A SiC f Residual stress control and optimization method of Ti3Al composites

Abstract

The present invention belongs to the technical field of metal matrix composite materials, and specifically relates to a SiC f / Ti3Al composite material residual stress control and optimization method. The present invention introduces an interface stress release layer on the surface of SiC fiber, which significantly improves the interface adaptability between SiC fiber and Ti3Al matrix, and effectively reduces the residual stress induced by the difference in thermal expansion coefficient at the interface; matrix stress release layers with high plasticity are alternately introduced into the Ti3Al matrix to construct a laminated structure, which can effectively release the residual stress of SiC / Ti3Al composite material and prevent the material from failing due to stress accumulation during service. The preparation of composite materials using the SiC / Ti3Al pioneer wire provided by the present invention can achieve residual stress control and optimization, effectively solve the problem of high residual stress, and improve the stability of materials during processing and service, which is of great significance to the application research of SiC / Ti3Al composite materials.

Description

Technical Field

[0001] The present invention belongs to the technical field of metal matrix composite materials, and specifically relates to a SiC f / Ti3Al composite material residual stress control and optimization method. Background Art

[0002] SiC / Ti3Al composite materials can couple the excellent properties of continuous SiC fibers with the advantages of Ti3Al alloys to obtain composite materials with high specific strength, high specific stiffness, low thermal expansion coefficient, high temperature resistance, fatigue resistance and other properties. They are ideal choices for materials such as bolt fasteners, thrust rods, turbine shafts, skins, and stiffeners for hypersonic aircraft, and have become a key new material in the aerospace manufacturing field.

[0003] Since SiC / Ti3Al composites are typically formed by hot pressing, the difference in thermal expansion coefficients between the SiC fibers and the Ti3Al matrix during the manufacturing process inevitably leads to high residual stresses in the SiC / Ti3Al composites. The presence of residual stresses can have a significant impact on the composite's various mechanical properties and service life. In particular, during the service life of SiC / Ti3Al composites, the uneven residual stresses within the composite can cause crack initiation and propagation, leading to catastrophic failure.

[0004] It can be seen that the existence of high residual stress is a key factor limiting the application of SiC / Ti3Al composites. Therefore, how to reduce the residual stress in SiC / Ti3Al composites without affecting the performance of the composites has become an urgent problem to be solved. Summary of the Invention

[0005] The present invention aims to provide a SiC f / Ti3Al composite material residual stress control and optimization method, the method provided by the present invention can effectively reduce SiC f / Ti3Al composite material internal residual stress, SiC prepared by the control and optimization method of the present invention f / Ti3Al composite materials can be used as a high-performance, low residual stress strategic aerospace material.

[0006] In order to achieve the above object, the present invention provides the following technical solutions:

[0007] The present invention provides a SiC f The method for regulating and optimizing residual stress of a Ti3Al composite material comprises the following steps:

[0008] (1) ion cleaning the carbon-coated SiC fiber under argon conditions to obtain pretreated SiC fiber;

[0009] (2) using Mo as a sputtering target, magnetron sputtering the pretreated SiC fiber under argon conditions to obtain a SiC fiber with a Mo interface stress release layer deposited;

[0010] (3) Using Ti3Al alloy and Ti2AlNb alloy as sputtering targets, magnetron sputtering is performed on the SiC fiber deposited with the Mo interface stress release layer under argon conditions, and Ti3Al matrix layer and Ti2AlNb matrix stress release layer are alternately deposited on the surface of the SiC fiber deposited with the Mo interface stress release layer to obtain SiC f / Ti3Al composite precursor wire;

[0011] (4) The precursor wires are evenly arranged and hot isostatically pressed to obtain SiC with controlled and optimized residual stress. f / Ti3Al composite materials.

[0012] Preferably, the diameter of the SiC fiber containing the carbon coating is 90-110 μm, and the thickness of the carbon coating is 2-4 μm.

[0013] Preferably, the magnetron sputtering parameters in step (2) include: the gas pressure in the coating chamber is 0.6~1.2Pa; the argon flow rate is 60~100sccm; the deposition bias is -50~-300V; the sputtering current is 0.9~2.5A; the sputtering power is 300~600W; and the deposition rate is 0.8~2.4μm / h.

[0014] Preferably, the thickness of the Mo interface stress release layer is 0.5 to 3.5 μm.

[0015] Preferably, the target magnetron sputtering parameters in step (3) include: argon gas flow rate of 60 to 100 sccm, gas pressure in the coating chamber of 0.5 to 1.1 Pa, deposition bias of -50 to -300 V, sputtering current of 1.6 to 2.4 A, sputtering power of 600 to 800 W, and deposition rate of 2 to 4 μm / h.

[0016] Preferably, the repetition period of the alternate deposition of the Ti3Al matrix layer and the Ti2AlNb matrix stress release layer is ≥3;

[0017] The single layer thickness of the Ti3Al matrix layer is 2 to 4 μm; the single layer thickness of the Ti2AlNb matrix stress release layer is 0.5 to 4 μm; and the total thickness of the alternately deposited Ti3Al matrix layer and Ti2AlNb matrix stress release layer is 18 to 38 μm.

