CN103378364A - Composite electrolyte material based on zirconium oxide based oxide - Google Patents
Composite electrolyte material based on zirconium oxide based oxide Download PDFInfo
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Abstract
The invention relates to a composite electrolyte material based on a zirconium oxide based oxide for a solid oxide fuel battery. The composite electrolyte material is characterized by being prepared by steps of adequately grinding and sintering the zirconium oxide based oxide, inorganic slat, and/or other oxides or an oxide-doped mixture after thermal treatment. The composite electrolyte material provided by the invention has the advantages that the advantages of a zirconium oxide based electrolyte which is stable in property, compact in structure, high in voltage of an open circuit of a battery and the like are maintained, the conductive capacity of oxygen ions can be improved, the problem that the output voltage quickly attenuates along with increase of current density, and the output performance of the battery is improved. The composite electrolyte material is simple in preparation process and low in preparation cost.
Description
Technical field
The present invention relates to a kind of compound electrolyte material for Solid Oxide Fuel Cell.
Background technology
Solid Oxide Fuel Cell (SOFCs) is a kind of cleaning, efficient novel energy converter device, because its strong adaptability to fuel, but do not need to use noble metal to receive much concern as advantages such as catalyst and focus Electricity Federation are used in conjunction.Solid-oxide fuel battery electrolyte commonly used comprises the lanthanum gallate of zirconia base oxide, ion doping ceria and doping etc.
Tradition SOFCs adopts yttria stabilized zirconia (YSZ) as electrolyte, and the material oxidation Reductive stability is good, densified sintering product is good, mechanical strength is high, battery open circuit voltage is higher.But owing to be subject to zirconium oxide base electrolyte material in low problem (＜800 ℃) restriction that oxygen ionic conductivity is lower, the working temperature of SOFCs is generally about 1000 ℃.Jeffrey W.Fergus is at " power technology (Joumal of Power Sources, 162,30-40,2006) reported, along with the reduction of temperature, the zirconium oxide base electrolyte conductivity descends rapidly, and is lower above an order of magnitude than cerium oxide base electrolyte in the time of 400-600 ℃.For a long time the high temperature height is done work, tends to cause the problems such as reaction, thermal coefficient of expansion between the battery component do not mate, and has also seriously limited the selection of battery component and ancillary equipment material, makes its cost high.In addition, S.Souza etc. are at " ECS's magazine " (Joumal of the Electrochemical Society, 144, L35-L37,1997) although reported with the battery open circuit voltage of zirconium oxide base electrolyte preparation higher, but along with the increase of current density, output voltage descends rapidly, causes the reduction of battery power output.Cause the application of zirconium oxide base electrolyte material in Solid Oxide Fuel Cell to be seriously influenced.
Summary of the invention
The object of the present invention is to provide a kind of compound electrolyte material based on the zirconia base oxide, both can keep the advantages such as zirconium oxide base electrolyte stable performance, compact structure, can improve again the oxygen ion conduction ability simultaneously, improve fuel battery performance; Preparation technology is simple, reduces cost.
Based on the compound electrolyte material of zirconia base oxide, this composite electrolyte is after heat treatment fully to be ground and sintering forms by following component mixture:
Zirconia 50～99wt% that zirconia or oxide are stable
One or more inorganic salts 0～50wt%
One or more other oxides or doping oxide 1～50wt%
Oxide is in the stable zirconia of wherein said oxide: scandium oxide, titanium oxide, vanadium oxide, yittrium oxide, niobium oxide, molybdenum oxide, lanthana, and this oxide and zirconia form solid solution;
Wherein said inorganic salts are: lithium metasilicate, sodium metasilicate, potassium silicate, magnesium silicate, calcium silicates, strontium silicate, barium silicate, lithium phosphate, sodium phosphate, potassium phosphate, magnesium phosphate, calcium phosphate, strontium phosphate, barium phosphate, lithium sulfate, sodium sulphate, potassium sulfate, magnesium sulfate, calcium sulfate, strontium sulfate, barium sulfate,
Wherein said other oxides are: lithia, magnesium oxide, aluminium oxide, silica, calcium oxide, manganese oxide, iron oxide, cobalt oxide, nickel oxide, cupric oxide, zinc oxide, gallium oxide, germanium oxide, bismuth oxide, strontium oxide strontia, barium monoxide, lanthana, cerium oxide, praseodymium oxide, neodymia, samarium oxide, gadolinium oxide, dysprosia, described doping oxide are the oxide that described other oxides form through ion doping.
