CN115852190B - Directional arrangement TiB reinforced titanium-based composite material and preparation method and application thereof - Google Patents
Directional arrangement TiB reinforced titanium-based composite material and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to the technical field of titanium alloy, in particular to a directional arrangement TiB reinforced titanium-based composite material, and a preparation method and application thereof. The invention provides a preparation method of a directional arrangement TiB reinforced titanium-based composite material, which comprises the following steps: mixing a boron source and titanium alloy, and performing ball milling to obtain mixed powder; the rotation speed of the ball milling is 300-600 r/min; sequentially carrying out annealing treatment, vibration and rapid hot-pressing sintering treatment on the mixed powder to obtain the directional arrangement TiB reinforced titanium-based composite material; the heating rate of the rapid hot-pressing sintering treatment is 100-300 ℃/min. The preparation method can realize directional arrangement of TiB and enhance the high dynamic performance of the titanium-based composite material.
Description
Technical Field
The invention belongs to the technical field of titanium alloy, and particularly relates to a directional arrangement TiB reinforced titanium-based composite material, and a preparation method and application thereof.
Background
Currently, steel is the primary protective material because of its high density (7.8 g/cm 3 ) Is unfavorable for light combat, and directly affects the maneuverability and the survivability of the battlefield. For light material titanium alloy, the titanium alloy has the advantages of small density, high specific strength and the like, chinese patent CN201510421029.1 discloses a high dynamic performance near alpha titanium alloy and a preparation method thereof, and discloses the traditional TC4 titanium alloy which has low dynamic performance and average rheological stress of about 1319MPa and cannot meet the increasingly-promoted requirement. The titanium-based composite material has better performance than titanium alloy, and is widely focused by researchers, and is widely applied to the fields of aerospace, weapons, ships and the like. Among them, the one-dimensional TiB whisker has a similar thermal expansion coefficient to the titanium matrix and high thermodynamic stability, so that it has a firm interface bonding capability with the titanium matrix, and therefore, it is regarded as an ideal reinforcing material in the titanium matrix composite material.
Ma Fengcang, et al, shanghai university of transportation (Mechanical properties and strengthening effects of in situ (TiB+TiC)/Ti-1100 composite at elevated temperatures[J ]. Materials Science and Engineering: A, 2016, 654: 352-358.) studied the effect of different orientations of TiB on the strength of titanium-based composite materials by experimental and computational methods, and the results of the study showed that the regulation of the orientation angle of TiB whiskers could be achieved by adjusting extrusion ratio, and that when the directions of whiskers and applied stresses were the same, the reinforcing efficiency of TiB was the highest. Zhang Changjiang et al (Evolution of microstructural characteristic and tensile properties during preparation of TiB/Ti composite sheet [ J ]. Materials & Design (1980-2015), 2012, 36:505-510) at Harbin university of industry also regulates the orientation of TiB by rolling, improving the strength of TiB reinforced titanium matrix composites. Although the TiB can obtain uniform orientation by deformation modes such as hot rolling and hot extrusion, the TiB orientation obtained by the modes is not consistent with the loading direction of the protective material, and the strengthening effect of the TiB whisker is difficult to be exerted to the greatest extent.
Therefore, how to prepare TiB reinforced phases which are arranged in an oriented manner and consistent with the dynamic loading direction, and at the same time, tiB reinforced titanium-based composite materials with high dynamic performance are the problems of various nationists at present.
Disclosure of Invention
The invention aims to provide a directional arrangement TiB reinforced titanium-based composite material, and a preparation method and application thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a directional arrangement TiB reinforced titanium-based composite material, which comprises the following steps:
mixing a boron source and titanium alloy, and performing ball milling to obtain mixed powder; the rotation speed of the ball milling is 300-600 r/min;
sequentially carrying out annealing treatment, vibration and rapid hot-pressing sintering treatment on the mixed powder to obtain the directional arrangement TiB reinforced titanium-based composite material;
the heating rate of the rapid hot-pressing sintering treatment is 100-300 ℃/min.
