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化学进展 2023, Vol. 35 Issue (5): 794-806 DOI: 10.7536/PC221104 前一篇   

• 综述 •

制备固体氧化物燃料电池中电解质薄膜的电泳沉积法

赵秉国1, 刘亚迪2,*(), 胡浩然1,2, 张扬军1, 曾泽智1,*()   

  1. 1 清华大学汽车安全与节能国家重点实验室 北京 100084
    2 北京思伟特新能源科技有限公司 北京 100192
  • 收稿日期:2022-11-07 修回日期:2023-01-04 出版日期:2023-05-24 发布日期:2023-02-20
  • 作者简介:

    刘亚迪 2014年毕业于中科院上海硅酸盐研究所,获得材料物理与化学专业博士。2018年,清华大学博士后出站,化学科学与工程专业。主要从事新能源方向的研究,包括高温固体氧化物燃料电池、低温聚合物燃料电池及电解池和Li-S电池等,已发表SCI期刊论文13篇。

    曾泽智 博士毕业于加州大学洛杉矶分校机械工程系。主要从事高温燃料电池热质传输研究,重点研究固体氧化物燃料电池功率密度与循环寿命提升机制。研究成果共发表SCI论文18篇,EI论文6篇,其中以第一作者发表SCI论文10篇。

  • 基金资助:
    先进航空动力创新工作站项目和清华大学自主科研计划课题资助
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Electrophoretic Deposition in the Preparation of Electrolyte Thin Films for Solid Oxide Fuel Cells

Bingguo Zhao1, Yadi Liu2(), Haoran Hu1,2, Yangjun Zhang1, Zezhi Zeng1()   

  1. 1 State Key Laboratory of Automotive Safety and Energy, Tsinghua University,Beijing 100084, China
    2 Beijing Swift New Energy Technologies Co., Ltd, Beijing 100192, China
  • Received:2022-11-07 Revised:2023-01-04 Online:2023-05-24 Published:2023-02-20
  • Contact: * e-mail: liuyadi@swifth2.com (Yadi Liu); zezhizeng@mail.tsinghua.edu.cn (Zezhi Zeng)
  • Supported by:
    Advanced Aviation Power Innovation institution and the Aero Engine Academy of China, and the Tsinghua University Initiative Scientific Research Program

固体氧化物燃料电池(SOFCs)是一种高效、清洁的全固态能量转化装置,但过高的工作温度(700~900 ℃)限制了其使用范围和寿命,SOFC中低温化已成为当前研究热点。制备超薄电解质(厚度<10 μm)可缩短氧离子传导路径,有效降低欧姆损耗并提升中低温SOFC输出功率。电泳沉积工艺因其成本低、制备速度快等优势,极具大规模商业化生产电解质薄膜的潜力。本文归纳了近十年来电泳沉积工艺在SOFC电解质薄膜生产中的研究进展,并针对电泳沉积过程中的基体选择及预处理、稳定悬浮液制备、气泡消除及热处理过程等瓶颈问题展开讨论。结合大规模商业化薄膜制备应用的需求分析,给出了电泳沉积工艺未来研究方向的建议。

关键词： 电泳沉积法, 致密, 电解质薄膜, 中低温, 固体氧化物燃料电池

Solid oxide fuel cells (SOFCs) are power generation devices with high efficiency and low emissions. The high operating temperature (700~900 ℃) has impeded the wider adoption of SOFC stacks and limited their lifetime. This has motivated intense research efforts in developing SOFC stacks which can operate at lower temperatures. The thin electrolytes with a thickness smaller than 10 μm could shorten the ion conductive paths and reduce the associated ohmic loss, effectively improving the electrical performance of the low-temperature SOFC. The electrophoretic deposition process has the advantages of low cost and fast manufacturing speed. It is a potential candidate for large-scale commercial production of electrolyte thin films for low-temperature SOFC. In the present article, the research progress of electrophoretic deposition during the past ten years has been summarized. The key results and achievements for the important procedures of the electrophoretic deposition process, which are respectively substrate selection and pretreatment, stable suspension preparation, bubble elimination and heat treatment process, are also discussed and analyzed. The suggestions for future development of the electrophoretic deposition are also provided based on the requirements of large-scale commercialization of thin electrolyte for low-temperature SOFC.