[0018] Preferably, the SiC f In the precursor fibers of the SiC / Ti3Al composite materials, the total thickness of the SiC fiber surface film layer is 20 to 40 μm.

[0019] Preferably, the hot isostatic pressing is performed at a temperature of 930 to 980° C., a pressure of 120 to 200 MPa, and a time of 1 to 5 hours.

[0020] The present invention also provides a SiC composite material prepared by the above-mentioned preparation method with controlled and optimized residual stress. f / Ti3Al composite material, composed of SiC f / Ti3Al composite precursor wires are evenly arranged and then formed by hot isostatic pressing; a single SiC f The precursor wire of the Ti3Al / Ti3Al composite material includes SiC fiber, carbon coating, Mo interface stress release layer and alternating Ti3Al matrix layer and Ti2AlNb matrix stress release layer from the inside to the outside.

[0021] The present invention also provides the SiC f Application of Ti3Al / Ti3Al composite materials in aerospace field.

[0022] The present invention provides a SiC f The residual stress control and optimization method of SiC / Ti3Al composite materials was studied. The Mo interface stress release layer was introduced between the continuous SiC fiber and the Ti3Al matrix to significantly reduce the residual stress at the interface of the composite material. The Mo coating is not only a strong stabilizing element of the β-Ti isomorphous type, but also has a moderate thermal expansion coefficient (the thermal expansion coefficient of the Mo coating is between that of the SiC fiber and the Ti3Al matrix). It is introduced into the SiC as an interface stress release layer. f In SiC / Ti3Al composites, it can not only reduce the residual stress at the interface of the composite material caused by the difference in thermal expansion coefficient between the fiber and the matrix, but also induce the formation of a β-Ti tough transition layer at the interface, alleviate the stress concentration at the interface between the continuous SiC fiber and the Ti3Al matrix, and reduce the failure risk of the composite material.

[0023] Furthermore, the highly plastic Ti2AlNb matrix stress-relieving layers, alternating within the Ti3Al matrix, are Ti2AlNb intermetallic compounds, forming a good interface bond between the two. Compared to Ti3Al, Ti2AlNb possesses greater toughness, effectively relieving residual stress. By constructing a multilayer Ti3Al / Ti2AlNb matrix, the composite material improves overall toughness while effectively reducing residual stress within the composite.

[0024] The present invention provides a SiCf The method for regulating and optimizing residual stress of SiC / Ti3Al composite materials aims to effectively reduce the unevenly distributed residual stress in the composite material by simultaneously regulating and optimizing the residual stress at the composite material interface and in the matrix, thereby improving the processing and service stability of the composite material and thus increasing the application potential of the composite material. f The application research of / Ti3Al composite materials is of great significance.

[0025] In particular, the present invention is through the above-mentioned SiC f / Ti3Al composite residual stress control and optimization method can make SiC f The residual stress of the SiC / Ti3Al composite material is effectively reduced, thereby ensuring f The processing and service stability of Ti3Al / Ti3Al composite materials make it suitable for use as a new aerospace material. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0027] Figure 1 The present invention provides SiC f Residual stress control and optimization method of SiC / Ti3Al composites f Flowchart of / Ti3Al composite materials;

[0028] Figure 2 This is a cross-sectional SEM image of the SiC / Ti3Al composite material obtained in Example 1;

[0029] Figure 3 This is a cross-sectional SEM image of the SiC / Ti3Al composite material obtained in Comparative Example 1;

[0030] Figure 4 This is a cross-sectional SEM image of the SiC / Ti3Al composite material obtained in Comparative Example 3;

[0031] Figure 5 Flowchart for detecting residual stress of SiC / Ti3Al composite materials using corrosion method;

[0032] Figure 6 3 is a comparison diagram of the matrix axial residual stress of the SiC / Ti3Al composite materials obtained in Examples 1 to 3 and Comparative Examples 1 to 3 measured by corrosion method and X-ray diffraction method. DETAILED DESCRIPTION

[0033] The present invention provides a SiC f The method for regulating and optimizing residual stress of a Ti3Al composite material comprises the following steps:

[0034] (1) ion cleaning the carbon-coated SiC fiber under argon conditions to obtain pretreated SiC fiber;

[0035] (2) using Mo as a sputtering target, magnetron sputtering the pretreated SiC fiber under argon conditions to obtain a SiC fiber with a Mo interface stress release layer deposited;

[0036] (3) Using Ti3Al alloy and Ti2AlNb alloy as sputtering targets, magnetron sputtering is performed on the SiC fiber deposited with the Mo interface stress release layer under argon conditions, and Ti3Al matrix layer and Ti2AlNb matrix stress release layer are alternately deposited on the surface of the SiC fiber deposited with the Mo interface stress release layer to obtain SiC f / Ti3Al composite precursor wire;

[0037] (4) The precursor wires are evenly arranged and hot isostatically pressed to obtain SiC with controlled and optimized residual stress. f / Ti3Al composite materials.

[0038] In the present invention, unless otherwise specified, all raw materials are commercially available products well known to those skilled in the art.

[0039] The present invention performs ion cleaning on SiC fibers containing a carbon coating under argon conditions to obtain pretreated SiC fibers.

