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CN117444232A - A dual-structure titanium-based composite material based on additive manufacturing and method thereof - Google Patents

A dual-structure titanium-based composite material based on additive manufacturing and method thereof Download PDF

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Publication number
CN117444232A
CN117444232A CN202311209402.8A CN202311209402A CN117444232A CN 117444232 A CN117444232 A CN 117444232A CN 202311209402 A CN202311209402 A CN 202311209402A CN 117444232 A CN117444232 A CN 117444232A
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powder
additive manufacturing
based composite
ball milling
printing
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彭华新
刘宸玮
王欢
高翔
李建超
贾延东
何洲洋
李长丰
麻子硕
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Zhejiang University ZJU
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Zhejiang University ZJU
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    • 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
    • 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
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/30—Process control
    • B22F10/32—Process control of the atmosphere, e.g. composition or pressure in a building chamber
    • 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
    • B22F10/30—Process control
    • B22F10/34—Process control of powder characteristics, e.g. density, oxidation or flowability
    • 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
    • C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
    • C22C47/14—Making alloys containing metallic or non-metallic fibres or filaments by powder metallurgy, i.e. by processing mixtures of metal powder and fibres or filaments
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
    • C22C49/02—Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
    • C22C49/10—Refractory metals
    • C22C49/11—Titanium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
    • C22C49/14—Alloys containing metallic or non-metallic fibres or filaments characterised by the fibres or filaments
    • 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
    • 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
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy

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  • Powder Metallurgy (AREA)

Abstract

The invention discloses a double-structure titanium-based composite material based on additive manufacturing and a method thereof, in particular relates to a preparation method of a double-structure titanium-based composite material capable of being used for adjusting and controlling the content of an enhanced phase, the mesh size and the continuity of a mesh structure area, and belongs to the field of microstructure design of titanium-based composite materials. The preparation operation flow comprises the following steps: screening and preprocessing metal and reinforcing phase powder; ball milling and powder mixing with low energy; printing pretreatment; setting printing parameters of additive manufacturing; and (3) feeding powder simultaneously according to different proportions by using the double spray heads to print the block. The method ensures that the size, the content of the reinforcing phase and the continuous degree of the area of the network structure are flexible and controllable, and simultaneously has the characteristics of raw material saving, simple operation, high dimensional accuracy and the like, and has better and balanced mechanical properties.

Description

Dual-structure titanium-based composite material based on additive manufacturing and method thereof
Technical Field
The invention belongs to the field of microstructure design and preparation of titanium-based composite materials, and particularly relates to a double-structure titanium-based composite material based on direct energy deposition additive manufacturing and a method thereof. In this method, the size of the network, the content of the reinforcing phase, and the continuity of the network region are controlled.
Background
The titanium-based composite material has the characteristics of high specific strength and high specific modulus, and has good high-temperature resistance and corrosion resistance, so that the titanium-based composite material is widely applied to the fields of aerospace, vehicle engineering, biomedicine and the like. Additive manufacturing of titanium alloys, particularly the dual phase titanium alloy TC4, has been widely studied and is well-established in various fields. Due to the extremely fast cooling rate, additive manufacturing TC4 exhibits an acicular, alpha-phase martensitic structure, which results in a higher strength, but lower elongation, often below 10%. For additive manufacturing TC4, higher strength, and better strong plastic matching, have been pursued by researchers. Although the addition of the reinforcing phase greatly increases the strength of TC4, it also causes severe plastic degradation and even brittle fracture. To avoid this problem, the microstructure design of titanium-based composites has become a hotspot problem in extensive research. The titanium-based composite material with the reticular structure prepared by the traditional modes including sintering, powder metallurgy and the like often has better strong plastic matching performance, and certain plasticity can be maintained while the strength is greatly improved. After the net-shaped structural design is introduced into the additive to manufacture the titanium-based composite material, the strength can be improved greatly, but due to the growth of the longitudinal thick beta dendrites, the whisker is distributed along the printing direction in the XOZ plane, the preferential growth of the whisker can lead the material to generate early fracture, and a growth polymerization route is provided for the expansion of cracks, so that the material cannot obtain deflection kinking of the cracks. From the mechanical property results of the additive manufacturing net-shaped titanium-based composite material, the elongation rate of the titanium-based composite material tends to be reduced, and the titanium-based composite material has the defect of unstable performance. Therefore, the patent proposes a titanium-based composite material with a double structure, so that the whiskers grow along the initial beta crystal, but have a microstructure structure with discontinuous distribution of regions with a net structure, and sufficient deflection torsion space is provided for crack expansion and growth, thereby realizing cooperative promotion of mechanical properties.
