微管式固体氧化物燃料电池的制备及其性能研究
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摘要
微管式固体氧化物燃料电池(MT-SOFC)由于直径可以小到1毫米或百微米级,显现出多种优势,如机械性能增强,传质传热表面增大,体积功率密度提高,升降温速率加快等,在便携电源、交通运输动力电源和不间断电源(UPS)等领域具有广阔的应用前景。本文利用相转化-纺丝技术结合烧结工艺,制备了具有独特孔结构的中空纤维陶瓷微管,以此制备出微管式固体氧化物燃料电池,并对其性能进行了系统研究。
首先,以Y2O3稳定的ZrO2 (YSZ)和Sm2O3掺杂的CeO2 (SDC)为电解质材料,通过相转化法纺丝并烧结到1200~1600℃后,分别制备出YSZ和SDC中空纤维陶瓷微管,并以此制备了电解质支撑型MT-SOFC。研究发现,以纳米YSZ粉体为原料制备的电解质中空纤维陶瓷微管经过1600℃烧结后可以致密,抗弯强度最大355 MPa。以Ni/YSZ为阳极,La0.8Sr0.2MnO3-x (LSM)为阴极,以纯H2和O2分别为燃料气和氧化剂,在600℃,650℃,700℃,750℃,800℃和850℃操作时,燃料电池最大功率密度分别为13,24,35,48,61和87 mW·cm-2。以纳米SDC为原料的电解质中空纤维微管,经过1450℃烧结可以达到致密,抗弯强度超过200 MPa。使用Ni/SDC阳极和Ba0.5Sr0.5Co0.8Fe0.2O3-x (BSCF)阴极,以纯H2和O2为燃料气和氧化剂,在550℃,600℃,650℃,700℃和750℃操作时,燃料电池最大功率密度分别为27,45,67,89和106 mW·cm-2。两种电解质微管的直径为1.1~1.4 mm,壁厚210~230μm,因管壁中存在大量的指状孔结构,制约了电解质支撑型MT-SOFC功率密度进一步提高。
用改进的相转化纺丝-烧结工艺制备了多孔阳极中空纤维,经过1200~1400℃焙烧后获得NiO/YSZ阳极微管,并经H2还原得到Ni/YSZ金属陶瓷微管。在NiO/YSZ微管上,用浸渍-烧结法制备了一层致密YSZ电解质膜,然后在此阳极/电解质半电池上涂敷一层多孔La0.8Sr0.2MnO3-x (LSM)的阴极层,制备了阳极支撑型的MT-SOFC。研究表明,用改进的相转化纺丝-烧结工艺可以获得不对称孔结构的阳极微管,管壁内侧主要分布细长的指状孔层,而管壁的外侧主要分布着海绵状孔,微管表面则形成相对致密的表皮层。1400℃烧结的微管还原前后的孔隙率分别为21%和37%,还原前后抗弯强度分别为354MPa和178 MPa,常温至1400℃烧结直径收缩达到38%,1400℃烧结并还原的Ni/YSZ微管的电导率772S·cm-1。电解质浸渍液用EtOH/MEK溶剂体系,2%的PVB做粘结剂,5-6%的TEA做表面活性剂, YSZ含量为15%,在经过48h的球磨后,可以形成均匀稳定的悬浮浸渍液,经过2次浸渍可以制备成10μm的电解质膜。以LSM作为阴极材料,用EtOH/MEK溶剂体系配制的阴极浸渍液,浸渍一次并烧结至1200℃,形成20μm厚的阴极膜层。单电池的性能测试表明,对于该阳极支撑型MT-SOFC,以纯H2和O2做燃料气和氧化剂,工作温度为800℃时,最大功率密度为960 mW·cm-2,若以湿H2和空气作为燃料气和氧化剂,工作温度为800℃时,最大功率密度为820 mW·cm-2,以湿甲烷和空气为燃料气和氧化剂,工作温度为800℃时,最大功率密度为480 mW·cm-2,但容易积碳。
用相转化纺丝法结合烧结工艺制备中空纤维陶瓷的技术,为微管式固体氧化物燃料电池提供了一种简易,廉价,结构理想的制备方法。其中,电解质中空纤维支撑的燃料电池强度高,但是功率密度低;以阳极中空纤维上浸渍烧结形成致密的电解质膜和多孔的阴极膜,制备成多孔阳极支撑的高功率密度的单电池,其机械强度有所损失。
Micro tubular solid oxide fuel cells (MT-SOFCs) have millimeter or sub-millimeter grade diameters. They have attracted increasing interests due to their high volumetric power density, good mechanical properties, good thermo-cycling behavior, and quick start-up and shut-down operations. They will be applied in a variety of regions such as power sources for portable devices, uninterruptible power supplies (UPS) and dynamical power sources for automobiles. In this study, a phase inversion-sintering process has been developed to prepare the hollow fibre ceramic micro tubes with a special pore structure, from which the micro tubular solid oxide fuel cells with ideal structures and good performances were subsequently fabricated. It provides a new route to form the micro tubular solid oxide fuel cells with simplified operation and fairly low cost.
