CN107860674B - A kind of simple appraisal procedure of doping zirconic acid lanthanum base fuel battery electrolyte proton conductive - Google Patents
A kind of simple appraisal procedure of doping zirconic acid lanthanum base fuel battery electrolyte proton conductive Download PDFInfo
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Abstract
A kind of simple appraisal procedure of doping zirconic acid lanthanum base fuel battery electrolyte proton conductive, belongs to fuel battery electrolyte material Performance Evaluation technical field.The electrolyte be it is powdered, chemical formula be (1) La2Zr2‑yCayO7‑α, y=0.05,0.10,0.15 or 0.20；(2) La2Zr2‑xYxO7‑α, x=0.05,0.10,0.15,0.20 or 0.25；Specific step is as follows: being protonated using novel protonation reaction kettle to electrolyte；To the electrolyte sample thermogravimetric analysis after protonation.The invention has the advantages that novel protonation reaction kettle of the invention, electrolyte powder and water can be distinguished from, electrolyte powder could be contacted after liquid is water, cause contact area bigger in this way, reaction can be carried out more fully, the water needed can also greatly reduce, and be a kind of efficient, convenient and simple protonation techniques；The method of the present invention is realized in the case where directly not surveying conductivity, judges the ability of electric conductivity, has biggish feasibility and accuracy.
Description
Technical field
The invention belongs to fuel battery electrolyte material Performance Evaluation technical fields, and in particular to a kind of doping zirconic acid lanthanum base
The simple appraisal procedure of fuel battery electrolyte material proton conductive.
Background technique
Solid oxide fuel cell is applicable in all kinds of fuel gas, such as methane, coal gas etc., has high-conversion rate, high stability
The advantages that, thus be a kind of fuel cell of great development prospect.Wherein electrolyte is the core of fuel cell, current oxide
Ion-conducting electrolyte problems faced is exactly that operating temperature is excessively high (> 800 DEG C), only can just overcome ionic conduction at high temperature
Activation energy and realize diffusion mobility, seriously limit the use of solid oxide fuel cell.Because of the present circumstance, novel proton is led
Electric material causes everybody keen interest as Quality Research is electrolysed in fuel cell, and this kind of material has and proton (H+) move
The relatively low-activation energy moved and the higher conductivity in mesophilic range (200-500 DEG C), the zirconic acid lanthanum with pyrochlore constitution
Sill is considered as one of the candidate of high temperature and the conduction application of medium temperature proton, therefore, is led to zirconic acid lanthanum sill as proton
The feasibility study of body has great importance.
Proton conductor needs to work in the atmosphere existing for vapor, the oxonium ion in the presence of having water vapour, in hydrone
Become Lattice Oxygen into Lacking oxygen, two protons left become gap proton, migrate in lattice, proton conductive row occur
For.The condition that the test of conventional protic conductor conductivity needs is harsher, needs that gas is allowed to introduce the water into tube furnace or Muffle
In furnace, and need to carry out the test of AC impedance in the event of high temperatures, in addition, shadow of the consistency of electrolyte sheet to result
Sound is larger.
Summary of the invention
That the purpose of the present invention is to solve existing conventional protic conductor conductivity test conditions is harsh, to temperature requirement compared with
High problem provides a kind of doping zirconic acid lanthanum base fuel battery electrolyte proton conductive simple appraisal procedure, this method
The simple assessment of proton conductive is carried out by " protonation-thermogravimetric analysis " two-step method.
