CN110499432B - Preparation method of controllable reticular titanium carbide framework structure titanium-based material - Google Patents
Preparation method of controllable reticular titanium carbide framework structure titanium-based material Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- 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
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
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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
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/058—Mixtures of metal powder with non-metallic powder by reaction sintering (i.e. gasless reaction starting from a mixture of solid metal compounds)
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/005—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
- C22C29/067—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds comprising a particular metallic binder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
- C22C29/10—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds based on titanium carbide
Abstract
The invention discloses a preparation method of a controllable reticular titanium carbide framework structure titanium-based material, which comprises the following steps: firstly, putting graphite flakes with the width of 1-20 mu m and the thickness of 5-30 nm and titanium powder or titanium alloy powder with the granularity of 30-500 mu m into a planetary ball mill for ball milling and mixing to obtain mixed powder; and secondly, performing discharge plasma sintering on the mixed powder above the phase transition temperature of the corresponding titanium or titanium alloy, and cooling the mixed powder to room temperature along with the furnace to obtain the titanium-based material with the reticular titanium carbide framework structure. According to the invention, the size and the content of the raw material powder are controlled to adjust the distribution of the titanium carbide generated in situ in the titanium-based material to generate a continuous regular reticular titanium carbide framework structure, so that the titanium-based material with the reticular titanium carbide framework structure is obtained, the defect of discrete particle distribution in the titanium carbide generation process is overcome, the control of the reticular shape and the mesh size of the titanium carbide framework structure is realized, and the reinforcing phase effect of the titanium carbide is improved.
Description
Technical Field
The invention belongs to the technical field of metal matrix composite material preparation, and particularly relates to a preparation method of a controllable reticular titanium carbide framework structure titanium-based material.
Background
The titanium alloy is a light alloy with excellent mechanical property and corrosion resistance, and is used as a key structural material for manufacturing parts of airplanes, ships and automobiles. The finished titanium alloy mainly contains an alpha phase with a close-packed hexagonal structure and a beta phase with a body-centered cubic structure, and the structure and the performance of the titanium alloy are regulated and controlled by controlling the content, the orientation, the distribution and the shape of the two phases. Titanium carbide is a supersaturated precipitated phase of carbon element in a titanium matrix, the solid solubility of the carbon element in the titanium alloy matrix is low, the solid solubility limits of alpha phase and beta phase are 0.48% and 0.15% respectively at 920 ℃, and the addition of 0.1% of the carbon element in the titanium alloy can cause the carbon element to be supersaturated at room temperature to precipitate the titanium carbide. The titanium carbide has high strength, friction and abrasion resistance and stable high-temperature performance, and the addition of the titanium carbide as a reinforcing phase in the titanium alloy is an effective way for improving the performance of a titanium alloy matrix. Generally speaking, the titanium carbide precipitated in situ is a particle phase, and is discretely distributed in a titanium matrix as micron or nanometer titanium carbide particles, lacks certain structural characteristics and spatial continuity, and mainly plays a reinforcing role, such as a double-scale carbon carbide particle reinforced titanium-based composite material disclosed in CN 106929702 and a preparation method thereof.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a method for preparing a titanium-based material with a controllable mesh titanium carbide skeleton structure, aiming at the defects of the prior art. The method adjusts the distribution of the titanium carbide generated in situ in the titanium-based material by controlling the size and the content of the raw material powder to generate a continuous regular reticular titanium carbide framework structure, so that the titanium-based material with the reticular titanium carbide framework structure is obtained, the defect of discrete particle distribution in the titanium carbide generation process is overcome, the control of the reticular shape and the mesh size of the titanium carbide framework structure is realized, and the reinforcing phase effect of the titanium carbide is improved.
