Al2O3 ceramic reinforced metal matrix wear-resistant composite material and preparation method thereof
By using a multi-segment titanium tube constraint system and a precision sintering process, the problems of performance differentiation and dimensional accuracy control of metal matrix composites in high-end equipment have been solved. This has enabled precise positioning of the machinable parts of the material and interface strengthening, thereby improving the overall performance of the material.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- TANGSHAN COLLEGE
- Filing Date
- 2026-01-23
- Publication Date
- 2026-04-10
AI Technical Summary
Existing metal matrix composite material preparation technologies have shortcomings in achieving precise control of material properties and forming of complex components. In particular, they are difficult to meet the requirements of performance differentiation design and dimensional accuracy control in high-end equipment, and there is a problem of insufficient interfacial bonding strength during sintering.
A multi-segment titanium tube constraint system is adopted. By precisely controlling powder loading and segmented sintering, combined with Ti-Al interlayer and special geometric structure design, axial gradient distribution of material properties and interface strengthening are achieved. Vibration loading, bidirectional pressing and pulse pressurization processes are used to ensure precise positioning of machinable parts and improve interface shear strength.
It achieves precise positioning of the processable parts of composite materials and axial gradient distribution of performance indicators, solves the problems of dimensional deviation and insufficient interfacial bonding strength, improves the overall performance of the material, and is suitable for high-end manufacturing fields such as aerospace and energy equipment.
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Figure CN121826427A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of precision preparation technology of metal matrix composites, specifically to an Al2O3 ceramic-reinforced metal matrix wear-resistant composite material and its preparation method. Background Technology
[0002] Metal matrix composites, due to their excellent mechanical properties and wear resistance, have significant application value in high-end manufacturing fields such as aerospace, energy equipment, and precision machinery. Among them, Al2O3 ceramic-reinforced metal matrix composites have become a current research hotspot due to their high hardness, good high-temperature stability, and wear resistance. However, traditional preparation techniques still have significant limitations in achieving precise control of material properties and forming complex components.
[0003] Currently, the mainstream manufacturing process for metal matrix composites mainly adopts the integral sintering technology route. This processing method features high temperature, long-term heating, and heat preservation, enabling metallurgical bonding between Al2O3 ceramics and the metal matrix. Furthermore, this method is simple and widely accepted by many companies. However, it also has significant limitations. At the material design level, integral sintering makes it difficult to achieve differentiated design of machinability for different parts of the component, leading to numerous difficulties in subsequent machining. Due to the high hardness of the ceramic reinforcing phase, abnormal tool wear is easily caused during machining, making it difficult to guarantee machining accuracy, especially for complex components requiring precise local fits. Existing technologies often sacrifice overall material performance for machinability, which clearly cannot meet the stringent material performance requirements of high-end equipment.
[0004] Powder loading control in powder metallurgy is a crucial factor affecting the dimensional accuracy of the final product. Current technologies lack sufficient quantitative research on the relationship between powder loading amount and post-sintering height changes, and precise mathematical models are unavailable. In actual production, the reserved positions for machined parts are mainly estimated based on experience, leading to insufficient dimensional control accuracy (typically with an error range of ±2 mm or more). This uncertainty severely restricts the application of composite materials in precision components, especially in applications requiring strict dimensional fits.
[0005] In the high-temperature fabrication process, the interaction between the material and the container is a critical technical challenge that needs to be addressed. Conventional corundum crucibles are prone to reacting with active metals at high temperatures, introducing impurity phases and affecting material properties. Simultaneously, uneven distribution of thermal stress during sintering can lead to material deformation and cracking; these problems are particularly pronounced in the fabrication of large and complex components.
[0006] Current metal matrix composite material preparation technologies have significant shortcomings in areas such as material property gradient design, dimensional accuracy control, interfacial bonding strengthening, and complex component forming. There is an urgent need to develop new preparation methods and processes to overcome these technological bottlenecks. Especially in high-end applications such as aerospace engine components and precision hydraulic components, even more stringent requirements are placed on material properties, further highlighting the urgency of technological innovation. Therefore, this invention provides an Al2O3 ceramic-reinforced metal matrix wear-resistant composite material and its preparation method. Summary of the Invention
[0007] The technical problem to be solved by this invention is to provide an Al2O3 ceramic-reinforced metal-based wear-resistant composite material and its preparation method. The aim is to achieve precise positioning of the machinable parts of the composite material and continuous gradient control of the axial properties of the composite material.
[0008] The technical solution of the present invention to solve the above-mentioned technical problems is as follows: In a first aspect, there is an Al2O3 ceramic-reinforced metal-based wear-resistant composite material, which is obtained by sintering in a multi-segment titanium tube confinement system, and the composite material sequentially includes a high ceramic content region, a transition region, and a processing region. The high ceramic content region includes the following raw material components: Al2O3, matrix material and foaming agent, wherein the volume ratio of Al2O3 to the matrix material is 30~40:60~70; The transition zone includes the following raw material components: Al2O3 and matrix material; the volume ratio of Al2O3 to matrix material is 10~20:80~90, and the content of Al2O3 in the transition zone gradually decreases towards the processing zone; The processing area includes the base material.
[0009] Based on the above technical solution, the present invention can be further improved as follows.
[0010] Furthermore, the foaming agent comprises phosphate-coated TiH2; the phosphate-coated TiH2 accounts for 1% to 3% of the total weight of the raw materials in the high ceramic content region; The matrix material includes at least one of Cu, Sn, Ti, V, Al, Fe, C, Cr, Mo, and W; The Al2O3 includes submicron-sized Al2O3, micron-sized Al2O3, and millimeter-sized Al2O3; the volume ratio of the submicron-sized Al2O3, the micron-sized Al2O3, and the millimeter-sized Al2O3 is 5~10:10~20:20~80. In the transition zone, the volume content of Al2O3 decreases by 2% to 2.5% every 10 mm in height towards the processing zone.
[0011] Furthermore, a transition layer is provided between the transition zone and the processing zone; The transition layer is made of at least one of Ti-Al composite powder and Fe-Cr composite powder. Specifically, in the Ti-Al composite powder, the weight content of Al is 2% to 10%, with the balance being Ti; in the Fe-Cr composite powder, the weight content of Fe is 70% to 80%, with the balance being Cr.
[0012] Furthermore, the multi-segment titanium tube constraint system includes at least three segments of variable-diameter titanium tubes; a precision-fitting positioning step and a tapered transition area are provided between two adjacent segments of the variable-diameter titanium tubes; the diameter difference between two adjacent segments of the variable-diameter titanium tubes is 2 mm to 5 mm. Each section of the variable-diameter titanium tube has an annular thinning groove on its inner wall; preferably, the annular thinning groove is an annular groove with a processing depth of 0.3 mm to 1 mm and a width of 2 mm to 5 mm.
