CN107645000A - A kind of SOFC two-phase composite cathode material and preparation method thereof - Google Patents

A kind of SOFC two-phase composite cathode material and preparation method thereof Download PDF

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CN107645000A
CN107645000A CN201710737400.4A CN201710737400A CN107645000A CN 107645000 A CN107645000 A CN 107645000A CN 201710737400 A CN201710737400 A CN 201710737400A CN 107645000 A CN107645000 A CN 107645000A
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李付绍
夏书标
闫宇星
成飞翔
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Qujing Normal University
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Abstract

The invention belongs to intermediate temperature solid oxide fuel cell（SOFC）A kind of technical field, and in particular to SOFC two-phases composite cathode new material and preparation method thereof.The two-phase proportion for setting composite forms (1x)Ca3Co2O6/xCe1.8Sm0.2O1.9（0≤x＜ 1）, complex phase cathode material is synchronously prepared using sol-gal process " one pot ".First press the stoichiometric proportion preparing metal salt of compound composition（Nitrate or acetate）Solution；Total metal ion is pressed again：Ethylenediamine tetra-acetic acid：Citric acid=1：1：1 ratio adds two kinds of complexing agents, and pH to 89 is adjusted with ammoniacal liquor；Finally complex solution is dried again, calcined, target product can be obtained by annealing.Wherein, Ca3Co2O6For hexagonal structure, space group isR‑3C, Ce1.8Sm0.2O1.9For cubic structure, space group isFM3‑M。