In order to solve the technical problems, the invention adopts the technical scheme that: a preparation method of a controllable reticular titanium carbide framework structure titanium-based material is characterized by comprising the following steps:
putting graphite flakes with the width of 1-20 microns and the thickness of 5-30 nm and titanium powder or titanium alloy powder with the granularity of 35-100 microns into a planetary ball mill for ball milling and mixing to obtain mixed powder;
and step two, performing discharge plasma sintering on the mixed powder obtained in the step one above the phase transition temperature of the corresponding titanium or titanium alloy, and cooling the mixed powder to room temperature along with a furnace to obtain the titanium-based material with the reticular titanium carbide framework structure.
The invention adopts graphite flakes with the width of 1-20 mu m and the thickness of 5-30 nm and titanium powder or titanium alloy powder with the granularity of 30-500 mu m as raw materials to carry out ball milling and mixing, a large number of defects are introduced on the surfaces of the graphite flake and the titanium powder or the titanium alloy powder through the high-energy ball milling process, the surface chemical properties of the graphite flake and the titanium powder or the titanium alloy powder are improved, the activation effect is achieved, the graphite flake has a flake structure and the size of the graphite flake is far smaller than that of the titanium powder or the titanium alloy powder, the graphite flake is easy to attach to the surface of the titanium powder or the titanium alloy powder in the ball milling and mixing process to form mixed powder with the graphite flake in a net distribution, then the discharge plasma sintering is carried out in a beta single-phase area above the phase transition temperature of the corresponding titanium powder or titanium alloy in the mixed powder, in the process, the carbon element in the graphite sheet is fully diffused to the titanium powder or the titanium alloy powder near the contact surface of the graphite sheet and the titanium powder or the titanium alloy powder to generate chemical reaction: ti + C → TiC, the graphite flake distributed in the net shape generates a continuous regular net-shaped titanium carbide skeleton structure in situ, the titanium powder or titanium alloy powder in the middle of the net-shaped structure generates a titanium or titanium alloy matrix, the interface of the titanium carbide distributed in the net shape and the titanium or titanium alloy matrix is well combined, no obvious pore and defect exist, the titanium-based material with the net-shaped titanium carbide skeleton structure is obtained, and the defect of discrete particle distribution in the titanium carbide generation process is overcome. The invention controls the sizes and contents of the raw material graphite flakes and the titanium or titanium alloy powder to adjust the distribution of the titanium carbide generated in situ in the titanium-based material, thereby realizing the control of the mesh shape and the mesh size of the titanium carbide framework structure, improving the reinforcing phase effect of the titanium carbide and improving the performance of the titanium-based material.
The preparation method of the controllable reticular titanium carbide framework structure titanium-based material is characterized in that the mass content of the graphite flakes in the mixed powder in the first step is 0.3% -17%. The addition of the graphite flake avoids the formation of solid solution due to too low content of C element and the reduction of plasticity of the titanium-based material due to a great amount of TiC precipitated due to too high content of C element, thereby further improving the phase-strengthening effect of the titanium carbide.
The preparation method of the titanium-based material with the controllable reticular titanium carbide skeleton structure is characterized in that in the first step, the rotation speed for ball milling and mixing is 300-400 r/s, the ball-material ratio is (3:1) - (6:1), and the total volume of the balls accounts for one half of the volume of a revolving drum of the planetary ball mill. The ball milling parameters described above have relatively high energies that facilitate the thorough mixing of the graphite flakes with the titanium or titanium alloy powder and the introduction of crystal defects on the surface of the powder. The surface chemical properties of the graphite flake and the titanium alloy powder are improved, the graphite flake is promoted to be easily attached to the surface of the titanium powder or the titanium alloy powder, and mixed powder with the graphite flake in net distribution is formed.
The preparation method of the controllable reticular titanium carbide framework structure titanium-based material is characterized in that the technological parameters of the spark plasma sintering in the second step are as follows: the temperature is not less than 900 ℃, the vacuum degree is not more than 0.1MPa, the pressure is not less than 40MPa, the temperature rise speed is 70-120 ℃/min, and the sintering time is 5-10 min. The density of the graphite flake is 2.2g/cm3The density of the titanium alloy is 4.5g/cm3The density of the titanium carbide is 4.93g/cm3Therefore, the chemical reaction of Ti + C → TiC in the process of in-situ generation of titanium carbide in the invention is accompanied by volume shrinkage of about 25%. The square electric plasma sintering is carried out by adopting the process parameters, the pores formed by volume shrinkage are eliminated under the pressure action of not less than 40MPa, and the control on the reticular titanium carbide skeleton structure is further realized.
