CN113210627A - Preparation method of carbide-reinforced TiAl-based nanocomposite - Google Patents
Preparation method of carbide-reinforced TiAl-based nanocomposite Download PDFInfo
- Publication number
- CN113210627A CN113210627A CN202110423531.1A CN202110423531A CN113210627A CN 113210627 A CN113210627 A CN 113210627A CN 202110423531 A CN202110423531 A CN 202110423531A CN 113210627 A CN113210627 A CN 113210627A
- Authority
- CN
- China
- Prior art keywords
- tial
- powder
- carbide
- composite material
- electron beam
- 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.)
- Pending
Links
- 229910010038 TiAl Inorganic materials 0.000 title claims abstract description 94
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 89
- 239000000463 material Substances 0.000 claims abstract description 52
- 238000010894 electron beam technology Methods 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 36
- 239000002245 particle Substances 0.000 claims abstract description 35
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 31
- 239000000956 alloy Substances 0.000 claims abstract description 31
- 238000002844 melting Methods 0.000 claims abstract description 29
- 230000008018 melting Effects 0.000 claims abstract description 22
- 238000000498 ball milling Methods 0.000 claims abstract description 21
- 238000005516 engineering process Methods 0.000 claims abstract description 21
- 239000002105 nanoparticle Substances 0.000 claims abstract description 20
- 230000008569 process Effects 0.000 claims abstract description 17
- 239000000919 ceramic Substances 0.000 claims abstract description 16
- 239000011812 mixed powder Substances 0.000 claims abstract description 12
- 238000012545 processing Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 239000010410 layer Substances 0.000 claims description 32
- 238000010309 melting process Methods 0.000 claims description 17
- 239000000758 substrate Substances 0.000 claims description 17
- 239000007787 solid Substances 0.000 claims description 16
- 238000005094 computer simulation Methods 0.000 claims description 10
- 238000003892 spreading Methods 0.000 claims description 10
- 230000007480 spreading Effects 0.000 claims description 10
- 238000007596 consolidation process Methods 0.000 claims description 5
- 238000010422 painting Methods 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 239000002356 single layer Substances 0.000 claims description 5
- 239000011159 matrix material Substances 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 239000000654 additive Substances 0.000 abstract description 3
- 230000000996 additive effect Effects 0.000 abstract description 3
- 230000003014 reinforcing effect Effects 0.000 abstract description 2
- 239000002131 composite material Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 5
- 238000000879 optical micrograph Methods 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 229910052758 niobium Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910052720 vanadium Inorganic materials 0.000 description 3
- 206010067484 Adverse reaction Diseases 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000006838 adverse reaction Effects 0.000 description 2
- 230000002902 bimodal effect Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000008646 thermal stress Effects 0.000 description 2
- 238000009827 uniform distribution Methods 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 239000011156 metal matrix composite Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000004781 supercooling Methods 0.000 description 1
Images
Classifications
-
- B22F1/0003—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
-
- 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
- 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
-
- 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
- B33Y80/00—Products made by additive manufacturing
-
- 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
- C22C1/045—Alloys based on refractory metals
- C22C1/0458—Alloys based on titanium, zirconium or hafnium
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Civil Engineering (AREA)
- Composite Materials (AREA)
- Structural Engineering (AREA)
- Powder Metallurgy (AREA)
Abstract
A preparation method of carbide reinforced TiAl-based nano composite material comprises the following steps: (1) selecting TiC ceramic particles with purity of more than 99.9% and particle size of 50-500nm and TiAl alloy powder with particle size of 45-150 μm as raw materials; (2) mixing the two materials by using a mechanical ball milling method to obtain pre-mixed powder with TiC nano particles uniformly distributed on the surface of TiAl alloy powder, wherein the weight of the TiC nano particles accounts for 0.7-1.2 wt% of the total weight of the mixed powder; (3) and (3) utilizing an electron beam melting technology to form and prepare the TiAl-based nano composite material layer by layer until the processing of the three-dimensional block sample is finished. And adding a semi-melting step in the electron beam melting forming process to finally obtain the nearly fully-compact carbide-reinforced TiAl-based nano composite material. The adjustable range of technological parameters in the forming process is large, the microstructure of the matrix is uniform, the reinforcing phase is fine and dispersed, and the mechanical property is good. The preparation method of the TiAl-based nano composite material has the characteristics and advantages of electron beam additive manufacturing, and has great application potential in the field of aerospace.
Description
Technical Field
The invention belongs to the technical field of TiAl-based composite materials and additive manufacturing, and relates to a forming process of a carbide-reinforced TiAl-based composite material added with TiC ceramic nanoparticles based on an electron beam melting technology.
