CN108383527A - 一种石墨烯/碳化硼陶瓷复合材料的制备方法 - Google Patents
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Abstract
本发明提供一种石墨烯/碳化硼陶瓷复合材料的制备方法及根据该方法所制备的产品，制备步骤包括：将膨胀石墨粉末在超声下预处理，得到片状石墨烯悬浮液，而后与碳化硼粉末、成形剂混合研磨，然后进行喷雾造粒，得到粉料；在真空或氩气环境下采用双温热压工艺进行烧结，获得石墨烯/碳化硼陶瓷复合材料。本发明提出的热压工艺可降低碳化硼陶瓷的长时间加热温度、得到晶界完整、晶粒细小的组织，这种材料具有优异的力学性能，可用于防弹板或耐磨器件。本发明工艺能有效提高片状石墨烯在碳化硼中分散均匀性，且容易进行工业放大，适合于规模生产。
Description
技术领域
本发明属于无机非金属材料领域，涉及碳化硼陶瓷材料的制备工艺，尤其是一种石墨烯/碳化硼陶瓷复合材料的制备方法。
背景技术
碳化硼陶瓷材料具有高强、高硬、抗高温磨损性好、密度小、极好的弹道性能等诸多优点，能在提供防弹保护的同时降低防护器具本身的重量，是防弹背心及飞机座舱等高端防护装置的优选材料。但是，碳化硼陶瓷材料的烧结非常困难，需要在2300℃以上烧结才能获得较为致密的材料，并且其断裂脆性通常只有不超过2.5MPam1/2，制备成本高昂，防多发弹能力差，限制了其更为广泛的应用。为此，人们提出了许多增韧的方法，如长纤维增韧、晶须增韧、颗粒弥散增韧等，这些增韧方法有的工艺复杂，难以规模化生产，有的增韧效果有限，不能根本上解决碳化硼陶瓷材料的脆性问题。
石墨烯是目前已知强度最高的材料，其理想强度为110~130GPa，是各种复合材料的理想增强体。但是，石墨烯容易团聚，在陶瓷基体中往往会分散不均，难以达到预想的强韧化效果。
发明内容
本发明提供了高效率制备石墨烯/碳化硼陶瓷复合材料的方法，以解决石墨烯原料成本较高、分散困难的问题，以及碳化硼陶瓷的致密化烧结问题。本发明提出的双温快速热压工艺可明显降低长时间加热温度，石墨烯均匀分散于碳化硼，晶界组织完整、致密，从而得到性能优良的石墨烯/碳化硼陶瓷复合材料，并将这种材料应用于防弹装甲或耐磨器件。
本发明的技术方案是通过下述工艺步骤而得以实现的：
步骤一，将鳞片石墨在微波炉中加热膨胀，加热功率为900W，加热时间为20~40 s，再把得到的热膨胀石墨加入到去离子水中，并进行超声搅拌分散，膨胀石墨被撕碎为片状石墨烯；
步骤二，在片状石墨烯悬浮液中加入碳化硼粉末，并在行星球磨机中进行高能球磨20~40 h，球磨混合均匀后，喷雾造粒，得到粉料；
步骤三，将步骤二获得的粉料放入石墨模具中，在真空环境下，先以70~100℃/min的速度升温至2250℃，保温5 min后，快速降温至2050℃，并保温30~60 min，在整个烧结过程中施加30~50 MPa的压力。
优选地，所述热膨胀石墨、去离子水以及碳化硼粉末的质量份数比为：1-2：15-10：99-98。
优选地，步骤二所述碳化硼由粗细两种碳化硼粉末组成，粗粉的平均颗粒尺寸为3~8 μm，细粉的平均颗粒尺寸为0.2~0.5 μm，粗粉与细粉的质量比为1:(2~3)。
本发明的另一个目的是提供一种碳化硼陶瓷复合材料由碳化硼基体相和石墨烯组成，优选的，所述石墨烯在材料中的配比为0.5~5 wt%。
本发明的再一个目的是提供上述所述石墨烯/碳化硼陶瓷复合材料在制作防弹板或耐磨器件中的应用。
相对于现有技术，本发明具有以下优点：
1.本发明提供的制备工艺可降低长时间加热温度，石墨烯均匀分散于碳化硼，晶界组织完整、致密；
2.本发明制备的石墨烯/碳化硼陶瓷复合材料强度高、韧度大，特别适用于特种车辆的防护领域。
具体实施方式
以下结合两个具体实施例，示例性说明及帮助进一步理解本发明。但实施例具体细节仅是为了说明本发明，并不代表本发明构思下的全部技术方案，因此不应理解为对本发明的技术方案的限定。一些不偏离本发明构思的非实质性改动，例如以具有相同或相似技术效果的技术特征简单改变或替换，均属本发明权利保护范围。
实施例1
一种石墨烯/碳化硼陶瓷复合材料的制备方法，制备工艺包括以下步骤：
步骤一，将鳞片石墨在微波炉中加热膨胀，加热功率为900W，加热时间为30 s，得到的热膨胀石墨；称取1份（质量份数）加入到10份去离子水中，超声搅拌2h，得到片状石墨烯悬浮液；
步骤二，在上述片状石墨烯悬浮液中加入碳化硼粉末99份（质量份数），在行星球磨机中进行高能球磨40 h，球磨混合均匀后，喷雾造粒，得到粉料；其中，碳化硼由粗细两种粉末组成，粗粉的平均颗粒尺寸为8 μm，细粉的平均颗粒尺寸为0.5 μm，粗粉与细粉的质量比为1:2。
步骤三，将步骤二获得的粉料放入石墨模具中，在真空环境下，先以100℃/min的速度升温至2250℃，保温5 min后，快速降温至2050℃，并保温45 min，在整个烧结过程中施加50 MPa的压力。
步骤四，烧结保温结束后，关掉加热电源，随炉冷却，即制成致密的石墨烯/碳化硼陶瓷复合材料。所得复合材料的弯曲强度大于450MPa，断裂韧度大于6.5 MPam1/2，维氏硬度大于31 GPa。
