CN112159914A - TiAl micron crystal prepared under high pressure and method thereof - Google Patents
TiAl micron crystal prepared under high pressure and method thereof Download PDFInfo
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- CN112159914A CN112159914A CN202010988738.9A CN202010988738A CN112159914A CN 112159914 A CN112159914 A CN 112159914A CN 202010988738 A CN202010988738 A CN 202010988738A CN 112159914 A CN112159914 A CN 112159914A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
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- 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
- C22C1/02—Making non-ferrous alloys by melting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
- C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
Abstract
The invention discloses TiAl micro-crystals prepared under high pressure and a preparation method thereof, wherein the preparation method comprises the following steps: s1: respectively pretreating the titanium sponge, the high-purity Al and the high-purity Nb alloy, and then carrying out vacuum arc melting on the titanium sponge, the high-purity Al and the high-purity Nb alloy to obtain Ti-45Al-8Nb alloy cast ingots in at%; s2: cutting the alloy cast ingot to obtain an alloy sample; s3: pretreating the alloy sample, assembling a pressing block to enable the pressing block to be in a sealing state for compactness, and obtaining an alloy pressing block; s4: and (3) placing the alloy pressing block in a press, pressurizing to 3-5 GPa, then heating to 1600-1700 ℃, keeping the temperature for 10-15 min, cooling the alloy pressing block to room temperature under the condition of keeping the pressure unchanged, and relieving the pressure to obtain the TiAl microcrystal. The TiAl microcrystal has high hardness and excellent mechanical property, and is simple in process, convenient to operate, suitable for industrial production and wide in application prospect.
Description
Technical Field
The invention belongs to the technical field of metal material preparation, and particularly relates to TiAl micro-crystals prepared under high pressure and a method thereof.
Background
With the rapid development of the aerospace industry, the automotive industry, and the shipbuilding industry, the demand of people on the modern industry cannot be met by common traditional materials and common material processing technologies. As a novel metal compound structural material, the TiAl-based alloy has the advantages of low density, high melting point, high specific strength, high specific rigidity, excellent high-temperature oxidation resistance and the like, and has the advantages of metal and ceramic, so that the TiAl-based alloy is highly valued by people. The TiAl-based alloy can even replace some Ni-based high-temperature alloys to be used for manufacturing key parts of airplanes, so that the TiAl-based alloy can be better used in a high-temperature environment and has wide application prospect. However, the TiAl-based alloy also faces the problem to be solved, and the defects of low room temperature plasticity, poor thermal deformation capability, poor processability and the like cause the TiAl-based alloy to be severely restricted in application. Therefore, the manufacturing industry puts more strict requirements on high-temperature structural materials, such as higher high-temperature oxidation resistance, high-temperature specific strength, excellent fatigue fracture resistance and high-temperature corrosion resistance.
Fine grain strengthening is generally accepted as the only method that improves both the strength and plasticity of an alloy. Particularly, when the grains are refined to the micrometer scale, the strength is remarkably improved. The microcrystalline material has excellent mechanical strength due to its fine crystal grains, and the strength can be increased several times as compared with conventional coarse-grained materials. The alloy's rheological stress increases with decreasing grain size, and its strengthening mechanism is due to increased grain boundaries. The grain boundaries are transition layers between crystal grains, and when the atomic arrangement is irregular, the crystal lattice is severely distorted. When the dislocations in the grains move to the vicinity of the grain boundaries, they are hindered by the grain boundaries, and thus a dislocation plug product is generated. The finer the crystal grain, the larger the proportion of the grain boundary, the more the barrier to the movement of dislocations, and the deformation resistance of the alloy material continues to increase. Meanwhile, as the crystal grains are fine, the difference between the strain degrees in the crystal grains and near the crystal boundary is small, and the deformation distribution is uniform, the phenomenon of cracking caused by stress concentration is reduced, which shows that the alloy can bear larger deformation amount before fracture, and the plasticity of the alloy is improved.