To achieve the above object, the technical solution adopted by the present invention is as follows:
A kind of simple appraisal procedure of doping zirconic acid lanthanum base fuel battery electrolyte proton conductive, the electrolysis material
Expect to be powdered, chemical formula is (1) La2Zr2-yCayO7-α, y=0.05,0.10,0.15 or 0.20；(2) La2Zr2-xYxO7-α, x=
0.05,0.10,0.15,0.20 or 0.25；
Specific step is as follows for the simple appraisal procedure:
Step 1: weighing 0.4-0.7g electrolyte and 0.3-0.5g distilled water, by distillation water droplet in novel protonation
In the blind hole of reaction kettle, electrolyte is placed in the annular groove around blind hole, sprawls uniformly, tightens novel protonation reaction
Novel protonation reaction kettle is placed in homogeneous reactor and reacts by kettle, temperature setting be 170 DEG C, keep for 24 hours to get
To the electrolyte sample of protonation；
Step 2: Instrument is reset, and 10 ~ 12 mg of electrolyte sample for the protonation for taking step 1 to obtain is placed on crucible
It is interior, then crucible is placed in Instrument, it under argon atmosphere, is started to warm up with the heating rate of 5 DEG C/min from 30 DEG C, tests model
It is trapped among between 30 ~ 600 DEG C, obtains thermogravimetric curve；In test process, purge gass and protection gas are opened, purge gass flow is 80
ML/min, protection air-flow amount are 20mL/min.
The beneficial effect of the present invention compared with the existing technology is:
(1) present invention selection proton conductor La2Zr2O7(A2B2O7) it is used as electrolyte material system, in B doping divalent sun
Ion Ca2+Or Tricationic Y3+, more Lacking oxygens are introduced after doping, the ability for introducing hydroxyl in lattice can be improved, into
And improve La2Zr2O7Protonated degree.
(2) the novel protonation reaction kettle that the present invention uses, electrolyte powder and water can be distinguished from, liquid aqueous vapor
Electrolyte powder could be contacted after change, causes contact area bigger in this way, and reaction can be carried out more fully, the water needed
It can greatly reduce, be a kind of efficient, convenient and simple protonation techniques.
(3) present invention carries out the assessment of proton conductive using " protonation-thermogravimetric analysis " two-step method, after protonation
Electrolyte powder, directly test thermogravimetric, realize not directly survey conductivity in the case where, judge the ability of electric conductivity, have
There are biggish feasibility and accuracy.
Detailed description of the invention
Fig. 1 is the novel protonation reaction kettle device structure chart that the present invention uses；
Wherein, 1 is annular groove, and 2 be blind hole, and 3 be shell of reactor, and 4 be reactor inner sleeve, and 5 be inner cover, and 6 be outer top cover；
Fig. 2 is La in embodiment 1,3,5,72Zr2-yCayO7-α, y=0.05,0.10,0.15,0.20, XRD spreads out after sintering
Penetrate figure；
Fig. 3 is La in embodiment 2,4,6,82Zr2-yCayO7-α, y=0.05,0.10,0.15,0.20, thermogravimetric after protonation
Curve graph；
Fig. 4 is La in comparative example 1,2,3,42Zr2-yCayO7-αSolid electrolyte sheet, y=0.05,0.10,0.15,0.20,
The Arrhenius curve graph of conductivity in humid air.
Specific embodiment
Further description of the technical solution of the present invention with reference to the accompanying drawings and examples, and however, it is not limited to this,
It is all that modifying or equivalently replacing the technical solution of the present invention, without departing from the spirit and scope of the technical solution of the present invention,
It should all cover within the protection scope of the present invention.
Specific embodiment 1: present embodiment record is a kind of doping zirconic acid lanthanum base fuel battery electrolyte matter
The simple appraisal procedure of subconductivity, the electrolyte be it is powdered, chemical formula be (1) La2Zr2-yCayO7-α, y=0.05,
0.10,0.15 or 0.20；(2) La2Zr2-xYxO7-α, x=0.05,0.10,0.15,0.20 or 0.25；
Specific step is as follows for the simple appraisal procedure:
Step 1: weighing 0.4-0.7g electrolyte and 0.3-0.5g distilled water, by distillation water droplet in novel protonation
In the blind hole 2 of reaction kettle, electrolyte is placed in the annular groove 1 around blind hole 2, sprawls uniformly, tightens novel protonation
Novel protonation reaction kettle is placed in homogeneous reactor and reacts by reaction kettle, and temperature setting is 170 DEG C, keeps for 24 hours,
The electrolyte sample protonated；
Step 2: Instrument is reset, and 10 ~ 12 mg of electrolyte sample for the protonation for taking step 1 to obtain is placed on crucible
It is interior, then crucible is placed in Instrument, it under argon atmosphere, is started to warm up with the heating rate of 5 DEG C/min from 30 DEG C, tests model
It is trapped among between 30 ~ 600 DEG C, obtains thermogravimetric curve；In test process, purge gass and protection gas are opened, purge gass flow is 80
ML/min, protection air-flow amount are 20mL/min.
