doi:10.1088/2752-5724/ac88e7

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Microstructure and long-term stability of Ni-YSZ anode supported fuel cells: a review

doi: 10.1088/2752-5724/ac88e7

1.
Department of Chemical and Materials Engineering, University of Alberta, Edmonton, Alberta T6G 1H9, Canada
2.
Instituto de Nanociencia y Materiales de Aragn (INMA), CSIC-Universidad de Zaragoza, C/Pedro Cerbuna 12, Zaragoza E-50009, Spain

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Corresponding author: E-mail: malaguna@unizar.es

摘要

Abstract: Nickel-yttria stabilized zirconia (Ni-YSZ) cermet is the most commonly used anode in solid oxide fuel cells (SOFCs). The current article provides an insight into parameters which affect cell performance and stability by reviewing and discussing the related publications in this field. Understanding the parameters which affect the microstructure of Ni-YSZ such as grain size (Leng et al 2003 J. Power Sources 117 26-34) and ratio of Ni to YSZ, volume fraction of porosity, pore size and its distribution, tortuosity factor, characteristic pathway diameter and density of triple phase boundaries is the key to designing a fuel cell which shows high electrochemical performance. Lack of stability has been the main barrier to commercialization of SOFC technology. Parameters influencing the degradation of Ni-YSZ supported SOFCs such as Ni migration inside the anode during prolonged operation are discussed. The longest Ni-supported SOFC tests reported so far are examined and the crucial role of chromium poisoning due to interconnects, stack design and operating conditions in degradation of SOFCs is highlighted. The importance of calcination and milling of YSZ to development of porous structures suitable for Ni infiltration is explained and several methods to improve the electrochemical performance and stability of Ni-YSZ anode supported SOFCs are suggested.
- long-term stability /
- Ni /
- YSZ /
- microstructure /
- SOFC /
- anode
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Figure 1. Schematic of (a) an oxygen ion conducting and (b) proton conducting SOFC.

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Figure 2. (a) SEM image taken by a low acceleration voltage (1 kV) secondary electron detector. Bright, gray and dark colors are Ni, YSZ and epoxy, respectively. Reprinted from [21]. Copyright (2008), with permission from Elsevier. (b) Schematic of TPB region inside a typical Ni-YSZ AFL. [26] John Wiley & Sons. [© 2018 John Wiley & Sons, Ltd].

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Figure 3. (a) Reconstructed 3D anode microstructures (Ni: yellow, 8 YSZ: blue, pore: transparent), (b) the corresponding Ni phase of each sample illustrates that Ni grains are not percolated in samples A1 and A2 while they are almost totally percolated in sample A3. Reprinted from [41]. Copyright (2011), with permission from Elsevier.

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Figure 4. Schematic of the characteristic pathway diameter concept. (Red arrows highlight the characteristic pathway for the Ni phase, and percolating TPB between Ni (red), YSZ (gray) and pore (transparent) are circled in green). Reproduced from [52]. © 2019 The Electrochemical Society.

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Figure 5. Cross-sections SEM images of (a)-(c) pure Ni anodes reduced at 500 C, (d), (e) 800 C and (f), (g) 1000 C, (a) right after reduction, (b), (d), (f) before operation and (c), (e), (g) after operation and kept at 800 C under humidified hydrogen for 100 h [64].

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Figure 6. TEM images of YSZ powders after 72 h milling. (a) As-received Tosoh YSZ (b) calcined at 1300, milled for 72 h (c) calcined at 1400, milled for 72 h and (d) calcined at 1500, milled for 72 h. [79] John Wiley & Sons. [© 2011 The American Ceramic Society].

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Figure 7. (a) YSZ zeta potential curve as a function of pH and (b) amount of acid or base per unit of YSZ surface consumed for pH adjustment. Reprinted from [76]. Copyright (2012), with permission from Elsevier.

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Figure 8. SEM images of the YSZ substrate sintered at 1350 C. (a) Tosoh YSZ + 20 vol.% graphite, (b) Tosoh YSZ + 20 vol.% PMMA, (c) calcined 1500 C-milled YSZ + 20 vol.% graphite and (d) calcined 1500 C-milled YSZ + 20 vol.% PMMA. [79] John Wiley & Sons. [© 2011 The American Ceramic Society].

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Figure 9. (a) Ni-YSZ coverage by SDC near the interface of the fuel electrode and electrolyte, (b) YSZ coverage by LSM near the interface of the cathode and electrolyte. Reprinted from [99]. Copyright (2014), with permission from Elsevier.

