CN105261765B - A kind of method that high temperature phase separation prepares LSM YSZ nanometer combined electrodes - Google Patents
A kind of method that high temperature phase separation prepares LSM YSZ nanometer combined electrodes Download PDFInfo
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- 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
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- 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
Abstract
This patent provides a kind of high temperature phase separation and prepares the method that solid-oxide fuel battery nano composite cathode improves battery performance and stability.(1) method that LSM electronic conductors and YSZ ion conductors are separated by high temperature is introduced into cell cathode simultaneously, the interphase interaction of two-phase, and more Lacking oxygens for being advantageous to oxygen reduction reaction are formd in material surface；(2) LSM and YSZ is covered in YSZ skeletons surface, the active sites three phase boundary of oxygen reduction reaction is not only present between LSM nano particles and YSZ skeletons, also it is dispersed throughout between LSM YSZ nano particles, dramatically speeds up oxygen reduction reaction, battery performance is improved to 2~3 times of conventional cathode；(3) the former body that drives used in this method is metal ion and the mixed liquor after complexing agent complexing, and each metal ion species reach the uniform mixing of atomic level, and two-phase is in close contact after high temperature is separated, limitation is grown up mutually, the stability of electrode significantly improves, 800 DEG C, 0.92A/cm2Constant-current discharge, 500h are undamped.
Description
Technical field
The present invention relates to compound cathode of solid oxide fuel battery, specifically a kind of high temperature phase separation prepares solid
The method of the nano combined negative electrodes of oxide fuel cell LSM-YSZ.
Background technology
SOFC is the energy conversion device that a kind of chemical energy by fuel is converted into electric energy,
It can be used for compact power, cogeneration and large power generating equipment, its efficiency high is pollution-free, and fuel range of choice is wide, hydrogen
The hydrocarbons such as gas, methane, biogas can be used as the fuel of SOFC, have a extensive future, because
And as the focus of numerous scholar's research.SOFC membrane electrode includes anode, electrolyte and negative electrode three parts,
Corresponding most classical electrode material is NiO/YSZ composite anodes, YSZ electrolyte and LSM/YSZ mechanical mixture negative electrodes respectively.It is right
For pandemic NiO/YSZ composite anodes support YSZ hull cells, produced in now on LSM/YSZ mechanical mixture negative electrodes
Raw polarization loss is to restrict the principal element of battery performance.In negative electrode, the electrochemical reducting reaction of oxygen is mainly happens is that, is wrapped
The oxygen included in gas phase is diffused into cathode surface by mesopore, thereon occur absorption, dissociation, and receive electronics change into oxygen from
Son enters several processes such as electrolyte lattice.And said process is required for very high reaction activity in addition to gas diffusion, reaction
Speed is slow【M.J.and M.Mogensen/Journal of The Electrochemical Society,
148(5),(2001),A433-A442；X.J.Chen et al./Journal of Power Sources,123,(2003),
17–25】, caused polarization loss is high, thus as the principal element of restriction solid-oxide fuel battery performance.Therefore study
Prepare high-performance and cathode material steady in a long-term be there is an urgent need to.(La1-xSrx)CoO3-δ(LSC)【O.Yamamoto；
Y.Takeda；R.Kanno；M.Noda./Solid State Ionics,22,(1987),241–246.】,(La1-xSrx)
(Co1-yFey)O3-δ(LSCF)【H.Y.Tu；Y.Takeda；N.Imanishi；O.Yamamoto/Solid State Ionics,
117,(1999),277–281.】,(Ba1-xSrx)(Co1-yFey)O3-δ(BSCF)【Z.P.Shao；S.M.Haile./Nature,
431,(2004),170-173.】Improved a lot Deng cathode performance compared with LSM, but the ability that poisons of its resistant to carbon dioxide compared with
It is low【A.Y.Yan；M.J.Cheng；Y.L.Dong；W.S.Yang；V.Maragou；S.Q.Song；P.Tsiakaras./
Appl.Catal.B-Environ.66,(2006),64-71.】So that the practical application of these materials receives very big limit
System.Therefore LSM/YSZ cathode systems are still the cathode material for solid-oxide fuel cell for most having application prospect, how to be improved
The chemical property of LSM/YSZ composite cathodes becomes particularly important.
