CN114807831A - Metal bonding layer with controllable aluminum content and preparation method thereof - Google Patents
Metal bonding layer with controllable aluminum content and preparation method thereof Download PDFInfo
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 83
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 66
- 239000002184 metal Substances 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 79
- 239000000956 alloy Substances 0.000 claims abstract description 79
- 239000007789 gas Substances 0.000 claims abstract description 79
- 238000005269 aluminizing Methods 0.000 claims abstract description 70
- 239000001257 hydrogen Substances 0.000 claims abstract description 59
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 59
- 238000006243 chemical reaction Methods 0.000 claims abstract description 53
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 52
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical group [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 52
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000012298 atmosphere Substances 0.000 claims abstract description 40
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 40
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 26
- 239000011248 coating agent Substances 0.000 claims abstract description 15
- 238000000576 coating method Methods 0.000 claims abstract description 15
- 239000013078 crystal Substances 0.000 claims abstract description 12
- 230000003213 activating effect Effects 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims description 21
- 238000001816 cooling Methods 0.000 claims description 13
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000004321 preservation Methods 0.000 abstract description 12
- 239000012720 thermal barrier coating Substances 0.000 abstract description 8
- 238000004140 cleaning Methods 0.000 description 21
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 20
- 229910000601 superalloy Inorganic materials 0.000 description 15
- 239000000758 substrate Substances 0.000 description 13
- 125000004429 atom Chemical group 0.000 description 12
- 229910052786 argon Inorganic materials 0.000 description 10
- 239000012808 vapor phase Substances 0.000 description 10
- 230000001276 controlling effect Effects 0.000 description 8
- 238000005260 corrosion Methods 0.000 description 8
- 230000007797 corrosion Effects 0.000 description 8
- 150000002431 hydrogen Chemical class 0.000 description 7
- 230000003647 oxidation Effects 0.000 description 7
- 238000007254 oxidation reaction Methods 0.000 description 7
- 239000012071 phase Substances 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 230000004913 activation Effects 0.000 description 6
- 229910002804 graphite Inorganic materials 0.000 description 6
- 239000010439 graphite Substances 0.000 description 6
- 238000007599 discharging Methods 0.000 description 5
- 238000005520 cutting process Methods 0.000 description 4
- 238000011049 filling Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 229910000943 NiAl Inorganic materials 0.000 description 3
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 238000007733 ion plating Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 229910052702 rhenium Inorganic materials 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 229910052715 tantalum Inorganic materials 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical group [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000005488 sandblasting Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
- C23C10/06—Solid state diffusion of only metal elements or silicon into metallic material surfaces using gases
- C23C10/08—Solid state diffusion of only metal elements or silicon into metallic material surfaces using gases only one element being diffused
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B31/00—Diffusion or doping processes for single crystals or homogeneous polycrystalline material with defined structure; Apparatus therefor
- C30B31/06—Diffusion or doping processes for single crystals or homogeneous polycrystalline material with defined structure; Apparatus therefor by contacting with diffusion material in the gaseous state
- C30B31/08—Diffusion or doping processes for single crystals or homogeneous polycrystalline material with defined structure; Apparatus therefor by contacting with diffusion material in the gaseous state the diffusion materials being a compound of the elements to be diffused
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B31/00—Diffusion or doping processes for single crystals or homogeneous polycrystalline material with defined structure; Apparatus therefor
- C30B31/06—Diffusion or doping processes for single crystals or homogeneous polycrystalline material with defined structure; Apparatus therefor by contacting with diffusion material in the gaseous state
- C30B31/18—Controlling or regulating
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Abstract
The invention provides a metal bonding layer with controllable aluminum content and a preparation method thereof, belonging to the technical field of thermal barrier coatings. The invention provides a preparation method of a metal bonding layer with controllable aluminum content, which comprises the following steps: (1) preheating the high-temperature alloy and aluminum in a hydrogen atmosphere to obtain a preheated high-temperature alloy and preheated aluminum; (2) activating the preheated aluminum by using a mixed gas of hydrogen and hydrogen chloride to obtain an activated gas; (3) carrying out aluminizing reaction on the preheated high-temperature alloy in the atmosphere of the activated gas to obtain a metal bonding layer; the high-temperature alloy is nickel-based single crystal high-temperature alloy or high-temperature alloy with a nickel-based coating attached to the surface; the flow ratio of the hydrogen to the hydrogen chloride is (10-80): 1; and the heat preservation time of the aluminizing reaction is 4-8 h. The invention achieves the purpose of controlling the aluminum content in the metal bonding layer by controlling the aluminizing time and the flow ratio of the hydrogen to the hydrogen chloride.