[0013] Among them, the variable diameter structure design: the diameter difference between adjacent pipe sections is controlled within the range of 2 mm to 5 mm. This gradual structure can effectively alleviate the thermal stress concentration caused by the difference in thermal expansion coefficient.
[0014] Positioning step structure: Precision machined steps with a height of 3 mm to 8 mm are set at the connection of each section, and a transition cone angle of 30 to 45° is used. This design not only provides accurate axial positioning, but also improves the interface shear strength by increasing the contact area.
[0015] Annular thinning groove design: An annular groove with a depth of 0.3 mm to 1 mm and a width of 2 mm to 5 mm is machined at a specific location on the tube wall. This structural innovation has three functions: first, it serves as a stress relief groove to reduce thermal stress during sintering; second, it serves as a visual marker for powder filling height to facilitate process control; and third, it serves as a positioning reference for subsequent machining.
[0016] Secondly, a method for preparing an Al2O3 ceramic-reinforced metal-based wear-resistant composite material includes the following steps: (1) Precision segmented powder filling: A mixture of raw materials from the high ceramic content zone is loaded into the lower layer of a multi-segment titanium tube confinement system using a vibration loading method, so that the relative density reaches 60%~72%; By employing a compositional gradient variation method, the raw materials in the transition zone are loaded into the middle layer of a multi-segment titanium tube confinement system, so that the volume content of Al2O3 decreases by 2%~2.5% every 10 mm of height towards the processing zone; The upper layer of the multi-segment titanium tube constraint system for each raw material in the processing area; A bidirectional pressing method is used to achieve a relative density of 92% to 95%. (2) Segmented sintering: First sintering stage: Heat to 250℃~350℃, fully degas, degrease and remove glue; Second sintering stage: Continue heating to 500℃, and introduce a rotating magnetic field to orient the raw materials; Third sintering stage: continue to raise the temperature to 1000℃~1400℃, and use pulse pressure to promote densification; (3) Segmented cooling.
[0017] A 0.1-0.5 mm thick Ti foil or tantalum foil intermediate layer is added to the interface between each section of the high ceramic content zone, transition zone, and processing zone. Nano-Al2O3 particles (area coverage of 30%-40%) are pre-formed on the foil surface. During sintering, a composite interface of Ti-Al intermetallic compound and ceramic particles is formed, which improves the interfacial shear strength.
[0018] The height of the powder filling in the high ceramic content zone accounts for 14% to 25% of the total powder filling height; The height of the powder filling in the transition zone accounts for 27% to 28% of the total powder filling height; The height of the powder filling in the processing area accounts for 53% to 60% of the total powder filling height.
[0019] Furthermore, the vibration loading method used in step (1) is as follows: the multi-segment titanium tube constraint system is preheated and loaded with vibration in three stages: the first vibration parameters are a frequency of 40Hz~50Hz, an amplitude of 0.45 mm~0.55 mm, a time of 4 min~5 min, and a target relative density of 50%~60%; the second vibration parameters are a frequency of 140Hz~150Hz, an amplitude of 0.15 mm~0.25 mm, a time of 9 min~10 min, and a target relative density of 60%~70%; the third vibration parameters are a frequency of 190Hz~210Hz, an amplitude of 0.1 mm~0.2 mm, a time of 4 min~5 min, and a target relative density of 70%~72%. The bidirectional pressing method in step (1) is as follows: a floating mold structure is adopted, and the pressing parameters are: pre-pressing upper pressure head 100MPa~120MPa, lower ejector rod pressure 45MPa~55MPa, holding time 25 s~35 s; main pressure upper pressure head 380MPa~420MPa, lower ejector rod pressure 290MPa~310MPa, holding time 85 s~95 s; pressure relief upper pressure head step pressure relief, lower ejector rod synchronous pressure reduction, holding time 55 s~65 s.
[0020] Vibration, the segmented sintering in step (2) includes the following specific steps: First sintering stage: Heat to 250℃~350℃ at a rate of 2℃ / min, perform vacuum sintering, hold for 30min~50min, and ensure the exhaust flow rate is <0.1 L / min and the vacuum degree is restored to 5×10⁻⁶. -3 The process of venting, degreasing, and removing adhesive is completed within 1 hour. Second sintering stage: The temperature is increased to 500℃ at a rate of 5℃ / min. A rotating magnetic field is introduced at 350℃ with an initial strength of 0.3T, which increases by 0.1T for every 50℃ increase, so that the raw materials are oriented. The third sintering stage: the temperature is further increased to 1000℃~1400℃ at a rate of 8~10℃ / min, and the holding time is 90 min~150 min. Pulse pressurization is used to promote densification. The parameters of the pulse pressurization method are: base pressure 30MPa, pulse amplitude 15MPa, frequency 10~15 times / min, and duty cycle 0.6.
[0021] Furthermore, step (3) segmented cooling specifically includes: First cooling stage: Cool down to 800℃~1000℃ at a rate of 10~15℃ / min (to avoid quenching cracks); Second cooling stage: Cooling to 600℃~800℃ at a rate of 3~5℃ / min (phase change control); (3) Third cooling stage: furnace cooling to 300℃ before unloading.
[0022] The beneficial effects of this invention are: (1) Precise positioning of machinable parts in composite materials: Traditional manufacturing processes mainly rely on empirical estimation to determine the position of machinable parts, lacking scientific quantitative control methods. Due to the complex shrinkage behavior of metal-ceramic composite materials during sintering, the shrinkage rate of different component regions can vary by 15-20%, resulting in a large deviation between the actual position of the reserved processing area and the design position (usually exceeding ±2 mm). This uncertainty makes it difficult to accurately position the parts during subsequent machining, seriously affecting the assembly accuracy and performance of the components. To address the existing technical problems, this invention establishes a precise mathematical model of powder filling-sintering height (Formula (I)), comprehensively considering multiple factors such as powder characteristics (particle size distribution, loose packing density), sintering parameters (temperature, pressure, time) and constraint conditions (titanium tube stiffness, interface friction), achieving a breakthrough in the position control accuracy of machinable parts to ±0.5 mm, providing technical support for the precision manufacturing of complex components.
[0023] (2) Axial gradient distribution of performance indicators: The composite materials prepared by the existing constant diameter titanium tube constraint process exhibit uniform performance along the axial direction, which cannot meet the differentiated performance requirements of different sections of modern equipment. Taking the turbine blade of an aero-engine as an example, the root part requires high strength and wear resistance, while the tip part requires good impact resistance. In view of the problem of the uniformity of the overall performance of existing composite materials, this invention innovatively adopts a multi-segment variable diameter titanium tube design, and by precisely controlling the ceramic reinforcing phase content, metal matrix composition and sintering process parameters of each segment, it achieves an axial gradient distribution of performance indicators such as material hardness (HRC 20-55), wear resistance (wear rate difference can reach 3 times) and toughness. This performance designability allows a single component to meet the service requirements of different parts at the same time, significantly improving the overall performance of the component.