Specific embodiment 2: a kind of doping zirconic acid lanthanum base fuel battery electrolyte described in specific embodiment one
The simple appraisal procedure of proton conductive, in step 2, the purge gass and protection gas are argon gas.
Specific embodiment 3: a kind of doping zirconic acid lanthanum base fuel battery electrolyte described in specific embodiment one or two
The simple appraisal procedure of material proton conductive, in step 1, the novel protonation reaction kettle includes shell of reactor 3, interior
Lid 5, outer top cover 6 and reactor inner sleeve 4；
3 shape of shell of reactor is cylindrical body, and 3 periphery upper end of shell of reactor is equipped with external screw thread, reactor
Reactor inner sleeve 4 is closely housed in shell 3, is equipped with groove, the middle part of the groove in the middle part of 4 top surface of reactor inner sleeve
Equipped with cylindrical boss one, the height of the cylindrical boss one is lower than the height of 4 top surface of reactor inner sleeve, cylindrical boss
Annular groove 1 is formed between one periphery and groove inner wall, the middle part of cylindrical boss one is equipped with blind hole 2,4 top surface of reactor inner sleeve
With 3 either flush of shell of reactor, the 6 inner headed face lower part of outer top cover is equipped with internal screw thread, and the inner cover 5 is mounted on outer top
Top in lid 6 is equipped with cylindrical boss two, the groove of the two insertion reaction device inner sleeve 4 of cylindrical boss in the middle part of inner cover 5
Interior, outer top cover 6 is threadedly coupled with shell of reactor 3.
Embodiment 1:
According to La2Zr1.95Ca0.05O7-αStoichiometric ratio, weigh 1.95 moles of Zr (NO3)4, 2 moles of La (NO3)3、
0.05 mole of Ca (NO3)2, be put into 250 mL beakers, with 100 mL deionized water dissolvings, then, according to metal ion 2:1
Ratio add citric acid (CA) complexing agent, it is heated, stir, be dissolved to clear solution, be put in water-bath in 80 DEG C of water-bath
4 hours, solution became thick clear gel, then put gel in a vacuum drying oven, adjusting vacuum degree to 0.1MPa,
It is 3 hours dry at 150 DEG C, obtain the loose white xerogel of material.Xerogel is fully ground into powder, is put into tube furnace
Middle N2600 DEG C of -5h of pre-burning in atmosphere sinter phase into then at 1000 DEG C of -10h, and La is made2Zr1.95Ca0.05O7-αElectrolyte powder.
The present embodiment prepares electrolyte powder material using sol-gal process, and this method, which has, to be uniformly distributed, sinters phase into
Temperature is low, stoichiometry is accurate, is easy to the advantages that being mass produced.
Embodiment 2:
Weigh the La of 0.6 g embodiment 1 preparation2Zr1.95 Ca 0.05O7-αElectrolyte powder, and 0.4 g of water is weighed, it uses
Novel protonation reaction kettle shown in FIG. 1, liquid water are placed in blind hole 2, and powder is placed in 2 peripheral circular slot 1 of blind hole, and in equal
It is reacted in phase reaction device.Reaction temperature is 170 DEG C, and the reaction time is that for 24 hours, obtained product is warm within the scope of 20-600 DEG C
Weight analysis.
Embodiment 3:
According to La2Zr1.95Ca0.10O7-αStoichiometric ratio, weigh 1.95 moles of Zr (NO3)4, 2 moles of La (NO3)3、
0.10 mole of Ca (NO3)2, be put into 250 mL beakers, with 100 mL deionized water dissolvings, then, according to metal ion 2:1
Ratio add citric acid (CA) complexing agent, it is heated, stir, be dissolved to clear solution, be put in water-bath in 80 DEG C of water-bath
4 hours, solution became thick clear gel, then put gel in a vacuum drying oven, adjusted vacuum degree to 0.1, In
150 DEG C drying 3 hours, obtain the loose white xerogel of material.Xerogel is fully ground into powder, is put into tube furnace
N2600 DEG C of -5h of pre-burning in atmosphere sinter phase into then at 1000 DEG C of -10h, and La is made2Zr1.95Ca0.10O7-αElectrolyte powder.
