CN116730723B - 一种Al3BC陶瓷材料及其制备方法和应用 - Google Patents

一种Al3BC陶瓷材料及其制备方法和应用 Download PDF

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CN116730723B
CN116730723B CN202310923150.9A CN202310923150A CN116730723B CN 116730723 B CN116730723 B CN 116730723B CN 202310923150 A CN202310923150 A CN 202310923150A CN 116730723 B CN116730723 B CN 116730723B
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马霞
赵永峰
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Abstract

本发明属于陶瓷材料领域，特别涉及一种Al3BC陶瓷材料及其制备方法和应用。本发明提供一种Al3BC陶瓷材料，其特征在于，基于100wt%的所述Al3BC陶瓷材料中，Al3BC含量为90wt%~98wt%，B4C含量为0wt%~1.5wt%，Al含量2wt%~10wt%。本发明同时提供了一种Al3BC陶瓷材料的制备方法：将原材料粉末混合均匀，所述原材料包括铝粉、硼质体粉末及碳质体粉末；将上述混合均匀的原材料粉末加入球磨机中，以去离子水或酒精作为球磨介质，进行湿磨处理；将湿磨处理的粉末放入干燥箱进行干燥，将干燥后的粉末进行研磨、筛分；将筛分后的粉末放入热压模具中，进行三段式热压烧结，得到Al3BC陶瓷。Al3BC陶瓷材料可应用于防弹陶瓷领域。

