MAX-phase two-position solid solution material and preparation method thereof
By using a specific composition of raw material powder to sinter at low temperature in the preparation of MAX phase double-position solid solution materials, the problems of high synthesis temperature and additional pressurization in the prior art are solved, and the preparation of pure MAX phase double-position solid solution materials are realized, which reduces the process difficulty and cost and promotes industrial application.
Patent Information
- Application Number
- CN202510217915.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-26
- Publication Date
- 2025-05-13
AI Technical Summary
The preparation of existing MAX phase double-position solid solution materials has the problem of high synthesis temperature and additional pressurization, which leads to increased production difficulty and limited industrial application.
The specific composition of Ti-Al alloy or V-Al alloy, M' elemental substance, M' carbide and/or M'-Al alloy, A' elemental substance and/or A' carbide, and a carbon source as raw material powder, were used to heat up to 800°C to 1250°C for reaction sintering to prepare a pure phase MAX phase biposition solid solution material without pressurization.
It reduces the difficulty of preparation, saves energy, reduces costs, facilitates mass production, and increases the type and processability of materials.
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Figure CN119977576A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the field of MAX phase material preparation, and particularly relates to a MAX phase binary solid solution material and a preparation method thereof. Background Art
[0002] Ternary MAX phase ceramic material is a ternary layered metal ceramic compound composed of early transition metal element M, main group element A (III or IV group element), and X (carbon or nitrogen or carbon nitrogen). It has excellent electrical conductivity, thermal conductivity, and seismic resistance of metal materials and high yield strength, melting point, stable thermal properties and oxidation resistance of ceramics. It has broad application prospects in aerospace, electromagnetic shielding, energy industry and other fields. The chemical formula of ternary MAX phase ceramic material is M n+1 AX n , where n = 1, 2 or 3. Depending on the value of n, the MAX phase can be divided into 211 phase, 312 phase and 413 phase. They have the same hexagonal crystal system. Among them, the 211 phase and the 312 phase have excellent chemical stability and mechanical properties and are the most widely studied and applied ternary ceramic materials. In order to further meet the demand for comprehensive performance in practical applications, researchers have added elements to the M, A or X positions for alloying treatment to form a MAX phase solid solution with lattice distortion to obtain better comprehensive performance.
[0003] For example, Zhou et al. (see YC Zhou et al., Strengthening of Ti3AlC2 by Incorporation of Si to Form Ti3Al 1-x Si x C2 Solid Solutions[J], Acta Materialia, 2006) used Ti, Al, Si and graphite powder as raw materials, and synthesized the product by in-situ hot pressing / solid-liquid reaction method and achieved densification. 1-x Si x C2 solid solution, the synthesis temperature is 1500℃, the reaction time is 60 minutes, and the final hot pressing pressure is 30MPa. 1-x Si x When C2 solid solution is greater than 0.25, a significant strengthening effect is observed. 0.75 Si 0.25The Vickers hardness, flexural strength and compressive strength of C2 solid solution increased by 26%, 12% and 29% respectively. Compared with single solid solution at M or A position, double solid solution at M and A position is more conducive to improving the comprehensive performance. Zheng et al. (see LYZheng et al, Strengthening of Ti3(Si,Al)C2 by Doping with Tungsten[J], Journal of the American Ceramic Society, 2012) adopted the in-situ hot pressing / solid-liquid reaction method, using titanium, tungsten, silicon, aluminum and graphite powder as raw materials to prepare Ti3(Si,Al)C2 bulk samples doped with W with W contents ranging from 0 to 7.5at.%. In all samples, about 5at.% of Si was replaced by Al to eliminate TiC impurities. The hot pressing temperature and time were 1600℃ and 0.5h, respectively, and the products were annealed at 30MPa pressure for 0.5h. Among them, the flexural strength of Ti3(Si,Al)C2 doped with 5at.% W was increased by 176% and 170% at room temperature and 1200℃. It can be seen that the dual-site solid solution of the M and A sites of the ternary MAX phase ceramic material can significantly improve the room temperature and high temperature mechanical properties of the material.
[0004] However, in the above-mentioned related technologies, the preparation of MAX phase binary solid solution materials has the defects of high synthesis temperature and the need for additional pressurization, which increases the difficulty of preparing MAX phase binary solid solution materials and limits their industrial application. Summary of the invention
[0005] The purpose of the present invention is to provide a MAX phase binary solid solution material and a preparation method, which can improve the defects of the MAX phase binary solid solution material in the related art, such as high synthesis temperature and need for additional pressurization, reduce the difficulty of preparation, and be conducive to promoting industrialization and application.
[0006] In a first aspect, the present invention provides a method for preparing a MAX phase binary solid solution material, comprising the following preparation steps:
[0007] S1. Raw material mixing: weighing raw material powders according to a ratio, and mixing the weighed raw material powders uniformly to obtain mixed powders; the raw material powders include M-Al alloy, simple substance M', carbide of M' and / or M'-Al alloy, simple substance A' and / or carbide of A', and a carbon source; the element M of the M-Al alloy is selected from Ti or V, the simple substance M', carbide of M' and / or element M' of the M'-Al alloy is independently selected from at least one of Ti, W, V, Ta and Cr, and at least one of the elements M' is different from the element M, and the simple substance A' and / or element A' of the carbide of A' is independently selected from at least one of Si, Sn and Ge;
[0008] S2. Sintering of the mixed powder: Place the mixed powder in a protective atmosphere or vacuum, heat it to 800 °C to 1250 °C for sintering to prepare a MAX-phase double-site solid solution material, and the molecular formula of the MAX-phase double-site solid solution material is expressed as (Ti 1-x M′ x )3(Al 1-y A′ y )C2 or (V 1-x M′ x )2(Al 1-y A′ y )C, where x and y are atomic ratios, 0 < x ≤ 0.5, 0 < y ≤ 0.5, and the MAX-phase double-site solid solution material is a pure-phase solid solution.
[0009] Optionally, in step S1, when the element M is Ti, the M-Al alloy is a Ti3Al alloy; when the element M is V, the M-Al alloy is selected from at least one of a V5Al alloy and a V5Al8 alloy.
[0010] Optionally, the carbon source is selected from at least one of graphite, carbon black, or glucose.
[0011] Optionally, in step S1, the particle sizes of the M-Al alloy, the elemental M′, the carbide of M′, the M′-Al alloy, the elemental A′, and the carbide of A′ are 0.6 to 15 μm.