The solidification of the alloy under the traditional conditions can only obtain the common phase structure in the equilibrium phase diagram, and the properties of the alloy structure obtained under the equilibrium conditions can not meet the requirements of modern industry. The extreme conditions are applied to the alloy, and the obtained alloy structure is different from a conventional solidification structure and has special properties. The high-pressure solidification technology is a process of changing an original electron orbit and a bonding mode in a substance by reducing the distance between atoms and electrons, forming a crystal structure different from the original crystal structure in the substance and generating a new substance. Moreover, the high pressure can also inhibit the diffusion of elements in the alloy by improving the melting point of the alloy material, increasing the supercooling degree and reducing the diffusion coefficient, so that the phase composition in the alloy material is changed and the mechanical property of the alloy material is influenced. The high-pressure technology is widely applied in the fields of superhard materials, superconducting materials, nanocrystalline and the like at present, the preparation of metastable materials is realized, and the research on the traditional industrial alloy is deficient, so the invention provides a method for preparing TiAl microcrystalline under high pressure by utilizing the high-pressure technology and selecting proper alloy materials and process parameters.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides TiAl micro-crystals prepared under high pressure and a method thereof. The TiAl micron crystal is prepared by utilizing a high-pressure solidification technology, has high hardness and excellent mechanical property, and has the advantages of simple preparation process, convenience in operation and wide application prospect.
The invention adopts the following specific technical scheme:
a method for preparing TiAl micro-crystals at high pressure comprises the following steps:
s1: respectively pretreating the titanium sponge, the high-purity Al and the high-purity Nb alloy, and then carrying out vacuum arc melting on the titanium sponge, the high-purity Al and the high-purity Nb alloy to obtain Ti-45Al-8Nb alloy cast ingots in at%;
s2: cutting the alloy cast ingot to obtain an alloy sample;
s3: pretreating the alloy sample, and assembling and pressing a block to obtain an alloy pressing block;
s4: and (3) placing the alloy pressing block in a press, pressurizing to 3-5 GPa, then heating to 1600-1700 ℃, keeping the temperature for 10-15 min, cooling the alloy pressing block to room temperature under the condition of keeping the pressure unchanged, and relieving the pressure to obtain the TiAl micro-crystals.
Preferably, the purities of the titanium sponge, the high-purity Al and the high-purity Nb alloy in S1 are respectively 99.9%, 99.99% and 99.99%.
Preferably, the pretreatment in S1 refers to grinding the surface oxide with 400-mesh carborundum paper.
Preferably, the number of vacuum arc melting in S1 is 4, and the vacuum arc melting is turned over and subjected to two times of gas washing treatment after each melting.
Preferably, in the step S2, the alloy ingot is cut by electric spark to a size that is suitable for the assembly of cubic press compacts.
Further, in the step S2, the alloy ingot is cut into
The size of (c).
Preferably, the pretreatment in S3 is to wash the alloy sample with 5% HF solution, polish off the oxide on the surface, and finally ultrasonically wash in absolute ethanol.
Preferably, materials used in assembling the compact described in S3 include pyrophyllite, graphite, molybdenum sheets, boron nitride, and zirconia ceramics.
Preferably, the press in S4 is a cubic press.
Another object of the present invention is to provide TiAl nanocrystals prepared according to any of the above methods.
Compared with the prior art, the invention has the beneficial effects that:
1) the TiAl microcrystal has high hardness and excellent mechanical property, and is simple in process, convenient to operate and suitable for industrial production;
2) according to the invention, the power is manually adjusted in the high-pressure solidification process, and the temperature of the hammer head is accurately controlled, so that the real-time temperature obtained by a sample can be monitored in real time;
3) the TiAl micron-crystal metal material has great application potential in the fields of aerospace, automobile manufacturing, ship manufacturing and the like.