Description

A kind of SOFC two-phase composite cathode material and preparation method thereof
Technical field
The invention belongs to intermediate temperature solid oxide fuel cell（SOFC）Technical field, and in particular to a kind of SOFC two-phases are answered Close negative electrode new material (1-x)Ca3Co2O6/xCe1.8Sm0.2O1.9（0 ≤x＜ 1）And preparation method thereof.
Technical background
SOFC（Solid-oxide fuel cells, SOFC）It is a kind of directly that hydrocarbon fuel is straight Switch through the TRT for turning to electric energy, there is efficiency high, pollute small, fuel-flexible.Traditional SOFC operation temperature is high Up to 1000 oC or so, this proposes very high requirement, the construction and fortune of battery to electrode material, battery component and auxiliary device Row maintenance cost is high.Reduce matching degree, the reduction operating cost that operation temperature is beneficial between improvement each part of battery.So And once reduce operation temperature, the Ohmic resistance of electrolyte and the interface impedance of electrode can increase therewith again.With anode-supported The application of type battery structure and perfect, the polarization resistance in sofc cathode during hydrogen reduction of electrolytic thin-membrane preparation technology Then turn into the most important impedance source of battery, the output characteristics of battery will be played a decisive role.Therefore, the suitable catalysis of selection Component is one of essential measure for improving electrochemical cathode performance.
In middle low temperature SOFC, ABO3Type perovskite structure has obtained numerous studies containing cobalt/cobalt oxide.This type oxide With good oxygen reduction reaction catalytic activity and higher " ion-electron " mixed conductivity, be it is current it is wide it is concerned in One of low temperature sofc cathode material, mainly there is La1-x Sr x CoO3-δ （δIt is as follows for oxygen vacancy）、Ba1-x Sr x Co1-y Fe y O3-δ 、 Sr1-x RE x CoO3-δ （RE is rare earth element）、REBaCo2O5+δ And its derivative etc..However, the thermal coefficient of expansion of such material （Thermal expansion coefficient, TEC）It is mostly very high, differed with the TEC of main flow SOFC electrolytes compared with Greatly, such as Y2x Zr1-2x O2-x （YSZ）、Ce1-x Sm x O2-δ （SDC）And La1-x Sr x Ga1-y Mg y O3-δ （LSGM）Deng so as to add electricity The sintering difficulty of pond part, also it is unfavorable for the stability operation of battery.In addition, wherein many cathode materials, electrical conductivity is low, lattice Heat endurance difference the problems such as it is also very prominent.
Therefore, using the relatively small new cobalt base oxide Ca of thermal coefficient of expansion3Co2O6Have as sofc cathode material There is obvious advantage.However, the cathode material of this electrothermic type equally faces huge challenge, be purely by way of negative electrode, by its six The limitation of square lattice structure, oxygen ion transport performance and cubic structure or the ABO of quasi- cubic structure3Type cobalt-based Perovskite Phase compares Difference, cause its catalytic performance not high.It can be changed to a certain extent by means such as doping, other compound cobalt-based perovskite compounds Kind Ca3Co2O6The chemical property of cathode material is purely by way of, but these conventional methods all have such or such office Limit.For example, improvement of the doping to the intrinsic performance of material is limited, other compound cobalt-based perovskites then introduce more cobalt members Element, so that negative electrode thermal coefficient of expansion can increase again.
The content of the invention
Further to play hexagonal lattice structure oxide Ca3Co2O6Cathode catalysis potentiality, improve Ca3Co2O6Electrode Performance, the present invention is using introducing fast-ionic conductor Ce0.8Sm0.2O1.9（SDC）Method overcome the material in oxygen ion transport Deficiency on energy, to extend Ca3Co2O6" three-phase " interface during work, so as to devise a kind of structure and composition novelty SOFC two-phase composite cathode materials.
The chemical composition of SOFC two-phase composite cathode material prepared by the present invention forms：(1-x) Ca3Co2O6/xCe0.8Sm0.2O1.9（xFor nominal mole accountings of the SDC in complex phase composition）, wherein Ca3Co2O6For hexagonal structure, Space group isR-3C；Ce1.8Sm0.2O1.9It is for cubic structure, space groupFM3-M。
SOFC two-phase composite cathode material (1-x)Ca3Co2O6/xCe1.8Sm0.2O1.9Preparation side Method, comprise the following steps.
Two-phase composite cathode material (1-s of the A by cerous nitrate and calcium nitrate according to SOFCx) Ca3Co2O6/xCe1.8Sm0.2O1.9Middle calcium and respective mole of accounting of Ce elements are configured to the mixed solution of calcium cerium nitrate, cerium, The concentration of calcium nitrate solution is 2-3 mol/L.
Two-phase composite cathode material (1-s of the B by cobalt acetate or cobalt nitrate according to SOFCx) Ca3Co2O6/xCe1.8Sm0.2O1.9Mole accounting of middle cobalt element, it is added to the calcium cerium nitrate mixed solution that step A is configured to In, and be stirred, metal cation mixed solution is obtained, the wherein concentration of cobalt acetate or cobalt nitrate solution is 2-3 mol/L.
C is by Sm2O3According to the two-phase composite cathode material (1- of SOFCx)Ca3Co2O6/xCe1.8Sm0.2O1.9Mole accounting of middle samarium element, add low-grade fever stirring and dissolving in concentrated nitric acid solution and obtain samarium nitrate solution, nitre The concentration of sour samarium solution is 2-3 mol/L.
