CN105261765A - Method for preparing LSM-YSZ nanocomposite electrode through high temperature phase separation - Google Patents
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Abstract
A method for preparing an LSM-YSZ nanocomposite electrode through high temperature phase separation is disclosed. The invention provides a method for preparing a solid oxide fuel battery nanocomposite negative electrode, for improving performance and stability of batteries, through the high temperature phase separation. The method comprises the steps of (1) an LSM electronic conductor and a YSZ ionic conductor are introduced into a battery negative electrode at the same time through a high temperature phase separation method, and the two phases of the LSM and the YSZ are reacting with each other to form more oxygen vacancies favorable for an oxygen reduction reaction on the surface of the material; (2) the YSZ framework is covered by the LSM and the YSZ, wherein the activity site-three-phase interface of the oxygen reduction reaction not only exists between the LSM nanoparticles and the YSZ framework, but also full exists among the LSM-YSZ nanoparticles, so that the oxygen reduction reaction is accelerated dramatically, and the battery performance is improved to 2-3 times of that of the conventional negative electrode; and (3), the precursor adopted by the method is a mixed solution by complexing metal ions with a complexing agent, the metal ions are uniformly mixed at the atomic level, and then through the high temperature phase separation, the two phases of the LSM and the YSZ are tightly contacted and the growth of the two phases are limited by each other, so that the stability of the electrode is greatly improved; and when the constant-current discharge is performed at the 0.92A/cm2 at the temperature of 800 DEG C for 500 hours, the performance of the electrode is not degraded.
Description
Technical field
The present invention relates to compound cathode of solid oxide fuel battery, specifically a kind of high-temperature-phase is separated the method preparing the nano combined negative electrode of Solid Oxide Fuel Cell LSM-YSZ.
Background technology
Solid Oxide Fuel Cell is a kind of energy conversion device chemical energy in fuel being converted into electric energy, may be used for compact power, cogeneration and large power generating equipment, its efficiency is high, pollution-free, and fuel range of choice is wide, hydrogen, methane, the hydrocarbons such as biogas can be used as the fuel of Solid Oxide Fuel Cell, have a extensive future, thus become the focus of numerous scholar's research.Solid Oxide Fuel Cell membrane electrode comprises anode, electrolyte and negative electrode three part, and the most classical corresponding electrode material is NiO/YSZ composite anode respectively, YSZ electrolyte and LSM/YSZ mechanical mixture negative electrode.Support YSZ hull cell for present pandemic NiO/YSZ composite anode, the polarization loss that LSM/YSZ mechanical mixture negative electrode produces is the principal element of restriction battery performance.At negative electrode, main what occur is the electrochemical reducting reaction of oxygen, and the oxygen comprised in gas phase is diffused into cathode surface by mesopore, adsorbs thereon, dissociates, and accepts electronics and change into oxonium ion and enter several processes such as electrolyte lattice.And said process is except gas diffusion, all need very high reaction activity, the slow [M.J. of reaction rate
andM.Mogensen/JournalofTheElectrochemicalSociety, 148 (5), (2001), A433-A442; X.J.Chenetal./JournalofPowerSources, 123, (2003), 17 – 25], the polarization loss of generation is high, thus becomes the principal element of restriction solid-oxide fuel battery performance.Therefore research preparation high-performance and cathode material steady in a long-term in the urgent need to.(La
1-xsr
x) CoO
3-δ(LSC) [O.Yamamoto; Y.Takeda; R.Kanno; M.Noda./SolidStateIonics, 22, (1987), 241 – 246.], (La
1-xsr
x) (Co
1-yfe
y) O
3-δ(LSCF) [H.Y.Tu; Y.Takeda; N.Imanishi; O.Yamamoto/SolidStateIonics, 117, (1999), 277 – 281.], (Ba
1-xsr
x) (Co
1-yfe
y) O
3-δ(BSCF) [Z.P.Shao; S.M.Haile./Nature, 431, (2004), 170-173.] etc. cathode performance comparatively LSM improve a lot, but the lower [A.Y.Yan of the ability that its resistant to carbon dioxide poisons; M.J.Cheng; Y.L.Dong; W.S.Yang; V.Maragou; S.Q.Song; P.Tsiakaras./Appl.Catal.B-Environ.66, (2006), 64-71.], the practical application of these materials is limited by very large.Therefore LSM/YSZ cathode systems remains the cathode material for solid-oxide fuel cell having application prospect most, and the chemical property how improving LSM/YSZ composite cathode becomes particularly important.
