CN110588096A - Continuous metal Mo wireStrong Ti/Al3Ti laminated composite material and preparation method thereof - Google Patents

Continuous metal Mo wireStrong Ti/Al3Ti laminated composite material and preparation method thereof Download PDF

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CN110588096A
CN110588096A CN201910910549.7A CN201910910549A CN110588096A CN 110588096 A CN110588096 A CN 110588096A CN 201910910549 A CN201910910549 A CN 201910910549A CN 110588096 A CN110588096 A CN 110588096A
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composite material
foil
wire
equal
pressure
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姜风春
常云鹏
牛中毅
王振强
果春焕
李秀才
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Harbin Engineering University
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Harbin Engineering University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/16—Drying; Softening; Cleaning
    • B32B38/162—Cleaning
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/16—Drying; Softening; Cleaning
    • B32B38/164—Drying
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04—Interconnection of layers
    • B32B7/10—Interconnection of layers at least one layer having inter-reactive properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • B32B9/04—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B9/041—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material of metal
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
    • C22C47/20—Making alloys containing metallic or non-metallic fibres or filaments by subjecting to pressure and heat an assembly comprising at least one metal layer or sheet and one layer of fibres or filaments
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
    • C22C49/02—Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
    • C22C49/12—Intermetallic matrix material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B2038/0052—Other operations not otherwise provided for
    • B32B2038/0064—Smoothing, polishing, making a glossy surface
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/10—Inorganic fibres
    • B32B2262/103—Metal fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B32B2307/546—Flexural strength; Flexion stiffness
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B32B2307/558—Impact strength, toughness
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/72—Density
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2311/00—Metals, their alloys or their compounds
    • B32B2311/18—Titanium

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  • Materials Engineering (AREA)
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  • Metallurgy (AREA)
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  • Ceramic Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Fluid Mechanics (AREA)
  • Manufacture Of Alloys Or Alloy Compounds (AREA)

Abstract

The invention provides a continuous metal Mo wire reinforced Ti/Al3The Ti layered composite material and the preparation method thereof comprise the following steps: mixing TC4Pretreating the foil, the Al foil and the Mo wire; pre-treated TC4Foil, Al foil and Mo wire according to "TC4‑Al‑Mo‑Al‑TC4"is a unit stack with the outermost layer being TC4A foil; and putting the stacked sample into a vacuum hot-pressing furnace, setting process parameters and sintering. Due to the special laminated structure and the fiber reinforcement effect of the laminated composite material prepared by the invention, the failure analysis result of the composite material shows that: al (Al)3The failure of the Ti substrate is transgranular fracture, the behaviors of debonding and pulling out the metal molybdenum wire and the like, and the toughness of the composite material is obviously improved by the Ti layer of the toughness layer.

Description

Continuous metal Mo wire reinforced Ti/Al3Ti laminated composite material and preparation method thereof
Technical Field
The invention relates to a composite material and a preparation method thereof, in particular to continuous metal Mo wire reinforced Ti/Al3A Ti laminated composite material and its preparing process, which belongs to the field of composite material, includes such technological steps as toughening fibres, reinforcing fibres and special laminated high-energy-absorbing material.
Background
With the rapid development of modern industry and the gradual change of material science and technology, a single metal or alloy cannot meet the requirements of the modern industry on the comprehensive properties of materials, and the requirements of various industries on high-performance composite materials are increasingly urgent. In the aerospace field, which has been rapidly developed in recent years, the requirements for the adopted high-temperature structural materials are stricter and more urgent. For an aviation aircraft, the total weight of the aircraft is reduced, the working temperature of an engine of the aircraft is increased, the thrust-weight ratio of the aircraft can be increased, and fuel consumed by the aircraft can be saved, so that the aircraft has better flight performance. Therefore, the requirements of the aviation material with light weight, high strength, high modulus, high temperature resistance, oxidation resistance and creep resistance make the high temperature nickel-based alloy which is generally applied to the aerospace field originally not well meet the requirements. The disadvantages that superalloys gradually exhibit have shifted their attention to composites, such as ceramic matrix composites, C/C composites, refractory metal silicide based composites, intermetallic compound based composites, and the like. In the research of novel high-temperature materials, intermetallic compound-based composite materials attract great attention.