The samarium nitrate solution that D obtains step C is mixed to get solid oxygen with the metal cation mixed solution in step B Composite cathode material (the 1- of compound fuel cellx)Ca3Co2O6/xCe1.8Sm0.2O1.9Whole metal ions of required mole of accounting Source.
Ethylenediamine tetra-acetic acid is added in the solution that E obtains to step D（EDTA）With citric acid as complexing agent, matter is added Amount ratio is total metal ion：Ethylenediamine tetra-acetic acid：Citric acid=1：1：1（Mol ratio）, and be stirred continuously.
Mixtures of the F into step E adds concentrated ammonia liquor, until ethylenediamine tetra-acetic acid all dissolving and solution clarifications, are used in combination Concentrated ammonia liquor and dust technology adjust solution ph to 8-9, and finally give brown solution.
The brown solution obtained in step F is put into evaporation in 100 oC baking oven and obtains sticky gel by G, then will Sticky gel is put into 150 oC baking oven and thoroughly dries its moisture, obtains xerogel.
Xerogel in step G is put into the h of combustion decomposition 5 in 450 oC Muffle furnace by H, obtains the production of black burnning ash shape Thing.
I is levigate by the black burnning ash shape product in step H, is put into 960-1020 oC high temperature air stove and anneals 10 H, you can obtain the two-phase composite cathode material (1- of SOFCx)Ca3Co2O6/xCe1.8Sm0.2O1.9.High temperature The temperature control process of air furnace is：960-1020 oC temperature is heated to from room temperature with 2 oC/min programming rate, then is incubated 10 H, room temperature is then cooled to 3 oC/min cooling rate.
Beneficial effects of the present invention：A kind of good novel solid oxidation fuel cell cathodes of chemical property have been invented to urge Change component (1-x)Ca3Co2O6/xCe1.8Sm0.2O1.9, wherein 0≤x＜ 1, using " one pot " synchronous preparation of sol-gel process Double-phase composite even particle size distribution, without the generation of any other impurities phase, at the same with the preparation of conventional compounding ingredients Process is compared, and " one pot " synchronous preparation can greatly simplify the preparation process of material.Compared to single phase cathode material C a3Co2O6, The thermal expansion of two-phase composite cathode material is smaller, interface impedance（Area specific resistance,ASR）It is lower；800 Under oC, it is using hydrogen as fuel, to formxWhen=0.5 composite is as negative electrode, electrolyte-supporting type monocell it is defeated It is 620 mWcm to go out power peak-2Left and right.The present invention requires low to synthesis device, and simple to operate, battery sintering process is without spy It is different to require.Synthesized material structure is stable, and electrode combination property is more preferably.
Brief description of the drawings
Fig. 1 is the SEM spectrum of the product of the embodiment of the present invention 1.
Fig. 2 is product of the embodiment of the present invention (1-x)Ca3Co2O6/xCe1.8Sm0.2O1.9XRD spectra.
Fig. 3 is the electrochemical impedance spectroscopy of the product of the embodiment of the present invention 1.
Fig. 4 be the product of the embodiment of the present invention 1 monocell at different temperatures operating voltage and power density with electric current Variable density tendency chart.
Fig. 5 is the SEM spectrum of the product of the embodiment of the present invention 2.
Fig. 6 is the electrochemical impedance spectroscopy of the product of the embodiment of the present invention 2.
Fig. 7 be the product of the embodiment of the present invention 2 monocell at different temperatures operating voltage and power density with electric current Variable density tendency chart.
Fig. 8 is the SEM spectrum of the product of the embodiment of the present invention 3.
Fig. 9 is the electrochemical impedance spectroscopy of the product of the embodiment of the present invention 3.
Figure 10 be the product of the embodiment of the present invention 3 monocell at different temperatures operating voltage and power density with electric current Variable density tendency chart.
Embodiment
With reference to specific embodiment, the invention will be further described.
Embodiment 1
According to the single phase cathode material C a of SOFC3Co2O6（I.e.x= 0）Middle calcium with cobalt element is respective rubs That accounting, weighs calcium nitrate, cobalt acetate is made into mixed solution；Ethylenediamine tetra-acetic acid is added into calcium cobalt mixed ion solutions （EDTA）With citric acid as complexing agent, addition mass ratio is total metal ion：Ethylenediamine tetra-acetic acid：Citric acid=1：1：1 （Mol ratio）, and be stirred continuously, while concentrated ammonia liquor is added, until ethylenediamine tetra-acetic acid all dissolves and clarifies solution, and adjust Solution ph is saved to 8-9, obtains brown-red solution；Brown-red solution is put into baking oven and first toasted with 100 oC temperature, will Sticky gel is obtained after most moisture evaporations, then is toasted with 150 oC temperature, the moisture in sticky gel is thorough Xerogel is obtained after the drying of bottom；Xerogel is put into the h of combustion decomposition 5 in 450 oC Muffle furnace, obtains the production of black burnning ash shape Thing；After taking-up black burnning ash shape product is levigate, places into 960 oC air furnace 10 h that anneal and can obtain soild oxide Fuel cell single phase cathode material C a3Co2O6。
