碳材料表面抗氧化涂层的制备及性能研究
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摘要
随着碳材料在各个领域的广泛应用,碳复合材料的研发得到了迅猛发展。但是由于碳材料在氧化性气氛下极易氧化,大大限制了其使用环境,应用范围缩小。因此在碳材料表面制备抗氧化涂层成为提高其应用性的主要途径。在碳材料表面制备防护涂层不仅能够提高其抗氧化性能,同时还能够提高其力学性能,并且不影响基体的自身机能。本文围绕碳材料抗氧化涂层的制备,利用场发射扫描电子显微镜(FESEM)、X射线衍射仪(XRD)、透射电子显微镜(TEM)、热分析仪(TG/DSC)、傅里叶变换红外光谱(FTIR)以及拉曼光谱(Raman)等分析手段对涂层及增强体的形貌、组织结构、成分、热性能、化学结构等进行表征测试,对纯SiC涂层的失效机理、增强体对涂层性能的影响、涂层制备工艺、增强体引入方法等进行了研究。
通过包埋法在碳材料表面制备一层纯SiC涂层,通过氧化及热震实验,对比其实验前后形貌及结构变化,分析涂层对基体的防护及失效机理,得到以下结论：所制备的纯SiC涂层对石墨基体具有一定的抗氧化作用,但是其效果并不显著,在1400℃下氧化2h,进行3次循环后氧化失重不能满足实际应用要求。纯SiC涂层能够在一定程度上提高碳材料的抗氧化性能且表现出一定的自愈合能力,但是其自愈合过程中对于涂层本身的消耗较大,这也对其防护作用造成了一定程度的影响。热震实验中的失效主要是由于其本身致密性较低,不能在低温起到很好的防护作用,且热失配造成的涂层开裂较为严重。纯SiC涂层在对基体的抗氧化过程中主要受两个阶段的控制：当温度较低时,氧化过程由氧化反应和扩散反应共同控制,基体发生均匀氧化反应；温度较高时,氧化过程由扩散速度控制,基体发生不均匀氧化反应。纯SiC涂层在高温氧化实验和热震实验中的裂纹产生机理不同：高温氧化实验最初是涂层外表面微裂纹的生成,且在反复氧化实验中,裂纹能够自愈合,随着涂层的自身消耗,裂纹贯穿涂层直到基体表面而失效；而在热震实验中,涂层表面裂纹不愈合,且随着实验的进行,产生于涂层与基体界面结合处的裂纹相互串联扩展,并最终导致SiC涂层脱落。
以纯SiC涂层的失效机理研究为基础,通过引入SiC晶须层,改善包埋法制备的SiC涂层性能,通过氧化实验,对比了其不同温度氧化实验前后形貌及结构变化,分析涂层对基体的防护机理。以低成本的H-PSO为原料引入SiC晶须后制备的涂层,表现出较好的高温抗氧化性能。在氧化过程中,涂层表面微孔能够愈合,1400℃下氧化4h,氧化失重仅为0.71%。SiC晶须的存在,对Si的过度渗透有一定的抑制作用,但是由于涂层本身仍存在微孔,因此涂层的抗氧化性能仍有待提高。
通过物理掺杂引入MoSi2增强体,在石墨基体表面制备MOSi2改性SiC复合涂层,通过氧化及热震实验,对比其实验前后形貌及结构变化,分析了涂层对基体的防护机理。通过均匀设计试验研究了复合涂层的最佳制备工艺,结果表明：包埋法制备复合涂层的工艺参数中对涂层性能影响最大的是热处理的保温时间。根据实验结果及条件允许范围,我们选用的试验参数是：热处理温度为1600℃,保温时间为2h,气流量为150ml/min。经过循环静态空气氧化实验发现MoSi2改性SiC涂层能够较好的起到抗氧化作用,其1400℃下的氧化失重明显低于纯SiC涂层,经1400℃氧化8h,氧化失重小于4%。MoSi2增强体的引入有利于涂层与基体间热应力调节,减少了涂层制备过程中由于热应力作用产生的裂纹。此外,由于MoSi2自身的高温软塑性及体积膨胀使得所制备的涂层致密性提高。然而,MOSi2增强体的引入对提高试样的低温抗热震性能作用不大。
用H-PSO作先驱体,分别以石墨材料和C/C复合材料为基体,通过浸渍烧结引入SiC晶须层,此方法制备工艺简单,成本低。在碳材料表面制备SiC晶须层的基础上又经过二次包埋制备SiC/Si/MoSi2复合涂层。涂层厚度约为300μm,且涂层与基体结合较好,涂层表面连续致密。通过1000℃和1400℃下氧化实验及热震实验,分析了改性涂层的效果。以石墨材料为基体制备的试样在氧化实验前,1400℃的4h的预氧化处理使得试样产生0.045%的增重。之后的氧化循环实验表明,所制备的SiC/Si/MOSi2复合涂层具有良好的抗氧化性能,它能够使石墨材料在1000℃氧化12h后,氧化失重低于1%,且在氧化过程中,涂层表现出一定的自愈合能力。SiC晶须层不仅能够有效调节应力,减少裂纹的产生,同时能够有效减小熔融Si的渗透深度,得到厚度适中且连续致密的SiC/Si/MoSi2复合涂层。MOSi2的引入能够有效提高涂层抗氧化性能。其中的MoSi2在氧化过程中快速生成的SiO2能够及时填补涂层自身孔隙,起到自愈合的作用。而以MoSi2为增强体相较于Mo表现出更好的效果,1400℃下氧化10h,氧化失重约为1%。对于C/C复合材料基体制备的涂层,引入SiC晶须层能够一定程度的抑制熔融Si的过度渗入,调节涂层与基体热膨胀差异,但是其在1400℃下的抗氧化性能还有待提高。在石墨基体表面制备SiC/Si/MOSi2复合涂层能够有效地改善试样的抗热震性能。