Contents

1 Introduction

2 Fundamentals of the electrophoretic deposition process

3 Technical challenges and research progress of electrophoretic deposition process for the preparation of electrolyte thin films

3.1 Substrate selection and pretreatment

3.2 Stable suspension preparation

3.3 Bubble elimination

3.4 Heat treatment process

4 Conclusion and outlook

Key words: electrophoretic deposition, dense, electrolyte thin films, intermediate and low temperature, solid oxide fuel cell
()
图1 SOFC 工作原理[5]
Fig. 1 Working principle of SOFC[5]
图2 近20年SOFC薄膜制备工艺发展趋势(可通过Web of science 检索获取)[32]
Fig. 2 Development of SOFC thin film preparation process in recent 20 years (utilizing web of science to access the data)[32]
图3 电泳沉积系统示意图[37]
Fig. 3 Schematic of the electrophoretic deposition system[37]
图4 电泳沉积工艺基本原理示意图[38]
Fig. 4 Schematic of the working principle of electrophoretic deposition process[38]
图5 不导电基体上电泳沉积机制示意图[41]
Fig. 5 Schematic of mechanism of electrophoretic deposition on the non-conductive substrate[41]
图6 粒子双电层区域及ζ(zeta)电位示意图[54]
Fig. 6 Schematic of particle electric double layer and ζ(zeta) potential[54]
图7 不同脉冲宽度下电解质薄膜质量对比(镍基体,20 V外加电压)[80]
Fig. 7 Quality comparison of electrolyte films under different pulse widths (Ni substrate, 20 V applied voltage)[80]
图8 沉积的BCZYYbO-CuO/SDC双层电解质光学照片:(a)沉积干燥后;(b)1400 ℃空气中烧结5 h[87]
Fig. 8 Optical photographs of the deposited BCZYYbO -CuO/SDC bilayer electrolyte: (a) after deposition and drying; (b) sintered in air at 1400 ℃ for 5 h[87]
图9 1000 ℃烧结下(a)GDC 薄膜表面和(b)GDC/LSCF支撑体横截面的扫描电镜图片;(c)和(d)分别为(a)和(b)图的高倍率放大图[88]
Fig. 9 Surface and cross-sectional SEM images of (a) GDC film and (b) GDC film/LSCF support sintered at 1000 ℃. High-magnification of the (c) surface and (d) cross-sectional SEM images of (a) and (b), respectively[88]
表1 电泳沉积法制备SOFC超薄电解质薄膜工艺热处理过程
Table 1 Heat treatment process of SOFC electrolyte thin films prepared by electrophoretic deposition
Electrolyte/
thickness/size		 Substrate/dispersant/dispersion medium Heat treatment(temperature, atmosphere) EPD mode/
deposition time		 Distance between substrate and electrode Electrochemical performance ref
YSZ/2.95 μm/- Substrate: porous NiO-YSZ anode prepared by PIM method
Dispersant: 5 wt%
polyethylene glycol
Dispersion medium: ethanol		 Sintering: co-sintered at 1200~1400 ℃ for 1h (heating rate 3 ℃/min); Air atmosphere
Reduction: reduced at 1250~1350 ℃ until open circuit voltage and impedance did not change; humidified H2 atmosphere		 Voltage: 20~30 V
Deposition time: 30~180 s		 — Peak power density: 0.013 W/cm2
(800 ℃)		 44
GDC/~
7.5 μm/-		 Substrate: porous NiO-YSZ anode
Dispersant: polyethyleneimine
Dispersion medium: ethanol		 Sintering: co-sintered at
1400 ℃ for 2 h		 Voltage: 50 V(DC) 2 cm Peak power density: 0.011 W/cm2
(800 ℃)		 50
SDC/10 μm/~1.2 cm2 Substrate: porous NiO-BCS-CuO
Dispersant: none
Dispersion medium: isopropanol and acetylacetone		 Drying: dried at room temperature for 24 h after EPD
