CN109536883B - Method for improving high-temperature oxidation resistance of Ti-45Al-8.5Nb alloy - Google Patents

Method for improving high-temperature oxidation resistance of Ti-45Al-8.5Nb alloy Download PDF

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CN109536883B
CN109536883B CN201811456032.7A CN201811456032A CN109536883B CN 109536883 B CN109536883 B CN 109536883B CN 201811456032 A CN201811456032 A CN 201811456032A CN 109536883 B CN109536883 B CN 109536883B
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王永胜
王亚榕
高洁
于盛旺
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Taiyuan University of Technology
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Abstract

A method for improving the high-temperature oxidation resistance of Ti-45Al-8.5Nb alloy belongs to the field of surface modification of titanium-aluminum alloy materials, and relates to a method for preparing a high-temperature oxidation resistance coating on the surface of the titanium-aluminum alloy by using a surface technology. The method is carried out on a Ti-45Al-8.5Nb alloyThe surface is coated with a metallic chromium (Cr) coating to improve the oxidation resistance. Placing the prepared Ti-45Al-8.5Nb alloy in a double-layer glow ion metal infiltration furnace, taking a Cr plate as a supply source, carrying out metal infiltration for 1-3 hours at the temperature of 800-1000 ℃, and changing the thickness of the coating and the bonding capacity of the Ti-45Al-8.5Nb alloy by adjusting the metal infiltration temperature and time to obtain the coating which is firmly bonded with the Ti-45Al-8.5Nb alloy. The results of isothermal oxidation weight increment experiments on the Ti-45Al-8.5Nb alloy with the prepared coating at 900 ℃ show that a large amount of compact Cr is formed when the Cr coating on the surface of the alloy is oxidized2O3Protective films, resulting in significantly lower oxidation weight gain than the uncoated alloy. Therefore, the method can effectively improve the high-temperature oxidation resistance of the Ti-45Al-8.5Nb alloy, and has important significance for the industrial application of the titanium-aluminum-niobium alloy.

Description

Method for improving high-temperature oxidation resistance of Ti-45Al-8.5Nb alloy
Technical Field
The invention belongs to the field of surface modification of titanium-aluminum alloy, and relates to a method for improving the high-temperature oxidation resistance of the titanium-aluminum alloy through a surface protective coating technology.
Background
With the development of industry, titanium-aluminum alloy in light alloy has excellent mechanical properties such as low density, high specific strength, high elastic modulus, high creep resistance and the like, and is widely applied to various industries. In which the working environment of many mechanical parts and electronic devices is severe, and is usually high temperature, high speed, high pressure, heavy load, strong corrosion, etc., so that it is necessary to improve the properties of wear resistance, heat resistance, corrosion resistance, fatigue resistance, etc. of the surface of the base material of the element. Adding a proper amount of niobium (Nb) element into the common titanium-aluminum alloy, and optimizing the strength, creep resistance, high-temperature oxidation resistance and the like. Under the high-temperature working conditions in the aerospace field, the titanium-aluminum alloy is required to have higher oxidation resistance besides good comprehensive mechanical properties. Under high temperature conditions, Al is formed2O3And TiO2Has very close standard Gibbs free energy, so that the preferential oxidation of Al can not be carried out, and Al can be formed on the surface2O3And TiO2A mixed layer of TiO2Loose and porous, resulting in oxygen atoms rapidlyQuickly diffused into the alloy matrix, and the oxidation resistance of the alloy matrix is rapidly reduced under high-temperature conditions. Therefore, attention is paid to how to improve the high-temperature oxidation resistance of the light titanium-aluminum alloy.
