CN114560699A - 一种中高熵陶瓷材料及其制备方法与应用 - Google Patents
一种中高熵陶瓷材料及其制备方法与应用 Download PDFInfo
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- 229910052691 Erbium Inorganic materials 0.000 claims abstract description 13
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 13
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- 239000000126 substance Substances 0.000 claims abstract description 11
- 229910052693 Europium Inorganic materials 0.000 claims abstract description 10
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 10
- 229910052772 Samarium Inorganic materials 0.000 claims abstract description 10
- 229910052775 Thulium Inorganic materials 0.000 claims abstract description 10
- 229910052692 Dysprosium Inorganic materials 0.000 claims abstract description 9
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 8
- 229910052688 Gadolinium Inorganic materials 0.000 claims abstract description 8
- 229910052689 Holmium Inorganic materials 0.000 claims abstract description 8
- 229910052771 Terbium Inorganic materials 0.000 claims abstract description 8
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 8
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Abstract
本发明公开了一种中高熵陶瓷材料及其制备方法与应用。所述中高熵陶瓷材料具有的化学通式为RExByCz,其中RE为Sc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu中的任意三种及以上的组合,x:y:z选自1:1:1、1:2:1、1:2:2中的任一者。本发明提供的中高熵陶瓷材料具有优异地热学、电学、磁学、光学及力学等性能,可应用于中子吸收材料、中子屏蔽材料、超导材料、磁性材料、电磁屏蔽材料、吸波材料、结构材料等领域。
Description
技术领域
本发明属于新材料技术领域,具体涉及一种中高熵陶瓷材料及其制备方法与应用。
背景技术
“高熵”是一种新型的材料设计理念,其概念最初是源于中国台湾学者叶均蔚教授提出的高熵合金。随着研究的深入,高熵的概念逐步拓展到高熵玻璃、高熵陶瓷、高熵热电材料、高熵聚合物材料等。高熵陶瓷通常是指五种或以上陶瓷组元形成的多组元单相固溶体,因其独特的高熵效应及优越的性能,近年来已经成为陶瓷领域的热点之一。其设计原理是基于通过增加化合物中的构型熵来降低系统的吉布斯自由能,从而获得具有高强度、高硬度、高导电性、低导热和优良的抗氧化性的陶瓷材料。构型熵通常可以表示为:
