CN114657501A - Method for improving high-temperature oxidation resistance of high Nb-TiAl alloy - Google Patents

Method for improving high-temperature oxidation resistance of high Nb-TiAl alloy Download PDF

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CN114657501A
CN114657501A CN202210189090.8A CN202210189090A CN114657501A CN 114657501 A CN114657501 A CN 114657501A CN 202210189090 A CN202210189090 A CN 202210189090A CN 114657501 A CN114657501 A CN 114657501A
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alloy
tial alloy
temperature
oxidation resistance
oxidation
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CN114657501B (en
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王永胜
于盛旺
穆雁洵
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Taiyuan University of Technology
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • C23C8/10Oxidising
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C14/00Alloys based on titanium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium
    • C22C21/003Alloys based on aluminium containing at least 2.6% of one or more of the elements: tin, lead, antimony, bismuth, cadmium, and titanium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C30/00Alloys containing less than 50% by weight of each constituent
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/02Pretreatment of the material to be coated

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Turbine Rotor Nozzle Sealing (AREA)

Abstract

A method for improving the high-temperature oxidation resistance of a high Nb-TiAl alloy belongs to the field of high-temperature oxidation resistance of the surface of the high Nb-TiAl alloy. The method is characterized in that a sodium fluoride solution is used for treating the surface of the high Nb-TiAl alloy, and then a sample is subjected to high-temperature oxidation treatment to generate an oxide film on the surface of the high Nb-TiAl alloy, so that the long-term oxidation resistance of the high Nb-TiAl alloy is improved. The specific method and the process are as follows: treating the surface of the high Nb-TiAl alloy for 15-30 s by using an aqueous solution of sodium fluoride, wherein the concentration of fluorine ions is 0.08-0.12 mol/L; then, washing the surface of the product by using deionized water, then washing the product by using alcohol and then drying the product; in a heat treatment furnace, the temperature is raised to 900-950 ℃ for oxidation treatment for 3-5 h, so that a compact aluminum oxide film is generated on the surface of the aluminum oxide film. The invention has simple process and easy engineering application.