Disclosure of Invention
The invention aims to solve the problems of high preparation cost, complex flow and high subsequent processing difficulty of a titanium-based composite material with a reticular structure or a double-structure in additive manufacturing, and provides a double-structure titanium-based composite material based on additive manufacturing and a method thereof. Wherein TiB is w The reinforcing phase exhibits a network distribution but the network region does notThe method can lead the content of the reinforcing phase in the network structure, the size of the network size and the continuity of the network structure area to be flexible and controllable, and is convenient for the design and preparation of materials.
The specific technical scheme adopted by the invention is as follows:
in a first aspect, the invention provides a preparation method of a dual-structure titanium-based composite material based on additive manufacturing, which comprises the following steps:
s1: vacuum drying Ti6Al4V metal powder and TiB 2 Mixing the powder, performing low-energy ball milling, and realizing TiB on the premise of ensuring that the powder has good sphericity and integrity 2 Inlay attachment of powder on Ti6Al4V metal powder; carrying out vacuum drying treatment on the ball-milled product to obtain mixed powder;
s2: based on additive manufacturing equipment, placing Ti6Al4V metal powder into a first powder carrying tank, and placing the mixed powder into a second powder carrying tank; and (3) carrying out powder feeding by utilizing the double spray heads according to the set powder feeding speed proportion, finishing printing, and obtaining the titanium-based composite material with the double structure, wherein the reinforced phase distribution shows a netlike law, but the netlike region shows a discontinuous distribution law.
Preferably, in the step S1, the Ti6Al4V spherical metal particles have a particle size distribution of 65 to 150 μm, a Hall flow rate of 28.1S/50g, and a bulk density of 2.37g/cm 3 Tap density of 2.75g/cm 3 ；TiB 2 The particles are used as reactants for in-situ generation of titanium boride whisker reinforced phase, and the particle size distribution is 1-3 mu m.
Preferably, the vacuum drying treatment is performed as follows: the material was placed in a glass dish and incubated for one hour at 120℃under vacuum.
Preferably, the ball milling process of the step S1 is specifically as follows:
59.49g (or 58.98 g) of Ti6Al4V metal powder after drying pretreatment and TiB are respectively weighed 2 0.51g (or 1.02 g) of powder, selecting 300g of ball-milling beads with the particle size of 6mm and 10mm, and performing ball milling in a ceramic ball-milling tank; ball milling speed is 200-225.5 rpm, ball-material ratio is5:1, ball milling time is 6-8h, and the ball milling atmosphere is argon atmosphere; in-situ formation of reinforcing phase TiB after ball milling w The mass fraction is 0.5% (or 1%).
Preferably, the model of the additive manufacturing device is BLT-C400, and the pretreatment operation before use is as follows:
argon is flushed into the additive manufacturing equipment to carry out gas washing operation, the oxygen content in the cabin is kept to be lower than 200ppm, the pressure maintaining is started, and the pressure in the cabin is kept to be constant at 0.6Mpa.
Preferably, the operation of setting the printing parameters of the additive manufacturing device before use is specifically as follows:
establishing a printing block model by utilizing Magic three-dimensional modeling software; setting printing parameters for the printing block model by using BLT-BP software, generating a scanning path nc file and storing the nc file into additive manufacturing equipment; the method comprises the steps of setting a printing idle stroke speed to be 1000mm/min, setting a printing mode to be a platform mode, setting a scanning sequence to be an inner filling additional outer ring, setting a layer thickness to be 0.4mm, setting the number of outer rings to be 0, setting the diameter of a light spot to be 1mm, selecting an inner filling mode to be used, setting a continuous scanning mode, setting a path interval to be 1mm, setting a rotation starting angle to be 0, setting a rotation increasing angle to be 90 degrees, setting a laser power to be 750-800W, setting a scanning speed to be 700-800mm/min, setting a powder carrying speed to be 6L/min, setting a dust removing fan speed to be 2, and setting a lens air to be 22L/min.
