CN101552344A - Method for preparing composite oxides mischcrystal jelly glue with gadolinium oxide adulterating cerium oxide - Google Patents

Method for preparing composite oxides mischcrystal jelly glue with gadolinium oxide adulterating cerium oxide Download PDF

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CN101552344A
CN101552344A CNA2009100620018A CN200910062001A CN101552344A CN 101552344 A CN101552344 A CN 101552344A CN A2009100620018 A CNA2009100620018 A CN A2009100620018A CN 200910062001 A CN200910062001 A CN 200910062001A CN 101552344 A CN101552344 A CN 101552344A
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gadolinium
acetylacetone
oxide
pentanedione
hydrate
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CN101552344B (en
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沈春晖
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Wuhan University of Technology WUT
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    • 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

Abstract

The present invention relates to a method for preparing composite oxides mischcrystal jelly glue with gadolinium oxide adulterating cerium oxide. The method has characteristics of including steps as follows: (1) selecting raw material: weighing each raw material by weight part as follows: acetylacetone cerium aqua compound 1.5-2.5, acetylacetone gadolinium aqua compound 0.35-0.45, methanol 20-30, N, N-dimethylformamide 0.3-0.5; (2) mixing in room temperature and stirring 40-60 minutes, obtaining the colloidal solution; (3) gelating the colloidal solution in 45-70 DEG C and dehydrating dealcoholize 8-30 hours; (4) when the colloidal solution becomes viscous, the gelating reaction continues 40-60 minutes for obtaining jelly glue; (5) displacing the jelly glue to a vacuum drying case, vacuum drying 1-2 hours in 130 DEG C, and obtaining the composite oxides mischcrystal jelly glue with gadolinium oxide adulterating cerium oxide. The product has high denseness and low jelly glue porosity which is benefit for low temperature sintering into a gadolinium oxide adulterating cerium oxide electrolytes film with compact and high density.