Wherein said sintering temperature is between 500-1500 ℃.
Advantage of the present invention is as follows:
One, of the present inventionly compares with single-phase zirconia-based material based on zirconia base oxide compound electrolyte material, greatly reduce with cost of its preparation Solid Oxide Fuel Cell, be expected to realize the low-cost commercialization of SOFC.
Two, the compound electrolyte material based on the zirconia base oxide of the present invention, can keep not only that zirconium oxide base electrolyte is stable, fine and close, battery open circuit voltage is than advantages of higher, simultaneously can improve oxygen ionic conductivity again, conductivity is 0.5～1.0Scm-1 in the time of 800 ℃, improved the increase along with current density, output voltage descends rapidly the degradation problem, can improve the SOFC fuel battery performance.
Description of drawings
Fig. 1 is the x-ray diffraction pattern of material of the present invention
Fig. 2 is that material of the present invention and YSZ are as the i-v curve of the battery of electrolyte preparation
Fig. 3 is that material of the present invention and YSZ electrolytic conductivity vary with temperature the Arrhenius curve
Embodiment
The present invention uses zirconia, perhaps stable Zirconium oxide powder and inorganic salts of oxide, perhaps other oxide powders evenly mix by a certain percentage, biased sample after heat treatment, grinding can be used.Also can be as required, at zirconia, perhaps on the stable Zirconium oxide powder of oxide and the basis that inorganic salts mix, add again a certain proportion of other oxides, such as lithia, magnesium oxide, aluminium oxide, silica, calcium oxide, manganese oxide, iron oxide, cobalt oxide, zinc oxide, bismuth oxide.
Further specify the present invention below by embodiment.
Get the stable Zirconium powder of 8.0g oxide (80%), such as yttria stabilized zirconia (YSZ), add 2.0g sodium metasilicate (20%), fully ground and mixed can be used.Maybe the material that mixes is put into 1050 ℃ of heat treatments of Muffle furnace 2.5 hours, again ground after the cooling, obtain the composite electrolyte powder.
Get the stable Zirconium powder of 6.5g oxide (65%), such as yttria stabilized zirconia (YSZ), add 3.5g calcium phosphate (35%), fully ground and mixed can be used.Maybe the material that mixes is put into 1125 ℃ of heat treatments of Muffle furnace 2 hours, again ground after the cooling, obtain the composite electrolyte powder.
Get the stable Zirconium powder of 7.6g oxide (76%), such as yttria stabilized zirconia (YSZ), add 2.4g lithium sulfate (24%), fully ground and mixed can be used.Maybe the material that mixes is put into 950 ℃ of heat treatments of Muffle furnace 2 hours, again ground after the cooling, obtain the composite electrolyte powder.
Embodiment 4
Get the stable Zirconium powder of 7.0g oxide (70%), such as the zirconia (ScSZ) of scandia stabilized, add 2.1g potassium silicate (21%) and 0.9g lithium metasilicate (9%), fully ground and mixed can be used.Maybe the material that mixes is put into 900 ℃ of heat treatments of Muffle furnace 0.5 hour, again ground after the cooling, obtain the composite electrolyte powder.
Get the stable Zirconium powder of 7.0g oxide (70%), zirconia (ScSZ) such as scandia stabilized, add 1.0g magnesium silicate (10%), 1.0g strontium silicate (10%) and 1.0g barium silicate (10%), fully ground and mixed can be used.Maybe the material that mixes is put into 875 ℃ of heat treatments of Muffle furnace 0.5 hour, again ground after the cooling, obtain the composite electrolyte powder.
Get the stable Zirconium powder of 5.0g oxide (50%), such as the zirconia (ScSZ) of scandia stabilized, add 2.5g lithium phosphate (25%) and 2.5g strontium phosphate (25%), fully ground and mixed can be used.Maybe the material that mixes is put into 1000 ℃ of heat treatments of Muffle furnace 1 hour, again ground after the cooling, obtain the composite electrolyte powder.
Get the stable Zirconium powder of 5.5g oxide (55%), such as the stable zirconia of titanium oxide (TiSZ), add 1.5g magnesium phosphate (15%), 1.5g sodium phosphate (15%) and 1.5g potassium phosphate (15%), fully ground and mixed can be used.Maybe the material that mixes is put into 980 ℃ of heat treatments of Muffle furnace 1 hour, again ground after the cooling, obtain the composite electrolyte powder.