Drawings
FIG. 1 is a schematic view of the assembly of a Ti-45Al-8Nb alloy in assembling a compact;
FIG. 2 is an SEM photograph of sample 1 in example 1;
FIG. 3 is an SEM photograph of sample 2 of example 2;
fig. 4 is an SEM image of sample 3 in example 3.
Detailed Description
The invention will be further elucidated and described with reference to the drawings and the detailed description. The technical features of the embodiments of the present invention can be combined correspondingly without mutual conflict.
The invention provides a method for preparing TiAl micro-crystals at high pressure, which comprises the following steps:
s1: respectively polishing surface oxides of titanium sponge with the purity of 99.9%, high-purity Al with the purity of 99.99% and high-purity Nb alloy with the purity of 99.99% by 400-mesh carborundum paper to finish pretreatment, and then carrying out vacuum arc melting on the pretreated titanium sponge, high-purity Al and high-purity Nb alloy. In the vacuum arc melting process, high-purity Al is placed at the bottom of a crucible, and then titanium sponge and high-purity Nb alloy are added into the crucible. The number of vacuum arc melting is 4, and the melted material is turned over and subjected to two times of gas washing treatment after each melting is finished. After the vacuum arc melting is completely finished, Ti-45Al-8Nb (in at%) alloy ingots are obtained.
S2: the alloy ingot obtained by the processing of S1 was cut by electric spark into a size conforming to the operation of the top press to obtain an alloy sample. In the present embodiment, six faces are employedJacking machines, whereby the alloy ingots are cut into
For subsequent pressure treatment.
S3: pretreating the alloy sample obtained in S2, namely cleaning the cylindrical alloy sample by using 5% HF, then polishing off oxides on the surface of the cylindrical alloy sample, and finally carrying out ultrasonic cleaning in absolute ethyl alcohol. And assembling and briquetting the alloy sample subjected to pretreatment operation, wherein the assembling material ensures the compactness of the materials so as to realize the transmission of current and prevent blasting.
The materials adopted in the assembly of the pressing block in the embodiment comprise pyrophyllite, graphite and zirconia ceramics, the specific assembly pressing block mode is shown in fig. 1, the assembly modes of the upper surface and the lower surface of the alloy sample are the same and are alloy sample/boron nitride/zirconia/boron nitride/graphite/molybdenum/pyrophyllite; the assembly modes of the left surface and the right surface of the alloy sample are the same, and the alloy sample is alloy sample/boron nitride/graphite/boron nitride/zirconium oxide/pyrophyllite. The pyrophyllite has the advantages of good pressure transmission, good heat resistance and heat preservation, good sealing performance, good insulation performance and the like.
S4: and (3) placing the alloy pressing block in the S3 into a cubic press to be pressurized to 3-5 GPa, manually adjusting power to slowly increase the temperature of the hammer head, transferring the temperature to the alloy pressing block in the module through pyrophyllite heat conduction, cooling the alloy pressing block to room temperature under the condition of keeping the pressure unchanged after the temperature is increased to 1600-1700 ℃ and is kept for 10-15 min, and releasing the pressure to obtain the TiAl microcrystal.
Example 1
S1: respectively polishing surface oxides of titanium sponge with the purity of 99.9%, high-purity Al with the purity of 99.99% and high-purity Nb alloy with the purity of 99.99% by 400-mesh carborundum paper to finish pretreatment, and then carrying out vacuum arc melting on the pretreated titanium sponge, high-purity Al and high-purity Nb alloy. In the vacuum arc melting process, high-purity Al is placed at the bottom of a crucible, and then titanium sponge and high-purity Nb alloy are added into the crucible. The number of vacuum arc melting is 4, and the melted material is turned over and subjected to two times of gas washing treatment after each melting is finished. After the vacuum arc melting is completely finished, Ti-45Al-8Nb (in at%) alloy ingots are obtained.
S2: cutting the alloy ingot obtained by the S1 processing procedure into pieces by electric spark
For subsequent pressure treatment.
