CN115259853A - 一种高熵萤石氧化物靶材及其制备方法 - Google Patents
一种高熵萤石氧化物靶材及其制备方法 Download PDFInfo
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- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 title claims abstract description 43
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Abstract
本发明公开了一种高熵萤石氧化物靶材及其制备方法,S1、称取ZrO2、HfO2、CeO2、Y2O3、La2O3、Pr6O11粉末分别置于坩埚中,在马弗炉中煅烧以去除水分和杂质;S2、将煅烧后的ZrO2、HfO2、CeO2、Y2O3、La2O3、Pr6O11粉末混合置于行星式球磨机中,球磨结束后,将浆料置于干燥箱中烘干得到成分均匀的高熵陶瓷粉体;S3、将高熵陶瓷粉体造粒后依次放入液压机和冷等静压机机中压制得到陶瓷生胚;S4、将陶瓷生坯置于气氛烧结炉中,获得(ZrHfCeYLaPr)O2‑δ高熵陶瓷块体,随后对(ZrHfCeYLaPr)O2‑δ高熵陶瓷块体进行机械加工后清洗烘干,得到具有萤石结构的高熵氧化物靶材。本发明采用上述结构的一种高熵萤石氧化物靶材及其制备方法,使用等摩尔比的氧化物粉末,制备出纯度以及致密度较高的六组分高熵氧化物靶材。
Description
技术领域
本发明涉及高熵萤石氧化物靶材技术领域,特别是涉及一种高熵萤石氧化物靶材及其制备方法。
背景技术
近年来,高熵材料,特别是高熵合金和高熵陶瓷,引起了人们的极大兴趣。在高度无序、多组分的***中,高熵材料拥有优异的性质。高熵氧化物陶瓷是具有一个或多个Wyckoff位的无机化合物的固溶体,多主元素的原子比相等或接近相等。相比于其它陶瓷材料,高熵氧化物陶瓷具有更好的稳定性、机械性能、非晶态热导率以及超大介电常数、超离子电导率。高熵氧化物陶瓷在超音速飞行器的超高温热防护和隔热、锂离子电池的高速干切削、热电材料、催化剂、电磁波吸收和电磁干扰屏蔽等结构和功能领域具有广阔的应用前景。萤石型结构是一种具有面心立方晶格的单相结构,2017年,Djenadic等人首次制备了单相萤石结构高熵氧化物。
镀膜靶材是通过磁控溅射、多弧离子镀或其他类型的镀膜***在适当工艺条件下溅射在基板上形成各种功能薄膜的溅射源。其中,陶瓷靶材的纯度、强度以及致密度是溅射薄膜的性能的主要影响指标。通过高熵材料的性能可裁剪性,改变特定元素的组成以及比例,可以制备出不同结构和性质的高熵氧化物靶材。
发明内容
本发明的目的是提供一种高熵萤石氧化物靶材及其制备方法,使用等摩尔比的氧化物粉末,制备出纯度以及致密度较高的六组分高熵氧化物靶材。
为实现上述目的,本发明提供了一种高熵萤石氧化物靶材及其制备方法,高熵萤石氧化物靶材的制备方法如下:
S1、称取ZrO2、HfO2、CeO2、Y2O3、La2O3、Pr6O11粉末分别置于坩埚中,在马弗炉中煅烧以去除水分和杂质;
S2、将煅烧后的ZrO2、HfO2、CeO2、Y2O3、La2O3、Pr6O11粉末混合置于行星式球磨机中,球磨结束后,将浆料置于干燥箱中烘干得到成分均匀的高熵陶瓷粉体;
S3、将高熵陶瓷粉体造粒后依次放入液压机和冷等静压机机中压制得到陶瓷生胚;
