CN111348941B - Carbide-derived carbon/rhenium/iridium coating on surface of C/C composite material and preparation method thereof - Google Patents
Carbide-derived carbon/rhenium/iridium coating on surface of C/C composite material and preparation method thereof Download PDFInfo
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
- C04B41/90—Coating or impregnation for obtaining at least two superposed coatings having different compositions at least one coating being a metal
Abstract
The invention relates to a C/C composite material surface carbide-derived carbon/rhenium/iridium coating and a preparation method thereof. The carbide-derived carbon/rhenium/iridium coating can perfectly give consideration to coating combination, coating substrate thermal mismatch mitigation and coating system high-temperature thermochemical compatibility, and has wide application prospect.
Description
Technical Field
The invention belongs to the technical field of high-temperature materials, relates to an ultrahigh-temperature antioxidant coating system and a preparation method thereof, and particularly relates to a structural design and a preparation method of a carbide-derived carbon/rhenium/iridium (CDC-C/Re/Ir) coating on the surface of a C/C composite material.
Background
The carbon/carbon composite material (C/C composite material) taking carbon fiber as a reinforcing phase and carbon as a matrix is closely concerned by researchers by a series of excellent performances such as low density, low thermal expansion, high specific strength specific modulus, thermal shock resistance and creep resistance, especially the characteristic that the strength is increased along with the temperature rise in an inert environment at the temperature of 1000-2300 ℃, and is widely applied to hot end parts of aerospace high-precision equipment such as a solid rocket engine nozzle and a throat liner, a hypersonic aircraft and a thermal protection system of a missile.
However, the C/C composite material has air temperature over 370 ℃, water vapor temperature over 650 ℃ and CO temperature over 750 DEG C2The oxidation is easy to occur, the oxidation rate is rapidly increased along with the temperature rise, and the internal structure of the C/C composite material can be damaged in a short time, so that the performance of the C/C composite material is greatly reduced and even fails. This makes the C/C composite material unusable alone in high temperature oxygen-containing environments.
In order to solve the problem of high-temperature oxidation of the C/C composite material, the preparation of the high-temperature oxidation-resistant coating on the surface of the C/C composite material becomes an economic and efficient oxidation-resistant modification means. The iridium Ir has high melting point (2440 ℃), high hardness, high elastic modulus, extremely low vapor pressure at high temperature and lowest oxygen permeability (10-10 ℃) in all the known materials at present-14g·cm-1·s-1) Therefore, the composite material is an important candidate material for the high-temperature oxidation-resistant coating on the surface of the C/C composite material. However, the thermophysical compatibility between Ir coatings and C/C composites is poor. On one hand, the solid solubility of C in Ir is extremely low, so that the combination between the Ir coating and the C/C composite material is poor; on the other hand, there is a large mismatch in thermal expansion (CTE: Ir: 6.2X 10)-6℃-1；C/C：0～2×10-6℃-1) The Ir coating on the surface of the C/C composite material is cracked and even peeled off due to thermal stress generated in the preparation and service processes.
In order to solve the thermophysical compatibility problem between the C/C composite and the Ir coating, researchers have proposed many solutions. A W transition layer is prepared between the C/C composite material and the Ir coating by an aging peak and the like, so that the combination of the Ir and the C/C composite material is improved, but the W, the C and the Ir form brittle compounds at high temperature, so that the high-temperature thermal shock resistance of the W, the C and the Ir is insufficient; pemsler et al first treat the surface of the C/C composite material to selectively oxidize the carbon matrix on the surface, leaving only carbon fibers, and then prepare an Ir coating to form a structure of a C fiber reinforced Ir coating, wherein the coating structure significantly enhances the bonding between Ir and the C/C composite material, but still cannot overcome the cracking of the coating caused by thermal expansion mismatch; mumtaz and the like firstly deposit pyrolytic carbon on the surface of the C/C composite material as a transition layer, enhance the combination of an Ir coating and a matrix and play a certain thermal mismatch relieving role by utilizing the thermal expansion coefficient centered by the pyrolytic carbon, but the problems of overlarge thermal expansion coefficient difference at certain positions and brittleness and cracking of a pyrolytic carbon layer caused by the extremely strong anisotropy of C/C still exist; considering that Re has good thermochemical compatibility with Ir and C (a low-melting-point phase or a brittle compound is not formed at high temperature), Huang Yongle and the like select Re as a transition layer and adopt Co as an alloying modification element, the plasticity of Re near a crack is improved through alloying, the repair of the surface crack of Re is realized, and the Ir coating without the crack is prepared and obtained. These studies have played a certain role in coating bonding or thermal expansion transition of the coating substrate, but all fail to perfectly consider the problems in coating bonding, thermal mismatch mitigation of the coating substrate, and high-temperature thermochemical compatibility of the coating system (such as formation of brittle compounds, low-melting substances, etc. at high temperature).
