CN111069614A - Additive manufacturing method of in-situ synthesized micro-nano TiC reinforced titanium-based composite material - Google Patents
Additive manufacturing method of in-situ synthesized micro-nano TiC reinforced titanium-based composite material Download PDFInfo
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Abstract
The invention discloses an additive manufacturing method of an in-situ synthesized micro-nano TiC reinforced titanium-based composite material, which comprises the following steps of: firstly, adding titanium powder or titanium alloy powder and amorphous nano carbon powder into absolute ethyl alcohol for mixing, performing ball milling and drying to obtain ball-milled powder, spraying aerosol, uniformly stirring, and drying to obtain composite powder; and secondly, forming the in-situ synthesized micro-nano TiC reinforced titanium-based composite material by using the composite powder as a raw material and adopting a laser additive manufacturing method. According to the invention, a uniform and stable composite powder raw material is obtained by a ball-milling mixing method and adding aerosol, and then based on the extremely high cooling rate in the laser additive manufacturing process, a micro-nano TiC reinforcing phase which is uniformly distributed and has a good interface transition is precipitated while a titanium matrix is additively formed, so that the problem that the size and distribution of the reinforcing phase are difficult to control in the process of preparing a particle reinforced composite material is effectively solved, and the plasticity and strength of the titanium matrix composite material are improved at the same time.
Description
Technical Field
The invention belongs to the technical field of titanium-based composite material preparation, and particularly relates to an additive manufacturing method of an in-situ synthesized micro-nano TiC reinforced titanium-based composite material.
Background
In recent years, the titanium-based composite material has higher specific strength, specific rigidity and creep property than the titanium alloy, and simultaneously makes up for the defects of poor wear resistance and low hardness of the titanium alloy, so the titanium-based composite material has very large application value and potential in the aspects of aerospace and the like. The particle reinforced titanium-based composite material has attracted wide attention due to the characteristics of low preparation cost, isotropy and the like. The preparation method of the particle reinforced titanium-based composite material can be divided into an external addition method and an in-situ autogenous method. The size of the reinforcing phase of the external method mainly depends on the size of the reinforcing body which is initially added, the size is generally dozens of micrometers, and the method of adding the nano reinforcing phase is adopted at present, but the preparation cost is expensive. The in-situ autogenous method can not only solve a series of problems of wettability of the reinforcement and the matrix, interface reaction of the reinforcement phase/the metal matrix, high cost and the like generated by preparing the titanium-based composite material by an external addition method, but also can prepare the titanium-based composite material with clean reinforcement/matrix interface, no impurity pollution and good combination. However, the in-situ self-generated reinforcing phase of the titanium-based composite material prepared by the traditional method has limited size and the uniformity of distribution is difficult to control. The additive manufacturing technology is based on the manufacturing principle of discrete + layer-by-layer accumulation and the characteristic of rapid free forming, and has great application potential in the process of preparing materials. The laser additive manufacturing technology as an advanced high-performance metal manufacturing technology can be divided into a laser forming technology for synchronous material feeding and a selective laser melting technology for powder laying. The laser additive manufacturing method with the synchronous material feeding mode has obvious advantages in preparing gradient materials, and is high in forming efficiency and high in flexibility.
Disclosure of Invention
The invention aims to solve the technical problem of providing an additive manufacturing method of an in-situ synthesized micro-nano TiC reinforced titanium-based composite material aiming at the defects of the prior art. According to the method, uniform and stable composite powder is obtained by a ball-milling mixing method and adding aerosol and is used as a raw material, and then an authigenic micro-nano TiC reinforcing phase which is uniformly distributed and has good interface transition is formed in a titanium matrix formed by additive based on extremely high cooling rate in a laser additive manufacturing process, so that the problem that the size and distribution of the reinforcing phase are difficult to control in the process of preparing the particle reinforced titanium-based composite material is effectively solved, and the plasticity and strength of the titanium-based composite material are improved at the same time.