[0040] In the present invention, the diameter of the SiC fiber containing the carbon coating is 90 to 110 μm, and in a specific embodiment, it can be 100 μm; the thickness of the carbon coating can be 2 to 4 μm, and in a specific embodiment, it can be 3 μm; the SiC fiber containing the carbon coating can be a SiC fiber containing a carbon coating and a tungsten core; the diameter of the tungsten core is 14 to 16 μm, and in a specific embodiment, it can be 15 μm.

[0041] In the present invention, the ion cleaning can be performed in the coating chamber of the magnetron sputtering system; the argon gas flow rate of the ion cleaning can be 40 to 70 sccm, and in a specific embodiment, it can be 60 sccm; the ion source voltage can be 600 to 900 V, and in a specific embodiment, it can be 800 V; the sample holder rotation speed can be 1 to 5 r / min, and in a specific embodiment, it can be 3 r / min; the cleaning time can be 10 to 30 min, and in a specific embodiment, it can be 20 min.

[0042] After obtaining the pretreated SiC fiber, the present invention uses Mo as a sputtering target and performs magnetron sputtering on the pretreated SiC fiber under argon conditions to obtain a SiC fiber with a Mo interface stress release layer deposited thereon.

[0043] In the present invention, the magnetron sputtering parameters include: the argon flow rate can be 60 to 100 sccm, and in a specific embodiment, it can be 80 sccm; the gas pressure in the coating chamber can be 0.6 to 1.2 Pa, and in a specific embodiment, it can be 0.8 Pa or 1 Pa; the deposition bias can be -50 to -300 V, and in a specific embodiment, it can be -100 V or -200 V; the sputtering current can be 0.9 to 2.5 A, and in a specific embodiment, it can be 1.5 A or 2 A; the sputtering power can be 300 to 600 W, and in a specific embodiment, it can be 400 W or 500 W; the deposition rate can be 0.8 to 2.4 μm / h, and in a specific embodiment, it can be 1 μm / h, 1.5 μm / h or 2 μm / h.

[0044] In the present invention, the thickness of the Mo interface stress release layer may be 0.5 to 3.5 μm, and in a specific embodiment, may be 1 μm, 2 μm or 3 μm.

[0045] After obtaining the SiC fiber deposited with the Mo interface stress release layer, the present invention uses Ti3Al alloy and Ti2AlNb alloy as sputtering targets, performs magnetron sputtering on the SiC fiber deposited with the Mo interface stress release layer under argon conditions, and alternately deposits Ti3Al matrix layers and Ti2AlNb matrix stress release layers on the surface of the SiC fiber deposited with the Mo interface stress release layer to obtain SiC f / Ti3Al composite pioneer wire.

[0046] In the present invention, the magnetron sputtering parameters include: the argon flow rate can be 60 to 100 sccm, and in a specific embodiment, it can be 80 sccm; the gas pressure in the coating chamber can be 0.5 to 1.1 Pa, and in a specific embodiment, it can be 0.8 Pa or 1 Pa; the deposition bias can be -50 to -300 V, and in a specific embodiment, it can be -100 V or -200 V; the sputtering current can be 1.6 to 2.6 A, and in a specific embodiment, it can be 1.8 A or 2 A; the sputtering power can be 600 to 1000 W, and in a specific embodiment, it can be 700 W or 800 W; the deposition rate can be 2 to 4 μm / h, and in a specific embodiment, it can be 3 μm / h or 4 μm / h.

[0047] In the present invention, the repetition period of the alternately deposited Ti3Al matrix layer and the Ti2AlNb matrix stress release layer is ≥3, and in a specific embodiment, it can be 4, 6 or 10; the single layer thickness of the Ti3Al matrix layer is 2 to 4 μm, and in a specific embodiment, it can be 3 μm; the single layer thickness of the Ti2AlNb matrix stress release layer is 0.5 to 4 μm, and in a specific embodiment, it can be 2 μm; the total thickness of the alternately deposited Ti3Al matrix layer and the Ti2AlNb matrix stress release layer is 18 to 38 μm, and in a specific embodiment, it can be 24 μm or 30 μm.

[0048] In the present invention, the SiC f In the precursor yarn of the SiC / Ti3Al composite material, the total thickness of the SiC fiber surface film layer is 20-40 μm, and in a specific embodiment, can be 26 μm or 32 μm.

[0049] The interface stress release layer on the surface of the SiC fiber, the Ti3Al layer and the matrix stress release layer in the present invention will affect the volume percentage of the SiC fiber in the composite material. When preparing the composite material, if the thickness of the interface stress release layer, the Ti3Al layer and the matrix stress release layer on the surface of the SiC fiber is too thin, the gaps between the SiC fibers cannot be completely filled, and there will be many holes in the hot-pressed composite material. If the thickness of the interface stress release layer, the Ti3Al layer and the matrix stress release layer is too thick, the volume percentage of the SiC fiber in the composite material will be too small, affecting the mechanical properties of the composite material. The preparation method of the SiC / Ti3Al precursor wire provided by the present invention can achieve near-net shaping of the precursor wire of the composite material and accurately control the thickness of each layer.

[0050] Obtaining the SiC f After the precursor wire of the / Ti3Al composite material is formed, the precursor wire is evenly arranged and hot isostatic pressing is performed to obtain SiC with controlled and optimized residual stress. f / Ti3Al composite materials.