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a carbide-derived carbon/rhenium/iridium coating on the surface of a C/C composite material and a preparation method thereof, wherein the carbide-derived carbon/rhenium/iridium coating can perfectly give consideration to coating combination, coating substrate thermal mismatch alleviation and coating system high-temperature thermochemical compatibility.
In order to solve the above problems, the present invention adopts the following technical solutions.
A C/C composite material surface carbide-derived carbon/rhenium/iridium coating is characterized in that a C/C composite material is used as a base body, a carbide-derived carbon layer, a rhenium coating and an iridium coating are sequentially arranged on the surface of the C/C composite material from bottom to top, the carbide-derived carbon layer is a thermal expansion transition layer generated in situ on the surface of the C/C composite material, and the rhenium coating is a bonding layer between the carbide-derived carbon layer and the iridium coating.
Preferably, the carbide-derived carbon layer has a thickness of 10 to 30 μm, the rhenium coating has a thickness of 10 to 100 μm, and the iridium coating has a thickness of 20 to 200 μm.
As a general technical scheme, the invention also discloses a preparation method of the carbide derived carbon/rhenium/iridium coating on the surface of the C/C composite material, which comprises the following steps:
(1) preparing a pure Si layer on a C/C composite material substrate by adopting an atmospheric plasma spraying method;
(2) carrying out heat preservation and heat treatment on the C/C composite material matrix with the pure Si layer sprayed on the surface under the protection of inert gas at 1400-1600 ℃ to generate a SiC layer, thus obtaining the C/C composite material containing the SiC layer;
(3) pretreating the C/C composite material containing the SiC layer obtained in the step (2);
(4) under the protection of argon, heating the C/C composite material containing the SiC layer pretreated in the step (3) to 1000-1700 ℃, and introducing chlorine gas for etching to convert the SiC layer into a carbide derived carbon layer, thereby obtaining the C/C composite material containing the carbide derived carbon layer on the surface;
(5) depositing a rhenium coating on the surface of the C/C composite material containing the carbide-derived carbon layer obtained in the step (4);
(6) and (4) depositing an iridium coating on the rhenium coating obtained in the step (5) to finally obtain the carbide-derived carbon/rhenium/iridium coating on the surface of the C/C composite material.
Preferably, in the step (4), the flow rate of argon is 100mL/min to 500mL/min, the flow rate of chlorine is 10mL/min to 80mL/min, and the etching time of chlorine is 50s to 300 s.
In the above method for preparing the carbide-derived carbon/rhenium/iridium coating on the surface of the C/C composite material, preferably, in the step (4), the heating temperature is 1000 ℃ to 1550 ℃.
In the above method for preparing the carbide-derived carbon/rhenium/iridium coating on the surface of the C/C composite material, preferably, in the step (1), the thickness of the pure Si layer is controlled to be 100 μm to 200 μm, in the step (5), the thickness of the rhenium coating is controlled to be 10 μm to 100 μm, and in the step (6), the thickness of the iridium coating is controlled to be 20 μm to 200 μm.
In the above method for preparing the carbide-derived carbon/rhenium/iridium coating on the surface of the C/C composite material, preferably, in the step (2), the heat treatment time is 1h to 3 h.
Preferably, in the step (1), the C/C composite material substrate is prepared by quasi-3D needling or puncturing, and the density of the C/C composite material substrate is 1.80g/cm3～1.95g/cm3。
In the above method for preparing the carbide-derived carbon/rhenium/iridium coating on the surface of the C/C composite material, preferably, in the step (3), the pretreatment includes cleaning and drying.
The carbide precursor of the carbide derived carbon is selected from SiC, and the preparation method is thermal treatment after plasma spraying of Si.
The main innovation points of the invention are as follows:
the invention firstly proposes that the carbide derived carbon layer is applied to the field of thermal transition layers, and simultaneously, the carbon element of the carbide derived carbon layer in the invention is derived from the C/C composite material and is generated by in-situ extraction on the surface of the C/C composite material, so that the carbide derived carbon layer has natural and good interface combination with a substrate as the transition layer. On the other hand, the transition layer and the substrate are both carbon, no chemical essential difference exists, no other elements are introduced, and no adverse effect is generated on the thermochemical compatibility of the coating system, so that the compatibility is good, and the applicable coating system is wide.