同样以H-PSO为先驱体,通过粉末法制备SiC晶须,并以结晶率为指标,用正交试验法研究制备工艺对晶须生长的影响。通过不同温度下生成物的结构及形貌变化,研究了SiC晶须的生长机理。此外,以新的SiC晶须制备方法在石墨基体表面引入了晶须层,经二次包埋烧结制备出最终的复合涂层。通过相应的氧化实验及热震实验,借助测试手段观察涂层的形貌及物相变化,得到以下结论：热处理温度是影响SiC晶须生成最重要的因素,其影响程度远远大于其他参数。高的热处理温度、较高的气流量、较小的孔隙率、长的保温时间有利于SiC晶须的生成长大。所生成的SiC晶须是以结晶相的β一SiC为核,以硅氧化物为壳的核壳结构,且沿(111)晶面方向生长的。晶须形貌均一,呈长直态分布在基体表面,长径比大。碳基体的存在有利于SiC晶须的生成长大,且SiC晶须的生成先后遵循defect-vapor-vapor及Vapor-liquid-defect-solid反应机理。以新方法引入SiC晶须层,再通过包埋法制备的复合涂层使得试样的抗氧化能力得到明显的提高,在1400℃下氧化10h,其热失重不超过1%。
Due to excellent high-temperature performance, carbon materials were widely used in many industries. However, the deadly problem for the application of these materials lay in their quick oxidation at high temperature in the presence of oxygen, which seriously affected the performance and service life of carbon materials. Thus, preparing anti-oxidation coating on the surface of the matrix was the ideal method to improve oxidation resistance and mechanical property of carbon materials without bad influence on the matrix's own performance. The article centered on preparation of oxidation resistance coating, and characterized the organization structure, composition, thermal property, and chemical structure by field emission scanning electron microscopy (FESEM), X-Ray Diffraction (XRD), transmission electron microscope (TEM), thermo-analytical instrument (TG/DSC), Fourier transform infrared spectroscopy (FTIR) and Raman spectroscopy (Raman). Based on the above, the failure mechanism of pure SiC coating, effect of the reinforcement on the performance of the coating, preparation technology of the coating, and the introduction methods of the reinforcement were investigated.
