CN101585558A - The preparation method of nano-powder of cathode of solid oxide fuel cell - Google Patents
The preparation method of nano-powder of cathode of solid oxide fuel cell Download PDFInfo
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- CN101585558A CN101585558A CNA2008100616319A CN200810061631A CN101585558A CN 101585558 A CN101585558 A CN 101585558A CN A2008100616319 A CNA2008100616319 A CN A2008100616319A CN 200810061631 A CN200810061631 A CN 200810061631A CN 101585558 A CN101585558 A CN 101585558A
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Abstract
A kind of preparation method of nano-powder of cathode of solid oxide fuel cell in turn includes the following steps: a. is according to (La
1-xSr
x)
1-zCo
1-yFeyO
3-δThe stoichiometric ratio of chemical formula is with the La (NO of matched doses
3)
36H
2O, Sr (NO
3)
2, Co (NO
3)
26H
2O, Fe (NO
3)
39H
2O is dissolved in a certain amount of deionized water, stirs into the metallic ion mixed liquor that uniform concentration is 0.75～1.25mol/L, wherein 0≤x≤0.4,0≤y≤0.8,0≤z≤0.1; B. under 70～80 ℃, add complexing agent and stir formation colloidal solution in metallic ion mixed liquor, heated and stirred 8～20 hours forms the heavy-gravity gel until the colloidal solution dehydration; C. with this gel between 90～200 ℃ dry 5～10 hours, pre-treatment was 5～10 hours between 200～400 ℃, obtains bulk precursor powder; D. precursor powder was calcined between 500～800 ℃ 2～5 hours, obtained nano-powder of cathode of solid oxide fuel cell.Compared with prior art, the invention has the advantages that: the present invention is by adopting the method for the compound complexing of citric acid-ethylenediamine tetraacetic acid (EDTA), the solution metal ion is evenly spread in the reticulated structure of complex compound and go, avoided the segregation of composition, more solved agglomeration traits, prepared powder is very even, and pattern is good.
Description
Technical field
The present invention relates to a kind of nanometer grade powder preparation method who can be used as Solid Oxide Fuel Cell (SOFC) cathode material.
Background technology
Existing Solid Oxide Fuel Cell (SOFC) is a kind of energy conversion device that directly chemical energy is converted into electric energy, have high-level efficiency, remarkable advantage such as pollution-free, all solid state, in large, medium and small type power house, portable, compact power, and there is wide application prospect in fields such as military affairs, aerospace.Monocell is a SOFC essentially consist unit, and the internal resistance of monocell is mainly from the polarization resistance of negative electrode.It is most important to the performance that improves the SOFC monocell to reduce cathodic polarization resistance.Studies show that, the key that reduces cathodic polarization resistance is to keep the nano-micro structure of negative electrode that negative electrode is combined with ionogen closely, referring to Wei Guo Wang, Mogens Mogensen, High-performancelanthanum-ferrite-base cathode for SOFC.Solid State Ionics, 2005,176,452-462.This requires high performance SOFC cathode material should be nanometer grade powder, and is evenly distributed, hard aggregation-free, regular shape almost spherical.
The SOFC of development in early stage need be 800～1000 ℃ of operations down, and higher working temperature has proposed some harsh requirements for selecting for use of associated materials, has restricted the commercialization of SOFC technology.The trend of SOFC development is to reduce its operating temperature, but along with the reduction of operating temperature, the electrode especially speed of reaction of negative electrode descends, and polarization of electrode increases, and therefore needs to seek to satisfy the cathode material that SOFC uses under middle low temperature.(La
1-xSr
x)
1-zCo
1-yFeyO
3-δBe that perovskite oxide is good ion-electron mixing conductor material, can reach 1*10 at 800 ℃ of its electronic conductivities
2-1*10
3Scm-1, oxygen ionic conductivity reaches 1*10
-1Scm
-1, referring to Teroka Y, Zhang H.M., Okamoto K., et al.Mixed ionic-electronic conductivity of La
1-xSr
xCo
1-yFeyO
3Perovskite-type oxides.MaterialResearch Bulletin, 1998,23 (1): 51-58, have better chemical stability and thermostability simultaneously, and with a new generation such as CGO in low temperature SOFC electrolyte good consistency is arranged, be one of at present ideal middle low temperature SOFC cathode material.
