CN114888289B - Gradient titanium-based composite material and preparation method thereof - Google Patents

Gradient titanium-based composite material and preparation method thereof Download PDF

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CN114888289B
CN114888289B CN202210502356.XA CN202210502356A CN114888289B CN 114888289 B CN114888289 B CN 114888289B CN 202210502356 A CN202210502356 A CN 202210502356A CN 114888289 B CN114888289 B CN 114888289B
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titanium
based composite
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volume fraction
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CN114888289A (en
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黄陆军
纪明
王帅
安琦
孙枫泊
陈昕
耿林
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Harbin Institute of Technology
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
    • C22C32/0073—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only borides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/14—Both compacting and sintering simultaneously
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
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  • Metallurgy (AREA)
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  • Manufacture Of Alloys Or Alloy Compounds (AREA)

Abstract

The invention provides a gradient titanium-based composite material and a preparation method thereof, and relates to the technical field of composite materials, wherein the gradient titanium-based composite material comprises a surface layer, an intermediate layer and a core layer; the surface layer, the middle layer, the core layer, the middle layer and the surface layer are sequentially arranged along the thickness direction of the gradient titanium-based composite material; the surface layer is a titanium alloy layer; the middle layer and the core layer are titanium-based composite layers with reinforcing phases, and the volume fraction of the reinforcing phases in the middle layer is lower than that in the core layer; wherein the titanium-based composite layer is prepared from titanium alloy powder and ceramic powder. The gradient titanium-based composite material provided by the invention has excellent strength and plasticity and toughness, no obvious interface transition layer, and the preparation method is simple and stable and is suitable for preparing the large-size gradient layered titanium-based composite material.

Description

Gradient titanium-based composite material and preparation method thereof
Technical Field
The invention relates to the technical field of composite materials, in particular to a gradient titanium-based composite material and a preparation method thereof.
Background
The titanium alloy as one kind of engineering material has the advantages of low density, high specific strength, high temperature performance, etc. and may be used widely in aviation, astronautics, chemical industry, marine, biological and other fields. Compared with titanium alloy, the titanium-based composite material obtained by introducing the reinforcing phase into the titanium alloy has a certain improvement in strength, wear resistance and the like, however, the introduction of the reinforcing phase can lead to the reduction of the plasticity and toughness of the titanium-based composite material. In recent years, most of the prepared titanium-based composite materials are single-component titanium-based composite materials, for example, chinese patent application No. CN200810136852.8 discloses a single-component discontinuous fiber reinforced titanium-based composite material, and the strength is improved and the plasticity is obviously reduced. Thus, it is difficult to meet both high strength and high toughness requirements with a homogeneous single material.
Researchers find that biological materials such as bamboo, shells and the like in nature have excellent mechanical properties such as fracture toughness, so that the multi-component combined layered titanium-based composite material is designed based on the bionics idea to improve the toughness. However, the existing layered titanium-based composite materials are mostly obtained by combining the existing layered titanium-based composite materials by adopting a stacked hot rolling method disclosed in the patent with the application number of CN201210138430.0 or a welding diffusion method disclosed in the patent with the application number of CN 201310498988.4. The materials of each layer are obtained through wire cutting after preparing the block or are directly purchased, however, the method for obtaining the materials of each layer has high cost and complex operation; the thickness and the components of each layer are difficult to adjust after the direct purchase, so the designability and the controllability of the layered material are limited, and the preparation process of the material is complicated. And the interface bonding strength of the layered titanium-based composite material prepared by combining layers is generally low, so that the overall plasticity of the material is low.
Disclosure of Invention
The embodiment of the invention provides a gradient titanium-based composite material and a preparation method thereof, wherein the gradient titanium-based composite material has excellent strength and plastic toughness, no obvious interface transition layer exists between layers, and the preparation method is simple and stable and is suitable for preparing large-size gradient layered titanium-based composite materials.
In a first aspect, the present invention provides a gradient titanium-based composite comprising a skin layer, an intermediate layer, and a core layer; the surface layer, the middle layer, the core layer, the middle layer and the surface layer are sequentially arranged along the thickness direction of the gradient titanium-based composite material;
the surface layer is a titanium alloy layer;
the middle layer and the core layer are titanium-based composite layers with reinforcing phases, and the volume fraction of the reinforcing phases in the middle layer is lower than that in the core layer; wherein the titanium-based composite layer is prepared from titanium alloy powder and ceramic powder.