S3: pretreating the alloy sample obtained in S2, namely cleaning the cylindrical alloy sample by using 5% HF, then polishing off oxides on the surface of the cylindrical alloy sample, and finally carrying out ultrasonic cleaning in absolute ethyl alcohol. Sample 1 was obtained for microstructure observation.
The scanning electron microscope image of the sample 1 is shown in fig. 2, and it can be seen from the image that the morphology of the sample 1 which is not subjected to the high-pressure operation process is similar to the morphology of the high Nb-TiAl alloy system, and more B2 phases exist in the matrix structure, so that the sample 1 is very easy to have the defects of macro composition segregation, looseness, shrinkage cavity and the like, and the long-time stable operation of the sample 1 in the high-temperature (800 ℃ -1000 ℃) environment is not utilized.
Example 2
S1: respectively polishing surface oxides of titanium sponge with the purity of 99.9%, high-purity Al with the purity of 99.99% and high-purity Nb alloy with the purity of 99.99% by 400-mesh carborundum paper to finish pretreatment, and then carrying out vacuum arc melting on the pretreated titanium sponge, high-purity Al and high-purity Nb alloy. The number of vacuum arc melting is 4, and the melted material is turned over and subjected to two times of gas washing treatment after each melting is finished. After the vacuum arc melting is completely finished, Ti-45Al-8Nb (in at%) alloy ingots are obtained.
S2: cutting the alloy ingot obtained by the S1 processing procedure into pieces by electric spark
For subsequent pressure treatment.
S3: pretreating the alloy sample obtained in S2, namely cleaning the cylindrical alloy sample by using 5% HF, then polishing off oxides on the surface of the cylindrical alloy sample, and finally carrying out ultrasonic cleaning in absolute ethyl alcohol. And assembling and briquetting the alloy sample subjected to the pretreatment operation to enable the alloy sample to be in a sealed state, thereby obtaining the alloy briquette.
S4: and (3) placing the alloy pressing block in the S3 into a cubic press to be pressurized to 3GPa, manually adjusting power to slowly increase the temperature of the hammer head, transferring the temperature to the alloy pressing block in the module through pyrophyllite heat conduction, cooling the alloy pressing block to room temperature under the condition of keeping the pressure unchanged after the temperature is increased to 1600-1700 ℃ and is kept for 10-15 min, and releasing the pressure to obtain the sample 2.
The scanning electron micrograph of sample 2 is shown in fig. 3, and it can be seen that the microstructure of sample 2 treated at a high pressure of 3GPa is completely different from that of sample 1 treated at normal pressure. The matrix of sample 2 is "embedded" with the solid solution phase precipitated after high pressure solidification, with clear outline and angular edges.
Example 3
The procedure of this example was the same as in example 2, but the sample was pressurized to 5GPa in a cubic press at S4 to obtain sample 3.
The scanning electron micrograph of sample 3 is shown in fig. 4, and it can be seen that sample 3 obtained after the 5GPa high-pressure treatment has a microstructure completely different from that of sample 1 subjected to the atmospheric pressure treatment, and is similar to sample 2 obtained after the 3GPa high-pressure treatment. However, in comparison with sample 2, sample 3 obtained in this example had a matrix structure almost covered with an off-white solid solution, and a large number of micron-sized grains were found at the grain boundaries of the off-white solid solution. The volume fraction of the solid solution in sample 3 was larger than that in sample 2, indicating that the solid solution strengthening effect of the sample after high-pressure solidification at 5GPa was stronger than that of sample 2. And secondly, the micron crystal particles distributed on the crystal boundary of the sample 3 play a role in fine crystal strengthening, so that the mechanical property of the alloy material can be further improved.
Example 4
S1: samples 1, 2 and 3 were subjected to a grinding and polishing treatment, and the height of each sample was 8mm or less.
