CN116199515B - 一种碳化硅/高熵碳氮化物复合粉体及其制备方法和应用 - Google Patents

一种碳化硅/高熵碳氮化物复合粉体及其制备方法和应用 Download PDF

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CN116199515B
CN116199515B CN202310156839.3A CN202310156839A CN116199515B CN 116199515 B CN116199515 B CN 116199515B CN 202310156839 A CN202310156839 A CN 202310156839A CN 116199515 B CN116199515 B CN 116199515B
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entropy
silicon carbide
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CN116199515A (zh
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黄坤恒
郭伟明
刘洋
林华泰
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Guangdong University of Technology
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Abstract

本发明属于非氧化物粉体技术领域，公开了一种碳化硅/高熵碳氮化物复合粉体及其制备方法和应用。该方法是将TiO2粉、ZrO2粉、Nb2O5粉、Ta2O5粉、MoO3粉、C粉和Si3N4粉混合，制得混合粉体；将混合粉体加入无水乙醇，超声搅拌制得浆料；然后将Si3N4介质球加入浆料经辊式球磨，经干燥、烘干、过筛后装入石墨模具，干压成坯体；在保护气氛下，将坯体在1500～1700℃无压烧结，或者将坯体在1400～1600℃热处理，制得碳化硅/高熵碳氮化物复合粉体，其组成为SiC/(Ti,Zr,Nb,Ta,Mo)CN。该复合粉体具有纯度高，粒度小等优势，可应用在制备切削难加工材料中。