Preferably, the boron source comprises B or TiB 2 。
Preferably, the mass ratio of the boron source to the titanium alloy is (0.1-10.0): (99.9 to 90.0).
Preferably, the grain diameter of the titanium alloy is less than or equal to 60 mu m;
the particle size of the boron source is less than or equal to 100nm.
Preferably, the ball milling mode is wet ball milling; the ball milling medium of the wet ball milling is absolute ethyl alcohol;
the diameter of a grinding ball used for ball milling is 3-10 mm, and the ball-to-material ratio is (10-50): and 1, ball milling is carried out for 8-36 hours.
Preferably, after the wet ball milling is completed, the method further comprises the step of cleaning the obtained mixed slurry;
the cleaning agent adopted in the cleaning is absolute ethyl alcohol, and the cleaning times are 3-6 times.
Preferably, the annealing treatment is carried out at a temperature of 450-650 ℃ for 1-4 hours.
Preferably, the rapid hot-press sintering treatment mode is spark plasma sintering or rapid hot-press sintering;
the temperature of the rapid hot pressing sintering treatment is 850-1150 ℃, the pressure is 15-80 MPa, and the time is 5-30 min.
The invention also provides the directional arrangement TiB reinforced titanium-based composite material prepared by the preparation method.
The invention also provides application of the directional arrangement TiB reinforced titanium-based composite material in the fields of aerospace, weapons or ships.
The invention provides a preparation method of a directional arrangement TiB reinforced titanium-based composite material, which comprises the following steps: mixing a boron source and titanium alloy, and performing ball milling to obtain mixed powder; the rotation speed of the ball milling is 300-600 r/min; sequentially carrying out annealing treatment, vibration and rapid hot-pressing sintering treatment on the mixed powder to obtain the directional arrangement TiB reinforced titanium-based composite material; the heating rate of the rapid hot-pressing sintering treatment is 100-300 ℃/min. The invention adopts the ball milling process with the rotating speed to grind the titanium alloy into flake powder, thereby refining the grain size of the matrix powder; the boron source is uniformly dispersed on the surface of the titanium alloy powder, and in addition, as the flaky powder has larger length-diameter ratio (diameter: thickness), the boron source is mainly distributed on two surfaces of the flaky powder, which lays a foundation for generating TiB whiskers which are directionally distributed; meanwhile, the vibration can enable the mixed flaky powder to be arranged according to the mutually overlapped sequence, so that the TiB whisker is ensured to grow in an oriented manner along the pressurizing direction; the rapid hot-pressing sintering treatment can prepare a composite material with high density and small grain size, tiB nanowhiskers generated in situ in the sintering process have clean surfaces, are uniformly distributed in a matrix without agglomeration, and have good interface combination with a titanium matrix; the TiB whisker grows directionally, is consistent with the pressurizing direction, can exert the strengthening effect of the TiB whisker to the greatest extent according to a load transfer mechanism, and obviously improves the mechanical property of the composite material; finally, the preparation method provided by the invention is simple and feasible, short in period and strong in practicability, and is beneficial to realizing industrial production.
Drawings
FIG. 1 is a microstructure of the annealed mixed powder prepared in example 1;
FIG. 2 is a graph of the microstructure profile of the side of the titanium matrix composite of example 1;
FIG. 3 is a microstructure topography of the bottom surface of the titanium-based composite of example 1.
Detailed Description
The invention provides a preparation method of a directional arrangement TiB reinforced titanium-based composite material, which comprises the following steps:
mixing a boron source and titanium alloy, and performing ball milling to obtain mixed powder; the rotation speed of the ball milling is 300-600 r/min;
sequentially carrying out annealing treatment, vibration and rapid hot-pressing sintering treatment on the mixed powder to obtain the directional arrangement TiB reinforced titanium-based composite material;
the heating rate of the rapid hot-pressing sintering treatment is 100-300 ℃/min.
In the present invention, all the preparation materials are commercially available products well known to those skilled in the art unless specified otherwise.
