Anti-oxidation material, structural member, preparation method of structural member, brake disc and vehicle

Abstract

The invention provides an anti-oxidation material, a structural member, a preparation method of the structural member, a brake disc and a vehicle, and the anti-oxidation material comprises 35-65 wt% of SiO2, 2-10 wt% of B2O3, 4-16 wt% of Al2O3, 2-8 wt% of Y2O3, 6-25 wt% of ZrSiO4, 2-20 wt% of MoSi2 and 3-15 wt% of Si3N4 on the basis of the total mass of the anti-oxidation material. The anti-oxidation coating prepared from the anti-oxidation material disclosed by the invention has good anti-oxidation performance in a high-temperature environment.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of anti-oxidation materials, in particular to an anti-oxidation material, a structural member and a preparation method thereof, a brake disc and a vehicle. BACKGROUND

[0002] At present, the anti-oxidation coating used in the carbon ceramic brake disc is prone to cracks during use, and can only achieve oxidation resistance below 800℃ in a low-temperature environment, which cannot meet the oxidation resistance demand in a high-temperature environment, thereby limiting the use of the brake disc in a high-temperature working condition. SUMMARY

[0003] Therefore, the present application provides an anti-oxidation material, a structural member and a preparation method thereof, a brake disc and a vehicle, wherein the anti-oxidation material comprises ZrSiO4, MoSi2 and Si3N4 components, and the anti-oxidation performance of the anti-oxidation material in a high-temperature environment is realized through the self-healing property of the glass component and the high-temperature resistance and toughening effect of zirconium silicate.

[0004] In a first aspect, the present application provides an anti-oxidation material, wherein, based on the total mass of the anti-oxidation material, the anti-oxidation material comprises 35-65wt% of SiO2, 2-10wt% of B2O3, 4-16wt% of Al2O3, 2-8wt% of Y2O3, 6-25wt% of ZrSiO4, 2-20wt% of MoSi2 and 3-15wt% of Si3N4.

[0005] Optionally, the anti-oxidation material comprises 40-50wt% of SiO2, 4-7wt% of B2O3, 6-12wt% of Al2O3, 3-5wt% of Y2O3, 10-20wt% of ZrSiO4, 12-18wt% of MoSi2 and 7-11wt% of Si3N4.

[0006] Optionally, the mass ratio of ZrSiO4, MoSi2 and Si3N4 in the anti-oxidation material is 1: (0.1-1.5): (0.3-1.3).

[0007] In a second aspect, the present application provides a structural member, which comprises a base body and an anti-oxidation coating arranged on the surface of the base body, and the anti-oxidation coating comprises the anti-oxidation material according to the first aspect of the present application.

[0008] Optionally, the thickness of the anti-oxidation coating is 30-150μm.

[0009] Optionally, a transition layer is further arranged between the base body and the anti-oxidation coating.

[0010] Optionally, the thickness of the transition layer is 50-300μm.

[0011] Optionally, the thickness ratio of the anti-oxidation coating to the transition layer is 1: (2-3).

[0012] Optionally, the transition layer comprises SiC.

[0013] Optionally, the material of the substrate comprises one of graphite, C / C composite material, C / SiC composite material or C / C-SiC composite material.

[0014] Optionally, the fracture toughness of the anti-oxidation coating is at least 1.5 MPa·m 1 / 2 .

[0015] In a third aspect, the application provides a preparation method of a structural member, wherein the anti-oxidation material of the first aspect of the application is prepared into a slurry and coated on the surface of a substrate, and a first heat treatment is performed to form an anti-oxidation coating on the surface of the substrate.

[0016] Optionally, a transition layer is prepared on the surface of the substrate before the anti-oxidation material is prepared into a slurry and coated on the surface of the substrate; wherein the transition layer comprises SiC.

[0017] Optionally, the temperature of the first heat treatment is 1200-1400℃, and the time of the first heat treatment is 2-4h.

[0018] In a fourth aspect, the application provides a brake disc, which comprises the anti-oxidation material of the first aspect of the application or the structural member of the second aspect of the application.

[0019] In a fifth aspect, the application provides a vehicle, which comprises the brake disc of the fourth aspect of the application.

[0020] According to the above technical solution, the anti-oxidation material of the application comprises 35-65wt% of SiO2, 2-10wt% of B2O3, 4-16wt% of Al2O3, 2-8wt% of Y2O3, 6-25wt% of ZrSiO4, 2-20wt% of MoSi2 and 3-15wt% of Si3N4, based on the total mass of the anti-oxidation material. The anti-oxidation material improves the anti-oxidation performance and impact resistance of the anti-oxidation coating comprising the anti-oxidation material through the synergistic effect of the above components, especially ZrSiO4, MoSi2 and Si3N4, thereby improving the service life and stability of the brake disc comprising the anti-oxidation coating.

[0021] Other features and advantages of the application will be described in detail in the following specific embodiments. BRIEF DESCRIPTION OF DRAWINGS

[0022] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings needed to be used in the description of the embodiments will be briefly introduced. Obviously, the drawings in the following description only represent some of the embodiments of the present application, and other drawings can be obtained by those skilled in the art without any creative effort on the basis of these drawings.

[0023] Figure 1 is a structural diagram of the structure of the structure described in the present application.

