CN114734040B - Preparation method of in-situ authigenic titanium-aluminum composite material distributed in network shape - Google Patents
Preparation method of in-situ authigenic titanium-aluminum composite material distributed in network shape Download PDFInfo
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Abstract
The preparation method of the in-situ authigene titanium aluminum composite material in network distribution comprises the steps of adding graphene nano sheets and dodecylbenzene sulfonic acid into deionized water, and then carrying out ultrasonic dispersion treatment to obtain a graphene solution; adding spherical Ti powder and graphene solution into absolute ethyl alcohol, and then heating, ultrasonic stirring and drying to obtain Ti/graphene composite powder with a graphene coating on the surface; adding spherical Al powder and Ti/graphene composite powder into a ball mill for ball milling, and carrying out laser selective melting forming on the obtained Ti/Al/graphene composite powder to prepare in-situ autogenous Ti distributed in a network shape 2 AlC/TiAl composite material. According to the invention, through the method of mutually matching heating ultrasonic stirring, ball milling and laser selective melting forming, the in-situ self-generated Ti2AlC reinforcing phase is uniformly distributed in the TiAl matrix in a network shape, and the existence of the network structure improves the integral coordinated deformability of the material, passivates cracks, prevents crack growth, and improves the toughness of the material while improving the strength.
Description
Technical Field
The invention relates to the field of titanium-aluminum composite materials, in particular to a preparation method of an in-situ authigenic titanium-aluminum composite material distributed in a network shape.
Background
As an advanced high-temperature structural material, the TiAl alloy has the excellent performances of light weight, high specific strength, high wear resistance, high temperature resistance, corrosion resistance, creep resistance, oxidation resistance and the like, and has wide application prospect in the fields of aerospace, armored ships and the like. However, the wide application of TiAl alloy is limited by the disadvantages of poor room temperature plasticity and the like. For the purpose ofThe most common method for improving the mechanical properties of TiAl alloy is to add alloying elements or introduce reinforcing phases for compounding treatment. At present, as the research of MAX phase is gradually in progress, the development of MAX/TiAl composite materials is promoted by the excellent performance of MAX phase. Wherein Ti is 2 AlC phase is a ternary layered ceramic, has excellent characteristics of metal and ceramic, has high elastic modulus, thermal stability and good machining performance, and therefore uses Ti 2 AlC reinforcing phase can regulate TiAl alloy structure and raise alloy performance.
At present, the traditional ingot metallurgy and precision casting and other technological methods are widely applied, and because of the intrinsic brittleness of the TiAl alloy, the traditional technology is difficult to prepare the TiAl alloy parts with complex shapes. The laser selective melting technology is used for manufacturing parts by melting and solidifying materials layer by means of computer aided design based on the idea of calculus. The part forming precision of the SLM forming technology is high, the surface quality is good, and the net forming of the part can be realized; however, the repeated rapid heating and cooling in the forming process makes the forming process extremely easy to generate larger thermal stress and crack defects difficult to control. Therefore, the configuration design of introducing the reinforcing phase is particularly important, and the distribution mode of the reinforcing phase has great influence on the start, movement, and the secant of dislocation in a crystal structure, so that the mechanical property is influenced. The second phase distributed in the network can improve the integral coordinated deformation capability, passivate cracks, prevent crack growth and reduce the splitting effect of the reinforcing phase, thereby improving the room temperature plasticity of the alloy and improving the strength of the alloy, and has a certain research significance for solving the problem of 'toughness inversion'.
Disclosure of Invention
The invention aims to provide a preparation method of an in-situ authigenic titanium-aluminum composite material distributed in a network shape, which improves the strength of the titanium-aluminum composite material and improves the plasticity and toughness of the titanium-aluminum composite material.
