CN105244523B - A kind of SOFC with anti-carbon function - Google Patents

A kind of SOFC with anti-carbon function Download PDF

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CN105244523B
CN105244523B CN201510540168.6A CN201510540168A CN105244523B CN 105244523 B CN105244523 B CN 105244523B CN 201510540168 A CN201510540168 A CN 201510540168A CN 105244523 B CN105244523 B CN 105244523B
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anode
catalyst
catalyst layer
sofc
ysz
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CN105244523A (en
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陈绘丽
王芬
常宏
李思殿
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Shanxi University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/10—Fuel cells with solid electrolytes
    • H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88—Processes of manufacture
    • H01M4/8825—Methods for deposition of the catalytic active composition
    • H01M4/8864—Extrusion
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/90—Selection of catalytic material
    • H01M4/9016—Oxides, hydroxides or oxygenated metallic salts
    • H01M4/9025—Oxides specially used in fuel cell operating at high temperature, e.g. SOFC
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Sustainable Development (AREA)
  • Sustainable Energy (AREA)
  • Inert Electrodes (AREA)

Abstract

The invention provides a kind of SOFC with anti-carbon function, belongs to the SOFC based on nickel anode, including anode, electrolyte, negative electrode, quartzy airway tube, is characterized in setting independent catalyst layer in anode-side.Described catalyst layer is made up of substrate and catalyst；Described base material is the high oxide material of hardness；Described catalyst is the material for having to hydrocarbon fuel high oxidation catalytic activity.The present invention not only solves battery caused by catalyst mismatches with anode material hot expansibility and is split up problem, and effectively inhibits anode carbon distribution, substantially increases the stability and reliability of SOFC.

