CN114516758A - 一种含碲三元层状硼化物及其制备方法 - Google Patents
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- 229910052714 tellurium Inorganic materials 0.000 title claims abstract description 22
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 15
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- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910003862 HfB2 Inorganic materials 0.000 description 1
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- 238000005260 corrosion Methods 0.000 description 1
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- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 1
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- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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Abstract
本发明公开了一种含碲三元层状硼化物及其制备方法，该含碲三元层状硼化物的化学式为Hf2TeB，Hf2TeB的空间群为P63/mmc，晶格参数分别为
其中Hf原子位于(1/3，2/3，0.57505，Te原子位于(1/3，2/3，1/4)，B原子位于(0，0，0)。本发明为首次发现的含Te的MAX相，新的三元层状化合物相Hf2TeB的发现与制备，对MAX相体系的完善有着重大的意义。
Description
技术领域
本发明属于新材料技术领域，具体涉及到一种含碲三元层状硼化物及其制备方法。
背景技术
Mn+1AXn相(n＝1-3)作为一类三元层状化合物，最早由Nowotny等人在二十世纪六十年代首先提出，其中M为早期过渡族金属，A通常为主族元素，X为B、C或N元素。这一类化合物的结构特点在于Mn+1Xn层与A元素层交替排列，随着n值的不同有着不同的排列组合，分别称为211(n＝1)、312(n＝2)、413(n＝3)相。Barsoum等人在二十世纪九十年代通过热压合成了致密的块体MAX相化合物Ti3SiC2并报道了其一系列独特的性能，包括高导热、导电能力，很好的机械强度及高温强度，优异的可加工性，非常好的抗腐蚀及抗氧化性等。随着研究的进一步深入，人们确认了这一族化合物同时具有金属及陶瓷的优异性能，这也让MAX相陶瓷在几十年来始终被研究人员所关注。作为一种元素可调的三元层状化合物，研究人员对这一族物质进行了大量的计算及预测，目前已有超过650种MAX相经计算确定为热力学稳定相，但遗憾的是，只有80多种MAX相在实验室中成功合成。
传统的MAX相材料主要集中在碳化物和氮化物体系，已经有了大量的研究基础，而MAX相硼化物体系研究起步很晚。2019年Rackl等人最先通过固相法合成了纯净的Nb2SB粉末，我们使用类似的工艺合成了纯度为99wt％的Hf2SB及纯度为85wt％的Zr2SB粉末，由此开启了MAX相硼化物的研究。随着近年来含Se的MAX相硼化物Zr2SeB和Hf2SeB被发现，MAX相硼化物已经初步形成了体系。
但目前尚未发现Te作为A层元素的MAX相，因此对于含Te的MAX相研究对MAX相家族的完善具有重大的意义。
发明内容
本发明的目的是提供一种含碲三元层状硼化物及其制备方法，该含碲三元层状硼化物的化学式为Hf2TeB，并通过X射线衍射、第一性原理计算、扫描电镜及透射电镜等检测分析方法，确定了新相的晶格结构及其原子位置。Hf2TeB是纳米层状结构的三元过渡金属硼化物，属于MAX相陶瓷中的211相，也是首次发现的含Te的MAX相。这一种新物质的发现证明了Te可以作为MAX相材料的A层元素，对MAX相家族的完善有重大的意义。