Compared with the prior art, the invention has the following advantages:
1. the invention adjusts the distribution of the titanium carbide generated in situ in the titanium-based material by controlling the size and the content of the raw material powder to generate a continuous regular reticular titanium carbide skeleton structure, obtains the titanium-based material with the reticular titanium carbide skeleton structure, overcomes the defect of discrete particle distribution in the titanium carbide generation process, realizes the control of the reticular shape and the mesh size of the titanium carbide skeleton structure, improves the reinforcing phase effect of the titanium carbide, improves the performance of the titanium-based material, and particularly plays a strong role in attenuating the vibration of a certain specific frequency.
2. According to the invention, a large number of defects are introduced on the surfaces of the graphite flake, the titanium powder or the titanium alloy powder through high-energy ball milling, so that the surface chemical properties of the graphite flake, the titanium powder or the titanium alloy powder are improved, an activation effect is achieved, and the rapid and sufficient progress of a titanium carbide generation reaction in the subsequent sintering process is promoted.
3. The invention adopts a pressurizing method in the sintering process to eliminate pores formed by volume shrinkage due to the difference between the density of the raw material and the density of the titanium carbide product, and further realizes the control of the reticular titanium carbide skeleton structure.
4. The method has the advantages of simple process, low cost, easy operation and easy realization of industrial production.
The technical solution of the present invention is further described in detail by the accompanying drawings and examples.
Drawings
FIG. 1 is a microstructure diagram of a Ti-Cr-Sn material with a reticular titanium carbide skeleton structure prepared in example 1 of the present invention.
FIG. 2 is an X-ray diffraction pattern of a Ti-Cr-Sn material having a net-like titanium carbide skeleton structure prepared in example 1 of the present invention.
Detailed Description
Example 1
The method of the embodiment comprises the following steps:
step one, putting 0.6g of graphite flakes with the width of 1-20 microns and the thickness of 5-30 nm and 200g of spherical Ti-Cr-Sn titanium alloy powder with the granularity of 100 microns into a planetary ball mill for ball milling and mixing to obtain mixed powder; the rotation speed of ball milling mixing is 300 revolutions per second, and the ball-material ratio is 4: 1, the total volume of the ball materials accounts for one half of the volume of a revolving drum of the planetary ball mill, and the ball milling time is 3 hours;
step two, putting the mixed powder obtained in the step one into a die with the diameter of 60mm, then putting the die into a spark plasma sintering furnace of SPS-80-T-20 for spark plasma sintering, and cooling the die to room temperature to obtain a Ti-Cr-Sn material with a reticular titanium carbide skeleton structure; the sintering process parameters are as follows: the temperature is 900 ℃, the vacuum degree is 0.1MPa, the pressure is 60MPa, the temperature rise speed is 100 ℃/min, and the sintering time is 5 min.
Through detection, the equivalent diameter of the reticular pores in the reticular titanium carbide skeleton structure Ti-Cr-Sn material obtained in the embodiment is 100 μm.
Fig. 1 is a microstructure diagram of the Ti-Cr-Sn material with a reticular titanium carbide skeleton structure prepared in this example, and as can be seen from fig. 1, in the Ti-Cr-Sn material with a reticular titanium carbide skeleton structure prepared in this example, in-situ generated titanium carbide is distributed in a titanium alloy matrix in a reticular skeleton structure, and the equivalent diameter of reticular pores of titanium carbide is 100 μm.