First of all, the YSZ (Y2O3 stabilized ZrO2) and SDC (Sm2O3 doped CeO2) electrolyte hollow fibers were prepared by the phase inversion-sintering process. The obtained YSZ and SDC hollow fibers have a diameter of 1.1~1.4mm and wall thickness of 210~230μm. Gas-tight YSZ hollow fibers may be obtained by sintering at temperatures higher than 1500℃, and their bending strength may attain up to 355MPa when sintered at 1600℃, while the SDC hollow fibers may be sintered into gas-tight micro tubes under temperatures higher than 1450℃with the bending strength of higher than 200MPa. The electrolyte-supported micro tubular SOFCs were fabricated by dip-coating Ni/YSZ anode and LSM (La0.8Sr0.2MnO3-x) cathode (for YSZ tube) or Ni/SDC anode and BSCF (Ba0.5Sr0.5Co0.8Fe0.2O3) cathode (for SDC tube) on the outer and inner surfaces of the YSZ or SDC electrolyte micro tubes. The YSZ and the SDC hollow fiber supported micro cells exhibit the highest output densities of 87 mW·cm-2 at 850℃and 106 mW·cm-2 at 750℃, respectively with H2/O2 as the fuel/oxidant. The low output power density is the result of the large thicknesses (210~230μm) of the electrolyte hollows and the finger-like pores conserved in the fiber walls. Therefore, the Ni containing anode-supported micro cells with an ultra thin electrolyte film may be a more favorable structure to give high output power densities.
The NiO/YSZ anode micro tubes have been prepared through an improved phase inversion-sintering process. NiO/YSZ anode powders were dispersed under stirring in the PESf/NMP polymer solution with PVP as the dispersant and pore-maker to form a spinning solution. Following the same procedures as for the preparation of YSZ and SDC fibers, NiO/YSZ hollow fibers were obtained. These fibers were then reduced by H2 at 800℃to form the Ni/YSZ cermet anode micro tubes. The effects of sintering temperature on the properties of the anode fibers have been extensively investigated. The resultant anode micro tubes possess an asymmetric structure comprising of a micro porous outer layer integrated with a finger-like porous sub-layer. Furthermore, the outer surface of the micro tubes is very smooth and is favorable for coating electrolyte films. As the sintering temperature was increased from 1200°C to 1400°C, the mechanical strength and the electrical conductivity of the Ni/YSZ hollow fibers increased from 35 MPa to 178 MPa and from 30S·cm-1 to 772 S·cm-1, respectively but the porosity decreased from 64.2% to 37.0%. The optimum sintering temperature was found to be between 1350°C and 1400°C for Ni/YSZ hollow fibers applied as the anode support for micro tubular SOFCs.
A dip-coating and co-sintering technique was applied to form the thin and dense YSZ electrolyte films on the outer surface of the NiO/YSZ micro tubes to form anode/electrolyte half cells. A suspension containing 15wt% of YSZ powder, 2wt% PVB binder, 5~6wt% TEA/YSZ surfactant and a small amount of DBP and lubricant PEG was firstly produced. The NiO/YSZ hollow fiber precursor was then dipped into the suspension for about 1 min so as to form a green YSZ film. Each dip-coating operation may finally produce a YSZ film of around 5μm thickness. In order to make a thin but dense enough electrolyte film, twice dip-coating operation resulting in a 10μm thickness film has proved to be the best. The one-coating resulted films (~5μm) may contain defects but three-coating resulted films (~15μm) are susceptible to crack in addition to the high electrical resistance. The coated NiO-YSZ hollow fibers were then co-sintered at 1400°C to form the dense electrolyte films that are integrated tightly with the porous anode micro tubes. On the outer surface of the anode/electrolyte half cell, a layer of porous LSM membrane was coated as the cathode so as to form a complete single micro tubular cell. The sintering temperature for the cathode integration is 1200°C, and the thickness of the final cathode is about 20μm.
