CN114657525B - FeCrAl/Ta alloy coating and preparation method thereof - Google Patents
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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
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
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- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
- C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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Abstract
The invention discloses a FeCrAl/Ta alloy coating and a preparation method thereof, comprising a Ta transition layer and a FeCrAl layer deposited on the surface of the Ta transition layer; the FeCrAl coating has chemical composition Fe to Cr to Al atomic percent of 79:10:11at%. The method has the advantages that the FeCrAl/Ta alloy coating is prepared on the polished zirconium alloy substrate by adopting a magnetron sputtering method, the Ta transition layer is deposited between the FeCrAl coating and the zirconium alloy substrate by controlling the deposition sequence of the Ta target and the FeCrAl alloy target, the intermediate transition layer prepared by the method has flat surface and less defects, the influence on the upper layer coating structure is less, the interface of the double-layer coating is clear and stable, the interface bonding performance of the film substrate is facilitated, and the obtained film has uniform components and compact structure; the addition of the Ta intermediate transition layer can effectively improve the service correlation of the FeCrAl coating.
Description
Technical Field
The invention relates to the field of metal surface modification, in particular to a FeCrAl/Ta alloy coating and a preparation method thereof.
Background
FeCrAl alloy is widely applied to the fields of aerospace, military industry, nuclear reactors and the like due to excellent high-temperature oxidation resistance and mechanical properties. In the high-temperature oxidation process, cr and Al elements in the alloy can rapidly form compact Cr on the surface of a sample 2 O 3 And Al 2 O 3 The oxide layer prevents oxygen from further corroding inwards, and shows excellent high-temperature oxidation resistance. Compared with the active zirconium alloy cladding material, the oxidation kinetic rate constant of the FeCrAl alloy is reduced by 3-5 orders of magnitude, and meanwhile, the good high-temperature mechanical property is maintained. Thus, it is listed as a candidate for a reactor accident tolerant fuel zirconium alloy cladding coating.
The surface modification is carried out on the active Zr alloy, namely, a layer of oxidation-resistant and corrosion-resistant protective coating is prepared on the surface of the cladding, the physical isolation of the zirconium cladding and the coolant is realized on the premise of not changing the structural design of the reactor, the accident fault-tolerant capability of the zirconium cladding is improved, and the method is the most practical and feasible solution for improving the service safety of the nuclear cladding in a short period of time.
However, feCrAl coating is directly deposited on the surface of Zr alloy, because the eutectic temperature of Fe-Zr is only 928 ℃, when water loss accident occurs, the cladding temperature can reach 1200 ℃, in the oxidation process of high-temperature vapor, serious interdiffusion can occur between the coating and matrix elements, a large number of cavities are formed in the interdiffusion zone due to the dissolution of Fe-Zr eutectic and the Kendall effect, the mechanical property of matrix and the interface combination of film base are seriously deteriorated, and even the matrix is deformed and the coating is fallen off.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a FeCrAl/Ta alloy coating and a preparation method thereof, and the prepared FeCrAl/Ta coating has uniform and compact microstructure and excellent high-temperature oxidation resistance.
The invention is realized by the following technical scheme:
a FeCrAl/Ta alloy coating comprises a Ta transition layer and a FeCrAl layer deposited on the surface of the Ta transition layer;
the crystal grains of the FeCrAl layer and the Ta transition layer are nano columnar crystals, the size of the nano columnar crystals is 50-80 nm, and the thickness of the Ta layer is 20-200nm.
Preferably, the atomic percentages of the elements in the FeCrAl layer are: 10-20at.% of Cr, 11at.% of Al and the balance of Fe.
Preferably, the thickness of the FeCrAl layer is 2.3+/-0.2 mu m.
A method of preparing a FeCrAl/Ta coating system comprising the steps of:
step 2, sputtering and depositing a Ta transition layer and a FeCrAl layer on the alloy substrate obtained in the step 1 in sequence by adopting a magnetron sputtering mode, and cooling to room temperature to obtain a FeCrAl/Ta alloy coating;
the Ta target adopts radio frequency electricity to carry out source sputtering, the sputtering power is 100W, and the deposition time of the Ta transition layer is 332s-3320s.
