CN107742729A - A kind of preparation method of double-perovskite cathode material - Google Patents
A kind of preparation method of double-perovskite cathode material Download PDFInfo
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- CN107742729A CN107742729A CN201710970652.1A CN201710970652A CN107742729A CN 107742729 A CN107742729 A CN 107742729A CN 201710970652 A CN201710970652 A CN 201710970652A CN 107742729 A CN107742729 A CN 107742729A
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- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
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Abstract
The invention provides a kind of preparation method of double-perovskite cathode material, comprise the following steps：A) respectively by the La of pure phase2O3, NiO and MnCO3It is heat-treated, the raw material after being handled；B) by after the raw material after processing and dispersant grinding, calcined, obtain calcined product；C calcined after) calcined product is ground；D) repeat step C), obtain double-perovskite cathode material.The inventive method passes through to raw material (La2O3、NiO、MnCO3) pre-processed, on the premise of ensureing that its purity will not have an impact to end product quality, 211 type double-perovskite cathode material La have been synthesized using high temperature solid-state method2NiMnO6.The crystalline form for the double-perovskite cathode material that the present invention is prepared is preferable, cathode material as SOFC, carrier transfer rate is high, preferable with the thermally matched properties of electrolyte CGO, improves the performance of the cathode material as SOFC.
Description
Technical field
The invention belongs to solid fuel cell technical field, and in particular to a kind of preparation side of double-perovskite cathode material
Method.
Background technology
A mostly important element during cathode material forms as fuel cell, it should have higher catalytic activity,
Higher electrical conductivity, relatively low thermal coefficient of expansion.Traditional cathode material for solid-oxide fuel cell lanthanum-strontium manganese 800 DEG C~
There is higher stability and relatively low polarization resistance, however as the reduction of operating temperature, less than 800 under the conditions of 1000 DEG C
Its chemical property is significantly reduced under the conditions of DEG C.After this, people have developed the cathode material with more preferable performance again,
Lanthanum-strontium ferro-cobalt and barium strontium ferro-cobalt, but they have higher thermal coefficient of expansion, and during exploitation and utilization, pin
For cobalt element, its cost is higher, and this is unfavorable for application in practice.
Double perovskite materials have higher total conductivity, can make oxygen reduction reaction betide cathode material body phase with
Three phase boundary, chemical property can be greatly improved, while the diffusion coefficient of double-perovskite and surface exchange coefficient are all higher,
Be advantageous to the absorption, dissociation and diffusion of oxygen.
The processes such as contact, reaction, nucleation, crystal growth are passed through at the solid particle interface of existing high temperature solid-state method synthesis,
By original one or several kinds of generation composite oxides.The material grainses crystal formation that this method obtains is bad, as solid oxidation
The cathode material carrier transfer rate of thing fuel cell is low, poor with electrolyte CGO thermal matchings, and reduction is used as solid oxidation
The performance of the cathode material of thing fuel cell.
The content of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of preparation side of double-perovskite cathode material
Method, the crystalline form for the double-perovskite cathode material that the present invention is prepared is preferable, can improve as SOFC
Cathode material performance.
The invention provides a kind of preparation method of double-perovskite cathode material, comprise the following steps：
A) respectively by the La of pure phase2O3, NiO and MnCO3After being heat-treated, grind, mixed with dispersant
Thing；
B ground after) mixture is calcined；
C) repeat step B), obtain double-perovskite cathode material.
Prime minister of the present invention is by the La of pure phase2O3, NiO and MnCO3It is heat-treated, the raw material after being handled.
In the present invention, the raw material La is determined2O3, NiO and MnCO3Whether be pure phase method be carry out XRD detections.
Then, after detection, the La of pure phase2O3, NiO and MnCO3It is heat-treated, wherein, the La of the pure phase2O3Heat
Processing method is：It is heat-treated 24 hours under conditions of 850 DEG C~950 DEG C.
The NiO of pure phase heat treatment method is：24h is heat-treated under conditions of 140 DEG C~160 DEG C.
The MnCO of the pure phase3Heat treatment method be：24h is heat-treated under conditions of 140 DEG C~160 DEG C.
According to double-perovskite cathode material La2NiMnO6Middle La, Ni and Mn stoichiometric number ratio 2：1：1 will be through overheat at
La after reason2O3, NiO and MnCO3Mixed.That is, described La2O3, NiO and MnCO3Mol ratio be 1:1:1.