Therefore, study suitable perovskite powder preparation method, make it satisfied simultaneously (La
1-xSr
x)
1-zCo
1-yFe
yO
3-δBe the high-performance and the mass preparation of perovskite oxide, the commercialization of low temperature SOFC technology in promoting is had great importance.At present, the method for synthetic perovskite powder has a lot, as solid phase method, coprecipitation method, spray pyrolysis, Citrate trianion method, and the EDTA-CA complex method, these methods respectively have characteristics, some problems but go back ubiquity.
Solid phase method needs high-temperature calcination, and the powder homogeneity is very poor, and sintering activity is low; The coprecipitation process complexity, powder reuniting is serious, referenced patent number is ZL02822542.2, denomination of invention, and (Granted publication number: Chinese invention patent CN1285138C), this patent adopt high-temperature roasting to obtain (La for " Solid Oxide Fuel Cell with composite oxides and manufacture method thereof "
1-xSr
x)
1-zCo
1-yFe
yO
3-δNano-powder.
Spray pyrolysis is higher to equipment requirements, referring to the patent No. is that ZL200510061747.9, denomination of invention are " preparation method of fuel battery powder of solid oxide and purposes " (Granted publication number: CN1315211C), this method also needs roasting except spraying, technology is more complicated also, and preparation cost is higher.
The Citrate trianion method, the EDTA-CA complex method need be controlled the pH value of solution, the EDTA-CA complex method also needs earlier EDTA to be dissolved in the ammoniacal liquor, these have increased the difficulty of operation, and the affiliation that adds of a large amount of ammoniacal liquor causes producing too much gas in the last handling process, makes that presoma is serious to expand even with the powder ejection, product is difficult to collect, productive rate is lower, is unsuitable for industry and amplifies.As application number is that 02126556.9., name are called " a kind of method for preparing the intermediate temperature solid oxide fuel cell electrolyte superfine powder " (publication number: CN1471188A) the Chinese invention patent application is open, need to add ammoniacal liquor in this method and regulate the pH value, complex process, productive rate are also lower.
Summary of the invention
Technical problem to be solved by this invention is the preparation method that the nano-powder of cathode of solid oxide fuel cell that a kind of technology is simple, the products obtained therefrom performance is good is provided at the above-mentioned state of the art.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: a kind of preparation method of nano-powder of cathode of solid oxide fuel cell in turn includes the following steps:
A, according to (La
1-xSr
x)
1-zCo
1-yFe
yO
3-δThe stoichiometric ratio of chemical formula is with the La (NO of matched doses
3)
36H
2O, Sr (NO
3)
2, Co (NO
3)
26H
2O, Fe (NO
3)
39H
2O is dissolved in a certain amount of deionized water, stirs into uniform 0.75～1.25mol/L metallic ion mixed liquor, wherein 0≤x≤0.4,0≤y≤0.8,0≤z≤0.1;
B, under 70～80 ℃, in metallic ion mixed liquor, add complexing agent and stir and form uniform colloidal solution, heated and stirred 8～20 hours forms the heavy-gravity gel until the colloidal solution dehydration;
C, with this gel between 90～200 ℃ dry 5～10 hours, pre-treatment is 5～10 hours between 200～400 ℃, obtains bulk precursor powder;
D, precursor powder were calcined between 500～800 ℃ 2～5 hours, promptly obtained high performance nano-powder of cathode of solid oxide fuel cell (La
1-xSr
x)
1-zCo
1-yFe
yO
3-δ
Complexing agent described in the described step b can be citric acid and ethylenediamine tetraacetic acid (EDTA), and wherein, the mol ratio of citric acid and metal ion is 0.1: 1～10: 1, and the mol ratio of ethylenediamine tetraacetic acid (EDTA) and metal ion is 0.1: 1～5: 1.
As preferably, the nano-powder of cathode of solid oxide fuel cell particle diameter described in the steps d is evenly distributed with 50～100mm, and the shape approximation spheroid is good.