Preferably, the method for polishing and cleaning the alloy substrate in the step 1 is as follows:
and (3) carrying out sand paper grinding and polishing on the alloy matrix, and carrying out ultrasonic cleaning and drying on the polished alloy matrix.
Preferably, the vacuum etching method comprises the following steps:
and (3) conveying the cleaned alloy substrate into a magnetron sputtering coating chamber, and carrying out etching after vacuumizing, wherein the etching power is 200W, and the etching time is 5min.
Preferably, the method for sequentially depositing the Ta transition layer and the FeCrAl layer in the step 2 is as follows:
firstly, carrying out Ta transition layer deposition on a Ta target by adopting radio frequency power sputtering, and then carrying out double-target co-sputtering on two FeCrAl alloy targets by adopting a direct current power supply.
Preferably, the purity of the Ta target is 99.99wt.%, the sputtering power is 100W, the deposition air pressure is set to be 0.3Pa, the deposition temperature is room temperature, and the rotating speed of the substrate is 15r/min.
Preferably, the alloy matrix is a zirconium alloy, a steel matrix or a titanium alloy.
Compared with the prior art, the invention has the following beneficial technical effects:
a FeCrAl/Ta alloy coating, pure metal Ta has low solubility in Zr alloy, low interdiffusion coefficient with Zr matrix and similar thermal expansion coefficient with FeCrAl alloy coating, the intermediate transition layer should be selected as much as possible to be material with larger atomic size, the material with larger atomic size has higher diffusion activation energy, and the replacement compatibility between atomic sizes is smaller, thereby being capable of preventing interdiffusion between elements, ta has larger atomic size, the morphology is nano columnar crystal, the structure is compact and uniform, the material can be used as the preferable material of the intermediate transition layer of FeCrAl coating and Zr alloy matrix, and the Ta can be used as the intermediate transition layer to improve the service performance of FeCrAl coating.
According to the preparation method of the FeCrAl/Ta alloy coating, the magnetron sputtering is used for alternately sputtering the pure metal Ta target and the FeCrAl alloy target, the deposited coating has obvious interface and high deposition rate; the scattering effect of the working gas argon on sputtered atoms is weak, and the deposition efficiency and the adhesion of the film are further improved. Therefore, the deposited film is uniform and compact, has few defects, high purity and strong adhesive force. According to the invention, the transition layer is deposited between the FeCrAl coating and the Zr alloy matrix by controlling the deposition sequence of the pure metal Ta target and the FeCrAl alloy target, the intermediate transition layer prepared by the method has the advantages of smooth surface, few defects, convenience in depositing an upper coating, less influence on the upper coating structure, clear and stable interface of the double-layer coating, and convenience in subsequent study on interface characteristics and rules. The FeCrAl alloy target adopts direct current power of 200W, and the pure metal Ta target adopts radio frequency power source power of 100W.
And finally, naturally cooling the finished product to room temperature in a vacuum coating chamber, avoiding debonding and breaking of the film from the substrate caused by the difference of the thermal expansion coefficients of the film and the substrate, and preventing the film from being oxidized.
Drawings
FIG. 1 is a SEM surface photograph and EDS surface scanning element distribution diagram of a FeCrAl/Ta alloy coating of the invention.
FIG. 2 is a SEM photograph of a cross-section of a FeCrAl/Ta alloy coating according to the invention.
FIG. 3 is a TEM photograph of a low-magnification cross-section of a FeCrAl/Ta alloy coating of the invention.
Detailed Description
The invention will now be described in further detail with reference to the accompanying drawings, which illustrate but do not limit the invention.
A FeCrAl/Ta alloy coating comprises a Ta transition layer and a FeCrAl layer deposited on the surface of the Ta transition layer; the Ta transition layer is pure metal Ta, the atomic percentage of each element in the FeCrAl layer is Cr 10-20at%, al 11at% and the balance Fe; the grains of the Ta transition layer and the FeCrAl layer are nano columnar crystals, the size of the columnar crystals is 50-80 nm, the thickness of Ta is 20-200nm, and the thickness of the FeCrAl alloy coating is 2.3+/-0.2 mu m.
