CN114959396A - TiC/Mo alloy with lattice structure and selective laser melting preparation method thereof - Google Patents
TiC/Mo alloy with lattice structure and selective laser melting preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
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Abstract
A TiC/Mo alloy with lattice structure and its selective laser melting preparation method are disclosed. The invention belongs to the technical field of alloy rapid forming capable of designing a structure. The invention aims to solve the technical problem that the molybdenum-based alloy prepared by the existing selective laser melting method cannot meet the requirements of modern equipment parts and components mainly represented by aerospace on light weight and structural rigidity due to the characteristics of high density, high brittleness at normal temperature and the like. The TiC/Mo alloy with the lattice structure is prepared from molybdenum powder and titanium carbide powder by a selective laser melting technology, wherein the mass fraction of the titanium carbide powder in the TiC/Mo alloy is 19-21%. The invention innovatively provides a concept of adopting a ceramic brittle second phase to compositely strengthen a normal-temperature high-brittleness matrix, realizes the expected goal of strengthening brittleness and brittleness toughness through reasonable design of material components and synergistic interaction of a forming process, and finally forms a molybdenum-based alloy with a designable complex lattice structure. Has better mechanical property and oxidation resistance.
Description
Technical Field
The invention belongs to the technical field of alloy rapid forming capable of designing a structure, and particularly relates to a TiC/Mo alloy with a lattice structure and a selective laser melting preparation method thereof.
Background
Molybdenum alloy is used as a rare metal, has wide application space in the fields of electronic industry, die manufacturing, high-temperature elements, aerospace, nuclear industry and the like, and is an extremely important strategic resource. Molybdenum has a melting point of up to 2620 ℃ and belongs to the group VIB element of the fifth period (the second long period) of the periodic system of elements, next to carbon, tungsten, rhenium, tantalum and osmium. The density of the molybdenum is 10.22g/cm at 20 DEG C 3 Only about 1/2 for tungsten. The linear expansion coefficient of the molybdenum is (5.8-6.2) x 10 -6 1/3-1/2 of common steel, and the low linear expansion coefficient makes the molybdenum material stable in size at high temperature. Molybdenum has a very high elastic modulus, is one of the highest elastic moduli in the industry, is less affected by temperature, is higher than the ordinary steel at room temperature even at 800 ℃, has better ductility than tungsten, and is easy to press-process into very thin foils and very thin wires. Molybdenum also has a very small thermal neutron capture surface, which enables it to be used as a central structural material for nuclear reactors, a highly new developmentThe technology realizes the national modernization and builds the important basic material of modern national defense.
Selective laser melting is one of the most promising technologies in the field of laser rapid prototyping manufacturing. The method is based on a layered superposition manufacturing principle, metal powder is melted layer by layer through laser beams to form a metal part with a complex structure, the technology has the characteristics that the flexibility degree of the manufacturing process is high, the manufactured part has excellent mechanical property and chemical property, the influence of the size and the complexity degree of a product on the processing difficulty is small, and the like, and compared with other conventional manufacturing technologies, the method has irreplaceable advantages and becomes a research hotspot in recent years. At present, most refractory metals are formed by powder metallurgy, and the forming process needs an expensive tooling die and has a complex process and is difficult to form parts with complex three-dimensional structures.
Molybdenum and molybdenum alloy are used as refractory metal for replacing nickel-based alloy, the traditional forming process is easy to oxidize and has higher ductile-brittle transition temperature, the properties of the molybdenum and the molybdenum alloy severely restrict the processing and forming of molybdenum-based parts, and the application of the molybdenum alloy as a structural material in the field of aerospace is also limited. The molybdenum-based alloy prepared by the existing selective laser melting has the characteristics of high density, high brittleness at normal temperature and the like, so that the molybdenum-based alloy can not meet the requirements of modern equipment parts mainly represented by aerospace on light weight and structural rigidity.