In order to solve the technical problems, the invention adopts the technical scheme that: the additive manufacturing method of the in-situ synthesized micro-nano TiC reinforced titanium-based composite material is characterized by comprising the following steps of:
step one, a powder preparation process: adding titanium powder or titanium alloy powder and amorphous nano carbon powder into absolute ethyl alcohol for mixing, then placing the mixture into a ball mill for ball milling treatment, obtaining ball milling powder through primary drying, spraying aerosol into the ball milling powder, uniformly stirring, and obtaining composite powder through secondary drying; the size of the titanium powder or the titanium alloy powder is 15-200 mu m; the amorphous nanocarbon powder has an average size of less than 100 nm;
and step two, taking the composite powder obtained in the step one as a raw material, adopting a laser additive manufacturing method, fixing the base material on a workbench, then moving a laser spot in an XY horizontal plane of the base material to complete one-layer scanning to obtain single-layer entity slices, and repeating the scanning process until a plurality of single-layer entity slices are stacked layer by layer to form the in-situ self-generated micro-nano TiC reinforced titanium-based composite material.
The invention firstly mixes titanium powder or titanium alloy powder with amorphous carbon nanopowder, then ball-milling treatment is carried out, the mixing uniformity of the titanium powder or titanium alloy powder and the amorphous carbon nanopowder is improved, the amorphous carbon nanopowder is stably coated on the titanium powder or titanium alloy powder by spraying aerosol to obtain composite powder, the aerosol is a macromolecular polymer, the amorphous carbon nanopowder can be effectively coated on the titanium powder or titanium alloy powder without falling off, the bonding firmness of the titanium powder or titanium alloy powder and the amorphous carbon nanopowder is improved, the agglomeration problem and the falling problem caused by volume fraction and particle size difference in the composite powder are effectively solved, the stability of the composite powder is ensured, and then the composite powder is used as a raw material to obtain the in-situ self-generated micro nano TiC reinforced titanium-based composite material by adopting a laser material increase manufacturing method, the composite powder is heated and melted under the action of high-energy laser to form a tiny molten pool, because the temperature of the central area of the molten pool is higher than the surrounding dimensions, the surface tension corresponding to the central area can be less than the surrounding surface tension, a flow field flowing from the middle to the surrounding is formed, namely Marangoni convection, under the stirring action of strong Marangoni convection, the composite powder melt in the molten pool is fully mixed and then is uniformly distributed and simultaneously reacts, the titanium powder or the titanium alloy powder and the amorphous nano-carbon powder self-generate TiC reinforced phase which is uniformly distributed in situ and are separated out in the rapid cooling process of the molten pool, and the TiC reinforced phase is fast in separation speed and cannot grow into dendrite, so that the in-situ self-generated TiC reinforced phase has small size to micro-nano size, is uniformly distributed, the interface with the titanium-based body is well transited without obvious sharp edges, and the local stress concentration probability around the TiC reinforced phase is greatly, the strength and the plasticity of the in-situ synthesized micro-nano TiC reinforced titanium-based composite material are improved at the same time.
The additive manufacturing method of the in-situ synthesized micro-nano TiC reinforced titanium-based composite material is characterized in that in the first step, the addition amount of the amorphous nano carbon powder is 0.3% -5% of the total mass of the titanium powder or the titanium alloy powder and the amorphous nano carbon powder. The method effectively ensures the uniform and stable compounding of the amorphous carbon nanopowder and the titanium powder or the titanium alloy powder, and reduces the addition amount of the amorphous carbon nanopowder.
The additive manufacturing method of the in-situ synthesized micro-nano TiC reinforced titanium-based composite material is characterized in that in the first step, the ratio of the addition volume of the absolute ethyl alcohol to the total mass of the titanium powder and the amorphous nano carbon powder and the ratio of the addition volume of the absolute ethyl alcohol to the total mass of the titanium alloy powder and the amorphous nano carbon powder are (0.25-0.75): 1, wherein the volume is in mL and the mass is in g. The addition volume of the optimized anhydrous ethanol ensures the smooth proceeding of the ball milling process, is beneficial to fully and uniformly mixing the titanium powder or the titanium alloy powder and the amorphous carbon nanopowder, and simultaneously reduces the energy consumption of primary drying.
The additive manufacturing method of the in-situ synthesized micro-nano TiC reinforced titanium-based composite material is characterized in that in the first step, the rotation speed adopted by ball milling treatment is 100 r/min-300 r/min, the ball-material ratio is 1 (1.5-3), and the time is 2 h-5 h. The technological parameters of the optimized ball milling treatment not only ensure the sufficient and uniform composition of the amorphous carbon nano-powder and the titanium powder or the titanium alloy powder, but also avoid the phenomenon of processing hardening of the ball milling powder caused by the thinning of the ball milling powder particles due to excessive ball milling, and are not beneficial to the subsequent additive manufacturing.