We prepared pure SiC coating on carbon materials by embedding method, and contrasted the morphology and structure changes before and after oxidation test and thermal shock test, then analyzed the protection and failure mechanism of the coating to the matrix. The results showed that the pure SiC coating had a certain antioxidant effect on graphite matrix, but its effect was not significant. The oxidation weightless could not satisfy the practical application, with oxidation for2h at1400℃after three cycles. Pure SiC coating had a certain degree of oxidation resistance for carbon materials and showed some self-healing ability, but self-consumption of the coating was bigger in the self-healing process, which caused a degree of negative influence to its protection. In thermal shock test, the failure was mainly due to its own low density, which induced the coating not able to play well protection at low temperature, and the cracking of the coating caused by thermal mismatch was more serious. Pure SiC coating in the oxidation test was mainly controlled by two stages:When the temperature was low, the oxidation process was controlled by both oxidation and diffusion reaction, and homogeneous oxidation reaction occurred on the surface of the matrix; at higher temperature, the oxidation process was controlled by the diffusion rate, and uneven oxidation reaction occurred on the surface of the matrix. The crack mechanisms of the pure SiC coatings were different in high temperature oxidation test and thermal shock test. The micro crack formation was on outside the surface of coating in high temperature oxidation test, and with the oxidation test repeated, the crack could be self-healing. However, in thermal shock test, the cracks were through the coating to the matrix surface, and as the experiment progressed, the crack didn't heal, eventually led to fall off.
Taking the research on failure mechanism of the pure SiC coating as the foundation, through the introduction of SiC whisker layer, we improved the performance of SiC coating prepared by the embedding method. Comparing the morphology and structural changes before and after the oxidation tests, we analyzed the protection mechanism of the coating to the matrix. Introduction of SiC whisker with H-PSO as a raw material before preparation of the final coating, which made the coating showed good oxidation resistance at high temperature. In the process of oxidation, micro pores of the coating surface could heal. The oxidation weight loss was only0.71%after oxidation at1400℃for4h. The presence of SiC whisker had a certain inhibition for excessive penetration of silicon, but because there was still a micro porous coating, the oxidation resistance of coating still needed to be improved.
We prepared the composite coating on surface of graphite matrix. The coating was reinforced by MoSi2through physical doping. Comparing the morphology and structure changes before and after the oxidation and thermal shock tests, the protection mechanism of the coating to the matrix was analyzed. The best preparation process of the composite coating was studied by uniform design experiment. The results showed that the most important parameter influence on composite coating prepared by embedding method was the holding time. According to the experimental results and conditions permissible range, we chose the test parameters were:heat temperature was1600℃, holding time was2h, and gas flow rate was150ml/min. After cyclic static air oxidation test, the coating showed better antioxidant property, and its weightlessness was lower than that of pure SiC coating, after oxidation at1400℃for8h, and the oxidation weight loss was less than4%. The introduction of MoSi2was beneficial to thermal stress adjustment between coating and matrix, and reduced the coating cracks due to thermal stress generated in the process of preparation. Because of high temperature plasticity and volume expansion, MoSi2made the density of the coating increased. However, as strengthen body, the introduction of MoSi2was not obvious for thermal shock effect at low temperature.
