CN111254372A - Method for reducing oxidation of TiAl alloy - Google Patents
Method for reducing oxidation of TiAl alloy Download PDFInfo
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- CN111254372A CN111254372A CN202010093920.8A CN202010093920A CN111254372A CN 111254372 A CN111254372 A CN 111254372A CN 202010093920 A CN202010093920 A CN 202010093920A CN 111254372 A CN111254372 A CN 111254372A
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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
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/68—Temporary coatings or embedding materials applied before or during heat treatment
- C21D1/70—Temporary coatings or embedding materials applied before or during heat treatment while heating or quenching
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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
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
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Abstract
When a box-type resistance furnace is used for carrying out heat treatment on a TiAl alloy sample, the TiAl alloy sample is wrapped by asbestos and then is buried in sand in a container. The heat treatment temperature is 700-1400 ℃, the heat preservation is carried out for 0.5-100 h, and the temperature of the sample is raised and lowered along with the furnace. And taking out the sample after the furnace temperature is cooled to room temperature. When the TiAl alloy is embedded in sand for heat treatment, the oxygen content in the surface structure of the casting is low, and an oxide layer is thin; after the sample which is not treated is subjected to heat treatment, the oxygen content in the surface structure is obviously increased, and the thickness of the oxidation layer is obviously increased, which shows that the sand covers the surface of the casting to slow down the action of oxygen and the casting, thereby obviously reducing the oxidation of the surface of the casting and improving the surface quality of the casting. The method is simple and easy to operate, the sand can be repeatedly used, and the cost is saved.
Description
Technical Field
The invention relates to the technical field of oxidation prevention, in particular to a method for reducing oxidation of TiAl alloy.
Background
The titanium-aluminum alloy is widely applied to the fields of aviation, aerospace, automobiles and the like due to the excellent high-temperature performance of the titanium-aluminum alloy. Heat treatment is an important thermal process to improve texture and performance. Suitable heat treatment processes can improve the microstructure and mechanical properties. The TiAl alloy can generate four typical structures of a near gamma structure, a two-state structure, a near lamellar structure and a full lamellar structure in the heat treatment process, wherein the lamellar structure is an ideal structure under the high-temperature service condition of the TiAl alloy. The TiAl alloy needs to be subjected to heat treatment in a high temperature region above 1000 ℃ in order to obtain a lamellar structure. In addition, the TiAl alloy castings generally need to be subjected to high-temperature heat treatment to eliminate microsegregation and improve the uniformity of the structure. However, when the TiAl alloy is subjected to heat treatment in a high-temperature region, the surface of the alloy is seriously oxidized, the surface structure of the alloy is changed due to oxygen absorption through high-temperature oxidation, the surface performance of the alloy is deteriorated, and the performance of the TiAl alloy is uneven.
The oxidation of the alloy during the heat treatment is generally prevented by placing the alloy in a vacuum furnace or an inert gas-protected heat treatment furnace for heat treatment, but this increases the cost of the heat treatment.
Zhao Huijun in "written in Chinese non ferrous metals (English edition)" 2015 (6): 1881-. The vacuum sealing method can provide a vacuum environment, but the quartz glass tube is easy to break under the conditions of rapid cooling, rapid heating and high temperature. While the TiAl alloy is often heat-treated at temperatures above 1000 ℃ for a long time, the quartz glass tube is easily broken during the heat treatment.
The invention with the publication number of CN109320267A provides a preparation method of a temporary protective coating used in the heat treatment process of titanium alloy, which adopts a coating system consisting of enamel glaze and fillers such as quartz, clay and the like to coat the surface of a workpiece to reduce the oxidation in the heat treatment process of titanium alloy. After the heat treatment is finished, the coating is removed by sandblasting. However, the coating process and operation used in the method are complex and high in cost.
In summary, there are few reports on methods for reducing oxidation of TiAl alloys, and heat treatment is an important thermal processing procedure for improving alloy structure and properties. Therefore, a simple and feasible method for reducing oxidation of TiAl alloy is urgently needed.
Disclosure of Invention
In order to overcome the defect that the TiAl alloy is easy to oxidize in the high-temperature heat treatment process in the prior art, the invention provides a method for reducing the oxidation of the TiAl alloy.