The intermetallic compound not only has excellent physical and chemical properties, but also has a plurality of excellent properties such as high specific strength, excellent high-temperature mechanical property, oxidation resistance, high creep resistance and the like. Meanwhile, the bonding mode of the intermetallic compound is the characteristic of coexistence of metallic bond and covalent bond. The use temperature of the material can be between that of metal super alloy and ceramic, the material has higher use temperature compared with metal alloy and lower brittleness compared with ceramic, and the material is a novel high-temperature structural material developed in the 90 s of the 20 th century. The advantages of the intermetallic compound make the intermetallic compound have wide application prospect in many industrial fields such as aerospace, transportation, mechanical and chemical engineering and the like.
Despite the advantages of the intermetallic compounds, not all intermetallic compounds can be used as high-temperature structural materials, and only the intermetallic compounds with beryllide, aluminide and silicide meet the requirements of new high-temperature structural materials, and the intermetallic compounds with aluminide are the most well studied. In recent years, a large amount of research has been conducted on intermetallic compounds such as Ti-Al, Fe-Al, and Ni-Al systems at home and abroad.
Among them, the research on more and mature Ti-Al intermetallic compounds has become one of the hot spots in the research on light high temperature structural materials in recent years. The Ti-Al intermetallic compound has the advantages of low density, high specific strength, high specific modulus, high oxidation resistance and the like, so that the Ti-Al intermetallic compound becomes an ideal material for replacing high-temperature nickel-based alloy which is commonly applied to the field of aerospace. TiAl intermetallic compounds are the most studied Ti-Al intermetallic compounds at present. Compared with other intermetallic compounds, the Al with the minimum density, the highest specific strength and the best high-temperature oxidation resistance3Ti people also proceedA great deal of research effort has been devoted to this work. However, the practical application of intermetallic compounds in engineering is limited to a great extent due to the defects of large low-temperature brittleness, poor plasticity, low fracture toughness, low fatigue toughness and the like. In order to overcome the defects, researchers have conducted a great deal of research and study experiments, and the defects of poor room temperature plasticity are overcome by adding alloy elements to perform alloying, thermo-mechanical treatment and the like to obtain fine, uniform and less-segregation alloy structures, but research proves that the method can improve Al to a certain extent3The strength of Ti intermetallic compound improves the fracture toughness, but the problem of large brittleness cannot be effectively solved, so that Al3The wide use of Ti intermetallics is limited. And far from reaching the level of practical application.
Because various materials in the composite material can mutually make up for deficiencies in terms of performance to generate a synergistic effect, the comprehensive performance of the composite material is superior to that of each original composition material, and thus, various different requirements can be met. People think that the problem of poor plasticity of intermetallic compounds is solved by introducing metal with good plasticity and toughness to prepare the layered composite material, namely introducing metal Ti with good mechanical property and preparing the Ti/Al with low density and high strength by utilizing the bionic design of a shell structure in the nature3Ti intermetallic compound based layered composite material. The problem of poor room temperature plastic toughness of the composite material is improved to a great extent.
On the other hand, continuous fibers are receiving general attention because of their excellent properties exhibited by composites for reinforcement. The continuous fiber reinforcement is introduced into the composite material, so that the comprehensive performance of the composite material can be improved to a great extent. The fiber reinforcement with good performance, whether ceramic or metal fiber reinforcement, is used as a main supporting body, so that the composite material has high strength, high toughness and good high-temperature performance at the same time, the unique performance advantages of the continuous fiber reinforced composite material are shown, and the use potential is huge.
Disclosure of Invention
The invention aims to provide a continuous metal Mo wire reinforced Ti/Al wire with simple process, low cost, stable and reliable performance3Ti layered composite material and its preparation method.
The purpose of the invention is realized as follows:
continuous metal Mo wire reinforced Ti/Al3The preparation method of the Ti layered composite material comprises the following steps:
the method comprises the following steps: mixing TC4Pretreating the foil, the Al foil and the Mo wire;
step two: pre-treated TC4Foil, Al foil and Mo wire according to "TC4-Al-Mo-Al-TC4"is a unit stack with the outermost layer being TC4A foil;
step three: and putting the stacked sample into a vacuum hot-pressing furnace, setting process parameters and sintering.