Compared with prior art, the invention has the advantages that: the present invention is by adopting the method for the compound complexing of citric acid-ethylenediamine tetraacetic acid (EDTA), the solution metal ion evenly spread in the reticulated structure of complex compound to go, and avoided the segregation of composition, more solved agglomeration traits, prepared powder is very even, and pattern is good, gets final product pure phase at a lower temperature, particle diameter is little, be evenly distributed, hard aggregation-free, sintering activity is good; Raw material is that molecular level mixes, and can accurately control chemical dosage ratio; Need not to introduce ammoniacal liquor and control pH value of solution value, not high to equipment requirements, technology is simple, the productive rate height; The amplification test result is well stable, is suitable for suitability for industrialized production.
Description of drawings
Fig. 1 is that embodiment 1 is at 700 ℃ of processing (La after 5 hours
1-xSr
x)
1-zCo
1-yFe
yO
3-δThe XRD graphic representation of powder.
Fig. 2 is that embodiment 1 is at 700 ℃ of processing (La after 5 hours
1-xSr
x)
1-zCo
1-yFe
yO
3-δThe FESEM figure of powder.
Fig. 3 is that embodiment 2 is at 700 ℃ of processing (La after 5 hours
1-xSr
x)
1-zCo
1-yFe
yO
3-δPowder the XRD graphic representation.
Fig. 4 is that embodiment 2 is at 700 ℃ of processing (La after 5 hours
1-xSr
x)
1-zCo
1-yFe
yO
3-δThe FESEM figure of powder.
Embodiment
Embodiment describes in further detail the present invention below in conjunction with accompanying drawing.
Embodiment 1, with reference to illustrated in figures 1 and 2.
Press La: Sr: Co: Fe :=0.6: 0.4: 0.2: 0.8 chemical dosage ratio, with the La (NO of respective amount
3)
36H
2O, Sr (NO
3)
2, Co (NO
3)
26H
2O, Fe (NO
3)
39H
2O joins in the deionized water of 100ml, makes the metal ion solution of 1mol/L, mixes.Being warming up to 75 ℃, is 2: 1 according to the mol ratio of citric acid and metal ion, and the mol ratio of ethylenediamine tetraacetic acid (EDTA) and metal ion is that 1: 1 dosage adds citric acid and ethylenediamine tetraacetic acid (EDTA), continues to stir 8 hours, and solution dehydrates is the heavy-gravity gel.This gel was descended dry 5 hours at 130 ℃,,, obtain the La of about 10g perovskite structure 700 ℃ of calcinings 5 hours 250 ℃ of pre-treatment 5 hours
0.6Sr
0.4Co
0.2Fe
0.8O
3-δNanometer powder, as seen from Figure 1, product is a perovskite structure, no dephasign.Diameter of particle is 50～100nm as seen from Figure 2, does not have and reunites, and is evenly distributed.Because (La
1-xSr
x)
1-zCo
1-yFe
yO
3-δIn mixed Sr, Fe make O can't keep LaCoO
3In the integer chemical dosage ratio, produced the oxygen room, δ is used for representing the existence in oxygen room, but the quantity in oxygen room is owing to the complicacy of reacting can't quantitatively provide, so the general proportioning that only need write out La, Sr, Co, Fe gets final product, the oxygen room degree of corresponding proportioning compound has just been determined.
Press La: Sr: Co: Fe :=0.6: 0.4: 0.2: 0.8 chemical dosage ratio, with the La (NO of respective amount
3)
36H
2O, Sr (NO
3)
2, Co (NO
3)
26H
2O, Fe (NO
3)
39H
2O joins in the deionized water of 1000ml, makes the metal ion solution of 1mol/L, mixes.Being warming up to 70 ℃, is 2: 1 according to the mol ratio of citric acid and metal ion, and the mol ratio of ethylenediamine tetraacetic acid (EDTA) and metal ion is that 1: 1 dosage adds citric acid and ethylenediamine tetraacetic acid (EDTA), continues to stir 16 hours, and solution dehydrates is the heavy-gravity gel.This gel was descended dry 9 hours at 130 ℃,,, obtain the La of about 100g perovskite structure 700 ℃ of calcinings 5 hours 250 ℃ of pre-treatment 9 hours
0.6Sr
0.4Co
0.2Fe
0.8O
3-δNanometer powder, as seen from Figure 3, product is a perovskite structure, no dephasign.Diameter of particle is 50～100nm as seen from Figure 4, does not have and reunites, and is evenly distributed.
