CN104193397A - Perovskite structured porous Ba0.5 Sr0.5 Co0.8 Fe0.2O3-delta material and preparation method thereof - Google Patents
Perovskite structured porous Ba0.5 Sr0.5 Co0.8 Fe0.2O3-delta material and preparation method thereof Download PDFInfo
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- CN104193397A CN104193397A CN201410428960.8A CN201410428960A CN104193397A CN 104193397 A CN104193397 A CN 104193397A CN 201410428960 A CN201410428960 A CN 201410428960A CN 104193397 A CN104193397 A CN 104193397A
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Abstract
The invention provides a perovskite structured porous Ba0.5 Sr0.5 Co0.8 Fe0.2 O3-delta material and a preparation method thereof. The method comprises the following steps: 1) preparing a mixed aqueous solution containing Ba<2+>, Sr<2+>, Co<2+> and Fe<3+>; 2) adding a complexing agent and a structure stabilizer into the mixed aqueous solution, and uniformly mixing, so that a transparent solution or sol is obtained; 3) adding carbon balls into the transparent solution or sol, and stirring so as to enable the carbon balls to be uniformly dispersed, so that a turbid liquid is obtained; 4) stirring the turbid liquid while heating until solvents in the turbid liquid are dried and volatilized, so that xerogel is obtained; and 5) carrying out heat treatment on the xerogel at a temperature of 900-1000 DEG C.
Description
Technical field
The invention belongs to technical field of inorganic nanometer material, be specifically related to a kind of perovskite structure porous Ba
0.5sr
0.5co
0.8fe
0.2o
3-δmaterial and preparation method thereof.
Background technology
There is perovskite structure ABO
3material-the Ba of type
0.5sr
0.5co
0.8fe
0.2o
3-δ, A position is Ba
0.5sr
0.5, B position is Co
0.8fe
0.2, be a kind of conventional fuel battery negative pole electrocatalyst materials, be widely used in the positive electrode material of Solid Oxide Fuel Cell of 400～800 DEG C.In recent years, particularly within 2011, be published in research work on Science taking the Yang SH of Massachusetts Polytechnics and point out as representative, this Ba
0.5sr
0.5co
0.8fe
0.2o
3-δcan show at normal temperatures high oxygen catalytic reduction activity (ORR); The people's such as Emiliana Fabbri in 2014 research work has further confirmed this phenomenon, and this result of study has just been published on ACS Catalysis.This is Ba
0.5sr
0.5co
0.8fe
0.2o
3-δyishanmen has been opened in application in the cathode material of low-temperature fuel cell.
But, adopt conventional sol-gel method (Sol-Gel) to prepare the Ba with perovskite structure
0.5sr
0.5co
0.8fe
0.2o
3-δ, often need at the temperature of>=1000 DEG C, synthesize generally lower (≤10m of the specific surface area of the powder body material that obtains
2/ g).The catalyst powder material with high-specific surface area exposes more catalytic activity point, also will be conducive to and promote the carrying out of catalyzed reaction.Thereby this field is in the urgent need to the synthetic specific area Ba of a kind of low temperature
0.5sr
0.5co
0.8fe
0.2o
3-δthe method of material.
Summary of the invention
The present invention is intended to overcome existing Ba
0.5sr
0.5co
0.8fe
0.2o
3-δthe defect of material aspect performance and preparation method, the invention provides a kind of perovskite structure porous Ba
0.5sr
0.5co
0.8fe
0.2o
3-δmaterial and preparation method thereof.
The invention provides a kind of perovskite structure porous Ba
0.5sr
0.5co
0.8fe
0.2o
3-δthe preparation method of material, described method comprises:
1) preparation meets chemical formula Ba
0.5sr
0.5co
0.8fe
0.2o
3-δbetween middle Ba, Sr, Co, Fe mol ratio, contain Ba
2+, Sr
2+, Co
2+, Fe
3+mixed aqueous solution;
2) to step 1) add complexing agent and structural stabilizing agent in the mixed aqueous solution prepared, and mix, obtain clear solution or colloidal sol;
3) to step 2) add carbon ball in the clear solution prepared or colloidal sol, and stir and make carbon ball dispersed, obtain suspension liquid;
4) the lower whipping step 3 of heating) in the suspension liquid of preparation volatilize wherein solvent and obtain xerogel;
5) by step 4) xerogel prepared heat-treats at 900～1000 DEG C, removes carbon ball, obtains described perovskite structure porous Ba
0.5sr
0.5co
0.8fe
0.2o
3-δmaterial.