The process parameters are specifically as follows: at 10-3The temperature is raised to 640 ℃ within 100min under the conditions of low vacuum degree of Pa and initial pressure of 3MPa, the temperature is kept for about 20min to ensure that the sample is uniformly heated, and at the moment, although the melting point of Al is not reached, the softening phenomenon of Al can occur, so that the pressure needs to be reduced to prevent the phenomenon that the Al is extruded too much after melting, the pressure is reduced to 2MPa, and the temperature is raised to about 660 ℃ within 20 min. When the temperature reaches the melting point 660 ℃ of Al, the pressure head pressure needs to be stopped, the pressure is gradually changed from 2MPa to 0 at the moment, the pressure is gradually adjusted to 2MPa after heat preservation is carried out for 140min, and heating is stopped after heat preservation is continuously carried out for 40 min.
The invention also includes such features:
the pretreatment specifically comprises the following steps: original TC of sand paper polishing4Edges and surfaces of foils, Al foils and Mo wires; cleaning and polishing TC by using ultrasonic cleaner4Foils, Al foils, and Mo wires; soaking in acetone solution for 10 min; then soaking and cleaning TC by alcohol4The surfaces of the foil, the Al foil and the Mo wire are subjected to drying treatment;
the Al content of the Al foil is more than or equal to 99.6 percent;
the Mo content in the molybdenum wire is more than or equal to 99.93 percent;
continuous metal Mo wire reinforced Ti/Al3The Ti laminated composite material comprises the following chemical components: mo is more than or equal to 99.93 percent, and other elements are less than or equal to 0.07 percent;
the other elements are specifically: fe is less than or equal to 0.30, carbon is less than or equal to 0.10, nitrogen is less than or equal to 0.05, hydrogen is less than or equal to 0.015, oxygen is less than or equal to 0.20, aluminum is 5.5-6.8, vanadium is 3.5-4.5, and the balance is titanium.
The innovation points of the invention are as follows:
(1) the fiber reinforced composite material applied at present does not have the structural and performance characteristics of a layered material, and the continuous Mo wire reinforced Ti/Al prepared by the method3The Ti layered composite material has a special high energy absorption laminated structure and has excellent performance in the aspect of mechanical property.
(2) The invention adopts a vacuum hot-pressing sintering preparation method, which is a low-temperature foil metallurgy technology, can meet the reaction requirement at a lower temperature, saves energy and simultaneously can keep the performance of raw materials;
the invention can conveniently design the structure and the performance of the composite material by changing the thickness of the initial metal foil, the type of the foil, the arrangement sequence and the size of the continuous Mo wire, and optimize the performance of the composite material to prepare the high-performance structure-function integrated composite material.
Compared with the prior art, the invention has the beneficial effects that:
(1) the special technological parameters set by the invention are favorable for generating single-phase matrix Al by reaction3Ti, and other intermetallic compounds of Ti-Al series (such as TiAl and AlTi)3) In contrast, Al3Ti has higher elastic modulus (215GPa) and lower density (3.3 g/cm)3) Therefore, the continuous Mo reinforced laminated composite material has the mechanical properties of low density, high strength, high modulus and the like.
(2) Due to the special laminated structure and the fiber reinforcement effect of the laminated composite material prepared by the invention, the failure analysis result of the composite material shows that: al (Al)3The failure of the Ti matrix is transgranular fracture, the behaviors of debonding, pulling out and the like of the metal molybdenum wire and the toughness of the composite material improved obviously by the Ti layer of the toughness layer.
(3) The continuous Mo wire prepared by the invention strengthens Ti/Al3The interface of the Ti layered composite material layer and the fiber interface form a defect-free and high-quality interface combination through metallurgical combination, and the tough metal Ti has a toughening effectWhile the addition of continuous Mo wire makes Mo-Ti/Al3The tensile strength and the bending strength of the Ti composite material are greatly improved.
(4) The invention uses commercial metal foils (TC4 foil and aluminum foil) with wide sources, and the composite material has low temperature, no toxicity, energy saving and environmental protection in the preparation process, simple and easy process, low cost and stable and reliable performance.
Drawings
FIG. 1 is a flow diagram of composite material preparation;
FIG. 2 is a schematic view of the arrangement of metal foils; according to "TC4-Al-Mo-Al-TC4"is a unit stack with the outermost layer being TC4A foil;
FIGS. 3a-b are continuous Mo filaments and Al filaments in example 13Scanning electron microscope photos of Ti matrix interface;
FIG. 4 shows the continuous Mo wire and Al wire in example 23Metallographic pictures of Ti matrix interface;
FIGS. 5a-b are continuous Mo filaments and Al filaments in example 33And (5) scanning electron microscope pictures of Ti matrix interfaces.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
The method successfully prepares the Mo-Ti/Al by introducing the Ti layer as the toughness layer, adding the high-performance continuous metal molybdenum wire and adopting a vacuum hot-pressing sintering mode3A Ti layered composite material.