S4、将陶瓷生坯置于气氛烧结炉中,获得(ZrHfCeYLaPr)O2-δ高熵陶瓷块体,随后对(ZrHfCeYLaPr)O2-δ高熵陶瓷块体进行机械加工后清洗烘干,得到具有萤石结构的高熵氧化物靶材。
优选的,S2中的所述高熵陶瓷粉体,ZrO2、HfO2、CeO2、Y2O3、La2O3、Pr6O11的摩尔比为1∶1∶1∶1∶1∶1。
优选的,S2中的所述高熵陶瓷粉体中,ZrO2、HfO2、CeO2、Y2O3、La2O3、Pr6O11的纯度为99.99%。
优选的,S1中马弗炉中煅烧温度为850℃,煅烧时间为2h。
优选的,S2中所述行星式球磨机以玛瑙球为研磨介质,乙醇为分散剂进行球磨,所述行星式球磨机中球料比为6:1,转速为250~300r/min,有效球磨的时间为6~8h,所述行星式球磨机在研磨时每研磨30min休息10min。
优选的,S2中浆料的烘干温度为60℃,烘干时间为12h。
优选的,S3中造粒使用的粘接剂为5wt%的PVA水溶液,粘接剂的用量为高熵陶瓷粉体体积的8%。
优选的,S3中所述液压机的压力为200~250Mpa,压力保持时间为3~5min,所述冷等静压机的压力为250~300Mpa,压力保持时间为15~20min。
优选的,S4中热处理温度为1200~1600℃,热处理时间大于等于2h。
因此,本发明采用上述结构的一种高熵萤石氧化物靶材及其制备方法,使用等摩尔比的氧化物粉末,制备出纯度以及致密度较高的高熵氧化物靶材。
下面通过附图和实施例,对本发明的技术方案做进一步的详细描述。
附图说明
图1是本发明一种高熵萤石氧化物靶材及其制备方法实施例1的X射线衍射图;
图2是本发明一种高熵萤石氧化物靶材及其制备方法对比例1的X射线衍射图。
具体实施方式
以下通过附图和实施例对本发明的技术方案作进一步说明。
除非另外定义,本发明使用的技术术语或者科学术语应当为本发明所属领域内具有一般技能的人士所理解的通常意义。本发明中使用的“第一”、“第二”以及类似的词语并不表示任何顺序、数量或者重要性,而只是用来区分不同的组成部分。“包括”或者“包含”等类似的词语意指出现该词前面的元件或者物件涵盖出现在该词后面列举的元件或者物件及其等同,而不排除其他元件或者物件。“连接”或者“相连”等类似的词语并非限定于物理的或者机械的连接,而是可以包括电性的连接,不管是直接的还是间接的。“上”、“下”、“左”、“右”等仅用于表示相对位置关系,当被描述对象的绝对位置改变后,则该相对位置关系也可能相应地改变。
图1是本发明一种高熵萤石氧化物靶材及其制备方法实施例1的X射线衍射图,图2是本发明一种高熵萤石氧化物靶材及其制备方法对比例1的X射线衍射图,如图所示,一种高熵萤石氧化物靶材及其制备方法,S1、称取ZrO2、HfO2、CeO2、Y2O3、La2O3、Pr6O11粉末分别置于坩埚中,在马弗炉中煅烧温度为850℃,煅烧时间为2h。煅烧以去除水分和杂质,降低水分和杂质对高熵萤石氧化物产生的不利影响。
S2、将煅烧后的ZrO2、HfO2、CeO2、Y2O3、La2O3、Pr6O11粉末混合置于行星式球磨机中,以玛瑙球为研磨介质,乙醇为分散剂进行球磨,球料比为6:1。行星式球磨机的转速为250~300r/min,正反向交替间隔运行,有效球磨的时间为6~8h,行星式球磨机在研磨时每研磨30min休息10min。
球磨结束后,将浆料置于60℃干燥箱中烘干12h得到成分均匀的高熵陶瓷粉体。高熵陶瓷粉体中,ZrO2、HfO2、CeO2、Y2O3、La2O3、Pr6O11的摩尔比为1∶1∶1∶1∶1∶1,ZrO2、HfO2、CeO2、Y2O3、La2O3、Pr6O11的纯度为99.99%。