The invention also utilizes the loose structure of the carbide derived carbon to eliminate the anisotropy of the surface of the C/C composite material, and can relieve the thermal stress concentration caused by overlarge difference of the thermal expansion coefficients of certain positions on the surface of the C/C composite material.
Si used in the preparation method of the invention is only a tool for generating carbide, or a tool for extracting C element, and is also a 'template' generated by a derivative carbon layer, and the Si is finally removed by chlorination after being introduced, and the process is shown in figure 2. This provides a more feasible solution for the preparation of the transition layer.
Compared with the prior art, the invention has the advantages that:
(1) the carbide-derived carbon/rhenium/iridium coating on the surface of the C/C composite material is a three-layer structure coating, and the CDC-C/Re/Ir high-temperature oxidation-resistant coating with good thermal physical and chemical compatibility is prepared on the surface of the C/C composite material by adopting carbide-derived carbon (CDC-C) generated in situ on the surface of the C/C composite material as a thermal expansion transition layer and Re with good thermal chemical compatibility with Ir and C as an adhesive layer between Ir and CDC-C. The CDC-C generated in situ on the surface of the C/C composite material has a loose stacking structure, and the carbon layer is derived from the carbon-carbon composite material, so that the carbon-carbon composite material can play a good role in combination and thermal expansion relief, and in addition, other elements are not introduced, so that the thermochemical compatibility of a coating system is not influenced, and the coating combination, the coating matrix thermal mismatch relief and the high-temperature thermochemical compatibility of the coating system can be considered at the same time. Compared with other schemes provided by the existing research, the scheme of the CDC-C/Re thermal expansion transition layer and the bonding layer provided by the invention can effectively solve the problems of thermophysical compatibility and chemical compatibility between the Ir coating and the C/C composite material substrate.
(2) The technical scheme of the invention can obviously improve the thermophysical compatibility of the C/C composite material and the ultrahigh-temperature oxidation-resistant coating system, and achieves the purpose of thermal transition. The loose structure of the carbide derived carbon layer adopted by the invention can also relieve local thermal stress concentration caused by the anisotropy of the surface of the C/C composite material, which can not be solved by the prior art, mostly. Meanwhile, the transition layer is generated by in-situ extraction, so that the transition layer is better combined with the matrix, and the transition layer is not chemically different from the matrix, so that the compatibility is good, and the method is suitable for other coating systems. In addition, the invention also provides a concept of template extraction, which provides more realization possibilities for preparation under various conditions and industrial production.
Drawings
FIG. 1 is a schematic structural diagram of a carbide-derived carbon/rhenium/iridium coating on the surface of a C/C composite material in example 1 of the present invention.
Fig. 2 is a schematic flow chart of forming a CDC layer on the surface of the C/C composite material using silicon as a template in the preparation method of embodiment 1 of the present invention.
Fig. 3 is a microscopic morphology diagram of the SiC coating etched by chlorine in example 1 of the present invention, where a and b are surface morphologies and c is a cross-sectional morphology.
FIG. 4 is a photo of macro morphology of a flat plate sample of a product in example 1 and a flat plate sample without a carbon transition layer before and after thermal shock ablation examination, wherein a and b are photos of the flat plate sample without the carbon transition layer before and after examination, and c and d are photos of the flat plate sample with the carbon transition layer in example 1 before and after examination.
FIG. 5 is a SEM topography of the central cross-section of samples (a) without transition layer and samples (b) with transition layer of example 1 of the present invention examined by thermal shock ablation.
Detailed Description
The invention is further described below with reference to the drawings and specific preferred embodiments of the description, without thereby limiting the scope of protection of the invention.
The materials and equipment used in the following examples are commercially available.
Example 1:
a C/C composite material surface carbide-derived carbon/rhenium/iridium coating, namely a CDC-C/Re/Ir coating, is shown in figure 1, the C/C composite material is taken as a substrate, a carbide-derived carbon layer, a rhenium coating and an iridium coating are sequentially arranged on the surface of the C/C composite material from bottom to top, the carbide-derived carbon layer is a thermal expansion transition layer generated in situ on the surface of the C/C composite material, and the rhenium coating is a bonding layer between the carbide-derived carbon layer and the iridium coating.
In this example, the carbide-derived carbon layer is about 20 μm thick, the rhenium coating is 60 μm thick, and the iridium coating is 50 μm thick.
