CN108002421A - A kind of preparation method with fluorite type structure nano-powder - Google Patents
A kind of preparation method with fluorite type structure nano-powder Download PDFInfo
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- CN108002421A CN108002421A CN201711414299.5A CN201711414299A CN108002421A CN 108002421 A CN108002421 A CN 108002421A CN 201711414299 A CN201711414299 A CN 201711414299A CN 108002421 A CN108002421 A CN 108002421A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/30—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6
- C01F17/32—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6 oxide or hydroxide being the only anion, e.g. NaCeO2 or MgxCayEuO
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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Abstract
Metal-doped fluorite type structure nano-powder is prepared with cryogenic temperature freezing drying technology, including ZrO as template and fuel using nonionic surfactant the present invention relates to one kind2Base or CeO2Base oxide.The material is adapted to the fields such as solid oxide fuel cell, oxygen permeation membrane and photocatalysis.The technology dissolves nonionic surface active agent, transition metal and lanthanide metal nitrate, and by mixed solution cryogenic freezing, vacuum freezing drying dehydration obtains presoma.By presoma, pre-burning is carbonized in nitrogen, through 600 800 DEG C of calcinings, you can form powder.The powder has the features such as low reunion, extra specific surface area, very high sintering activity.The present invention can solve current ZrO2Base or CeO2Based ceramic powder body is difficult to the problem of sintering at a lower temperature, can make the sintering temperature of electrolyte reduce by 100 200 DEG C, is conducive to expand the co-sintering technology of solid oxide fuel cell.
Description
Technical field
The present invention relates to a kind of new technology of preparing with fluorite type structure nano-powder, including Y2O3、
Sc2O3Stablize ZrO2Or Y2O3、Sm2O3The CeO of doping2.The nano-powder prepared using the technology is conducive to fire in soild oxide
There is superior performance in the fields such as material battery, ferroelectric, ceramic oxygen-permeable membrane, photocatalysis.
Background technology
Fine and close oxygen ion conductor ceramic oxygen-permeable membrane, when film both sides are there are during partial pressure of oxygen under specific temperature conditions, oxonium ion
Conductor oxygen permeation membrane has permselective property to oxygen, continuously can separate ultra-high purity oxygen from air or other oxygen-containing atmospheres,
Or oxonium ion is migrated in film.By oxygen separation and aerobic industry（Selective oxidation and hydrogen production reaction such as low-carbon hydro carbons）
It is coupling in membrane reactor, can significantly simplifies running unit, reduces natural gas liquefaction（GTL）Cost of investment, has significantly exploitation
Advantage.Compact ceramic oxygen permeable membrane is widely used to field, the solids such as pure oxygen production, oxygen-enriched combusting power generation, membrane reactor at present
The fields such as oxide fuel battery electrolyte, ferroelectric, photocatalysis.The oxide of fluorite structure, cation are arranged with face-centered cubic
Row, anion（Oxonium ion）All tetrahedral interstices are occupied, this structure is a kind of open knot there are a large amount of octahedral voids
Structure, it is possible to achieve the quick diffusion of oxonium ion, is pure oxygen ion conductor.Current most widely used fluorite structure oxide includes
Y2O3、Sc2O3Adulterate ZrO2Or Y2O3、Sm2O3The CeO of doping2Deng.Such membrane material needs high temperature when in use, high keto sectional pressure,
Therefore membrane material should not only have higher Stable Oxygen infiltration rate, should also there is a higher mechanical strength, relatively low thermal coefficient of expansion,
Good creep resistance and chemical stability.Fine and close oxygen ion conductor ceramic oxygen-permeable membrane should also have stronger anti-gas to invade at the same time
Erosion ability.
