CN106187259A - 一种石墨烯纳米片增韧的复合陶瓷刀具及其微波制备工艺 - Google Patents

一种石墨烯纳米片增韧的复合陶瓷刀具及其微波制备工艺 Download PDF

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CN106187259A
CN106187259A CN201610567168.XA CN201610567168A CN106187259A CN 106187259 A CN106187259 A CN 106187259A CN 201610567168 A CN201610567168 A CN 201610567168A CN 106187259 A CN106187259 A CN 106187259A
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程寓
张勇
付乾辰
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Nanjing University of Science and Technology
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Abstract

本发明公开了一种石墨烯纳米片增韧的复合陶瓷刀具及其微波制备工艺，属于机械加工刀具制造技术领域。所述的陶瓷刀具，它是以Al2O3为基体，以TiC和石墨烯纳米片为增强相，并添加一定量的金属粘结剂和助烧剂，其组成按质量百分比为：Al2O3：50.2‑60.2%、TiC：20‑40%、Ni：3‑5%、Mo：3‑5%、MgO：0.5‑1%、Y2O3：0.5‑1%、石墨烯纳米片：0.1‑0.8%；本发明的复合陶瓷刀具以微波介质作热源，在氩气气氛保护下，通过优化配比、烧结温度和保温时间等工艺参数，采用微波烧结技术制备得到。本发明制备的复合陶瓷刀具中石墨烯纳米片分布均匀，刀具的断裂韧性得到了极大的提高，硬度最高为19.12 GPa，断裂韧性为8.73MPa m1/2，综合力学性能较好，制备工艺简单。

Description

一种石墨烯纳米片增韧的复合陶瓷刀具及其微波制备工艺
技术领域
本发明涉及一种石墨烯纳米片增韧的复合陶瓷刀具及其微波制备方法，属于机械加工刀具制造技术领域。
背景技术
相比于传统的硬质合金和高速钢刀具，陶瓷刀具具有高硬度、耐高温、抗氧化、耐腐蚀性强、化学稳定性好、高耐磨性和不易于金属发生粘结等优点，在高速切削领域具有很大的应用潜力。但是，陶瓷刀具较低的强度和断裂韧性在切削难加工时，易造成刀具的失效和断裂，限制了刀具的应用。因此，改善陶瓷刀具的脆性，成为陶瓷刀具研制的关键问题。
目前，对于陶瓷刀具主要的增韧方式包括，相变增韧、颗粒增韧和晶须、纤维增韧。但是相变增韧应用范围有限，基本仅限于ZrO2的相转化。颗粒增韧通过晶粒的钉扎可提高刀具的韧性，但是效果不显著。晶须、纤维可显著提高刀具韧性，但是一维的纤维、碳纳米管易发生团聚，不利于刀具综合力学性能的改善。
石墨烯，碳纳米管的同素异构体，一种由sp2杂化的碳原子以六边形周期排列形成的二维结构。石墨烯具有非常优异的物化和力学性能，导热系数高达5000Wm-1K-1，强度达130GPa，断裂强度约为125GPa。其独特的2D片状结构，可以有效的抑制石墨烯的团聚。石墨烯纳米片是由几层石墨烯构成，具有超高的表面积和极好的力学性能。因此，石墨烯纳米片在陶瓷刀具增韧补强方面应用前景广阔，且其超高的导热性能也是陶瓷刀具必需的。
陶瓷刀具大多数是通过热压烧结得到的，热压烧结在加压的同时进行加热，利于颗粒的接触、扩散和流动，容易得到接近理论密度的烧结体的性能较高。但热压烧结效率较低，很难大批量生产且成本也高。
发明内容
本发明的目的在于克服目前陶瓷刀具韧性较低且制备效率低下的缺点，利用微波烧结技术，制备出具有较高综合力学性能的新型陶瓷刀具。
本发明的基本构思是在脆性基体中加入TiC颗粒和石墨烯纳米片，在保持其高硬度的基础上，提高刀具的断裂韧性。利用微波烧结具有的加热均匀和升温快速的优点，在维持石墨烯纳米片稳定的2D片状结构的同时，通过优化配比、烧结温度和保温时间等工艺参数，提供性能优良、工艺简单和成本低廉的新型陶瓷刀具。
实现本发明目的的技术方案如下：一种石墨烯纳米片增韧的复合陶瓷刀具，它是以Al2O3为基体，以TiC和石墨烯纳米片为增强相，并添加一定量的金属粘结剂和烧结助剂，其组成按质量百分比为：Al2O3：50.2-60.2%、TiC：20-40%、Ni：3-5%、Mo：3-5%、MgO：0.5-1%、Y2O3：0.5-1%、石墨烯纳米片：0.1-0.8%。
上述石墨烯纳米片增韧的复合陶瓷刀具，其制备工艺为：
（1）将石墨烯纳米片加入到1-甲基-2-吡咯烷酮中，超声分散1-2h得到石墨烯悬浮液；
（2）将亚微米的Al2O3 、TiC和微米Ni、Mo、Y2O3和MgO，同时加入到步骤（1）石墨烯悬浮液中，超声分散并搅拌，得到混合溶液；
（3）将步骤（2）中的混合溶液进行球磨；
（4）球磨结束前两个小时加入1-10wt%的聚乙烯醇溶液进行造粒；
（5）将造粒后的混合料在100-120℃下真空干燥，然后研磨并过筛；
（6）将筛选后的粉料压制成型，成型压力为150MPa-300MPa，保压时间为2-3min；
（7）将成型后的素坯置于微波烧结炉中，在氩气的氛围下以30℃/min 的速率加热至1600℃-1700℃，并保温5-30min，然后随炉冷却制得复合陶瓷刀具。
步骤（1）中，石墨烯纳米片的厚度为5-10nm， 片径为1-10μ，石墨烯悬浮液浓度为2.5-5mg/ml。
步骤（2）中，亚微米Al2O3 、TiC的粒径均不大于0.5μm，微米Ni、Mo、Y2O3和MgO的粒径不大于2μm。
步骤（3）中，球磨是将混合溶液放入行星球磨罐中，球料比为8:1-10:1，球磨时间为36-60小时。
与现有技术相比，本发明的优点是：
（1）本发明构思新颖，通过在Al2O3基体中加入TiC和石墨烯纳米片，充分发挥了TiC和石墨烯纳米片的增韧补强的作用。复合陶瓷刀具的硬度最高达19.12 GPa，断裂韧度为8.73MPa m1/2。增韧机制主要是石墨烯纳米片的拔出、裂纹桥接以及裂纹偏转等，提高了陶瓷刀具的综合力学性能。
（2）本发明中微波电磁场可以保护石墨烯纳米片的组织结构不受破坏，且具有烧结温度低，升温时间短的特点。该工艺设备简单，成本低廉，具有较高的市场推广价值。
附图说明
图1为实施例2中中制备的刀具断口扫面电镜照片。
图2 为实施例3中刀具表面维氏压痕的扫描电镜照片。
具体实施方式
按实例参数附表称取石墨烯纳米片，在1-甲基-2-吡咯烷酮中超声分散2h，制备悬浮液；然后按实例附表称取亚微米Al2O3、TiC和微米Ni、Mo、Y2O3和MgO加入到石墨烯纳米片的悬浮液中，超声分散并机械搅拌20min；将混合溶液加入到行星球磨罐中，球磨48小时；制备质量浓度为5wt%的聚乙烯醇溶液，并在球磨结束前两个小时加入到溶液中进行造粒；球磨后的混合料置于真空干燥箱中在110±10℃下干燥，然后研磨并过100目筛筛选粉料；将筛选后的粉料压制成型，成型压力为200MPa，保压时间为3min，得到烧结素坯。素坯置于微波烧结炉中进行微波烧结，烧结工艺为：在氩气（纯度为99.99%）的氛围下以30℃/min 的速率加热至1600℃-1700℃，并保温5-30min，然后随炉冷却制得复合陶瓷刀具。经测试所得力学性能见附表。
实施例参数附表
实施例力学性能附表
图1 是根据实施例2中所得到的陶瓷刀具的断口形貌，可以看到石墨烯纳米片钉扎在晶界处。晶界处的石墨烯纳米片由于具有极好的力学性能可以阻止裂纹的扩展，产生裂纹的偏转。而且，在材料断裂过程中，石墨烯纳米片会产生拔出效应和裂纹桥连。石墨烯的这种分布方式，会消耗较多的断裂能，可有效的提高材料的力学性能。
图2是根据实施例3中所得到的陶瓷刀具表面维式压痕的扫描电镜照片，在TiC颗粒和石墨烯纳米片的共同作用下，裂纹发生了分支、偏转和桥连等现象，可以有效的提高刀具的断裂韧性。

