CN105565816A - 一种MoSi2/MoB/SiC三相陶瓷的制备方法 - Google Patents

一种MoSi2/MoB/SiC三相陶瓷的制备方法 Download PDF

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CN105565816A
CN105565816A CN201510913910.3A CN201510913910A CN105565816A CN 105565816 A CN105565816 A CN 105565816A CN 201510913910 A CN201510913910 A CN 201510913910A CN 105565816 A CN105565816 A CN 105565816A
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张小立
徐坚
杨亚伟
孙斌
范积伟
樊平
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Zhongyuan University of Technology
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Abstract

本发明公开了一种MoSi2/MoB/SiC三相陶瓷的制备方法，它的步骤如下：（1）首先，将MoSi2、SiC、C及B4C元素粉球磨混料，混合时间为8-72hr，并模压成型，得到坯料；（2）将坯料室温晾干，然后入烘箱烘干1-200hr，得到烘干后的坯料；（3）将烘干后的坯料移入铺有金属Si粉的真空烧结炉中，冷却后获得MoSi2/MoB/SiC三相陶瓷。本发明利用MoSi2、SiC、C及B4C混合元素粉模压成型，所得材料孔隙率低于10%或以下，强度大于200MPa。该方法补充了现有高温抗氧化强度材料品种，适合工业规模。