ZrO at present2Base or CeO2Main problem existing for sill is that the temperature of such material sintering densification is up to 1400
More than DEG C, and easily occurs the defects of hole in sintering process.In order to reduce membrane material sintering temperature, it is necessary to control initial
The features such as the particle diameter of powder, pattern.Y2O3、Sc2O3Adulterate ZrO2Or Y2O3、Sm2O3The CeO of doping2Mainly using solid phase method, molten
It is prepared by glue-gel method.The powder granule prepared using solid phase method is larger, occurs very big sintering crystal grain after high temperature sintering, and
And easily there is hole.The diameter of particle prepared using wet chemistry method such as sol-gel process is substantially reduced, and improves the burning of material
Tie performance.The invention provides a kind of new powder preparation method, the powder prepared using the invention has low reunion, super large
The features such as specific surface area, very high sintering activity.The present invention can solve current ZrO2Base or CeO2Based ceramic powder body is compared with low temperature
The problem of being difficult to sintering under degree, compared with business powder, can make the sintering temperature of electrolyte reduce 100-200 DEG C, save
The energy.The technology is applied to field of solid oxide fuel at the same time, the reduction of electrolyte sintering temperature can be made, be conducive to
Further expand the application of the co-sintering technology of solid oxide fuel cell.The nano-powder of the Technique Popularizing is conducive at the same time
There is superior performance in fields such as ferroelectric, ceramic oxygen-permeable membrane, photocatalysis.
The content of the invention
The purpose of the present invention is exactly to use a kind of new nano-powder technology of preparing, and preparation has fluorite type structure nanometer
Powder.Powder prepared by the technology can solve current ZrO2Base or CeO2Based ceramic powder body is difficult to what is sintered at a lower temperature
Problem, compared with business powder, powder prepared by the present invention can drop the sintering temperature of fine and close oxygen ion conductor ceramics oxygen flow
Low 100-200 DEG C, be conducive to save the energy.
The purpose of the present invention is what is be achieved through the following technical solutions：
1. preferred above-mentioned nano-powder is a kind of metal-doped fluorite type structure ZrO2Base or CeO2The base nano-powder material
Suitable for fields such as solid oxide fuel cell, ferroelectric, ceramic oxygen-permeable membrane, photocatalysis.
2. ZrO in the present invention2The general structure of original washing powder body is NxZr1-xO2-δ, CeO2The general structure of original washing powder body is
MxCe1-xO2-δ, wherein M, N is the one or more of transition metal or lanthanide metal ion, 0≤x≤1,0≤δ≤1.
3. surfactant polyoxyethylene polyoxypropylene ether block copolymers or polyvinylpyrrolidone are placed in water,
When stirring 4~12 is small, surface-active solvent swell is set to form micro- micellar solution.And by target product NxZr1-xO2-δOr MxCe1-xO2-δ
According to the element ratio of chemical formula, the metal nitrate for weighing stoichiometric ratio respectively is dissolved in above-mentioned surfactant solution
In.
4. the polyester film surface that mixed solution is poured over to -20~-70 DEG C of superfreeze freezes, then it is transferred to super
Dry obtained presoma in low-temperature freeze-drying machine.
5. above-mentioned presoma is placed in 200 DEG C~600 DEG C carbonizations of nitrogen atmosphere stove, then in air atmosphere 600~800
DEG C calcining, you can obtain fluorite type structure nano-powder.
Preferably, the surfactant uses polyoxyethylene poly-oxygen propylene aether block copolymer P123
（EO20PO70EO20）、F127（ EO106PO70EO106）Or F88（EO100PO39EO100）And polyvinylpyrrolidone（PVP）In one
Kind is several, and the mass concentration of nonionic surfactant is 1%-10%.
Preferably, the fluorite type structure ZrO2Base or CeO2Base is Y2O3、Sc2O3Adulterate ZrO2Or Y2O3、Sm2O3Doping
CeO2。
Preferably, powder of the invention is applicable to solid oxide fuel cell, ferroelectric, ceramic oxygen-permeable membrane, light and urges
The fields such as change.