Mixing a boron source and titanium alloy, and performing ball milling to obtain mixed powder; the rotation speed of the ball milling is 300-600 r/min.
In the present invention, the particle size of the boron source is preferably 100nm or less; in the present invention, the boron source preferably comprises B or TiB 2 。
In the present invention, the grain size of the titanium alloy is preferably 60 μm or less. In the present invention, the titanium alloy is preferably a TC4 alloy.
In the invention, the mass ratio of the boron source to the titanium alloy is preferably (0.1-10.0): (99.9 to 90.0), more preferably (2.0 to 8.0): (99.0 to 91.0), most preferably (4.0 to 6.0): (96.0 to 94.0).
In the invention, the ball milling mode is preferably wet ball milling, and the ball milling medium of the wet ball milling is absolute ethyl alcohol; the amount of the absolute ethyl alcohol is not particularly limited in the present invention, and may be any amount known to those skilled in the art. In the invention, the diameter of the grinding ball used for ball milling is preferably 3-10 mm, more preferably 4-8 mm, and most preferably 5-6 mm; the ball-to-material ratio is preferably (10-50): 1, more preferably (20 to 40): 1, most preferably (25 to 35): 1, a step of; the ball milling time is preferably 8-36 hours, more preferably 10-30 hours, and most preferably 15-25 hours; the rotation speed of the ball milling is 300-600 r/min, preferably 350-550 r/min, and more preferably 400-500 r/min.
After the wet ball milling is finished, the invention also preferably comprises the step of cleaning the obtained mixed slurry;
the cleaning agent used for cleaning is preferably absolute ethyl alcohol, and the cleaning times are preferably 3-6 times, more preferably 4-5 times. In the invention, the cleaning process is preferably to keep the mixed slurry for 10-30 min, remove the suspension at the upper layer, add absolute ethyl alcohol, stir, keep the mixture for 10-30 min, remove the suspension, and repeat for 3-5 times.
In the invention, the cleaning function is to remove impurities such as oxides and the like introduced in the ball milling process, thereby greatly increasing the brittleness of the titanium-based composite material. Impurities are removed by repeated washing.
After the cleaning is finished, the method also preferably comprises rotary steaming and drying which are sequentially carried out; the process of spin-steaming and drying is not particularly limited in the present invention, and may be performed by a process well known to those skilled in the art.
After the mixed powder is obtained, the mixed powder is subjected to annealing treatment, vibration and rapid hot-pressing sintering treatment in sequence, so that the directional arrangement TiB reinforced titanium-based composite material is obtained.
In the invention, the temperature of the annealing treatment is preferably 450-650 ℃, more preferably 500-600 ℃, and most preferably 530-560 ℃; the time is preferably 1 to 4 hours, more preferably 2 to 3 hours.
In the present invention, the annealing treatment is preferably performed in a vacuum heat treatment furnace.
In the present invention, the annealing treatment serves to eliminate stress concentration generated during the ball milling process.
In the present invention, the process of shaking is preferably to put the mixed powder into a cylindrical graphite mold, and put the mold into a high-speed oscillator for shaking. The condition of the oscillation is not particularly limited in the present invention, and may be performed by using a condition well known to those skilled in the art.
In the invention, the vibration can enable the mixed flaky powder to be arranged according to the mutually overlapped sequence, thereby further ensuring the directional growth of TiB whiskers along the pressurizing direction.
In the invention, the rapid hot press sintering treatment mode is preferably spark plasma sintering or rapid hot press sintering.
In the invention, the temperature of the rapid hot pressed sintering treatment is preferably 850-1150 ℃, more preferably 900-1100 ℃, and most preferably 950-1050 ℃; the heating rate is 100-300 ℃/min, preferably 100-200 ℃/min; the pressure is preferably 15-80 MPa, more preferably 30-70 MPa, and most preferably 40-60 MPa; the time is preferably 5 to 30min, more preferably 10 to 25min, and most preferably 15 to 20min.