FIG. 1 shows SEM surface pictures and surface EDS scanning element distribution diagrams of a FeCrAl/Ta coating system of the invention; FIG. 2 shows SEM cross-sectional pictures of FeCrAl/Ta coating systems of the invention; FIG. 3 shows a low resolution TEM section image of a FeCrAl/Ta coating system of the invention. According to the FeCrAl/Ta coating system, the internal alloy elements are uniformly distributed, and the crystal grains are nano columnar crystals. The FeCrAl/Ta coating system provided by the invention has uniform and compact structure and excellent oxidation resistance.
A preparation method of a FeCrAl/Ta alloy coating comprises the following steps:
step 1: and grinding and polishing the alloy matrix to remove the oxide layer on the surface of the alloy matrix.
The polishing method comprises the steps of sequentially grinding the zirconium alloy matrix by adopting a cross grinding method, sequentially grinding 600, 1000, 1500 and 2000-mesh sand paper, polishing on a polishing machine, sequentially grinding the other surfaces by adopting 600, 1000 and 1500-mesh sand paper, and grinding the surface oxide layer until no scratch exists on the surface.
The alloy matrix is zirconium alloy, steel matrix or titanium alloy.
Step 2: and (3) carrying out ultrasonic cleaning on the alloy matrix subjected to grinding and polishing in the step (1).
Specifically, taking an alloy substrate with single-sided polishing, sequentially ultrasonically cleaning in acetone and ethanol for 10 minutes and drying, ensuring that the surface of the substrate is clean and free of stains and dust adhesion, and ultrasonically cleaning the polished alloy substrate, thereby being beneficial to improving the binding force of a film and the substrate.
Step 3: and (3) etching the alloy matrix obtained in the step (2) under the vacuum condition to remove impurities on the surface of the alloy matrix.
Specifically, the alloy matrix is glued to the base plate by conductive adhesive and is sent into a coating chamber, and the vacuum degree of the back bottom is pumped to 4.0 multiplied by 10 -4 And the etching power is 200W below Pa, and the etching time is 5min.
Step 4: and sequentially sputtering and depositing a Ta transition layer and a FeCrAl layer on the alloy substrate by adopting a magnetron sputtering method, sequentially sputtering and depositing to a preset thickness, and cooling to room temperature to obtain the FeCrAl/Ta alloy coating.
Specifically, an alloy substrate after ultrasonic cleaning is fixed on a base plate, an automatic machine is carried into a magnetron sputtering coating chamber, and vacuum is pumped until the vacuum degree of the back bottom is 4.0 multiplied by 10 -4 Pa or below.
And sequentially depositing a Ta transition layer and a FeCrAl layer on the alloy substrate by adopting a Ta target and a FeCrAl alloy target, and sputtering and depositing to a preset thickness, wherein the temperature is increased in the deposition process to ensure that the internal stress of a sample is small and prevent the sample from being oxidized in air, and taking out the substrate after the substrate is cooled to room temperature in a high vacuum coating chamber to obtain the FeCrAl/Ta alloy coating.
The purity of the FeCrAl alloy target is 99.9 wt%, the atomic percentage of each element in the FeCrAl layer is 10-20 at%, the Al is 11at%, and the rest is Fe. The FeCrAl alloy target is sputtered by a direct current power supply with the power of 200W.
Ta target purity 99.99wt.% adopts radio frequency power supply sputtering, power 100W, deposition air pressure setting 0.3Pa, deposition temperature is room temperature, substrate rotating speed 15r/min, vacuum degree is 4.0X10 -4 And (3) starting deposition preparation under Pa, wherein the deposition time of the Ta intermediate transition layer is 332s-3320s, the deposition time of the FeCrAl coating is 10800s, the thickness of the finally obtained Ta intermediate transition layer is 20-200nm, and the thickness of the FeCrAl coating is 2.3+/-0.2 mu m.
The principle of depositing a coating on the surface of a substrate by adopting a magnetron sputtering method is as follows: ar ionized from Ar gas + The target atoms sputtered from the target are deposited on the matrix by accelerating bombardment of the surface of the cathode target under the action of an electric field, and the sputtered secondary electrons are bound in a plasma region close to the surface of the target under the action of the electric field and a magnetic field, so that the collision probability with Ar is increased, and more Ar is ionized + A higher deposition rate is achieved. After the deposition is finished, the substrate is taken out after being fully cooled in a high vacuum coating chamber, so that the debonding and cracking caused by the difference of the thermal expansion coefficients of the substrate and the film material and the oxidation of high-temperature air are prevented. Finally, a FeCrAl/Ta coating system with an intermediate transition layer Ta is deposited.