Preferably, the intermediate layer consists of at least two sub-intermediate layers; wherein the volume fraction of the reinforcing phase in the different sub-interlayers is different.
Preferably, the volume fraction of the reinforcing phase in the at least two sub-intermediate layers is distributed in a gradient increasing manner in the thickness direction from the surface layer to the core layer.
Preferably, the skin layer is made of TC4 powder.
Preferably, the titanium-based composite layer is formed by TC4 powder and TiB 2 And (5) preparing powder.
Preferably, the TC4 powder has a particle size of 80-120 μm;
the TiB is 2 The particle size of the powder is 1-8 mu m.
Preferably, the volume fraction of the reinforcing phase in the titanium-based composite layer is 3-20%.
Preferably, the volume fraction of the reinforcing phase in the intermediate layer is 3-10%;
the volume fraction of the reinforcing phase in the core layer is 9-20%.
More preferably, the volume fraction of the reinforcing phase in the core layer is 9 to 15%.
Preferably, the intermediate layer comprises a first sub-intermediate layer and a second sub-intermediate layer;
the volume fraction of the reinforcing phase in the first sub-intermediate layer is 3-5%, and the volume fraction of the reinforcing phase in the second sub-intermediate layer is 5-10%;
the first sub-interlayer is adjacent to the skin layer; the second sub-interlayer is adjacent to the core layer.
Preferably, the thicknesses of the sub-intermediate layer, the surface layer and the core layer are all the same.
In a second aspect, the present invention provides a method for preparing the gradient titanium-based composite material according to the first aspect, the method comprising:
(1) Ball milling is carried out on the titanium alloy powder and the ceramic powder to obtain mixed powder for preparing the intermediate layer and the core layer;
(2) Sequentially laying titanium alloy powder, mixed powder for preparing an intermediate layer, mixed powder for preparing a core layer, mixed powder for preparing an intermediate layer and titanium alloy powder in a mould, and then performing hot-pressing sintering to obtain the gradient titanium-based composite material comprising a surface layer, the intermediate layer and the core layer;
wherein the intermediate layer and the core layer are titanium-based composite layers having a reinforcing phase, and the volume fraction of the reinforcing phase in the intermediate layer is lower than the volume fraction of the reinforcing phase in the core layer.
Preferably, in step (1):
the ball milling rotating speed of the ball milling treatment is 180-220 rpm, preferably 200rpm;
the ball milling time is preferably 5h, and the ball-to-material ratio is preferably 5:1.
Preferably, in step (2):
the vacuum degree of the hot pressed sintering is not higher than 1 multiplied by 10 -2 Pa, sintering temperature 1300 ℃, pressure 25MPa and heat preservation time 1.5h.
Compared with the prior art, the invention has at least the following beneficial effects:
according to the invention, the titanium-based composite layer with higher reinforcing phase content and the titanium-based composite layer with lower reinforcing phase content are combined, and on the basis of ensuring the interface strength, the strain localization of the titanium-based composite layer in the deformation process is effectively relieved by virtue of the gradient layered structure, so that the structural advantage of the material is fully exerted, the deformation is more stable and uniform, the problem of inversion of the strength and the toughness of a single titanium-based composite material is solved, and the prepared gradient titanium-based composite material has good comprehensive performance.
The invention adopts the powder spreading method to realize the gradient layered structure design, and the gradient components and the layered thickness are controllable. Meanwhile, the hot-pressed sintering technology is adopted, the preparation method is simple, the prepared gradient titanium-based composite material interface is metallurgically bonded, the interfaces between layers are flat and well bonded, no obvious interface transition layer exists, and the problem of poor interface bonding force of layered materials prepared by other existing methods is solved.
Drawings
FIG. 1 is a flow chart of a method for preparing a gradient titanium matrix composite according to an embodiment of the present invention;
FIG. 2 is a graph comparing three-point bending properties of the gradient titanium-based composite material prepared in example 1 of the present invention and the titanium-based composite material prepared in comparative example 1;
FIG. 3 is a scanning electron microscope image of the gradient titanium matrix composite material prepared in example 1 of the present invention;
fig. 4 is a schematic diagram of a powder paving method according to an embodiment of the present invention.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments, and all other embodiments obtained by persons of ordinary skill in the art without making creative efforts based on the embodiments of the present invention are all within the scope of protection of the present invention.
