CN114101704B - High-strength TC4-BN alloy containing mixed structures of equiaxed crystals and columnar crystals and preparation method thereof - Google Patents

High-strength TC4-BN alloy containing mixed structures of equiaxed crystals and columnar crystals and preparation method thereof Download PDF

Info

Publication number
CN114101704B
CN114101704B CN202111390873.4A CN202111390873A CN114101704B CN 114101704 B CN114101704 B CN 114101704B CN 202111390873 A CN202111390873 A CN 202111390873A CN 114101704 B CN114101704 B CN 114101704B
Authority
CN
China
Prior art keywords
alloy
powder
ball milling
strength
crystals
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202111390873.4A
Other languages
Chinese (zh)
Other versions
CN114101704A (en
Inventor
王利卿
张震
赵占勇
白培康
李晓峰
王宇
刘斌
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
North University of China
Original Assignee
North University of China
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by North University of China filed Critical North University of China
Priority to CN202111390873.4A priority Critical patent/CN114101704B/en
Publication of CN114101704A publication Critical patent/CN114101704A/en
Application granted granted Critical
Publication of CN114101704B publication Critical patent/CN114101704B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/20—Direct sintering or melting
    • B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/60—Treatment of workpieces or articles after build-up
    • B22F10/64—Treatment of workpieces or articles after build-up by thermal means
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00—Processes of additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
    • B33Y40/20—Post-treatment, e.g. curing, coating or polishing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C22C1/058—Mixtures of metal powder with non-metallic powder by reaction sintering (i.e. gasless reaction starting from a mixture of solid metal compounds)
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C14/00—Alloys based on titanium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • C22F1/18—High-melting or refractory metals or alloys based thereon
    • C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Structural Engineering (AREA)
  • Composite Materials (AREA)
  • Civil Engineering (AREA)
  • Ceramic Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Plasma & Fusion (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses a high-strength TC4-BN alloy containing mixed structures of equiaxed crystals and columnar crystals and a preparation method thereof, wherein the BN addition amount in the TC4-BN alloy is 0.3 to 0.8 weight percent, and the microstructure of the alloy presents the mixed structures of the equiaxed crystals and the columnar crystals with micron dimensions, and the compressive strength reaches 1600 to 2200MPa. The preparation method comprises the following steps: sieving BN powder and TC4 powder, mixing the BN powder and the TC4 powder with stainless steel balls in proportion, and placing the mixture in a ball milling tank; uniformly mixing TC4 powder and BN powder by using a planetary ball mill, and then preserving the mixture by vacuum packaging; taking the mixed powder as a raw material, taking TC4 alloy as a substrate, and 3D printing by using SLM equipment to prepare TC4-BN alloy; and (5) integrally placing the substrate and the 3D printing piece in a vacuum annealing furnace for stress relief annealing. The invention forms the mixed structure of equiaxed crystal and columnar crystal in the titanium alloy prepared by SLM by adding BN, and the mixed structure is mixed with TiB and TiB 2 The TiN synergistic strengthening obviously improves the alloy strength; the transformation of the 3D printing titanium alloy microstructure from columnar crystal to equiaxial crystal and columnar crystal mixed structure is realized.