Embodiment 8
Get the stable Zirconium powder of 7.5g oxide (75%), such as the stable zirconia of titanium oxide (TiSZ), add 1.6g barium sulfate (16%) and 0.9g potassium sulfate (9%), fully ground and mixed can be used.Maybe the material that mixes is put into 850 ℃ of heat treatments of Muffle furnace 0.5 hour, again ground after the cooling, obtain the composite electrolyte powder.
Get the stable Zirconium powder of 6.4g oxide (64%), such as the stable zirconia of titanium oxide (TiSZ), add 1.5g lithium sulfate (15%), 1.5g sodium sulphate (15%) and 0.6g magnesium sulfate (6%), fully ground and mixed can be used.Maybe the material that mixes is put into 800 ℃ of heat treatments of Muffle furnace 0.5 hour, again ground after the cooling, obtain the composite electrolyte powder.
Embodiment 10
Get the stable Zirconium powder of 8.6g oxide (86%), such as the stable zirconia of niobium oxide (NbSZ), add 1.0g calcium silicates (10%) and 0.4g calcium phosphate (4%), fully ground and mixed can be used.Maybe the material that mixes is put into 960 ℃ of heat treatments of Muffle furnace 1.5 hours, again ground after the cooling, obtain the composite electrolyte powder.
Embodiment 11
Get the stable Zirconium powder of 8.6g oxide (86%), such as the stable zirconia of niobium oxide (NbSZ), add 1.2g potassium silicate (10%) and 0.2g strontium phosphate (%), fully ground and mixed can be used.Maybe the material that mixes is put into 920 ℃ of heat treatments of Muffle furnace 1.5 hours, again ground after the cooling, obtain the composite electrolyte powder.
Embodiment 12
Get the stable Zirconium powder of 7.5g oxide (75%), such as the stable zirconia of niobium oxide (NbSZ), add 1.5g silicon magnesium phosphate (15%) and 1.0g barium sulfate (10%), fully ground and mixed can be used.Maybe the material that mixes is put into 880 ℃ of heat treatments of Muffle furnace 0.5 hour, again ground after the cooling, obtain the composite electrolyte powder.
Embodiment 13
Get the stable Zirconium powder of 6.4g oxide (64%), such as the stable zirconia of lanthana (LaSZ), add 1.2g lithium phosphate (12%), 1.2g sodium metasilicate (12%) and 1.2 potassium sulfates (12%), fully ground and mixed can be used.Maybe the material that mixes is put into 1250 ℃ of heat treatments of Muffle furnace 1 hour, again ground after the cooling, obtain the composite electrolyte powder.
Embodiment 14
Get the stable Zirconium powder of 9.9g oxide (99%), such as the stable zirconia of lanthana (LaSZ), add 0.1g lithia (1%), fully ground and mixed can be used.Maybe the material that mixes is put into 500 ℃ of heat treatments of Muffle furnace 1 hour, again ground after the cooling, obtain the composite electrolyte powder.
Embodiment 15
Get the stable Zirconium powder of 9.5g oxide (95%), such as the stable zirconia of lanthana (LaSZ), add 0.5g lithia (5%), fully ground and mixed can be used.Maybe the material that mixes is put into 500 ℃ of heat treatments of Muffle furnace 1 hour, again ground after the cooling, obtain the composite electrolyte powder.
Embodiment 16
Get the stable Zirconium powder of 9.5g oxide (95%), such as the stable zirconia of vanadium oxide (VSZ), add 0.5g cobalt oxide (5%), fully ground and mixed can be used.Maybe the material that mixes is put into 650 ℃ of heat treatments of Muffle furnace 1 hour, again ground after the cooling, obtain the composite electrolyte powder.
Embodiment 17
Get the stable Zirconium powder of 9.9g oxide (95%), such as the stable zirconia of vanadium oxide (VSZ), add 0.1g calcium oxide (1%), fully ground and mixed can be used.Maybe the material that mixes is put into 550 ℃ of heat treatments of Muffle furnace 1 hour, again ground after the cooling, obtain the composite electrolyte powder.
Embodiment 18
Get the stable Zirconium powder of 9.5g oxide (95%), such as the stable zirconia of vanadium oxide (VSZ), add 0.5g silica (5%), fully ground and mixed can be used.Maybe the material that mixes is put into 1500 ℃ of heat treatments of Muffle furnace 5 hours, again ground after the cooling, obtain the composite electrolyte powder.