The technical scheme adopted by the invention for solving the technical problems is as follows: the preparation method of the in-situ authigenic titanium-aluminum composite material distributed in a network shape comprises the following steps:
adding graphene nano sheets and dodecylbenzene sulfonic acid into deionized water, and then performing ultrasonic dispersion treatment to uniformly disperse graphene in a single layer in the solution to obtain a graphene solution;
adding spherical Ti powder and the graphene solution obtained in the step one into absolute ethyl alcohol, then heating, ultrasonically stirring until the solution is evaporated, and then placing the evaporated solid into a vacuum drying oven for drying treatment to obtain Ti/graphene composite powder with a graphene coating on the surface;
adding the spherical Al powder and the Ti/graphene composite powder obtained in the step two into a ball mill for ball milling to obtain uniformly mixed Ti/Al/graphene composite powder;
adding the Ti/Al/graphene composite powder obtained in the step three into a forming cylinder of a laser selective melting device, paving powder on a lifting table of the forming cylinder, then placing a pure titanium substrate, carrying out laser selective melting forming, taking argon as protective gas, adopting two adjacent layers of perpendicular S-shaped paths as laser scanning paths, preheating the substrate at 300-400 ℃, and preparing the in-situ self-generated Ti in network distribution, wherein the laser scanning distance is 80-140 mu m, the scanning speed is 500-800 mm/S, and the laser power is 100-300W 2 AlC/TiAl composite material.
Preferably, in the first step, the thickness of the graphene nano sheet is 3-10 nm, and the sheet diameter is 5-10 mu m.
Preferably, in the second step, the temperature of the heating ultrasonic stirring treatment is 80 ℃, the temperature of the drying treatment is 60-80 ℃, and the drying time is 8-10 hours.
Preferably, in the third step, zirconia balls are used as ball milling media, the ball diameter is 5mm, and the ball-to-material ratio is 10:1, the rotating speed is 100-120 r/min, and the ball milling time is 10-12 h.
Preferably, in the fourth step, powder is paved in a single-cylinder one-way powder paving mode by automatically feeding powder.
According to the technical scheme, the invention has the beneficial effects that:
according to the invention, spherical Ti powder and graphene solution are added into absolute ethyl alcohol for heating and ultrasonic stirring, so that a graphene coating is formed on the surface of the spherical Ti powder, spherical Al powder uniformly surrounds the periphery of the graphene/spherical Ti powder through ball milling, a network-shaped structure is formed inside the Ti/Al/graphene composite powder, and a network-shaped Ti2AlC reinforcing phase is generated in situ at the position of the network-shaped structure during selective laser melting.
The invention adopts the process method of mutually matching heating ultrasonic stirring, ball milling and laser selective melting forming, so that the in-situ self-generated Ti2AlC reinforcing phase is uniformly distributed in the TiAl matrix in a network shape, the existence of the network structure improves the integral coordinated deformability of the material, passivates cracks, prevents crack growth, and improves the toughness of the material while improving the strength.
Compared with the traditional process method, the laser selective melting technology has no restriction on part structures, can process complex structures with arbitrary shapes, has good forming surface quality, can realize the net forming of parts, has high processing efficiency, can shorten the processing period, reduces the waste of materials and saves the cost.
Detailed Description
The preparation method of the in-situ authigenic titanium-aluminum composite material distributed in a network shape comprises the following steps:
adding graphene nano sheets and dodecylbenzene sulfonic acid into deionized water, and then performing ultrasonic dispersion treatment to uniformly disperse graphene in a single layer in the solution to obtain a graphene solution; the thickness of the graphene nano sheet is 3-10 nm, and the sheet diameter is 5-10 mu m.
And step two, adding the spherical Ti powder and the graphene solution obtained in the step one into absolute ethyl alcohol, and then heating, carrying out ultrasonic stirring treatment at the temperature of 80 ℃ until the solution is evaporated. And then placing the evaporated solid into a vacuum drying oven for drying treatment at the temperature of 60-80 ℃ for 8-10 hours to obtain the Ti/graphene composite powder with the graphene coating on the surface.