Preferably, step 1) in, with Ba (NO
3)
2, Sr (NO
3)
2, Co (NO
3)
26H
2o, Fe (NO
3)
39H
2o is raw material.
Preferably, step 1) in, in mixed aqueous solution, Ba
2+volumetric molar concentration be 0.05～0.1mol/L.
Preferably, step 2) described in complexing agent and the volumetric molar concentration of structural stabilizing agent in mixing solutions be metal ion volumetric molar concentration sum 0.5-4 doubly.
Preferably, step 3) the middle carbon ball using, before using, carry out alkaline purification, after soaking in basic solution by carbon ball, leach, dry, the diameter of carbon ball is 0.5-8 μ m.
Preferably, step 5) in, the heat treated time is 4～6 hours.
The invention provides perovskite structure porous Ba prepared by a kind of aforesaid method again,
0.5sr
0.5co
0.8fe
0.2o
3-δmaterial, described perovskite structure porous Ba
0.5sr
0.5co
0.8fe
0.2o
3-δmaterial consist of Ba
0.5sr
0.5co
0.8fe
0.2o
3-δ, aperture size is 0.5～8 μ m, specific surface area is 58～100m
2/ g.
Beneficial effect of the present invention:
(1) adopting carbon ball is mould material, is forming perovskite structure Ba
0.5sr
0.5co
0.8fe
0.2o
3-δtime, burn carbon template and form vesicular structure;
(2) the perovskite structure Ba that prepared by the method
0.5sr
0.5co
0.8fe
0.2o
3-δspecific surface area be greatly improved;
(3) the method is simple, preparation condition gentleness, and calcining temperature is low, saves the energy.
Brief description of the drawings
Fig. 1 shows the perovskite structure porous Ba preparing in an embodiment of the invention
0.5sr
0.5co
0.8fe
0.2o
3-δxRD figure;
Fig. 2 shows the perovskite structure porous Ba preparing in an embodiment of the invention
0.5sr
0.5co
0.8fe
0.2o
3-δxRD figure;
Fig. 3 shows the perovskite structure porous Ba preparing in an embodiment of the invention
0.5sr
0.5co
0.8fe
0.2o
3-δfE-SEM photo;
Fig. 4 shows the perovskite structure porous Ba preparing in an embodiment of the invention
0.5sr
0.5co
0.8fe
0.2o
3-δfE-SEM photo.
Embodiment
Further illustrate the present invention below in conjunction with accompanying drawing and following embodiment, should be understood that accompanying drawing and following embodiment are only for the present invention is described, and unrestricted the present invention.
The invention provides one and simply prepare perovskite structure porous Ba
0.5sr
0.5co
0.8fe
0.2o
3-δthe method of material.Taking diameter as micron order, (0.5～8 μ carbon ball m) is template to the method, taking citric acid or EDTA as complexing agent and structural stabilizing agent, taking metal nitrate soluble in water as precursor, as metal nitrate ion (Ba
2+, Sr
2+, Co
2+, Fe
3+) while forming uniform solution or colloidal sol, add carbon ball template, form metal ion uniform ring and be around in carbon ball xerogel around, through the thermal treatment of 900～1000 DEG C under air atmosphere, when burning carbon ball template, reactive metal oxide original position forms Ba
0.5sr
0.5co
0.8fe
0.2o
3-δ, obtain the porous Ba of perovskite structure
0.5sr
0.5co
0.8fe
0.2o
3-δmaterial.Control respectively size and the Ba of resulting materials pore structure by the diameter of simple regulation and control carbon ball template and the height of calcining temperature
0.5sr
0.5co
0.8fe
0.2o
3-δthe purity of phase.Prepared perovskite structure porous Ba
0.5sr
0.5co
0.8fe
0.2o
3-δspecific surface area (the 58-100m of material
2/ g), hole is of a size of 0.5～8 μ m.Present method preparation process is simple, mild condition, and easy handling removes carbon template when perovskite structure forms, and power saving saves time.The method belongs to the synthetic field of inorganic nano material.
Diameter by controlling carbon ball is to regulate and control described Ba
0.5sr
0.5co
0.8fe
0.2o
3-δthe aperture in material duct, aperture size is 0.5～8 μ m, specific surface area is 58～100m
2/ g.
The diameter of described carbon ball is 0.5～8 μ m.
The volumetric molar concentration of described complexing agent and structural stabilizing agent is 0.5～4 times of ionizable metal salt volumetric molar concentration.
Described metal-salt precursor is nitrate soluble in water.
Described metal nitrate is Ba (NO
3)
2, Sr (NO
3)
2, Co (NO
3)
26H
2o, Fe (NO
3)
39H
2o.
