CN113087540A - 一种在碳纤维预制体表面制备氮化硅涂层的方法 - Google Patents
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Abstract
本发明公开了一种在碳纤维预制体表面制备氮化硅涂层的方法,该方法包括:一、制备碳纤维预制体并进行热处理;二、再次热处理;三、碳纤维预制体增密;四、制备悬浮液;五、喷涂或刷涂悬浮液;六、烧结制备表面具有氮化硅涂层的碳纤维预制体。本发明采用高温炉对碳纤维预制体进行两次热处理,能够有效去除碳纤维预制体中的灰分;采用化学气相渗透和树脂液相致密工艺对碳纤维预制体进行增密,缩短了制造周期,有效降低了生产成本;采用喷涂或刷涂含有氮化硅粉和氮化硼粉的酚醛树脂胶液,经烧结后在碳纤维预制体表面形成掺杂有硼的氮化硅涂层,涂层结合牢固,可以有效抑制含硅蒸气对材料表面的侵蚀,大幅提高使用寿命。
Description
技术领域
本发明属于碳纤维复合材料涂层制备技术领域,具体涉及一种在碳纤维预制体表面制备氮化硅涂层的方法。
背景技术
炭材料坩埚在使用过程中,硅蒸气及含硅气体均可与炭材料发生化学反应,导致炭材料坩埚被侵蚀,直至失效,因此,如何有效抑制炭材料的侵蚀是提高炭材料坩埚使用寿命的关键。碳氮化硅材料具有超高硬度、低热膨胀系数、抗氧化、耐腐蚀等优异性能,有望应用于航空、航天和石化等领域的极端环境中。但目前制备SiCN材料的主要方法是聚合物前驱体裂解法和气相沉积法,工艺复杂且成本高。
发明内容
本发明所要解决的技术问题在于针对上述现有技术的不足,提供一种在碳纤维预制体表面制备氮化硅涂层的方法。该方法采用喷涂或刷涂含有氮化硅粉和氮化硼粉的酚醛树脂胶液,经烧结后在碳纤维预制体表面形成掺杂有硼晶须的氮化硅涂层,涂层结合牢固,可以有效抑制含硅蒸气对材料表面的侵蚀,大幅提高使用寿命。
为解决上述技术问题,本发明采用的技术方案是:一种在碳纤维预制体表面制备氮化硅涂层的方法,其特征在于,该方法包括以下步骤:
步骤一、将连续碳纤维制成碳纤维预制体,将制备的碳纤维预制体置于高温炉中,在惰性气体保护下,温度为2300℃~2400℃的条件下热处理1h~3h,然后随炉冷却;
步骤二、将步骤一中冷却后的碳纤维预制体置于高温炉中,在惰性气体保护下,温度为2000℃~2200℃的条件下热处理1h~3h,然后随炉冷却;
步骤三、将步骤二中冷却后的碳纤维预制体增密至密度为1.2g/cm3~1.5g/cm3;
步骤四、将氮化硅粉和氮化硼粉加入酚醛树脂胶液中,混合均匀,得到悬浮液;
步骤五、将步骤四中所述悬浮液喷涂或刷涂于步骤三中增密后的碳纤维预制体表面形成涂层,晾干后置于烘箱中固化;
步骤六、将步骤五中固化后的碳纤维预制体置于高温炉内,在氮气或惰性气体保护下烧结,随炉冷却得到表面具有氮化硅涂层的碳纤维预制体;所述烧结的过程为:在升温速率为5℃/h~100℃/h的条件下升温至900℃~1500℃,保温2h~6h,然后在升温速率为50℃/h~200℃/h的条件下升温至2000℃~2500℃,保温2h~6h。
上述的一种在碳纤维预制体表面制备氮化硅涂层的方法,其特征在于,步骤三中所述增密的方法为:采用碳源气体对炭纤维预制体进行化学气相渗透;然后将经化学气相渗透后的炭纤维预制体用酚醛树脂进行压力浸渍后置于炭化炉中炭化。
上述的一种在碳纤维预制体表面制备氮化硅涂层的方法,其特征在于,所述碳源气体为丙烯或天然气,碳源气体流量为50L/min~200L/min,化学气相渗透的温度为900℃~1100℃,保温时间为30h~60h。
上述的一种在碳纤维预制体表面制备氮化硅涂层的方法,其特征在于,所述压力浸渍的压力为1.0MPa~2.5MPa,保压时间为0.5h~5h。
上述的一种在碳纤维预制体表面制备氮化硅涂层的方法,其特征在于,所述炭化的温度为900℃~1000℃,保温时间为2h~5h。
上述的一种在碳纤维预制体表面制备氮化硅涂层的方法,其特征在于,步骤四中所述氮化硅粉、氮化硼粉和酚醛树脂胶液的质量比为2:1:10。
上述的一种在碳纤维预制体表面制备氮化硅涂层的方法,其特征在于,步骤五中所述固化的温度为200℃~300℃,时间为1h~2h。