为达上述目的，本发明提供了一种含碲三元层状硼化物的制备方法，包括以下步骤：
(1)将Hf粉、Te粉和B粉按照摩尔比2:1-5:1称重后混合均匀；
(2)将步骤(1)混匀后的粉体升温烧结，冷却后破碎，制得含碲三元层状硼化物的粉体。
进一步地，混合的过程依次包括机械搅拌和球磨，机械搅拌的时间为10-15h。
进一步地，粉体的粒径为过200目筛。
进一步地，升温速率为1-3℃/s，烧结的温度为350-450℃，烧结的压力为18-22MPa。
进一步地，本发明还提供了一种采用含碲三元层状硼化物的制备方法制备得到的含碲三元层状硼化物。
进一步地，含碲三元层状硼化物的化学式为Hf2TeB，Hf2TeB的空间群为P63/mmc，晶格参数分别为
其中Hf原子位于(1/3，2/3，0.57505)，Te原子位于(1/3，2/3，1/4)，B原子位于(0，0，0)。
综上所述，本发明具有以下优点：
1、本发明发现了一种新的MAX相Hf2TeB，通过X射线衍射、第一性原理计算、扫描电镜及透射电镜等检测分析方法，确定了新相的晶格结构及其原子位置。
2、本发明为首次发现的含Te的MAX相，新的三元层状化合物相Hf2TeB的发现与制备，对MAX相体系的完善有着重大的意义。
附图说明
图1为实施例1中新的三元层状化合物相Hf2TeB陶瓷粉体和具有类似结构的Hf2SB与Hf2SeB陶瓷粉体的X射线衍射图谱对比。
图2为实施例1中新的三元层状化合物相Hf2TeB陶瓷粉体的SEM图。
图3为实施例1中新的三元层状化合物相Hf2TeB
面的TEM图。
图4为实施例1中新的三元层状化合物相Hf2TeB陶瓷粉体的Rietveld拟合图。
具体实施方式
本发明提供了一种含碲三元层状硼化物Hf2TeB的制备方法，包括以下步骤：
(1)将Hf粉、Te粉和B粉按摩尔配比2:1-1.5:1称重，混合后于滚筒式混料机上混料10-15h至混合均匀，将混合均匀的物料再使用球磨研磨，得到均匀混合粉体；
(2)将步骤(1)所得到的均匀混合粉体放入放电等离子体烧结炉(SPS)，使用1-3℃/s左右的升温速率及18-22MPa的压力迅速升温至350-450℃，此时即会发生热爆炸烧结，样品随炉冷却后得到反应产物；
(3)将步骤(2)得到的小块样品使用万能破碎机破碎，过200目筛后，得到最终的粉体。
本发明还对得到的粉体进行了图谱检测和Rietveld拟合，具体包括以下步骤：
S1将粉体使用X射线衍射(XRD)进行基本物相检测，使用扫描电镜(SEM)进行微观形貌观测并使用高分辨率透射电镜(HRTEM)确定晶体的结构类型；
S2将S1得到的XRD图谱进行识别，结合EDS/TEM得到的目标陶瓷粉体的晶格结构，用Materials Studio软件建立模型并进行结构优化；
S3将XRD图谱与步S2优化后的晶格模型作为输入参数，在Full-Prof软件中进行Rietveld拟合，得到目标陶瓷粉体的晶格常数与原子位置。
以下结合实施例对本发明的原理和特征进行描述，所举实例只用于解释本发明，并非用于限定本发明的范围。实施例中未注明具体条件者，按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者，均为可以通过市售购买获得的常规产品。
实施例1
本实施例提供了一种含碲三元层状硼化物Hf2TeB的制备方法，包括以下步骤：
(1)将Hf粉(99.9％，400目)、Te粉(99.99％，200目)和硼粉(99％，2500目)按摩尔配比2:1:1称重，混合后于滚筒式混料机上混料12h至混合均匀，将混合均匀的物料再使用球磨研磨，得到均匀混合粉体；
(2)取步骤(1)所得到的均匀混合粉体25g放入到垫有石墨纸的石墨模具中，套上石墨毡，装载到SPS炉中，压力设置为20MPa，在真空下使用2℃/s的升温速率加热约200s，发生热爆炸烧结过程后，随炉冷却后得到反应产物；
(3)将步骤(2)得到的小块样品使用万能破碎机破碎，过200目筛后，得到最终的粉体。
本发明还对得到的粉体进行了图谱检测和Rietveld拟合，具体包括以下步骤：
S1将粉体使用X射线衍射(XRD)进行基本物相检测，如图1所示，标出了一系列的杂质相。
使用扫描电镜(SEM)进行微观形貌观测(如图2所示)并使用高分辨率透射电镜(HRTEM)确定晶体的结构类型。
S2将S1得到的XRD图谱进行识别，结合EDS/TEM得到的目标陶瓷粉体的晶格结构，用Materials Studio软件建立模型并进行结构优化得到Hf2TeB的稳定晶体结构，并与TEM图一一对应(如图3所示)。