In the invention, the rapid hot-pressing sintering treatment is preferably carried out by placing a cylindrical graphite mold filled with mixed powder in a rapid hot-pressing sintering system for sintering.
In the invention, the rapid hot-pressing sintering treatment realizes metallurgical bonding among powders, obtains TiB generated in situ, and obtains the TiB reinforced titanium-based composite material with orientation consistent with the pressurizing direction. The prepared directional arrangement TiB reinforced titanium-based composite material has high density and small grain size by controlling the conditions of the rapid hot-pressing sintering.
The invention also provides the directional arrangement TiB reinforced titanium-based composite material prepared by the preparation method.
The invention also provides application of the directional arrangement TiB reinforced titanium-based composite material in the fields of aerospace, weapons or ships. The method of the present invention is not particularly limited, and may be carried out by methods known to those skilled in the art.
The titanium-based composite material, the preparation method and application thereof provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Note that: the TC4 powders of examples 1-3 and comparative examples 1-2 were all purchased from Beijing Xingrong sources, inc., were nearly spherical, had a particle size of 15-60 μm, an average particle size of 40 μm, and had a purity of 99.9wt% or more;
nano TiB 2 The powder is purchased from Shanghai super-Wei nano technology Co., ltd, the purity is more than or equal to 99.5wt%, and the particle size is 50-100 nm;
absolute ethanol is produced by Beijing Tong Guangdong fine chemical company;
the rapid hot press sintering system is purchased from FHP-828, a company of haven, su;
example 1
0.02g of nano TiB 2 Adding the powder and 19.98g of TC4 powder into a ball milling tank of a planetary ball mill, adding grinding balls with the diameter of 6mm according to the mass ratio of the balls to the materials of 10:1, adding excessive absolute ethyl alcohol, and ball milling for 8 hours at the rotating speed of 600r/min to obtain mixed slurry;
standing the mixed slurry for 10min, removing the suspension at the upper layer, adding absolute ethyl alcohol for cleaning, repeating for 3 times to remove oxides, pouring the cleaned slurry into a vacuum rotary evaporator, performing rotary evaporation drying to obtain mixed powder, and placing the mixed powder into a vacuum annealing treatment furnace for annealing at 450 ℃ for 4h to obtain annealed mixed powder;
and placing 20g of the annealed mixed powder into a cylindrical graphite mold, placing the mold into a high-speed oscillator for oscillation, enabling TC4 flaky powder to be arranged according to the mutual lamination sequence, placing the mold into a rapid hot-pressing sintering system for sintering, wherein the sintering temperature is 850 ℃ (the heating rate is 100 ℃/min), the sintering pressure is 80MPa, the heat preservation time is 30min, taking out a composite material block obtained after sintering, and polishing by sand paper to remove graphite paper on the surface of the block to obtain the titanium-based composite material.
Example 2
1g of nano TiB 2 Adding the powder and 19g of TC4 powder into a ball milling tank of a planetary ball mill, adding grinding balls with the diameter of 5mm according to the ball material mass ratio of 30:1, adding excessive absolute ethyl alcohol, and ball milling for 24 hours at the rotating speed of 400r/min to obtain mixed slurry;
standing the mixed slurry for 20min, removing the suspension at the upper layer, adding absolute ethyl alcohol for cleaning, repeating for 4 times to remove oxides, pouring the cleaned slurry into a vacuum rotary evaporator, performing rotary evaporation drying to obtain mixed powder, and placing the mixed powder into a vacuum annealing treatment furnace for annealing at 550 ℃ for 2h to obtain annealed mixed powder;
and placing 20g of the annealed mixed powder into a cylindrical graphite mold, placing the mold into a high-speed oscillator for oscillation, enabling TC4 flaky powder to be arranged according to the mutual lamination sequence, placing the mold into a rapid hot-pressing sintering system for sintering, wherein the sintering temperature is 950 ℃ (the heating rate is 100 ℃/min), the sintering pressure is 50MPa, the heat preservation time is 10min, taking out a composite material block obtained after sintering, and polishing by sand paper to remove graphite paper on the surface of the block to obtain the titanium-based composite material.