Description

High-strength TC4-BN alloy containing mixed structures of equiaxed crystals and columnar crystals and preparation method thereof
Technical Field
The invention belongs to the technical field of additive manufacturing, and particularly relates to a high-strength TC4-BN alloy containing mixed structures of equiaxed crystals and columnar crystals and a preparation method thereof.
Technical Field
The molten pool formed by 3D printing of the metal material has small size and large temperature gradient, so that the characteristics of epitaxial growth are shown between layers, coarse columnar grains are generated along the construction direction, and the remarkable performance anisotropy, the mechanical property reduction and the hot cracking tendency increase are further caused. In contrast, a fine equiaxed grain structure may improve performance anisotropy, which is beneficial for reducing thermal stress and reducing thermal cracking tendency. Therefore, the replacement of coarse columnar crystals with fine equiaxed crystals is an important direction for the 3D printing research of metallic materials. The key point of the columnar crystal orientation equiaxial crystal transformation is that the nucleation rate in a molten pool is greatly improved, and the current technical method comprises the steps of regulating and controlling technological parameters, changing the temperature gradient and the solidification rate of the molten pool, applying ultrasonic vibration in the 3D printing process, alloying design and introducing heterogeneous nucleation points. The introduction of heterogeneous nuclear particles has certain influence on alloy components, and meanwhile, the application range is wider, the dependency on equipment is smaller, and the method has very high practical application value.
For titanium alloys, common heterogeneous nucleating agents include C, B, si, rare earth oxides, and the like. The B is a very efficient heterogeneous nucleating agent, and beta grains which are precipitated first can be obviously thinned in the traditional cast titanium alloy and the 3D printing titanium alloy, but the strength of the B is not obviously improved, so that the B becomes a main factor for limiting the application of the B in the titanium alloy, particularly the 3D printing titanium alloy. Therefore, adding a third alloying element to B to obtain equiaxed grains and improving the alloy strength becomes a new search direction.
Disclosure of Invention
Aiming at the problem of performance anisotropy caused by 3D printing titanium alloy columnar crystals, the preparation of the high-strength titanium alloy containing fine equiaxed crystal and columnar crystal mixed structures is successfully realized by adding BN and adopting a laser selective melting (SLM) technology, and technical support is provided for 3D printing titanium alloy microstructure and mechanical property regulation.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the high-strength TC4-BN alloy containing mixed structures of equiaxed crystals and columnar crystals, wherein the addition amount of BN in the high-strength TC4-BN alloy is 0.3 to 0.8 weight percent, and the alloy has the mixed structures of the equiaxed crystals and the columnar crystals, and the compressive strength of the alloy reaches 1600 to 2200MPa.
The preparation method of the high-strength TC4-BN alloy with the mixed structure of the equiaxed crystal and the columnar crystal comprises the following steps:
(1) Screening irregular BN powder and spherical TC4 alloy powder, mixing the obtained BN powder, TC4 alloy powder and stainless steel balls in proportion, placing the mixture in a ball milling tank, and vacuumizing the ball milling tank;
(2) Fixing a ball milling tank in a planetary ball mill for ball milling, uniformly mixing the two powders, and vacuum packaging and storing the obtained powder after ball milling;
(3) Taking TC4 and BN mixed powder as raw materials, taking TC4 alloy as a substrate, and 3D printing by using SLM equipment to prepare TC4-BN alloy;
(4) And (3) integrally placing the substrate and the 3D printing part in a vacuum annealing furnace, vacuumizing, filling high-purity argon, performing stress relief annealing, and finally cooling to room temperature along with the furnace to obtain the high-strength TC4-BN alloy.
In the step (1), after sieving, the obtained BN powder has a particle size of 1-3 mu m, TC4 alloy powder has a particle size of 15-53 mu m, the diameter of the stainless steel ball is 3mm, the mass ratio of the stainless steel ball to the powder is 3:1-8:1, and the pressure in the ball milling tank is below 0.05MPa after the ball milling tank is vacuumized.
Further, the ball milling process parameters in the step (2) include: the rotating speed is 200-300 r/min, the ball milling time is 2-4 hours, and the starting and stopping time ratio of the ball mill is 1:1-2:1.
Further, the parameters used by the SLM in the step (3) are: the laser power is 180-300W, the laser scanning speed is 400-1200 mm/s, the laser scanning interval is 0.08-0.16 mm, the powder spreading thickness is 45 mu m, the laser scanning path adopts a checkerboard scanning strategy with a rotation angle of 67 degrees, and the oxygen content in a bin is maintained below 0.15wt% in the printing process.