[0051] In the present invention, the hot pressing further includes cutting and ion beam packaging; the ion beam packaging can be performed in an alloy sleeve; the alloy sleeve is a Ti3Al alloy sleeve.

[0052] In the present invention, the temperature of the hot isostatic pressing can be 930-980°C, and in a specific embodiment, it can be 960°C; the pressure can be 120-200 MPa, and in a specific embodiment, it can be 150 MPa or 180 MPa; the time can be 1-5 hours, and in a specific embodiment, it can be 2 hours or 4 hours.

[0053] The present invention also provides a SiC composite material prepared by the above-mentioned preparation method with controlled and optimized residual stress. f / Ti3Al composite material, composed of SiC f / Ti3Al composite precursor wires are evenly arranged and then formed by hot isostatic pressing; a single SiC f The precursor wire of the Ti3Al / Ti3Al composite material includes SiC fiber, carbon coating, Mo interface stress release layer and alternating Ti3Al matrix layer and Ti2AlNb matrix stress release layer from the inside to the outside.

[0054] The SiC / Ti3Al composite material provided by the present invention has low residual stress, can improve the processing and service stability of the composite material, and thus improve the application potential of the composite material, which is of great significance to the application research of the SiC / Ti3Al composite material.

[0055] The present invention also provides the SiC f / Ti3Al composite materials can be used in the aerospace field.

[0056] In the present invention, the aerospace field includes aerospace engine materials, hypersonic spacecraft materials or aerospace launch vehicle materials; the present invention does not have any special restrictions on the application process of the SiC / Ti3Al precursor wire or SiC / Ti3Al composite material in the aerospace field, and can be applied in a manner familiar to those skilled in the art.

[0057] To further illustrate the present invention, the SiC / Ti3Al precursor wire, composite material, preparation method and application thereof provided by the present invention are described in detail below with reference to the accompanying drawings and examples, but they should not be construed as limiting the scope of protection of the present invention.

[0058] Figure 1 The present invention provides SiC f Residual stress control and optimization method of SiC / Ti3Al composites f Flow chart of the / Ti3Al composite material, and the specific steps are shown in Examples 1 to 3.

[0059] Example 1

[0060] The SiC provided by the present invention f Residual stress control and optimization method of SiC / Ti3Al composites f / Ti3Al composite material, SiC fiber diameter is 100μm, carbon coating thickness is 2μm, Mo coating thickness at the interface is 2μm, Ti2AlNb coating thickness in the matrix is ​​2μm, Ti3Al coating thickness is 2μm, and 6 cycles of co-deposition are performed. The specific steps are as follows:

[0061] (1) Cleaning: After placing the Mo target, Ti3Al target, Ti2AlNb target and SiC fiber in the designated position in the coating chamber of the multi-target magnetron sputtering system, the vacuum degree in the coating chamber is lower than 6×10 -4 Pa, turn on the sample holder rotation switch, the rotation rate is 3r / min, introduce argon gas at a flow rate of 60sccm, and control the pressure in the coating chamber at 0.8 Pa. Turn on the ion source power supply, the initial voltage is about 200V, then reduce the argon gas flow rate to 800V, clean for 20 minutes, turn off the ion source, and complete the cleaning.

[0062] (2) Mo interface layer preparation: The target material used is Mo metal target, and the target surface is clean and pollution-free. The vacuum degree in the coating room is less than 6×10 -4 Pa, maintaining an argon flow rate of 60 sccm, and controlling the gas pressure in the coating chamber to 0.8 Pa. The deposition bias voltage was -100 V. The Mo target was sputtered using a DC power supply with a sputtering current of 1.5 A and a sputtering power of 600 W, depositing a 2 μm Mo coating on the SiC fiber surface.

[0063] (3) Preparation of stress release layer on Ti3Al substrate and Ti2AlNb substrate: The targets used were Ti3Al alloy target and Ti2AlNb alloy target. The two targets were placed at different target positions, and the target surfaces were clean and free of contamination. The argon flow rate was kept constant at 60 sccm, and the gas pressure in the coating chamber was controlled at 0.8 Pa. The deposition bias was kept at -100 V. The DC power supplies of the Ti3Al target and Ti2AlNb target were turned on respectively for target sputtering. During the deposition of the Ti3Al layer, the sputtering current was 1.9 A and the sputtering power was 700 W; during the deposition of the Ti2AlNb layer, the sputtering current was 2 A and the sputtering power was 750 W. The sample holder speed was controlled at 3 r / min, and a 2 μm thick Ti3Al layer and a 2 μm thick Ti2AlNb layer were alternately deposited on the surface of the SiC fiber. The thickness ratio of the Ti3Al layer to the Ti2AlNb layer was 1:1. The alternating deposition was repeated for 6 cycles to obtain a precursor wire with an interface stress release layer and a matrix stress release layer.

[0064] (4) Preparation of composite materials: The cut precursor wires are arranged tightly and evenly, placed in a Ti3Al alloy sleeve for ion beam packaging, and then the prefabricated sample is hot isostatically pressed at 960℃ / 150MPa for 2h and then formed. After the hot isostatic pressing is completed, the sample is cooled to room temperature in the furnace to obtain SiC f / C / Mo / (Ti3Al / Ti2AlNb)6 composite material.