Background
The TiAl alloy has high specific elastic modulus, high specific strength, high temperature oxidation resistance and high temperature creep resistance, and thus has wide application foreground in aerospace structure material. But the intrinsic brittleness and difficult processability limit its large-scale application. The nano-particle compounding is expected to improve the mechanical property of the TiAl alloy. Ti2The AlC phase has good toughness and can effectively hinder the crack from expanding. Compared with graphite and carbon nano tubes, the composite material prepared by adding TiC serving as a carbon source into TiAl alloy can obtain higher hardness and strength.
The existing TiAl-based composite material preparation methods comprise a casting method and a powder metallurgy method. However, because the ceramic particles and the metal matrix have different thermal expansion coefficients and wettability, the technology can cause the agglomeration of the nano particles and the adverse reaction of the nano particles and TiAl melt, cause gas inclusion and thermal stress, and cause the phenomena of holes, cracks, poor interface bonding and the like. In addition, the traditional technology has complex process and higher cost, and is difficult to prepare parts with complex shapes.
The Electron Beam Melting (EBM) technology can prepare parts with complex structures by melting and forming solid parts through powder layer by layer, shortens the production period and has great application prospect in the field of aerospace. The EBM preparation technology has the characteristics of preheating, vacuum environment forming and high cooling rate, can effectively reduce the thermal stress and cracking condition, improves the distribution of particles and elements, and is particularly suitable for preparing TiAl alloy and nano composite materials. However, few studies on the EBM production of TiAl-based composites have been reported. The metal matrix composite material prepared by additive manufacturing mostly adopts mechanical ball milling to mix matrix powder and external particles in advance, and then is formed. For EBM technology, the addition of ceramic particles reduces the conductivity of the premixed powder and charge build-up during the manufacturing process causes severe "blow-off". This results in some of the powder not being fused, porous pores within the material, and a decrease in density. In severe cases, the manufacturing process is terminated and the power supply life is reduced. Therefore, the solution of the problems is of great significance for preparing carbide-reinforced TiAl-based nano composite materials.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a novel preparation method of a TiAl-based nano composite material. The method has stable preparation process and adjustable forming parameter window for preparing the TiAl-based composite material by the EBM. Can prepare the nearly fully-compact TiAl-based nano composite material with uniform microstructure and dispersed nano particles, and has good mechanical property.
In order to achieve the purpose, the invention adopts the technical scheme that: the Electron Beam Melting (EBM) technology is adopted for the first time, and the EBM technology is combined with a semi-melting scanning strategy to obtain the required material by controlling the EBM technology;
the method specifically comprises the following steps:
(1) selecting TiC ceramic particles with purity of more than 99.9% and particle size of 50-500nm and TiAl alloy powder with particle size of 45-150 μm as raw materials;
(2) mixing the two materials by using a mechanical ball milling method to obtain pre-mixed powder with TiC nano particles uniformly distributed on the surface of TiAl alloy powder, wherein the weight of the TiC nano particles accounts for 0.7-1.2 wt% of the total weight of the mixed powder;
(3) and (3) preparing the TiAl-based nano composite material by layer-by-layer forming by utilizing an electron beam melting technology. Constructing a three-dimensional solid geometric model in a computer and carrying out layered slicing; laying a forming substrate in the forming cavity, putting the premixed powder into a powder box of the EBM equipment, sealing the cavity and starting a vacuum system; establishing a processing task, and setting the powder spreading thickness to be 70 mu m; in the forming process, the powder spreading system firstly controls the painting to uniformly lay a layer of premixed powder on a forming substrate, and then adopts high-energy electron beams to preheat; scanning the premixed powder by a defocused high-energy electron beam according to a layered path of a computer model to partially melt (semi-melt) the premixed powder so as to realize powder consolidation to a certain degree; scanning the semi-solid powder by using a focused high-energy electron beam according to a layered path of a computer model to completely melt the semi-solid powder to form a single-layer section of a sample; then the forming substrate is descended by a layer thickness distance, and the steps are repeated after the powder is spread again; and preparing the TiAl-based nano composite material layer by layer until the three-dimensional block sample is processed.
Preferably, in the step (2), the mass ratio of the ball materials of the mechanical ball milling is 1:1, the rotating speed is 24r/min, and the ball milling time is 9-11 hours;
preferably, in the step (3), the EBM is prepared by adopting an accelerating voltage of 60kV, the forming is carried out in a vacuum environment controlled by high-purity Ar, and the vacuum degree is maintained to be 10-2mbar。
Preferably, in the step (3), the preheating process is two-step preheating, the scanning speed of the first step preheating is 16000mm/s, the current is 20-26mA, the scanning speed of the second step preheating is 18000mm/s, the current is 20-26mA, and the forming temperature is maintained at 1030-1080 ℃.
Preferably, in the step (3), the scanning speed adopted in the semi-melting process is 2500-6000mm/s, the current is 6-8mA, the line spacing is 0.03mm, and the defocusing amount is 50 mA.