The specific process of the invention is as follows:
step 1, preparing a TiAl alloy sample.
And 2, preparing a container. The vessel is filled with sand. The sand container is filled with mullite sand, zirconia sand or yttria sand.
And 3, carrying out heat treatment. Carrying out heat treatment on the TiAl alloy sample by adopting a box-type resistance furnace, which comprises the following steps:
and wrapping the TiAl alloy sample by using asbestos and then embedding the wrapped TiAl alloy sample into sand in a container. The heat treatment temperature is 700-1400 ℃, the heat preservation is carried out for 0.5-100 h, and the temperature of the sample is raised and lowered along with the furnace. And taking out the sample after the furnace temperature is cooled to room temperature.
Comparing fig. 1 and 2, it was found that the near surface tissue and oxygen content are significantly different. When the TiAl alloy is embedded in sand for heat treatment, the oxygen content in the surface structure of the casting is low, and an oxide layer is thin; after the sample which is not treated is subjected to heat treatment, the oxygen content in the surface structure is obviously increased, and the thickness of the oxidation layer is obviously increased, which shows that the sand covers the surface of the casting to slow down the action of oxygen and the casting, thereby obviously reducing the oxidation of the surface of the casting and improving the surface quality of the casting. The method is simple and easy to operate, the sand can be repeatedly used, and the cost is saved.
Drawings
FIG. 1 is SEM and EDS diagrams of near-surface structure of a sand-buried Ti-48Al-7Nb-2.5V-1Cr alloy sample; wherein: 1a is an SEM image of the near-surface tissue, and 1b is an EDS image of the oxygen content distribution in the near-surface tissue.
FIG. 2 is SEM and EDS diagrams of near-surface structure of untreated as-cast Ti-48Al-7Nb-2.5V-1Cr alloy samples; wherein 2a is an SEM image of the near-surface tissue, and 2b is an EDS image of the oxygen content distribution in the near-surface tissue.
Fig. 3 is a flow chart of the present invention.
Detailed Description
Example 1
This example is a method for mitigating oxidation of cylindrical TiAl alloy coupons. The specific process is as follows:
step 1, preparing a sample. The test sample is a TiAl alloy test sample. The TiAl alloy sample is a cylindrical sample of Ti-48Al-7Nb-2.5V-1Cr alloy, and the size is phi 12 multiplied by 10 mm.
And 2, preparing a container. The vessel had a diameter of 100mm and a height of 150 mm. The container was filled with mullite sand.
And 3, carrying out heat treatment. Wrapping the TiAl alloy sample by using asbestos, burying the wrapped TiAl alloy sample into sand in a container, and putting the container into a box-type resistance furnace. The box-type resistance furnace is heated to 1400 ℃ according to a conventional method, and the temperature is kept for 1 hour. And after the heat preservation is finished, cooling the TiAl alloy sample in the box-type resistance furnace to room temperature along with the furnace. The sample was taken out. Obtaining a TiAl alloy sample after heat treatment.
In order to verify the effect of the embodiment, the invention further provides a comparative example 1 of the embodiment, specifically:
step 1, preparing a sample. The TiAl alloy test piece is the same as the TiAl alloy test piece in the embodiment 1, is a cylindrical test piece of Ti-48Al-7Nb-2.5V-1Cr alloy and has the size of phi 12 multiplied by 10 mm.
And 2, preparing a container. The vessel had a diameter of 100mm and a height of 150 mm. The container was filled with mullite sand.
And 3, carrying out heat treatment. And placing the prepared TiAl alloy sample in a box-type resistance furnace. The box-type resistance furnace is heated to 1360 ℃ according to a conventional method, and the temperature is kept for 4 hours. And after the heat preservation is finished, cooling the TiAl alloy sample in the box-type resistance furnace to room temperature along with the furnace. The sample was taken out. Obtaining a TiAl alloy sample after heat treatment.