SEM morphology analysis, shown in Fig. 1, Ca are carried out to synthesized positive electrode3Co2O6The fruit of " honey raisin tree " is commonly called as with one kind Son is extremely similar to, and particle is relatively large.XRD diffraction is carried out to the positive electrode of preparation, test result is shown in Fig. 2x=0, contrast It is pure that figure Plays spectral line can be seen that synthetic sample, without impurity peaks, Ca3Co2O6For hexagonal structure, space group isR-3C。 Electrochemical impedance spectrometry is carried out to the interface of sample cathode material and electrolyte, as a result as shown in Figure 3, it can be seen that interface Impedance is about 0.28 Ω .cm2.The monocell for making negative electrode with specimen material is tested, as a result as shown in figure 4, monocell In 800 oC, power output peak value is 410 mW.cm-2Left and right.
Embodiment 2
According to the two-phase composite cathode material 0.75Ca of SOFC3Co2O6/0.25Ce1.8Sm0.2O1.9（I.e.x = 0.25）Middle respective mole of accounting of calcium cerium cobalt element, weighs calcium nitrate, cerous nitrate, cobalt acetate and is made into mixed solution；According still further to solid The composite cathode material 0.75Ca of oxide body fuel cell3Co2O6/0.25Ce1.8Sm0.2O1.9Mole accounting of middle samarium element, Weigh Sm2O3Dissolved in input concentrated nitric acid solution, the solution of calcic, cerium, cobalt ions is mixed into after solution clarification；To calcium cerium cobalt samarium Ethylenediamine tetra-acetic acid is added in solion（EDTA）With citric acid as complexing agent, addition mass ratio is total metal ion： Ethylenediamine tetra-acetic acid：Citric acid=1：1：1（Mol ratio）, and be stirred continuously, while concentrated ammonia liquor is added, until ethylenediamine tetrem It is sour all to dissolve and clarify solution, and solution ph is adjusted to 8-9, obtain brown-red solution；Brown-red solution is put into baking First toasted in case with 100 oC temperature, sticky gel, then the temperature with 150 oC will be obtained after most moisture evaporations Baking, xerogel will be obtained after the moisture in sticky gel thoroughly drying；Xerogel is put into 450 oC Muffle furnace and fired Burn and decompose 5 h, obtain black burnning ash shape product；After taking-up black burnning ash shape product is levigate, place into 990 oC air furnace 10 h that anneal can obtain the composite cathode material 0.75Ca of SOFC3Co2O6/0.25Ce1.8Sm0.2O1.9。
SEM morphology analysis is carried out to synthesized positive electrode, shown in Fig. 5, the feature of two-phase component is obvious, an a kind of phase It is uniformly adhered in another phase.XRD diffraction is carried out to the positive electrode of preparation, test result is shown in Fig. 2x=0.25, contrast It is pure that figure Plays spectral line can be seen that synthetic sample, does not have any third-party impurity peaks beyond target composition phase, Ce1.8Sm0.2O1.9For cubic structure, space group isFM3-M.Electrochemistry has been carried out to the interface of sample cathode material and electrolyte Impedance spectrometry, as a result as shown in Figure 6, it can be seen that interface impedance is about 0.25 Ω .cm2.Negative electrode is made with specimen material Monocell is tested, as a result as shown in fig. 7, monocell power output peak value in 800 oC is 420 mW.cm-2Left and right.
Embodiment 3
According to the two-phase composite cathode material 0.5Ca of SOFC3Co2O6/0.5Ce1.8Sm0.2O1.9（I.e.x = 0.5）Middle respective mole of accounting of calcium cerium cobalt element, weighs calcium nitrate, cerous nitrate, cobalt acetate and is made into mixed solution；According still further to solid The composite cathode material 0.5Ca of oxide body fuel cell3Co2O6/0.5Ce1.8Sm0.2O1.9Mole accounting of middle samarium element, claim Take Sm2O3Dissolved in input concentrated nitric acid solution, the solution of calcic, cerium, cobalt ions is mixed into after solution clarification；To calcium cerium cobalt samarium from Ethylenediamine tetra-acetic acid is added in sub- solution（EDTA）With citric acid as complexing agent, addition mass ratio is total metal ion：Second Ethylenediamine tetraacetic acid (EDTA)：Citric acid=1：1：1（Mol ratio）, and be stirred continuously, while concentrated ammonia liquor is added, until ethylenediamine tetra-acetic acid All dissolve and clarify solution, and adjust solution ph to 8-9, obtain brown-red solution；Brown-red solution is put into baking oven It is middle first to be toasted with 100 oC temperature, sticky gel will be obtained after most moisture evaporations, then dried with 150 oC temperature It is roasting, xerogel will be obtained after the moisture in sticky gel thoroughly drying；Xerogel is put into 450 oC Muffle furnace and burnt 5 h are decomposed, obtain black burnning ash shape product；After taking-up black burnning ash shape product is levigate, places into 1020 oC air furnace and move back 10 h of fire are the composite cathode material 0.5Ca that can obtain SOFC3Co2O6/0.5Ce1.8Sm0.2O1.9。
SEM morphology analysis is carried out to synthesized positive electrode, as shown in figure 8, the feature of two-phase component is obvious, Yi Zhongyi Mutually it is uniformly adhered in another phase.XRD diffraction is carried out to the positive electrode of preparation, test result is shown in Fig. 2x=0.5, it is right It is pure that synthetic sample is can be seen that than figure Plays spectral line, without any third-party impurity peaks beyond target composition phase.To sample The interface of product cathode material and electrolyte has carried out electrochemical impedance spectrometry, as a result as shown in Figure 9, it can be seen that interface impedance About 0.12 Ω .cm2.The monocell for making negative electrode with specimen material is tested, and as a result as shown in Figure 10, monocell exists Power output peak value is 620 mW.cm during 800 oC-2Left and right, it is much higher than the chemical property of single phase cathode.