Compared with prior art, the present invention has the advantages that：
Small with powder granule using fluorite nano-powder prepared by method provided by the invention, diameter of particle narrowly distributing, compares table
The advantages that area is big, good dispersion, powder pure no dephasign.The powder has very high sintering activity, can be by powder sintering
Densification temperature reduces by 100~200 DEG C, and the co-sintering for being conducive to such material and other materials uses, and has expanded making for material
Use scope.Electrolyte using powder prepared by this method as solid oxide fuel cell, prepares with conventional method
Material is compared, and this material lowers the sintering temperature of electrolyte, is conducive to expand solid-oxide fuel battery electrolyte and electricity
The application of pole co-sintering technology.
Brief description of the drawings
Fig. 1 is Sm in the embodiment of the present invention 10.2Ce0.8O2-δThe X ray diffracting spectrum of powder.
Fig. 2 is Sm in the embodiment of the present invention 10.2Ce0.8O2-δThe scanning electron microscope (SEM) photograph of powder.
Fig. 3 is Sm in the embodiment of the present invention 10.2Ce0.8O2-δThrough going through 1300 degree of calcinings 4 after powder is tabletted in grinding tool
The sectional view of hour.
Fig. 4 is Gd in the embodiment of the present invention 20.1Ce0.9O2-δThe X ray diffracting spectrum of powder.
Fig. 5 is Sm in the embodiment of the present invention 30.1Ce0.9O2-δThe X ray diffracting spectrum of powder.
Embodiment
Embodiment 1：Sm0.2Ce0.8O2-δThe preparation of powder.
By Sm0.2Ce0.8O2-δThe element ratio of chemical formula, weighs the Sm (NO of stoichiometric ratio respectively3)3·6H2O and Ce
(NH4)2(NO3)6It is dissolved in a small amount of ionized water, is configured to solution A.By surfactant polyoxyethylene polyethenoxy ether block
Copolymer F127 is placed in deionized water, and 40 DEG C of heating stirrings make surface-active solvent swell form micro- micellar solution.It is molten to form B
Liquid.Will solution A add B solution in stirring reaction 24 it is small when, wherein wherein metal ion：F127=1：1~2.
Mixed solution is poured on polyester film, is placed in superfreeze refrigerator and freezes, cryogenic temperature is (- 30 DEG C)
~(-70℃).Then frozen samples are transferred to progress low-temperature vacuum drying dehydration in ultra low temperature vacuum freeze drying box, obtained
Presoma.Above-mentioned presoma is placed in atmosphere furnace in 600 DEG C of carbonizations in nitrogen, is then transferred to the presoma of carbonization general
Logical Muffle furnace is in 800 DEG C of calcinings, you can forms the Sm with extra specific surface area0.2Ce0.8O2-δPowder.It is prepared by attached drawing 1
Sm0.2Ce0.8O2-δX ray diffracting spectrum of the powder at 600 DEG C, 700 DEG C and 800 DEG C.Fig. 2 is in the embodiment of the present invention 1
Sm0.2Ce0.8O2-δThe scanning electron microscope (SEM) photograph of powder.Fig. 3 is Sm in the embodiment of the present invention 10.2Ce0.8O2-δPowder is pressed into grinding tool
Through going through 1300 DEG C of sectional views for calcining hour after piece.
Embodiment 2：Gd0.2Ce0.8O2-δThe preparation of powder
By Gd0.2Ce0.8O2-δThe element ratio of chemical formula, weighs the Gd (NO of stoichiometric ratio respectively3)3·6H2O and Ce (NH4)2
(NO3)6It is dissolved in a small amount of ionized water, is configured to solution A.By surfactant polyoxyethylene polyoxypropylene ether block copolymers
P123 is placed in deionized water, and room temperature heating stirring makes surface-active solvent swell form micro- micellar solution.Form B solution.A is molten
When stirring reaction 24 is small in liquid addition B solution, wherein wherein metal ion：F127=1：1~2.
Mixed solution is poured on polyester film, is placed in superfreeze refrigerator and freezes, cryogenic temperature is (- 30 DEG C)
~(-70℃).Then frozen samples are transferred to progress low-temperature vacuum drying dehydration in ultra low temperature vacuum freeze drying box, obtained
Presoma.Above-mentioned presoma is placed in atmosphere furnace in 600 DEG C of carbonizations in nitrogen, is then transferred to the presoma of carbonization general
Logical Muffle furnace is in 800 DEG C of calcinings, you can forms the Sm with extra specific surface area0.2Ce0.8O2-δPowder.It is prepared by attached drawing 4
Gd0.2Ce0.8O2-δThe X ray diffracting spectrum of powder.