其中kB为玻尔兹曼常数,xi为i组分的摩尔分数,n表示组元数。由公式可知材料的构型熵主要与所含组分数目及各组分所占的摩尔分数有关,即材料的组成成分越多,各组分所占的摩尔数越接近,材料的构型熵越大。根据材料的构型熵的大小可将材料分为低熵(s<0.69R)、中熵(0.69R≤s≤1.61R)、高熵(s>1.61R)材料。目前合成出来的高熵陶瓷主要有萤石结构、钙钛矿结构、尖晶石结构的高熵氧化物陶瓷以及硼化物、碳化物、氮化物、硅化物等非氧化物高熵陶瓷。而关于稀土硼碳化合物的中高熵陶瓷未见有报道。
稀土元素具有特殊的磁学、光学、电学等性质,在超导材料,催化材料,磁性材料,能源材料,陶瓷材料等领域具有广泛的应用前景。因此开发一种新型的中高熵陶瓷材料是亟待解决的问题。
发明内容
本发明的主要目的在于提供一种中高熵陶瓷材料及其制备方法与应用,以克服现有技术的不足。
为实现前述发明目的,本发明采用的技术方案包括:
本发明实施例提供了一种中高熵陶瓷材料,所述中高熵陶瓷材料具有的化学通式为RExByCz,其中RE为Sc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu中的任意三种及以上的组合,x:y:z选自1:1:1、1:2:1、1:2:2中的任一者。
在一些较为具体的实施方案中,当x:y:z为1:2:2时,所述中高熵陶瓷材料的具有的化学通式为RE1B2C2,其中REi=Sc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu,xi为REi组分在RE中的摩尔常数,n=3~17。
本发明实施例还提供了前述的中高熵陶瓷材料的制备方法,其包括:采用熔盐法或固相反应法中的任意一种方法制得中高熵陶瓷材料。
本发明实施例还提供了前述的中高熵陶瓷材料于制备中子吸收材料、中子屏蔽材料、超导材料、磁性材料、电磁屏蔽材料、吸波材料或结构材料中的用途。
与现有技术相比,本发明的有益效果在于:
(1)本发明首次制得一种新型的RExByCz中高熵陶瓷材料;
(2)本发明的中高熵陶瓷材料由性质丰富的稀土元素组成,将会赋予中高熵陶瓷材料诸多的新性能,如热学、电学、磁学、光学及力学等性能;
(3)中高熵陶瓷材料相比于传统陶瓷,具有热力学的高熵效应、结构的晶格畸变效应、动力学的迟滞扩散效应以及性能上的“鸡尾酒”效应,有利于提高中高熵陶瓷材料的相稳定性以及性能的协同增强作用;
(4)本发明的中高熵陶瓷材料具有高中子吸收截面的稀土元素与B元素的共同作用,有助于提高本发明的中高熵陶瓷材料的中子和γ射线屏蔽能力,具有热中子俘获截面大、耐辐照、轻毒、无弱吸收区等优点,可在核能及放射医疗等中子屏蔽或中子吸收材料领域而应用。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明中记载的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。
图1是本发明实施例1中制备的(Y0.25Yb0.25Er0.25Dy0.25)B2C2陶瓷材料的XRD图;
图2是本发明实施例1中制备的(Y0.25Yb0.25Er0.25Dy0.25)B2C2陶瓷材料的SEM图;
图3a-图3d是本发明实施例1中制备的(Y0.25Yb0.25Er0.25Dy0.25)B2C2陶瓷材料的EDS图。
具体实施方式
鉴于现有技术的缺陷,本案发明人经长期研究和大量实践,得以提出本发明的技术方案,下面将对本发明的技术方案进行清楚、完整地描述,显然,所描述的实施例是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
具体的,作为本发明技术方案的一个方面,其所涉及的一种中高熵陶瓷材料具有的化学通式为RExByCz,其中RE为Sc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu稀土元素中的任意三种及以上的组合,x:y:z选自1:1:1、1:2:1、1:2:2中的任一者。
在一些优选实施方案中,当x:y:z为1:2:2时,所述中高熵陶瓷材料的具有的化学通式为RE1B2C2,其中REi=Sc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu,xi为REi组分在RE中的摩尔常数,n=3~17。
