CN116607039A - Preparation method of graphene reinforced TC4 titanium-based composite material - Google Patents
Preparation method of graphene reinforced TC4 titanium-based composite material Download PDFInfo
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Abstract
The invention discloses a preparation method of a graphene reinforced TC4 titanium-based composite material, which relates to the technical field of titanium-based composite materials, and comprises the following steps: performing low-temperature high-energy ball milling on the TC4 titanium alloy powder to obtain nano-scale TC4 titanium alloy powder; in-situ self-generating graphene on the surface of nano TC4 titanium alloy powder by adopting a chemical vapor deposition method to obtain graphene-coated TC4 titanium alloy powder; and treating the TC4 titanium alloy powder coated by the graphene by adopting a spark plasma sintering method to obtain the graphene reinforced TC4 titanium-based composite material. The high-energy ball milling can reduce the activity of the titanium alloy on one hand and avoid the reaction between the titanium alloy and a ball milling tank to the greatest extent; on the other hand, the brittleness of the titanium alloy can be increased, and the size of the powder is conveniently refined. In addition, the chemical vapor deposition method is used for generating graphene on the surface of the nano TC4 titanium alloy powder in situ, and the graphene is tightly combined with a matrix phase interface, so that the material strength is improved, and the high plasticity is maintained.
Description
Technical Field
The invention relates to the technical field of titanium-based composite materials, in particular to a preparation method of a graphene reinforced TC4 titanium-based composite material.
Background
Titanium alloys are being favored in the aerospace and marine equipment fields because of their high strength and excellent corrosion resistance, and are gradually replacing traditional steels. However, as the material strength requirements increase, it is difficult to break through the existing titanium alloy strength by means of compositional optimization and thermo-mechanical treatment alone. Accordingly, titanium-based composite materials incorporating reinforcing phases have received increasing attention.
At present, a ceramic material is selected as the reinforcing phase, the reinforcing phase and titanium powder are mixed in a ball milling mode and the like, and a powder metallurgy mode is adopted to prepare the titanium-based composite material. However, the composite material prepared by adopting the mechanical mixing and powder metallurgy method has poor interface combination between the reinforcing phase and the matrix phase, so that the plasticity is seriously reduced, the dispersibility of the reinforcing phase is poor, and the preparation of large-size materials is difficult to develop.
Disclosure of Invention
The invention aims to provide a preparation method of a graphene reinforced TC4 titanium-based composite material, which is used for solving the technical problems.
In order to achieve the above object, the present invention provides a preparation method of a graphene reinforced TC4 titanium-based composite material, the method comprising:
performing low-temperature high-energy ball milling on the TC4 titanium alloy powder to obtain nano-scale TC4 titanium alloy powder;
adopting a chemical vapor deposition method to generate graphene in situ on the surface of the nano-scale TC4 titanium alloy powder to obtain graphene-coated TC4 titanium alloy powder;
and treating the TC4 titanium alloy powder coated by the graphene by adopting a spark plasma sintering method to obtain the graphene reinforced TC4 titanium-based composite material.
Optionally, performing low-temperature high-energy ball milling on the TC4 titanium alloy powder to obtain nano-scale TC4 titanium alloy powder, which comprises the following steps: and performing low-temperature ball milling on the TC4 titanium alloy powder by adopting a high-energy ball milling method in a low-temperature environment to obtain the nano-grade TC4 titanium alloy powder.
Optionally, the nano-scale TC4 titanium alloy powder is TC4 titanium alloy powder with the granularity distribution of 60-90nm, and the low-temperature ball milling time is 40-60min.
Optionally, in-situ self-generating graphene on the surface of the nano-scale TC4 titanium alloy powder by adopting a chemical vapor deposition method to obtain graphene-coated TC4 titanium alloy powder, which comprises the following steps:
placing the nano-scale TC4 titanium alloy powder into a constant temperature part of a CVD tube furnace;
after vacuumizing and removing residual air in the tube, heating the CVD tube furnace to a preset temperature in an argon and hydrogen atmosphere, and preserving heat;
and after the heat preservation is finished, introducing methane gas and maintaining for 15-20min to obtain the TC4 titanium alloy powder coated by the graphene.
