制备工艺对塑性热电材料Ag2S0.4Te0.6结构与性能的影响

doi:10.15541/jim20260018

无机材料学报 ›› 2026, Vol. 41 ›› Issue (7): 939-946.DOI: 10.15541/jim20260018

制备工艺对塑性热电材料Ag₂S_0.4Te_0.6结构与性能的影响

刘今霄¹^,²(), 刘镇汉¹^,², 陈星宇¹^,², 周钲洋¹^,², 仇鹏飞¹^,², 张家伟¹^,²(), 史迅¹^,²()

¹ 中国科学院上海硅酸盐研究所, 关键陶瓷材料全国重点实验室, 上海 200050
² 中国科学院大学材料科学与光电技术学院, 北京 100049

收稿日期:2026-01-13 修回日期:2026-03-14 出版日期:2026-03-18 网络出版日期:2026-03-18
通讯作者: 张家伟, 研究员. E-mail: jiaweizhang@mail.sic.ac.cn;
史迅, 研究员. E-mail: xshi@mail.sic.ac.cn
作者简介:刘今霄(2000-), 女, 硕士研究生. E-mail: liujinxiao23@mails.ucas.ac.cn
基金资助:
国家自然科学基金(52302329);上海市自然科学基金面上项目(23ZR1472800);中国科学院上海分院“抢占制高点青年攀登计划”(CASSHB-QNPD-2023-003)

Influence of Preparation Processes on the Structure and Properties of the Ductile Thermoelectric Material Ag₂S_0.4Te_0.6

LIU Jinxiao¹^,²(), LIU Zhenhan¹^,², CHEN Xingyu¹^,², ZHOU Zhengyang¹^,², QIU Pengfei¹^,², ZHANG Jiawei¹^,²(), SHI Xun¹^,²()

¹ State Key Laboratory of High Performance Ceramics, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050, China
² Center of Materials Science and Optoelectronics Engineering, University of Chinese Academy of Sciences, Beijing 100049, China

Received:2026-01-13 Revised:2026-03-14 Published:2026-03-18 Online:2026-03-18
Contact: ZHANG Jiawei, professor. E-mail: jiaweizhang@mail.sic.ac.cn;
SHI Xun, professor. E-mail: xshi@mail.sic.ac.cn
About author:LIU Jinxiao (2000-), female, Master candidate. E-mail: liujinxiao23@mails.ucas.ac.cn
Supported by:
National Natural Science Foundation of China(52302329);Shanghai Natural Science Foundation General Program(23ZR1472800);Talent Plan of Shanghai Branch, Chinese Academy of Sciences(CASSHB-QNPD-2023-003)

摘要/Abstract

摘要：

Ag₂S_0.4Te_0.6作为一种具有良好塑性及热电性能的无机半导体材料, 在可穿戴电子设备领域具有潜在的应用价值。近期研究表明, 优化制备工艺(如退火处理)可显著提升其塑性, 而该性能与材料的相结构密切相关。本研究收集了退火前后Ag₂S_0.4Te_0.6粉末样品在110 ~700 K温度范围内的高分辨率同步辐射粉末X射线衍射数据, 结合Rietveld结构精修、高分辨透射电子显微镜以及原子对分布函数技术, 详细分析了退火工艺对粉末样品的相组成与结构演变行为的影响。结果表明, 退火前Ag₂S_0.4Te_0.6粉末样品主要为非晶态, 仅含有少量结晶性很差的单斜相。在升温过程中, 材料逐渐结晶并首先出现单斜相, 随后转变为体心立方(bcc)与面心立方(fcc)共存的混合相; 降至室温后, 样品依然保持以bcc相为主的立方结晶/非晶混合态。退火处理后, Ag₂S_0.4Te_0.6粉末样品在室温下即为立方结晶与少量非晶混合态, 且在升温过程中未观察到明显的相变行为。此外, 退火未对Ag₂S_0.4Te_0.6块体样品的热电性能产生明显影响。本研究为进一步理解退火改善Ag₂S_0.4Te_0.6材料的塑性提供了结构依据。

关键词: Ag₂S_0.4Te_0.6, 热电材料, 同步辐射, 结构演变, 退火

Abstract:

Ag₂S_0.4Te_0.6 is an inorganic semiconductor with favorable ductility and thermoelectric performance, showing potential for applications in wearable electronics. Recent studies have indicated that optimization of preparation processes, such as annealing, can significantly enhance the ductility of the material, which is closely related to its phase composition and crystal structure. In this work, high-resolution synchrotron radiation powder X-ray diffraction data of the Ag₂S_0.4Te_0.6 powder sample before and after annealing were collected over a temperature range of 110-700 K. By combining Rietveld structural refinement, high-resolution transmission electron microscopy, and atomic pair distribution function analysis, the influence of the annealing process on the phase composition and structural evolution behavior of the powder samples was investigated in detail. The results show that the pristine Ag₂S_0.4Te_0.6 powder is predominantly amorphous, containing only a small amount of poorly crystalline monoclinic phase. During heating, the material gradually crystallizes, first forming a monoclinic phase, which subsequently transforms into mixed body-centered cubic (bcc) and face-centered cubic (fcc) phases. After cooling back to room temperature, the sample remains in a mixed state of bcc-dominated cubic crystallinity and amorphous phase. In contrast, the annealed powder sample already exhibits a mixed cubic crystalline/amorphous state at room temperature, and no obvious phase transition behavior is observed during heating. Moreover, the thermoelectric properties of Ag₂S_0.4Te_0.6 bulk sample remain largely unaffected by the annealing process. This study provides structural insights for further understanding the annealing-induced improvement in ductility of Ag₂S_0.4Te_0.6 materials.