The TiAl alloy samples obtained in the examples and the TiAl alloy samples obtained in the comparative examples were subjected to SEM observation and EDS analysis of the microstructure, respectively. FIG. 1 is SEM and EDS images of a near-surface structure of a sample buried in sand and subjected to a heat treatment, and FIG. 2 is SEM and EDS images of a near-surface structure of a sample subjected to a heat treatment without any treatment. Comparing fig. 1 and fig. 2, it is found that the depth of the near-surface oxidation layer of the sample which is wrapped by asbestos and buried in sand for heat treatment is 40 μm, and the depth of the near-surface oxidation layer of the sample which is not treated is 600 μm, which proves that the oxidation of TiAl alloy can be effectively reduced and the surface quality of the casting can be improved by wrapping the sample by asbestos and burying the sample in sand for high-temperature heat treatment. The operation is simple, the sand can be recycled, and the cost is saved.
Example 2
The embodiment is a method for reducing blade oxidation, and the specific process is as follows:
step 1, preparing a sample. The test piece is a TiAl alloy blade. The TiAl alloy blade is a Ti-44Al-4Nb-2Cr alloy blade.
And 2, preparing a container. The vessel had a diameter of 100mm and a height of 150 mm. The container was filled with yttria sand.
And 3, carrying out heat treatment. Wrapping the TiAl alloy blade by using asbestos and burying the wrapped TiAl alloy blade into yttrium oxide sand in a container. The container was placed in a box-type resistance furnace. The box-type resistance furnace is heated to 1260 ℃ according to a conventional method, and the temperature is kept for 0.5 hour. And after the heat preservation is finished, cooling the TiAl alloy blade in the box-type resistance furnace to room temperature along with the furnace. The sample was taken out. Obtaining the TiAl alloy blade after heat treatment.
In order to verify the effect of the embodiment 2, the invention also provides a comparative example 2 of the embodiment, which specifically comprises the following steps:
step 1, preparing a sample. The TiAl alloy blade is the same as the TiAl alloy blade in the embodiment 2 and is a Ti-44Al-4Nb-2Cr alloy blade.
And 2, preparing a container. The vessel had a diameter of 100mm and a height of 150 mm. The container was filled with yttria sand.
And 3, carrying out heat treatment. And placing the prepared TiAl alloy blade in a box-type resistance furnace. The box-type resistance furnace is heated to 1260 ℃ according to a conventional method, and the temperature is kept for 0.5 hour. And after the heat preservation is finished, cooling the TiAl alloy blade in the box-type resistance furnace to room temperature along with the furnace. The sample was taken out. Obtaining the TiAl alloy blade after heat treatment.
SEM observation and EDS analysis of the microstructure were performed on the TiAl alloy blade obtained in example 2 and the TiAl alloy blade obtained in comparative example 2, respectively. Analysis shows that the oxidation degree of the blade is obviously reduced after the blade is wrapped by asbestos, embedded in sand and then subjected to heat treatment.
Example 3
The embodiment is a method for reducing the oxidation of a supercharged turbine, and the specific process is as follows:
step 1, preparing a sample. The sample is a Ti-48Al-2Nb-2Cr alloy supercharging turbine.
And 2, preparing a container. The vessel had a diameter of 150mm and a height of 20 mm. The vessel was filled with zirconia sand.
And 3, carrying out heat treatment. And wrapping the Ti-48Al-2Nb-2Cr alloy supercharged turbine by asbestos, and burying the wrapped asbestos in zirconia sand in a container. The container was placed in a box-type resistance furnace. The box-type resistance furnace is heated to 700 ℃ according to a conventional method, and the temperature is kept for 100 hours. And after the heat preservation is finished, cooling the Ti-48Al-2Nb-2Cr alloy supercharged turbine positioned in the box-type resistance furnace to room temperature along with the furnace. The sample was taken out. Obtaining the Ti-48Al-2Nb-2Cr alloy supercharged turbine after heat treatment.
In order to verify the effect of example 3, the invention also provides comparative example 3 of the present embodiment, specifically:
step 1, preparing a sample. The sample was the same as the sample in example 3, and was a Ti-48Al-2Nb-2Cr alloy turbo.
And 2, preparing a container. The vessel had a diameter of 150mm and a height of 200 mm. The vessel was filled with zirconia sand.
And 3, carrying out heat treatment. And placing the Ti-48Al-2Nb-2Cr alloy supercharging turbine into a box type resistance furnace. The box-type resistance furnace is heated to 700 ℃ according to a conventional method, and the temperature is kept for 100 hours. And after the heat preservation is finished, cooling the Ti-48Al-2Nb-2Cr alloy supercharged turbine positioned in the box-type resistance furnace to room temperature along with the furnace. The sample was taken out. Obtaining the Ti-48Al-2Nb-2Cr alloy supercharged turbine after heat treatment.