The acquisition of conventional composite negative electrode be by by the composite cathode high temperature sintering of mechanical mixture on dielectric film, there is the problem that mixing is uneven, and material will through powder and electrode twice high temperature sintering (>=1100 DEG C), particle growth is comparatively serious, seriously, therefore battery performance is on the low side for specific surface and three phase boundary loss.The present invention proposes a kind of simple and effective method preparing the nano combined negative electrode raising battery performance of Solid Oxide Fuel Cell LSM-YSZ and stability, object is that the microstructure by optimizing electrode improves cathode performance and stability, obtained nano combined negative electrode has LSM Perovskite Phase and YSZ fluorite phase simultaneously, and two-phase interacts and makes material surface generate the more Lacking oxygen being conducive to oxygen reduction reaction; And it is low many that the method sintering temperature compares traditional LSM/YSZ negative electrode, particle size 30 ~ 70nm, be covered in YSZ skeleton surface, oxygen reduction reaction active sites-three phase boundary is made not exist only between LSM nano particle and YSZ skeleton, also be dispersed throughout between LSM-YSZ Nano composite granules, remarkable quickening oxygen reduction reaction, battery performance is 2 ~ 3 times of conventional cathode; And metal ion drives in liquid solution former the Homogeneous phase mixing reaching atomic level, two-phase close contact after high-temperature-phase is separated, restriction is grown up mutually, and the stability of electrode significantly improves, 800 DEG C, 0.92A/cm
2constant-current discharge, 500h is undamped.
Summary of the invention
The present invention proposes a kind of high-temperature-phase and is separated the method preparing the nano combined negative electrode of Solid Oxide Fuel Cell LSM-YSZ.
Described a kind of high-temperature-phase is separated the method preparing the nano combined negative electrode of Solid Oxide Fuel Cell LSM-YSZ, specifically comprises the following steps,
1) prepare YSZ skeleton: by YSZ material and n-butanol, polyvinyl butyral resin (PVB), fish oil, pore creating material and binding agent is ultrasonic mix after, be coated in the dielectric film surface of anode electrolysis plasma membrane two-in-one component, high temperature sintering obtains the YSZ skeleton of porous;
The consumption of pore creating material is, pore creating material: YSZ=1:4 ~ 1:1 (mass ratio);
The consumption of YSZ material and n-butanol, PVB, fish oil, pore creating material and binding agent is (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) prepare and formerly drive liquid solution: the nitrate taking La, Sr, Mn, Y, Zr metal ion in LSM-YSZ composite cathode according to stoichiometric proportion, be dissolved in deionized water, complexing agent is added after dissolving completely, regulation system Ph=1-3 makes it clarify, after 70-80 DEG C of heating complexing 2 ~ 3h, use volumetric flask constant volume;
3) by step 2) in configure formerly drive liquid solution vacuum impregnation to step 1) in preparation YSZ skeleton in, then at 400 ~ 600 DEG C of sintering 1-3 hour, reduce nitrate and remove the organic substance in maceration extract;
4) step 3 is repeated) 2-10 time until after reaching required pickup, finally at 800 ~ 1000 DEG C of sintering 1 ~ 2h, obtain in the dielectric film surface of anode electrolysis plasma membrane two-in-one component composite cathode YSZ skeleton adhering to nanometer LSM-YSZ particle.
Described step 1) in, during preparation YSZ skeleton, pore creating material used is the mixture of one or two or more kinds in graphite, polystyrene (PS), polymethyl methacrylate (PMMA); Binding agent is the ethyl cellulose solution of 6% (mass ratio), and solvent is terpinol; The YSZ skeleton thickness of porous is about 10-50 micron.
Described step 1) in, the preferable amount of pore creating material is, pore creating material: YSZ=1:1 (mass ratio).
Described step 1) in, high temperature sintering is that temperature programming is fired, when YSZ skeleton is fired in temperature programming,
Being 0.5-1 DEG C/min from the heating rate of room temperature to 400 DEG C, is 2-5 DEG C/min from the heating rates of 400 DEG C to 800 DEG C, from 800 DEG C to the heating rate of sintering temperature be 1-2 DEG C/min; The sintering temperature of YSZ skeleton is 1100 ~ 1300 DEG C, preferably 1180 DEG C; Sintering time 1-4 hour.
Described step 2) in, LSM:YSZ=30:70 ~ 70:30 (mass ratio), preferred LSM:YSZ=45:55 ~ 60:40 (mass ratio) in the nano combined negative electrode of LSM-YSZ, wherein the general formula of LSM is (La
1-xsr
x)
1-ymnO
3, x=0.1 ~ 0.3, y=0 ~ 0.15;
Wherein YSZ consist of (Y
2o
3)
0.08(ZrO2)
0.92or (Y
2o
3)
0.03(ZrO2)
0.97.
