CN103165930A - Method for Improving Sintering Performance of Proton Conductor Solid Oxide Fuel Cell Electrolyte - Google Patents
Method for Improving Sintering Performance of Proton Conductor Solid Oxide Fuel Cell Electrolyte Download PDFInfo
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- CN103165930A CN103165930A CN2013100987663A CN201310098766A CN103165930A CN 103165930 A CN103165930 A CN 103165930A CN 2013100987663 A CN2013100987663 A CN 2013100987663A CN 201310098766 A CN201310098766 A CN 201310098766A CN 103165930 A CN103165930 A CN 103165930A
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Abstract
本发明属于固体氧化物燃料电池（SOFC）电解质材料领域，具体涉及一种提高质子导体氧化物燃料电池电解质烧结性能的方法，可用于制备高温质子导体的致密的电解质。其具体步骤如下：A、用干压的方法将电解质粉体制备成具有多孔骨架结构的高温质子导体坯体；B、制备烧结助剂溶液，并用微量注射器向步骤A制得的高温质子导体坯体中浸渍烧结助剂溶液；C、将浸渍烧结助剂溶液的高温质子导体坯体放入马弗炉中进行焙烧，得到了致密的电解质层。此方法制作工艺简单，免除了高温烧结制备多孔骨架的步骤，节约了能源和制备时间，并且省去了传统方法中在粉体合成过程中添加烧结助剂进行预混合和的步骤，能够使烧结助剂均匀的分散于质子导体电解质材料中。The invention belongs to the field of solid oxide fuel cell (SOFC) electrolyte materials, and in particular relates to a method for improving the sintering performance of the proton conductor oxide fuel cell electrolyte, which can be used to prepare dense electrolytes for high-temperature proton conductors. The specific steps are as follows: A. Prepare the electrolyte powder into a high-temperature proton conductor green body with a porous skeleton structure by dry pressing; B. Prepare a sintering aid solution and inject it into the high-temperature proton conductor green body prepared in step A with a micro-injector. Immerse the sintering aid solution in the body; C. put the high-temperature proton conductor body impregnated with the sintering aid solution into a muffle furnace for roasting, and obtain a dense electrolyte layer. This method has a simple manufacturing process, eliminates the step of high-temperature sintering to prepare the porous skeleton, saves energy and preparation time, and eliminates the step of adding sintering aids for pre-mixing and mixing during the powder synthesis process in the traditional method, enabling sintering The auxiliary agent is uniformly dispersed in the proton conductor electrolyte material.
Description
Technical field
The invention belongs to field of solid oxide fuel, a kind of method that improves proton conductor oxide fuel battery electrolyte sintering character can be used for preparing the electrolyte of the densification of high-temperature proton-conductor.
Background technology
Solid Oxide Fuel Cell (SOFC) is a kind of energy conversion device of efficient, cleaning.It is electrolyte that traditional SOFC technology is based on YSZ, and this needs higher operating temperature greatly about 800～1000 ° of C.This higher operating temperature has been brought larger obstruction to the practical application of SOFC, such as the demand to expensive material, and long start-up time and higher heat energy life-span that can reduce battery.So the research tendency in this field is to pursue temperatureization in operating temperature, with all technology and the material difficulty that overcomes conventional high-temperature SOFC.The operating temperature that reduces SOFC not only can also be conducive to develop portable SOFC by Cost reduction.In attempting developing the SOFC process that to work in mesophilic range (500～700 ° of C), need to reduce electrolytical ohmage.Therefore, High-temperature proton conductor material has caused every researcher's great interest in the last few years.The high-temperature proton-conductor electrolyte has higher proton conductivity in the atmosphere of hydrogen or humidification hydrogen, especially have lower activation energy at the traditional oxygen ion conductor of mesophilic range internal ratio.