At present, two methods are mainly used for improving the high-temperature oxidation resistance of the titanium-aluminum alloy. The first is alloying, including multi-component alloying and micro-component alloying, the commonly used multi-component alloying elements include W, Mo, Cr, Si, Nb, etc., and the trace elements include Zr, Y, etc., the addition of W, Mo, etc. can reduce the diffusion rate of Ti and inhibit TiO2Promoting the formation of Al2O3Forming; the addition of a small amount of Zr and Y elements improves the adhesion of the oxide film. Ti- (42-45) Al- (0-4) (Cr, Mn, V) - (5-10) (Nb, Ta, Mo) - (0-1) (W, Si, C, B) alloy developed by Beijing university of science and technology shows excellent high-temperature oxidation resistance. However, the improvement of the high-temperature oxidation resistance of the titanium-aluminum alloy through alloying can bring adverse effects on mechanical properties of the titanium-aluminum alloy, such as toughness, strength and the like. A second method of improving the oxidation resistance of titanium aluminum alloys is surface modification techniques, including surface alloying and surface coating. The surface alloying is divided into ion implantation, diffusion and infiltration, surface chemical treatment and the like. Research shows that the high-temperature oxidation resistance of the titanium-aluminum alloy can be improved by ion implantation of elements such as Nb + Al, Nb + C or Nb + Si and the like on the surface of the titanium-aluminum alloy or diffusion carburization or silicon and the like, but the depth and the element content of the ion implantation are limited, and the diffusion carburized layer thickness and high-temperature internal oxidation are not easy to control, so that the high-temperature oxidation resistance of the titanium-aluminum alloy is limited. Surface coating systems include NiCrAlY, TiAlCr coating systems, TiAl-based coatings, ceramic coatings, and the like. Research shows that TiAl3The high-temperature oxidation resistance of the titanium-aluminum alloy is obviously improved by the coating, the ceramic coating and the like, but the bonding strength of the coating and the matrix and the reaction and mutual diffusion of the coating and the matrix in different degrees still remain problems. Therefore, the alloying material or surface technology alone cannot solve the problem.
Under the large background of high-speed development of science and technology at present, the power of an engine in the aerospace field is higher and higher, the working temperature is higher and higher, and compared with the condition that the surface of the traditional titanium-aluminum alloy is infiltrated with metal, the Nb-containing titanium-aluminum alloy is used for alloyingThe surface of Ti-Al alloy is infiltrated with metal chromium (Cr) to raise its oxidation resistance. The double-layer glow ion metal infiltration technology has unique advantages. A thicker alloy layer can be formed when metal ions are diffused, the metal content of the alloy layer is gradually changed, and the alloy layer has gradient, so that compared with a coating, the film is more firmly combined with a matrix and is not easy to fall off; ions moving at high speed in the glow discharge process can impact the surface of the workpiece, so that metal ions can better penetrate into the surface of the workpiece; the double-layer glow ion metal infiltration technology has wide application range, the parameters of metal infiltration materials, temperature, time and the like can be adjusted, and the coating materials, the coating thickness, the infiltration layer form and the like can be controlled by adjusting the parameters; from the environmental point of view, the technology is non-toxic and does not pollute the environment. There are problems in improving the high temperature oxidation resistance of alloys by adding Cr to titanium aluminum alloys, and when the amount of Cr added is more than 7%, Ti (Cr, Al) in the oxide film is promoted2 The formation of Laves phase is detrimental to the toughness of the alloy, and Cr content less than 4% promotes TiO formation2This is detrimental to the oxidation resistance of the alloy. However, Cr is more formable at high temperature than Al2O3Denser Cr2O3The oxide film, its thermal and chemical properties are also very stable. Therefore, the surface of the Ti-45Al-8.5Nb alloy is infiltrated with Cr by a double-layer glow ion technology, so that the Cr coating forms compact Cr at high temperature2O3The protective film can be used as a new method for improving the high-temperature oxidation resistance of the titanium-aluminum alloy.