Optionally, the inflow rates of the argon, the hydrogen and the methane are 280-320sccm, 80-120sccm and 20-30sccm respectively.
Optionally, the preset temperature is 650-750 ℃, and the heat preservation time is 20-30min.
Optionally, a discharge plasma sintering method is adopted to process the graphene-coated TC4 titanium alloy powder to obtain a graphene-reinforced TC4 titanium-based composite material, which comprises the following steps:
placing the graphene-coated TC4 titanium alloy powder into a graphite mold;
and sintering the graphene-coated TC4 titanium alloy powder in the graphite mold by adopting a discharge plasma sintering furnace to obtain the graphene-reinforced TC4 titanium-based composite material.
Optionally, the sintering conditions include: sintering at 950-1050 deg.c and 80-100 MPa for 2min.
Optionally, the method further comprises: and performing hot extrusion on the graphene reinforced TC4 titanium-based composite material to obtain a target bar.
Optionally, hot extrusion is performed at 860-900 ℃.
The invention has the technical effects and advantages that:
the invention provides a preparation method of a graphene reinforced TC4 titanium-based composite material, which comprises the following steps: performing low-temperature high-energy ball milling on the TC4 titanium alloy powder to obtain nano-scale TC4 titanium alloy powder; adopting a chemical vapor deposition method to generate graphene in situ on the surface of the nano-scale TC4 titanium alloy powder to obtain graphene-coated TC4 titanium alloy powder; and treating the TC4 titanium alloy powder coated by the graphene by adopting a spark plasma sintering method to obtain the graphene reinforced TC4 titanium-based composite material.
The method adopts low-temperature high-energy ball milling to further refine the purchased TC4 titanium alloy spherical powder, so as to obtain nano TC4 titanium alloy powder, and enhance the surface activity of the powder; the activity of the titanium alloy can be reduced on the one hand by carrying out high-energy ball milling in a low-temperature environment, and the reaction between the titanium alloy and a ball milling tank is avoided to the greatest extent; on the other hand, the brittleness of the titanium alloy can be increased, and the size of the powder is conveniently refined. In addition, graphene is generated on the surface of the nano-scale TC4 titanium alloy powder in situ by a chemical vapor deposition method, the TC4 titanium alloy powder coated by the graphene is obtained, and after spark plasma sintering, a compact graphene reinforced TC4 titanium-based composite material can be obtained, and the graphene obtained by the in situ self-generation method is tightly combined with a matrix phase interface, so that the strength of the material is improved, and meanwhile, the high plasticity is maintained.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention may be realized and attained by the structure particularly pointed out in the written description and drawings.
Drawings
Fig. 1 is a flow chart of a preparation method of a graphene reinforced TC4 titanium-based composite material.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which some, but not all embodiments of the invention are shown. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be noted that, the structures, proportions, sizes and the like shown in the drawings attached to the present specification are used for understanding and reading only in conjunction with the disclosure of the present specification, and are not intended to limit the applicable limitations of the present invention, so that any modification of the structures, variation of proportions or adjustment of sizes of the structures, proportions and the like should not be construed as essential to the present invention, and should still fall within the scope of the disclosure of the present invention without affecting the efficacy and achievement of the present invention. Also, the terms such as "upper," "lower," "left," "right," "middle," and "a" and the like recited in the present specification are merely for descriptive purposes and are not intended to limit the scope of the invention, but are intended to provide relative positional changes or modifications without materially altering the technical context in which the invention may be practiced.
In order to solve the defects in the prior art, the invention discloses a preparation method of a graphene reinforced TC4 titanium-based composite material, which comprises the following steps: performing low-temperature high-energy ball milling on the TC4 titanium alloy powder to obtain nano-scale TC4 titanium alloy powder; adopting a chemical vapor deposition method to generate graphene in situ on the surface of the nano-scale TC4 titanium alloy powder to obtain graphene-coated TC4 titanium alloy powder; and treating the TC4 titanium alloy powder coated by the graphene by adopting a spark plasma sintering method to obtain the graphene reinforced TC4 titanium-based composite material.
