CN106745261B - A kind of method of synthesis of solid oxide fuel battery electrolyte material nanometer lanthanum molybdate - Google Patents

A kind of method of synthesis of solid oxide fuel battery electrolyte material nanometer lanthanum molybdate Download PDF

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CN106745261B
CN106745261B CN201611062320.5A CN201611062320A CN106745261B CN 106745261 B CN106745261 B CN 106745261B CN 201611062320 A CN201611062320 A CN 201611062320A CN 106745261 B CN106745261 B CN 106745261B
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oxide fuel
molybdate
fuel battery
electrolyte material
battery electrolyte
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CN106745261A (en
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田长安
吉冬冬
阳杰
谢劲松
尹奇异
程继海
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Hefei University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00—Compounds of molybdenum
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/10—Fuel cells with solid electrolytes
    • H01M8/1016—Fuel cells with solid electrolytes characterised by the electrolyte material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/10—Fuel cells with solid electrolytes
    • H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
    • H01M8/124—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte
    • H01M8/1246—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte the electrolyte consisting of oxides
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • 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
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

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  • Chemical & Material Sciences (AREA)
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Abstract

The present invention relates to solid-oxide fuel battery electrolyte material manufacturing technology field, more particularly to a kind of method of synthesis of solid oxide fuel battery electrolyte material nanometer lanthanum molybdate.It is placed in after ammonium molybdate aqueous solution and lanthanum nitrate aqueous solution are mixed in reactor and adds precipitating reagent and carries out hydrothermal homogeneous precipitation reaction；After reaction completely solid-oxide fuel battery electrolyte material nanometer lanthanum molybdate is obtained through post processing.The method of the synthesis of solid oxide fuel battery electrolyte material nanometer lanthanum molybdate of the present invention, it has, and simple and easy, safe and reliable, production cost is low, yield is high, the advantages that suitable for industrialized production.Meanwhile the nanometer lanthanum molybdate subglobular of synthesis, shaping and sintering in easy subsequent technique, the defects of product is unfavorable for electrolyte later stage preparation technology is prepared so as to overcome existing part.