[0024] (3) Quantification of sintering shrinkage rate and powder loading: Addressing the issue that traditional processes rely on empirical methods to understand powder sintering shrinkage behavior, lacking theoretical guidance; this invention, through systematic research, establishes a system that includes intrinsic material properties (raw material powder loose density)... Theoretical density of composite materials The system employs a precise mathematical model (as shown in Equation (Ⅰ)) for process parameters (densification coefficient η) and thermodynamic factors (thermal expansion coefficient α, temperature change ΔT). This model improves the height prediction accuracy to over 95% by introducing a temperature field-stress field coupling correction factor. In practical applications, for mixed powders with different compositions, the system can automatically calculate the required powder loading height and, combined with a three-dimensional vibration compaction process (frequency 50Hz~200Hz), ensure the uniformity of powder loading density (fluctuation <3%), fundamentally solving the dimensional deviation problem caused by uncertain shrinkage rate.
[0025] (4) Avoiding the problem of insufficient interfacial bonding strength in multi-segment composite materials: In view of the defect of weakened interfacial bonding in existing gradient material preparation technology, test data shows that the interfacial shear strength of traditional layered composite materials is usually no more than 200 MPa, which is only 50%~60% of the matrix strength. However, the present invention adopts three innovative solutions: First, a 0.1 mm~0.5 mm thick Ti foil intermediate layer is added at the inter-segment interface to promote diffusion welding by utilizing the high activity of titanium; Second, a special tube wall geometry is designed (such as a positioning step with a height of 3 mm~8 mm and a cone angle of 30°~45°) to increase the mechanical interlocking effect; Finally, the sintering process is optimized by using stepped heating (heating rate of 5~10℃ / min) and pressure holding (pressure of 20MPa~30 MPa) in the interfacial region. Through these measures, the interfacial shear strength is increased to 280 MPa~320 MPa, reaching more than 85% of the matrix strength, while the interfacial toughness is increased by 40%~50%, effectively solving the problem of interlayer delamination failure.
[0026] (5) By precisely controlling the position of the machinable parts, realizing performance gradient design, quantifying shrinkage behavior and strengthening interface bonding, this invention enables composite materials to better meet the needs of modern equipment to develop towards high performance, lightweight and long life, and provides a brand-new technical path for the development of a new generation of high performance wear-resistant parts, especially with broad application prospects in high-end manufacturing fields such as aerospace and energy equipment. Attached Figure Description
[0027] Figure 1 This is a schematic diagram of the multi-segment titanium tube structure for the turbine blades of an aero-engine according to the present invention; Figure 2 This is a diagram of the interface of the composite material of the present invention. Detailed Implementation
[0028] The principles and features of this invention are described below. The examples given are for illustrative purposes only and are not intended to limit the scope of the invention. Where specific techniques or conditions are not specified in the embodiments, they should be performed according to the techniques or conditions described in the literature in this field, or according to the product instructions. Reagents or instruments whose manufacturers are not specified are all conventional products that can be purchased through legitimate channels.
[0029] This embodiment relates to an Al2O3 ceramic-reinforced metal-based wear-resistant composite material, which is obtained by sintering in a multi-segment titanium tube confinement system. The composite material sequentially includes a high ceramic content region, a transition region, and a processing region. The high ceramic content region includes the following raw material components: Al2O3, matrix material and foaming agent, wherein the volume ratio of Al2O3 to the matrix material is 30~40:60~70; The transition zone includes the following raw material components: Al2O3 and matrix material; the volume ratio of Al2O3 to matrix material is 10~20:80~90, and the content of Al2O3 in the transition zone gradually decreases towards the processing zone; The processing area includes the base material.
[0030] Preferably, the height of the composite material in this embodiment is predicted using the model shown in the following formula (I): (I); In formula (Ⅰ) This refers to the actual height of the composite material after sintering. The loose packing density of the raw material powder; This represents the theoretical density of the composite material. This refers to the initial height at which the raw material powder is loaded. It is the densification coefficient (positively correlated with sintering pressure, with a value of 0.92-0.98). The coefficient of thermal expansion; The temperature difference between the sintering temperature and room temperature is expressed in °C. Titanium tube constraint coefficient; Stress correction factor.
[0031] Since powder sintering is essentially a volume shrinkage process, and the final product height determines the product's processing accuracy, the powder loading control model (Formula (I)) established in the above embodiment is a key technological innovation to ensure dimensional accuracy. Furthermore, the introduction of a correction factor significantly improves the accuracy of sintering height prediction. Among these improvements, the following parameters are added: The constraint coefficient for the titanium tube is (1.05-1.15), taking into account the constraint effect of the tube wall on powder shrinkage; The pressure correction factor (0.98-1.02) reflects the effect of axial pressure on densification; due to the constraint of titanium tube, the actual powder loading height correction value is set to 1.40, and the pressure correction value is set to 0.85~0.98.
[0032] Preferably, the Al2O3 content in the transition zone gradually decreases towards the processing zone; wherein the powder loading in the transition zone is calculated based on height, as shown in formula (II): (II); In formula (II) R is the height (mm) from the bottom of the multi-segment titanium tube constraint system; R is the radius of the titanium tube in the multi-segment titanium tube constraint system. For the layer thickness, e.g., 10 mm; such as 0.0025. The volume percentage decrease per 10 mm of Al2O3 (0.0025) It is 2.5 vol%), and the percentage decreases by 0.2~0.25 vol% per 10 mm.
[0033] The formula for calculating the volume content of Al2O3 in the transition zone is shown in equation (Ⅲ): (III); In formula (Ⅲ) V 陶 The percentage of Al2O3 content per 10 mm of filler volume.
[0034] Preferably, the foaming agent in this embodiment includes phosphate-coated TiH2; the phosphate-coated TiH2 accounts for 1% to 3% of the total weight of the raw materials in the high ceramic content region; by adding phosphate-coated TiH2 as a foaming agent, a controllable pore structure is formed, which ensures both wear resistance and improves thermal shock resistance.
[0035] The method for preparing the phosphate-coated TiH2 foaming agent is as follows: TiH2 powder (particle size 1~3 μm) is immersed in a phosphate ethanol solution (5 vol%) and dried at 60℃ to form a 20~50 nm phosphate coating layer.