The invention adopts the following technical scheme: vacuum hot-pressing method for preparing continuous metal Mo wire reinforced Ti/Al3A Ti layered composite material. The raw material used by the method is TC4 titanium alloy, and the alloy comprises the following chemical components: the balance of titanium (Ti), iron (Fe) is less than or equal to 0.30, carbon (C) is less than or equal to 0.10, nitrogen (N) is less than or equal to 0.05, hydrogen (H) is less than or equal to 0.015, oxygen (O) is less than or equal to 0.20, aluminum (Al) is 5.5-6.8, and vanadium (V) is 3.5-4.5; the Al foil is 1060 industrial pure aluminum, and the Al content is more than or equal to 99.6 percent; the molybdenum fiber adopts molybdenum wire with the mark of MO1, the element content Mo in the molybdenum fiber is more than or equal to 99.93 percent, and other elements are less than or equal to 0.07 percent. There are no other added elements.
The preparation method of the invention comprises the following steps:
using metallographic sandThe paper is prepared by polishing original foil and fiber, removing oxidation layer, cleaning foil and fiber with ultrasonic cleaner for 15-20min, soaking in acetone solution for 10min, and cleaning metal foil and fiber surface with alcohol. In order to prevent the surface of the foil from being oxidized and polluted again, the surface of the foil is dried by a blower, the foil is put into a vacuum drying box for drying, and the foil is taken out after being dried completely and is wrapped by a preservative film for later use. After drying treatment according to "TC4-Al-Mo-Al-TC4"is a unit stack (see figure 2), with the outermost layer being TC4A foil. The whole stacked sample is put into a vacuum hot pressing furnace for sintering, and the flow chart is shown in attached figure 1.
The main technological parameters are as follows: at 10-3The temperature is raised to 640 ℃ within 100min under the conditions of low vacuum degree of Pa and initial pressure of 3MPa, the temperature is kept for about 20min to ensure that the sample is uniformly heated, and at the moment, although the melting point of Al is not reached, the softening phenomenon of Al can occur, so that the pressure needs to be reduced to prevent the phenomenon that the Al is extruded too much after melting, the pressure is reduced to 2MPa, and the temperature is raised to about 660 ℃ within 20 min. When the temperature reaches the melting point 660 ℃ of Al, the pressure head pressure needs to be stopped, the pressure is gradually changed from 2MPa to 0 at the moment, the pressure is gradually adjusted to 2MPa after heat preservation is carried out for 140min, and heating is stopped after heat preservation is continuously carried out for 40 min.
The technical solutions of the present invention are described in detail by the following specific examples, it should be understood that these examples are for illustrating the present invention, but not limiting the present invention, and the present invention is simply modified on the premise of the concept of the present invention, and all of them fall into the scope of the claimed invention.
Example 1
Cutting TC4 foil and Al foil into square foils with the size of 100mm multiplied by 100mm, cutting metal Mo wire fibers into fibers with the length of 10mm, polishing the original foils and fibers by using metallographic abrasive paper, removing an oxidation layer, cleaning the foils and the fibers by using an ultrasonic cleaner (the time is 15-20min), taking out the foils and the fibers, soaking the foils and the fibers in acetone solution for 10min, and cleaning the surfaces of the metal foils and the fibers by using alcohol. Drying the foil surface with blower in vacuum drying oven until the foil surface is oxidized and polluted againAfter being completely dried, the mixture is taken out and wrapped by a preservative film for standby. After drying treatment according to "TC4-Al-Mo-Al-TC4"is a unit stack with the outermost layer being TC4A foil.
