CN117604303A - Ultrahigh-strength and high-toughness titanium-based composite material with solid solution reinforced reticular structure and preparation method thereof - Google Patents
Ultrahigh-strength and high-toughness titanium-based composite material with solid solution reinforced reticular structure and preparation method thereof Download PDFInfo
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- 239000010936 titanium Substances 0.000 title claims abstract description 169
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 164
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 163
- 239000002131 composite material Substances 0.000 title claims abstract description 150
- 239000006104 solid solution Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 112
- 229910001069 Ti alloy Inorganic materials 0.000 claims abstract description 63
- 238000005728 strengthening Methods 0.000 claims abstract description 54
- 239000011159 matrix material Substances 0.000 claims abstract description 53
- 238000005245 sintering Methods 0.000 claims abstract description 45
- 238000000034 method Methods 0.000 claims abstract description 41
- 229910052796 boron Inorganic materials 0.000 claims abstract description 28
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910021392 nanocarbon Inorganic materials 0.000 claims abstract description 24
- 238000000498 ball milling Methods 0.000 claims abstract description 23
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 238000012545 processing Methods 0.000 claims abstract description 17
- 238000000280 densification Methods 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 33
- 238000005096 rolling process Methods 0.000 claims description 27
- 229910021389 graphene Inorganic materials 0.000 claims description 26
- 238000004321 preservation Methods 0.000 claims description 24
- 239000000126 substance Substances 0.000 claims description 24
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- 239000000463 material Substances 0.000 claims description 17
- 239000002994 raw material Substances 0.000 claims description 12
- 230000002194 synthesizing effect Effects 0.000 claims description 11
- 229910052799 carbon Inorganic materials 0.000 claims description 10
- 239000006229 carbon black Substances 0.000 claims description 10
- 239000002243 precursor Substances 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 4
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- 230000008569 process Effects 0.000 abstract description 15
- 239000013078 crystal Substances 0.000 abstract description 14
- 239000007795 chemical reaction product Substances 0.000 abstract description 4
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- 238000009826 distribution Methods 0.000 description 15
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
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- 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
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
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- 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
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- B22F9/00—Making metallic powder or suspensions thereof
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- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
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Abstract
The invention discloses a solid solution strengthening net structure ultrahigh strength and toughness titanium-based composite material and a preparation method thereof, wherein the method comprises the following steps: 1. sequentially carrying out multi-step low-energy ball milling mixing on nano carbide containing beta stable elements, a nano carbon source/boron source and titanium alloy matrix powder; 2. and (5) densification is carried out, and thermal deformation processing is carried out after rapid sintering, so that the titanium-based composite material is obtained. The invention adopts multi-step low-energy ball milling mixing, and introduces beta stable element into the crystal of the solid solution reinforced titanium matrix through carbideTiC is formed at the grain boundary by utilizing the interfacial reaction product of the nano carbon source/boron source and titanium p Or TiB w The discontinuous network structure surrounding the grain boundary strengthens the grain boundary, and simultaneously precipitates high-density needle-shaped alpha' precipitated phases in the equiaxial beta-Ti matrix in the thermal deformation processing process.
Description
Technical Field
The invention belongs to the technical field of metal matrix composite materials, and particularly relates to a solid solution reinforced net-shaped structure ultrahigh-strength and high-toughness titanium matrix composite material and a preparation method thereof.
Background
With the development of aerospace industry, structural materials are required to have lower density, longer service life and to be able to withstand more complex and severe service conditions. Compared with titanium alloys, titanium-based composite materials have excellent strength, higher heat resistance temperature, excellent wear resistance, hardness, and the like, and are attracting attention as a novel strategic structural material. Through the research of the titanium-based composite material in the last decade, the bottleneck problem of poor plasticity of the traditional uniform titanium-based composite material can be solved through the design optimization of the spatial configuration of the reinforcement, and the strong plasticity matching level and the processability of the titanium-based composite material are obviously improved.
Nanometer carbon material such as graphene and the like is taken as a material prepared from sp 2 The two-dimensional carbon nanomaterial consisting of the hybrid track has excellent mechanical properties, such as high elastic modulus and high breaking strength, and is considered to be one of ideal reinforcing materials for the metal matrix composite. The research of graphene/titanium composite materials is highly emphasized in China, and related researches are sequentially carried out by scientific research institutions such as northwest nonferrous metal research institute, beijing university of science and university of south east. Because of poor chemical compatibility of carbon and titanium, the carbon and the titanium are easy to react chemically in the forming process, so that the graphene nano reinforcing phase is damaged. According to the Fick diffusion principle, the diffusion of carbon and titanium atoms can be inhibited by reducing the high-temperature residence time or adopting low-temperature sintering and the like, and the intrinsic structure of the graphene is kept from being damaged. However, the reduction of sintering temperature and high temperature residence time causes problems such as poor formability and low density of the composite material, and a large number of cracks and voids exist in the molded sampleDefects such as holes and the like. Therefore, how to regulate the interface reaction between graphene and the titanium matrix becomes a key to improve the performance of the titanium-based composite material. However, in the graphene/titanium-based composite materials reported in the current large amounts of the prior art (Mater. Des.,140 (2018) 431-441; mater. Des.,196 (2020) 109119;Compos.Part A136 (2020) 105971; J. Mater. Sci. Technol.96 (2022) 85-93, etc.), the retained graphene or a small amount of the interfacial reaction product TiC is distributed only on the titanium grain boundaries without any strengthening effect on the crystal interior, resulting in limited synergic strengthening effect.