Raw material after processing and dispersant are ground, obtain mixture；Wherein, the dispersant is selected from ethanol.Institute
Grinding is stated preferably by the way of high-energy ball milling, the time of the grinding is 40~60min, preferably 45~55min.
Then, ground after the mixture is calcined.
The temperature of the calcining is 1000~1150 DEG C, preferably 1050~1100 DEG C, time of the calcining for 24~
48 hours, preferably by the way of high-energy ball milling, time of the grinding was 40~60min for the grinding, preferably 45~
55min。
After grinding terminates, the step of repeating above-mentioned calcining, grind, the number of the repetition is preferably 2 times.
In the present invention, in the step of repeatedly calcining, grinding, the grinding repeated each time and the condition of calcining can
With it is identical can also be different.Finally, survey XRD and determine that final synthetic is mutually 211 type double-perovskite cathode material La2NiMnO6。
Then the present invention is carried out abundant by being pre-processed to raw material by the way of high-energy ball milling to solid particle
Mixed grinding processing, is then sintered repeatedly at high temperature, and the distance between particle can be less and less, and its density and intensity can be more next
Bigger, crystal structure degree is higher.Also, raw material are heat-treated, impurity and moisture therein can be removed, make synthesis
Sample crystal formation is preferable.
The specimen material better performances synthesized using the preparation method of the present invention, available for SOFC
Generate electricity, value is higher, can provide the heat needed for gas renormalizing, is followed producing steam and combining with gas turbine composition
In terms of ring, it can all be used, it is very useful in distributed power generation.
In addition, the synthetic method is simple, available for the preferable specimen material of Fast back-projection algorithm quality.
Compared with prior art, the invention provides a kind of preparation method of double-perovskite cathode material, including following step
Suddenly：A) respectively by the La of pure phase2O3, NiO and MnCO3It is heat-treated, the raw material after being handled；B) by the raw material after processing
After being ground with dispersant, calcined, obtain calcined product；C calcined after) calcined product is ground；D) weight
Multiple step C), obtain double-perovskite cathode material.The inventive method passes through to raw material (La2O3、NiO、MnCO3) located in advance
Reason, on the premise of ensureing that its purity will not have an impact to end product quality, the double calcium of 211 types are synthesized using high temperature solid-state method
Titanium ore cathode material La2NiMnO6.The particle crystalline form for the double-perovskite cathode material that the present invention is prepared is preferable, as solid
The cathode material of oxide fuel cell, carrier transfer rate is high, preferable with the thermally matched properties of electrolyte CGO, improves conduct
The performance of the cathode material of SOFC.
Brief description of the drawings
Fig. 1 is La2O3XRD spectra；
Fig. 2 is NiO XRD spectra；
Fig. 3 is MnCO3XRD spectra；
Fig. 4 is the XRD spectra of double-perovskite cathode material prepared by embodiment 2；
Fig. 5 is the XRD spectra of double-perovskite cathode material prepared by embodiment 3；
Fig. 6 is the XRD spectra of double-perovskite cathode material prepared by embodiment 4；
Fig. 7 is La2NiMnO6Conductivity data figure；
Fig. 8 is La2NiMnO6Thermodilatometric analysis figure；
Fig. 9 is La2NiMnO6The complex impedance spectrogram measured on CGO electrolyte；
Figure 10 is La2NiMnO6With CGO compatibility data figure.
Embodiment
For a further understanding of the present invention, with reference to embodiment to ultracapacitor provided by the invention with graphene/
The preparation method of manganese dioxide composite electrode material is illustrated, and protection scope of the present invention is not limited by the following examples.
Embodiment 1
Select a little La2O3XRD is surveyed in advance, as a result sees Fig. 1, Fig. 1 La2O3XRD spectra, the results showed that, by Fig. 1's
La2O3XRD spectra material corresponding with JADE5.0 databases XRD contrast, it is pure phase to show the material, be can be used for
Compound experiment.Then it is placed in Muffle furnace, 24 hours is handled under conditions of 900 DEG C, it is wherein a small amount of to remove
Carbonate and moisture.