Description

A kind of method of synthesis of solid oxide fuel battery electrolyte material nanometer lanthanum molybdate
Technical field
The present invention relates to solid-oxide fuel battery electrolyte material manufacturing technology field, more particularly to a kind of synthesis is solid The method of oxide body fuel battery electrolyte material nanometer lanthanum molybdate.
Background technology
SOFC (Solid oxide fuel cells, SOFC) be it is a kind of directly can be by fuel gas Chemical energy in body is converted into the reaction unit of electric energy, because it has structure of whole solid state, corrosion-free, No leakage, without expensive Metallic catalyst, it is environment-friendly, capacity usage ratio is high the advantages that, so as to cause extensive concern.Requirements of the SOFC to operating temperature The ionic conductivity of dielectric substrate is depended primarily on, traditional SOFC uses the zirconium oxide (YSZ) of stabilized with yttrium oxide as electrolyte Material, the SOFC using YSZ as electrolyte must be in 1000 DEG C or so work.It is high, close that high operating temperature brings such as cost Envelope is difficult, matches a series of problems, such as difficult with electrode material.Lanthanum molybdate (La2Mo2O9) electrolyte is because its electrical conductivity is high, former The advantages such as material price is cheap, sintering temperature is low are as one of SOFC hot-candidate material of electrolyte.At present, molybdic acid is prepared Lanthanum (La2Mo2O9) electrolyte mainly be made up of techniques such as high-temperature solid phase reaction method, hydrothermal synthesis methods.
Conventional high-temperature solid reaction process obtains preparation process often using lanthana and molybdenum oxide as raw material, is ground by mechanical mixture Mill, then through high-temperature roasting obtain target product however, high-temperature roasting products therefrom granularity is larger, product it is broken with disperseing Journey often brings numerous impurity and granularity uneven, brings difficulty to practical application, or even largely effect on solid oxide fuel The use quality and service life of battery.
China Patent Publication No. is that the A of CN 102502843 patent application text discloses a kind of microwave irradiation preparation The method of lanthanum molybdate nano tube material, using ammonium molybdate and lanthanum nitrate as raw material, using distilled water as solvent.Wherein, lanthanum molybdate nano The external diameter of tube material is 50~150 nanometers, wall thickness is 25~50 nanometers, consisting of La2MoO6And La2Mo4O15Mixed phase.It is mixed La in phase2Mo4O15It is relatively low to result in the purity of lanthanum molybdate product, and the material is not suitable as solid oxide fuel The electrolyte of battery.Meanwhile this is in hollow structure nanotube, can be unfavorable for electrolyte in later stage preparation technology (sintering), so as to cause its densification degree to be difficult to ensure that, and then there is the problem of ionic conductance is low.
China Patent Publication No. is that the A of CN 102502837 patent application text discloses a kind of lanthanum molybdate ultrathin nanometer The preparation method of sheet material, it uses cetyl trimethylammonium bromide assisted microwave synthesis radiotechnology to control the micro- of nano material Structure is seen, and is that initial reaction raw material, distilled water as solvent, cetyl trimethylammonium bromide are knot using ammonium molybdate and lanthanum nitrate Structure directed agents.The surface of synthesized ultrathin lanthanum molybdate nano sheet material is smooth, crystallinity is high, and thickness is only 5~15 nanometers, and Products therefrom specific surface area is big, and flocks together to form 3 D stereo network structure each other.This molybdenum in ultrathin nanometer piece Sour lanthanum material, which is easily caused in electrolyte subsequent machining technology, is difficult to dry-pressing or flow casting molding, so as to electrolyte Processing brings the problem of new.
The content of the invention
The purpose of the present invention is to propose to a kind of side of synthesis of solid oxide fuel battery electrolyte material nanometer lanthanum molybdate Method, to overcome the defects of prior art, the nanometer lanthanum molybdate subglobular of synthesis, shaping and burning in easy subsequent technique Knot.
To realize the purpose, present invention employs following technical scheme：
A kind of method of synthesis of solid oxide fuel battery electrolyte material nanometer lanthanum molybdate, by ammonium molybdate aqueous solution and It is placed in after lanthanum nitrate aqueous solution mixing in reactor and adds precipitating reagent and carries out hydrothermal homogeneous precipitation reaction, reaction temperature 200 ~300 DEG C, the reaction time is 10~24h, ammonium molybdate aqueous solution, the molar concentration of lanthanum nitrate aqueous solution be followed successively by 0.005~ 0.08mol/L, 0.15~4mol/L, the volume ratio between ammonium molybdate aqueous solution and lanthanum nitrate aqueous solution are 1~50：1；React Quan Houjing post-processes to obtain solid-oxide fuel battery electrolyte material nanometer lanthanum molybdate.
Preferably, precipitating reagent is one or both of ammoniacal liquor, sodium hydroxide, potassium hydroxide, urea, ammonium hydrogencarbonate. Mol ratio between precipitating reagent and lanthanum nitrate is 10~50：1.Precipitating reagent is added into reactor using form is slowly added dropwise, 1~2h of strong stirring after addition.
As a further improvement, reactor is placed in constant temperature blast drying oven and carried out by hydrothermal homogeneous precipitation reaction. Post processing is by reaction product separation of solid and liquid, washs and be placed in thermostatic drying chamber and be dried, and drying temperature is 20~60 DEG C, drying time is 3~10h.