上述的一种在碳纤维预制体表面制备氮化硅涂层的方法,其特征在于,步骤六中所述烧结的过程为:在升温速率为20℃/h的条件下升温至1200℃,保温4h,然后在升温速率为100℃/h的条件下升温至2300℃,保温4h。
本发明与现有技术相比具有以下优点:
1、本发明采用高温炉对碳纤维预制体进行两次热处理,能够有效去除碳纤维预制体中的灰分,处理后的碳纤维预制体中灰分的质量含量不高于0.05%。
2、本发明采用化学气相渗透和树脂液相致密工艺对碳纤维预制体进行增密,缩短了制造周期,有效降低了生产成本。
3、本发明采用喷涂或刷涂含有氮化硅粉和氮化硼粉的酚醛树脂胶液,经烧结后在碳纤维预制体表面形成掺杂有硼的氮化硅涂层,涂层结合牢固,可以有效抑制含硅蒸气对材料表面的侵蚀,大幅提高使用寿命。
下面通过实施例,对本发明的技术方案做进一步的详细描述。
具体实施方式
实施例1
步骤一、将连续碳纤维制成碳纤维预制体,将制备的碳纤维预制体置于高温炉中,在惰性气体保护下,温度为2300℃的条件下热处理3h,然后随炉冷却;
步骤二、将步骤一中冷却后的碳纤维预制体置于高温炉中,在惰性气体保护下,温度为2000℃的条件下热处理3h,然后随炉冷却;
步骤三、将步骤二中冷却后的碳纤维预制体增密至密度为1.2g/cm3;增密方法为:采用碳源气体对炭纤维预制体进行化学气相渗透;然后将经化学气相渗透后的炭纤维预制体用酚醛树脂进行压力浸渍后置于炭化炉中炭化;所述碳源气体为丙烯或天然气,碳源气体流量为50L/min,化学气相渗透的温度为900℃,保温时间为60h;所述压力浸渍的压力为1.0MPa,保压时间为0.5h;所述炭化的温度为900℃,保温时间为5h;
步骤四、将氮化硅粉和氮化硼粉加入酚醛树脂胶液中,混合均匀,得到悬浮液;所述氮化硅粉、氮化硼粉和酚醛树脂胶液的质量比为2:1:10;
步骤五、将步骤四中所述悬浮液喷涂或刷涂于步骤三中增密后的碳纤维预制体表面形成涂层,晾干后置于烘箱中固化;所述固化的温度为200℃,时间为2h;
步骤六、将步骤五中固化后的碳纤维预制体置于高温炉内,在氮气或惰性气体保护下烧结,随炉冷却得到表面具有氮化硅涂层的碳纤维预制体;所述烧结的过程为:在升温速率为5℃/h的条件下升温至900℃,保温6h,然后在升温速率为50℃/h的条件下升温至2000℃,保温6h。
实施例2
步骤一、将连续碳纤维制成碳纤维预制体,将制备的碳纤维预制体置于高温炉中,在惰性气体保护下,温度为2400℃的条件下热处理1h,然后随炉冷却;
步骤二、将步骤一中冷却后的碳纤维预制体置于高温炉中,在惰性气体保护下,温度为2200℃的条件下热处理1h,然后随炉冷却;
步骤三、将步骤二中冷却后的碳纤维预制体增密至密度为1.5g/cm3;增密方法为:采用碳源气体对炭纤维预制体进行化学气相渗透;然后将经化学气相渗透后的炭纤维预制体用酚醛树脂进行压力浸渍后置于炭化炉中炭化;所述碳源气体为丙烯或天然气,碳源气体流量为200L/min,化学气相渗透的温度为1100℃,保温时间为30h;所述压力浸渍的压力为2.5MPa,保压时间为5h;所述炭化的温度为1000℃,保温时间为2h;
步骤四、将氮化硅粉和氮化硼粉加入酚醛树脂胶液中,混合均匀,得到悬浮液;所述氮化硅粉、氮化硼粉和酚醛树脂胶液的质量比为2:1:10;
步骤五、将步骤四中所述悬浮液喷涂或刷涂于步骤三中增密后的碳纤维预制体表面形成涂层,晾干后置于烘箱中固化;所述固化的温度为300℃,时间为1h;
步骤六、将步骤五中固化后的碳纤维预制体置于高温炉内,在氮气或惰性气体保护下烧结,随炉冷却得到表面具有氮化硅涂层的碳纤维预制体;所述烧结的过程为:在升温速率为100℃/h的条件下升温至1500℃,保温2h,然后在升温速率为200℃/h的条件下升温至2500℃,保温2h。
实施例3
步骤一、将连续碳纤维制成碳纤维预制体,将制备的碳纤维预制体置于高温炉中,在惰性气体保护下,温度为2350℃的条件下热处理2h,然后随炉冷却;
步骤二、将步骤一中冷却后的碳纤维预制体置于高温炉中,在惰性气体保护下,温度为2100℃的条件下热处理2h,然后随炉冷却;
