溶胶-凝胶法制备氧化锡基薄膜及薄膜晶体管的研究进展

刘贤哲; 张旭; 陶洪; 黄健朗; 黄江夏; 陈艺涛; 袁炜健; 姚日晖; 宁洪龙; 彭俊彪

doi:10.7498/aps.69.20200653

摘要

透明导电氧化物 (transparent conductive oxides, TCOs)薄膜和透明氧化物半导体 (transparent oxide semiconductors, TOSs) 薄膜具有高透明度和良好的导电率等特点, 广泛应用于太阳能电池、平板显示、智能窗以及透明柔性电子器件等领域. 大多数TCOs和TSOs薄膜主要是以氧化铟、氧化锌和氧化锡三种材料为基础衍生来的, 其中, 氧化铟薄膜中In元素有毒、含量稀少且价格昂贵, 会造成环境污染; 氧化锌薄膜对酸或碱刻蚀液敏感, 薄膜图形化困难; 氧化锡薄膜不仅无毒、无污染、价格低廉, 还具有良好的电学性能和化学稳定性, 具有巨大的发展潜力. 目前, 薄膜的制备主要依赖于真空镀膜技术. 此类技术的缺点在于设备结构复杂且价格昂贵、能耗高、工艺复杂、生产成本高等. 相比传统真空镀膜技术, 溶胶-凝胶法具有工艺简单、成本低等优点, 受到了人们的广泛关注. 本文从TCOs和TSOs薄膜的发展现状和发展趋势出发, 先介绍了氧化锡薄膜的结构特性、导电机制、元素掺杂理论以及载流子散射机理, 然后介绍了溶胶-凝胶法原理和制备方法, 接着介绍了近些年来溶胶-凝胶法制备氧化锡基薄膜在n型透明导电薄膜、薄膜晶体管以及p型半导体薄膜中的应用和发展, 最后总结了当前存在的问题以及今后研究的方向.

关键词:

Abstract

Transparent conductive oxide (TCO) films and transparent oxide semiconductor (TOS) films have been widely adopted in solar cells, flat panel displays, smart windows, and transparent flexible electronic devices due to their advantages of high transparency and good conductivity and so on. Most of TCO and TOS films are mainly derived from indium oxide, zinc oxide and tin oxide. Among these materials, the In element is toxic, rare and expensive for indium oxide film, which will cause environmental pollution; zinc oxide film is sensitive to acid or alkali etchants, resulting in a poor formation of film patterning; tin oxide film is not only non-toxic, eco-friendly, and cheap but also has good electrical properties and strong chemical stability. Thus, tin oxide has a great potential for developing the TCO and TOS films. At present, the film is prepared mainly by the vacuum deposition technique. The drawbacks of this technique are complex and expensive equipment system, high energy consumption, complicated process and high-cost production. However, compared with the vacuum deposition technique, the sol-gel method has attracted extensive attention because of its virtues such as simple process and low cost. In this paper, we review the development status and trend of TCO and TOS films. First, the structural characteristics, conductive mechanism, element doping theory and carrier scattering mechanism of tin oxide thin films are introduced. Then the principle of sol-gel method and correlative film fabrication techniques are illustrated. Subsequently, the application and development of tin oxide-based thin films prepared by sol-gel method in n-type transparent conductive films, thin-film transistors and p-type semiconductor films in recent years are described. Finally, current problems and future research directions are also pointed out.

Keywords:

作者及机构信息

1.
华南理工大学发光材料与器件国家重点实验室, 高分子光电材料与器件研究所, 广州　510641

2.
广州新视界光电科技有限公司, 广州　510530

通信作者: 陶洪, tao.h@scut.edu.cn ; 宁洪龙, ninghl@scut.edu.cn ;

基金项目: 广东省基础与应用基础研究重大项目(批准号: 2019B030302007)、国家自然科学基金(批准号: 51771074, 61574061)、国家自然科学基金重大集成项目(批准号: U1601651)、广州市科技计划项目(批准号: 201904010344)、中央高校基本科研业务费专项资金(批准号: 2019MS012)、2019年广东大学生科技创新培育“攀登计划”专项资金 (批准号: pdjh2019a0028, pdjh2019b0041)、国家级大学生创新创业训练计划(批准号: 201910561005, 201910561007)和华南理工大学百步梯攀登计划研究项目(批准号: j2tw201902475, j2tw201902203)资助的课题.

Authors and contacts

1.
Institute of Polymer Optoelectronic Materials and Devices, State Key Laboratory of Luminescence Materials and Devices, South China University of Technology, Guangzhou 510641, China

2.
New Vision Opto-Electronic Technology Co., Ltd, Guangzhou 510530, China

Corresponding author: Tao Hong, tao.h@scut.edu.cn ; Ning Hong-Long, ninghl@scut.edu.cn ;

Funds: Project supported by the Major project of Basic and Applied Basic Research in Guangdong Province, China(Grant No. 2019B030302007), the National Natural Science Foundation of China (Grant Nos. 51771074, 61574061), Major Integration Project of the National Natural Science Foundation of China (Grant No.U1601651), Guangzhou Science and Technology Project, China (Grant No. 201904010344), Special Funds for Basic Scientific Research Operating Expenses of Central Universities, China (Grant No. 2019MS012), Special Fund for "Climbing Plan" of Science and Technology Innovation Cultivation for Guangdong University Students in 2019 (Grant Nos. pdjh2019a0028, pdjh2019b0041), National Innovation and Entrepreneurship Training Program for College Students (Grant Nos. 201910561005, 201910561007), and the South China University of Technology BaiBu Ladder Climbing Program Research Project (Grant Nos. j2tw201902475, j2tw201902203).