Described step 2) in, former total concentration of driving metal ion in body is 1.5 ~ 3mol/L, preferred 2mol/L.
Described step 2) in, the complexing agent of use is citric acid, ammonium citrate, glycine or urea, optimization citric acid and ammonium citrate; In complexing agent and composite cathode material, the mol ratio of metal ion sum is 0.5:1 ~ 1:2, preferred 1:1.
Described step 4) in, the final solid impregnating Liang≤50 ~ 70wt% of nanometer LSM-YSZ particle in composite cathode;
Described step 4) in, preferred sintering temperature is 950 DEG C.
Described step 4) in, in prepared nano combined negative electrode, LSM and YSZ particle size is at 20 ~ 70nm.
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 ratio).
Beneficial effect of the present invention:
The method that the present invention adopts high-temperature-phase to be separated prepares the nano combined negative electrode of Solid Oxide Fuel Cell LSM-YSZ, LSM electronic conductor and YSZ ion conductor are introduced in cathode construction simultaneously, the interphase interaction of two-phase, defines the Lacking oxygen being conducive to oxygen reduction reaction at material surface more; LSM electronic conductor and YSZ ion conductor particle size are 30 ~ 70nm, be covered in YSZ skeleton surface, active sites-the three phase boundary of oxygen reduction reaction does not exist only between LSM nano particle and YSZ skeleton, also be dispersed throughout between LSM-YSZ Nano composite granules, significantly accelerate oxygen reduction reaction, raising battery performance is to 2 ~ 3 times of conventional cathode; Metal ion drives in liquid solution former the Homogeneous phase mixing reaching atomic level, two-phase close contact after high-temperature-phase is separated, and restriction is grown up mutually, and the stability of electrode significantly improves, 800 DEG C, 0.92A/cm
2constant-current discharge, 500h is undamped.
Accompanying drawing explanation
Fig. 1 is the electromicroscopic photograph of the YSZ skeleton prepared on anode electrolysis plasma membrane two-in-one component.
Fig. 2 adopts ammonium citrate to be separated the nanometer (La obtained as complexing agent high-temperature-phase
0.8sr
0.2)
0.9mnO
3+d(LSM)/(Y
2o
3)
0.08(ZrO
2)
0.92(YSZ) the XRD collection of illustrative plates of powder after composite cathode material 950 DEG C of roastings of=60:40 (mass ratio).
Fig. 3 is that high-temperature-phase is separated preparation (La
0.8sr
0.2)
0.9mnO
3 ± dthe stereoscan photograph of/YSZ=60:40wt% nanometer combined electrode.
Fig. 4 is impregnated cathode battery and conventional cathode battery, the comparison of impedance at 800 DEG C.
Specific embodiment
Embodiment 1 prepares YSZ skeleton
The compound adopting NiO:YSZ=45:55 is anode substrate, (Y
2o
3)
0.08(ZrO2)
0.92for the anode electrolysis plasma membrane two-in-one component of dielectric film, its dielectric film is prepared YSZ skeleton, and YSZ consists of (Y
2o
3)
0.08(ZrO2)
0.92.The consumption of YSZ material and n-butanol, PVB, fish oil, pore creating material [flake graphite: PMMA=50:50% (mass ratio)] and binding agent is (mass ratio), 17.3:40.6:17.3:0.6:17.3:6.9, after ultrasonic for said mixture mixing, be coated on the dielectric film side of anode electrolysis plasma membrane two-in-one component, be placed in high temperature furnace Program intensification sintering, temperature programming system is as follows: heating rate 1 DEG C/min rises to 280 DEG C from room temperature, insulation 30min; 280 DEG C are warming up to the heating rate of 1 DEG C/min, insulation 60min from 280 DEG C; 800 DEG C are warming up to the heating rate of 2 DEG C/min, insulation 120min from 400 DEG C; Be warming up to 1180 DEG C from 800 DEG C with the heating rate of 2 DEG C/min, cool with stove after insulation 120min.The thickness observing YSZ skeleton on the anode electrolysis plasma membrane two-in-one component that obtains from ESEM is about 30 microns, as shown in Figure 1.