The additive manufacturing method of the in-situ synthesized micro-nano TiC reinforced titanium-based composite material is characterized in that the temperature of primary drying in the step one is 60-100 ℃, and the time is 3-6 hours. The technological parameters of the optimized primary drying can effectively remove the absolute ethyl alcohol in the mixed solution after the ball milling treatment.
The additive manufacturing method of the in-situ synthesized micro-nano TiC reinforced titanium-based composite material is characterized in that in the first step, the aerosol is polyvinyl alcohol aerosol with the volume fraction of 2.7%, and the addition amount of the aerosol is 1-3% of the mass of the ball-milled powder. The polyvinyl alcohol aerosol has unique strong adhesion and better dispersibility, thereby not only ensuring the firmness of adhesion, but also ensuring the uniformity of adhered powder; the addition amount of the optimized aerosol further promotes the aerosol to be uniformly distributed in the ball-milled powder, ensures that the amorphous carbon nano-powder is firmly adhered to the surface of the titanium powder or the titanium alloy powder, and simultaneously avoids the defects of reinforcing in-situ authigenic submicron and air holes in the nano-particle reinforced composite material and the like caused by excessive addition.
The additive manufacturing method of the in-situ synthesized micro-nano TiC reinforced titanium-based composite material is characterized in that in the first step, secondary drying is carried out in a vacuum drying oven, the temperature of the secondary drying is 100-120 ℃, and the time is 1-3 hours. The vacuum drying oven and the optimized secondary drying technological parameters can effectively prevent the composite powder from being oxidized in the high-temperature secondary drying process, and ensure the quality of the in-situ synthesized submicron and nano particle reinforced composite material.
The additive manufacturing method of the in-situ synthesized micro-nano TiC reinforced titanium-based composite material is characterized in that the laser additive manufacturing method in the second step is a pulse laser forming method or a selective laser melting method. The cooling speed in the molten pool formed in the process of the two optimal selection methods is faster, the Marangoni convection in the molten pool is stronger, and the size fineness and the uniformity degree of the TiC reinforcing phase generated in situ by self-generation are further improved.
The additive manufacturing method of the in-situ synthesized micro-nano TiC reinforced titanium-based composite material is characterized in that high-purity argon is introduced in the laser additive manufacturing method in the second step, so that the oxygen content in the manufacturing process is reduced to be below 500 ppm. By the oxygen control process, the adverse effect of impurity elements on the in-situ synthesized submicron and nano particle reinforced composite material is effectively reduced, and the mechanical property of the in-situ synthesized submicron and nano particle reinforced composite material is ensured.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, uniform and stable composite powder is obtained by a ball-milling mixing method and adding aerosol as a raw material, and then an authigenic micro-nano TiC reinforcing phase which is uniformly distributed and has good interface transition is formed in a titanium matrix formed by additive based on extremely high cooling rate in a laser additive manufacturing process, so that the problem that the size and distribution of the reinforcing phase are difficult to control in the process of preparing the particle reinforced titanium-based composite material is effectively solved, and the plasticity and strength of the titanium-based composite material are improved at the same time.
2. The amorphous carbon nano powder particles selected by the invention are small and have low addition amount, and are completely melted in a molten pool under the action of high-energy laser, so that the obtained in-situ synthesized micro-nano TiC reinforced titanium-based composite material is not mixed with refractory powder, and is favorable for obtaining TiC reinforced phase particles with small size, and the interface of the TiC reinforced phase and a titanium matrix or a titanium alloy matrix has good transition, thereby further improving the reinforcing effect of the TiC reinforced phase.
3. According to the invention, the interface reaction between the titanium matrix or the titanium alloy matrix in the in-situ synthesized micro-nano TiC reinforced titanium-based composite material and the reinforcing phase is avoided through the in-situ synthesized TiC reinforcing phase, and the pollution problem caused by the introduction of additional particles is avoided, so that the interface is clean and the combination is good.
4. According to the invention, through a ball-milling mixing method and addition of aerosol, the mixing uniformity of the titanium powder or the titanium alloy powder and the amorphous carbon nanopowder is improved, so that the amorphous carbon nanopowder particles are uniformly and stably coated around the titanium powder or the titanium alloy powder, the problem of agglomeration caused by volume fraction and particle size difference in the composite powder is effectively solved, the bonding firmness degree of the titanium powder or the titanium alloy powder and the amorphous carbon nanopowder is improved, and the stability of the composite powder is ensured.