Example 1
Step 1: the zirconium alloy substrate is sanded and polished.
Step 2: the zirconium alloy substrate polished on one side is respectively ultrasonically cleaned in acetone and ethanol for 10min, and dried by a blower.
Step 3: fixing zirconium alloy base on base plateThen mechanically and automatically carried into a vacuum coating chamber, wherein the vacuum degree of the back and the bottom before deposition is lower than 4.0x10 -4 Pa, and etching for 5min, wherein the etching power is 200W.
Step 4: and sequentially sputtering and depositing a Ta transition layer and a FeCrAl layer on the zirconium alloy base by adopting a magnetron sputtering method, sequentially sputtering and depositing to a preset thickness, and cooling to room temperature to obtain the FeCrAl/Ta alloy coating.
Wherein, the purity of the FeCrAl alloy target is 99.9wt.%, the atomic percentage of Fe to Cr to Al is 79:10:11at.%, the sputtering of direct current power supply power is adopted, the sputtering of radio frequency power supply power is adopted for 99.9wt.%, the deposition air pressure is 0.3Pa, the deposition temperature is room temperature, the rotating speed of the base plate is 15r/min, the deposition time of the Ta transition layer is 1660s, the deposition time of the FeCrAl coating is 10800s, the thickness of the finally obtained Ta transition layer is 100+/-20 nm, and the thickness of the FeCrAl coating is 2.3+/-0.2 mu m.
Step 5: and after the deposition is finished, naturally cooling the zirconium alloy base in a high vacuum sputtering chamber for 4 hours, and taking out to obtain the FeCrAl/Ta coating system.
The prepared FeCrAl/Ta coating system is subjected to microstructure characterization and oxidation performance test, and EDS element distribution data show that Fe: cr: al atomic percentage is 79:10:11at%, crystal grains are nano columnar crystals, and the coating system has excellent high-temperature oxidation resistance.
Example 2
Step 1: the steel substrate is sanded and polished.
Step 2: the single-sided polished steel substrate was ultrasonically cleaned in acetone and ethanol, respectively, for 10 minutes, and dried with a blower.
Step 3: fixing steel substrate on the substrate, mechanically and automatically feeding into vacuum coating chamber, and vacuum degree of back bottom before deposition is lower than 4.0X10 -4 Pa, and etching for 5min, wherein the etching power is 200W.
Step 4: and sequentially sputtering and depositing a Ta transition layer and a FeCrAl layer on the steel substrate by adopting a magnetron sputtering method, sequentially sputtering and depositing to a preset thickness, and cooling to room temperature to obtain the FeCrAl/Ta alloy coating.
Wherein, the purity of the FeCrAl alloy target is 99.9wt.%, the atomic percentage of Fe to Cr to Al is 74:15:11at.%, the sputtering of direct current power supply power is adopted, the sputtering of radio frequency power supply power is adopted for 99.9wt.%, the deposition air pressure is 0.3Pa, the deposition temperature is room temperature, the rotating speed of the base plate is 15r/min, the deposition time of the Ta intermediate transition layer is 332s, the deposition time of the FeCrAl coating is 10800s, the thickness of the finally obtained Ta transition layer is 20nm, and the thickness of the FeCrAl coating is 2.3+/-0.2 mu m.
Step 5: and after the deposition is finished, naturally cooling the steel matrix in a high vacuum sputtering chamber for 4 hours, and taking out to obtain the FeCrAl/Ta coating system.
The prepared FeCrAl/Ta coating system is subjected to microstructure characterization and oxidation performance test, and EDS element distribution data show that Fe: cr: al atomic percentage is 74:15:11at%, crystal grains are nano columnar crystals, and the coating system has excellent high-temperature oxidation resistance.
Example 3
Step 1: the titanium alloy substrate is sanded and polished.
Step 2: the single-sided polished titanium alloy substrate was ultrasonically cleaned in acetone and ethanol, respectively, for 10 minutes, and dried with a blower.