Conventional composite negative electrode is obtained by, by the composite cathode high temperature sintering of mechanical mixture to dielectric film, existing
The problem of uneven is mixed, and material will pass through powder and electrode high temperature sintering (>=1100 DEG C) twice, and particle growth is more tight
Weight, it is more serious than surface and three phase boundary loss, therefore battery performance is relatively low.The present invention proposes that one kind is simple and effective and prepares solid
The method that the nano combined negative electrodes of oxide fuel cell LSM-YSZ improve battery performance and stability, it is therefore an objective to by optimizing electricity
The microstructure of pole improves cathode performance and stability, obtained nano combined negative electrode have simultaneously LSM Perovskite Phases and
YSZ fluorite phases, two-phase, which interacts, causes material surface to generate the more Lacking oxygen for being advantageous to oxygen reduction reaction；And the party
Method sintering temperature wants low more, 30~70nm of particle size compared to traditional LSM/YSZ negative electrodes, is covered in YSZ skeletons surface so that
Oxygen reduction reaction active sites-three phase boundary is not only present between LSM nano particles and YSZ skeletons, is also dispersed throughout LSM-YSZ and is received
Between rice composite particles, oxygen reduction reaction is dramatically speeded up, battery performance is 2~3 times of conventional cathode；And metal ion is in original
The uniform mixing for reaching atomic level in liquid solution is driven, two-phase is in close contact after high temperature is separated, and limitation mutually is grown up, electrode
Stability significantly improves, 800 DEG C, 0.92A/cm2Constant-current discharge, 500h are undamped.
The content of the invention
The present invention proposes that a kind of high temperature phase separation prepares the side of the nano combined negative electrodes of SOFC LSM-YSZ
Method.
The method that a kind of described high temperature phase separation prepares the nano combined negative electrodes of SOFC LSM-YSZ,
Specifically include following steps,
1) YSZ skeletons are prepared：By YSZ materials and n-butanol, polyvinyl butyral resin (PVB), fish oil, pore creating material and bonding
After agent ultrasonic mixing is uniform, the dielectric film surface coated in anode electrolysis plasma membrane two-in-one component, high temperature sintering obtains porous
YSZ skeletons；
The dosage of pore creating material is pore creating material：YSZ=1:4~1:1 (mass ratio)；
YSZ materials and n-butanol, PVB, fish oil, the dosage of pore creating material and binding agent are (mass ratio), 17.3：40.6:
17.3:0.6:17.3:6.9 or 11.0:51.2:22.0:0.4:11.0:4.4.
2) former drive liquid solution is prepared：La, Sr, Mn, Y, Zr metal in LSM-YSZ composite cathodes are weighed according to stoichiometric proportion
The nitrate of ion, is dissolved in deionized water, and complexing agent is added after being completely dissolved, and regulation system Ph=1-3 makes its clarification, 70-
After 80 DEG C of 2~3h of heating complexing, volumetric flask constant volume is used；
3) in the YSZ skeletons for preparing the former drive liquid solution vacuum impregnation configured in step 2) into step 1), then
1-3 hours are sintered at 400~600 DEG C, reduces nitrate and removes the organic matter in maceration extract；
4) repeat step 3) 2-10 times after the pickup for reaching required, finally sinter 1 at 800~1000 DEG C~
2h, obtain adhering to answering for nanometer LSM-YSZ particles on YSZ skeletons in the dielectric film surface of anode electrolysis plasma membrane two-in-one component
Close negative electrode.
In the step 1), pore creating material used is graphite, polystyrene (PS), polymethylacrylic acid when preparing YSZ skeletons
One or two or more kinds of mixtures in methyl esters (PMMA)；Binding agent be 6% (mass ratio) ethyl cellulose solution, solvent
For terpinol；Porous YSZ skeletons thickness about 10-50 microns.
In the step 1), the preferable amount of pore creating material is pore creating material：YSZ=1:1 (mass ratio).
In the step 1), high temperature sintering is fired for temperature programming, when YSZ skeletons are fired in temperature programming,
Be 0.5-1 DEG C/min from room temperature to 400 DEG C of heating rate, the heating rate from 400 DEG C to 800 DEG C be 2-5 DEG C/
Min, it is 1-2 DEG C/min from 800 DEG C to the heating rate of sintering temperature；The sintering temperature of YSZ skeletons is 1100~1300 DEG C, excellent
Select 1180 DEG C；Sintering time 1-4 hours.
In the step 2), LSM in the nano combined negative electrodes of LSM-YSZ:YSZ=30:70~70:30 (mass ratioes), preferably
LSM:YSZ=45:55~60:40 (mass ratioes), wherein LSM formula are (La1-xSrx)1-yMnO3, x=0.1~0.3, y=0
~0.15；
Wherein YSZ composition is (Y2O3)0.08(ZrO2)0.92Or (Y2O3)0.03(ZrO2)0.97。
In the step 2), the total concentration that original drives metal ion in body is 1.5~3mol/L, preferably 2mol/L.