5. The two preferable additive manufacturing methods can provide higher cooling speed, so that the reinforced particles are not long enough to grow, the formation of dendritic crystal TiC is further reduced, the formation of fine and uniform TiC reinforced phases is ensured, and the improvement of the plasticity of the in-situ synthesized micro-nano TiC reinforced titanium-based composite material is further facilitated.
6. The amorphous carbon nanopowder adopted by the invention has good adhesion performance on the surface of the titanium powder or the titanium alloy powder, so that the smooth operation of the preparation process is ensured, and the amorphous carbon nanopowder has relatively low price, so that the preparation cost is effectively reduced compared with the added expensive TiC, graphene and the like.
The technical solution of the present invention is further described in detail by the accompanying drawings and examples.
Drawings
FIG. 1 is a flow chart of the process for preparing the composite powder of the present invention.
Fig. 2 is an SEM image of the in-situ synthesized micro-nano TiC reinforced titanium-based composite material formed in example 1 of the present invention.
Fig. 3 is an SEM image of the in-situ synthesized micro-nano TiC reinforced titanium-based composite material formed in embodiment 2 of the present invention.
Fig. 4 is an SEM image of the in-situ synthesized micro-nano TiC reinforced titanium-based composite material formed in embodiment 3 of the present invention.
Fig. 5 is an SEM image of the in-situ synthesized micro-nano TiC reinforced titanium-based composite material formed in embodiment 4 of the present invention.
Detailed Description
As shown in fig. 1, the preparation process of the composite powder of the present invention comprises: adding titanium powder or titanium alloy powder and amorphous nano carbon powder into absolute ethyl alcohol, then carrying out ball milling treatment, adding aerosol after primary drying, stirring, and then carrying out secondary drying to obtain composite powder of amorphous nano carbon powder uniformly coated with titanium powder or titanium alloy powder.
Example 1
The embodiment comprises the following steps:
step one, a powder preparation process: adding 79.76g of pure titanium powder with the size of 45-100 microns and the mass purity of 99.5 percent and 0.24g of amorphous nano carbon powder with the average size of 90nm and the mass purity of 99 percent into 20mL of absolute ethyl alcohol for mixing, then placing the mixture into a ball mill for ball milling treatment, then placing the mixture into a vacuum drying oven for primary drying for 3 hours at the temperature of 60 ℃ to obtain ball milled powder, spraying 0.8g of polyvinyl alcohol aerosol with the volume fraction of 2.7 percent into the ball milled powder, stirring for 20 minutes, placing the mixture into a vacuum drying oven for secondary drying for 1 hour at the temperature of 100 ℃, and sieving to remove particles with the size of more than 120 microns to obtain composite powder; the rotation speed adopted by the ball milling treatment is 100r/min, the ball-material ratio is 1:1.5, and the time is 5 h;
step two, taking the composite powder obtained in the step one as a raw material, adopting a YAG pulse laser glove box system to perform pulse laser additive manufacturing, fixing a TC4 titanium alloy base material on a workbench, then moving a laser spot in an XY horizontal plane to complete one-layer scanning to obtain single-layer entity slices, repeating the scanning process until a plurality of single-layer entity slices are stacked layer by layer to form an in-situ self-generated micro-nano TiC reinforced titanium-based composite material; argon with the mass purity of 99% is introduced in the pulse laser additive manufacturing process, so that the oxygen content in the manufacturing process is reduced to be below 500ppm, and the process parameters of the pulse laser additive manufacturing are as follows: the current 115A, the working frequency 15Hz, the pulse width 7ms, the laser power 85W and the lifting amount 0.15 mm.
The microstructure of the in-situ synthesized micro-nano TiC reinforced titanium-based composite material formed in the embodiment is observed, and the mechanical property is tested. Fig. 2 is an SEM image of the in-situ synthesized micro-nano TiC reinforced titanium-based composite material formed in the present embodiment, and as can be seen from fig. 2, the average size of TiC reinforcing phase particles in the in-situ synthesized micro-nano TiC reinforced titanium-based composite material formed in the present embodiment is 370nm, the distribution is uniform, and the interface transition with the titanium matrix is good; the mechanical property test result shows that: the tensile strength of the in-situ synthesized micro-nano TiC reinforced titanium-based composite material formed in the embodiment is 563MPa, and the elongation is 29.8%, which shows that the in-situ synthesized micro-nano TiC reinforced titanium-based composite material provided by the invention has excellent strength and plasticity.