FIG. 2 is an X-ray diffraction pattern of the Ti-Cr-Sn material with a reticular titanium carbide skeleton structure prepared in this example, and it can be seen from FIG. 2 that the Ti-Cr-Sn material with a reticular titanium carbide skeleton structure prepared in this example contains three phases, namely a beta-Ti phase, an alpha-Ti phase and a TiC phase, and the existence of the in-situ generated TiC phase in the Ti-Cr-Sn material is confirmed by X-ray phase analysis.
Example 2
The method of the embodiment comprises the following steps:
step one, putting 3.1g of graphite flakes with the width of 1-20 microns and the thickness of 5-30 nm and 150g of spherical pure titanium powder with the granularity of 70 microns into a planetary ball mill for ball milling and mixing to obtain mixed powder; the rotation speed of ball milling mixing is 400 r/s, the ball-to-material ratio is 3:1, the total volume of the ball materials accounts for one half of the volume of a revolving drum of the planetary ball mill, and the ball milling time is 3 hours;
step two, putting the mixed powder obtained in the step one into a die with the diameter of 60mm, then putting the die into a spark plasma sintering furnace of SPS-80-T-20 for spark plasma sintering, and cooling the die to room temperature to obtain a titanium-based material with a reticular titanium carbide framework structure; the sintering process parameters are as follows: the temperature is 1000 ℃, the vacuum degree is 0.08MPa, the pressure is 60MPa, the temperature rise speed is 80 ℃/min, and the sintering time is 6 min.
Through detection, the equivalent diameter of the mesh pores in the titanium-based material with the mesh titanium carbide framework structure obtained in the embodiment is 70 μm.
Example 3
The method of the embodiment comprises the following steps:
step one, putting 1g of graphite flakes with the width of 1-20 microns and the thickness of 5-30 nm and 200g of spherical Ti-Cr-Sn titanium alloy powder with the granularity of 100 microns into a planetary ball mill for ball milling and mixing to obtain mixed powder; the rotation speed of ball milling mixing is 300 revolutions per second, and the ball-material ratio is 4: 1, the total volume of the ball materials accounts for one half of the volume of a revolving drum of the planetary ball mill, and the ball milling time is 3 hours;
step two, putting the mixed powder obtained in the step one into a die with the diameter of 60mm, then putting the die into a spark plasma sintering furnace of SPS-80-T-20 for spark plasma sintering, and cooling the die to room temperature to obtain a Ti-Cr-Sn material with a reticular titanium carbide skeleton structure; the sintering process parameters are as follows: the temperature is 900 ℃, the vacuum degree is 0.1MPa, the pressure is 60MPa, the temperature rise speed is 100 ℃/min, and the sintering time is 5 min.
Through detection, the equivalent diameter of the reticular pores in the reticular titanium carbide skeleton structure Ti-Cr-Sn material obtained in the embodiment is 100 μm.
Example 4
The method of the embodiment comprises the following steps:
step one, putting 12.8g of graphite flakes with the width of 1-20 microns and the thickness of 5-30 nm and 200g of spherical pure titanium powder with the granularity of 35 microns into a planetary ball mill for ball milling and mixing to obtain mixed powder; the rotation speed of ball milling mixing is 300 revolutions per second, and the ball-material ratio is 6:1, the total volume of the ball materials accounts for one half of the volume of a revolving drum of the planetary ball mill, and the ball milling time is 3 hours;
step two, putting the mixed powder obtained in the step one into a die with the diameter of 50mm, then putting the die into a spark plasma sintering furnace of SPS-80-T-20 for spark plasma sintering, and cooling the die to room temperature to obtain a titanium-based material with a reticular titanium carbide framework structure; the sintering process parameters are as follows: the temperature is 1100 ℃, the vacuum degree is 0.08MPa, the pressure is 40MPa, the temperature rise speed is 120 ℃/min, and the sintering time is 10 min.
Through detection, the equivalent diameter of the mesh pores in the titanium-based material with the mesh titanium carbide skeleton structure obtained in the embodiment is 35 μm.