In the step 2), the complexing agent that uses is citric acid, ammonium citrate, glycine or urea, optimization citric acid and
Ammonium citrate；The mol ratio of complexing agent and metal ion sum in composite cathode material is 0.5:1~1:2, preferably 1:1.
In the step 4), final solid impregnating Liang≤50~70wt% of nanometer LSM-YSZ particles in composite cathode；
In the step 4), preferably sintering temperature is 950 DEG C.
In the step 4), LSM and YSZ particle sizes are in 20~70nm in prepared nano combined negative electrode.
The dielectric film that anode electrolysis plasma membrane two-in-one component is adhered to by anode and one side surface forms；
Anode material is NiO:YSZ=40:60~60:40 (mass ratioes).
Beneficial effects of the present invention：
The method that the present invention is separated using high temperature prepares the nano combined negative electrodes of SOFC LSM-YSZ,
LSM electronic conductors and YSZ ion conductors are introduced into cathode construction simultaneously, the interphase interaction of two-phase, formed in material surface
More Lacking oxygens for being advantageous to oxygen reduction reaction；LSM electronic conductors and YSZ ion conductors particle size are 30~70nm, are covered
Be placed on YSZ skeletons surface, active sites-three phase boundary of oxygen reduction reaction be not only present in LSM nano particles and YSZ skeletons it
Between, also it is dispersed throughout between LSM-YSZ Nano composite granules, has dramatically speeded up oxygen reduction reaction, improves battery performance to traditional the moon
2~3 times of pole；Metal ion reaches the uniform mixing of atomic level in former drive liquid solution, and two-phase is close after high temperature is separated
Contact, mutually limitation are grown up, and the stability of electrode significantly improves, 800 DEG C, 0.92A/cm2Constant-current discharge, 500h are undamped.
Brief description of the drawings
Fig. 1 is the electromicroscopic photograph of the YSZ skeletons prepared on anode electrolysis plasma membrane two-in-one component.
Fig. 2 is using the ammonium citrate nanometer (La isolated as complexing agent high-temperature-phase0.8Sr0.2)0.9MnO3+d
(LSM)/(Y2O3)0.08(ZrO2)0.92(YSZ)=60:Powder after 950 DEG C of roastings of composite cathode material of 40 (mass ratioes)
XRD spectrum.
Fig. 3 is that high temperature phase separation prepares (La0.8Sr0.2)0.9MnO3±d/ YSZ=60:40wt% nanometer combined electrodes are swept
Retouch electromicroscopic photograph.
Fig. 4 is impregnated cathode battery and conventional cathode battery, the comparison of impedance at 800 DEG C.
Specific embodiment
Embodiment 1 prepares YSZ skeletons
Using NiO:YSZ=45:55 compound is anode substrate, (Y2O3)0.08(ZrO2)0.92For the sun of dielectric film
Pole dielectric film two-in-one component, YSZ skeletons are prepared on its dielectric film, YSZ composition is (Y2O3)0.08(ZrO2)0.92。
YSZ materials and n-butanol, PVB, fish oil, pore creating material【Flake graphite：PMMA=50:50% (mass ratio)】With the dosage of binding agent
For (mass ratio), 17.3：40.6:17.3:0.6:17.3:6.9, by said mixture ultrasonic mixing it is uniform after, coated on anode
The dielectric film side of dielectric film two-in-one component, is placed in high temperature furnace Program heating sintering, and temperature programming system is as follows：Rise
Warm 1 DEG C/min of speed rises to 280 DEG C from room temperature, is incubated 30min；280 DEG C are warming up to from 280 DEG C of heating rates with 1 DEG C/min,
It is incubated 60min；800 DEG C are warming up to from 400 DEG C of heating rates with 2 DEG C/min, is incubated 120min；From 800 DEG C with 2 DEG C/min's
Heating rate is warming up to 1180 DEG C, is incubated furnace cooling after 120min.Obtained anodolyte is observed from ESEM
The thickness of YSZ skeletons is about 30 microns on film two-in-one component, as shown in Figure 1.
