CN113403594B - High-temperature-resistant, water-oxygen-resistant and low-infrared-emissivity composite film for ceramic matrix composite and preparation method thereof - Google Patents
High-temperature-resistant, water-oxygen-resistant and low-infrared-emissivity composite film for ceramic matrix composite and preparation method thereof Download PDFInfo
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- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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Abstract
The invention relates to a high temperature resistant, anti-oxyhydrogen and low-infrared-emissivity composite film for a ceramic matrix composite and a preparation method thereof. The film is a high-temperature conductive composite film which is continuously formed, the main components of the film comprise two types, a high-conductivity metal material is used as a component with low infrared emissivity, and an environment barrier coating material for a ceramic matrix composite material is used as a protection component. After the process is optimized, the composite film can realize that the emissivity of 2-22 mu m is less than 0.1 after the composite film is used for 2 hours in a high-temperature air environment at 1000 ℃, has the excellent performances of low emissivity, high temperature resistance, water resistance and the like, and has simple preparation process and simple operation.
Description
Technical Field
The invention belongs to the field of infrared stealth, and relates to a high-temperature-resistant, water-oxygen-resistant and low-infrared-emissivity composite film for a ceramic matrix composite material and a preparation method thereof.
Background
With the continuous development of the aviation industry, the related technical requirements of military aviation gas turbine engines are continuously improved, and ceramic matrix composite materials have the performance advantages of high temperature resistance, low density, oxidation resistance, high specific strength and the like, so that the ceramic matrix composite materials become key materials of hot end components (tail nozzles and the like) of the next generation of aviation gas turbine engines with high thrust-weight ratios. With the rapid development of modern military detection technology, the survival of warplanes in modern wars is greatly challenged, the stealth technology becomes an important research direction in the military technical field, and the infrared stealth occupies a very important position in the stealth technology, so that the realization of the infrared stealth of the ceramic matrix composite material is very important.
Infrared stealth is achieved by reducing the intensity of externally radiated infrared rays by a target below the sensitivity of an infrared detector,the probability of the target being detected by the infrared detector is reduced. According to stefan-boltzmann's law: infrared radiation intensity of target M = ε σ T 4 (ε is the infrared emissivity,. Sigma.is the Boltzmann constant, and T is the surface temperature of the target). Therefore, the main factors influencing the infrared radiation energy of an object are the surface temperature and the infrared emissivity of the object, so that two main technical approaches are available for realizing infrared stealth: firstly, the surface infrared emissivity of the target is reduced, and secondly, the surface temperature of the target is controlled.
In addition, the hot end part of the gas turbine engine needs to face severe environmental conditions such as high temperature, water oxygen, hot corrosion and the like when working, and the service temperature is often over 1000 ℃. When applied, the ceramic matrix composite is also resistant to corrosion of complex environments, so that it is also very important to improve the environmental resistance of the ceramic matrix composite, such as high temperature resistance, water-oxygen corrosion resistance and the like.
In the field of military equipment, currently mainstream infrared stealth materials include low infrared emissivity coatings and films. The low infrared emissivity coating mainly relies on the excellent electric conductivity of metal filler to realize low infrared emissivity, but gas turbine engine hot-end part need face adverse environmental conditions such as high temperature, water oxygen when the during operation, and under this kind of environment, metal material easily oxidizes, and the electric conductivity descends, has lost the effect of infrared stealthy. Patent CN 108913018B discloses a high-temperature-resistant infrared low-emissivity coating and a preparation method thereof, wherein aluminum/nickel (Al/Ni) core-shell pigment is used as a low-emissivity filler, the coating has certain temperature resistance, and the highest service temperature of the coating is not more than 500 ℃. In addition, the low infrared emissivity thin film is largely classified into a metal thin film and a semiconductor thin film. Correspondingly, the metal film is difficult to meet the requirement of high-temperature application, and the novel high-temperature-resistant low-emissivity semiconductor oxide and ceramic material comprises tin-doped indium oxide (ITO), aluminum-doped zinc oxide (ZAO) and the like, can obtain lower emissivity in a room-temperature environment, but have the defects of inter-substance diffusion, unstable material performance and the like in a complex high-temperature environment, and are difficult to stably use. The patent CN 111321382A discloses a high-temperature-resistant and antioxidant infrared low-emissivity composite film and a preparation method thereof, wherein a high-temperature conductive ceramic film is used as a low-emissivity functional layer, the film has certain temperature resistance, and the maximum service temperature of the film is not more than 750 ℃.