The method adopts low-temperature high-energy ball milling to further refine the purchased TC4 titanium alloy spherical powder, so as to obtain nano TC4 titanium alloy powder, and enhance the surface activity of the powder; the activity of the titanium alloy can be reduced on the one hand by carrying out high-energy ball milling in a low-temperature environment, and the reaction between the titanium alloy and a ball milling tank is avoided to the greatest extent; on the other hand, the brittleness of the titanium alloy can be increased, and the size of the powder is conveniently refined. In addition, graphene is generated on the surface of the nano-scale TC4 titanium alloy powder in situ by a chemical vapor deposition method, the TC4 titanium alloy powder coated by the graphene is obtained, and after spark plasma sintering, a compact graphene reinforced TC4 titanium-based composite material can be obtained, and the graphene obtained by the in situ self-generation method is tightly combined with a matrix phase interface, so that the strength of the material is improved, and meanwhile, the high plasticity is maintained.
In order to better understand the scheme, the following describes the preparation method of the graphene reinforced TC4 titanium-based composite material in detail with reference to fig. 1, and the specific steps are as follows:
and step 1, performing low-temperature high-energy ball milling on the TC4 titanium alloy powder to obtain nano-scale TC4 titanium alloy powder.
The high-energy ball milling method is to mechanically mix the powder of different materials according to a certain proportion, and the powder is subject to collision, impact, shearing and extrusion under the repeated collision of grinding ball medium, and is continuously deformed, broken and welded, so that the powder is fully uniform and refined by long-time grinding with high strength, and finally the powder is the composite powder with the reinforcement dispersed.
Preferably, the low-temperature high-energy ball milling is carried out on the TC4 titanium alloy powder to obtain nano-scale TC4 titanium alloy powder, which comprises the following steps: and performing low-temperature ball milling on the TC4 titanium alloy powder by adopting a high-energy ball milling method in a low-temperature environment to obtain the nano-grade TC4 titanium alloy powder. Wherein the nano-scale TC4 titanium alloy powder is TC4 titanium alloy powder with granularity distribution of 60-90nm, and the low-temperature ball milling time is 40-60min.
This step can be understood in particular as: placing the purchased TC4 titanium alloy spherical powder (powder with other shapes can also be used) with the granularity of 200-300 mu m into an alumina ceramic ball milling pot in a vacuum glove box; and (3) taking out, and performing low-temperature ball milling for 40-60min by using a low-temperature splay vibration high-energy ball mill to obtain nano TC4 titanium alloy powder with the particle size distribution of 60-90 nm. The low-temperature environment can reduce the activity of the titanium alloy on one hand and avoid the reaction between the titanium alloy and the ball milling tank to the greatest extent; on the other hand, the brittleness of the titanium alloy can be increased, and the size of the powder is conveniently refined.
And 2, adopting a chemical vapor deposition method to generate graphene in situ on the surface of the nano-scale TC4 titanium alloy powder to obtain the TC4 titanium alloy powder coated by the graphene.
Chemical vapor deposition (Chemical VaporDeposition, CVD) is a Chemical technology that mainly uses one or more vapor compounds or simple substances containing thin film elements to perform Chemical reaction on the surface of a substrate to form a thin film. Chemical vapor deposition technology is a process that uses gaseous materials to produce chemical reactions, transport reactions, etc. on solids and produce solid deposits, and generally comprises three steps: (1) forming a volatile material; (2) transferring said substance to a deposition area; (3) Chemical reactions occur on the solids and produce solid materials. The most basic chemical vapor deposition reactions include thermal decomposition reactions, chemical synthesis reactions, and chemical transport reactions.