Embodiment 2 (La
0.8sr
0.2)
0.9mnO
3+d(LSM)/(Y
2o
3)
0.08(ZrO
2)
0.92(YSZ) the former preparation of driving liquid solution of=60:40wt%
The maceration extract 50ml of preparation LSM/YSZ=60:40wt%: wherein concentration of metal ions is 2.0molL
-1, take 10.0401gLa (NO
3)
36H
2o (analyzing pure), 1.2328gSr (NO
3)
2(analyzing pure), 11.5244gMn (NO
3)
2(analyzing pure 50wt% solution), 14.1418gZr (NO
3)
45H
2o (analyzing pure), 2.1941gY (NO
3)
36H
2o (analyzing pure), be dissolved in 20ml deionized water completely, then according to ammonium citrate: the ratio of metal ion total mole number=1:1 (mol ratio) adds 18.5178g ammonium citrate (analyzing pure), and to reconcile the pH value of mixed liquor with nitric acid be 1.5 until solution clarification, be heated to after 80 DEG C of complexing 3h with 50ml volumetric flask constant volume.Get partial immersion liquid, adopt the sintering procedure identical with impregnated electrode 950 DEG C of roastings to carry out XRD sign after 1 hour, as shown in Figure 2.
Embodiment 3 high-temperature-phase is separated the nano combined cathode cell of LSM-YSZ processed
By the maceration extract vacuum impregnation in embodiment 2 in the YSZ skeleton in embodiment 1, at 600 DEG C of Roasting Decomposition nitrate and removing organic substance after each dipping, after 8 times dipping reaches required pickup, 950 DEG C of roastings obtain nanometer combined electrode in 1 hour.Its electromicroscopic photograph as shown in Figure 3, can be found out: in nano combined negative electrode, LSM and YSZ particle size is at 20 ~ 70nm.Electrochemical property test is carried out to nano combined cathode cell, and compares with the battery [V.A.C.Haanappeletal./JournalofPowerSources141 (2005) 216 – 226] of traditional mechanical mixture negative electrode.In anode-side, the hydrogen of humidification is as fuel (volumetric concentration 3%H
2o, 100mlmin
-1), at cathode side, oxygen is as oxidant (100mlmin
-1).High-temperature-phase is separated the nano combined cathode cell of LSM-YSZ processed at 800 DEG C, and the power density under 0.7V reaches 2.36Wcm
-2far away higher than the 1.08Wcm of mechanical mixture cathode cell
-2.The intermediate frequency arc (125Hz) that its impedance spectrogram (Fig. 4) also shows to represent in nano combined cathode cell hydrogen reduction process is significantly less than traditional mechanical mixture cathode cell, and hydrogen reduction process mainly occurs in three phase boundary place, this phenomenon also shows that the three phase boundary of nano combined negative electrode considerably increases.Obtain the surface analysis of two kinds of negative electrodes outside two, the specific area of nano combined negative electrode is 3.4m
2/ g, is far longer than the 0.78m of traditional mechanical mixture negative electrode
2/ g, this also illustrates that the three phase boundary of nanometer combined electrode will be far longer than mechanical mixture negative electrode, and have higher oxygen reduction activity, battery performance is higher.
The invention provides a kind of high-temperature-phase and be separated preparation Solid Oxide Fuel Cell (LaSr) MnO
3-(Y
2o
3)
0.08(ZrO
2)
0.92(LSM-YSZ) nano combined negative electrode improves the method for battery performance and stability.(1) method that LSM electronic conductor and YSZ ion conductor are separated by high-temperature-phase is introduced in cell cathode simultaneously, and the interphase interaction of two-phase, defines the Lacking oxygen being conducive to oxygen reduction reaction at material surface more; (2) LSM electronic conductor and YSZ ion conductor particle size are 30 ~ 70nm, be covered in YSZ skeleton surface, active sites-the three phase boundary of oxygen reduction reaction does not exist only between LSM nano particle and YSZ skeleton, also be dispersed throughout between LSM-YSZ nano particle, remarkable quickening oxygen reduction reaction, battery performance is increased to 2 ~ 3 times of conventional cathode; (3) used former of the method drives body is mixed liquor after metal ion and complexing agent complexes, and each metal ion species reaches the Homogeneous phase mixing of atomic level, two-phase close contact after high-temperature-phase is separated, mutual restriction is grown up, the stability of electrode significantly improves, 800 DEG C, 0.92A/cm
2constant-current discharge, 500h is undamped.The compound cathode of solid oxide fuel battery of the present invention to these classics of LSM-YSZ improves in microstructure, prepare the LSM-YSZ composite cathode of nanostructure, its Lacking oxygen and three phase boundary number increase greatly, performance and the stability of Solid Oxide Fuel Cell can be significantly improved, the development of solid oxide fuel and application are significant.