Embodiment 4:
Weigh the La of 0.6 g embodiment 3 preparation2Zr1.95Ca0.10O7-αElectrolyte powder, and weigh 0.4 g of water, liquid water
It is placed in blind hole 2, powder is placed in 2 peripheral circular slot 1 of blind hole, and is reacted in homogeneous reactor.Reaction temperature is 170
DEG C, the reaction time is obtained product thermogravimetric analysis within the scope of 20-600 DEG C for 24 hours.
Embodiment 5:
According to La2Zr1.95Ca0.15O7-αStoichiometric ratio, weigh 1.95 moles of Zr (NO3)4, 2 moles of La (NO3)3、
0.15 mole of Ca (NO3)2, be put into 250 mL beakers, with 100 mL deionized water dissolvings, then, according to metal ion 2:1
Ratio add citric acid (CA) complexing agent, it is heated, stir, be dissolved to clear solution, be put in water-bath in 80 DEG C of water-bath
4 hours, solution became thick clear gel, then put gel in a vacuum drying oven, adjusted vacuum degree to 0.1, In
150 DEG C drying 3 hours, obtain the loose white xerogel of material.Xerogel is fully ground into powder, is put into tube furnace
N2600 DEG C of -5h of pre-burning in atmosphere sinter phase into then at 1000 DEG C of -10h, and La is made2Zr1.95Ca0.15O7-αElectrolyte powder.
Embodiment 6:
Weigh the La of 0.6 g embodiment 5 preparation2Zr1.95 Ca 0.15O7-αElectrolyte powder, and weigh 0.4 g of water, liquid
Water is placed in blind hole 2, and powder is placed in 2 peripheral circular slot 1 of blind hole, and is reacted in homogeneous reactor.Reaction temperature is
170 DEG C, the reaction time is obtained product thermogravimetric analysis within the scope of 20-600 DEG C for 24 hours.
Embodiment 7:
According to La2Zr1.95Ca0.20O7-αStoichiometric ratio, weigh 1.95 moles of Zr (NO3)4, 2 moles of La (NO3)3、
0.20 mole of Ca (NO3)2, be put into 250 mL beakers, with 100 mL deionized water dissolvings, then, according to metal ion 2:1
Ratio add citric acid (CA) complexing agent, it is heated, stir, be dissolved to clear solution, be put in water-bath in 80 DEG C of water-bath
4 hours, solution became thick clear gel, then put gel in a vacuum drying oven, adjusted vacuum degree to 0.1, In
150 DEG C drying 3 hours, obtain the loose white xerogel of material.Xerogel is fully ground into powder, is put into tube furnace
N2600 DEG C of -5h of pre-burning in atmosphere sinter phase into then at 1000 DEG C of -10h, and La is made2Zr1.95Ca0.20O7-αElectrolyte powder.
Embodiment 8:
Weigh the La of 0.6 g embodiment 7 preparation2Zr1.95 Ca 0.20O7-αElectrolyte powder, and weigh 0.4 g of water, liquid
Water is placed in blind hole 2, and powder is placed in 2 peripheral circular slot 1 of blind hole, and is reacted in homogeneous reactor.Reaction temperature is
170 DEG C, the reaction time is obtained product thermogravimetric analysis within the scope of 20-600 DEG C for 24 hours.
Fig. 2 is La in embodiment 1,3,5,72Zr2-yCayO7-α, y=0.05,0.10,0.15,0.20, XRD spreads out after sintering
Figure is penetrated, by Ca2+Dopant material sinters the XRD characterization result after phase into and standard card compares, it can be seen that peak type and position
Set basic and La2Zr2O7Standard PDF card it is consistent, it was demonstrated that the product after being sintered meets the requirements, and gently towards low-angle
Offset more obviously, illustrates to adulterate Ca in y=0.102+It equally will increase lattice parameter.