Further, a preferred embodiment of the present invention: in the step (4), the stress relief annealing treatment is carried out, and the pressure in the furnace reaches 1 multiplied by 10 -3 And (3) filling high-purity argon after Pa, wherein the annealing temperature is 450-650 ℃, the heat preservation time is 0.5-2 hours, and then cooling to room temperature along with a furnace.
The beneficial effects are that:
1. according to the invention, the BN powder and the TC4 alloy powder are uniformly mixed by using a ball milling method, and the TC4 alloy powder still maintains high sphericity through reasonable setting of the ball-material ratio, the ball milling time and the start-stop time, so that the requirements of the SLM powder spreading process on the morphology and the flowability of the powder can be met, and the smooth execution of the SLM forming process is ensured.
2. The invention takes BN as a heterogeneous nucleating agent, and utilizes the reaction of BN and titanium alloy melt to generate TiB, tiB2 and TiN, thereby forming heterogeneous nucleation points at the front edge of a solid-liquid interface to improve the nucleation rate of the titanium alloy melt, finally forming a large number of fine equiaxed crystals with the size below 5 mu m in the titanium alloy, and simultaneously refining the width of columnar crystals to below 20 mu m. The refining effect is obviously higher than C, B, B 4 C, etc. Fine grain strengthening, second phase strengthening (TiB ) 2 And TiN) to improve the compressive strength of the titanium alloy to more than 2000MPa, thereby realizing the regulation and control of the microstructure and mechanical properties of the 3D printed titanium alloy.
3. The invention discloses a whole set of technical method for high-strength TC4-BN alloy containing mixed structures of equiaxed crystals and columnar crystals, which specifically comprises a powder raw material preparation process, a 3D printing process and a heat treatment process. The technology has the characteristics of low cost and wide application range, and the 3D printing alloy component uniform distribution, defect control and microstructure regulation and control are successfully realized through reasonable matching of BN addition and a laser scanning strategy. Provides a new idea and method for improving the mechanical property of the 3D printing titanium alloy and expanding the application field of the 3D printing titanium alloy.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a graph showing the morphology of TC4-BN alloy powder obtained by ball milling and distribution of Ti and B elements;
FIG. 2 is a graph showing the appearance of internal pore defects of the TC4-BN alloy prepared by the invention;
FIG. 3 shows the metallographic structure of TC4-BN alloy prepared by the invention;
FIG. 4 is a graph showing the room temperature compressive stress strain curve of the TC4-BN alloy prepared by the invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A high-strength TC4-BN alloy containing mixed structures of equiaxed crystals and columnar crystals and a preparation method thereof comprise the following steps:
(1) Sieving BN powder and TC4 alloy powder respectively, mixing the obtained BN powder with the particle size of 1-3 mu m, TC4 alloy powder with the particle size of 15-53 mu m and stainless steel balls with the diameter of 3mm in proportion, placing the mixture into a ball milling tank, wherein the adding amount of BN is 0.5wt%, the mass ratio of the stainless steel balls to the powder is 4:1, and vacuumizing the ball milling tank to ensure that the pressure in the tank is below 0.05 MPa.
(2) Fixing a ball milling tank in a planetary ball mill for ball milling, wherein the rotating speed is 250r/min, the ball milling time is 3 hours, the starting-stopping time ratio of the ball mill is 2:1, enabling the two powders to be uniformly mixed, and then carrying out vacuum packaging and preservation on the obtained powders.
(3) Taking TC4-0.5wt% BN mixed powder as a raw material, taking TC4 alloy as a substrate, and performing 3D printing by using SLM equipment to prepare the TC4-BN alloy, wherein the laser power is 200W, the laser scanning speed is 600mm/s, the laser scanning interval is 0.1mm, the powder laying thickness is 45 mu m, the laser scanning path adopts a checkerboard scanning strategy with a rotation angle of 67 degrees, and the oxygen content in a bin is maintained below 0.15wt% in the printing process.
(4) Placing the substrate and the 3D printing piece into a vacuum annealing furnace integrally, and vacuumizing to enable the pressure in the furnace to reach 1 multiplied by 10 -3 And (3) filling high-purity argon after Pa, performing stress relief annealing at 500 ℃ for 1 hour, and cooling to room temperature along with a furnace.
The morphology of the TC4-0.5wt% BN mixed powder prepared by the embodiment and the distribution of Ti and B elements are shown as shown in figure 1, so that the powder still maintains higher sphericity, and the B elements are uniformly distributed on the surface of the TC4 alloy powder, thereby providing qualified powder raw materials for an SLM process. The defect morphology and metallographic structure of the prepared TC4-0.5wt% BN alloy are shown as figures 2 and 3, and the defect morphology and metallographic structure of the prepared TC4-0.5wt% BN alloy do not form obvious cracks in the alloy, only have a small number of micropores with the size of less than 5 mu m, and the alloy consists of fine equiaxed crystals with the size of less than 5 mu m and columnar crystals with the width of less than 20 mu m. The room temperature compressive stress strain curve of the prepared TC4-0.5wt% BN alloy is shown in figure 4, and the compressive strength of the alloy is up to about 1900MPa. In a word, the preparation of the high-strength TC4-BN alloy with the mixed structure of the equiaxed crystal and the columnar crystal is realized through the embodiment, and the purposes of 3D printing of the microstructure and mechanical property regulation and control of the titanium alloy are achieved.
