CN115304382A - 一种低热导新型四元高熵金属二硼化物及其制备方法 - Google Patents
一种低热导新型四元高熵金属二硼化物及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种新型四元高熵金属二硼化物及其制备方法，属于超高温陶瓷材料技术领域。所述高熵金属二硼化物化学式记为(Hf0.25Zr0.25Ta0.25Sc0.25)B2，其中Hf，Zr，Ta和Sc金属元素为等摩尔比，摩尔比总和为1；(Hf0.25Zr0.25Ta0.25Sc0.25)B2处理具有优异的相稳定性，优异的力学性能外，(Hf0.25Zr0.25Ta0.25Sc0.25)B2的热导率仅有13.9W·m‑1·K‑1，比传统HfB2，ZrB2降低了86.7％，76.8％。因此，(Hf0.25Zr0.25Ta0.25Sc0.25)B2适宜在超高温隔热领域推广应用。
Description
技术领域
本发明涉及一种新型四元高熵金属二硼化物及其制备方法，属于超高温陶瓷材料技术领域。
背景技术
在超高温陶瓷(UHTCs)中，过渡金属二硼化物(TMB2)因其高熔点、高硬度、良好的抗热震性和化学稳定性，被广泛应用于高超声速飞行器、核反应堆、飞机前缘和鼻锥等领域。然而，单组元TMB2(HfB2，ZrB2)热导率可达到60-120W·m-1·K-1，较高的热导率是阻碍金属二硼化物在超高温隔热领域应用的主要原因。先前的研究表明4-5种TMB2经过高熵固溶后可以增强声子散射率，从而显著降低超高温陶瓷的热导率。目前，高熵过渡金属二硼化物(HE TMB2)的组分主要为HfB2，ZrB2，TaB2，NbB2和TiB2。首先，这些TMB2都是高热导材料，并且数量较少，使得多数研究以(Hf0.2Zr0.2Ta0.2Nb0.2Ti0.2)B2作为HE TMB2的主要研究对象，导致HE TMB2的材料设计空间较窄。研究在HE TMB2中引入稀土金属二硼化物ScB2对其结构和性能的影响。
发明内容
有鉴于此，本发明为了扩大HE TMB2的材料设计空间，通过高熵的概念在TMB2引入了稀土金属二硼化物(REB2)—ScB2。设计了一种新型的四元高熵金属二硼化物—(Hf0.25Zr0.25Ta0.25Sc0.25)B2。该金属二硼化物是由Hf、Zr、Ta、Sc以及B组成的，不仅力学性能优异，而且可以显著降低传统TMB2的热导率；而且该四元高熵金属二硼化物可以在1700℃低温下制备成单相粉体，制备工艺易于操作，制备成本低，适宜工业推广。
本发明的目的是通过以下技术方案实现的。
一种四元高熵金属二硼化物，所述高熵金属二硼化物化学式简记为(Hf0.25Zr0.25Ta0.2Sc0.25)B2，Hf、Zr、Ta和Sc的原子摩尔比为0.25(原子摩尔比总和为1)。
一种四元高熵金属二硼化物的制备方法，所述方法包括以下步骤：
将HfO2,ZrO2,Ta2O5,Sc2O3和B4C粉体按照化学计量比配料，B4C粉体的加入料过量20％以保证反应的充分和弥补高温下B源的损失。将五种粉体先混合均匀，然后将混合粉体转移至高温真空条件下，温度为1700℃以上(包含1700℃)并保温1h～3h，得到四元高熵金属二硼化物的粉体；
将制备得到的四元高熵金属二硼化物粉体的装入石墨模具中，采用放电感应等离子烧结(SPS)在真空或惰性气体保护气氛下烧结，烧结温度为1900℃～2200℃，烧结压力为30MPa～50MPa，烧结时间(以保温时间为主)为15min～35min，得到单相高熵金属二硼化物块体。
优选地，HfO2,ZrO2,Ta2O5,Sc2O3和B4C粉体在球磨罐中球磨混合，溶剂为乙醇，球料比为(3～6)：1，转速为300rpm～500rpm，球磨时间为2h～6h。
优选地，四元高熵金属二硼化物粉体在真空高温气氛中的制备过程，升温速率为5℃/min～10℃/min。
优选地，四元高熵金属二硼化物粉体制备过程中，保温温度为1700℃～1950℃。
优选地，采用放电感应等离子烧结(SPS)制备四元高熵金属二硼化物块体的过程中，保温温度为1900～2200℃。
有益效果：
(1)本发明首次设计及制备了一种新型四元高熵金属二硼化物，(Hf0.25Zr0.25Ta0.2Sc0.25)B2具有优异的相稳定性，不仅在较低温度下可以合成纯相的粉体，而且还具有优异的力学性能。