进一步地,所述中高熵陶瓷材料的空间群为P4/mbm,所述中高熵陶瓷材料的晶胞由稀土原子层与B-C层交替堆叠而成。
本发明实施例的另一个方面还提供了前述的中高熵陶瓷材料的制备方法,其包括:采用熔盐法或固相反应法中的任意一种方法制得中高熵陶瓷材料。
在一些优选实施方案中,所述制备方法包括:在保护性气氛和/或真空条件下,使包含至少三种不同的含稀土元素材料、含硼材料和含碳材料的混合物,采用熔盐法或固相反应法在600-2000℃反应制得所述中高熵陶瓷材料。
进一步地,所述含稀土元素材料包括稀土元素单质、稀土元素氢化物、稀土元素氧化物、稀土元素碳化物、稀土元素硼化物中的任意一种或两种以上的组合,且不限于此。
进一步地,所述含硼材料包括硼单质、碳化硼、氧化硼、硼酸、硼烷、碳硼烷中的任意一种或两种以上的组合,且不限于此。
进一步地,所述含碳材料包括碳单质、酚醛树脂、葡萄糖、淀粉中的任意一种或两种以上的组合,且不限于此。
进一步地,所述至少三种不同的含稀土元素材料、含硼材料与含碳材料的摩尔比为1~10:1~10:1~10。
进一步地,所述混合物中各种含稀土元素材料的物质的量相同。
在一些更为具体的实施方案中,所述中高熵陶瓷材料的制备方法包括:取三种或三种以上的含稀土元素材料,硼单质或者含硼化合物,碳单质或含碳化合物,按照目标相RExByCz各元素比例混合,在一定温度和气氛保护或者真空条件下,采用熔盐法或者固相反应法获得中高熵陶瓷材料。
作为优选,所述三种或三种以上的含稀土元素材料按照等摩尔比或者接近等摩尔比混合。
本发明实施例的另一个方面还提供了前述的中高熵陶瓷材料于制备中子吸收材料、中子屏蔽材料、超导材料、磁性材料、电磁屏蔽材料、吸波材料、结构材料中的用途。
下面结合若干优选实施例及附图对本发明的技术方案做进一步详细说明,本实施例在以发明技术方案为前提下进行实施,给出了详细的实施方式和具体的操作过程,但本发明的保护范围不限于下述的实施例。
下面所用的实施例中所采用的实验材料,如无特殊说明,均可由常规的生化试剂公司购买得到。
实施例1
本实施例中,中高熵陶瓷材料为(Y0.25Yb0.25Er0.25Dy0.25)B2C2陶瓷材料,该(Y0.25Yb0.25Er0.25Dy0.25)B2C2陶瓷材料的制备方法如下:
(1)取稀土元素Y、Yb、Er、Dy的稀土氢化物,等摩尔量进行称量。将稀土氢化物混合物与B4C与碳粉按照2:1:3的摩尔比混合。
(2)所得混合物于惰性气氛中采用放电等离子烧结技术,在1800℃固相反应烧结10min,获得中高熵陶瓷材料,即:(Y0.25Yb0.25Er0.25Dy0.25)B2C2陶瓷材料。
图1为实施例中(Y0.25Yb0.25Er0.25Dy0.25)B2C2陶瓷材料的XRD图,可以看出(Y0.25Yb0.25Er0.25Dy0.25)B2C2陶瓷材料的XRD特征峰与单稀土元素硼碳化合物极为接近。因此,可以证明成功合成了(Y0.25Yb0.25Er0.25Dy0.25)B2C2陶瓷材料。图2为高(Y0.25Yb0.25Er0.25Dy0.25)B2C2陶瓷材料的SEM图。由微观形貌可以看出,(Y0.25Yb0.25Er0.25Dy0.25)B2C2陶瓷材料具有明显的层状结构;能谱分析(如图3a-图3d所示)进一步验证了四种稀土元素在(Y0.25Yb0.25Er0.25Dy0.25)B2C2陶瓷材料中能够均匀分布,符合实验设计与XRD分析结果。
实施例2
本实施例中,中高熵陶瓷材料为(Y0.25Ho0.25Er0.25Yb0.25)B2C2陶瓷材料。该(Y0.25Ho0.25Er0.25Yb0.25)B2C2陶瓷材料的制备方法如下:
(1)取稀土元素Y、Ho、Er、Yb的稀土氢化物,等摩尔量进行称量。将稀土氢化物混合物与B4C与碳粉按照2:1:3的摩尔比混合。
(2)所得混合物于惰性气氛中采用放电等离子烧结技术,在1800℃反应烧结10min,获得中高熵陶瓷材料,即:(Y0.25Ho0.25Er0.25Yb0.25)B2C2陶瓷材料。
实施例3