With H-PSO as a pioneer body, we introduced SiC whisker layer on the graphite or C/C matrix surface by dipping sintering process. The preparation of SiC whisker was simple and low cost. A SiC/Si/MoSi2coating for carbon materials was prepared by subsequent embedding technique. The thickness of the coating was about300μm. In addition, the coating combined with matrix well, and the surface was continuous and dense. Through oxidation test at1000℃or1400℃and thermal shock test at800℃, the performance of the coating was investigated. For graphite matrix coated by the SiC/Si/MoSi2coating, the oxidation pretreatment experiment was carried out in the static air at1400℃for4h before oxidation test and the sample had0.045%weight gain. Subsequent oxidation test showed that, the SiC/Si/MoSi2multi-coating had excellent anti-oxidation property, which could protect graphite materials from oxidation at1000℃in air for12h and the corresponding weight loss was below1%. Based on the surface morphology changes, oxidation pretreatment experiment and oxidation test enhanced densification of multi-coating and the coating had a certain self-healing ability. SiC whisker layer on the matrix surface could effectively regulated stress and reduced the generation of cracks. In addition, the existence of the whisker layer could effectively inhibit excess infiltration of molten Si and control the thickness of the coating. The introduction of MoSi2could effectively improve oxidation resistance of the coating. The formation of SiO2during oxidation process of MoSi2could fill the pores of the coating itself, showing the self-healing property. MoSi2had better effect compared with Mo, which could protect graphite materials from oxidation at1400℃in air for10h and the corresponding weight loss was about1%. For C/C composite, introduction of SiC whisker layer could inhibit excess infiltration of molten Si at a certain degree, and adjust thermal expansion differences between coating and matrix, but anti-oxidation property at1400℃needed to be improved. In addition, preparation of SiC/Si/MoSi2composite coating on graphite matrix could effectively improve the thermal shock resistance of the coating.
Same with H-PSO as the pioneer body, we introduced of SiC whisker layer on the graphite matrix surface by powder method, and used orthogonal test method to research the influence of preparation technology on growth of SiC whisker, with the crystalline fraction as target. The growth mechanism of SiC whisker was studied through comparing the changes of structure and morphology of the products at different temperatures. In addition, introducing SiC whisker layer by the new method, the final composite coating was formed on graphite matrix after subsequent embedding technique. By the corresponding oxidation test and thermal shock test, with the help of the test method to observe the changes of the coating morphology and phase, we got the following conclusion:The heat treatment temperature (T) was the most important factor that influenced the growth of SiC whisker, far exceeding the other factors. High temperature, higher gas flow, lower porosity and longer holding time were favorable to whisker generation. The SiC whisker was of core-shell structure with SiC phase as core and silicon oxide as the shell, growing along the direction of (111). The morphology of the whisker was uniform, distributing