Claims (7)

1.一种石墨烯纳米片增韧的复合陶瓷刀具，其特征在在于，它是以Al2O3为基体，以TiC和石墨烯纳米片为增强相，并添加一定量的金属粘结剂和烧结助剂，其组成按质量百分比为：Al2O3：50.2-60.2%、TiC：20-40%、Ni：3-5%、Mo：3-5%、MgO：0.5-1%、Y2O3：0.5-1%、石墨烯纳米片：0.1-0.8%。
2.如权利要求1所述的石墨烯纳米片增韧的复合陶瓷刀具，其特征在在于，由如下步骤制备：
（1）将石墨烯纳米片加入到1-甲基-2-吡咯烷酮中，超声分散1-2h得到石墨烯悬浮液；
（2）将亚微米的Al2O3 、TiC和微米Ni、Mo、Y2O3和MgO，同时加入到步骤（1）石墨烯悬浮液中，超声分散并搅拌，得到混合溶液；
（3）将步骤（2）中的混合溶液进行球磨；
（4）球磨结束前两个小时加入聚乙烯醇溶液进行造粒；
（5）将造粒后的混合料在100-120℃下真空干燥，然后研磨并过筛；
（6）将筛选后的粉料压制成型，成型压力为150MPa-300MPa，保压时间为2-3min；
（7）将成型后的素坯置于微波烧结炉中，在氩气的氛围下以30℃/min 的速率加热至1600℃-1700℃，并保温5-30min，然后随炉冷却制得复合陶瓷刀具。
3.如权利要求2所述的石墨烯纳米片增韧的复合陶瓷刀具，其特征在在于，步骤（1）中，石墨烯纳米片的厚度为5-10nm， 片径为1-10μ，石墨烯悬浮液浓度为2.5-5mg/ml。
4.如权利要求2所述的石墨烯纳米片增韧的复合陶瓷刀具，其特征在在于，步骤（2）中，亚微米Al2O3 、TiC的粒径均不大于0.5μm，微米Ni、Mo、Y2O3和MgO的粒径不大于2μm。
5.如权利要求2所述的石墨烯纳米片增韧的复合陶瓷刀具，其特征在在于，步骤（3）中，球磨是将混合溶液放入行星球磨罐中，球料比为8:1-10:1，球磨时间为36-60小时。
6.如权利要求2所述的石墨烯纳米片增韧的复合陶瓷刀具，其特征在在于，步骤（4）中，聚乙烯醇溶液浓度为1-10wt%。
7.如权利要求1-6任一所述的石墨烯纳米片增韧的复合陶瓷刀具的制备工艺。
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Application publication date: 20161207