CN106887627B - A kind of intermediate temperature solid oxide fuel cell electrolyte and preparation method thereof - Google Patents
A kind of intermediate temperature solid oxide fuel cell electrolyte and preparation method thereof Download PDFInfo
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- CN106887627B CN106887627B CN201710242588.5A CN201710242588A CN106887627B CN 106887627 B CN106887627 B CN 106887627B CN 201710242588 A CN201710242588 A CN 201710242588A CN 106887627 B CN106887627 B CN 106887627B
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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
- H01M8/1016—Fuel cells with solid electrolytes characterised by the electrolyte material
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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
- H01M2300/00—Electrolytes
- H01M2300/0085—Immobilising or gelification of electrolyte
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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
- H01M2300/00—Electrolytes
- H01M2300/0088—Composites
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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
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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Abstract
The invention belongs to the preparation fields of solid electrolyte, and in particular to a kind of intermediate temperature solid oxide fuel cell electrolyte and preparation method thereof.A kind of intermediate temperature solid oxide fuel cell electrolyte Ce is prepared using nitrate micro-gel flooding and solid reaction process0.8Gd0.2O1.9‑BaCe0.8Y0.2O3‑δ‑Bi1.5Er0.5O3, relative density reaches 97% or more；The electrolyte in air atmosphere 750 DEG C when ionic conductivity reach 1.31 × 10‑2S/cm is suitable for middle cryogenic applications.
Description
Technical field
The invention belongs to the preparation fields of solid electrolyte, and in particular to a kind of intermediate temperature solid oxide fuel cell electrolysis
Matter and preparation method thereof.
Background technique
With the development of global industry and increasing rapidly for population, tellurian resource will be increasingly shorter.American energy
Information administration (EIA) statistical framework shows that world energy sources demand in 2010 has reached 10,600,000,000 tons of oil equivalents, it was predicted that 2025
It is up to 136.5 hundred million tons of oil equivalents.And traditional generation mode is by the chemical energy in the fossil energies such as petroleum, natural gas mostly
It is thermal energy by burning conversion, then pushes mechanical equipment to generate mechanical energy by thermal energy, is ultimately converted to electric energy.This energy conversion
Not only limited by Carnot cycle, can also generate the harmful substances such as a large amount of dust, carbon dioxide, nitrogen oxides and sulfide and
Noise；Solid oxide fuel cell (Solid Oxide Fuel Cell, abbreviation SOFC) wide, energy with fuel tolerance
The advantages that high conversion efficiency, all solid state, modularization assembling, no pollution, can directly use hydrogen, carbon monoxide, natural gas,
A variety of hydrocarbon fuels such as liquefied gas, coal gas and biogas.In large-scale centralized power supply, medium-sized point of electricity and small-sized household cogeneration
Equal civil fields have wide as stationary electric power plant, and as mobile power sources such as ship power power supply, vehicular traffic electrical source of power
Wealthy application prospect.
The operating temperature of traditional SOFC must just have higher output power, high fortune in 800 DEG C or more of running temperature
Trip temperature not only has very high requirement to the connection sealing of battery, but also accelerates the generation of the side reaction between battery component,
Cell performance decay rate increases, and keeps the cost of battery high, greatly limits the commercialized development of SOFC.Therefore, it
Make SOFC commercialized development it is necessary to reduce its operating temperature, low temperature SOFC has become inexorable trend in exploitation.In SOFC system
In, electrolyte is the core of battery, and the performance of electrolyte directly decides the operating temperature and performance of battery.Traditional electrolyte
It can not be suitable for middle cryogenic conditions, therefore must just seek the electrolyte under middle low temperature with high conductivity.Of the invention
Composite electrolyte has conductivity high, can meet in low temperature use condition.
Summary of the invention
The purpose of the present invention is to provide a kind of intermediate temperature solid oxide fuel cell electrolyte and preparation method thereof, use
Nitrate micro-gel flooding and solid reaction process prepare novel C e0.8Gd0.2O1.9-BaCe0.8Y0.2O3-δ-Bi1.5Er0.5O3(GBE)
Composite electrolyte, relative density reach 97%；In air atmosphere 750 DEG C when conductivity be 1.31 × 10-2S/cm。
Specific preparation method:
Bi1.5Er0.5O3The preparation method comprises the following steps:
1) Bi is weighed according to stoichiometric ratio2O3,Er2O3。
2) by Bi2O3And Er2O3Mixing and ball milling is for 24 hours；Then 12h is dried；
3) mixture after ball milling is calcined to 16 ± 0.1h at 800 DEG C ± 10 DEG C, obtains Bi1.5Er0.5O3。
Ce0.8Gd0.2O1.9-BaCe0.8Y0.2O3-δ(GDC-BCY) preparation method:
1) Ce0.8Gd0.2O1.9Preparation: stoichiometrically weigh Ce (NO3)3·6H2The 70% of O weight, is denoted as [Ce
(NO3)3·6H2O] * 0.7, it is same: Gd2O3* 0.7, complexing agent citric acid is weighed by [n (CA): n (metal cation)=1.5:1].