The method of the synthesis of solid oxide fuel battery electrolyte material nanometer lanthanum molybdate of the present invention, is mainly solved existing Impurity of the high-temperature solid phase reaction method through high-temperature roasting and broken dispersion train is more, and performance particle diameter is big, and quality is unstable etc. Problem.Hydrothermal homogeneous precipitation one-step method provided by the present invention prepares lanthanum molybdate nano material, and it has simple and easy, safety can Lean on, production cost is low, yield is high, the advantages that suitable for industrialized production.Meanwhile the nanometer lanthanum molybdate subglobular of synthesis, easily Shaping and sintering in subsequent technique, so as to overcome the preparation production present in the A of the CN 102502843 and A of CN 102502837 Thing is unfavorable for the defects of electrolyte later stage preparation technology.
Brief description of the drawings
Fig. 1 is the XRD of the products therefrom of embodiment 1.
Fig. 2 is that the TEM of the products therefrom of embodiment 1 schemes.
Fig. 3 is the XRD of the products therefrom of embodiment 2.
Fig. 4 is that the TEM of the products therefrom of embodiment 2 schemes.
Embodiment
The synthesis of solid oxide fuel battery electrolyte of the present invention is further described below by way of specific embodiment The method of material nano lanthanum molybdate.
Embodiment 1
The synthesis of solid-oxide fuel battery electrolyte material nanometer lanthanum molybdate：
Weigh 1.236g ammonium molybdate [(NH4)6Mo7O24·4H2O] and 3.031g lanthanum nitrate [La (NO3)3·6H2O], Both are dissolved in 100mL and 35mL distilled water respectively, it is the uniform of 0.01mol/L and 0.20mol/L that stirring, which forms concentration, Solution, it is transferred to after two kinds of solution are mixed in the reactor that volume is 200mL, ammoniacal liquor is slowly added dropwise, and (addition is according to precipitation Mol ratio between agent and lanthanum nitrate is 18：1), sealed after strong stirring 2h, reactor is placed in constant temperature blast drying oven and heated To 250 DEG C insulation 15h, stop heating naturally cooling to room temperature, by product it is filtered, washing, drying (50 DEG C, 3h), consolidate Oxide body fuel battery electrolyte material lanthanum molybdate (La2Mo2O9) nano-powder.
Fig. 1 is the XRD spectrum of the products therefrom of embodiment 1.Its compared with standard card JCPDS No.23-1145 understand, Have at 21.4 °, 24.8 °, 27.9 °, 30.5 °, 37.5 °, 41.8 °, 47.5 °, 51.0 °, 52.6 °, 54.2 °, 55.9 °, 59.0 ° Diffraction maximum occur, respectively correspond to (111), (200), (210), (211), (300), (311), (321), (400), (410), (330), (331), (421) crystal face, it is Emission in Cubic La to show product2Mo2O9, product purity is higher.According to diffraction maximum (210) number La is calculated according to using Scherrer formula2Mo2O9The average grain size of powder is 23nm.
Fig. 2 is that the TEM of the products therefrom of embodiment 1 schemes, as shown in Figure 2, resulting lanthanum molybdate (La2Mo2O9) nano-powder Subglobular, its pattern is homogeneous, and particle mean size is about 55nm, and good crystallinity.
Embodiment 2
The synthesis of solid-oxide fuel battery electrolyte material nanometer lanthanum molybdate：
Weigh 6.180g ammonium molybdate [(NH4)6Mo7O24·4H2O] and 15.155g lanthanum nitrate [La (NO3)3·6H2O], Both are dissolved in 100mL and 70mL distilled water respectively, it is the uniform of 0.05mol/L and 0.50mol/L that stirring, which forms concentration, Solution, it is transferred to after two kinds of solution are mixed in the reactor that volume is 250mL, sodium hydroxide solution (addition is slowly added dropwise It is 20 according to the mol ratio between precipitating reagent and lanthanum nitrate：1), sealed after strong stirring 2h, reactor is placed in constant temperature forced air drying Be heated in case 300 DEG C insulation 20h, stop heating naturally cooling to room temperature, by product it is filtered, washing, drying (40 DEG C, 5h), solid-oxide fuel battery electrolyte material lanthanum molybdate (La is obtained2Mo2O9) nano-powder.
Fig. 3 is the XRD spectrum of the products therefrom of embodiment 2.Its compared with standard card JCPDS No.23-1145 understand, 21.4 °, 24.9 °, 27.9 °, 30.6 °, 37.5 °, 41.8 °, 47.5 °, 51.0 °, 52.6 °, 54.2 °, 55.9 °, 59.0 °, 66.5 °, 68.1 °, have diffraction maximum appearance at 70.7, correspond to respectively (111), (200), (210), (211), (300), (311), (321), (400), (410), (330), (331), (421), (510), (511), (521) crystal face, it is Emission in Cubic to show product La2Mo2O9, product purity is higher.La is calculated using Scherrer formula according to diffraction maximum (210) data2Mo2O9Powder Average grain size is 30nm.
Fig. 4 is that the TEM of the products therefrom of embodiment 2 schemes, as shown in Figure 4, resulting lanthanum molybdate (La2Mo2O9) nano-powder Subglobular, its pattern is homogeneous, and particle mean size is about 100nm, and good crystallinity.
Embodiment 3
Weigh 6.180g ammonium molybdate [(NH4)6Mo7O24·4H2O] and 43.304g lanthanum nitrate [La (NO3)3·6H2O], Both are dissolved in 100mL and 50mL distilled water respectively, it is the uniform molten of 0.05mol/L and 2mol/L that stirring, which forms concentration, Liquid, volume is transferred to as in 200mL reactor, urea is slowly added dropwise after mixing by two kinds of solution and (use dropwise addition form to mix) (addition is 30 according to the mol ratio between precipitating reagent and lanthanum nitrate to solution：1), sealed after strong stirring 1h, reactor is placed in Be heated in constant temperature blast drying oven 200 DEG C insulation 24h, stop heating naturally cooling to room temperature, by product it is filtered, washing, Dry (30 DEG C, 8h), obtain solid-oxide fuel battery electrolyte material lanthanum molybdate (La2Mo2O9) nano-powder.
It is pointed out that the present invention is not limited only to embodiment listed above, it is every can be direct from present invention Export or enlightenment, which join conceivable correlation technique, all should belong to the scope that the present invention covers protection.