[0024] Reference signs: 1-oxidation-resistant coating, 2-transition layer, 3-matrix. DETAILED DESCRIPTION

[0025] The technical solutions in the embodiments of the present application will be described clearly and completely below. Obviously, the described embodiments only represent some of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without any creative effort belong to the scope of protection of the present application.

[0026] The present application provides an oxidation-resistant material, which comprises 35-65wt% of SiO2, 2-10wt% of B2O3, 4-16wt% of Al2O3, 2-8wt% of Y2O3, 6-25wt% of ZrSiO4, 2-20wt% of MoSi2 and 3-15wt% of Si3N4, based on the total mass of the oxidation-resistant material. The combination of the above components, especially the combination of ZrSiO4, MoSi2 and Si3N4, enables the oxidation-resistant coating prepared from the oxidation-resistant material to have excellent oxidation-resistant performance. Further, the oxidation-resistant material can preferably comprise 40-50wt% of SiO2, 4-7wt% of B2O3, 6-12wt% of Al2O3, 3-5wt% of Y2O3, 10-20wt% of ZrSiO4, 12-18wt% of MoSi2 and 7-11wt% of Si3N4; the further preferred combination is conducive to better synergistic effect of the components and improvement of the oxidation resistance. Meanwhile, when the mass ratio of ZrSiO4, MoSi2 and Si3N4 in the oxidation-resistant material satisfies 1:(0.1-1.5):(0.3-1.3), the advantages of high-temperature resistance and oxidation resistance can be better synergistically exerted.

[0027] The present application provides a structure, such as Figure 1As shown in the embodiment of the present application, the structural member comprises an oxidation-resistant coating 1, a transition layer 2 and a substrate 3; specifically, the transition layer 2 and the oxidation-resistant coating 1 are sequentially stacked outward along the surface of the substrate 3. The transition layer 2 is located between the substrate 3 and the oxidation-resistant coating 1. Specifically, the oxidation-resistant coating 1 can form a barrier layer on the transition layer 2 and the surface of the substrate 3, effectively preventing the invasion of oxygen; at high temperatures, the oxidation-resistant coating 1 can exist stably and is not easily destroyed by oxidation, thereby prolonging the service life of the structural member. In addition, the oxidation-resistant coating 1 can also improve the mechanical properties, such as increasing the bending strength of the structural member, etc.

[0028] In an embodiment of the present application, based on the total mass of the oxidation-resistant coating, the oxidation-resistant coating 1 comprises 35-65wt% of SiO2, 2-10wt% of B2O3, 4-16wt% of Al2O3, 2-8wt% of Y2O3, 6-25wt% of ZrSiO4, 2-20wt% of MoSi2 and 3-15wt% of Si3N4. Through the collocation and synergistic effect of the above components, the oxidation-resistant coating 1 also has good oxidation resistance in a high-temperature environment.

[0029] In an embodiment of the present application, in order to further improve the oxidation resistance of the oxidation-resistant coating 1 and improve the synergistic effect of the components, based on the total mass of the oxidation-resistant coating 1, the oxidation-resistant coating 1 is further preferably composed of 40-50wt% of SiO2, 4-7wt% of B2O3, 6-12wt% of Al2O3, 3-5wt% of Y2O3, 10-20wt% of ZrSiO4, 12-18wt% of MoSi2 and 7-11wt% of Si3N4.

[0030] The oxidation-resistant coating 1 described in the present application is prepared from the oxidation-resistant material described in the present application. On the one hand, the glass component in the oxidation-resistant material has self-healing property and can achieve oxidation resistance in a low-temperature environment; on the other hand, the oxidation-resistant coating 1 comprises ZrSiO4, MoSi2 and Si3N4, which have the advantages of high-temperature resistance and oxidation resistance, and ZrSiO4 can also deflect cracks, slow down the stress concentration effect of crack tips and hinder crack propagation, thereby playing a toughening role, so that the fracture toughness of the oxidation-resistant coating is at least 1.5MPa·m 1 / 2MoSi2 and Mo5Si3, and the formation of SiO2 further hinders the continuous oxidation of MoSi2 and Mo5Si3, i.e., the anti-oxidation coating 1 prevents oxygen from further entering the SiC coating 2 and the substrate 3 (2MoSi2+7O2=4SiO2+2MoO3, wherein MoO3 is directly volatilized in the gas phase; 5MoSi2+7O2=Mo5Si3+7SiO2); Mo5Si3 has good high-temperature creep resistance, which can keep the anti-oxidation coating 1 intact under high-temperature oxidation conditions, and reduce the occurrence of cracking and delamination. Si3N4 has a low thermal expansion coefficient, and the thermal expansion coefficient thereof is 2.35×10 -6 / K; and the thermal expansion coefficient of the glass component is relatively high. The addition of Si3N4 can appropriately reduce the thermal expansion coefficient of the anti-oxidation coating 1, so that the thermal expansion coefficients of the anti-oxidation coating 1, the transition layer 2 and the substrate 3 are more close, and the phenomena of delamination and cracking are reduced, thereby further improving the anti-oxidation performance of the anti-oxidation coating. The above advantages synergistically enhance the anti-oxidation ability of the anti-oxidation coating.

