移动区熔法生长全无机钙钛矿型CsPbBr3晶体及其性能研究

doi:10.15541/jim20180234

无机材料学报 ›› 2018, Vol. 33 ›› Issue (11): 1253-1258.DOI: 10.15541/jim20180234

所属专题：钙钛矿材料

• • 上一篇

移动区熔法生长全无机钙钛矿型CsPbBr₃晶体及其性能研究

徐家跃¹, 梁肖肖¹, 金敏², 曾海波^1,3, KIMURAHideo⁴, 胡皓阳², 邵和助², 申慧¹, 田甜¹, 李海霞¹

(1. 上海应用技术大学材料科学与工程学院, 晶体生长研究所, 上海 201418; 2. 上海电机学院材料学院, 上海 201306; 3. 南京理工大学材料科学与工程学院, 纳米光电材料研究所, 南京 210094; 4. National Institute for Materials Science, 1-2-1 Sengen, Tsukuba, Ibaraki 305-0047, Japan)

收稿日期:2018-05-21 出版日期:2018-11-16 网络出版日期:2018-10-20
作者简介:徐家跃. E-mail: xujiayue@sit.edu.cn

Growth and Characterization of All-inorganic Perovskite CsPbBr₃ Crystal by a Traveling Zone Melting Method

XU Jia-Yue¹, LIANG Xiao-Xiao¹, JIN Min², ZENG Hai-Bo^1,3, KIMURA Hideo⁴, HU Hao-Yang², SHAO He-Zhu², SHEN Hui¹, TIAN Tian¹, LI Hai-Xia¹

(1. Institute of Crystal Growth, School of Materials Science and Engineering, Shanghai Institute of Technology, Shanghai 201418, China; 2.

College of Materials, Shanghai Dianji University, Shanghai 201306, China; 3. Institute of Optoelectronics and Nanomaterials, College of Materials Science and Engineering, Nanjing University of Science and Technology, Nanjing 210094, China; 4. National Institute for Materials Science, 1-2-1 Sengen, Tsukuba, Ibaraki 305-0047, Japan)

Received:2018-05-21 Published:2018-11-16 Online:2018-10-20
About author:XU Jia-Yue (1966-), professor. E-mail: xujiayue@sit.edu.cn
Supported by:
Foundation item: National Natural Science Foundation of China (51472263, 51572175, 61605116);Ningbo Natural Science Foundation (2017A610009);Public Projects of Zhejiang Province (2017C31006);Shanghai Natural Science Foundation (15ZR1440600)

摘要/Abstract

摘要：

利用自制移动区熔炉生长了CsPbBr₃晶体, 事先采用相同工艺合成了高纯多晶原料以去除杂质和水分。通过工艺优化获得了大尺寸CsPbBr₃晶体, 达到ϕ25 mm× 60 mm。该晶体呈橘红色, 在600~2000 nm波长范围内具有透过率达78.6%的优异透光性能。热分析表明, 所得CsPbBr₃晶体在88.1℃和131.25℃时存在正交-四方和四方-立方相变。计算得到CsPbBr₃晶体的带宽E_g= 2.25 eV。上述结果表明移动区熔法是一种具有应用潜力的制备高质量大尺寸CsPbBr₃晶体的生长方法。

关键词: 移动区熔法, CsPbBr3晶体, 透过率, 带隙

Abstract:

A self-designed traveling zone melting method was employed to fabricate perovskite CsPbBr₃ crystals, which is helpful for impurities removing and moisture excluding. A large-size CsPbBr₃ crystal with a dimension of ϕ 25 mm× 60 mm is successfully obtained. The as-grown crystal shows orange color and displays an excellent transmittance of 78.6% in the range of 600 nm - 2000 nm wavelength. It is revealed by DSC analysis that there is phase transition at 88.1℃ and 131.25℃, respectively. The band gap E_g of the crystal is calculated to be 2.25 eV. The above results prove that the traveling zone melting method is indeed a potential approach for large size and high quality CsPbBr₃ crystal preparation.

Key words: traveling zone melting method, CsPbBr3 crystal, transmittance, band gap

中图分类号:

TQ174

徐家跃, 梁肖肖, 金敏, 曾海波, KIMURAHideo, 胡皓阳, 邵和助, 申慧, 田甜, 李海霞. 移动区熔法生长全无机钙钛矿型CsPbBr₃晶体及其性能研究[J]. 无机材料学报, 2018, 33(11): 1253-1258.

XU Jia-Yue, LIANG Xiao-Xiao, JIN Min, ZENG Hai-Bo, KIMURA Hideo, HU Hao-Yang, SHAO He-Zhu, SHEN Hui, TIAN Tian, LI Hai-Xia. Growth and Characterization of All-inorganic Perovskite CsPbBr₃ Crystal by a Traveling Zone Melting Method[J]. Journal of Inorganic Materials, 2018, 33(11): 1253-1258.

图/表 11

参考文献 12

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Materials	Method	Conditions
CsPbBr₃ polycrystalline Synthesis	Synthesis method	Rocking technique
	Raw material	99.99% CsBr and PbBr₂, 132 g
	Crucible	Quartz tube
	Vacuum	<10^-3 Pa
	Synthesis temperature	620℃
	Rocking rate	30 r/min
	Rocking time	20 min
CsPbBr₃ crystal growth	Growth method	Traveling zone melting
	Crucible	Quartz tube
	Vacuum	<10^-3 Pa
	Furnace temperature	585℃
	Temperature gradient	30℃/cm-40℃/cm
	Growth rate	1.0 mm/h
	Cooling rate	50℃/h

Materials	Method	Conditions
CsPbBr₃ polycrystalline Synthesis	Synthesis method	Rocking technique
	Raw material	99.99% CsBr and PbBr₂, 132 g
	Crucible	Quartz tube
	Vacuum	<10^-3 Pa
	Synthesis temperature	620℃
	Rocking rate	30 r/min
	Rocking time	20 min
CsPbBr₃ crystal growth	Growth method	Traveling zone melting
	Crucible	Quartz tube
	Vacuum	<10^-3 Pa
	Furnace temperature	585℃
	Temperature gradient	30℃/cm-40℃/cm
	Growth rate	1.0 mm/h
	Cooling rate	50℃/h

Growth method	Crystal size/mm³	Color	Band gap, E_g/eV	Highest transmittance/%	Phase transition temperature/℃		Ref.
Traveling zone melting	ϕ25×60	Orange	2.250	78.6	Orthorhombic→Tetragonal 88.1	Tetragonal→ Cubic 131.25	This work
Vertical Bridgman	ϕ7×12	Orange	2.250	-	88	130	[2]
Solution grown	7×2×4	Orange	2.254	-	-	-	[11]
Electronic dynamic gradient	ϕ8×58	Orange	2.252	75	87	127	[10]

Growth method	Crystal size/mm³	Color	Band gap, E_g/eV	Highest transmittance/%	Phase transition temperature/℃		Ref.
Traveling zone melting	ϕ25×60	Orange	2.250	78.6	Orthorhombic→Tetragonal 88.1	Tetragonal→ Cubic 131.25	This work
Vertical Bridgman	ϕ7×12	Orange	2.250	-	88	130	[2]
Solution grown	7×2×4	Orange	2.254	-	-	-	[11]
Electronic dynamic gradient	ϕ8×58	Orange	2.252	75	87	127	[10]

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移动区熔法生长全无机钙钛矿型CsPbBr₃晶体及其性能研究

Growth and Characterization of All-inorganic Perovskite CsPbBr₃ Crystal by a Traveling Zone Melting Method

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