本实施例中,中高熵陶瓷材料为(La0.2Ce0.2Nd0.2Sm0.2Eu0.2)B2C2陶瓷材料。该(La0.2Ce0.2Nd0.2Sm0.2Eu0.2)B2C2陶瓷材料的制备方法如下:
(1)取稀土元素La、Ce、Nd、Sm、Eu的稀土氢化物,等摩尔量进行称量。将稀土氢化物混合物与B4C与碳粉按照2:1:3的摩尔比混合。
(2)所得混合物放入球磨罐中,在球磨机上进行球磨处理,使反应物粉末充分接触,得到预制粉末。
(3)取适量球磨粉末于石墨模具内,然后放置在真空热压烧结炉内进行烧结成型,同时在烧结过程不断抽真空使烧结炉内压强始终保持低于0.1Pa,得到原位合成的中高熵陶瓷材料,即:(La0.2Ce0.2Nd0.2Sm0.2Eu0.2)B2C2的块体材料。
实施例4
本实施例中,中高熵陶瓷材料为(Er0.25Tm0.25Yb0.25Lu0.25)B2C2陶瓷材料。该(Er0.25Tm0.25Yb0.25Lu0.25)B2C2陶瓷材料的制备方法如下:
(1)取稀土元素Er、Tm、Yb、Lu的稀土氢化物,等摩尔量进行称量。将稀土氢化物混合物与B4C与碳粉按照2:1:3的摩尔比混合,以NaCl为助熔剂,加入原料质量4倍的NaCl。
(2)将样品置于氧化铝球磨罐中,酒精为球磨介质,氧化锆为球磨子,球磨4h。干燥后,得到充分混合的粉末。
(3)将混合物粉末置于氧化铝坩埚中,升温至1100℃热处理4h,利用蒸馏水将反应后的熔盐混合物中的盐溶解,充分洗涤过滤,然后置于真空烘箱干燥,得到中高熵陶瓷材料,即:(Er0.25Tm0.25Yb0.25Lu0.25)B2C2陶瓷材料。
实施例5
本实施例中,中高熵陶瓷材料为(Nd0.2Sm0.2Eu0.2Y0.2Yb0.2)B2C2陶瓷材料。该(Nd0.2Sm0.2Eu0.2Y0.2Yb0.2)B2C2陶瓷材料的制备方法如下:
(1)取稀土元素Nd、Sm、Eu、Y、Yb的稀土氢化物,等摩尔量进行称量。将稀土氢化物混合物与B4C与碳粉按照2:1:3的摩尔比混合。
(2)所得混合物放入球磨罐中,在球磨机上进行球磨处理,使反应物粉末充分接触,得到预制粉末。
(3)取适量球磨粉末于石墨模具内,保护气氛下放置在放电等离子烧结炉中进行烧结。1700℃烧结10min,得到中高熵陶瓷材料,即:(Nd0.2Sm0.2Eu0.2Y0.2Yb0.2)B2C2陶瓷材料。
实施例6
本实施例中,中高熵陶瓷材料为(Gd1/6Tb1/6Dy1/6Tm1/6Yb1/6Lu1/6)B2C2陶瓷材料。该Gd1/6Tb1/6Dy1/6Tm1/6Yb1/6Lu1/6)B2C2陶瓷材料的制备方法如下:
(1)取稀土元素Gd、Tb、Dy、Tm、Yb、Lu的稀土氢化物,等摩尔量进行称量。将稀土氢化物混合物与B4C与碳粉按照2:1:3的摩尔比混合。
(2)所得混合物放入球磨罐中,在球磨机上进行球磨处理,使反应物粉末充分接触,得到预制粉末。
(3)取适量球磨粉末于石墨模具内,保护气氛下放置在放电等离子烧结炉中进行烧结。1900℃烧结10min,得到中高熵陶瓷材料,即:Gd1/6Tb1/6Dy1/6Tm1/6Yb1/6Lu1/6)B2C2陶瓷材料。
实施例7
本实施例中,中高熵陶瓷材料为(Y0.2Yb0.2Lu0.2Eu0.2Er0.2)B2C2陶瓷材料。该(Y0.2Yb0.2Lu0.2Eu0.2Er0.2)B2C2陶瓷材料的制备方法如下:
(1)取稀土元素Y、Yb、Lu、Eu、Er的稀土氢化物,等摩尔量进行称量。将稀土氢化物混合物与B4C与碳粉按照2:1:3的摩尔比混合。
(2)所得混合物放入球磨罐中,在球磨机上进行球磨处理,使反应物粉末充分接触,得到预制粉末。
(3)取适量球磨粉末于石墨模具内,保护气氛下放置在放电等离子烧结炉中进行烧结。1800℃烧结120min,得到中高熵陶瓷材料,即:(Y0.2Yb0.2Lu0.2Eu0.2Er0.2)B2C2陶瓷材料。
实施例8
本实施例中,中高熵陶瓷材料为(Yb0.25Y0.25Lu0.25Er0.25)B2C2陶瓷材料。该(Yb0.25Y0.25Lu0.25Er0.25)B2C2陶瓷材料的制备方法如下:
(1)取稀土元素Yb、Y、Lu、Er的稀土氢化物,等摩尔量进行称量。将稀土氧化物混合物与B4C与碳粉按照2:1:3的摩尔比混合。