In order to solve the problems that the graphene/titanium-based composite material prepared by the prior art has limited performance improvement and serious 'inversion' of strong plasticity, the strong plasticity matching level with the strength of more than 1500MPa and the elongation of more than 5% is not broken through yet. There is an urgent need to design and develop a titanium-based composite material with ultrahigh strength and toughness, and the material has important application potential, so as to find a new growth point for the development of the titanium-based composite material.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a solid solution reinforced net-shaped structure ultrahigh-strength and high-toughness titanium-based composite material aiming at the defects in the prior art. According to the method, nano carbide containing beta stable elements and a nano carbon source/boron source are uniformly wrapped and dispersed on the surface of titanium alloy matrix powder sequentially through multi-step low-energy ball milling mixing, so that the uniform dispersibility of the nano carbon source/boron source on the surface of the titanium alloy matrix powder is promoted, the rapid sintering and thermal deformation processing of densification are combined, the metal elements in the nano carbide are promoted to be in concentration gradient distribution, the titanium alloy particle grains are strengthened, and TiC is formed at the grain boundary of the titanium alloy particles p Or TiB w The titanium-based composite material has the advantages that the grain boundary is reinforced by a discontinuous net-shaped structure, and meanwhile, a high-density needle-shaped alpha' precipitated phase is precipitated in an equiaxed beta-Ti matrix in the thermal deformation processing process, so that the titanium-based composite material has ultrahigh strength and maintains excellent room temperature elongation, an excellent strong plastic matching level is realized, and the bottleneck of strong plastic inversion of the conventional net-shaped structure titanium-based composite material is overcome.
In order to solve the technical problems, the invention adopts the following technical scheme: the preparation method of the ultrahigh-strength and high-toughness titanium-based composite material with the solid solution strengthening net structure is characterized by comprising the following steps of:
step one, selecting powder raw materials and synthesizing with low damage: the spherical TC4 prealloy powder prepared by a rotary electrode method is used as titanium alloy matrix powder, nano carbide containing beta stable elements and a nano carbon source/boron source are respectively used as an intragranular solid solution strengthening reinforcing phase and a grain boundary reticular structure reinforcing body nano precursor, and the nano carbide containing the beta stable elements and the nano carbon source/boron source are sequentially added into the titanium alloy matrix powder for multi-step low-energy ball milling mixing, so that low-damage titanium-based composite powder with uniformly dispersed nano carbide and nano carbon source/boron source is obtained;
preparing a titanium-based composite material: densification and rapid sintering are carried out on the titanium-based composite powder obtained in the step one, a titanium-based composite material blank is obtained, and then the solid solution strengthening net-shaped structure ultrahigh-strength and high-toughness titanium-based composite material is obtained through thermal deformation processing; the strength of the ultrahigh-strength and high-toughness titanium-based composite material with the solid solution strengthening reticular structure is more than 1500MPa, and the elongation is more than 8%.
The method sequentially uniformly wraps and disperses an intragranular solid solution strengthening reinforcing phase, namely nano carbide containing beta stable elements and a grain boundary reticular structure reinforcing body nano precursor, namely a nano carbon source/boron source, on the surface of titanium alloy matrix powder through multi-step low-energy ball milling mixing, and obtains the titanium alloy matrix powder with intragranular gradient solid solution strengthening and grain boundary TiC through plasma rapid sintering p Or TiB w The net-shaped structure reinforced titanium-based composite material blank is subjected to thermal deformation processing to prepare solid solution reinforced ultrahigh-strength and high-toughness TiC p Or TiB w Titanium matrix composite materials of network structure.
Specifically, the method comprises the steps of uniformly coating nano carbide containing beta stable element on the surface of titanium alloy matrix powder through multi-step low-energy ball milling, so that on one hand, the surface roughness of the titanium alloy matrix powder is improved, more sites are provided for the subsequent uniform coating of nano carbon source/boron source, and on the other hand, a carbide transition layer is formed on the surface of the titanium alloy matrix powder, so that the non-wetting interface between titanium and carbon is improved to be a wetting interface, and the division of the nano carbon source/boron source on the surface of the titanium alloy matrix powder is improvedThe dispersion effect is favorable for forming the net-shaped TiC distribution in the subsequent sintering process p Or TiB w The functions of pinning grain boundary, refining grains and transferring load are achieved. Under the combined action of the two, the problem of uneven dispersion of carbon sources such as graphene on the surface of the titanium alloy in the existing direct ball milling process is effectively solved.