Embodiment 3
Press La: Sr: Co: Fe :=0.6: 0.4: 0.2: 0.8 chemical dosage ratio, with the La (NO of respective amount
3)
36H
2O, Sr (NO
3)
2, Co (NO
3)
26H
2O, Fe (NO
3)
39H
2O joins in the deionized water of 100ml, makes the metal ion solution of 1mol/L, mixes.Being warming up to 80 ℃, is 2: 1 according to the mol ratio of citric acid and metal ion, and the mol ratio of ethylenediamine tetraacetic acid (EDTA) and metal ion is that 1: 1 dosage adds citric acid and ethylenediamine tetraacetic acid (EDTA), continues to stir 8 hours, and solution dehydrates is the heavy-gravity gel.This gel was descended dry 6 hours at 100 ℃,,, obtain (the La of about 10g perovskite structure 700 ℃ of calcinings 5 hours 300 ℃ of pre-treatment 4 hours
0.6Sr
0.4)
0.9Co
0.2Fe
0.8O
3-δNanometer powder, product are perovskite structure, no dephasign.Diameter of particle is 50～100nm, does not have and reunites, and is evenly distributed.
Embodiment 4
Press La: Sr: Co: Fe :=0.6: 0.4: 0.2: 0.8 chemical dosage ratio, with the La (NO of respective amount
3)
36H
2O, Sr (NO
3)
2, Co (NO
3)
26H
2O, Fe (NO
3)
39H
2O joins in the deionized water of 1000ml, makes the metal ion solution of 1mol/L, mixes.Being warming up to 70 ℃, is 2: 1 according to the mol ratio of citric acid and metal ion, and the mol ratio of ethylenediamine tetraacetic acid (EDTA) and metal ion is that 1: 1 dosage adds citric acid and ethylenediamine tetraacetic acid (EDTA), continues to stir 16 hours, and solution dehydrates is the heavy-gravity gel.This gel was descended dry 8 hours at 150 ℃,,, obtain the La of about 100g perovskite structure 700 ℃ of calcinings 5 hours 180 ℃ of pre-treatment 10 hours
0.6Sr
0.4Co
0.2Fe
0.8O
3-δNanometer powder, product are perovskite structure, no dephasign.Diameter of particle is 50～100nm, does not have and reunites, and is evenly distributed.
Claims (3)
1, a kind of preparation method of nano-powder of cathode of solid oxide fuel cell in turn includes the following steps:
A, according to (La
1-xSr
x)
1-zCo
1-yFe
yO
3-δThe stoichiometric ratio of chemical formula is with the La (NO of matched doses
3)
36H
2O, Sr (NO
3)
2, Co (NO
3)
26H
2O, Fe (NO
3)
39H
2O is dissolved in a certain amount of deionized water, stirs into the metallic ion mixed liquor that uniform concentration is 0.75～1.25mol/L, wherein 0≤x≤0.4,0≤y≤0.8,0≤z≤0.1;
B, under 70～80 ℃, in metallic ion mixed liquor, add complexing agent and stir and form colloidal solution, heated and stirred 8～20 hours forms the heavy-gravity gel until the colloidal solution dehydration;
C, with this gel between 90～200 ℃ dry 5～10 hours, pre-treatment is 5～10 hours between 200～400 ℃, obtains bulk precursor powder;
D, precursor powder were calcined between 500～800 ℃ 2～5 hours, obtained nano-powder of cathode of solid oxide fuel cell.
2, preparation method according to claim 1, it is characterized in that the complexing agent described in the described step b is citric acid and ethylenediamine tetraacetic acid (EDTA), wherein, the mol ratio of citric acid and metal ion is 0.1: 1～10: 1, and the mol ratio of ethylenediamine tetraacetic acid (EDTA) and metal ion is 0.1: 1～5: 1.