[0036] The matrix material includes at least one of Cu, Sn, Ti, V, Al, Fe, C, Cr, Mo, and W; The Al2O3 includes submicron-sized Al2O3 (0.5 μm~1 μm), micron-sized Al2O3 (5 μm~10 μm), and millimeter-sized Al2O3 (1 mm~5 mm); the volume ratio of the submicron-sized Al2O3, the micron-sized Al2O3, and the millimeter-sized Al2O3 is 5~10:10~20:20~80; wherein, the submicron-sized Al2O3 (0.5 μm~1 μm) is used for micron-sized gaps; the micron-sized Al2O3 (5 μm~10 μm) is mainly used for millimeter-sized gaps; and the millimeter-sized Al2O3 (1 mm~5 mm) is used for the framework; In the transition zone, the volume content of Al2O3 decreases by 2% to 2.5% every 10 mm in height towards the processing zone.
[0037] Preferably, in this embodiment, a transition layer is provided between the transition zone and the processing zone; the material of the transition layer is at least one of Ti-Al composite powder and Fe-Cr composite powder. Specifically, in the Ti-Al composite powder, the weight content of Al is 2%~10%, with the balance being Ti; in the Fe-Cr composite powder, the weight content of Fe is 70%~80%, with the balance being Cr.
[0038] The specific process is as follows: After spreading Ti-Al, Fe-Cr and other composite powders to a thickness of 70 μm to 80 μm on the surface of the transition layer, spray ethanol mist at a rate of 0.1 to 0.15 mL / cm. 2 A transition layer is formed by applying light pressure.
[0039] Preferably, the multi-segment titanium tube constraint system of this embodiment includes at least three segments of variable-diameter titanium tubes; a precision-fitting positioning step and a tapered transition area are provided between two adjacent segments of the variable-diameter titanium tubes; the diameter difference between two adjacent segments of the variable-diameter titanium tubes is 2 mm to 5 mm; an annular thinning groove is provided on the inner wall of each segment of the variable-diameter titanium tube; preferably, the annular thinning groove is an annular groove with a processing depth of 0.3 mm to 1 mm and a width of 2 mm to 5 mm.
[0040] Among them, the variable diameter structure design: the diameter difference between adjacent pipe sections is controlled within the range of 2 mm to 5 mm. This gradual structure can effectively alleviate the thermal stress concentration caused by the difference in thermal expansion coefficient.
[0041] Positioning step structure: Precision machined steps with a height of 3 mm to 8 mm are set at the connection of each section, and a transition cone angle of 30 to 45° is used. This design not only provides accurate axial positioning, but also improves the interface shear strength by increasing the contact area.
[0042] Annular thinning groove design: An annular groove with a depth of 0.3 mm to 1 mm and a width of 2 mm to 5 mm is machined at a specific location on the tube wall. This structural innovation has three functions: first, it serves as a stress relief groove to reduce thermal stress during sintering; second, it serves as a visual marker for powder filling height to facilitate process control; and third, it serves as a positioning reference for subsequent machining.
[0043] This embodiment also relates to a method for preparing an Al2O3 ceramic-reinforced metal-based wear-resistant composite material, including the following steps: (1) Precision segmented powder filling: A mixture of raw materials from the high ceramic content zone is loaded into the lower layer of a multi-segment titanium tube confinement system using a vibration loading method, so that the relative density reaches 60%~72%; A compositional gradient approach is used to load the raw materials in the transition zone into the middle layer of a multi-segment titanium tube confinement system, ensuring that the Al2O3 content decreases by 2%~2.5% per 10 mm of height towards the processing zone. For example, a centrifugal powder loading device (300~500 rpm) is used to achieve a natural gradient distribution of the reinforcing phase under centrifugal force, avoiding interface defects caused by artificial stratification. The centrifugation process is protected by argon gas (oxygen content <100 ppm). The upper layer of the multi-segment titanium tube constraint system for each raw material in the processing area; A bidirectional pressing method is used to achieve a relative density of 92% to 95%. (2) Segmented sintering: First sintering stage: Heat to 250℃~350℃, fully degas, degrease and remove glue; Second sintering stage: Continue heating to 500℃, and introduce a rotating magnetic field to orient the raw materials; Third sintering stage: continue to raise the temperature to 1000℃~1400℃, and use pulse pressure to promote densification; (3) Segmented cooling.
[0044] A 0.1 mm to 0.5 mm thick Ti foil or tantalum foil interlayer is added to the interfaces between the high ceramic content zone, the transition zone, and the processing zone. Nano-Al2O3 particles (area coverage of 30 to 40%) are pre-formed on the foil surface. During sintering, a composite interface between Ti-Al intermetallic compounds and ceramic particles is formed, which improves the interfacial shear strength.
[0045] Preferably, in this embodiment, the height of the powder filling in the high ceramic content zone accounts for 14% to 25% of the total powder filling height; The height of the powder filling in the transition zone accounts for 27% to 28% of the total powder filling height; The height of the powder filling in the processing area accounts for 53% to 60% of the total powder filling height.
[0046] Preferably, the vibration loading method used in step (1) of this embodiment is as follows: the multi-segment titanium tube constraint system is preheated, for example, to 80°C, and then vibrated and loaded in three stages: the first vibration parameters are a frequency of 40Hz~50Hz, an amplitude of 0.45 mm~0.55 mm, a time of 4 min~5 min, and a target relative density of 50%~60%; the second vibration parameters are a frequency of 140Hz~150Hz, an amplitude of 0.15 mm~0.25 mm, a time of 9 min~10 min, and a target relative density of 60%~70%; the third vibration parameters are a frequency of 190Hz~210Hz, an amplitude of 0.1 mm~0.2 mm, a time of 4 min~5 min, and a target relative density of 70%~72%. The bidirectional pressing method in step (1) is as follows: a floating mold structure is adopted, and the pressing parameters are: pre-pressing upper pressure head 100MPa~120MPa, lower ejector rod pressure 45MPa~55MPa, holding time 25 s~35 s; main pressure upper pressure head 380MPa~420MPa, lower ejector rod pressure 290MPa~310MPa, holding time 85 s~95 s; pressure relief upper pressure head step pressure relief, lower ejector rod synchronous pressure reduction, holding time 55 s~65 s.