Sintering: co-sintered at
1450 ℃ for 5 h		 Voltage: 200 V
Deposition time: 60 s		 10 mm Power density:
0.072 W/cm2
(750 ℃, 0.5 V)		 67
YSZ/~
3 μm/25×
25 mm2		 Substrate: porous NiO-YSZ anode with a conductive steel plane at the back
Dispersant: Phosphate ester (PE)
Dispersion medium: isopropanol		 Sintering: sintered at 1000~1200 ℃ for 2 h Voltage: 10~70 V
Deposition time:
1~6 min		 4 cm Peak power density: 0.90 W/cm2
(800 ℃)		 70
YSZ/7.98 μm/- Substrate: Stainless steel AISI-310
Dispersant: iodine
Dispersion medium: isopropanol or acetone		 Preheating: substrate is
preheated at 300 ℃ for
60 min; air atmosphere		 Current: 3~10 mA
Deposition time: 5~25 min		 1 cm — 73
GDC/1 ~
2 μm /25 ×
25 mm2		 Substrate: LSCF cathode
Dispersant: 1.25% polyacrylic acid ammonium (PAAA)
Dispersion medium: water		 Drying: dried at 60 ℃ for 1 h
Sintering: co-sintered at
1000 ℃ for 2 h (heating rate
2 ℃/min)		 Voltage: 100 V
(DC)
Deposition time:
2 min		 15 mm — 88
GDC/6 μm /4 cm2 Substrate: YSZ electrolyte
Dispersant: iodine
Dispersion medium: ethanol		 Sintering: YSZ and NiO-YSZ are co-sintered at 1400 ℃ for 4 h
Sintering: GDC and LSCF-GDC are co-sintered at
1150 ℃ for 1.5 h		 Voltage: -100 V ~
+80 V (AC)		 1 cm Peak power density: 0.99 W/cm2
(800 ℃)		 94
38
YSZ/
2.92 μm /-		 Substrate: Ni-YSZ anode
Dispersant: none
Dispersion medium: acetylacetone		 Drying: dried at room temperature for a night after EPD
Sintering: co-sintered at
1400 ℃ for 2 h		 Voltage: 25 V
Deposition time:
3 min		 1 cm Peak power density: 0.477 W/cm2
(800 ℃, H2)		 99
YSZ/10 μm/- Substrate: porous NiO-YSZ anode
Dispersant: Darvan 821-A
Dispersion medium: acetylacetone		 Drying: dried at room temperature for a night after EPD
Sintering: co-sintered at
1450 ℃ for 5 h		 Voltage: 50~300 V (DC)
Deposition time: 1~5 min		 10 mm Peak power density: 0.624 W/cm2
(800 ℃)		 100
YSZ/5 μm/- Substrate: porous NiO-YSZ anode
Dispersant: 0.1 g/L iodine, 5 vol% acetylacetone and 2 vol% water
Dispersion medium: isopropanol		 Sintering: co-sintered at
1400 ℃ for 6 h (heating to 800 ℃ with heating rate of
50 ℃/h and then keeping
30 min; then heating to
1400 ℃ with heating rate of
75 ℃/h and keeping 6 h)		 Voltage: 15~40 V (DC)
Deposition time: 1~4 min		 2 cm Power density: 0.91 W/cm2 (800 ℃, 0.7 V) 101
YSZ/
~2.5 μm/-		 — Sintering: co-sintered at
1400 ℃ for 2 h (heating rate 1 ℃/min)		 Voltage: 30 V
Deposition time:
2 min		 — Peak power density: 0.077 W/cm2
(800 ℃)		 102
BCSCuO/
8 μm/
~1.2 cm2		 Substrate: SDC
Dispersant: iodine
Dispersion medium: isopropanol and acetylacetone		 Sintering: co-sintered at
1450 ℃ for 5 h		 Voltage: 20~80 V
Deposition time: 1~ 3 min		 1 cm — 103
BSCF/
10 μm/-		 Substrate: porous BSCF
Dispersant: polymethylmethacrylate
Dispersion medium: reagent-grade ethanol		 Sintering: co-sintered at
1100 ℃ for 3 h		 Voltage: 150 V
Deposition time:
5 min		 10 mm — 104
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