The resultant anode-supported micro tubular cells were finally tested at various conditions. When H2/O2, H2/Air or CH4/Air were used as the fuel/oxidant gases, the highest power density of the anode-supported cell attains up to 960, 820 or 480 mW·cm-2 at 800°C, respectively. However, carbon deposition has been observed in the use of methane as fuel, leading to the fast degradation of the cell output density.
首先,以Y2O3稳定的ZrO2 (YSZ)和Sm2O3掺杂的CeO2 (SDC)为电解质材料,通过相转化法纺丝并烧结到1200~1600℃后,分别制备出YSZ和SDC中空纤维陶瓷微管,并以此制备了电解质支撑型MT-SOFC。研究发现,以纳米YSZ粉体为原料制备的电解质中空纤维陶瓷微管经过1600℃烧结后可以致密,抗弯强度最大355 MPa。以Ni/YSZ为阳极,La0.8Sr0.2MnO3-x (LSM)为阴极,以纯H2和O2分别为燃料气和氧化剂,在600℃,650℃,700℃,750℃,800℃和850℃操作时,燃料电池最大功率密度分别为13,24,35,48,61和87 mW·cm-2。以纳米SDC为原料的电解质中空纤维微管,经过1450℃烧结可以达到致密,抗弯强度超过200 MPa。使用Ni/SDC阳极和Ba0.5Sr0.5Co0.8Fe0.2O3-x (BSCF)阴极,以纯H2和O2为燃料气和氧化剂,在550℃,600℃,650℃,700℃和750℃操作时,燃料电池最大功率密度分别为27,45,67,89和106 mW·cm-2。两种电解质微管的直径为1.1~1.4 mm,壁厚210~230μm,因管壁中存在大量的指状孔结构,制约了电解质支撑型MT-SOFC功率密度进一步提高。
用改进的相转化纺丝-烧结工艺制备了多孔阳极中空纤维,经过1200~1400℃焙烧后获得NiO/YSZ阳极微管,并经H2还原得到Ni/YSZ金属陶瓷微管。在NiO/YSZ微管上,用浸渍-烧结法制备了一层致密YSZ电解质膜,然后在此阳极/电解质半电池上涂敷一层多孔La0.8Sr0.2MnO3-x (LSM)的阴极层,制备了阳极支撑型的MT-SOFC。研究表明,用改进的相转化纺丝-烧结工艺可以获得不对称孔结构的阳极微管,管壁内侧主要分布细长的指状孔层,而管壁的外侧主要分布着海绵状孔,微管表面则形成相对致密的表皮层。1400℃烧结的微管还原前后的孔隙率分别为21%和37%,还原前后抗弯强度分别为354MPa和178 MPa,常温至1400℃烧结直径收缩达到38%,1400℃烧结并还原的Ni/YSZ微管的电导率772S·cm-1。电解质浸渍液用EtOH/MEK溶剂体系,2%的PVB做粘结剂,5-6%的TEA做表面活性剂, YSZ含量为15%,在经过48h的球磨后,可以形成均匀稳定的悬浮浸渍液,经过2次浸渍可以制备成10μm的电解质膜。以LSM作为阴极材料,用EtOH/MEK溶剂体系配制的阴极浸渍液,浸渍一次并烧结至1200℃,形成20μm厚的阴极膜层。单电池的性能测试表明,对于该阳极支撑型MT-SOFC,以纯H2和O2做燃料气和氧化剂,工作温度为800℃时,最大功率密度为960 mW·cm-2,若以湿H2和空气作为燃料气和氧化剂,工作温度为800℃时,最大功率密度为820 mW·cm-2,以湿甲烷和空气为燃料气和氧化剂,工作温度为800℃时,最大功率密度为480 mW·cm-2,但容易积碳。
用相转化纺丝法结合烧结工艺制备中空纤维陶瓷的技术,为微管式固体氧化物燃料电池提供了一种简易,廉价,结构理想的制备方法。其中,电解质中空纤维支撑的燃料电池强度高,但是功率密度低;以阳极中空纤维上浸渍烧结形成致密的电解质膜和多孔的阴极膜,制备成多孔阳极支撑的高功率密度的单电池,其机械强度有所损失。
Micro tubular solid oxide fuel cells (MT-SOFCs) have millimeter or sub-millimeter grade diameters. They have attracted increasing interests due to their high volumetric power density, good mechanical properties, good thermo-cycling behavior, and quick start-up and shut-down operations. They will be applied in a variety of regions such as power sources for portable devices, uninterruptible power supplies (UPS) and dynamical power sources for automobiles. In this study, a phase inversion-sintering process has been developed to prepare the hollow fibre ceramic micro tubes with a special pore structure, from which the micro tubular solid oxide fuel cells with ideal structures and good performances were subsequently fabricated. It provides a new route to form the micro tubular solid oxide fuel cells with simplified operation and fairly low cost.