[0031] In an embodiment of the present application, the mass ratio of ZrSiO4, MoSi2 and Si3N4 in the anti-oxidation coating is 1:(0.1-1.5):(0.3-1.3). In order to make the ZrSiO4, MoSi2 and Si3N4 in the anti-oxidation coating better synergistically exert the advantages of high-temperature resistance and oxidation resistance, the mass ratio of ZrSiO4, MoSi2 and Si3N4 can be further preferably 1:(0.5-1.5):(0.4-1.0). Specifically, the mass ratio of ZrSiO4, MoSi2 and Si3N4 can be 1:1:0.53, 1:1.36:0.82, 1:1.2:0.67, 1:1.5:0.8, 1:0.63:0.42, 1:1:0.33 or 1:0.12:0.32, etc.

[0032] In the present application, the anti-oxidation coating 1 can reduce the contact of the substrate 3 with external oxygen, and the transition layer 2 can be a SiC coating, which is characterized by high hardness and wear resistance, and is helpful to prolong the service life of the brake disc. On the other hand, the transition layer 2 can further reduce the contact of the substrate 3 with external oxygen, and can match the thermal expansion coefficients of the substrate 3 and the anti-oxidation coating 1. The thickness of the anti-oxidation coating 1 and the transition layer 2 and the ratio of the thicknesses of the two coatings directly affect the anti-oxidation performance and service life of the brake disc. When the anti-oxidation coating 1 is thicker, it can better fill surface defects and block the penetration of oxygen; but excessive thickness can cause the anti-oxidation coating 1 to be more easily damaged or peeled off during braking. When the transition layer 2 is thicker, it can provide better wear resistance and hardness, but it can also affect the overall anti-oxidation performance of the structural member.

[0033] In an embodiment of the present application, the thickness of the oxidation-resistant coating 1 is 30-150 μm, and the thickness of the transition layer 2 is 50-300 μm. Specifically, the thickness of the oxidation-resistant coating 1 can be 110 μm, and the thickness of the transition layer 2 can be 200 μm. The thicknesses of the oxidation-resistant coating 1 and the transition layer 2 in this range can ensure the mechanical strength of the coating and at the same time have better oxidation resistance.

[0034] In an embodiment of the present application, the thickness ratio of the oxidation-resistant coating 1 to the transition layer 2 is 1:(2-3). Specifically, the thickness ratio of the oxidation-resistant coating 1 to the transition layer 2 can be 1:2, 1:3, or 11:20. In an embodiment of the present application, the thickness ratio of the oxidation-resistant coating 1 to the transition layer 2 is 11:20. The thickness ratio of the oxidation-resistant coating 1 to the transition layer 2 in this range can ensure excellent performance and long service life of the brake disc.

[0035] In an embodiment of the present application, the material of the substrate 3 comprises one of graphite, C / C composite material, C / SiC composite material, or C / C-SiC composite material. Specifically, the material of the substrate 3 can be graphite, C / C composite material, C / SiC composite material, or C / C-SiC composite material. C / C composite material is a carbon fiber reinforced carbon matrix composite material, which combines the high strength of carbon fiber and the good thermal conductivity of carbon matrix, so that the C / C composite material brake disc has excellent performance in high temperature and high speed environment. C / SiC composite material, also known as carbon ceramic brake material, is made of carbon fiber reinforced silicon carbide composite material, which has the advantages of low density, high strength, stable friction performance, and high temperature resistance. C / C-SiC composite material is a carbon fiber reinforced carbon and silicon carbide ceramic matrix composite material, which inherits the advantages of C / C composite material and improves the friction coefficient and the oxidation resistance by introducing silicon carbide component. The material of the substrate 3 has a wide variety of choices, which can be selected according to different needs in practical applications.

[0036] In an embodiment of the present application, the fracture toughness of the oxidation-resistant coating 1 is at least 1.5 MPa·m 1 / 2 , and further, the fracture toughness of the oxidation-resistant coating 1 is 1.5-3.0 MPa·m 1 / 2 . Specifically, the fracture toughness of the oxidation-resistant coating 1 can be, but is not limited to, 2.4 MPa·m 1 / 2 , 1.8 MPa·m 1 / 2 , 2.2 MPa·m 1 / 2 , 1.6 MPa·m 1 / 2 , 1.9 MPa·m 1 / 2, 1.7 MPa·m 1 / 2 , 1.7 MPa·m 1 / 2 and the like. The fracture toughness of the brake disc oxidation-resistant coating is an important performance indicator, which determines the ability of the oxidation-resistant coating to resist fracture when subjected to external stress or impact. High fracture toughness means that the oxidation-resistant coating can maintain its integrity when subjected to a certain degree of stress and is not prone to fracture or damage. The oxidation-resistant coating 1 described in the present application has strong resistance to external stress or impact, thereby improving the service life and performance stability of the brake disc.

[0037] The present application also provides a preparation method of the above structural member, specifically comprising the following steps: S1, pretreating the substrate 3; S2, preparing a transition layer 2 on the surface of the substrate 3; S3, preparing a slurry of the oxidation-resistant material, coating the slurry on the surface of the transition layer 2, drying, and performing heat treatment in an inert atmosphere to form the oxidation-resistant coating 1 on the surface of the transition layer 2.

[0038] In an embodiment of the present application, in the step S1, the pretreatment of the substrate 3 includes cutting the material of the substrate 3 into a size of 50 mm x 50 mm x 10 mm, polishing the surface of the substrate 3 with 500 mesh sandpaper, then ultrasonic cleaning with anhydrous ethanol for 15-25 min, and then drying in a 70-90℃ oven for 22-26 h.