Description

A kind of preparation method of composite oxide solid solution gel of gadolinium oxide doped cerium oxide
Technical field
The present invention relates to contain the preparation method of the composite oxide solid solution gel of gadolinium, cerium.This type of composite oxide solid solution gel can be used for the electrolyte of Solid Oxide Fuel Cell.
Background technology
Multinomial premium properties such as cerium oxide is a kind of important compound in the rare earth family,, carried metal decentralization height good with its storage oxygen performance and getting most of the attention.The conductivity of pure zirconia cerium is not high, and the ionic conductivity in the time of 600 ℃ has only 10 -5S/cm.But after mixing, its oxygen ionic conductivity can improve greatly.Gadolinium oxide doped cerium oxide (gadolinia doped ceria, GDC) under middle temperature (500～700 ℃) ionic conductivity than the traditional electrolyte oxidation of Solid Oxide Fuel Cell according to stable high 1～2 order of magnitude of zirconia (YSZ), desirable in, the low-temperature solid oxide fuel cell electrolyte.The dielectric substrate of Solid Oxide Fuel Cell (SOFC) is to have fine and close micro-structural to guarantee the air-tightness of battery to the primary requirement of material, at present, the greatest difficulty of preparation cerium base SOFC is that cerium oxide is a kind of material than hard-to-sinter, densification temperature is higher, and the micron order cerium oxide powder of conventional method preparation could realized complete densification more than 1500 ℃.For fear of a series of problems such as chemical incompatibility, thermal expansion mismatch between the too high caused battery component of densification sintering temperature, require the cerium oxide base electrolyte to realize the low temperature sintering, on the other hand, the dielectric substrate of preparation should have suitable thickness to be beneficial to reduce ohmic loss on the dielectric substrate.As seen, the doped cerium oxide electrolyte film of preparation low temperature densification sintering is one of difficult problem of exploitation cerium base SOFC.
Adopt the solid phase doping method to prepare the doped cerium oxide solid-solution material, though equipment and technology are simple, easy control of reaction conditions, cost is low, and is low in the pollution of the environment, but the purity of prepared powder body material can not get guaranteeing, particle size is bigger, particle size distribution inequality, doped chemical also have been difficult to the better chemical uniformity, and these shortcomings all will badly influence electrical property, sintering character and the mechanical performance of follow-up sintering body.In early days in the research, may be the influence of doped chemical because of the emphasis of research to electrical property, so mostly adopt the solid phase doping method, the emphasis that present stage is studied has been transferred to the employing liquid phase method, in the hope of obtaining the nanometer grade powder of uniform doping, and then improve electrical property, sintering character and the mechanical performance of material.Liquid phase method prepares the doped cerium oxide solid-solution material roughly hydro-thermal solvent method, sol-gel (sol-gel) method, glycine mononitrate method (GNP), coprecipitation and sluggish precipitation etc.These methods all are at first the calcining of reaction precursor body to be obtained the doped cerium oxide powder, again powder is dispersed in and is made into slurry in the solvent and prepares film with certain viscosity, the chance that reuniting appears in powder in this serial link directly becomes base much more with respect to powder, thereby the powder that causes having good sintering activity is unsatisfactory by the sintering character of above method film forming rear film, the fine and close doped cerium oxide electrolyte film of the preparation difficulty that becomes in the porous electrode substrate.
When adopting sol-gel (sol-gel) legal system to be equipped with gadolinium oxide doped cerium oxide solid solution, mostly select for use gadolinium nitrate, cerous nitrate or their alkoxide compound as precursor, because their reactivities are too high just to have occurred precipitation when causing hydrolysis and polymerization reaction just to begin, what obtain at last remains nanometer grade powder.When preparation solid-oxide fuel battery electrolyte film, also difficulty is avoided the problems referred to above.
Summary of the invention
The preparation method who the purpose of this invention is to provide the composite oxide solid solution gel of kind of gadolinium oxide doped cerium oxide, the composite oxide solid solution gel of this method preparation has highdensity characteristics.
To achieve these goals, technical scheme of the present invention is: a kind of preparation method of composite oxide solid solution gel of gadolinium oxide doped cerium oxide is characterized in that it comprises the steps:
1) choosing of raw material: each raw material is according to following parts by weight weighing:
Acetylacetone,2,4-pentanedione cerium hydrate 1.5-2.5
Acetylacetone,2,4-pentanedione gadolinium hydrate 0.35-0.45,
Methyl alcohol 20-30,
N, dinethylformamide 0.3-0.5;
2) in being housed, the there-necked flask of electromagnetic agitation adds acetylacetone,2,4-pentanedione cerium hydrate, acetylacetone,2,4-pentanedione gadolinium hydrate, methyl alcohol and N, dinethylformamide, stirring at room 1-2 hour;
3) will stablize limpid sol solution and pour in the glass culture dish, put into baking oven after covering the culture dish lid, 45-70 ℃ of gelation dehydration dealcoholysis 8-30 hour;
4) when sol solution becomes thickness, remove the culture dish lid, continued gelation reaction 40-60 minute, obtain not having the gel of macroscopic cracking;
5) gel that will not have a macroscopic cracking is transferred to vacuum drying chamber, at 130 ℃ of vacuumize 1-2 hours, obtains the composite oxide solid solution gel of gadolinium oxide doped cerium oxide.
