CN110951016B - Preparation method of high-strength carbon nanotube/TiAl composite material - Google Patents
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Abstract
The invention discloses a preparation method of a high-strength carbon nanotube/TiAl composite material, which comprises the following steps: (1) preparing a maleic anhydride grafted carbon nano tube; (2) mixing; (3) hot pressing; (4) sintering; the preparation method of the high-strength carbon nanotube/TiAl composite material provided by the invention has good surface hardness and excellent tensile strength, and can greatly improve the application field of the carbon nanotube/TiAl composite material.
Description
Technical Field
The invention belongs to the technical field of nano composite processing, and particularly relates to a preparation method of a high-strength carbon nano tube/TiAl composite material.
Background
Since the early nineties, nanomaterials, as represented by carbon nanotubes, have attracted considerable attention for their unique structures and properties. In recent years, with the continuous and deep research of carbon nanotubes and nanomaterials, the wide application prospect of the carbon nanotubes and nanomaterials is continuously shown. For example, due to the unique electromagnetic, optical, mechanical, chemical, etc. properties of carbon nanotubes, a great deal of research on their applications in fields of field emission electron sources, sensors, novel optical materials, soft ferromagnetic materials, etc. has been reported. The existing titanium-aluminum composite material has general strength and cannot meet the market demand, so that the performance of the titanium-aluminum composite material needs to be improved to improve the performance of the titanium-aluminum composite material.
Disclosure of Invention
The invention is realized by the following technical scheme.
A preparation method of a high-strength carbon nanotube/TiAl composite material comprises the following steps:
(1) preparing a maleic anhydride grafted carbon nano tube:
dissolving polytetrahydrofuran diol in an organic solvent, heating to 60-70 ℃, stirring for 2 hours at the rotating speed of 500r/min to obtain polytetrahydrofuran diol solution, then adding 10-12% by mass of carbon nano tubes into the polytetrahydrofuran diol solution, performing ultrasonic dispersion treatment for 4-6 minutes, then adding into a reaction kettle, adding maleic anhydride 5% by mass of the carbon nano tubes into the reaction kettle under an inert atmosphere, adjusting the temperature to 80-85 ℃, stirring for 15 minutes, then adding 20% by mass of a cross-linking agent into the reaction kettle, continuing stirring for reaction for 4-6 hours, then performing suction filtration, cleaning with deionized water, and drying to constant weight to obtain maleic anhydride grafted carbon nano tubes; the maleic anhydride grafted carbon nanotube is prepared and added into the titanium-aluminum composite material, so that the defect that the carbon nanotube is easy to aggregate due to a small molecular effect can be greatly improved, the maleic anhydride grafted carbon nanotube can be uniformly dispersed in a titanium-aluminum composite material system, the compatibility between the maleic anhydride grafted carbon nanotube and a titanium-aluminum alloy tissue is greatly improved, a stable crosslinking action point is formed in the titanium-aluminum alloy tissue, a stable network structure is formed, and the hardness performance of the titanium-aluminum alloy composite material is greatly improved;
(2) mixing:
uniformly mixing the maleic anhydride grafted carbon nano tube obtained in the step (1) with titanium-aluminum alloy powder and rare earth to obtain a mixture, and introducing the rare earth to ensure that the titanium-aluminum alloy has fine crystal grains, reduce anisotropy and improve the processability, so that the tensile strength, the elongation at break and the surface hardness of the titanium-aluminum alloy composite material are improved; the nanometer size of the maleic anhydride grafted carbon nano tube and the rare earth with high surface activity can mutually promote and reinforce, and the maleic anhydride grafted carbon nano tube and the rare earth with high surface activity are uniformly dispersed and distributed in the internal structure of the titanium-aluminum alloy composite material, so that the comprehensive mechanical property of the titanium-aluminum alloy composite material is greatly improved;
(3) hot pressing:
adding the mixture obtained in the step (2) into a die for hot press forming to obtain a blank;
(4) and (3) sintering:
and (4) sintering the blank obtained in the step (3) to obtain a finished product.
In the step (1), the organic solvent is N, N-dimethylformamide.
In the step (1), the mixing mass ratio of the N, N-dimethylformamide to the polytetrahydrofuran diol is 100: 13.
