CN114351029A - SLM CoCrNi alloy based on grain boundary segregation enhancement and preparation method thereof - Google Patents
SLM CoCrNi alloy based on grain boundary segregation enhancement and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of medium entropy alloys, and discloses an SLM CoCrNi alloy enhanced based on grain boundary segregation and a preparation method thereof. The powder of the medium entropy alloy comprises the following components in percentage by mass: 31-34% of Co, 28-30% of Cr, 31-35% of Ni and 1-10% of TiC, and the average grain diameter of the added TiC adopted by the invention is 5 microns. Partial TiC is melted by using higher laser power, and C element is segregated along grain boundary in the solidification process, so that medium-entropy synthesis is inhibitedHeat crack of gold in SLM forming and simultaneous segregation behavior to induce TiC and Cr23C6And the grain boundary is generated, so that the strength of the entropy alloy part in SLM forming is improved.
Description
Technical Field
The invention belongs to the technical field of alloy materials, and particularly relates to a high-strength medium-entropy alloy material based on SLM forming and a preparation method thereof.
Background
Selective Laser Melting (SLM) is a revolutionary and promising additive manufacturing technique featuring ultra-high temperature rise and cooling rates, with solid-liquid interface cooling rates up to 10 in a tiny melt pool3-108K·s-1. Currently, SLM has been widely used in various fields such as aerospace industry, biomedical engineering, automobile industry, mold industry, and the like. The CoCrNi intermediate entropy alloy is widely concerned due to the excellent mechanical property and is an emerging front edge of the metal material boundary. As a novel solid solution alloy, the CoCrNi intermediate entropy alloy shows four different 'core effects' from the traditional alloy, namely a high entropy effect, a slow diffusion effect, a lattice distortion effect and a cocktail effect, so that the CoCrNi intermediate entropy alloy shows good mechanical properties. SLM is more favorable to promote the development of CoCrNi alloys than traditional manufacturing processes. On the one hand, the high-energy laser beam in the SLM can obtain parts close to full density by melting layer by layer; on the other hand, the rapid cooling action inhibits the diffusion of elements, prevents the formation of intermetallic compounds, and obtains a refined microstructure. Due to the rapid cooling behavior and lattice distortion effects, SLM manufacturing of crack-free, high density CoCrNi alloys becomes more and more difficult. Currently, an effective solution to thermal cracking is grain refinement. During SLM manufacturing, nanoparticles are introduced to control the nucleation process. It can provide a nucleation barrier of low energy. The method has been successfully applied to 7075 and 6060 series aluminum alloys. However,high-entropy alloy and medium-entropy alloy are used as emerging frontiers of metal material boundaries, and a perfect database is not provided for rapidly screening a proper nucleating agent. Meanwhile, nanoparticles (TiC and TiB) were used2) The thermal cracking of the CoCrNi alloy cannot be suppressed. Thus, grain refinement may not be suitable for improving thermal cracking of high and medium entropy alloys. However, during solidification, grain boundary segregation may directly affect the bonding behavior of the grains, and the solidification behavior of the molten pool may also be affected by the segregation elements. Therefore, the grain boundary segregation can suppress the occurrence of thermal cracks during SLM.
Theoretical basis of grain boundary segregation: the mechanism for suppressing the segregation of the thermal crack grain boundaries was analyzed from the energy point of view. The interfacial energy before solidification is solid-liquid interfacial energy (gamma)s) The interface energy after solidification is the crystal boundary energy (gamma)GB). Along with the solidification process, the columnar structure of the CoCrNi alloy gradually grows up along the heat flow direction, and a liquid film exists between the two columnar structures. At this time, the interfacial energy is equal to 2 γs. After complete solidification, the interfacial energy is equal to gammaGB. When 2 gamma iss>γGBThe total interface energy decreases. From an energy point of view, the stable existence of the liquid film is not facilitated. Therefore, the two columnar structures may attract each other, promoting adhesion of the two columnar structures. Meanwhile, the liquid film of the columnar structure is rapidly consumed, resulting in a shortened solidification time. When 2 gamma iss<γGBThe total interface energy is increased. Therefore, the two columnar structures may repel each other, delaying the adhesion of the two columnar structures. The solidification of the liquid film requires a lower degree of supercooling. The residence time in the solidification stage is extended. In order to analyze the influence of grain boundary segregation on the interface performance, a physical quantity W needs to be introducedd. It represents the work done by grain boundary bonding per unit area.
