CN113429213A - 一种具有尖晶石结构的高发射率红外节能高熵材料的制备方法 - Google Patents

一种具有尖晶石结构的高发射率红外节能高熵材料的制备方法 Download PDF

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CN113429213A
CN113429213A CN202110805503.6A CN202110805503A CN113429213A CN 113429213 A CN113429213 A CN 113429213A CN 202110805503 A CN202110805503 A CN 202110805503A CN 113429213 A CN113429213 A CN 113429213A
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王刚
王曲
张琪
刘鹏程
王来稳
杜鹏辉
梁鹏鹏
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Sinosteel Luoyang Institute of Refractories Research Co Ltd
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Abstract

本发明提供了一种具有尖晶石结构的高发射率红外节能高熵材料的制备方法，属于红外节能技术领域。所述制备具有尖晶石结构的高发射率红外节能高熵材料以尖晶石结构（A3O4结构）为主相，A位为Co、Cr、Fe、Mn、Ni、Mg、Cu、Zn、Al的三种到五种金属元素。该材料的发射率在0.80‑0.95。所述的制备方法为高温固相合成法。本发明的具有尖晶石结构的高发射率红外节能高熵材料的有益效果是：发射率最高达0.95、低热导、良好的高温稳定性，在热工窑炉节能领域具有巨大的潜力。