[0039] In an embodiment of the present application, the transition layer 2 comprises SiC, and the step S2 specifically comprises: weighing 70-85wt% Si powder, 5-15wt% graphite, and 2-10wt% Al2O3, mixing the above powders uniformly in a graphite crucible, then completely burying the substrate 3 in the mixed powders, and heat treating at 1600-1800℃ for 2-3h to prepare the transition layer 2, wherein the thickness of the transition layer 2 is 50-300μm.

[0040] In an embodiment of the present application, the step S3 specifically comprises: weighing the anti-oxidation material, specifically comprising 35-65wt% of SiO2, 2-10wt% of B2O3, 4-16wt% of Al2O3, 2-8wt% of Y2O3, 6-25wt% of ZrSiO4, 2-20wt% of MoSi2 and 3-15wt% of Si3N4, and then performing heat treatment under a nitrogen atmosphere at 1500-1700℃ for 1-2h, and then performing water quenching and crushing to obtain a mixed powder, and then preparing the mixed powder into a slurry. Further, the anti-oxidation material can preferably comprise 40-50wt% of SiO2, 4-7wt% of B2O3, 6-12wt% of Al2O3, 3-5wt% of Y2O3, 10-20wt% of ZrSiO4, 12-18wt% of MoSi2 and 7-11wt% of Si3N4, which is beneficial to better synergistic effect of the components. Then the slurry prepared from the anti-oxidation material is uniformly coated on the surface of the transition layer 2, the coating thickness is 30-150μm, and the coating is dried at a temperature of 100-120℃ for 3-5h; then heat treatment is performed under a nitrogen atmosphere at a temperature of 1200-1400℃ for 2-4h, to obtain an anti-oxidation coating 1, so that the prepared structure comprises the anti-oxidation coating 1, the SiC coating 2 and the substrate 3.

[0041] The present application provides a brake disc comprising the anti-oxidation material or the structure as described in the present application, which has strong anti-oxidation ability under high-temperature working conditions, long service life and good stability.

[0042] The present application provides a vehicle comprising the brake disc as described in the present application, which has excellent braking performance.

[0043] The effects of the technical scheme of the present application are further described below through specific examples.

[0044] Embodiment 1 S1, substrate pretreatment: cutting a C / C-SiC composite substrate into 50mm×50mm×10mm, polishing the surface of the substrate with 500-mesh sandpaper, then ultrasonic cleaning with anhydrous ethanol for 20min, and then placing the substrate in a 80℃ oven for drying treatment for 24h.

[0045] S2, transition layer preparation: weighing 80wt% of Si powder, 10wt% of graphite and 10wt% of Al2O3 powder, mixing uniformly, then placing the mixed powder in a graphite crucible, then completely filling the mixed powder in the C / C-SiC composite substrate, and then performing heat treatment at 1800℃ for 2h to obtain a transition layer, the thickness of the transition layer is 200μm.

[0046] S3, Preparation of the oxidation-resistant material: 45wt% SiO2, 6wt% B2O3, 7wt% Al2O3, 4wt% Y2O3, 15wt% ZrSiO4, 15wt% MoSi2 and 8wt% Si3N4 were weighed, heat-treated at 1500°C, then water-quenched, crushed to obtain mixed powder, and the mixed powder was prepared into the oxidation-resistant material.

[0047] S4, Preparation of the oxidation-resistant coating: the oxidation-resistant material was prepared into slurry, uniformly coated on the surface of the transition layer with a coating thickness of 110 μm, then dried at 100°C for 6h, heat-treated at 1250°C for 30min in a nitrogen atmosphere to obtain the C / C-SiC composite material comprising the oxidation-resistant coating and the transition layer.

[0048] Example 2 S1, Pretreatment of the substrate: the C / C-SiC composite material substrate was cut into 50mm×50mm×10mm, the surface of the substrate was polished with 500-mesh sandpaper, then ultrasonically cleaned with anhydrous ethanol for 20min, and placed in a 80°C oven for drying treatment for 24h.

[0049] S2, Preparation of the transition layer: 80wt% Si powder, 10wt% graphite and 10wt% Al2O3 powder were weighed, uniformly mixed, then placed in a graphite crucible, and the C / C-SiC composite material substrate was completely embedded in the mixed powder, heat-treated at 1800°C for 2h to obtain the transition layer, and the thickness of the transition layer was 200μm.

[0050] S3, Preparation of the oxidation-resistant material: 36wt% SiO2, 6wt% B2O3, 10wt% Al2O3, 5wt% Y2O3, 10wt% ZrSiO4, 20wt% MoSi2 and 13wt% Si3N4 were weighed, heat-treated at 1500°C, then water-quenched, crushed to obtain mixed powder, and the mixed powder was prepared into the oxidation-resistant material.

[0051] S4, Preparation of the oxidation-resistant coating: the oxidation-resistant material was prepared into slurry, uniformly coated on the surface of the transition layer with a coating thickness of 110 μm, then dried at 100°C for 6h, heat-treated at 1250°C for 30min in a nitrogen atmosphere to obtain the C / C-SiC composite material comprising the oxidation-resistant coating and the transition layer.

[0052] Example 3 S1, Pretreatment of the substrate: the C / C-SiC composite material substrate was cut into 50mm×50mm×10mm, the surface of the substrate was polished with 500-mesh sandpaper, then ultrasonically cleaned with anhydrous ethanol for 20min, and placed in a 80°C oven for drying treatment for 24h.