The ultrasonic frequency of the ultrasonic dispersion in the step (1) is 30kHz, and the power is 250W.
And (2) the inert atmosphere in the step (1) is a nitrogen atmosphere.
The cross-linking agent in the step (1) is diethylaminopropylamine.
In the step (2), the mass ratio of the maleic anhydride grafted carbon nano tube to the titanium-aluminum alloy powder to the rare earth is (2.6-2.8: 100): 0.13-0.15.
The rare earth is cerium chloride.
The hot pressing condition in the step (3) is as follows: the temperature is 450 ℃, and the hot pressing pressure is 550-560 MPa.
The sintering conditions in the step (4) are as follows: the temperature is 660 ℃, and the sintering pressure is 750-760 MPa.
According to the technical scheme, the beneficial effects of the invention are as follows:
the preparation method of the high-strength carbon nanotube/TiAl composite material provided by the invention has good surface hardness and excellent tensile strength, and can greatly improve the application field of the carbon nanotube/TiAl composite material; the maleic anhydride grafted carbon nanotube is prepared and added into the titanium-aluminum composite material, so that the defect that the carbon nanotube is easy to aggregate due to a small molecular effect can be greatly improved, the maleic anhydride grafted carbon nanotube can be uniformly dispersed in a titanium-aluminum composite material system, the compatibility between the maleic anhydride grafted carbon nanotube and a titanium-aluminum alloy structure is greatly improved, a stable crosslinking action point is formed in the titanium-aluminum alloy structure, and a stable network structure is further formed, so that the strength performance and the surface hardness performance of the titanium-aluminum alloy composite material are greatly improved, and the titanium-aluminum alloy structure can be made into fine grains through the introduction of rare earth cerium chloride, so that the anisotropy is reduced, the processing performance is improved, and the tensile strength, the breaking elongation and the corrosion resistance of the titanium-aluminum alloy composite material are improved; the nanometer size of the maleic anhydride grafted carbon nanotube and the rare earth cerium chloride with high surface activity can mutually promote and reinforce, and the maleic anhydride grafted carbon nanotube and the rare earth cerium chloride are uniformly dispersed and distributed in the internal structure of the titanium-aluminum alloy composite material, so that the comprehensive mechanical property of the titanium-aluminum alloy composite material is greatly improved.
Detailed Description
The invention provides a preparation method of a high-strength carbon nanotube/TiAl composite material, and a person skilled in the art can use the content for reference and appropriately improve the process parameters to realize the preparation. It is expressly intended that all such similar substitutes and modifications apparent to those skilled in the art are deemed to be within the scope of the invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and modifications in the methods and applications described herein, as well as other suitable variations and combinations, may be made to implement and use the techniques of this invention without departing from the spirit and scope of the invention.
Example 1
A preparation method of a high-strength carbon nanotube/TiAl composite material comprises the following steps:
(1) preparing a maleic anhydride grafted carbon nano tube:
dissolving polytetrahydrofuran diol in an organic solvent N, N-dimethylformamide, heating to 60 ℃, stirring for 2 hours at the rotating speed of 500r/min to obtain polytetrahydrofuran diol solution, wherein the mixing mass ratio of the N, N-dimethylformamide to the polytetrahydrofuran diol is 100:13, then adding 10% by mass of carbon nano tubes into the polytetrahydrofuran diol solution, carrying out ultrasonic dispersion treatment for 4 minutes, the ultrasonic frequency of ultrasonic dispersion is 30kHz, the power is 250W, then adding into a reaction kettle, adding maleic anhydride with the mass of 5% by mass of the carbon nano tubes into the reaction kettle under the nitrogen atmosphere, adjusting the temperature to 80 ℃, stirring for 15 minutes, then adding cross-linking agent diethylaminopropylamine with the mass of 20% by mass of the maleic anhydride, continuing to stir for 4-6 hours, then carrying out suction filtration, cleaning by using deionized water, drying to constant weight, obtaining maleic anhydride grafted carbon nano-tubes;
(2) mixing:
uniformly mixing the maleic anhydride grafted carbon nano tube obtained in the step (1) with titanium-aluminum alloy powder and rare earth to obtain a mixture, wherein the mixing mass ratio of the maleic anhydride grafted carbon nano tube to the titanium-aluminum alloy powder to the rare earth is (2.6: 100): 0.13;
(3) hot pressing:
adding the mixture obtained in the step (2) into a die for hot press molding, wherein the temperature is 450 ℃, and the hot press pressure is 550MPa, so as to obtain a blank;
(4) and (3) sintering:
and (4) sintering the blank obtained in the step (3) at the temperature of 660 ℃ and the sintering pressure of 750MPa to obtain a finished product.