The embodiment of the invention provides a gradient titanium-based composite material, which comprises a surface layer, an intermediate layer and a core layer; the surface layer, the middle layer, the core layer, the middle layer and the surface layer are sequentially arranged along the thickness direction of the gradient titanium-based composite material;
the surface layer is a titanium alloy layer;
the middle layer and the core layer are titanium-based composite layers with reinforcing phases, and the volume fraction of the reinforcing phases in the middle layer is lower than that in the core layer; wherein the titanium-based composite layer is prepared from titanium alloy powder and ceramic powder.
In the present invention, the layered structure of the gradient titanium-based composite material is, in the thickness direction: skin-middle layer-core layer-middle layer-skin; namely, the outermost side is a titanium alloy layer with good plasticity and low strength (namely, the volume fraction of the reinforcing phase is 0%), the core layer is a titanium-based composite layer with the highest reinforcing phase content in three layers, the core layer has the highest compressive strength and poorer stretching and bending properties in the three layers, the reinforcing phase content of the middle layer is between the surface layer and the core layer, and a gradient structure with the reinforcing phase content sequentially increasing from two sides to the center is formed. The gradient structure can effectively relieve the strain localization of the material in the deformation process, so that the structural advantage of the material can be fully exerted, and the deformation is more stable and uniform, thereby improving the problem of inversion of the strength and the plasticity of a single titanium-based composite material, and the prepared gradient titanium-based composite material has good comprehensive mechanical properties.
According to some preferred embodiments, the intermediate layer consists of at least two sub-intermediate layers; wherein the volume fraction of the reinforcing phase in the different sub-interlayers is different.
According to some preferred embodiments, the volume fraction of the reinforcing phase in the at least two sub-intermediate layers is distributed in a gradient increasing manner in the thickness direction from the skin layer to the core layer.
According to the invention, the gradient layered structure of the gradient titanium-based composite material can be flexibly designed by arranging at least two sub-intermediate layers in the intermediate layer, and the gradient transition from the surface layer to the core layer is more refined by adding the sub-intermediate layers, so that the strain localization in the deformation process is relieved more stably and uniformly, and the gradient titanium-based composite material with high strength and high toughness is prepared.
The traditional titanium-based composite material is mainly uniformly compounded, has uniform components and density, and therefore has single performance. However, the gradient titanium-based composite material can be provided with an optimized composition and structure in a proper area according to actual application conditions, so that the local characteristics of the material are adapted to specific requirements of the material, and the gradient titanium-based composite material has various performance advantages and is favorable for fully playing the performance of each layer.
According to some preferred embodiments, the skin layer is made of TC4 powder.
According to some preferred embodiments, the titanium-based composite layer is composed of TC4 powder and TiB 2 And (5) preparing powder.
According to some preferred embodiments, the TC4 powder has a particle size of 80 to 120 μm (e.g., may be 80 μm, 85 μm, 90 μm, 95 μm, 100 μm, 105 μm, 110 μm, 115 μm, or 120 μm);
TiB 2 the particle size of the powder is 1 to 8 μm (for example, 1 μm, 1.5 μm, 2 μm, 2.5 μm, 3 μm, 3.5 μm, 4 μm, 4.5 μm, 5)μm, 5.5 μm, 6 μm, 6.5 μm, 7 μm, 7.5 μm or 8 μm).
In the present invention, TC4 powder and TiB 2 Generating TiBw after in-situ autogenous reaction of the powder to obtain a titanium-based composite layer, wherein TiBw is a reinforcing phase and TC4 is a matrix phase in the titanium-based composite layer.
The thicknesses of the surface layer and the titanium-based composite layer are specifically defined according to the particle size of the powder and the requirements of the gradient titanium-based composite material. In the present invention, the thicknesses of the surface layer and the titanium-based composite layer may be not less than 100. Mu.m, for example, 100. Mu.m, 150. Mu.m, 200. Mu.m, 400. Mu.m, 500. Mu.m, 600. Mu.m, 800. Mu.m, 1mm, 1.5mm, etc.
According to some preferred embodiments, the volume fraction of the reinforcement phase in the titanium-based composite layer is 3-20% (e.g., may be 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, or 20%).