[0047] For example, three-stage temperature control is implemented in the corundum crucible. The assembled multi-segment titanium tubes are placed vertically in the corundum crucible, and a 3 mm thick ZrO2 buffer pad is laid at the bottom of the crucible. The segmented sintering in step (2) includes the following specific steps: First sintering stage: Heat to 250℃~350℃ at a rate of 2℃ / min, perform vacuum sintering, hold for 30min~50min, and ensure the exhaust flow rate is <0.1 L / min and the vacuum degree is restored to 5×10⁻⁶. -3 The process of venting, degreasing, and removing adhesive is completed within 1 hour. Second sintering stage: The temperature is increased to 500℃ at a rate of 5℃ / min. A rotating magnetic field is introduced at 350℃ with an initial strength of 0.3T, which increases by 0.1T for every 50℃ increase, so that the raw materials are oriented. The third sintering stage: the temperature is increased to 1000℃~1400℃ at a rate of 8~10℃ / min, and the holding time is 90 min~150 min. Pulse pressurization is used to promote densification. The pulse pressurization parameters are: base pressure 30MPa, pulse amplitude 15MPa, frequency 10~15 times / min, and duty cycle 0.6.
[0048] Preferably, step (3) of this embodiment, segmented cooling, specifically includes: First cooling stage: Cool down to 800℃~1000℃ at a rate of 10~15℃ / min (to avoid quenching cracks); Second cooling stage: Cooling to 600℃~800℃ at a rate of 3~5℃ / min (phase change control); Third cooling stage: furnace cooling to 300℃ before unloading.
[0049] (3) Upper processable area: Reserved pure metal powder area (height 15 mm-25 mm), using ultra-fine spherical powder and bidirectional pressing process to achieve a relative density of 92%~95%.
[0050] As can be seen, this invention, through precise control of the location of machinable parts, realization of performance gradient design, quantification of shrinkage behavior, and strengthening of interface bonding, enables composite materials to better meet the demands of modern equipment development towards high performance, lightweight, and long service life. It provides a completely new technical path for developing a new generation of high-performance wear-resistant components, and has particularly broad application prospects in high-end manufacturing fields such as aerospace and energy equipment. The following specific embodiments further illustrate this: Example 1: Aero-engine turbine blade.
[0051] The method for manufacturing turbine blades for aero-engines includes the following steps: (1) Multi-segment titanium tube confinement system, such as Figure 1 As shown: Variable diameter structure design: Five-stage variable diameter design (Φ42 / 38 / 35 / 32 / 30 mm), with the diameter changing from the blade root section to the blade tip section; The positioning step height is 3 mm, and the cone angle is 30°. The pipe wall thinning groove is 0.3 mm deep and 2 mm wide.
[0052] (2) Precision control model for powder filling and segmented powder filling gradient control technology: (2-1) Lower layer high ceramic content zone (leaf root segment): ① Raw materials: The matrix composition is Ti-6Al-4V and ceramic particles Al2O3; the mixed powder is Ti-6Al-4V + 30 vol% Al2O3; the powder gradation is 20 wt% 0.5 μm submicron powder + 30 wt% 5 μm micron powder + 50% 1 mm powder. ② TiH2 treatment: 1wt% coated powder (phosphate ethanol treatment), immerse TiH2 powder (particle size 1 μm) in phosphate ethanol solution (5 vol%), dry at 60℃ to form a 20 nm phosphate coating layer; mix at 200 rpm for 30 min in a three-dimensional mixer at a ratio of 1% of the total powder weight.
[0053] ③ Powder filling calculation: according to (I); We can conclude that: The post-sintering height is set to 60 mm, the sintering temperature to 1050℃, and the room temperature and short-rate temperature rise to 100℃. =950℃, we get: ; ; ; Due to the constraint of the titanium tube, the actual powder loading height correction value is set to 1.10, and the pressure correction value is set to 0.84. The actual powder loading height is 92.2 × 1.10 × 0.84 = 85.2 mm; the actual powder loading height is 85.5 mm (including 0.3 mm) as compensation.
[0054] ④ Vibration compaction: For vibration filling, the powder filling mold needs to be preheated to 80℃, and filling should be done in three stages: Stage 1: Frequency 40 Hz, amplitude 0.45 mm, time 4 min, reaching a density of 60%; Stage 2: Frequency 140 Hz, amplitude 0.15 mm, time 9 min, reaching a density of 70%; Stage 3: Frequency 190Hz, amplitude 0.1 mm, time 4 min, reaching a density of 72%; (2-2) Middle transition zone: The middle layer is 40 mm high, and the Al2O3 content per 10 mm is 20 vol% of the volume of the single layer. ① Gradient design: Al2O3 decreases by 2.5 vol% for every 10 mm, with a layer thickness ΔH = 10 mm.
[0055] ② Centrifugal loading of powder; according to formulas (II) and (III), we can obtain: ; ; In practical engineering, a calibration compensation factor of 10 is adopted. ; When x=85.5, the layered powder filling method is shown in Table 1: Table 1 Centrifugal powder loading settings Parameters: Rotation speed 500 rpm, argon protection (O2 < 100 ppm) (2-3) Upper processing zone (blade tip section): ① Reserve a pure metal powder area (15 mm high), spread Ti / Al composite powder to a depth of 70 μm on the surface of the transition zone, and then spray ethanol mist at a rate of 0.1 mL / cm. 2 A transition layer is formed by light pressing; pure Ti-6Al-4V powder (D50=20 μm) is made of ultrafine spherical powder.
[0056] ② Two-way suppression: Pre-compression stage: upper pressure head 100MPa, lower push rod 45MPa, pressure holding for 25 seconds; Main pressure stage: upper pressure head 380MPa, lower push rod 290MPa, pressure holding for 85 seconds.
[0057] The pressure is released in a stepped manner by the upper pressure head, and the pressure is simultaneously reduced by the lower push rod, with a pressure holding time of 55 seconds. The relative density of the powder after pressing reaches 92%.
[0058] (3) Interface strengthening process: Interface reinforcement: 0.1 mm Ti foil (30% coverage of nano-Al2O3).
[0059] (4) Sintering process: ① 300℃ Stage: The assembled multi-segment titanium tubes are vertically placed in an alumina crucible, with a 3 mm thick ZrO2 buffer pad at the bottom; the heating rate is 2℃ / min, and the target temperature is 300℃; vacuum sintering is performed during the sintering process. The holding time is 30 min, and the process continues until the exhaust flow rate reaches 0.08 L / min and the vacuum level recovers to 5×10⁻⁶. -3 At Pa, the heat preservation, degassing, degreasing, and adhesive removal steps at 300℃ are completed.
[0060] ② 500℃ stage: Heating is coupled with magnetic field, and the temperature is increased to 500℃ at a rate of 5℃ / min; when the temperature is 350℃, the rotating magnetic field is started with an initial strength of 0.3T, which increases by 0.1T for every 50℃ increase, and reaches 0.5T when the temperature reaches 500℃.