SEM observation and EDS analysis of the microstructure were performed on the Ti-48Al-2Nb-2Cr alloy turbo obtained in example 3 and the Ti-48Al-2Nb-2Cr alloy turbo obtained in comparative example 3, respectively. Analysis shows that the oxidation degree of the supercharged turbine is obviously reduced after the supercharged turbine is wrapped with asbestos, buried in sand and then subjected to heat treatment.
Example 7
This example is a method for mitigating oxidation of cylindrical TiAl alloy coupons. The specific process is as follows:
step 1, preparing a sample. The test sample is a TiAl alloy test sample. The TiAl alloy sample is a cylindrical sample of Ti-42Al-3.5Nb-1Mo alloy, and the size is phi 12 multiplied by 8 mm.
And 2, preparing a container. The vessel had a diameter of 100mm and a height of 150 mm. The vessel was filled with zirconia sand.
And 3, carrying out heat treatment. Wrapping the TiAl alloy sample by using asbestos, burying the wrapped TiAl alloy sample into sand in a container, and putting the container into a box-type resistance furnace. The box-type resistance furnace is heated to 900 ℃ according to a conventional method, and the temperature is kept for 50 hours. And after the heat preservation is finished, cooling the TiAl alloy sample in the box-type resistance furnace to room temperature along with the furnace. The sample was taken out. Obtaining a TiAl alloy sample after heat treatment.
In order to verify the effect of the embodiment, the invention further provides a comparative example 7 of the embodiment, which specifically comprises the following steps:
step 1, preparing a sample. The TiAl alloy test piece is the same as the TiAl alloy test piece in the embodiment 1, is a cylindrical test piece of Ti-42Al-3.5Nb-1Mo alloy and has the size of phi 12 multiplied by 8 mm.
And 2, preparing a container. The vessel had a diameter of 100mm and a height of 150 mm. The vessel was filled with zirconia sand.
And 3, carrying out heat treatment. And placing the prepared TiAl alloy sample in a box-type resistance furnace. The box-type resistance furnace is heated to 900 ℃ according to a conventional method, and the temperature is kept for 50 hours. And after the heat preservation is finished, cooling the TiAl alloy sample in the box-type resistance furnace to room temperature along with the furnace. The sample was taken out. Obtaining a TiAl alloy sample after heat treatment.
SEM observation and EDS analysis of the microstructure were performed on the Ti-42Al-3.5Nb-1Mo alloy cylindrical sample casting obtained in example 7 and the Ti-42Al-3.5Nb-1Mo alloy cylindrical sample obtained in comparative example 7, respectively. Analysis shows that the oxidation degree of the cylindrical sample is obviously reduced after the cylindrical sample is wrapped by asbestos, embedded in sand and then subjected to heat treatment.
Example 8
This example is a method for mitigating oxidation of cylindrical TiAl alloy coupons. The specific process is as follows:
step 1, preparing a sample. The test sample is a TiAl alloy test sample. The TiAl alloy sample is a cylindrical sample of Ti-48Al-7Nb-2.5V-1Cr alloy, and the size is phi 12 x 71 mm.
And 2, preparing a container. The vessel had a diameter of 100mm and a height of 150 mm. The container was filled with mullite sand.
And 3, carrying out heat treatment. Wrapping the TiAl alloy sample by using asbestos, burying the wrapped TiAl alloy sample into sand in a container, and putting the container into a box-type resistance furnace. The box-type resistance furnace is heated to 850 ℃ according to a conventional method, and the temperature is kept for 20 hours. And after the heat preservation is finished, cooling the TiAl alloy sample in the box-type resistance furnace to room temperature along with the furnace. The sample was taken out. Obtaining a TiAl alloy sample after heat treatment.
In order to verify the effect of the embodiment, the invention further provides a comparative example 1 of the embodiment, specifically:
step 1, preparing a sample. The TiAl alloy test piece is the same as the TiAl alloy test piece in the embodiment 1, is a cylindrical test piece of Ti-48Al-7Nb-2.5V-1Cr alloy and has the size of phi 12 x 71 mm.