[0012] Optionally, in step S1, the weighed raw material powders are mixed evenly by ball milling, the rotation speed of the ball milling is 50 to 250 r / min, the ball-to-material ratio is 12:1 to 25:1, and the ball milling time is 8 to 45 hours.
[0013] Optionally, in step S1, when the element M is Ti, the mass percentage of the total carbon mass in the carbide of M′, the carbide of A′, and the carbon source to the mass of the M-Al alloy is 10 to 16%; when the element M is V, the mass percentage of the total carbon mass in the carbide of M′, the carbide of A′, and the carbon source to the mass of the M-Al alloy is 9 to 10%.
[0014] Optionally, when the raw material powder in step S1 is Ti-Al alloy, M' simple substance, M' carbide and / or M'-Al alloy, A' carbide, and a carbon source, step S2 is heated to above 880°C for sintering to prepare the MAX phase binary solid solution material; when the raw material powder in step S1 is Ti-Al alloy, M' simple substance, M' carbide and / or M'-Al alloy, A' simple substance, and a carbon source, step S2 is heated to above 950°C for sintering to prepare the MAX phase binary solid solution material.
[0015] Optionally, when the raw material powder in step S1 is V-Al alloy, M′ element, M′ carbide and / or M′-Al alloy, A′ element and / or A′ carbide, and a carbon source, step S2 heats the temperature to 800-1000° C. for sintering to prepare the MAX phase binary solid solution material.
[0016] Optionally, in step S2, the particle size of the product powder of the prepared MAX phase binary solid solution material is 1 to 30 μm.
[0017] In a second aspect, the present invention provides a MAX phase binary solid solution material, comprising a product powder obtained by the preparation method of the MAX phase binary solid solution material described in any of the preceding items and at least one of a block, a film, a plate, a strip, a tube, and a rod prepared from the product powder.
[0018] In summary, the present invention has at least one of the following beneficial effects:
[0019] The present invention provides a method for preparing a MAX phase binary solid solution material, which uses a Ti-Al alloy or a V-Al alloy of a specific composition, a simple substance of M', a carbide of M' and / or an M'-Al alloy, a simple substance of A' and / or a carbide of A', and a carbon source as raw material powders, and heats the raw material powder to 800° C. to 1250° C. for reaction sintering to prepare a pure phase MAX phase binary solid solution material, the molecular formula of which is (Ti 1-x M′ x )3(Al 1-y A′ y )C2 or (V 1-x M′ x )2(Al 1-y A′ y)C, where x and y are atomic ratios, 0 < x ≤ 0.5, 0 < y ≤ 0.5. The sintering temperature is low and no additional pressure is required, which can save energy and reduce costs, thus being beneficial to mass production. In addition, it is also possible to flexibly control the solid solution amount of elements M′ and A′ within a wide range according to different performance requirements, and a pure-phase double-site solid solution material can be prepared, increasing the variety of MAX-phase double-site solid solution materials. At the same time, the prepared MAX-phase double-site solid solution product powder has strong processability and can be used to prepare any one of bulk materials, thin films, plates, strips, tubes, and rods. Description of the Drawings
[0020] Figure 1-1 XRD pattern of the product powder prepared in Example 1.
[0021] Figure 1-2 SEM image of the product powder prepared in Example 1.
[0022] Figure 1-3 EDS spectrum of the product powder prepared in Example 1.
[0023] Figure 2-1 XRD pattern of the product powder prepared in Example 2.
[0024] Figure 2-2 SEM image of the product powder prepared in Example 2.
[0025] Figure 2-3 EDS spectrum of the product powder prepared in Example 2.
[0026] Figure 3-1 XRD pattern of the product powder prepared in Example 3.
[0027] Figure 3-2 SEM image of the product powder prepared in Example 3.
[0028] Figure 3-3 EDS spectrum of the product powder prepared in Example 3.
[0029] Figure 4-1 XRD pattern of the product powder prepared in Example 4.
[0030] Figure 4-2 SEM image of the product powder prepared in Example 4.
[0031] Figure 4-3 EDS spectrum of the product powder prepared in Example 4.
[0032] Figure 5-1 XRD pattern of the product powder prepared in Example 5.
[0033] Figure 5-2 This is the SEM image of the product powder prepared in Example 5.
[0034] Figure 5-3 This is the EDS image of the product powder prepared in Example 5.
[0035] Figure 6-1 This is the XRD pattern of the product powder prepared in Example 6.
[0036] Figure 6-2 This is the SEM image of the product powder prepared in Example 6.
[0037] Figure 6-3 This is the EDS image of the product powder prepared in Example 6.
[0038] Figure 7-1 This is the XRD pattern of the product powder prepared in Example 7.
[0039] Figure 7-2 This is the SEM image of the product powder prepared in Example 7.
[0040] Figure 7-3 This is the EDS image of the product powder prepared in Example 7.
[0041] Figure 8 The XRD diagrams of the product powders prepared in Example 1 and Comparative Examples 1 and 2 are shown.
[0042] Fig. 9 The XRD diagrams of the product powders prepared in Example 5 and Comparative Example 3 are shown. DETAILED DESCRIPTION
[0043] The present invention provides a MAX phase binary solid solution material and a preparation method. To make the purpose, technical solution and effect of the present invention clearer and more specific, the present invention is further described in detail below. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the present invention.
[0044] In recent years, researchers have obtained MAX phase solid solution materials by solid dissolving elements into MAX phase ceramic materials. The formed MAX phase solid solution materials usually have excellent comprehensive properties. The unit solid solution MAX phase refers to a position in which solid solution occurs at the M position, A position or X position, and is occupied by two or more elements, while the other two positions remain unchanged and are still occupied by a single element. The double-position solid solution MAX phase refers to a position in which element solid solution occurs at both the M position and the A position, and the solid solution position is occupied by two or more elements, while the X position remains unchanged and is still occupied by a single element. Compared with the unit solid solution MAX phase, the double-position solid solution MAX phase is considered to be more conducive to improving the overall performance. However, the synthesis of the double-position solid solution MAX phase is relatively difficult. In order to obtain a pure phase double-position solid solution MAX material, it is often necessary to sinter the raw material powder under high temperature and pressure, which increases the difficulty of preparation. After long-term experimental research, the applicant has creatively proposed a MAX phase binary solid solution material and preparation method, using Ti-Al alloy powder or V-Al powder, carbon source powder, M' single powder, M' carbide powder and / or M'-Al alloy powder and A' single powder and / or A' carbide powder as raw material powders, mixing evenly, heating to 800℃~1250℃ for reaction sintering, and preparing MAX phase binary solid solution material without pressurization. In addition, the prepared MAX phase binary solid solution material was detected by XRD, and the test results showed that the MAX phase binary solid solution material was a pure phase solid solution, and no second phase was detected. The preparation method provided by the present invention can prepare a pure phase MAX phase binary solid solution material by sintering at low temperature (below 1250℃) and without pressurization with raw material powder of a specific composition, while improving the comprehensive performance, reducing the process difficulty, improving the controllability, and promoting industrial application and promotion.