[0061] ③ Target Temperature Stage: Denseization is promoted by pulse pressurization (10 times / min). The pulse pressurization parameters for the target temperature are: target temperature 1050℃, heating rate 10℃ / min, and holding time 90 min. The pulse pressurization process parameters are: base pressure 30 MPa, pulse amplitude 15 MPa, frequency 12 times / min, and duty cycle 0.6.
[0062] (5) Cooling process: First stage: 10℃ / min → 800℃ (to avoid quenching cracks); Second stage: 5℃ / min → 600℃ (phase change control); Third stage: furnace cooling to 300℃ before unloading.
[0063] The prepared aero-engine turbine blades have a root hardness of HRC53, a tip hardness of HRC35, and an interfacial strength of 318 MPa. Images of their interfacial microstructure are shown below. Figure 2 As shown, the machining allowance position deviation is +0.3 mm.
[0064] Example 2: Hydraulic system plunger sleeve.
[0065] (1) Multi-segment titanium tube confinement system: Variable diameter structure design: three-section variable diameter (Φ50 / 45 / 40 mm); The positioning step height is 8 mm, and the cone angle is 45°. The pipe wall thinning groove is 1 mm deep and 5 mm wide.
[0066] (2) Precision control model for powder filling and segmented powder filling gradient control technology: (2-1) Lower layer with high ceramic content (leaf root segment) ① Raw materials: The matrix composition is Cu-10Sn and ceramic particles Al2O3; the mixed powder is Cu-10Sn + 40 vol% Al2O3. Powder gradation: 20wt% 1μm submicron powder + 20wt% 10μm micron powder + 60wt% 5mm powder; ② TiH2 treatment: 3wt% coated powder (phosphate ethanol treatment), TiH2 powder (particle size 3μm) is immersed in phosphate ethanol solution (5vol%), dried at 60℃ to form a 50nm phosphate coating layer; mixed at 200rpm for 30 min in a three-dimensional mixer at a ratio of 2% of the total powder weight.
[0067] ③ Powder filling calculation: based on (I); We can conclude that: The post-sintering height is set to 40 mm, the sintering temperature to 1000℃, and the room temperature and short-rate temperature rise to 100℃. =900℃, therefore: ; ; ; Due to the constraint of the titanium tube, the actual powder loading height correction value is set to 1.20, and the pressure correction value is set to 0.98. The actual powder loading height is 57.6 × 1.21 × 0.983 = 67.74 mm. The actual powder loading height is 68.5 mm (including 0.8 mm) as compensation.
[0068] ④ Vibration compaction: For vibration filling, the powder filling mold needs to be preheated to 80℃, and filling should be done in three stages: Stage 1: Frequency 50Hz, amplitude 0.55 mm, time 5 min, reaching a density of 50%; Stage 2: Frequency 150Hz, amplitude 0.25 mm, time 10 min, reaching a density of 60%; Stage 3: Frequency 210Hz, amplitude 0.2 mm, time 5 min, reaching a density of 70%; (2-2) Middle layer transition zone: The middle layer height is 35 mm, and the Al2O3 content per 10 mm is 10 vol% of the volume of the single layer.
[0069] ① Gradient design: Al2O3 decreases by 2 vol% for every 10 mm, with a layer thickness ΔH = 10 mm.
[0070] ② Centrifugal powder loading: According to equations (II) and (III), we can obtain: ; ; In practical engineering, a calibration compensation factor of 10 is adopted. When x=68.5, the layered powder filling method is shown in Table 2: Table 2 Centrifugal powder loading settings Parameters: Rotation speed 500 rpm, argon protection (O2 < 100 ppm).
[0071] (2-3) Upper processing zone (blade tip section): ① Reserve a pure metal powder area (25 mm high), spread 80 μm of Ti / Al composite powder on the VV transition zone surface, and then spray 0.15 mL / cm of ethanol mist.2 A transition layer is formed by light pressing. Pure Ti-6Al-4V powder (D50=20μm) is produced using ultrafine spherical powder.
[0072] ② Two-way suppression: Pre-compression stage: upper pressure head 120MPa, lower push rod 55MPa, pressure holding for 35 seconds; Main pressure stage: upper pressure head 420MPa, lower push rod 310MPa, pressure holding for 95 seconds.
[0073] The pressure is released in a stepped manner by the upper pressure head, and the pressure is simultaneously reduced by the lower push rod, with a pressure holding time of 65 seconds. The relative density of the powder after pressing reaches 95%.
[0074] (3) Interface strengthening process: Interface reinforcement: 0.5 mm Ti foil (40% coverage of nano-Al2O3).
[0075] (4) Sintering process: ① 300℃ Stage: The assembled multi-segment titanium tubes are vertically placed in an alumina crucible, with a 3 mm thick ZrO2 buffer pad at the bottom; the heating rate is 2℃ / min, and the target temperature is 300℃; vacuum sintering is performed during the sintering process. The holding time is 50 min, and the process continues until the exhaust flow rate reaches 0.09 L / min and the vacuum degree recovers to 5 × 10⁻⁶. -3 At Pa, the heat preservation, degassing, degreasing, and adhesive removal steps at 300℃ are completed.
[0076] ② 500℃ stage: Heating is coupled with magnetic field, and the temperature is increased to 500℃ at a rate of 5℃ / min; when the temperature is 350℃, the rotating magnetic field is started with an initial strength of 0.3T, which increases by 0.1T for every 50℃ increase, and reaches 0.5T when the temperature reaches 500℃.
[0077] ③ Target Temperature Stage: Denseization is promoted using pulsed pressurization (15 times / min). The pulsed pressurization parameters for the target temperature are: target temperature 1000℃, heating rate 10℃ / min, and holding time 150 min. The pulsed pressurization process parameters are: base pressure 30MPa, pulse amplitude 15MPa, frequency 12 times / min, and duty cycle 0.6.
[0078] (5) Cooling process First stage: 10℃ / min → 800℃ (to avoid quenching cracks); Second stage: 5℃ / min → 600℃ (phase change control); Third stage: furnace cooling to 300℃ before unloading.
[0079] The prepared hydraulic system plunger sleeve has a hardness of HRC55, an interfacial strength of 315MPa, a porosity of 10.8% in the sealing section, and no interlayer defects (ultrasonic testing grade A).
[0080] Example 3: High-speed steel-based ceramic-reinforced wear-resistant cutting tools.
[0081] The preparation method of high-speed steel-based ceramic-reinforced wear-resistant cutting tools includes the following steps: (1) Multi-segment titanium tube confinement system: Variable diameter structure design: three-stage variable diameter (Φ45 / 40 / 35 mm).
[0082] The positioning step height is 6 mm, and the cone angle is 40°. The pipe wall thinning groove is 0.8 mm deep and 5 mm wide.
