CN110790587A - 一种ZrB2-MoSi2-SiC超高温陶瓷抗氧化涂层的制备方法 - Google Patents
一种ZrB2-MoSi2-SiC超高温陶瓷抗氧化涂层的制备方法 Download PDFInfo
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Abstract
本发明公开一种ZrB2‑MoSi2‑SiC超高温陶瓷抗氧化涂层的制备方法,属于抗氧化涂层的技术领域。本发明以ZrB2、MoSi2、SiC粉末为原料,在碳基试样表面以放电等离子烧结的方式,直接制备组分和厚度可控,组织细小、均匀致密且无明显缺陷的ZrB2‑MoSi2‑SiC超高温陶瓷抗氧化涂层,通过涂层保护提高碳基材料高温抗氧化性能。本发明通过控制复合粉体配比及添加量来实现对涂层组分及厚度的控制;通过调整放电等离子烧结参数,实现对ZrB2‑MoSi2‑SiC涂层致密性及与碳基体结合强度的调控。与传统无压类烧结制备涂层的方法相比,本发明得到的抗氧化涂层组分及厚度可控、致密度高、制备时间短、工艺简单,实用价值高。
Description
技术领域
本发明涉及一种高温陶瓷抗氧化涂层的制备方法,特别是一种碳材料表面ZrB2-MoSi2-SiC超高温陶瓷抗氧化涂层的制备方法。
背景技术
碳结构材料(石墨或碳碳复合材料)有着良好的耐高温性能,在无氧条件下碳结构材料可以承受3000℃以上的高温,同时具有高导电性、高导热性,密度低,高比模量、比强度高,震动衰减率小等性能。由于其以上诸多优点,其在日常生活以及航天航空领域均有着广泛的应用。但碳结构材料的局限性在于其抗氧化性差,在400℃以上的空气中便会与氧气发生化学反应,使碳结构材料制品失效。因此,碳材料在应用中的关键点是防氧化。目前,在碳材料的表面制备抗氧化涂层是碳材料防氧化的有效途径。抗氧化涂层不仅需要有效地隔绝碳材料和氧气,还需要拥有良好的耐高温、抗氧化、高致密度等性能。而且,随着碳材料应用的日趋广泛,碳材料制品必须具备宽温域抗氧化的能力。
在诸多抗氧化涂层中,超高温陶瓷硼化物ZrB2与SiC组成的复合涂层在氧化时可以生成具有不同熔点和防护温区范围的多组分氧化产物,并形成一层可以自愈合密封缺陷且致密稳定的复合玻璃相,呈现了极大的宽温域氧化防御潜力。Kircher等在“Engineeringlimitations of MoSi2 coatings”中报道了MoSi2在作为高温氧化防护涂层时,可以在宽温域下充分保护基体。由于MoSi2相具有优异高温抗氧化能力,其作为改性相可以有效提升ZrB2-SiC涂层在超高温下的防氧化效果,因此本发明通过在ZrB2-SiC涂层中加入MoSi2相,通过多组分涂层组元在防氧化过程中的协同效应,增强涂层在宽温域下的稳定性。
目前,在碳材料表面制备ZrB2-MoSi2-SiC涂层的方法主要为包埋法、原位反应法和等离子喷涂法等。传统反应法虽然具有成本较低、简单易行、合成相均匀分布等优点,但因其涂层中ZrB2-MoSi2-SiC的含量以及涂层的厚度难以控制、涂层疏松易脱落等缺点,得不到较好的抗氧化性能。而放电等离子烧结法以其低温热压快烧的优点吸引了众多关注。用该种方法制备的涂层解决了传统工艺无法解决的问题,制备出的内层结合紧密、不易脱落,且制备周期短、使用寿命长、对基体的伤害小,最大程度保护了基体的力学性能、提高了碳材料的抗氧化性,实用性强。
发明内容