[0045] The present invention is obtained on the basis of this research. The present invention is further described in detail below in conjunction with specific implementation methods.
[0046] In some embodiments of the present invention, a method for preparing a MAX phase binary solid solution material comprises the following preparation steps:
[0047] S1. Raw material mixing: Weigh the raw material powders according to the ratio, and mix the weighed raw material powders evenly to obtain a mixed powder; the raw material powders include M-Al alloy, the elemental M' in its elemental form, the carbide of M' and / or M'-Al alloy, the elemental A' in its elemental form and / or the carbide of A', and a carbon source; the element M of the M-Al alloy is selected from Ti or V, the elemental M' of the elemental M', the carbide of M' and / or M'-Al alloy is independently selected from at least one of Ti, W, V, Ta, and Cr, and at least one of the elemental M' is different from the element M, and the elemental A' of the elemental A' and / or the carbide of A' is independently selected from at least one of Si, Sn, and Ge. Optionally, the raw material powders include M-Al alloy, the elemental M' in its elemental form and / or the carbide of M', the elemental A' in its elemental form and / or the carbide of A', and a carbon source. Optionally, the raw material powders include M-Al alloy, the carbide of M', the elemental A' in its elemental form and / or the carbide of A', and a carbon source. Optionally, the raw material powders include M-Al alloy, the elemental M' in its elemental form, the elemental A' in its elemental form and / or the carbide of A', and a carbon source. Optionally, the raw material powders include M-Al alloy, M'-Al alloy and / or the carbide of M', the elemental A' in its elemental form and / or the carbide of A', and a carbon source. Optionally, the elemental A' of the elemental A' and / or the carbide of A' is independently selected from at least one of Si and Sn.
[0048] S2. Sintering of the mixed powder: Place the mixed powder in a protective atmosphere or vacuum, heat it up to 800 °C to 1250 °C for sintering to prepare a MAX-phase double-site solid solution material. The molecular formula of the MAX-phase double-site solid solution material is expressed as (Ti 1-x M′ x )3(Al 1-y A′ y )C2 or (V 1-x M′ x )2(Al 1-y A′ y )C, where the element M' is dissolved in the M site of the MAX phase, the element A' is dissolved in the A site of the MAX phase, x represents the atomic ratio of the element M' to the total amount of elements in the M site of the MAX phase, y represents the atomic ratio of the element A' to the total amount of elements in the A site of the MAX phase, 0 < x ≤ 0.5, x can be any value among 0.01 / 0.02 / 0.03 / 0.04... / 0.1 / 0.11 / 0.12 / 0.13 / 0.14 / ... / 0.2 / ... / 0.3 / ... / ... / 0.4 / ... / 0.5, 0 < y ≤ 0.5, y can be any value among 0.01 / 0.02 / 0.03 / 0.04... / 0.1 / 0.11 / 0.12 / 0.13 / 0.14 / ... / 0.2 / ... / 0.3 / ... / ... / 0.4 / ... / 0.5, (Ti 1-xM′ x )3(Al 1-y A′ y )C2 or (V 1-x M′ x )2(Al 1-y A′ y ) The values of x and y in C can be any combination of the aforementioned values. The MAX phase binary solid solution material is a pure phase solid solution. When XRD is used for phase detection, only the MAX phase binary solid solution material is detected, and no other second phase is detected.
[0049] In some embodiments of the present invention, in step S1, when the element M is Ti, the M-Al alloy is a Ti3Al alloy; when the element M is V, the M-Al alloy is selected from at least one of a V5Al alloy and a V5Al8 alloy.
[0050] In some embodiments of the present invention, the carbon source is selected from at least one of graphite, carbon black or glucose; optionally, the carbon source is graphite.
[0051] In some embodiments of the present invention, in step S1, the particle size of the M-Al alloy, the simple substance of M', the carbide of M', the M'-Al alloy, the simple substance of A' and the carbide of A' is 0.6-15 μm; it can be optionally 1-10 μm; it can be further optionally 1-8 μm; it can be further optionally 1-5 μm; it can be further optionally 3-5 μm.
[0052] In some embodiments of the present invention, in step S1, the weighed raw material powder is evenly mixed by ball milling, and the rotation speed of the ball mill is 50-250 r / min, and the rotation speed can be optionally 80-200 r / min; further can be optionally 100-180 r / min; the ball-to-material ratio is 12:1-25:1, and the ball-to-material ratio can be optionally 14:1-20:1; the ball milling time is 8-45 hours, and can be optionally 14-36 hours; further can be optionally 20-28 hours.
[0053] In some embodiments of the present invention, in step S1, when the element M is Ti, the mass percentage of the total mass of the carbide of M', the carbide of A' and the carbon in the carbon source to the M-Al alloy is 10-16%; optionally, when the element M is Ti, the mass percentage of the total mass of the carbide of M' and the carbon in the carbon source to the M-Al alloy is 10-16%; optionally, when the element M is Ti, the mass percentage of the total mass of the carbide of A' and the carbon in the carbon source to the M-Al alloy is 10-16%. When the element M is V, the mass percentage of the total mass of the carbide of M', the carbide of A' and the carbon in the carbon source to the M-Al alloy is 9-10%.