实施例2
一种石墨烯/碳化硼陶瓷复合材料的制备方法，制备工艺包括以下步骤：
步骤一，将鳞片石墨在微波炉中加热膨胀，加热功率为900W，加热时间为40 s，得到的热膨胀石墨；称取2份（质量份数）加入到15份去离子水中，超声搅拌2h，得到片状石墨烯悬浮液；
步骤二，在上述片状石墨烯悬浮液中加入碳化硼粉末98份（质量份数），在行星球磨机中进行高能球磨40 h，球磨混合均匀后，喷雾造粒，得到粉料；其中，碳化硼由粗细两种粉末组成，粗粉的平均颗粒尺寸为6 μm，细粉的平均颗粒尺寸为0.4 μm，粗粉与细粉的质量比为1:2。
步骤三，将步骤二获得的粉料放入石墨模具中，在真空环境下，先以80℃/min的速度升温至2250℃，保温5 min后，快速降温至2050℃，并保温60 min，在整个烧结过程中施加40 MPa的压力。
步骤四，烧结保温结束后，关掉加热电源，随炉冷却，即制成致密的石墨烯/碳化硼陶瓷复合材料。所得复合材料的弯曲强度大于420MPa，断裂韧度大于7.5 MPam1/2，维氏硬度大于30 GPa。
Claims (5)
1.一种石墨烯/碳化硼陶瓷复合材料的制备方法，其特征是制备方法包括如下步骤：
(1) 将鳞片石墨在微波炉中加热膨胀，加热功率为900W，加热时间为20~40 s，再把得到的热膨胀石墨加入到去离子水中，并进行超声搅拌分散，膨胀石墨被撕碎为片状石墨烯；
(2) 在得到的片状石墨烯悬浮液中加入碳化硼粉末，并在行星球磨机中进行高能球磨20~40 h，球磨混合均匀后，喷雾造粒，得到粉料；
(3) 将步骤(2)获得的粉料放入石墨模具中，在真空环境下，先以70~100℃/min的速度升温至2150℃，保温5 min后，快速降温至1950℃，保温30 min，在整个烧结过程中施加30~50 MPa的压力。
2.根据权利要求1所述的石墨烯/碳化硼陶瓷复合材料的制备方法，其特征在于：所述热膨胀石墨、去离子水以及碳化硼粉末的质量份数比为：1-2：15-10：99-98。
3. 根据权利要求2所述的石墨烯/碳化硼陶瓷复合材料的制备方法，其特征在于：其特征在于：步骤(2)所述碳化硼由粗细两种碳化硼粉末组成，粗粉的平均颗粒尺寸为3~8 μm，细粉的平均颗粒尺寸为0.2~0.5 μm，粗粉与细粉的质量比为1:(2~3)。
4. 根据权利要求1-3任意一项所述的制备方法得到的石墨烯/碳化硼陶瓷复合材料，其特征在于：该复合材料由碳化硼基体相和石墨烯组成，所述石墨烯在材料中的配比为0.5~5 wt%。
5.如权利4所述的石墨烯/碳化硼陶瓷复合材料用于制作防弹板或耐磨器件。
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| CN111499385A (zh) * | 2020-03-19 | 2020-08-07 | 武汉理工大学 | 一种碳化硼-石墨烯微叠层复合材料及其制备方法 |
| CN111925214A (zh) * | 2020-05-15 | 2020-11-13 | 浙江立泰复合材料股份有限公司 | 一种热压烧结用石墨烯/碳化硼复合粉末及其制备方法以及陶瓷产品的制备方法 |
| CN112174672A (zh) * | 2020-09-03 | 2021-01-05 | 香河星通科技有限公司 | 一种碳化硼复合陶瓷板的制备方法及防弹插板 |
| CN112723889A (zh) * | 2021-02-05 | 2021-04-30 | 武汉理工大学 | 一种高强韧碳化硼-硼化钛-石墨烯复合陶瓷及其制备方法 |
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| CN112174672A (zh) * | 2020-09-03 | 2021-01-05 | 香河星通科技有限公司 | 一种碳化硼复合陶瓷板的制备方法及防弹插板 |
| CN112723889A (zh) * | 2021-02-05 | 2021-04-30 | 武汉理工大学 | 一种高强韧碳化硼-硼化钛-石墨烯复合陶瓷及其制备方法 |
| CN112723889B (zh) * | 2021-02-05 | 2022-09-13 | 武汉理工大学 | 一种高强韧碳化硼-硼化钛-石墨烯复合陶瓷及其制备方法 |
| CN113788681A (zh) * | 2021-10-12 | 2021-12-14 | 景德镇学院 | 一种碳化硼轻质防弹材料及其制备方法 |
| CN116409998A (zh) * | 2023-03-02 | 2023-07-11 | 宁夏北伏科技有限公司 | 一种碳化硅石墨烯复合防弹陶瓷及制备方法 |
| CN116409998B (zh) * | 2023-03-02 | 2024-04-05 | 宁夏北伏科技有限公司 | 一种碳化硅石墨烯复合防弹陶瓷及制备方法 |
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