Adding the spherical Al powder and the Ti/graphene composite powder obtained in the step two into a ball mill for ball milling, wherein zirconia balls are used as ball milling media, the ball diameter is 5mm, and the ball-to-material ratio is 10:1, the rotating speed is 100-120 r/min, the ball milling time is 10-12 h, and the uniformly mixed Ti/Al/graphene composite powder is obtained.
And step four, adding the Ti/Al/graphene composite powder obtained in the step three into a forming cylinder of a laser selective melting device, and paving the powder on a forming cylinder lifting table in a mode of automatic powder feeding and single-cylinder unidirectional powder paving. Then placing a pure titanium substrate, carrying out laser selective melting forming, taking argon as protective gas, adopting two adjacent layers of perpendicular S-shaped paths for laser scanning paths, preheating the substrate at 300-400 ℃, and preparing the in-situ self-generated Ti in network distribution, wherein the laser scanning distance is 80-140 mu m, the scanning speed is 500-800 mm/S, and the laser power is 100-300W 2 AlC/TiAl composite material.
Example 1:
in-situ autogenous Ti distributed in network shape 2 The AlC/TiAl composite material and the preparation method thereof specifically comprises the following steps:
uniformly dispersing graphene nano sheets into deionized water, simultaneously adding an organic solvent dodecylbenzene sulfonic acid, wherein the concentration of the graphene solution is 5-10 mg/ml, and obtaining a single-layer uniformly dispersed graphene solution (the thickness of the graphene nano sheets is 3-10 nm, and the sheet diameter is 5-10 mu m) through ultrasonic dispersion.
And step two, adding the spherical titanium powder and the graphene dispersion liquid obtained in the step one into absolute ethyl alcohol for heating and ultrasonic stirring (80 ℃), wherein a graphene coating is formed on the surface of the TiAl powder, carrying out ultrasonic stirring until the solution is evaporated, and then carrying out drying treatment (the temperature is 60-80 ℃ for 8-10 h) in a vacuum drying oven to obtain the Ti/graphene composite powder.
And thirdly, taking zirconia balls as ball milling media (ball diameter is 5 mm), and performing low-energy ball milling (ball material ratio is 10:1, rotating speed is 100-120 r/min and ball milling time is 10-12 h) on the spherical Al and the graphene/spherical Ti powder composite powder obtained in the second step to obtain the uniformly mixed Ti/Al/graphene composite powder. Wherein the purity of Ti powder and Al powder is 99.99%, the average grain diameter is 15-25 μm, the atomic percentage of Ti-Al-C is 53.5:44:2.5, calculated, and the Ti formed by SLM is formed 2 In AlC/TiAl composite material, ti 2 The volume fraction of AlC is about 10%.
Step four:
filling the composite powder into a material cylinder, laying powder 5mm on a lifting table of a forming cylinder for heat preservation, adopting an automatic feeding mode for laying powder, adopting single-cylinder unidirectional powder laying, then placing a substrate (the substrate adopts a pure titanium substrate with better wettability with TiAl alloy), carrying out preheating treatment (the preheating temperature is 350 ℃) on the substrate at higher power and higher scanning speed, taking argon as protective gas, and adopting the technical parameters of SLM forming as follows: the laser scanning interval is 80 μm, the scanning speed is 500mm/s, and the laser power is 200W. Thus, in-situ self-generated Ti distributed in a network shape is prepared by the method 2 AlC/TiAl composite material.
Example 2:
this embodiment is the same as the embodiments of steps one to three in example 1, except that: the laser scanning interval is 100 μm, the scanning speed is 600mm/s, and the laser power is 150W. Compared with the example 1, the grain structure is obviously thinned, and Ti in the TiAl-based composite material 2 The AlC enhancement phase is still distributed in a network.
Example 3:
this embodiment is the same as the embodiments of steps one to three in example 1, except that: the laser scanning interval is 120 μm, the scanning speed is 700mm/s, and the laser power is 100W. The grain structure is further refined compared to examples 1 and 2, resulting in further improvement in composite properties.