Description
Technical Field
The invention relates to the technical field of thermal barrier coatings, in particular to a metal bonding layer with controllable aluminum content and a preparation method thereof.
Background
The nickel-based single crystal superalloy blade is widely applied to gas turbines and aero-engines, and the thermal barrier coating has excellent heat insulation, high temperature resistance, oxidation corrosion resistance, abrasion resistance and other properties, so that the thermal barrier coating plays a role in heat insulation protection on the surface of the nickel-based single crystal superalloy blade. The structure of the thermal barrier coating of the turbine blade in practical application is a double-layer structure, namely a ceramic layer and a metal bonding layer. The metal bonding layer has the function of relieving the thermal mismatch between the ceramic layer and the alloy substrate, and meanwhile, because the metal bonding layer contains Al element, the Al element can be gradually oxidized in the service process of an engine to form a layer of continuous and compact Al 2 O 3 The film plays a role in delaying or preventing the high-temperature alloy from being continuously oxidized, so that the high-temperature oxidation corrosion resistance of the blade is improved. Because the content of Al element in the metal bonding layer is opposite to Al 2 O 3 The growth speed, the components, the integrity of the oxide layer, the binding force with a substrate and other factors have a determining function, and the factors directly influence the service life of the thermal barrier coating, so that the aluminizing treatment of the metal bonding layer is carried out to improve the aluminum content in the metal bonding layer, and the method is a general method for improving the high-temperature oxidation resistance and the heat corrosion resistance of the high-temperature alloy.
The currently used aluminizing methods mainly include: pack aluminizing, VPA vapor phase aluminizing and CVD vapor phase aluminizing, but CVD vapor phase aluminizing is gradually replacing due to process advantagesTwo other aluminizing processes. CVD gas phase aluminizing refers to a process in which a workpiece is not in direct contact with an aluminizing agent in the aluminizing process, but is suspended in an aluminizing atmosphere, and active Al atoms are transported to the surface of an alloy substrate through the aluminizing atmosphere and react with the alloy substrate. Generally, the CVD vapor phase aluminizing process includes four steps: (1) reacting aluminum atom-providing raw material such as aluminum powder or ferroaluminum powder with hydrogen chloride gas at high temperature to produce active Al atom [ Al [ ]]Gaseous AlCl of 3 (ii) a (2) Containing active Al atoms [ Al]AlCl of 3 Diffusion transmission to the surface of the base sample; (3) active Al atom [ Al]The adsorption on the surface of the sample reduces the area of the active surface of the sample; (4) active Al atom [ Al ] on sample surface after adsorption]And combines with Ni atoms diffused to the surface in the matrix to form a compound phase.
However, in the process of forming the NiAl phase by adopting CVD vapor phase aluminizing, the Al content is difficult to control, mutual diffusion between the metal bonding layer and the high-temperature alloy is easy to cause serious, so that the degradation speed of the metal bonding layer is higher, and the service life of the thermal barrier coating is reduced; meanwhile, the NiAl coating is easy to have obvious brittleness and crack and peel off, and the use of the thermal barrier coating is limited.
Therefore, a method capable of controlling the aluminum content in the process of forming the NiAl phase by vapor phase aluminizing is provided, so that the metal bonding layer is not easy to crack and peel, and the metal bonding layer and the substrate are not easy to diffuse mutually, which becomes a technical problem to be solved in the field.