Preferably, in the step (3), the scanning speed of the complete melting process is 1500-13000mm/s, the current is 10mA, the line spacing is 0.02-0.2mm, and the defocusing amount is 20 mA.
The time for the preheating, semi-melting, and full melting is determined by the scan speed and the size of the sample.
The invention designs a carbide-reinforced TiAl-based nano composite material based on an electron beam melting technology and a preparation method thereof, and no relevant report is found at present. Wherein, the powder is mixed by mechanical ball milling to obtain premixed powder with uniformly distributed nano ceramic particles. The semi-melting step is added in the electron beam melting preparation process, so that the stabilization of the preparation process is realized, the density of the composite material is improved, and the feasibility of preparing the TiAl-based nano composite material by the electron beam melting technology is proved. By changing the scanning parameters in the melting process, the design and processing conditions of the composite material are optimized, and the composite material with controllable tissue structure and excellent mechanical property is obtained. Meanwhile, the electron beam melting preparation has obvious advantages in the aspect of forming TiAl-based nano composite material structural parts with complex shapes
The invention has the following beneficial effects:
1. according to the invention, the TiAl alloy powder is not damaged by mechanical ball milling of the mixed powder after the parameters are optimized, and the ceramic particles can be uniformly adhered to the surface of the TiAl powder, so that conditions are provided for uniform distribution of the nano particles in a melt.
2. According to the invention, a semi-melting step (partial melting of powder) is added in the electron beam melting forming process, so that on one hand, the powder is metallurgically bonded to a certain extent, the phenomenon of powder blowing caused by the decrease of the integral conductivity of the powder after the ceramic particles are adhered is effectively inhibited, and the preparation process is stabilized; on the other hand, the two times of melting increases the wettability between the melt and the nano particles, so that the two are fully contacted, the agglomeration is reduced, and the porosity is reduced. No significant holes or cracks were observed inside the material. In addition, the semi-melting technology adopted by the invention can expand the parameter regulation and control range of EBM forming, thereby optimizing the distribution uniformity of matrix tissues and reinforcing phases.
3. Electron beam melting/solidification is a non-equilibrium process, has high supercooling degree and cooling rate, and thermal circulation caused by layer-by-layer scanning is beneficial to uniform distribution of elements, so that a good matrix microstructure can be obtained; in addition, the existing time of the melt is short, the agglomeration, the growth or the adverse reaction of the nano particles can not be caused, and the stirring effect of the high-energy electron beam on the molten pool is beneficial to the dispersion of the nano particles.
4. The TiAl-based nano composite material prepared by the invention has good hardness and compression performance, and is expected to solve the problems of room temperature brittleness, difficult processing and high temperature strength improvement of TiAl alloy.
5. The invention provides a carbide-reinforced TiAl-based nano composite material and a preparation method thereof, which are formed by adopting an electron beam melting technology, can effectively solve the problems of preparation of difficult-to-process materials and formation of complex parts, shorten the preparation period and have great application potential in the field of aerospace.
Drawings
In order to make the object, technical scheme and beneficial effect of the invention more clear, the invention provides the following drawings for explanation:
FIG. 1 is a photograph of EBM samples of carbide-reinforced TiAl-based nanocomposites prepared in example 1 and comparative example 1.
FIG. 2 is an optical micrograph (a) of the carbide reinforced TiAl-based nanocomposite prepared in example 1 and (b) of the carbide reinforced TiAl-based nanocomposite prepared in comparative example 1.
FIG. 3 is an SEM photograph of the microstructure of the carbide-reinforced TiAl-based nanocomposite prepared in example 2.
FIG. 4 is a graphical representation of the morphology of the pre-mixed powder after mechanical ball milling prepared in example 4.
FIG. 5 is an optical micrograph of the carbide-reinforced TiAl-based nanocomposite prepared in example 4.
FIG. 6 is an SEM photograph of the microstructure of the carbide-reinforced TiAl-based nanocomposite prepared in example 4.
FIG. 7 is an X-ray diffraction pattern of the carbide-reinforced TiAl-based nanocomposite prepared in example 4.
Detailed Description
The invention is further illustrated with reference to the following figures and examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that it would be obvious to those skilled in the art that various changes and modifications can be made without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1:
a carbide reinforced TiAl-based nano composite material and a preparation method thereof, wherein high Nb-TiAl alloy is taken as a matrix, and TiC ceramic particles with the purity of more than 99.9 percent and the average particle size of 200nm are taken as additional particles.
The high Nb-TiAl alloy is prepared from high Nb-TiAl alloy powder with the particle size of 45-150 mu m and D50 of 87 mu m by a plasma rotating electrode method, and comprises the following chemical components: 47.17 at.% Al, 7.41 at.% Nb,0.86 at.% Cr,1.90 at.% V, balance Ti.