Comparative example 1
This comparative example comprises the following steps:
step one, a powder preparation process: adding 79.76g of pure titanium powder with the size of 45-100 microns and the mass purity of 99.5 percent and 0.24g of amorphous nano carbon powder with the average size of 90nm and the mass purity of 99 percent into 20mL of absolute ethyl alcohol for mixing, then placing the mixture into a ball mill for ball milling treatment, then placing the mixture into a vacuum drying oven for primary drying for 3 hours at the temperature of 60 ℃ to obtain ball milled powder, spraying 0.8g of polyvinyl alcohol aerosol with the volume fraction of 2.7 percent into the ball milled powder, stirring for 20 minutes, placing the mixture into a vacuum drying oven for secondary drying for 1 hour at the temperature of 100 ℃, and sieving to remove particles with the size of more than 120 microns to obtain composite powder; the rotation speed adopted by the ball milling treatment is 100r/min, the ball-material ratio is 1:1.5, and the time is 5 h;
step two, sintering the composite powder obtained in the step one into a cylindrical blank with the diameter of 42.0mm and the height of 32.0mm by adopting spark plasma sintering equipment, preheating the cylindrical blank to 1000 ℃, keeping the temperature for 180s in an argon atmosphere, and extruding by adopting a hydraulic press at an extrusion ratio of 37:1 to obtain the in-situ synthesized TiC reinforced titanium-based composite material; the sintering temperature is 1000 ℃, the time is 1.8ks, and the pressure is 30 MPa.
And observing the microstructure of the in-situ synthesized TiC reinforced titanium-based composite material formed in the comparative example, and testing the mechanical property. Microstructure observations showed: the average size of TiC reinforcing phase particles in the in-situ synthesized TiC reinforced titanium-based composite material formed by the comparative example is about 2 mu m; the mechanical property test result shows that: the tensile strength of the in-situ synthesized micro-nano TiC reinforced titanium-based composite material formed by the comparative example is 590MPa, and the elongation is 18.6%.
Comparing the embodiment 1 with the comparative example 1, it can be seen that the adoption of the laser additive manufacturing method effectively promotes the pure titanium powder and the amorphous nano carbon powder to generate TiC reinforcing phases with uniform distribution in situ, and the TiC reinforcing phases are separated out in the rapid cooling process of a molten pool to form the TiC reinforcing phases with submicron and nanometer sizes, and the combination transition of the TiC reinforcing phases and a titanium matrix is good, so that the plasticity and the strength of the titanium-based composite material are improved at the same time.
Comparative example 2
The embodiment comprises the following steps:
step one, a powder preparation process: adding 79.76g of pure titanium powder with the size of 45-100 microns and the mass purity of 99.5 percent and 0.24g of amorphous nano carbon powder with the average size of 90nm and the mass purity of 99 percent into 20mL of absolute ethyl alcohol for mixing, then placing the mixture into a ball mill for ball milling treatment, then placing the mixture into a vacuum drying oven for primary drying for 3 hours at the temperature of 60 ℃ to obtain ball-milled powder, then placing the ball-milled powder into the vacuum drying oven for secondary drying for 1 hour at the temperature of 100 ℃, and screening to remove particles with the size of more than 120 microns to obtain composite powder; the rotation speed adopted by the ball milling treatment is 100r/min, the ball-material ratio is 1:1.5, the time is 5 hours, and the ball milling treatment process is carried out;
step two, taking the composite powder obtained in the step one as a raw material, adopting a YAG pulse laser glove box system to perform pulse laser additive manufacturing, fixing a TC4 titanium alloy base material on a workbench, then moving a laser spot in an XY horizontal plane to complete one-layer scanning to obtain single-layer entity slices, repeating the scanning process until a plurality of single-layer entity slices are stacked layer by layer to form an in-situ self-generated micro-nano TiC reinforced titanium-based composite material; argon with the mass purity of 99% is introduced in the pulse laser additive manufacturing process, so that the oxygen content in the manufacturing process is reduced to be below 500ppm, and the process parameters of the pulse laser additive manufacturing are as follows: the current 115A, the working frequency 15Hz, the pulse width 7ms, the laser power 85W and the lifting amount 0.15 mm.