It is meant a pure alloy of the elements,
indicates an alloy having grain boundary segregation.
When the columnar structures attract each other from an energy point of view, the requirements of the principle must be satisfied:
namely:
orΔγs<ΔγGB(5)
therefore, the thermodynamic condition for inducing grain boundary coagulation by grain boundary segregation is that gamma is satisfied in the solidification processGBIs greater than gammas。
Disclosure of Invention
In order to solve the problem of thermal cracking of the CoCrNi alloy in the SLM preparation process, the invention adds the micron TiC, so that part of the TiC is melted at higher laser power, and in the solidification process, C element is segregated along the grain boundary, thereby promoting the consumption of liquid films among crystal grains, inhibiting the thermal cracking of the medium-entropy alloy in the SLM forming process, and simultaneously inducing TiC and Cr by segregation behavior23C6And the grain boundary is generated, so that the strength of the entropy alloy part in SLM forming is improved.
The invention content is as follows:
in order to inhibit the thermal cracking of the CoCrNi alloy in the SLM preparation process, the invention aims to provide an SLM preparation method and a powder formula for preparing a crack-free high-strength medium-entropy alloy through grain boundary segregation.
The purpose of the invention is realized by the following technical scheme:
an SLM CoCrNi alloy based on grain boundary segregation enhancement comprises the following components in percentage by mass: 33.48 percent of Co, 29.50 percent of Cr, 34.02 percent of Ni and 1 to 10 percent of TiC.
Furthermore, the content of Cr is obviously higher than that of Co and Ni, which is beneficial to improving the strength and high-temperature performance of the alloy.
Further, the paint comprises the following components in percentage by mass: co 33.48%, Cr 29.50%, Ni 34.02% and TiC 1-10%
Further, the average particle diameter of TiC particles is 5 μm.
Further, the particle size distribution of the CoCrNi alloy powder is 15-53 μm.
A preparation method of SLM CoCrNi alloy based on grain boundary segregation enhancement comprises the following steps:
(1) carrying out low-energy ball milling on CoCrNi alloy powder and TiC particles to obtain uniformly mixed powder;
(2) drying the ball-milled powder to remove water;
(3) drawing a three-dimensional model of a sample to be processed through three-dimensional modeling software SolidWorks, and storing the three-dimensional model as an STL format file;
(4) adding sufficient alloy powder into a powder cylinder before printing; because the forming cylinder and the powder cylinder of a common 3D printer are equal in size, the amount of the added alloy powder is not less than twice of the height of a formed part; before printing, inert protective gas is introduced into the printing chamber to ensure that the oxygen content in the printing chamber is less than 0.05%, and then printing and forming are started.
In the method, in the step (1), the ball milling rotation speed is 180rad, the ball milling time is 48h, and the ball-to-material ratio is 5: 1, the ball milling atmosphere is argon atmosphere.
In the method, in the step (2), the drying temperature is 80 ℃, the drying time is 24 hours, and the drying environment is a vacuum environment.
In the above method, in the step (4), the substrate is preheated to 180 ℃ before printing.
In the above method, in step (4), the parameters adopted by the entropy alloy in SLM preparation are set as: the laser power is 400-450w, the scanning speed is 600-1000mm/s, the powder layer thickness is 25-35 μm, and the scanning interval is 0.10-0.13 mm.
In the method, in the step (4), the flow of the inert protective gas is more than 1.2Lpm in the whole printing and forming process.
In the method, a part of TiC is melted by using higher laser power, and C element is segregated along a grain boundary in the solidification process, so that the thermal cracking of the medium-entropy alloy in SLM (selective laser melting) forming is inhibited.
In the above method, the segregation behavior induces TiC and Cr23C6Formed at grain boundaries, and Cr23C6The interface with the substrate is coherent. Thereby improving the strength of the entropy alloy part in SLM forming.