Example 3
2g of nano TiB 2 Adding the powder and 18g of TC4 powder into a ball milling tank of a planetary ball mill, adding grinding balls with the diameter of 3mm according to the ball material mass ratio of 50:1, adding excessive absolute ethyl alcohol, and ball milling for 36 hours at the rotating speed of 300r/min to obtain mixed slurry;
standing the mixed slurry for 30min, removing the suspension on the upper layer, adding absolute ethyl alcohol for cleaning, repeating for 5 times to remove oxides, pouring the cleaned slurry into a vacuum rotary evaporator, performing rotary evaporation drying to obtain mixed powder, and placing the mixed powder into a vacuum annealing treatment furnace for annealing at 650 ℃ for 1h to obtain annealed mixed powder;
and placing 20g of the annealed mixed powder into a cylindrical graphite mold, placing the mold into a high-speed oscillator for oscillation, enabling TC4 flaky powder to be arranged according to the mutual lamination sequence, placing the mold into a rapid hot-pressing sintering system for sintering, wherein the sintering temperature is 1150 ℃, the sintering pressure is 20MPa, the heat preservation time is 5min, taking out a composite material block obtained after sintering, and polishing graphite paper on the surface of the block by sand paper to obtain the titanium-based composite material.
Comparative example 1
0.02g of nano TiB 2 Adding the powder and 19.98g of TC4 powder into a ball milling tank of a planetary ball mill, adding grinding balls with the diameter of 5mm according to the mass ratio of ball materials of 10:1, adding excessive absolute ethyl alcohol, and ball milling for 8 hours at the rotating speed of 200r/min to obtain mixed slurry;
pouring the mixed slurry into a vacuum rotary evaporator, and performing rotary evaporation drying to obtain mixed powder;
and (3) placing the mixed powder into a cylindrical graphite mould, placing the mould into a rapid hot-pressing sintering system for sintering, wherein the sintering temperature is 850 ℃, the sintering pressure is 80MPa, the heat preservation time is 30min, taking out a composite material block obtained after sintering, and polishing by sand paper to remove graphite paper on the surface of the block to obtain the titanium-based composite material.
Comparative example 2
Putting TC4 powder into a cylindrical graphite mould, putting the mould into a rapid hot-pressing sintering system for sintering, wherein the sintering temperature is 850 ℃, the sintering pressure is 80MPa, the heat preservation time is 30min, taking out a TC4 block obtained after sintering, and polishing by sand paper to remove graphite paper on the surface of the block to obtain the titanium-based composite material.
Test case
Microstructure observation (using a field emission scanning electron microscope (SEM, hitachi S-4800N, hitachi, japan)) was performed on the titanium-based composite materials described in examples 1 to 3 and comparative examples 1 to 2:
wherein FIG. 1 is a microstructure of the annealed mixed powder prepared in example 1. As can be seen from FIG. 1, the original spherical TC4 powder is flaked under the high-speed action of the grinding balls after ball milling, while nano TiB 2 The powder is uniformly distributed on the surface of the flaky TC4 powder, and the flaky TC4 powder can effectively promote the in-situ generated TiB to grow in an oriented manner along the surface of the vertical TC4 powder;
fig. 2 is a microstructure chart of a side surface of the titanium-based composite material in example 1, fig. 3 is a microstructure chart of a bottom surface of the titanium-based composite material in example 1, and as can be seen from fig. 2 to 3, tiB on a surface along a pressurizing direction appears to be rod-shaped, while TiB perpendicular to the pressurizing direction only shows that an end surface appears to be granular, which indicates that TiB whiskers grow directionally along the pressurizing direction, i.e., grow perpendicular to a surface of the original flaky TC4 powder;