Step 3: fixing steel substrate on the substrate, mechanically and automatically feeding into vacuum coating chamber, and vacuum degree of back bottom before deposition is lower than 4.0X10 -4 Pa, and etching for 5min, wherein the etching power is 200W.
Step 4: and sequentially sputtering and depositing a Ta transition layer and a FeCrAl layer on the titanium alloy substrate by adopting a magnetron sputtering method, sequentially sputtering and depositing to a preset thickness, and cooling to room temperature to obtain the FeCrAl/Ta alloy coating.
Wherein, the purity of the FeCrAl alloy target is 99.9wt.%, the atomic percentage of Fe to Cr to Al is 69:20:11at.%, the sputtering of direct current power supply power is adopted, the sputtering of radio frequency power supply power is adopted for 99.9wt.%, the deposition air pressure is 0.3Pa, the deposition temperature is room temperature, the rotating speed of the base plate is 15r/min, the deposition time of the Ta intermediate transition layer is 3320s, the deposition time of the FeCrAl coating is 10800s, the thickness of the finally obtained Ta intermediate layer is 200nm, and the thickness of the FeCrAl coating is 2.3+/-0.2 mu m.
Step 5: and after the deposition is finished, naturally cooling the titanium alloy matrix in a high vacuum sputtering chamber for 4 hours, and taking out to obtain the FeCrAl/Ta coating system.
The prepared FeCrAl/Ta coating system is subjected to microstructure characterization and oxidation performance test, and EDS element distribution data show that Fe: cr: al atomic percentage is 69:20:10at%, and crystal grains are nano columnar crystals, so that the coating system has excellent high-temperature oxidation resistance.
The above is only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited by this, and any modification made on the basis of the technical scheme according to the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (5)
1. The FeCrAl/Ta alloy coating is characterized by comprising a Ta transition layer and a FeCrAl layer deposited on the surface of the Ta transition layer;
the crystal grains of the FeCrAl layer and the Ta transition layer are nano columnar crystals, the size of the nano columnar crystals is 50-80 nm, and the thickness of the Ta layer is 20-200 nm;
the FeCrAl layer comprises the following elements in atomic percent: 10-20: 20 at% of Cr, 11at% of Al and the balance of Fe;
the preparation method of the FeCrAl/Ta coating comprises the following steps:
step 1, grinding, cleaning and vacuum etching are carried out on a zirconium alloy matrix;
step 2, sputtering and depositing a Ta transition layer and a FeCrAl layer on the zirconium alloy substrate obtained in the step 1 in sequence by adopting a magnetron sputtering mode, and cooling to room temperature to obtain a FeCrAl/Ta alloy coating;
the method for sequentially sputtering and depositing the Ta transition layer and the FeCrAl layer comprises the following steps:
firstly, carrying out Ta transition layer deposition on a Ta target by adopting radio frequency power sputtering, and then carrying out double-target co-sputtering on two FeCrAl alloy targets by adopting a direct current power supply;
the Ta target adopts a radio frequency power supply to carry out sputtering, the sputtering power is 100W, the deposition time of the Ta transition layer is 332s-3320s, and the FeCrAl alloy target adopts a direct current power of 200W.
2. A FeCrAl/Ta alloy coating according to claim 1, wherein the FeCrAl layer has a thickness of 2.3±0.2 μm.
3. A FeCrAl/Ta alloy coating according to claim 1, wherein the method of grinding and cleaning the zirconium alloy substrate in step 1 is as follows:
and grinding and polishing the zirconium alloy matrix by sand paper, and ultrasonically cleaning and drying the polished zirconium alloy matrix.
4. A FeCrAl/Ta alloy coating according to claim 1, characterized in that the vacuum etching method is as follows:
and (3) conveying the cleaned zirconium alloy substrate into a magnetron sputtering coating chamber, and carrying out etching after vacuumizing, wherein the etching power is 200W, and the etching time is 5min.
5. The FeCrAl/Ta alloy coating of claim 1, wherein the Ta target has a purity of 99.99 wt%, a sputtering power of 100W, a deposition gas pressure setting of 0.3Pa, a deposition temperature of room temperature, and a substrate speed of 15r/min.
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| CN113846295B (en) * | 2021-09-27 | 2022-11-18 | 重庆文理学院 | Preparation method of FeCrAl/Cr composite coating |
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