy lump material with the oxide layer and the surface oil stain removed in the step (2) at the upper part of the mixed powder packet A in the melting crucible, melting for 30-60 min at 1400-1500 ℃, and then refining for 2-8 min at the temperature of 1500-1550 ℃ and high superheat degree, wherein the refining aims to ensure that the melt is sufficiently convected under the action of induced current and the added solid nano carbide particles are uniformly distributed; and (3) cooling to 1400-1470 ℃, quickly pouring the mixture into the casting mould dried and insulated in the step (2), and inducing a large amount of MC type carbide to be dispersed and separated out by solid nano carbide particles uniformly distributed in a melt in the solidification process to obtain the MC type carbide reinforced nickel-based high-temperature alloy composite ingot.
2. The preparation method of the MC type carbide reinforced nickel-based superalloy composite material according to claim 1, wherein the rotation speed of mechanical ball milling in the step (1) is 300-500 rpm/min, and the ball milling time is 30-60 min.
3. The method for preparing the MC type carbide reinforced nickel-base superalloy composite material according to claim 1, wherein the drying temperature in the step (2) is 200 ℃ and the drying time is 4 hours.
4. The preparation method of the MC type carbide reinforced nickel-based superalloy composite material according to claim 1, wherein the grain size of the high-melting-point carbide nano powder in the step (1) is 40-500 nm, the carbide type is the carbide type contained in the nickel-based superalloy, and the purity is more than or equal to 99.99%.
5. The preparation method of the MC type carbide reinforced nickel-based superalloy composite material as claimed in claim 1, wherein the Ni micron powder in the step (1) has a particle size distribution range of 40-70 μm and a purity of not less than 99.99%.
6. An MC type carbide reinforced nickel-base superalloy composite material prepared by the method of any one of claims 1 to 8, wherein the MC type carbide reinforced nickel-base superalloy composite material is composed of an austenite matrix phase and a plurality of MC type carbide reinforced phases in a dispersed manner; wherein, the MC type carbide reinforcing phase is induced and separated out by adding high melting point nano carbide ceramic particles.
7. The application of the MC type carbide reinforced nickel-based superalloy composite material as described in claim 6, wherein the composite material is applied to the field of additive manufacturing, a composite material ingot is converted into metal alloy composite powder reinforced by nano ceramic particles, and the metal alloy composite powder with the particle size required in the additive manufacturing process is obtained through screening.
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| CN116334422A (en) * | 2023-03-17 | 2023-06-27 | 西安航天发动机有限公司 | Forming method capable of realizing grain refinement of K4202 superalloy |
| CN116815004A (en) * | 2023-06-08 | 2023-09-29 | 辽宁红银金属有限公司 | Cobalt-based superalloy and preparation method thereof |
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