Description

一种具有尖晶石结构的高发射率红外节能高熵材料的制备 方法
技术领域
本发明属于红外节能技术领域，具体涉及一种具有尖晶石结构的高发射率红外节能高熵材料的制备方法。
背景技术
近年来，已经研究了各种高熵陶瓷以及他们的结构和性质，如氧化物，碳化物，硼化物，氮化物和硅化物等。在这些晶体高熵陶瓷中，高熵氧化物由于应用潜力，引起了极大的研究兴趣，如岩盐、尖晶石、钙钛矿和萤石。
从热工技术的角度看，在大于800℃的高温环境下，辐射传热在向工件的三种传热方式中（辐射、对流、传导）的理论占比超过 80%，是决定高温炉窑热工效率的主导因素。因此，强化辐射传热是实现热工炉窑节能的必由之路。高熵材料晶格中不同原子质量、原子半径元素的相互掺杂，使晶格的非线性振动增强，从而减小声子的平均自由程，进一步加剧声子间的散射作用，导致热导率较低。近红外高发射率材料主要是通过掺杂不同价态和价键结构的离子，在局部形成杂质能级，从而达到提高发射率的目的。因此，制备出兼具高发射率和低热导的高熵材料是解决窑炉节能领域的关键问题。
发明内容
本发明的目的主要是提供一种具有尖晶石结构的高发射率红外节能高熵材料的制备方法，使其能兼具高发射率和低热导的特性，解决窑炉节能领域的关键问题。
本发明目的是通过以下技术方案实现的：
根据半导体能带理论，在近红外波段内起主导作用的吸收机制是光-电跃迁吸收，通过掺杂不同价态和价键结构的离子，在局部形成杂质能级，增强自由载流子由价带到导带跃迁的可能性，促进价带中的自由载流子（电子、空穴等）浓度的增加及带隙间的跃迁，从而提高近红外发射率；由于Cr、Mn、Fe、Co、Ni均为多价态原子，契合了制备近红外高发射率材料的掺杂条件。
一种具有尖晶石结构的高发射率红外节能高熵材料的制备方法，制备方法包括以下步骤：
一种具有尖晶石结构的高发射率红外节能高熵材料及其制备方法，其特征在于，包括以下步骤，
（1）（1）配料：将具有尖晶石结构的高发射率红外节能高熵材料的原料进行配料，按照A位金属原子Co、Cr、Fe、Mn、Ni、Mg、Cu、Zn、Al摩尔比为1:1:1或1:1:1:1或1:1:1:1:1的比例分别称取3种到5种金属氧化物粉体，所述金属氧化物粉体的为氧化钴、氧化铬、氧化铁、氧化锰、氧化镍、氧化铜、氧化镁、氧化锌、氧化铝中的3种到5种；
（2）对步骤（1）中称取的粉体进行球磨；
（3）煅烧：将步骤（1）配料后的原料在900~1400℃的空气气氛中煅烧180~1200min，使其发生高温固相反应，最终制备得到具有尖晶石结构的高发射率红外节能高熵材料的粉体。
所述步骤2中的球磨采用行星式球磨，球磨时间为4～20h。
所述的具有尖晶石结构的高发射率红外节能高熵材料的发射率为0.80~0.95。
本发明提供的一种具有尖晶石结构的高发射率红外节能高熵材料；本发明制备具有尖晶石结构的高发射率红外节能高熵材料时，由于Cr、Mn、Fe、Co、Ni均为多价态原子，在高温固相反应中部分氧原子溢出形成氧空位，为了保持电荷平衡，部分离子将发生变价，从而在局部形成杂质能级，增强杂质吸收和自由载流子吸收，从而提高材料的发射率。
本发明具有尖晶石结构的高发射率红外节能高熵材料的有益效果是：
（1）本发明所制备的具有尖晶石结构的高发射率红外节能高熵材料的发射率最高可达0.93，高于现有高温氧化物体系红外节能材料的发射率。
（2）晶格中不同原子质量、原子半径元素的相互掺杂，使晶格的非线性振动增强，从而减小声子的平均自由程，进一步加剧声子间的散射作用，导致热导率较低。
（3）本发明所制备的具有尖晶石结构的高发射率红外节能高熵材料的原料易得，制备工艺简单，生产成本低，易于工业生产。
附图说明
图1为实施例1中(CoCrFeMnNi)3O4高熵氧化物的X射线衍射图谱。
图2为实施例1中(CoCrFeMnNi)3O4高熵氧化物在近红外（0.76~2.5 μm）波段的发射率图谱。
具体实施方式
下面结合具体实例对本发明做进一步的说明，但不应以此限制本发明的保护范围。
结合附图和具体实施例对本发明加以说明：
实施例1：把氧化钴、氧化铬、氧化铁、氧化锰、氧化镍按照摩尔比Cr:Mn:Fe:Co:Ni=1:1:1:1:1进行配料并球磨6 h，干燥后在1050 ℃空气气氛中煅烧1200 min，使其发生高温固相反应，最终制备得到具有尖晶石结构的高发射率红外节能高熵材料，该高发射率红外节能高熵材料的发射率为0.92。
从图1可以看出：本实施案例中合成的高发射率红外节能高熵材料的衍射峰位于五种单组分之间，与Fe3O4的衍射峰几乎完全重合，同时衍射峰发生宽化，表明五种元素在晶格中固溶良好，等摩尔比形成的高构型熵促进了元素间相容性及固溶体的形成，没有其他杂峰与第二相出现，晶体结构为尖晶石结构，表明成功合成了具有单一相的高熵材料(CoCrFeMnNi)3O4。
从图2可以看出：本实施案例中高发射率红外节能高熵材料在近红外（0.76~2.5 μm）波段的发射率达0.91，这是目前已发现的最高发射率氧化物材料之一。
实施例2：把氧化钴、氧化铬、氧化铁、氧化锰、氧化镍按照摩尔比Cr:Mn:Fe:Co:Ni=1:1:1:1:1进行配料并球磨20 h，干燥后在1100 ℃空气气氛中煅烧600 min，使其发生高温固相反应，最终制备得到具有尖晶石结构的高发射率红外节能高熵材料，该高发射率红外节能高熵材料的发射率为0.93。
实施例3：把氧化钴、氧化铬、氧化铁、氧化锰、氧化铜按照摩尔比Cr:Mn:Fe:Co:Cu=1:1:1:1:1进行配料并球磨18 h，干燥后在1400 ℃空气气氛中煅烧180 min，使其发生高温固相反应，最终制备得到具有尖晶石结构的高发射率红外节能高熵材料，该高发射率红外节能高熵材料的发射率为0.95。
实施例4：把氧化钴、氧化铬、氧化铁、氧化锰、氧化镁按照摩尔比Cr:Mn:Fe:Co:Mg=1:1:1:1:1进行配料并球磨10 h，干燥后在1200 ℃空气气氛中煅烧300 min，使其发生高温固相反应，最终制备得到具有尖晶石结构的高发射率红外节能高熵材料，该高发射率红外节能高熵材料的发射率为0.91。
实施例5：把氧化钴、氧化铬、氧化铁、氧化铝、氧化镍按照摩尔比Cr:Al:Fe:Co:Ni=1:1:1:1:1进行配料并球磨12 h，干燥后在1300 ℃空气气氛中煅烧200 min，使其发生高温固相反应，最终制备得到具有尖晶石结构的高发射率红外节能高熵材料，该高发射率红外节能高熵材料的发射率为0.89。
实施例6：把氧化钴、氧化铬、氧化铁、氧化锰、氧化锌按照摩尔比Cr:Mn:Fe:Co:Zn=1:1:1:1:1进行配料并球磨10 h，干燥后在1100 ℃空气气氛中煅烧360 min，使其发生高温固相反应，最终制备得到具有尖晶石结构的高发射率红外节能高熵材料，该高发射率红外节能高熵材料的发射率为0.92。
实施例7：把氧化锰、氧化铬、氧化铁、氧化镍按照摩尔比Cr:Mn:Fe:Ni=1:1:1:1进行配料并球磨20 h，干燥后在1300 ℃空气气氛中煅烧300 min，使其发生高温固相反应，最终制备得到具有尖晶石结构的高发射率红外节能高熵材料，该高发射率红外节能高熵材料的发射率为0.93。
实施例8：把氧化钴、氧化铬、氧化锰、氧化镍按照摩尔比Cr:Mn:Co:Ni=1:1:1:1进行配料并球磨8 h，干燥后在1400 ℃空气气氛中煅烧180 min，使其发生高温固相反应，最终制备得到具有尖晶石结构的高发射率红外节能高熵材料，该高发射率红外节能高熵材料的发射率为0.88。
实施例9：把氧化钴、氧化铁、氧化铬、氧化镍按照摩尔比Cr:Fe:Co:Ni=1:1:1:1进行配料并球磨8 h，干燥后在1400 ℃空气气氛中煅烧240 min，使其发生高温固相反应，最终制备得到具有尖晶石结构的高发射率红外节能高熵材料，该高发射率红外节能高熵材料的发射率为0.90。
实施例10：把氧化钴、氧化铁、氧化锰、氧化镍按照摩尔比Mn:Fe:Co:Ni=1:1:1:1进行配料并球磨8 h，干燥后在1250 ℃空气气氛中煅烧300 min，使其发生高温固相反应，最终制备得到具有尖晶石结构的高发射率红外节能高熵材料，该高发射率红外节能高熵材料的发射率为0.90。
实施例11：把氧化铬、氧化铁、氧化锰按照摩尔比Cr:Mn:Fe=1:1:1进行配料并球磨16 h，干燥后在1200 ℃空气气氛中煅烧720 min，使其发生高温固相反应，最终制备得到具有尖晶石结构的高发射率红外节能高熵材料，该高发射率红外节能高熵材料的发射率为0.92。
实施例12：把氧化钴、氧化铁、氧化镍按照摩尔比Fe:Co:Ni=3:1:1:1进行配料并球磨12 h，干燥后在900 ℃空气气氛中煅烧960 min，使其发生高温固相反应，最终制备得到具有尖晶石结构的高发射率红外节能高熵材料，该高发射率红外节能高熵材料的发射率为0.88。
实施例13：把氧化钴、氧化锰、氧化镍按照摩尔比Mn:Co:Ni=1:1:1进行配料并球磨20 h，干燥后在1300 ℃空气气氛中煅烧420 min，使其发生高温固相反应，最终制备得到具有尖晶石结构的高发射率红外节能高熵材料，该高发射率红外节能高熵材料的发射率为0.87。
实施例14：把氧化钴、氧化铬、氧化铁、氧化锰、氧化镍按照摩尔比Cr:Fe:Al=1:1:1进行配料并球磨4 h，干燥后在1200 ℃空气气氛中煅烧300 min，使其发生高温固相反应，最终制备得到具有尖晶石结构的高发射率红外节能高熵材料，该高发射率红外节能高熵材料的发射率为0.83。
实施例15：把氧化铬、氧化铁、氧化镍按照摩尔比Cr:Fe:Ni=1:1:1进行配料并球磨6 h，干燥后在1100 ℃空气气氛中煅烧280 min，使其发生高温固相反应，最终制备得到具有尖晶石结构的高发射率红外节能高熵材料，该高发射率红外节能高熵材料的发射率为0.88。