Fig. 3 is La in embodiment 2,4,6,82Zr2-yCayO7-α, y=0.05,0.10,0.15,0.20, thermogravimetric after protonation
Curve graph can be seen that with doping Ca2+Increase, fluid loss first increases, in 0.10 Ca2+Place reaches maximum, then begins to
Decline, 0.20 Ca2+Weight loss is close to 0.05 Ca2+Place, illustrate that higher doping can not be obviously improved protonation journey
Degree.
Comparative example 1:
Weigh the La of the preparation of 0.3g embodiment 12Zr1.95Ca0.05O7-αPowder is placed in mold, is protected under 20 Mpa pressure
Hold 5 min compression mouldings.Electrolyte sheet after molding is sintered 1000 DEG C of -10h in air.Then polishing surface polishes,
Filamentary silver is sticked on electrolyte sheet with high-temperature repairing agent, dries 120 DEG C of -2h in an oven, coats silver paste, 600 DEG C of sintering-later
3h.The solid electrolyte piece coated after silver paste is placed in tube furnace, in humid air atmosphere, using two-terminal electricity
Pole method measures the electrochemical impedance spectroscopy of sample, and by being fitted map, La is calculated by correlation formula2Zr1.95Ca0.05O7-αElectricity
Conductance.
Comparative example 2:
Weigh the La of the preparation of 0.3g embodiment 32Zr1.95Ca0.10O7-αPowder is placed in mold, is protected under 20 Mpa pressure
Hold 5 min compression mouldings.Electrolyte sheet after molding is sintered 1000 DEG C of -10h in air.Then polishing surface polishes,
Filamentary silver is sticked on electrolyte sheet with high-temperature repairing agent, dries 120 DEG C of -2h in an oven, coats silver paste, 600 DEG C of sintering-later
3h.The solid electrolyte piece coated after silver paste is placed in tube furnace, in humid air atmosphere, using two-terminal electricity
Pole method measures the electrochemical impedance spectroscopy of sample, and by being fitted map, La is calculated by correlation formula2Zr1.95Ca10O7-αElectricity
Conductance.
Comparative example 3:
Weigh the La of the preparation of 0.3g embodiment 52Zr1.95Ca0.15O7-αPowder is placed in mold, is protected under 20 Mpa pressure
Hold 5 min compression mouldings.Electrolyte sheet after molding is sintered 1000 DEG C of -10h in air.Then polishing surface polishes,
Filamentary silver is sticked on electrolyte sheet with high-temperature repairing agent, dries 120 DEG C of -2h in an oven, coats silver paste, 600 DEG C of sintering-later
3h.The solid electrolyte piece coated after silver paste is placed in tube furnace, in humid air atmosphere, using two-terminal electricity
Pole method measures the electrochemical impedance spectroscopy of sample, and by being fitted map, La is calculated by correlation formula2Zr1.95Ca0.15O7-αElectricity
Conductance.
Comparative example 4:
Weigh the La of the preparation of 0.3g embodiment 72Zr1.95Ca0.20O7-αPowder is placed in mold, is protected under 20 Mpa pressure
Hold 5 min compression mouldings.Electrolyte sheet after molding is sintered 1000 DEG C of -10h in air.Then polishing surface polishes,
Filamentary silver is sticked on electrolyte sheet with high-temperature repairing agent, dries 120 DEG C of -2h in an oven, coats silver paste, 600 DEG C of sintering-later
3h.The solid electrolyte piece coated after silver paste is placed in tube furnace, in humid air atmosphere, using two-terminal electricity
Pole method measures the electrochemical impedance spectroscopy of sample, and by being fitted map, La is calculated by correlation formula2Zr1.95Ca0.20O7-αElectricity
Conductance.
Fig. 4 is La in comparative example 1,2,3,42Zr2-yCayO7-αSolid electrolyte sheet, y=0.05,0.10,0.15,0.20,
The Arrhenius curve graph of conductivity in humid air.In Ca2+Doping is to La2Zr2O7In the influence of conductivity, with Ca2+It mixes
Miscellaneous increase, the conductance of solid electrolyte take the lead in reducing after increasing, and in y=0.10, that is, doping is 0.10 Ca2+, conductance
Rate reaches maximum.With Ca2+Protonation after Thermogravimetric Data trend match, this shows " protonation-thermogravimetric analysis " two step proton
The simple appraisal procedure of electric conductivity is accurately, can to judge its matter under the premise of not surveying the conductivity of solid electrolyte sheet directly
Sonization and conductive capability size.