S2: the surface of each sample was tested using a nanoindenter hardness tester (DUH-211S), in which the load: 500mN, Poisson's ratio: 0.335.
fixing the sample on a workbench, selecting a proper matrix tissue position by using an eyepiece, moving the workbench to the position below a pressure head, and clicking Test to Test.
S3: when a test is completed, the indenter will automatically return to the original position. And moving the workbench to the position below an ocular lens, selecting an analysis function in software to intercept the contact area of the pressure head in the matrix tissue, and calculating the hardness value of the test.
S4: the specimen was moved and another basal body tissue was obtained under the eyepiece in the same manner as in S2 and S3 described above, and after 10 tests, the data were counted and the average value was calculated.
The nano-hardness test method is adopted for all the samples 1 to 3, and the results show that the hardness values of the sample 2 and the sample 3 are higher than that of the sample 1.
The above-described embodiments are merely preferred embodiments of the present invention, which should not be construed as limiting the invention. Various changes and modifications may be made by one of ordinary skill in the pertinent art without departing from the spirit and scope of the present invention. Therefore, the technical scheme obtained by adopting the mode of equivalent replacement or equivalent transformation is within the protection scope of the invention.
Claims (10)
1. A method for preparing TiAl micro-crystals at high pressure is characterized by comprising the following steps:
s1: respectively pretreating the titanium sponge, the high-purity Al and the high-purity Nb alloy, and then carrying out vacuum arc melting on the titanium sponge, the high-purity Al and the high-purity Nb alloy to obtain Ti-45Al-8Nb alloy cast ingots in at%;
s2: cutting the alloy cast ingot to obtain an alloy sample;
s3: pretreating the alloy sample, and assembling and pressing a block to obtain an alloy pressing block;
s4: and (3) placing the alloy pressing block in a press, pressurizing to 3-5 GPa, then heating to 1600-1700 ℃, keeping the temperature for 10-15 min, cooling the alloy pressing block to room temperature under the condition of keeping the pressure unchanged, and relieving the pressure to obtain the TiAl microcrystal.
2. The method for preparing TiAl microcrystals under high pressure according to claim 1, wherein the purities of the titanium sponge, the high-purity Al and the high-purity Nb alloy in S1 are respectively 99.9%, 99.99% and 99.99%.
3. The method for preparing TiAl nanocrystals under high pressure as claimed in claim 1, wherein the pretreatment in S1 refers to grinding the surface oxide with 400-mesh emery paper.
4. The method for preparing TiAl micro-crystals at high pressure according to claim 1, wherein the number of times of vacuum arc melting in S1 is 4, and the vacuum arc melting is turned over and subjected to two times of gas washing treatment after each melting is finished.
5. The method for preparing TiAl microcrystals under high pressure according to claim 1, wherein the alloy ingot is cut into the size which is in accordance with the cubic press briquetting assembly by electric spark in S2.
6. The method for preparing TiAl micro-crystals under high pressure according to claim 5, wherein the alloy ingot is cut into pieces in S2
The size of (c).
7. The method for preparing TiAl micro-crystals under high pressure according to claim 1, wherein the pretreatment in S3 is to clean the alloy sample with 5% HF solution, then polish off the oxide on the surface, and finally ultrasonically clean in absolute ethyl alcohol.
8. The method for preparing TiAl nanocrystals under high pressure as claimed in claim 1, wherein the materials used in assembling the compact in S3 include pyrophyllite, graphite, molybdenum sheets, boron nitride, and zirconia ceramics.
9. The method for preparing TiAl nanocrystals under high pressure as claimed in claim 1, wherein the press in S4 is a cubic press.
10. TiAl nanocrystals prepared according to the process of any one of claims 1 to 9.
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2020
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| EP3553193A1 (en) * | 2014-07-14 | 2019-10-16 | MTU Aero Engines GmbH | Al-rich high temperature tial alloy |
| CN104746128A (en) * | 2015-02-10 | 2015-07-01 | 中国科学院物理研究所 | Large-size high-pressure oxide single crystal growth method |
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