Then, the densification rapid sintering process is adopted, and as the sintering time is shorter, the metal elements in the nano carbide containing the beta stable elements are not fully diffused and homogenized in the crystal, so that the metal elements are distributed in a concentration gradient manner in the crystal to strengthen titanium grains, the volume fraction of beta phase is increased, the slip system multiple characteristics of beta phase are utilized, the plasticity of the titanium-based composite material is improved, and more strengthening phases are introduced in the grain boundary distribution under the processable plasticity condition. Meanwhile, in the densification rapid sintering process, the nano carbon source or the boron source uniformly coated on the outer layer of the titanium-based composite powder reacts with the titanium alloy in situ to form ceramic reinforcing phase TiC at the grain boundary p Or TiB w And the titanium-based composite material is distributed in a reticular structure, has pinning effect on grain boundaries, and limits rapid growth of grains so as to strengthen the titanium-based composite material. The reinforcing phase aggregation area forms a structure of three-dimensional communication, discrete distribution of reinforcing phase depletion areas and reinforcing phase cladding soft phase matrix, and an excellent reinforcing effect is ensured. In addition, tiC generated at grain boundary p Or TiB w The ceramic phase can effectively bear load, so that the strength of the titanium-based composite material is improved, the soft phase matrix can passivate cracks, prevent crack growth, realize plastic deformation, and especially ensure that the precipitated high-density needle-shaped alpha' precipitated phase in the equiaxed beta-Ti matrix in the thermal deformation processing process always keeps coherent twin deformation with the matrix in the loading deformation process, so that the plasticity of the titanium-based composite material is ensured.
Finally, the invention adopts thermal deformation processing to lead the metal element in the nano carbide to be evenly solid-solution strengthened in the crystal, and the ceramic strengthening phase TiC at the grain boundary p Or TiB w Further dispersed and distributed along the thermal deformation processing direction and distributed in a discontinuous net shape. Meanwhile, the matrix undergoes thermal deformation reinforcement, so that the strength of the titanium-based composite material is further improved, and the density of the titanium-based composite material is further improvedFurther improves, and the larger ceramic reinforcing phase is crushed and refined. In addition, the thermal deformation processing refines the size of alpha crystal grains in the crystal, refines the matrix structure, and along with the increase of the deformation degree, the dislocation density in the titanium-based composite material continuously rises, the dislocation is easy to form barriers such as dislocation plug clusters, cutting steps and the like during the dislocation movement, the dislocation is hindered from further movement, the deformation resistance is increased, meanwhile, the interaction between a high-density needle-shaped alpha' precipitated phase and the dislocation is precipitated in the equiaxed beta-Ti matrix in the thermal deformation processing process, and the strength of the titanium-based composite material is further improved.
In conclusion, under the action of the multiple strengthening mechanisms, the solid solution strengthening reticular structure ultrahigh-strength and high-strength titanium-based composite material with ultrahigh strength and good room temperature elongation is obtained, and the nano carbon source or boron source (such as graphene and TiB) is overcome 2 Etc.) in a titanium matrix, and the residual graphene or local reaction products of the prior art are distributed only on grain boundaries, resulting in the problem of insufficient level of strong plastic matching of the titanium-based composite material.
The preparation method of the ultra-high strength and toughness titanium-based composite material with the solid solution reinforced reticular structure is characterized in that in the first step, the spherical TC4 prealloy powder is prepared by a plasma rotary electrode method, the granularity is 15-53 mu m, the sphericity is good, no planetary powder exists, and the chemical composition meets the requirements of GB/T3620.1-2007 titanium and titanium alloy brands and chemical composition standards; the nano carbide containing the beta stabilizing element is spherical Mo 2 C powder with granularity of 20-800 nm. The invention adopts spherical Mo 2 C powder as nano carbide containing beta stable element and Mo introduced into the nano carbide 2 And C, the solid solution is strengthened in the crystal, so that the volume fraction of the beta phase is improved, and the plasticity of the titanium-based composite material is improved.
The preparation method of the ultrahigh-strength and high-toughness titanium-based composite material with the solid solution reinforced reticular structure is characterized in that the nano carbon source in the first step is reduced graphene oxide or carbon black particles, the sheet diameter of the reduced graphene oxide is 4-7 mu m, the thickness is 5nm, and the average size of the carbon black particles is 25nm. The selection of the above-mentioned kinds of nanocarbon sources is advantageous in improving the dispersibility thereof.
The solid solution strengthening net structure is superThe preparation method of the high-strength and high-toughness titanium-based composite material is characterized in that the nano boron source in the first step is TiB 2 、B 4 One or more of the C and B powders, and TiB 2 The average size of the powder was 40nm.
The preparation method of the ultrahigh-strength and high-toughness titanium-based composite material with the solid solution reinforced reticular structure is characterized in that the rotating speed of the multi-step low-energy ball milling mixing in the first step is 150-250 r/min, the ball milling time is 5-10 h, and the ball-material ratio is 5:1. More preferably, the rotational speed of the multi-stage low energy ball mill mixing is 200r/min. The ball shape of the titanium alloy matrix powder is guaranteed to the greatest extent by controlling the rotating speed, the time and the ball material ratio, and the uniform coating of the nano carbon source/boron source on the titanium matrix powder is guaranteed.