[0053] S2, transition layer preparation: 80wt% Si powder, 10wt% graphite and 10wt% Al2O3 powder were weighed, mixed uniformly and then put into a graphite crucible, then the C / C-SiC composite material substrate was completely filled in the mixed powder, and a transition layer was obtained by heat treatment at 1800°C for 2h, the thickness of the transition layer was 200μm.

[0054] S3, oxidation-resistant material preparation: 40wt% SiO2, 6wt% B2O3, 15wt% Al2O3, 4wt% Y2O3, 11wt% ZrSiO4, 15wt% MoSi2 and 9wt% Si3N4 were weighed, heat treated at 1500°C, then water quenched, crushed to obtain a mixed powder, and the mixed powder was prepared into an oxidation-resistant material.

[0055] S4, oxidation-resistant coating preparation: the oxidation-resistant material was prepared into a slurry, uniformly coated on the surface of the transition layer, the coating thickness was 110μm, then dried at 100°C for 6h, and heat treated at 1250°C for 30min in a nitrogen atmosphere to obtain a C / C-SiC composite material including an oxidation-resistant coating and a transition layer.

[0056] Example 4 S1, substrate pretreatment: the C / C-SiC composite material substrate was cut into 50mm×50mm×10mm, the surface of the substrate was polished with 500 mesh sandpaper, then ultrasonically cleaned with anhydrous ethanol for 20min, and then placed in an 80°C oven for drying treatment for 24h.

[0057] S2, transition layer preparation: 80wt% Si powder, 10wt% graphite and 10wt% Al2O3 powder were weighed, mixed uniformly and then put into a graphite crucible, then the C / C-SiC composite material substrate was completely filled in the mixed powder, and a transition layer was obtained by heat treatment at 1800°C for 2h, the thickness of the transition layer was 200μm.

[0058] S3, oxidation-resistant material preparation: 40wt% SiO2, 6wt% B2O3, 7wt% Al2O3, 4wt% Y2O3, 15wt% ZrSiO4, 18wt% MoSi2 and 10wt% Si3N4 were weighed, heat treated at 1500°C, then water quenched, crushed to obtain a mixed powder, and the mixed powder was prepared into an oxidation-resistant material.

[0059] S4, oxidation-resistant coating preparation: the oxidation-resistant material was prepared into a slurry, uniformly coated on the surface of the transition layer, the coating thickness was 110μm, then dried at 100°C for 6h, and heat treated at 1250°C for 30min in a nitrogen atmosphere to obtain a C / C-SiC composite material including an oxidation-resistant coating and a transition layer.

[0060] Example 5 S1, substrate pretreatment: the C / C-SiC composite substrate was cut into 50 mm x 50 mm x 10 mm, the surface of the substrate was polished with 500 mesh sandpaper, then ultrasonic cleaned with anhydrous ethanol for 20 min, and then dried in an 80°C oven for 24 h.

[0061] S2, transition layer preparation: 80wt% Si powder, 10wt% graphite and 10wt% Al2O3 powder were weighed, mixed uniformly and then placed in a graphite crucible, then the C / C-SiC composite substrate was completely embedded in the mixed powder, and a transition layer was obtained by heat treatment at 1800°C for 2h, the thickness of the transition layer was 200μm.

[0062] S3, preparation of oxidation-resistant material: 45wt% SiO2, 6wt% B2O3, 10wt% Al2O3, 5wt% Y2O3, 8wt% ZrSiO4, 16wt% MoSi2 and 10wt% Si3N4 were weighed, heat treated at 1500°C, then water quenched, crushed to obtain a mixed powder, and the mixed powder was prepared into an oxidation-resistant material.

[0063] S4, preparation of oxidation-resistant coating: the oxidation-resistant material was prepared into a slurry, which was uniformly coated on the surface of the transition layer with a coating thickness of 110μm, then dried at 100°C for 6h, and heat treated at 1250°C for 30min in a nitrogen atmosphere to obtain a C / C-SiC composite including an oxidation-resistant coating and a transition layer.

[0064] Example 6 S1, substrate pretreatment: the C / C-SiC composite substrate was cut into 50 mm x 50 mm x 10 mm, the surface of the substrate was polished with 500 mesh sandpaper, then ultrasonic cleaned with anhydrous ethanol for 20 min, and then dried in an 80°C oven for 24 h.

[0065] S2, transition layer preparation: 80wt% Si powder, 10wt% graphite and 10wt% Al2O3 powder were weighed, mixed uniformly and then placed in a graphite crucible, then the C / C-SiC composite substrate was completely embedded in the mixed powder, and a transition layer was obtained by heat treatment at 1800°C for 2h, the thickness of the transition layer was 200μm.

[0066] S3, preparation of oxidation-resistant material: 50wt% SiO2, 6wt% B2O3, 7wt% Al2O3, 4wt% Y2O3, 10wt% ZrSiO4, 15wt% MoSi2 and 8wt% Si3N4 were weighed, heat treated at 1500°C, then water quenched, crushed to obtain a mixed powder, and the mixed powder was prepared into an oxidation-resistant material.

[0067] S4, Anti-oxidation coating preparation: the anti-oxidation material is prepared into a slurry, which is uniformly coated on the surface of the transition layer with a coating thickness of 110 μm, then dried at 100 ℃ for 6 h, and heat treated at 1250 ℃ for 30 min in a nitrogen atmosphere to obtain a C / C-SiC composite material comprising an anti-oxidation coating and a transition layer.