Disclosure of Invention
The invention aims to solve the technical problem that the molybdenum-based alloy prepared by the existing selective laser melting cannot meet the requirements of modern equipment parts mainly represented by aerospace on light weight and structural rigidity due to the characteristics of high density, high brittleness at normal temperature and the like, and provides a TiC/Mo alloy with a lattice structure and a selective laser melting preparation method thereof.
The TiC/Mo alloy with the lattice structure is prepared from molybdenum powder and titanium carbide powder by a selective laser melting technology, wherein the mass fraction of the titanium carbide powder in the TiC/Mo alloy is 19-21%.
Further limit, the granularity of the molybdenum powder and the granularity of the TiC powder are both 15-55 mu m.
The selective laser melting preparation method of the TiC/Mo alloy with the lattice structure is carried out according to the following steps:
step 1: ball-milling and mixing molybdenum powder and titanium carbide powder, sieving and drying to obtain Mo-TiC mixed powder;
step 2: adding Mo-TiC mixed powder into a powder storage cavity of selective laser melting equipment, and setting technological parameters of selective laser melting: the laser power is 240W-260W, the scanning speed is 800 mm/s-1000 mm/s, the scanning interval is 0.08 mm-0.10 mm, and a Zigzag scanning mode is adopted;
and step 3: preheating a pure molybdenum substrate to 120-140 ℃, spreading powder and processing layer by layer, melting, solidifying and remelting mixed powder of each layer, then starting forming processing, cooling after printing, and separating the alloy from the substrate to obtain the TiC/Mo alloy with the lattice structure.
Further limiting, in the step 1, the ball milling rotation speed is 250r/min, the ball milling time is 15min, and the milling ball is an aluminum oxide ceramic milling ball.
Further, the laser power in step 2 is 250W, the scanning speed is 900mm/s, and the scanning interval is 0.09 mm.
Further defined, the pure molybdenum substrate is preheated to 130 ℃ in step 3.
Further limiting, the powder spreading thickness of each layer in the step 3 is 0.03 mm.
Further, the forming process in step 3 is performed under the protection of argon with a purity of 99.9%.
Further, in step 3, the alloy is separated from the substrate by a wire electric discharge machine.
Compared with the prior art, the invention has the following remarkable effects:
the invention innovatively provides a concept of adopting a ceramic brittle second phase to compositely strengthen a normal-temperature high-brittleness matrix, breaks through the inherent range of adopting a brittle phase to strengthen a toughness phase and a toughness phase to strengthen the brittleness phase in the prior art, overcomes the barrier that the brittle phase cannot be strengthened, realizes the expected aim of strengthening brittleness and brittleness as toughness through reasonable design of material components and synergistic interaction of a forming process, and finally forms a designable molybdenum-based alloy with a complex lattice structure, and has the following specific advantages:
1) the mechanical spherical molybdenum powder and TiC powder adopted by the invention have the granularity of 15-55 mu m, and have the advantages of good spheroidization, rough surface and high laser absorption rate.
2) TiC is added to generate compact TiO on the surface of the alloy 2 The holes on the surface of the alloy are filled, so that the oxygen is reduced, the further oxidation is hindered, the oxidation resistance of the alloy is improved, and the weight loss rate is reduced.
3) The TiC particles are dispersed in the matrix, so that the molybdenum alloy grains can be refined, the room-temperature toughness and the high-temperature mechanical property of the alloy are improved, in addition, the TiC aggregated at the grain boundary of the alloy prevents the grain boundary dislocation motion, the recrystallization strength is improved, and the strength of the alloy is further improved. In addition, the addition of TiC can change the alloy from an edgewise fracture mode to a mixed mode of edgewise fracture and transgranular fracture, and simultaneously, because the melting point of TiC is very high, dislocation and grain boundary can be pinned even at 1800 ℃, so that the grain boundary strength of the alloy is enhanced.
