CN108550874A - A kind of cerium oxide-barium cerate base solid-oxide fuel battery electrolyte and preparation method - Google Patents
A kind of cerium oxide-barium cerate base solid-oxide fuel battery electrolyte and preparation method Download PDFInfo
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- 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
- H01M8/02—Details
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
- H01B1/08—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances oxides
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- 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
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- 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
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Abstract
The present invention relates to a kind of cerium oxide barium cerate base solid-oxide fuel battery electrolyte and preparation method, the main component of electrolyte is Ce0.8Bi x Re(0.2‑x)O2‑δ‑BaCe0.8Bi x Re(0.2‑x)O3‑δ(0≤x≤0.2), wherein Re are one kind in La, Nd, Eu, Gd, Dy, Er, Yb.Using solid reaction process single sintering Ce0.8Bi x Re(0.2‑x)O2‑δ‑BaCe0.8Bi x Re(0.2‑x)O3‑δComposite granule prepares composite electrolyte by granulation, compression moulding, high-temperature calcination.The electrolyte has the advantages that firing temperature is low and ionic conductivity is high, which has the advantages that be simple and efficient and be convenient for industrialization.
Description
Technical field
The present invention relates to the electrolyte fields of solid oxide fuel cell, and in particular to a kind of cerium oxide-barium cerate base
Solid-oxide fuel battery electrolyte and preparation method.
Background technology
Solid oxide fuel cell（SOFCs）Because energy transformation ratio is high, pollution-free and fuel diversity the advantages that due to
As the research hotspot of fuel cell field.Electrolyte is the key that SOFCs and core material.Currently, YSZ（Yttrium oxide doping
Zirconium oxide）It is to develop SOFCs electrolytes the most ripe.But, YSZ usually 1000 DEG C or more just have it is higher from
Electron conductivity, excessively high operating temperature bring a series of problems to SOFCs, such as：Electrode activity reduces, to metallic interconnection materials
It is required that it is high, cell sealing is bad etc..Therefore, the operating temperature for reducing SOFCs is to expand battery component material selection range and carry
The important development direction of high battery longtime running stability.But with the reduction of operating temperature, the conductivity of YSZ electrolyte
It is rapid to decline, cause battery performance to drastically reduce.It is current to develop novel intermediate temperature solid oxide fuel cell electrolyte
Focus on research direction.
Chinese patent document CN101000966 discloses " a kind of composite doped cerium oxide electrolyte and preparation method thereof ",
The composite doped cerium oxide electrolyte is to meet Ce1-xGdx-yYyO2-0.5xCerium oxide, gadolinium oxide and the yttrium oxide of stoichiometric ratio
Composite oxides, conductivity under 600 DEG C of air conditions is 0.038 Scm-1.Chinese patent document CN102544559A
" a kind of ceria-based electrolyte and preparation method thereof for solid oxide fuel cell " is disclosed, by cerium oxide
Middle addition lanthana, vanadium oxide reduce firing temperature, and conductivity of the electrolyte under 600 DEG C of air conditions is 0.0178
S·cm-1.But the Ce in ceria-based electrolyte4+It is easily partially reduced to Ce under low oxygen partial pressure or reducing atmosphere3+,
Electronic conductance is generated, causes the open-circuit voltage of SOFCs to decline, and then battery performance is caused to reduce.
Chinese patent document CN103086716A disclose " based on rare earth oxide adulterate barium cerate composite proton lead
Body material and preparation method thereof ", which is the barium cerate of gadolinium oxide or Yttrium oxide doping, under 550 DEG C of air conditions
Conductivity is higher than 10-2 S·cm-1.But barium cerate electrolyte is containing CO2、H2It is unstable under conditions of O, chemistry easily occurs
Reaction generates barium carbonate, barium hydroxide etc., and then conductivity is caused to decline.
Wenping Sun etc.（A novel electronic current-blocked stable mixed ionic
conductor for solid oxide fuel cells, Journal of Power Sources, 2011, 196(1):
62-68）Describe a kind of rare earth doped CeO2/BaCeO3Composite electrolyte realizes ceria-based electrolyte and barium cerate
The performance advantage of base electrolyte is complementary, solves ceria-based electrolyte and is easily partially reduced with barium cerate base electrolyte chemistry not
Stable problem.But the firing temperature of the composite electrolyte is higher（1350 DEG C of ＞）, boundary is easy to happen between two kinds of electrolyte
Face is reacted or elements diffusion, causes conductivity relatively low.
