Graphene / TA1 composite material and preparation method thereof

Abstract

The application discloses a graphene / TA1 composite material and a preparation method thereof, and belongs to the technical field of graphene / titanium-based composite material preparation. In order to solve the problem of the rolled high-strength plastic graphene / TA1 composite material in a high-load service environment, Sn powder, Y2O3 powder and TA1 titanium alloy powder are uniformly mixed, then the mixture is added into a ball mill tank, graphene powder is added in batches, and multiple ball milling is carried out to obtain a composite powder; a mold filled with the composite powder is placed in a sintering furnace, an axial pressure is applied to the mold, and plasma sintering treatment is carried out to obtain a sintered composite material blank; the sintered composite material blank is subjected to oxidation scale removal and round billet cutting treatment, and then is subjected to sandpaper polishing to obtain a hot rolling initial sample; and multiple pass rolling is carried out until the total reduction is 75%, and then air cooling is carried out to room temperature to obtain the graphene / TA1 composite material. The application improves the overall properties of the high-strength plastic graphene / TA1 composite material.

Description

Technical Field

[0001] This invention belongs to the field of graphene / titanium-based composite material preparation technology, specifically relating to a graphene / TA1 composite material and its preparation method. Background Technology

[0002] Titanium and titanium alloys are widely used in aerospace, chemical, power, and biomedical fields due to their high specific strength, good corrosion resistance, and excellent biocompatibility. TA1, a typical industrial pure titanium, possesses good plasticity and toughness, but its yield strength and tensile strength are relatively low, making it difficult to meet the requirements of lightweight and safety redundancy for high-specific-strength, high-reliability service components. Therefore, how to significantly improve the strength of TA1 while maintaining a certain level of plasticity has always been a key focus in the field of titanium-based structural materials.

[0003] Graphene is a novel carbon material with a two-dimensional honeycomb crystal structure, possessing extremely high elastic modulus and tensile strength, as well as excellent thermal and electrical conductivity. Introducing graphene as a reinforcing phase into a titanium matrix is ​​expected to improve the material's strength and stiffness without significantly increasing density. Existing technologies have reported the preparation of graphene / titanium-based composites using powder metallurgy, ball milling, spark plasma sintering, hot pressing, and subsequent hot deformation processes. However, existing graphene / titanium-based composites generally suffer from the following problems: First, graphene is prone to agglomeration and breakage during ball milling and sintering, making it difficult to achieve a stable and uniform dispersion, thus causing localized stress concentration. Second, during high-temperature sintering or hot deformation, graphene readily reacts with titanium to form a brittle TiC phase and a coarse interfacial reaction layer. While this is beneficial for improving strength, it is often accompanied by a significant decrease in elongation, exhibiting the characteristics of "high strength, low plasticity." Third, some preparation processes are complex, requiring strict control over temperature, atmosphere, and equipment conditions, resulting in insufficient density and microstructure uniformity, which limits engineering applications.

[0004] To improve the overall mechanical properties of titanium-based composites, existing technologies propose introducing trace elements such as Sn and Y into the titanium matrix through microalloying. Sn, as an element with a certain solid solution capability in titanium, can improve matrix strength and regulate plasticity through solid solution strengthening and influencing phase transformation behavior. Rare earth element Y and its oxide dispersed phases help purify grain boundaries, refine grains, and stabilize the second phase, thereby improving the microstructure and mechanical properties of the material. Existing research shows that appropriate Sn / Y microalloying design can alleviate the plasticity reduction problem caused by graphene to a certain extent, achieving a better strength-elongation match. For example, existing technologies have proposed a Sn / Y synergistic microalloyed graphene / TA1 composite material. Through compositional control and powder metallurgy processes, it significantly improves the fracture elongation at a moderately high strength level, resulting in a significant increase in tensile strength, yield strength, and elongation compared to pure TA1. This belongs to a graphene / TA1 composite material system that emphasizes "high elongation."