Disclosure of Invention
The invention aims to provide a method for improving the high-temperature oxidation resistance of a titanium-aluminum alloy by using a double-layer glow ion metal infiltration technology. The combination between the metal infiltrated layer prepared by the technology and the matrix belongs to metallurgical combination, the combination of the coating and the Ti-45Al-8.5Nb alloy has no interface with abrupt performance, the combination is firmer, the metal content of the coating is gradually changed, and the chemical performance is more stable. When the Ti-45Al-8.5Nb alloy is subjected to isothermal oxidation at 900 ℃ for a long time, dense Cr is formed on the surface of the alloy2O3The oxidation film and the oxidation weight gain rate are obviously lower than the result when no coating is made, and the high-temperature oxidation resistance of the alloy is effectively improved. The specific process steps are as follows:
(1) smelting high-purity Ti (more than 99.99 percent), Al (more than 99.95 percent) and Nb (more than 99.95 percent) into titanium-aluminum alloy with the mass fraction of Ti-45Al-8.5Nb by adopting a vacuum arc furnace, and then casting the titanium-aluminum alloy into an alloy ingot by using a copper mold;
(2) cutting the alloy ingot into square alloy samples with the size of 10 multiplied by 5mm by wire cutting, polishing the periphery of the alloy samples from 600# to 2000# by SiC abrasive paper, putting the alloy samples into ultrasonic waves, cleaning the alloy samples by alcohol, and airing the alloy samples to prepare for double-layer glow ion metal infiltration;
(3) and infiltrating Cr on the surface of the Ti-45Al-8.5Nb by a double-layer glow ion metallization technology. The used equipment is a double-layer glow ion metal infiltration furnace, a sample is placed in the double-layer glow metal infiltration furnace, and argon with the purity of 99.99 percent is filled in the furnace;
(4) setting the metal infiltration time for 1-3h and the temperature of 800-1000 ℃ to obtain coatings in different forms;
(5) placing the Ti-45Al-8.5Nb alloy without the coating and the Ti-45Al-8.5Nb alloy with the coating into a high-temperature furnace with the temperature of 900 ℃ for isothermal oxidation, recording the weight gain, calculating an oxidation weight gain curve, representing the phase composition of an oxide film by XRD, and observing the microscopic morphology of the oxide film by SEM;
(6) and analyzing an oxidation weight gain curve and an oxide form to obtain that the high-temperature oxidation resistance of the alloy with the coating is obviously improved.
The metal infiltration source is a Cr plate, the metal infiltration time is 1-3h, and the temperature is 800-1000 ℃.
The invention has the advantages that the metal content of the metal infiltration layer is gradient, the combination between the coating and the Ti-45Al-8.5Nb alloy is firmer, and the chemical property is stable. The coating with different thickness and different metal content can be obtained by adjusting the temperature and the time of metal infiltration. The Cr is infiltrated on the surface of the alloy, and the mechanical property of the alloy is not greatly influenced. Cr (chromium) component2O3The oxide film is compact, the growth speed is slow, the performance is more stable, and Cr element also has great influence on hot corrosion, so the metal-infiltrated source electrode is selected to be Cr. The new method has no harm to the environment, the technical operation is simple, and the preparation cost can be saved.
Drawings
Cross section appearance after 1800 ℃ double-layer glow ion Cr-diffusion
FIG. 2 is a graph showing the oxidation kinetics of Ti-45Al-8.5Nb at 900 ℃ for isothermal oxidation for 90h
FIG. 3800 ℃ oxidation kinetics curve of isothermal oxidation of Cr-infiltrated alloy at 900 ℃ for 90h
FIG. 4800 XRD pattern of Cr-infiltrated alloy oxidized at 900 deg.C for 90h
FIG. 5 microscopic morphology of the sample surface after oxidation of Ti-45Al-8.5Nb for 90h
FIG. 6800 micro-morphology of sample surface after oxidation of Cr-infiltrated alloy at 6800 deg.C for 90h
FIG. 7 is an oxidation kinetics curve of Ti-45Al-8.5Nb alloy isothermal oxidation for 300h
FIG. 8800 ℃ Cr-infiltrated alloy oxidation kinetics curve at 900 ℃ for isothermal oxidation for 300h
FIG. 9800 ℃ XRD pattern of Cr-infiltrated alloy oxidized at 900 ℃ for 300h
FIG. 10 microscopic morphology of sample surface after oxidation of Ti-45Al-8.5Nb for 300h
Figure 11800 ℃ micro-morphology of the sample surface after oxidation of Cr-infiltrated alloy for 300h
Cross section morphology of 121000 deg.C double-layer glow ion Cr-infiltrated
FIG. 131000 ℃ oxidation kinetics curve of isothermal oxidation of Cr-infiltrated alloy for 90h
FIG. 141000 XRD pattern of Cr-infiltrated alloy oxidized at 900 deg.C for 90h
FIG. 151000 micro-topography of sample surface after oxidation of Cr-infiltrated alloy at 151000 deg.C for 90h
FIG. 161000 ℃ oxidation kinetics curve of isothermal oxidation of Cr-infiltrated alloy for 300h
