CN114671710B - Double-period multilayer TaC/HfC ultrahigh-temperature ceramic anti-ablation coating and preparation method thereof - Google Patents
Double-period multilayer TaC/HfC ultrahigh-temperature ceramic anti-ablation coating and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a bi-period multilayer TaC/HfC ultra-high temperature ceramic ablation-resistant coating and a preparation method thereof, aiming at improving the ablation resistance of the existing ultra-high temperature ceramic coating. The technical scheme is that a multilayer alternating TaC/HfC ultrahigh-temperature ceramic ablation-resistant coating can be prepared on the surface of a carbon/carbon composite material by adopting a low-pressure chemical vapor deposition (LPCVD) technology in one step. The TaC and HfC double-period multilayer structure can inhibit the initiation and the propagation of cracks; a solid solution oxide layer of Hf-Ta-O with a compact structure can also be formed during the ablation process. Compared with a single-layer structure, the prepared double-period multilayer TaC/HfC coating has more excellent ablation resistance under the oxyacetylene ablation environment.
Description
Technical Field
The invention belongs to the field of material protection, and relates to a bi-periodic multilayer TaC/HfC ultrahigh-temperature ceramic anti-ablation coating and a preparation method thereof.
Background
The carbon/carbon (C/C) composite material can keep excellent mechanical properties at high temperature, and has a series of excellent characteristics such as low density and thermal shock resistance, so that the carbon/carbon (C/C) composite material becomes an excellent thermal structure candidate material for aerospace vehicles and power systems thereof. However, in practical applications, unprotected C/C composites suffer severe chemical ablation and mechanical degradation, resulting in rapid degradation of their mechanical properties. One of the methods for solving the problem is to prepare an anti-ablation coating on the surface of the C/C composite material. The existing coating system mainly uses HfC, zrC and other ultrahigh-temperature ceramic coatings, an oxide layer formed by the coatings after long-time ablation has a porous structure, and a large number of penetrating cracks are formed due to high-speed heat flow scouring, so that the coatings are easy to crack and even peel off, and the protective effect on a C/C matrix is lost.
To solve this problem, inspired by natural "shell-like" structures, a tortuous crack propagation path is formed during impact. Document 1"gim j, schnitzer n, otter L m, et al nanoscale development mechanical recovery in narre of Pinna nobilis shell nature communications,10 (2019) 1-8" reports that this biomimetic "shell-like" multilayer structure has excellent fracture toughness, and the existence of a large number of interfaces can effectively inhibit crack propagation, reduce crack propagation energy, and thus improve the strength of the material. Therefore, the bi-periodic multilayer structure has attracted great attention from researchers.
At the same time, the user can select the desired position,in the selection of the periodic layer material, taC belongs to one of ultra-high temperature ceramics, not only has high melting point, but also has oxide Ta 2 O 5 It also has the characteristics of high melting point and low vapor pressure. According to the document 2"Feng G H, li H J, yang L, et al, investigation on the implantation performance and mechanism of HfC coating modified with TaC.Corration science,170 (2020) 108649", it is reported that during high temperature ablation, both oxides can react to form dense Hf 6 Ta 2 O 17 The oxide layer can bear the air current scouring and obstruct the oxygen infiltration. Therefore, the two coating materials are used for constructing a double-period multilayer structure, namely different functions or advantages are combined, the synergistic protection effect advantage of the layered structure is exerted, and the ablation resistance of the coating is expected to be comprehensively improved.
However, ultra-high temperature ceramic coatings produced by conventional chemical vapor deposition are accompanied by temperature increases and decreases, resulting in residual thermal stresses within the coating. For multilayer structures, as the number of depositions increases, the thermal stresses inside the coating also increase, which is detrimental to the service of the coating in an ablative environment. Therefore, the one-step preparation of the double-period multilayer TaC/HfC ultra-high temperature ceramic anti-ablation coating can avoid the occurrence of easy cracking and shedding of the coating caused by stress concentration.
Disclosure of Invention
Technical problem to be solved
Compared with the traditional periodic layer SiC, the periodic transition layer adopted in the invention is TaC, and the molten Ta is generated under the ablation environment of more than or equal to 1800 DEG C 2 O 5 Can effectively self-heal cracks and is combined with HfO 2 The reaction produces a dense oxide layer. Meanwhile, the thermal stress in the coating is reduced by adopting one-step preparation, and the risk that the coating is easy to crack and fall off is reduced. Thereby improving the ablation resistance of the coating C/C composite material.