[0054] In some embodiments of the present invention, when the raw material powder in step S1 is Ti-Al alloy, M′ element, M′ carbide and / or M′-Al alloy, A′ carbide, and carbon source, step S2 is heated to above 880°C for sintering to prepare the MAX phase binary solid solution material; it can be sintered at above 900°C, further optionally heated to 900°C to 1200°C for reaction sintering, and further optionally heated to 900°C to 1100°C for reaction sintering. When the raw material powder in step S1 is Ti-Al alloy, M' single substance, M' carbide and / or M'-Al alloy, A' single substance, and a carbon source, step S2 heats the temperature to above 950°C for sintering to prepare the MAX phase binary solid solution material; it can be optionally heated to 1000-1250°C for reaction sintering; it can further be optionally heated to 1100-1250°C for reaction sintering; it can further be optionally heated to 1200-1250°C for reaction sintering. When the raw material powder in step S1 is V-Al alloy, M' single substance, M' carbide and / or M'-Al alloy, A' single substance and / or A' carbide, and a carbon source, step S2 is heated to 800-1000°C for sintering to prepare the MAX phase binary solid solution material; further optionally, sintering is performed at 800-900°C; further optionally, sintering is performed at 800-850°C.
[0055] In some embodiments of the present invention, in step S2, the sintering time may be selected to be 90 min to 360 min, further selected to be 100 min to 280 min, and further selected to be 120 min to 240 min.
[0056] In some embodiments of the present invention, in step S2, the product powder particle size of the prepared MAX phase binary solid solution material is 1 to 30 μm, optionally 3 to 30 μm, further optionally 3 to 25 μm, further optionally 3 to 20 μm, further optionally 3 to 15 μm; further optionally 3 to 10 μm.
[0057] In some embodiments of the present invention, the form of the MAX phase binary solid solution material of the present invention can be the prepared MAX phase binary solid solution product powder, or it can be at least one of a block, a film, a plate, a strip, a tube, and a rod prepared from the product powder using a conventional preparation method in the art. Conventional powder molding preparation methods in the art include but are not limited to sintering, spraying, cladding, spinning, extrusion, bonding or crimping, etc.
[0058] The present invention is further described in detail below by specific embodiments. In the embodiments of the present invention, the raw materials Ti3Al alloy powder, V5Al alloy powder, V5Al8 alloy powder, WC powder, VC powder, TaC powder, Cr3C2 powder, SiC powder, pure titanium powder, TiC powder and single substance Sn powder have a purity of more than 99wt% and a particle size of 3-5μm, and the graphite has a purity of 99.99wt% and a particle size of 40-50nm, all of which are commercially available.
[0059] Example 1
[0060] Example 1 provides a method for preparing a MAX phase binary solid solution material, and the specific preparation steps are as follows:
[0061] S1. Raw material mixing: weigh the raw material powders according to the ratio, the raw material powders are 84g Ti3Al powder, 3g WC powder, 2g SiC powder and 11g graphite, the mass percentage of the total mass of carbon in WC, SiC and graphite to Ti3Al is 14.04%, the weighed raw material powders are ball-milled, cemented carbide grinding balls are used, and anhydrous ethanol is added as the ball-milling medium, the mass ratio of cemented carbide grinding balls to raw material powders is 16:1, the ball-milling speed is 120r / min, the ball-milling time is 24 hours, and after the ball-milling, the obtained mixed wet material is vacuum-dried at 70°C to obtain a mixed powder;
[0062] S2. Sintering of mixed powder: The mixed powder obtained in step S1 is loaded into a corundum boat and placed in a tubular furnace. Then, argon is introduced into the tubular furnace at a flow rate of 100 mL / min. In an atmosphere of flowing argon, the temperature is increased to 1100°C at a heating rate of 5°C / min and sintered for 4 hours. After the sintering is completed, the furnace is cooled to room temperature to obtain a sintered product. The sintered product is manually lightly ground into particles to obtain a product powder.
[0063] The product powder prepared in Example 1 was tested by X-ray diffractometer (XRD), and its XRD pattern was as follows: Figure 1-1 As shown, from Figure 1-1 It can be seen that the product powder prepared in Example 1 is a single-phase (Ti, W)3(Al, Si)C2 binary solid solution, and no other second phase is detected.
[0064] The product powder prepared in Example 1 was observed using a scanning electron microscope (SEM), and its SEM image is as follows: Figure 1-2 As shown, the element analysis is carried out by combining with energy dispersive spectrometer (EDS), and the energy spectrum is as follows Figure 1-3 As shown, from Figure 1-2 It can be seen that the product powder prepared in Example 1 has a layered structure and retains the structural characteristics of the MAX phase ternary ceramic material. The particle size of the product powder is about 5 to 25 μm. Figure 1-3 It can be seen that the basic element distribution of Ti atoms and W atoms is consistent, and the basic element distribution of Al atoms and Si atoms is consistent. It can be seen that W atoms are solid dissolved in the position of Ti atoms, and Si atoms are solid dissolved in the position of Al atoms, which further proves that the prepared product powder is a (Ti, W) 3 (Al, Si) C2 binary solid solution material. The EDS element quantitative analysis results show that the element W accounts for 1at% of the total amount of elements in the M position of the MAX phase, and the element Si accounts for 10at% of the total amount of elements in the A position. Therefore, the molecular formula of the MAX phase binary solid solution material is expressed as (Ti 0.99 W 0.01 )3(Al 0.9 Si 0.1 )C2.
[0065] Example 2
[0066] Example 2 provides a method for preparing a MAX phase binary solid solution material, and the specific preparation steps are as follows:
[0067] S1. Raw material mixing: weigh the raw material powder according to the ratio, the raw material powder is Ti3Al powder 78.5g, VC powder 9.5g, SiC powder 2g and graphite 10g, the mass percentage of the total mass of carbon in VC, SiC and TiC and Ti3Al is 15.8%, the weighed raw material powder is ball-milled, using carbide grinding balls, and adding anhydrous ethanol as the ball-milling medium, the mass ratio of carbide grinding balls to raw material powder is 16:1, the ball-milling speed is 120r / min, the ball-milling time is 24 hours, and after the ball-milling, the obtained mixed wet material is vacuum-dried at 70°C to obtain a mixed powder;
[0068] S2. Sintering of mixed powder: The mixed powder obtained in step S1 is loaded into a corundum boat and placed in a tubular furnace. Then, argon is introduced into the tubular furnace at a flow rate of 100 mL / min. In an atmosphere of flowing argon, the temperature is increased to 900°C at a heating rate of 5°C / min and sintered for 4 hours. After the sintering is completed, the furnace is cooled to room temperature to obtain a sintered product. The sintered product is manually lightly ground into particles to obtain a product powder.