Description

Method for improving high-temperature oxidation resistance of high Nb-TiAl alloy
Technical Field
The invention belongs to the field of intermetallic compound high-temperature structural materials, and particularly relates to a method for improving the high-temperature oxidation resistance of the surface of a high Nb-TiAl alloy.
Background
The thrust-weight ratio of the engine is increased along with the weight reduction of the aircraft, the engine serving as a core component of the aerospace aircraft directly influences the overall weight of the aircraft, and the aircraft engine with high thrust-weight ratio is sought by engine manufacturers in various countries. The gamma-TiAl alloy is an important material for high thrust-weight ratio aircraft engine blades and low-pressure turbine blades due to light weight, high-temperature strength, good high-temperature creep and the like, and has important application value in the field of aerospace. However, its insufficient high-temperature oxidation resistance is one of the major problems that prevent its practical industrial application. The high Nb-TiAl alloy (Nb content is 5-10%, Al content is 43-49%) is used as a new member of a gamma-TiAl alloy system, and has more excellent comprehensive performance. For example, compared with common gamma-TiAl, the Ti- (43-45) Al- (8-10Nb) - (W, B, Y) alloy has the advantages that the melting point is higher by 100 ℃, the yield strength at 900 ℃ is higher by 150MPa, the high-temperature creep resistance is improved by 2-10 times, and the oxidation resistance at 750-800 ℃ is good. Therefore, the service temperature of the high Nb-TiAl alloy is improved by 100 ℃ compared with that of the common gamma-TiAl alloy. However, the alloy also has the problem of insufficient oxidation resistance at the service temperature, so that the actual working temperature of the material is far lower than the target service temperature, the advantages of high-temperature mechanical properties cannot be fully exerted, and the practical engineering application of the alloy in the fields of aerospace and the like is limited. Therefore, the preparation of the high-temperature protective coating on the surface of the high Nb-TiAl alloy and the high-temperature oxidation resistance mechanism of the high Nb-TiAl alloy are researched, theoretical reference is provided for the design and manufacture of high-performance and high-reliability aeroengine parts, and the engineering application of the alloy in the fields of aerospace and the like can be promoted.
From the aspect of engineering application effect, the protective effect can be formed on the TiAl base material as long as the surface film or the coating of the gamma-TiAl alloy can play an anti-oxidation function in the service process and the bonding performance with the base material is ensured. German schau tze et al investigated the effect of halogen element injection on the oxidation behavior of TiAl alloys. At the oxide film/substrate interface, the ion implanted halogen first reacts with Al to form a thermodynamically stable aluminum halide. Although the ion implantation is performed at a low temperature and has a small influence on the substrate, the ion implantation is easily degraded at a high temperature with a very limited implantation amount and depth, and the ion implantation is performed at a room temperature and has a small influence on the substrate, the ion implantation is easily degraded at a high temperature with a very limited implantation amount and depth, and the ion implantation equipment is expensive and cannot process the grooves and the complex-shaped portions of the parts. The blade in practical application has a complex shape, and with the improvement of the plasticity and the processing technology of the TiAl alloy, the TiAl alloy blade is likely to be subjected to hollowing treatment like a nickel-based blade in the future. Conventional coating preparation and ion implantation approaches have difficulty providing protection both inside and outside such blades. Therefore, there is a need to find a process for antioxidant treatment of blades that can be used on both complex blades and hollow blades.
Disclosure of Invention
The invention aims to overcome the problem of insufficient high-temperature oxidation resistance of a high Nb-TiAl alloy and provides a treatment method for improving the oxidation resistance of the high Nb-TiAl alloy at 900-950 ℃.
A method for improving the high-temperature oxidation resistance of a high Nb-TiAl alloy is characterized by comprising the following steps:
(1) performing surface treatment on the high Nb-TiAl alloy by adopting a sodium fluoride aqueous solution with the fluorine ion concentration of 0.08-0.12mol/L for 30-60s, cleaning the surface of the Nb-TiAl alloy by using deionized water for 5-10min, cleaning by using alcohol for 5-10min, and drying by using a blower; wherein the selected alloy components are as follows: the Al content is: (43-46) at.%; the Nb content is: (6-10) at.%; the trace elements (W, B, Y) are: (0.3-1) at.%, and the balance Ti, wherein the original structure of the alloy is in a casting state, a forging state, a rolling state or a 3D printing state;
(2) raising the temperature to 900-950 ℃ for oxidation treatment for 3-5 h to promote alpha-Al by fluoride ions2O3Formation of continuous film, sodium ion promoted Al2O3And TiO2Formation of Al2TiO5Obtaining compact Al on the surface of Nb-TiAl alloy2O3A film; and during long-term oxidation, Al2O3A transition layer rich in niobium is generated in situ under the film, thereby improving the bonding performance of the surface oxide film and the high Nb-TiAl alloy.
Compared with the prior art, the invention has the following beneficial effects:
compared with the existing coating technology (thermal spraying, thermal barrier coating, laser surface cladding, magnetron sputtering, anodic oxidation, evaporation and the like), the method has the advantages that the sodium fluoride introduced into the alloy surface has low density and low content, the weight of the treated alloy is increased very low before oxidation, the oxidation resistance of an oxide film generated in the oxidation process can be effectively improved, the bonding property of the oxide and the toughness phase at the interface of an alloy matrix can be effectively improved, and according to an oxidation resistance determination experiment method (national standard 5858-2000) of steel and high-temperature alloy, the high-Nb-TiAl alloy treated by the method reaches the level of complete oxidation resistance at 900-950 ℃. In addition, the process method is simple, easy to operate and easy to realize engineering application. Therefore, the result of the invention has important significance for improving the high-temperature oxidation resistance and protection of high-Nb-TiAl alloy aeroengine parts (blades and turbine discs).
Drawings
FIG. 1 is a graph showing the kinetics of cyclic oxidation of Ti-45 Al-8.5 Nb- (W, B, Y) alloy at 950 ℃ for 1000 hours.
FIG. 2 shows the surface morphology of Ti-45 Al-8.5 Nb- (W, B, Y) alloy after cyclic oxidation at 950 ℃ for 1000 h.
FIG. 3 shows the cross-sectional morphology of Ti-45 Al-8.5 Nb- (W, B, Y) alloy after 1000h cyclic oxidation at 950 ℃.
FIG. 4 shows XRD results of Ti-45 Al-8.5 Nb- (W, B, Y) alloy after cyclic oxidation at 950 ℃ for 1000 h.
FIG. 5 shows the room temperature tensile fracture of Ti-45 Al-8.5 Nb- (W, B, Y) alloy after cyclic oxidation at 950 ℃ for 1000 h.
FIG. 6 shows XRD results of isothermal oxidation of Ti-45 Al-8.5 Nb- (W, B, Y) alloy at 900 ℃ for 100 h.
FIG. 7 shows XRD results of 950 ℃ isothermal oxidation for 100h of Ti-45 Al-8.5 Nb- (W, B, Y) alloy.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
(1) selecting and casting Ti-45 Al-8.5 Nb- (W, B, Y) alloy according to the national standard size of 20 x 10 x 1.5mm3Cutting a sample, and then grinding, polishing, ultrasonic alcohol cleaning and drying by a blower.
(2) The fluorine treatment method comprises the following steps: weighing sodium fluoride salt by using an electronic balance (accurate to 0.0001) to prepare an aqueous solution with the concentration of fluoride ions of 0.1mol/L, placing the alloy sample prepared in the previous step in the aqueous solution for waiting for 60s, then taking out the sample to place in a deionized water beaker, carrying out ultrasonic vibration cleaning for 10min, then taking out the sample to place in alcohol, carrying out ultrasonic vibration cleaning for 10min, and then taking out the sample to blow dry by using a blower.
(3) The heat treatment process comprises the following steps: firstly, raising the temperature of a heat treatment furnace to 950 ℃, and placing the sample treated in the previous step into the heat treatment furnace for oxidation treatment for 3 hours to obtain an oxide layer on the surface of the sample; good oxidation resistance and bonding performance are obtained in the subsequent long-term oxidation (1000 h). FIG. 1 is a graph showing the oxidation kinetics curves of Ti-45 Al-8.5 Nb- (W, B, Y) alloy at 950 ℃ cyclic oxidation for 1000h, and the oxidation weight gain is about 0.5mg/cm2The oxidation resistance of the product can reach the complete oxidation resistance level according to the national standard; FIG. 2 shows the surface morphology of Ti-45 Al-8.5 Nb- (W, B, Y) alloy after cyclic oxidation at 950 ℃ for 1000h, which indicates that the surface is mainly Al2O3(ii) a FIG. 3 shows the cross-sectional morphology of Ti-45 Al-8.5 Nb- (W, B, Y) alloy after cyclic oxidation at 950 ℃ for 1000h, and it can be seen that there are no holes, cracks, etc. between the oxide cross-section and the alloy matrix. FIG. 4 shows XRD results of Ti-45 Al-8.5 Nb- (W, B, Y) alloy after cyclic oxidation at 950 ℃ for 1000h, and Al can be detected2O3、TiO2And Al2TiO5. FIG. 5 shows tensile fracture at room temperature after Ti-45 Al-8.5 Nb- (W, B, Y) alloy is cyclically oxidized at 950 ℃ for 1000h, and the separation and peeling of the oxide layer can be seen from the fracture, which shows that the bonding performance of the oxide layer and the alloy matrix is good.
Example 2:
(1) the alloy component is Ti-45 Al-8.5 Nb- (W, B, Y), and the original structure is in a forging state. The rest is the same as in example 1.
(2) The fluorine treatment method comprises the following steps: as in example 1, the concentration of the sodium fluoride solution was 0.12 mol/L.
(3) The heat treatment process comprises the following steps: the heat treatment temperature was 950 ℃ for 5 hours as in example 1; good oxidation resistance and bonding performance are obtained in the subsequent oxidation (100 h). FIG. 6 shows XRD results of Ti-45 Al-8.5 Nb- (W, B, Y) alloy in forged state after cyclic oxidation at 950 ℃ for 100h, and Al as an oxide can be detected2O3、TiO2And Al2TiO5
Example 3:
(1) the alloy component is Ti-45 Al-8.5 Nb- (W, B, Y), and the original structure is in a rolling state. The rest is the same as in example 1.
(2) The fluorine treatment method comprises the following steps: the concentration of the sodium fluoride solution was 0.08mol/L as in example 1.
(3) The heat treatment process comprises the following steps: the heat treatment temperature was 900 ℃ for 5 hours as in example 1; good oxidation resistance and bonding performance are obtained in the subsequent oxidation (100 h). FIG. 7 shows XRD results of Ti-45 Al-8.5 Nb- (W, B, Y) alloy after cyclic oxidation at 950 ℃ for 100h, and Al can be detected2O3、TiO2And Al2TiO5