Example 2
A high-strength TC4-BN alloy containing mixed structures of equiaxed crystals and columnar crystals and a preparation method thereof comprise the following steps:
(1) Sieving BN powder and TC4 alloy powder respectively, mixing the obtained BN powder with the particle size of 1-3 mu m, TC4 alloy powder with the particle size of 15-53 mu m and stainless steel balls with the diameter of 3mm in a ball milling tank according to a proportion, wherein the adding amount of BN is 0.3wt%, the mass ratio of the stainless steel balls to the powder is 3:1, and vacuumizing the ball milling tank to ensure that the pressure in the tank is below 0.05 MPa.
(2) Fixing a ball milling tank in a planetary ball mill for ball milling, wherein the rotating speed is 300r/min, the ball milling time is 2 hours, the starting-stopping time ratio of the ball mill is 2:1, enabling the two powders to be uniformly mixed, and then carrying out vacuum packaging and preservation on the obtained powder.
(3) Taking TC4-0.3wt% BN mixed powder as a raw material, taking TC4 alloy as a substrate, and performing 3D printing by using SLM equipment to prepare the TC4-BN alloy, wherein the laser power is 180W, the laser scanning speed is 1200mm/s, the laser scanning interval is 0.08mm, the powder laying thickness is 45 mu m, the laser scanning path adopts a checkerboard scanning strategy with a rotation angle of 67 degrees, and the oxygen content in a bin is maintained below 0.15wt% in the printing process.
(4) Placing the substrate and the 3D printing piece into a vacuum annealing furnace integrally, and vacuumizing to enable the pressure in the furnace to reach 1 multiplied by 10 -3 And (3) filling high-purity argon after Pa, performing stress relief annealing at the annealing temperature of 450 ℃ for 2 hours, and cooling to room temperature along with a furnace.
The morphology and Ti and B element distribution of the TC4-0.3wt% BN mixed powder of the embodiment are shown in the figure, and the defect morphology and metallographic structure of the prepared TC4-0.3wt% BN alloy are similar to those of the embodiment 1 and are not provided. The compressive strength of the TC4-0.3wt% BN alloy prepared by the embodiment reaches about 1600MPa, the preparation of the high-strength TC4-BN alloy containing the mixed structure of equiaxed crystals and columnar crystals is realized by the embodiment, and the purpose of regulating and controlling the microstructure and the mechanical properties of the 3D printing titanium alloy is achieved.
Example 3
A high-strength TC4-BN alloy containing mixed structures of equiaxed crystals and columnar crystals and a preparation method thereof comprise the following steps:
(1) Sieving BN powder and TC4 alloy powder respectively, mixing the obtained BN powder with the particle size of 1-3 mu m, TC4 alloy powder with the particle size of 15-53 mu m and stainless steel balls with the diameter of 3mm in proportion, placing the mixture into a ball milling tank, wherein the adding amount of BN is 0.8wt%, the mass ratio of the stainless steel balls to the powder is 8:1, and vacuumizing the ball milling tank to ensure that the pressure in the tank is below 0.05 MPa.
(2) Fixing a ball milling tank in a planetary ball mill for ball milling, wherein the rotating speed is 200r/min, the ball milling time is 4 hours, the starting-stopping time ratio of the ball mill is 1:1, enabling the two powders to be uniformly mixed, and then carrying out vacuum packaging and preservation on the obtained powder.
(3) Taking TC4-0.8wt% BN mixed powder as a raw material, taking TC4 alloy as a substrate, and performing 3D printing by using SLM equipment to prepare the TC4-BN alloy, wherein the laser power is 300W, the laser scanning speed is 400mm/s, the laser scanning interval is 0.16mm, the powder laying thickness is 45 mu m, the laser scanning path adopts a checkerboard scanning strategy with a rotation angle of 67 degrees, and the oxygen content in a bin is maintained below 0.15wt% in the printing process.
(4) Placing the substrate and the 3D printing piece into a vacuum annealing furnace integrally, and vacuumizing to enable the pressure in the furnace to reach 1 multiplied by 10 -3 And (3) filling high-purity argon after Pa, performing stress relief annealing at 650 ℃ for 0.5 hour, and cooling to room temperature along with a furnace.
The morphology and Ti and B element distribution of the TC4-0.8wt% BN mixed powder of the embodiment are shown in the figure, and the defect morphology and metallographic structure of the prepared TC4-0.8wt% BN alloy are similar to those of the embodiment 1 and are not provided. The compressive strength of the TC4-0.8wt% BN alloy prepared by the embodiment reaches about 2200MPa, the preparation of the high-strength TC4-BN alloy containing the mixed structure of the equiaxed crystal and the columnar crystal is realized by the embodiment, and the purpose of regulating and controlling the microstructure and the mechanical property of the 3D printing titanium alloy is achieved.