[0068] Example 7 S1, Substrate pretreatment: the C / C-SiC composite material substrate is cut into 50 mm x 50 mm x 10 mm, the surface of the substrate is polished with 500 mesh sandpaper, then ultrasonic cleaned with anhydrous ethanol for 20 min, and dried in an 80 ℃ oven for 24 h.

[0069] S2, Transition layer preparation: 80 wt% Si powder, 10 wt% graphite and 10 wt% Al2O3 powder are weighed, mixed uniformly, and then placed in a graphite crucible, then the C / C-SiC composite material substrate is completely embedded in the mixed powder, and heat treated at 1800 ℃ for 2 h to obtain a transition layer, the thickness of the transition layer is 200 μm.

[0070] S3, Anti-oxidation material preparation: 45 wt% SiO2, 6 wt% B2O3, 7 wt% Al2O3, 3 wt% Y2O3, 19 wt% ZrSiO4, 12 wt% MoSi2 and 8 wt% Si3N4 are weighed, heat treated at 1500 ℃, then water quenched, crushed to obtain a mixed powder, and the mixed powder is prepared into an anti-oxidation material.

[0071] S4, Anti-oxidation coating preparation: the anti-oxidation material is prepared into a slurry, which is uniformly coated on the surface of the transition layer with a coating thickness of 110 μm, then dried at 100 ℃ for 6 h, and heat treated at 1250 ℃ for 30 min in a nitrogen atmosphere to obtain a C / C-SiC composite material comprising an anti-oxidation coating and a transition layer.

[0072] Example 8 S1, Substrate pretreatment: the C / C-SiC composite material substrate is cut into 50 mm x 50 mm x 10 mm, the surface of the substrate is polished with 500 mesh sandpaper, then ultrasonic cleaned with anhydrous ethanol for 20 min, and dried in an 80 ℃ oven for 24 h.

[0073] S2, Transition layer preparation: 80 wt% Si powder, 10 wt% graphite and 10 wt% Al2O3 powder are weighed, mixed uniformly, and then placed in a graphite crucible, then the C / C-SiC composite material substrate is completely embedded in the mixed powder, and heat treated at 1800 ℃ for 2 h to obtain a transition layer, the thickness of the transition layer is 200 μm.

[0074] S3, Preparation of the oxidation-resistant material: 45wt% SiO2, 10wt% B2O3, 4wt% Al2O3, 6wt% Y2O3, 15wt% ZrSiO4, 15wt% MoSi2 and 5wt% Si3N4 were weighed, and then heat-treated at 1500°C, followed by water quenching, crushing to obtain a mixed powder, and then the mixed powder was prepared into the oxidation-resistant material.

[0075] S4, Preparation of the oxidation-resistant coating: the oxidation-resistant material was prepared into a slurry, which was uniformly coated on the surface of the transition layer with a coating thickness of 110 μm, and then dried at 100°C for 6h, and heat-treated at 1250°C for 30min in a nitrogen atmosphere to obtain a C / C-SiC composite material comprising an oxidation-resistant coating and a transition layer.

[0076] Example 9 S1, Pretreatment of the substrate: the C / C-SiC composite material substrate was cut into 50mm×50mm×10mm, and the surface of the substrate was polished with 500-mesh sandpaper, and then ultrasonically cleaned with anhydrous ethanol for 20min, and then placed in a 80°C oven for drying treatment for 24h.

[0077] S2, Preparation of the transition layer: 80wt% Si powder, 10wt% graphite and 10wt% Al2O3 powder were weighed, mixed uniformly, and then placed in a graphite crucible, and then the C / C-SiC composite material substrate was completely embedded in the mixed powder, and then heat-treated at 1800°C for 2h to obtain a transition layer, and the thickness of the transition layer was 200μm.

[0078] S3, Preparation of the oxidation-resistant material: 45wt% SiO2, 6wt% B2O3, 9wt% Al2O3, 4wt% Y2O3, 25wt% ZrSiO4, 3wt% MoSi2 and 8wt% Si3N4 were weighed, and then heat-treated at 1500°C, followed by water quenching, crushing to obtain a mixed powder, and then the mixed powder was prepared into the oxidation-resistant material.

[0079] S4, Preparation of the oxidation-resistant coating: the oxidation-resistant material was prepared into a slurry, which was uniformly coated on the surface of the transition layer with a coating thickness of 110 μm, and then dried at 100°C for 6h, and heat-treated at 1250°C for 30min in a nitrogen atmosphere to obtain a C / C-SiC composite material comprising an oxidation-resistant coating and a transition layer.

[0080] Comparative Example 1 S1, Pretreatment of the substrate: the C / C-SiC composite material substrate was cut into 50mm×50mm×10mm, and the surface of the substrate was polished with 500-mesh sandpaper, and then ultrasonically cleaned with anhydrous ethanol for 20min, and then placed in a 80°C oven for drying treatment for 24h.

[0081] S2, transition layer preparation: 80wt% Si powder, 10wt% graphite and 10wt% Al2O3 powder were weighed, mixed uniformly and then put into a graphite crucible, then the C / C-SiC composite material substrate was completely filled in the mixed powder, and a transition layer was obtained by heat treatment at 1800°C for 2h, the thickness of the transition layer was 200μm.

