CN107910574A - A kind of composite solid electrolyte preparation method for fuel cell - Google Patents
A kind of composite solid electrolyte preparation method for fuel cell Download PDFInfo
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- CN107910574A CN107910574A CN201711129827.2A CN201711129827A CN107910574A CN 107910574 A CN107910574 A CN 107910574A CN 201711129827 A CN201711129827 A CN 201711129827A CN 107910574 A CN107910574 A CN 107910574A
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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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- 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
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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
- 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
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Abstract
The invention discloses a kind of composite solid electrolyte preparation method for fuel cell.This method is first respectively according to Zr0.8Ni0.2O1.9And TiCe0.8La0.2O2.9The ratio between stoichiometric number obtain respective solution A and B, then by sol-gal process, obtain both mixed gels, finally sinter, obtain composite solid electrolyte.The composite solid electrolyte that this method is prepared is at 800 DEG C, the electrical conductivity of material electrodes reaches more than 0.114S/cm, 700 DEG C are issued to more than 0.268S/cm, 600 DEG C reach more than 0.106S/cm, therefore middle low temperature can not be suitable for compared to traditional electrolyte matter, composite solid electrolyte material of the invention uses under conditions of being applicable to 600 800 DEG C；The method of the present invention preparation process is controllable, and sintering temperature is low, it can be achieved that industrialized production.
Description
Technical field
The invention belongs to fuel cell field, and in particular to a kind of middle low temperature composite solid electrolyte for fuel cell
And preparation method thereof.
Background technology
The energy is human survival and the essential material base of social development, wherein coal, oil and natural gas etc.
Carbon compound is referred to as carbon-based fuel, and carbon-based fuel a generating efficiency is only 30% or so at present, exists and pollutes big, greenhouse
The defects of gas discharge is more.And solid oxide fuel cell (SOFC) is a kind of directly can be converted into the chemical energy of fuel
The electrochemical generating unit of electric energy, one time generating efficiency is up to 50-60%, has the advantages that high efficiency, low stain.
In single battery, the sintering character thermal matching of electrode material and electrolyte is poor, electrolyte electrical conductivity
Structure destruction etc. caused by unstable and battery strength is weaker, may cause the decay of whole stack performance, and tradition
SOFC operating temperatures generally at 1000 DEG C, work at such high temperatures so that SOFC there are electrode be densified, connector
The problems such as material requirements is high, battery hermetization is bad, adds the cost of SOFC, therefore study solid oxide fuel now
Battery is typically all to improve electrolyte so that SOFC can be in, low operating temperatures, such as patent 201710237453.X
Disclose electrical conductivity under a kind of 750 DEG C of operating conditions of medium temperature and reach 1.45 × 10-2The composite electrolyte of S/cm, patent
201510609504.8 175mS/cm can be reached in 850 DEG C of electrical conductivity by disclosing composite solid electrolyte material.But in height
The lower electrical conductivity of temperature and temperature are in correlation, can be increased rapidly with temperature rise electrical conductivity, therefore develop novel solid electrolysis material
Material so that it is current research hotspot still to have high conductance in, under cryogenic conditions.
The content of the invention
The purpose of the present invention is for existing solid electrolyte material in, under low temperature the not high deficiency of electrical conductivity, there is provided
A kind of NEW TYPE OF COMPOSITE solid electrolyte and preparation method thereof, the composite solid electrolyte that this method is prepared is at 600-800 DEG C
Under still there is higher electrical conductivity.
In order to achieve the object of the present invention, the present inventor is as follows by a large number of experiments research and unremitting effort, final acquisition
Technical solution：A kind of composite solid electrolyte preparation method for fuel cell, includes the following steps：
(1) according to Zr0.8Ni0.2O1.9The ratio between stoichiometric number weigh zirconates and nickel salt, respectively with after deionized water dissolving
Mixing, then citric acid is added into mixed liquor, citric acid is (5-8) with metal cation molar ratio total in mixed liquor：1, stir
Mix uniformly, obtain solution A；
(2) according to TiCe0.8La0.2O2.9The ratio between stoichiometric number weigh titanium salt, cerium salt and lanthanum salt, use deionization respectively
After water is dissolved and mixed, the mixture of ethylene glycol and citric acid, wherein citric acid are added into mixed liquor：Ethylene glycol：Mixed liquor
In total metal cation molar ratio be (4-8)：(3-5)：1, stir evenly, obtain solution B；
(3) together with solution A is poured into solution B, it is 8-9 that weak base, which is added dropwise, and adjusts pH of mixed, heating water bath to 65-75
DEG C, and stir, until forming gel；
(4) after gel drying, 30-60min is first calcined after xerogel is ground at 580-650 DEG C, then in 1000-1150
DEG C calcining 6-8h, obtain composite solid electrolyte.