on the matrix surface with long straight state and larger length-diameter ratio. The existence of carbon matrix was beneficial to the growth of SiC whisker, and the growth of SiC whisker had followed defect-vapor-vapor and vapor-liquid-defect-solid mechanism. Introduction of SiC whisker layer by the new method, and then the composite coating prepared by embedding method enhanced the anti-oxidation property of the materials obviously. The coating could protect graphite materials from oxidation at1400℃in air for10h and the corresponding weight loss was below1%.
通过包埋法在碳材料表面制备一层纯SiC涂层,通过氧化及热震实验,对比其实验前后形貌及结构变化,分析涂层对基体的防护及失效机理,得到以下结论：所制备的纯SiC涂层对石墨基体具有一定的抗氧化作用,但是其效果并不显著,在1400℃下氧化2h,进行3次循环后氧化失重不能满足实际应用要求。纯SiC涂层能够在一定程度上提高碳材料的抗氧化性能且表现出一定的自愈合能力,但是其自愈合过程中对于涂层本身的消耗较大,这也对其防护作用造成了一定程度的影响。热震实验中的失效主要是由于其本身致密性较低,不能在低温起到很好的防护作用,且热失配造成的涂层开裂较为严重。纯SiC涂层在对基体的抗氧化过程中主要受两个阶段的控制：当温度较低时,氧化过程由氧化反应和扩散反应共同控制,基体发生均匀氧化反应；温度较高时,氧化过程由扩散速度控制,基体发生不均匀氧化反应。纯SiC涂层在高温氧化实验和热震实验中的裂纹产生机理不同：高温氧化实验最初是涂层外表面微裂纹的生成,且在反复氧化实验中,裂纹能够自愈合,随着涂层的自身消耗,裂纹贯穿涂层直到基体表面而失效；而在热震实验中,涂层表面裂纹不愈合,且随着实验的进行,产生于涂层与基体界面结合处的裂纹相互串联扩展,并最终导致SiC涂层脱落。
以纯SiC涂层的失效机理研究为基础,通过引入SiC晶须层,改善包埋法制备的SiC涂层性能,通过氧化实验,对比了其不同温度氧化实验前后形貌及结构变化,分析涂层对基体的防护机理。以低成本的H-PSO为原料引入SiC晶须后制备的涂层,表现出较好的高温抗氧化性能。在氧化过程中,涂层表面微孔能够愈合,1400℃下氧化4h,氧化失重仅为0.71%。SiC晶须的存在,对Si的过度渗透有一定的抑制作用,但是由于涂层本身仍存在微孔,因此涂层的抗氧化性能仍有待提高。
通过物理掺杂引入MoSi2增强体,在石墨基体表面制备MOSi2改性SiC复合涂层,通过氧化及热震实验,对比其实验前后形貌及结构变化,分析了涂层对基体的防护机理。通过均匀设计试验研究了复合涂层的最佳制备工艺,结果表明：包埋法制备复合涂层的工艺参数中对涂层性能影响最大的是热处理的保温时间。根据实验结果及条件允许范围,我们选用的试验参数是：热处理温度为1600℃,保温时间为2h,气流量为150ml/min。经过循环静态空气氧化实验发现MoSi2改性SiC涂层能够较好的起到抗氧化作用,其1400℃下的氧化失重明显低于纯SiC涂层,经1400℃氧化8h,氧化失重小于4%。MoSi2增强体的引入有利于涂层与基体间热应力调节,减少了涂层制备过程中由于热应力作用产生的裂纹。此外,由于MoSi2自身的高温软塑性及体积膨胀使得所制备的涂层致密性提高。然而,MOSi2增强体的引入对提高试样的低温抗热震性能作用不大。
用H-PSO作先驱体,分别以石墨材料和C/C复合材料为基体,通过浸渍烧结引入SiC晶须层,此方法制备工艺简单,成本低。在碳材料表面制备SiC晶须层的基础上又经过二次包埋制备SiC/Si/MoSi2复合涂层。涂层厚度约为300μm,且涂层与基体结合较好,涂层表面连续致密。通过1000℃和1400℃下氧化实验及热震实验,分析了改性涂层的效果。以石墨材料为基体制备的试样在氧化实验前,1400℃的4h的预氧化处理使得试样产生0.045%的增重。之后的氧化循环实验表明,所制备的SiC/Si/MOSi2复合涂层具有良好的抗氧化性能,它能够使石墨材料在1000℃氧化12h后,氧化失重低于1%,且在氧化过程中,涂层表现出一定的自愈合能力。SiC晶须层不仅能够有效调节应力,减少裂纹的产生,同时能够有效减小熔融Si的渗透深度,得到厚度适中且连续致密的SiC/Si/MoSi2复合涂层。MOSi2的引入能够有效提高涂层抗氧化性能。其中的MoSi2在氧化过程中快速生成的SiO2能够及时填补涂层自身孔隙,起到自愈合的作用。而以MoSi2为增强体相较于Mo表现出更好的效果,1400℃下氧化10h,氧化失重约为1%。对于C/C复合材料基体制备的涂层,引入SiC晶须层能够一定程度的抑制熔融Si的过度渗入,调节涂层与基体热膨胀差异,但是其在1400℃下的抗氧化性能还有待提高。在石墨基体表面制备SiC/Si/MOSi2复合涂层能够有效地改善试样的抗热震性能。
同样以H-PSO为先驱体,通过粉末法制备SiC晶须,并以结晶率为指标,用正交试验法研究制备工艺对晶须生长的影响。通过不同温度下生成物的结构及形貌变化,研究了SiC晶须的生长机理。此外,以新的SiC晶须制备方法在石墨基体表面引入了晶须层,经二次包埋烧结制备出最终的复合涂层。通过相应的氧化实验及热震实验,借助测试手段观察涂层的形貌及物相变化,得到以下结论：热处理温度是影响SiC晶须生成最重要的因素,其影响程度远远大于其他参数。高的热处理温度、较高的气流量、较小的孔隙率、长的保温时间有利于SiC晶须的生成长大。所生成的SiC晶须是以结晶相的β一SiC为核,以硅氧化物为壳的核壳结构,且沿(111)晶面方向生长的。晶须形貌均一,呈长直态分布在基体表面,长径比大。碳基体的存在有利于SiC晶须的生成长大,且SiC晶须的生成先后遵循defect-vapor-vapor及Vapor-liquid-defect-solid反应机理。以新方法引入SiC晶须层,再通过包埋法制备的复合涂层使得试样的抗氧化能力得到明显的提高,在1400℃下氧化10h,其热失重不超过1%。
Due to excellent high-temperature performance, carbon materials were widely used in many industries. However, the deadly problem for the application of these materials lay in their quick oxidation at high temperature in the presence of oxygen, which seriously affected the performance and service life of carbon materials. Thus, preparing anti-oxidation coating on the surface of the matrix was the ideal method to improve oxidation resistance and mechanical property of carbon materials without bad influence on the matrix's own performance. The article centered