the titanium-based composite materials described in examples 1 to 3 and comparative examples 1 to 2 were subjected to mechanical property test, dynamic property test was performed on a split hopkins bar (SHPB), each sample was tested five times, and the average value thereof was taken as the actual property of the sample. The method can obtain the following performance parameters of the composite material: dynamic strength and dynamic strain; the test results are: mechanical properties of the titanium-based composite described in example 1: the dynamic strength is 1513MPa, and the dynamic strain is 23%; mechanical properties of the titanium-based composite described in example 2: dynamic strength is 1620MPa, and fracture strain is 18%; mechanical properties of the titanium-based composite described in example 3: the dynamic strength was 2130MPa and the dynamic strain was 9%. The compressive strength of the titanium-based composite material described in comparative example 1 was 1341MPa, and the strain at break was 18%. The dynamic strength of the titanium-based composite material described in comparative example 2 was 1258MPa, and the dynamic strain was 19%. Compared with comparative examples 1 and 2, the average rheological stress of the composite materials prepared in examples 1, 2 and 3 is greatly improved compared with comparative examples 1 and 2, because the TiB reinforced titanium-based composite material consistent with the loading direction is prepared in the examples through structural design, the stress bearing effect of TiB whiskers is exerted to the greatest extent, the matrix is reinforced, and the strength of the composite material is improved.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (10)
1. The preparation method of the directional arrangement TiB reinforced titanium-based composite material is characterized by comprising the following steps of:
mixing a boron source and titanium alloy, and performing ball milling to obtain mixed powder; the rotation speed of the ball milling is 300-600 r/min;
sequentially carrying out annealing treatment, vibration and rapid hot-pressing sintering treatment on the mixed powder to obtain the directional arrangement TiB reinforced titanium-based composite material;
the heating rate of the rapid hot-pressing sintering treatment is 100-300 ℃/min;
the diameter of a grinding ball used for ball milling is 3-10 mm, and the ball-to-material ratio is (20-50): 1, ball milling is carried out for 8-36 hours;
the temperature of the rapid hot pressing sintering treatment is 850-1150 ℃, the pressure is 15-80 MPa, and the time is 5-30 min.
2. The method of claim 1, wherein the boron source comprises B or TiB 2 。
3. The production method according to claim 2, wherein the mass ratio of the boron source to the titanium alloy is (0.1 to 10.0): (99.9 to 90.0).
4. The method according to claim 3, wherein the titanium alloy has a particle size of 60 μm or less;
the particle size of the boron source is less than or equal to 100nm.
5. The method according to any one of claims 1 to 4, wherein the ball milling is performed by wet ball milling; the ball milling medium of the wet ball milling is absolute ethyl alcohol.
6. The method according to claim 5, further comprising washing the obtained mixed slurry after the wet ball milling is completed;
the cleaning agent adopted in the cleaning is absolute ethyl alcohol, and the cleaning times are 3-6 times.
7. The method according to claim 1, wherein the annealing treatment is performed at a temperature of 450 to 650 ℃ for 1 to 4 hours.
8. The method of claim 1, wherein the rapid thermal sintering process is spark plasma sintering or rapid thermal sintering.
9. The directionally arranged TiB reinforced titanium-based composite material prepared by the preparation method of any one of claims 1-8.
10. The use of the directionally arranged TiB-reinforced titanium-based composite of claim 9 in the field of aerospace, weapons, or marine applications.
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| CN108796264B (en) * | 2018-06-28 | 2020-06-09 | 北京理工大学 | Preparation method of TiB whisker reinforced titanium-based composite material in oriented arrangement |
| CN109136608B (en) * | 2018-08-22 | 2020-06-09 | 北京理工大学 | Preparation method of TiB whisker reinforced titanium-based composite material with controllable orientation |
| CN109112439B (en) * | 2018-10-08 | 2020-07-14 | 中国科学院上海硅酸盐研究所 | Whisker oriented reinforced aluminum-based composite material and preparation method thereof |
| CN111945027B (en) * | 2020-07-29 | 2022-01-28 | 北京理工大学 | Method for strengthening GNPs/Ti composite material interface combination by directional growth of TiBw |
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