Claims (6)

  1. A kind of 1. SOFC two-phase composite cathode material, it is characterised in that the chemical composition group of the composite Turn into：(1-x)Ca3Co2O6/xCe0.8Sm0.2O1.9；Phase composition can be according to the molar ratio of two-phase in compositexCarry out flexible Allotment, wherein 0≤x＜ 1；Ca3Co2O6It is for hexagonal structure, space groupR-3C；Ce1.8Sm0.2O1.9For cubic structure, space Group beFM3-M。
  2. 2. a kind of preparation method of SOFC two-phase composite cathode material, it is characterised in that including following step Suddenly：
    Two-phase composite cathode material (1-s of the A by cerous nitrate and calcium nitrate according to SOFCx)Ca3Co2O6/xCe1.8Sm0.2O1.9Middle calcium is configured to nitrate mixed solution with respective mole of accounting of Ce elements；
    Two-phase composite cathode material (1-s of the B by cobalt acetate or cobalt nitrate according to SOFCx)Ca3Co2O6/xCe1.8Sm0.2O1.9Mole accounting of middle cobalt element, it is added in the calcium cerium nitrate mixed solution that step A is configured to, and carries out Stirring, obtains metal cation mixed solution；
    C is by Sm2O3According to the two-phase composite cathode material (1- of SOFCx)Ca3Co2O6/xCe1.8Sm0.2O1.9 Mole accounting of middle samarium element, add micro- heating stirring in concentrated nitric acid solution and dissolve to obtain samarium nitrate solution；
    The samarium nitrate solution that D obtains step C is mixed to get soild oxide with the metal cation mixed solution in step B Composite cathode material (the 1- of fuel cellx)Ca3Co2O6/xCe1.8Sm0.2O1.9Whole metal ion sources of required mole of accounting；
    Two kinds of complexing agents of ethylenediamine tetra-acetic acid and citric acid are added in the mixed solution that E obtains to step D, add mass ratio For total metal ion：Ethylenediamine tetra-acetic acid：Citric acid=1：1：1, and be stirred continuously；
    Mixtures of the F into step E adds concentrated ammonia liquor, until ethylenediamine tetra-acetic acid all dissolving and solution clarifications, and with dense ammonia Water and dust technology adjust solution ph to 8-9, and finally give brown solution；
    The brown solution obtained in step F is put into evaporation in 100 oC baking oven and obtains sticky gel by G, then will be sticky Gel be put into 150 oC baking oven and thoroughly dry its moisture, obtain xerogel；
    Xerogel in step G is put into the h of combustion decomposition 5 in 450 oC Muffle furnace by H, obtains black burnning ash shape product；
    I is levigate by the black burnning ash shape product in step H, is put into 960-1020 oC high temperature air stove 10 h that anneal, i.e., It can obtain the two-phase composite cathode material (1- of SOFCx)Ca3Co2O6/xCe1.8Sm0.2O1.9。
  3. 3. the preparation method of SOFC two-phase composite cathode material according to claim 2, its feature It is：Cerium, the concentration of calcium nitrate solution are 2-3 mol/L in the step A.
  4. 4. the preparation method of SOFC two-phase composite cathode material according to claim 2, its feature It is：The cobalt acetate or the concentration of cobalt nitrate solution added in the step B is 2-3 mol/L.
  5. 5. the preparation method of SOFC two-phase composite cathode material according to claim 2, its feature It is：The concentration of samarium nitrate solution in the step C is 2-3 mol/L.
  6. 6. the preparation method of SOFC two-phase composite cathode material according to claim 2, its feature It is：The temperature control process of the step I high temperature stoves is：960-1020 o are heated to from room temperature with 2 oC/min programming rate C temperature, then 10 h are incubated, room temperature is then cooled to 3 oC/min cooling rate.
CN201710737400.4A 2017-08-24 2017-08-24 Solid oxide fuel cell two-phase composite cathode material and preparation method thereof Active CN107645000B (en)

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CN116034091A (en) * 2020-05-05 2023-04-28 华威大学 Ion conductor

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CN116034091A (en) * 2020-05-05 2023-04-28 华威大学 Ion conductor
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