It is further preferred that composite solid electrolyte preparation method of the present invention, wherein zirconates is described in step (1)
Any one in zirconium nitrate, zirconium oxychloride.
It is further preferred that composite solid electrolyte preparation method of the present invention, wherein nickel salt is described in step (1)
Any one in nickel acetate, nickel nitrate, nickel sulfate or nickel chloride.
It is further preferred that composite solid electrolyte preparation method of the present invention, wherein titanium salt is described in step (2)
Soluble inorganic titanium salt or Titanium alkoxides.
It is further preferred that composite solid electrolyte preparation method of the present invention, wherein cerium salt is described in step (2)
Any one in cerous nitrate, cerous sulfate.
It is further preferred that composite solid electrolyte preparation method of the present invention, wherein lanthanum salt is described in step (2)
Any one in lanthanum nitrate, lanthanum chloride, lanthanum sulfate.
It is further preferred that composite solid electrolyte preparation method of the present invention, citric acid wherein described in step (1)
It is (6.5-7) with metal cation molar ratio total in mixed liquor：1.
It is further preferred that composite solid electrolyte preparation method of the present invention, lemon wherein described in step (2)
Acid：Ethylene glycol：Total metal cation molar ratio is (6-7) in mixed liquor：(3.5-4)：1.
It is further preferred that described in composite solid electrolyte preparation method of the present invention, wherein step (1) and (2)
After metal salt deionized water dissolving, respective concentration is respectively 0.8-1.5g/mL.
It is further preferred that speed of agitator is in composite solid electrolyte preparation method of the present invention, wherein step (3)
80-150rpm。
In addition, the present invention also provides the composite solid electrolyte being prepared using the above method.
The present invention has the following technical effect that relative to the prior art：
(1) for the composite solid electrolyte that the present invention is prepared at 800 DEG C, the electrical conductivity of material electrodes reaches 0.114
More than S/cm, 700 DEG C are issued to more than 0.268S/cm, and 600 DEG C reach more than 0.106S/cm, therefore compared to traditional electrolyte matter
It can not be suitable for middle low temperature, composite solid electrolyte material of the invention uses under conditions of being applicable to 600-800 DEG C；
(2) the method for the present invention preparation process is controllable, and sintering temperature is low, it can be achieved that industrialized production.
Embodiment
The embodiment of the present invention is described further below.
Embodiment 1
Step (1)：According to Zr0.8Ni0.2O1.9The ratio between stoichiometric number weigh Zr (NO3)4·5H2O 23.62g、Ni
(NO3)2·6H2O 4.0g, respectively with deionized water dissolving, solution concentration difference 1g/mL, is mixed to obtain mixed liquor afterwards,
Citric acid 66.07g is added into mixed liquor again, stirs evenly, obtains solution A；
Step (2)：According to TiCe0.8La0.2O2.9The ratio between stoichiometric number weigh TiCl4 13.1438g、Ce(NO3)3·
6H2O 24.06g and La (NO3)3·6H2O 6g, respectively with after deionized water dissolving and mixing, solution concentration distinguishes 1.2g/mL,
It is mixed to obtain mixed liquor afterwards, the mixing of ethylene glycol 25.80787g and citric acid 106.5224g is added into mixed liquor
Thing, wherein citric acid：Ethylene glycol：Total metal cation molar ratio is 4 in mixed liquor：3：1, stir evenly, obtain solution B；
Step (3)：By solution A and solution B according to Zr0.8Ni0.2O1.9：TiCe0.8La0.2O2.9For 2：1 mixed in molar ratio,
It is 8 that weak base is added dropwise after mixing and adjusts pH of mixed, and heating water bath is to 65 DEG C and stirs, until forming gel；
Step (4) gel is placed in baking oven, after dry at 50 DEG C, be ground into powder, calcined afterwards at 580 DEG C
60min, then 7h is calcined at 1000 DEG C, obtain composite solid electrolyte.