Similarly above, a great deal of research has been conducted on low ir emissivity materials for use in high temperature environments, but to date, among the reported research results, materials that can be stably used in environments exceeding 1000 ℃ have been found to be still yielding. Therefore, for the ceramic matrix composite material for the hot end component of the aviation gas turbine engine, a material which can stably work in a complex high-temperature environment and has low infrared emissivity is urgently needed to meet the performance requirement of an aerospace aircraft. The design of the high-temperature-resistant, anti-oxyhydrogen and low-infrared-emissivity coating/film for the ceramic matrix composite material with high use temperature and stable performance has important significance.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a high-temperature-resistant, water-oxygen-resistant and low-infrared-emissivity composite film for a ceramic matrix composite and a preparation method thereof. Aiming at various problems of the existing material under severe working environment and overcoming the defects of the prior art, the composite film can be used in the environment with high temperature of more than 1000 ℃ and water oxygen, has the characteristics of low infrared emissivity, high temperature resistance and water oxygen resistance, and has simple structure and easy preparation.
Technical scheme
A preparation method of a high-temperature-resistant, anti-oxyhydrogen and low-infrared-emissivity composite film for preparing a ceramic matrix composite material is characterized in that the high-temperature-resistant, anti-oxyhydrogen and low-infrared-emissivity composite film for the ceramic matrix composite material is a composite film formed by uniformly mixing and doping a high-conductivity metal material and an environment barrier coating material on the surface of a target object by using a magnetron sputtering method, wherein the content of the high-conductivity metal material is 30-70 vol%;
the preparation method comprises the following steps:
step 1: cleaning the surface of a target object, and fixing the target object on a magnetron sputtering deposition platform deck;
step 2: metal and ceramic target material are used as magnetron sputtering target, and sputtering background vacuum is less than 8 x 10 -1 Pa；
And 3, step 3: introducing argon with purity of 99.99% or more, and regulating sputtering pressure to (3-9) x 10 -1 Pa, setting the sputtering power to be 100-400W;
and 4, step 4: and (3) performing direct-current magnetron sputtering on metal, performing radio-frequency magnetron sputtering on a ceramic target for 30-60 minutes at a sputtering rate of 10-50nm/min, and preparing the low-infrared-emissivity composite film. The highly conductive metal material includes, but is not limited to, gold, silver, titanium, or platinum.
The environmental barrier coating material for the ceramic matrix composite material comprises but is not limited to mullite, barium strontium aluminum silicon, yttrium silicate, scandium silicate or rare earth silicate.
The sputtering rate of the direct-current magnetron sputtering metal and radio-frequency magnetron sputtering ceramic target material depends on the regulation and control of the content of the metal material component between 30 and 70 vol.%.
The film is a high-temperature conductive composite film continuously formed, and the thickness of the film is more than or equal to 100nm.
Advantageous effects
The invention provides a high temperature resistant, anti-oxyhydrogen and low-infrared-emissivity composite film for a ceramic matrix composite and a preparation method thereof. The film is a high-temperature conductive composite film which is continuously formed, the main components of the film comprise two types, a high-conductivity metal material is used as a component with low infrared emissivity, and an environment barrier coating material for a ceramic matrix composite material is used as a protection component. After the process is optimized, the composite film can realize that the emissivity of 2-22 mu m is less than 0.1 after the composite film is used for 2 hours in a high-temperature air environment at 1000 ℃, has the excellent performances of low emissivity, high temperature resistance, water resistance and the like, and has simple preparation process and simple operation.