First of all, the YSZ (Y2O3 stabilized ZrO2) and SDC (Sm2O3 doped CeO2) electrolyte hollow fibers were prepared by the phase inversion-sintering process. The obtained YSZ and SDC hollow fibers have a diameter of 1.1~1.4mm and wall thickness of 210~230μm. Gas-tight YSZ hollow fibers may be obtained by sintering at temperatures higher than 1500℃, and their bending strength may attain up to 355MPa when sintered at 1600℃, while the SDC hollow fibers may be sintered into gas-tight micro tubes under temperatures higher than 1450℃with the bending strength of higher than 200MPa. The electrolyte-supported micro tubular SOFCs were fabricated by dip-coating Ni/YSZ anode and LSM (La0.8Sr0.2MnO3-x) cathode (for YSZ tube) or Ni/SDC anode and BSCF (Ba0.5Sr0.5Co0.8Fe0.2O3) cathode (for SDC tube) on the outer and inner surfaces of the YSZ or SDC electrolyte micro tubes. The YSZ and the SDC hollow fiber supported micro cells exhibit the highest output densities of 87 mW·cm-2 at 850℃and 106 mW·cm-2 at 750℃, respectively with H2/O2 as the fuel/oxidant. The low output power density is the result of the large thicknesses (210~230μm) of the electrolyte hollows and the finger-like pores conserved in the fiber walls. Therefore, the Ni containing anode-supported micro cells with an ultra thin electrolyte film may be a more favorable structure to give high output power densities.
The NiO/YSZ anode micro tubes have been prepared through an improved phase inversion-sintering process. NiO/YSZ anode powders were dispersed under stirring in the PESf/NMP polymer solution with PVP as the dispersant and pore-maker to form a spinning solution. Following the same procedures as for the preparation of YSZ and SDC fibers, NiO/YSZ hollow fibers were obtained. These fibers were then reduced by H2 at 800℃to form the Ni/YSZ cermet anode micro tubes. The effects of sintering temperature on the properties of the anode fibers have been extensively investigated. The resultant anode micro tubes possess an asymmetric structure comprising of a micro porous outer layer integrated with a finger-like porous sub-layer. Furthermore, the outer surface of the micro tubes is very smooth and is favorable for coating electrolyte films. As the sintering temperature was increased from 1200°C to 1400°C, the mechanical strength and the electrical conductivity of the Ni/YSZ hollow fibers increased from 35 MPa to 178 MPa and from 30S·cm-1 to 772 S·cm-1, respectively but the porosity decreased from 64.2% to 37.0%. The optimum sintering temperature was found to be between 1350°C and 1400°C for Ni/YSZ hollow fibers applied as the anode support for micro tubular SOFCs.
A dip-coating and co-sintering technique was applied to form the thin and dense YSZ electrolyte films on the outer surface of the NiO/YSZ micro tubes to form anode/electrolyte half cells. A suspension containing 15wt% of YSZ powder, 2wt% PVB binder, 5~6wt% TEA/YSZ surfactant and a small amount of DBP and lubricant PEG was firstly produced. The NiO/YSZ hollow fiber precursor was then dipped into the suspension for about 1 min so as to form a green YSZ film. Each dip-coating operation may finally produce a YSZ film of around 5μm thickness. In order to make a thin but dense enough electrolyte film, twice dip-coating operation resulting in a 10μm thickness film has proved to be the best. The one-coating resulted films (~5μm) may contain defects but three-coating resulted films (~15μm) are susceptible to crack in addition to the high electrical resistance. The coated NiO-YSZ hollow fibers were then co-sintered at 1400°C to form the dense electrolyte films that are integrated tightly with the porous anode micro tubes. On the outer surface of the anode/electrolyte half cell, a layer of porous LSM membrane was coated as the cathode so as to form a complete single micro tubular cell. The sintering temperature for the cathode integration is 1200°C, and the thickness of the final cathode is about 20μm.
The resultant anode-supported micro tubular cells were finally tested at various conditions. When H2/O2, H2/Air or CH4/Air were used as the fuel/oxidant gases, the highest power density of the anode-supported cell attains up to 960, 820 or 480 mW·cm-2 at 800°C, respectively. However, carbon deposition has been observed in the use of methane as fuel, leading to the fast degradation of the cell output density.
引文
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