[0065] Figure 2The cross-sectional SEM image of the SiC / Ti3Al composite material obtained in this embodiment is shown in FIG. Figure 2 It can be seen that the present embodiment successfully prepared a SiC / Ti3Al composite material having a Mo interface stress release layer and a Ti2AlNb matrix stress release layer.

[0066] Example 2

[0067] The SiC provided by the present invention f Residual stress control and optimization method of SiC / Ti3Al composites f / Ti3Al composite material, SiC fiber diameter is 100μm, carbon coating thickness is 2μm, Mo coating thickness at the interface is 2μm, Ti2AlNb coating thickness in the matrix is ​​2μm, Ti3Al coating thickness is 4μm, and co-deposition is performed for 4 cycles. The specific steps are as follows:

[0068] (1) Cleaning: After placing the Mo target, Ti3Al target, Ti2AlNb target and SiC fiber in the designated position in the coating chamber of the multi-target magnetron sputtering system, the vacuum degree in the coating chamber is lower than 6×10 -4 Pa, turn on the sample holder rotation switch, the rotation rate is 3r / min, introduce argon gas at a flow rate of 60sccm, and control the pressure in the coating chamber at 0.8 Pa. Turn on the ion source power supply, the initial voltage is about 200V, then reduce the argon gas flow rate to 800V, clean for 20 minutes, turn off the ion source, and complete the cleaning.

[0069] (2) Mo interface layer preparation: The target material used is Mo metal target, and the target surface is clean and pollution-free. The vacuum degree in the coating room is less than 6×10 -4 Pa, maintaining an argon flow rate of 60 sccm, and controlling the gas pressure in the coating chamber to 0.8 Pa. The deposition bias voltage was -100 V. The Mo target was sputtered using a DC power supply with a sputtering current of 1.5 A and a sputtering power of 600 W, depositing a 2 μm Mo coating on the SiC fiber surface.

[0070] (3) Preparation of stress release layer on Ti3Al substrate and Ti2AlNb substrate: The targets used were Ti3Al alloy target and Ti2AlNb alloy target. The two targets were placed at different target positions, and the target surfaces were clean and free of contamination. The argon flow rate was kept constant at 60 sccm, and the gas pressure in the coating chamber was controlled at 0.8 Pa. The deposition bias was kept at -100 V. The DC power supplies of the Ti3Al target and Ti2AlNb target were turned on respectively for target sputtering. During the deposition of the Ti3Al layer, the sputtering current was 1.9 A and the sputtering power was 700 W; during the deposition of the Ti2AlNb layer, the sputtering current was 2 A and the sputtering power was 750 W. The sample holder speed was controlled at 3 r / min, and a 4 μm thick Ti3Al layer and a 2 μm thick Ti2AlNb layer were alternately deposited on the surface of the SiC fiber. The thickness ratio of the Ti3Al layer to the Ti2AlNb layer was 2:1. The alternating deposition was repeated for 4 cycles to obtain a precursor wire with an interface stress release layer and a matrix stress release layer.

[0071] (4) Preparation of composite materials: The cut precursor wires are arranged tightly and evenly, placed in a Ti3Al alloy sleeve for ion beam packaging, and then the prefabricated sample is hot isostatically pressed at 960℃ / 150MPa for 2h and then formed. After the hot isostatic pressing is completed, the sample is cooled to room temperature in the furnace to obtain SiC f / C / Mo / (Ti3Al / Ti2AlNb)4 composite material.

[0072] Example 3

[0073] The SiC provided by the present invention f Residual stress control and optimization method of SiC / Ti3Al composites f / Ti3Al composite material, SiC fiber diameter is 100μm, carbon coating thickness is 2μm, Mo coating thickness at the interface is 2μm, Ti2AlNb coating thickness in the matrix is ​​2μm, Ti3Al coating thickness is 6μm, and co-deposition is performed for 3 cycles. The specific steps are as follows:

[0074] (1) Cleaning: After placing the Mo target, Ti3Al target, Ti2AlNb target and SiC fiber in the designated position in the coating chamber of the multi-target magnetron sputtering system, the vacuum degree in the coating chamber is lower than 6×10 -4 Pa, turn on the sample holder rotation switch, the rotation rate is 3r / min, introduce argon gas at a flow rate of 60sccm, and control the pressure in the coating chamber at 0.8 Pa. Turn on the ion source power supply, the initial voltage is about 200V, then reduce the argon gas flow rate to 800V, clean for 20 minutes, turn off the ion source, and complete the cleaning.

[0075] (2) Mo interface layer preparation: The target material used is Mo metal target, and the target surface is clean and pollution-free. The vacuum degree in the coating room is less than 6×10 -4 Pa, maintaining an argon flow rate of 60 sccm, and controlling the gas pressure in the coating chamber to 0.8 Pa. The deposition bias voltage was -100 V. The Mo target was sputtered using a DC power supply with a sputtering current of 1.5 A and a sputtering power of 600 W, depositing a 2 μm Mo coating on the SiC fiber surface.