[0069] The product powder prepared in Example 2 was detected by X-ray diffractometer (XRD), and its XRD pattern was as follows: Figure 2-1 As shown, from Figure 2-1 It can be seen that the product powder prepared in Example 2 is a single-phase (Ti, V)3(Al, Si)C2 binary solid solution, and no other second phase is detected.
[0070] The product powder prepared in Example 2 was observed using a scanning electron microscope (SEM), and its SEM image is as follows: Figure 2-2As shown, the element analysis is carried out by combining with energy dispersive spectrometer (EDS), and the energy spectrum is as follows Figure 2-3 As shown, from Figure 2-2 It can be seen that the product powder prepared in Example 2 has a layered structure and retains the structural characteristics of the MAX phase ternary ceramic material. The particle size of the product powder is about 3 to 10 μm. Figure 2-3 It can be seen that the basic distribution of elements of Ti atoms and V atoms is consistent, and the basic distribution of elements of Al atoms and Si atoms is consistent. It can be seen that V atoms are solid dissolved in the position of Ti atoms, and Si atoms are solid dissolved in the position of Al atoms, which further proves that the prepared product powder is a (Ti, V) 3 (Al, Si) C2 binary solid solution material. The results of EDS element quantitative analysis show that the element V accounts for 10at% of the total amount of elements in the M position of the MAX phase, and the element Si accounts for 10at% of the total amount of elements in the A position. Therefore, the molecular formula of the MAX phase binary solid solution material is expressed as (Ti 0.9 V 0.1 )3(Al 0.9 Si 0.1 )C2.
[0071] Example 3
[0072] Example 3 provides a method for preparing a MAX phase binary solid solution material, and the specific preparation steps are as follows:
[0073] S1. Raw material mixing: weigh the raw material powders according to the ratio, the raw material powders are 84g Ti3Al powder, 1g TaC powder, 4g SiC powder and 12g graphite, the mass percentage of the total mass of carbon in TaC, SiC and graphite to Ti3Al is 15.8%, the weighed raw material powders are ball-milled, cemented carbide grinding balls are used, and anhydrous ethanol is added as the ball-milling medium, the mass ratio of cemented carbide grinding balls to raw material powders is 16:1, the ball-milling speed is 120r / min, the ball-milling time is 24 hours, and after the ball-milling, the obtained mixed wet material is vacuum-dried at 70°C to obtain a mixed powder;
[0074] S2. Sintering of mixed powder: The mixed powder obtained in step S1 is loaded into a corundum boat and placed in a tubular furnace. Then, argon is introduced into the tubular furnace at a flow rate of 100 mL / min. In an atmosphere of flowing argon, the temperature is increased to 900°C at a heating rate of 5°C / min and sintered for 4 hours. After the sintering is completed, the furnace is cooled to room temperature to obtain a sintered product. The sintered product is manually lightly ground into particles to obtain a product powder.
[0075] The product powder prepared in Example 3 was detected by X-ray diffractometer (XRD), and its XRD pattern was as follows: Figure 3-1 As shown, from Figure 3-1It can be seen that the product powder prepared in Example 3 is a single-phase (Ti, Ta) 3 (Al, Si) C 2 binary solid solution, and no other second phase is detected.
[0076] The product powder prepared in Example 3 was observed using a scanning electron microscope (SEM). Figure 3-2 As shown, the element analysis is carried out by combining with energy dispersive spectrometer (EDS), and the energy spectrum is as follows Figure 3-3 As shown, from Figure 3-2 It can be seen that the product powder prepared in Example 3 has a layered structure, retaining the structural characteristics of the MAX phase ternary ceramic material, and the particle size of the product powder is about 5 to 15 μm. Figure 3-3 It can be seen that the basic element distribution of Ti atoms and Ta atoms is consistent, and the basic element distribution of Al atoms and Si atoms is consistent. It can be seen that Ta atoms are solid dissolved in the position of Ti atoms, and Si atoms are solid dissolved in the position of Al atoms. This further proves that the prepared product powder is a (Ti, Ta) 3 (Al, Si) C2 binary solid solution material. The EDS element quantitative analysis results show that the element Ta accounts for 1at% of the total amount of elements in the M position of the MXA phase, and the element Si accounts for 20at% of the total amount of elements in the A position. It can be seen that the molecular formula of the MAX phase binary solid solution material is expressed as (Ti 0.99 Ta 0.01 )3(Al 0.8 Si 0.2 )C2.
[0077] Example 4
[0078] Example 4 provides a method for preparing a MAX phase binary solid solution material, and the specific preparation steps are as follows:
[0079] S1. Raw material mixing: The raw material powders are weighed according to the ratio, the raw material powders are 61.5g Ti3Al powder, 32.5g Cr3C2 powder, 5.5g SiC powder and 0.5g graphite, the mass percentage of the total mass of carbon in Cr3C2, SiC and graphite and Ti3Al is 10.5%, the weighed raw material powders are ball milled, cemented carbide grinding balls are used, and anhydrous ethanol is added as the ball milling medium, the mass ratio of cemented carbide grinding balls to raw material powders is 16:1, the ball milling speed is 120r / min, the ball milling time is 24 hours, and after the ball milling, the obtained mixed wet material is vacuum dried at 70°C to obtain a mixed powder;
[0080] S2. Sintering of mixed powder: The mixed powder obtained in step S1 is loaded into a corundum boat and placed in a tubular furnace. Then, argon is introduced into the tubular furnace at a flow rate of 100 mL / min. In an atmosphere of flowing argon, the temperature is increased to 1100°C at a heating rate of 5°C / min and sintered for 2 hours. After the sintering is completed, the furnace is cooled to room temperature to obtain a sintered product. The sintered product is manually lightly ground into particles to obtain a product powder.
[0081] The product powder prepared in Example 4 was detected by X-ray diffractometer (XRD), and its XRD pattern was as follows: Figure 4-1 As shown, from Figure 4-1 It can be seen that the product powder prepared in Example 4 is a single-phase (Ti, Cr) 3 (Al, Si) C 2 binary solid solution, and no other second phase is detected.