And 2, preparing a container. The vessel had a diameter of 100mm and a height of 150 mm. The container was filled with mullite sand.
And 3, carrying out heat treatment. And placing the prepared TiAl alloy sample in a box-type resistance furnace. The box-type resistance furnace is heated to 850 ℃ according to a conventional method, and the temperature is kept for 20 hours. And after the heat preservation is finished, cooling the TiAl alloy sample in the box-type resistance furnace to room temperature along with the furnace. The sample was taken out. Obtaining a TiAl alloy sample after heat treatment.
SEM observation and EDS analysis of the microstructure were performed on the Ti-48Al-7Nb-2.5V-1Cr alloy cylindrical sample casting obtained in example 8 and the Ti-48Al-7Nb-2.5V-1Cr alloy cylindrical sample obtained in comparative example 8, respectively. Analysis shows that the oxidation degree of the cylindrical sample is obviously reduced after the cylindrical sample is wrapped by asbestos, embedded in sand and then subjected to heat treatment.
Example 9
This example is a method for mitigating oxidation of cylindrical TiAl alloy coupons. The specific process is as follows:
step 1, preparing a sample. The test sample is a TiAl alloy test sample. The TiAl alloy sample is a cylindrical sample of Ti-48Al-7Nb-2.5V-1Cr alloy, and the size is phi 12 multiplied by 7 mm.
And 2, preparing a container. The vessel had a diameter of 100mm and a height of 150 mm. The vessel was filled with zirconia sand.
And 3, carrying out heat treatment. Wrapping the TiAl alloy sample by using asbestos, burying the wrapped TiAl alloy sample into sand in a container, and putting the container into a box-type resistance furnace. The box-type resistance furnace is heated to 1000 ℃ according to a conventional method, and the temperature is kept for 60 hours. And after the heat preservation is finished, cooling the TiAl alloy sample in the box-type resistance furnace to room temperature along with the furnace. The sample was taken out. Obtaining a TiAl alloy sample after heat treatment.
In order to verify the effect of the embodiment, the invention further provides a comparative example 1 of the embodiment, specifically:
step 1, preparing a sample. The TiAl alloy test piece is the same as the TiAl alloy test piece in the embodiment 1, is a cylindrical test piece of Ti-48Al-7Nb-2.5V-1Cr alloy and has the size of phi 12 multiplied by 7 mm.
And 2, preparing a container. The vessel had a diameter of 100mm and a height of 150 mm. The vessel was filled with zirconia sand.
And 3, carrying out heat treatment. And placing the prepared TiAl alloy sample in a box-type resistance furnace. The box-type resistance furnace is heated to 1000 ℃ according to a conventional method, and the temperature is kept for 60 hours. And after the heat preservation is finished, cooling the TiAl alloy sample in the box-type resistance furnace to room temperature along with the furnace. The sample was taken out. Obtaining a TiAl alloy sample after heat treatment.
SEM observation and EDS analysis of the microstructure were performed on the Ti-48Al-7Nb-2.5V-1Cr alloy cylindrical sample casting obtained in example 8 and the Ti-48Al-7Nb-2.5V-1Cr alloy cylindrical sample obtained in comparative example 8, respectively. Analysis shows that the oxidation degree of the cylindrical sample is obviously reduced after the cylindrical sample is wrapped by asbestos, embedded in sand and then subjected to heat treatment.
Claims (2)
1. A method for reducing oxidation of TiAl alloy is characterized by comprising the following specific steps:
step 1, preparing a TiAl alloy sample;
step 2, preparing a container; the container is filled with sand;
step 3, heat treatment; carrying out heat treatment on the TiAl alloy sample by adopting a box-type resistance furnace, which comprises the following steps:
wrapping the TiAl alloy sample by using asbestos and then embedding the wrapped TiAl alloy sample into sand in a container; temperature of heat treatment
Keeping the temperature at 700-1400 ℃ for 0.5-100 h, and heating and cooling the sample along with the furnace; and taking out the sample after the furnace temperature is cooled to room temperature.
2. The method of mitigating oxidation of TiAl alloys of claim 1, wherein the sand vessel is filled with mullite sand or zirconia sand or yttria sand.
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