4) The alloy has a three-dimensional hollowed lattice structure with high symmetry, the hollowed structures can be regularly arranged and randomly distributed according to requirements, the lattice structure design can be in transition arrangement with gradient density, so that the weight of parts can be reduced, the mechanical property of the parts can be ensured, and the material consumption of the lattice structure design can be reduced by more than 50% under the same volume condition.
5) According to the method, the molybdenum alloy is prepared by using the selective laser melting technology, argon can be used as a protective gas in the forming process during printing, the reduction of powder quality caused by the reaction of printing powder and oxygen in the air is greatly reduced, and the quality of formed parts is effectively guaranteed.
Drawings
FIG. 1 is a schematic structural view of a TiC/Mo alloy of lattice structure of the present invention;
FIG. 2 is a flow chart of a selective laser melting preparation method of the present invention;
FIG. 3 is a surface microscope picture of a TiC/Mo alloy of the lattice structure of example 1.
Detailed Description
Embodiment one (see fig. 1): the TiC/Mo alloy with the lattice structure is prepared from molybdenum powder and titanium carbide powder by a selective laser melting technology, wherein the mass fraction of the titanium carbide powder in the TiC/Mo alloy is 19-21%.
Further limited, the granularity of the molybdenum powder and the granularity of the TiC powder are both 15-55 mu m. The adopted mechanized spherical molybdenum powder and TiC powder have the granularity of 15-55 mu m, and have the advantages of good spheroidization, rough surface and high laser absorption rate.
Embodiment two (see fig. 2): the method for preparing the TiC/Mo alloy with the lattice structure in the first embodiment comprises the following steps of:
step 1: ball-milling and mixing molybdenum powder and titanium carbide powder, sieving and drying to obtain Mo-TiC mixed powder; the ball milling speed is 250r/min, the ball milling time is 15min, and the grinding balls are alumina ceramic grinding balls;
step 2: adding Mo-TiC mixed powder into a powder storage cavity of selective laser melting equipment, and setting technological parameters of selective laser melting: the laser power is 250W, the scanning speed is 900mm/s, the scanning distance is 0.09mm, and a Zigzag scanning mode is adopted;
and step 3: preheating a pure molybdenum substrate to 130 ℃, starting powder paving and layer-by-layer processing, melting, solidifying and remelting mixed powder of each layer, then starting forming processing, wherein the forming processing is carried out under the protection of argon with the purity of 99.9%, the powder paving thickness of each layer is 0.03mm, after printing, cooling is carried out, and separating the alloy from the substrate by using a wire-cut electrical discharge machine to obtain the TiC/Mo alloy with a lattice structure.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The experimental procedures used in the following examples are conventional unless otherwise specified. The materials, reagents, methods and apparatus used, unless otherwise specified, are conventional in the art and are commercially available to those skilled in the art.
Example 1: the TiC/Mo alloy of the lattice structure (see fig. 1) of this embodiment is prepared by performing selective laser melting on molybdenum powder and titanium carbide powder, wherein the mass fraction of the titanium carbide powder in the TiC/Mo alloy is 20%, the particle size of the molybdenum powder and the particle size of the TiC powder are both 15 μm to 55 μm, and the adopted mechanized spherical molybdenum powder and TiC powder have particle sizes of 15 μm to 55 μm, and are better in spheroidization, rough in surface and high in laser absorption rate.