(2)本发明所述新型四元高熵金属二硼化物的制备过程中添加了过量的B4C，因为HfO2,ZrO2,Ta2O5,Sc2O3和B4C粉体在高温反应下会发生热还原反应，中间反应产物B2O3和BO较低的沸点在真空和高温下会快速挥发导致硼源的流失，导致热还原反应不完全，因此为了能够充分反应添加了过量的B4C。
(3)本发明所述新型四元高熵金属二硼化物块体具有较低的热导率，可以在超高温隔热材料领域应用。
附图说明
图1为实施例1制备的(Hf0.25Zr0.25Ta0.2Sc0.25)B2粉体的X射线衍射(XRD)谱图。
图2为实施例1制备的(Hf0.25Zr0.25Ta0.2Sc0.25)B2块体的X射线衍射(XRD)谱图。
图3为实施例1制备的(Hf0.25Zr0.25Ta0.2Sc0.25)B2块体的元素分析图谱。
具体实施方式
下面结合具体实施方式对本发明作进一步阐述，其中，所述方法如无特别说明均为常规方法，所述原材料如无特别说明均能从公开商业途径获得。
以下实施例中：
HfO2、ZrO2、Ta2O5、Sc2O3和B4C粉体的粒径均为500nm～3μm；
弹性模量采用脉冲激发共振法测得，测试样品尺寸为3mm×15mm×40mm的长方体；
维氏硬度采用HXD-1000B型显微硬度计(上海泰明光学仪器有限公司)，测试样品尺寸3mm×4mm×15mm，测试面抛光至镜面，载荷分别为0.5、1、2、3、5和10N，保压时间为10s；其中，为了避免压痕之间的相互影响，压痕在不同的位置进行，并且两个压痕点之间的距离要大于凹陷对角线长度的三倍以上；
弯曲强度通过三点弯曲实验得到，测试设备为万能力学试验机，测试样品的尺寸为3mm×4mm×36mm，跨距为30mm，压头移动速度为0.5mm/min；其中，在测试前，样品进行三面抛光，且受拉面作45°倒角处理以降低边缘性破坏的可能性；
热扩散系数采用激光闪射法来测量，测试设备为激光热导仪，样品的尺寸为直径12.7mm×1.0mm的圆片。热导率通过公式σ＝σ0+Kd0.5进行计算。。
实施例1
(1)将HfO2、ZrO2、Ta2O5、Sc2O3和B4C粉体按照摩尔比2:2:1:1:5.71和乙醇一起加入尼龙材质的球磨罐中，球料比为6:1，在350rpm转速下球磨混合5h，得到混合均匀的混合粉体；
(2)将混合粉体在100℃的条件下干燥后，放至真空条件下，以10℃/min的升温速率加热至1700℃并保温3h，得到四元高熵金属二硼化物粉体，化学式为(Hf0.25Zr0.25Ta0.2Sc0.25)B2；
(3)将制备得到的(Hf0.25Zr0.25Ta0.2Sc0.25)B2粉体装入石墨模具中，采用放电感应等离子烧结在真空气氛下进行块体的烧结，烧结温度为2000℃，烧结压力为40MPa，烧结时间30min，得到单相(Hf0.25Zr0.25Ta0.2Sc0.25)B2块体。
对步骤(2)获得的(Hf0.25Zr0.25Ta0.2Sc0.25)B2粉体进行XRD表征，从图1中可以看出，(Hf0.25Zr0.25Ta0.2Sc0.25)B2粉体的衍射峰与六方AlB2型结构的一致，没有检测到其他相结构的衍射峰，说明合成的(Hf0.25Zr0.25Ta0.2Sc0.25)B2粉体为均匀的单相结构。
步骤(3)所获得的(Hf0.25Zr0.25Ta0.2Sc0.25)B2块体采用扫描电子显微镜的EDS功能进行元素分析，根据图3的检测分析结果可知，Hf、Ta、Zr和Sc四种金属元素分布均匀，没有检测到团聚或偏析的现象，说明(Hf0.25Zr0.25Ta0.2Sc0.25)B2块体具有均匀的四元高熵结构。
对步骤(3)制备的(Hf0.25Zr0.25Ta0.2Sc0.25)B2块体进行力学性能测试，测试结果如表1所示。从表1中可以看出，(Hf0.25Zr0.25Ta0.2Sc0.25)B2具有比传统TMB2更优异的力学性能，其中硬度高30％，弯曲强度高22％。
表1
对步骤(3)制备的(Hf0.25Zr0.25Ta0.2Sc0.25)B2块体进行热扩散测试，测试结果及通过公式计算得到的热导率如表1所示，表1列出了传统TMB2的结果进行对比。从表1中可以看出，(Hf0.25Zr0.25Ta0.2Sc0.25)B2的热导率为13.9W·m-1·K-1，(Hf0.25Zr0.25Ta0.2Sc0.25)B2的热导率分别比传统HfB2，ZrB2降低了86.7％，76.8％。