3, preparation method according to claim 1 is characterized in that the nano-powder of cathode of solid oxide fuel cell particle diameter described in the described steps d is 50～100mm, is evenly distributed the shape approximation spheroid.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102180669A (en) * | 2011-03-18 | 2011-09-14 | 中国科学院宁波材料技术与工程研究所 | Method for co-sintering cathode and anode of electrolyte-supported solid oxide fuel cell |
| CN105428667A (en) * | 2015-12-10 | 2016-03-23 | 武汉科技大学 | Method for preparing cathode material of solid oxide fuel cell |
| CN108565479A (en) * | 2018-04-16 | 2018-09-21 | 淮阴工学院 | Attapulgite composite material and its preparation method and application |
| CN109742414A (en) * | 2019-01-09 | 2019-05-10 | 渤海大学 | A kind of intermediate temperature solid oxide fuel cell cathode material and the preparation method and application thereof |
| CN112687886A (en) * | 2020-12-22 | 2021-04-20 | 上海应用技术大学 | Intermediate-temperature solid oxide fuel cell composite cathode and preparation method thereof |
| RU2749746C1 (en) * | 2020-12-18 | 2021-06-16 | Федеральное государственное бюджетное учреждение науки Институт высокотемпературной электрохимии Уральского отделения Российской Академии наук | Electrode material for electrochemical devices |
| CN113809343A (en) * | 2021-09-17 | 2021-12-17 | 中国科学技术大学 | Carbon dioxide resistant solid oxide fuel cell cathode material and preparation method thereof |
| CN115228474A (en) * | 2022-07-20 | 2022-10-25 | 中南大学 | Metal colloid catalyst for oxygen evolution reaction under alkaline condition and preparation method and application thereof |
-
2008
- 2008-05-20 CN CNA2008100616319A patent/CN101585558A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102180669A (en) * | 2011-03-18 | 2011-09-14 | 中国科学院宁波材料技术与工程研究所 | Method for co-sintering cathode and anode of electrolyte-supported solid oxide fuel cell |
| CN105428667A (en) * | 2015-12-10 | 2016-03-23 | 武汉科技大学 | Method for preparing cathode material of solid oxide fuel cell |
| CN105428667B (en) * | 2015-12-10 | 2018-10-16 | 武汉科技大学 | A kind of preparation method of cathode material for solid-oxide fuel cell |
| CN108565479A (en) * | 2018-04-16 | 2018-09-21 | 淮阴工学院 | Attapulgite composite material and its preparation method and application |
| CN108565479B (en) * | 2018-04-16 | 2020-09-25 | 淮阴工学院 | Attapulgite composite material and preparation method and application thereof |
| CN109742414A (en) * | 2019-01-09 | 2019-05-10 | 渤海大学 | A kind of intermediate temperature solid oxide fuel cell cathode material and the preparation method and application thereof |
| RU2749746C1 (en) * | 2020-12-18 | 2021-06-16 | Федеральное государственное бюджетное учреждение науки Институт высокотемпературной электрохимии Уральского отделения Российской Академии наук | Electrode material for electrochemical devices |
| CN112687886A (en) * | 2020-12-22 | 2021-04-20 | 上海应用技术大学 | Intermediate-temperature solid oxide fuel cell composite cathode and preparation method thereof |
| CN112687886B (en) * | 2020-12-22 | 2022-07-05 | 上海应用技术大学 | Intermediate-temperature solid oxide fuel cell composite cathode and preparation method thereof |
| CN113809343A (en) * | 2021-09-17 | 2021-12-17 | 中国科学技术大学 | Carbon dioxide resistant solid oxide fuel cell cathode material and preparation method thereof |
| CN115228474A (en) * | 2022-07-20 | 2022-10-25 | 中南大学 | Metal colloid catalyst for oxygen evolution reaction under alkaline condition and preparation method and application thereof |
| CN115228474B (en) * | 2022-07-20 | 2024-03-12 | 中南大学 | Metal colloid catalyst for oxygen evolution reaction under alkaline condition and preparation method and application thereof |
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Open date: 20091125 |