[0005] However, with the increasing demands on material performance from high-end equipment and high-load components, simply improving elongation at a moderate strength level is no longer sufficient. Existing Sn / Y synergistic microalloyed graphene / TA1 composites still exhibit limited strength in the sintered or slightly deformed state, particularly in yield strength, which is difficult to achieve the levels required for high-strength structural components. Furthermore, how to stably control the microstructure evolution of the graphene / TA1 composite system under conditions of significant plastic deformation (such as hot rolling), while considering densification, grain refinement, second-phase size and distribution, and interfacial reaction layer thickness, and avoiding a significant decrease in elongation while increasing strength, remains a key unresolved issue in current technology. Summary of the Invention

[0006] The problem to be solved by this invention is to obtain a rolled high-strength and high-plasticity graphene / TA1 composite material suitable for high-load service environments, and to propose a graphene / TA1 composite material and its preparation method.

[0007] To achieve the above objectives, the present invention provides the following technical solution:

[0008] A method for preparing a graphene / TA1 composite material includes the following steps:

[0009] S1. Weigh out a certain mass of graphene powder, Sn powder, Y2O3 powder, and TA1 titanium alloy powder according to the weight proportions, and set aside for later use;

[0010] S2. After mixing the Sn powder, Y2O3 powder and TA1 titanium alloy powder obtained in step S1 evenly, add them to a ball mill jar, and then add graphene powder in batches. Perform ball milling multiple times to obtain composite powder for later use.

[0011] S3. Place the mold filled with the composite powder obtained in step S2 into a sintering furnace, apply an axial pressure of 40~45MPa to the mold, and then perform plasma sintering treatment to obtain the sintered composite material preform.

[0012] S4. The sintered composite material preform obtained in step S3 is subjected to oxide scale removal and round blanking using a wire EDM device, and then sanded to obtain the initial hot-rolled sample.

[0013] S5. The initial hot-rolled sample obtained in step S4 is placed in a muffle furnace and heated for multiple passes. The rolling speed is 10 m / min, and the sample is reduced by 1 mm in each pass. After each pass, the sample is placed in the muffle furnace and held for 1.5 to 2 minutes. After the reduction reaches 5 mm, the sample is reduced by 0.5 mm in each pass. After each reduction, the sample is placed in the muffle furnace and held for 1 to 2 minutes until the total reduction is 75%. Then, the sample is air-cooled to room temperature to obtain a graphene / TA1 composite material.

[0014] Furthermore, in step S1, the weight parts of TA1 powder are 118.895~118.900 parts, the weight parts of graphene powder are 0.36~0.362 parts, the weight parts of Sn powder are 0.516~0.520 parts, and the weight parts of Y2O3 powder are 0.229~0.232 parts.

[0015] Furthermore, in step S1, the particle size range of TA1 powder is 45~75μm, the particle size range of graphene powder is 20~40μm, the particle size range of Sn powder is 50~100nm, and the particle size range of Y2O3 powder is 50~100nm.

[0016] Furthermore, in step S2, the ball-to-material ratio in the ball mill jar is 5~6:1. The ball mill jar is placed on the ball mill, the main disc speed is set to 200~220 rpm / min, the ball milling time for each batch is 1~1.2h, and graphene powder is added before the ball milling of the 2nd to 5th batches. The mass ratio of the added graphene powder is 1:1:1:0.6, and the total ball milling time is 6~7h.

[0017] Furthermore, in step S3, the plasma sintering treatment is carried out under a vacuum degree of less than 1.0 × 10⁻³ Pa. The mold filled with composite powder is placed in the sintering furnace, and an axial pressure of 40 MPa is applied to the mold. This pressure is maintained constant during the subsequent heating and holding stages. The temperature is increased from room temperature to 700~750℃ at a heating rate of 50℃ / min. Then, the heating rate is adjusted to 100℃ / min, and the temperature is increased to 1000~1200℃ and held at this temperature for 5~6 min. After the holding period, the temperature is reduced to 600~650℃ at a cooling rate of 50℃ / min. Then, the heating power is turned off, and the sample is cooled to room temperature by furnace cooling.

[0018] Furthermore, in step S4, the thickness of the cut round blank is 8 to 10 mm, and it is polished with 80 to 2000# sandpaper until the wire cutting marks are eliminated and the surface is smooth.