BaZrO
3Base oxide is a kind of electrolyte with development prospect of proton conductor oxide fuel cell, and it has higher ionic conductivity and for the CO in fuel atmosphere
2And H
2O has chemical stability preferably.In order to reduce BaZrO
3The sintering temperature of base oxide material, researchers have taked a lot of methods to improve its sintering character, such as other elements of doping reduce the ratio of Zr element, appropriate Ba is more than needed or defective, to BaZrO
3Add the methods such as sintering aid in base oxide material.Structure, double-layer tablet sintering character that but there is complex manufacturing process in above method, can destroy material such as do not mate at the shortcoming.Sintering aid commonly used has ZnO, CuO and NiO etc.Studies show that adding a small amount of metal oxide can reduce by 150～250 ° of C with its sintering temperature in the middle of material.Wherein Zn is considered to a kind of and can improves BaZrO
3The desirable auxiliary agent of base oxide High-temperature proton conductor material sintering character.But, directly use preparation method's more complicated of the method interpolation sintering aid of metal oxide and electrolyte mechanical mixture, the electrolyte for preparing easily ftractures later on through roasting, and metal ion can enter into the lattice of electrolyte, thereby reduces the conductivity of electrolyte.
Summary of the invention
The objective of the invention is in order to solve BaZrO
3The sintering character of base high-temperature proton-conductor electrolyte is poor, and the electrolyte densified sintering product needs higher temperature, and a kind of method that improves proton conductor oxide fuel battery electrolyte sintering character.And the method is not used other auxiliary equipment complicated and high price in preparation process, thereby technique simply is easy to repeat preparation.
Technical scheme of the present invention is: a kind of method that improves proton conductor oxide fuel battery electrolyte sintering character, can be used for preparing the electrolyte of the densification of high-temperature proton-conductor, its concrete steps are as follows: A, the electrolyte powder body is prepared into the high-temperature proton-conductor base substrate with porous skeleton structure with the method for dry-pressing; B, preparation sintering aid solution, and impregnation sintering compounding agent solution in the high-temperature proton-conductor base substrate that makes to steps A with micro syringe; C, the high-temperature proton-conductor base substrate of impregnation sintering compounding agent solution is put into Muffle furnace carry out roasting, obtained fine and close dielectric substrate.
The structural formula of preferred described electrolyte powder is BaZrO
3Or BaZr
0.8-xM
xY
0.2O
3-δ, wherein M=La, Ce, Pr, Nd, Sm, Eu, Gd, Yb, In, 0≤x≤0.8.
Preferred sintering aid solution is Zn (NO
3)
2, Cu (NO
3)
2Or Ni (NO
3)
2Ethanol solution, wherein to belong to the concentration of ion be 0.02～0.2mol L to the sintering aid GOLD FROM PLATING SOLUTION
-1It is characterized in that making solvent with absolute ethyl alcohol volatile, and the wetability of ethanol is good, large in the contact angle of solid phase surface, more easily be penetrated among porous skeleton structure, sintering aid is distributed more even.The pickup of sintering aid solution is 3%～8% of green body quality for the quality of controlling metal ion in sintering aid.
The pressure position 150～300MPa of preferred dry pressing pressing blank.The porosity of the high-temperature proton-conductor base substrate of dry-pressing formed porous skeleton structure is 65%～75%.
The sintering temperature of preferred high-temperature proton-conductor base substrate is 1150～1400 ° of C, and roasting time is 2～6 hours.
Immersion tool of the present invention is to use market accurate micro syringe on sale.
High-temperature proton-conductor oxide of the present invention, its synthetic method are sol-gel process, and its detailed process can be referring to document (W.Zhou, Z.P.Shao, R.Ran, R.Cai, Novel, Electrochem.Commun.10 (2008).
Beneficial effect:
The density of the resulting high-temperature proton-conductor electrolyte of the present invention has reached 93%～98%, and the temperature of material densified sintering product has been reduced by 150～250 ° of C, prepared the thin-film electrolyte structure of anode support type by the method for infusion process and multiple dry-pressing.