The carbide reinforced TiAl-based nano composite material and the preparation method thereof comprise the following steps:
(1) TiC ceramic particles and TiAl alloy powder are used as raw materials, and the added TiC content is 0.7 wt.%;
(2) mixing the two materials by using a mechanical ball milling method to obtain pre-mixed powder with TiC nano particles uniformly distributed on the surface of TiAl alloy powder;
(3) and (3) preparing the TiAl-based nano composite material by layer-by-layer forming by utilizing an electron beam melting technology. Constructing a three-dimensional solid geometric model in a computer and carrying out layered slicing; laying a forming substrate in the forming cavity, putting the premixed powder into a powder box of the EBM equipment, sealing the cavity and starting a vacuum system; establishing a processing task, and setting the powder spreading thickness to be 70 mu m; in the forming process, the powder spreading system firstly controls the painting to uniformly lay a layer of premixed powder on a forming substrate, and then adopts high-energy electron beams to preheat; scanning the premixed powder by a defocused high-energy electron beam according to a layered path of a computer model to partially melt (semi-melt) the premixed powder so as to realize powder consolidation to a certain degree; scanning the semi-solid powder by using a focused high-energy electron beam according to a layered path of a computer model to completely melt the semi-solid powder to form a single-layer section of a sample; then the forming substrate is descended by a layer thickness distance, and the steps are repeated after the powder is spread again; and preparing the TiAl-based nano composite material layer by layer until the three-dimensional block sample is processed.
ZrO is adopted for mechanical ball milling in the step (2)2Grinding balls, wherein the ball material mass ratio is 1:1, the rotating speed is 24r/min, and the ball milling time is 10 hours;
the EBM in the step (3) is prepared by adopting an accelerating voltage of 60kV, forming is carried out in a vacuum environment controlled by high-purity Ar, and the vacuum degree is maintained to be 10-2mbar。
The preheating process in the step (3) is two-step preheating, the scanning speed of the first step preheating is 16000mm/s, the current is 24mA, the scanning speed of the second step preheating is 18000mm/s, the current is 24mA, and the forming temperature is kept at 1060 ℃.
The scanning speed adopted in the semi-melting process in the step (3) is 2800mm/s, the current is 7mA, the line spacing is 0.03mm, and the defocusing amount is 50 mA.
In the step (3), the scanning speed in the melting process is 3000mm/s, the current is 10mA, the line spacing is 0.05mm, and the defocusing amount is 20 mA.
Comparative example 1:
the difference from example 1 is: in the step (3), the premixed powder is not scanned by defocused high-energy electron beams, and the rest is unchanged.
Fig. 1 shows photographs of EBM samples of the carbide-reinforced TiAl-based nanocomposite prepared in example 1 and comparative example 1, and it can be seen that the EBM samples prepared without scanning the premixed powder with a defocused high-energy electron beam have rough surfaces and are not fused seriously. The EBM sample prepared by scanning the premixed powder by a defocused high-energy electron beam has a smooth, flat and compact surface.
Fig. 2 shows an optical micrograph (a) of the carbide-reinforced TiAl-based nanocomposite prepared in example 1 and an optical micrograph (b) of the carbide-reinforced TiAl-based nanocomposite prepared in comparative example 1, and it can be seen that a large number of voids and unfused defects were present in the EBM sample prepared without scanning the premixed powder with the defocused high-energy electron beam, and the EBM sample prepared with scanning the premixed powder with the defocused high-energy electron beam was dense and almost defect-free in the interior.
Example 2:
the difference from example 1 is: the preheating process in the step (3) is two-step preheating, the scanning speed of the first step preheating is 16000mm/s, the current is 22mA, the scanning speed of the second step preheating is 18000mm/s, the current is 22mA, and the forming temperature is kept at 1030 ℃. The scanning speed adopted in the semi-melting process is 4000mm/s, the current is 7mA, the line spacing is 0.03mm, and the defocusing amount is 50 mA. The scanning speed in the melting process is 11000mm/s, the current is 10mA, the line spacing is 0.02mm, and the defocusing amount is 20 mA. The others are unchanged.
FIG. 3 is an SEM photograph showing the microstructure of the carbide-reinforced TiAl-based nanocomposite prepared in example 2, and it can be seen that the TiAl alloy matrix prepared by EBM has a uniform microstructure and is a bimodal structure. The black particles are carbides and are dispersed and distributed on the substrate in a nanometer scale.
The microhardness of the carbide-reinforced TiAl-based nanocomposite prepared in example 2 was determined to be 439HV0.2The tensile strength is 591MPa, the compressive yield strength is 1042MPa, the compressive strength is 2686MPa, and the compressive fracture strain is 25.8 percent.
Example 3:
the difference from example 2 is: in the step (3), the scanning speed in the melting process is 8000mm/s, the current is 10mA, the line spacing is 0.05mm, and the defocusing amount is 20 mA. The others are unchanged.