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Figure 10. (a) Electrochemical performance of the Ni-SDC infiltrated cell at different temperatures, (b) OCV curve during a redox cycling test at 650 C. Reproduced from [109]. © 2014 The Electrochemical Society.

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Figure 11. SEM images showing the microstructure of infiltrated porous YSZ support structures (a) within the Ni-SDC infiltrated porous YSZ anode and (b) within the middle of a typical Ni infiltrated porous YSZ support. Reprinted from [14]. Copyright (2014), with permission from Elsevier.

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Figure 12. SEM images of the cross-section of the anode after running under humidified hydrogen for 150 h. (a) Substrate with fine YSZ grains and pores (b) substrate with large pores. Reprinted from [110]. Copyright (2015), with permission from Elsevier.

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Figure 13. SEM images of the cell following testing. (a) Interfaces between cathode, electrolyte, and part of the cell anode, (b) interface between Ni-YSZ support and Ni-BZCYYb AFL. [122] John Wiley & Sons. [© 2017 The American Ceramic Society].

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Figure 14. Location of the samples taken from the inlet, middle and the outlet of the cell. Reprinted from [126]. Copyright (2015), with permission from Elsevier.

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Figure 15. Quantified microstructure parameters conducted for the reference sample and the sample after 3700 h of long-term SOFC operation for (a) TPB length density (b) average grain size (c) tortuosity factor and (d) volume fraction. Samples were taken at different locations of the cell in the vicinity of the anode/electrolyte interface. Reprinted from [126]. Copyright (2015), with permission from Elsevier.

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Figure 16. Stability test for a stack operating at 700 C with 0.5 A cm^-2. The fluctuations of the voltage for cell 6 is due to a contact wire issue and not the degradation. Reprinted from [126]. Copyright (2015), with permission from Elsevier.

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Figure 17. Visualization of skeletonized phase networks in the anode sample after redox cycling for Ni (top left), YSZ (top right), pores (bottom left) and all three skeletons superimposed. Reprinted from [153]. Copyright (2013), with permission from Elsevier.

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Figure 18. The F1004-08 four-cell stack with LSM/YSZ cathode fabricated at Julich operated at 800 C for 19 000 h. The composition of the single cells can be found in table 2. Reprinted from [128]. Copyright (2012), with permission from Elsevier.

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Figure 19. Stability tests of stacks developed at Julich with different IC protective coating, cathode contact material and IC materials (Crofer 22 APU vs ITM). Reprinted from [125]. Copyright (2020), with permission from Elsevier.

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Figure 20. Stability test of the stack F1004-21 fabricated at Julich. Reprinted from [131]. Copyright (2018), with permission from Elsevier. Details of the test condition are described in table 2.

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Figure 21. Stability of different stacks developed at Julich with WPS-MnO_x protective coating onto the IC at 700 C and 800 C. As can be seen, changing the IC material did not affect the degradation rate. Reprinted from [125]. Copyright (2020), with permission from Elsevier.

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Figure 22. The effect of fuel type and fuel utilization on the stability of two stacks at 700 C developed at Julich. The composition of the single cells is described in table 2. Stack 2018-07 undergoes a change of fuel utilization from 40% to 80% and type of fuel from hydrogen to liquefied natural gas. Reprinted from [125]. Copyright (2020), with permission from Elsevier.

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Table 1. Summary of the long-term stack and single cell tests mentioned in the text. SP, FL, TC, CD, FU, OU, WPS and T stand for screen print, functional layer thermal cycling, current density, fuel utilization, oxygen utilization, wet powder spray and temperature, correspondingly.