Key words: Ag₂S_0.4Te_0.6, thermoelectric material, synchrotron radiation, structural evolution, annealing

中图分类号:

TB34

刘今霄, 刘镇汉, 陈星宇, 周钲洋, 仇鹏飞, 张家伟, 史迅. 制备工艺对塑性热电材料Ag₂S_0.4Te_0.6结构与性能的影响[J]. 无机材料学报, 2026, 41(7): 939-946.

LIU Jinxiao, LIU Zhenhan, CHEN Xingyu, ZHOU Zhengyang, QIU Pengfei, ZHANG Jiawei, SHI Xun. Influence of Preparation Processes on the Structure and Properties of the Ductile Thermoelectric Material Ag₂S_0.4Te_0.6[J]. Journal of Inorganic Materials, 2026, 41(7): 939-946.

图/表 12

图1 (a)退火前和(b)退火后Ag2S0.4Te0.6块体样品的BSE图像, 以及Ag、Te和S的EDS元素分布图

Fig. 1 BSE images of (a) pristine and (b) annealed Ag2S0.4Te0.6 bulk samples, along with EDS elemental distribution mappings of Ag, Te and S

图2 (a, c)退火前和(b, d)退火后Ag2S0.4Te0.6粉末样品的(a, b) SPXRD图谱(λ=0.490027(0) Å)和(c, d) DSC曲线

Fig. 2 (a, b) SPXRD patterns (λ=0.490027(0) Å) and (c, d) DSC curves of (a, c) pristine and (b, d) annealed Ag2S0.4Te0.6 powder samples

图3 以(a)单斜Ag2Te、(b~f) bcc Ag2Te和(g~i) fcc Ag2Te为模型, 样品SPXRD数据的Rietveld精修

Fig. 3 Rietveld refinement of SPXRD data of samples using (a) monoclinic Ag2Te, (b-f) bcc Ag2Te, and (g-i) fcc Ag2Te as models

图4 (a)退火前Ag2S0.4Te0.6粉末样品的非晶区HRTEM照片(插图为白色方框区域对应的快速傅里叶变换(FFT)图像); (b)退火后Ag2S0.4Te0.6粉末样品的HRTEM照片(展示了bcc相结晶基质与非晶区, 插图为对应结晶区的FFT图像); (c, d)图(b)结晶区对应的(c) SAED图案及(d) IFFT图像

Fig. 4 (a) HRTEM image of amorphous region in the pristine Ag2S0.4Te0.6 powder sample with inset showing the fast Fourier transform (FFT) image corresponding to area marked by the white square; (b) HRTEM image of the annealed Ag2S0.4Te0.6 powder sample showing a crystalline matrix with a bcc structure embedded in an amorphous region with inset showing the FFT image of the crystalline area; (c) SAED pattern and (d) IFFT image corresponding to the crystalline region marked in panel Fig. (b)

图5 退火前后Ag2S0.4Te0.6块体样品的(a)电导率、(b) Seebeck系数、(c)功率因子、(d)总热导率及(e)热电优值zT随温度的变化曲线

Fig. 5 Temperature-dependent curves of (a) electrical conductivity, (b) Seebeck coefficient, (c) power factor, (d) total thermal conductivity, and (e) thermoelectric figure of merit zT for pristine and annealed Ag2S0.4Te0.6 bulk sample

图S1 (a)退火前及(b)退火后Ag2S0.4Te0.6块体样品的BSE图像

Fig. S1 BSE images of the (a) pristine and (b) annealed Ag2S0.4Te0.6 bulk samples Red circles indicate the selected regions for EDS point analysis

表S1 退火前块体样品指定检测点处元素分布的原子百分比

Table S1 Atomic percentages of the element distribution at the designated detection points in the pristine bulk sample

Point	#1	#2	#3	#4	#5	#6	#7	Average
Ag/%	67.5	67.5	67.4	67.0	67.8	67.1	67.4	67.4
Te/%	19.5	19.7	19.7	19.6	19.6	19.3	19.4	19.5
S/%	13.0	12.8	12.9	13.3	12.6	13.6	13.2	13.1

表S2 退火后块体样品指定检测点处元素分布的原子百分比

Table S2 Atomic percentages of the element distribution at the designated detection points in the annealed bulk sample