[0082] S3, oxidation-resistant material preparation: 60wt% SiO2, 18wt% B2O3, 12wt% Al2O3 and 10wt% Y2O3 were weighed, heat treated at 1500°C, then water quenched, crushed to obtain a mixed powder, and the mixed powder was prepared into an oxidation-resistant material.

[0083] S4, oxidation-resistant coating preparation: the oxidation-resistant material was prepared into a slurry, uniformly coated on the surface of the SiC coating, the coating thickness was 110μm, then dried at 100°C for 6h, and heat treated at 1250°C for 30min under nitrogen atmosphere to obtain a C / C-SiC composite material including an oxidation-resistant coating and a transition layer.

[0084] Comparative Example 2 S1, substrate pretreatment: the C / C-SiC composite material substrate was cut into 50mm×50mm×10mm, the surface of the substrate was polished with 500 mesh sandpaper, then ultrasonically cleaned with anhydrous ethanol for 20min, and then placed in an 80°C oven for drying treatment for 24h.

[0085] S2, transition layer preparation: 80wt% Si powder, 10wt% graphite and 10wt% Al2O3 powder were weighed, mixed uniformly and then put into a graphite crucible, then the C / C-SiC composite material substrate was completely filled in the mixed powder, and a transition layer was obtained by heat treatment at 1800°C for 2h, the thickness of the transition layer was 200μm.

[0086] S3, oxidation-resistant material preparation: 70wt% SiO2, 14wt% B2O3, 3wt% Al2O3, 1wt% Y2O3, 5wt% ZrSiO4, 5wt% MoSi2 and 2wt% Si3N4 were weighed, heat treated at 1500°C, then water quenched, crushed to obtain a mixed powder, and the mixed powder was prepared into an oxidation-resistant material.

[0087] S4, oxidation-resistant coating preparation: the oxidation-resistant material was prepared into a slurry, uniformly coated on the surface of the transition layer, the coating thickness was 110μm, then dried at 100°C for 6h, and heat treated at 1250°C for 30min under nitrogen atmosphere to obtain a C / C-SiC composite material including an oxidation-resistant coating and a transition layer.

[0088] Comparative Example 3 S1, substrate pretreatment: the C / C-SiC composite substrate was cut into 50 mm x 50 mm x 10 mm, the surface of the substrate was polished with 500 mesh sandpaper, then ultrasonic cleaned with anhydrous ethanol for 20 min, and then dried in an 80°C oven for 24 h.

[0089] S2, transition layer preparation: 80wt% Si powder, 10wt% graphite and 10wt% Al2O3 powder were weighed, mixed uniformly and then placed in a graphite crucible, then the C / C-SiC composite substrate was completely embedded in the mixed powder, and a transition layer was obtained by heat treatment at 1800°C for 2h, the thickness of the transition layer was 200μm.

[0090] S3, preparation of oxidation-resistant material: 30wt% SiO2, 14wt% B2O3, 3wt% Al2O3, 1wt% Y2O3, 28wt% ZrSiO4, 7wt% MoSi2 and 17wt% Si3N4 were weighed, heat treated at 1500°C, then water quenched, crushed to obtain a mixed powder, and the mixed powder was prepared into an oxidation-resistant material.

[0091] S4, preparation of oxidation-resistant coating: the oxidation-resistant material was prepared into a slurry, which was uniformly coated on the surface of the transition layer with a coating thickness of 110μm, then dried at 100°C for 6h, and heat treated at 1250°C for 30min in a nitrogen atmosphere to obtain a C / C-SiC composite including an oxidation-resistant coating and a transition layer.

[0092] Comparative Example 4 S1, substrate pretreatment: the C / C-SiC composite substrate was cut into 50 mm x 50 mm x 10 mm, the surface of the substrate was polished with 500 mesh sandpaper, then ultrasonic cleaned with anhydrous ethanol for 20 min, and then dried in an 80°C oven for 24 h.

[0093] S2, transition layer preparation: 80wt% Si powder, 10wt% graphite and 10wt% Al2O3 powder were weighed, mixed uniformly and then placed in a graphite crucible, then the C / C-SiC composite substrate was completely embedded in the mixed powder, and a transition layer was obtained by heat treatment at 1800°C for 2h, the thickness of the transition layer was 200μm.

[0094] S3, preparation of oxidation-resistant material: 50wt% SiO2, 6wt% B2O3, 10wt% Al2O3, 6wt% Y2O3, 5wt% ZrSiO4, 22wt% MoSi2 and 1wt% Si3N4 were weighed, heat treated at 1500°C, then water quenched, crushed to obtain a mixed powder, and the mixed powder was prepared into an oxidation-resistant material.

[0095] S4, Anti-oxidation coating preparation: the anti-oxidation material is prepared into a slurry, which is uniformly coated on the surface of the transition layer with a coating thickness of 110 μm, then dried at 100 ℃ for 6 h, and heat treated at 1250 ℃ for 30 min in a nitrogen atmosphere to obtain a C / C-SiC composite material comprising an anti-oxidation coating and a transition layer.

[0096] Performance test (1) Static oxidation weight loss rate test The samples of each example and the comparative example are treated at 1250 ℃ for 30 min, the mass of the sample before and after oxidation is weighed, and the static oxidation weight loss rate of the sample is measured, and the test results are shown in Table 1. The calculation formula is: static oxidation weight loss rate = ((mass after oxidation-mass before oxidation) / mass before oxidation) x 100%. The smaller the static oxidation weight loss rate, the better the anti-oxidation performance of the anti-oxidation coating.