[0076] (3) Preparation of stress release layer on Ti3Al substrate and Ti2AlNb substrate: The targets used were Ti3Al alloy target and Ti2AlNb alloy target. The two targets were placed at different target positions, and the target surfaces were clean and free of contamination. The argon flow rate was kept constant at 60 sccm, and the gas pressure in the coating chamber was controlled at 0.8 Pa. The deposition bias was kept at -100 V. The DC power supplies of the Ti3Al target and Ti2AlNb target were turned on respectively for target sputtering. During the deposition of the Ti3Al layer, the sputtering current was 1.9 A and the sputtering power was 700 W; during the deposition of the Ti2AlNb layer, the sputtering current was 2 A and the sputtering power was 750 W. The sample holder speed was controlled at 3 r / min, and a 6 μm thick Ti3Al layer and a 2 μm thick Ti2AlNb layer were alternately deposited on the surface of the SiC fiber. The thickness ratio of the Ti3Al layer to the Ti2AlNb layer was 3:1. The alternating deposition was repeated for 3 cycles to obtain a precursor wire with an interface stress release layer and a matrix stress release layer.

[0077] (4) Preparation of composite materials: The cut precursor wires are arranged tightly and evenly, placed in a Ti3Al alloy sleeve for ion beam packaging, and then the prefabricated sample is hot isostatically pressed at 960℃ / 150MPa for 2h and then formed. After the hot isostatic pressing is completed, the sample is cooled to room temperature in the furnace to obtain SiC f / C / Mo / (Ti3Al / Ti2AlNb)3 composite material.

[0078] Comparative Example 1

[0079] In this comparative example, there is no interface stress release layer and substrate stress release layer, and the thickness of the Ti3Al layer is 24 μm. The specific preparation steps are as follows:

[0080] (1) Cleaning: After placing the Mo target, Ti3Al target, Ti2AlNb target and SiC fiber in the designated position in the coating chamber of the multi-target magnetron sputtering system, the vacuum degree in the coating chamber is lower than 6×10 -4Pa, turn on the sample holder rotation switch, the rotation rate is 3r / min, introduce argon gas at a flow rate of 60sccm, and control the pressure in the coating chamber at 0.8 Pa. Turn on the ion source power supply, the initial voltage is about 200V, then reduce the argon gas flow rate to 800V, clean for 20 minutes, turn off the ion source, and complete the cleaning.

[0081] (2) Preparation of precursor wire: The target material used is Ti3Al alloy target material, and the target surface is clean and pollution-free. The argon flow rate is kept constant at 60sccm, and the gas pressure in the coating chamber is controlled at 0.8Pa. The deposition bias voltage is -100V. Turn on the DC power supply of the Ti3Al target to sputter the target, the sputtering current is 1.9A, the sputtering power is 700W, and the sample holder speed is controlled at 3r / min. A 24μm thick Ti3Al coating is alternately deposited on the surface of the SiC fiber to obtain SiC f / Ti3Al composites.

[0082] (3) Preparation of composite materials: The cut precursor wires are arranged tightly and evenly, placed in a Ti3Al alloy sleeve for ion beam packaging, and then the prefabricated sample is hot isostatically pressed at 960℃ / 150MPa for 2h to form. After the hot isostatic pressing is completed, the sample is cooled to room temperature in the furnace to obtain SiC f / C / Ti3Al composite materials.

[0083] Figure 3 The cross-sectional SEM image of the SiC / Ti3Al composite material obtained in this embodiment is shown in FIG. Figure 3 It can be seen that the comparative example prepared a SiC / Ti3Al composite material that contains neither a Mo interface stress release layer nor a Ti2AlNb matrix stress release layer.

[0084] Comparative Example 2

[0085] In this comparative example, the interface stress release layer is a Cr layer with a thickness of 2 μm, there is no substrate stress release layer, and the thickness of the Ti3Al layer is 24 μm. The specific preparation steps are as follows:

[0086] (1) Cleaning: After placing the Cr target, Ti3Al target, Ti2AlNb target and SiC fiber in the designated position in the coating chamber of the multi-target magnetron sputtering system, the vacuum degree in the coating chamber is lower than 6×10 -4 Pa, turn on the sample holder rotation switch, the rotation rate is 3r / min, introduce argon gas at a flow rate of 60sccm, and control the pressure in the coating chamber at 0.8 Pa. Turn on the ion source power supply, the initial voltage is about 200V, then reduce the argon gas flow rate to 800V, clean for 20 minutes, turn off the ion source, and complete the cleaning.

[0087] (2) Preparation of Cr interface layer: The target material used is Cr metal target, and the target surface is clean and pollution-free. The vacuum degree in the coating room is less than 6×10 -4 Pa, maintaining an argon flow rate of 60 sccm, and regulating the gas pressure in the coating chamber to 0.8 Pa. The deposition bias voltage was -100 V. The DC power supply to the Cr target was turned on for sputtering at a sputtering current of 1.5 A and a sputtering power of 600 W, depositing a 2 μm thick Cr coating on the SiC fiber surface.