[0019] Furthermore, in step S5, the temperature of the muffle furnace for heating is 900~920℃, and the holding time is 20~30min. The holding temperature of the muffle furnace is 900~920℃.

[0020] A method for preparing a graphene / TA1 composite material: The graphene / TA1 composite material is prepared in which Sn element is distributed in a solid solution state in the TA1 matrix, and Y2O3 particles are mainly distributed at the graphene / titanium matrix interface.

[0021] The beneficial effects of this invention are:

[0022] The present invention discloses a method for preparing a graphene / TA1 composite material, which regulates the graphene / Ti matrix and interface by adding different amounts of two alloying elements, Y and Sn, and strengthens the grid structure by changing the distribution of the second phase at the interface, thereby improving the overall properties of a high-strength and ductile graphene / TA1 composite material.

[0023] The specific technical effects of this invention are as follows:

[0024] (1) This invention achieves a synergistic improvement in strength and elongation by using reasonable component ratios and ball milling, sintering and rolling processes, providing a new approach for the research of graphene-reinforced titanium-based composite materials;

[0025] (2) The material prepared by this invention has a tensile strength of 631 MPa, a yield strength of 473 MPa, and an elongation at break of 37.7%;

[0026] (3) Compared with the graphene / TA1 composite material, the material prepared by this invention has an elongation increased by 63% and a tensile strength increased by 5.9%.

[0027] (4) The preparation method of the graphene / TA1 composite material described in this invention is simple and easy to operate, has high preparation efficiency, saves energy, and is environmentally friendly in the preparation process, without generating any toxic or harmful substances, and can be used for industrial production. Attached Figure Description

[0028] Figure 1 This is a metallographic image of the RD-TD plane of a graphene / TA1 composite material according to the present invention;

[0029] Figure 2 This is a SEM image of the RD–ND surface of a graphene / TA1 composite material described in this invention;

[0030] Figure 3 This is a schematic diagram of the room temperature tensile specimen used in the experiment of this invention. Detailed Implementation

[0031] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to the accompanying drawings and specific embodiments. It should be understood that the specific embodiments described herein are only for explaining the invention and are not intended to limit the invention; that is, the described specific embodiments are merely a part of the embodiments of the invention, and not all of them. The components of the specific embodiments of the invention described and shown in the accompanying drawings can generally be arranged and designed in various different configurations, and the invention may also have other embodiments.

[0032] Therefore, the following detailed description of specific embodiments of the invention provided in the accompanying drawings is not intended to limit the scope of the claimed invention, but merely to illustrate selected specific embodiments of the invention. All other specific embodiments obtained by those skilled in the art based on these specific embodiments without inventive effort are within the scope of protection of this invention.

[0033] To further understand the invention's content, features, and effects, the following specific embodiments are provided, along with accompanying drawings. Figure 1 - Appendix Figure 3 Detailed explanation is as follows:

[0034] Example 1:

[0035] A method for preparing a graphene / TA1 composite material includes the following steps:

[0036] S1. Weigh out a certain mass of graphene powder, Sn powder, Y2O3 powder, and TA1 titanium alloy powder according to the weight proportions, and set aside for later use;

[0037] Furthermore, in step S1, the weight percentages of TA1 powder are 118.895 parts, graphene powder is 0.36 parts, Sn powder is 0.516 parts, and Y2O3 powder is 0.229 parts.

[0038] Furthermore, in step S1, the particle size range of TA1 powder is 45~75μm, the particle size range of graphene powder is 20~40μm, the particle size range of Sn powder is 50~100nm, and the particle size range of Y2O3 powder is 50~100nm.

[0039] Furthermore, the chemical composition of the purchased TA1 was analyzed by X-ray diffraction, and the results are shown in Table 1.

[0040] Table 1

[0041]

[0042] Furthermore, the graphene is redox graphene;

[0043] S2. After mixing the Sn powder, Y2O3 powder and TA1 titanium alloy powder obtained in step S1 evenly, add them to a ball mill jar, and then add graphene powder in batches. Perform ball milling multiple times to obtain composite powder for later use.