Invention content
The present invention is directed to deficiencies of the prior art, proposes a kind of Bi doping types Ce0.8Bi x Re(0.2-x)O2-δ-
BaCe0.8Bi x Re(0.2-x)O3-δ(0≤x≤0.2, Re=La, Nd, Eu, Gd, Dy, Er, Yb etc.) composite electrolyte and preparation method.
Prepared electrolyte has many advantages, such as that firing temperature is low, conductivity is high.The preparation method proposed have it is simple for process, be convenient for
The advantages of industrialization.
The present invention is achieved by the following technical solutions, includes the following steps.
1、Ce0.8Bi x Re(0.2-x)O2-δ-BaCe0.8Bi x Re(0.2-x)O3-δThe preparation method of composite granule is as described below.
1.1 press Ce0.8Bi x Re(0.2-x)O2-δ-BaCe0.8Bi x Re(0.2-x) O3-δStoichiometric ratio weighs BaCO3、CeO2、
Bi2O3、Re2O3(Re=La, Nd, Eu, Gd, Dy, Er, Yb etc.), is put into polyurethane ball-milling pot, and absolute ethyl alcohol is added, with oxidation
Zirconium ball is medium ball milling 8~12 hours, raw material, zirconia ball, absolute ethyl alcohol mass ratio be 1:(2.5~3.5):(0.8~
0.9) slurry, is obtained.
1.2 drying, are granulated, and the compression moulding under 5~15MPa pressure obtains green body.
Green body is put into heating furnace by 1.3, is warming up to 900~1050 DEG C, keeps the temperature 10~15 hours, then furnace cooling.
1.4 are crushed the block after calcining, obtain Ce0.8BixRe(0.2-x)O2-δ-Ba Ce0.8BixRe(0.2-x)O3-δIt is compound
Powder.
2、Ce0.8BixRe(0.2-x)O2-δ-Ba Ce0.8BixRe(0.2-x)O3-δThe preparation method of composite electrolyte is as described below.
2.1 to Ce0.8BixRe(0.2-x)O2-δ-Ba Ce0.8BixRe(0.2-x)O3-δ1 wt.% bondings are added in composite granule
Agent is uniformly mixed, and is granulated, and the sheet electrolyte green body that thickness is 0.3~1.5 mm is pressed under 30~60MPa pressure.
Electrolyte green body is put into heating furnace by 2.2, is warming up to 1100~1250 DEG C, is kept the temperature 2~6 hours, is obtained solid oxygen
Compound fuel-cell electrolyte.
Heretofore described material purity is more than 99.9%；The absolute ethyl alcohol is to analyze pure grade.
Ce in step 1.1 of the present invention0.8Bi x Re(0.2-x)O2-δAnd BaCe0.8Bi x Re(0.2-x) O3-δMass ratio be
(95~50):(5~50).
According to currently preferred, Ce in step 1.10.8Bi x Re(0.2-x)O2-δ-BaCe0.8Bi x Re(0.2-x) O3-δIn 0.05
≤x≤0.12。
Drying temperature is 80~100 DEG C in step 1.2 of the present invention, and drying time is 12~15 hours.Pelletizing
Cross grit number be 40 mesh.
According to currently preferred, the temperature increasing schedule in step 1.3 is：950~1000 DEG C are warming up to 3~6 DEG C/min,
Heat preservation 11~13 hours.
Binder described in step 2.1 of the present invention is a concentration of 5wt.% PVA（Polyvinyl alcohol）Aqueous solution or PVB（Poly- second
Enol butyral）One kind in ethanol solution.
The grit number of crossing that powder is crushed according to currently preferred, in step 2.1 is 40 mesh.
According to currently preferred, the thickness of sheet electrolyte sheet is 0.6~1.2mm in step 2.1.
According to currently preferred, the temperature increasing schedule in step 1.3 is：It is warming up to 1150~1200 with 2~4 DEG C/min
DEG C, keep the temperature 3~5 hours.
Advantageous effect
1, firing temperature is low：Bi2O3Fusing point it is low, Bi is adulterated so that CeO2/BaCeO3The firing temperature of composite electrolyte reduces
100 DEG C or more.
2, oxygen ionic conductivity is high：CeO is adulterated with the single element undoped with Bi2/BaCeO3Composite electrolyte is compared, ion
High 3 times of conductivity or more.