Claims (10)
1. high-temperature-phase is separated the method preparing LSM-YSZ nanometer combined electrode, specifically comprises the following steps:
1) prepare YSZ skeleton: by YSZ material and n-butanol, polyvinyl butyral resin (PVB), fish oil, pore creating material and binding agent is ultrasonic mix after, be coated in the dielectric film surface of anode electrolysis plasma membrane two-in-one component, high temperature sintering obtains the YSZ skeleton of porous;
The consumption of pore creating material is, pore creating material: YSZ=1:4 ~ 1:1 (mass ratio);
The consumption of YSZ material and n-butanol, PVB, fish oil, pore creating material and binding agent is (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) prepare and formerly drive liquid solution: the nitrate taking La, Sr, Mn, Y, Zr metal ion in LSM-YSZ composite cathode according to stoichiometric proportion, be dissolved in deionized water, complexing agent is added after dissolving completely, regulation system Ph=1-3 makes it clarify, after 70-80 DEG C of heating complexing 2 ~ 3h, use volumetric flask constant volume;
3) by step 2) in configure formerly drive liquid solution vacuum impregnation to step 1) in preparation YSZ skeleton in, then at 400 ~ 600 DEG C of sintering 1-3 hour, reduce nitrate and remove the organic substance in maceration extract;
4) step 3 is repeated) 2-10 time until after reaching required pickup, finally at 800 ~ 1000 DEG C of sintering 1 ~ 2h, obtain in the dielectric film surface of anode electrolysis plasma membrane two-in-one component composite cathode YSZ skeleton adhering to nanometer LSM-YSZ particle.
2. method according to claim 1, it is characterized in that: described step 1) in, during preparation YSZ skeleton, pore creating material used is the mixture of one or two or more kinds in graphite, polystyrene (PS), polymethyl methacrylate (PMMA); Binding agent is the ethyl cellulose solution of 6% (mass ratio), and solvent is terpinol; The YSZ skeleton thickness of porous is about 10-50 micron.
3. method according to claim 1, is characterized in that:
Described step 1) in, the preferable amount of pore creating material is, pore creating material: YSZ=1:1 (mass ratio).
4. method according to claim 1, is characterized in that:
Described step 1) in, high temperature sintering is that temperature programming is fired, and when YSZ skeleton is fired in temperature programming, is 0.5-1 DEG C/min from the heating rate of room temperature to 400 DEG C, be 2-5 DEG C/min from the heating rates of 400 DEG C to 800 DEG C, from 800 DEG C to the heating rate of sintering temperature be 1-2 DEG C/min; The sintering temperature of YSZ skeleton is 1100 ~ 1300 DEG C, preferably 1180 DEG C; Sintering time 1-4 hour.
5. method according to claim 1, is characterized in that:
Described step 2) in, LSM:YSZ=30:70 ~ 70:30 (mass ratio), preferred LSM:YSZ=45:55 ~ 60:40 (mass ratio) in the nano combined negative electrode of LSM-YSZ, wherein the general formula of LSM is (La
1-xsr
x)
1-ymnO
3, x=0.1 ~ 0.3, y=0 ~ 0.15;
Wherein YSZ consist of (Y
2o
3)
0.08(ZrO2)
0.92or (Y
2o
3)
0.03(ZrO2)
0.97.
6. method according to claim 1, is characterized in that:
Described step 2) in, former total concentration of driving metal ion in body is 1.5 ~ 3mol/L, preferred 2mol/L;
Described step 2) in, the complexing agent of use is citric acid, ammonium citrate, glycine or urea, optimization citric acid and ammonium citrate; In complexing agent and composite cathode material, the mol ratio of metal ion sum is 0.5:1 ~ 1:2, preferred 1:1.
7. method according to claim 1, is characterized in that:
Described step 4) in, the final solid impregnating Liang≤50 ~ 70wt% of nanometer LSM-YSZ particle in composite cathode.
8. method according to claim 1, is characterized in that:
Described step 4) in, preferred sintering temperature is 950 DEG C.
9. method according to claim 1, is characterized in that:
Described step 4) in, in prepared nano combined negative electrode, LSM and YSZ particle size is at 20 ~ 70nm.
10. method according to claim 1, is characterized 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=40:60 ~ 60:40 (mass ratio).
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| CN114725457A (en) * | 2022-03-29 | 2022-07-08 | 上海交通大学 | Method for preparing membrane electrode for accelerating local oxygen mass transfer |
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