Preferably, in the step S2, the double spray heads send powder according to a set proportion, and the operation for preparing the double-structure titanium-based composite material is specifically as follows:
s21: placing TC4 metal powder into a first powder carrying tank, and placing mixed powder into a second powder carrying tank;
s22: setting the rotation speed of the first powder feeder to be 1% and the rotation speed of the second powder feeder to be 1%, and then starting printing as shown in a printing schematic diagram of fig. 1;
s23: finishing the printing operation to obtain TC4/TiB w A composite material; in the double-structure titanium-based composite material, as two powders are simultaneously used for mixed printing, the reinforced phase distribution shows a net structure rule, but the net region shows a discontinuous distribution rule, and structural parameters such as net size, net region continuity and the like are printed two by twoThe proportional relationship of the powders affects.
In a second aspect, the present invention provides a dual-structure titanium-based composite material obtained by the method of any one of the first aspects.
Compared with the preparation method of the reticular titanium matrix composite material or other structural metal matrix composite materials in the prior art, the preparation method has the following advantages:
the invention can be used for designing and preparing the metal-based composite material with a double structure, is an important research direction in the field of microstructure design of the metal-based composite material, and has reference significance for application of additive manufacturing and preparation of the metal-based composite material. Has high academic value and great industrial application prospect. Compared with other preparation methods of metal matrix composite materials with a reticular or semi-continuous reticular structure, such as ion electric spark sintering, accumulated rolling bonding, diffusion welding and the like, the method has the following characteristics:
1. the preparation process is clear, and the requirements on the external environment are lower. In the ball milling and material adding manufacturing process, the metal powder and the block are in a closed environment and are in the protection of argon environment, and are insensitive to external environmental factors.
2. The process is mature and easy to control. The ball milling process in the preparation flow is mature, the principle is easy to understand, the variable is less, and the control is easy. The additive manufacturing process and equipment technology are mature and stable, the preparation flow is implemented by software, and the operation is simple.
3. The preparation process is simple, and the time and raw materials are saved. The additive manufacturing preparation mode can realize near net forming of parts, avoid subsequent process processing and post-treatment, and realize saving of raw materials and time cost.
4. The design flexibility is strong, and the design variables are many. The method can flexibly design and adjust design variables such as the content of the reinforcing phase, the size of the network structure, the continuity of the network structure area and the like, and the preparation process and the preparation time are not increased.
5. The applicability is wide. The method is suitable for various alloy systems, can utilize different kinds of metal powder to prepare semi-continuous structures, and can also add other types of reinforcing phase particles into the semi-continuous structures to prepare different kinds of metal matrix composite materials.
The invention can be used for preparing TC4-TiB w A dual structure composite.
Drawings
FIG. 1 is a schematic illustration of printing of a semi-continuous network titanium matrix composite.
FIG. 2 shows TC4 powder (FIG. 2 (a)), TC4 and TiB 2 The mixed powder after ball milling (fig. 2 (b)) was subjected to scanning electron microscopy.
Fig. 3 is a photograph of a composite block prepared in example one.
FIG. 4 is a scanning electron micrograph of a titanium-based composite material having a bicontinuous structure prepared in example one, wherein the TC4 powder was 75% by weight during the preparation, TC4-TiB 2 (0.5%) of the mixed powder was 25%.
Fig. 5 is a graph showing tensile engineering stress strain curves of three kinds of dual-structure titanium matrix composites in the first to third embodiments. The green line is a tensile stress strain curve of mechanical properties of the common TC4 alloy prepared by direct laser three-dimensional molding additive manufacturing; the black line is a tensile stress strain curve of the mechanical property of the double-structure titanium-based composite material prepared by direct laser three-dimensional molding in the first embodiment; the red line is a tensile stress strain curve of the mechanical property of the double-structure titanium-based composite material prepared by direct laser three-dimensional molding in the third embodiment; the blue line is a tensile stress strain curve of the mechanical property of the double-structure titanium-based composite material prepared by direct laser three-dimensional molding in the fourth embodiment.
FIG. 6 is a scanning electron micrograph of a dual-structure titanium matrix composite in which white coils are drawn into a network region and red coils are drawn into a non-network region, wherein the reinforcing phases in the non-network region are uniformly distributed.
FIG. 7 is a scanning electron micrograph of a dual-structure titanium matrix composite in which white coils are drawn into a network region and red coils are drawn into a non-network region, wherein the reinforcing phases in the non-network region are uniformly distributed.