Description

一种Al3BC陶瓷材料及其制备方法和应用
技术领域
本发明属于陶瓷材料领域，特别涉及一种Al3BC陶瓷材料及其制备方法和应用。
背景技术
Al3BC为1985年在B4C/Al复合材料中被首次发现的一种金属间化合物，其具有较高的硬度、弹性模量及压缩强度，因此被应用于铝基复合材料的增强颗粒，并取得了优异的强化效果。然而，由于Al3BC制备上的困难，目前报道的相关文献及公开的发明专利均为低体积分数Al3BC颗粒增强铝基复合材料，尚未见Al3BC陶瓷材料及其制备方法的相关报道。
Al3BC陶瓷具有较高的硬度、弹性模量及压缩强度，是一种重要的结构材料，有望应用于防弹陶瓷等领域。同时，Al3BC是一种具有发展潜力的半导体材料，有望在热电领域取得应用。然而，目前并未有Al3BC陶瓷材料及制备方法的公开。基于此技术背景，本发明专利公开了一种Al3BC陶瓷材料及其制备方法。
发明内容
本发明提供一种Al3BC陶瓷材料，同时提供一种工艺简便、适合工业化生产的Al3BC陶瓷材料的制备方法及其应用。
根据本发明的一方面，提供一种Al3BC陶瓷材料。其特征在于，基于100wt%的所述Al3BC陶瓷材料中，Al3BC为主要相，还含有Al或B4C的一种或两种，其中Al3BC含量为90wt%~98wt%，B4C含量为0wt%~1.5wt%，Al含量2wt%~10wt%。
可选地，所述Al3BC陶瓷材料中的Al3BC由Al、硼质体及碳质体在热压烧结过程中原位反应合成。
可选地，Al3BC晶粒平均尺寸<1μm。
根据本发明的另一方面，提供一种Al3BC陶瓷材料的制备方法，所述制备方法包括以下步骤：
（1）将原材料粉末混合均匀，所述原材料包括铝粉、硼质体粉末及碳质体粉末；
（2）将上述混合均匀的原材料粉末加入球磨机中，以去离子水或酒精作为球磨介质，进行湿磨处理；
（3）将湿磨处理的粉末放入干燥箱进行干燥，将干燥后的粉末进行研磨、筛分；
（4）将筛分后的粉末放入热压模具中，进行三段式热压烧结，得到Al3BC陶瓷。
可选地，所述硼质体粉末包括B4C、硼粉的一种或两种，所述碳质体粉末包括石墨粉、炭黑的一种或两种。
可选地，基于100wt%的原料，硼质体粉末的含量为9.0wt%~13.5wt%，碳质体粉末的含量为7.9wt%~11.7wt%，其余为铝粉。
可选地，硼质体粉末平均粒径<5µm，碳质体粉末平均粒径<5µm，铝粉平均粒径<20µm。
可选地，所述步骤（2）中球磨机转速为200~400r/min，球磨时间为16~32h。
可选地，所述步骤（3）中筛分得到的粉末粒度<50µm。
可选地，所述步骤（4）中三段式热压烧结包括：第一段热压烧结温度为550~650℃，烧结时间为1~2h，烧结压力为40~100MPa；第二段热压烧结温度为700~800℃，烧结时间为2~5h，烧结压力为30~60MPa；第三段热压烧结温度为900~1000℃，烧结时间为1~3h，烧结压力为30~60MPa。
本发明同时提供一种Al3BC陶瓷材料的应用，所述Al3BC陶瓷材料应用于防弹陶瓷领域。
相对于现有技术成果，本发明有以下有益效果。
本发明所述Al3BC陶瓷材料中Al3BC含量为90wt%~98wt%，B4C含量为0wt%~1.5wt%，Al含量2wt%~10wt%，Al相在陶瓷材料中起到烧结助剂的作用，有利于填充孔隙，提高Al3BC陶瓷的致密度，同时起到粘结剂的作用，提高Al3BC陶瓷的结合强度及塑韧性，B4C可进一步提高陶瓷材料强度及硬度。
本发明所述Al3BC陶瓷材料中Al3BC颗粒由Al、硼质体及碳质体间的原位反应合成，Al3BC晶粒形貌、含量、尺寸等微观组织可调控是其优势，另外，Al3BC陶瓷颗粒原位反应合成温度较低，相较于传统陶瓷材料烧结温度大大降低，降低能源消耗的同时，保证Al3BC陶瓷晶粒间的纯净，避免晶粒间存在氧化物杂质，同时，原位自生Al3BC晶粒间原子结合，结合强度高，有利于提高其强度，Al3BC晶粒平均尺寸<1μm，晶粒细小，有利于提高陶瓷材料强度及塑性。
根据本发明所述Al3BC陶瓷的制备方法，所述硼质体粉末包括B4C、硼粉中的一种或两种，所述碳质体粉末包括石墨粉、炭黑的一种或两种，原材料选择性较广，原材料的种类对Al3BC陶瓷微观组织具有调控作用。
根据本发明所述Al3BC陶瓷的制备方法，所述硼质体粉末平均粒径<5µm，碳质体粉末平均粒径<5µm，铝粉平均粒径<20µm，较小的粉末尺寸，有利于降低Al3BC合成反应激活能，促进Al3BC原位合成。
根据本发明所述Al3BC陶瓷的制备方法，所述步骤（2）中的球磨结束后，原材料粉末间实现部分合金化，降低原材料粉末间的距离，提高原材料粉末能量，促进原材料粉末发生原位反应，最终合成Al3BC，湿磨处理可以保证降低原位反应激活能的同时，保证原材料粉末的分散性。
根据本发明所述Al3BC陶瓷的制备方法，所述步骤（3）中筛分后的的粉末粒度<50µm，较小的粉末粒度有利于烧结过程中实现陶瓷材料的致密化。
根据本发明所述Al3BC陶瓷的制备方法，所述步骤（4）中采用三段式热压烧结，三段式热压烧结工艺有益于提高Al3BC陶瓷的致密度及Al3BC的合成反应程度，获得更高强度的Al3BC陶瓷，第一段热压烧结温度低于Al3BC的合成反应温度，此时铝基体含量较高，有利于实现粉末的连接及致密化，第二段热压烧结，为Al3BC原位合成阶段，较低的反应温度保证Al3BC晶粒尺寸不致过度长大，第三段热压烧结则是提高烧结温度，进一步促进陶瓷材料的致密化。
本发明提供的Al3BC陶瓷材料具有高硬度、高弹性模量、高强度及高抗冲击等性能优势，可应用于防弹陶瓷领域，具有较优异的防弹能力。
附图说明
通过结合附图进行的详细描述，本申请的特征、优点及技术效果将被更清楚地理解，在附图中：
图1是实施例1制备的Al3BC陶瓷材料的微观组织；
图2是实施例1制备的Al3BC陶瓷材料的XRD图谱。
具体实施方式
下面将结合具体实施例及附图对本发明的技术方案进行清楚、完整的描述。
然而，本申请不应被解释为限于此阐述的具体实施例，提供这些实施例使得本申请将是彻底的和完整的。
应理解的是，当在说明书中使用术语“包括”和/或“包含”时，其列举存在所陈述的材料和/或成分，但不排除存在或添加一种或更多种其它材料和/或成分。