Description of drawings
Fig. 1 is that the later BZCY1 material of the dipping Zn of embodiment 1 is at 1150 ° of XRD collection of illustrative plates that the C roasting is later;
The section S EM figure that Fig. 2 is the later BZCY4 base substrate of the dipping Zn sintering aid of embodiment 1 after 1150 ° of C roastings 5 hours;
Fig. 3 is the section S EM figure take the later BZCY4 of dipping Zn as the Solid Oxide Fuel Cell of electrolytical anode support type of embodiment 4;
Fig. 4 is the battery performance figure take the later BZCY4 of dipping Zn as the Solid Oxide Fuel Cell of electrolytical anode support type of embodiment 4;
Fig. 5 is the Solid Oxide Fuel Cell chemical impedance spectrum take the later BZCY4 of dipping Zn as electrolytical anode support type of embodiment 4;
Fig. 6 be embodiment 5 for not flooding the sintering curre of BZCY6 material of Zn and dipping 4wt%Zn.
Embodiment
Method involved in the present invention comprises but is not limited to material in following examples.
Embodiment 1: with BaZr
0.1Ce
0.7Y
0.2O
3-δ(BZCY1) material is bone porous base substrate, adds the Zn sintering aid with the method for dipping to it.
(1) prepare BaZr with sol-gel process
0.1Ce
0.7Y
0.2O
3-δPowder: the preparation method of powder adopts sol-gel complexing method commonly used, its detailed process can be referring to document (W.Zhou, Z.P.Shao, R.Ran, R.Cai, Novel, Electrochem.Commun.10 (2008) 1647 – 1651), recently determine the consumption of raw material according to the stoichiometry of BZCY1 material.
(2) preparation Zn (NO
3)
2Ethanolic solution: take appropriate Zn (NO
3)
2Join in beaker, then add absolute ethyl alcohol in beaker, use at last the volumetric flask constant volume, the solubility of solution is 0.02mol L
-1
(3) the bone porous electrolyte base substrate of preparation: the BZCY1 powder of getting 0.5g is put in stainless cylindrical mould, is pressed into columniform porous green compact body under 300MPa, and relative density is 70%.
(4) dipping Zn sintering aid solution is to having in bone porous base substrate: the stephanoporate framework base substrate of BZCY1 is placed on experimental bench, then uses the accurate syringe of trace with Zn (NO
3)
2Ethanolic solution join in the middle of stephanoporate framework, the quality of the Zn of dipping is 3% of green body quality, after the alcohol solvent volatilization is complete, the base substrate that dipping is completed is put into Muffle furnace obtains densification after roasting 5h under 1150 ° of C electrolyte sheet, and the relative density that uses Archimedes's draining measurement to record is 97.6%.
Fig. 1 shows that for the base substrate later XRD spectra of roasting 5h under 1150 ° of C of the BZCY1 after flooding material has still kept stable perovskite structure, does not destroy original structure because of adding of Zn.
Fig. 2 floods the section S EM figure of the later BZCY1 base substrate of Zn sintering aid after 1150 ° of C roastings 5 hours, show to add 3wt%Zn can increase substantially the sintering character of material as sintering aid in BZCY1, just can obtain fine and close electrolyte sheet at 1150 ° of C.
Embodiment 2: with BaZr
0.1Ce
0.7Y
0.2O
3-δ(BZCY1) material is bone porous base substrate, adds the Ni sintering aid with the method for dipping to it.
(1) with the method in embodiment 1 (1).
(2) preparation Ni (NO
3)
2Ethanolic solution: take appropriate Ni (NO
3)
2Join in beaker, then add absolute ethyl alcohol in beaker, use at last the volumetric flask constant volume, the solubility of solution is 0.01mol L
-1.
(3) with the method in embodiment 1 (3).
(4) dipping Ni sintering aid solution is to having in bone porous base substrate: the stephanoporate framework base substrate of BZCY1 is placed on experimental bench, then uses the accurate syringe of trace with Ni (NO
3)
2Ethanolic solution join in the middle of stephanoporate framework, the quality of the Ni of dipping is 4% of green body quality, after the alcohol solvent volatilization is complete, the base substrate that dipping is completed is put into Muffle furnace obtains densification after roasting 5h under 1150 ° of C electrolyte sheet, and the relative density that uses Archimedes's draining measurement to record is 96.8%.。
Embodiment 3: with BaZr
0.8Y
0.2O
3-δ(BZY8) material is bone porous base substrate, adds the Cu sintering aid with the method for dipping to it.