According to some preferred embodiments, the volume fraction of reinforcing phase in the intermediate layer is 3-10% (e.g., may be 3%, 3.5%, 4%, 4.5%, 5%, 5.5%, 6%, 6.5%, 7%, 7.5%, 8%, 8.5%, 9%, 9.5%, or 10%);
the volume fraction of reinforcing phase in the core layer is 9-20% (e.g., may be 9%, 9.5%, 10%, 10.5%, 11%, 11.5%, 12%, 12.5%, 13%, 13.5%, 14%, 14.5%, 15%, 15.5%, 16%, 16.5%, 17%, 17.5%, 18%, 18.5%, 19%, 19.5%, or 20%).
According to some more preferred embodiments, the volume fraction of the reinforcing phase in the core layer is 9-15% (e.g., may be 9%, 9.5%, 10%, 10.5%, 11%, 11.5%, 12%, 12.5%, 13%, 13.5%, 14%, 14.5%, or 15%).
According to some more preferred embodiments, the intermediate layer comprises a first sub-intermediate layer and a second sub-intermediate layer;
the volume fraction of the reinforcing phase in the first sub-interlayer is 3 to 5% (e.g., may be 3%, 3.2%, 3.5%, 3.8%, 4%, 4.2%, 4.5%, 4.8%, or 5%), and the volume fraction of the reinforcing phase in the second sub-interlayer is 5 to 10% (e.g., may be 5%, 5.5%, 6%, 6.5%, 7%, 7.5%, 8%, 8.5%, 9%, 9.5%, or 10%);
the first sub-interlayer is adjacent to the skin layer; the second sub-interlayer is adjacent to the core layer.
Specifically, in one embodiment of the present invention, the layered structure of the gradient titanium-based composite material may be: skin-first sub-interlayer-second sub-interlayer-core-second sub-interlayer-first sub-interlayer-skin.
According to some preferred embodiments, the thicknesses of the sub-intermediate layer, the skin layer and the core layer are all the same.
The invention also provides a preparation method of the gradient titanium-based composite material, which is adopted to obtain the gradient titanium-based composite material provided by the invention, as shown in figure 1, and comprises the following steps:
(1) Ball milling is carried out on the titanium alloy powder and the ceramic powder to obtain mixed powder for preparing the intermediate layer and the core layer;
(2) Sequentially laying titanium alloy powder, mixed powder for preparing an intermediate layer, mixed powder for preparing a core layer, mixed powder for preparing an intermediate layer and titanium alloy powder in a mould, and then performing hot-pressing sintering to obtain a gradient titanium-based composite material comprising a surface layer, the intermediate layer and the core layer;
wherein the intermediate layer and the core layer are titanium-based composite layers having a reinforcing phase, and the volume fraction of the reinforcing phase in the intermediate layer is lower than the volume fraction of the reinforcing phase in the core layer.
According to the invention, mixed powder with different contents of ceramic powder is prepared according to the preset ratio of ceramic powder and titanium alloy powder, the titanium-based composite material with the gradient layered structure is prepared by adopting a mode of layer-by-layer powder laying and stacking and hot-pressing sintering molding, the preparation method is simple, the prepared gradient titanium-based composite material has metallurgical bonding interfaces, complete whole structure, no obvious defects such as holes and cracks, and the like, the interfaces between layers are flat and well bonded, no obvious interface transition layer is arranged, and the problem of poor bonding at the interfaces of layered materials prepared by other methods in the prior art is solved.
Specifically, since the volume fraction of the reinforcing phase is affected by the content of the ceramic powder in the mixed powder, the content of the ceramic powder in the mixed powder for preparing the intermediate layer is lower than that in the mixed powder for preparing the core layer.
The invention can control the thickness of each layer by adopting the matching of the graphite die and the gear screw rod, thereby realizing flexible design and control of each layer thickness.
According to some preferred embodiments, in step (1):
the ball milling speed of the ball milling treatment is 180 to 220rpm (for example, may be 180rpm, 190rpm, 200rpm, 210rpm or 220 rpm);
ball milling time is 5h, and ball-material ratio is 5:1.
The invention adopts a planetary ball mill.
In the invention, the adhesion of the small-size ceramic powder on the surface of the large-size titanium alloy powder is realized by low-energy ball milling.
According to some preferred embodiments, the ball milling speed of the ball milling process is 200rpm.