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施引文献

图 1 氧化锡　(a) 晶体结构; (b) XRD图谱^[22]; (c) 能带结构^[23]; (d) 能带结构示意图^[7]

Fig. 1. SnO₂: (a) Crystalline structure; (b) XRD pattern^[22]; (c) band structure^[23]; (d) band structure schematic^[7].

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图 2 氧化锡内部不同本征点缺陷的形成能^[26]

Fig. 2. Formation energy of intrinsic point defects in SnO₂^[26].

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图 3 不同半导体的能带图　(a)本征半导体; (b) n型掺杂半导体; (c) p型掺杂半导体

Fig. 3. The energy band schematic of semiconductors: (a) intrinsic (b) n type; (c) p type.

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图 4 晶界散射和电离杂质散射机制示意图^[31]

Fig. 4. The schematic of grain boundary scattering and ionized impurity scattering mechanism^[31].

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图 5 溶胶-凝胶技术原理^[33]

Fig. 5. The overview of the sol-gel technologies^[33].

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图 6 (a) 旋涂法^[35]; (b) 喷雾热解法^[36]; (c) 浸涂法^[37]; (d) 喷墨打印法^[38]

Fig. 6. The solution-processed fabrication techniques of thin film: (a) Spin coating^[35]; (b) spray pyrolysis^[36]; (c) dip coating^[37]; (d) inkjet print^[38].

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图 7 在不同SnF₂浓度下　(a) FTO薄膜 (110) 晶面衍射的半峰宽和晶粒尺寸的变化和 (b) FTO薄膜的电阻率、载流子浓度和迁移率的变化^[52]

Fig. 7. (a) Variation of full-width-at-half-maximum and grain size estimated along (1 1 0) diffraction and (b) electrical resistivity, carrier concentration and Hall mobility of the FTO films as a function of SnF₂ concentration, 0–10 mol%^[52].

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图 8 不同Sb掺杂浓度下　(a) 方阻和电阻率的变化和 (b) 迁移率和载流子浓度的变化^[56]

Fig. 8. The variation of (a) Sheet resistance and resistivity and (b) Hall mobility and carrier concentration for ATO film with different Sb concentrations^[56].

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图 9 在不同掺杂浓度下SnO₂基TCOs薄膜的电学性能变化　(a) Ta^[57]; (b) Nb^[58]; (c) Pr^[59]; (d) W^[60]

Fig. 9. The variation of electrical properties for SnO₂-based TCOs films with different dopants concentrations: (a) Ta^[57]; (b) Nb^[58]; (c) Pr^[59]; (d) W^[60].

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图 10 (a) 不同浓度SnO₂薄膜的厚度和电学性能^[63]; (b) SnO₂薄膜的XRD图谱和TFT的转移特性曲线^[64]; (c) Ga掺杂SnO₂的TFT示意图及其转移特性曲线^[65]

Fig. 10. (a) The thickness and electrical properties of SnO₂ films with different concentration^[63]; (b) the XRD pattern of SnO₂ film and the transfer characteristic curve of SnO₂ TFT^[64]; (c) the schematic cross-sectional diagram of Ga doped SnO₂ TFT and corresponding transfer characteristic curve^[65].

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图 11 (a) 不同锡前驱体溶液的热重分析曲线^[69]; (b) 不同原子的标准电极电位、带隙和电负性^[70]; (c) 不同氧化物介电材料的高介电常数和能带值^[71]; (d) 在标准条件下, 高介电常数的氧化物吸湿反应的吉布斯能量变化^[71]

Fig. 11. (a) Thermogravimetric analyses curves of various Sn precursors^[69]; (b) standard electrode potential, bandgap, and electronegativity of In, Zn, Sn, and carrier suppressible atoms^[70]; (c) permittivity and band gap for different oxide dielectrics^[71]; (d) Gibbs energy changes for moisture absorption reactions in high permittivity oxides under standard conditions^[71].

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图 12 不同掺杂浓度SnO₂基薄膜的透过率图谱　(a) Ga掺杂SnO₂^[75]; (b) Co掺杂SnO₂^[81]; (c) Mn掺杂SnO₂^[80]; (d) 不同掺杂浓度下Mg掺杂SnO₂薄膜的光学吸收图谱^[79]

Fig. 12. The transmittance spectra of SnO₂-based films with different dopant concentration: (a) Ga doped SnO₂^[75]; (b) Co doped SnO₂^[81]; (c) Mn doped SnO₂^[80]; (d) the optical absorption spectra of Mg-doped SnO₂ thin films with different concentration^[79].