The preparation method of the ultrahigh-strength and high-toughness titanium-based composite material with the solid solution strengthening reticular structure is characterized in that the densification rapid sintering in the second step is plasma activated sintering, hot pressing sintering or hot isostatic pressing sintering, the temperature of the plasma activated sintering is 800-1100 ℃, the heating speed is 100 ℃/min, the heat preservation time is 5-10 min, and the pressure is 30-60 MPa. More preferably, the temperature of the ion activated sintering is 1000 ℃, the temperature rising speed is 100 ℃/min, the heat preservation time is 5min, and the pressure is 40MPa. The sintering method and the technological parameters are favorable for the in-situ generation of TiC by the reaction of the nano carbon source or the nano boron source and the titanium matrix p Or TiB w 。
The preparation method of the ultrahigh-strength and high-toughness titanium-based composite material with the solid solution reinforced reticular structure is characterized in that the thermal deformation processing in the second step is rolling, the rolling temperature is 800-1000 ℃, the heat preservation time is 10-30 min, and the rolling deformation is 50-90%. More preferably, the rolling temperature is 900 ℃, the heat preservation time is 20min, and the rolling deformation is 75%. The thermal deformation processing mode and the technological parameters are beneficial to further improving the compactness of the titanium-based composite material, crushing larger TiC particles and TiB whiskers, improving the distribution of the TiC particles and TiB whiskers in a titanium matrix and optimizing the mechanical properties of the titanium-based composite material.
In addition, the invention also discloses a solid solution strengthening net structure ultrahigh strength and toughness titanium-based composite material, which is characterized by being prepared by the method.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, by utilizing the component structural characteristics of the titanium alloy, nano carbide containing beta stable elements and a nano carbon source/boron source are uniformly wrapped and dispersed on the surface of titanium alloy matrix powder sequentially through multi-step low-energy ball milling mixing, the carbide is introduced into beta stable element solid solution strengthening crystals and the volume fraction of beta phase is improved, the plasticity of the titanium-based composite material is improved by utilizing the sliding system of beta phase, and TiC is formed at the grain boundary of titanium alloy particles by combining the interfacial reaction product of the nano carbon source/boron source and titanium p Or TiB w The high-density needle-shaped alpha' precipitated phase is precipitated in the equiaxed beta-Ti matrix in the thermal deformation processing process, so that the ultra-high strength and toughness titanium-based composite material with ultra-high strength and excellent room temperature elongation is obtained, the excellent strong plasticity matching level of the titanium-based composite material is realized, and the problems that the performance improvement of the conventional powder metallurgy graphene reinforced titanium-based composite material is limited and the strong plasticity is seriously inverted are overcome.
2. According to the invention, the nano carbide containing the beta stable element is uniformly coated on the surface of the titanium alloy matrix powder in the multi-step low-energy ball milling mixing process, so that the dispersing effect of the nano carbon source/boron source on the surface of the titanium alloy matrix powder is improved, more sites are provided for coating, the uniform dispersion of the carbon source/boron source reinforcing material on the surface of the titanium alloy is promoted, the problem of uneven dispersion of the nano carbon source/boron source on the surface of the titanium alloy is solved, and a foundation is provided for the subsequent formation of the titanium-based composite material with the net-shaped structure distribution reinforcing body.
3. The invention adopts densification rapid sintering technology to promote the metal element in the nano carbide of beta stable element to be in concentration gradient distribution in the crystal to strengthen titanium crystal grains, ensures that the grain boundary distribution quantity of the strengthening phase is increased under the workable plastic condition, and simultaneously ensures TiC at the grain boundary p Or TiB w Is distributed in a net structure, and TiC p Or TiB w Respectively playing roles of strengthening and passivating cracks with the matrix, particularly, the interaction of high-density needle-shaped alpha' precipitated phases and dislocation precipitated in the equiaxed beta-Ti matrix is carried out at the same time in the loading deformation processThe titanium-based composite material always maintains a coherent twin relation with the matrix, and ensures the plasticity of the titanium-based composite material while ensuring excellent reinforcing effect.
4. The invention promotes the uniform solid solution strengthening of metal elements in nano carbide in crystal and the ceramic strengthening phase TiC at the grain boundary by thermal deformation processing p Or TiB w The dispersion distribution is discontinuous reticular distribution, and the ceramic reinforcing phase is crushed and refined, so that the matrix is thermally deformed and reinforced, and the density and the strength of the titanium-based composite material are improved.
5. The invention has the advantages of wide raw material sources, simple process, easy realization, obvious engineering prospect and popularization and application to near alpha titanium alloy.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
FIG. 1 is an SEM image of a titanium-based composite powder prepared according to example 1 of the invention.
Fig. 2a is an SEM image of a green body of a sintered titanium matrix composite material prepared in example 1 of the present invention.
Fig. 2b is a diagram showing the Mo element distribution in fig. 2 a.
Fig. 3a is an SEM image of a titanium matrix composite in a rolled state prepared in example 1 of the present invention.
Fig. 3b is a diagram showing the Mo element distribution in fig. 3 a.
FIG. 4 is a graph showing the mechanical properties of the titanium-based composite materials prepared in examples 1 to 2 according to the present invention, TC4 titanium alloy prepared in comparative example 1, and titanium-based composite materials prepared in comparative examples 2 to 3.