With dust technology by Gd2O3It is dissolved as nitrate, Ce (NO3)3·6H2O and citric acid deionized water dissolving, mix the above solution simultaneously
It stirs evenly；
2) BaCe0.8Y0.2O3-δPreparation: stoichiometrically weigh Ba (NO3)2*0.3、[Ce(NO3)3·6H2O]*
0.3、[Y(NO3)3·6H2O] * 0.3, complexing agent ethylenediamine tetra-acetic acid (EDTA) and citric acid by [n(metal cation):n
(EDTA):n(CA)=1:1:2] it weighs.Deionized water is added in nitrate, EDTA and citric acid respectively；By NH3·H2O drop
Enter in the deionized water of EDTA and makes it dissolve；
3) it is uniform to mix the above solution & stir；It is 7 that ammonium hydroxide (ammonia concn 15wt%-20wt%), which is added dropwise, and adjusts pH value；
4) it step 3) is obtained mixed solution is put into blender to be heated to 70 DEG C, be continuously stirred at 70 DEG C, and stirring
By adding ammonium hydroxide during mixing, the pH value of solution is set to be maintained at 7, until forming gel；
5) gel immigration evaporating dish is placed on electric furnace and is heated, until self-propagating combustion, which occurs, forms fluffy oxide
Powder；
6) powder is removed into organic matter in 600 DEG C of calcining 30min, then in 1000 DEG C of ± 10 DEG C of 5 ± 0.1h of calcining, is formed
GDC-BCY(GB) powder.
By GB:Bi1.5Er0.5O3Mass ratio 95:5 weighs two kinds of powder, for 24 hours by two kinds of powder mixing and ball millings, prepares 95%
GB-5%Bi1.5Er0.5O3Powder.
By manufactured 95%GB-5%Bi1.5Er0.5O3(GBE) powder is put into mold, and under the pressure of 300MPa, circle is made
Disk is heated to 1300 DEG C of ± 10 DEG C of 4 ± 0.1h of heat preservation with 3 DEG C of heating speed per minute, obtains required electrolysis by piece
Matter disk.
Remarkable advantage of the invention is:
(1) electrolyte of the present invention conductivity with higher, higher power in medium temperature (600 DEG C -800 DEG C) range is close
Degree.
(2) sintering temperature of electrolyte of the present invention is low, low for equipment requirements and energy saving.
(3) present invention electrolysis mass-energy is used for intermediate temperature solid oxide fuel cell.
Detailed description of the invention
The conductivity of GBE made from Fig. 1 embodiment 1 and the relation curve of test temperature.
Specific embodiment
In order to make content of the present invention easily facilitate understanding, With reference to embodiment to of the present invention
Technical solution is described further, but the present invention is not limited only to this.
Embodiment 1
1.Ce0.8Gd0.2O1.9-BaCe0.8Y0.2O3-δ(GDC-BCY) preparation method:
1) Ce0.8Gd0.2O1.9Preparation: stoichiometrically weigh Ce (NO3)3·6H2The 70% of O weight, is denoted as [Ce
(NO3)3·6H2O] * 0.7, it is same: Gd2O3* 0.7, complexing agent citric acid is weighed by [n (CA): n (metal cation)=1.5:1].
With dust technology by Gd2O3It is dissolved as nitrate, Ce (NO3)3·6H2O and citric acid deionized water dissolving, mix the above solution simultaneously
It stirs evenly；
2) BaCe0.8Y0.2O3-δPreparation: stoichiometrically weigh Ba (NO3)2*0.3、[Ce(NO3)3·6H2O]*
0.3、[Y(NO3)3·6H2O] * 0.3, complexing agent ethylenediamine tetra-acetic acid (EDTA) and citric acid by [n(metal cation):n
(EDTA):n(CA)=1:1:2] it weighs.Deionized water is added in nitrate, EDTA and citric acid respectively；By NH3·H2O drop
Enter in the deionized water of EDTA and makes it dissolve；
3) it is uniform to mix the above solution & stir；It is 7 that ammonium hydroxide (ammonia concn 15wt%-20wt%), which is added dropwise, and adjusts pH value；
4) it step 3) is obtained mixed solution is put into blender to be heated to 70 DEG C, be continuously stirred at 70 DEG C, and stirring
By adding ammonium hydroxide during mixing, the pH value of solution is set to be maintained at 7, until forming gel；
5) gel immigration evaporating dish is placed on electric furnace and is heated, until self-propagating combustion, which occurs, forms fluffy oxide
Powder；
6) powder is removed into organic matters in 600 DEG C of ± 10 DEG C of 30 ± 5min of calcining, then 1000 DEG C of ± 10 DEG C of calcinings 5 ±
0.1h forms GDC-BCY(GB) powder.