Detailed Description
The invention is further illustrated and described below with reference to the drawings and detailed description. The technical features of the embodiments of the invention can be combined correspondingly on the premise of no mutual conflict.
The invention provides a double-structure titanium-based composite material (TC 4-TiB) w Dual structure composite), the method mainly comprises: s1, mixing Ti6Al4V metal powder and TiB2 powder which are subjected to vacuum drying treatment respectively, and performing low-energy ball milling to realize TiB 2 The powder is inlaid and attached on Ti6Al4V metal powder to obtain mixed powder; s2, based on additive manufacturing equipment, placing Ti6Al4V metal powder into a first powder carrying tank, placing the mixed powder into a second powder carrying tank, feeding powder and performing block printing simultaneously to obtain the double-structure titanium-based composite material with different continuous degree reticular structure areas. The preparation method of the invention specifically comprises the following steps:
1. screening and preprocessing metal and reinforcing phase powder. The laser additive manufacturing method has higher requirements on fluidity, sphericity and the like of the metal powder. In the present invention, preferably, ti6Al4V (TC 4) spherical metal particles (d10= 58.84 μm, d50= 84.61 μm, d90=117.5 μm) with a particle size distribution of 65-150 μm are selected, the Hall flow rate is 28.1s/50g, and the apparent density is 2.37g/cm 3 Tap density of 2.75g/cm 3 Selecting TiB with granularity distribution of 1-3 mu m 2 The particles are used as in-situ generation titanium boride whisker (TiB) w ) The reactants of the enhancement phase. Applying TC4 metal powder to TiB 2 The powder is placed in a glass dish and a vacuum box for heat preservation. The powder is subjected to a drying pretreatment by heat preservation for one hour at 120 ℃ in a vacuum environment.
The TC4 powder particle size is preferably chosen here to be 65-150 μm, d50= 84.61 μm. TiB is preferably selected 2 The particle size of the powder is 1-3 μm. Titanium boride whiskers are generated by in-situ reaction in the additive manufacturing process, and whisker distribution shows the characteristic of a network structure, but TC4 powder and mixed powder are sent out together for printing, so that the area with the network structure shows a discontinuous special microstructure appearance, and the area with the network structure and the area without the network structure are interconnectedThrough, the network size and network area continuity are affected by the content of reinforcing phase and the ratio of mixed powder.
2. And (5) ball milling and powder mixing under low energy. Weighing a certain proportion of TC4 metal powder (figure 2 a) and TiB 2 Mixing the powder, performing low-energy ball milling, and realizing TiB on the premise of ensuring that the powder has good sphericity and integrity 2 The particles are more uniformly embedded and attached to the TC4 particles. In the present invention, it is preferable to weigh 59.49g (or 58.98 g) of TC4 powder with 0.51g (or 1.02 g) of TiB 2 Ball milling is carried out in a ceramic ball milling tank by selecting 300g of ball milling beads with the particle sizes of 6mm and 10 mm. The ball milling rotating speed is 200-225.5 revolutions per minute, the ball-material ratio is 5:1, the ball milling time is 6-8 hours, the ball milling atmosphere is argon atmosphere, and the method can obtain good and uniform mosaic adhesion effect on the basis of ensuring good sphericity and integrity (figure 2 b).
Here, 59.49g (or 58.98 g) of TC4 powder and 0.51g (or 1.02 g) of TiB are preferably selected 2 Ball milling is performed to generate the enhanced phase TiB in situ w The mass fraction is 0.5% (or 1%). Preferably, the ball milling parameters are selected to be 200-225.5 revolutions per minute, the ball-material ratio is 5:1, the ball milling time is 6-8 hours, the argon environment is adopted, and the ball milling beads are mixed with the size of 6mm and 10 mm. This is because, through 18 groups of orthogonal ball milling experiments including ball milling rotation speed, time and ball material ratio parameters, and scanning electron microscope observation of powder particles after ball milling of each group, the result shows that the parameters are optimal ball milling parameters, and TC4 powder and TiB can be formed on the premise of ensuring sphericity and integrity 2 Good and uniform inlay bonding effect of the powder.
3. And (5) printing pretreatment. And (3) placing the mixed powder obtained in the step two into a glass dish, and placing the glass dish into a vacuum box for vacuum heat preservation. In practical application, the powder is preferably kept at 120 ℃ for one hour under a vacuum environment to ensure that the powder is dried; meanwhile, the adopted additive manufacturing equipment BLT-C400 is scrubbed, argon is filled, the oxygen content in the cabin is kept to be lower than 200ppm, the pressure maintaining is started, and the pressure in the cabin is kept constant at 0.6MPa.