Disclosure of Invention
The invention aims to provide a metal bonding layer with controllable aluminum content and a preparation method thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a metal bonding layer with controllable aluminum content, which comprises the following steps:
(1) preheating the high-temperature alloy and aluminum in a hydrogen atmosphere to obtain a preheated high-temperature alloy and preheated aluminum;
(2) activating the preheated aluminum in the step (1) by using a mixed gas of hydrogen and hydrogen chloride to obtain an activated gas;
(3) carrying out aluminizing reaction on the preheated high-temperature alloy obtained in the step (1) in the atmosphere of the activated gas obtained in the step (2) to obtain a metal bonding layer;
the high-temperature alloy in the step (1) is nickel-based single crystal high-temperature alloy or high-temperature alloy with a nickel-based coating attached to the surface;
the flow ratio of the hydrogen to the hydrogen chloride in the step (2) is (10-80): 1;
and (4) keeping the temperature of the aluminizing reaction in the step (3) for 4-8 h.
Preferably, the pressure of the hydrogen atmosphere in the step (1) is 15 to 30 kPa.
Preferably, the temperature rise rate of the preheating in the step (1) is 5-15 ℃/min.
Preferably, the preheating temperature in the step (1) is 850-1080 ℃, and the preheating heat preservation time is 0.5-2 h.
Preferably, the gas pressure of the mixed gas in the step (2) is 15-30 kPa.
Preferably, the flow rate of the hydrogen chloride in the mixed gas in the step (2) is 0.5-1L/min.
Preferably, the temperature of the aluminizing reaction in the step (3) is 850-1080 ℃.
Preferably, the cooling mode of the aluminizing reaction in the step (3) is natural cooling.
The invention provides the metal bonding layer prepared by the preparation method in the technical scheme, and the thickness of the metal bonding layer is 10-50 mu m.
Preferably, the aluminum content in the metal bonding layer is 30-60 at.%.
The invention provides a preparation method of a metal bonding layer with controllable aluminum content, which comprises the following steps: (1) preheating the high-temperature alloy and aluminum in a hydrogen atmosphere to obtain a preheated high-temperature alloy and preheated aluminum; (2) the preheating aluminum in the step (1) is carried out by adopting a mixed gas of hydrogen and hydrogen chlorideActivating to obtain activated gas; (3) carrying out aluminizing reaction on the preheated high-temperature alloy obtained in the step (1) in the atmosphere of the activated gas obtained in the step (2) to obtain a metal bonding layer; the high-temperature alloy in the step (1) is a nickel-based single crystal high-temperature alloy or a high-temperature alloy with a nickel-based coating attached to the surface; the flow ratio of the hydrogen to the hydrogen chloride in the step (2) is (10-80): 1; and (4) keeping the temperature of the aluminizing reaction in the step (3) for 4-8 h. The invention uses hydrogen chloride gas as an activating agent to chlorinate aluminum to form gas-phase AlCl x Then through the gas phase AlCl x The nickel-based coating is aluminized, so that the content of Al in the bonding layer can be improved; mixing hydrogen chloride and hydrogen, reacting with aluminum, gas-phase aluminizing, and regulating the flow ratio of hydrogen to hydrogen chloride to regulate the content of active Al atom in the mixed gas]Gaseous AlCl of 3 The content of aluminum in the atmosphere during vapor phase aluminizing is controlled, and the aluminum content in the metal bonding layer is controlled by controlling the time of aluminizing reaction. The embodiment results show that the preparation method provided by the invention can control the aluminum content in the metal bonding layer within 30-60 at.%, so that the metal bonding layer is not easy to crack and peel under the condition of high-temperature oxidation corrosion resistance, and the interdiffusion between the metal bonding layer and a substrate is light.
Drawings
FIG. 1 is a sectional SEM image of a metal bonding layer prepared in example 4 of the invention.
Detailed Description
The invention provides a preparation method of a metal bonding layer with controllable aluminum content, which comprises the following steps:
(1) preheating the high-temperature alloy and aluminum in a hydrogen atmosphere to obtain a preheated high-temperature alloy and preheated aluminum;
(2) activating the preheated aluminum in the step (1) by using a mixed gas of hydrogen and hydrogen chloride to obtain an activated gas;
(3) and (3) carrying out aluminizing reaction on the preheated high-temperature alloy obtained in the step (1) in the atmosphere of the activated gas obtained in the step (2) to obtain the metal bonding layer.
According to the invention, the high-temperature alloy and the aluminum are preheated in the hydrogen atmosphere to obtain the preheated high-temperature alloy and the preheated aluminum.