This step can be understood in particular as: placing the obtained nano-grade TC4 titanium alloy powder at a constant temperature of a CVD tube furnace, vacuumizing and exhausting residual air in the tube, respectively introducing high-purity argon and hydrogen at the flow rates of 280-320sccm and 80-120sccm, heating the tube furnace to 650-750 ℃ under the atmosphere, preserving heat for 20-30min, introducing methane gas (the flow rate is controlled at 2030 sccm), maintaining the state for 15-20min, closing a hydrogen gas inlet valve and a methane inlet valve, closing an argon gas inlet valve after the sample is cooled to room temperature, opening the furnace door, and taking out the sample (graphene coated TC4 titanium alloy powder).
And step 3, treating the TC4 titanium alloy powder coated by the graphene by adopting a spark plasma sintering method to obtain the graphene reinforced TC4 titanium-based composite material.
Discharge plasma sintering: the spark plasma sintering is a new powder metallurgy sintering technology for preparing high-performance materials by filling metal powder into a mold made of graphite and the like, applying specific sintering power and pressing pressure to the sintered powder by using an upper die punch, a lower die punch and a power-on electrode, and performing spark activation, thermoplastic deformation and cooling.
This step can be understood in particular as: placing the graphene-coated TC4 titanium alloy powder obtained in the above step into a graphite mold with the outer diameter of 300mm and the inner diameter of 30mm, and sintering for 2min at 950-1050 ℃ and 80-100 MPa by adopting a discharge plasma sintering furnace, thereby preparing the compact graphene-reinforced TC4 titanium-based composite material.
And 4, performing hot extrusion on the graphene reinforced TC4 titanium-based composite material to obtain a target bar.
The method comprises the following steps: and hot extruding the obtained block material (the compact graphene reinforced TC4 titanium-based composite material) into bars with the diameter of 13mm at the temperature of 860-900 ℃.
Examples and comparative examples are also provided for better explanation of the present scheme.
Example 1:
step 1, ball milling at low temperature and high energy: placing the purchased TC4 titanium alloy spherical powder with the granularity of 200-300 mu m into an alumina ceramic ball milling tank in a vacuum glove box; and (3) taking out, and performing low-temperature ball milling for 40-60min by using a low-temperature splay vibration high-energy ball mill to obtain nano TC4 titanium alloy powder with the particle size distribution of 60-90 nm.
Step 2, chemical vapor deposition: placing the nano TC4 titanium alloy powder prepared in the step 1 at a constant temperature of a CVD tube furnace, vacuumizing and exhausting residual air in the tube, respectively introducing high-purity argon and hydrogen at the flow rates of 280-320sccm and 80-120sccm, heating the tube furnace to 650-750 ℃ under the atmosphere, preserving heat for 20-30min, and introducing methane gas, wherein the flow rate is controlled at 20-30sccm. And maintaining the state for 15-20min, closing the hydrogen gas inlet valve and the methane inlet valve, closing the argon gas inlet valve after the sample is cooled to room temperature, opening the furnace door, and taking out the sample (the TC4 titanium alloy powder coated by graphene).
Step 3, spark plasma sintering: placing the powder obtained in the step 2 into a graphite die with the outer diameter of 300mm and the inner diameter of 30mm, adopting a discharge plasma sintering furnace, and sintering for 2min at 950-1050 ℃ and under the pressure of 80-100 MPa, thereby preparing the compact graphene reinforced TC4 titanium-based composite material.
Step 4, hot extrusion: and (3) hot extruding the block material obtained in the step (3) into bars with the diameter of 13mm at the temperature of 860-900 ℃.
Comparative example 1:
this embodiment differs from example 1 in that step 2 is omitted and the graphene-free bulk material is prepared otherwise as in embodiment 1.
Comparative example 2:
the difference between the embodiment and the embodiment 1 is that in the step 2, a ball milling powder mixing mode is adopted, purchased graphene powder, the nano TC4 titanium alloy powder obtained in the step 1 and retrograde mixing are adopted, the mass ratio of added graphene is 0.3-0.5wt%, the ball milling time of mixed powder is 3min, and the graphene-free bulk material is prepared.
The bars prepared in the above examples and comparative examples were subjected to performance tests, and the results are shown in table 1. From the table, the tensile strength and the elongation of the graphene reinforced TC4 titanium-based composite material finally prepared by the method can reach 1650-1663MPa and 8.7-9.3 percent respectively.