The microhardness of the carbide-reinforced TiAl-based nanocomposite prepared in example 3 was tested to be 440HV0.2The tensile strength is 568MPa, the compressive yield strength is 1160MPa, the compressive strength is 2795MPa, and the compressive fracture strain is 24.8%.
Example 4:
a carbide reinforced TiAl-based nano composite material and a preparation method thereof, wherein high Nb-TiAl alloy is taken as a matrix, and TiC ceramic particles with the purity of more than 99.9 percent and the average particle size of 200nm are taken as additional particles.
The high Nb-TiAl alloy is prepared from high Nb-TiAl alloy powder with the particle size of 45-150 mu m and D50 of 87 mu m by a plasma rotating electrode method, and comprises the following chemical components: 47.17 at.% Al, 7.41 at.% Nb,0.86 at.% Cr,1.90 at.% V, balance Ti.
The carbide reinforced TiAl-based nano composite material and the preparation method thereof comprise the following steps:
(1) TiC ceramic particles and TiAl alloy powder are used as raw materials, and the added TiC content is 1.2 wt.%;
(2) mixing the two materials by using a mechanical ball milling method to obtain pre-mixed powder with TiC nano particles uniformly distributed on the surface of TiAl alloy powder;
(3) and (3) preparing the TiAl-based nano composite material by layer-by-layer forming by utilizing an electron beam melting technology. Constructing a three-dimensional solid geometric model in a computer and carrying out layered slicing; laying a forming substrate in the forming cavity, putting the premixed powder into a powder box of the EBM equipment, sealing the cavity and starting a vacuum system; establishing a processing task, and setting the powder spreading thickness to be 70 mu m; in the forming process, the powder spreading system firstly controls the painting to uniformly lay a layer of premixed powder on a forming substrate, and then adopts high-energy electron beams to preheat; scanning the premixed powder by a defocused high-energy electron beam according to a layered path of a computer model to partially melt (semi-melt) the premixed powder so as to realize powder consolidation to a certain degree; scanning the semi-solid powder by using a focused high-energy electron beam according to a layered path of a computer model to completely melt the semi-solid powder to form a single-layer section of a sample; then the forming substrate is descended by a layer thickness distance, and the steps are repeated after the powder is spread again; and preparing the TiAl-based nano composite material layer by layer until the three-dimensional block sample is processed.
(4) And (4) repeating the step (3), and preparing the TiAl-based nano composite material layer by layer until the three-dimensional block sample is processed.
ZrO is adopted for mechanical ball milling in the step (2)2Grinding balls, wherein the ball material mass ratio is 1:1, the rotating speed is 24r/min, and the ball milling time is 10 hours;
the EBM preparation in the step (3) adopts the accelerating voltage of 60kV, the forming is carried out in the vacuum environment controlled by high-purity Ar, and the vacuum degree is maintained to be 10-2mbar。
The preheating process in the step (3) is two-step preheating, the scanning speed of the first step preheating is 16000mm/s, the current is 20mA, the scanning speed of the second step preheating is 18000mm/s, the current is 22mA, and the forming temperature is kept at 1080 ℃.
The scanning speed adopted in the semi-melting process in the step (3) is 4000mm/s, the current is 8mA, the line spacing is 0.03mm, and the defocusing amount is 50 mA.
In the step (3), the scanning speed in the melting process is 2500mm/s, the current is 10mA, the line spacing is 0.1mm, and the defocusing amount is 20 mA.
Fig. 4 is a morphology diagram of the pre-mixed powder prepared in example 4 after mechanical ball milling, which shows that the surface of the TiAl alloy powder is not damaged, the sphericity is good, and the TiC nanoparticles are uniformly adhered to the surface of the TiAl alloy powder.
Fig. 5 is an optical micrograph of the carbide-reinforced TiAl-based nanocomposite prepared in example 4, and it can be seen that the TiAl-based nanocomposite prepared by the present invention has a dense interior, no unfused defect and crack are found, only a small amount of pores are present, and the density is 99.1% as measured by archimedes drainage.
FIG. 6 is a SEM photograph showing the microstructure of the carbide-reinforced TiAl-based nanocomposite prepared in example 4; FIG. 7 shows an X-ray diffraction pattern of the TiAl-based nanocomposite prepared in example 4. The results in FIGS. 6 and 7 show that the microstructure of the TiAl alloy matrix prepared by EBM is uniform and has a bimodal structure. Conversion of added TiC nanoparticles to Ti2AlC phase dispersed on the substrate in nanometer scale.
The microhardness of the carbide-reinforced TiAl-based nanocomposite prepared in example 3 was determined to be 433HV0.2The tensile strength is 657MPa, the compressive yield strength is 1085MPa, the compressive strength is 2698MPa, and the compressive fracture strain is 26.1%.
Example 5:
the difference from example 4 is: in the step (3), the scanning speed in the melting process is 13000mm/s, the current is 10mA, the line spacing is 0.02mm, and the defocusing amount is 20 mA. The others are unchanged.