In the invention, the high-temperature alloy is nickel-based single crystal high-temperature alloy or high-temperature alloy with a nickel-based coating attached to the surface. In the present invention, the superalloy having a nickel-based coating attached to the surface thereof is preferably a nickel-based single crystal superalloy or a cobalt-based single crystal superalloy; the nickel-based coating is preferably a NiCrAlYSi bondcoat. The specific composition and source of the alloy are not particularly limited in the present invention, and may be commercially available products well known to those skilled in the art or may be prepared by themselves. The preparation method of the alloy is not particularly limited, and the alloy can be prepared by adopting a multi-arc ion plating mode and the like which are well known to those skilled in the art.
In the present invention, the superalloy is preferably a clean-surface superalloy, and when the superalloy does not satisfy the above conditions, the present invention preferably performs a pretreatment on the superalloy. In the present invention, the pretreatment is preferably performed by degreasing cleaning or sand blast cleaning. The invention can remove impurities on the surface of the high-temperature alloy through pretreatment.
In the present invention, the preheating is preferably performed in a CVD apparatus. The CVD apparatus of the present invention is not particularly limited in its specific type, and may be a commercially available product known to those skilled in the art.
In the present invention, the alloy is preferably placed in a reaction chamber of a CVD apparatus, more preferably suspended over the interior of the reaction chamber; the aluminum is preferably placed in a graphite labyrinth of the reaction chamber. The invention has no special limit on the dosage of the aluminum, and the graphite labyrinth is filled.
Before preheating, the CVD equipment is preferably cleaned by the method. In the present invention, the cleaning is preferably performed by sequentially performing vacuum pumping and argon gas introduction. In the present invention, the degree of vacuum of the evacuation is not particularly limited, and may be determined according to the technical common knowledge of those skilled in the art. In the present invention, the pressure after the argon gas is introduced is preferably atmospheric pressure. The invention has no special limit on the cleaning times, and can completely remove the air. The invention can remove the air in the CVD equipment through cleaning, thereby reducing the content of impurities in the air, laying a foundation for the subsequent process, discharging oxygen and improving the safety of the process.
In the present invention, the pressure of the hydrogen atmosphere is preferably 15 to 30kPa, and more preferably 20 to 25 kPa. The invention can make the temperature of the raw material more uniform by preheating in the hydrogen atmosphere.
In the invention, the preheating temperature rise rate is preferably 5-15 ℃/min, and more preferably 10 ℃/min; the preheating temperature is preferably 850-1080 ℃, more preferably 900-1000 ℃, and further preferably 960-980 ℃; the preheating heat preservation time is preferably 0.5-2 hours, and more preferably 1-1.5 hours. The invention can lead the raw material to be more completely preheated and lead the temperature to reach the aluminizing temperature at the same time by controlling the preheating parameters, thereby being convenient for the subsequent aluminizing process.
After the preheated alloy and the aluminum are obtained, the method adopts the mixed gas of hydrogen and hydrogen chloride to activate the preheated aluminum to obtain activated gas.
In the invention, the gas pressure of the mixed gas is preferably 15 to 30kPa, and more preferably 20 to 25 kPa; the flow rate of the hydrogen chloride in the mixed gas is preferably 0.5-1L/min, and more preferably 0.6-0.8L/min; the flow ratio of the hydrogen to the hydrogen chloride is (10-80): 1, preferably (20-60): 1, more preferably (30 to 40): 1, more preferably 30: 1. the invention can control the flow ratio of hydrogen and hydrogen chloride to control the active Al atom (Al)]Gaseous AlCl of 3 The larger the flow ratio of the hydrogen to the hydrogen chloride is, the less active Al atoms are generated by activating with the aluminum, the smaller the flow ratio is, the more active Al atoms are generated by activating with the aluminum, so that the contact amount of the active Al atoms and a substrate in the subsequent aluminizing reaction process can be controlled, and the aim of controlling the aluminum content in the metal bonding layer is fulfilled.