4. Setting printing parameters of additive manufacturing. And establishing a printing block model by utilizing Magic three-dimensional modeling software. In actual use, the print parameters may be set for the model using BLT-BP software, and a scan path nc file is generated and stored in BLT-C400. The method comprises the steps of setting a printing idle stroke speed to be 1000mm/min, setting a printing mode to be a platform mode, setting a scanning sequence to be an inner filling additional outer ring, setting a layer thickness to be 0.4mm, setting the number of outer rings to be 0, setting the diameter of a light spot to be 1mm, selecting an inner filling mode to be used, setting a continuous scanning mode, setting a path interval to be 1mm, setting a rotation starting angle to be 0, setting a rotation increasing angle to be 90 degrees, setting a laser power to be 750-800W, setting a scanning speed to be 700-800mm/min, setting a powder carrying speed to be 6L/min, setting a dust removing fan speed to be 2, and setting a lens air to be 22L/min.
And carrying out single-pass and double-pass experiments on the additive manufacturing process including laser power and scanning speed parameters to obtain the optimal path distance and the layer cutting thickness under each group of parameters. Ten sets of orthogonal experiments are performed on printing parameters including laser power, scanning speed and powder feeding speed to obtain the optimal printing parameters, wherein the density of the block is 99.97%, and the maximum hole size is 70 microns.
5. And (3) carrying out bulk printing by using the double powder carrying tanks according to a set proportion and simultaneously feeding powder to obtain the double-structure titanium-based composite material.
Wherein, the operation of simultaneously feeding powder by the double powder carrying tanks according to the set proportion is specifically as follows:
placing TC4 metal powder into a first powder carrying tank, placing the mixed powder obtained in the third step into a second powder carrying tank, setting the rotation speed of the first powder feeder to be 1%, setting the rotation speed of the second powder feeder to be 1%, and starting printing. After the printing operation is completed, TC4/TiB is obtained w The reinforced phases are distributed according to a net-shaped rule, but the net-shaped area is in a discontinuous state, and the continuity degree is influenced by the powder feeding proportion.
Example 1
The embodiment prepares the double-structure titanium-based composite material, and the specific preparation method is carried out according to the following steps:
1. selecting Ti6Al4V (TC 4) spherical metal particles with particle size distribution of 65-150 μm (D10= 58.84 μm, D50= 84.61 μm, D90=117.5 μm), and Hall flow rate of 28.1s/50g, loose loadingDensity of 2.37g/cm 3 Tap density of 2.75g/cm 3 Selecting TiB with granularity distribution of 1-3 mu m 2 The particles are used as in-situ generation titanium boride whisker (TiB) w ) The reactants of the enhancement phase. Combining TC4 metal powder with TiB 2 The powder is placed in a glass dish and a vacuum box for heat preservation. The powder is subjected to a drying pretreatment by heat preservation for one hour at 120 ℃ in a vacuum environment.
2. 59.49g of TC4 powder and 0.51g of TiB were weighed out 2 Ball milling is carried out in a ceramic ball milling tank by selecting 300g of ball milling beads with the particle sizes of 6mm and 10 mm. Setting the ball milling rotating speed to 225.5 revolutions per minute, the ball-material ratio to 5:1, the ball milling time to 8 hours, and the ball milling atmosphere to argon atmosphere.
3. And (3) placing the mixed powder obtained in the step two into a glass dish, and placing the glass dish into a vacuum box for vacuum heat preservation. And (3) preserving heat for one hour at 120 ℃ in a vacuum environment, and ensuring the powder to be dried. And (3) washing the adopted additive manufacturing equipment BLT-C400, filling argon, keeping the oxygen content in the cabin to be reduced to below 200ppm, starting the pressure maintaining, and keeping the pressure in the cabin constant at 0.6MPa.