[0097] (2) Thermal cycle oxidation weight loss rate test The samples of each example and the comparative example are treated at 1500 ℃ for 10 min, then cooled to room temperature, and cycled 40 times, the mass of the sample before and after thermal cycle oxidation is weighed, and the thermal cycle oxidation weight loss rate of the sample is measured, and the test results are shown in Table 1. The calculation formula is: thermal cycle oxidation weight loss rate = ((mass after oxidation-mass before oxidation) / mass before oxidation) x 100%. The smaller the thermal cycle oxidation weight loss rate, the better the anti-oxidation performance of the anti-oxidation coating.

[0098] (3) Fracture toughness test The fracture toughness of the anti-oxidation coating in each example and the comparative example is tested according to GB / T 37900-2009 Ultra-thin glass hardness and fracture toughness test method, and the test results are shown in Table 1.

[0099] Table 1 Static oxidation weight loss rate / wt% Thermal cycling oxidation weight loss rate / wt% Fracture toughness of the oxidation resistant coating / MPa-m 1 / 2 ]] Example 1 0.6 0.23 2.4 Example 2 2.5 0.40 1.8 Example 3 2.2 0.28 1.8 Example 4 1.0 0.17 2.2 Example 5 3.6 0.52 1.6 Example 6 1.5 0.35 1.9 Example 7 1.2 0.26 2.0 Example 8 3.9 0.36 1.7 Example 9 3.0 0.34 1.9 Comparative Example 1 9.2 2.1 1.0 Comparative Example 2 7.5 1.5 1.3 Comparative Example 3 8.3 0.9 0.9 Comparative Example 4 7.9 1.2 0.7 As shown in Table 1, the static oxidation weight loss rate and the thermal cycle oxidation weight loss rate of the samples of each example are significantly lower than those of the comparative example, and the fracture toughness of the anti-oxidation coating of each example is significantly higher than that of the comparative example, indicating that the anti-oxidation coating prepared from the anti-oxidation material described in the present application also has excellent anti-oxidation performance and impact resistance under high temperature conditions.

[0100] The above is a preferred embodiment of the present application, but it cannot be interpreted as limiting the scope of the present application. It should be noted that for ordinary skilled persons in the art, without departing from the principles of the present application, a number of improvements and refinements can be made, which are also considered within the scope of protection of the present application.

Claims

1. An oxidation resistant material, characterized by, The anti-oxidation material comprises 35-65 wt% of SiO2, 2-10 wt% of B2O3, 4-16 wt% of Al2O3, 2-8 wt% of Y2O3, 6-25 wt% of ZrSiO4, 2-20 wt% of MoSi2 and 3-15 wt% of Si3N4, based on the total mass of the anti-oxidation material.

2. The oxidation resistant material of claim 1, wherein, The anti-oxidation material comprises 40-50 wt% of SiO2, 4-7 wt% of B2O3, 6-12 wt% of Al2O3, 3-5 wt% of Y2O3, 10-20 wt% of ZrSiO4, 12-18 wt% of MoSi2 and 7-11 wt% of Si3N4.

3. The oxidation resistant material of claim 1, wherein, The mass ratio of ZrSiO4, MoSi2 and Si3N4 in the anti-oxidation material is 1: (0.1-1.5): (0.3-1.3).

4. A structural member, characterized by The structural member comprises a base body and an anti-oxidation coating layer arranged on the surface of the base body, and the anti-oxidation coating layer comprises the anti-oxidation material according to any one of claims 1-3.

5. The structural member of claim 4, wherein The thickness of the anti-oxidation coating layer is 30-150 μm.

6. The structural member of claim 4, wherein A transition layer is further arranged between the base body and the anti-oxidation coating layer.

7. The structural member of claim 6, wherein The thickness of the transition layer is 50-300 μm.

8. The structural member of claim 6, wherein The thickness ratio of the anti-oxidation coating layer to the transition layer is 1: (2-3).

9. The structural member of claim 4, wherein The transition layer comprises SiC.

10. The structural member of claim 4, wherein The material of the base body comprises one of graphite, C / C composite material, C / SiC composite material or C / C-SiC composite material.

11. A structural member as claimed in any one of claims 4 to 10, wherein, The fracture toughness of the oxidation-resistant coating is at least 1.5 MPa-m 1 / 2 .

12. A method of producing a structural member, characterized by The anti-oxidation material according to any one of claims 1-3 is prepared into a slurry and coated on the surface of a base body, and then heat treated to form an anti-oxidation coating layer on the surface of the base body.

13. The method of producing a structural member according to claim 12, wherein Before the anti-oxidation material is prepared into a slurry and coated on the surface of a base body, a transition layer is prepared on the surface of the base body, and the transition layer comprises SiC.

14. The method of producing a structural member according to claim 12, wherein The temperature of the heat treatment is 1200-1400 ℃, and the time of the first heat treatment is 2-4 h.

15. A brake disc, characterized in that The brake disc comprises the anti-oxidation material according to any one of claims 1-3 or the structural member according to any one of claims 4-11.

16. A vehicle characterized by comprising: The vehicle comprises the brake disc according to claim 15.

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