Description

一种MoSi2/MoB/SiC三相陶瓷的制备方法
技术领域
本发明涉及MoSi2/MoB/SiC三相陶瓷的制备技术，属于新型强度陶瓷的低成本制备技术领域。
背景技术
选择航空用高温结构材料的三个最主要的参数是物质的熔点、比重以及高温抗氧化性能。高温陶瓷广泛应用于航空、航天、冶金及交通领域。从高温材料来看，目前工作在1000℃以下的高温抗氧化材料主要有镍基、钴基超合金。钛及钛铝中间化物以其比重小，在空间机械有广阔应用前景，但进一步研究发现，这类材料的使用温度与Ni基合金相比并无明显提高，工作温度为600-1000°C。碳复合材料可达2500°C，但抗氧化能力太差，只能用于火箭、导弹，且其制造成本十分昂贵由于金属间化合物MoSi2，具有高熔点(2030°C)、适中的密度(6.24×103kg/m3)、良好的导热性和导电性以及在所有金属硅化物中具有优良的高温抗氧化能力而成为最有希望满足这种要求的材料。SiC具有很高的高温强度和抗氧化能力，而且与MoSi2具有良好的化学相容性及热力学稳定性，因而SiC增强MoSi2复合材料的强韧性可以得到较大程度的改善。因而该复合材料具有较高的强韧性，尤其MoSi2/SiC复合陶瓷，拥有更高的使用温度和更好的抗氧化性能，质轻而力学性能好。由于MoB具有硬度高、耐蚀性能好、比碳化物陶瓷拥有更高的抗氧化性能、耐高温、突出的高温强度等特性，主要用作高温轴承、内燃机喷嘴、各种高温器件、处理熔融非铁金属器件。MoSi2/MoB/SiC三相陶瓷将有更广阔的高温氧化环境应用价值。
发明内容
本发明的目的在于利用真空反应熔渗烧结技术制备MoSi2/MoB/SiC三相陶瓷，补充现有高温二硅化钼复合材料的新的物相组成。该三相陶瓷中MoB和SiC均原位生成。该发明利用MoSi2、C、SiC及B4C元素粉模压成型，真空反应熔渗Si进行烧结。
本发明的技术方案是：一种MoSi2/MoB/SiC三相陶瓷的制备方法，它的步骤如下：
（1）首先，将MoSi2、SiC、C及B4C元素粉球磨混料，所述MoSi2、SiC、C及B4C的重量比为50-95：1-30：1-10：0.1-30，混合时间为8-72hr，再加入MoSi2、SiC、C及B4C元素粉总重量1-20%的酚醛树脂，并模压成型，得到坯料；
（2）将坯料室温晾干，然后入烘箱烘干1-200hr，得到烘干后的坯料；
（3）将烘干后的坯料移入铺有金属Si粉的真空烧结炉中，所述金属Si粉的重量为MoSi2、SiC、C及B4C元素粉总重量的2-30%，保持真空度在10-1-10-3Pa，升温速率为1-15℃/min，最后，在1200-1480℃保温10-60min，并降低真空度0-10-1Pa保持；升温至1500-1650℃保温10-60min，并降低真空度0-10-1Pa保持；升温至1650-1700℃保温10-40min，提高真空度≤10-2Pa保持，冷却后获得MoSi2/MoB/SiC三相陶瓷。
所述步骤（1）中MoSi2、SiC、C及B4C的重量比为70-80：5-10：3-8：2-8。
本发明的有益效果是：本发明利用MoSi2、SiC、C及B4C混合元素粉模压成型，通过调整真空度或气氛并原位反应熔渗Si进行烧结，获得MoSi2/MoB/SiC三相陶瓷，所得材料孔隙率低于10%或以下，强度大于200MPa。该方法补充了现有高温抗氧化强度材料品种，适合工业规模。
具体实施方式
一种MoSi2/MoB/SiC三相陶瓷的制备方法具体方法如下：
（1）、将MoSi2、SiC、C及B4C元素粉球磨混料，加入酚醛树脂，并模压成型；
（2）、将以上坯料室温晾干，然后入烘箱烘干；
（3）、将以上坯料移入铺有金属Si粉的真空烧结炉中。保持真空度在10-1-10-3Pa左右。升温速率为1-10℃/min。然后在1400-1480℃保温10-60min，并降低真空度保持；升温至1500-1550℃保温20-60min，并降低真空度保持；升温至1550-1700℃保温5-40min，提高真空度保持。冷却后获得MoSi2/MoB/SiC三相陶瓷。
实施例1
分别按比例称量MoSi2、SiC、C、B4C粉末180g、3g、6g、10g，均匀混合后球磨48hr，将以上粉料加入22g的酚醛树脂后混合并模压成型，空气中晾干后在110度烘箱中烘干，移至铺有15g金属硅粉的真空烧结炉中进行烧结，升温速度为5℃/min，真空度为10-3Pa，升温至1400-1450℃，降低真空度为10-1Pa，保温30min；升温至1550℃，保温30min，真空度为10-1Pa，升温至1650℃，保温10min，真空度为10-3Pa，然后随炉冷却，降温取料，测得MoSi2/MoB/SiC三相陶瓷孔隙率为10%，强度为200MPa。
实施例2
分别按比例称量MoSi2、SiC、C、B4C粉末170g、5g、7.5g、10g，均匀混合后球磨48hr，将以上粉料加入21g的酚醛树脂后混合并模压成型，空气中晾干后在100度烘箱中烘干，移至铺有13g金属硅粉的真空烧结炉中进行烧结，升温速度为10℃/min，真空度为10-3Pa，升温至1400-1450℃，降低真空度为10-1Pa，保温25min；升温至1550℃，保温30min，真空度为10-1Pa，升温至1650℃，保温10min，真空度为10-3Pa，然后随炉冷却，降温取料，测得MoSi2/MoB/SiC三相陶瓷孔隙率为7%，强度为210MPa。
实施例3
分别按比例称量MoSi2、SiC、C、B4C粉末190g、2g、2.5g、10g，均匀混合后球磨48hr，将以上粉料加入14%的酚醛树脂后混合并模压成型，空气中晾干后在100度烘箱中烘干，移至铺有13g金属硅粉的真空烧结炉中进行烧结，升温速度为3℃/min，真空度为10-3Pa，升温至1410-1450℃，降低真空度为10-1Pa，保温30min；升温至1550℃，保温30min，真空度为10-1Pa，升温至1700℃，保温10min，真空度为10-3Pa，然后随炉冷却，降温取料，测得MoSi2/MoB/SiC三相陶瓷孔隙率为4%，强度为205MPa。
实施例4
一种MoSi2/MoB/SiC三相陶瓷的制备方法，它的步骤如下：
（1）首先，将MoSi2、SiC、C及B4C元素粉球磨混料，所述MoSi2、SiC、C及B4C的重量比为50：1：1：0.1，混合时间为8hr，再加入MoSi2、SiC、C及B4C元素粉总重量1%的酚醛树脂，并模压成型，得到坯料；
（2）将坯料室温晾干，然后入烘箱烘干1hr，得到烘干后的坯料；
（3）将烘干后的坯料移入铺有金属Si粉的真空烧结炉中，所述金属Si粉的重量为MoSi2、SiC、C及B4C元素粉总重量的2%，保持真空度在10-1Pa，升温速率为1℃/min，最后，在1200℃保温10min，并降低真空度0-10-1Pa保持；升温至1500℃保温10min，并降低真空度0-10-1Pa保持；升温至1650℃保温10min，提高真空度≤10-2Pa保持，冷却后获得MoSi2/MoB/SiC三相陶瓷。
实施例5
一种MoSi2/MoB/SiC三相陶瓷的制备方法，它的步骤如下：
（1）首先，将MoSi2、SiC、C及B4C元素粉球磨混料，所述MoSi2、SiC、C及B4C的重量比为95：30：10：30，混合时间为72hr，再加入MoSi2、SiC、C及B4C元素粉总重量20%的酚醛树脂，并模压成型，得到坯料；
（2）将坯料室温晾干，然后入烘箱烘干200hr，得到烘干后的坯料；
（3）将烘干后的坯料移入铺有金属Si粉的真空烧结炉中，所述金属Si粉的重量为MoSi2、SiC、C及B4C元素粉总重量的30%，保持真空度在10-3Pa，升温速率为15℃/min，最后，在1480℃保温60min，并降低真空度10-1Pa保持；升温至1650℃保温60min，并降低真空度10-1Pa保持；升温至1700℃保温40min，提高真空度≤10-2Pa保持，冷却后获得MoSi2/MoB/SiC三相陶瓷。