[0044] Furthermore, in step S2, the ball-to-material ratio in the ball mill jar is 5:1. The ball mill jar is placed on the ball mill, the main disc speed is set to 200 rpm / min, the ball milling time for each batch is 1 hour, and graphene powder is added before the ball milling of the 2nd to 5th batches. The mass ratio of the added graphene powder is 1:1:1:0.6, and the total ball milling time is 6 hours.

[0045] S3. Place the mold filled with the composite powder obtained in step S2 into a sintering furnace, apply an axial pressure of 40 MPa to the mold, and then perform plasma sintering treatment to obtain the sintered composite material preform.

[0046] Furthermore, in step S3, the plasma sintering treatment is performed with a vacuum degree of less than 1.0 × 10⁻⁶. -³ Under the condition of Pa, the mold filled with composite powder was placed in the sintering furnace, and an axial pressure of 40 MPa was applied to the mold. This pressure was kept constant during the subsequent heating and holding stages. The temperature was increased from room temperature to 700°C at a heating rate of 50°C / min. Then the heating rate was adjusted to 100°C / min, and the temperature was increased to 1000°C and held at this temperature for 5 min. After the holding period, the temperature was reduced to 600°C at a cooling rate of 50°C / min. Then the heating power was turned off, and the sample was cooled to room temperature by furnace cooling.

[0047] S4. The sintered composite material preform obtained in step S3 is subjected to oxide scale removal and round blanking using a wire EDM device, and then sanded to obtain the initial hot-rolled sample.

[0048] Furthermore, in step S4, the thickness of the cut round blank is 8 to 10 mm, and it is polished with 80 to 2000# sandpaper until the wire cutting marks are eliminated and the surface is smooth.

[0049] S5. The initial hot-rolled sample obtained in step S4 is placed in a muffle furnace and heated for multiple passes. The rolling speed is 10 m / min, and the sample is reduced by 1 mm in each pass. After each pass, the sample is placed in the muffle furnace and held for 1.5 min. After the reduction is 5 mm, the sample is reduced by 0.5 mm in each pass. After each reduction, the sample is placed in the muffle furnace and held for 1 min until the total reduction is 75%. Then, the sample is air-cooled to room temperature to obtain a graphene / TA1 composite material.

[0050] Furthermore, in step S5, the temperature of the muffle furnace for heating is 900~920℃, and the holding time is 20~30min. The holding temperature of the muffle furnace is 900~920℃.

[0051] The graphene / TA1 composite material prepared by the method described in this embodiment is a graphene / TA1 composite material in which Sn element is distributed in a solid solution state in the TA1 matrix, and Y2O3 particles are mainly distributed at the graphene / titanium matrix interface.

[0052] Furthermore, the graphene / TA1 composite material is composed of the following components by mass percentage: 0.25~0.35%, Sn 0.4~0.5%, Y 0.10~0.20%, with the remainder being Ti and other unavoidable impurity elements.

[0053] Comparative Example 1

[0054] The specific method for preparing a pure TA1 alloy material as a comparative example is as follows:

[0055] S1. Clean the grinding jar made of hardened chromium steel and the steel grinding balls with clean water and a brush, let them dry, then clean them three times with anhydrous ethanol, and then blow them dry.

[0056] The chemical composition of the commercial TA1 powder used in Comparative Example 1 is consistent with the X-ray diffraction analysis results in Example 1.

[0057] According to the composition of TA1 shown in Table 1 of Example 1, the raw materials were weighed using an analytical balance at a ball-to-powder ratio of 5:1: 600g of steel grinding balls and 120g of commercial TA1 powder were added to a ball mill jar. The jar was then placed on a ball mill, and the main disc speed was set to 200 rpm / min for 6 hours. After mixing and ball milling, the composite powder was obtained.