Claims (8)
1.一种四元高熵金属二硼化物，其特征在于：所述四元高熵金属二硼化物化学式为(Hf0.25Zr0.25Ta0.2Sc0.25)B2，Hf、Zr、Ta和Sc四种金属元素为等原子摩尔比且原子摩尔比之和为1。
2.一种如权利要求1所述的四元高熵金属二硼化物的制备方法，其特征在于：所述方法包括以下步骤：
将HfO2,ZrO2,Ta2O5,Sc2O3和B4C粉体按照化学计量比配料，B4C粉体的加入料过量20％以保证反应的充分和弥补高温下B源的损失。将五种粉体先混合均匀，然后将混合粉体转移至高温真空条件下，温度为1700℃以上(包含1700℃)并保温1h～3h，得到四元高熵金属二硼化物的；
将制备得到的四元高熵金属二硼化物粉体的装入石墨模具中，采用放电感应等离子烧结(SPS)在真空或惰性气体保护气氛下烧结，烧结温度为1900℃～2200℃，烧结压力为30MPa～50MPa，烧结时间(以保温时间为主)为15min～35min，得到单相高熵金属二硼化物块体。
3.根据权利要求2所述的一种四元高熵金属二硼化物的制备方法，其特征在于：过量的B4C粉体为按照化学计量比加入的B4C粉体质量的115％～135％。
4.根据权利要求2所述的一种四元高熵金属二硼化物的制备方法，其特征在于HfO2,ZrO2,Ta2O5,Sc2O3和B4C粉体在球磨罐中球磨混合，球料比为(3～6)：1，转速为300rpm～500rpm，球磨时间为2h～6h。
5.根据权利要求2所述的一种四元高熵金属二硼化物的制备方法，其特征在于：四元高熵金属二硼化物粉体制备过程中，以5℃/min～10℃/min的升温速率加热至1700℃以上。
6.根据权利要求2所述的一种四元高熵金属二硼化物的制备方法，其特征在于：四元高熵金属二硼化物粉体制备过程中，加热温度为1700℃～1950℃。
7.根据权利要求2所述的一种四元高熵金属二硼化物的制备方法，其特征在于：将制备得到的四元高熵金属二硼化物粉体研磨并通过100-300目的筛子过筛，再采用放电感应等离子烧结制备成块体。
8.根据权利要求2所述的一种单相高熵金属二硼化物的制备方法，其特征在于：HfO2,ZrO2,Ta2O5,Sc2O3和B4C粉体的粒径均为500nm～3μm。
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| US5633214A (en) * | 1994-06-30 | 1997-05-27 | Nkk Corporation | Boron nitride-containing material and method thereof |
| CN114715907A (zh) * | 2022-03-18 | 2022-07-08 | 北京理工大学 | 一种单相高熵金属二硼化物及其制备方法 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5633214A (en) * | 1994-06-30 | 1997-05-27 | Nkk Corporation | Boron nitride-containing material and method thereof |
| CN114715907A (zh) * | 2022-03-18 | 2022-07-08 | 北京理工大学 | 一种单相高熵金属二硼化物及其制备方法 |
Non-Patent Citations (1)
| Title |
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| ZE ZHANG ET AL.: "Phase structure,mechanical properties and thermal properties of high-entropy diboride (Hf0.25Zr0.25Ta0.25Sc0.25)B2", 《JOURNAL OF THE EUROPEAN CERAMIC SOCIETY》 * |
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