Is a single-layer complex phase structure and is characterized in that: the high-conductivity metal material is used as a component with low infrared emissivity, the environment barrier coating material for the ceramic matrix composite material is used as a protective component, and the protective component is coated on the surface of a target object when in use.
Based on the principle of complementary functional advantages of the composite film, the invention firstly uses a high-conductivity metal material as a functional component with low infrared emissivity, and secondly uses an environmental barrier coating material for the ceramic matrix composite material as a protective component, so as to solve the problems of oxidation resistance and water-oxygen corrosion resistance of the metal film. The two components complement each other, and the content of the low infrared emissivity component is controlled to be 30-70 vol% (the change of the optimal content is changed according to different selections of the low infrared emissivity component and the protection component) by regulating and controlling the relative ratio of the two components, so that the coordination and unification of the low infrared emissivity, the high temperature resistance and the water and oxygen resistance are finally realized, and the low infrared emissivity is kept, and meanwhile, the high temperature resistance and the water and oxygen resistance are excellent. The prepared composite film is used as an infrared stealth material of a hot end part of an aviation gas turbine engine, stably works in a high-temperature and water-oxygen environment with the temperature of more than 1000 ℃, and the infrared emissivity is kept at a lower level.
Compared with the prior art, the composite film for the ceramic matrix composite material, which is provided by the invention, has the advantages of high temperature resistance, water and oxygen resistance and low infrared emissivity:
1. the composite film for the ceramic matrix composite material, which is high temperature resistant, water-oxygen resistant and low in infrared emissivity, can be stably used in a high-temperature environment of more than 1000 ℃ by optimizing the component proportion, and has excellent water-oxygen resistance and low infrared emissivity. The complex working environment faced by the ceramic matrix composite material in the using process is met, and the infrared stealth method has important significance for realizing the infrared stealth of the ceramic matrix composite material.
2. The high-temperature-resistant, anti-oxyhydrogen and low-infrared-emissivity composite film for the ceramic matrix composite material has a simple structure, is convenient for large-area preparation and application, mostly has the problems of poor interlayer bonding force and unmatched thermal expansion in the multilayer film or coating structure of other prior art, and can realize two functions of low infrared emissivity and complex high-temperature-resistant environment by the simple single-layer film structure without considering the problems.
3. The preparation process of the high-temperature-resistant, water-oxygen-resistant and low-infrared-emissivity composite film for the ceramic matrix composite material is simple and feasible, and has good repeatability and low equipment requirement.
Drawings
FIG. 1 is a schematic cross-sectional view of a low IR emissivity composite film in an embodiment of the invention.
FIG. 2 is a graph of the emissivity of the barium-strontium-aluminum-silicon/platinum composite film of example 1 before and after heat treatment at different temperatures, the emissivity is as low as 0.16 before heat treatment, and the emissivity is 0.10,0.07 and 0.09 after air heat treatment at 600, 800 and 1000 ℃ for 2 h.
FIG. 3 is a photograph of the barium-strontium-aluminum-silicon/platinum composite film of example 1 of the present invention before heat treatment, which has a smooth and flat surface.
FIG. 4 is a photograph of the barium-strontium-aluminum-silicon/platinum composite film in example 1 of the present invention after heat treatment at 1000 ℃ for 2 hours, wherein the film surface has no significant change and the structure is completely preserved.
FIG. 5 is a graph showing the emissivity of 2-22 μm before and after heat treatment at different temperatures of the scandium silicate/titanium composite film in example 2 of the present invention, where the emissivity is as low as 0.28 before heat treatment, and the emissivity is 0.24,0.19,0.26 after air heat treatment at 600, 800, and 1000 ℃ for 2 hours.