[0058] S2. The obtained composite powder is subjected to plasma sintering. The sintering process parameters are set as follows: vacuum degree less than 1.0 × 10⁻⁶. -³Under the condition of Pa, the mold filled with composite powder was placed in the sintering furnace, and an axial pressure of 40 MPa was applied to the mold. This pressure was kept constant during the subsequent heating and holding stages. The temperature was increased from room temperature to 700 ℃ at a heating rate of 50 ℃ / min. Then the heating rate was adjusted to 100 ℃ / min, and the temperature was increased to 1000 ℃ and held at this temperature for 5 min to complete the densification and microstructure stabilization treatment of the composite material. After the holding period, the temperature was reduced to 600 ℃ at a cooling rate of 50 ℃ / min. Then the heating power was turned off, and the sample was cooled to room temperature by furnace cooling.

[0059] S3. Using a wire EDM machine, take an 8 mm thick round billet from the sintered billet as the initial sample for hot rolling. Grind the billet with 80#-2000# sandpaper until the wire EDM marks are eliminated and the surface is smooth. Place it in a muffle furnace and heat to 900℃, holding for 20 min. Then perform multi-pass rolling at a rolling speed of 10 m / min, with a reduction of 1 mm per pass. After reducing to 5 mm, reduce by 0.5 mm per pass, then 1 mm per pass, and so on, until reaching 5 mm. After each pass, temper in a muffle furnace for 1.5 min. After each reduction of 5 mm, hold for 1 min after each reduction. The total reduction is 75%. Then air cool to room temperature. A pure TA1 alloy material is obtained after cooling to ambient temperature.

[0060] Comparative Example 2

[0061] The specific implementation method for preparing a graphene / TA1 composite material as a comparative example is as follows:

[0062] S1. Clean the grinding jar made of hardened chromium steel and the steel grinding balls with clean water and a brush, let them dry, then clean them three times with anhydrous ethanol, and then blow them dry.

[0063] The chemical composition of the commercial TA1 powder used in Comparative Example 1 is consistent with the X-ray diffraction analysis results in Example 1.

[0064] According to the composition of TA1 shown in Table 1 of Example 1, the raw materials were weighed using an analytical balance at a ball-to-powder ratio of 5:1: 600g of steel grinding balls, 119.64g of commercial TA1 powder, and 0.36g of graphene. The graphene was divided into four batches (0.1g, 0.1g, 0.1g, and 0.6g), and then mixed with the TA1 powder in sequence and poured into a ball mill jar. The ball mill jar was placed on a ball mill, and the main disc speed was set to 200 rpm / min. The ball milling time for each batch was 1 hour, and the total ball milling time was 6 hours. After the mixing and ball milling was completed, the composite powder was obtained.

[0065] S2. The obtained composite powder is subjected to plasma sintering. The sintering process parameters are set as follows: vacuum degree less than 1.0 × 10⁻⁶. -³ Under the condition of Pa, a mold filled with composite powder was placed in a sintering furnace, and an axial pressure of 40 MPa was applied to the mold, which was maintained constant during the subsequent heating and holding stages. The temperature was increased from room temperature to 700 °C at a heating rate of 50 °C / min, then the heating rate was adjusted to 100 °C / min, and the temperature was increased to 1000 °C and held at this temperature for 5 min to complete the densification and microstructure stabilization treatment of the composite material. After the holding period, the temperature was reduced to 600 °C at a cooling rate of 50 °C / min, and then the heating power was turned off. The sample was cooled to room temperature using a furnace cooling method.

[0066] S3. Using a wire EDM machine, an 8 mm thick circular billet was taken from the sintered billet as the initial sample for hot rolling. The billet was polished with 80#-2000# sandpaper until the wire EDM marks were eliminated and the surface was smooth. It was then placed in a muffle furnace and heated to 900℃ and held for 20 min before being rolled in multiple passes at a rolling speed of 10 m / min. Each pass reduced the thickness by 1 mm. After reducing the thickness to 5 mm, each pass reduced the thickness by 0.5 mm. After each pass, the billet was placed in a muffle furnace for tempering for 1.5 min. After each reduction of 5 mm, the thickness was reduced by 1 min and held for 1 min. The total reduction was 75%. The billet was then air-cooled to room temperature. The result was a graphene / TA1 composite material.