With reference to fig. 2, the method for preparing the TiC/Mo alloy of lattice structure of example 1 is carried out as follows:
step 1: ball-milling 2400g of molybdenum powder and 600g of titanium carbide powder, mixing, wherein the ball-milling rotation speed is 250r/min, the ball-milling time is 15min, the milling balls are aluminum oxide ceramic milling balls, and after ball-milling, sieving with a 200-mesh sieve and drying, Mo-TiC mixed powder is obtained;
and 2, step: adding Mo-TiC mixed powder into a powder storage cavity in selective laser melting equipment, and setting technological parameters of selective laser melting: the laser power is 250W, the scanning speed is 900mm/s, the scanning distance is 0.09mm, and a Zigzag scanning mode is adopted; the higher laser power can reduce the hole defects of the formed part and improve the quality of the formed part;
and step 3: preheating a pure molybdenum substrate to 130 ℃, starting powder paving and layer-by-layer processing, melting, solidifying and remelting mixed powder of each layer, then starting forming processing, carrying out the forming processing under the protection of argon with the purity of 99.9%, strictly controlling the oxygen content in a forming chamber, and separating the alloy from the substrate by using a spark wire cutting machine to obtain the TiC/Mo alloy with a lattice structure, wherein the standard is that the oxygen content in the forming chamber is less than or equal to 150ppm, the powder paving thickness of each layer is 0.03mm, and the alloy is cooled after printing.
The TiC/Mo alloy surface with lattice structure of example 1 is polished and then observed by electron microscope, and as shown in FIG. 3, it can be seen from FIG. 3 that the alloy hole defect formed under the selected process parameters in example 1 is few.
Comparative example 1: the TiC/Mo alloy of the lattice structure (see fig. 1) of this embodiment is prepared by performing selective laser melting on molybdenum powder and titanium carbide powder, wherein the mass fraction of the titanium carbide powder in the TiC/Mo alloy is 10%, the particle size of the molybdenum powder and the particle size of the TiC powder are both 15 μm to 55 μm, and the adopted mechanized spherical molybdenum powder and TiC powder have particle sizes of 15 μm to 55 μm, and are better in spheroidization, rough in surface and high in laser absorption rate.
With reference to fig. 2, the method for preparing the TiC/Mo alloy of lattice structure of comparative example 1 was carried out as follows:
step 1: ball-milling and mixing 2700g of molybdenum powder and 300g of titanium carbide powder at the ball-milling rotation speed of 250r/min for 15min, wherein the grinding balls are aluminum oxide ceramic grinding balls, sieving with a 200-mesh sieve after ball-milling, and drying to obtain Mo-TiC mixed powder;
step 2: adding Mo-TiC mixed powder into a powder storage cavity in selective laser melting equipment, and setting technological parameters of selective laser melting: the laser power is 250W, the scanning speed is 900mm/s, the scanning distance is 0.09mm, and a Zigzag scanning mode is adopted; the higher laser power can reduce the hole defects of the formed part and improve the quality of the formed part;
and step 3: preheating a pure molybdenum substrate to 130 ℃, starting powder paving and layer-by-layer processing, melting, solidifying and remelting mixed powder of each layer, then starting forming processing, carrying out the forming processing under the protection of argon with the purity of 99.9%, strictly controlling the oxygen content in a forming chamber, and separating the alloy from the substrate by using a spark wire cutting machine to obtain the TiC/Mo alloy with a lattice structure, wherein the standard is that the oxygen content in the forming chamber is less than or equal to 150ppm, the powder paving thickness of each layer is 0.03mm, and the alloy is cooled after printing.
Comparative example 2: the TiC/Mo alloy of the lattice structure (see fig. 1) of this embodiment is prepared by performing selective laser melting on molybdenum powder and titanium carbide powder, wherein the mass fraction of the titanium carbide powder in the TiC/Mo alloy is 30%, the particle size of the molybdenum powder and the particle size of the TiC powder are both 15 μm to 55 μm, and the adopted mechanized spherical molybdenum powder and TiC powder have particle sizes of 15 μm to 55 μm, and are better in spheroidization, rough in surface and high in laser absorption rate.