The SLM CoCrNi alloy powder reinforced based on grain boundary segregation and the forming process have the following advantages and beneficial effects:
compared with the prior art, the embodiment of the invention provides the SLM CoCrNi alloy powder enhanced based on grain boundary segregation and the forming process. The used micron TiC strengthens the CoCrNi alloy powder, thereby inhibiting hot cracks in the SLM process and simultaneously improving the strength of SLM forming parts, and particularly, the SLM CoCrNi alloy powder strengthened based on grain boundary segregation and the forming process have the following outstanding technical effects: at a laser power of 400-450w, the temperature of the molten pool will be higher, causing partial dissolution of the added TiC. Meanwhile, under high power, the cooling speed of the molten pool is reduced, so that dissolved C element is diffused along the grain boundary, the interface energy of the grain boundary is reduced, and the consumption of an intercrystalline liquid film is promoted, thereby inhibiting the generation of hot cracks. On the other hand, as shown in FIG. 1, the dissolved C element combines with the Cr element and the Ti element to form nano Cr23C6And nano TiC, so that the strength of the SLM CoCrNi alloy molded part is improved.
Drawings
FIG. 1 is a TEM photograph of a CoCrNi-3 wt% TiC sample, with TiC and Cr being predominant at grain boundaries23C6Mainly comprises the following steps.
FIG. 2 is a tensile curve of CoCrNi and CoCrNi-3 wt% TiC.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the embodiments of the present invention are not limited thereto, and may be carried out with reference to conventional techniques for process parameters not particularly noted.
Example 1
(1) 3000g of CoCrNi alloy powder + TiC powder (Co 33.48%, Cr 29.50%, Ni 34.02% and TiC 3%) were weighed, the particle size distribution of the CoCrNi alloy powder was 15-53 μm, and the average particle size of TiC was 5 μm.
(2) Carrying out low-energy ball milling on CoCrNi alloy powder and TiC particles to obtain uniformly mixed powder; the ball milling speed is 180rad, the ball milling time is 48h, and the ball-material ratio is 5: 1, the ball milling atmosphere is argon atmosphere.
(3) And drying the ball-milled powder to remove water, wherein the drying temperature is 80 ℃, the drying time is 24 hours, and the drying environment is a vacuum environment.
(4) And drawing a three-dimensional model of the sample to be processed by using three-dimensional modeling software SolidWorks, and storing the three-dimensional model as an STL format file.
(5) Adding sufficient alloy powder into a powder cylinder before printing; because the forming cylinder and the powder cylinder of a common 3D printer are equal in size, the amount of the added alloy powder is not less than twice of the height of a formed part; before printing, introducing inert protective gas into the printing chamber to ensure that the oxygen content in the printing chamber is less than 0.05%, and then starting printing and forming; in the whole printing and forming process, the flow of the inert protective gas is more than 1.2 Lpm.
(6) And (4) leading the file generated in the step (4) into equipment for SLM manufacturing, wherein the preheating temperature of the substrate is 180 ℃.
(7) SLM samples were prepared using a metal 3D printer with a laser power of 420W, a scanning speed of 800mm/s, a powder layer thickness of 30 μm and a scanning pitch of 0.11 mm.
The SLM CoCrNi alloy based on grain boundary segregation enhancement in the embodiment has yield strength of 1050MPa, elongation of 15.5% and no hot crack. The results are shown in FIG. 2. FIG. 2 is a tensile curve of a CoCrNi-3 wt% TiC alloy.
Example 2
(1) 3000g of CoCrNi alloy powder (Co 34.48%, Cr 31.50%, Ni 34.02%) was weighed out, and the particle size distribution of the CoCrNi alloy powder was 15 to 53 μm.
(2) Drying the powder to remove water, wherein the drying temperature is 80 ℃, the drying time is 24h, and the drying environment is a vacuum environment.
(3) And drawing a three-dimensional model of the sample to be processed by using three-dimensional modeling software SolidWorks, and storing the three-dimensional model as an STL format file.