Technical scheme
A bi-periodic multi-layer TaC/HfC ultra-high temperature ceramic anti-ablation coating, whichIs characterized in that: the SiC coating of the inner transition layer is selected from TaC, and molten Ta is generated in the ablation environment of more than or equal to 1800 DEG C 2 O 5 Self-healing of cracks and HfO 2 The reaction generates a compact oxide layer, namely a TaC/HfC coating.
The thickness of the inner transition layer SiC coating is 6-10 μm.
The single-layer thicknesses of the TaC coating and the HfC coating are respectively 6-8 mu m.
The total thickness of the TaC/HfC coating is 50-110 mu m.
A method for preparing the bi-periodic multilayer TaC/HfC ultra-high temperature ceramic ablation-resistant coating is characterized by comprising the following steps:
step 1: 100-300g of HfCl is respectively added into a powder feeder 4 And TaCl 5 Powder, and then connecting a powder feeder with a deposition furnace;
step 2: polishing, cleaning and drying the carbon-based material, binding the carbon-based material by using a molybdenum wire, and suspending the carbon-based material in a deposition furnace with a spiral powder feeder;
and step 3: opening a vacuum pump, pumping the pressure in the deposition furnace to 5-10KPa, maintaining the pressure, and checking the airtightness of the deposition furnace;
and 4, step 4: introducing Ar at a flow rate of 300ml/min, heating to 1200-1400 ℃ at a speed of 7-10 ℃/min in a deposition furnace, and introducing MTS and H at flow rates of 5-20ml/min and 2-4L/min 2 And H is closed after 1-3H of deposition 2 And MTS, obtaining an inner transition layer SiC coating;
and 5: regulating the flow rate of Ar to 2-4L/min, cleaning the deposition furnace, and keeping for 0.5-2h;
step 6: regulating Ar flow to 200-800ml/min and introducing H with flow of 50-600ml/min and 100-800ml/min respectively 2 And CH 4 Opened with TaCl 5 The spiral powder feeder sets the rotating speed to be 50-1000r/min, and H is closed after deposition for 1-3H 2 And CH 4 Obtaining a TaC coating; repeating the step 5;
and 7: regulating Ar flow to 200-800ml/min and introducing H with flow of 100-1000ml/min and 60-800ml/min respectively 2 And CH 4 Opened to contain HfCl 4 The spiral powder feeder sets the rotating speed50-1000r/min, and closing H after deposition for 1-3H 2 And CH 4 And a compact oxide layer, namely a TaC/HfC coating is generated.
And after the powder feeder is cleaned, drying in an oven at 70 ℃.
The carbon-based material is
The carbon-based material of (1).
Advantageous effects
The invention provides a double-period multilayer TaC/HfC ultrahigh-temperature ceramic ablation-resistant coating and a preparation method thereof, aiming at improving the ablation resistance of the conventional ultrahigh-temperature ceramic coating. The technical scheme is that a multilayer alternating TaC/HfC ultrahigh-temperature ceramic ablation-resistant coating can be prepared on the surface of a carbon/carbon composite material by adopting a low-pressure chemical vapor deposition (LPCVD) technology in one step. The TaC and HfC double-period multilayer structure can inhibit the initiation and the propagation of cracks; a solid solution oxide layer of Hf-Ta-O with a compact structure can also be formed during the ablation process. Compared with a single-layer structure, the prepared double-period multilayer TaC/HfC coating has more excellent ablation resistance under the oxyacetylene ablation environment.
According to the double-period multilayer TaC/HfC ultrahigh-temperature ceramic ablation-resistant coating and the one-step preparation method thereof, the periodic multilayer structure has high designability, on one hand, the thermal stress in the coating can be controlled by adjusting the layer thickness and the layer number, and on the other hand, the expansion of cracks can be inhibited due to the existence of a large number of interlayer interfaces, so that the toughness of the coating is improved. Compared with the SiC of the traditional periodic layer material, the TaC selected in the invention generates molten Ta under the ablation environment of more than or equal to 1800 DEG C 2 O 5 Can effectively self-heal cracks and is combined with HfO 2 The reaction generates a compact oxide layer, and the ablation resistance of the coating is improved. On the other hand, the one-step method preparation does not need repeated temperature rise and drop, so that the residual thermal stress in the coating is small, the cracking of the coating is reduced, and the unique ablation-resistant potential of the periodic multilayer coating is fully exerted.