A method for preparing a carbide-derived carbon/rhenium/iridium coating on the surface of a C/C composite material of the embodiment includes the following steps:
(1) spraying and preparing a Si layer on a C/C composite material substrate sample by using a Metco A-2000 type atmospheric plasma spraying instrument, wherein the pressure is 100mbar, the spraying distance is 300mm, the power is 42kW, and Ar is2Flow 50slpm, H2The flow rate was 10slpm and the powder feeding rate was 10g/min, and as shown in FIG. 2, a pure Si layer was obtained, the thickness of which was controlled to about 100 μm.
(2) And (3) carrying out heat preservation for 1h on the C/C composite material sample with the pure Si layer sprayed on the surface at 1435 ℃ in the inert gas protection, and generating a SiC layer as shown in figure 2 to obtain the C/C composite material containing the SiC layer.
(3) And (3) pretreating the C/C composite material containing the SiC layer prepared in the step (2), including cleaning and drying.
(4) And (3) under the protection of argon with the flow rate of 500mL/min, heating the sample pretreated in the step (3) to 1450 ℃ by using a medium-frequency induction heater, then introducing chlorine gas with the flow rate of 45mL/min for 150s, preparing a carbide-derived carbon layer, namely a CDC-C layer as shown in figure 2, obtaining a C/C composite material with the surface containing the carbide-derived carbon layer, and cleaning and drying the C/C composite material.
(5) And (4) depositing a rhenium coating, namely a Re coating, on the surface of the C/C composite material containing the carbide-derived carbon layer obtained in the step (4) by using a CVD method, controlling the thickness of the rhenium coating to be about 60 mu m, and cleaning and drying the Re coating.
(6) And (4) preparing an iridium coating, namely an Ir coating, on the rhenium coating obtained in the step (5) by adopting a molten salt electrodeposition method, wherein the thickness of the iridium coating is controlled to be about 50 mu m, and finally obtaining the carbide derived carbon/rhenium/iridium coating on the surface of the C/C composite material.
In step (1) of this example, the C/C composite material matrix can be prepared by quasi-3D needling or puncturing, and the density of the C/C composite material matrix is 1.85g/cm3。
FIG. 3 is a microscopic topography of the surface (FIG. 3a and FIG. 3b) and cross-section (FIG. 3C) of the sample etched with chlorine gas in step (4) of this example, which shows that the surface of the C/C composite substrate is covered with a loosely stacked CDC-C layer with a thickness of about 20 μm and an average grain diameter of about 15 μm. The careful observation shows that the CDC-C layer is well combined with the C/C matrix, the coverage is uniform and complete, most of the primary defects such as pores, cracks and the like on the C/C matrix are covered by the CDC-C layer, and the anisotropic characteristic of the surface of the C/C composite material is basically eliminated.
After the product sample prepared in this example and the sample without the carbon transition layer were subjected to high-temperature thermal shock and ablation examination (the highest temperature was 2400 ℃), the thermal expansion matching conditions of the "coating-substrate" of the system containing the transition layer and the system without the transition layer can be compared. FIG. 4 is a macro-morphology photograph before and after thermal shock ablation examination, from which the morphology change and comparison before and after ablation of two samples can be seen. After examination, ablation pits appear at the central parts of the two samples, but from the appearance of the coating around the pits, the samples without carbon layer transition have more surface cracks and the coating is lifted, and the average crack density of the coating is 8.3mm from that before ablation (figure 4a)-1Increased to 27.5mm after ablation (fig. 4b)-1. The samples of this example incorporating CDC-C layers have an average crack density of the coating, except for the ablation pits, of only 2.1mm from before ablation-1(FIG. 4c) increase to 3.1mm-1(FIG. 4 d). Fig. 5 is a cross-sectional photograph of the intact coating portion near the ablation pit in the center of the two coatings of the present embodiment and the comparative sample, which shows that the substrate and the coating are well bonded in the sample containing the carbon transition layer (fig. 5b), while the coating is more significantly peeled and cracked in the sample containing no carbon transition layer (fig. 5a), and these phenomena all indicate that the carbon transition layer plays a role in alleviating thermal expansion mismatch, so that the coating and the substrate can maintain good interface bonding after high-temperature thermal shock ablation examination.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner. Although the present invention has been described with reference to the preferred embodiments, it is not intended to be limited thereto. Those skilled in the art can make many possible variations and modifications to the disclosed embodiments, or equivalent modifications, without departing from the spirit and scope of the invention, using the methods and techniques disclosed above. Therefore, any simple modification, equivalent replacement, equivalent change and modification made to the above embodiments according to the technical essence of the present invention are still within the scope of the protection of the technical solution of the present invention.