[0082] The product powder prepared in Example 4 was observed using a scanning electron microscope (SEM), and its SEM image is as follows: Figure 4-2 As shown, the element analysis is carried out by combining with energy dispersive spectrometer (EDS), and the energy spectrum is as follows Figure 4-3 As shown, from Figure 4-2 It can be seen that the product powder prepared in Example 4 has a layered structure and retains the structural characteristics of the MAX phase ternary ceramic material. The particle size of the product powder is about 5 to 15 μm. Figure 4-3 It can be seen that the basic element distribution of Ti atoms and Cr atoms is consistent, and the basic element distribution of Al atoms and Si atoms is consistent. It can be seen that Cr atoms are solid dissolved in the position of Ti atoms, and Si atoms are solid dissolved in the position of Al atoms. This further proves that the prepared product powder is a (Ti, Cr) 3 (Al, Si) C2 binary solid solution material. The EDS element analysis results show that the element Cr accounts for 50at% of the total amount of elements in the M position of the MAX phase, and the element Si accounts for 40at% of the total amount of elements in the A position. It can be seen that the molecular formula of the MAX phase binary solid solution material is expressed as (Ti 0.5 Cr 0.5 )3(Al 0.6 Si 0.4 )C2.
[0083] Example 5
[0084] Example 5 provides a method for preparing a MAX phase binary solid solution material, and the specific preparation steps are as follows:
[0085] S1. Raw material mixing: weigh the raw material powders according to the ratio, the raw material powders are 82g Ti3Al powder, 2g WC powder, 6g elemental Sn powder and 11g graphite, the total mass percentage of carbon in WC and graphite to Ti3Al is 13.6%, the weighed raw material powders are ball-milled, cemented carbide grinding balls are used, and anhydrous ethanol is added as the ball-milling medium, the mass ratio of cemented carbide grinding balls to raw material powders is 16:1, the ball-milling speed is 120r / min, the ball-milling time is 24 hours, and after the ball-milling, the obtained mixed wet material is vacuum-dried at 70°C to obtain a mixed powder;
[0086] S2. Sintering of mixed powder: The mixed powder obtained in step S1 is loaded into a corundum boat and placed in a tubular furnace. Then, argon is introduced into the tubular furnace at a flow rate of 100 mL / min. In an atmosphere of flowing argon, the temperature is increased to 1200°C at a heating rate of 5°C / min and sintered for 4 hours. After the sintering is completed, the furnace is cooled to room temperature to obtain a sintered product. The sintered product is manually lightly ground into particles to obtain a product powder.
[0087] The product powder prepared in Example 5 was detected by X-ray diffractometer (XRD), and its XRD pattern was as follows: Figure 5-1 As shown, from Figure 5-1 It can be seen that the product powder prepared in Example 5 is a single-phase (Ti, W)3(Al, Sn)C2 binary solid solution, and no other second phase is detected.
[0088] The product powder prepared in Example 5 was observed using a scanning electron microscope (SEM). Figure 5-2 As shown, the element analysis is carried out by combining with energy dispersive spectrometer (EDS), and the energy spectrum is as follows Figure 5-3 As shown, from Figure 5-2 It can be seen that the product powder prepared in Example 5 has a layered structure and retains the structural characteristics of the MAX phase ternary ceramic material. The particle size of the product powder is about 3 to 15 μm. Figure 5-3 It can be seen that the basic element distribution of Ti atoms and W atoms is consistent, and the basic element distribution of Al atoms and Sn atoms is consistent. It can be seen that W atoms are solid dissolved in the position of Ti atoms, and Sn atoms are solid dissolved in the position of Al atoms, which further proves that the prepared product powder is a (Ti, W) 3 (Al, Sn) C2 binary solid solution material. The EDS element quantitative analysis results show that the element W accounts for 2at% of the total amount of elements in the M position of the MAX phase, and the element Sn accounts for 20at% of the total amount of elements in the A position. It can be seen that the molecular formula of the MAX phase binary solid solution material is expressed as (Ti 0.98 W 0.02 )3(Al 0.8 Sn 0.2 )C2.
[0089] Example 6
[0090] Example 6 provides a method for preparing a MAX phase binary solid solution material, and the specific preparation steps are as follows:
[0091] S1. Raw material mixing: weigh the raw material powders according to the ratio, the raw material powders are 53.5g of V5Al powder, 22.4g of V5Al8 powder, 2.8g of pure titanium powder, 14.1g of elemental Sn powder and 7.2g of graphite, the mass percentage of graphite and V-Al alloy is 9.5%, the weighed raw material powders are ball-milled, cemented carbide grinding balls are used, and anhydrous ethanol is added as the ball-milling medium, the mass ratio of cemented carbide grinding balls to raw material powders is 16:1, the ball-milling speed is 120r / min, the ball-milling time is 24 hours, and after the ball-milling, the obtained mixed wet material is vacuum-dried at 70°C to obtain a mixed powder;
[0092] S2. Sintering of mixed powder: The mixed powder obtained in step S1 is loaded into a corundum boat and placed in a tubular furnace. Then, argon gas is introduced into the tubular furnace at a flow rate of 100 mL / min. The temperature is increased to 850°C at a heating rate of 5°C / min under an atmosphere of flowing argon gas and the mixture is sintered for 4 hours. After the sintering is completed, the mixture is cooled to room temperature with the furnace to obtain a sintered product. The sintered product is manually lightly ground into particles to obtain a product powder.
[0093] The product powder prepared in Example 6 was detected by X-ray diffractometer (XRD), and its XRD pattern was as follows: Figure 6-1 As shown, from Figure 6-1 It can be seen that the product powder prepared in Example 6 is a single-phase (V, Ti) 2 (Al, Sn) C binary solid solution, and no other second phase is detected.
[0094] The product powder prepared in Example 6 was observed using a scanning electron microscope (SEM). Figure 6-2 As shown, the element analysis is carried out by combining with energy dispersive spectrometer (EDS), and the energy spectrum is as follows Figure 6-3 As shown, from Figure 6-2 It can be seen that the product powder prepared in Example 6 has a layered structure and retains the structural characteristics of the MAX phase ternary ceramic material. The particle size of the product powder is about 5 to 20 μm. Figure 6-3It can be seen that the basic element distribution of V atoms and Ti atoms is consistent, and the basic element distribution of Al atoms and Sn atoms is consistent. It can be seen that Ti atoms are solid dissolved in the position of V atoms, and Sn atoms are solid dissolved in the position of Al atoms, which further proves that the prepared product powder is a (V,Ti)2(Al,Sn)C binary solid solution material. The EDS element quantitative analysis results show that the element Ti accounts for 5at% of the total amount of elements in the M position of the MAX phase, and the element Sn accounts for 20at% of the total amount of elements in the A position. Therefore, the molecular formula of the MAX phase binary solid solution material is expressed as (V 0.95 Ti 0.05 )2(Al 0.8 Sn 0.2 )C.