Claims (5)
1. The preparation method of the in-situ authigenic titanium-aluminum composite material distributed in a network shape is characterized by comprising the following steps of:
adding graphene nano sheets and dodecylbenzene sulfonic acid into deionized water, and then performing ultrasonic dispersion treatment to uniformly disperse graphene in a single layer in the solution to obtain a graphene solution;
adding spherical Ti powder and the graphene solution obtained in the step one into absolute ethyl alcohol, then heating, ultrasonically stirring until the solution is evaporated, and then placing the evaporated solid into a vacuum drying oven for drying treatment to obtain Ti/graphene composite powder with a graphene coating on the surface;
adding the spherical Al powder and the Ti/graphene composite powder obtained in the step two into a ball mill for ball milling to obtain uniformly mixed Ti/Al/graphene composite powder;
adding the Ti/Al/graphene composite powder obtained in the step three into a forming cylinder of a laser selective melting device, paving powder on a lifting table of the forming cylinder, then placing a pure titanium substrate, carrying out laser selective melting forming, taking argon as protective gas, adopting two adjacent layers of perpendicular S-shaped paths as laser scanning paths, preheating the substrate at 300-400 ℃, and preparing the in-situ self-generated Ti in network distribution, wherein the laser scanning distance is 80-140 mu m, the scanning speed is 500-800 mm/S, and the laser power is 100-300W 2 AlC/TiAl composite material.
2. The method for preparing the in-situ self-produced titanium aluminum composite material distributed in a network shape according to claim 1, which is characterized in that: in the first step, the thickness of the graphene nano sheet is 3-10 nm, and the sheet diameter is 5-10 mu m.
3. The method for preparing the in-situ self-produced titanium aluminum composite material distributed in a network shape according to claim 1, which is characterized in that: in the second step, the temperature of heating ultrasonic stirring treatment is 80 ℃, the temperature of drying treatment is 60-80 ℃, and the drying time is 8-10 h.
4. The method for preparing the in-situ self-produced titanium aluminum composite material distributed in a network shape according to claim 1, which is characterized in that: in the third step, zirconia balls are used as ball milling media, the ball diameter is 5mm, and the ball-to-material ratio is 10:1, the rotating speed is 100-120 r/min, and the ball milling time is 10-12 h.
5. The method for preparing the in-situ self-produced titanium aluminum composite material distributed in a network shape according to claim 1, which is characterized in that: and step four, when powder is paved, a mode of automatic powder feeding and single-cylinder unidirectional powder paving is adopted.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109454240A (en) * | 2018-12-19 | 2019-03-12 | 西安增材制造国家研究院有限公司 | A kind of graphene alloy nano composite material preparation method and SLM forming technology |
| CN110257657A (en) * | 2019-07-25 | 2019-09-20 | 成都先进金属材料产业技术研究院有限公司 | The method for preparing graphene enhancing aluminum alloy materials based on selective laser smelting technology |
| WO2021232942A1 (en) * | 2020-05-18 | 2021-11-25 | 山东省科学院新材料研究所 | Method for preparing graphene-reinforced aluminum matrix composite material powder by means of short flow |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109454240A (en) * | 2018-12-19 | 2019-03-12 | 西安增材制造国家研究院有限公司 | A kind of graphene alloy nano composite material preparation method and SLM forming technology |
| CN110257657A (en) * | 2019-07-25 | 2019-09-20 | 成都先进金属材料产业技术研究院有限公司 | The method for preparing graphene enhancing aluminum alloy materials based on selective laser smelting technology |
| WO2021232942A1 (en) * | 2020-05-18 | 2021-11-25 | 山东省科学院新材料研究所 | Method for preparing graphene-reinforced aluminum matrix composite material powder by means of short flow |
Non-Patent Citations (1)
| Title |
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| 碳纳米材料改性TiAl基合金技术发展现状及展望;吴明宇;弭光宝;李培杰;黄旭;曹春晓;;航空材料学报(03);全文 * |
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