Putting the arranged metal foil blanks into a vacuum hot-pressing furnace, and preparing the composite material: at 10-3The temperature is raised to 640 ℃ within 100min under the conditions of low vacuum degree of Pa and initial pressure of 3MPa, the temperature is kept for about 20min to ensure that the sample is uniformly heated, and at the moment, although the melting point of Al is not reached, the softening phenomenon of Al can occur, so that the pressure needs to be reduced to prevent the phenomenon that the Al is extruded too much after melting, the pressure is reduced to 2MPa, and the temperature is raised to about 660 ℃ within 20 min. When the temperature reaches the melting point of Al of 660 ℃, the pressure of the pressure head needs to be stopped, the pressure is gradually changed from 2MPa to 0 at the moment, the heating is stopped after the temperature is kept for 2h, and the pressure is gradually adjusted to 2 MPa.
The continuous Mo wire obtained in this example strengthens Ti/Al3Scanning electron micrographs (figure 3) of Mo wires of the Ti layered composite material and a matrix show that the laminated layers are arranged neatly, the interfaces between the laminated layers are free of defects and are well combined, and metal fibers are uniformly arranged in the laminated layers and are well combined with the interfaces of the matrix. The middle gray black part is an unreacted Al layer, the original white area in the Al layer is a metal molybdenum wire, and the gray irregular original area around the molybdenum wire is a reaction product. The energy spectrum analysis and XRD analysis show that the composite material has several phase compositions, and the main phases include Mo, Ti, Al and Al3Ti、Al3Ti0.8V0.2、Al12Mo and Al3+ xMo1-x. Wherein the reaction layer capable of being marked obviously is Al12Mo phase, and Al3+xMo1-xIs another reaction product of Al-Mo.
The layered composite material Mo-Ti/Al prepared at this time3Ti, only a small amount of intermetallic compound Al is generated due to too short heat preservation time3Ti, and a large amount of unreacted Al is present. Therefore, this production method has not achieved Mo-Ti/Al production3And (5) Ti requirement. Therefore, improving the technological parameters of sintering preparation is the key of successful preparation.
Example 2
The pretreatment method of the raw materials is the same as that of the example 1, and the used process parameters are as follows: at 10-3The temperature is raised to 640 ℃ within 100min under the conditions of low vacuum degree of Pa and initial pressure of 3MPa, the temperature is kept for about 20min to ensure that the sample is uniformly heated, the softening phenomenon of Al can occur although the melting point of Al is not reached, so the pressure needs to be reduced to prevent the phenomenon that Al is extruded too much after melting, the pressure is reduced to 2MPa, the temperature is raised to about 680 ℃ within 20min, the pressure is gradually changed from 2MPa to 0, the pressure is gradually adjusted to 2MPa after the temperature is kept for 140min, and the heating is stopped after the temperature is kept for 40 min.
The continuous Mo wire obtained in this example strengthens Ti/Al3As can be seen from the metallographic photograph (figure 4) of the Mo wire and the matrix of the Ti layered composite material, Al can be completely generated after long-time reaction3Ti intermetallic compound, but because the reaction temperature is higher and the holding time is too long, the added metal molybdenum wire is completely reacted. The wire was fully reacted leaving a spindle-shaped white reaction zone. Due to the complete reaction of the high-performance metal molybdenum wire, the fiber reinforced Ti/Al3The purpose of Ti is contrary. Thus, such preparation process parameters do not compound the fiber reinforcement requirements.
For the Mo-Ti/Al prepared under the experimental conditions3XRD analysis of the Ti layered composite material shows that the composite material contains more phase components, and the main phases comprise Ti, Al and Al3Ti、Al3Ti0.8V0.2、Al12Mo、Al5Mo and Al3+xMo1-xAnd (4) phase(s). As is clear from comparison with example 1, the added phase in example 2 is Al5Mo, and the disappeared phase is a Mo phase. It was further confirmed by XRD scanning that the metallic Mo had reacted to completion.
Example 3
The pretreatment method of the raw materials is the same as that of the example 1, and the used process parameters are as follows: at 10-3Heating to 640 ℃ within 100min under the conditions of low vacuum degree of Pa and initial pressure of 3MPa, and keeping the temperature for about 20min to ensure that the sample is uniformly heated, wherein the softening of Al can occur at the moment although the melting point of Al is not reached at the momentLike this, it is therefore necessary to reduce the pressure to prevent the phenomenon of excessive extrusion of Al after melting, reduce the pressure to 2MPa and raise the temperature to around 660 ℃ within 20 min. When the temperature reaches the melting point 660 ℃ of Al, the pressure head pressure needs to be stopped, the pressure is gradually changed from 2MPa to 0 at the moment, the pressure is gradually adjusted to 2MPa after heat preservation is carried out for 140min, and heating is stopped after heat preservation is continuously carried out for 40 min.