on preparation of oxidation resistance coating, and characterized the organization structure, composition, thermal property, and chemical structure by field emission scanning electron microscopy (FESEM), X-Ray Diffraction (XRD), transmission electron microscope (TEM), thermo-analytical instrument (TG/DSC), Fourier transform infrared spectroscopy (FTIR) and Raman spectroscopy (Raman). Based on the above, the failure mechanism of pure SiC coating, effect of the reinforcement on the performance of the coating, preparation technology of the coating, and the introduction methods of the reinforcement were investigated.
We prepared pure SiC coating on carbon materials by embedding method, and contrasted the morphology and structure changes before and after oxidation test and thermal shock test, then analyzed the protection and failure mechanism of the coating to the matrix. The results showed that the pure SiC coating had a certain antioxidant effect on graphite matrix, but its effect was not significant. The oxidation weightless could not satisfy the practical application, with oxidation for2h at1400℃after three cycles. Pure SiC coating had a certain degree of oxidation resistance for carbon materials and showed some self-healing ability, but self-consumption of the coating was bigger in the self-healing process, which caused a degree of negative influence to its protection. In thermal shock test, the failure was mainly due to its own low density, which induced the coating not able to play well protection at low temperature, and the cracking of the coating caused by thermal mismatch was more serious. Pure SiC coating in the oxidation test was mainly controlled by two stages:When the temperature was low, the oxidation process was controlled by both oxidation and diffusion reaction, and homogeneous oxidation reaction occurred on the surface of the matrix; at higher temperature, the oxidation process was controlled by the diffusion rate, and uneven oxidation reaction occurred on the surface of the matrix. The crack mechanisms of the pure SiC coatings were different in high temperature oxidation test and thermal shock test. The micro crack formation was on outside the surface of coating in high temperature oxidation test, and with the oxidation test repeated, the crack could be self-healing. However, in thermal shock test, the cracks were through the coating to the matrix surface, and as the experiment progressed, the crack didn't heal, eventually led to fall off.
Taking the research on failure mechanism of the pure SiC coating as the foundation, through the introduction of SiC whisker layer, we improved the performance of SiC coating prepared by the embedding method. Comparing the morphology and structural changes before and after the oxidation tests, we analyzed the protection mechanism of the coating to the matrix. Introduction of SiC whisker with H-PSO as a raw material before preparation of the final coating, which made the coating showed good oxidation resistance at high temperature. In the process of oxidation, micro pores of the coating surface could heal. The oxidation weight loss was only0.71%after oxidation at1400℃for4h. The presence of SiC whisker had a certain inhibition for excessive penetration of silicon, but because there was still a micro porous coating, the oxidation resistance of coating still needed to be improved.