And observing the microstructure of the in-situ synthesized TiC reinforced titanium-based composite material formed in the comparative example, and testing the mechanical property. Microstructure observations showed: the average size of TiC reinforcing phase particles in the in-situ synthesized micro-nano reinforced titanium-based composite material formed by the comparative example is about 1.2 mu m; the mechanical property test result shows that: the tensile strength of the in-situ authigenic micro-nano reinforced titanium-based composite material formed by the comparative example is 571MPa, and the elongation is 15.4%.
Comparing the example 1 with the comparative example 2, it can be seen that the mixing uniformity of the titanium powder or the titanium alloy powder and the amorphous carbon nanopowder is improved by the ball milling mixing method and the addition of the aerosol, so that the amorphous carbon nanopowder particles are uniformly and stably coated around the titanium powder or the titanium alloy powder, the problem of agglomeration caused by volume fraction and particle size difference in the composite powder is effectively solved, the bonding firmness of the titanium powder or the titanium alloy powder and the amorphous carbon nanopowder is improved, the stability of the composite powder is ensured, the formation of fine and uniform TiC reinforcing phases is facilitated, and the improvement of the plasticity of the in-situ TiC reinforced titanium-based composite material is further facilitated.
Comparing the embodiment 1 with the comparative example 1 and the comparative example 2, the amorphous carbon nano powder is uniformly and firmly coated on the titanium powder or the titanium alloy powder by a ball milling mixing method and the action of adding aerosol to obtain uniform and stable composite powder, meanwhile, the in-situ synthesized micro-nano TiC reinforced titanium-based composite material is prepared by combining a laser additive manufacturing method, the TiC reinforced phase with uniformly distributed micro-nano sizes is generated in situ by utilizing the forming characteristic of the laser additive manufacturing method, the interface transition between the titanium matrix and the TiC reinforced phase is good, and the plasticity and the strength of the in-situ synthesized micro-nano TiC reinforced titanium-based composite material are improved.
Example 2
The embodiment comprises the following steps:
step one, a powder preparation process: adding 76g of pure titanium powder with the size of 15-45 microns and the mass purity of 99.5 percent and 4g of amorphous nano carbon powder with the average size of 40nm and the mass purity of 99 percent into 60mL of absolute ethyl alcohol to form a mixed solution, then placing the mixed solution into a ball mill for ball milling treatment, placing the mixed solution into a vacuum drying oven for primary drying for 6 hours at the temperature of 100 ℃ to obtain ball milled powder, spraying 2.4g of polyvinyl alcohol aerosol with the volume fraction of 2.7 percent into the ball milled powder, stirring for 20 minutes, placing the ball milled powder into a vacuum drying oven for secondary drying for 3 hours at the temperature of 120 ℃, and sieving to remove particles with the size of more than 50 microns to obtain composite powder; the rotation speed adopted by the ball milling treatment is 300r/min, the ball-material ratio is 1:3, and the time is 2 h;
step two, taking the composite powder obtained in the step one as a raw material, adopting AM250 Additive Metal laser three-dimensional forming equipment to perform selective laser Additive manufacturing, fixing a TC4 titanium alloy base material on a workbench, moving a laser spot in an XY horizontal plane to complete one-layer scanning to obtain single-layer entity slices, and repeating the scanning process until a plurality of single-layer entity slices are stacked layer by layer to form the in-situ self-generated micro-nano TiC reinforced titanium-based composite material; argon with the mass purity of 99% is introduced in the pulse laser additive manufacturing process, so that the oxygen content in the manufacturing process is reduced to be below 100ppm, and the process parameters of the pulse laser additive manufacturing are as follows: the laser power is 175W, the spot diameter is 0.1mm, the scanning speed is 700mm/s, and the lapping rate is 40%.
Observing the microstructure of the in-situ synthesized micro-nano TiC reinforced titanium-based composite material formed in the embodiment, and testing the mechanical property; fig. 3 is a SEM image of the in-situ synthesized micro-nano TiC reinforced titanium-based composite material formed in the present embodiment, and as can be seen from fig. 3, the average size of TiC reinforcing phase particles in the in-situ synthesized micro-nano TiC reinforced titanium-based composite material formed in the present embodiment is 550nm, and the particles have good interface transition with a titanium matrix and uniform distribution; the mechanical property test result shows that: the tensile strength of the in-situ synthesized micro-nano TiC reinforced titanium-based composite material formed in the embodiment is 770MPa, and the elongation is 24.1%, which shows that the in-situ synthesized micro-nano TiC reinforced titanium-based composite material provided by the invention has excellent strength and plasticity.