Description

A kind of SOFC with anti-carbon function
Technical field
The present invention relates to electrochmical power source, and in particular to the SOFC based on nickel anode, is more particularly to A kind of SOFC with anti-carbon function.
Background technology
SOFC (SOFC) is applied widely with energy conversion efficiency height, fuel, pollution-free etc. excellent Point becomes the fuel electricity that a new generation can be used for fixed power station, vehicles assist type power supply and small-sized movable power supply Pond.Ni-based Ceramic Composite anode because it has the advantages that high electrochemical activity, high electronic conductance, stability are good, cheap, Stable performance is shown when using hydrogen as fuel, is still the most frequently used anode material so far.But in view of hydrogen life Production, storage and transport in terms of technology restriction, using hydrogen as fuel SOFC over the next several years it is interior can not possibly obtain widely should With.Because SOFC is a kind of high-temperature power generation device (500 degree of -1000 degree), existing carbon-based fuel in principle can be in SOFC Generation is available for the hydrogen and CO to generate electricity, such as natural gas, coal bed gas, shale gas, biogas, gasoline, liquid under condition of work Liquefied oil gas etc., therefore these materials can serve as SOFC fuel.But under SOFC high temperature operating conditions, hydrocarbon fuel is all Inevitably it is cracked to form carbon distribution to be deposited on Ni anodes, on the one hand plugs Ni surface-actives site, catalytic performance Decline, on the other hand because the hot expansibility of carbon distribution and anode material mismatches, with increasing for carbon distribution, battery rises Split.Current many seminars are actively developing the improvement of the SOFC nickel anodes with anti-carbon performance.One of which method is The catalyst coat that one layer of promotion hydrocarbon fuel reforming is covered in anode surface causes hydrocarbon fuel reaching Ni anodes generation electricity Chemical reaction is before that in anode three phase boundary area electrochemistry oxygen occurs for CO and hydrogen, then hydrogen and CO first by catalytic reforming Change reaction so as to produce electric energy.But the hot expansibility of most catalyst materials and anode material is inconsistent, if catalysis Agent coating directly overlays galvanic anode surface using spraying or mode of printing, hot swollen due to material in battery temperature-rise period Swollen performance mismatches, and frequently results in temperature battery needed for not being raised to also and is just split up (Fig. 2 a).Therefore existing using sprays Or the catalytic amount that the catalyst layer of printing process preparation uses must be seldom, but catalyst amount deficiency causes fuel weight again The problem of whole insufficient.In addition, catalyst, which directly overlays anode surface, also plugs a part of anode stomata, increase combustion gas is expanded Dissipate resistance.
The content of the invention
It is an object of the invention to for it is existing based on the solid oxide fuel cell applications of nickel anode in hydrocarbon combustion The problem of anode carbon distribution is easily produced during material, there is provided a kind of stabilization can be used for hydrocarbon fuel and the solid with anti-carbon function Oxide fuel cell.
A kind of SOFC based on nickel anode provided by the invention, including negative electrode, electrolyte, anode, Quartzy airway tube, it is characterised in that independent catalyst layer is set in anode-side.
Described catalyst layer is prepared by a method comprising the following steps to obtain：(1) by base material and a small amount of pore-creating Agent is well mixed, and flakiness is molded with tablet press machine；(2) catalyst is well mixed with a small amount of pore creating material, paving is sprinkled upon step (1) system Into sheet surface, it is molded altogether, the demoulding, be placed in Muffle kiln roasting.
Described base material is Al2O3, zirconium dioxide, the high oxide material of hardness such as silica.
The described pore creating material such as high temperature combustible such as organic matter, carbon material.
Described catalyst is the material for having to hydrocarbon fuel high oxidation catalytic activity, including can produce oxygen vacancies Perovskite material, such as Sr2MoFeO6-δ, La0.6Sr0.4Co0.9Fe0.1O3-δDeng；Also include containing transition metal for example nickel, copper, iron, Cobalt, molybdenum, the material of cerium and its oxide, such as NiO/BaO/CeO2/Al2O3, NiO/BaO/CeO2。
A kind of preparation method of SOFC based on nickel anode provided by the invention, including following step Suddenly：
1) oxide material of high rigidity is well mixed with a small amount of pore creating material, flakiness is molded with tablet press machine；
2) catalyst is well mixed with a small amount of pore creating material, paving is sprinkled upon sheet surface made of step 1), molded altogether, takes off Mould, Muffle kiln roasting is placed in, obtains the catalyst layer being made up of substrate and catalyst；
3) catalyst layer of above-mentioned preparation is positioned over to the upper end of quartzy airway tube, catalyst is consolidated towards fuel-side with silver paste It is fixed；