The continuous Mo wire obtained in this example strengthens Ti/Al3The scanning electron micrograph (figure 5) of Mo wires and matrix of the Ti layered composite material shows that the whole is clean and tidy, the thicknesses of all phase layers are uniform, and the metal fiber molybdenum wires are uniformly arranged on Al3And at the middle position of the Ti layer, the interfaces are well combined, and no obvious interface defect exists at the interfaces. The interface of the amplified microscopic region has no obvious defects, which indicates that the composite material prepared by the hot-pressing sintering method is feasible. XRD analysis shows that the composite material obtained under the experimental conditions has 6 main phase compositions, namely Al, Ti, Mo and Al3Ti、Al3Ti0.8V0.2And Al3+ xMo1-xAnd (4) phase(s). Al (Al)3Ti0.8V0.2A solid solution in which Ti atoms are substituted for V atoms. Al (Al)3+xMo1-xThe phases are various Al-Mo compounds. Namely three reaction layer phases, and the combination of EDS analysis shows that the three reaction layer phases are Al8Mo3、Al5Mo、Al12Mo。
From a comparison of example 1, example 2 and example 3, it can be seen that different sintering temperatures and sintering times have different effects on the microstructure of the composite material. By the para-Mo-Ti/Al3The exploration of the preparation process of the Ti layered composite material can finally determine the optimized preparation process.
A continuous Mo wire reinforced intermetallic compound based layered composite material Ti/Al3A Ti preparation method. By utilizing the arrangement mode and the special overlapping structure of the fibers, the Ti layer is introduced as the toughness layer, and simultaneously, the high-performance continuous metal molybdenum wire is added, so that the Ti/Al is improved3The plasticity of the Ti laminated composite material is improved, and the strength is improved; the processing temperature is low in the preparation process of the composite material. EDS analysis shows that molybdenum only exists in metal Mo wire and molybdenum thereofThe reaction layer of the substrate does not diffuse into the substrate Al3In Ti. The combination condition of each interface in the composite material is analyzed, and each interface is well combined without obvious defects and holes. The main processing technological parameters are as follows:
at 10-3The temperature is raised to 640 ℃ within 100min under the conditions of low vacuum degree of Pa and initial pressure of 3MPa, and the temperature is kept for about 20min to ensure that the sample is uniformly heated, at the moment, although the melting point of Al is not reached, the softening phenomenon of Al can occur, so the pressure needs to be reduced to prevent the phenomenon that the Al is extruded too much after melting, the pressure is reduced to 2MPa, and the temperature is raised to about 660 ℃ within 20 min. When the temperature reaches the melting point 660 ℃ of Al, the pressure head pressure needs to be stopped, the pressure is gradually changed from 2MPa to 0 at the moment, the pressure is gradually adjusted to 2MPa after heat preservation is carried out for 140min, and heating is stopped after heat preservation is continuously carried out for 40 min.
In summary, the following steps: the invention discloses a continuous Mo wire reinforced intermetallic compound based layered composite material Ti/Al3The Ti preparation method adopts a metal foil metallurgy method. The optimized preparation process parameters are as follows: at 10-3The temperature is raised to 640 ℃ within 100min under the conditions of low vacuum degree of Pa and initial pressure of 3MPa, and the temperature is kept for about 20min to ensure that the sample is uniformly heated, at the moment, although the melting point of Al is not reached, the softening phenomenon of Al can occur, so the pressure needs to be reduced to prevent the phenomenon that the Al is extruded too much after melting, the pressure is reduced to 2MPa, and the temperature is raised to about 660 ℃ within 20 min. When the temperature reaches the melting point 660 ℃ of Al, the pressure head pressure needs to be stopped, the pressure is gradually changed from 2MPa to 0 at the moment, the pressure is gradually adjusted to 2MPa after heat preservation is carried out for 140min, and heating is stopped after heat preservation is continuously carried out for 40 min. The prepared continuous molybdenum wire reinforced laminated composite material has improved toughness (along with the increase of TC4 volume fraction, the compression performance of the composite material is greatly improved, particularly the compression strain is obviously improved relatively), the tensile property is obviously improved (the tensile strength and the failure strain are obviously improved, and along with the continuous increase of TC4 volume fraction in the composite material, Mo-Ti/Al3The tensile property of Ti is also greatly improved, wherein the most obvious improvement is the tensile failure strain of the composite material, and the volume fraction of Ti/Al is 15 percent compared with TC43The strain to failure of Ti is increased by several times). In addition, the metal molybdenum wires are added as reinforcing fibers, so that the bending performance of the composite material is greatly improved, and the bending strength perpendicular to the molybdenum wires is generally higher than that of a pressure head direction parallel to the molybdenum wires. The invention also has the advantages of simple preparation process, low cost, stable and reliable performance and the like.