The present invention devises " protonation-thermogravimetric analysis " two simple appraisal procedure of step proton conductive, after protonating
Electrolyte powder, directly test thermogravimetric can be seen that the electrolyte of doped chemical by more than analysis embodiment and comparative example
The ratio and doping that powder loses water are there are trend relationship, in conjunction with the conductivity for testing solid electrolyte piece under the same terms,
It was found that the size of conductivity matches with the number of dehydration, i.e., the electrolyte powder more than dehydration be made into electrolyte sheet after conductivity just
Greatly, vice versa.This method can not directly survey conductivity in the case where, judge the ability of electric conductivity, have it is biggish can
Row and accuracy.
Claims (2)
1. a kind of simple appraisal procedure of doping zirconic acid lanthanum base fuel battery electrolyte proton conductive, it is characterised in that: institute
Stating electrolyte is powdered, chemical formula La2Zr2-yCayO7-α, y=0.05,0.10,0.15 or 0.20；
Specific step is as follows for the simple appraisal procedure:
Step 1: weighing 0.4 ~ 0.7g electrolyte and 0.3 ~ 0.5g distilled water, by distillation water droplet in novel protonation reaction
In the blind hole (2) of kettle, electrolyte is placed in the annular groove (1) around blind hole (2), sprawls uniformly, tightens novel proton
Change reaction kettle, novel protonation reaction kettle is placed in homogeneous reactor and is reacted, temperature setting is 170 DEG C, is kept
For 24 hours to get the electrolyte sample for arriving protonation；
The novel protonation reaction kettle includes shell of reactor (3), inner cover (5), outer top cover (6) and reactor inner sleeve (4)；
Shell of reactor (3) shape is cylindrical body, and shell of reactor (3) periphery upper end is equipped with external screw thread, shell of reactor
(3) reactor inner sleeve (4) closely are housed in, are equipped with groove in the middle part of described reactor inner sleeve (4) top surface, in the groove
Portion is equipped with cylindrical boss one, and the height of the cylindrical boss one is lower than the height of reactor inner sleeve (4) top surface, cylindrical
Annular groove (1) is formed between one periphery of boss and groove inner wall, the middle part of cylindrical boss one is equipped with blind hole (2), reactor
Inner sleeve (4) top surface and shell of reactor (3) either flush, outer top cover (6) the inner headed face lower part is equipped with internal screw thread, described
Inner cover (5) is mounted on the top in outer top cover (6), is equipped with cylindrical boss two, the cylindrical boss two in the middle part of inner cover (5)
In the groove of insertion reaction device inner sleeve (4), outer top cover (6) is threadedly coupled with shell of reactor (3)；
Step 2: Instrument is reset, and the 10 ~ 12mg of electrolyte sample for the protonation for taking step 1 to obtain is placed in crucible, then
Crucible is placed in Instrument, under argon atmosphere, is started to warm up with the heating rate of 5 DEG C/min from 30 DEG C, test scope exists
Between 30 ~ 600 DEG C, thermogravimetric curve is obtained；In test process, purge gass and protection gas are opened, purge gass flow is 80mL/min,
Protection air-flow amount is 20mL/min；
Step 3: the electrolyte powder after protonating, directly test thermogravimetric, the electrolyte powder of doped chemical lose the ratio of water
Example and doping in conjunction with the conductivity for testing solid electrolyte piece under the same terms, find the big of conductivity there are trend relationship
Small to match with the number of dehydration, i.e., conductivity is just big after the electrolyte powder more than dehydration is made into electrolyte sheet, and vice versa.
2. a kind of doping zirconic acid lanthanum base fuel battery electrolyte proton conductive according to claim 1 is simply assessed
Method, it is characterised in that: in step 2, the purge gass and protection gas are argon gas.
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