Description

一种碳化硅/高熵碳氮化物复合粉体及其制备方法和应用
技术领域
本发明属于非氧化物粉体技术领域，更具体地，涉及一种碳化硅/高熵碳氮化物复合粉体及其制备方法和应用。
背景技术
高熵碳氮化物陶瓷已被应用于切削工具材料的制备中。其具有耐磨损、耐化学反应、耐热冲击等优异特性。可有效提高切削加工的速度和晶须，降低加工成本。相较于传统的硬质合金，高熵碳氮化物具有更为优异的抗氧化性能和高温抗弯强度。同时，高熵碳氮化物陶瓷具有较高的红硬性，且热导率较高，至目前最具前途的刀具材料，这就提升对高熵碳氮化物的粉体的需求。然而，目前高熵碳氮化物粉体的合成方法通常采用氮气氮化金属碳化物等方法。这些方法采用气态的氮源，难以对高熵碳氮化物的C、N含量作精确的调控。
发明内容
为了解决上述现有技术存在的不足和缺点，本发明的目的在于提供一种碳化硅/高熵碳氮化物复合粉体的制备方法。该方法工艺简单，得到的碳化硅复合高熵碳氮化物粉体具有高纯度和较小的粒度。
本发明的另一目的在于提供上述方法制备得到的碳化硅/高熵碳氮化物复合粉体。
本发明的再一目的在于提供上述碳化硅/高熵碳氮化物复合粉体的应用。
本发明的目的通过下述技术方案来实现：
一种碳化硅/高熵碳氮化物复合粉体的制备方法，包括以下步骤：
S1.将TiO2粉、ZrO2粉、Nb2O5粉、Ta2O5粉、MoO3粉、C粉和Si3N4粉混合，制得混合粉体；TiO2粉、ZrO2粉、Nb2O5粉、Ta2O5粉、MoO3粉、Si3N4粉和C粉的摩尔比为1:1:0.5:0.5:1:(2-5):(6-15)；
S2.将混合粉体加入无水乙醇，超声搅拌制得浆料；然后将Si3N4介质球加入浆料经辊式球磨，经干燥、烘干、过筛后装入石墨模具，干压成坯体；
S3.在保护气氛下，将坯体在1500～1700℃无压烧结，或者将坯体在1400～1600℃热处理，制得碳化硅/高熵碳氮化物复合粉体，其分子式为SiC/(Ti,Zr,Nb,Ta,Mo)CN。
优选地，步骤S1中所述的TiO2粉、ZrO2粉、Nb2O5粉、Ta2O5粉、MoO3粉的粒径均为1～5μm；Si3N4粉的粒径为2～4μm；C粉的粒径为500nm～1μm。
优选地，步骤S2中所述球磨的转速为100～300r/min，所述球磨的时间为18～36h；所述干燥的温度为60～80℃，所述干燥的时间为12～24h。
优选地，步骤S3中所述无压烧结的程序为：先以10～14℃/min的速率升温至1000～1200℃，开始充氮气至1个大气压，继续以6～8℃/min的速率升温至1500～1700℃；升温程序执行完毕后保温0.5～1h；然后以8～15℃/min的速率降温，降温至750～850℃后随炉降温。
优选地，步骤S3中所述热处理程序为：使用氮气流动气氛；先以10～14℃/min的速率升温到1000～1100℃，继续以6～8℃/min的速率升温至1400～1600℃；升温程序执行完毕后保温保压1～4h；然后以10～12℃/min的速率降温，降温至750～850℃后随炉降温。
一种碳化硅/高熵碳氮化物复合粉体，所述碳化硅/高熵碳氮化物复合粉体是由所述的方法制备得到。
优选地，所述的碳化硅/高熵碳氮化物复合粉体，所述碳化硅/高熵碳氮化物复合粉体的粒径为50～300nm，进一步地，粒径为100～250nm，更为优选地，粒径为50～100nm。
所述的碳化硅/高熵碳氮化物复合粉体在制备切削难加工材料中的应用。
与现有技术相比，本发明具有以下有益效果：
1.本发明采用了固态氮化硅作为氮源、可精确控制合成的高熵碳氮化物中C、N的配比，通过无压热处理工艺，该工艺简单、成本低、节约能源。
2.本发明制得的碳化硅/高熵碳氮化物复合粉体具有高纯度，粒度小的优点。
附图说明
图1为实施例1的SiC/(Ti,Zr,Nb,Ta,Mo)CN粉体显微照片；
图2为实施例2的SiC/(Ti,Zr,Nb,Ta,Mo)CN粉体显微照片。
具体实施方式
下面结合具体实施例进一步说明本发明的内容，但不应理解为对本发明的限制。若未特别指明，实施例中所用的技术手段为本领域技术人员所熟知的常规手段。除非特别说明，本发明采用的试剂、方法和设备为本技术领域常规试剂、方法和设备。
实施例1
1.将TiO2粉(粒径为1～5μm)、ZrO2粉(粒径为1～5μm)、Nb2O5粉(粒径为1～5μm)、Ta2O5粉(粒径为1～5μm)、MoO3粉(粒径为1～5μm)、C粉(粒径为500nm～1μm)和Si3N4粉(粒径为2～4μm)混合，制得混合粉体；TiO2粉、ZrO2粉、Nb2O5粉、Ta2O5粉、MoO3粉、Si3N4粉和C粉摩尔比为1:1:0.5:0.5:1:2.5:7.5；
2.将混合粉体加入无水乙醇，超声搅拌制得浆料；然后将氮化硅介质球加入浆料经辊式球磨机球磨，经干燥、烘干、过筛后装入石墨模具，干压成坯体；
3.将坯体先以10～14℃/min升温至1000～1200℃，开始充氮气至1个大气压，继续以6～8℃/min的速率升温至1500℃；升温程序执行完毕后保温0.5h；然后以8～15℃/min的速率降温，温度降至750～850℃后随炉降温，得到碳化硅/高熵碳氮化物复合粉体，其组成为SiC/(Ti,Zr,Nb,Ta,Mo)CN。
图1为实施例1的SiC/(Ti,Zr,Nb,Ta,Mo)CN粉体显微照片，从图1中可以，看到粉体呈等轴状形貌，颗粒分布均匀，无明显杂质，制得的碳化硅/高熵碳氮化物复合粉体的粒径为50～100nm。
实施例2
1.TiO2、ZrO2、Nb2O5、Ta2O5、MoO3粉、C粉、Si3N4粉体混合，制得混合粉体；TiO2粉、ZrO2粉、Nb2O5粉、Ta2O5粉、MoO3粉、Si3N4粉和C粉的摩尔比为1:1:0.5:0.5:1:3:9；
2.将混合粉体加入无水乙醇，超声搅拌制得浆料；然后将氮化硅介质球加入浆料经辊式球磨机球磨，经干燥、烘干、过筛后装入石墨模具，干压成坯体；
3.将坯体先以10～14℃/min的速率升温至1000～1200℃，开始充氮气至1个大气压，继续以6～8℃/min的速率升温至1600℃；升温程序执行完毕后保温1h；然后以8～15℃/min的速率降温，降温至750～850℃后随炉降温，得到碳化硅/高熵碳氮化物复合粉体，其组成为SiC/(Ti,Zr,Nb,Ta,Mo)CN。
图2为实施例2的SiC/(Ti,Zr,Nb,Ta,Mo)CN粉体显微照片，从图2中可以看到，粉体呈等轴状形貌，颗粒分布均匀，无明显杂质，制得的碳化硅/高熵碳氮化物复合粉体的粒径为250～300nm。
实施例3
1.将TiO2、ZrO2、Nb2O5、Ta2O5、MoO3粉体和碳粉、氮化硅粉体混合，制得混合粉体；TiO2粉、ZrO2粉、Nb2O5粉、Ta2O5粉、MoO3粉、Si3N4粉和C粉的摩尔比为1:1:0.5:0.5:1:5:15；
2.将混合粉体加入无水乙醇，超声搅拌制得浆料；然后将氮化硅介质球加入浆料经辊式球磨机球磨，经干燥、烘干、过筛后装入石墨模具，干压成坯体；
3.将坯体先以10～14℃/min的速率升温至1000～1200℃，开始充氮气至1个大气压，继续以6～8℃/min的速率升温至1600℃；升温程序执行完毕后保温1h；然后以8～15℃/min的速率降温，降温至750～850℃后随炉降温，得到碳化硅/高熵碳氮化物复合粉体，其组成为SiC/(Ti,Zr,Nb,Ta,Mo)CN。
本实施例制得的碳化硅/高熵碳氮化物复合粉体的粒径为250～300nm。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合和简化，均应为等效的置换方式，都包含在本发明的保护范围之内。