[0067] The following experiments were conducted on Example 1 and the comparative example:

[0068] The microstructure of a high-strength graphene / TA1 composite material obtained in Example 1 was observed using the following method:

[0069] A. A high-strength graphene / TA1 composite material obtained in Example 1 was wire-cut using wire cutting technology to obtain a sample block with a size of 5mm×5mm×5mm. The surface of the sample block was successively ground with 120#, 240#, and 600# sandpaper until there were no obvious scratches on the surface. Then, it was carefully polished on a polishing machine. Water was continuously injected while the polishing machine was rotating until the surface of the sample block reached a scratch-free and bright state.

[0070] B. Immerse the sample block for 3 seconds using an etching solution composed of 7 mL H₂O + 1 mL HF + 2 mL HNO₃. Then observe the sample block using a scanning electron microscope (SEM). The SEM backscattered image of a high-strength graphene / TA1 composite material is shown below. Figure 1 As shown.

[0071] Depend on Figure 1As can be seen, the microstructure of the graphene / TA1 composite material in Example 1 is characterized by the generation of discontinuously distributed TiC particles during the interfacial reaction process. These TiC particles are interconnected with Y2O3 particles to form a continuous network structure.

[0072] Mechanical properties were tested on the high-strength graphene / TA1 composite material prepared in Example 1, the pure TA1 alloy material prepared in Comparative Example 1, and the graphene / TA1 composite material prepared in Comparative Example 2. The methods are as follows:

[0073] Tensile tests were performed on the high-strength graphene / TA1 composite material prepared in Example 1, the pure TA1 alloy material prepared in Comparative Example 1, and the graphene / TA1 composite material prepared in Comparative Example 2 using an electronic universal testing machine (MTS810). To eliminate wire cutting and improve the accuracy and stability of tensile properties, sandpaper of different grit sizes was used, progressing from 240# to 2000#, to ensure that the surface roughness of each sample was basically the same. The sample dimensions are as follows. Figure 3 The test temperature was room temperature, the maximum load on the equipment was 100 kN, the tensile rate was 1 mm / min, and an extensometer was used throughout the room temperature tensile process. To maintain the accuracy of the tensile properties, three sets of parallel specimens were tested, and the average value was taken as the final strength and elongation values ​​as the final results. The test results are shown in Table 2.

[0074] Table 2

[0075]

[0076] As can be seen from Table 2, the high-strength graphene / TA1 composite material prepared by this invention exhibits significant advantages in several aspects: compared with pure TA1, the yield strength is increased by 62%, the tensile strength is increased by 44%, and the elongation is increased by 6%; compared with the graphene / TA1 composite material, the yield strength is increased by 32%, the tensile strength is increased by 26%, and the elongation is only reduced by 8%.

[0077] Therefore, the high-strength graphene / TA1 composite material prepared by this invention has a tensile strength of 854 MPa, a yield strength of 744 MPa, and an elongation at break of 27.2%. Compared with pure TA1, the yield strength is increased by 62%, the tensile strength is increased by 44%, and the elongation is increased by 6%. Compared with graphene / TA1 composite material, the yield strength is increased by 32%, the tensile strength is increased by 26%, and the elongation is only reduced by 8%. This invention, through reasonable microalloying composition control, ball milling, and sintering settings, enables the prepared high-strength graphene / TA1 composite material to achieve excellent comprehensive properties. The preparation method is simple, easy to operate, and environmentally friendly, generating no toxic or harmful substances.

[0078] It should be noted that relational terms such as "first" and "second" are used merely to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process, method, article, or apparatus. Without further limitations, an element defined by the phrase "comprising one..." does not exclude the presence of other identical elements in the process, method, article, or apparatus that includes said element.

[0079] Although this application has been described above with reference to specific embodiments, various modifications can be made and components can be replaced with equivalents without departing from the scope of this application. In particular, as long as there is no structural conflict, the features in the specific embodiments disclosed in this application can be combined with each other in any way. The lack of an exhaustive description of these combinations in this specification is merely for the sake of brevity and resource conservation. Therefore, this application is not limited to the specific embodiments disclosed herein, but includes all technical solutions falling within the scope of the claims.