(the La of embodiment 20.8Sr0.2)0.9MnO3+d(LSM)/(Y2O3)0.08(ZrO2)0.92(YSZ)=60:40wt% is former to drive body
The preparation of solution
Prepare LSM/YSZ=60:40wt% maceration extract 50ml：Wherein concentration of metal ions is 2.0molL-1, weigh
10.0401g La(NO3)3·6H2O (analysis is pure), 1.2328g Sr (NO3)2(analysis is pure), 11.5244g Mn (NO3)2(analysis
Pure 50wt% solution), 14.1418g Zr (NO3)4·5H2O (analysis is pure), 2.1941g Y (NO3)3·6H2O (analysis is pure), it is complete
Fully dissolved is in 20ml deionized waters, then according to ammonium citrate：Metal ion total mole number=1:The ratio of 1 (mol ratio) adds
Enter 18.5178g ammonium citrates (analysis pure), and the pH value of mixed liquor is reconciled as 1.5 until solution is clarified with nitric acid, be heated to 80
DEG C complexing 3h after use 50ml volumetric flask constant volumes.Partial immersion liquid is taken, is calcined using 950 DEG C with impregnated electrode identical sintering procedure
XRD signs are carried out after 1 hour, as shown in Figure 2.
The high temperature of the embodiment 3 phase separation nano combined cathode cells of LSM-YSZ processed
By the maceration extract vacuum impregnation in embodiment 2 into the YSZ skeletons in embodiment 1, every time in 600 DEG C of roastings after dipping
Burning reduces nitrate and removed organic matter, and after 8 dippings reach required pickup, 950 DEG C of roastings obtain nano combined electricity in 1 hour
Pole.Its electromicroscopic photograph is as shown in Figure 3, it can be seen that：LSM and YSZ particle sizes are in 20~70nm in nano combined negative electrode.To receiving
Rice composite cathode battery carries out electrochemical property test, and the battery of negative electrode is mixed with tradition machinery【V.A.C.Haanappel
et al./Journal of Power Sources141(2005)216–226】It is compared.In anode-side, the hydrogen of humidification
As fuel (volumetric concentration 3%H2O,100ml min-1), in cathode side, oxygen is as oxidant (100ml min-1).High temperature
Power density of the nano combined cathode cells of phase separation LSM-YSZ under 800 DEG C, 0.7V reaches 2.36Wcm-2It is significantly larger than mechanical
Mix the 1.08Wcm of cathode cell-2.Its impedance spectra (Fig. 4), which also indicates that, represents hydrogen reduction process in nano combined cathode cell
Intermediate frequency arc (125Hz) be significantly less than tradition machinery mixing cathode cell, and hydrogen reduction process occurs mainly in three phase boundary
Place, the phenomenon also indicate that the three phase boundary of nano combined negative electrode considerably increases.The two outer surface analysis to two kinds of negative electrodes obtain
Arrive, the specific surface area of nano combined negative electrode is 3.4m2/ g, it is far longer than the 0.78m of tradition machinery mixing negative electrode2/ g, this also illustrates
The three phase boundary of nanometer combined electrode will be far longer than mechanical mixture negative electrode, have higher oxygen reduction activity, battery performance
It is higher.
The present invention provides a kind of high temperature phase separation and prepares SOFC (LaSr) MnO3-(Y2O3)0.08
(ZrO2)0.92(LSM-YSZ) method that nano combined negative electrode improves battery performance and stability.(1) LSM electronic conductors and YSZ from
The method that sub- conductor is separated by high temperature is introduced into cell cathode simultaneously, the interphase interaction of two-phase, is formed in material surface
More Lacking oxygens for being advantageous to oxygen reduction reaction；(2) LSM electronic conductors and YSZ ion conductors particle size are 30~70nm,
Be covered in YSZ skeletons surface, active sites-three phase boundary of oxygen reduction reaction be not only present in LSM nano particles and YSZ skeletons it
Between, also it is dispersed throughout between LSM-YSZ nano particles, dramatically speeds up oxygen reduction reaction, battery performance improved to the 2 of conventional cathode~
3 times；(3) the former body that drives used in this method is metal ion and the mixed liquor after complexing agent complexing, and each metal ion species reach
The uniform mixing of atomic level, two-phase is in close contact after high temperature is separated, and limitation mutually is grown up, and the stability of electrode significantly carries
Height, 800 DEG C, 0.92A/cm2Constant-current discharge, 500h are undamped.The present invention soild oxide that this is classical to LSM-YSZ combustion
Material battery composite cathode is improved in microstructure, prepares the LSM-YSZ composite cathodes of nanostructured, its Lacking oxygen
Greatly increased with three phase boundary number, the performance and stability of SOFC can be significantly improved, to solid oxidation
The development and application of thing fuel are significant.