Example 4
A high-strength TC4-BN alloy containing mixed structures of equiaxed crystals and columnar crystals and a preparation method thereof comprise the following steps:
(1) Sieving BN powder and TC4 alloy powder respectively, mixing the obtained BN powder with the particle size of 1-3 mu m, TC4 alloy powder with the particle size of 15-53 mu m and stainless steel balls with the diameter of 3mm in proportion, placing the mixture into a ball milling tank, wherein the adding amount of BN is 0.4wt%, the mass ratio of the stainless steel balls to the powder is 5:1, and vacuumizing the ball milling tank to ensure that the pressure in the tank is below 0.05 MPa.
(2) Fixing a ball milling tank in a planetary ball mill for ball milling, wherein the rotating speed is 250r/min, the ball milling time is 3 hours, the starting-stopping time ratio of the ball mill is 2:1, enabling the two powders to be uniformly mixed, and then carrying out vacuum packaging and preservation on the obtained powders.
(3) Taking TC4-0.4wt% BN mixed powder as a raw material, taking TC4 alloy as a substrate, and performing 3D printing by using SLM equipment to prepare the TC4-BN alloy, wherein the laser power is 220W, the laser scanning speed is 1000mm/s, the laser scanning interval is 0.12mm, the powder laying thickness is 45 mu m, the laser scanning path adopts a checkerboard scanning strategy with a rotation angle of 67 degrees, and the oxygen content in a bin is maintained below 0.15wt% in the printing process.
(4) Placing the substrate and the 3D printing piece into a vacuum annealing furnace integrally, and vacuumizing to enable the pressure in the furnace to reach 1 multiplied by 10 -3 And (3) filling high-purity argon after Pa, carrying out stress relief annealing at 550 ℃ for 1.5 hours, and cooling to room temperature along with a furnace.
The morphology and Ti and B element distribution of the TC4-0.4wt% BN mixed powder of the embodiment are shown in the figure, and the defect morphology and metallographic structure of the prepared TC4-0.4wt% BN alloy are similar to those of the embodiment 1 and are not provided. The compressive strength of the TC4-0.4wt% BN alloy prepared by the embodiment reaches about 1800MPa, the preparation of the high-strength TC4-BN alloy containing the mixed structure of equiaxed crystals and columnar crystals is realized by the embodiment, and the purpose of regulating and controlling the microstructure and the mechanical properties of the 3D printing titanium alloy is achieved.
Example 5
A high-strength TC4-BN alloy containing mixed structures of equiaxed crystals and columnar crystals and a preparation method thereof comprise the following steps:
(1) Sieving BN powder and TC4 alloy powder respectively, mixing the obtained BN powder with the particle size of 1-3 mu m, TC4 alloy powder with the particle size of 15-53 mu m and stainless steel balls with the diameter of 3mm in proportion, placing the mixture into a ball milling tank, wherein the adding amount of BN is 0.6wt%, the mass ratio of the stainless steel balls to the powder is 5:1, and vacuumizing the ball milling tank to ensure that the pressure in the tank is below 0.05 MPa.
(2) Fixing a ball milling tank in a planetary ball mill for ball milling, wherein the rotating speed is 250r/min, the ball milling time is 4 hours, the starting-stopping time ratio of the ball mill is 1:1, enabling the two powders to be uniformly mixed, and then carrying out vacuum packaging and preservation on the obtained powders.
(3) Taking TC4-0.6wt% BN mixed powder as a raw material, taking TC4 alloy as a substrate, and performing 3D printing by using SLM equipment to prepare the TC4-BN alloy, wherein the laser power is 240W, the laser scanning speed is 600mm/s, the laser scanning interval is 0.14mm, the powder laying thickness is 45 mu m, the laser scanning path adopts a checkerboard scanning strategy with a rotation angle of 67 degrees, and the oxygen content in a bin is maintained below 0.15wt% in the printing process.
(4) Placing the substrate and the 3D printing piece into a vacuum annealing furnace integrally, and vacuumizing to enable the pressure in the furnace to reach 1 multiplied by 10 -3 And (3) filling high-purity argon after Pa, carrying out stress relief annealing at 550 ℃ for 1.5 hours, and cooling to room temperature along with a furnace.
The morphology and Ti and B element distribution of the TC4-0.6wt% BN mixed powder of the embodiment are shown in the graph, and the defect morphology graph and metallographic structure graph of the prepared TC4-0.6wt% BN alloy are similar to those of the embodiment 1 and are not provided. The compressive strength of the TC4-0.6wt% BN alloy prepared by the embodiment reaches about 2000MPa, the preparation of the high-strength TC4-BN alloy containing the mixed structure of equiaxed crystals and columnar crystals is realized by the embodiment, and the purposes of 3D printing of the microstructure and mechanical property regulation of the titanium alloy are achieved.
Although embodiments of the present invention have been described above, it will be apparent to those skilled in the art that modifications and substitutions can be made without departing from the principles and spirit of the invention.