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图 13 p-n结的电流-电压特性曲线　(a) SnO₂:Ga/ZnO:Al^[75]; (b) SnO₂:Ga/SnO₂:Si^[82]

Fig. 13. The current–voltage characteristics curve of p-n heterojunction: (a) SnO₂:Ga/ZnO:Al^[75]; SnO₂:Ga/SnO₂:Si^[82].

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表 1 不同卤素元素的电负性、X—H和X—Sn键解离能和原子半径^[31,50]

Table 1. The electronegativity, BDE of X—H and X— Sn, atomic radius for halogen elements^[31,50].

Element	Electroneg- ativity	BDE of X-H/kJ·mol^–1	Atomic radius/nm	BDE of X-Sn/kJ·mol^–1
F	4.0	569.68	0.42	476
Cl	3.0	431.36	0.79	350
Br	2.8	366.16	1.2	337
BDE: Bond dissociation energy

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表 2 不同元素掺杂SnO₂薄膜的电学参数和透过率

Table 2. The electrical parameters and transmittance of SnO₂ thin films with different dopants.

Doping elements	Conductivity/Ω^–1·cm^–1	Carrier density /cm^–3	Hall Mobility /cm²·V^–1·s^–1	Transmittance/%	Technique	Ref.
F	0.33 × 10³	2.62 × 10²⁰	7.96	86	spray pyrolysis	[51]
F	1.43 × 10³	1.10 × 10²¹	8.1	90	dip-coating	[52]
Li, F	2.70 × 10³	5.62 × 10²⁰	29.1	70	spray pyrolysis	[53]
P, F	4.0 × 10⁵	8.30 × 10²⁶	0.0032	86	spray pyrolysis	[54]
Sb	0.36 × 10³	6.37 × 10²¹	0.347	61	spin-coating	[55]
Sb	3.50 × 10³	1.68 × 10²¹	12.03	—	spray pyrolysis	[56]
Ta	0.50 × 10³	1.30 × 10²⁰	29.26	80	spray pyrolysis	[57]
Pr	0.26 × 10³	8.70 × 10¹⁹	18.75	80	spray pyrolysis	[59]
W	0.17 × 10³	7.60 × 10¹⁹	14.2	90	dip-coating	[60]
Nb	0.23 × 10³	5.00 × 10¹⁹	25	70	spray pyrolysis	[61]

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表 3 溶液法制备SnO₂基TFTs的电学性能

Table 3. Electrical properties of solution-processed SnO₂-based TFTs.

Solute	Dopant	Concentration /mol·L^–1	Substrate	Channel thickness/nm	Annealing temperature /℃	Mobility /cm²·V^–1·s^–1	I_on/I_off	SS/V·dec^–1	Ref.
SnCl₂·2H₂O	—	0.02	SiO₂/Si	3.8	500	11.2	6.8 × 10⁶	0.78	[63]
SnCl₂·2H₂O	—	0.167	HfO₂/Mo	9.2	300	99.16	1.7 × 10⁸	0.114	[64]
SnCl₂·2H₂O	Ga(NO₃)₃ ·xH₂O	0.12	SiO₂/Si	—	400	4.1	6.6 × 10⁶	0.77	[65]
SnCl₂·2H₂O	—	0.03	SiO₂/Si	—	500	12.18	5 × 10⁷	1.17	[66]
SnCl₂·2H₂O	—	0.1	ZrO₂/ITO	22	400	103	10⁴—10⁵	0.3	[67]
C₁₆H₃₀O₄Sn	—	0.5	Al₂O₃/ITO	15	350	96.4	2.2 × 10⁶	0.26	[68]

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表 4 溶液法制备p型SnO₂基薄膜的电学性能

Table 4. Electrical properties of solution-processed p type SnO₂-based films.

Solute	Dopant	Resistivity /Ω·cm	Carrier density/cm^–3	Hall Mobility /cm²·V^–1·s^–1	Bandgap/eV	Technique	Ref.
SnCl₂·2H₂O	AlCl₃	3.6 × 10^–2	6.7 × 10¹⁸	25.90	4.11	spray pyrolysis	[74]
SnCl₂·2H₂O	Ga(NO₃)₃·H₂O	1.6	1.70 × 10¹⁸	6.34	3.83	spin-coating	[75]
SnCl₂·2H₂O	InCl₃·4H₂O	20.4	1.85 × 10¹⁷	1.57	3.8	dip-coating	[76]
SnCl₂·2H₂O	InCl₃·4H₂O, GaCl₃	0.17	9.5 × 10¹⁷	39.2	3.38	spray pyrolysis	[77]
SnCl₂·2H₂O	FeCl₃·6H₂O	660	1.4 × 10¹⁵	6.75	3.75	dip-coating	[78]
SnCl₂·2H₂O	MgCl₂·6H₂O	2.5 × 10⁴	10¹⁴	1.6	3.73	spin-coating	[79]
SnCl₂·2H₂O	MnCl₂	359.1	6.72 × 10¹⁴	6.14	3.85	dip-coating	[80]
SnCl₂·2H₂O	CoCl₂·6H₂O	140	1.47 × 10¹⁵	8.25	3.81	spin-coating	[81]

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