[0083] (2) Precision control model for powder filling and segmented powder filling gradient control technology: (2-1) Lower layer high ceramic content zone (handle section): ① Raw materials: The matrix composition is M2 high-speed steel powder (Fe-0.8%C-4.2%Cr-5.0%Mo-6.4%W-1.9%V) and ceramic particles Al2O3; Mixed powder: Fe-0.8%C-4.2%Cr-5.0%Mo-6.4%W-1.9%V + 30vol% Al2O3; Powder gradation: 30wt% 1μm submicron powder + 50wt% 8μm micron powder + 20wt% 3mm powder; ② TiH2 treatment: 3wt% coated powder (phosphate ethanol treatment), TiH2 powder (particle size 2.5μm) was immersed in phosphate ethanol solution (5vol%) and dried at 60℃ to form a 50nm phosphate coating layer; at a ratio of 2% of the total powder weight, it was mixed in a three-dimensional mixer at 200rpm for 30 min.
[0084] ③ Powder filling calculation: according to (I); We can conclude that: The post-sintering height is set to 45 mm, the sintering temperature to 1400℃, and the room temperature and short-rate temperature rise to 100℃. =1300℃, we get: ; ; ; Due to the constraint of the titanium tube, the actual powder loading height correction value is set to 1.40, and the pressure correction value is set to 0.98. The actual powder loading height is 60.20 × 1.40 × 0.98 = 82.6 mm. The actual powder loading height is 83.2 mm (including 0.6 mm) with a compensation amount.
[0085] ④ Vibration compaction: For vibration filling, the powder filling mold needs to be preheated to 80℃, and filling should be done in three stages: Stage 1: Frequency 50Hz, amplitude 0.5 mm, time 5 min, reaching a density of 52%; Stage 2: Frequency 150Hz, amplitude 0.2 mm, time 10 min, reaching a density of 65%; Stage 3: Frequency 200Hz, amplitude 0.1 mm, time 5 min, reaching a density of 72%; 2-2) Middle Transition Zone: The middle layer is 40 mm high, and the Al2O3 content per 10 mm is 20 vol of the volume of the single layer.
[0086] ① Gradient design: Al2O3 decreases by 2.5 vol% for every 10 mm, with a layer thickness ΔH = 10 mm.
[0087] ② Centrifugal loading of powder; according to formulas (II) and (III), we can obtain: ; In practical engineering, a calibration compensation factor of 10 is adopted. ; When x=83.2, the layered powder filling method is shown in Table 3: Table 3 Centrifugal powder loading settings Parameters: Rotation speed 300 rpm, argon protection (O2 < 100 ppm).
[0088] (2-3) Upper processing zone (blade tip section): ① Reserve a pure metal powder area (20 mm high), spread Fe-Cr composite powder to a depth of 75 μm on the surface of the transition zone, and then spray 0.13 mL / cm of ethanol mist. 2 A transition layer is formed by light pressing. Pure M2 high-speed steel powder (D50=20μm) is used, employing ultrafine spherical powder.
[0089] ② Two-way suppression: Pre-compression stage: upper pressure head 115MPa, lower push rod 50MPa, pressure holding for 30 seconds; Main pressure stage: upper pressure head 390MPa, lower push rod 300MPa, pressure holding for 90s.
[0090] The pressure is released in a stepped manner by the upper pressure head, and the pressure is simultaneously reduced by the lower push rod, with a pressure holding time of 60 seconds. The relative density of the powder after pressing reaches 93%.
[0091] (3) Interface strengthening process: Interface reinforcement: 0.4 mm tantalum foil (35% coverage of nano Al2O3).
[0092] (4) Sintering process: ① 300℃ Stage: The assembled multi-segment titanium tubes are vertically placed in an alumina crucible, with a 3 mm thick ZrO2 buffer pad at the bottom; the heating rate is 2℃ / min, and the target temperature is 300℃; vacuum sintering is performed during the sintering process. The holding time is 50 min, and the process continues until the exhaust flow rate reaches 0.09 L / min and the vacuum level recovers to 5 × 10⁻⁶. -3 At Pa, the heat preservation, degassing, degreasing, and adhesive removal steps at 300℃ are completed.
[0093] ② 500℃ stage: Heating is coupled with magnetic field, and the temperature is increased to 500℃ at a rate of 5℃ / min; when the temperature is 350℃, the rotating magnetic field is started with an initial strength of 0.3T, which increases by 0.1T for every 50℃ increase, and reaches 0.5T when the temperature reaches 500℃.
[0094] ③ Target Temperature Stage: Denseization is promoted by pulse pressurization (15 times / min). The pulse pressurization parameters for the target temperature are: target temperature 1400℃, heating rate 8℃ / min, and holding time 100 min. The pulse pressurization process parameters are: base pressure 30MPa, pulse amplitude 15MPa, frequency 12 times / min, and duty cycle 0.6.
[0095] (5) Cooling process: First stage: 10℃ / min → 1000℃ (to prevent carbide precipitation); Second stage: 3℃ / min → 800℃ (to avoid martensitic phase transformation); The third stage: the furnace is cooled to 300°C and then unloaded to eliminate thermal stress.
[0096] The prepared high-speed steel-based ceramic-reinforced wear-resistant tools have a cutting life that is 3 times longer and a hardness that can reach 60 HRC.
[0097] Patent publication number CN202010488370.X, entitled "A High-Manganese High-Carbon Weldable Metal-Ceramic Block and Its Reinforced Roller Sleeve and Preparation Method," describes a method for preparing a high-manganese high-carbon weldable metal-ceramic block. This method involves alloying reinforcing particles, then performing liquid-phase sintering of the alloyed reinforcing particles, composite additive particles, and a matrix material. The resulting high-manganese high-carbon weldable metal-ceramic block is welded to a designated position on a roller sleeve, and finally cast into a roller sleeve assembly. However, this method produces reinforced blocks with relatively poor machinability, limiting its application to irregularly shaped or multi-dimensional components, and limiting its applicability to large-scale production and various scenarios. Compared to this patent publication number CN202010488370.X, this invention studies the quantitative relationship between powder loading and post-sintering height changes, providing more accurate control over product dimensional precision and expanding the product's applicability to applications requiring strict dimensional fit.
[0098] Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention. Those skilled in the art can make changes, modifications, substitutions and variations to the above embodiments within the scope of the present invention.
Claims
1. An Al203 ceramic reinforced metal matrix wear resistant composite material, characterized in that, The composite material is obtained by sintering in a multi-stage titanium tube constraint system, and sequentially comprises a high ceramic content zone, a transition zone and a processing zone; The high ceramic content zone comprises raw material components of Al2O3, a matrix material and a foaming agent, and the volume ratio of the Al2O3 and the matrix material is 30-40:60-70; The transition zone comprises raw material components of Al2O3 and a matrix material, and the volume ratio of the Al2O3 and the matrix material is 10-20:80-90, and the content of the Al2O3 gradually decreases in the transition zone towards the processing zone; The processing zone comprises a matrix material.