(4) Adding sufficient alloy powder into a powder cylinder before printing; because the forming cylinder and the powder cylinder of a common 3D printer are equal in size, the amount of the added alloy powder is not less than twice of the height of a formed part; before printing, introducing inert protective gas into the printing chamber to ensure that the oxygen content in the printing chamber is less than 0.05%, and then starting printing and forming; in the whole printing and forming process, the flow of the inert protective gas is more than 1.2 Lpm.
(5) And (4) leading the file generated in the step (4) into equipment for SLM manufacturing, wherein the preheating temperature of the substrate is 180 ℃.
(6) SLM samples were prepared using a metal 3D printer with a laser power of 420W, a scanning speed of 800mm/s, a powder layer thickness of 30 μm and a scanning pitch of 0.11 mm.
The SLM CoCrNi alloy based on grain boundary segregation enhancement in the embodiment has the yield strength of 170Mpa and the elongation of 1.5 percent through measurement, and a large number of thermal cracks are found in the alloy. The results are shown in FIG. 2. FIG. 2 is a tensile curve of a CoCrNi alloy.
Example 3
(1) 3000g of CoCrNi alloy powder + TiC powder (Co 34.0%, Cr 30.0%, Ni 35.0% and TiC 1%) were weighed, the particle size distribution of the CoCrNi alloy powder was 15-53 μm, and the average particle size of TiC was 5 μm.
(2) Carrying out low-energy ball milling on CoCrNi alloy powder and TiC particles to obtain uniformly mixed powder; the ball milling speed is 180rad, the ball milling time is 48h, and the ball-material ratio is 5: 1, the ball milling atmosphere is argon atmosphere.
(3) And drying the ball-milled powder to remove water, wherein the drying temperature is 80 ℃, the drying time is 24 hours, and the drying environment is a vacuum environment.
(4) And drawing a three-dimensional model of the sample to be processed by using three-dimensional modeling software SolidWorks, and storing the three-dimensional model as an STL format file.
(5) Adding sufficient alloy powder into a powder cylinder before printing; because the forming cylinder and the powder cylinder of a common 3D printer are equal in size, the amount of the added alloy powder is not less than twice of the height of a formed part; before printing, introducing inert protective gas into the printing chamber to ensure that the oxygen content in the printing chamber is less than 0.05%, and then starting printing and forming; in the whole printing and forming process, the flow of the inert protective gas is more than 1.2 Lpm.
(6) And (4) leading the file generated in the step (4) into equipment for SLM manufacturing, wherein the preheating temperature of the substrate is 180 ℃.
(7) SLM samples were prepared using a metal 3D printer with a laser power of 420W, a scanning speed of 800mm/s, a powder layer thickness of 30 μm and a scanning pitch of 0.11 mm.
According to the embodiment, the SLM CoCrNi alloy enhanced based on the grain boundary segregation has the yield strength of 510Mpa and the elongation of 8 percent, the number of internal thermal cracks of the alloy is obviously reduced, but the thermal cracks are not completely disappeared.
Example 4
(1) 3000g of CoCrNi alloy powder + TiC powder (Co 33.48%, Cr 28.50%, Ni 33.02% and TiC 5%) were weighed, the particle size distribution of the CoCrNi alloy powder was 15-53 μm, and the average particle size of TiC was 5 μm.
(2) Carrying out low-energy ball milling on CoCrNi alloy powder and TiC particles to obtain uniformly mixed powder; the ball milling speed is 180rad, the ball milling time is 48h, and the ball-material ratio is 5: 1, the ball milling atmosphere is argon atmosphere.
(3) And drying the ball-milled powder to remove water, wherein the drying temperature is 80 ℃, the drying time is 24 hours, and the drying environment is a vacuum environment.
(4) And drawing a three-dimensional model of the sample to be processed by using three-dimensional modeling software SolidWorks, and storing the three-dimensional model as an STL format file.
(5) Adding sufficient alloy powder into a powder cylinder before printing; because the forming cylinder and the powder cylinder of a common 3D printer are equal in size, the amount of the added alloy powder is not less than twice of the height of a formed part; before printing, introducing inert protective gas into the printing chamber to ensure that the oxygen content in the printing chamber is less than 0.05%, and then starting printing and forming; in the whole printing and forming process, the flow of the inert protective gas is more than 1.2 Lpm.