(2)所得混合物放入球磨罐中,在球磨机上进行球磨处理,使反应物粉末充分接触,得到预制粉末。
(3)取适量球磨粉末于石墨模具内,保护气氛下放置在放电等离子烧结炉中进行烧结。1500℃烧结10min,得到中高熵陶瓷材料,即:(Yb0.25Y0.25Lu0.25Er0.25)B2C2陶瓷材料。
实施例9
本实施例中,中高熵陶瓷材料为(Tm0.25Yb0.25Lu0.25)B2C2陶瓷材料。该(Tm0.25Yb0.25Lu0.25)B2C2陶瓷材料的制备方法如下:
(1)取稀土元素Tm、Yb、Lu的稀土氢化物,等摩尔量进行称量。将稀土氢化物混合物与B4C与碳粉按照2:1:3的摩尔比混合。
(2)所得混合物放入球磨罐中,在球磨机上进行球磨处理,使反应物粉末充分接触,得到预制粉末。
(3)取适量球磨粉末于石墨模具内,保护气氛下放置在放电等离子烧结炉中进行烧结。1800℃烧结10min,得到中高熵陶瓷材料,即:(Tm0.25Yb0.25Lu0.25)B2C2陶瓷材料。
实施例10
本实施例中,中高熵陶瓷材料为(Y0.2Nd0.2Sm0.2Eu0.2Er0.2)B2C2陶瓷材料。该(Y0.2Nd0.2Sm0.2Eu0.2Er0.2)B2C陶瓷材料的制备方法如下:
(1)取稀土元素Y、Nd、Sm、Eu、Er的稀土氢化物,等摩尔量进行称量。将稀土氢化物混合物与B4C与碳粉按照2:1:3的摩尔比混合。
(2)所得混合物放入球磨罐中,在球磨机上进行球磨处理,使反应物粉末充分接触,得到预制粉末。
(3)取适量球磨粉末于石墨模具内,保护气氛下放置在放电等离子烧结炉中进行烧结。1600℃烧结10min,得到中高熵陶瓷材料,即:(Y0.2Nd0.2Sm0.2Eu0.2Er0.2)B2C陶瓷材料。
此外,本案发明人还参照前述实施例,以本说明书述及的其它原料、工艺操作、工艺条件进行了试验,并均获得了较为理想的结果。
应当理解,本发明的技术方案不限于上述具体实施案例的限制,凡是在不脱离本发明宗旨和权利要求所保护的范围情况下,根据本发明的技术方案做出的技术变形,均落于本发明的保护范围之内。
Claims (10)
1.一种中高熵陶瓷材料,其特征在于,所述中高熵陶瓷材料具有的化学通式为RExByCz,其中RE为Sc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu中的任意三种及以上的组合,x:y:z选自1:1:1、1:2:1、1:2:2中的任一者。
3.根据权利要求2所述的中高熵陶瓷材料,其特征在于:所述中高熵陶瓷材料的空间群为P4/mbm,所述中高熵陶瓷材料的晶胞由稀土原子层与B-C层交替堆叠而成。
4.权利要求1-3中任一项所述的中高熵陶瓷材料的制备方法,其特征在于包括:采用熔盐法或固相反应法中的任意一种方法制得中高熵陶瓷材料。
5.根据权利要求4所述的制备方法,其特征在于包括:在保护性气氛和/或真空条件下,使包含至少三种不同的含稀土元素材料、含硼材料和含碳材料的混合物,于600~2000℃采用熔盐法或固相反应法反应制得所述中高熵陶瓷材料。
6.根据权利要求5所述的制备方法,其特征在于:所述含稀土元素材料包括稀土元素单质、稀土元素氢化物、稀土元素氧化物、稀土元素碳化物、稀土元素硼化物中的任意一种或两种以上的组合。
7.根据权利要求5所述的制备方法,其特征在于:所述含硼材料包括硼单质、碳化硼、氧化硼、硼酸、硼烷、碳硼烷中的任意一种或两种以上的组合。
8.根据权利要求5所述的制备方法,其特征在于:所述含碳材料包括碳单质、酚醛树脂、葡萄糖、淀粉中的任意一种或两种以上的组合。
9.根据权利要求5所述的制备方法,其特征在于:所述至少三种不同的含稀土元素材料、含硼材料与含碳材料的摩尔为1~10:1~10:1~10;
和或,所述混合物中各种含稀土元素材料的物质的量相同。
10.权利要求1-3中任一项所述的中高熵陶瓷材料于制备中子吸收材料、中子屏蔽材料、超导材料、磁性材料、电磁屏蔽材料、吸波材料或结构材料中的用途。
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