4. And establishing a printing block model by using Magic three-dimensional modeling software, wherein the model size is a cuboid of 55mm multiplied by 26mm multiplied by 15 mm. The scan path nc file is generated and stored in the BLT-C400 by setting print parameters for the model using BLT-BP software. The method comprises the steps of setting a printing idle stroke speed to be 1000mm/min, setting a printing mode to be a platform mode, setting a scanning sequence to be an inner filling additional outer ring, setting a layer thickness to be 0.4mm, setting the number of outer rings to be 0, setting the diameter of a light spot to be 1mm, selecting an inner filling mode to be used, setting a continuous scanning mode, setting a path interval to be 1mm, setting a rotation starting angle to be 0, setting a rotation increasing angle to be 90 degrees, setting a laser power to be 750W, setting a scanning speed to be 700mm/min, setting a powder carrying speed to be 6L/min, setting a dust removing fan speed to be 2, and setting a lens air to be 22L/min.
5. Placing TC4 metal powder obtained in the first step into a first powder carrying tank, placing mixed powder obtained in the third step into a second powder carrying tank, setting the rotation speed of the first powder feeder to be 1.5%, setting the rotation speed of the second powder feeder to be 0.5%, and starting printing. After the printing operation is completed, TC4/TiB is obtained w A dual structure composite (as shown in figures 3 and 4). Wherein FIG. 3 is a schematic diagram of the preparationFig. 4 is an SEM photograph of the material of this example, and it can be seen from the figure that the whiskers are substantially uniformly distributed due to the fact that the reinforcing phase content is small, so that the network structure and the double structure features are not obvious.
In the embodiment, the composite material with the bicontinuous structure is prepared by simultaneously feeding powder by using two powder feeders of the BLT-C400 equipment of the additive manufacturing equipment according to a set powder feeding rate. In this example, a tensile stress strain curve (black in fig. 5) was obtained by a tensile experiment. It can be seen that the modulus and the strength of the double-structure titanium-based composite material are improved to a certain extent, the strength reaches 1220MPa, and the elongation reaches 8.5%, which means that the current double-structure design is beneficial to the improvement of the strength and the modulus of the material, and the toughness is not greatly reduced.
Example two
The present example prepared a dual structure titanium-based composite, and the specific preparation method was substantially the same as example 1, except that: in the fifth step, the rotation speed of the first powder feeder is set to be 1%, and the rotation speed of the second powder feeder is set to be 1%. Finally, printing is completed, and a sample is obtained.
In the embodiment, the TiB is prepared by regulating and controlling the powder feeding rates of two powder feeders of BLT-C400 equipment of the additive manufacturing equipment and simultaneously feeding and printing w The reinforcing phase presents a network distribution, but the network region presents a discontinuous distribution of the dual-structure titanium-based composite material. The scanning electron microscope photograph of the double-structure titanium-based composite material is shown in fig. 6, wherein the area encircled by the white line is a net-shaped area, the area encircled by the red line is a non-net-shaped area, the material consists of the net-shaped area and the non-net-shaped area at the same time, and the reinforcing phase is uniformly distributed in the non-net-shaped area. As shown in the red line of FIG. 5, the tensile curve results in the embodiment show that the strength of the material is 1071MPa and the elongation is 11%, the structural design greatly improves the strength and modulus of the material, slightly improves the toughness, and achieves the effect of strengthening and toughening simultaneously.
Example III
The embodiment prepares a double-structure titanium-based composite material, and a specific preparation method and a specific application thereofExample 1 is essentially the same, except that: 58.98g of TC4 powder and 1.02g of TiB were weighed in step two 2 Mixing to prepare a mixed powder, and predicting TiB in the prepared material 2 The reinforcing phase accounts for 1%. In the fifth step, the rotation speed of the first powder feeder is set to be 1%, and the rotation speed of the second powder feeder is set to be 1%. Finally, printing is completed, and a sample is obtained.
In the embodiment, the TiB is prepared by regulating and controlling the powder feeding rates of two powder feeders of BLT-C400 equipment of the additive manufacturing equipment and simultaneously feeding and printing w The reinforcing phase presents a network distribution, but the network region presents a discontinuous distribution of the dual-structure titanium-based composite material. The scanning electron microscope photograph of the double-structure titanium-based composite material is shown in fig. 7, wherein the area encircled by the white line is a net-shaped area, the area encircled by the red line is a non-net-shaped area, the material consists of the net-shaped area and the non-net-shaped area at the same time, and the reinforcing phase is uniformly distributed in the non-net-shaped area. The tensile curve results in this example are shown in the blue line of fig. 5, and the strength of the material reaches 1074MPa, and the elongation is 8.1%. As can be seen from comparison, the structural design has the advantages of greatly improving the strength and modulus of the material and reducing the toughness to a lower degree.