The microhardness of the carbonized reinforced TiAl-based nano composite material prepared in the example 3 is 415HV0.2The tensile strength is 643MPa, the compressive yield strength is 916MPa, the compressive strength is 2740MPa, and the compressive fracture strain is 27.1%.
Example 6:
the difference from example 4 is: TiC ceramic particles with the purity of more than 99.9 percent and the average particle size of 500nm are taken as additional particles. In the step (3), the scanning speed adopted in the semi-melting process is 2500mm/s, the current is 6mA, the line spacing is 0.03mm, and the defocusing amount is 50 mA. The scanning speed in the melting process is 1500mm/s, the current is 10mA, the line spacing is 0.2mm, and the defocusing amount is 20 mA. The others are unchanged.
Example 7:
a carbide reinforced TiAl-based nano composite material and a preparation method thereof, wherein high Nb-TiAl alloy is taken as a matrix, and TiC ceramic particles with the purity of more than 99.9 percent and the average particle size of 50nm are taken as additional particles.
The high Nb-TiAl alloy is prepared from high Nb-TiAl alloy powder with the particle size of 45-150 mu m and D50 of 87 mu m by a plasma rotating electrode method, and comprises the following chemical components: 47.17 at.% Al, 7.41 at.% Nb,0.86 at.% Cr,1.90 at.% V, balance Ti.
The carbide reinforced TiAl-based nano composite material and the preparation method thereof comprise the following steps:
(1) TiC ceramic particles and TiAl alloy powder are used as raw materials, and the added TiC content is 0.7 wt.%;
(2) mixing the two materials by using a mechanical ball milling method to obtain pre-mixed powder with TiC nano particles uniformly distributed on the surface of TiAl alloy powder;
(3) and (3) preparing the TiAl-based nano composite material by layer-by-layer forming by utilizing an electron beam melting technology. Constructing a three-dimensional solid geometric model in a computer and carrying out layered slicing; laying a forming substrate in the forming cavity, putting the premixed powder into a powder box of the EBM equipment, sealing the cavity and starting a vacuum system; establishing a processing task, and setting the powder spreading thickness to be 70 mu m; in the forming process, the powder spreading system firstly controls the painting to uniformly lay a layer of premixed powder on a forming substrate, and then adopts high-energy electron beams to preheat; scanning the premixed powder by a defocused high-energy electron beam according to a layered path of a computer model to partially melt (semi-melt) the premixed powder so as to realize powder consolidation to a certain degree; scanning the semi-solid powder by using a focused high-energy electron beam according to a layered path of a computer model to completely melt the semi-solid powder to form a single-layer section of a sample; then the forming substrate is descended by a layer thickness distance, and the steps are repeated after the powder is spread again; and preparing the TiAl-based nano composite material layer by layer until the three-dimensional block sample is processed.
(4) And (4) repeating the step (3), and preparing the TiAl-based nano composite material layer by layer until the three-dimensional block sample is processed.
ZrO is adopted for mechanical ball milling in the step (2)2Grinding balls, wherein the ball material mass ratio is 1:1, the rotating speed is 24r/min, and the ball milling time is 10 hours;
the EBM preparation in the step (3) adopts the accelerating voltage of 60kV, the forming is carried out in the vacuum environment controlled by high-purity Ar, and the vacuum degree is maintained to be 10-2mbar。
The preheating process in the step (3) is two-step preheating, the scanning speed of the first step preheating is 16000mm/s, the current is 20mA, the scanning speed of the second step preheating is 18000mm/s, the current is 20mA, and the forming temperature is kept at 1030 ℃.
In the step (3), the scanning speed adopted in the semi-melting process is 6000mm/s, the current is 8mA, the line spacing is 0.03mm, and the defocusing amount is 50 mA.
In the step (3), the scanning speed in the melting process is 9000mm/s, the current is 10mA, the line spacing is 0.03mm, and the defocusing amount is 20 mA.
Finally, it is noted that the above-mentioned embodiments illustrate rather than limit the invention, and that, although the invention has been described with reference to the above-mentioned embodiments, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the scope of the invention as defined by the appended claims.