Detailed Description
Example 1
The embodiment comprises the following steps:
step one, selecting powder raw materials and synthesizing with low damage: spherical TC4 prealloy powder is used as titanium alloy matrix powder, and Mo is used as Mo 2 C and reduced graphene oxide are respectively an intragranular solid solution strengthening reinforcing phase and a grain boundary reticular structure reinforcing body nano precursor, and 1.2g of spherical Mo with granularity of 800nm is added 2 C, adding 120g of spherical TC4 titanium alloy powder into the mixture at the rotating speed of 200r/min with the ball-to-material ratio ofMixing for 5 hours by low-energy ball milling under the condition of 5:1, then adding 0.6g of reduced graphene oxide in batches, and continuing the low-energy ball milling and mixing for 10 hours under the condition of 200r/min of rotating speed and 5:1 of ball-to-material ratio to obtain low-damage spherical Mo 2 C and the reduced graphene oxide are uniformly dispersed;
the spherical TC4 prealloy powder is prepared by a plasma rotary electrode method, has the granularity of 15-53 mu m, good sphericity and no planetary powder, and the chemical components meet the requirements of GB/T3620.1-2007 titanium and titanium alloy brand and chemical component standard; the sheet diameter of the reduced graphene oxide is 4-7 mu m, and the thickness is 5nm;
preparing a titanium-based composite material: and (3) performing plasma activated sintering on the titanium-based composite powder obtained in the step (I), wherein the temperature of the plasma activated sintering is 1000 ℃, the temperature rising speed is 100 ℃/min, the heat preservation time is 5min, the pressure is 40MPa, a titanium-based composite material blank is obtained, and then the titanium-based composite material blank is rolled, wherein the rolling temperature is 900 ℃, the heat preservation time is 20min, and the rolling deformation is 75%, so that the ultrahigh-strength and high-toughness titanium-based composite material with the solid solution strengthening network structure, namely the TiC/TC4 composite material with the Mo solid solution strengthening network structure, is obtained.
FIG. 1 is an SEM image of a titanium-based composite powder prepared according to the present example, and it can be seen from FIG. 1 that the titanium-based composite powder still maintains a spherical morphology, and Mo 2 C and the reduced graphene oxide are uniformly coated on the surface of the spherical TC4 titanium alloy powder.
FIG. 2a is an SEM image of a sintered titanium-based composite material blank prepared according to this example, as can be seen from FIG. 2a, tiC after sintering p The Mo element is distributed in gradient in the grain boundary of the titanium-based composite material blank in a netlike discontinuous structure, the Mo element is enriched in the grain boundary, and the Mo element is relatively less in the grain boundary; fig. 2b is a graph showing Mo element distribution in fig. 2a, and it can be seen from fig. 2b that Mo element in the sintered titanium matrix composite blank forms a gradient solid solution distribution characteristic.
FIG. 3a is an SEM image of a rolled titanium-based composite material prepared according to this example, and it can be seen from FIG. 3a in combination with FIG. 2a that the thermal deformation process promotes TiC p The grains are thinned and distributed in a fibrous discontinuous network;fig. 3b shows the Mo element distribution diagram in fig. 3a, and it can be seen from fig. 3b in combination with fig. 2b that the heat deformation process promotes homogenization of Mo element, thereby further solid-solution strengthening the titanium matrix.
Densification rapid sintering of the present embodiment may also be replaced with hot press sintering or hot isostatic pressing sintering.
Comparative example 1
The comparative example comprises the following steps:
step one, selecting powder raw materials and synthesizing with low damage: taking spherical TC4 prealloy powder as titanium alloy matrix powder; the spherical TC4 prealloy powder is prepared by a plasma rotary electrode method, has the granularity of 15-53 mu m, good sphericity and no planetary powder, and the chemical components meet the requirements of GB/T3620.1-2007 titanium and titanium alloy brand and chemical component standard;
step two, preparing TC4 titanium alloy: and (3) performing plasma activated sintering on the titanium alloy matrix powder selected in the step one, wherein the plasma activated sintering temperature is 1000 ℃, the heating speed is 100 ℃/min, the heat preservation time is 5min, the pressure is 40MPa, and the TC4 titanium alloy blank is obtained, and then rolling is performed, wherein the rolling temperature is 900 ℃, the heat preservation time is 20min, and the rolling deformation is 75%, so that the TC4 titanium alloy is obtained.
Comparative example 2
The comparative example comprises the following steps:
step one, selecting powder raw materials and synthesizing with low damage: spherical TC4 prealloy powder is used as titanium alloy matrix powder, and Mo is used as Mo 2 C is an intragranular solid solution strengthening reinforcing phase, and 0.6g of spherical Mo with granularity of 800nm 2 C is added into 120g of spherical TC4 titanium alloy powder, and ball milling and mixing are carried out for 5 hours under the conditions of 200r/min rotating speed and 5:1 ball material ratio, thus obtaining low-damage spherical Mo 2 C uniformly dispersed titanium-based composite powder;
the spherical TC4 prealloy powder is prepared by a plasma rotary electrode method, has the granularity of 15-53 mu m, good sphericity and no planetary powder, and the chemical components meet the requirements of GB/T3620.1-2007 titanium and titanium alloy brand and chemical component standard;
preparing a titanium-based composite material: and (3) performing plasma activated sintering on the titanium-based composite powder obtained in the step (I), wherein the plasma activated sintering temperature is 1000 ℃, the heating speed is 100 ℃/min, the heat preservation time is 5min, the pressure is 40MPa, a titanium-based composite material blank is obtained, and then the titanium-based composite material blank is rolled, wherein the rolling temperature is 900 ℃, the heat preservation time is 20min, and the rolling deformation is 75%, so that the solid solution reinforced titanium-based composite material, namely the Mo solid solution reinforced TC4 composite material, is obtained.