Described raw material comprises deionized water, and shared parts by weight are: deionized water 0.2-0.4; Deionized water is in step 2) add acetylacetone,2,4-pentanedione cerium hydrate, acetylacetone,2,4-pentanedione gadolinium hydrate, methyl alcohol and N, in the dinethylformamide.
The chemical expression of described acetylacetone,2,4-pentanedione cerium hydrate is: Ce (CH 3COCHCOCH 3) 3XH 2O, x=3-4 (comprising any number between 3 and 4).
The chemical expression of described acetylacetone,2,4-pentanedione gadolinium hydrate is: Gd (CH 3COCHCOCH 3) 3XH 2O, x=3-4 (comprising any number between 3 and 4).
It is pure that described methyl alcohol, N, dinethylformamide are analysis, and purity is greater than 98wt%.
The present invention and existing method relatively have following advantage:
1) the present invention adopts the acetylacetone,2,4-pentanedione cerium hydrate with low in hydrolysis activity, acetylacetone,2,4-pentanedione gadolinium hydrate is as the precursor of sol-gel, can make have high density and the composite oxide solid solution gel of gadolinium oxide doped cerium oxide, rather than powder, the preparation of mischcrystal jelly and film forming can disposablely be finished, avoided the two-step film forming that needs of powder-product, thereby improved the sintering activity of mischcrystal jelly, therefore, the present invention has overcome the too high problem of sintering temperature when preparing fine and close gadolinium oxide doped cerium oxide electrolyte film in the porous electrode substrate.
The composite oxide solid solution gel of the gadolinium oxide doped cerium oxide of this method preparation, density height, gel porosity are low, and this helps low-temperature sintering and becomes fine and close, highdensity GDC dielectric film.
2) preparation technology of the present invention is simple, reaction temperature low (45-70 ℃), the little [surface area (m of product specific surface 2/ g): 1.08-1.86].
Embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to the following examples.
Embodiment 1:
A kind of preparation method of composite oxide solid solution gel of gadolinium oxide doped cerium oxide, it comprises the steps:
1) choosing of raw material: each raw material is according to following weight weighing: acetylacetone,2,4-pentanedione cerium hydrate [Ce (CH 3COCHCOCH 3) 33H 2O] 1.554g, acetylacetone,2,4-pentanedione gadolinium hydrate [Gd (CH 3COCHCOCH 3) 33H 2O] 0.355g, methyl alcohol 25.37g, N, dinethylformamide 0.415g; Described methyl alcohol, N, dinethylformamide is pure for analyzing, and purity is greater than 98wt%;
2) in being housed, the there-necked flask of electromagnetic agitation adds acetylacetone,2,4-pentanedione cerium hydrate [Ce (CH 3COCHCOCH 3) 33H 2O], acetylacetone,2,4-pentanedione gadolinium hydrate [Gd (CH 3COCHCOCH 3) 33H 2O], methyl alcohol and N, dinethylformamide, 1.5 hours (not adding deionized water) of stirring at room;
3) will stablize limpid sol solution and pour in the glass culture dish, put into baking oven after covering the culture dish lid, 68 ℃ of gelations dehydration dealcoholysis 24 hours;
4) when sol solution becomes thickness, remove the culture dish lid, continue gelation reaction 50 minutes (68 ℃ of reaction temperatures), obtain not having the gel of macroscopic cracking;
5) gel that will not have a macroscopic cracking is transferred to vacuum drying chamber, 130 ℃ of vacuumizes 1.5 hours, obtains the composite oxide solid solution gel of gadolinium oxide doped cerium oxide.
The basic physical property test result such as the table 1 of the composite oxide solid solution gel of the gadolinium oxide doped cerium oxide that obtains.
Embodiment 2:
The preparation method is with embodiment 1, only the step 2 of embodiment 1) in the deionized water that do not add be replaced by and add deionized water 0.315g.Its basic physical property test result such as table 1.
Embodiment 3:
A kind of preparation method of composite oxide solid solution gel of gadolinium oxide doped cerium oxide, it comprises the steps:
1) choosing of raw material: each raw material is according to following weight weighing: acetylacetone,2,4-pentanedione cerium hydrate [Ce (CH 3COCHCOCH 3) 33H 2O] 1.554g, acetylacetone,2,4-pentanedione gadolinium hydrate [Gd (CH 3COCHCOCH 3) 33H 2O] 0.355g, methyl alcohol 25.37g, N, dinethylformamide 0.415g, deionized water 0.315g; Described methyl alcohol, N, dinethylformamide is pure for analyzing, and purity is greater than 98wt%;
2) in being housed, the there-necked flask of electromagnetic agitation adds acetylacetone,2,4-pentanedione cerium hydrate [Ce (CH 3COCHCOCH 3) 33H 2O], acetylacetone,2,4-pentanedione gadolinium hydrate [Gd (CH 3COCHCOCH 3) 33H 2O], methyl alcohol and N, dinethylformamide added the deionized water stirring at room 1 hour;
3) will stablize limpid sol solution and pour in the glass culture dish, put into baking oven after covering the culture dish lid, 65 ℃ of gelations dehydration dealcoholysis 24 hours;
4) when sol solution becomes thickness, remove the culture dish lid, continue gelation reaction 40 minutes (65 ℃ of reaction temperatures), obtain not having the gel of macroscopic cracking;
5) gel that will not have a macroscopic cracking is transferred to vacuum drying chamber, 130 ℃ of vacuumizes 1 hour, obtains the composite oxide solid solution gel of gadolinium oxide doped cerium oxide.The basic physical property test result such as the table 1 of the composite oxide solid solution gel of gadolinium oxide doped cerium oxide.
Embodiment 4:
A kind of preparation method of composite oxide solid solution gel of gadolinium oxide doped cerium oxide, it comprises the steps:
1) choosing of raw material: each raw material is according to following weight weighing: acetylacetone,2,4-pentanedione cerium hydrate [Ce (CH 3COCHCOCH 3) 34H 2O] 1.554g, acetylacetone,2,4-pentanedione gadolinium hydrate [Gd (CH 3COCHCOCH 3) 34H 2O] 0.355g, methyl alcohol 25.37g, N, dinethylformamide 0.415g; Described methyl alcohol, N, dinethylformamide is pure for analyzing, and purity is greater than 98wt%;