In the invention, the activation temperature is preferably 850-1080 ℃, more preferably 900-1000 ℃, and further preferably 960-980 ℃. The invention uses the mixed gas of hydrogen and hydrogen chlorideActivation with preheated aluminum can convert hydrogen chloride to active Al atom]Gaseous AlCl of 3 Thereby facilitating the subsequent vapor phase aluminizing.
After the activated gas is obtained, the invention carries out aluminizing reaction on the preheated high-temperature alloy in the atmosphere of the activated gas to obtain the metal bonding layer.
In the invention, the temperature of the aluminizing reaction is preferably 850-1080 ℃, more preferably 900-1000 ℃, and further preferably 960-980 ℃; the heat preservation time of the aluminizing reaction is 4-8 h, preferably 5-7 h, and more preferably 6 h. The invention can better carry out the aluminizing reaction by controlling the parameters of the aluminizing reaction, the longer the aluminizing reaction time is, the more the aluminum content is, the short the aluminizing reaction time is, the less the aluminum content is, and the effect of controlling the aluminum content can be further achieved by controlling the aluminizing time.
In the invention, the tail gas flowing out from the aluminizing reaction is preferably discharged into the atmosphere after being introduced into an alkali pool. The specific components of the alkali pool are not particularly limited, and the hydrogen chloride in the tail gas can be completely absorbed. The invention can reduce the pollution of the tail gas to the air by the treatment mode.
After the completion of the aluminizing reaction, the present invention preferably cools the product of the aluminizing reaction. In the present invention, the cooling is preferably performed in an argon atmosphere; the cooling is preferably natural cooling. By cooling under the above conditions, the invention can avoid further aluminizing during cooling, so that the aluminum content in the bonding layer is too high.
When the aluminum is activated, the hydrogen is selected as the carrier gas to mix the hydrogen chloride and the aluminum for activation, the flow ratio of the hydrogen to the hydrogen chloride is controlled, the content of activated aluminum atoms can be controlled, then the aluminum is contacted with the high-temperature alloy for vapor phase aluminizing, and the time of the vapor phase aluminizing is controlled, so that the purpose of controlling the aluminum content in the metal bonding layer is achieved, the high-temperature oxidation resistance and the heat corrosion resistance of the metal bonding layer can be adjusted, the problem that the metal bonding layer is easy to crack and peel is solved, and the service life of the metal bonding layer is prolonged.
The metal bonding layer prepared by the preparation method provided by the invention has the thickness of 10-50 μm, preferably 15-45 μm, more preferably 15-40 μm, and further preferably 15-30 μm. The thickness of the metal bonding layer is controlled within the range, so that the metal bonding layer has good high-temperature oxidation resistance and heat corrosion resistance, meanwhile, the metal bonding layer is not easy to crack and peel, the interdiffusion between the metal bonding layer and the substrate is light, and the coating is not easy to degrade.
In the invention, the aluminum content in the metal bonding layer is preferably 30-60 at.%. The invention controls the aluminum content in the metal bonding layer within the range, thereby not only having good high temperature resistance and corrosion resistance, but also being not easy to crack.
The invention provides the application of the metal bonding layer in the technical scheme in gas turbines and aircraft engines.
In the present invention, the metallic bond coat is preferably used in superalloy blades in gas turbines and aircraft engines.