S3、将高熵陶瓷粉体造粒后依次放入液压机和冷等静压机机中压制得到陶瓷生胚,造粒使用的粘接剂为5wt%的PVA水溶液,粘接剂的用量为高熵陶瓷粉体体积的8%。液压机的压力为200~250Mpa,压力保持时间为3~5min,冷等静压机的压力为250~300Mpa,压力保持时间为15~20min。
S4、将陶瓷生坯置于气氛烧结炉中,热处理温度为1200~1600℃,热处理时间大于等于2h,获得(ZrHfCeYLaPr)O2-δ高熵陶瓷块体。随后对(ZrHfCeYLaPr)O2-δ高熵陶瓷块体进行机械加工后清洗烘干,得到具有萤石结构的高熵氧化物靶材。
实施例1
S1、称取等摩尔比的ZrO2、HfO2、CeO2、Y2O3、La2O3、Pr6O11粉末分别置于坩埚中,在马弗炉中850℃煅烧2h。
S2、煅烧后的ZrO2、HfO2、CeO2、Y2O3、La2O3、Pr6O11粉末混合置于行星式球磨罐中,以玛瑙球为研磨介质,乙醇为分散剂进行球磨,球料比6:1。行星式球磨机正反向交替间隔运行的转速为250r/min,交替运行时间为20min,交替运行间隔停机时间为10min。
球磨结束后,将浆料与玛瑙球分离,浆料置于60℃干燥箱中烘干12h得到成分均匀的高熵陶瓷粉体。随后将高熵陶瓷粉体置于玛瑙研钵中造粒,一边手工研磨一边滴加5wt%的PVA水溶液,粘接剂的用量为高熵陶瓷粉体体积的8%。
S3、将造粒后的高熵陶瓷粉体置于模具中,利用液压机施加压力到200Mpa,保压3min。随后置于冷等静压机中,以50MPa/min升压至250MPa,保压15min,再以50MPa/min降为0Mpa,得到陶瓷生胚。
S4、将陶瓷生坯置于气氛烧结炉中,以2℃/min的速率缓慢排胶,随后在800℃保温2h,以5℃/min的速率升温至1200℃,2℃/min的速率升温至1600℃,保温4h。保温结束后2℃/min的速率降温至1200℃,5℃/min的速率降温至500℃后随炉冷却。对(ZrHfCeYLaPr)O2-δ高熵陶瓷块体进行机械加工后清洗烘干,由图1可知,最终获得了一种单相萤石结构的高熵氧化物靶材。
对比例1
S1、称取等摩尔比的ZrO2、HfO2、CeO2、Y2O3、Sc2O3、Pr6O11粉末分别置于坩埚中,在马弗炉中850℃煅烧2h。
S2、煅烧后的ZrO2、HfO2、CeO2、Y2O3、Sc2O3、Pr6O11粉末混合置于行星式球磨罐中,以玛瑙球为研磨介质,乙醇为分散剂进行球磨,球料比6:1。行星式球磨机正反向交替间隔运行的转速为250r/min,交替运行时间为20min,交替运行间隔停机时间为10min。
球磨结束后,将浆料与玛瑙球分离,浆料置于60℃干燥箱中烘干12h得到成分均匀的高熵陶瓷粉体。随后将高熵陶瓷粉体置于玛瑙研钵中造粒,一边手工研磨一边滴加5wt%的PVA水溶液,粘接剂的用量为高熵陶瓷粉体体积的8%。
S3、将造粒后的高熵陶瓷粉体置于模具中,利用液压机施加压力到200Mpa,保压3min。随后置于冷等静压机中,以50MPa/min升压至250MPa,保压15min,再以50MPa/min降为0Mpa,得到陶瓷生胚。
S4、将陶瓷生坯置于气氛烧结炉中,以2℃/min的速率缓慢排胶,随后在800℃保温2h,以5℃/min的速率升温至1200℃,2℃/min的速率升温至1600℃,保温4h。保温结束后2℃/min的速率降温至1200℃,5℃/min的速率降温至500℃后随炉冷却。对(ZrHfCeYLaPr)O2-δ高熵陶瓷块体进行机械加工后清洗烘干,由图2可知,最终获得了一种单相萤石结构的高熵氧化物靶材。