[0088] (3) Preparation of precursor wire: The target material used is Ti3Al alloy target material, and the target surface is clean and pollution-free. The argon flow rate is kept constant at 60sccm, and the gas pressure in the coating chamber is controlled at 0.8Pa. The deposition bias is kept at -100V. Turn on the DC power supply of the Ti3Al target to sputter the target, the sputtering current is 1.9A, the sputtering power is 700W, and the sample holder speed is controlled at 3r / min. A 24μm thick Ti3Al coating is alternately deposited on the surface of the SiC fiber to obtain SiC f / Ti3Al composites.

[0089] (4) Preparation of composite materials: The cut precursor wires are arranged tightly and evenly, placed in a Ti3Al alloy sleeve for ion beam packaging, and then the prefabricated sample is hot isostatically pressed at 960℃ / 150MPa for 2h and then formed. After the hot isostatic pressing is completed, the sample is cooled to room temperature in the furnace to obtain SiC f / C / Cr / Ti3Al composite material.

[0090] Comparative Example 3

[0091] In this comparative example, there is no substrate stress release layer, and the thickness of the Ti3Al layer is 24 μm. The specific preparation steps are as follows:

[0092] (1) Cleaning: After placing the Mo target, Ti3Al target, Ti2AlNb target and SiC fiber in the designated position in the coating chamber of the multi-target magnetron sputtering system, the vacuum degree in the coating chamber is lower than 6×10 -4 Pa, turn on the sample holder rotation switch, the rotation rate is 3r / min, introduce argon gas at a flow rate of 60sccm, and control the pressure in the coating chamber at 0.8 Pa. Turn on the ion source power supply, the initial voltage is about 200V, then reduce the argon gas flow rate to 800V, clean for 20 minutes, turn off the ion source, and complete the cleaning.

[0093] (2) Mo interface layer preparation: The target material used is Mo metal target, and the target surface is clean and pollution-free. The vacuum degree in the coating room is less than 6×10 -4Pa, maintaining an argon flow rate of 60 sccm, and controlling the gas pressure in the coating chamber to 0.8 Pa. The deposition bias voltage was -100 V. The Mo target was sputtered using a DC power supply with a sputtering current of 1.5 A and a sputtering power of 600 W, depositing a 2 μm Mo coating on the SiC fiber surface.

[0094] (3) Preparation of precursor wire: The target material used is Ti3Al alloy target material, and the target surface is clean and pollution-free. The argon flow rate is kept constant at 60sccm, and the gas pressure in the coating chamber is controlled at 0.8Pa. The deposition bias is kept at -100V. Turn on the DC power supply of the Ti3Al target to sputter the target, the sputtering current is 1.9A, the sputtering power is 700W, and the sample holder speed is controlled at 3r / min. A 24μm thick Ti3Al coating is alternately deposited on the surface of the SiC fiber to obtain SiC f / Ti3Al composites.

[0095] (4) Preparation of composite materials: The cut precursor wires are arranged tightly and evenly, placed in a Ti3Al alloy sleeve for ion beam packaging, and then the prefabricated sample is hot isostatically pressed at 960℃ / 150MPa for 2h and then formed. After the hot isostatic pressing is completed, the sample is cooled to room temperature in the furnace to obtain SiC f / C / Mo / Ti3Al composite materials.

[0096] Figure 4 The cross-sectional SEM image of the SiC / Ti3Al composite material obtained in this embodiment is shown in FIG. Figure 4 It can be seen that the SiC / Ti3Al composite material with a Mo interface stress release layer was prepared in this comparative example.

[0097] Test Example 1

[0098] The residual stress of the SiC / Ti3Al composite matrix of Examples 1 to 3 and Comparative Examples 1 to 3 was tested by corrosion method. The test process is as follows: Figure 5 The specific steps are as follows:

[0099] 1. Slice and polish the SiC / Ti3Al composite material to a thickness of 2 to 3 mm;

[0100] 2. Cut grooves into the polished composite material. The groove depth is determined by the corrosion depth. After cutting grooves, the polished surface of the composite material is laser marked. The selected marking points are located on both sides of the groove.

[0101] 3. Record the fiber height difference near the marking points on both sides;

[0102] 4. Protect one side of the grooved composite material and then perform corrosion treatment on it;

[0103] 5. After the corrosion is completed, record the fiber height difference near the marked points on both sides again;

[0104] 6. The residual stress of the composite material can be calculated using the following formula.

[0105] When the corrosion method is used to analyze the residual stress of the composite material, the corrosion depth of the SiC fiber is set to l, and the fiber growth after corrosion is Δ. Then the axial strain of the fiber is:

[0106]

[0107] The stress of the fiber in the axial direction can be expressed as:

[0108]

[0109] Elastic modulus E of the composite material along the axial direction c Calculated by the law of mixtures:

[0110] E c =V f E f +(1-V f )E m

[0111] The stress of the matrix alloy in the axial direction can be obtained by the following formula:

[0112]

[0113] Where V f is the fiber volume percentage, ν is the fiber Poisson's ratio, E f is the fiber elastic modulus, E m is the matrix elastic modulus.

[0114] The test results of residual stress of SiC / Ti3Al composite matrix by corrosion method are shown in Figure 6 .