Embodiment 3：Sm0.1Ce0.9O2-δThe preparation of powder.
By Sm0.1Ce0.9O2-δThe element ratio of chemical formula, weighs the Sm (NO of stoichiometric ratio respectively3)3·6H2O and Ce
(NH4)2(NO3)6It is dissolved in a small amount of ionized water, is configured to solution A.By surfactant polyoxyethylene polyethenoxy ether block
Copolymer F127 is placed in deionized water, and 40 DEG C of heating stirrings make surface-active solvent swell form micro- micellar solution.It is molten to form B
Liquid.Will solution A add B solution in stirring reaction 24 it is small when, wherein wherein metal ion：F127=1：1~2.
Mixed solution is poured on polyester film, is placed in superfreeze refrigerator and freezes, cryogenic temperature is (- 30 DEG C)
~(-70℃).Then frozen samples are transferred to progress low-temperature vacuum drying dehydration in ultra low temperature vacuum freeze drying box, obtained
Presoma.Above-mentioned presoma is placed in atmosphere furnace in 600 DEG C of carbonizations in nitrogen, is then transferred to the presoma of carbonization general
Logical Muffle furnace is in 800 DEG C of calcinings, you can forms the Sm with extra specific surface area0.2Ce0.8O2-δPowder.It is prepared by attached drawing 5
Sm0.1Ce0.9O2-δThe X ray diffracting spectrum of powder.
The specific embodiment of the present invention is described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring the substantive content of the present invention.
Claims (6)
1. one kind, as template and fuel, is mixed using nonionic surfactant even if preparing metal with cryogenic temperature freezing drying
Miscellaneous fluorite type structure ZrO2Base or CeO2The preparation method of base nano ceramic powder body material；The material is adapted to soild oxide
The application of electrolyte, oxygen permeation membrane and the photocatalysis field of fuel cell etc..
2. application according to claim 1, it is characterised in that the CeO2The general structure of the nano-ceramic powder of base is
MxCe1-xO2-δ, wherein M is the one or more of transition metal or lanthanide metal ion, 0≤x≤1,0≤δ≤1.
3. application according to claim 1, it is characterised in that the ZrO2The general structure of the nano-ceramic powder of base is
NxZr1-xO2-δ, wherein N be transition metal ions one or more, 0≤x≤1,0≤δ≤1.
4. according to claim 1, the metal-nitrate solutions of dissolving will be mixed with nonionic surfactant solution, wherein it is non-from
Sub- surfactant uses polyoxyethylene poly-oxygen propylene aether block copolymer P123（EO20PO70EO20）、F127（
EO106PO70EO106）Or F88（EO100PO39EO100）, polyvinylpyrrolidone（PVP）In one or more, non-ionic surface
The mass concentration of activating agent is 1%-10%.
5. according to claim 1, the mixed solution in above-mentioned 4 needs to be poured over the polyester film of -20~-70 DEG C of superfreeze
Freezing, is then transferred in cryogenic temperature freezing drying machine dry obtained presoma.
6. according to the method described in claim 1, above-mentioned presoma is placed in 200 DEG C ~ 600 DEG C carbonizations of nitrogen atmosphere stove, then
In 600~800 DEG C of calcinings of air atmosphere, you can obtain fluorite type structure nano-powder.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110156487A (en) * | 2019-05-20 | 2019-08-23 | 陈松 | A kind of preparation method of oxygen permeation membrane |
| CN112490475A (en) * | 2020-10-28 | 2021-03-12 | 西安交通大学 | Method for synthesizing electrolyte powder based on complexation-freeze drying method and obtained electrolyte powder |
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Cited By (2)
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Application publication date: 20180508 |