Claims (6)

1. The high-strength TC4-BN alloy containing mixed structures of equiaxed crystals and columnar crystals is characterized in that: the addition amount of BN in the high-strength TC4-BN alloy is 0.3 to 0.8 weight percent, the alloy has a mixed structure of equiaxed crystals and columnar crystals, and the compressive strength of the alloy reaches 1600 to 2200MPa.
2. The preparation method of the high-strength TC4-BN alloy with the mixed structure of the equiaxed crystal and the columnar crystal is characterized by comprising the following steps of: the method comprises the following steps:
(1) Screening irregular BN powder and spherical TC4 alloy powder, mixing the obtained BN powder, TC4 alloy powder and stainless steel balls in proportion, placing the mixture in a ball milling tank, and vacuumizing the ball milling tank;
(2) Fixing a ball milling tank in a planetary ball mill for ball milling, uniformly mixing the two powders, and vacuum packaging and storing the obtained powder after ball milling;
(3) Taking TC4 and BN mixed powder as raw materials, taking TC4 alloy as a substrate, and 3D printing by using SLM equipment to prepare TC4-BN alloy;
(4) And (3) integrally placing the substrate and the 3D printing part in a vacuum annealing furnace, vacuumizing, filling high-purity argon, performing stress relief annealing, and finally cooling to room temperature along with the furnace to obtain the high-strength TC4-BN alloy.
3. The preparation method according to claim 2, characterized in that: in the step (1), after sieving, the grain diameter of the obtained BN powder is 1-3 mu m, the grain diameter of the TC4 alloy powder is 15-53 mu m, the diameter of the stainless steel ball is 3mm, the mass ratio of the stainless steel ball to the powder is 3:1-8:1, and the pressure in the ball milling tank is below 0.05MPa after the ball milling tank is vacuumized.
4. The preparation method according to claim 2, characterized in that: the ball milling process parameters in the step (2) comprise: the rotating speed is 200-300 r/min, the ball milling time is 2-4 hours, and the starting and stopping time ratio of the ball mill is 1:1-2:1.
5. The preparation method according to claim 2, characterized in that: the parameters used by the SLM in the step (3) are as follows: the laser power is 180-300W, the laser scanning speed is 400-1200 mm/s, the laser scanning interval is 0.08-0.16 mm, the powder spreading thickness is 45 mu m, the laser scanning path adopts a checkerboard scanning strategy with a rotation angle of 67 degrees, and the oxygen content in a bin is maintained below 0.15wt% in the printing process.
6. The preparation method according to claim 2, characterized in that: in the stress relief annealing treatment in the step (3), the pressure in the furnace reaches 1×10 -3 Post Pa charge heightPure argon gas, annealing temperature of 450-650 deg.c and heat preservation time of 0.5-2 hr, and cooling to room temperature in the furnace.
CN202111390873.4A 2021-11-23 2021-11-23 High-strength TC4-BN alloy containing mixed structures of equiaxed crystals and columnar crystals and preparation method thereof Active CN114101704B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111390873.4A CN114101704B (en) 2021-11-23 2021-11-23 High-strength TC4-BN alloy containing mixed structures of equiaxed crystals and columnar crystals and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111390873.4A CN114101704B (en) 2021-11-23 2021-11-23 High-strength TC4-BN alloy containing mixed structures of equiaxed crystals and columnar crystals and preparation method thereof