根据本发明专利，基于100wt%的所述Al3BC陶瓷中，Al3BC含量为90wt%~98wt%，B4C含量为0wt%~1.5wt%，Al含量2wt%~10wt%，Al3BC由Al、硼质体及碳质体在热压烧结过程中原位反应合成，晶粒平均尺寸<1μm。
图1所示为实施例1中根据本发明制备的Al3BC陶瓷的微观组织，Al3BC含量约为95wt%，Al3BC晶粒尺寸细小，该条件下晶粒尺寸<500nm，图2所示为实施例1制备的Al3BC陶瓷的XRD图谱，可以看到其主要含有Al3BC相，还含有少量Al。
根据本发明的实施例，本发明所述Al3BC陶瓷的制备方法包括以下步骤：
（1）将原材料粉末混合均匀，所述原材料包括铝粉、硼质体粉末及碳质体粉末；
优选地，所述硼质体粉末包括B4C、硼粉的一种或两种，所述碳质体粉末包括石墨粉、炭黑的一种或两种；
优选地，基于100wt%的原料，硼质体粉末的含量为9.0wt%~13.5wt%，碳质体粉末的含量为7.9wt%~11.7wt%，其余为铝粉；
优选地，硼质体粉末平均粒径<5µm，碳质体粉末平均粒径<5µm，铝粉平均粒径<20µm；
（2）将上述混合均匀的原材料粉末加入球磨机中，以去离子水或酒精作为球磨介质，进行湿磨处理；
优选地，该步骤中球磨机转速为200~400r/min，球磨时间为16~32h；
将湿磨处理的粉末放入干燥箱进行干燥，将干燥后的粉末进行研磨、筛分；
优选地，筛分得到的粉末粒度<50µm；
（4）将筛分后的粉末放入热压模具中，进行三段式热压烧结，得到Al3BC陶瓷；
优选地，三段式热压烧结包括：第一段热压烧结温度为550~650℃，烧结时间为1~2h，烧结压力为40~100MPa，第二段热压烧结温度为700~800℃，烧结时间为2~5h，烧结压力为30~60MPa；第三段热压烧结温度为900~1000℃，烧结时间为1~3h，烧结压力为30~60MPa。
以下，将描述根据本发明的实施例的Al3BC陶瓷的制备方法的具体实施例。
实施例1
（1）将以下原材料粉末混合均匀，包括12.6wt%B4C粉、8.2wt%炭黑粉，剩余为铝粉，B4C粉平均粒径为5µm，炭黑粉平均粒径为2µm，铝粉平均粒径为10µm。
（2）将上述混合均匀的原材料粉末加入球磨机中，加入去离子水作为球磨介质，进行湿磨处理，球磨机转速为300r/min，球磨时间为24h。
（3）将湿磨处理后的粉末放入干燥箱，在80℃干燥48h，研磨、筛分后得到粒度<50µm的粉末。
（4）将筛分后粉末放入热压模具中，首先升高温度至600℃，在80MPa压力下烧结2h，进一步升高温度至750℃，在40MPa压力下烧结4h，进一步升高温度至950℃，在40MPa压力下烧结2h，制备得到Al3BC陶瓷。
该工艺下制备的Al3BC陶瓷中Al3BC含量约为95wt%，Al3BC晶粒尺寸<500nm，剩余为Al。
实施例2
（1）将以下原材料粉末混合均匀，包括13.5wt%B4C粉、7.9wt%石墨粉，剩余为铝粉，B4C粉平均粒径为5µm，石墨粉平均粒径为5µm，铝粉平均粒径为20µm。
（2）将上述混合均匀的原材料粉末加入球磨机中，加入酒精作为球磨介质，进行湿磨处理，球磨机转速为200r/min，球磨时间为16h。
（3）将湿磨处理后的粉末放入干燥箱，在80℃干燥48h，研磨、筛分后得到粒度<50µm的粉末。
（4）将上述粉末放入热压模具中，首先升高温度至550℃，在40MPa压力下烧结1h，进一步升高温度至700℃，在30MPa压力下烧结2h，进一步升高温度至900℃，在30MPa压力下烧结1h，制备得到Al3BC陶瓷。
该工艺下制备的Al3BC陶瓷中Al3BC含量约为90wt%，Al3BC晶粒尺寸<500nm，含有1.5wt%B4C，剩余为Al。
实施例3
（1）将以下原材料粉末混合均匀，包括10.5wt%硼粉、11.5wt%炭黑粉，剩余为铝粉，硼粉平均粒径为5µm，炭黑粉平均粒径为2µm，铝粉平均粒径为20µm。
（2）将上述混合均匀的原材料粉末加入球磨机中，加入酒精作为球磨介质，进行湿磨处理，球磨机转速为400r/min，球磨时间为32h。
（3）将湿磨处理后的粉末放入干燥箱，在80℃干燥48h，研磨、筛分后得到粒度<50µm的粉末。
（4）将筛分后的粉末放入热压模具中，首先升高温度至650℃，在100MPa压力下烧结2h，进一步升高温度至800℃，在60MPa压力下烧结5h，进一步升高温度至1000℃，在60MPa压力下烧结3h，制备得到Al3BC陶瓷。
该工艺下制备的Al3BC陶瓷中Al3BC含量约为98wt%，Al3BC晶粒尺寸<1μm，剩余为Al。
实施例4
（1）将以下原材料粉末混合均匀，包括9.0wt%硼粉、10.8wt%石墨粉，剩余为铝粉，硼粉平均粒径为5µm，石墨粉平均粒径为5µm，铝粉平均粒径为20µm。
（2）将上述混合均匀的原材料粉末加入球磨机中，加入去离子水作为球磨介质，进行湿磨处理，球磨机转速为200r/min，球磨时间为16h。
（3）将湿磨处理的粉末放入干燥箱，在80℃干燥48h，研磨、筛分后得到粒度<50µm的粉末。
（4）将筛分后的粉末放入热压模具中，首先升高温度至600℃，在80MPa压力下烧结1h，进一步升高温度至800℃，在40MPa压力下烧结3h，进一步升高温度至900℃，在40MPa压力下烧结2h，制备得到Al3BC陶瓷。
该工艺下制备的Al3BC陶瓷中Al3BC含量约为90wt%，Al3BC晶粒尺寸<500nm，剩余为Al。
实施例5
（1）将以下原材料粉末混合均匀，包括13.5wt%B4C粉、8.6wt%石墨粉，剩余为铝粉，B4C粉平均粒径为5µm，石墨粉平均粒径为5µm，铝粉平均粒径为20µm。
（2）将上述混合均匀的原材料粉末加入球磨机中，加入去离子水作为球磨介质，进行湿磨处理，球磨机转速为400r/min，球磨时间为32h。
（3）将湿磨处理的粉末放入干燥箱，在80℃干燥48h，研磨、筛分后得到粒度<50µm的粉末。
（4）将筛分后的粉末放入热压模具中，首先升高温度至650℃，在100MPa压力下烧结2h，进一步升高温度至800℃，在60MPa压力下烧结5h，进一步升高温度至1000℃，在60MPa压力下烧结3h，制备得到Al3BC陶瓷。
该工艺下制备的Al3BC陶瓷中Al3BC含量约为98wt%，Al3BC晶粒尺寸<1μm，剩余为Al。