By NiO and MnCO3Material sample to be measured, tested by XRD and determine that raw material is pure phase, as a result see Fig. 2 and Fig. 3, Fig. 2
For NiO XRD spectra, Fig. 3 MnCO3XRD spectra, the results showed that, by Fig. 2 NiO XRD spectra and Fig. 3 MnCO3
XRD spectra material corresponding with JADE5.0 databases XRD contrast, show that two materials are pure phase, available for closing
Into experiment.Then NiO is placed in 150 DEG C of heat treatment 24h, by MnCO3150 DEG C of heat treatment 24h are placed in, drier is placed in after drying
Middle preservation, it is easy to the use in later stage.
Embodiment 2
According to La, Ni, Mn stoichiometric proportion 2:1:1 ratio weighs the La of respective quality2O3, NiO and MnCO3, it is put into agate
In Nao mortars, add a small amount of absolute ethyl alcohol and grind 40min to 1h as dispersant.After three kinds of solids are thoroughly mixed, room temperature
Under dry, then tabletting machine, sample strip is put into roast 24h in 1000 DEG C of high temperature furnace is placed in crucible.Roast is completed
It is cooled to room temperature afterwards etc. to be drawn off and be ground into powder, surveys XRD and check thing phase.Repeat above step 2 times, second and the
Firing temperature three times is respectively 1050 DEG C, 1100 DEG C, time 24h, 48h.Pulverized after completing roast, survey XRD and determine
The final type double-perovskite cathode material La of synthetic phase 2112NiMnO6, it is double calcium titaniums prepared by embodiment 2 as a result to see Fig. 4, Fig. 4
The XRD spectra of ore deposit cathode material.
Embodiment 3
According to La, Ni, Mn stoichiometric proportion 2:1:1 ratio weighs the La of respective quality2O3, NiO and MnCO3, it is put into agate
In Nao mortars, add a small amount of absolute ethyl alcohol and grind 40min to 1h as dispersant.After three kinds of solids are thoroughly mixed, room temperature
Under dry, then tabletting machine, sample strip is put into roast 24h in 1150 DEG C of high temperature furnace is placed in crucible.Roast is completed
It is cooled to room temperature afterwards etc. to be drawn off and be ground into powder, surveys XRD and check thing phase.Repeat above step 2 times, second and the
Firing temperature three times is respectively 1050 DEG C, 1100 DEG C, time 24h, 48h.Pulverized after completing roast, survey XRD and determine
The final type double-perovskite cathode material La of synthetic phase 2112NiMnO6, it is double calcium titaniums prepared by embodiment 3 as a result to see Fig. 5, Fig. 5
The XRD spectra of ore deposit cathode material.
Embodiment 4
According to La, Ni, Mn stoichiometric proportion 2:1:1 ratio weighs the La of respective quality2O3, NiO and MnCO3, it is put into agate
In Nao mortars, add a small amount of absolute ethyl alcohol and grind 40min to 1h as dispersant.After three kinds of solids are thoroughly mixed, room temperature
Under dry, then tabletting machine, sample strip is put into roast 48h in 1150 DEG C of high temperature furnace is placed in crucible.Roast is completed
It is cooled to room temperature afterwards etc. to be drawn off and be ground into powder, surveys XRD and check thing phase.Repeat above step 2 times, second and the
Firing temperature three times is respectively 1050 DEG C, 1100 DEG C, time 24h, 48h.Pulverized after completing roast, survey XRD and determine
The final type double-perovskite cathode material La of synthetic phase 2112NiMnO6, it is double calcium titaniums prepared by embodiment 4 as a result to see Fig. 6, Fig. 6
The XRD spectra of ore deposit cathode material.
Embodiment 5
Double-perovskite cathode material prepared by embodiment 4 is cut into the cuboid that thickness is about 1mm, in its two short connection
Two a diameter of 0.2mm filamentary silver, then by sample both ends filamentary silver access conductivity measurement, double-perovskite cathode material with
Filamentary silver contact position coats conductive silver paste.It is the small polaron hopping using electronics conduction as electrically conducting manner in electrical conductivity test process
For electrical conduction mechanism.With the rise of temperature, resistance is constantly declining, and belongs to thermal excitation.Tested, as a result see that Fig. 7, Fig. 7 are
La2NiMnO6Conductivity data figure.
As shown in Figure 7, La is expressed as according to the slope of the Arrhenius formula figures2NiMnO6Activation energy, and try to achieve
La2NiMnO6Activation energy be 0.32eV.