(6) And (4) leading the file generated in the step (4) into equipment for SLM manufacturing, wherein the preheating temperature of the substrate is 180 ℃.
(7) SLM samples were prepared using a metal 3D printer with a laser power of 420W, a scanning speed of 800mm/s, a powder layer thickness of 30 μm and a scanning pitch of 0.11 mm.
The SLM CoCrNi alloy based on grain boundary segregation enhancement in the embodiment has yield strength of 1090MPa, elongation of 8% and disappearance of internal thermal cracks of the alloy through measurement.
Example 5
(1) 3000g of CoCrNi alloy powder and TiC powder (Co 32.48%, Cr 28.50%, Ni 31.02%, TiC 8%) were weighed, the particle size distribution of the CoCrNi alloy powder was 15-53 μm, and the average particle size of TiC was 5 μm.
(2) Carrying out low-energy ball milling on CoCrNi alloy powder and TiC particles to obtain uniformly mixed powder; the ball milling speed is 180rad, the ball milling time is 48h, and the ball-material ratio is 5: 1, the ball milling atmosphere is argon atmosphere.
(3) And drying the ball-milled powder to remove water, wherein the drying temperature is 80 ℃, the drying time is 24 hours, and the drying environment is a vacuum environment.
(4) And drawing a three-dimensional model of the sample to be processed by using three-dimensional modeling software SolidWorks, and storing the three-dimensional model as an STL format file.
(5) Adding sufficient alloy powder into a powder cylinder before printing; because the forming cylinder and the powder cylinder of a common 3D printer are equal in size, the amount of the added alloy powder is not less than twice of the height of a formed part; before printing, introducing inert protective gas into the printing chamber to ensure that the oxygen content in the printing chamber is less than 0.05%, and then starting printing and forming; in the whole printing and forming process, the flow of the inert protective gas is more than 1.2 Lpm.
(6) And (4) leading the file generated in the step (4) into equipment for SLM manufacturing, wherein the preheating temperature of the substrate is 180 ℃.
(7) SLM samples were prepared using a metal 3D printer with a laser power of 420W, a scanning speed of 800mm/s, a powder layer thickness of 30 μm and a scanning pitch of 0.11 mm.
The SLM CoCrNi alloy based on grain boundary segregation enhancement in the embodiment has the yield strength of 1100MPa, the elongation of 3 percent and no internal thermal crack of the alloy.
Example 6
(1) 3000g of CoCrNi alloy powder and TiC powder (Co 31.0%, Cr 28.0%, Ni 31.0%, TiC 10%) were weighed, the particle size distribution of the CoCrNi alloy powder was 15 to 53 μm, and the average particle size of TiC was 5 μm.
(2) Carrying out low-energy ball milling on CoCrNi alloy powder and TiC particles to obtain uniformly mixed powder; the ball milling speed is 180rad, the ball milling time is 48h, and the ball-material ratio is 5: 1, the ball milling atmosphere is argon atmosphere.
(3) And drying the ball-milled powder to remove water, wherein the drying temperature is 80 ℃, the drying time is 24 hours, and the drying environment is a vacuum environment.
(4) And drawing a three-dimensional model of the sample to be processed by using three-dimensional modeling software SolidWorks, and storing the three-dimensional model as an STL format file.
(5) Adding sufficient alloy powder into a powder cylinder before printing; because the forming cylinder and the powder cylinder of a common 3D printer are equal in size, the amount of the added alloy powder is not less than twice of the height of a formed part; before printing, introducing inert protective gas into the printing chamber to ensure that the oxygen content in the printing chamber is less than 0.05%, and then starting printing and forming; in the whole printing and forming process, the flow of the inert protective gas is more than 1.2 Lpm.
(6) And (4) leading the file generated in the step (4) into equipment for SLM manufacturing, wherein the preheating temperature of the substrate is 180 ℃.
(7) SLM samples were prepared using a metal 3D printer with a laser power of 420W, a scanning speed of 800mm/s, a powder layer thickness of 30 μm and a scanning pitch of 0.11 mm.