Embodiment 2
Step (1)：According to Zr0.8Ni0.2O1.9The ratio between stoichiometric number weigh Zr (NO3)4·5H2O 34.35g、Ni
(NO3)2·6H2O 58.16g, respectively with deionized water dissolving, solution concentration difference 1g/mL, is mixed is mixed afterwards
Liquid, then citric acid 153.712g is added into mixed liquor, citric acid is 8 with metal cation molar ratio total in mixed liquor：1,
Stir evenly, obtain solution A；
Step (2)：According to TiCe0.8La0.2O2.9The ratio between stoichiometric number weigh TiCl4 18.971g、Ce(NO3)3·
6H2O 34.7296g and La (NO3)3·6H2O 8.66g, respectively with after deionized water dissolving and mixing, solution concentration is distinguished
1.2g/mL, is mixed to obtain mixed liquor afterwards, adds ethylene glycol 62.068g and citric acid 307.424g's into mixed liquor
Mixture, wherein citric acid：Ethylene glycol：Total metal cation molar ratio is 8 in mixed liquor：5：1, stir evenly, obtain molten
Liquid B；
Step (3)：By solution A and solution B according to Zr0.8Ni0.2O1.9：TiCe0.8La0.2O2.9For 6：1 mixed in molar ratio,
It is 9 that weak base is added dropwise after mixing and adjusts pH of mixed, and heating water bath is to 75 DEG C and stirs, until forming gel；
Step (4)：Gel is placed in baking oven, after dry at 50 DEG C, be ground into powder, first calcined at 650 DEG C
35min, then 6h is calcined at 1150 DEG C, obtain composite solid electrolyte.
Embodiment 3
Step (1)：According to Zr0.8Ni0.2O1.9The ratio between stoichiometric number weigh Zr (NO3)4·5H2O 23.62g、Ni
(NO3)2·6H2O 4.0g, respectively with deionized water dissolving, solution concentration difference 1g/mL, is mixed to obtain mixed liquor afterwards,
Citric acid 85.86256g, citric acid and metal cation molar ratio 6.5 total in mixed liquor are added into mixed liquor again：1, stir
Mix uniformly, obtain solution A；
Step (2)：According to TiCe0.8La0.2O2.9The ratio between stoichiometric number weigh TiCl4 13.1438g、Ce(NO3)3·
6H2O 24.06g and La (NO3)3·6H2O 6g (433), respectively with after deionized water dissolving and mixing, solution concentration is distinguished
1.2g/mL, is mixed to obtain mixed liquor afterwards, and ethylene glycol 30.1091868g and citric acid are added into mixed liquor
159.7836g mixture, wherein citric acid：Ethylene glycol：Total metal cation molar ratio is 6 in mixed liquor：3.5：1, stir
Mix uniformly, obtain solution B；
Step (3)：By solution A and solution B according to Zr0.8Ni0.2O1.9：TiCe0.8La0.2O2.9For 4：1 mixed in molar ratio,
It is 8.5 that weak base is added dropwise after mixing and adjusts pH of mixed, and heating water bath is to 70 DEG C and stirs, until forming gel；
After the grinding of step (4) gel drying, 50min is first calcined at 600 DEG C, then 8h is calcined at 1100 DEG C, is obtained compound
Solid electrolyte.