4) silver wire is bonded respectively in the negative electrode and anode of battery, and be positioned over catalyst layer towards catalyst layer by anode-side Top, battery and catalyst layer are sealed on quartz ampoule together with high-temperature electric conduction silver paste.
NiO/BaO/CeO provided by the invention2/Al2O3Catalyst, it is prepared by the method comprised the following steps：Press Ni:BaO:CeO2:Al2O3Mass fraction is 13:2:42.5:42.5 weigh nickel nitrate, barium nitrate, cerous nitrate, aluminum nitrate, spend Mol ratio (the G/M of glycine, glycine and metal ion is added after ionized water dissolvingn+) than being 3:1.Heating on electric furnace is placed in stir Mix, after water is evaporated can spontaneous combustion obtain primary powder, be put into baking oven 240 DEG C and dry 8 hours.After cooling 850 in Muffle furnace DEG C calcining 2h, heating rate is 5 DEG C of min-1。
NiO/BaO/CeO provided by the invention2Catalyst, it is prepared by the method comprised the following steps：By Ni:BaO: CeO2Mass fraction is 13:2:85 weigh nickel nitrate respectively, barium nitrate, cerous nitrate, with adding glycine after deionized water dissolving, Mol ratio (the G/M of glycine and total metal ionn+) it is 3:1.Heating stirring on electric furnace is placed in, spontaneous combustion acquisition is first after water is evaporated Level powder, it is then placed in baking oven 240 DEG C and dries 8 hours.850 DEG C of calcining 2h, heating rate are 5 DEG C in Muffle furnace after cooling min-1。
Compared with prior art, the present invention has following beneficial effect：First, do not have between catalyst layer and anode layer Substantial close contact, independently of anode layer, it will not occur because the hot expansibility of catalyst and anode material mismatches Caused by battery be split up (Fig. 2 a), it is often more important that cell discharge performance is good.Secondly, fuel gas first passes through catalyst layer and entered Row catalytic reforming reaction generates CO and hydrogen, and then both gases reach galvanic anode by catalyst substrate and carry out electrochemistry Reaction produces electric energy.By the stop of catalyst layer, the hydrocarbon fuel concentration of Ni anode surfaces substantially reduces, and reduces cracking Deposition of the carbon in anode；3rd, because catalyst layer and battery are independent of each other, the amount that can increase catalyst is improved to fuel Catalytic conversion efficiency.Although embodiment is using wet methane as fuel, it is contemplated that different hydrocarbon fuels have corresponding reforming catalyst, The battery thus prepared according to the inventive method is applicable to any hydrocarbon fuel.Therefore, the present invention not only solves catalyst Battery caused by thermal expansion is split up problem, and effectively inhibits anode carbon distribution so that battery performance is stable.
Brief description of the drawings
Fig. 1 is described solid oxide fuel cell structure schematic diagram
Fig. 2 (a) is that catalyst is sprayed in the temperature-rise period of galvanic anode surface due to hot expansibility with art spray gun Battery is split up caused by mismatch
Fig. 2 (b) is the electricity after wet methane constant-current discharge is tested 40 hours with the SOFC of the present invention Pond pattern
Fig. 3 is the discharge performance life test being not added with the blank SOFC equal conditions of catalyst layer
Fig. 4 is SOFC discharge performance life test prepared by embodiment 1
Fig. 5 is SOFC discharge performance life test prepared by embodiment 2
Fig. 6 is SOFC discharge performance life test prepared by embodiment 3
Fig. 7 is SOFC discharge performance life test prepared by embodiment 4
Fig. 8 is SOFC discharge performance life test prepared by embodiment 5
Fig. 9 is SOFC discharge performance life test prepared by embodiment 6
Embodiment
With reference to specific embodiment, the present invention is described in detail, and following examples will be helpful to the technology of this area Personnel further appreciate that the present invention, but do not limit the scope of the invention.
YSZ refers to 8% yttria stabilized zirconia in following examples, and LSM refers to La0.8Sr0.2MnO3-δ.Pore-creating Agent PVB refers to polyvinyl butyral resin.
Embodiment 1
Monocell, Al are used as using the NiO-YSZ/YSZ/LSM-YSZ of classics2O3As the substrate of catalyst layer, by certain ratio The NiO/BaO/CeO of example synthesis2Mixture is catalyst：
(1) prepared by catalyst powder：By Ni:BaO:CeO2Mass fraction is 13:2:85 weigh nickel nitrate, nitric acid respectively Barium, cerous nitrate, with the mol ratio (G/M that glycine, glycine and total metal ion are added after deionized water dissolvingn+) it is 3:1.Put In heating stirring on electric furnace, after water is evaporated spontaneous combustion obtain primary powder, be then placed in baking oven 240 DEG C and dry 8 hours.After cooling 850 DEG C of calcining 2h in Muffle furnace, heating rate is 5 DEG C of min-1。
(2) prepared by catalyst layer：0.3g mass ratioes are weighed as 9:1 Al2O3The powder being well mixed with PVB, in 144MPa It is lower to suppress catalyst layer substrate with compression mold, then 0.03g is mixed with to 10%PVB catalyst powder and is dispersed in substrate Surface, 240MPa is molded altogether, the demoulding, and 900 degree of roastings obtain the catalyst layer being made up of substrate and catalyst in 4 hours.