本发明提供一种于较低烧结温度下在碳基材料表面快速烧结制备ZrB2-MoSi2-SiC超高温陶瓷抗氧化涂层的方法,制备方法简单,可以实现对ZrB2-MoSi2-SiC涂层组分、厚度、致密性和与碳基体结合强度的调控,增强碳基体的抗氧化能力。
为实现上述目的,本发明采用的技术方案如下:
首先配置不同含量配比的MoSi2、SiC、ZrB2复合粉体,经过均匀混合之后,在石墨磨具中用复合粉体包裹碳基体,再经过放电等离子烧结合成涂层。
具体步骤为:
步骤1:碳基体表面处理:用不同粗糙度的砂纸打磨碳基体表面,打磨之后用酒精清洗,最后干燥;
步骤2:混料:称取一定质量分数的ZrB2、MoSi2、SiC粉体,随后通过球磨使其混合均匀得到ZrB2-MoSi2-SiC复合粉体;
步骤3:装模:用经过步骤2得到的ZrB2-MoSi2-SiC复合粉体在石墨模具内将经过步骤1处理后的碳基体充分包裹;
步骤4:放电等离子烧结:将完成上述步骤的石墨模具放入放电等离子烧结炉中烧结,烧结温度为1200-1900℃,保温时间5-300min,压力为5-50MPa,升温速率为5-200℃/min,烧结之后即可在碳基体表面得到所设计的组分和厚度可控的ZrB2-MoSi2-SiC超高温陶瓷抗氧化涂层。
有益效果及优点:
1.利用放电等离子烧结法在碳基材料表面制备的HfB2-MoSi2-SiC抗氧化涂层与碳材料基体的结合强度高,不容易剥落,抗氧化性能好。
2.利用放电等离子烧结法在碳基材料表面制备的HfB2-MoSi2-SiC抗氧化涂层致密性良好,组织细小,各相分布和涂层厚度均匀。
3.利用放电等离子烧结法在碳基材料表面制备的HfB2-MoSi2-SiC抗氧化涂层,烧结温度低、制备时间短,可以有效抑制晶粒长大,大大降低了杂质产生的几率。
4.本发明所用方法简单实用,使得碳基体的抗氧化性能大幅提高,且涂层综合性能优异,具有广阔的发展前景。
附图说明
为了更清晰地说明本申请实施方式中的技术方案,下面将对实施方式描述中所需要使用的附图作简单地介绍。
图1为本发明实施例1在石墨基体表面制备的60%ZrB2-10%MoSi2-30%SiC抗氧化涂层表面的XRD图谱。
图2为本发明实施例1在石墨基体表面制备的60%ZrB2-10%MoSi2-30%SiC抗氧化涂层表面的SEM照片。
图3为本发明实施例2在石墨基体表面制备的60%ZrB2-20%MoSi2-20%SiC抗氧化涂层表面的XRD图谱。
图4为本发明实施例2在石墨基体表面制备的60%ZrB2-20%MoSi2-20%SiC抗氧化涂层表面的SEM照片。
图5为本发明实施例3在石墨基体表面制备的60%ZrB2-30%MoSi2-10%SiC抗氧化涂层表面的XRD图谱。
图6为本发明实施例3在石墨基体表面制备的60%ZrB2-30%MoSi2-10%SiC抗氧化涂层表面的SEM照片。
图7为本发明实施例4在石墨基体表面制备的60%ZrB2-40%MoSi2抗氧化涂层表面的XRD图谱。
图8为本发明实施例4在石墨基体表面制备的60%ZrB2-40%MoSi2抗氧化涂层表面的SEM照片。
其中:1- ZrB2,2-MoSi2,3-SiC。
具体实施方式
首先配置不同含量配比的MoSi2、SiC、ZrB2复合粉体,经过均匀混合之后,在石墨磨具中用复合粉体包裹碳基体,再经过放电等离子烧结合成涂层。
具体步骤为:
步骤1:碳基体表面处理:用不同粗糙度的砂纸打磨碳基体表面,打磨之后用酒精清洗,最后干燥;
步骤2:混料:称取一定质量分数的ZrB2、MoSi2、SiC粉体,随后通过球磨使其混合均匀得到ZrB2-MoSi2-SiC复合粉体;