The above embodiment is only a preferred embodiment of the present invention, but it is not intended to limit the present invention. Various changes and modifications may be made by one of ordinary skill in the pertinent art without departing from the spirit and scope of the present invention. Therefore, all the technical schemes obtained by adopting the equivalent substitution or equivalent transformation are within the protection scope of the invention.

Claims (8)

1.一种基于增材制造的双结构钛基复合材料的制备方法，其特征在于，具体如下：1. A method for preparing dual-structure titanium-based composite materials based on additive manufacturing, which is characterized by the following: S1：将分别经过真空干燥处理的Ti6Al4V金属粉末以及TiB2粉末混合，并进行低能球磨，在保证粉末具有良好球形度及完整度的前提下，实现TiB2粉末在Ti6Al4V金属粉末上的镶嵌附着；将经过球磨后的产物进行真空干燥处理，得到混合粉末；S1: Mix the Ti6Al4V metal powder and TiB 2 powder that have been vacuum dried respectively, and perform low-energy ball milling to achieve the mosaic attachment of the TiB 2 powder on the Ti6Al4V metal powder while ensuring that the powder has good sphericity and integrity; The ball-milled product is vacuum dried to obtain a mixed powder; S2：基于增材制造设备，将Ti6Al4V金属粉末放入第一载粉罐，将所述混合粉末放入第二载粉罐；利用双喷头按照设定的送粉速度比例，同时送粉并进行块体打印，得到具有不同连续程度网状结构区域的双结构钛基复合材料。S2: Based on the additive manufacturing equipment, put the Ti6Al4V metal powder into the first powder carrier tank, and put the mixed powder into the second powder carrier tank; use dual nozzles to simultaneously feed powder according to the set powder feeding speed ratio and perform Through block printing, dual-structure titanium-based composite materials with different degrees of continuous network structure areas are obtained. 2.根据权利要求1所述的一种基于增材制造的双结构钛基复合材料的制备方法，其特征在于，所述步骤S1中，Ti6Al4V球状金属颗粒的粒度分布为75-160μm，霍尔流速为28.1s/50g，松装密度为2.37g/cm3，振实密度为2.75g/cm3；TiB2颗粒的粒度分布为1-3μm。2. A method for preparing a dual-structure titanium-based composite material based on additive manufacturing according to claim 1, characterized in that in step S1, the particle size distribution of the Ti6Al4V spherical metal particles is 75-160 μm, and the Hall effect is 75-160 μm. The flow rate is 28.1s/50g, the bulk density is 2.37g/cm 3 , and the tap density is 2.75g/cm 3 ; the particle size distribution of TiB 2 particles is 1-3 μm. 3.根据权利要求1所述的一种基于增材制造的双结构钛基复合材料的制备方法，其特征在于，所述真空干燥处理操作如下：将材料置于玻璃皿中，并于120℃的真空环境下保温一小时。3. A method for preparing dual-structure titanium-based composite materials based on additive manufacturing according to claim 1, characterized in that the vacuum drying operation is as follows: the material is placed in a glass dish and dried at 120°C. Keep warm in a vacuum environment for one hour. 4.根据权利要求1所述的一种基于增材制造的双结构钛基复合材料的制备方法，其特征在于，所述步骤S1的球磨过程具体如下：4. A method for preparing dual-structure titanium-based composite materials based on additive manufacturing according to claim 1, characterized in that the ball milling process of step S1 is as follows: 分别称取经干燥预处理后的Ti6Al4V金属粉末以及TiB2粉末，选取粒径为6mm和10mm球磨珠共300g，共同于陶瓷球磨罐中进行球磨；球磨转速为每分钟200-225.5转，球料比为5:1，球磨时间6-8h，球磨氛围为氩气气氛；经球磨后原位生成增强相TiBw；Weigh the Ti6Al4V metal powder and TiB2 powder after drying and pretreatment respectively, select a total of 300g of ball mill beads with particle sizes of 6mm and 10mm, and conduct ball milling in a ceramic ball mill tank together; the ball milling speed is 200-225.5 rpm, and the ball-to-material ratio The ratio is 5:1, the ball milling time is 6-8h, and the ball milling atmosphere is argon atmosphere; after ball milling, the reinforcing phase TiB w is generated in situ; 在球磨过程中，取Ti6Al4V金属粉末59.49g、TiB2粉末0.51g，此时经球磨后原位生成增强相TiBw质量分数为0.5％；或者在球磨过程中，取Ti6Al4V金属粉末58.98g、TiB2粉末1.02g，此时经球磨后原位生成增强相TiBw质量分数为1％。