(1) prepare BaZr with sol-gel process
0.8Y
0.2O
3-δPowder: the preparation method of powder adopts sol-gel complexing method commonly used, its detailed process can be referring to document (W.Zhou, Z.P.Shao, R.Ran, R.Cai, Novel, Electrochem.Commun.10 (2008) 1647 – 1651), recently determine the consumption of raw material according to the stoichiometry of BZY8 material.
(2) preparation Cu (NO
3)
23H
2The ethanolic solution of O: take appropriate Cu (NO
3)
2Join in beaker, then add absolute ethyl alcohol in beaker, use at last the volumetric flask constant volume, the solubility of solution is 0.2mol L
-1
(3) the bone porous electrolyte base substrate of preparation: the BZY8 powder of getting 0.5g is put in stainless cylindrical mould, is pressed into columniform porous green compact body under 150MPa, and relative density is 65%.
(4) dipping Cu sintering aid solution is to having in bone porous base substrate: the stephanoporate framework base substrate of BZY8 is placed on experimental bench, then uses the accurate syringe of trace with Cu (NO
3)
2Ethanolic solution join in the middle of stephanoporate framework, the quality of the Cu of dipping is 8% of green body quality, after the alcohol solvent volatilization is complete, the base substrate that dipping is completed is put into Muffle furnace obtains densification after roasting 3h under 1400 ° of C electrolyte sheet, and the relative density that uses Archimedes's draining measurement to record is 95.7%.。
Embodiment 4: with the BaZr of dipping Zn sintering aid
0.4Ce
0.4Y
0.2O
3-δ(BZCY4) be the application of electrolytical proton conductor oxide fuel cell
(1) preparation of anode-supported monocell: the anode support type monocell adopts the method preparation of dry-pressing-co-sintering.Now the BZCY4 powder mixed according to the ratio of mass ratio 4:6 and adds appropriate ethanol with the NiO powder, taking out and dry after the rotating speed ball milling 30min with 400rmp in high-energy ball milling, obtaining required anode powder.Taking 0.4g anode powder is to be to suppress under 100MPa at pressure in the stainless steel mould of 15mm at diameter, then the BZCY4 electrolyte powder that takes 0.02g is layered on anode substrate equably, presses altogether the anode that obtains anode support type-double-deck base substrate of electrolyte under 300MPa pressure.
(2) preparation Zn (NO
3)
2Ethanolic solution: take appropriate Zn (NO
3)
2Join in beaker, then add absolute ethyl alcohol in beaker, use at last the volumetric flask constant volume, the solubility of solution is 0.1mol L
-1
(3) base substrate with preparation in step (1) is placed on smooth experimental bench, then thinks base substrate electrolyte one side dipping Zn (NO with accurate micro syringe
3)
2Ethanolic solution, in the sintering aid of dipping, the quality of Zn is the 5wt% of electrolyte quality, after alcohol solvent volatilization was complete, the base substrate that dipping is completed was put into Muffle furnace and is being obtained the bilayer cells sheet after roasting 5h under 1400 ° of C.
(4) Ba
0.5Sr
0.5Co
0.8Fe
0.2O
3-δ(BSCF) preparation of cathode slurry and spraying: a certain amount of ethylene glycol, isopropyl alcohol and glycerine are joined in BSCF cathode powder with sol-gel process preparation, with in high-energy ball milling under the rotating speed of 400rmp ball milling 40min make cathode slurry.Then pulp spraying is coated in the electrolyte one side of the double-layer tablet of preparation in step (3), and under 1000 ° of C roasting 2h.Use the elargol of dilution and silver-colored line respectively as current collector and the wire of electrode.
(5) test of battery: the marking of cell piece is exposed in air, act as a fuel with the wet hydrogen of humidification 3% and pass into anode one side, the digital instrument that adopts computer to control records I-V and the I-P curve of battery, the flow of hydrogen is controlled by flow controller, with the AC impedance spectrogram of Impedance Analysis instrument test electrical measurement under open circuit.