The metal bonding layer provided by the invention can improve the high-temperature oxidation resistance and the heat corrosion resistance of high-temperature alloy blades in gas turbines and aeroengines, and meanwhile, the blades are not easy to crack and peel, so that the service life of the blades is prolonged.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. 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
A preparation method of a metal bonding layer with controllable aluminum content comprises the following steps:
(1) suspending the high-temperature alloy above a reaction chamber of CVD equipment after deoiling and cleaning, filling aluminum in a graphite labyrinth of the reaction chamber, cleaning the CVD equipment, introducing hydrogen into the CVD equipment, and preheating in a hydrogen atmosphere to obtain a preheated alloy and preheated aluminum; the high-temperature alloy is a high-temperature alloy with a nickel-based coating attached to the surface; the cleaning mode is that the CVD equipment is sequentially vacuumized and argon is introduced to the atmosphere, and the cleaning times are 3 times; the pressure of the hydrogen atmosphere is 20 kPa; the preheating heating rate is 10 ℃/min, the preheating temperature is 960 ℃, and the preheating heat preservation time is 1 h;
(2) after the preheating is finished, stopping introducing hydrogen, continuously introducing a preheated mixed gas of hydrogen and hydrogen chloride, and activating the preheated aluminum in the step (1) by using the mixed gas of hydrogen and hydrogen chloride to obtain an activated gas; the gas pressure of the mixed gas is 20kPa, the flow rate of hydrogen chloride in the mixed gas is 0.6L/min, and the flow rate ratio of hydrogen to hydrogen chloride is 30: 1; the temperature of the activation is 960 ℃;
(3) carrying out aluminizing reaction on the preheated high-temperature alloy obtained in the step (1) in the atmosphere of the activated gas obtained in the step (2) to obtain a metal bonding layer, discharging tail gas flowing out of the aluminizing reaction into the atmosphere after passing through an alkaline pool, stopping introducing mixed gas after the aluminizing reaction is finished, continuously introducing argon, and naturally cooling to room temperature to obtain the metal bonding layer; the temperature of the aluminizing reaction is 960 ℃, and the heat preservation time of the aluminizing reaction is 4 hours;
the preparation method of the high-temperature alloy in the step (1) comprises the following steps:
1) using commercial IC21 nickel-based single crystal superalloy as a base material, cutting the base alloy into pieces with the specification of 10 × 8 × 3mm by a wire cutting method 3 The two ends of the sample are respectively cut with a hole with the diameter of 1mm, so that the sample is hung on a bracket when the metal bonding layer is prepared; sequentially grinding six surfaces of the cut matrix sample by using No. 200, No. 600 and No. 800 water grinding sandpaper to ensure that the surface roughness Ra of the matrix is<0.8, then, chamfering all 12 edges into a fillet, carrying out sand blasting on the obtained sample (the mesh number of the used fine sand is 20 meshes, the pressure is 0.2MPa), carrying out ultrasonic cleaning on the obtained substrate sample for 15min by using absolute ethyl alcohol and acetone in sequence, and drying to obtain a pretreated nickel-based high-temperature alloy substrate;
2) with NiCThe rAlYSi alloy is taken as a target material and consists of the following elements in percentage by mass: cr19.3 percent, Al12.12 percent, Y0.41 percent, Si0.85 percent and the balance of Ni, the surface of the nickel-based superalloy substrate pretreated by the step 1) is subjected to multi-arc ion plating, the arc current of the multi-arc ion plating is 170A, the bias voltage is 15V, and the background vacuum degree is 2 multiplied by 10 -3 Pa; the temperature of the pretreated nickel-based superalloy substrate is 350 ℃, and a NiCrAlYSi layer is formed to obtain the superalloy.
Example 2
A preparation method of a metal bonding layer with controllable aluminum content comprises the following steps:
(1) suspending the high-temperature alloy above a reaction chamber of CVD equipment after deoiling and cleaning, filling aluminum in a graphite labyrinth of the reaction chamber, cleaning the CVD equipment, introducing hydrogen into the CVD equipment, and preheating in a hydrogen atmosphere to obtain a preheated alloy and preheated aluminum; the high-temperature alloy is a high-temperature alloy with a nickel-based coating attached to the surface; the cleaning mode is that the CVD equipment is sequentially vacuumized and argon is introduced to the atmosphere, and the cleaning times are 3 times; the pressure of the hydrogen atmosphere is 20 kPa; the preheating heating rate is 10 ℃/min, the preheating temperature is 960 ℃, and the preheating heat preservation time is 1 h;
(2) after the preheating is finished, stopping introducing hydrogen, continuously introducing a preheated mixed gas of hydrogen and hydrogen chloride, and activating the preheated aluminum in the step (1) by using the mixed gas of hydrogen and hydrogen chloride to obtain an activated gas; the gas pressure of the mixed gas is 20kPa, the flow rate of hydrogen chloride in the mixed gas is 0.6L/min, and the flow rate ratio of hydrogen to hydrogen chloride is 30: 1; the temperature of the activation is 960 ℃;
(3) carrying out aluminizing reaction on the preheated high-temperature alloy obtained in the step (1) in the atmosphere of the activated gas obtained in the step (2), discharging tail gas flowing out of the aluminizing reaction into the atmosphere after passing through an alkaline pool, stopping introducing mixed gas after the aluminizing reaction is finished, continuously introducing argon, and naturally cooling to room temperature to obtain a metal bonding layer; the temperature of the aluminizing reaction is 960 ℃, and the heat preservation time of the aluminizing reaction is 6 hours;
the high-temperature alloy in the step (1) is Ni3 Al-based single crystal high-temperature alloy IC21, and the components of the high-temperature alloy are as follows (atomic percent): al: 16.5%, Mo: 8.7%, Ta: 0.8 percent; cr: 2.3%, Re: 0.2%, Y: 0.03% and Ni: the balance; the alloy was cut in the (001) direction using wire cutting into disks 14mm in diameter and 2mm in thickness.