Example 3
The embodiment comprises the following steps:
step one, a powder preparation process: adding 79.2g of Ti60 powder with the size of 45-100 microns and the mass purity of 99.5 percent and 0.8g of amorphous nano-carbon powder with the average size of 60nm into 40mL of absolute ethyl alcohol for mixing, then placing the mixture into a ball mill for ball milling treatment, then placing the mixture into a vacuum drying oven for primary drying for 4.5 hours at the temperature of 85 ℃ to obtain ball-milled powder, spraying 1.6g of polyvinyl alcohol aerosol with the volume fraction of 2.7 percent into the ball-milled powder, stirring for 20 minutes, placing the mixture into the vacuum drying oven for secondary drying for 2 hours at the temperature of 110 ℃, and sieving to remove particles with the size of more than 120 microns to obtain composite powder; the rotation speed adopted by the ball milling treatment is 200r/min, the ball-material ratio is 1:2, and the time is 3 h;
step two, taking the composite powder obtained in the step one as a raw material, adopting a YAG pulse laser glove box system to perform pulse laser additive manufacturing, fixing a TC4 titanium alloy base material on a workbench, then moving a laser spot in an XY horizontal plane to complete one-layer scanning to obtain single-layer entity slices, repeating the scanning process until a plurality of single-layer entity slices are stacked layer by layer to form an in-situ self-generated micro-nano TiC reinforced titanium-based composite material; argon with the mass purity of 99% is introduced in the pulse laser additive manufacturing process, so that the oxygen content in the manufacturing process is reduced to be below 500ppm, and the process parameters of the pulse laser additive manufacturing are as follows: the current is 85A, the working frequency is 15Hz, the pulse width is 7ms, the laser power is 135W, and the lifting amount is 0.2 mm.
The microstructure of the in-situ synthesized micro-nano TiC reinforced titanium-based composite material formed in the embodiment is observed, and the mechanical property is tested. Fig. 4 is an SEM image of the in-situ synthesized micro-nano TiC reinforced titanium-based composite material formed in the present embodiment, and as can be seen from fig. 4, the average size of TiC reinforcing phase particles in the in-situ synthesized micro-nano TiC reinforced titanium-based composite material formed in the present embodiment is 330nm, and the particles have good interface transition with the titanium matrix and uniform distribution; the mechanical property test result shows that: the tensile strength of the in-situ synthesized micro-nano TiC reinforced titanium-based composite material formed in the embodiment is 1350MPa, and the elongation is 14.2%, which shows that the in-situ synthesized micro-nano TiC reinforced titanium-based composite material provided by the invention has excellent strength and plasticity.
Example 4
The embodiment comprises the following steps:
step one, a powder preparation process: adding 79.4g of pure titanium powder with the size of 15-45 microns and the mass purity of 99.5 percent and 0.6g of amorphous nano carbon powder with the average size of 40nm and the mass purity of 99 percent into 50mL of absolute ethyl alcohol for mixing, then placing the mixture into a ball mill for ball milling treatment, then placing the mixture into a vacuum drying oven for primary drying for 5.5 hours at the temperature of 70 ℃ to obtain ball milled powder, spraying 1.6g of polyvinyl alcohol aerosol with the volume fraction of 2.7 percent into the ball milled powder, stirring for 20 minutes, placing the mixture into a vacuum drying oven for secondary drying for 2 hours at the temperature of 120 ℃, and sieving to remove particles with the size of more than 50 microns to obtain composite powder; the rotation speed adopted by the ball milling treatment is 150r/min, the ball-material ratio is 1:2, and the time is 4 h;
step two, taking the composite powder obtained in the step one as a raw material, adopting AM250 Additive Metal laser three-dimensional forming equipment to perform selective laser Additive manufacturing, fixing a TC4 titanium alloy base material on a workbench, moving a laser spot in an XY horizontal plane to complete one-layer scanning to obtain single-layer entity slices, and repeating the scanning process until a plurality of single-layer entity slices are stacked layer by layer to form the in-situ self-generated micro-nano TiC reinforced titanium-based composite material; argon with the mass purity of 99% is introduced in the pulse laser additive manufacturing process, so that the oxygen content in the manufacturing process is reduced to be below 100ppm, and the process parameters of the pulse laser additive manufacturing are as follows: the laser power is 175W, the spot diameter is 0.1mm, the scanning speed is 700mm/s, and the lapping rate is 40%.