Fig. 3 can find out that for the section S EM figure after testing take 5%Zn-BZCY4 as electrolytical monocell dielectric substrate is very fine and close, can satisfy the requirement of battery testing.
Fig. 4 is I-V and I-P curve take 5wt%Zn-BZCY4 as electrolytical monocell, and when 700 ° of C, the OCV of battery is 0.96V, and performance is 325mW cm
-2
Fig. 5 is take 5wt%Zn-BZCY4 as electrolytical monocell electrochemical impedance spectrogram.
Embodiment 5: the BaZr of dipping Zn sintering aid
0.6Pr
0.2Y
0.2O
3-δ(BZPY6) sintering curre after
(1) prepare BaZr with sol-gel process
0.6Pr
0.2Y
0.2O
3-δPowder: the preparation method of powder adopts sol-gel complexing method commonly used, its detailed process can be referring to document (W.Zhou, Z.P.Shao, R.Ran, R.Cai, Novel, Electrochem.Commun.10 (2008) 1647 – 1651), recently determine the consumption of raw material according to the stoichiometry of BZPY6 material.
(2) preparation Zn (NO
3)
2Ethanolic solution: take appropriate Zn (NO
3)
2Join in beaker, then add absolute ethyl alcohol in beaker, use at last the volumetric flask constant volume, the solubility of solution is 0.2mol L
-1
(3) the bone porous electrolyte base substrate of preparation: the BZPY6 powder of getting 0.5g is put in stainless cylindrical mould, is pressed into columniform porous green compact body under 150MPa, and relative density is 71%.
(4) dipping Zn sintering aid solution is to having in bone porous base substrate: the stephanoporate framework base substrate of BZCY6 is placed on experimental bench, then uses the accurate syringe of trace with Zn (NO
3)
2Ethanolic solution join in the middle of stephanoporate framework, the quality of the Zn of dipping is 7% of green body quality.
(5) test of sintering curre: the BZCY6 base substrate that will flood the Zn sintering aid and not flood the Zn sintering aid adopts thermal dilatometer to study its sintering curre, and temperature range is by room temperature to 1400 ° C, and sintering time is 5 hours.
Fig. 6 is the sintering curre that flooded the Zn sintering aid and do not flood Zn sintering aid BZCY6 base substrate, can find to have increased significantly through the sintering character of BZCY6 material after flooding.
Embodiment 6: with BaZrO
3Material is bone porous base substrate, adds the Zn sintering aid with the method for dipping to it.
(1) use sol-gel process BaZrO
3Powder: the preparation method of powder adopts sol-gel complexing method commonly used, its detailed process can be referring to document (W.Zhou, Z.P.Shao, R.Ran, R.Cai, Novel, Electrochem.Commun.10 (2008) 1647 – 1651), recently determine the consumption of raw material according to the stoichiometry of powder body material.
(2) preparation Zn (NO
3)
2Ethanolic solution: take appropriate Zn (NO
3)
2Join in beaker, then add absolute ethyl alcohol in beaker, use at last the volumetric flask constant volume, the solubility of solution is 0.02mol L
-1
(3) the bone porous electrolyte base substrate of preparation: the BaZrO that gets 0.5g
3Powder is put in stainless cylindrical mould, is pressed into columniform porous green compact body under 150MPa, and relative density is 70%.
(4) dipping Zn sintering aid solution is to having in bone porous base substrate: with BaZrO
3The stephanoporate framework base substrate be placed on experimental bench, then use the trace accurate syringe with Zn (NO
3)
2Ethanolic solution join in the middle of stephanoporate framework, the quality of the Zn of dipping is 3% of green body quality, after the alcohol solvent volatilization is complete, the base substrate that dipping is completed is put into Muffle furnace obtains densification after roasting 3h under 1400 ° of C electrolyte sheet, and the relative density that uses Archimedes's draining measurement to record is 96.3%.
