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本文使用静态扩散法结合常规X射线粉末衍射和电子探针技术, 在Ag-In-Se体系中发现了AgyIn3.33–y/3Se5新化合物. 其结构属于三方晶系, 空间群为P3m1, 是二维层状结构, 单层晶胞由9个原子量子层按照Se1-In1-Se2-In2-Se3-Ag/In3 -Se4-In4-Se5顺序排布构成, 层间由弱范德瓦耳斯力结合. 烧结的块体样品表现出强烈的取向性, 在平行压力方向上具有极低的晶格热导率(在873 K为0.15 W·m–1·K–1). 这种本征低的晶格热导率主要源于材料的低声速和低频光学支声子与声学支声子强耦合作用. AgyIn3.33–y/3Se5样品表现为n型传导, 室温下电导率约为4 × 104 S·m–1, Seebeck系数约为–80 μV·K–1, 样品在宽温度范围内均表现出较好的电传输性能, 在450—800 K范围内的功率因子为5 μW·cm–1·K–2左右. 由于在平行压力方向上低的晶格热导率, 最终Ag0.407In3.198Se5样品在873 K达到最大热电优值ZT为1.01, 在300—850 K的平均ZT为0.45. 该化合物的发现, 扩充了铜属硫基化合物体系的n型材料, 为铜属硫基化合物体系的应用奠定了重要基础.
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关键词:
- Ag-In-Se基化合物 /
- 二维层状结构 /
- 超低晶格热导率 /
- 热电性能
In this study, we find new AgyIn3.33–y/3Se5 compounds in Ag-In-Se system by static diffusion method combined with common X-ray diffraction and backscattering electron analysis. The crystal structure belongs to the trilateral system with the P3m1 space group, which features a two-dimensional layered structure. The unit cell is composed of 9-atom quantum layers arranged in the sequence of Se1-In1-Se2-In2-Se3-Ag/In3-Se4-In4-Se5, and in-between these layers are bonded by the weak van der Waals force. The sintered bulk samples show highly anisotropic transport properties and have an ultra-low lattice thermal conductivity along the direction parallel to sintering pressure about 0.15 W·m–1·K–1 at 873 K. The intrinsically ultra-low lattice thermal conductivity mainly comes from low phonon velocity and the strong coupling between low frequency optical phonon and acoustic phonons. The AgyIn3.33–y/3Se5 compounds behave as an n-type conduction. The electrical conductivity is 4×104 S·m–1 and the Seebeck coefficient is –80 μV·K–1 at room temperature. Therefore, AgyIn3.33–y/3Se5 compounds show high electrical transport properties in a wide temperature range, and the power factor is around 5 μW·cm–1·K–2 in a range of 450–800 K. Owing to the ultra-low lattice thermal conductivity along the direction parallel to sintering pressure, Ag0.407In3.198Se5 reaches a maximum ZT of 1.01 at 873 K and an average ZT of 0.45 at 300–850 K. The discovery of AgyIn3.33–y/3Se5 expands the n-type copper based chalcogenide and lays an important foundation for the application of copper based chalcogenide.-
Keywords:
- Ag-In-Se based compounds /
- two-dimensional layered structure /
- ultralow lattice thermal conductivity /
- thermoelectric properties
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图 1 (a) 三元Ag-In-Se系统示意相图; (b) 图(a)中红色区域的放大图
Fig. 1. (a) Schematic ternary phase diagram of Ag-In-Se; (b) enlarged view of the red area in Fig.1 (a).
图 2 (a) (Ag2Se)x(In2Se3)100–x (x = 0—20)的粉末XRD图谱; (b) x = 0, 3.3, 5.3, 10.9, 13.6和16的背散射图片; (c) 所合成x = 0, 3.3, 5.3, 8.3, 10.9, 13.6和16的样品不同衬度区域电子能谱组成Ag/In比, 紫色虚线为合成样品名义组成线, 红色圆圈标出的为单相组成
Fig. 2. (a) Powder XRD pattern of (Ag2Se)x(In2Se3)100–x (x = 0–20); (b) backscattering electron (BSE) image of the samples with x = 0, 3.3, 5.3, 10.9, 13.6 and 16; (c) the ratio of Ag/In in x = 0, 3.3, 5.3, 8.3, 10.9, 13.6 and 16, the purple dotted line is the nominal composition line, and the red circle is marked as single-phase composition.
图 3 (Ag2Se)x(In2Se3)100–x (x = 10.9)样品的慢扫XRD(红色)(10°—90°), 精修得到的衍射峰(黑色), Bragg 峰位 (绿色), 衍射峰的差异(蓝色), Rp = 6.84%, Rwp = 9.31%.
Fig. 3. Rietveld refinement of (Ag2Se)x(In2Se3)100–x (x = 10.9), experimental (red point), calculated (black), Bragg position (green), defference (blue) Rp = 6.84%, Rwp = 9.31%.
图 4 AgyIn3.33–y/3Se5的晶体结构图 (a) a轴投影; (b) c轴投影; (c) 单个晶胞的a轴投影; (d) 多面体的堆叠; (e) 以阳离子为中心的多面体
Fig. 4. Crystal structure diagram of AgyIn3.33–y/3Se5: (a) a-axis projection; (b) c-axis projection; (c) a-axis projection of a single cell; (d) stacking of polyhedron; (e) cation centered polyhedron.
图 5 (a)—(c) Ag0.392In3.203Se5烧结块体自由断裂面的不同放大倍数的场发射扫描电镜照片
Fig. 5. (a)–(c) Field emission scanning electron microscope images of freshly fractured surface for Ag0.392In3.203Se5 bulk sample with different magnifications.