2.Bi1.5Er0.5O3Preparation method
1) according to Bi1.5Er0.5O3Stoichiometric ratio assay balance precise raw material Bi2O3And Er2O3；
2) by Bi2O3And Er2O3Add alcohol mixing and ball milling for 24 hours, then dries 12h；
3) by the Bi after drying2O3And Er2O3Mixture calcines 16 ± 0.1h at 800 DEG C ± 10 DEG C, obtains final product
Bi1.5Er0.5O3；
3. pressing GB:Bi1.5Er0.5O3Mass ratio 95:5 weighs two kinds of powder, for 24 hours using mixing and ball milling by the two sample, makes
It grinds sufficiently and uniform.
It is specific:
The preparation of 100 grams of GBE:
1) 1 mole of Ce is prepared0.8Gd0.2O1.9-BaCe0.8Y0.2O3-δ(GDC-BCY)
The preparation of 0.7molGDC
Weigh 0.56 mole of Ce (NO3)3·6H2O:0.56*434.22=243.16 gram
Weigh 0.07 mole of Gd2O3: 0.07*362.5=25.37 gram
Weigh 1.05 moles of citric acid: 1.05*210.14=220.65 gram
With dust technology by Gd2O3It is dissolved as nitrate；By Ce (NO3)3·6H2Distilled water dissolution is added in O and citric acid；It will be upper
State solution pour into respectively in gadolinium nitrate solution be uniformly mixed；
The preparation of 0.3molBCY
Weigh 0.24 mole of Ce (NO3)3·6H2O:0.24*434.22=104.21 gram
Weigh 0.3 mole of Ba (NO3)2: 0.3*261.35=78.40 gram
Weigh 0.06 mole of Y (NO3)3·6H2O:0.06*383.01=22.98 gram
Weigh 0.6 mole of complexing agent EDTA:0.6*292.24=175.34 gram
Weigh 1.2 molar citric acids: 1.2*210.14=252.16 gram
Appropriate amount of deionized water is added in nitrate and complexing agent, by NH3·H2O instills EDTA and makes it dissolve；After dissolving
EDTA solution be added to Ba (NO3)2It makes it dissolve completely；It is uniform to mix the above solution & stir
By the above-mentioned GDC prepared, BCY solution is mixed evenly, and is added ammonium hydroxide tune pH to 7, is put into water-bath and heats
It to 70 DEG C, is continuously stirred at 70 DEG C, and so that the pH value of solution is maintained at 7, until being formed by adding ammonium hydroxide in whipping process
Gel；Gel immigration evaporating dish is placed on electric furnace and is heated, until self-propagating combustion, which occurs, forms fluffy oxide powder；
Powder is removed into organic matters in 600 DEG C of ± 10 DEG C of 30 ± 5min of calcining, then 1000 DEG C of ± 10 DEG C of calcinings 5 ±
0.1h forms the GDC-BCY(GB that molar ratio is 7:3) powder.
2) 1 mole of Bi is prepared1.5Er0.5O3
Weigh 0.75 mole of Bi2O3: 0.75*465.96=349.47 gram
Weigh 0.25 mole of Er2O3: 0.25*382.52=95.63 gram
The Bi that will be weighed up2O3And Er2O3Add alcohol mixing and ball milling for 24 hours, dry 12h, calcine 16 at 800 DEG C ± 10 DEG C ±
0.1h obtains final product Bi1.5Er0.5O3；
3) 100 grams of 95%GB-5%Bi1.5Er0.5O3Preparation
Weigh 95 grams of GB；
Weigh 5 grams of Bi1.5Er0.5O3；
For 24 hours with mixing and ball milling by above-mentioned latter two powder, make its grinding sufficiently and uniform, obtain 95%GB-5%
Bi1.5Er0.5O3(GBE) powder.
Embodiment 2
The preparation of disk: the GBE powder that embodiment 1 is prepared into is put into mold, under the pressure of 300MPa, is made straight
Diameter is the disk of 13mm ± 0.1mm, thickness 0.5mm ± 0.1mm, and disk is heated to 1300 with 3 DEG C of heating speed per minute
DEG C ± 10 DEG C of 4 ± 0.1h of heat preservation, electrolyte disk required for obtaining.