	Year	Anode	Electrolyte	Cathode	Studied parameters	Reason for degradation	Improving factor	Degradation rate (% in mV kh^-1)	Test condition	Duration (h)	Reference
1	2015Six-cell stack SOFC power Co.	Ni-YSZ240 m	YSZ	GDC + LSCF/GDC 50 mLSCF contact layer	Ni-YSZ anode microstructureFIB-SEM 3D reconstruction	Ni coarsening specially at the inlet of the cellReduction of Ni:YSZ ratio from 50:50 vol.% to lower value a sign of the diffusion of Ni from FL to the Supp.Reduction of TBP density from 5 to 3 m m^-3 close to the electrolyte	Improvement of the mixed conducting LSCF cathode kinetics graduallyIncrease of the volume fraction of the YSZ close to the electrolyte extending the reaction zoneDesign factors such as the gas distributor channels and temperature management affect the microstructure locally	0	T: 800 CH₂ 1.8 l min^-1 N₂ 1.2 l min^-1 Air 18 l min^-1 FU 75% Air inlet 630 C Fuel inlet 550 C	3700	[126]
2	2017Commercial cell	Ni-YSZ500 m Ni-YSZ FL 12 m	3-YSZ	GDC(2 m) + LSC (10-20 m)	Performance of the stack at high flow of H₂ and airPerformance of the stack at low flow of H₂ and air60 thermal cycles (700 C-250 C and 700 C-50 C)	For long-term test before the thermal cycles: Ni agglomeration at anode (also new pore formation)After thermal cycles: vertical cracks inside the cathode + cathode/GDC interface separation (CTE mismatch)	Cells were resistant to thermal cyclesFor 700 C-250 C and 700 C-50 C thermal cycles: almost the same degradation ratesIncreasing the T from 700 C to 800 C and returning back to 700 C power recovery for 8.1%	1.16 for I2.64 for II	T: 700 CI: 3000 h: H₂ 0.8 l min^-1 and air 2 LPM II: 2000 h: H₂ 0.5 LPM and air 1.5 LPM CD 0.4 A cm^-2 TC 1 C min^-1	5000	[127]
3	2012Four-cell stack	Ni-YSZ	YSZ	LSM	The effect of spinel protective coating onto the IC to suppress Cr species evaporation and migration at cathode side	Mn diffusion from LSM into the YSZ grain boundary YSZ fracture + short circuiting the cell	MCF coating protective spinel onto the IC and LCC10 contact suppressing Cr evaporation and migration into the cathode	0.5	T 800 CFU 39.8% OU 26.6% CD 0.5 A cm^-2	19 000	[128]
4	2011Two-cell stack F1002-95	Ni-YSZ	YSZ	GDC (7 m) + LSCF (40 m)Cr-retention layer	Post-mortem analysis of the microstructure and composition	Interaction between LSCF and Cr evaporated from the ICSrCrO₄ crystals formation at IC/cathode interface and forming insulating layer graduallyIron oxide corroded spots close to the IC/protective coat interface due to the lack of Cr inside the IC	MnO_x protective coat and perovskite contact layer onto the IC at the air side suppressing Cr species evaporation from IC	1	T 700 CCD 0.5 A cm^-2 Fuel: 3% humidified H₂ FU 40% Air	17 660	[129]
5	2013Stack F1002-97	Ni-8 YSZ(1 mm)	YSZ10 m	GDC(5 m SP) + LSCF (SP) MnO_x protective layer + LCC12 contact layer by WPS	The effect of protective layer coated onto the IC on the stability of the cellCoating methods of layers	Cr poisoning of the cathode from the ICThermomechanical stress onto the sealing materialTemperature gradient inside the large cell surface and stress into the sealing gas leakage	Protective later onto the IC to trap the Cr speciesOptimized sealing material reliable sealing in long-termChanging the design of the ICs for better gas flow and sealing issuesAdding LCC10 contact layer to reduce the degradation (compared 3500 h without this layer)	0.9(before 4 kh) 0.3 (40-70 kh) 0.6 (0-70 kh average)	T 700 CCD 0.5 A cm^-2 H₂ 1.400 SLM H₂O 0.373 SLM Air 5.280 SLM (dried with due point of -40 C) FU 40% OU 25%	45 000	[130]
6	2013Four-cell stack F1004-21	Ni-8 YSZ	8-YSZ	GDC/LSCF	The effect of protective layer coated onto the IC on stabilityCoating methods of layers		Compared to 45 000 h:Coating GDC layer by physical vapor deposition (PVD) for a denser layer less unwanted diffusions into the electrolyteIC protective layer is coated by atmospheric plasma spray (APS) method denser layer and less Cr diffusion into the cathode	0.12	T 700 CAir 5280 SLM H₂ 1400 SLM H₂O 0.373 SLM FU 40% CD 0.5 A cm^-2	15 000	[130]
7	2018Four-cell stack F1004-21	Ni-YSZSupp. 500 m FL 7 m Tape cast	YSZ10 m (SP)	GDC(PVD 1 m) + LSCF 50 m LCC12 contact WPS Cr-retention layer APS	Post-mortem microstructural analysisProviding a hypothesis for degradation reason	Delamination of the anode/electrolyte interface (Mn diffusion from contact layer coated onto the IC to the YSZ grain boundaries) manganese oxide containing secondary phase formation inside YSZ grain boundaries YSZ fracture and possibly gas leakage	Cr-retention layer was coated by APS denser layer to suppress Cr diffusion into the cathodeVery low Cr content inside the cathode was found after the test low degradation rate is attributed to low Cr species inside the cathodeVolatize manganese oxide species should be avoided at cathode contact layer replacing contact layer to a contact layer without Mn	0.2	T 700 CCD 0.5 A cm^-2 H₂ 2.8 nl min^-1 H₂O 0.747 nl min^-1 Air 6.64 nl min^-1 FU 40%	35 000	[131]
8	2020Julich stacks comparison Electrolyte-supported cell	Ni-YSZNi:YSZ Vol ratio = 60:40	YSZ1500 C sinter	GDC + LSCFLSM-YSZ	Different protective coatings for Cr retention (WPS MnO_x vs APS-MCF)Different contact layer on cathode side (LCC12, LCC10, LSCF)Different IC material (ITM vs Crofer 22 APU)Operation temperature (700 C vs 800 C)Different fuel utilizationsDifferent fuels (H₂ vs CH₄)	Increasing the operation T by 100 C, increases the degradation rate by a factor of 1.5-2Applying cathode protective coat with WPS cannot suppress Cr diffusion into the cathode completelyMn diffuses from the contact layer (in the case of existing Mn inside contact layer) or LSM (being as the cathode) into the electrolyte grain boundaries	Changing the coating method of Cr retention layer from WPS to APS denser layer for suppressing Cr diffusion into the cathodeNo remarkable change in degradation using IC materialsChanging the Mn containing contact layer to LSFC possibly reduces Mn diffusion into the YSZ grainsApplying GDC by PVD method instead of SP method denser layer and less Sr-zirconate formation at electrolyte surfaceNo change in degradation rate is noticed by increasing the FU or changing the fuel to liquid natural gasChanging the cathode from LSM/YSZ to LSCF without MnGlass ceramic crystallization at 850 C for 10 h no interaction with the IC	0.2(the least voltage degradation value reported by them)	T 700 C and 800 CCD 0.5 A cm^-2 Fuels: H₂ (20% humidified) Dry H₂ CH₄/H₂ FU 40%-80%	For different stacks (5450-93 kh)	[125]
9	2018Five-cell stack	Ni-YSZ	YSZ	LCN-YSZ	Degradation of the interfaces (anode/electrolyte/cathode current collector interface)	Oxidation of IC at cathode side due to leakage of hydrogen and accelerating the iron oxides formation	Coating Ni paste at anode side between Ni foam and the anodeMn₂O₃-LCN layer formation at oxide scale of the IC on cathode side lowering the contact resistance and suppressing the oxidation of steel IC	1.5	T 750 CH₂: 1.67 SLM Air: 3 SLM CD 335 mA cm^-2	4400	[132]