图 6 (a) Ag0.392In3.203Se5样品的低倍高角度环形暗场像(HAADF-STEM); (b)—(d) 图(a)中Ag-In-Se元素的能谱面扫描图(EDS-Map)
Fig. 6. (a) HAADF-STEM (high-angle annular dark-field STEM) image of Ag0.392In3.203Se5; (b)–(d) EDS elemental mapping of Ag, In, and Se of Fig. 6 (a).
图 7 Ag0.392In3.203Se5 样品的微观图像 (a) [001]晶向的高倍高角度环形暗场像(HAADF-STEM); (b) 图(a)区域的选取电子衍射(SAED)和模拟的选取电子衍射(SAED); (c) [010] 晶向的高倍高角度环形暗场像(HAADF-STEM); (d) 图(c)区域的选取电子衍射(SAED)和模拟的选取电子衍射(SAED); (e), (f) 图(c)的染色放大图
Fig. 7. Microstructure of Ag0.392In3.203Se5: (a) High-magnification HAADF-STEM image along the [001]; (b) SAED pattern and calculation of (a); (c) high-magnification HAADF-STEM image along the [010]; (d) SAED pattern and calculation of (c); (e), (f) enlarged image of Fig.7 (c).
图 A1 AgyIn3.33–y/3Se5 (y = 0.384, 0.392, 0.400, 0.407, 0.415)的XRD图谱
Fig. A1. Powder XRD patterns of AgyIn3.33–y/3Se5 (y = 0.384, 0.392, 0.400, 0.407, 0.415).
图 A2 AgyIn3.33–y/3Se5 (y = 0.384, 0.392, 0.400, 0.407, 0.415) 的背散射图片和元素面分布图
Fig. A2. Backscattering electron (BSE) image and elemental distribution map of AgyIn3.33–y/3Se5 (y = 0.384, 0.392, 0.400, 0.407, 0.415).
图 8 AgyIn3.33–y/3Se5 (y = 0.384, 0.392, 0.400, 0.407, 0.415)电输运性能 (a) 电导率; (b) 赛贝克系数; (c) 功率因子; (d) 单抛带模型计算载流子有效质量
Fig. 8. Temperature dependences of (a) the electrical conductivity, (b) Seebeck coefficient, and (c) power factor for the AgyIn3.33–y/3Se5 (y = 0.384, 0.392, 0.400, 0.407, 0.415) samples; (d) Seebeck coefficients as a function of the charge carrier concentration at 300 K, where the dashed lines are Pisarenko plots based on the SPB model.
图 9 AgyIn3.33–y/3Se5 (y = 0.384, 0.392, 0.400, 0.407, 0.415) 热输运性能和热电优值 (a) 热导率; (b) AgyIn3.33–y/3Se5 与AgInSe2[35], AgInTe2[38], AgIn5Se8[30]和CuInSe2[39]的晶格热导率; (c) AgyIn3.33–y/3Se5, AgInSe2[35], AgIn5Se8[30], Ag1.03In5Se8[30], Ag0.9Cd0.1InSe8[35], Ag1.02InSe2[35], Ag1.6InSe2.3[40]的ZT值, 300—873 K; (d) 300—850 K的平均ZTavg值
Fig. 9. (a) The temperature-dependent of the total thermal conductivity for AgyIn3.33–y/3Se5; (b) the lattice thermal conductivity for AgyIn3.33–y/3Se5, AgInSe2[35], AgInTe2[38], AgIn5Se8[30] and CuInSe2[39]; (c) merit ZT for AgyIn3.33–y/3Se5, AgInSe2[35], AgIn5Se8[30], Ag1.03In5Se8[30], Ag0.9Cd0.1InSe8[35], Ag1.02InSe2[35], Ag1.6InSe2.3[40], at 300-873 K; (d) the average ZT at 300–850 K.
图 10 Ag0.392In0.203Se5样品的低温热容 (a)
$C_{\rm p}/T^3\text-T$ ; (b)$ C_{\rm p}/T\text-T^2 $ Fig. 10. (a) The relationship between
$ C_{\rm p}/T^3 $ and T, (b) Cp/T and T 2 of Ag0.392In0.203Se5.表 1 AgyIn3.33–y/3Se5样品的室温载流子浓度和迁移率
Table 1. The carrier concentration and Hall mobility of AgyIn3.33–y/3Se5 at room temperature.
Sample y = 0.384 y = 0.392 y = 0.400 y = 0.407 y = 0.415 μH / (cm2·V–1·s–1) 136.42 141.21 144.80 131.40 130.69 nH /(1019 cm–3) 1.88 1.70 1.68 1.93 1.85 
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表 2 Ag0.392In0.203Se5样品使用德拜-爱因斯坦模型拟合低温热容的参数
Table 2. Parameters obtained by fitting the experimental low-temperature heat capacity data to the Debye-Einstein model of Ag0.392In0.203Se5.
Sample γ/
(mJ·mol–1·K–2)b/
(mJ·mol–1·K–4)A1 θE1/K A2 θE1/K θD/K y = 0.392 0.02813 2.95 × 10–4 13.43 40.18 57.01 82.63 164
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表 3 Ag0.392In0.203Se5, AgInSe2[44]和AgIn5Se8[30]的室温杨氏模量E、格林艾森常数常数γ对比
Table 3. Comparisons of Elastic properties and Grüneisen parameters at room temperature between Ag0.392In0.203Se5, AgInSe2[44], and AgIn5Se8[30].
Parameter Ag0.392In3.203Se5 AgInSe2 AgIn5Se8 vl/(m·s–1) 3058 3584 3778 vs/(m·s–1) 1527 1530 1803 va/(m·s–1) 1713 1729 2028 E /GPa 35.0 52.5 50.6 γ 2.00 2.87 2.20
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