Heat treated temperature is 900～1000 DEG C.The described heat treated time is 4～6 hours.
The invention provides one and prepare perovskite structure porous Ba
0.5sr
0.5co
0.8fe
0.2o
3-δmethod, adopting carbon ball is template, selects suitable complexing agent and structural stabilizing agent to make ionizable metal salt be looped around uniformly the surface of carbon ball, at the synthetic Ba of thermal treatment
0.5sr
0.5co
0.8fe
0.2o
3-δtime remove carbon ball, thereby obtain the porous Ba of perovskite structure
0.5sr
0.5co
0.8fe
0.2o
3-δ, also greatly improving the specific surface area of this material, this has no report in the world.
In the present invention, perovskite structure porous Ba
0.5sr
0.5co
0.8fe
0.2o
3-δa specific solution of material is as follows:
(1) according to document (Carbon 39 (2001) 2211 – 2214) hydrothermal method preparation or directly buy from the market the carbon ball of different diameter (0.5～8 μ is m) as mould material;
(2) this carbon ball material is soaked in to 1h in NaOH that concentration is 0.05M or ammonia soln, filter be placed in 60～100 DEG C of baking ovens, dry 2～8h hour for subsequent use;
(3) be mBa (NO by metal nitrate according to volumetric molar concentration
3)
2: m Sr (NO
3)
2: m Co (NO
3)
26H
2o:mFe (NO
3)
39H
2the ratio of O=0.5:0.5:0.8:0.2 is dissolved in 100～200ml deionized water, and after stirring, adding volumetric molar concentration is citric acid or the EDTA of 0.5～4 times of ionizable metal salt, continues to stir the solution of 1～3h formation homogeneous transparent;
(4) clear solution in (2) is added to 5 times to the carbon ball material of metal-salt mole number, continue to stir after 2h, gained suspension liquid is under 150～300 DEG C of stirrings, and the moisture that volatilizees gradually forms xerogel;
(5) after the xerogel obtaining in step (3) is ground, be placed in 900～1000 DEG C of thermal treatment 4～6h under retort furnace air atmosphere, obtain the porous Ba of perovskite structure
0.5sr
0.5co
0.8fe
0.2o
3-δmaterial.
Advantage of the present invention is as follows:
(1) adopting carbon ball is mould material, is forming perovskite structure Ba
0.5sr
0.5co
0.8fe
0.2o
3-δtime, burn carbon template and form vesicular structure;
(2) the perovskite structure Ba that prepared by the method
0.5sr
0.5co
0.8fe
0.2o
3-δspecific surface area be greatly improved;
(3) the method is simple, preparation condition gentleness, and calcining temperature is low, saves the energy.
Below further list some exemplary embodiments so that the present invention to be described better.Should understand; the above-mentioned embodiment that the present invention describes in detail; and following examples are only not used in and limit the scope of the invention for the present invention is described, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjust and all belong to protection scope of the present invention.In addition, concrete proportioning in following processing parameter, time, temperature etc. are only also exemplary, and those skilled in the art can select suitable value in the scope of above-mentioned restriction.
Embodiment 1
According to technique scheme of the present invention and technical process, first preparing diameter according to document is that the carbon ball of 8 μ m is as mould material, then this carbon ball material is soaked in to 1h in the NaOH solution that concentration is 0.05M, through filter be placed in 60 DEG C of baking ovens, dry 8h hour for subsequent use.Be mBa (NO by metal nitrate according to volumetric molar concentration
3)
2: mSr (NO
3)
2: mCo (NO
3)
26H
2o:mFe (NO
3)
39H
2the ratio of O=0.5:0.5:0.8:0.2, the i.e. Ba (NO of 1.31g
3)
2, the Sr (NO of 1.1g
3)
2, the Co (NO of 2.328g
3)
26H
2o, the Fe (NO of 0.81g
3)
39H
2o, is dissolved in 200ml deionized water, and after stirring, adding volumetric molar concentration is the citric acid 8.4g of 2 times of left and right of ionizable metal salt, continues to stir the solution of 3h formation homogeneous transparent.Afterwards, add 5 times to the carbon ball material 1.2g of metal-salt mole number, continue to stir after 2h, gained suspension liquid is under 300 DEG C of stirrings, and the moisture that volatilizees gradually forms xerogel.Xerogel, after grinding, is placed in the lower 900 DEG C of thermal treatment 6h of retort furnace air atmosphere, obtains the porous Ba of perovskite structure
0.5sr
0.5co
0.8fe
0.2o
3-δmaterial;
The specific surface area of prepared material is: 58m
2/ g (table 1), aperture size is～8 μ m, as shown in the SEM photo of A in Fig. 3.
Embodiment 2
According to (with embodiment 1) described in technical process, first preparing diameter according to document is that the carbon ball of 6 μ m is as mould material, and gained xerogel, after grinding, is placed in the lower 900 DEG C of thermal treatment 5h of retort furnace air atmosphere, other operational conditions are same with embodiment 1.The Ba that the structure that obtains material is perovskite typed
0.5sr
0.5co
0.8fe
0.2o
3-δ, as shown in the black spectral line in Fig. 1 XRD figure spectrum (900 DEG C/5h), specific surface area is 72m
2/ g (table 1), aperture size is～5.5 μ m, as shown in the SEM photo of B in Fig. 3.
Embodiment 3
According to (with embodiment 1) described in technical process, first preparing diameter according to document is that the carbon ball of 5 μ m is as mould material, and gained xerogel, after grinding, is placed in the lower 1000 DEG C of thermal treatment 5h of retort furnace air atmosphere, and other operational conditions are with embodiment 1.The Ba that the structure that obtains material is perovskite typed
0.5sr
0.5co
0.8fe
0.2o
3-δ, and the increase of the purity of Perovskite Phase, can find out by the red spectral line (1000 DEG C/5h) from Fig. 1 XRD figure spectrum, specific surface area is 78m
2/ g (table 1), aperture size is～5 μ m, as shown in the SEM photo of C in Fig. 3.
Embodiment 4
According to technique scheme of the present invention and technical process, first preparing diameter according to document is that the carbon ball of 2 μ m is as mould material, then this carbon ball material is soaked in to 1h in the ammonia soln that concentration is 0.05M, through filter be placed in 100 DEG C of baking ovens, dry 2h hour for subsequent use.Be mBa (NO by metal nitrate according to volumetric molar concentration
3)
2: mSr (NO
3)
2: mCo (NO
3)
26H
2o:mFe (NO
3)
39H
2the ratio of O=0.5:0.5:0.8:0.2, the i.e. Ba (NO of 2.62g
3)
2, the Sr (NO of 2.2g
3)
2, the Co (NO of 4.656g
3)
26H
2o, the Fe (NO of 1.62g
3)
39H
2o, is dissolved in 100ml deionized water, and after stirring, adding volumetric molar concentration is the EDTA 8.4g of 0.7 times of left and right of ionizable metal salt, continues to stir the solution of 1h formation homogeneous transparent.Afterwards, add 5 times to the carbon ball material 2.4g of metal-salt mole number, continue to stir after 2h, gained suspension liquid is under 150 DEG C of stirrings, and the moisture that volatilizees gradually forms xerogel.Xerogel, after grinding, is placed in the lower 1000 DEG C of thermal treatment 4h of retort furnace air atmosphere, obtains the porous Ba of perovskite structure
0.5sr
0.5co
0.8fe
0.2o
3-δmaterial;
The specific surface area of prepared material is: 80m
2/ g (table 1), aperture size is～2 μ m, as shown in the SEM photo of D in Fig. 3.
Embodiment 5
According to (with embodiment 4) described in technical process, first preparing diameter according to document is that the carbon ball of 0.5 μ m is as mould material, gained xerogel, after grinding, is placed in the lower 900 DEG C of thermal treatment 5h of retort furnace air atmosphere, obtains the porous Ba of perovskite structure
0.5sr
0.5co
0.8fe
0.2o
3-δmaterial;
The specific surface area of prepared material is: 100m
2/ g (table 1), aperture size is～0.5 μ m, as shown in the SEM photo of A in Fig. 4.
Comparative example 1
According to (with embodiment 1) described in technical process, do not add carbon ball, other operate with embodiment 1, and prepared material is also perovskite structure, and as shown in the XRD figure spectrum in Fig. 2, but specific surface area is lower, only has 9.5m
2/ g (table 1).
Comparative example 2
According to (with embodiment 4) described in technical process, do not add carbon ball, other operate with embodiment 4, and prepared material does not contain vesicular structure, as shown in the SEM photo of B in Fig. 4.
The prepared perovskite structure porous of table 1 Ba
0.5sr
0.5co
0.8fe
0.2o
3-δthe specific surface area of material
| Sample | BET specific surface area/m 2.g -1 |
| 8 μ mCS-BSCF (example 1) | 58 |
| 6 μ mCS-BSCF (example 2) | 72 |
| 5 μ mCS-BSCF (example 3) | 78 |
| 2 μ mCS-BSCF (example 4) | 80 |
| 0.5 μ mCS-BSCF (example 5) | 100 |
| BSCF (comparative example 1) | 9.5 |
Claims (8)
1. a perovskite structure porous Ba
0.5sr
0.5co
0.8fe
0.2o
3-δthe preparation method of material, is characterized in that, described method comprises:
1) preparation meets chemical formula Ba
0.5sr
0.5co
0.8fe
0.2o
3-δbetween middle Ba, Sr, Co, Fe mol ratio, contain Ba
2+, Sr
2+, Co
2+, Fe
3+mixed aqueous solution;
2) in the mixed aqueous solution of preparing to step 1), add complexing agent and structural stabilizing agent, and mix, obtain clear solution or colloidal sol;
3) to step 2) add carbon ball in the clear solution prepared or colloidal sol, and stir and make carbon ball dispersed, obtain suspension liquid;
4) the lower whipping step 3 of heating) in the suspension liquid of preparation volatilize wherein solvent and obtain xerogel;
5) xerogel of being prepared by step 4) is heat-treated at 900～1000 DEG C, removes carbon ball, obtains described perovskite structure porous Ba
0.5sr
0.5co
0.8fe
0.2o
3-δmaterial.
2. preparation method according to claim 1, is characterized in that, in step 1), with Ba (NO
3)
2, Sr (NO
3)
2, Co (NO
3)
26H
2o, Fe (NO
3)
39H
2o is raw material.
3. preparation method according to claim 1 and 2, is characterized in that, in step 1), and in mixed aqueous solution, Ba
2+volumetric molar concentration be 0.05～0.1mol/L.
4. according to arbitrary described preparation method in claim 1-3, it is characterized in that step 2) in the complexing agent and the structural stabilizing agent that use be citric acid and/or EDTA.
5. according to arbitrary described preparation method in claim 1-4, it is characterized in that step 2) described in complexing agent and the volumetric molar concentration of structural stabilizing agent in mixing solutions be metal ion volumetric molar concentration sum 0.5-4 doubly.
6. according to arbitrary described preparation method in claim 1-5, it is characterized in that, the carbon ball using in step 3), leaches, dries after before using, carbon ball being soaked in basic solution, and the diameter of carbon ball is 0.5-8 μ m.
7. according to arbitrary described preparation method in claim 1-6, it is characterized in that, in step 5), the heat treated time is 4～6 hours.
8. the perovskite structure porous Ba that in a claim 1-7 prepared by arbitrary described method
0.5sr
0.5co
0.8fe
0.2o
3-δmaterial, is characterized in that, described perovskite structure porous Ba
0.5sr
0.5co
0.8fe
0.2o
3-δmaterial consist of Ba
0.5sr
0.5co
0.8fe
0.2o
3-δ, aperture size is 0.5～8 μ m, specific surface area is 58～100m
2/ g.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104923083A (en) * | 2015-06-04 | 2015-09-23 | 上海穗杉实业有限公司 | Stainless steel doped perovskite ceramic two-phase composite hollow fiber oxygen-permeating membrane and preparation method thereof |
| CN106582659A (en) * | 2016-11-08 | 2017-04-26 | 华东理工大学 | Mixed ion-electron conductor oxide/diatomite composite soot combustion catalyst and preparation method thereof |
| CN108117086A (en) * | 2016-11-26 | 2018-06-05 | 中国科学院大连化学物理研究所 | A kind of preparation method of oxygen absorbent |
| CN108114688A (en) * | 2016-11-26 | 2018-06-05 | 中国科学院大连化学物理研究所 | A kind of oxygen absorbent for oxygen coalescence |
| WO2023065400A1 (en) * | 2021-10-22 | 2023-04-27 | 武汉工程大学 | Porous multi-doped perovskite catalyst and preparation method therefor |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104923083A (en) * | 2015-06-04 | 2015-09-23 | 上海穗杉实业有限公司 | Stainless steel doped perovskite ceramic two-phase composite hollow fiber oxygen-permeating membrane and preparation method thereof |
| CN106582659A (en) * | 2016-11-08 | 2017-04-26 | 华东理工大学 | Mixed ion-electron conductor oxide/diatomite composite soot combustion catalyst and preparation method thereof |
| CN108117086A (en) * | 2016-11-26 | 2018-06-05 | 中国科学院大连化学物理研究所 | A kind of preparation method of oxygen absorbent |
| CN108114688A (en) * | 2016-11-26 | 2018-06-05 | 中国科学院大连化学物理研究所 | A kind of oxygen absorbent for oxygen coalescence |
| WO2023065400A1 (en) * | 2021-10-22 | 2023-04-27 | 武汉工程大学 | Porous multi-doped perovskite catalyst and preparation method therefor |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104193397B (en) | 2016-03-23 |
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