Example 3
A preparation method of a metal bonding layer with controllable aluminum content comprises the following steps:
(1) suspending the high-temperature alloy above a reaction chamber of CVD equipment after deoiling and cleaning, filling aluminum in a graphite labyrinth of the reaction chamber, cleaning the CVD equipment, introducing hydrogen into the CVD equipment, and preheating in a hydrogen atmosphere to obtain a preheated alloy and preheated aluminum; the high-temperature alloy is a high-temperature alloy with a nickel-based coating attached to the surface; the cleaning mode is that the CVD equipment is sequentially vacuumized and argon is introduced to the atmosphere, and the cleaning times are 3 times; the pressure of the hydrogen atmosphere is 20 kPa; the preheating heating rate is 10 ℃/min, the preheating temperature is 960 ℃, and the preheating heat preservation time is 1 h;
(2) after the preheating is finished, stopping introducing the hydrogen, continuously introducing the preheated mixed gas of the hydrogen and the hydrogen chloride, and activating the preheated aluminum in the step (1) by adopting the mixed gas of the hydrogen and the hydrogen chloride to obtain activated gas; the gas pressure of the mixed gas is 20kPa, the flow rate of hydrogen chloride in the mixed gas is 0.6L/min, and the flow rate ratio of hydrogen to hydrogen chloride is 30: 1; the temperature of the activation is 960 ℃;
(3) carrying out aluminizing reaction on the preheated high-temperature alloy obtained in the step (1) in the atmosphere of the activated gas obtained in the step (2), discharging tail gas flowing out of the aluminizing reaction into the atmosphere after passing through an alkaline pool, stopping introducing mixed gas after the aluminizing reaction is finished, continuously introducing argon, and naturally cooling to room temperature to obtain a metal bonding layer; the heat preservation time of the aluminizing reaction is 8 hours;
the high-temperature alloy in the step (1) is Ni3 Al-based single crystal high-temperature alloy IC21, and the components of the high-temperature alloy are as follows (atomic percent): al: 16.5%, Mo: 8.7%, Ta: 0.8 percent; cr: 2.3%, Re: 0.2%, Y: 0.03% and Ni: the balance; the alloy was cut in the (001) direction using wire cutting into disks 14mm in diameter and 2mm in thickness.
Example 4
A preparation method of a metal bonding layer with controllable aluminum content comprises the following steps:
(1) suspending the high-temperature alloy above a reaction chamber of CVD equipment after deoiling and cleaning, filling aluminum in a graphite labyrinth of the reaction chamber, cleaning the CVD equipment, introducing hydrogen into the CVD equipment, and preheating in a hydrogen atmosphere to obtain a preheated alloy and preheated aluminum; the high-temperature alloy is a high-temperature alloy with a nickel-based coating attached to the surface; the cleaning mode is that the CVD equipment is sequentially vacuumized and argon is introduced to the atmosphere, and the cleaning times are 3 times; the pressure of the hydrogen atmosphere is 20 kPa; the preheating heating rate is 10 ℃/min, the preheating temperature is 960 ℃, and the preheating heat preservation time is 1 h;
(2) after the preheating is finished, stopping introducing hydrogen, continuously introducing a preheated mixed gas of hydrogen and hydrogen chloride, and activating the preheated aluminum in the step (1) by using the mixed gas of hydrogen and hydrogen chloride to obtain an activated gas; the gas pressure of the mixed gas is 20kPa, the flow rate of hydrogen chloride in the mixed gas is 0.5L/min, and the flow rate ratio of hydrogen to hydrogen chloride is 20: 1; the temperature of the activation is 960 ℃;
(3) carrying out aluminizing reaction on the preheated high-temperature alloy obtained in the step (1) in the atmosphere of the activated gas obtained in the step (2), discharging tail gas flowing out of the aluminizing reaction into the atmosphere after passing through an alkaline pool, stopping introducing mixed gas after the aluminizing reaction is finished, continuously introducing argon, and naturally cooling to room temperature to obtain a metal bonding layer; the temperature of the aluminizing reaction is 960 ℃, and the heat preservation time of the aluminizing reaction is 5 hours;
the superalloy in step (1) is the same as in example 1.