With reference to fig. 2, the method for preparing the TiC/Mo alloy of lattice structure of comparative example 2 was performed as follows:
step 1: ball-milling and mixing 2100g of molybdenum powder and 900g of titanium carbide powder at the ball-milling rotation speed of 250r/min for 15min, wherein the grinding balls are aluminum oxide ceramic grinding balls, sieving with a 200-mesh sieve after ball-milling, and drying to obtain Mo-TiC mixed powder;
step 2: adding Mo-TiC mixed powder into a powder storage cavity in selective laser melting equipment, and setting technological parameters of selective laser melting: the laser power is 250W, the scanning speed is 900mm/s, the scanning distance is 0.09mm, and a Zigzag scanning mode is adopted; the higher laser power can reduce the hole defects of the formed part and improve the quality of the formed part;
and step 3: preheating a pure molybdenum substrate to 130 ℃, starting powder paving and layer-by-layer processing, melting, solidifying and remelting mixed powder of each layer, then starting forming processing, carrying out the forming processing under the protection of argon with the purity of 99.9%, strictly controlling the oxygen content in a forming chamber, and separating the alloy from the substrate by using a spark wire cutting machine to obtain the TiC/Mo alloy with a lattice structure, wherein the standard is that the oxygen content in the forming chamber is less than or equal to 150ppm, the powder paving thickness of each layer is 0.03mm, and the alloy is cooled after printing.
The results of the examination of the TiC/Mo alloy obtained in example 1 and the TiC/Mo alloys obtained in comparative examples 1-2 are shown in Table 1.
TABLE 1 Performance parameters of TiC/Mo alloys formed by selective laser melting
| Compressive strain (%) | Tensile strength at 800 ℃ (MPa) | Density (%) | |
| Example 1 | 8 | 201 | 97.1 |
| Comparative example 1 | 5 | 156 | 91.4 |
| Comparative example 2 | 6 | 187 | 92.5 |
Claims (9)
1. The TiC/Mo alloy with a lattice structure is characterized in that the alloy is prepared from molybdenum powder and titanium carbide powder by a selective laser melting technology, and the mass fraction of the titanium carbide powder in the TiC/Mo alloy is 19-21%.
2. A TiC/Mo alloy of lattice structure as claimed in claim 1, wherein the particle size of Mo powder and the particle size of TiC powder are both 15 μm-55 μm.
3. A selective laser melting process for the preparation of TiC/Mo alloys of lattice structure according to claim 1 or 2, characterized in that it is carried out by the following steps:
step 1: ball-milling and mixing molybdenum powder and titanium carbide powder, sieving and drying to obtain Mo-TiC mixed powder;
step 2: adding Mo-TiC mixed powder into a powder storage cavity of selective laser melting equipment, and setting technological parameters of selective laser melting: the laser power is 240W-260W, the scanning speed is 800 mm/s-1000 mm/s, the scanning interval is 0.08 mm-0.10 mm, and a Zigzag scanning mode is adopted;
and step 3: preheating a pure molybdenum substrate to 120-140 ℃, spreading powder and processing layer by layer, melting, solidifying and remelting mixed powder of each layer, then starting forming processing, cooling after printing, and separating the alloy from the substrate to obtain the TiC/Mo alloy with the lattice structure.
4. The selective laser melting preparation method of TiC/Mo alloy with lattice structure of claim 3, wherein in step 1, the ball milling rotation speed is 250r/min, the ball milling time is 15min, and the milling ball is alumina ceramic milling ball.
5. The selective laser melting preparation method of TiC/Mo alloy with lattice structure of claim 3, wherein in step 2 the laser power is 250W, the scanning speed is 900mm/s, and the scanning distance is 0.09 mm.
6. The selective laser melting preparation method of TiC/Mo alloy with lattice structure of claim 3, wherein in step 3 the pure molybdenum substrate is preheated to 130 ℃.
7. The selective laser melting preparation method of TiC/Mo alloy with lattice structure of claim 3, wherein the powder-laying thickness of each layer in step 3 is 0.03 mm.
8. The method of claim 3, wherein the forming process in step 3 is performed under argon atmosphere with a purity of 99.9%.
9. The selective laser melting preparation method of TiC/Mo alloy with lattice structure as claimed in claim 3, wherein in step 3, the alloy is separated from the substrate by wire cut electrical discharge machining.
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