2) in being housed, the there-necked flask of electromagnetic agitation adds acetylacetone,2,4-pentanedione cerium hydrate [Ce (CH 3COCHCOCH 3) 34H 2O], acetylacetone,2,4-pentanedione gadolinium hydrate [Gd (CH 3COCHCOCH 3) 34H 2O], methyl alcohol and N, dinethylformamide did not add the deionized water stirring at room 2 hours;
3) will stablize limpid sol solution and pour in the glass culture dish, put into baking oven after covering the culture dish lid, 45-50 ℃ of gelation dehydration dealcoholysis 30 hours;
4) when sol solution becomes thickness, remove the culture dish lid, continue gelation reaction 60 minutes (reaction temperature 45-50 ℃), obtain not having the gel of macroscopic cracking;
5) gel that will not have a macroscopic cracking is transferred to vacuum drying chamber, 130 ℃ of vacuumizes 2 hours, obtains the composite oxide solid solution gel of gadolinium oxide doped cerium oxide.The basic physical property test result such as the table 1 of the composite oxide solid solution gel of gadolinium oxide doped cerium oxide.
Embodiment 5:
A kind of preparation method of composite oxide solid solution gel of gadolinium oxide doped cerium oxide, it comprises the steps:
1) choosing of raw material: each raw material is according to following parts by weight weighing: acetylacetone,2,4-pentanedione cerium hydrate [Ce (CH 3COCHCOCH 3) 34H 2O] 1.554g, acetylacetone,2,4-pentanedione gadolinium hydrate [Gd (CH 3COCHCOCH 3) 34H 2O] 0.355g, methyl alcohol 25.37g, N, dinethylformamide 0.415g; Described methyl alcohol, N, dinethylformamide is pure for analyzing, and purity is greater than 98wt%;
2) in being housed, the there-necked flask of electromagnetic agitation adds acetylacetone,2,4-pentanedione cerium hydrate [Ce (CH 3COCHCOCH 3) 34H 2O], acetylacetone,2,4-pentanedione gadolinium hydrate [Gd (CH 3COCHCOCH 3) 34H 2O], methyl alcohol and N, dinethylformamide did not add the deionized water stirring at room 1.2 hours;
3) will stablize limpid sol solution and pour in the glass culture dish, put into baking oven after covering the culture dish lid, 66 ℃ of gelations dehydration dealcoholysis 8 hours;
4) when sol solution becomes thickness, remove the culture dish lid, continue gelation reaction 45 minutes (66 ℃ of reaction temperatures), obtain not having the gel of macroscopic cracking;
5) gel that will not have a macroscopic cracking is transferred to vacuum drying chamber, 130 ℃ of vacuumizes 1.2 hours, obtains the composite oxide solid solution gel of gadolinium oxide doped cerium oxide.The basic physical property test result such as the table 1 of the composite oxide solid solution gel of gadolinium oxide doped cerium oxide.
Embodiment 6:
A kind of preparation method of composite oxide solid solution gel of gadolinium oxide doped cerium oxide, it comprises the steps:
1) choosing of raw material: each raw material is according to following weight weighing: acetylacetone,2,4-pentanedione cerium hydrate [Ce (CH 3COCHCOCH 3) 33H 2O] 1.5g, acetylacetone,2,4-pentanedione gadolinium hydrate [Gd (CH 3COCHCOCH 3) 33H 2O] 0.35g, methyl alcohol 20g, N, dinethylformamide 0.3g, deionized water 0.2g; It is pure that described methyl alcohol, N, dinethylformamide are analysis, and purity is greater than 98wt%;
2) add acetylacetone,2,4-pentanedione cerium hydrate, acetylacetone,2,4-pentanedione gadolinium hydrate, methyl alcohol and N in the there-necked flask of electromagnetic agitation is housed, dinethylformamide added the deionized water stirring at room 1 hour;
3) will stablize limpid sol solution and pour in the glass culture dish, put into baking oven after covering the culture dish lid, 65 ℃ of gelations dehydration dealcoholysis 24 hours;
4) when sol solution becomes thickness, remove the culture dish lid, continue gelation reaction 40 minutes (65 ℃ of reaction temperatures), obtain not having the gel of macroscopic cracking;
5) gel that will not have a macroscopic cracking is transferred to vacuum drying chamber, 130 ℃ of vacuumizes 1 hour, obtains the composite oxide solid solution gel of gadolinium oxide doped cerium oxide.
Embodiment 7:
A kind of preparation method of composite oxide solid solution gel of gadolinium oxide doped cerium oxide, it comprises the steps:
1) choosing of raw material: each raw material is according to following weight weighing: acetylacetone,2,4-pentanedione cerium hydrate [Ce (CH 3COCHCOCH 3) 34H 2O] 2.5g, acetylacetone,2,4-pentanedione gadolinium hydrate [Gd (CH 3COCHCOCH 3) 34H 2O] 0.45g, methyl alcohol 30g, N, dinethylformamide 0.5g deionized water 0.4g; It is pure that described methyl alcohol, N, dinethylformamide are analysis, and purity is greater than 98wt%;
2) add acetylacetone,2,4-pentanedione cerium hydrate, acetylacetone,2,4-pentanedione gadolinium hydrate, methyl alcohol and N in the there-necked flask of electromagnetic agitation is housed, dinethylformamide added the deionized water stirring at room 2 hours;
3) will stablize limpid sol solution and pour in the glass culture dish, put into baking oven after covering the culture dish lid, 70 ℃ of gelations dehydration dealcoholysis 24 hours;
4) when sol solution becomes thickness, remove the culture dish lid, continue gelation reaction 60 minutes (70 ℃ of reaction temperatures), obtain not having the gel of macroscopic cracking;
5) gel that will not have a macroscopic cracking is transferred to vacuum drying chamber, 130 ℃ of vacuumizes 2 hours, obtains the composite oxide solid solution gel of gadolinium oxide doped cerium oxide.
Table 1, the composite oxide solid solution gelling performance test result of gadolinium oxide doped cerium oxide
Figure A20091006200100071
As known from Table 1, the density (g/cm of the composite oxide solid solution gel of the gadolinium oxide doped cerium oxide of the present invention's preparation 3) be 5.97-6.93, have highdensity characteristics; Gel porosity low [gel mould pore volume (cc/g) is 0.0025-0.0096]; Characteristics with no macroscopic cracking.
The bound of each raw material of the present invention, interval value, and the bound of technological parameter (as temperature, time etc.), interval value can both realize the present invention, do not enumerate embodiment one by one at this.