Comparative example 3
The comparative example comprises the following steps:
step one, selecting powder raw materials and synthesizing with low damage: taking spherical TC4 prealloy powder as titanium alloy matrix powder, taking reduced graphene oxide as a crystal boundary reticular structure reinforcement nano precursor, adding 0.6g of reduced graphene oxide into 120g of spherical TC4 titanium alloy powder, and carrying out low-energy ball milling and mixing for 5 hours under the conditions of 200r/min of rotating speed and 5:1 of ball material ratio to obtain low-damage and uniformly dispersed titanium-based composite powder of the reduced graphene oxide;
the spherical TC4 prealloy powder is prepared by a plasma rotary electrode method, has the granularity of 15-53 mu m, good sphericity and no planetary powder, and the chemical components meet the requirements of GB/T3620.1-2007 titanium and titanium alloy brand and chemical component standard; the sheet diameter of the reduced graphene oxide is 4-7 mu m, and the thickness is 5nm;
preparing a titanium-based composite material: and (3) performing plasma activated sintering on the titanium-based composite powder obtained in the step (I), wherein the temperature of the plasma activated sintering is 1000 ℃, the temperature rising speed is 100 ℃/min, the heat preservation time is 5min, the pressure is 40MPa, a titanium-based composite material blank is obtained, and then the titanium-based composite material blank is rolled, wherein the rolling temperature is 900 ℃, the heat preservation time is 20min, and the rolling deformation is 75%, so that the net-shaped titanium-based composite material, namely the TiC reinforced TC4 composite material, is obtained.
Example 2
The embodiment comprises the following steps:
step one, selecting powder raw materials and synthesizing with low damage: spherical TC4 prealloy powder is used as titanium alloy matrix powder, and Mo is used as Mo 2 C and TiB 2 Strengthening body with crystal internal solid solution strengthening phase and grain boundary net structure respectivelyNanometer precursor, and 1.2g of spherical Mo with granularity of 800nm 2 C. 1.08g of TiB with an average size of 40nm 2 Sequentially adding 120g of spherical TC4 titanium alloy powder, and carrying out low-energy ball milling and mixing for 10 hours under the conditions of 200r/min rotating speed and 5:1 ball-to-material ratio to obtain low-damage spherical Mo 2 C and TiB 2 Uniformly dispersed titanium-based composite powder;
the spherical TC4 prealloy powder is prepared by a plasma rotary electrode method, has the granularity of 15-53 mu m, good sphericity and no planetary powder, and the chemical components meet the requirements of GB/T3620.1-2007 titanium and titanium alloy brand and chemical component standard;
preparing a titanium-based composite material: and (3) performing plasma activated sintering on the titanium-based composite powder obtained in the step (I), wherein the temperature of the plasma activated sintering is 1000 ℃, the temperature rising speed is 100 ℃/min, the heat preservation time is 5min, the pressure is 40MPa, a titanium-based composite material blank is obtained, and then the titanium-based composite material blank is rolled, wherein the rolling temperature is 900 ℃, the heat preservation time is 20min, and the rolling deformation is 75%, so that the ultra-high-strength and high-toughness titanium-based composite material with the solid solution strengthening network structure, namely the TiB/TC4 composite material with the Mo solid solution strengthening network structure, is obtained.
The nano-boron source in this embodiment can be replaced with other than TiB 2 Other than TiB 2 、B 4 One or more of the C and B powders
FIG. 4 is a graph showing the mechanical properties of the titanium-based composite materials prepared in examples 1-2 and the TC4 titanium alloy prepared in comparative example 1 and the titanium-based composite materials prepared in comparative examples 2-3, and it can be seen from FIG. 4 that, compared with the TC4 titanium alloy of comparative example 1, the Mo solution reinforced TC4 composite material of comparative example 2 and the TiC reinforced TC4 composite material of comparative example 3, the strength of the Mo solution reinforced reticular structure TiC/TC4 composite material of the invention is remarkably improved to 1500 MPa-1650 MPa, the room temperature elongation is more than 10%, the excellent strong plasticity matching level is achieved, the problem of disorder of strong plasticity in the prior art is overcome, and the preparation method of the invention is illustrated to overcome the problems of limited improvement of the performance and serious inversion of strong plasticity of the conventional powder metallurgy graphene reinforced titanium-based composite material.