FIG. 6 is a graph showing IR emissivity of 2-22 μm before and after heat treatment at different temperatures of the titanium thin film of example 3 of the present invention (comparative example), which is as low as 0.16 before heat treatment, and which is as high as 0.37,0.46 and 0.68 after heat treatment at 600, 800 and 1000 ℃ for 2 hours in air.
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
the various raw materials, reagents, instruments, equipment, etc. used in the present invention are commercially available or can be prepared by existing methods.
Example 1: and preparing the barium-strontium-aluminum-silicon/platinum composite film with the thickness of 150 nm.
A high temperature resistant, anti-oxyhydrogen, low infrared emissivity composite film for ceramic matrix composite material as shown in figure 1 comprises barium strontium aluminum silicon/platinum (BSAS/Pt) as main component. The film is a single-layer complex phase structure, 1 is the surface of a target object, 2 is the prepared BSAS/Pt composite film, and the film and a substrate are mechanically combined in a main combination mode. In this embodimentLow IR emissivity film deposited on SiO 2 (1) On a substrate.
In the embodiment, the thickness of the BSAS/Pt film is 150nm, wherein the protective component is prepared by adopting a radio frequency magnetron sputtering method, the used target material is a BSAS ceramic target (the purity is 99.95%), the low infrared emissivity component is prepared by adopting a direct current magnetron sputtering method, and the used target material is a Pt metal target (the purity is 99.99%).
After the proportion optimization of the early-stage experiment, the preparation method of the low infrared emissivity composite film in the embodiment comprises the following steps:
(1) SiO with the size of phi 30mm multiplied by 2mm 2 Sequentially placing the substrate in acetone, absolute ethyl alcohol and deionized water, respectively ultrasonically cleaning for 5 minutes, and then cleaning the cleaned SiO 2 The substrate is blown with compressed air to remove the deionized water on the surface for standby.
(2) Drying the SiO dried in the step 1 2 The substrate is fixed on a magnetron sputtering carrying platform, BSAS and Pt sputtering targets are fixed, a sputtering cavity is vacuumized until the air pressure in the cavity reaches 8 multiplied by 10 -4 Pa。
(3) Argon with the purity of more than or equal to 99.99 percent is introduced into the sputtering cavity, the sputtering pressure is adjusted to be 0.8Pa, the direct-current sputtering power is 50W, the radio-frequency sputtering power is 200W, and the sputtering time is controlled for 30min.
(4) And (5) closing the gas circuit and the voltage after the sputtering time is finished, keeping the water-cooling state, vacuumizing for 30 minutes, and opening the cavity to take out the sample.
The ceramic matrix composite material prepared by the method is used for a high temperature resistant, anti-water oxygen and low infrared emissivity composite film, the component proportion is tested, the volume fraction of Pt is 46vol.%, the 2-22 μm infrared emissivity is tested to be less than 0.2, and the infrared emissivity is tested to be less than 0.1 after heat treatment is carried out for 2 hours in 600 ℃, 800 and 1000 ℃ air environments respectively (see figure 2).
The photos of the film of the embodiment before and after heat treatment for 2h in the air environment at 1000 ℃ are respectively shown in fig. 3 and fig. 4, and it can be seen from the pictures that the high temperature resistant, anti-oxyhydrogen low-infrared-emissivity composite film of the invention has a complete structure preservation in the high temperature environment, is not easily damaged, and has excellent oxidation resistance. And the barium, strontium, aluminum and silicon have excellent water and oxygen resistance, so that the film has excellent water and oxygen resistance.
Through a comparison experiment, the volume fraction of Pt can reach the optimal proportion when being about 50vol.%, the low infrared emissivity and the oxidation resistance of the film reach the optimal performance at the moment, when the volume fraction of Pt is reduced, the infrared emissivity of the film is increased, the infrared stealth capability is reduced, and when the volume fraction of Pt is increased, the infrared emissivity after the high-temperature heat treatment of the film is increased, and the high-temperature resistance capability is reduced.