步骤3:装模:用经过步骤2得到的ZrB2-MoSi2-SiC复合粉体在石墨模具内将经过步骤1处理后的碳基体充分包裹;
步骤4:放电等离子烧结:将完成上述步骤的石墨模具放入放电等离子烧结炉中烧结,烧结温度为1200-1900℃,保温时间5-300min,压力为5-50MPa,升温速率为5-200℃/min,烧结之后即可在碳基体表面得到所设计的组分和厚度可控的ZrB2-MoSi2-SiC超高温陶瓷抗氧化涂层。
下面结合附图和实施例对本发明做进一步的详细描述。
实施例1:
步骤1:碳基体表面处理:用不同粗糙度的砂纸打磨石墨基体表面,打磨之后用酒精清洗,最后干燥;
步骤2:混料:分别称取质量分数的60%ZrB2、10%MoSi2、30%SiC粉体,其粒度≤50μm,纯度≥99.0%,随后以100r/min的转速球磨5h均匀混合,最后得到60%ZrB2-10%MoSi2-30%SiC复合粉体;
步骤3:装模:用经过步骤2得到的60%ZrB2-10%MoSi2-30%SiC复合粉体在石墨模具内将经过步骤1处理后的石墨基体充分包裹;
步骤4:放电等离子烧结:将完成上述步骤的石墨模具放入放电等离子烧结炉中烧结,烧结参数为:在575℃烧结1s,迅速升温至600℃后保温2min,在5min内升温至1500℃后保温5min,升温速率为180℃/min ,压力为30MPa,烧结时间为12min。烧结之后即可在石墨基体表面得到60%ZrB2-10%MoSi2-30%SiC超高温陶瓷抗氧化涂层。
其物相分析如图1所示,其表面形貌如图2所示。
实施例2:
步骤1:碳基体表面处理:用不同粗糙度的砂纸打磨石墨基体表面,打磨之后用酒精清洗,最后干燥;
步骤2:混料:分别称取质量分数的60%ZrB2、20%MoSi2、20%SiC粉体,其粒度≤50μm,纯度≥99.0%,随后以200r/min的转速球磨2.5h均匀混合,最后得到60%ZrB2-20%MoSi2-20%SiC复合粉体;
步骤3:装模:用经过步骤2得到的60%ZrB2-20%MoSi2-20%SiC复合粉体在石墨模具内将经过步骤1处理后的石墨基体充分包裹;
步骤4:放电等离子烧结:将完成上述步骤的石墨模具放入放电等离子烧结炉中烧结,烧结参数为:在575℃烧结1s,迅速升温至700℃后保温1min,在6min内升温至1600℃后保温6min,升温速率为200℃/min ,压力为40MPa,烧结时间为13min。烧结之后即可在石墨基体表面得到60%ZrB2-20%MoSi2-20%SiC超高温陶瓷抗氧化涂层。
其物相分析如图3所示,其表面形貌如图4所示。
实施例3:
步骤1:碳基体表面处理:用不同粗糙度的砂纸打磨石墨基体表面,打磨之后用酒精清洗,最后干燥;
步骤2:混料:分别称取质量分数的60%ZrB2、30%MoSi2、10%SiC粉体,其粒度≤50μm,纯度≥99.0%,随后以1000r/min的转速球磨1h均匀混合,最后得到60%ZrB2-30%MoSi2-10%SiC复合粉体;
步骤3:装模:用经过步骤2得到的60%ZrB2-30%MoSi2-10%SiC复合粉体在石墨模具内将经过步骤1处理后的石墨基体充分包裹;
步骤4:放电等离子烧结:将完成上述步骤的石墨模具放入放电等离子烧结炉中烧结,烧结参数为:在575℃烧结1s,迅速升温至1000℃后保温3min,在8min内升温至1800℃后保温10min,升温速率为100℃/min ,压力为50MPa,烧结时间为21min。烧结之后即可在石墨基体表面得到60%ZrB2-30%MoSi2-10%SiC超高温陶瓷抗氧化涂层。