Point	#1	#2	#3	#4	#5	#6	#7	Average
Ag/%	67.5	68.0	67.4	68.2	67.9	67.4	67.4	67.7
Te/%	19.5	19.3	19.7	19.0	19.5	19.8	19.9	19.5
S/%	13.0	12.7	12.9	12.8	12.6	12.8	12.7	12.8

表S3 SPXRD数据bcc Ag2Te相的Rietveld精修

Table S3 Rietveld refinement of SPXRD data for the bcc Ag2Te phase

Temperature		600 K (pristine)	700 K (pristine)	300 K (pristine, after cycling)	300 K (annealed)	300 K (annealed, after cycling)
No. of points		30052	30052	30057	30062	30059
No. of reflections		52	53	51	52	52
No. of parameters		15	16	16	16	16
R_p/%		1.84	1.84	2.08	2.20	2.12
R_wp/%		3.12	4.12	3.78	3.05	3.66
GOF		4.54	5.02	5.48	2.20	2.98
a=b=c/Å		5.1031(8)	5.1263(13)	5.0481(6)	5.0420(2)	5.0536(10)
Volume/Å³		132.8930(4)	134.7170(6)	128.6440(3)	128.1770(9)	129.0650(4)
U_iso/Å²	Ag1	0.2084(6)	0.2077(7)	0.1917(18)	0.1861(18)	0.1892(13)
	Te1	0.1068(7)	0.1102(13)	0.0887(7)	0.0944(15)	0.0955(9)
	S1	0.1068(7)	0.1102(13)	0.0887(7)	0.0944(15)	0.0955(9)
Occupancy	Ag1	0.3333	0.3333	0.3522(15)	0.3333	0.3461(12)
	Te1	0.6	0.6	0.6(6)	0.6	0.6
	S1	0.4	0.4	0.3999(6)	0.4	0.4

表S4 SPXRD数据fcc Ag2Te相的Rietveld精修

Table S4 Rietveld refinement of the SPXRD data for the fcc Ag2Te phase

Temperature		700 K (pristine)	300 K (annealed)	300 K (annealed, after cycling)
No. of points		30052	30062	30059
No. of reflections		58	62	58
No. of parameters		17	17	16
R_p/%		1.34	2.29	3.23
R_wp/%		2.44	4.01	5.43
GOF		2.87	3.13	4.42
a=b=c/Å		6.4927(14)	6.4140(4)	6.3978(6)
Volume/Å³		273.6970(10)	263.9000(3)	261.8700(4)
U_iso/Å²	Ag1	0.0546(4)	0.0547(3)	0.0550(4)
	Ag2	0.1926(4)	0.1800(3)	0.1795(4)
	Te1	0.1795(2)	0.1752(3)	0.1750(7)
	S1	0.1795(2)	0.1752(3)	0.1750(7)
Occupancy	Ag1	0.1345(6)	0.1330(2)	0.1435(3)
	Ag2	0.0703(6)	0.0766(2)	0.0613(3)
	Te1	0.6050(7)	0.6060(3)	0.6094(4)
	S1	0.3950(7)	0.3940(3)	0.3906(4)

图S2 (a)退火前和(b)退火后粉末样品在2~40 Å范围内不同温度下的PDF图谱(插图为2~6 Å短程范围内的PDF图谱);(c)退火前700 K和(d)退火后300 K粉末样品在2~6 Å范围内由Im$\bar{3}$m和Fm$\bar{3}$m空间群平均结构拟合的同步辐射X射线PDF图谱, 以及不同原子对的PDF数据; (e) Ag2S0.4Te0.6退火前700 K在2~30 Å范围内的同步辐射X射线PDF图谱

Fig. S2 (a, b) PDF spectra at different temperatures for (a) pristine and (b) annealed powder samples in the range of 2-40 Å with inset showing the PDF spectra in the short range of 2-6 Å; (c, d) Synchrotron radiation X-ray PDF spectra of (c) pristine powder at 700 K and (d) annealed powder at 300 K in the range of 2-6 Å fitted with average structures from the Im$\bar{3}$m and Fm$\bar{3}$m space groups, together with partial PDF data for different atomic pairs; (e) Synchrotron radiation X-ray PDF spectra for pristine Ag2S0.4Te0.6 at 700 K in the range of 2-30 Å Blue circles are fitted using the average structures of the Im¯3m and Fm¯3m space groups, with the fitting model displayed as a red line and the difference curve as a green line (with offset shown below the data and fit)

图S3 (a)退火前600 K及(b)退火后300 K Ag2S0.4Te0.6粉末的同步辐射X射线PDF图谱

Fig. S3 Synchrotron radiation X-ray PDF patterns of Ag2S0.4Te0.6 powder (a) before annealing at 600 K and (b) after annealing at 300 K

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制备工艺对塑性热电材料Ag₂S_0.4Te_0.6结构与性能的影响

Influence of Preparation Processes on the Structure and Properties of the Ductile Thermoelectric Material Ag₂S_0.4Te_0.6

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