步骤三、将步骤二中冷却后的碳纤维预制体增密至密度为1.4g/cm3;增密方法为:采用碳源气体对炭纤维预制体进行化学气相渗透;然后将经化学气相渗透后的炭纤维预制体用酚醛树脂进行压力浸渍后置于炭化炉中炭化;所述碳源气体为丙烯或天然气,碳源气体流量为100L/min,化学气相渗透的温度为1000℃,保温时间为40h;所述压力浸渍的压力为2.0MPa,保压时间为2h;所述炭化的温度为1050℃,保温时间为3h;
步骤四、将氮化硅粉和氮化硼粉加入酚醛树脂胶液中,混合均匀,得到悬浮液;所述氮化硅粉、氮化硼粉和酚醛树脂胶液的质量比为2:1:10;
步骤五、将步骤四中所述悬浮液喷涂或刷涂于步骤三中增密后的碳纤维预制体表面形成涂层,晾干后置于烘箱中固化;所述固化的温度为250℃,时间为1.5h;
步骤六、将步骤五中固化后的碳纤维预制体置于高温炉内,在氮气或惰性气体保护下烧结,随炉冷却得到表面具有氮化硅涂层的碳纤维预制体;所述烧结的过程为:在升温速率为20℃/h的条件下升温至1200℃,保温4h,然后在升温速率为100℃/h的条件下升温至2300℃,保温4h。
以上所述,仅是本发明的较佳实施例,并非对本发明做任何限制,凡是根据发明技术实质对以上实施例所作的任何简单修改、变更以及等效结构变化,均仍属于本发明技术方案的保护范围内。
Claims (8)
1.一种在碳纤维预制体表面制备氮化硅涂层的方法,其特征在于,该方法包括以下步骤:
步骤一、将连续碳纤维制成碳纤维预制体,将制备的碳纤维预制体置于高温炉中,在惰性气体保护下,温度为2300℃~2400℃的条件下热处理1h~3h,然后随炉冷却;
步骤二、将步骤一中冷却后的碳纤维预制体置于高温炉中,在惰性气体保护下,温度为2000℃~2200℃的条件下热处理1h~3h,然后随炉冷却;
步骤三、将步骤二中冷却后的碳纤维预制体增密至密度为1.2g/cm3~1.5g/cm3;
步骤四、将氮化硅粉和氮化硼粉加入酚醛树脂胶液中,混合均匀,得到悬浮液;
步骤五、将步骤四中所述悬浮液喷涂或刷涂于步骤三中增密后的碳纤维预制体表面形成涂层,晾干后置于烘箱中固化;
步骤六、将步骤五中固化后的碳纤维预制体置于高温炉内,在氮气或惰性气体保护下烧结,随炉冷却得到表面具有氮化硅涂层的碳纤维预制体;所述烧结的过程为:在升温速率为5℃/h~100℃/h的条件下升温至900℃~1500℃,保温2h~6h,然后在升温速率为50℃/h~200℃/h的条件下升温至2000℃~2500℃,保温2h~6h。
2.根据权利要求1所述的一种在碳纤维预制体表面制备氮化硅涂层的方法,其特征在于,步骤三中所述增密的方法为:采用碳源气体对炭纤维预制体进行化学气相渗透;然后将经化学气相渗透后的炭纤维预制体用酚醛树脂进行压力浸渍后置于炭化炉中炭化。
3.根据权利要求2所述的一种在碳纤维预制体表面制备氮化硅涂层的方法,其特征在于,所述碳源气体为丙烯或天然气,碳源气体流量为50L/min~200L/min,化学气相渗透的温度为900℃~1100℃,保温时间为30h~60h。
4.根据权利要求2所述的一种在碳纤维预制体表面制备氮化硅涂层的方法,其特征在于,所述压力浸渍的压力为1.0MPa~2.5MPa,保压时间为0.5h~5h。
5.根据权利要求2所述的一种在碳纤维预制体表面制备氮化硅涂层的方法,其特征在于,所述炭化的温度为900℃~1000℃,保温时间为2h~5h。
6.根据权利要求1所述的一种在碳纤维预制体表面制备氮化硅涂层的方法,其特征在于,步骤四中所述氮化硅粉、氮化硼粉和酚醛树脂胶液的质量比为2:1:10。
7.根据权利要求1所述的一种在碳纤维预制体表面制备氮化硅涂层的方法,其特征在于,步骤五中所述固化的温度为200℃~300℃,时间为1h~2h。
8.根据权利要求1所述的一种在碳纤维预制体表面制备氮化硅涂层的方法,其特征在于,步骤六中所述烧结的过程为:在升温速率为20℃/h的条件下升温至1200℃,保温4h,然后在升温速率为100℃/h的条件下升温至2300℃,保温4h。
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