Embodiment 4
Step (1)：According to Zr0.8Ni0.2O1.9The ratio between stoichiometric number weigh Zr (NO3)4·5H2O 23.62g、Ni
(NO3)2·6H2O 4.0g, respectively with deionized water dissolving, solution concentration difference 1g/mL, is mixed to obtain mixed liquor afterwards,
Citric acid 66.07g is added into mixed liquor again, citric acid is 7 with metal cation molar ratio total in mixed liquor：1, stirring is equal
It is even, obtain solution A；
Step (2)：According to TiCe0.8La0.2O2.9The ratio between stoichiometric number weigh TiCl4 13.1438g、Ce(NO3)3·
6H2O 24.06g and La (NO3)3·6H2O 6g, respectively with after deionized water dissolving and mixing, solution concentration distinguishes 1.2g/mL,
It is mixed to obtain mixed liquor afterwards, the mixture of ethylene glycol and citric acid, wherein citric acid is added into mixed liquor：Second two
Alcohol：Total metal cation molar ratio is 7 in mixed liquor：4：1, stir evenly, obtain solution B；
Step (3)：By solution A and solution B according to Zr0.8Ni0.2O1.9：TiCe0.8La0.2O2.9For 5：1 mixed in molar ratio,
It is 9 that weak base is added dropwise after mixing and adjusts pH of mixed, and heating water bath is to 75 DEG C and stirs, until forming gel；
After the grinding of step (4) gel drying, 40min is first calcined at 620 DEG C, then 7h is calcined at 1000 DEG C, is obtained compound
Solid electrolyte.
Comparative example 1
According to Zr0.8Ni0.2O1.9The ratio between stoichiometric number weigh Zr (NO3)4·5H2O 23.62g(429.32)、Ni
(NO3)2·6H2O 4.0g (290.81), respectively with deionized water dissolving, solution concentration difference 1g/mL, is mixed afterwards
To mixed liquor, then citric acid 66.07g (192.14) is added into mixed liquor, citric acid and metal cation total in mixed liquor
Molar ratio is 7：1, stir evenly, it is 9 that weak base is added dropwise afterwards and adjusts pH of mixed, and heating water bath is to 75 DEG C and stirs, until shape
Into gel；After gel drying grinding, 40min is calcined at present 620 DEG C, then 7h is calcined at 1000 DEG C, obtains solid electrolyte.
Comparative example 2
According to TiCe0.8La0.2O2.9The ratio between stoichiometric number weigh TiCl4 13.1438g(189.71)、Ce(NO3)3·
6H2O 24.06g (434.12) and La (NO3)3·6H2O 6g (433), respectively with after deionized water dissolving and mixing, solution is dense
Degree difference 1.2g/mL, is mixed to obtain mixed liquor afterwards, ethylene glycol (density 1.1155, molecular weight is added into mixed liquor
62.068) with the mixture of citric acid, wherein citric acid：Ethylene glycol：0.1386mol moles total of metal cation in mixed liquor
Than for 7：4：1, stir evenly, it is 9 that weak base is added dropwise afterwards and adjusts pH of mixed, and heating water bath is to 75 DEG C and stirs, until being formed
Gel；After gel drying grinding, 40min is first calcined at 620 DEG C, then 7h is calcined at 1000 DEG C, obtains solid electrolyte.
Comparative example 3
The gel drying that comparative example 1 and comparative example 2 obtain is pulverized, according to Zr0.8Ni0.2O1.9：
TiCe0.8La0.2O2.9For (2-6)：1 mixed in molar ratio, powder after mixing
Both compound calcinings obtain electrolyte and 40min are first calcined at 620 DEG C, then calcine 7h at 1000 DEG C, obtain solid
Electrolyte.
Embodiment 5
Taking electrolyte powder, adds a little absolute ethyl alcohol to be fully ground as binding agent, uniformly mixed powder is positioned over
In mould for tabletting press, diameter 30mm is obtained after pressurize 3min under 30MPa pressure, the electrolyte matrix of thickness 1mm, will be pressed into
The electrolyte sheet of type is positioned in Muffle furnace, is warming up to 3 DEG C/min at 1300 DEG C and is kept the temperature 2h, obtains electrolyte sheet.
To survey its electrical conductivity, it is necessary to prepare Ag Symmetrical cells, detailed process is as follows：Electrolyte sheet both sides are polished smooth,
Making sample, thickness is uniform everywhere；Using Ag glue as electrode, tested electrolyte sheet both sides symmetrically are applied to, form symmetry electrode；
Then Ag are stained with and is used as conducting wire, electrolyte sheet is warming up to 800 DEG C with constant heating rate and keeps the temperature 1h, room is down to stove
Temperature, obtains covering the electrolyte sample of uniform Ag electrodes.