Example 2: and preparing a scandium silicate/titanium composite film with the thickness of 600 nm.
A high temperature resistant, anti-oxyhydrogen, low infrared emissivity composite film for ceramic matrix composite material as shown in FIG. 1 comprises scandium silicate/titanium (Sc) as main ingredient 2 Si 2 O 7 /Ti). The film is of a single-layer complex phase structure, 1 is the surface of a target object, and 2 is the prepared Sc 2 Si 2 O 7 The composite film/Ti has mechanical combination with the substrate as the main combination mode. In this embodiment, the low IR emissivity film is deposited on SiO 2 (1) On a substrate.
Examples Sc 2 Si 2 O 7 The thickness of the Ti film is 600nm, wherein the protective component is prepared by adopting a radio frequency magnetron sputtering method, and the target material is Sc 2 Si 2 O 7 The ceramic target (purity 99.95%) and the low infrared emissivity component are prepared by a direct current magnetron sputtering method, and the target material is a Ti metal target (purity 99.99%).
The preparation method of the low infrared emissivity composite film in the embodiment comprises the following steps:
(1) SiO with the size of phi 30mm multiplied by 2mm 2 Sequentially placing the substrate in acetone, absolute ethyl alcohol and deionized water, respectively ultrasonically cleaning for 5 minutes, and then cleaning the cleaned SiO 2 The substrate is blown with compressed air to remove the deionized water on the surface for standby.
(2) Drying the SiO dried in the step 1 2 The substrate is fixed on a magnetron sputtering carrier and is fixed with Sc 2 Si 2 O 7 And Ti sputtering target material, vacuumizing the sputtering cavity until the air pressure in the cavity reaches 8 multiplied by 10 -4 Pa。
(3) Argon with the purity of more than or equal to 99.99 percent is introduced into the sputtering cavity, the sputtering pressure is adjusted to be 0.6Pa, the direct-current sputtering power is 200W, the radio-frequency sputtering power is 200W, and the sputtering time is controlled to be 60min.
(4) And (5) closing the gas circuit and the voltage after the sputtering time is finished, keeping the water-cooling state, vacuumizing for 30 minutes, and opening the cavity to take out the sample.
According to the composite film for the ceramic matrix composite material, which is prepared by the method, the component proportion is tested, the volume fraction of Ti is 65vol.%, the infrared emissivity of 2-22 mu m is less than 0.3, and the infrared emissivity of the composite film is less than 0.3 after heat treatment in air environment at 600 ℃, 800 and 1000 ℃ for 2 hours (see figure 5).
The film of the embodiment has no obvious change before and after heat treatment for 2 hours in an air environment of 1000 ℃, and the high-temperature-resistant, anti-oxyhydrogen and low-infrared-emissivity composite film has a complete structure preservation in a high-temperature environment and has excellent oxidation resistance. And the scandium silicate has excellent water and oxygen resistance due to the excellent water and oxygen resistance of the scandium silicate.
Example 3: preparation of a titanium thin film having a thickness of 600nm (comparative example).
In contrast, a low ir emissivity film as shown in fig. 1 was prepared, which had titanium (Ti) as a main component. The film is a single-layer structure, 1 is the surface of a target object, 2 is the prepared Ti film, and the film and a substrate are mechanically combined in a main combination mode. In this embodiment, the low IR emissivity film is deposited on SiO 2 (1) On a substrate.
In the embodiment, the thickness of the Ti film is 600nm, the Ti film is prepared by a direct current magnetron sputtering method, and the used target material is a Ti metal target (the purity is 99.99%).
The preparation method of the low infrared emissivity composite film in the embodiment comprises the following steps:
(1) SiO with the size of phi 30mm multiplied by 2mm 2 Sequentially placing the substrate in acetone, absolute ethyl alcohol and deionized water, respectively ultrasonically cleaning for 5 minutes, and then cleaning the cleaned SiO 2 The substrate is blown with compressed air to remove the deionized water on the surface for standby.