The test method of conductivity:
The conductance for alternating current of electrolyte is measured using two-terminal method.By the gained after 4 ± 0.1h of sintering at 1300 DEG C ± 10 DEG C
95%GB-5%Bi1.5Er0.5O3Silver paste is coated on electrolyte disk two sides, and silver electrode is then made after 450 DEG C of roasting 2h.With silver
The silver electrode at both ends is connect by silk with alternating current impedance instrument.The alternating current impedance instrument used is Shanghai Chen Hua Instrument Ltd. model
CHI660E electrochemical workstation measures frequency range 1kHz-20MHz using current potential 10mV, and the temperature for measuring conductance for alternating current is
It 750 DEG C, is measured in air atmosphere.Conductivity is calculated using following formula:
In formula, σ is electrolytic conductivity, S/cm；
H is electrolyte sheet thickness, unit cm；
R is bath resistance, unit Ω；
S is electrolyte sheet cross-sectional area, unit cm2。
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (3)
1. a kind of intermediate temperature solid oxide fuel cell electrolyte preparation method, it is characterised in that: the electrolyte is
Ce0.8Gd0.2O1.9-BaCe0.8Y0.2O3-δ-Bi1.5Er0.5O3Composite electrolyte, wherein 0 < δ≤0.1；Specific preparation method include with
Lower step:
(1) Bi1.5Er0.5O3The preparation method comprises the following steps:
A. Bi is weighed according to stoichiometric ratio2O3, Er2O3；
B. by Bi2O3And Er2O3Mixing and ball milling is for 24 hours；Then 12h is dried；
C., mixture after ball milling is calcined to 16 ± 0.1h at 800 DEG C ± 10 DEG C, obtains Bi1.5Er0.5O3；
(2) Ce0.8Gd0.2O1.9-BaCe0.8Y0.2O3-δPreparation method:
a. Ce0.8Gd0.2O1.9Preparation: stoichiometrically weigh Ce (NO3)3·6H2O, Gd2O3；And by metal cation with
The molar ratio of citric acid is that 1:1.5 weighs citric acid；With dust technology by Gd2O3It is dissolved as nitrate, Ce (NO3)3·6H2O and lemon
Lemon acid deionized water dissolving, it is uniform to mix the above solution & stir；
b. BaCe0.8Y0.2O3-δPreparation: stoichiometrically weigh Ba (NO3)2、Ce(NO3)3·6H2O、Y(NO3)3·6H2O；
And weigh EDTA and citric acid；Deionized water is added in nitrate, EDTA and citric acid respectively；By NH3·H2O is instilled
It is made it dissolve in the deionized water of EDTA；
C. it is uniform to mix the above solution & stir；It is 7 that ammonium hydroxide, which is added dropwise, and adjusts pH value；
D. step c is obtained mixed solution and be put into blender to be heated to 70 DEG C, be continuously stirred at 70 DEG C, and stirred
By adding ammonium hydroxide in journey, the pH value of solution is set to be maintained at 7, until forming gel；
E. gel immigration evaporating dish is placed on electric furnace and is heated, until self-propagating combustion, which occurs, forms fluffy oxide powder；
F. powder is removed into organic matter in 600 DEG C of calcining 30min, then in 1000 DEG C of ± 10 DEG C of 5 ± 0.1h of calcining, formation rubs
You are than the Ce for 7:30.8Gd0.2O1.9-BaCe0.8Y0.2O3-δPowder；
(3) Ce is pressed0.8Gd0.2O1.9-BaCe0.8Y0.2O3-δWith step (1) Bi1.5Er0.5O3Mass ratio 95:5 weighs two kinds of powder, will
Two kinds of powder mixing and ball millings are for 24 hours；
(4) the step of being made (3) powder is put into mold, under the pressure of 300MPa, disk is made, by disk with per minute
3 DEG C of heating speed is heated to 1300 DEG C of ± 10 DEG C of 4 ± 0.1h of heat preservation, electrolyte disk required for obtaining.
2. intermediate temperature solid oxide fuel cell electrolyte preparation method according to claim 1, it is characterised in that: step
Suddenly (2) BaCe0.8Y0.2O3-δPreparation in the molar ratio of metal cation and EDTA and citric acid be 1:1:2.
3. intermediate temperature solid oxide fuel cell electrolyte preparation method according to claim 1, it is characterised in that: ammonia
The concentration of water is 15wt%-20wt%.
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