Example 2
A preparation method of a high-strength carbon nanotube/TiAl composite material comprises the following steps:
(1) preparing a maleic anhydride grafted carbon nano tube:
dissolving polytetrahydrofuran diol in an organic solvent N, N-dimethylformamide, heating to 70 ℃, stirring for 2 hours at the rotating speed of 500r/min to obtain polytetrahydrofuran diol solution, adding carbon nano tubes with the mass of 12% of that of the polytetrahydrofuran diol solution into the polytetrahydrofuran diol solution, performing ultrasonic dispersion treatment for 6 minutes at the ultrasonic frequency of 30kHz and the power of 250W, adding into a reaction kettle, adding maleic anhydride with the mass of 5% of that of the carbon nano tubes into the reaction kettle under the nitrogen atmosphere, adjusting the temperature to 85 ℃, stirring for 15 minutes, adding cross-linking agent diethylaminopropylamine with the mass of 20% of the maleic anhydride, continuing to perform stirring reaction for 6 hours, performing suction filtration, cleaning with deionized water, drying to constant weight, obtaining maleic anhydride grafted carbon nano-tubes;
(2) mixing:
uniformly mixing the maleic anhydride grafted carbon nano tube obtained in the step (1) with titanium-aluminum alloy powder and rare earth to obtain a mixture, wherein the mass ratio of the maleic anhydride grafted carbon nano tube to the titanium-aluminum alloy powder to the rare earth is (2.8: 100): 0.15;
(3) hot pressing:
adding the mixture obtained in the step (2) into a die for hot press molding, wherein the temperature is 450 ℃, and the hot press pressure is 560MPa, so as to obtain a blank;
(4) and (3) sintering:
and (4) sintering the blank obtained in the step (3) at 660 ℃ and 760MPa to obtain a finished product.
Example 3
A preparation method of a high-strength carbon nanotube/TiAl composite material comprises the following steps:
(1) preparing a maleic anhydride grafted carbon nano tube:
dissolving polytetrahydrofuran diol in an organic solvent N, N-dimethylformamide, heating to 65 ℃, stirring for 2 hours at the rotating speed of 500r/min to obtain polytetrahydrofuran diol solution, adding 11 mass percent of carbon nano tubes into the polytetrahydrofuran diol solution, performing ultrasonic dispersion treatment for 5 minutes at the ultrasonic frequency of 30kHz and the power of 250W, adding into a reaction kettle, adding maleic anhydride with the mass percent of 5 percent of the carbon nano tubes into the reaction kettle under the nitrogen atmosphere, adjusting the temperature to 82 ℃, stirring for 15 minutes, adding cross-linking agent diethylaminopropylamine with the mass percent of 20 percent of the maleic anhydride, continuously stirring for 5 hours, performing suction filtration, cleaning by using deionized water, drying to constant weight, obtaining maleic anhydride grafted carbon nano-tubes;
(2) mixing:
uniformly mixing the maleic anhydride grafted carbon nano tube obtained in the step (1) with titanium-aluminum alloy powder and rare earth to obtain a mixture, wherein the mixing mass ratio of the maleic anhydride grafted carbon nano tube to the titanium-aluminum alloy powder to the rare earth is (2.7: 100): 0.14;
(3) hot pressing:
adding the mixture obtained in the step (2) into a die for hot press molding, wherein the temperature is 450 ℃, and the hot press pressure is 552MPa, so as to obtain a blank;
(4) and (3) sintering:
and (4) sintering the blank obtained in the step (3) at the temperature of 660 ℃ and the sintering pressure of 756MPa to obtain a finished product.