Claims

1. A method for preparing a graphene / TA1 composite material, characterized in that, Includes the following steps: S1. Weigh out a certain mass of graphene powder, Sn powder, Y2O3 powder, and TA1 titanium alloy powder according to the weight proportions, and set aside for later use; S2. After mixing the Sn powder, Y2O3 powder and TA1 titanium alloy powder obtained in step S1 evenly, add them to a ball mill jar, and then add graphene powder in batches. Perform ball milling multiple times to obtain composite powder for later use. S3. Place the mold filled with the composite powder obtained in step S2 into a sintering furnace, apply an axial pressure of 40~45MPa to the mold, and then perform plasma sintering treatment to obtain the sintered composite material preform. S4. The sintered composite material preform obtained in step S3 is subjected to oxide scale removal and round blanking using a wire EDM device, and then sanded to obtain the initial hot-rolled sample. S5. The initial hot-rolled sample obtained in step S4 is placed in a muffle furnace and heated for multiple passes. The rolling speed is 10 m / min, and the sample is reduced by 1 mm in each pass. After each pass, the sample is placed in the muffle furnace and held for 1.5 to 2 minutes. After the reduction reaches 5 mm, the sample is reduced by 0.5 mm in each pass. After each reduction, the sample is placed in the muffle furnace and held for 1 to 2 minutes until the total reduction is 75%. Then, the sample is air-cooled to room temperature to obtain a graphene / TA1 composite material.

2. The method for preparing a graphene / TA1 composite material according to claim 1, characterized in that, In step S1, the weight parts of TA1 powder are 118.895~118.900, the weight parts of graphene powder are 0.36~0.362, the weight parts of Sn powder are 0.516~0.520, and the weight parts of Y2O3 powder are 0.229~0.

232.

3. The method for preparing a graphene / TA1 composite material according to claim 2, characterized in that, In step S1, the particle size range of TA1 powder is 45~75μm, the particle size range of graphene powder is 20~40μm, the particle size range of Sn powder is 50~100nm, and the particle size range of Y2O3 powder is 50~100nm.

4. The method for preparing a graphene / TA1 composite material according to claim 3, characterized in that, In step S2, the ball-to-material ratio in the grinding jar is 5~6:

1. The grinding jar is placed on the ball mill, and the main disc speed is set to 200~220 rpm / min. The grinding time for each batch is 1~1.2h. Graphene powder is added before the grinding of the 2nd to 5th batches. The mass ratio of the added graphene powder is 1:1:1:0.

6. The total grinding time is 6~7h.

5. The method for preparing a graphene / TA1 composite material according to claim 4, characterized in that, In step S3, the plasma sintering treatment is performed with a vacuum degree of less than 1.0 × 10⁻⁶. -³ Under the condition of Pa, the mold filled with composite powder was placed in the sintering furnace, and an axial pressure of 40 MPa was applied to the mold. This pressure was kept constant during the subsequent heating and holding stages. The temperature was increased from room temperature to 700-750°C at a heating rate of 50°C / min. Then the heating rate was adjusted to 100°C / min, and the temperature was increased to 1000-1200°C and held at this temperature for 5-6 min. After the holding period, the temperature was decreased to 600-650°C at a cooling rate of 50°C / min. Then the heating power was turned off, and the sample was cooled to room temperature by furnace cooling.

6. The method for preparing a graphene / TA1 composite material according to claim 5, characterized in that, In step S4, the thickness of the cut round blank is 8-10mm. It is then polished with 80-2000# sandpaper until the wire cutting marks are eliminated and the surface is smooth.

7. The method for preparing a graphene / TA1 composite material according to claim 6, characterized in that, In step S5, the temperature of the muffle furnace for heating is 900~920℃, and the holding time is 20~30min. The holding temperature of the muffle furnace is 900~920℃.

8. A graphene / TA1 composite material prepared by a method according to any one of claims 1-7, characterized in that, Sn elements are distributed in a solid solution state in the TA1 matrix, while Y2O3 particles are mainly distributed at the graphene / titanium matrix interface.

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