FIG. 171000 ℃ XRD pattern of Cr-impregnated alloy oxidized at 900 ℃ for 300h
FIG. 181000 ℃ microscopic morphology of sample surface after oxidation of Cr-infiltrated alloy for 300h
Detailed Description
Example 1
(1) Smelting high-purity Ti (more than 99.99 percent), Al (more than 99.95 percent) and Nb (more than 99.95 percent) into high-Nb titanium-aluminum alloy with the mass fraction of Ti-45Al-8.5Nb by adopting a vacuum arc furnace, and then casting the alloy ingot by using a copper mold;
(2) cutting the alloy into square alloy samples with the size of 10 multiplied by 5mm by wire cutting, grinding the periphery of the samples from 600# to 2000# by SiC sand paper, putting the samples into ultrasonic waves, cleaning the samples by alcohol and airing the samples to prepare for double-layer glow ion metal infiltration;
(3) carrying out Cr infiltration on the surface of Ti-45Al-8.5Nb by a double-layer glow ion metal infiltration technology, placing a sample into a double-layer glow metal infiltration furnace, and filling argon with the purity of 99.99 percent into the furnace;
(4) the metal infiltration time is 2h, the temperature is 800 ℃, when the actual temperature reaches the set temperature, low-voltage heavy current is introduced to the two ends of the grid electrode to obtain a coating (figure 1) with the thickness of 2 mu m, the coating is compact and firmly combined with Ti-45Al-8.5Nb alloy, and the surface Cr content also reaches to form single compact Cr2O3The critical concentration of (c);
(5) placing the Ti-45Al-8.5Nb alloy without the coating and the Ti-45Al-8.5Nb alloy with the coating into a high-temperature furnace at 900 ℃ for isothermal oxidation for 90 hours and 300 hours, and characterizing by XRD, SEM and the like;
(6) the comparative study shows that the growth rate is faster at the initial stage of oxidation, the growth rate is parabolic at 90h of oxidation (figure 2), the advantages of the coated Ti-45Al-8.5Nb alloy are more and more obvious along with the prolonging of the oxidation time, and the oxidation weight gain rate is obviously lower than that of the uncoated Ti-45Al-8.5Nb alloy (figure 5, the rate of the uncoated Ti-45Al-8.5Nb alloy is 1.98 mg/cm)2H, the rate of the coated Ti-45Al-8.5Nb (800 ℃ Cr-infiltrated) alloy is 1.17mg/cm2H) while a dense Cr is formed on the surface of the coated Ti-45Al-8.5Nb alloy2O3The oxide film (fig. 3, 4, 6, 7) effectively prevents oxygen in the air from entering the alloy matrix, which is why the oxidation rate of the coated alloy is more and more stable.
Example 2
(1) Smelting high-purity Ti (more than 99.99 percent), Al (more than 99.95 percent) and Nb (more than 99.95 percent) into titanium-aluminum alloy with the mass fraction of Ti-45Al-8.5Nb by adopting a vacuum arc furnace, and then casting the titanium-aluminum alloy into an alloy ingot by using a copper mold;
(2) cutting the alloy ingot into square alloy samples with the size of 10 multiplied by 5mm by wire cutting, polishing the periphery of the alloy samples from 600# to 2000# by SiC abrasive paper, putting the alloy samples into ultrasonic waves, cleaning the alloy samples by alcohol, and airing the alloy samples to prepare for double-layer glow ion metal infiltration;
(3) carrying out Cr infiltration on the surface of Ti-45Al-8.5Nb by a double-layer glow ion metal infiltration technology, placing a sample into a double-layer glow metal infiltration furnace, and filling high-purity argon into the furnace;
(4) the metal infiltration time is 2h, the temperature is 1000 ℃, when the actual temperature reaches the set temperature, low-voltage heavy current is introduced to the two ends of the grid electrode, a coating with the thickness of about 10 mu m is obtained (figure 8), the coating is compact and firmly combined with Ti-45Al-8.5Nb alloy, and the surface Cr content also reaches to form single compact Cr2O3The critical concentration of (c);
(5) placing the Ti-45Al-8.5Nb alloy without the coating and the Ti-45Al-8.5Nb alloy with the coating into a high-temperature furnace at 900 ℃ for isothermal oxidation for 90 hours and 300 hours, and characterizing by XRD and SEM;
(6) the comparative study shows that the growth rate is faster at the initial stage of oxidation, the growth rate is parabolic at 90h of oxidation (figure 9), the advantages of the coated Ti-45Al-8.5Nb alloy are more and more obvious along with the prolonging of the oxidation time, and the oxidation weight gain rate is obviously lower than that of the uncoated Ti-45Al-8.5Nb alloy (figure 12, the rate of the uncoated Ti-45Al-8.5Nb alloy is 1.98 mg/cm)2H, the coated Ti-45Al-8.5Nb (Cr infiltration at 1000 ℃ C.) rate was 1.03mg/cm2H) with the formation of denser Cr on the coated alloy surface2O3The oxidation film (FIGS. 9, 10, 12, 13) had an oxidation rate significantly lower than that of the uncoated Ti-45Al-8.5Nb alloy and also lower than that of the coated Ti-45Al-8.5Nb alloy of example 1, which is more resistant to oxidation at high temperatures.