The thickness of the metallic bonding layer prepared in example 4 was 15 μm.
The aluminum content of the metal bonding layers prepared in examples 1-3 is shown in table 1:
TABLE 1 aluminum content in Metal adhesion layers prepared in examples 1-3
| Examples | Aluminum content (at.%) |
| Example 1 | 39.23％ |
| Example 2 | 45.45％ |
| Example 3 | 51.83％ |
As can be seen from Table 1, the aluminum content in the metal bonding layer gradually increases with the increase of the aluminizing reaction time, which indicates that the technical scheme of the invention can achieve the purpose of artificially regulating the aluminum content in the metal bonding layer.
The cross-sectional SEM morphology of the metallic bonding layer prepared in example 4 is shown in fig. 1. As can be seen from FIG. 1, the metal bonding layer is tightly combined with the substrate, and the interdiffusion condition is light, so that the degradation of the coating can be avoided.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of a metal bonding layer with controllable aluminum content comprises the following steps:
(1) preheating the high-temperature alloy and aluminum in a hydrogen atmosphere to obtain a preheated high-temperature alloy and preheated aluminum;
(2) activating the preheated aluminum in the step (1) by using a mixed gas of hydrogen and hydrogen chloride to obtain an activated gas;
(3) carrying out aluminizing reaction on the preheated high-temperature alloy obtained in the step (1) in the atmosphere of the activated gas obtained in the step (2) to obtain a metal bonding layer;
the high-temperature alloy in the step (1) is nickel-based single crystal high-temperature alloy or high-temperature alloy with a nickel-based coating attached to the surface;
the flow ratio of the hydrogen to the hydrogen chloride in the step (2) is (10-80): 1;
and (4) keeping the temperature of the aluminizing reaction in the step (3) for 4-8 h.
2. The production method according to claim 1, wherein the pressure of the hydrogen atmosphere in the step (1) is 15 to 30 kPa.
3. The preparation method according to claim 1, wherein the temperature rise rate of the preheating in the step (1) is 5-15 ℃/min.
4. The preparation method according to claim 1, wherein the preheating temperature in the step (1) is 850-1080 ℃, and the preheating holding time is 0.5-2 h.
5. The method according to claim 1, wherein the gas pressure of the mixed gas in the step (2) is 15 to 30 kPa.
6. The method according to claim 1, wherein the flow rate of the hydrogen chloride in the mixed gas of the step (2) is 0.5 to 1L/min.
7. The method according to claim 1, wherein the temperature of the aluminizing reaction in the step (3) is 850 to 1080 ℃.
8. The method according to claim 1, wherein the cooling of the aluminizing reaction in the step (3) is natural cooling.
9. The metal bonding layer prepared by the preparation method of any one of claims 1 to 8, wherein the thickness of the metal bonding layer is 10 to 50 μm.
10. The metallic bonding layer according to claim 9, wherein the aluminum content in the metallic bonding layer is 30 to 60 at.%.
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| CN115786759A (en) * | 2022-11-11 | 2023-03-14 | 广州众山精密科技有限公司 | Equipment and method for preparing near-net-shape aluminum-based silicon carbide foil by gas-phase aluminizing |
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| CN113789556A (en) * | 2021-09-16 | 2021-12-14 | 北航（四川）西部国际创新港科技有限公司 | Method for preparing composite bonding layer by combining electroplating and chemical vapor deposition and composite bonding layer |
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