Claims (3)

1.一种具有尖晶石结构的高发射率红外节能高熵材料的制备方法，其特征在于，包括以下步骤，
（1）配料：将具有尖晶石结构的高发射率红外节能高熵材料的原料进行配料，按照A位金属原子Co、Cr、Fe、Mn、Ni、Mg、Cu、Zn、Al摩尔比为1:1:1或1:1:1:1或1:1:1:1:1的比例分别称取3种到5种金属氧化物粉体，所述金属氧化物粉体的为氧化钴、氧化铬、氧化铁、氧化锰、氧化镍、氧化铜、氧化镁、氧化锌、氧化铝中的3种到5种；
（2）对步骤（1）中称取的粉体进行球磨；
（3）煅烧：将步骤（1）配料后的原料在900~1400℃的空气气氛中煅烧180~1200 min，使其发生高温固相反应，最终制备得到具有尖晶石结构的高发射率红外节能高熵材料的粉体。
2.根据权利要求1所述的一种具有尖晶石结构的高发射率红外节能高熵材料的制备方法，其特征在于，所述步骤2中的球磨采用行星式球磨，球磨时间为4～20h。
3.根据权利要求1所述的一种具有尖晶石结构的高发射率红外节能高熵材料的制备方法，其特征在于，所述的具有尖晶石结构的高发射率红外节能高熵材料的发射率为0.80~0.95。
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