We prepared the composite coating on surface of graphite matrix. The coating was reinforced by MoSi2through physical doping. Comparing the morphology and structure changes before and after the oxidation and thermal shock tests, the protection mechanism of the coating to the matrix was analyzed. The best preparation process of the composite coating was studied by uniform design experiment. The results showed that the most important parameter influence on composite coating prepared by embedding method was the holding time. According to the experimental results and conditions permissible range, we chose the test parameters were:heat temperature was1600℃, holding time was2h, and gas flow rate was150ml/min. After cyclic static air oxidation test, the coating showed better antioxidant property, and its weightlessness was lower than that of pure SiC coating, after oxidation at1400℃for8h, and the oxidation weight loss was less than4%. The introduction of MoSi2was beneficial to thermal stress adjustment between coating and matrix, and reduced the coating cracks due to thermal stress generated in the process of preparation. Because of high temperature plasticity and volume expansion, MoSi2made the density of the coating increased. However, as strengthen body, the introduction of MoSi2was not obvious for thermal shock effect at low temperature.
With H-PSO as a pioneer body, we introduced SiC whisker layer on the graphite or C/C matrix surface by dipping sintering process. The preparation of SiC whisker was simple and low cost. A SiC/Si/MoSi2coating for carbon materials was prepared by subsequent embedding technique. The thickness of the coating was about300μm. In addition, the coating combined with matrix well, and the surface was continuous and dense. Through oxidation test at1000℃or1400℃and thermal shock test at800℃, the performance of the coating was investigated. For graphite matrix coated by the SiC/Si/MoSi2coating, the oxidation pretreatment experiment was carried out in the static air at1400℃for4h before oxidation test and the sample had0.045%weight gain. Subsequent oxidation test showed that, the SiC/Si/MoSi2multi-coating had excellent anti-oxidation property, which could protect graphite materials from oxidation at1000℃in air for12h and the corresponding weight loss was below1%. Based on the surface morphology changes, oxidation pretreatment experiment and oxidation test enhanced densification of multi-coating and the coating had a certain self-healing ability. SiC whisker layer on the matrix surface could effectively regulated stress and reduced the generation of cracks. In addition, the existence of the whisker layer could effectively inhibit excess infiltration of molten Si and control the thickness of the coating. The introduction of MoSi2could effectively improve oxidation resistance of the coating. The formation of SiO2during oxidation process of MoSi2could fill the pores of the coating itself, showing the self-healing property. MoSi2had better effect compared with Mo, which could protect graphite materials from oxidation at1400℃in air for10h and the corresponding weight loss was about1%. For C/C composite, introduction of SiC whisker layer could inhibit excess infiltration of molten Si at a certain degree, and adjust thermal expansion differences between coating and matrix, but anti-oxidation property at1400℃needed to be improved. In addition, preparation of SiC/Si/MoSi2composite coating on graphite matrix could effectively improve the thermal shock resistance of the coating.
Same with H-PSO as the pioneer body, we introduced of SiC whisker layer on the graphite matrix surface by powder method, and used orthogonal test method to research the influence of preparation technology on growth of SiC whisker, with the crystalline fraction as target. The growth mechanism of SiC whisker was studied through comparing the changes of structure and morphology of the products at different temperatures. In addition, introducing SiC whisker layer by the new method, the final composite coating was formed on graphite matrix after subsequent embedding technique. By the corresponding oxidation test and thermal shock test, with the help of the test method to observe the changes of the coating morphology and phase, we got the following conclusion:The heat treatment temperature (T) was the most important factor that influenced the growth of SiC whisker, far exceeding the other factors. High temperature, higher gas flow, lower porosity and longer holding time were favorable to whisker generation. The SiC whisker was of core-shell structure with SiC phase as core and silicon oxide as the shell, growing along the direction of (111). The morphology of the whisker was uniform, distributing on the matrix surface with long straight state and larger length-diameter ratio. The existence of carbon matrix was beneficial to the growth of SiC whisker, and the growth of SiC whisker had followed defect-vapor-vapor and vapor-liquid-defect-solid mechanism. Introduction of SiC whisker layer by the new method, and then the composite coating prepared by embedding method enhanced the anti-oxidation property of the materials obviously. The coating could protect graphite materials from oxidation at1400℃in air for10h and the corresponding weight loss was below1%.
引文
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