Claims (5)

1. the preparation method of the composite oxide solid solution gel of a gadolinium oxide doped cerium oxide is characterized in that it comprises the steps:
1) choosing of raw material: each raw material is according to following parts by weight weighing:
Acetylacetone,2,4-pentanedione cerium hydrate 1.5-2.5
Acetylacetone,2,4-pentanedione gadolinium hydrate 0.35-0.45,
Methyl alcohol 20-30,
N, dinethylformamide 0.3-0.5;
2) in being housed, the there-necked flask of electromagnetic agitation adds acetylacetone,2,4-pentanedione cerium hydrate, acetylacetone,2,4-pentanedione gadolinium hydrate, methyl alcohol and N, dinethylformamide, stirring at room 1-2 hour;
3) will stablize limpid sol solution and pour in the glass culture dish, put into baking oven after covering the culture dish lid, 45-70 ℃ of gelation dehydration dealcoholysis 8-30 hour;
4) when sol solution becomes thickness, remove the culture dish lid, continued gelation reaction 4060 minutes, obtain not having the gel of macroscopic cracking;
5) gel that will not have a macroscopic cracking is transferred to vacuum drying chamber, at 130 ℃ of vacuumize 1-2 hours, obtains the composite oxide solid solution gel of gadolinium oxide doped cerium oxide.
2. the preparation method of the composite oxide solid solution gel of a kind of gadolinium oxide doped cerium oxide according to claim 1 is characterized in that: described raw material comprises deionized water, and shared parts by weight are: deionized water 0.2-0.4; Deionized water is in step 2) add acetylacetone,2,4-pentanedione cerium hydrate, acetylacetone,2,4-pentanedione gadolinium hydrate, methyl alcohol and N, in the dinethylformamide.
3. the preparation method of the composite oxide solid solution gel of a kind of gadolinium oxide doped cerium oxide according to claim 1 is characterized in that: the chemical expression of described acetylacetone,2,4-pentanedione cerium hydrate is: Ce (CH 3COCHCOCH 3) 3XH 2O, x=3-4.
4. the preparation method of the composite oxide solid solution gel of a kind of gadolinium oxide doped cerium oxide according to claim 1 is characterized in that: the chemical expression of described acetylacetone,2,4-pentanedione gadolinium hydrate is: Gd (CH 3COCHCOCH 3) 3XH 2O, x=3-4.
5. the preparation method of the composite oxide solid solution gel of a kind of gadolinium oxide doped cerium oxide according to claim 1 is characterized in that: it is pure that described methyl alcohol, N, dinethylformamide are analysis, and purity is greater than 98wt%.
CN2009100620018A 2009-05-05 2009-05-05 Method for preparing composite oxides mischcrystal jelly glue with gadolinium oxide adulterating cerium oxide Expired - Fee Related CN101552344B (en)

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