Claims (14)
- A kind of method for preparing LSM-YSZ nanometer combined electrodes 1. high temperature is separated, specifically includes following steps：1）Prepare YSZ skeletons：By YSZ materials and n-butanol, polyvinyl butyral resin（PVB）, fish oil, pore creating material and binding agent surpass After sound is well mixed, the dielectric film surface coated in anode electrolysis plasma membrane two-in-one component, high temperature sintering obtains porous YSZ Skeleton；The sintering temperature of YSZ skeletons is 1100 ~ 1300oC；The dosage of pore creating material is pore creating material：YSZ mass ratio=1:4 ~ 1:1；The quality ratio dosage of YSZ materials and n-butanol, PVB, fish oil, pore creating material and binding agent is 17.3:40.6:17.3:0.6: 17.3:6.9 or 11.0:51.2:22.0:0.4:11.0:4.4；2）Prepare former drive liquid solution：La, Sr, Mn, Y, Zr metal ion in LSM-YSZ composite cathodes are weighed according to stoichiometric proportion Nitrate, be dissolved in deionized water, complexing agent added after being completely dissolved, regulation system Ph=1-3 makes its clarification, 70-80oC adds After 2 ~ 3h of heat complexing, volumetric flask constant volume is used；3）By step 2）Middle configured original drives liquid solution vacuum impregnation to step 1）In the YSZ skeletons of middle preparation, Ran Hou 400~600oC sinters 1-3 hours, reduces nitrate and removes the organic matter in maceration extract；4）Repeat step 3）2-10 times after the pickup for reaching required, finally 800 ~ 1000oC sinters 1 ~ 2h, in anode The dielectric film surface of dielectric film two-in-one component obtains the composite cathode for adhering to nanometer LSM-YSZ particles on YSZ skeletons.
- 2. according to the method for claim 1, it is characterised in that：The step 1）In, pore creating material used when preparing YSZ skeletons For graphite, polystyrene（PS）, polymethyl methacrylate（PMMA）In one or two or more kinds of mixtures；Binding agent is The ethyl cellulose solution of mass ratio 6%, solvent are terpinol；Porous YSZ skeletons thickness is 10-50 microns.
- 3. according to the method for claim 1, it is characterised in that：The step 1）In, the dosage of pore creating material is pore creating material：YSZ mass ratio=1:1.
- 4. according to the method for claim 1, it is characterised in that：The step 1）In, high temperature sintering is that temperature programming is fired, when YSZ skeletons are fired in temperature programming, from room temperature to 400oC's Heating rate is 0.5-1oC/min, from 400oC to 800oC heating rate is 2-5oC/min, from 800oLiters of the C to sintering temperature Warm speed is 1-2oC/min；Sintering time 1-4 hours.
- 5. according to the method for claim 1, it is characterised in that：The step 2）In, LSM in the nano combined negative electrodes of LSM-YSZ:YSZ mass ratio=30:70 ~70:30, wherein LSM Formula be (La1-xSrx)1-yMnO3, x=0.1 ~ 0.3, y=0 ~ 0.15；Wherein YSZ composition is (Y2O3)0.08(ZrO2)0.92Or (Y2O3)0.03(ZrO2)0.97。
- 6. according to the method for claim 5, it is characterised in that：LSM:YSZ mass ratio=45:55 ~60:40.
- 7. according to the method for claim 1, it is characterised in that：The step 2）In, the total concentration that original drives metal ion in body is 1.5 ~ 3 mol/L；The step 2）In, the complexing agent that uses is citric acid, ammonium citrate, glycine or urea, complexing agent and composite cathode The mol ratio of metal ion sum is 0.5 in material:1~1:2.
- 8. according to the method for claim 7, it is characterised in that：The step 2）In, the total concentration that original drives metal ion in body is 2mol/L；The step 2）In, the mol ratio of complexing agent and metal ion sum in composite cathode material is 1:1.
- 9. according to the method for claim 1, it is characterised in that：The step 2）In, the complexing agent used is citric acid and ammonium citrate.
- 10. according to the method for claim 1, it is characterised in that：The step 4）In, the wt % of final solid impregnating Liang≤50 of nanometer LSM-YSZ particles in composite cathode ~ 70.
- 11. according to the method for claim 1, it is characterised in that：The step 4）In, sintering temperature 1180oC。
- 12. according to the method for claim 1, it is characterised in that：The step 4）In, sintering temperature 950oC。
- 13. according to the method for claim 1, it is characterised in that：The step 4）In, LSM and YSZ particle sizes are in 20 ~ 70nm in prepared nano combined negative electrode.
- 14. according to the method for claim 1, it is characterised in that：The dielectric film that anode electrolysis plasma membrane two-in-one component is adhered to by anode and one side surface forms；Anode material is NiO:YSZ mass ratio=40:60 ~ 60:40.
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| CN101083324A (en) * | 2007-06-22 | 2007-12-05 | 中国科学技术大学 | Solid-oxide fuel battery complex cathode and method for making same |
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