Claims (6)
1. A preparation method of carbide reinforced TiAl-based nano composite material is characterized in that Electron Beam Melting (EBM) technology is adopted for the first time, and is combined with a semi-melting scanning strategy, and the required material is obtained by controlling the EBM technology;
the preparation method comprises the following specific steps:
(1) selecting TiC ceramic particles with purity of more than 99.9% and particle size of 50-500nm and TiAl alloy powder with particle size of 45-150 μm as raw materials;
(2) mixing the two materials by using a mechanical ball milling method to obtain pre-mixed powder with TiC nano particles uniformly distributed on the surface of TiAl alloy powder, wherein the weight of the TiC nano particles accounts for 0.7-1.2 wt% of the total weight of the mixed powder;
(3) and (3) preparing the TiAl-based nano composite material by layer-by-layer forming by utilizing an electron beam melting technology. Constructing a three-dimensional solid geometric model in a computer and carrying out layered slicing; laying a forming substrate in the forming cavity, putting the premixed powder into a powder box of the EBM equipment, sealing the cavity and starting a vacuum system; establishing a processing task, and setting the powder spreading thickness to be 70 mu m; in the forming process, the powder spreading system firstly controls the painting to uniformly lay a layer of premixed powder on a forming substrate, and then adopts high-energy electron beams to preheat; scanning the premixed powder by a defocused high-energy electron beam according to a layered path of a computer model to partially melt the premixed powder so as to realize powder consolidation to a certain degree; scanning the semi-solid powder by using a focused high-energy electron beam according to a layered path of a computer model to completely melt the semi-solid powder to form a single-layer section of a sample; then the forming substrate is descended by a layer thickness distance, and the steps are repeated after the powder is spread again; and preparing the TiAl-based nano composite material layer by layer until the three-dimensional block sample is processed.
2. The method for preparing the carbide-reinforced TiAl-based nanocomposite material as claimed in claim 1, wherein in the step (2), the mass ratio of the ball and the material obtained by mechanical ball milling is 1:1, the rotating speed is 24r/min, and the ball milling time is 9-11 hours.
3. The method of claim 1, wherein in step (3), the EBM is applied at an accelerating voltage of 60kV, the forming is performed in a high-purity Ar-controlled vacuum environment, and the vacuum degree is maintained at 10%-2mbar。
4. The method for preparing carbide-reinforced TiAl-based nanocomposite as claimed in claim 1, wherein in the step (3), the preheating process comprises two preheating steps, wherein the scanning speed of the first preheating step is 16000mm/s, the current is 20-26mA, the scanning speed of the second preheating step is 18000mm/s, the current is 20-26mA, and the forming temperature is maintained at 1030-1080 ℃.
5. The method for preparing the carbide-reinforced TiAl-based nanocomposite as claimed in claim 1, wherein in the step (3), the scanning speed adopted in the semi-melting process is 2500-.
6. The method for preparing the carbide-reinforced TiAl-based nanocomposite as claimed in claim 1, wherein in the step (3), the scanning speed in the melting process is 1500-13000mm/s, the current is 10mA, the line spacing is 0.02-0.2mm, and the defocusing amount is 20 mA.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202110423531.1A CN113210627A (en) | 2021-04-20 | 2021-04-20 | Preparation method of carbide-reinforced TiAl-based nanocomposite |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202110423531.1A CN113210627A (en) | 2021-04-20 | 2021-04-20 | Preparation method of carbide-reinforced TiAl-based nanocomposite |
Publications (1)
Publication Number | Publication Date |
---|---|
CN113210627A true CN113210627A (en) | 2021-08-06 |
Family
ID=77088155
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202110423531.1A Pending CN113210627A (en) | 2021-04-20 | 2021-04-20 | Preparation method of carbide-reinforced TiAl-based nanocomposite |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN113210627A (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN115502412A (en) * | 2022-09-28 | 2022-12-23 | 中国航空制造技术研究院 | Electron beam selective melting additive manufacturing method of TiAl single crystal material |
CN117483799A (en) * | 2023-12-29 | 2024-02-02 | 西安赛隆增材技术股份有限公司 | Powder bed electron beam additive manufacturing method of aluminum alloy |
Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5366570A (en) * | 1993-03-02 | 1994-11-22 | Cermics Venture International | Titanium matrix composites |
WO2018133799A1 (en) * | 2017-01-22 | 2018-07-26 | 清华大学 | Additive manufacturing equipment utilizing combined electron beam selective melting and electron beam butting |
CN110064756A (en) * | 2019-04-23 | 2019-07-30 | 阳江市五金刀剪产业技术研究院 | A kind of method of selective laser melting (SLM) molding |
CN110181048A (en) * | 2019-05-24 | 2019-08-30 | 清华大学 | A kind of electron beam increasing material manufacturing method of molybdenum-base alloy powder |