Claims (4)

1.一种碳化硅/高熵碳氮化物复合粉体的制备方法，其特征在于，包括以下步骤：
S1. 将TiO2粉、ZrO2粉、Nb2O5粉、Ta2O5粉、MoO3粉、C粉和Si3N4粉混合，制得混合粉体；TiO2粉、ZrO2粉、Nb2O5粉、Ta2O5粉、MoO3粉、Si3N4粉和C粉的摩尔比为1:1:0.5:0.5:1:（2~5）:（6~15）；所述的TiO2粉、ZrO2粉、Nb2O5粉、Ta2O5粉、MoO3粉的粒径均为1~5μm；Si3N4粉的粒径为2~4μm；C粉的粒径为500nm~1μm；
S2. 将混合粉体加入无水乙醇，超声搅拌制得浆料；然后将Si3N4介质球加入浆料经辊式球磨，经干燥、烘干、过筛后装入石墨模具，干压成坯体；
S3. 在保护气氛下，将坯体在1500~1700℃无压烧结，制得碳化硅/高熵碳氮化物复合粉体，其组成为SiC/(Ti,Zr,Nb,Ta,Mo)CN；所述碳化硅/高熵碳氮化物复合粉体的粒径为50~300nm；所述无压烧结的程序为：先以10~14℃/min的速率升温至1000~1200℃，开始充氮气至1个大气压，继续以6~8℃/min的速率升温至1500~1700℃；升温程序执行完毕后保温0.5~1h；然后以8~15℃/min的速率降温，降温至750~850℃后随炉降温。
2.根据权利要求1所述的碳化硅/高熵碳氮化物复合粉体的制备方法，其特征在于，步骤S2中所述球磨的转速为100~300 r/min，所述球磨的时间为18~36h；所述干燥的温度为60~80℃，所述干燥的时间为12~24h。
3.一种碳化硅/高熵碳氮化物复合粉体，其特征在于，所述碳化硅/高熵碳氮化物复合粉体是由权利要求1或2所述的方法制备得到。
4.根据权利要求3所述的碳化硅/高熵碳氮化物复合粉体在制备切削难加工材料中的应用。
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