3, composite mixed CeO can be prepared by single step reaction2/BaCeO3Powder does not need subsequent hybrid technique,
Technological process is simple, is convenient for industrialization.
Specific implementation mode
Technical scheme of the present invention is described further with reference to embodiment, but institute's protection domain of the present invention is not limited to
This.
Embodiment 1
By 90wt.% Ce0.8Bi0.1La0.1O2-δ-10 wt.% BaCe0.8Bi0.1La0.1O3-δStoichiometric ratio weighs BaCO3、
CeO2、Bi2O3、La2O3, it is put into polyurethane ball-milling pot, absolute ethyl alcohol is added, using zirconia ball for medium ball milling 10 hours, original
Material, zirconia ball, absolute ethyl alcohol mass ratio be 1: 3:0.8, obtain slurry.It is 12 hours dry at 90 DEG C, it crosses 40 mesh sieve and makes
Grain, the compression moulding under 10MPa pressure obtain green body.Green body is put into heating furnace, is warming up to 1000 DEG C with 3 DEG C/min, heat preservation
12 hours, then furnace cooling.Block after calcining is crushed, 90wt.% Ce are obtained0.8Bi0.1La0.1O2-δ-10 wt.%
BaCe0.8Bi0.1La0.1O3-δComposite granule.1 wt.% PVA aqueous solutions are added into composite granule, are uniformly mixed, cross 40 mesh sieve
It is granulated, the sheet electrolyte green body that thickness is 1.0 mm is pressed under 50MPa pressure.Electrolyte green body is put into heating furnace,
1150 DEG C are warming up to 3 DEG C/min, 4 hours is kept the temperature, obtains solid-oxide fuel battery electrolyte.
Using electrochemical workstation（Shanghai Chen Hua, CHI660E）Test, 90wt.% Ce0.8Bi0.1La0.1O2-δ-10 wt.%
BaCe0.8Bi0.1La0.1O3-δIonic conductivity of the composite electrolyte under 600 DEG C of air conditions is 0.031 S cm-1。
Embodiment 2
By 70wt.% Ce0.8Bi0.1Gd0.1O2-δ-30 wt.% BaCe0.8Bi0.1Gd0.1O3-δStoichiometric ratio weighs BaCO3、
CeO2、Bi2O3、Gd2O3, it is put into polyurethane ball-milling pot, absolute ethyl alcohol is added, using zirconia ball for medium ball milling 10 hours, original
Material, zirconia ball, absolute ethyl alcohol mass ratio be 1: 3.1:0.9, obtain slurry.It is 15 hours dry at 80 DEG C, cross 40 mesh sieve
It is granulated, the compression moulding under 8MPa pressure obtains green body.Green body is put into heating furnace, is warming up to 980 DEG C with 5 DEG C/min, heat preservation
13 hours, then furnace cooling.Block after calcining is crushed, 70wt.% Ce are obtained0.8Bi0.1Gd0.1O2-δ-30 wt.%
BaCe0.8Bi0.1Gd0.1O3-δComposite granule.1 wt.% PVB ethanol solutions are added into composite granule, are uniformly mixed, cross 40 mesh
Sieve is granulated, and the sheet electrolyte green body that thickness is 0.9 mm is pressed under 40MPa pressure.Electrolyte green body is put into heating
Stove is warming up to 1200 DEG C with 4 DEG C/min, keeps the temperature 5 hours, obtain solid-oxide fuel battery electrolyte.
Using electrochemical workstation（Shanghai Chen Hua, CHI660E）Test, 70wt.% Ce0.8Bi0.1Gd0.1O2-δ-30 wt.%
BaCe0.8Bi0.1Gd0.1O3-δIonic conductivity of the composite electrolyte under 600 DEG C, air conditions is 0.028 S cm-1。
Comparative example 1
As described in Example 1, unlike：Undoped with Bi elements.I.e.：The ingredient of composite electrolyte is 90wt.%
Ce0.8La0.2O2-δ-10 wt.% BaCe0.8La0.2O3-δ.The firing temperature of the electrolyte is 1300 DEG C.In 600 DEG C, air conditions
Under ionic conductivity be 0.0078 S cm-1。
Comparative example 2
As described in Example 1, unlike：Undoped with Bi elements.I.e.：The ingredient of composite electrolyte is 70wt.%
Ce0.8Gd0.2O2-δ-30 wt.% BaCe0.8Gd0.2O3-δ.The firing temperature of the electrolyte is 1350 DEG C.In 600 DEG C, air conditions
Under ionic conductivity be 0.0071 S cm-1。
Compared with comparative example 1-2, firing temperature significantly reduces 1-2 of the embodiment of the present invention, and conductivity improves 3 times or more.It says
Bright Bi element dopings advantageously reduce CeO2/BaCeO3The firing temperature of composite electrolyte and its ionic conductivity of raising.