2. The Al203 ceramic reinforced metal matrix wear resistant composite material according to claim 1, characterized in that, The foaming agent comprises phosphate-coated TiH2, and the phosphate-coated TiH2 accounts for 1-3% of the total weight of the raw materials of the high ceramic content zone; The matrix material comprises at least one of Cu, Sn, Ti, V, Al, Fe, C, Cr, Mo and W; The Al2O3 comprises sub-micron Al2O3, micron Al2O3 and millimeter Al2O3, and the volume ratio of the sub-micron Al2O3, the micron Al2O3 and the millimeter Al2O3 is 5-10:10-20:20-80; The decreasing volume content of the Al2O3 in the transition zone is 2-2.5% per 10 mm height towards the processing zone.
3. The Al203 ceramic reinforced metal matrix wear resistant composite material according to claim 1, characterized in that, A transition layer is arranged between the transition zone and the processing zone; The material of the transition layer is at least one of Ti-Al composite powder and Fe-Cr composite powder.
4. The Al203 ceramic reinforced metal matrix wear resistant composite material according to any one of claims 1 to 3, characterized in that, The multi-stage titanium tube constraint system comprises at least three sections of variable-diameter titanium tubes, and a positioning step and a conical transition zone are arranged between two adjacent sections of the variable-diameter titanium tubes for cooperation; the diameter difference between two adjacent sections of the variable-diameter titanium tubes is 2-5 mm; and an annular thinning groove is arranged on the inner wall of each section of the variable-diameter titanium tube.
5. A method for producing an Al203 ceramic reinforced metal matrix wear resistant composite material according to any one of claims 1 to 4, characterized in that, The method comprises the following steps: (1) Precise segmented powder loading: The mixture of raw materials of the high ceramic content zone is loaded into the lower layer of the multi-stage titanium tube constraint system by using a vibration loading method, so that the relative density is 60-72%; The raw materials of the transition zone are loaded into the middle layer of the multi-stage titanium tube constraint system by using a composition gradient change method, so that the decreasing volume content of the Al2O3 loading is 2-2.5% per 10 mm height towards the processing zone; The raw materials of the processing zone are loaded into the upper layer of the multi-stage titanium tube constraint system, and a bidirectional pressing method is adopted, so that the relative density is 92-95%; (2) Segmented sintering: In the first sintering stage, the temperature is raised to 250-350℃, and sufficient degassing, debinding and degumming are performed; In the second sintering stage, the temperature is continuously raised to 500℃, and a rotating magnetic field is introduced to make the raw materials directional arrangement; In the third sintering stage, the temperature is continuously raised to 1000-1400℃, and a pulse pressurization method is adopted to promote densification; (3) Segmented cooling.
6. The method for preparing an Al2O3 ceramic-reinforced metal-based wear-resistant composite material according to claim 5, characterized in that, The height of the composite material is predicted by the following formula (I) model: (Ⅰ); In formula (I) is the actual height of the composite after sintering; is the apparent density of the raw material powder; is the theoretical density of the composite; is the initial height of the raw material powder; is the densification coefficient; is the thermal expansion coefficient; is the temperature difference between the sintering temperature and room temperature; is the titanium tube constraint coefficient; is the pressure correction factor.
7. The method for preparing an Al2O3 ceramic-reinforced metal-based wear-resistant composite material according to claim 5, characterized in that, The powder loading height of the high ceramic content zone accounts for 14-25% of the total powder loading height; The powder loading height of the transition zone accounts for 27-28% of the total powder loading height; The powder filling height of the processing zone accounts for 53% to 60% of the total powder filling height.
8. The method according to claim 5, wherein the Al2O3 ceramic reinforced metal matrix wear-resistant composite material is prepared by, The vibration filling method used in step (1) is as follows: the multi-section titanium tube restraint system is preheated, and then filled by vibration for three times: the first vibration parameters are frequency of 40-50 Hz, amplitude of 0.45-0.55 mm, time of 4-5 min, and target relative density of 50-60%; the second vibration parameters are frequency of 140-150 Hz, amplitude of 0.15-0.25 mm, time of 9-10 min, and target relative density of 60-70%; and the third vibration parameters are frequency of 190-210 Hz, amplitude of 0.1-0.2 mm, time of 4-5 min, and target relative density of 70-72%. The two-way pressing method in step (1) is as follows: a floating die sleeve structure is used, and the pressing parameters are as follows: pre-pressing upper punch of 100-120 MPa, lower ejector rod pressure of 45-55 MPa, and pressure maintaining time of 25-35 s; main pressing upper punch of 380-420 MPa, lower ejector rod pressure of 290-310 MPa, and pressure maintaining time of 85-95 s; and unloading upper punch of stepwise unloading, lower ejector rod of synchronous pressure reduction, and pressure maintaining time of 55-65 s.
9. The method for preparing an Al2O3 ceramic-reinforced metal-based wear-resistant composite material according to claim 6, characterized in that, The step (2) of segmented sintering includes the following specific steps: The first sintering stage: the temperature is raised to 250-350℃ at a rate of 2℃ / min, vacuum sintering is performed, the holding time is 30-50 min, and when the exhaust flow is <0.1 L / min, the vacuum degree is recovered to 5×10 -3 Pa, the exhaust and degreasing are completed. The second sintering stage: continue to heat at a rate of 5 ℃ / min to 500 ℃, introduce a rotating magnetic field at 350 ℃, the initial strength is 0.3 T, and increase by 0.1 T every 50 ℃, so as to arrange the raw materials in a direction; The third sintering stage: continue to heat at a rate of 8-10 ℃ / min to 1000-1400 ℃, and maintain for 90-150 min, and pulse pressure is used to promote densification; The pulse pressure parameters are as follows: base pressure of 30 MPa, pulse amplitude of 15 MPa, frequency of 10-15 times / min, and duty cycle of 0.
6.
10. The method for preparing an Al2O3 ceramic-reinforced metal-based wear-resistant composite material according to claim 6, characterized in that, The step (3) of segmented cooling specifically includes: The first cooling stage: cool at a rate of 10-15 ℃ / min to 800-1000 ℃; The second cooling stage: cool at a rate of 3-5 ℃ / min to 600-800 ℃; The third cooling stage: furnace cooling to 300 ℃ and then taken out.
Citation Information
Patent Citations
A high-manganese, high-carbon weldable metal-ceramic block, its reinforced roller sleeve, and its preparation method.
CN111621721B