TABLE 1 room temperature tensile Properties of TC4 Bar
Finally, it should be noted that: the foregoing description is only illustrative of the preferred embodiments of the present invention, and although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described, or equivalents may be substituted for elements thereof, and any modifications, equivalents, improvements or changes may be made without departing from the spirit and principles of the present invention.
Claims (10)
1. The preparation method of the graphene reinforced TC4 titanium-based composite material is characterized by comprising the following steps of:
performing low-temperature high-energy ball milling on the TC4 titanium alloy powder to obtain nano-scale TC4 titanium alloy powder;
adopting a chemical vapor deposition method to generate graphene in situ on the surface of the nano-scale TC4 titanium alloy powder to obtain graphene-coated TC4 titanium alloy powder;
and treating the TC4 titanium alloy powder coated by the graphene by adopting a spark plasma sintering method to obtain the graphene reinforced TC4 titanium-based composite material.
2. The preparation method of the graphene reinforced TC4 titanium-based composite material according to claim 1, wherein the preparation method comprises the steps of performing low-temperature high-energy ball milling on TC4 titanium alloy powder to obtain nano-scale TC4 titanium alloy powder, and comprises the following steps: and performing low-temperature ball milling on the TC4 titanium alloy powder by adopting a high-energy ball milling method in a low-temperature environment to obtain the nano-grade TC4 titanium alloy powder.
3. The preparation method of the graphene reinforced TC4 titanium-based composite material according to claim 2, wherein the nano-scale TC4 titanium alloy powder is TC4 titanium alloy powder with particle size distribution of 60-90nm, and the low-temperature ball milling time is 40-60min.
4. The method for preparing the graphene-reinforced TC4 titanium-based composite material according to claim 1, wherein graphene is generated on the surface of the nano-scale TC4 titanium alloy powder in situ by chemical vapor deposition, and the method for preparing the graphene-coated TC4 titanium alloy powder comprises the steps of:
placing the nano-scale TC4 titanium alloy powder into a constant temperature part of a CVD tube furnace;
after vacuumizing and removing residual air in the tube, heating the CVD tube furnace to a preset temperature in an argon and hydrogen atmosphere, and preserving heat;
and after the heat preservation is finished, introducing methane gas and maintaining for 15-20min to obtain the TC4 titanium alloy powder coated by the graphene.
5. The method for preparing the graphene-reinforced TC4 titanium-based composite material of claim 4, wherein the flow rates of said argon gas, said hydrogen gas and said methane are 280-320sccm, 80-120sccm and 20-30sccm, respectively.
6. The preparation method of the graphene reinforced TC4 titanium-based composite material according to claim 4, wherein the preset temperature is 650-750 ℃, and the heat preservation time is 20-30min.
7. The method for preparing the graphene-reinforced TC4 titanium-based composite material according to claim 1, wherein the graphene-coated TC4 titanium alloy powder is treated by a spark plasma sintering method to obtain the graphene-reinforced TC4 titanium-based composite material, comprising:
placing the graphene-coated TC4 titanium alloy powder into a graphite mold;
and sintering the graphene-coated TC4 titanium alloy powder in the graphite mold by adopting a discharge plasma sintering furnace to obtain the graphene-reinforced TC4 titanium-based composite material.
8. The method for preparing a graphene-reinforced TC4 titanium-based composite material of claim 7, wherein said sintering conditions include: sintering at 950-1050 deg.c and 80-100 MPa for 2min.
9. The method of preparing a graphene reinforced TC4 titanium-based composite material of claim 1, further comprising: and performing hot extrusion on the graphene reinforced TC4 titanium-based composite material to obtain a target bar.
10. The method for preparing a graphene-reinforced TC4 titanium-based composite material of claim 9, wherein hot extrusion is performed at 860-900 ℃.
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| CN118268561A (en) * | 2024-04-17 | 2024-07-02 | 开禾科技(宁波)有限公司 | Titanium alloy powder for additive manufacturing and preparation method thereof |
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