其物相分析如图5所示,其表面形貌如图6所示。
实施例4:
步骤1:碳基体表面处理:用不同粗糙度的砂纸打磨石墨基体表面,打磨之后用酒精清洗,最后干燥;
步骤2:混料:分别称取质量分数的60%ZrB2、40%MoSi2粉体,其粒度≤50μm,纯度≥99.0%,随后以500r/min的转速球磨5h均匀混合,最后得到60%ZrB2-40%MoSi2复合粉体;
步骤3:装模:用经过步骤2得到的60%ZrB2-40%MoSi2复合粉体在石墨模具内将经过步骤1处理后的石墨基体充分包裹;
步骤4:放电等离子烧结:将完成上述步骤的石墨模具放入放电等离子烧结炉中烧结,烧结参数为:在575℃烧结1s,迅速升温至650℃后保温2min,在5min内升温至1650℃后保温7min,升温速率为200℃/min ,压力为45MPa,烧结时间为14min。烧结之后即可在石墨基体表面得到60%ZrB2-40%MoSi2超高温陶瓷抗氧化涂层。
其物相分析如图7所示,其表面形貌如图8所示。
以上所述,仅为本发明的较好实施例,因此本发明实施的范围不能依据以上实施例进行限定,依据本发明专利范围和说明书内容进行的等效修饰与变化,依然为本发明涵盖的范围。
Claims (6)
1.一种ZrB2-MoSi2-SiC超高温陶瓷抗氧化涂层的制备方法,其特征在于:首先配置不同含量配比的ZrB2-MoSi2-SiC复合粉体,经过均匀混合之后,在石墨模具中用复合粉体包裹碳基体,经过放电等离子烧结合成超高温陶瓷抗氧化涂层。
2.根据权利要求1所述的ZrB2-MoSi2-SiC超高温陶瓷抗氧化涂层的制备方法,其特征在于具体步骤为:
步骤1:碳基体表面处理:用不同粗糙度的砂纸打磨碳基体表面,打磨之后用酒精清洗,最后干燥;
步骤2:混料:称取一定质量分数的ZrB2、MoSi2、SiC粉体,随后通过球磨使其混合均匀得到ZrB2-MoSi2-SiC复合粉体;
步骤3:装模:用经过步骤2得到的ZrB2-MoSi2-SiC复合粉体在石墨模具内将经过步骤1处理后的碳基体充分包裹;
步骤4:放电等离子烧结:将完成上述步骤的石墨模具放入放电等离子烧结炉中烧结,烧结温度为1300-1900℃,保温时间2-300min,压力为2-50MPa,升温速率为10-200℃/min,烧结之后即可在碳基体表面得到所设计的组分和厚度可控的ZrB2-MoSi2-SiC超高温陶瓷抗氧化涂层。
3.根据权利要求2所述的ZrB2-MoSi2-SiC超高温陶瓷抗氧化涂层的制备方法,其特征在于:所述的碳基体为碳碳复合材料或石墨。
4.根据权利要求2所述的ZrB2-MoSi2-SiC超高温陶瓷抗氧化涂层的制备方法,其特征在于:在上述步骤2中,ZrB2-MoSi2-SiC复合粉体中ZrB2的质量分数为5%-95%,MoSi2的质量分数为5%-95%,SiC的质量分数为5%-95%,球磨机转速为50-1000r/min,球磨时间为0.5-10h。
5.根据权利要求2所述的ZrB2-MoSi2-SiC超高温陶瓷抗氧化涂层的制备方法,其特征在于:在上述步骤2所述ZrB2、MoSi2、SiC粉体的粒度≤60μm,纯度≥99.0%。
6.根据权利要求2所述的ZrB2-MoSi2-SiC超高温陶瓷抗氧化涂层的制备方法,其特征在于:在上述步骤4中,碳基体表面得到的ZrB2-MoSi2-SiC涂层的厚度为10μm~3mm。
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