Claims (6)

1. Continuous metal Mo wire reinforced Ti/Al3The preparation method of the Ti layered composite material is characterized by comprising the following steps:
the method comprises the following steps: mixing TC4Pretreating the foil, the Al foil and the Mo wire;
step two: pre-treated TC4Foil, Al foil and Mo wire according to "TC4-Al-Mo-Al-TC4"is a unit stack with the outermost layer being TC4A foil;
step three: and putting the stacked sample into a vacuum hot-pressing furnace, setting process parameters and sintering.
The process parameters are specifically as follows: at 10-3The temperature is raised to 640 ℃ within 100min under the conditions of low vacuum degree of Pa and initial pressure of 3MPa, the temperature is kept for about 20min to ensure that the sample is uniformly heated, and at the moment, although the melting point of Al is not reached, the softening phenomenon of Al can occur, so that the pressure needs to be reduced to prevent the phenomenon that the Al is extruded too much after melting, the pressure is reduced to 2MPa, and the temperature is raised to about 660 ℃ within 20 min. When the temperature reaches the melting point 660 ℃ of Al, the pressure head pressure needs to be stopped, the pressure is gradually changed from 2MPa to 0 at the moment, the pressure is gradually adjusted to 2MPa after heat preservation is carried out for 140min, and heating is stopped after heat preservation is continuously carried out for 40 min.
2. The continuous metallic Mo wire reinforced Ti/Al of claim 13The preparation method of the Ti layered composite material is characterized in that the pretreatment specifically comprises the following steps: original TC of sand paper polishing4Edges and surfaces of foils, Al foils and Mo wires; cleaning and polishing TC by using ultrasonic cleaner4Foils, Al foils, and Mo wires; soaking in acetone solution for 10 min; then soaking and cleaning TC by alcohol4Foil, Al foil and Mo wire surface, followed byAnd (5) drying.
3. The continuous metallic Mo wire reinforced Ti/Al of claim 1 or 23The preparation method of the Ti layered composite material is characterized in that the Al content of the Al foil is more than or equal to 99.6%.
4. The continuous metallic Mo wire reinforced Ti/Al of claim 1 or 23The preparation method of the Ti layered composite material is characterized in that the Mo content in the molybdenum wire is more than or equal to 99.93 percent.
5. The continuous metallic Mo wire reinforced Ti/Al of claim 33The preparation method of the Ti layered composite material is characterized in that the Mo content in the molybdenum wire is more than or equal to 99.93 percent.
6. Continuous metal Mo wire reinforced Ti/Al3The Ti laminated composite material is characterized by comprising the following chemical components: mo is more than or equal to 99.93 percent, and other elements are less than or equal to 0.07 percent;
the other elements are specifically: fe is less than or equal to 0.30, carbon is less than or equal to 0.10, nitrogen is less than or equal to 0.05, hydrogen is less than or equal to 0.015, oxygen is less than or equal to 0.20, aluminum is 5.5-6.8, vanadium is 3.5-4.5, and the balance is titanium.
CN201910910549.7A 2019-09-25 2019-09-25 Continuous metal Mo wireStrong Ti/Al3Ti laminated composite material and preparation method thereof Pending CN110588096A (en)

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CN113172228A (en) * 2021-04-26 2021-07-27 中北大学 TC (tungsten carbide)4-Al3Ti laminated composite board and preparation method thereof
CN115070037A (en) * 2022-06-21 2022-09-20 哈尔滨理工大学 Method for enhancing Ti-Al series layered composite material by utilizing AlCoCrFeNi high-entropy alloy
CN116275022A (en) * 2023-03-28 2023-06-23 华南理工大学 Ultrahigh-toughness porous Ti-based memory alloy composite material and preparation method thereof

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