Embodiment 6
Double-perovskite cathode material cut growth and a width of 2mm square prepared by embodiment 4, carry out thermal expansion survey
Examination.Test contrasts the thermal coefficient of expansion of the thermal coefficient of expansion of sample and electrolyte after terminating, and whether material synthesized by judgement may be used
To be used as electrode, Fig. 8, Fig. 8 La are as a result seen2NiMnO6Thermodilatometric analysis figure：
As shown in Figure 8, it is 10.9 × 10-6K by calculating the thermal coefficient of expansion measured-1, by its standard electrolyte CGO's
The coefficient of expansion is compared, and finds their expansion coefficient similar, it is possible thereby to prove La2NiMnO6It is preferable with CGO thermal matching.
Embodiment 7
Composite impedance test is carried out to double-perovskite cathode material prepared by embodiment 4, test condition is scan frequency
1MHz~10MHz, test temperature are 300~700 DEG C.As a result Fig. 9, Fig. 9 La are seen2NiMnO6What is measured on CGO electrolyte answers
Impedance spectra.
As seen from Figure 9, the circular arc of two flattenings in EIS spectrograms be present, corresponded to two different oxygen reduction reactions,
Small arc corresponds to high frequency arc, and big arc corresponds to low frequency arc.The front end and low frequency end of each circular arc and the difference of real axis are exactly impedance
Value, it represents the polarization resistance value of the electrode process corresponding to this circular arc.In the figure, low frequency arc is more than high frequency arc, says
Bright low frequency arc is ratedeterming step.
Embodiment 8
Analysis of Compatibility with CGO is carried out to double-perovskite cathode material prepared by embodiment 4, by the electrode material of synthesis
Mixed with electrolyte, 40min~1h is ground in mortar, ground sample is put into 1000 DEG C of burning 24h of high temperature furnace, is cooled to
Room temperature, survey XRD.As a result Figure 10, Figure 10 La are seen2NiMnO6With CGO compatibility data figure.
The XRD spectra of single-phase CGO powders has been given in Figure 10.For La2NiMnO6Sample, it can be seen that upon mixing its
Significant change does not occur for the diffraction maximum of spectrogram, and each of which keeps original diffraction maximum, illustrates not react.Peak position
Do not shift and cleave.So it is considered that La under the high temperature conditions2NiMnO6Electrode material does not occur with CGO electrolyte
Chemical reaction, both have good high temeperature chemistry compatibility.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (8)
1. a kind of preparation method of double-perovskite cathode material, it is characterised in that comprise the following steps：
A) respectively by the La of pure phase2O3, NiO and MnCO3After being heat-treated, ground with dispersant, obtain mixture；
B ground after) mixture is calcined；
C) repeat step B), obtain double-perovskite cathode material.
2. preparation method according to claim 1, it is characterised in that the La of the pure phase2O3Heat treatment method be：
It is heat-treated 24 hours under conditions of 850 DEG C~950 DEG C.
3. preparation method according to claim 1, it is characterised in that the NiO of pure phase heat treatment method is：
24h is heat-treated under conditions of 140 DEG C~160 DEG C.
4. preparation method according to claim 1, it is characterised in that the MnCO of the pure phase3Heat treatment method be：
24h is heat-treated under conditions of 140 DEG C~160 DEG C.
5. preparation method according to claim 1, it is characterised in that the La2O3, NiO and MnCO3Mol ratio be 1:
1:1。
6. preparation method according to claim 1, it is characterised in that the dispersant is selected from ethanol.
7. preparation method according to claim 1, it is characterised in that step B) in, the temperature of the calcining for 1000~
1150 DEG C, the time of the calcining is 24~48 hours, and the time of the grinding is 40~60min.
8. preparation method according to claim 1, it is characterised in that the repeat step B) number be 2 times.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109665841A (en) * | 2019-01-14 | 2019-04-23 | 杭州电子科技大学 | A kind of low temperature synthesizes the preparation method of nearly room temperature ferromagnetic body |
| CN112125341A (en) * | 2020-09-23 | 2020-12-25 | 齐齐哈尔大学 | Double perovskite type semi-metallic material and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109665841A (en) * | 2019-01-14 | 2019-04-23 | 杭州电子科技大学 | A kind of low temperature synthesizes the preparation method of nearly room temperature ferromagnetic body |
| CN112125341A (en) * | 2020-09-23 | 2020-12-25 | 齐齐哈尔大学 | Double perovskite type semi-metallic material and preparation method thereof |
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