S3将XRD图谱与步S2优化后的晶格模型作为输入参数，在Full-Prof软件中进行Rietveld拟合，得到的目标陶瓷粉体的Rietveld拟合图如图4所示，得到目标陶瓷粉体的晶格常数、原子位置(表1)以及不同晶面对应计算与实验的2θ、d、I值(表2)。
表1原子位置
表2不同晶面对应计算与实验的2θ、d、I值
如图1所示，实施例1所制备Hf2TeB的粉体X射线衍射具有一系列与MAX相硼化物Hf2SB和Hf2SeB相似的峰位，符合我们对它的预测。
如图2所示，实施例1所制备的粉体Hf2TeB具有一定的层状特征，可以观察到板条状的晶粒，即一定程度上具有典型的MAX相晶粒的特点。
如图3所示，实施例1所制备的粉体Hf2TeB的
面的TEM图，显示出明显的层状特征，也证明了其属于MAX相结构。
如图4所示，Hf2TeB样品的纯度为61.02wt％(其中含有27.17wt％的铪单质和11.81wt％的HfB2)，其可靠性因子在合理范围内R-P＝9.54％，R-WP＝13.60％。
实施例2
本实施例提供了一种含碲三元层状硼化物Hf2TeB的制备方法，包括以下步骤：
(1)将Hf粉(99.9％，400目)、Te粉(99.99％，200目)和硼粉(99％，2500目)按摩尔配比2:1.5:1称重，混合后于滚筒式混料机上混料15h至混合均匀，将混合均匀的物料再使用球磨研磨，得到均匀混合粉体；
(2)取步骤(1)所得到的均匀混合粉体25g放入到垫有石墨纸的石墨模具中，套上石墨毡，装载到SPS炉中，压力设置为20MPa，在真空下使用3℃/s的升温速率加热约150s，发生热爆炸烧结过程后，随炉冷却后得到反应产物；
(3)将步骤(2)得到的小块样品使用万能破碎机破碎，过200目筛后，得到最终的粉体。
实施例3
本实施例提供了一种含碲三元层状硼化物Hf2TeB的制备方法，包括以下步骤：
(1)将Hf粉(99.9％，400目)、Te粉(99.99％，200目)和硼粉(99％，2500目)按摩尔配比2:1:1称重，混合后于滚筒式混料机上混料10h至混合均匀，将混合均匀的物料再使用球磨研磨，得到均匀混合粉体；
(2)取步骤(1)所得到的均匀混合粉体25g放入到垫有石墨纸的石墨模具中，套上石墨毡，装载到SPS炉中，压力设置为22MPa，在真空下使用1℃/s的升温速率加热约400s，发生热爆炸烧结过程后，随炉冷却后得到反应产物；
(3)将步骤(2)得到的小块样品使用万能破碎机破碎，过200目筛后，得到最终的粉体。
本发明采用合适配比混合了Hf、Te、B粉，在设置的升温速率及压力下这些粉体会在SPS炉中发生热爆炸烧结，得到目标小块体的Hf2TeB，这些小块体经过万能破碎机破碎后得到目标粉体。
本发明涉及到的是一种新的三元层状化合物相(含碲三元层状硼化物)Hf2TeB及其制备方法，采用本发明方法成功制备出了新的MAX相Hf2TeB陶瓷，并给出了Hf2TeB的晶格结构参数和X射线衍射数据，是首次报道的含Te的MAX相，对于MAX相家族的完善有重大的意义。
虽然对本发明的具体实施方式进行了详细地描述，但不应理解为对本专利的保护范围的限定。在权利要求书所描述的范围内，本领域技术人员不经创造性劳动即可作出的各种修改和变形仍属本专利的保护范围。
Claims (6)
1.一种含碲三元层状硼化物的制备方法，其特征在于，包括以下步骤：
(1)将Hf粉、Te粉和B粉按照摩尔比2:1-5:1称重后混合均匀；
(2)将步骤(1)混匀后的粉体升温烧结，冷却后破碎，制得含碲三元层状硼化物的粉体。
2.如权利要求1所述的含碲三元层状硼化物的制备方法，其特征在于，所述混合的过程依次包括机械搅拌和球磨，所述机械搅拌的时间为10-15h。
3.如权利要求1所述的含碲三元层状硼化物的制备方法，其特征在于，所述粉体的粒径为过200目筛。
4.如权利要求1所述的含碲三元层状硼化物的制备方法，其特征在于，所述升温速率为1-3℃/s，所述烧结的温度为350-450℃，所述烧结的压力为18-22MPa。
5.采用权利要求1-4任一项所述的含碲三元层状硼化物的制备方法制备得到的含碲三元层状硼化物。
6.如权利要求5所述的含碲三元层状硼化物，其特征在于，所述含碲三元层状硼化物的化学式为Hf2TeB，所述Hf2TeB的空间群为P63/mmc，晶格参数分别为
其中Hf原子位于(1/3，2/3，0.57505)，Te原子位于(1/3，2/3，1/4)，B原子位于(0，0，0)。
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