According to some preferred embodiments, in step (2):
the degree of vacuum of hot press sintering is not higher than 1×10 -2 Pa (e.g., may be 1X 10) -2 Pa、5×10 -3 Pa、1×10 - 3 Pa、5×10 -4 Pa or 1X 10 -4 Pa, etc.), the sintering temperature is 1300 ℃, the pressure is 25MPa, and the heat preservation time is 1.5h.
In order to more clearly illustrate the technical scheme and advantages of the present invention, a gradient titanium-based composite material and a preparation method thereof are described in detail below through several embodiments.
Example 1
The layered structure of the gradient titanium-based composite material is as follows in the thickness direction: skin layer (TC 4 layer) -first sub-intermediate layer (4% reinforcement phase volume fraction) -second sub-intermediate layer (8% reinforcement phase volume fraction) -core layer (12% reinforcement phase volume fraction) -second sub-intermediate layer (8% reinforcement phase volume fraction) -first sub-intermediate layer (4% reinforcement phase volume fraction) -skin layer (TC 4 layer);
the preparation method for preparing the gradient titanium-based composite material comprises the following steps:
(1) TC4 powder (particle diameter of 80-100 μm) and TiB 2 Ball milling the powder (with the particle size of 5-8 mu m) according to a certain proportion to obtain mixed powder for preparing the first sub-intermediate layer, the second sub-intermediate layer and the core layer respectively;
wherein the ball milling rotating speed in the ball milling treatment is 200rpm, the ball milling time is 5h, and the ball-material ratio is 5:1;
(2) Sequentially laying TC4 powder, mixed powder for preparing a first sub-intermediate layer, mixed powder for preparing a second sub-intermediate layer, mixed powder for preparing a core layer, mixed powder for preparing a second sub-intermediate layer, mixed powder for preparing a first sub-intermediate layer and TC4 powder in a graphite mold, wherein the height of a lower pressing head of the graphite mold can be changed through a gear screw, and particularly as shown in fig. 4, the thickness of each layer is controlled to be 1mm through the gear screw;
after the laying is completed, the die is placed in a hot-pressing sintering furnace, and vacuum is pumped to ensure that the vacuum degree of the hot-pressing sintering furnace reaches 10 -2 Pa, and preserving heat for 1.5h under the conditions of the sintering temperature of 1300 ℃ and the pressure of 25MPa, and cooling along with a furnace to obtain the gradient titanium-based composite material.
Example 2
Example 2 is substantially the same as example 1 except that:
the layered structure of the gradient titanium-based composite material is as follows in the thickness direction: skin layer (TC 4 layer) -first sub-intermediate layer (reinforcing phase volume fraction 5%) -second sub-intermediate layer (reinforcing phase volume fraction 10%) -core layer (reinforcing phase volume fraction 15%) -second sub-intermediate layer (reinforcing phase volume fraction 10%) -first sub-intermediate layer (reinforcing phase volume fraction 5%) -skin layer (TC 4 layer).
Example 3
Example 3 is substantially the same as example 1 except that:
the layered structure of the gradient titanium-based composite material is as follows in the thickness direction: skin layer (TC 4 layer) -first sub-intermediate layer (3% reinforcement phase volume fraction) -second sub-intermediate layer (6% reinforcement phase volume fraction) -core layer (9% reinforcement phase volume fraction) -second sub-intermediate layer (6% reinforcement phase volume fraction) -first sub-intermediate layer (3% reinforcement phase volume fraction) -skin layer (TC 4 layer).
Example 4
Example 4 is substantially the same as example 1 except that:
the layered structure of the gradient titanium-based composite material is as follows in the thickness direction: skin layer (TC 4 layer) -first sub-intermediate layer (reinforcing phase volume fraction 6%) -core layer (reinforcing phase volume fraction 12%) -second sub-intermediate layer (reinforcing phase volume fraction 6%) -skin layer (TC 4 layer).
Example 5
Example 5 is substantially the same as example 1 except that:
surface layer (TC 4 layer) -first sub-intermediate layer (3% reinforcement phase volume fraction) -second sub-intermediate layer (6% reinforcement phase volume fraction) -third sub-intermediate layer (9% reinforcement phase volume fraction) -core layer (12% reinforcement phase volume fraction) -third sub-intermediate layer (9% reinforcement phase volume fraction) -second sub-intermediate layer (6% reinforcement phase volume fraction) -first sub-intermediate layer (3% reinforcement phase volume fraction) -surface layer (TC 4 layer).