Example 3
The embodiment comprises the following steps:
step one, selecting powder raw materials and synthesizing with low damage: spherical TC4 prealloy powder is used as titanium alloy matrix powder, and Mo is used as Mo 2 C and carbon black are respectively an intragranular solid solution strengthening reinforcing phase and a grain boundary reticular structure reinforcing body nano precursor, and 0.6g of spherical Mo with 20nm granularity is added 2 C. 0.36g of carbon black with the average size of 25nm is sequentially added into 120g of spherical TC4 titanium alloy powder, and the mixture is subjected to low-energy ball milling and mixing for 10 hours under the conditions of 200r/min of rotating speed and 5:1 of ball-to-material ratio, so that low-damage spherical Mo is obtained 2 C and carbon black uniformly dispersed titanium-based composite powder;
the spherical TC4 prealloy powder is prepared by a plasma rotary electrode method, has the granularity of 15-53 mu m, good sphericity and no planetary powder, and the chemical components meet the requirements of GB/T3620.1-2007 titanium and titanium alloy brand and chemical component standard;
preparing a titanium-based composite material: and (3) performing plasma activated sintering on the titanium-based composite powder obtained in the step (I), wherein the temperature of the plasma activated sintering is 1000 ℃, the temperature rising speed is 100 ℃/min, the heat preservation time is 5min, the pressure is 40MPa, a titanium-based composite material blank is obtained, and then the titanium-based composite material blank is rolled, wherein the rolling temperature is 900 ℃, the heat preservation time is 20min, and the rolling deformation is 75%, so that the ultrahigh-strength and high-toughness titanium-based composite material with the solid solution strengthening network structure, namely the TiC/TC4 composite material with the Mo solid solution strengthening network structure, is obtained.
The strength of the titanium-based composite material prepared by the embodiment is greater than 1500MPa, and the elongation is greater than 8 percent.
Example 4
The embodiment comprises the following steps:
step one, selecting powder raw materials and synthesizing with low damage: spherical TC4 prealloy powder is used as titanium alloy matrix powder, and Mo is used as Mo 2 C and TiB 2 Nano precursors of strengthening phases of intragranular solid solution and strengthening bodies of grain boundary net structure respectively, and 0.6g of spherical Mo with granularity of 500nm 2 C. 0.6g of TiB with an average size of 40nm 2 Sequentially adding 120g of spherical TC4 titanium alloy powder, and carrying out low-energy ball milling and mixing for 10 hours under the conditions of 200r/min rotating speed and 5:1 ball-material ratio to obtainTo low damage and spherical Mo 2 C and TiB 2 Uniformly dispersed titanium-based composite powder;
the spherical TC4 prealloy powder is prepared by a plasma rotary electrode method, has the granularity of 15-53 mu m, good sphericity and no planetary powder, and the chemical components meet the requirements of GB/T3620.1-2007 titanium and titanium alloy brand and chemical component standard;
preparing a titanium-based composite material: and (3) performing plasma activated sintering on the titanium-based composite powder obtained in the step (I), wherein the temperature of the plasma activated sintering is 1000 ℃, the temperature rising speed is 100 ℃/min, the heat preservation time is 5min, the pressure is 40MPa, a titanium-based composite material blank is obtained, and then the titanium-based composite material blank is rolled, wherein the rolling temperature is 900 ℃, the heat preservation time is 20min, and the rolling deformation is 75%, so that the ultra-high-strength and high-toughness titanium-based composite material with the solid solution strengthening network structure, namely the TiB/TC4 composite material with the Mo solid solution strengthening network structure, is obtained.
The strength of the titanium-based composite material prepared by the embodiment is greater than 1500MPa, and the elongation is greater than 8 percent.
Example 5
The embodiment comprises the following steps:
step one, selecting powder raw materials and synthesizing with low damage: spherical TC4 prealloy powder is used as titanium alloy matrix powder, and Mo is used as Mo 2 C and TiB 2 Nano precursors of strengthening phases of intragranular solid solution and strengthening bodies of grain boundary net structure respectively, and 0.6g of spherical Mo with granularity of 800nm 2 C. 0.36g of TiB with an average size of 40nm 2 Sequentially adding 120g of spherical TC4 titanium alloy powder, and carrying out low-energy ball milling and mixing for 5 hours under the conditions of 150r/min rotating speed and 5:1 ball material ratio to obtain low-damage spherical Mo 2 C and TiB 2 Uniformly dispersed titanium-based composite powder;
the spherical TC4 prealloy powder is prepared by a plasma rotary electrode method, has the granularity of 15-53 mu m, good sphericity and no planetary powder, and the chemical components meet the requirements of GB/T3620.1-2007 titanium and titanium alloy brand and chemical component standard;
preparing a titanium-based composite material: and (3) performing plasma activated sintering on the titanium-based composite powder obtained in the step one, wherein the temperature of the plasma activated sintering is 800 ℃, the temperature rising speed is 100 ℃/min, the heat preservation time is 10min, the pressure is 60MPa, a titanium-based composite material blank is obtained, and then the titanium-based composite material blank is rolled, wherein the rolling temperature is 800 ℃, the heat preservation time is 10min, and the rolling deformation is 90%, so that the ultra-high-strength and high-toughness titanium-based composite material with the solid solution strengthening network structure, namely the TiB/TC4 composite material with the Mo solid solution strengthening network structure, is obtained.
The strength of the titanium-based composite material prepared by the embodiment is greater than 1500MPa, and the elongation is greater than 8 percent.