[0095] Example 7
[0096] Example 7 provides a method for preparing a MAX phase binary solid solution material, and the specific preparation steps are as follows:
[0097] S1. Raw material mixing: The raw material powders were weighed according to the ratio, the raw material powders were 83.7 g Ti3Al powder, 1.8 g V5Al powder, 2.2 g SiC powder, 10.3 g graphite and 2 g TiC powder, the mass percentage of the sum of the mass of graphite, SiC and carbon in TiC to the sum of Ti3Al and V5Al was 13.3%, the weighed raw material powders were ball milled, cemented carbide grinding balls were used, and anhydrous ethanol was added as the ball milling medium, the mass ratio of cemented carbide grinding balls to raw material powders was 16:1, the ball milling speed was 120 r / min, the ball milling time was 24 hours, and after the ball milling, the obtained mixed wet material was vacuum dried at 70 ° C to obtain a mixed powder;
[0098] S2. Sintering of mixed powder: The mixed powder obtained in step S1 is loaded into a corundum boat and placed in a tubular furnace. Then, argon is introduced into the tubular furnace at a flow rate of 100 mL / min. In an atmosphere of flowing argon, the temperature is increased to 1200°C at a heating rate of 5°C / min and sintered for 4 hours. After the sintering is completed, the furnace is cooled to room temperature to obtain a sintered product. The sintered product is manually lightly ground into particles to obtain a product powder.
[0099] The product powder prepared in Example 7 was detected by X-ray diffractometer (XRD), and its XRD pattern was as follows: Figure 7-1 As shown, from Figure 7-1 It can be seen that the product powder prepared in Example 7 is a single-phase (Ti, V)3(Al, Si)C2 binary solid solution, and no other second phase is detected.
[0100] The product powder prepared in Example 7 was observed using a scanning electron microscope (SEM), and its SEM image is as follows: Figure 7-2As shown, the element analysis is carried out by combining with energy dispersive spectrometer (EDS), and the energy spectrum is as follows Figure 7-3 As shown, from Figure 7-2 It can be seen that the product powder prepared in Example 7 has a layered structure and retains the structural characteristics of the MAX phase ternary ceramic material. The particle size of the product powder is about 3 to 20 μm. Figure 7-3 It can be seen that the basic distribution of elements of Ti atoms and V atoms is consistent, and the basic distribution of elements of Al atoms and Si atoms is consistent. It can be seen that Ti atoms are solid dissolved in the position of V atoms, and Si atoms are solid dissolved in the position of Al atoms, which further proves that the prepared product powder is a (Ti, V) 3 (Al, Si) C2 binary solid solution material. The results of EDS element quantitative analysis show that the element V accounts for 2at% of the total amount of elements in the M position of the MAX phase, and the element Si accounts for 10at% of the total amount of elements in the A position. Therefore, the molecular formula of the MAX phase binary solid solution material is expressed as (Ti 0.98 V 0.02 )3(Al 0.9 Si 0.1 )C2.
[0101] Comparative Example 1
[0102] Comparative Example 1 provides a method for preparing a MAX phase binary solid solution material, and the specific preparation steps are as follows:
[0103] S1. Raw material mixing: weigh the raw material powders according to the ratio, the raw material powders are 84g Ti3Al powder, 3g WC powder, 2g SiC powder and 11g graphite, the mass percentage of the total mass of carbon in WC, SiC and graphite to Ti3Al is 14.04%, the weighed raw material powders are ball-milled, cemented carbide grinding balls are used, and anhydrous ethanol is added as the ball-milling medium, the mass ratio of cemented carbide grinding balls to raw material powders is 16:1, the ball-milling speed is 120r / min, the ball-milling time is 24 hours, and after the ball-milling, the obtained mixed wet material is vacuum-dried at 70°C to obtain a mixed powder;
[0104] S2. Sintering of mixed powder: The mixed powder obtained in step S1 is loaded into a corundum boat and placed in a tubular furnace. Then, argon is introduced into the tubular furnace at a flow rate of 100 mL / min. The temperature is increased to 750°C at a heating rate of 5°C / min under an atmosphere of flowing argon. The mixture is sintered for 4 hours. After the sintering is completed, the mixture is cooled to room temperature with the furnace to obtain a sintered product. The sintered product is manually lightly ground into particles to obtain a product powder.
[0105] The product powder prepared in Comparative Example 1 was tested by X-ray diffractometer (XRD), and its XRD pattern was as follows: Figure 8 As shown, from Figure 8It can be seen that in addition to the (Ti, W)3(Al, Si)C2 binary solid solution phase, the second phase TiC was also detected in the product powder prepared in Comparative Example 1. Compared with Example 1, due to the low sintering temperature of Comparative Example 1, a single-phase binary solid solution product cannot be obtained.
[0106] Comparative Example 2
[0107] Comparative Example 2 provides a method for preparing a MAX phase binary solid solution material, and the specific preparation steps are as follows:
[0108] S1. Raw material mixing: The raw material powders are weighed according to the ratio, the raw material powders are 84g Ti3Al powder, 3g WC powder, 2g SiC powder and 7g graphite, the mass percentage of the total mass of carbon in WC, SiC and graphite to Ti3Al is 9.26%, the weighed raw material powders are ball milled, cemented carbide grinding balls are used, and anhydrous ethanol is added as the ball milling medium, the mass ratio of cemented carbide grinding balls to raw material powders is 16:1, the ball milling speed is 120r / min, the ball milling time is 24 hours, and after the ball milling, the obtained mixed wet material is vacuum dried at 70°C to obtain a mixed powder;
[0109] S2. Sintering of mixed powder: The mixed powder obtained in step S1 is loaded into a corundum boat and placed in a tubular furnace. Then, argon is introduced into the tubular furnace at a flow rate of 100 mL / min. The temperature is increased to 1100°C at a heating rate of 5°C / min in an atmosphere of flowing argon and sintered for 4 hours. After the heat preservation and sintering is completed, the furnace is cooled to room temperature to obtain a sintered product. The sintered product is manually lightly ground into particles to obtain a product powder.
[0110] The product powder prepared in Comparative Example 2 was tested by X-ray diffractometer (XRD), and its XRD pattern was as follows: Figure 8 As shown, from Figure 8 It can be seen that in addition to the (Ti, W)3(Al, Si)C2 binary solid solution phase, the second phase Ti2AlC was also detected in the product powder prepared in Comparative Example 2. Compared with Example 1, the graphite doping amount in Comparative Example 2 is not appropriate, a second phase product appears, and a single-phase binary solid solution product is not obtained.