Publications (2)

Publication Number Publication Date
CN114101704A CN114101704A (en) 2022-03-01
CN114101704B true CN114101704B (en) 2023-11-28

Family

ID=80439526

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111390873.4A Active CN114101704B (en) 2021-11-23 2021-11-23 High-strength TC4-BN alloy containing mixed structures of equiaxed crystals and columnar crystals and preparation method thereof

Country Status (1)

Country Link
CN (1) CN114101704B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115433851B (en) * 2022-10-20 2024-01-16 西北工业大学 Preparation method of low-cost high-strength and high-toughness 3D printing Ti-Fe-O alloy

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10265867A (en) * 1997-03-25 1998-10-06 Hitachi Ltd High performance alloy, its production and use
CN103710662A (en) * 2013-12-18 2014-04-09 大连海事大学 Oxide thermal barrier coating with micron/nanometer equiaxed crystal structure and preparation method for oxide thermal barrier coating
CN111118339A (en) * 2020-01-06 2020-05-08 华南理工大学 Si-containing high-strength low-modulus medical titanium alloy and additive manufacturing method and application thereof
CN111215624A (en) * 2018-11-26 2020-06-02 南京工业大学 Addition of B4Method for improving additive manufacturing titanium alloy microstructure through in-situ self-generation of C nano particles
CN111230113A (en) * 2020-02-28 2020-06-05 沈阳工业大学 Method for preparing TC4/TiAl gradient material by synchronously feeding powder through laser
CN111644614A (en) * 2019-06-05 2020-09-11 南京工业大学 Additive manufacturing alloy powder based on adjustment and control of mismatching degree of titanium alloy and boron carbide particles
CN112593106A (en) * 2020-11-26 2021-04-02 首都航天机械有限公司 Laser additive manufacturing method capable of conveniently obtaining fine equiaxed grains
JP2021080519A (en) * 2019-11-19 2021-05-27 日本製鉄株式会社 α+β TYPE TITANIUM ALLOY ROD STOCK, AND MANUFACTURING METHOD OF α+β TYPE TITANIUM ALLOY ROD STOCK