[0115] Test Example 2

[0116] The residual stress of the SiC / Ti3Al composite matrix of Examples 1 to 3 and Comparative Examples 1 to 3 was detected by X-ray diffraction. The detection process is as follows: Figure 5 The specific steps are as follows:

[0117] 1. Select the high-angle diffraction peak and Measurements were performed at different ψ angles at three angles: 45° and 90°;

[0118] 2. Calculate separately The interplanar spacing d of the selected crystal planes corresponding to different ψ angles at three angles of 45° and 90°;

[0119] 3. Yes Make a scatter plot and perform linear fitting to obtain Slope at 45° and 90°

[0120] 4. Obtain the intercept of the fitted line after linear fitting And The average value is d(average,ψ=0).

[0121] 5. The residual stress of the composite material can be calculated using the following formula:

[0122]

[0123] The results of X-ray diffraction test on the residual stress of SiC / Ti3Al composite matrix are shown in Figure 6 .

[0124] Depend on Figure 6 It can be seen that the SiC / Ti3Al composite material obtained by using the SiC / Ti3Al precursor wire provided by the present invention can realize residual stress regulation and optimization, effectively reduce residual stress, and the reduction of residual stress can improve the processing and service stability of the composite material, thereby improving the application potential of the composite material. It can be seen that the present invention is of great significance to the application research of SiC / Ti3Al composite materials.

[0125] Although the above embodiment provides a detailed description of the present invention, it is only a part of the embodiments of the present invention, not all of the embodiments. Other embodiments can be obtained based on this embodiment without creativity, and these embodiments all fall within the scope of protection of the present invention.

Claims

1. A SiC f / Ti3Al composite material residual stress control and optimization method, characterized in that, The following steps are involved: (1) ion cleaning the carbon-coated SiC fiber under argon conditions to obtain pretreated SiC fiber; (2) using Mo as a sputtering target, magnetron sputtering the pretreated SiC fiber under argon conditions to obtain a SiC fiber with a Mo interface stress release layer deposited; (3) Using Ti3Al alloy and Ti2AlNb alloy as sputtering targets, magnetron sputtering is performed on the SiC fiber deposited with the Mo interface stress release layer under argon conditions, and Ti3Al matrix layer and Ti2AlNb matrix stress release layer are alternately deposited on the surface of the SiC fiber deposited with the Mo interface stress release layer to obtain SiC f / Ti3Al composite precursor wire; (4) The precursor wires are evenly arranged and hot isostatically pressed to obtain SiC with controlled and optimized residual stress. f / Ti3Al composite materials.

2. The residual stress control and optimization method according to claim 1, characterized in that: The diameter of the SiC fiber containing the carbon coating is 90 to 110 μm, and the thickness of the carbon coating is 2 to 4 μm.

3. The residual stress control and optimization method according to claim 1, characterized in that: The magnetron sputtering parameters in step (2) include: a gas pressure in the coating chamber of 0.6 to 1.2 Pa; an argon flow rate of 60 to 100 sccm; a deposition bias of -50 to -300 V; a sputtering current of 0.9 to 2.5 A; a sputtering power of 300 to 600 W; and a deposition rate of 0.8 to 2.4 μm / h.

4. The residual stress control and optimization method according to claim 1 or 3, characterized in that: The thickness of the Mo interface stress release layer is 0.5 to 3.5 μm.

5. The residual stress control and optimization method according to claim 1, characterized in that: The target magnetron sputtering parameters in step (3) include: argon gas flow rate of 60 to 100 sccm, gas pressure in the coating chamber of 0.5 to 1.1 Pa, deposition bias of -50 to -300 V, sputtering current of 1.6 to 2.4 A, sputtering power of 600 to 800 W, and deposition rate of 2 to 4 μm / h.

6. The residual stress control and optimization method according to claim 1 or 5, characterized in that: The repetition period of the alternate deposition of the Ti3Al matrix layer and the Ti2AlNb matrix stress release layer is ≥3; The single layer thickness of the Ti3Al matrix layer is 2 to 4 μm; the single layer thickness of the Ti2AlNb matrix stress release layer is 0.5 to 4 μm; and the total thickness of the alternately deposited Ti3Al matrix layer and Ti2AlNb matrix stress release layer is 18 to 38 μm.

7. The residual stress control and optimization method according to claim 1, characterized in that: The SiC f In the precursor fibers of the SiC / Ti3Al composite materials, the total thickness of the SiC fiber surface film layer is 20 to 40 μm.

8. The residual stress control and optimization method according to claim 1, characterized in that: The hot isostatic pressing process is performed at a temperature of 930 to 980° C., a pressure of 120 to 200 MPa, and a time of 1 to 5 hours.

9. The SiC after residual stress control and optimization obtained by the residual stress control and optimization method according to any one of claims 1 to 8 f / Ti3Al composite material, characterized in that SiC f / Ti3Al composite precursor wires are evenly arranged and then formed by hot isostatic pressing; a single SiC f The precursor wire of the Ti3Al / Ti3Al composite material includes SiC fiber, carbon coating, Mo interface stress release layer and alternating Ti3Al matrix layer and Ti2AlNb matrix stress release layer from the inside to the outside.

10. The SiC after residual stress control and optimization according to claim 9 f Application of Ti3Al / Ti3Al composite materials in aerospace field.

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