Drawings
FIG. 1 is a schematic diagram of a TaC/HfC coating layer of a bi-periodic multi-layer structure ultra-high temperature ceramic structure;
FIG. 2 is a surface SEM image, a cross-sectional SEM image and a corresponding EDS energy spectrum of a double-period multilayer structure ultra-high temperature ceramic TaC/HfC coating;
FIG. 3 shows a thermal flux of 2.4MW/m of a TaC/HfC coating of an ultra-high temperature ceramic with a bi-periodic multi-layer structure 2 The surface appearance of the ablated oxyacetylene flame;
FIG. 4 shows a thermal flux of 4.2MW/m for a TaC/HfC coating layer of a bi-periodic multi-layer ultra-high temperature ceramic 2 The surface appearance of the ablated oxyacetylene flame.
FIG. 5a is a SiC/HfC ultra high temperature ceramic anti-ablation coating; FIG. 5b shows SiC/HfC and multilayer structure (TaC/HfC) 4 The quality and the line ablation rate of the ultra-high temperature ceramic ablation-resistant coating after 60s of oxyacetylene flame ablation.
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
in order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments 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:
cleaning powder feeder, drying in 70-100 deg.C oven, and adding 100g HfCl into the powder feeder 4 And TaCl 5 Powder, and then connecting a powder feeder with a deposition furnace; cutting the C/C composite material into
Respectively polishing with 500, 800 and 1000-mesh silicon carbide abrasive paper, soaking in alcohol, ultrasonically cleaning, and drying in a 100 ℃ oven; binding the prepared C/C composite material by using a molybdenum wire, and suspending the C/C composite material in a chemical vapor deposition furnace connected with a spiral powder feeder; opening a vacuum pump, pumping the pressure in the deposition furnace to 5KPa, maintaining the pressure, and checking the airtightness of the deposition furnace; setting the heating rate to be 7 ℃/min, and introducing Ar protective gas with the flow rate of 300 ml/min; heating the chemical vapor deposition furnace to 1200 ℃, and introducing MTS and H with flow rates of 5ml/min and 2L/min respectively 2 Adjusting the pressure in the furnace to 5KPa, and closing H after 1H of deposition 2 And MTS, obtaining an inner transition layer SiC coating with the thickness of 6 mu m; regulating the flow rate of Ar to 2L/min, keeping for 0.5h, and cleaning the deposition furnace; then the flow of Ar is adjusted to 200ml/min and H is introduced at a flow of 50ml/min and 100ml/min respectively 2 And CH 4 Opened with TaCl 5 The spiral powder feeder sets the rotating speed to be 50r/min, and H is closed after 1H of deposition 2 And CH 4 Obtaining a TaC coating with the thickness of 6 mu m; regulating the flow rate of Ar to 2L/min, keeping for 0.5h, and cleaning the deposition furnace; then the flow of Ar is adjusted to 200ml/min and H is introduced at a flow of 100ml/min and 60ml/min respectively 2 And CH 4 Opened to contain HfCl 4 The spiral powder feeder sets the rotating speed to be 50r/min, and H is closed after 1H of deposition 2 And CH 4 Obtaining an HfC coating with the thickness of 6 mu m; regulating the flow rate of Ar to 2L/min, and keeping for 0.5h to clean the deposition furnace; the above steps are repeated 4 times in sequence (as shown in fig. 1), and a (TaC/HfC) ultra-high temperature ceramic ablation-resistant coating having a multilayer structure with a total thickness of about 60 μm is obtained.
Simultaneously respectively coating the layers at a heat flux of 2.4MW/m 2 And 4.2MW/m 2 The topography after ablation is shown in fig. 3 and fig. 4. At 2.4MW/m 2 Lower mass and linear ablation rate R m =0.38mg/s and R l =0.44 μm/s; at 4.2MW/m 2 The lower coating showed higher mass and linear ablation rates of 0.82mg/s and 0.87 μm/s, respectively.