Claims (2)

1.一种MoSi2/MoB/SiC三相陶瓷的制备方法，其特征在于，它的步骤如下：
（1）首先，将MoSi2、SiC、C及B4C元素粉球磨混料，所述MoSi2、SiC、C及B4C的重量比为50-95：1-30：1-10：0.1-30，混合时间为8-72hr，再加入MoSi2、SiC、C及B4C元素粉总重量1-20%的酚醛树脂，并模压成型，得到坯料；
（2）将坯料室温晾干，然后入烘箱烘干1-200hr，得到烘干后的坯料；
（3）将烘干后的坯料移入铺有金属Si粉的真空烧结炉中，所述金属Si粉的重量为MoSi2、SiC、C及B4C元素粉总重量的2-30%，保持真空度在10-1-10-3Pa，升温速率为1-15℃/min，最后，在1200-1480℃保温10-60min，并降低真空度0-10-1Pa保持；升温至1500-1650℃保温10-60min，并降低真空度0-10-1Pa保持；升温至1650-1700℃保温10-40min，提高真空度≤10-2Pa保持，冷却后获得MoSi2/MoB/SiC三相陶瓷。
2.根据权利要求1所述的MoSi2/MoB/SiC三相陶瓷的制备方法，其特征在于：所述步骤（1）中MoSi2、SiC、C及B4C的重量比为70-80：5-10：3-8：2-8。
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CN106278280A (zh) * 2016-08-09 2017-01-04 中原工学院 一种抵抗pest的复合陶瓷的制备方法
CN110590373A (zh) * 2019-10-28 2019-12-20 中原工学院 一种Flashing法制备MoSi2-MoB-SiC三相复合材料的方法
CN110590374A (zh) * 2019-10-28 2019-12-20 中原工学院 一种Flashing法制备MoSi2-SiC复合材料的方法

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CN102515770A (zh) * 2011-11-25 2012-06-27 中原工学院 一种制备纳米SiC增强MoSi2复合材料的方法
CN104451319A (zh) * 2014-11-20 2015-03-25 中原工学院 反应熔渗法制备Mo(Si,Al)2-SiC金属陶瓷复合材料的方法

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CN106278280B (zh) * 2016-08-09 2019-05-17 中原工学院 一种抵抗pest的复合陶瓷的制备方法
CN110590373A (zh) * 2019-10-28 2019-12-20 中原工学院 一种Flashing法制备MoSi2-MoB-SiC三相复合材料的方法
CN110590374A (zh) * 2019-10-28 2019-12-20 中原工学院 一种Flashing法制备MoSi2-SiC复合材料的方法

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