According to the embodiment, the SLM CoCrNi alloy based on grain boundary segregation enhancement has the yield strength of 630MPa and the elongation of 4 percent, and a small amount of cracks appear in the alloy.
It should be understood that the above detailed description of the embodiments of the present invention with reference to the preferred embodiments is illustrative and not restrictive, and it should not be considered that the detailed description of the embodiments of the present invention is limited thereto, and it should be understood that those skilled in the art to which the present invention pertains that modifications may be made to the embodiments described in the embodiments or that equivalents may be substituted for some of the features thereof without departing from the spirit of the present invention and the scope of the patent protection is defined by the claims to be filed with the present invention.
Claims (10)
1. An SLM CoCrNi alloy based on grain boundary segregation enhancement is characterized by comprising the following components in percentage by mass: 31-34% of Co, 28-30% of Cr, 31-35% of Ni and 1-10% of TiC.
2. The SLM CoCrNi alloy enhanced based on grain boundary segregation as claimed in claim 1, characterized by comprising by mass percent: 33.48 percent of Co, 29.50 percent of Cr, 34.02 percent of Ni and 1 to 10 percent of TiC.
3. The grain boundary segregation-based enhanced SLM CoCrNi alloy according to claim 1, characterized in that the average grain size of the TiC particles is 5 μ ι η.
4. The SLM CoCrNi alloy enhanced based on grain boundary segregation as claimed in claim 1, wherein the particle size distribution of the CoCrNi alloy powder is 15-53 μm.
5. The method for preparing the SLM CoCrNi alloy based on grain boundary segregation enhancement according to claim 1, is characterized in that: the method comprises the following steps:
(1) carrying out low-energy ball milling on CoCrNi alloy powder and TiC particles to obtain uniformly mixed powder;
(2) drying the ball-milled powder to remove water;
(3) drawing a three-dimensional model of a sample to be processed through three-dimensional modeling software SolidWorks, and storing the three-dimensional model as an STL format file;
(4) adding sufficient alloy powder into a powder cylinder before printing; because the forming cylinder and the powder cylinder of a common 3D printer are equal in size, the amount of the added alloy powder is not less than twice of the height of a formed part; before printing, inert protective gas is introduced into the printing chamber to ensure that the oxygen content in the printing chamber is less than 0.05%, and then printing and forming are started.
6. The method for preparing the SLM CoCrNi alloy based on grain boundary segregation enhancement according to claim 5, wherein the method comprises the following steps: in the step (1), the ball milling rotation speed is 180rad, the ball milling time is 48h, and the ball-to-material ratio is 5: 1, the ball milling atmosphere is argon atmosphere.
7. The method for preparing the SLM CoCrNi alloy based on grain boundary segregation enhancement according to claim 5, wherein the method comprises the following steps: in the step (2), the drying temperature is 80 ℃, the drying time is 24 hours, and the drying environment is a vacuum environment.
8. The method for preparing the SLM CoCrNi alloy based on grain boundary segregation enhancement according to claim 5, wherein the method comprises the following steps: in step (4), the substrate is preheated to 180 ℃ before printing.
9. The method for preparing the SLM CoCrNi alloy based on grain boundary segregation enhancement according to claim 5, wherein the method comprises the following steps: in the step (4), the parameters adopted by the entropy alloy in the SLM preparation are set as follows: the laser power is 400-450w, the scanning speed is 600-1000mm/s, the powder layer thickness is 25-35 μm, and the scanning interval is 0.10-0.13 mm.
10. The method for preparing the SLM CoCrNi alloy based on grain boundary segregation enhancement according to claim 5, wherein the method comprises the following steps: in the step (4), the flow of the inert protective gas is more than 1.2Lpm in the whole printing and forming process.
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|---|---|---|---|---|
| CN115533116A (en) * | 2022-09-19 | 2022-12-30 | 华东理工大学 | Multicomponent alloy composite material and preparation method thereof |
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| CN116727686A (en) * | 2023-06-09 | 2023-09-12 | 广东工业大学 | Method for manufacturing CoCrNi medium entropy alloy by TiC ceramic powder reinforced laser additive |
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