Example 2
Cleaning the powder feeder, drying in an oven at 70 ℃, and respectively adding 200g of HfCl into the powder feeder 4 And TaCl 5 Powder, and then connecting the powder feeder with a deposition furnace; cutting the C/C composite material into
Respectively polishing with 500, 800 and 1000-mesh silicon carbide abrasive paper, soaking in alcohol, ultrasonically cleaning, and drying in a 100 ℃ oven; binding the prepared C/C composite material by using a molybdenum wire, and suspending the C/C composite material in a chemical vapor deposition furnace connected with a spiral powder feeder; opening a vacuum pump, pumping the pressure in the deposition furnace to 7.5KPa, maintaining the pressure, and checking the airtightness of the deposition furnace; setting the heating rate to be 8.5 ℃/min, and introducing Ar protective gas with the flow rate of 300 ml/min; heating the chemical vapor deposition furnace to 1300 ℃, and introducing MTS and H with the flow rates of 12.5ml/min and 3L/min respectively 2 Adjusting the pressure in the furnace to 7.5KPa, and closing H after 2H of deposition 2 And MTS, obtaining an inner transition layer SiC coating with the thickness of 8 mu m; regulating the flow rate of Ar to 3L/min, and keeping for 1.25h to clean the deposition furnace; then the flow rate of Ar is adjusted to 500ml/min and H with the flow rate of 325ml/min and 450ml/min is introduced 2 And CH 4 Opened with TaCl 5 The spiral powder feeder sets the rotating speed to 525r/min, and closes H after 2H of deposition 2 And CH 4 Obtaining a TaC coating with the thickness of 7 mu m; regulating the flow rate of Ar to 3L/min, and keeping for 1.25h for cleaning the deposition furnace; the Ar flow is subsequently adjusted to 500ml/min and H is introduced at a flow of 550ml/min and 430ml/min respectively 2 And CH 4 Opened to contain HfCl 4 The spiral powder feeder sets the rotating speed to 525r/min, and closes H after 2H of deposition 2 And CH 4 Obtaining an HfC coating with the thickness of 7 mu m; regulating the flow rate of Ar to 3L/min, and keeping for 1.25h to clean the deposition furnace; the above steps were repeated 5 times in sequence to obtain a (TaC/HfC) ultra-high temperature ceramic ablation-resistant coating having a multilayer structure with a total thickness of 78 μm.
Example 3
Cleaning the powder feeder, drying in an oven at 70 ℃, and respectively adding 300g of HfCl into the powder feeder 4 And TaCl 5 Powder, then powder feeder and depositionConnecting the furnaces; cutting the C/C composite material into
Respectively polishing with 500, 800 and 1000-mesh silicon carbide abrasive paper, soaking with alcohol, ultrasonically cleaning, and drying in a 100 ℃ oven; binding the prepared C/C composite material by using a molybdenum wire, and suspending the C/C composite material in a chemical vapor deposition furnace with a spiral powder feeder; opening a vacuum pump, pumping the pressure in the deposition furnace to 10KPa, maintaining the pressure, and checking the airtightness of the deposition furnace; setting the heating rate to be 10 ℃/min, and introducing Ar protective gas with the flow rate of 300 ml/min; heating the chemical vapor deposition furnace to 1400 ℃, and introducing MTS and H with the flow rates of 20ml/min and 4L/min respectively 2 Adjusting the pressure in the furnace to 10KPa, and closing H after 3H of deposition 2 And MTS, obtaining an inner transition layer SiC coating with the thickness of 10 mu m; regulating the flow rate of Ar to 4L/min, and keeping for 2h to clean the deposition furnace; then the flow rate of Ar is adjusted to 800ml/min and H with the flow rate of 600ml/min and 800ml/min is introduced 2 And CH 4 Opened with TaCl 5 The spiral powder feeder sets the rotating speed to 1000r/min, and H is closed after 3 hours of deposition 2 And CH 4 Obtaining TaC coating with the thickness of 8 mu m; regulating the flow rate of Ar to 4L/min, keeping for 2h, and cleaning the deposition furnace; then the flow rate of Ar is adjusted to 800ml/min and H with the flow rate of 1000ml/min and 800ml/min is introduced 2 And CH 4 Opened to contain HfCl 4 The spiral powder feeder sets the rotating speed to 1000r/min, and H is closed after 3 hours of deposition 2 And CH 4 Obtaining an HfC coating with the thickness of 8 mu m; regulating the flow rate of Ar to 4L/min, keeping for 2 hours, and cleaning the deposition furnace; the above steps were repeated 6 times in sequence to obtain a (TaC/HfC) ultra-high temperature ceramic ablation-resistant coating having a multilayer structure with a total thickness of 106 μm (as shown in FIG. 2).