US20200055118A1 (en) * | 2016-11-30 | 2020-02-20 | Abdelmadjid Djemai | Process for manufacturing a titanium zirconium alloy and its embodiment by additive manufacturing |
CN111036899A (en) * | 2019-11-20 | 2020-04-21 | 中国船舶重工集团公司第十二研究所 | Forming method of particle reinforced aluminum matrix composite material part |
CN111172404A (en) * | 2020-03-10 | 2020-05-19 | 南昌航空大学 | Electron beam remelting device and method for particle-reinforced aluminum-based composite material |
-
2021
- 2021-04-20 CN CN202110423531.1A patent/CN113210627A/en active Pending
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5366570A (en) * | 1993-03-02 | 1994-11-22 | Cermics Venture International | Titanium matrix composites |
US20200055118A1 (en) * | 2016-11-30 | 2020-02-20 | Abdelmadjid Djemai | Process for manufacturing a titanium zirconium alloy and its embodiment by additive manufacturing |
WO2018133799A1 (en) * | 2017-01-22 | 2018-07-26 | 清华大学 | Additive manufacturing equipment utilizing combined electron beam selective melting and electron beam butting |
CN110064756A (en) * | 2019-04-23 | 2019-07-30 | 阳江市五金刀剪产业技术研究院 | A kind of method of selective laser melting (SLM) molding |
CN110181048A (en) * | 2019-05-24 | 2019-08-30 | 清华大学 | A kind of electron beam increasing material manufacturing method of molybdenum-base alloy powder |
CN111036899A (en) * | 2019-11-20 | 2020-04-21 | 中国船舶重工集团公司第十二研究所 | Forming method of particle reinforced aluminum matrix composite material part |
CN111172404A (en) * | 2020-03-10 | 2020-05-19 | 南昌航空大学 | Electron beam remelting device and method for particle-reinforced aluminum-based composite material |
Non-Patent Citations (1)
Title |
---|
阚文斌: "电子束选区熔化技术制备高Nb-TiAl合金的成形工艺和组织调控研究", 《中国优秀博硕士学位论文全文数据库(博士)工程科技Ⅰ辑》 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN115502412A (en) * | 2022-09-28 | 2022-12-23 | 中国航空制造技术研究院 | Electron beam selective melting additive manufacturing method of TiAl single crystal material |
CN117483799A (en) * | 2023-12-29 | 2024-02-02 | 西安赛隆增材技术股份有限公司 | Powder bed electron beam additive manufacturing method of aluminum alloy |
CN117483799B (en) * | 2023-12-29 | 2024-04-02 | 西安赛隆增材技术股份有限公司 | Powder bed electron beam additive manufacturing method of aluminum alloy |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
US20240060156A1 (en) | Method for preparing nano-phase reinforced nickel-based high-temperature alloy using micron ceramic particles | |
WO2022041258A1 (en) | Nano ceramic metal composite powder for 3d printing, and application | |
CN111957967B (en) | Method for preparing multi-scale ceramic phase reinforced metal composite material through 3D printing | |
CN111069614B (en) | Additive manufacturing method of in-situ synthesized micro-nano TiC reinforced titanium-based composite material | |
CN112935252A (en) | Method for preparing high-toughness eutectic high-entropy alloy based on selective laser melting technology | |
CN113210627A (en) | Preparation method of carbide-reinforced TiAl-based nanocomposite | |
CN110744047A (en) | Preparation method of aluminum-based composite material | |
CN111451502B (en) | Partition regulation and control method for in-situ synthesized TiC-reinforced titanium-based composite material in additive manufacturing | |
CN113201664A (en) | In-situ synthesized titanium-based composite material and additive manufacturing and forming method and component thereof | |
CN110744058A (en) | Preparation method for in-situ synthesis of copper-based composite material | |
CN112695220A (en) | Selective laser melting forming nano TiB2Preparation method of reinforced aluminum-based composite material | |
CN111531172A (en) | 3D printing process method of high-strength aluminum-silicon alloy | |
CN112191843A (en) | Method for preparing Ti-1Al-8V-5Fe alloy material by selective laser melting | |
CN114393209B (en) | Titanium-based composite powder with core-shell structure and preparation method and application thereof | |
CN112008087A (en) | Method for improving comprehensive performance of carbon nano material reinforced nickel-based high-temperature alloy | |
CN114480901B (en) | Method for manufacturing nickel-based superalloy performance through carbide reinforced additive, nickel-based superalloy powder and application of nickel-based superalloy powder | |
CN109665848B (en) | Ultrahigh-temperature SiC-HfB2Composite ceramic and preparation method and application thereof | |
Xiong et al. | Role of scanning speed on the microstructure and mechanical properties of additively manufactured Al2O3‒ZrO2 | |
CN111945026A (en) | Preparation method of laser-formed silicon carbide reinforced aluminum-based composite material | |
CN115430842B (en) | In-situ in additive manufacturingBit synthesis of MgAlB 4 Or MgAl 2 O 4 Whisker reinforced aluminium-base composite material and its preparation | |
CN112609180A (en) | In-situ synthesized nano TiC particle reinforced gradient composite coating and preparation method thereof | |
CN116727684A (en) | TiAl-based light high-temperature material based on laser 3D printing and preparation method thereof | |
CN113751707B (en) | Method for preparing nano carbide particle dispersion strengthening alloy powder | |
Wanliang et al. | Microstructure of TiC dendrites reinforced titanium matrix composite layer by laser cladding. | |
CN110819860B (en) | Aluminum-copper-manganese porous composite material and preparation method and application thereof |
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 |