Example 6
Example 6 is substantially the same as example 1 except that:
the grain diameter of TC4 powder is 100-120 mu m, tiB 2 The grain diameter of the powder is 1-5 mu m;
the thickness of each layer is controlled to be 1.5mm through a gear screw.
Comparative example 1
The volume fraction of the reinforcing phase of the traditional uniformly compounded titanium-based composite material is 5.1 percent.
The preparation method for preparing the titanium-based composite material comprises the following steps:
TC4 powder (particle diameter of 80-100 μm) and TiB 2 Ball milling the powder (with the grain diameter of 5-8 mu m) according to a certain proportion to obtain mixed powder for preparing the titanium-based composite material;
the mixed powder is laid in a graphite mould, and the thickness of the laid powder is equal to7mm, after the laying is completed, placing the die in a hot-pressing sintering furnace, and vacuumizing to ensure that the vacuum degree of the hot-pressing sintering furnace reaches 10 -2 Pa, and preserving heat for 1.5h under the conditions of the sintering temperature of 1300 ℃ and the pressure of 25MPa, and cooling along with a furnace to obtain the titanium-based composite material.
Comparative example 2
Comparative example 2 is substantially the same as example 1 except that:
the layered structure of the gradient titanium-based composite material is as follows in the thickness direction: surface layer (TC 4 layer) -first sub-intermediate layer (4% volume fraction of reinforcing phase) -second sub-intermediate layer (8% volume fraction of reinforcing phase) -core layer (12% volume fraction of reinforcing phase).
Comparative example 3
Comparative example 3 is substantially the same as example 1 except that:
the layered structure of the titanium-based composite material is as follows in the thickness direction: skin (TC 4 layer) -core (12% reinforcement phase volume fraction) -skin (TC 4 layer).
Since the densities of the reinforcing phase and TC4 are almost equal, the theoretical densities of the surface layer, the intermediate layer, and the core layer are substantially the same, and the error is negligible. Thus, for example 1, the average content of reinforcement phase in the gradient titanium matrix composite was about 5.1%, i.e., 5.1% = (4% +8% +12% +8% + 4%)/7, at the same layer thicknesses; for comparative example 3, the average content of reinforcing phase in the titanium-based composite material was about 5.1%, i.e., 5.1% = (12% +12% + 12%)/7, at the same layer thicknesses.
In the present invention, the gradient titanium-based composite material prepared in example 1 and the titanium-based composite material prepared in comparative example 1 were subjected to a room temperature three-point bending test, and room temperature stress strain curves thereof were shown in fig. 2.
In example 1, the prepared gradient titanium-based composite material has the lowest strength of the outermost TC4 layer, but better plasticity; while a titanium-based composite layer with 4vol.% reinforcing phase has higher plasticity but lower strength; the titanium-based composite layer with the reinforcing phase content of 8vol.% has higher strength but poorer plasticity; the titanium-based composite layer having a reinforcing phase content of 12vol.% has the highest reinforcing phase content with the highest compressive strength, but poor tensile and flexural properties. Through mechanical property test, the three-point bending strength of the gradient titanium-based composite material reaches more than 1800MPa, and the breaking strain can reach about 5 percent; the gradient layered material exhibited a higher strain at break without loss of flexural strength than the single titanium-based composite material having a reinforcing phase content of 5.1vol.% obtained in comparative example 1. Meanwhile, as shown in fig. 3, the whole structure of the gradient layered titanium-based composite material is perfect, no obvious defects such as holes and cracks exist, and the material shows a rule of gradually decreasing the gradient of the designed reinforcing phase content in the powder layer laying direction. In addition, it can be seen from the evaluation of the toughness of the material by the area under the load displacement curve in the bending test that the gradient titanium-based composite material of example 1 has improved the bending toughness by more than 2 times as compared with the titanium-based composite material of comparative example 1, and the overall exhibits better comprehensive mechanical properties (the load displacement curve can be obtained by the curve processing in fig. 2). The gradient titanium-based composite material prepared in the comparative example 2 is not symmetrically designed, so that the mechanical property of the material is greatly influenced by the loading direction; the titanium-based composite material prepared in comparative example 3 was alternately layered using only two component powders, the resulting titanium-based composite material did not form a gradient distribution in structure, and the layered titanium-based composite material had limited improvement in toughness.