XRD is X-ray diffraction pattern; SEM is scanning electron microscope;
the above description is about the embodiments of the present invention having significant effects. Here, it should be noted that this method is not limited to the above embodiment.

Claims (4)

1. A method for improving the high-temperature oxidation resistance of Ti-45Al-8.5Nb alloy is characterized by comprising the following steps:
(1) smelting Ti, Al and Nb with the purity of more than 99.95 percent into alloy with the mass fraction of Ti-45Al-8.5Nb by adopting a vacuum arc furnace, then casting the alloy ingot by using a copper die, cutting the alloy ingot into square blocks with the size of 10 multiplied by 5mm, and polishing and cleaning;
(2) placing the sample into a double-layer glow metal infiltration furnace, and filling argon with the purity of 99.99% into the furnace, wherein the metal infiltration material is Cr; setting the metal infiltration time to be 1-3h, setting the metal infiltration temperature to be 800-1000 ℃, and introducing low-voltage heavy current to two ends of the grid when the actual temperature reaches the set temperature to obtain coatings with different thicknesses, wherein the coatings are compact and firmly combined with Ti-45Al-8.5Nb alloy;
(3) adjusting the temperature and time of metal infiltration to obtain an infiltration layer which is firmly combined with the Ti-45Al-8.5Nb alloy but has a different form;
(4) placing the Ti-45Al-8.5Nb alloy without the coating and the Ti-45Al-8.5Nb alloy with the coating into a high-temperature furnace at 900 ℃ for isothermal oxidation, characterizing the oxidation behavior of the samples by XRD and SEM, and analyzing the high-temperature oxidation behavior of two experimental samples; when the sample is put into a high-temperature furnace at 900 ℃ for isothermal oxidation, a layer of Cr is formed on the surface of the alloy with the coating2O3The dense oxide film results in a significantly lower rate of oxidation weight gain than would be the case without the coating, thereby improving the oxidation resistance of the Ti-45Al-8.5Nb alloy.
2. The method for improving the high-temperature oxidation resistance of the Ti-45Al-8.5Nb alloy according to claim 1, wherein the selected matrix alloy is the Ti-45Al-8.5Nb alloy, and the oxidation resistance of the Ti-Al alloy is improved by performing double-layer glow ion metal infiltration on the surface of the alloy.