Example 6
The embodiment comprises the following steps:
step one, selecting powder raw materials and synthesizing with low damage: spherical TC4 prealloy powder is used as titanium alloy matrix powder, and Mo is used as Mo 2 C and carbon black are respectively an intragranular solid solution strengthening reinforcing phase and a grain boundary reticular structure reinforcing body nano precursor, and 1.2g of spherical Mo with the granularity of 800nm is added 2 C. 0.36g of carbon black with the average size of 25nm is sequentially added into 120g of spherical TC4 titanium alloy powder, and the mixture is subjected to low-energy ball milling and mixing for 15 hours under the conditions of the rotating speed of 250r/min and the ball-to-material ratio of 5:1, so that low-damage spherical Mo is obtained 2 C and carbon black uniformly dispersed titanium-based composite powder;
the spherical TC4 prealloy powder is prepared by a plasma rotary electrode method, has the granularity of 15-53 mu m, good sphericity and no planetary powder, and the chemical components meet the requirements of GB/T3620.1-2007 titanium and titanium alloy brand and chemical component standard;
preparing a titanium-based composite material: and (3) performing plasma activated sintering on the titanium-based composite powder obtained in the step (I), wherein the temperature of the plasma activated sintering is 1100 ℃, the temperature rising speed is 100 ℃/min, the heat preservation time is 5min, the pressure is 30MPa, a titanium-based composite material blank is obtained, and then the titanium-based composite material blank is rolled, wherein the rolling temperature is 800 ℃, the heat preservation time is 30min, and the rolling deformation is 50%, so that the ultrahigh-strength and high-toughness titanium-based composite material with the solid solution strengthening network structure, namely the TiC/TC4 composite material with the Mo solid solution strengthening network structure, is obtained.
The strength of the titanium-based composite material prepared by the embodiment is greater than 1500MPa, and the elongation is greater than 8 percent.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the present invention. Any simple modification, variation and equivalent variation of the above embodiments according to the technical substance of the invention still fall within the scope of the technical solution of the invention.
Claims (8)
1. The preparation method of the ultrahigh-strength and high-toughness titanium-based composite material with the solid solution strengthening net structure is characterized by comprising the following steps of:
step one, selecting powder raw materials and synthesizing with low damage: the spherical TC4 prealloy powder prepared by a rotary electrode method is used as titanium alloy matrix powder, nano carbide containing beta stable elements and a nano carbon source/boron source are respectively used as an intragranular solid solution strengthening reinforcing phase and a grain boundary reticular structure reinforcing body nano precursor, and the nano carbide containing the beta stable elements and the nano carbon source/boron source are sequentially added into the titanium alloy matrix powder for multi-step low-energy ball milling mixing, so that low-damage titanium-based composite powder with uniformly dispersed nano carbide and nano carbon source/boron source is obtained;
preparing a titanium-based composite material: densification and rapid sintering are carried out on the titanium-based composite powder obtained in the step one, a titanium-based composite material blank is obtained, and then the solid solution strengthening net-shaped structure ultrahigh-strength and high-toughness titanium-based composite material is obtained through thermal deformation processing; the strength of the ultrahigh-strength and high-toughness titanium-based composite material with the solid solution strengthening reticular structure is more than 1500MPa, and the elongation is more than 8%.
2. The method for preparing the ultra-high strength and toughness titanium-based composite material with the solid solution strengthening reticular structure, which is characterized in that in the first step, the spherical TC4 prealloy powder is prepared by a plasma rotary electrode method, the granularity is 15-53 mu m, the sphericity is good, no planetary powder exists, and the chemical composition meets the requirements of GB/T3620.1-2007 titanium and titanium alloy brands and chemical composition standards; the nano carbide containing the beta stabilizing element is spherical Mo 2 C powder with granularity of 20-800 nm.
3. The method for preparing the ultrahigh-strength and high-toughness titanium-based composite material with the solid solution strengthening network structure according to claim 1, wherein in the first step, the nano carbon source is reduced graphene oxide or carbon black particles, the sheet diameter of the reduced graphene oxide is 4-7 μm, the thickness is 5nm, and the average size of the carbon black particles is 25nm.
4. The method for preparing a solid solution strengthening net structured ultra-high strength and toughness titanium-based composite material according to claim 1, wherein in the first step, the nano boron source is TiB 2 、B 4 One or more of the C and B powders, and TiB 2 The average size of the powder was 40nm.
5. The method for preparing the ultrahigh-strength and high-toughness titanium-based composite material with the solid solution strengthening reticular structure, which is characterized in that the rotating speed of the multi-step low-energy ball milling and mixing in the first step is 150-250 r/min, the ball milling time is 5-10 h, and the ball-material ratio is 5:1.
6. The method for preparing the ultrahigh-strength and high-toughness titanium-based composite material with the solid solution strengthening network structure according to claim 1, wherein in the second step, the densification rapid sintering is plasma activated sintering, hot press sintering or hot isostatic pressing sintering, the temperature of the plasma activated sintering is 800-1100 ℃, the heating rate is 100 ℃/min, the heat preservation time is 5-10 min, and the pressure is 30-60 MPa.
7. The method for preparing the ultrahigh-strength and high-toughness titanium-based composite material with the solid solution strengthening net structure according to claim 1, wherein in the second step, the thermal deformation processing is rolling, the rolling temperature is 800-1000 ℃, the heat preservation time is 10-30 min, and the rolling deformation is 50-90%.
8. A solution-strengthened network structure ultrahigh-strength and high-toughness titanium-based composite material, characterized in that the composite material is prepared by the method of any one of claims 1-7.
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