During the ball milling process, take 59.49g of Ti6Al4V metal powder and 0.51g of TiB2 powder. At this time, the reinforcing phase TiB w mass fraction generated in situ after ball milling is 0.5%; or during the ball milling process, take 58.98g of Ti6Al4V metal powder and TiB2 powder. 2. 1.02g of powder. At this time, the reinforcing phase TiB w mass fraction generated in situ after ball milling is 1%. 5.根据权利要求1所述的一种基于增材制造的双结构钛基复合材料的制备方法，其特征在于，所述增材制造设备型号为BLT-C400，在使用前的预处理操作如下：5. A method for preparing dual-structure titanium-based composite materials based on additive manufacturing according to claim 1, characterized in that the additive manufacturing equipment model is BLT-C400, and the pretreatment operation before use is as follows : 向增材制造设备中冲入氩气以进行洗气操作，保持机舱内氧含量下降至200ppm以下，开启保压，维持舱内气压恒定0.6Mpa。Inject argon gas into the additive manufacturing equipment for gas scrubbing operation, keep the oxygen content in the cabin below 200ppm, turn on the pressure holding, and maintain a constant air pressure of 0.6Mpa in the cabin. 6.根据权利要求1所述的一种基于增材制造的双结构钛基复合材料的制备方法，其特征在于，所述增材制造设备在使用前的打印参数设置操作具体如下：6. A method for preparing dual-structure titanium-based composite materials based on additive manufacturing according to claim 1, characterized in that the printing parameter setting operation of the additive manufacturing equipment before use is as follows: 利用Magic三维建模软件，建立打印块体模型；利用BLT-BP软件对所述打印块体模型设定打印参数，生成扫描路径.nc文件并存入增材制造设备中；其中，设定打印空程速度为1000mm/min，打印模式为平台模式，扫描顺序为内填充附加外圈，层厚为0.4mm，外圈数量0，光斑直径1mm，选择应用内填充，填充模式为连续扫描模式，路径间距为1mm，旋转开始角为0°，旋转增加角为90°，激光功率为750-800W，扫描速率为700-800mm/min，设定载粉气速度为6L/min，除尘风机速度2，镜头气22L/min。Use Magic three-dimensional modeling software to establish a printing block model; use BLT-BP software to set printing parameters for the printing block model, generate a scan path .nc file and store it in the additive manufacturing equipment; wherein, set printing The idle speed is 1000mm/min, the printing mode is platform mode, the scanning sequence is internal filling and additional outer ring, the layer thickness is 0.4mm, the number of outer rings is 0, the spot diameter is 1mm, select internal filling, and the filling mode is continuous scanning mode. The path spacing is 1mm, the rotation starting angle is 0°, the rotation increasing angle is 90°, the laser power is 750-800W, the scanning rate is 700-800mm/min, the carrier powder gas speed is set to 6L/min, and the dust removal fan speed is 2 , lens gas 22L/min. 7.根据权利要求1所述的一种基于增材制造的双结构钛基复合材料的制备方法，其特征在于，所述步骤S2中，开始打印后，设定与第一载粉罐相连的第一送粉器的旋转速度为1％，与第二载粉罐相连的第二载粉器的旋转速度为1％，使得两个载粉罐向双喷头同时送粉进行打印，直至完成打印。7. A method for preparing dual-structure titanium-based composite materials based on additive manufacturing according to claim 1, characterized in that in step S2, after starting printing, set the The rotation speed of the first powder feeder is 1%, and the rotation speed of the second powder carrier connected to the second powder carrier tank is 1%, so that the two powder carrier tanks feed powder to the dual nozzles at the same time for printing until the printing is completed. . 8.一种利用权利要求1～7任一所述制备方法得到的双结构钛基复合材料。8. A dual-structure titanium-based composite material obtained by the preparation method according to any one of claims 1 to 7.
CN202311209402.8A 2023-09-19 2023-09-19 A dual-structure titanium-based composite material based on additive manufacturing and method thereof Pending CN117444232A (en)

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