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10265867A (en) * 1997-03-25 1998-10-06 Hitachi Ltd High performance alloy, its production and use
CN103710662A (en) * 2013-12-18 2014-04-09 大连海事大学 Oxide thermal barrier coating with micron/nanometer equiaxed crystal structure and preparation method for oxide thermal barrier coating
CN111215624A (en) * 2018-11-26 2020-06-02 南京工业大学 Addition of B4Method for improving additive manufacturing titanium alloy microstructure through in-situ self-generation of C nano particles
CN111644614A (en) * 2019-06-05 2020-09-11 南京工业大学 Additive manufacturing alloy powder based on adjustment and control of mismatching degree of titanium alloy and boron carbide particles
JP2021080519A (en) * 2019-11-19 2021-05-27 日本製鉄株式会社 α+β TYPE TITANIUM ALLOY ROD STOCK, AND MANUFACTURING METHOD OF α+β TYPE TITANIUM ALLOY ROD STOCK
CN111118339A (en) * 2020-01-06 2020-05-08 华南理工大学 Si-containing high-strength low-modulus medical titanium alloy and additive manufacturing method and application thereof
CN111230113A (en) * 2020-02-28 2020-06-05 沈阳工业大学 Method for preparing TC4/TiAl gradient material by synchronously feeding powder through laser
CN112593106A (en) * 2020-11-26 2021-04-02 首都航天机械有限公司 Laser additive manufacturing method capable of conveniently obtaining fine equiaxed grains

Also Published As

Publication number Publication date
CN114101704A (en) 2022-03-01

Similar Documents

Publication Publication Date Title
CN110218907B (en) Boron-containing titanium-based composite powder for 3D printing and preparation method thereof
WO2021077598A1 (en) Thermal treatment method with controllable additive manufacturing aluminum alloy strength and elongation
CN109022920B (en) Crack-free 4D printing titanium-nickel shape memory alloy and preparation method thereof
EP2951332B1 (en) Sputter target with Ga-Na, In-Na or Ga-In-Na intermetallic phases
CN111872386A (en) 3D printing process method of high-strength aluminum-magnesium alloy
CN109778050B (en) WVTaTiZr refractory high-entropy alloy and preparation method thereof
CN114101704B (en) High-strength TC4-BN alloy containing mixed structures of equiaxed crystals and columnar crystals and preparation method thereof
CN111850332A (en) 3D printing process method of high-strength aluminum-zinc alloy
JPWO2014077110A1 (en) Cu-Ga alloy sputtering target and method for producing the same
CN108555297B (en) Method for eliminating primary β grain boundary of TC4 alloy by adding B induction heating during laser additive manufacturing
Ren et al. Effects of different heat treatments on anisotropy of cold sprayed 7075 Al deposits
CN116727684A (en) TiAl-based light high-temperature material based on laser 3D printing and preparation method thereof
CN108531784B (en) Method for preparing aluminum-titanium-magnesium ternary intermetallic compound powder by mechanical alloying
CN113909733B (en) Aluminum magnesium alloy welding wire for arc fuse additive manufacturing and preparation method thereof
TW201343941A (en) Cu-Ga alloy sputtering target and its manufacturing method
CN116079072A (en) Method for providing high silicon aluminum alloy performance and high silicon aluminum alloy
CN112775436B (en) Manufacturing method for promoting titanium alloy additive manufacturing process to generate isometric crystals
CN110253000B (en) Preparation method of multi-grain-scale multi-layer high-entropy alloy
CN109986061B (en) Preparation method of multi-scale precipitated lamellar structure magnesium alloy
CN113444908B (en) Ti-Zr-B grain refiner, preparation method thereof and application thereof in magnesium alloy
CN109943738A (en) One kind magnesium-rare earth of high-modulus containing aluminium and preparation method thereof
CN115070052B (en) Novel bimodal tissue nickel-titanium shape memory alloy, 4D printing preparation method and application thereof
CN115074580B (en) Ni 2 Al 3 -TiC high-temperature alloy refiner, preparation method and application
CN115725874B (en) TiAlCrre alloy with strength and plasticity and preparation method thereof
CN108044124B (en) Preparation method of near-eutectic Nb-Si-Mo alloy with lamellar structure oriented arrangement characteristic

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant