CN101789501B - Preparation method for perovskite powder material for cathode of electrolytic tank of solid oxide - Google Patents

Preparation method for perovskite powder material for cathode of electrolytic tank of solid oxide Download PDF

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CN101789501B
CN101789501B CN2010100345189A CN201010034518A CN101789501B CN 101789501 B CN101789501 B CN 101789501B CN 2010100345189 A CN2010100345189 A CN 2010100345189A CN 201010034518 A CN201010034518 A CN 201010034518A CN 101789501 B CN101789501 B CN 101789501B
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nitrate
moo
citric acid
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CN101789501A (en
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马景陶
葛奔
艾德生
邓长生
林旭平
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Tsinghua University
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Abstract

The invention relates to a preparation method for a perovskite powder material for a cathode of an electrolytic tank of a solid oxide, belonging to the technical field of new materials and energy sources. In the preparation method, citric acid is adopted as a chelating agent, and ammonium nitrate is adopted as a combustion-supporting agent; after being dissolved together, the citric acid, the ammonium nitrate and metal nitrate form a water-soluble coordination compound with deionized water; after the pH value of solution is adjusted, water-bath evaporation is carried out on redundant moisture to form viscous gel; finally, the gel is continuously heated in a vacuum constant-temperature oven till combustion, and combustion products are collected and ground to obtain needed ultra-fine powder. By utilizing the preparation method in the invention, the ultra-fine powder that adopts a single perovskite structure and has a grain diameter within the range of tens of nanometers can be directly prepared. With simple equipment, low cost and simple processing, the preparation method can be used for preparing a fuel battery of the solid oxide, an electrode of the electrolytic tank of the solid oxide, an electrolyte powder material and a composite oxide powder material for other purposes on a small scale in a laboratory.

Description

The preparation method who is used for the perovskite powder material of cathode of electrolytic tank of solid oxide
Technical field
The present invention relates to a kind of preparation method who is used for the perovskite powder material of cathode of electrolytic tank of solid oxide, belong to new material and energy technology field.
Background technology
The crystal structure of perovskite material uniqueness causes it to have various good performances, as dielectricity, ferroelectricity, high catalytic activity, high-temperature superconductivity, unique electromagnetic performance or the like.Last century Mo, perovskite material was extensively paid attention to by scientific circles with the discovery of excellent electrochemical properties, and perovskite is used for electrode material and has anti-carbon, high catalytic activity, Stability Analysis of Structures, redox-stable or the like advantage.Perovskite material begins to be widely used in the electrode material of battery before and after 21 century.The double-perovskite material is paid close attention to the discovery of giant magnetoresistance effect, and it is more outstanding than perovskite to find that afterwards it shows aspect chemical property, and therefore having begun it is applied to the broad research of electrode material.Studies show that, adopt ultra-fine electrode powder body material to help improving the chemical property of entire cell.
The method of traditional synthetic perovskite powder mainly contains solid reaction process, coprecipitation, hydrothermal synthesis method, sol-gel process, and pluses and minuses are respectively arranged.This experiment adopts citric acid collosol and gel combustion synthesis method to prepare double-perovskite oxide S r 2Fe 1-xM xMoO 6-δ(M is Sc, Mn, Ni, Co etc.) serial powder body material.This method possesses following advantage: 1. reactive component can evenly mix on molecule, ionic level; 2. can prepare the Ca-Ti ore type superfine powder of particle diameter in the tens nanometer scope, and the even particle size distribution of powder; 3. become the phase temperature low; 4. equipment is simple, technology is simple, cost is low.
Summary of the invention
The present invention relates to a kind of preparation method who is used for the perovskite powder material of cathode of electrolytic tank of solid oxide, be applied to solid oxide electrolysis cell (SOEC) negative electrode, and reduce production costs, simplify technical process.
The preparation method of the perovskite powder material that is used for cathode of electrolytic tank of solid oxide that the present invention proposes may further comprise the steps:
(1) raw material:
In scandium nitrate, manganese nitrate, nickel nitrate or the cobalt nitrate any,
Strontium nitrate,
Ferric nitrate,
Ammonium molybdate,
Citric acid;
(2) by molecular formula Sr 2Fe 1-xM xMoO 6-δIn each metallic element mole proportioning (Sr: Fe: M: Mo=2: (1-x): x: 1), calculate the required metal nitrate of weighing, ammonium molybdate ((NH respectively 4) 6Mo 7O 244H 2O), concrete mol ratio is as follows:
Strontium nitrate: Sr 2Fe 1-xM xMoO 6-δ=2: 1, ferric nitrate: Sr 2Fe 1-xM xMoO 6-δ=(1-x): 1, any in scandium nitrate, manganese nitrate, nickel nitrate or the cobalt nitrate: Sr 2Fe 1-xM xMoO 6-δ=x: 1, ammonium molybdate ((NH 4) 6Mo 7O 244H 2O): Sr 2Fe 1-xM xMoO 6-δ=(1/7): 1, citric acid: Sr 2Fe 1-xM xMoO 6-δ=(6～10): 1, weighing combustion adjuvant NH in molar ratio 4NO 3: ammonium nitrate: Sr 2Fe 1-xM xMoO 6-δ=(25～50): 3;
(3) citric acid with above-mentioned weighing is dissolved in the deionized water, forms the citric acid supersaturated solution;
(4) all nitrate with above-mentioned weighing join in the above-mentioned citric acid saturated solution together with combustion adjuvant, add appropriate amount of deionized water, stir to form the brownish red mixed solution;
(5) ammonium molybdate with above-mentioned weighing is dissolved in deionized water, behind the formation clear solution, joins in the above-mentioned brownish red mixed solution, stirs;
(6) the pH value of regulating above-mentioned mixed solution with ammoniacal liquor is to 2-4, places that the heating evaporation excessive moisture forms thick gel under the water-bath environment;
(7) gel is heated to 150-200 ℃ under closed environment, until burning, combustion product is collected in the cooling back, grinds, and obtains powder.
The preparation method of the perovskite powder material that is used for cathode of electrolytic tank of solid oxide that the present invention proposes can prepare the perovskite powder of particle diameter 20～30 nanometers.After the combustion adjuvant that adds capacity, violent combustion reaction fully can make combustion product directly generate with the form of perovskite structure in airtight space, does not need follow-up calcining step substantially.Utilize the inventive method can directly prepare the superfine powder of the single perovskite structure of particle diameter in the tens nanometer scope.And the preparation process equipment needed thereby of this method is simple, technical process is easy to control, production cost is low, can be used for electrode and electrolyte powder material that the laboratory prepares Solid Oxide Fuel Cell, electrolytic tank of solid oxide on a small scale, and the composite oxide powder material of other purposes.
Description of drawings
Fig. 1 is the stereoscan photograph of the embodiment 1 preparation powder of the inventive method.
Fig. 2 is the XRD spectra of embodiment 1 powder.
Fig. 3 is the stereoscan photograph of embodiment 2 powders.
Embodiment
The preparation method of the perovskite powder material that is used for cathode of electrolytic tank of solid oxide that the present invention proposes may further comprise the steps:
(1) raw material:
In scandium nitrate, manganese nitrate, nickel nitrate or the cobalt nitrate any,
Strontium nitrate,
Ferric nitrate,
Ammonium molybdate,
Citric acid;
(2) by molecular formula Sr 2Fe 1-xM xMoO 6-δIn each metallic element mole proportioning (Sr: Fe: M: Mo=2: (1-x): x: 1), calculate the required metal nitrate of weighing, ammonium molybdate ((NH respectively 4) 6Mo 7O 244H 2O), concrete mol ratio is as follows:
Strontium nitrate: Sr 2Fe 1-xM xMoO 6-δ=2: 1, ferric nitrate: Sr 2Fe 1-xM xMoO 6-δ=(1-x): 1, any in scandium nitrate, manganese nitrate, nickel nitrate or the cobalt nitrate: Sr 2Fe 1-xM xMoO 6-δ=x: 1, ammonium molybdate ((NH 4) 6Mo 7O 244H 2O): Sr 2Fe 1-xM xMoO 6-δ=(1/7): 1, citric acid: Sr 2Fe 1-xM xMoO 6-δ=(6～10): 1, weighing combustion adjuvant NH in molar ratio 4NO 3: ammonium nitrate: Sr 2Fe 1-xM xMoO 6-δ=(25～50): 3;
(3) citric acid with above-mentioned weighing is dissolved in the deionized water, forms the citric acid supersaturated solution;
(4) all nitrate with above-mentioned weighing join in the above-mentioned citric acid saturated solution together with combustion adjuvant, add appropriate amount of deionized water, stir to form the brownish red mixed solution;
(5) ammonium molybdate with above-mentioned weighing is dissolved in deionized water, behind the formation clear solution, joins in the above-mentioned brownish red mixed solution, stirs;
(6) the pH value of regulating above-mentioned mixed solution with ammoniacal liquor is to 2-4, places that the heating evaporation excessive moisture forms thick gel under the water-bath environment;
(7) gel is heated to 150-200 ℃ under closed environment, until burning, combustion product is collected in the cooling back, grinds, and obtains powder.
The Sr that the inventive method is related 2Fe 1-xM xMoO 6-δThe series powder body material, wherein M be Sc, Mn, Ni, Co etc.+2 or+transition metal of 3 valencys.
The related preparation method of the inventive method also can be used for the preparation of other Ca-Ti ore type powder body material, is not limited to electrode material, and wherein perovskite-type material also is not limited to Sr 2Fe 1-xM xMoO 6-δSystem.
Among the preparation method of the present invention, separately with (NH 4) 6Mo 7O 244H2O is dissolved in deionized water, and forms clear solution, and then just adds mixed solution, and this is because (NH 4) 6Mo 7O 244H 2Can form the iron molybdate precipitation under O and the ferric nitrate solutions of weak acidity, precipitation can be decomposed by ammoniacal liquor, but the surface can generate the iron hydroxide film, has hindered further dissolving, and then hinders (NH 4) 6Mo 7O 244H 2The dissolving of O therefore must be separately with (NH 4) 6Mo 7O 244H 2O adds mixed solution after forming solution again, can avoid above-mentioned phenomenon, accelerates the experiment process.
Among the preparation method of the present invention, by the content of regulating combustion adjuvant, the pH value of solution, the particle diameter of may command product powder.The pH of solution is advisable with about 3, when the pH value greater than 4 the time, solution has precipitation in heating process and separates out, and is unfavorable for powder preparing.
Below introduce the embodiment of the inventive method:
Embodiment 1, Sr 2Fe 0.8Sc 0.2MoO 6-δSynthesizing of powder:
(1) raw material: strontium nitrate (Sr (NO 3) 2), ferric nitrate (Fe (NO 3) 39H 2O), scandium nitrate (Sc (NO 3) 25H 2O), ammonium molybdate ((NH 4) 6Mo 7O 244H 2O), citric acid.
(2) press 0.06mol Sr 2Fe 0.8Sc 0.2MoO 6-δTheoretical yield is by molecular formula Sr 2Fe 0.8Sc 0.2MoO 6-δIn each metallic element mole proportioning (Sr: Fe: Sc: Mo=2: 0.8: 0.2: 1), press citric acid: Sr 2Fe 0.8Sc 0.2MoO 6-δ=6: 1 mol ratio is calculated weighing strontium nitrate, ferric nitrate, scandium nitrate, ammonium molybdate and citric acid respectively, presses ammonium nitrate (NH 4NO 3): Sr 2Fe 0.8Sc 0.2MoO 6-δ=50: 3 mol ratio is calculated weighing combustion adjuvant NH 4NO 3
(3) citric acid is dissolved in the 100ml deionized water and forms supersaturated solution, purpose is to reduce the consumption of deionized water as far as possible, and it is consuming time oversize to avoid follow-up water-bath to evaporate;
(4) load weighted all nitrate are added citric acid solution, add about 500ml deionized water again, form the brownish red clear solution by magnetic stirring apparatus;
(5) with load weighted (NH 4) 6Mo 7O 244H 2O is dissolved in deionized water, form clear solution after, add in the above-mentioned brownish red mixed solution and stir (note, must be completed into behind the settled solution mixed again);
(6) add ammoniacal liquor mixed solution pH is transferred to 3;
(7) mixed solution that mixes up is placed the heating evaporation excessive moisture forms thick gel under 80 ℃ of water-bath environment; Gel placed in 160 ℃ of vacuum constant temperature baking ovens continue heating until burning, combustion product is collected in the cooling back, grinds, and obtains powder just.
(8) pattern of observation powder under ESEM, as shown in Figure 1.Fig. 2 is the XRD spectra of first powder, as seen from the figure, and the Sr that utilizes above-mentioned preparation method to prepare 2Fe 0.8Sc 0.2MoO 6-δPowder has basically formed single perovskite structure under the situation without calcining.
Embodiment 2, Sr 2Fe 0.8Mn 0.2MoO 6-δSynthesizing of powder
(1) raw material: strontium nitrate (Sr (NO 3) 2), ferric nitrate (Fe (NO 3) 39H 2O), manganese nitrate (50%wt), ammonium molybdate ((NH 4) 6Mo 7O 244H 2O), citric acid.
(2) press 0.06mol Sr 2Fe 0.8Mn 0.2MoO 6-δTheoretical yield is by molecular formula Sr 2Fe 0.8Mn 0.2MoO 6-δIn each metallic element mole proportioning (Sr: Fe: Mn: Mo=2: 0.8: 0.2: 1), press citric acid: Sr 2Fe 0.8Mn 0.2MoO 6-δ=8: 1 mol ratio is calculated weighing strontium nitrate, ferric nitrate, manganese nitrate, ammonium molybdate and citric acid respectively, presses ammonium nitrate (NH 4NO 3): Sr 2Fe 0.8Sc 0.2MoO 6-δ=25: 3 mol ratio is calculated weighing combustion adjuvant NH 4NO 3
(3) citric acid is dissolved in about 100ml deionized water and forms the satiety supersaturated solution;
(4) load weighted nitrate or solution are added citric acid solution, and add about 400ml deionized water, form the brownish red clear solution by magnetic stirring apparatus;
(5) with load weighted (NH 4) 6Mo 7O 244H 2O is dissolved in deionized water, form clear solution after, add in the above-mentioned brownish red mixed solution and stir;
(6) adding ammoniacal liquor transfers to mixed solution pH to about 3;
(7) mixed solution that mixes up is placed the heating evaporation excessive moisture forms thick gel under 97 ℃ of water-bath environment; Gel placed in 170 ℃ of vacuum constant temperature baking ovens continue heating until burning, combustion product is collected in the cooling back, grinds, and obtains powder just;
(8) Fig. 3 is the stereoscan photograph of powder, finds out that by figure diameter of particle is in the tens nanometer level.
Embodiment 3:
(1) raw material: strontium nitrate (Sr (NO 3) 2), ferric nitrate (Fe (NO 3) 39H 2O), nickel nitrate (Ni (NO 3) 26H 2O), ammonium molybdate ((NH 4) 6Mo 7O 244H 2O), citric acid.
(2) press 0.06mol Sr 2Fe 0.8Ni 0.2MoO 6-δTheoretical yield is by molecular formula Sr 2Fe 0.8Ni 0.2MoO 6-δIn each metallic element mole proportioning (Sr: Fe: Ni: Mo=2: 0.8: 0.2: 1), press citric acid: Sr 2Fe 0.8Mn 0.2MoO 6-δ=8: 1 mol ratio is calculated weighing strontium nitrate, ferric nitrate, scandium nitrate, ammonium molybdate and citric acid respectively, presses ammonium nitrate (NH 4NO 3): Sr 2Fe 0.8Sc 0.2MoO 6-δ=40: 3 mol ratio is calculated weighing combustion adjuvant NH 4NO 3
(3) citric acid is dissolved in the 80ml deionized water and forms supersaturated solution;
(4) load weighted all nitrate are added citric acid solution, add about 400ml deionized water again, form the brownish red clear solution by magnetic stirring apparatus;
(5) with load weighted (NH 4) 6Mo 7O 244H 2O is dissolved in deionized water, form clear solution after, add in the above-mentioned brownish red mixed solution and stir;
(6) add ammoniacal liquor mixed solution pH is transferred to 2;
(7) mixed solution that mixes up is placed the heating evaporation excessive moisture forms thick gel under 90 ℃ of water-bath environment; Gel placed in 170 ℃ of vacuum constant temperature baking ovens continue heating until burning, combustion product is collected in the cooling back, grinds, and obtains the powder that particle diameter is about 20-30nm.
Embodiment 4
(1) raw material: strontium nitrate (Sr (NO 3) 2), ferric nitrate (Fe (NO 3) 39H 2O), cobalt nitrate (Co (NO 3) 26H 2O), ammonium molybdate ((NH 4) 6Mo 7O 244H 2O), citric acid.
(2) press 0.06mol Sr 2Fe 0.8Co 0.2MoO 6-δTheoretical yield is by molecular formula Sr 2Fe 0.8Co 0.2MoO 6-δIn each metallic element mole proportioning (Sr: Fe: Co: Mo=2: 0.8: 0.2: 1), press citric acid: Sr 2Fe 0.8Mn 0.2MoO 6-δ=10: 1 mol ratio is calculated weighing strontium nitrate, ferric nitrate, scandium nitrate, ammonium molybdate and citric acid respectively, presses ammonium nitrate (NH 4NO 3): Sr 2Fe 0.8Sc 0.2MoO 6-δ=10: 1 mol ratio is calculated weighing combustion adjuvant NH 4NO 3
(3) citric acid is dissolved in the 80ml deionized water and forms supersaturated solution;
(4) load weighted all nitrate are added citric acid solution, add about 400ml deionized water again, form the brownish red clear solution by magnetic stirring apparatus;
(5) with load weighted (NH 4) 6Mo 7O 244H 2O is dissolved in deionized water, form clear solution after, add in the above-mentioned brownish red mixed solution and stir;
(6) add ammoniacal liquor mixed solution pH is transferred to 4;
(7) mixed solution that mixes up is placed the heating evaporation excessive moisture forms thick gel under 97 ℃ of water-bath environment; Gel placed in 175 ℃ of vacuum constant temperature baking ovens continue heating until burning, combustion product is collected in the cooling back, grinds, and obtains the powder that particle diameter is about 30-40nm.

Claims (1)

1. preparation method who is used for the perovskite powder material of cathode of electrolytic tank of solid oxide is characterized in that this preparation method may further comprise the steps:
(1) raw material:
In scandium nitrate, manganese nitrate, nickel nitrate or the cobalt nitrate any,
Strontium nitrate,
Ferric nitrate,
Ammonium molybdate,
Citric acid;
(2) by molecular formula Sr 2Fe 1-xM xMoO 6-δIn each metallic element mole proportioning Sr: Fe: M: Mo=2: (1-x): x: 1, calculate the required metal nitrate of weighing, ammonium molybdate (NH respectively 4) 6Mo 7O 244H 2O, concrete mol ratio is as follows:
Strontium nitrate: Sr 2Fe 1-xM xMoO 6-δ=2: 1, ferric nitrate: Sr 2Fe 1-xM xMoO 6-δ=(1-x): 1, any in scandium nitrate, manganese nitrate, nickel nitrate or the cobalt nitrate: Sr 2Fe 1-xM xMoO 6-δ=x: 1, ammonium molybdate (NH 4) 6Mo 7O 244H 2O: Sr 2Fe 1-xM xMoO 6-δ=(1/7): 1, citric acid: Sr 2Fe 1-xM xMoO 6-δ=(6～10): 1, weighing combustion adjuvant ammonium nitrate NH in molar ratio 4NO 3: Sr 2Fe 1-xM xMoO 6-δ=(25～50): 3; Wherein M be Sc, Mn, Ni or Co+2 or+transition metal of 3 valencys;
(3) citric acid with above-mentioned weighing is dissolved in the deionized water, forms the citric acid supersaturated solution;
(4) all nitrate with above-mentioned weighing join in the above-mentioned citric acid saturated solution together with combustion adjuvant, add appropriate amount of deionized water, stir to form the brownish red mixed solution;
(5) ammonium molybdate with above-mentioned weighing is dissolved in deionized water, behind the formation clear solution, joins in the above-mentioned brownish red mixed solution, stirs;
(6) the pH value of regulating above-mentioned mixed solution with ammoniacal liquor is to 2-4, places that the heating evaporation excessive moisture forms thick gel under the water-bath environment;
(7) gel is heated to 150-200 ℃ under closed environment, until burning, combustion product is collected in the cooling back, grinds, and obtains powder.
CN2010100345189A 2010-01-22 2010-01-22 Preparation method for perovskite powder material for cathode of electrolytic tank of solid oxide Expired - Fee Related CN101789501B (en)

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CN103825038B (en) * 2014-01-22 2016-02-10 清华大学 A kind of electrolyte of perovskite structure
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CN107855074A (en) * 2017-11-28 2018-03-30 桂林电子科技大学 A kind of particle diameter thinning method that metal oxide materials are prepared using nitrate as raw material
CN112250437B (en) * 2019-11-05 2022-08-05 济南大学 Solid oxide electrolytic cell supported by oxygen electrode and preparation method thereof
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