Example 4
Cleaning the powder feeder, drying in an oven at 70 ℃, and respectively adding 300g of HfCl into the powder feeder 4 Then connecting the powder feeder with a deposition furnace; cutting the C/C composite material into
Respectively 500 and 800Polishing 1000-mesh silicon carbide abrasive paper, soaking in alcohol, ultrasonically cleaning, and drying in a 100-DEG C oven; binding the prepared C/C composite material by using a molybdenum wire, and suspending the C/C composite material in a chemical vapor deposition furnace with a spiral powder feeder; opening a vacuum pump, pumping the pressure in the deposition furnace to 10KPa, maintaining the pressure, and checking the airtightness of the deposition furnace; setting the heating rate to be 10 ℃/min, and introducing Ar protective gas with the flow rate of 300 ml/min; heating the chemical vapor deposition furnace to 1200 ℃, and introducing MTS and H with the flow rate of 20ml/min and 4L/min respectively 2 Adjusting the pressure in the furnace to 10KPa, and closing H after 3H of deposition 2 And MTS, obtaining an inner transition layer SiC coating with the thickness of 10 mu m; regulating the flow rate of Ar to 4L/min, and keeping for 2h to clean the deposition furnace; then the flow rate of Ar is adjusted to 800ml/min and H with the flow rate of 600ml/min and 800ml/min is introduced 2 And CH 4 Opened to contain HfCl 5 The spiral powder feeder sets the rotating speed to 1000r/min, and H is closed after 8 hours of deposition 2 And CH 4 A HfC coating having a thickness of 50 μm was obtained. A SiC/HfC ultra high temperature ceramic ablation-resistant coating having a total thickness of about 66 μm was obtained (as shown in fig. 5 a). Both the quality and the line ablation rate after 60s of oxyacetylene flame ablation were higher than the periodic multilayer TaC/HfC coating (as shown in fig. 5 b).
The double-period multilayer TaC/HfC ultra-high temperature ceramic anti-ablation coating prepared by one step by the preparation method can effectively relieve the generation of thermal stress and inhibit the cracking of the coating, fully exerts the unique anti-ablation potential and realizes the application of the composite material in extreme environments.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (3)
1. A method for preparing a double-period multilayer TaC/HfC ultrahigh-temperature ceramic ablation-resistant coating is characterized by comprising the following steps:
step 1: 100-300g of HfCl is respectively added into a powder feeder 4 And TaCl 5 Powder bodyThen connecting the powder feeder with a deposition furnace;
step 2: polishing, cleaning and drying the carbon-based material, binding the carbon-based material by using a molybdenum wire, and suspending the carbon-based material in a deposition furnace with a spiral powder feeder;
and step 3: opening a vacuum pump, pumping the pressure in the deposition furnace to 5-10KPa, maintaining the pressure, and checking the airtightness of the deposition furnace;
and 4, step 4: introducing Ar at the flow rate of 300mL/min, heating to 1200-1400 ℃ at the speed of 7-10 ℃/min in the deposition furnace, and introducing MTS and H at the flow rates of 5-20mL/min and 2-4L/min respectively 2 And H is closed after 1-3H of deposition 2 And MTS, obtaining an inner transition layer SiC coating;
and 5: regulating the flow rate of Ar to 2-4L/min, cleaning the deposition furnace, and keeping for 0.5-2h;
step 6: regulating Ar flow to 200-800mL/min and introducing H with flow of 50-600mL/min and 100-800mL/min respectively 2 And CH 4 Opened to contain TaCl 5 The spiral powder feeder sets the rotating speed to be 50-1000r/min, and H is closed after deposition for 1-3H 2 And CH 4 Obtaining a TaC coating; repeating the step 5;
and 7: regulating Ar flow to 200-800mL/min and introducing H with flow of 100-1000mL/min and 60-800mL/min respectively 2 And CH 4 Opened to contain HfCl 4 The spiral powder feeder sets the rotating speed to be 50-1000r/min, and H is closed after deposition for 1-3H 2 And CH 4 Generating a compact anti-ablation coating, namely a TaC/HfC coating;
in the coating, the thickness of the SiC coating of the inner transition layer is 6-10 μm; the single-layer thicknesses of the TaC coating and the HfC coating are respectively 6-8 mu m; the total thickness of the TaC/HfC coating is 50-110 μm;
the coating is prepared by a one-step method, and repeated temperature rise and drop are not performed, so that residual thermal stress in the coating is small, and cracking of the coating is reduced;
the coating generates molten Ta in an ablation environment at the temperature of more than or equal to 1800 DEG C 2 O 5 Self-healing of cracks and HfO 2 The reaction produces a dense oxide layer.
2. The method of claim 1, wherein: and after the powder feeder is cleaned, drying in an oven at 70 ℃.
3. The method of claim 1, wherein: the carbon-based material is
The carbon-based material of (1). />
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