Example 5
The method of the embodiment comprises the following steps:
step one, putting 15g of graphite flakes with the width of 1-20 microns and the thickness of 5-30 nm and 200g of spherical Ti-60 titanium alloy powder with the granularity of 50 microns into a planetary ball mill for ball milling and mixing to obtain mixed powder; the rotation speed of ball milling mixing is 350 revolutions per second, and the ball-material ratio is 3:1, the total volume of the ball materials accounts for one half of the volume of a revolving drum of the planetary ball mill, and the ball milling time is 3 hours;
step two, putting the mixed powder obtained in the step one into a die with the diameter of 50mm, then putting the die into a spark plasma sintering furnace of SPS-80-T-20 for spark plasma sintering, and cooling the die to room temperature to obtain a net-shaped titanium carbide skeleton structure Ti-60 material; the sintering process parameters are as follows: the temperature is 1000 ℃, the vacuum degree is 0.1MPa, the pressure is 60MPa, the temperature rise speed is 70 ℃/min, and the sintering time is 10 min.
Through detection, the equivalent diameter of the reticular pores in the reticular titanium carbide skeleton structure Ti-60 material obtained in the embodiment is 50 μm.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (4)
1. A preparation method of a controllable reticular titanium carbide framework structure titanium-based material is characterized by comprising the following steps:
putting graphite flakes with the width of 1-20 microns and the thickness of 5-30 nm and titanium powder or titanium alloy powder with the granularity of 35-100 microns into a planetary ball mill for ball milling and mixing to obtain mixed powder; the rotation speed for ball milling mixing is 300-400 r/s;
and step two, performing discharge plasma sintering on the mixed powder obtained in the step one above the phase transition temperature of the corresponding titanium or titanium alloy, and cooling the mixed powder to room temperature along with a furnace to obtain the titanium-based material with the reticular titanium carbide framework structure.
2. The method for preparing the titanium-based material with the controllable reticular titanium carbide framework structure according to claim 1, wherein the mass content of graphite flakes in the mixed powder in the first step is 0.3-7%.
3. The method for preparing the titanium-based material with the controllable reticular titanium carbide skeleton structure according to claim 1, wherein the ball-milling mixing in the first step adopts the ball-material ratio of (3:1) - (6:1) and the total volume of the ball material accounts for one half of the volume of a revolving drum of a planetary ball mill.
4. The method for preparing the titanium-based material with the controllable reticular titanium carbide skeleton structure according to claim 1, wherein the technological parameters of the spark plasma sintering in the second step are as follows: the temperature is not less than 900 ℃, the vacuum degree is not more than 0.1MPa, the pressure is not less than 40MPa, the temperature rise speed is 70-120 ℃/min, and the sintering time is 5-10 min.
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| CN102676863A (en) * | 2011-03-14 | 2012-09-19 | 中国科学院金属研究所 | TiC/Ti composite foam material and preparation method thereof |
| CN108588457A (en) * | 2018-04-09 | 2018-09-28 | 西安交通大学 | A kind of preparation method of high-strength wearable titanium alloy |
| CN109022907A (en) * | 2018-07-20 | 2018-12-18 | 东南大学 | A kind of graphene enhancing titanium composite material and its preparation method and application that three-dimensional network shape is distributed |
| CN109439998A (en) * | 2018-10-19 | 2019-03-08 | 北京科技大学 | A kind of method that the cold printing self- propagating of 3D prepares TiC base steel bonded carbide |
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| CN102676863A (en) * | 2011-03-14 | 2012-09-19 | 中国科学院金属研究所 | TiC/Ti composite foam material and preparation method thereof |
| CN108588457A (en) * | 2018-04-09 | 2018-09-28 | 西安交通大学 | A kind of preparation method of high-strength wearable titanium alloy |
| CN109022907A (en) * | 2018-07-20 | 2018-12-18 | 东南大学 | A kind of graphene enhancing titanium composite material and its preparation method and application that three-dimensional network shape is distributed |
| CN109439998A (en) * | 2018-10-19 | 2019-03-08 | 北京科技大学 | A kind of method that the cold printing self- propagating of 3D prepares TiC base steel bonded carbide |
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