[0111] Comparative Example 3
[0112] Comparative Example 3 provides a method for preparing a MAX phase binary solid solution material, and the specific preparation steps are as follows:
[0113] S1. Raw material mixing: weigh the raw material powders according to the ratio, the raw material powders are 82g Ti3Al powder, 2g WC powder, 6g elemental Sn powder and 7.5g graphite, the total mass percentage of carbon in WC and graphite to Ti3Al is 9.30%, the weighed raw material powders are ball-milled, cemented carbide grinding balls are used, and anhydrous ethanol is added as the ball-milling medium, the mass ratio of cemented carbide grinding balls to raw material powders is 16:1, the ball-milling speed is 120r / min, the ball-milling time is 24 hours, and after the ball-milling, the obtained mixed wet material is vacuum-dried at 70°C to obtain a mixed powder;
[0114] S2. Sintering of mixed powder: The mixed powder obtained in step S1 is loaded into a corundum boat and placed in a tubular furnace. Then, argon is introduced into the tubular furnace at a flow rate of 100 mL / min. In an atmosphere of flowing argon, the temperature is increased to 1200°C at a heating rate of 5°C / min and sintered for 4 hours. After the sintering is completed, the furnace is cooled to room temperature to obtain a sintered product. The sintered product is manually lightly ground into particles to obtain a product powder.
[0115] The product powder prepared in Comparative Example 3 was tested by X-ray diffractometer (XRD), and its XRD pattern was as follows: Fig. 9 As shown, from Fig. 9 It can be seen that in addition to the (Ti, W)3(Al, Sn)C2 binary solid solution, the second phase Ti2AlC was also detected in the product powder prepared in Comparative Example 3. Compared with Example 5, the graphite doping amount in Comparative Example 3 is not appropriate, and a single-phase binary solid solution product cannot be obtained.
[0116] It should be understood that the application of the present invention is not limited to the above examples. For ordinary technicians in this field, improvements or changes can be made based on the above description. All these improvements and changes should fall within the scope of protection of the claims attached to the present invention.
Claims
1. A method for preparing a MAX phase binary solid solution material, characterized in that: The method comprises the following preparation steps: S1. Raw material mixing: weighing raw material powders according to a ratio, and mixing the weighed raw material powders uniformly to obtain mixed powders; the raw material powders include M-Al alloy, simple substance M', carbide of M' and / or M'-Al alloy, simple substance A' and / or carbide of A', and a carbon source; the element M of the M-Al alloy is selected from Ti or V, the simple substance M', carbide of M' and / or element M' of the M'-Al alloy is independently selected from at least one of Ti, W, V, Ta and Cr, and at least one of the elements M' is different from the element M, and the simple substance A' and / or element A' of the carbide of A' is independently selected from at least one of Si, Sn and Ge; S2. Sintering of the mixed powder: Place the mixed powder in a protective atmosphere or vacuum, heat it to 800 °C to 1250 °C for sintering to prepare a MAX-phase double-site solid solution material, and the molecular formula of the MAX-phase double-site solid solution material is expressed as (Ti 1- x M′ x )3(Al 1-y A′ y )C2 or (V 1-x M′ x )2(Al 1-y A′ y )C, where x and y are atomic ratios, 0 < x ≤ 0.5, 0 < y ≤ 0.5, and the MAX-phase double-site solid solution material is a pure-phase solid solution.
2. The method for preparing the MAX phase binary solid solution material according to claim 1, characterized in that: In step S1, when the element M is Ti, the M-Al alloy is a Ti3Al alloy; when the element M is V, the M-Al alloy is selected from at least one of a V5Al alloy and a V5Al8 alloy.
3. The method for preparing the MAX phase binary solid solution material according to claim 1 or 2, characterized in that: The carbon source is selected from at least one of graphite, carbon black or glucose.
4. The method for preparing the MAX phase binary solid solution material according to claim 1 or 2, characterized in that: In step S1, the particle sizes of the M-Al alloy, the simple substance of M', the carbide of M', the M'-Al alloy, the simple substance of A' and the carbide of A' are 0.6-15 μm.
5. The method for preparing the MAX phase binary solid solution material according to claim 1 or 2, characterized in that: In step S1, the weighed raw material powder is mixed uniformly by ball milling, the rotation speed of the ball mill is 50 to 250 r / min, the ball-to-material ratio is 12:1 to 25:1, and the ball milling time is 8 to 45 hours.
6. The method for preparing the MAX phase binary solid solution material according to claim 1 or 2, characterized in that: In step S1, when the element M is Ti, the mass percentage of the total mass of the carbide of M′, the carbide of A′ and the carbon in the carbon source to the M-Al alloy is 10-16%; when the element M is V, the mass percentage of the total mass of the carbide of M′, the carbide of A′ and the carbon in the carbon source to the M-Al alloy is 9-10%.
7. The method for preparing the MAX phase binary solid solution material according to claim 1 or 2, characterized in that: When the raw material powder in step S1 is Ti-Al alloy, M' single substance, M' carbide and / or M'-Al alloy, A' carbide, and carbon source, step S2 is heated to above 880°C for sintering to prepare the MAX phase binary solid solution material; when the raw material powder in step S1 is Ti-Al alloy, M' single substance, M' carbide and / or M'-Al alloy, A' single substance, and carbon source, step S2 is heated to above 950°C for sintering to prepare the MAX phase binary solid solution material.
8. The method for preparing the MAX phase binary solid solution material according to claim 1 or 2, characterized in that: When the raw material powder in step S1 is V-Al alloy, M' single substance, M' carbide and / or M'-Al alloy, A' single substance and / or A' carbide, and a carbon source, step S2 heats the temperature to 800-1000° C. for sintering to prepare the MAX phase binary solid solution material.
9. The method for preparing the MAX phase binary solid solution material according to claim 1 or 2, characterized in that: In step S2, the particle size of the product powder of the prepared MAX phase binary solid solution material is 1 to 30 μm.
10. A MAX phase binary solid solution material, comprising a product powder obtained by the preparation method of a MAX phase binary solid solution material according to any one of claims 1 to 9, and at least one of a block, a film, a plate, a strip, a tube, and a rod prepared from the product powder.