Claims (9)
1. A C/C composite material surface carbide-derived carbon/rhenium/iridium coating is characterized in that a C/C composite material is used as a base body, a carbide-derived carbon layer, a rhenium coating and an iridium coating are sequentially arranged on the surface of the C/C composite material from bottom to top, the carbide-derived carbon layer is a thermal expansion transition layer generated in situ on the surface of the C/C composite material, and the rhenium coating is a bonding layer between the carbide-derived carbon layer and the iridium coating;
the preparation method of the C/C composite material surface carbide derived carbon/rhenium/iridium coating comprises the following steps:
(1) preparing a pure Si layer on a C/C composite material substrate by adopting an atmospheric plasma spraying method;
(2) carrying out heat preservation and heat treatment on the C/C composite material matrix with the pure Si layer sprayed on the surface under the protection of inert gas at 1400-1600 ℃ to generate a SiC layer, thus obtaining the C/C composite material containing the SiC layer;
(3) pretreating the C/C composite material containing the SiC layer obtained in the step (2);
(4) under the protection of argon, heating the C/C composite material containing the SiC layer pretreated in the step (3) to 1000-1700 ℃, and introducing chlorine gas for etching to convert the SiC layer into a carbide derived carbon layer, thereby obtaining the C/C composite material containing the carbide derived carbon layer on the surface;
(5) depositing a rhenium coating on the surface of the C/C composite material containing the carbide-derived carbon layer obtained in the step (4);
(6) and (4) depositing an iridium coating on the rhenium coating obtained in the step (5) to finally obtain the carbide-derived carbon/rhenium/iridium coating on the surface of the C/C composite material.
2. The C/C composite surface carbide-derived carbon/rhenium/iridium coating according to claim 1, wherein the carbide-derived carbon layer has a thickness of 10 to 30 μ ι η, the rhenium coating has a thickness of 10 to 100 μ ι η, and the iridium coating has a thickness of 20 to 200 μ ι η.
3. A preparation method of a C/C composite material surface carbide derived carbon/rhenium/iridium coating comprises the following steps:
(1) preparing a pure Si layer on a C/C composite material substrate by adopting an atmospheric plasma spraying method;
(2) carrying out heat preservation and heat treatment on the C/C composite material matrix with the pure Si layer sprayed on the surface under the protection of inert gas at 1400-1600 ℃ to generate a SiC layer, thus obtaining the C/C composite material containing the SiC layer;
(3) pretreating the C/C composite material containing the SiC layer obtained in the step (2);
(4) under the protection of argon, heating the C/C composite material containing the SiC layer pretreated in the step (3) to 1000-1700 ℃, and introducing chlorine gas for etching to convert the SiC layer into a carbide derived carbon layer, thereby obtaining the C/C composite material containing the carbide derived carbon layer on the surface;
(5) depositing a rhenium coating on the surface of the C/C composite material containing the carbide-derived carbon layer obtained in the step (4);
(6) and (4) depositing an iridium coating on the rhenium coating obtained in the step (5) to finally obtain the carbide-derived carbon/rhenium/iridium coating on the surface of the C/C composite material.
4. The method for preparing the carbide-derived carbon/rhenium/iridium coating on the surface of the C/C composite material according to claim 3, wherein in the step (4), the flow rate of the argon gas is 100-500 mL/min, the flow rate of the chlorine gas is 10-80 mL/min, and the etching time of the chlorine gas is 50-300 s.
5. The method for preparing the carbide-derived carbon/rhenium/iridium coating on the surface of the C/C composite material according to the claim 3, wherein the heating temperature in the step (4) is 1000-1550 ℃.
6. The method for preparing the carbide-derived carbon/rhenium/iridium coating on the surface of the C/C composite material according to the claim 3, wherein the thickness of the pure Si layer in the step (1) is controlled to be 100-200 μm, the thickness of the rhenium coating in the step (5) is controlled to be 10-100 μm, and the thickness of the iridium coating in the step (6) is controlled to be 20-200 μm.
7. The method for preparing the carbide-derived carbon/rhenium/iridium coating on the surface of the C/C composite material according to any one of claims 3 to 6, wherein in the step (2), the heat treatment time is 1-3 h.
8. The method for preparing the carbide-derived carbon/rhenium/iridium coating on the surface of the C/C composite material according to any one of claims 3 to 6, wherein in the step (1), the C/C composite material matrix is prepared by adopting a quasi 3D needling or puncturing mode, and the density of the C/C composite material matrix is 1.80g/cm3～1.95g/cm3。
9. The method for preparing the carbide-derived carbon/rhenium/iridium coating on the surface of the C/C composite material according to any one of claims 3 to 6, wherein in the step (3), the pretreatment comprises cleaning and drying.
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