In fig. 3, TC4 is used to characterize the surface layer in the gradient titanium-based composite material, 4vol.% TiB is used to characterize the first sub-intermediate layer in the gradient titanium-based composite material, 8vol.% TiB is used to characterize the second sub-intermediate layer in the gradient titanium-based composite material, and 12vol.% TiB is used to characterize the core layer in the gradient titanium-based composite material.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention. The invention is not described in detail in a manner known to those skilled in the art.

Claims (13)

1. The gradient titanium-based composite material is characterized by comprising a surface layer, an intermediate layer and a core layer; the surface layer, the middle layer, the core layer, the middle layer and the surface layer are sequentially arranged along the thickness direction of the gradient titanium-based composite material;
the surface layer is a titanium alloy layer;
the middle layer and the core layer are titanium-based composite layers with reinforcing phases, and the volume fraction of the reinforcing phases in the middle layer is lower than that in the core layer; wherein the titanium-based composite layer is prepared from titanium alloy powder and ceramic powder; the volume fraction of the reinforcing phase in the intermediate layer is 3-10%; the volume fraction of the reinforcing phase in the core layer is 9-20%.
2. The gradient titanium-based composite of claim 1, wherein:
the middle layer consists of at least two sub middle layers; wherein the volume fraction of the reinforcing phase in the different sub-interlayers is different.
3. The gradient titanium-based composite of claim 2, wherein:
the volume fraction of the reinforcing phase in the at least two sub-intermediate layers is distributed in a gradient increasing manner along the thickness direction from the surface layer to the core layer.
4. The gradient titanium-based composite of claim 1, wherein:
the surface layer is prepared from TC4 powder;
the titanium-based composite layer is formed by TC4 powder and TiB 2 And (5) preparing powder.
5. The gradient titanium matrix composite of claim 4, wherein:
the grain diameter of the TC4 powder is 80-120 mu m;
the TiB is 2 The particle size of the powder is 1-8 mu m.
6. The gradient titanium-based composite of claim 1, wherein:
the volume fraction of the reinforcing phase in the titanium-based composite layer is 3-20%.
7. The gradient titanium-based composite of claim 1, wherein:
the volume fraction of the reinforcing phase in the core layer is 9-15%.
8. The gradient titanium-based composite of claim 2, wherein:
the intermediate layer comprises a first sub-intermediate layer and a second sub-intermediate layer;
the volume fraction of the reinforcing phase in the first sub-intermediate layer is 3-5%, and the volume fraction of the reinforcing phase in the second sub-intermediate layer is 5-10%;
the first sub-interlayer is adjacent to the skin layer; the second sub-interlayer is adjacent to the core layer.
9. The gradient titanium-based composite of claim 2, wherein:
the thicknesses of the sub-intermediate layer, the surface layer and the core layer are all the same.
10. A method of preparing a gradient titanium matrix composite material according to any one of claims 1 to 9, characterized in that the method of preparing comprises:
(1) Ball milling is carried out on the titanium alloy powder and the ceramic powder to obtain mixed powder for preparing the intermediate layer and the core layer;
(2) Sequentially laying titanium alloy powder, mixed powder for preparing an intermediate layer, mixed powder for preparing a core layer, mixed powder for preparing an intermediate layer and titanium alloy powder in a mould, and then performing hot-pressing sintering to obtain the gradient titanium-based composite material comprising a surface layer, the intermediate layer and the core layer;
wherein the intermediate layer and the core layer are titanium-based composite layers having a reinforcing phase, and the volume fraction of the reinforcing phase in the intermediate layer is lower than the volume fraction of the reinforcing phase in the core layer.
11. The method of claim 10, wherein in step (1):
the ball milling rotating speed of the ball milling treatment is 180-220 rpm.
12. The method of claim 10, wherein in step (1):
the ball milling rotating speed of the ball milling treatment is 200rpm;
ball milling time is 5h, and ball-material ratio is 5:1.
13. The preparation method according to any one of claims 11 to 12, wherein in step (2):
the vacuum degree of the hot pressed sintering is not higher than 1 multiplied by 10 -2 Pa, sintering temperature 1300 ℃, pressure 25MPa and heat preservation time 1.5h.
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