Experiment tests the electrical conductivity of material using two-probe method, and Ag electrode Symmetrical cells to be measured are put into high temperature
In tube furnace, with Ag conducting wires connection Ag nets current collector and exterior electrochemical operation instrument (Shanghai Chen Hua CHI660D).Slowly rise pipe
The temperature of formula stove, carries out ac impedance measurement at 400-800 DEG C, and each test temperature keeps the temperature 50min after reaching test temperature,
So that test data is stablized, a temperature spot is tested every 100 DEG C, alternating-current magnitude 10mV, measures frequency 1kHz-20MHz, surveys
The temperature for determining conductance for alternating current is 750 DEG C, is measured in air atmosphere, and electrical conductivity is calculated using equation below：σ=h/ (RS), formula
Middle σ is electrolytic conductivity, unit S/cm；H is electrolyte sheet thickness, unit cm；R is bath resistance, unit Ω；S is electricity
Solve matter piece cross-sectional area, unit cm2。
The material obtained respectively to embodiment 1-4, comparative example 1-3 carries out electrical conductivity test, and the results are shown in Table 1.
1 different materials of table conductivity measurement data at different temperatures
The conductivity data that wherein "-" representative measures is less than minimum requirements 0.01 × 10 of the present invention-2S/cm。
Claims (10)
1. a kind of composite solid electrolyte preparation method, it is characterised in that include the following steps：
(1) according to Zr0.8Ni0.2O1.9The ratio between stoichiometric number weigh zirconates and nickel salt, mixed respectively with after deionized water dissolving
Close, then citric acid is added into mixed liquor, citric acid is (5-8) with metal cation molar ratio total in mixed liquor：1, stirring
Uniformly, solution A is obtained；
(2) according to TiCe0.8La0.2O2.9The ratio between stoichiometric number weigh titanium salt, cerium salt and lanthanum salt, it is molten with deionized water respectively
After solving and mixing, the mixture of ethylene glycol and citric acid, wherein citric acid are added into mixed liquor：Ethylene glycol：It is total in mixed liquor
Metal cation molar ratio be (4-8)：(3-5)：1, stir evenly, obtain solution B；
(3) by solution A and solution B according to Zr0.8Ni0.2O1.9：TiCe0.8La0.2O2.9For (2-6)：1 mixed in molar ratio, mixing
It is 8-9 that weak base is added dropwise afterwards and adjusts pH of mixed, and heating water bath is to 65-75 DEG C and stirs, until forming gel；
(4) after gel drying, 30-60min is first calcined after xerogel is ground at 580-650 DEG C, then forge at 1000-1150 DEG C
6-8h is burnt, obtains composite solid electrolyte.
2. composite solid electrolyte preparation method according to claim 1, it is characterised in that：Zirconates is described in step (1)
Any one in zirconium nitrate, zirconium oxychloride.
3. composite solid electrolyte preparation method according to claim 1, it is characterised in that：Nickel salt is described in step (1)
Any one in nickel acetate, nickel nitrate, nickel sulfate or nickel chloride.
4. composite solid electrolyte preparation method according to claim 1, it is characterised in that：Titanium salt is described in step (2)
Soluble inorganic titanium salt or Titanium alkoxides.
5. composite solid electrolyte preparation method according to claim 1, it is characterised in that：Cerium salt is described in step (2)
Any one in cerous nitrate, cerous sulfate.
6. composite solid electrolyte preparation method according to claim 1, it is characterised in that：Lanthanum salt is described in step (2)
Any one in lanthanum nitrate, lanthanum chloride, lanthanum sulfate.
7. composite solid electrolyte preparation method according to claim 1, it is characterised in that：Citric acid described in step (1)
It is (6.5-7) with metal cation molar ratio total in mixed liquor：1.
8. composite solid electrolyte preparation method according to claim 1, it is characterised in that：Citric acid described in step (2)：
Ethylene glycol：Total metal cation molar ratio is (6-7) in mixed liquor：(3.5-4)：1.
9. composite solid electrolyte preparation method according to claim 1, it is characterised in that：It is golden described in step (1) and (2)
After belonging to salt deionized water dissolving, respective concentration is respectively 0.8-1.5g/mL.
A kind of 10. complex solid being prepared using any one of the claim 1-9 composite solid electrolyte preparation methods
Electrolyte.
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| CN112194372A (en) * | 2020-10-08 | 2021-01-08 | 天津工业大学 | Glass-ceramic composite film solid garnet electrolyte and preparation method thereof |
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