3. A method for improving the high-temperature oxidation resistance of Ti-45Al-8.5Nb alloy is characterized by comprising the following steps:
(1) smelting Ti with the purity of more than 99.99 percent, Al with the purity of more than 99.95 percent and Nb with the purity of more than 99.95 percent into high-Nb titanium-aluminum alloy with the mass fraction of Ti-45Al-8.5Nb by adopting a vacuum arc furnace, and then casting the alloy ingot by using a copper mold;
(2) cutting the alloy into square alloy samples with the thickness of 10 multiplied by 5mm by linear cutting, grinding the periphery of the samples from 600# to 2000# by SiC abrasive paper, putting the samples into ultrasonic waves, cleaning the samples by alcohol and airing the samples to prepare for double-layer glow ion metal infiltration;
(3) carrying out Cr infiltration on the surface of Ti-45Al-8.5Nb by a double-layer glow ion metal infiltration technology, placing a sample into a double-layer glow metal infiltration furnace, and filling argon with the purity of 99.99 percent into the furnace;
(4) the metal infiltration time is 2h, the temperature is 800 ℃, when the actual temperature reaches the set temperature, low-voltage heavy current is introduced to the two ends of the grid electrode to obtain a coating with the thickness of 2 mu m, the coating is compact and firmly combined with Ti-45Al-8.5Nb alloy, and the surface Cr content also reaches to form single compact Cr2O3The critical concentration of (c);
(5) placing the Ti-45Al-8.5Nb alloy without the coating and the Ti-45Al-8.5Nb alloy with the coating into a high-temperature furnace at 900 ℃ for isothermal oxidation for 90h and 300h, and characterizing by XRD, SEM and the like;
(6) the oxidation time is 90 hours, the growth rate is parabolic, the advantages of the coated Ti-45Al-8.5Nb alloy are more and more obvious along with the prolonging of the oxidation time, the oxidation weight gain rate is obviously lower than the result when the coating is not made, and the rate of the uncoated Ti-45Al-8.5Nb alloy is 1.98mg/cm2H, rate of coated Ti-45Al-8.5Nb alloy 1.17mg/cm2H, the surface of the coated Ti-45Al-8.5Nb alloy forms dense Cr2O3The oxide film effectively prevents oxygen in the air from entering the alloy matrix.
4. A method for improving the high-temperature oxidation resistance of Ti-45Al-8.5Nb alloy is characterized by comprising the following steps:
(1) smelting Ti with the purity of more than 99.99 percent, Al with the purity of more than 99.95 percent and Nb with the purity of more than 99.95 percent into titanium-aluminum alloy with the mass fraction of Ti-45Al-8.5Nb by adopting a vacuum arc furnace, and then casting the titanium-aluminum alloy into an alloy ingot by using a copper mold;
(2) cutting the alloy ingot into square alloy samples with the size of 10 multiplied by 5mm by wire cutting, polishing the periphery of the alloy samples from 600# to 2000# by SiC abrasive paper, putting the alloy samples into ultrasonic waves, cleaning the alloy samples by alcohol, and airing the alloy samples to prepare for double-layer glow ion metal infiltration;
(3) carrying out Cr infiltration on the surface of Ti-45Al-8.5Nb by a double-layer glow ion metal infiltration technology, placing a sample into a double-layer glow metal infiltration furnace, and filling high-purity argon into the furnace;
(4) the metal infiltration time is 2h, the temperature is 1000 ℃, when the actual temperature reaches the set temperature, low-voltage heavy current is introduced to the two ends of the grid electrode to obtain a coating with the thickness of about 10 mu m, the coating is compact and firmly combined with Ti-45Al-8.5Nb alloy, and the surface Cr content also reaches to form single compact Cr2O3The critical concentration of (c);
(5) placing the Ti-45Al-8.5Nb alloy without the coating and the Ti-45Al-8.5Nb alloy with the coating into a high-temperature furnace at 900 ℃ for isothermal oxidation for 90h and 300h, and characterizing by XRD and SEM;
(6) the comparative research shows that the growth rates of the Ti-45Al-8.5Nb alloy are all faster in the initial oxidation stage and are parabolic after being oxidized for 90 hours, the advantages of the coated Ti-45Al-8.5Nb alloy are more and more obvious along with the prolonging of the oxidation time, the oxidation weight gain rate is obviously lower than the result when the coating is not made, and the rate of the uncoated Ti-45Al-8.5Nb alloy is 1.98mg/cm2H, the coated Ti-45Al-8.5Nb rate was 1.03mg/cm2H, simultaneously forming denser Cr on the surface of the coated alloy2O3An oxide film having an oxidation rate significantly lower than that of the uncoated Ti-45Al-8.5Nb alloy.
CN201811456032.7A 2019-01-21 2019-01-21 Method for improving high-temperature oxidation resistance of Ti-45Al-8.5Nb alloy Expired - Fee Related CN109536883B (en)

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