Claims (1)

1. A method for improving the high-temperature oxidation resistance of a high Nb-TiAl alloy is characterized by comprising the following steps:
carrying out fluorine treatment on the high Nb-TiAl alloy for 30-60s by adopting a sodium fluoride aqueous solution with the fluorine ion concentration of 0.08-0.12mol/L, cleaning the surface of the high Nb-TiAl alloy for 5-10min by using deionized water, cleaning for 5-10min by using alcohol, and drying by using a blower; the alloy comprises the following components: the Al content is: (43-46) at.%; the Nb content is: (6-10) at.%; the content of W is: (0.3-1) at.%; the content of B is: (0.3-1) at.%; the content of Y is as follows: (0.3-1) at.%, and the balance Ti, wherein the original structure of the alloy is in a casting state, a forging state, a rolling state or a 3D printing state;
(2) raising the temperature to 900-950 ℃ for oxidation treatment for 3-5 h to promote alpha-Al by fluoride ions2O3Form a continuous film, and form sodium ionsPromotion of Al2O3And TiO2Formation of Al2TiO5Obtaining compact Al on the surface of Nb-TiAl alloy2O3A film; and during long-term oxidation, Al2O3A transition layer rich in niobium is generated in situ under the film, thereby improving the bonding performance of the surface oxide film and the high Nb-TiAl alloy.
CN202210189090.8A 2022-02-28 2022-02-28 Method for improving high-temperature oxidation resistance of high-Nb-TiAl alloy Active CN114657501B (en)

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