Embodiment 7: with BaZr
0.7Nd
0.1Y
0.2O
3-δ(BZNY7) material is bone porous base substrate, adds the Ni sintering aid with the method for dipping to it.
(1) prepare BaZr with sol-gel process
0.7Nd
0.1Y
0.2O
3-δPowder: the preparation method of powder adopts sol-gel complexing method commonly used, its detailed process can be referring to document (W.Zhou, Z.P.Shao, R.Ran, R.Cai, Novel, Electrochem.Commun.10 (2008) 1647 – 1651), recently determine the consumption of raw material according to the stoichiometry of BZNY7 material.
(2) preparation Ni (NO
3)
2Ethanolic solution: take appropriate Ni (NO
3)
2Join in beaker, then add absolute ethyl alcohol in beaker, use at last the volumetric flask constant volume, the solubility of solution is 0.01mol L
-1.
(3) with the method in embodiment 1 (3).
(4) dipping Ni sintering aid solution is to having in bone porous base substrate: the stephanoporate framework base substrate of BZNY7 is placed on experimental bench, then uses the accurate syringe of trace with Ni (NO
3)
2Ethanolic solution join in the middle of stephanoporate framework, the quality of the Ni of dipping is 4% of green body quality, after the alcohol solvent volatilization is complete, the base substrate that dipping is completed is put into Muffle furnace obtains densification after roasting 6h under 1350 ° of C electrolyte sheet, and the relative density that uses Archimedes's draining measurement to record is 95.8%.
Claims (6)
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103825039A (en) * | 2014-02-27 | 2014-05-28 | 盐城工学院 | Electrolyte material and preparation method for intermediate and low-temperature solid oxide fuel cells |
| CN106602136A (en) * | 2016-12-22 | 2017-04-26 | 中国矿业大学 | Barium zirconate-based electrolyte material system and preparation method thereof |
| CN109346752A (en) * | 2018-09-11 | 2019-02-15 | 山西大学 | A kind of preparation method of electrolyte-supported solid oxide fuel cell zirconium-based electrolyte membrane |
| CN110224146A (en) * | 2019-05-23 | 2019-09-10 | 湖北大学 | A kind of online densifying method of fuel-cell electrolyte low temperature |
| CN111732434A (en) * | 2020-07-07 | 2020-10-02 | 韶关学院 | A kind of ceramic preparation method using in-situ generated oxide as sintering aid |
| WO2024012802A1 (en) * | 2022-07-11 | 2024-01-18 | Forschungszentrum Jülich GmbH | Production of a component with a gas-tight ion-conducting functional layer, and component |
| CN117466652A (en) * | 2023-10-11 | 2024-01-30 | 山东科技大学 | A preparation method for improving the stability of proton conductor electrolyte in carbon dioxide |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103825039A (en) * | 2014-02-27 | 2014-05-28 | 盐城工学院 | Electrolyte material and preparation method for intermediate and low-temperature solid oxide fuel cells |
| CN106602136A (en) * | 2016-12-22 | 2017-04-26 | 中国矿业大学 | Barium zirconate-based electrolyte material system and preparation method thereof |
| CN109346752A (en) * | 2018-09-11 | 2019-02-15 | 山西大学 | A kind of preparation method of electrolyte-supported solid oxide fuel cell zirconium-based electrolyte membrane |
| CN110224146A (en) * | 2019-05-23 | 2019-09-10 | 湖北大学 | A kind of online densifying method of fuel-cell electrolyte low temperature |
| CN111732434A (en) * | 2020-07-07 | 2020-10-02 | 韶关学院 | A kind of ceramic preparation method using in-situ generated oxide as sintering aid |
| WO2024012802A1 (en) * | 2022-07-11 | 2024-01-18 | Forschungszentrum Jülich GmbH | Production of a component with a gas-tight ion-conducting functional layer, and component |
| CN117466652A (en) * | 2023-10-11 | 2024-01-30 | 山东科技大学 | A preparation method for improving the stability of proton conductor electrolyte in carbon dioxide |
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Application publication date: 20130619 |