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Table 2. Components for different stacks developed at Julich. SP, WPS and IC stand for screen print, wet powder spray and interconnect. All cells are composed of Ni-YSZ anode and YSZ electrolyte. Reprinted from [125]. Copyright (2020), with permission from Elsevier.

	Composition					Operation parameter
Stack (reference)	Cathode	Barrier layer	Cathode contact layer	IC Cr-retention layer	IC	Temp (C)	Current density (A cm^-2)	Fuel	Fuel utilization (%)	Operation time	Voltage degradation rate (%kh^-1)	Reference
F1002-95	LSCF	GDC (SP)	LCC12	WPS-MnO_x	Crofer22APU	700	0.5	H₂	40	17 660	1-1.4	[129]
F1002-97	LSCF	GDC (SP)	LCC10	WPS-MnO_x	TIM	700	0.5	H₂	40	>93 000	1/0.55	[123]
F1004-21	LSCF	GDC (PVD)	LCC12	APS-MCF	Crofer22APU	700	0.5	H₂	40	34 500	0.2	[131]
F1004-67	LSCF	GDC (SP)	LSCF	APS-MCF	Crofer22APU	700	0.5	H₂	40	>23 500	0.3	[201]
F1002-132	LSCF	GDC (SP)	LCC12	WPS-MnO_x	ITM	800	0.5	H₂	40	15 144	1.5	[202]
F1004-08	LSM/8 YSZ		LCC10	APS-MCF	Crofer22APU	800	0.5	H₂	40	19 036	0.4	[128]
F2018-07	LSCF	GDC (SP)	LCC10	APS-MCF	Crofer22APU	700	0.5	CH₄/H₂	70-80	5450	0.3	[203]

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