It should be noted that listed above is only several specific embodiments of the present invention, it is clear that the present invention is not only
It is limited to above example, there can also be other deformations.Those skilled in the art directly exported from the disclosure of invention or
All deformations for connecing amplification, are considered as protection scope of the present invention.
Claims (5)
1. a kind of CeO2/BaCeO3Base solid-oxide fuel battery electrolyte, which is characterized in that main component is
Ce0.8Bi x Re(0.2-x)O2-δ - BaCe0.8Bi x Re(0.2-x)O3-δ (0≤x≤0.2), wherein Re be La, Nd, Eu, Gd, Dy, Er,
One kind in Yb.
2. Ce according to claim 10.8Bi x Re(0.2-x)O2-δ - BaCe0.8Bi x Re(0.2-x)O3-δThe preparation side of electrolyte
Method, which is characterized in that include the following steps：
（1）Ce0.8Bi x Re(0.2-x)O2-δ-BaCe0.8Bi x Re(0.2-x)O3-δThe preparation of composite granule：
By Ce0.8Bi x Re(0.2-x)O2-δ-BaCe0.8Bi x Re(0.2-x) O3-δStoichiometric ratio weighs BaCO3、CeO2、Bi2O3、Re2O3
(Re=La, Nd, Eu, Gd, Dy, Er, Yb etc.), is put into polyurethane ball-milling pot, absolute ethyl alcohol is added, using zirconia ball as medium
Ball milling 8~12 hours, raw material, zirconia ball, absolute ethyl alcohol mass ratio be 1:(2.5~3.5):(0.8~0.9), obtains
Slurry；
Drying, is granulated, and the compression moulding under 5~15MPa pressure obtains green body；
Green body is put into heating furnace, is warming up to 900~1050 DEG C, keeps the temperature 10~15 hours, then furnace cooling；
Block after calcining is crushed, Ce is obtained0.8BixRe(0.2-x)O2-δ-Ba Ce0.8BixRe(0.2-x)O3-δComposite granule；
（2）Ce0.8BixRe(0.2-x)O2-δ-Ba Ce0.8BixRe(0.2-x)O3-δThe preparation of composite electrolyte：
To Ce0.8BixRe(0.2-x)O2-δ-Ba Ce0.8BixRe(0.2-x)O3-δ1 wt.% binders are added in composite granule, mixing is equal
It is even, it is granulated, the sheet electrolyte green body that thickness is 0.3~1.5 mm is pressed under 30~60MPa pressure；
Electrolyte green body is put into heating furnace, is warming up to 1100~1250 DEG C, 2~6 hours is kept the temperature, obtains solid oxide fuel
Cell electrolyte.
3. Ce according to claim 10.8Bi x Re(0.2-x)O2-δ - BaCe0.8Bi x Re(0.2-x)O3-δElectrolyte, feature exist
In Ce0.8Bi x Re(0.2-x)O2-δAnd BaCe0.8Bi x Re(0.2-x) O3-δMass ratio be (95~50):(5~50).
4. Ce according to claim 20.8Bi x Re(0.2-x)O2-δ - BaCe0.8Bi x Re(0.2-x)O3-δThe preparation side of electrolyte
Method, which is characterized in that the drying temperature is 80~100 DEG C, and drying time is 12~15 hours；Pelletizing crosses grit number
For 40 mesh.
5. Ce according to claim 20.8Bi x Re(0.2-x)O2-δ - BaCe0.8Bi x Re(0.2-x)O3-δThe preparation side of electrolyte
Method, which is characterized in that the binder is 5wt.% PVA（Polyvinyl alcohol）Aqueous solution or PVB（Polyvinyl butyral）Second
One kind in alcoholic solution.
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Cited By (1)
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| CN109148948A (en) * | 2018-09-30 | 2019-01-04 | 武汉理工大学 | A kind of solid electrolyte and preparation method thereof of high-lithium ion conductivity |
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