Claims (1)

  1. A kind of 1. method of synthesis of solid oxide fuel battery electrolyte material nanometer lanthanum molybdate, it is characterised in that：By molybdic acid It is placed in after aqueous ammonium and lanthanum nitrate aqueous solution mixing in reactor and adds precipitating reagent and carries out hydrothermal homogeneous precipitation reaction, reaction Temperature is 200~300 DEG C, and the reaction time is 10~24h, and ammonium molybdate aqueous solution, the molar concentration of lanthanum nitrate aqueous solution are followed successively by 0.005~0.08mol/L, 0.15~4mol/L, the volume ratio between ammonium molybdate aqueous solution and lanthanum nitrate aqueous solution are 1~50： 1；After reaction completely solid-oxide fuel battery electrolyte material nanometer lanthanum molybdate is obtained through post processing；
    Precipitating reagent is ammoniacal liquor, sodium hydroxide, potassium hydroxide, urea, one or both of ammonium hydrogencarbonate, precipitating reagent and lanthanum nitrate Between mol ratio be 10~50：1；Precipitating reagent is added into reactor using form is slowly added dropwise, strong stirring 1 after addition ~2h；
    Reactor is placed in constant temperature blast drying oven by hydrothermal homogeneous precipitation reaction to be carried out；
    Post processing is by reaction product separation of solid and liquid, washs and be placed in thermostatic drying chamber and be dried, drying temperature 20 ~60 DEG C, drying time is 3~10h.
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CN109942293B (en) * 2019-03-21 2021-04-16 合肥学院 Method for preparing LMO-YSZ composite solid electrolyte by microwave combustion-supporting method
CN117941101A (en) * 2022-06-08 2024-04-26 宁德时代新能源科技股份有限公司 Positive electrode active material, preparation method thereof, pole piece, secondary battery and power utilization device
CN116443932A (en) * 2023-06-07 2023-07-18 武汉姜一三新材料科技有限公司 Preparation method of rare earth molybdate

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