(3) catalyst layer of above-mentioned preparation is positioned over to the upper end of quartzy airway tube, catalyst is consolidated towards fuel-side with silver paste It is fixed；
(4) silver wire is bonded respectively in the negative electrode and anode of NiO-YSZ/YSZ/LSM-YSZ batteries, and urged by anode-side court Agent layer is positioned over the top of catalyst layer, is sealed in battery and catalyst layer on quartz ampoule together with high-temperature electric conduction silver paste.
With wet methane (97% methane, 3% vapor) for fuel, according to conventional solid oxide fuel battery testing method Chemical property and battery discharge life-span are tested, battery is in 333mA/cm2The steady 13 hours electricity afterwards that discharge under load current Pressure is stable (see Fig. 4), battery surface crack-free.
Control：The battery of the same catalyst layer prepared using art spray gun spraying process, temperature do not rise to required temperature also Degree battery is split up (Fig. 2 (a)), can not test.
Embodiment 2
Using NiO-YSZ/YSZ/LSM-YSZ as monocell, YSZ is as catalyst substrate, the NiO/BaO/CeO of synthesis2 For catalyst：
Preparation method is with embodiment 1, and difference is in by the Al in embodiment 12O3Replace with YSZ, the electric discharge longevity of battery Life is shown in Fig. 5.
Embodiment 3
Using NiO-YSZ/YSZ/LSM-YSZ as monocell, Al2O3As catalyst substrate, synthesize by a certain percentage NiO/BaO/CeO2/Al2O3For catalyst：
(1) prepared by catalyst powder：By Ni:BaO:CeO2:Al2O3Mass fraction is 13:2:42.5:42.5 weigh nitric acid Nickel, barium nitrate, cerous nitrate, aluminum nitrate, with the mol ratio that glycine, glycine and metal ion are added after deionized water dissolving (G/Mn+) than being 3:1.Heating stirring on electric furnace is placed in, the primary powder of meeting spontaneous combustion acquisition, is put into baking oven 240 DEG C after water is evaporated Drying 8 hours.After cooling in Muffle furnace 850 DEG C calcining 2h, heating rate is 5 DEG C of min-1。
(2) Fig. 6 is seen in-(5) with embodiment 1, the constant-current discharge life-span of battery.
Embodiment 4
Using NiO-YSZ/YSZ/LSM as monocell, YSZ is as catalyst substrate, the NiO/BaO/CeO of synthesis2/Al2O3 For catalyst：
Preparation method is with embodiment 3, and difference is in by the Al in embodiment 32O3YSZ is replaced with, the constant current of battery is put Electric life is shown in Fig. 7.
Embodiment 5
Using NiO-YSZ/YSZ/LSM as monocell, Al2O3As catalyst substrate, the double calcium titaniums synthesized by a certain percentage Pit wood material Sr2MoFeO6-δFor catalyst：
(1) prepared by catalyst powder：By SrMo0.5Fe0.5O3Chemical formula metering ratio, take a certain amount of Sr (NO3)2、 (NH4)6Mo7O24·4H2O and Fe (NO3)3, deionized water stirring is added until being completely dissolved.By ethylenediamine tetra-acetic acid (EDTA) Ammonia spirit is added in the metal ion solution, adds a certain amount of citric acid, wherein, EDTA:Citric acid:Metal ion: NH3·H2O=1:2:1:10 (mol ratios).Finely tune appropriate citric acid cause the pH of precursor solution for faintly acid (pH=6~ 7).After heating removes excessive moisture, gained gel presoma is put in air dry oven, dried at 250 DEG C by 8h Obtain solid precursor.Finally solid precursor is put into Muffle furnace, 2h is calcined under 1100 degree of air atmospheres to be obtained Sr2MoFeO6-δPowder.Powder is tested by X-ray powder diffractions.
(2) prepared by catalyst layer：It is 25 in mass ratio by alumina powder and PVB powder end:After 3 is well mixed, weigh The 0.3g powder loads Φ 13mm steel moulds, first suppresses the base powder with 144MPa pressure by tablet press machine, obtains substrate Powder；Again by Sr1Mo0.5Fe0.5Powder and PVB powder end are 12 in mass ratio:After 5 is well mixed, the 0.3g catalyst powders are weighed Body, and it is uniformly layered on substrate powder, secondary press mold (240MPa), pressurize 1min are carried out by tablet press machine, compacting is formed Catalyst/substrate dual-layer green body body, 4h is calcined at 900 DEG C, and it is 5 DEG C of min to control heating rate-1, obtain catalyst layer.
(3)-(5) preparation method is shown in Fig. 8 with embodiment 1, the discharge life of battery.
Embodiment 6
Using NiO-YSZ/YSZ/LSM as monocell, Al2O3As catalyst substrate, the perovskite synthesized by a certain percentage Material La0.6Sr0.4Co0.9Fe0.1O3-δFor catalyst：
(1) prepared by catalyst powder：By La0.6Sr0.4Co0.9Fe0.1O3-δChemical formula metering ratio, take a certain amount of La (NO3)3、Sr(NO3)2、Co(NO3)3And Fe (NO3)3, deionized water stirring is added until being completely dissolved.By ethylenediamine tetra-acetic acid (EDTA) ammonia spirit is added in the metal ion solution, adds a certain amount of citric acid, wherein, EDTA:Citric acid:Gold Belong to ion:NH3·H 2O=1:2:1:10 (mol ratios).Finely tune appropriate citric acid and make it that the pH of precursor solution is faintly acid (pH=6~7).After heating removes excessive moisture, gained gel presoma is put in air dry oven, 250oPassed through under C Cross 8h and be dried to obtain solid precursor.Finally solid precursor is put into Muffle furnace, 2h is calcined under 900 degree of air atmospheres is La can be obtained0.6Sr0.4Co0.9Fe0.1O3-δPowder.Powder is tested by X-ray powder diffractions.
(2)-(5) preparation method is shown in Fig. 9 with embodiment 1, the discharge life of battery.