(2) Will be described in detail1 blown dry SiO 2 The substrate is fixed on a magnetron sputtering carrier, meanwhile, a Ti sputtering target material is fixed, a sputtering cavity is vacuumized until the air pressure in the cavity reaches 8 multiplied by 10 -4 Pa。
(3) And introducing argon with the purity of more than or equal to 99.99 percent into the sputtering cavity, adjusting the sputtering pressure to be 0.6Pa, adjusting the direct-current sputtering power to be 200W, and controlling the sputtering time to be 100min.
(4) And (5) closing the gas circuit and the voltage after the sputtering time is finished, keeping the water-cooling state, vacuumizing for 30 minutes, and opening the cavity to take out the sample.
The low infrared emissivity film prepared by the method has the infrared emissivity of 2-22 mu m less than 0.2, and the infrared emissivity of the film gradually rises and the infrared stealth capability of the film seriously decreases after the film is subjected to heat treatment for 2 hours in air environments of 600 ℃, 800 and 1000 ℃ respectively (see figure 6).
The Ti film is a common single-component low-infrared-emissivity film, the infrared emissivity reaches 0.68 after heat treatment for 2 hours at 1000 ℃ in an air environment, and the performance is seriously deteriorated. Comparison shows that Sc of the same thickness as prepared in example 2 2 Si 2 O 7 The Ti composite film has excellent oxidation resistance, and the infrared emissivity of the Ti composite film is 0.26 after heat treatment for 2 hours in an air environment at the temperature of 1000 ℃. Visible, antioxidant phase (Sc) 2 Si 2 O 7 ) The oxidation resistance of the film is greatly improved, and the low infrared emissivity of the film is kept.
In conclusion, based on the principles of composite film function superposition and advantage complementation, the invention utilizes a high-conductivity metal material as a low-infrared-emissivity functional component, and utilizes an environment barrier coating material used by the ceramic matrix composite material when the ceramic matrix composite material works under the severe environment conditions of high temperature and water oxygen as a protective component, so that the coordination and unification of the low-infrared-emissivity, high temperature resistance and water oxygen resistance are finally realized, the low-infrared-emissivity is maintained, the high-temperature-resistant and water oxygen-resistant performance is also excellent, and a foundation is laid for realizing the infrared stealth of the ceramic matrix composite material.
Claims (3)
1. A preparation method of a high temperature resistant, anti-water oxygen and low infrared emissivity composite film for preparing a ceramic matrix composite material is characterized by comprising the following steps: the composite film for the ceramic matrix composite material is prepared by uniformly mixing and doping a high-conductivity metal material and an environmental barrier coating material on the surface of a target object by using a magnetron sputtering method, wherein the content of the high-conductivity metal material is 30-70 vol%;
the preparation method comprises the following steps:
step 1: cleaning the surface of a target object, and fixing the target object on a magnetron sputtering deposition platform deck;
and 2, step: metal and ceramic target material are used as magnetron sputtering target, and sputtering background vacuum is less than 8 x 10 -1 Pa；
And step 3: introducing argon with purity of 99.99% or more, and regulating sputtering pressure to (3-9) x 10 -1 Pa, setting the sputtering power to be 100-400W;
and 4, step 4: sputtering the ceramic target material for 30-60 minutes at the sputtering rate of 10-50nm/min by using direct current magnetron sputtering metal and radio frequency magnetron sputtering, and preparing the low infrared emissivity composite film;
the film is a high-temperature conductive composite film continuously formed, and the thickness of the film is more than or equal to 100nm;
the environment barrier coating material is barium strontium aluminum silicon.
2. The method of claim 1, wherein: the sputtering rate of the direct-current magnetron sputtering metal and radio-frequency magnetron sputtering ceramic target material depends on the regulation and control of the content of the metal material component between 30 and 70 vol.%.
3. The method of claim 1, wherein: the high-conductivity metal material is gold, silver, titanium or platinum.
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