Claims (6)

1.一种Al3BC陶瓷材料，其特征在于，基于100wt％的所述Al3BC陶瓷材料中，Al3BC含量为90wt％～98wt％，B4C含量为0wt％～1.5wt％，Al含量2wt％～10wt％，Al3BC晶粒平均尺寸<1μm，Al3BC由Al、硼质体及碳质体在热压烧结过程中原位反应合成，所述Al3BC陶瓷材料通过以下方法制备：(1)将原材料粉末混合均匀，所述原材料包括铝粉、硼质体粉末及碳质体粉末；(2)将上述混合均匀的原材料粉末加入球磨机中，以酒精作为球磨介质进行湿磨处理；(3)将湿磨处理的粉末放入干燥箱进行干燥，将干燥后的粉末进行研磨、筛分；(4)将筛分后的粉末放入热压模具中，进行三段式热压烧结得到Al3BC陶瓷，第一段热压烧结温度为550～650℃，烧结时间为1～2h，烧结压力为40～100MPa，第二段热压烧结温度为700～800℃，烧结时间为2～5h，烧结压力为30～60MPa，第三段热压烧结温度为900～1000℃，烧结时间为1～3h，烧结压力为30～60MPa。
2.根据权利要求1所述的一种Al3BC陶瓷材料，其特征在于，所述硼质体粉末包括B4C、硼粉的一种或两种，所述碳质体粉末包括石墨粉、炭黑的一种或两种。
3.根据权利要求1所述的一种Al3BC陶瓷材料，其特征在于，基于100wt％的原料，硼质体粉末的含量为9.0wt％～13.5wt％，碳质体粉末的含量为7.9wt％～11.7wt％，其余为铝粉。
4.根据权利要求1所述的一种Al3BC陶瓷材料，其特征在于，硼质体粉末平均粒径<5μm，碳质体粉末平均粒径<5μm，铝粉平均粒径<20μm。
5.根据权利要求1所述的一种Al3BC陶瓷材料，其特征在于，球磨机转速为200～400r/min，球磨时间为16～32h。
6.一种根据权利要求1所述的Al3BC陶瓷材料的应用，其特征在于，所述Al3BC陶瓷材料应用于防弹陶瓷领域。
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