Claims (4)

1. a kind of SOFC based on nickel anode, including negative electrode, electrolyte, anode, quartzy airway tube, it is special Sign is, independent catalyst layer is set in anode-side；
Described catalyst layer is prepared by a method comprising the following steps to obtain：1) base material is mixed with a small amount of pore creating material Uniformly, it is molded flakiness with tablet press machine；2) catalyst is well mixed with a small amount of pore creating material, paving is sprinkled upon thin slice made of step 1) Surface, it is molded altogether, the demoulding, it is placed in Muffle kiln roasting.
A kind of 2. SOFC based on nickel anode as claimed in claim 1, it is characterised in that described base Bottom material is the high oxide material of hardness；
The high oxide material of the hardness is Al2O3Or YSZ, the YSZ refer to 8% yttria stabilized zirconia.
3. a kind of SOFC based on nickel anode as claimed in claim 1, it is characterised in that described urges Agent is that can produce the perovskite material of oxygen vacancies, or the material of the oxide containing transition metal oxide and cerium.
4. a kind of preparation method of the SOFC based on nickel anode, it is characterised in that comprise the following steps：
1) oxide material of high rigidity is well mixed with a small amount of pore creating material, flakiness is molded with tablet press machine；
2) catalyst being well mixed with a small amount of pore creating material, paving is sprinkled upon sheet surface made of step 1), molded altogether, the demoulding, Muffle kiln roasting is placed in, obtains the catalyst layer being made up of substrate and catalyst；
3) catalyst layer of above-mentioned preparation is positioned over to the upper end of quartzy airway tube, catalyst is fixed towards fuel-side with silver paste；
4) silver wire is bonded respectively in the negative electrode and anode of battery, and be positioned over the upper of catalyst layer towards catalyst layer by anode-side Battery and catalyst layer, are sealed on quartz ampoule by side together with high-temperature electric conduction silver paste.
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CN107919485B (en) * 2017-11-10 2021-04-09 北京英博新能源有限公司 Fuel cell cooling assembly and fuel cell system
CN108869017A (en) * 2018-05-29 2018-11-23 薛平 A kind of flameless combustion class hydrogen internal combustion engine
CN108598494B (en) * 2018-06-21 2020-09-22 西安科技大学 Fuel cell anode and fuel cell using same
CN109904497B (en) * 2019-01-09 2020-07-10 华中科技大学 Anti-carbon-deposition metal-supported solid oxide fuel cell and preparation method thereof
CN111883800A (en) * 2020-06-19 2020-11-03 广东工业大学 Processing equipment of solid oxide fuel cell
CN114361471A (en) * 2022-01-10 2022-04-15 国家能源集团新能源有限责任公司 Integrated independent catalytic layer, preparation method and application

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