The microstructure of the in-situ synthesized micro-nano TiC reinforced titanium-based composite material formed in the embodiment is observed, and the mechanical property is tested. Fig. 5 is an SEM image of the in-situ synthesized micro-nano TiC reinforced titanium-based composite material formed in the present embodiment, and as can be seen from fig. 5, the average size of TiC reinforcing phase particles in the in-situ synthesized micro-nano TiC reinforced titanium-based composite material formed in the present embodiment is 460nm, and the particles have good interface transition with the titanium matrix and uniform distribution; the mechanical property test result shows that: the tensile strength of the in-situ synthesized micro-nano TiC reinforced titanium-based composite material formed in the embodiment is 586MPa, and the elongation is 31.4%, which shows that the in-situ synthesized micro-nano TiC reinforced titanium-based composite material provided by the invention has excellent strength and plasticity.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (9)
1. The additive manufacturing method of the in-situ synthesized micro-nano TiC reinforced titanium-based composite material is characterized by comprising the following steps of:
step one, a powder preparation process: adding titanium powder or titanium alloy powder and amorphous nano carbon powder into absolute ethyl alcohol for mixing, then placing the mixture into a ball mill for ball milling treatment, obtaining ball milling powder through primary drying, spraying aerosol into the ball milling powder, uniformly stirring, and obtaining composite powder through secondary drying; the size of the titanium powder or the titanium alloy powder is 15-200 mu m; the amorphous nanocarbon powder has an average size of less than 100 nm;
and step two, taking the composite powder obtained in the step one as a raw material, adopting a laser additive manufacturing method, fixing the base material on a workbench, then moving a laser spot in an XY horizontal plane of the base material to complete one-layer scanning to obtain single-layer entity slices, and repeating the scanning process until a plurality of single-layer entity slices are stacked layer by layer to form the in-situ self-generated micro-nano TiC reinforced titanium-based composite material.
2. The in-situ synthesis micro-nano TiC enhanced titanium-based composite material additive manufacturing method according to claim 1, wherein in the first step, the addition amount of the amorphous carbon nano-powder is 0.3-5% of the total mass of the titanium powder or the titanium alloy powder and the amorphous carbon nano-powder.
3. The in-situ synthesis micro-nano TiC enhanced titanium-based composite material additive manufacturing method according to claim 1, wherein the ratio of the addition volume of the absolute ethyl alcohol to the total mass of the titanium powder and the amorphous nano carbon powder and the ratio of the addition volume of the absolute ethyl alcohol to the total mass of the titanium alloy powder and the amorphous nano carbon powder in the step one are both (0.25-0.75): 1, wherein the volume is in mL and the mass is in g.
4. The additive manufacturing method of in-situ synthesized micro-nano TiC reinforced titanium-based composite material according to claim 1, wherein the rotation speed adopted by the ball milling treatment in the first step is 100 r/min-300 r/min, the ball-to-material ratio is 1 (1.5-3), and the time is 2 h-5 h.
5. The additive manufacturing method of in-situ synthesized micro-nano TiC reinforced titanium-based composite material according to claim 1, wherein the temperature of primary drying in the first step is 60-100 ℃, and the time is 3-6 h.
6. The in-situ synthesis micro-nano TiC enhanced titanium-based composite material additive manufacturing method according to claim 1, wherein in the first step, the aerosol is polyvinyl alcohol aerosol with a volume fraction of 2.7%, and the addition amount of the aerosol is 1-3% of the mass of the ball-milled powder.
7. The in-situ synthesis micro-nano TiC enhanced titanium-based composite material additive manufacturing method according to claim 1, characterized in that in the first step, the secondary drying is carried out in a vacuum drying oven, the temperature of the secondary drying is 100-120 ℃, and the time is 1-3 h.
8. The in-situ synthesis micro-nano TiC enhanced titanium-based composite material additive manufacturing method according to claim 1, wherein the laser additive manufacturing method in the second step is a pulse laser forming method or a selective laser melting method.
9. The in-situ synthesis micro-nano TiC enhanced titanium-based composite material additive manufacturing method according to claim 1, characterized in that in the second step, high-purity argon is introduced in the laser additive manufacturing method process to reduce the oxygen content in the manufacturing process to below 500 ppm.
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