Testing;
and (3) microhardness detection, namely sequentially selecting 3 points from the center to the edge of the surfaces of the samples of the embodiment and the control group at equal intervals to measure the hardness, calculating an average value, and measuring the hardness by using a domestic HV-1000 type microhardness tester, wherein the applied load is 4.705N, and the pressure maintaining time is 10 s:
TABLE 1
| Hardness HV | |
| Example 1 | 625.89 |
| Example 2 | 638.14 |
| Example 3 | 619.83 |
| Comparative example 1 | 512.35 |
| Comparative example 2 | 569.27 |
Comparative example 1: the difference from example 1 is that no rare earth is added;
comparative example 2: the difference from example 1 is that untreated carbon nanotubes are used.
As can be seen from Table 1, the carbon nanotube/TiAl composite material prepared by the method has excellent surface hardness, and the hardness performance of the titanium-aluminum composite material prepared by adding no rare earth or adopting untreated carbon nanotubes is obviously reduced, so that the rare earth and maleic anhydride grafted carbon nanotubes added in the method have the function of obviously improving the hardness of the titanium-aluminum composite material.
It is to be understood that the above description is not intended to limit the present invention, and the present invention is not limited to the above examples, and those skilled in the art should understand that they can make various changes, modifications, additions and substitutions within the spirit and scope of the present invention.
The invention is realized by the following technical scheme.
Claims (9)
1. A preparation method of a high-strength carbon nano tube/TiAl composite material is characterized in that,
the method comprises the following steps:
(1) preparing a maleic anhydride grafted carbon nano tube:
dissolving polytetrahydrofuran diol in an organic solvent, heating to 60-70 ℃, stirring at the rotating speed of 500r/min for 2 hours to obtain polytetrahydrofuran diol solution, then adding 10-12% by mass of carbon nano tubes into the polytetrahydrofuran diol solution, performing ultrasonic dispersion treatment for 4-6 minutes, then adding into a reaction kettle, adding maleic anhydride 5% by mass of the carbon nano tubes into the reaction kettle under an inert atmosphere, adjusting the temperature to 80 ℃, stirring for 15 minutes, then adding 20% by mass of a cross-linking agent of the maleic anhydride, continuing stirring for reaction for 4-6 hours, then performing suction filtration, cleaning by using deionized water, and drying to constant weight to obtain maleic anhydride grafted carbon nano tubes, wherein the cross-linking agent is diethylaminopropylamine;
(2) mixing:
uniformly mixing the maleic anhydride grafted carbon nano tube obtained in the step (1) with titanium-aluminum alloy powder and rare earth to obtain a mixture;
(3) hot pressing:
adding the mixture obtained in the step (2) into a die for hot press forming to obtain a blank;
(4) and (3) sintering:
and (4) sintering the blank obtained in the step (3) to obtain a finished product.
2. The method for preparing a high-strength carbon nanotube/TiAl composite material according to claim 1, wherein the organic solvent in step (1) is N, N-dimethylformamide.
3. The method for preparing the high-strength carbon nanotube/TiAl composite material according to claim 2, wherein the mixing mass ratio of the N, N-dimethylformamide to the polytetrahydrofuran diol in the step (1) is 100: 13.
4. The method for preparing a high-strength carbon nanotube/TiAl composite material as claimed in claim 1, wherein the ultrasonic frequency of the ultrasonic dispersion in the step (1) is 30kHz and the power is 250W.
5. The method for preparing a high-strength carbon nanotube/TiAl composite material according to claim 1, wherein the inert atmosphere in the step (1) is a nitrogen atmosphere.
6. The method for preparing the high-strength carbon nanotube/TiAl composite material according to claim 1, wherein in the step (2), the mass ratio of the maleic anhydride grafted carbon nanotube to the titanium-aluminum alloy powder to the rare earth is (2.6-2.8: 100): 0.13-0.15.
7. The method of claim 1, wherein the rare earth is cerium chloride.
8. The method for preparing a high-strength carbon nanotube/TiAl composite material as claimed in claim 1, wherein the hot-pressing conditions in step (3) are as follows: the temperature is 450 ℃, and the hot pressing pressure is 550-560 MPa.
9. The method for preparing a high-strength carbon nanotube/TiAl composite material as claimed in claim 1, wherein the sintering conditions in step (4) are as follows: the temperature is 660 ℃, and the sintering pressure is 750-760 MPa.
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