表1为高熵氧化物靶材的性能数据表
组分 | 是否单相 | 致密度 | |
实施例1 | (ZrHfCeYLaPr)O | 是 | 97.70% |
对比例1 | (ZrHfCeYScPr)O | 是 | 90.80% |
由表1可知,实施例1中的高熵萤石氧化物靶材的结构以及致密度优于对比例1中的高熵萤石氧化物靶材的结构以及致密度。
因此,本发明采用上述结构的一种高熵萤石氧化物靶材及其制备方法,使用等摩尔比的氧化物粉末,制备出纯度以及致密度较高的高熵氧化物靶材。
最后应说明的是:以上实施例仅用以说明本发明的技术方案而非对其进行限制,尽管参照较佳实施例对本发明进行了详细的说明,本领域的普通技术人员应当理解:其依然可以对本发明的技术方案进行修改或者等同替换,而这些修改或者等同替换亦不能使修改后的技术方案脱离本发明技术方案的精神和范围。
Claims (9)
1.一种高熵萤石氧化物靶材及其制备方法,其特征在于:高熵萤石氧化物靶材的制备方法如下:
S1、称取ZrO2、HfO2、CeO2、Y2O3、La2O3、Pr6O11粉末分别置于坩埚中,在马弗炉中煅烧以去除水分和杂质;
S2、将煅烧后的ZrO2、HfO2、CeO2、Y2O3、La2O3、Pr6O11粉末混合置于行星式球磨机中,球磨结束后,将浆料置于干燥箱中烘干得到成分均匀的高熵陶瓷粉体;
S3、将高熵陶瓷粉体造粒后依次放入液压机和冷等静压机机中压制得到陶瓷生胚;
S4、将陶瓷生坯置于气氛烧结炉中,获得(ZrHfCeYLaPr)O2-δ高熵陶瓷块体,随后对(ZrHfCeYLaPr)O2-δ高熵陶瓷块体进行机械加工后清洗烘干,得到具有萤石结构的高熵氧化物靶材。
2.根据权利要求1所述的一种高熵萤石氧化物靶材及其制备方法,其特征在于:S2中的所述高熵陶瓷粉体,ZrO2、HfO2、CeO2、Y2O3、La2O3、Pr6O11的摩尔比为1∶1∶1∶1∶1∶1。
3.根据权利要求1所述的一种高熵萤石氧化物靶材及其制备方法,其特征在于:S2中的所述高熵陶瓷粉体中,ZrO2、HfO2、CeO2、Y2O3、La2O3、Pr6O11的纯度为99.99%。
4.根据权利要求1所述的一种高熵萤石氧化物靶材及其制备方法,其特征在于:S1中马弗炉中煅烧温度为850℃,煅烧时间为2h。
5.根据权利要求1所述的一种高熵萤石氧化物靶材及其制备方法,其特征在于:S2中所述行星式球磨机以玛瑙球为研磨介质,乙醇为分散剂进行球磨,所述行星式球磨机中球料比为6:1,转速为250~300r/min,有效球磨的时间为6~8h,所述行星式球磨机在研磨时每研磨30min休息10min。
6.根据权利要求1所述的一种高熵萤石氧化物靶材及其制备方法,其特征在于:S2中浆料的烘干温度为60℃,烘干时间为12h。
7.根据权利要求1所述的一种高熵萤石氧化物靶材及其制备方法,其特征在于:S3中造粒使用的粘接剂为5wt%的PVA水溶液,粘接剂的用量为高熵陶瓷粉体体积的8%。
8.根据权利要求1所述的一种高熵萤石氧化物靶材及其制备方法,其特征在于:S3中所述液压机的压力为200~250Mpa,压力保持时间为3~5min,所述冷等静压机的压力为250~300Mpa,压力保持时间为15~20min。
9.根据权利要求1所述的一种高熵萤石氧化物靶材及其制备方法,其特征在于:S4中热处理温度为1200~1600℃,热处理时间大于等于2h。
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