Embodiment 19
Get the stable Zirconium powder of 9.5g oxide (95%), such as the stable zirconia of molybdenum oxide (MoSZ), add 0.1g aluminium oxide (1%) and 0.4g silica (4%), fully ground and mixed can be used.Maybe the material that mixes is put into 1350 ℃ of heat treatments of Muffle furnace 4 hours, again ground after the cooling, obtain the composite electrolyte powder.
Get the stable Zirconium powder of 8.5g oxide (85%), such as the stable zirconia of molybdenum oxide (MoSZ), add 0.5g iron oxide (5%), 0.5g zinc oxide (5%) and 0.5g manganese oxide (5%), fully ground and mixed can be used.Maybe the material that mixes is put into 1200 ℃ of heat treatments of Muffle furnace 2 hours, again ground after the cooling, obtain the composite electrolyte powder.
Embodiment 21
Get the stable Zirconium powder of 9.5g oxide (95%), such as the stable zirconia of molybdenum oxide (MoSZ), add 0.5g cerium oxide (5%), fully ground and mixed can be used.Maybe the material that mixes is put into 1400 ℃ of heat treatments of Muffle furnace 2 hours, again ground after the cooling, obtain the composite electrolyte powder.
Embodiment 22
Get the stable Zirconium powder of 7.0g oxide (70%), such as yttria stabilized zirconia (YSZ), add 3.0g cerium oxide (30%), fully ground and mixed can be used.Maybe the material that mixes is put into 1400 ℃ of heat treatments of Muffle furnace 2 hours, again ground after the cooling, obtain the composite electrolyte powder.
Embodiment 23
Get the stable Zirconium powder of 7.0g oxide (70%), such as yttria stabilized zirconia (YSZ), add 3.0g ion doping cerium oxide (30%), such as samarium doped cerium oxide (SDC), fully ground and mixed can be used.Maybe the material that mixes is put into 1400 ℃ of heat treatments of Muffle furnace 2 hours, again ground after the cooling, obtain the composite electrolyte powder.
Embodiment 24
Get the stable Zirconium powder of 5.0g oxide (50%), such as yttria stabilized zirconia (YSZ), add 5.0g ion doping cerium oxide (50%), such as samarium doped cerium oxide (SDC), fully ground and mixed can be used.Maybe the material that mixes is put into 1400 ℃ of heat treatments of Muffle furnace 2 hours, again ground after the cooling, obtain the composite electrolyte powder.
Embodiment 25
Get the stable Zirconium powder of 7.0g oxide (70%), such as yttria stabilized zirconia (YSZ), add 2.0g praseodymium oxide (20%) and 1.0g sodium phosphate (10%), fully ground and mixed can be used.Maybe the material that mixes is put into 1300 ℃ of heat treatments of Muffle furnace 2.5 hours, again ground after the cooling, obtain the composite electrolyte powder.
Embodiment 26
Get the stable Zirconium powder of 5.0g oxide (50%), such as yttria stabilized zirconia (YSZ), add 1.5g dysprosia (15%), 1.0g gadolinium oxide (10%), 1.0g magnesium silicate (10%) and 1.5g sodium sulphate (15%), fully ground and mixed can be used.Maybe the material that mixes is put into 1000 ℃ of heat treatments of Muffle furnace 1 hour, again ground after the cooling, obtain the composite electrolyte powder.
Embodiment 27
Get the stable Zirconium powder of 7.0g oxide (70%), such as yttria stabilized zirconia (YSZ), add 2.0g ion doping cerium oxide (20%), such as gadolinium doped cerium oxide (GDC), with 1.0g barium silicate (10%), fully ground and mixed can be used.Maybe the material that mixes is put into 1450 ℃ of heat treatments of Muffle furnace 1 hour, again ground after the cooling, obtain the composite electrolyte powder.
Embodiment 28
Get the stable Zirconium powder of 7.0g oxide (70%), such as yttria stabilized zirconia (YSZ), add 2.0g ion doping cerium oxide (30%), such as lanthanum doped cerium oxide (LDC), with 1.0g lithium sulfate (10%), fully ground and mixed can be used.Maybe the material that mixes is put into 800 ℃ of heat treatments of Muffle furnace 0.5 hour, again ground after the cooling, obtain the composite electrolyte powder.
This material namely can be used as electrolytical powder and uses only by sufficient ground and mixed.But the sample that mixes through 500～1500 ℃ high-temperature heat treatment after, have better battery performance and mechanical strength.
As seen from Figure 1, in the YSZ-SDC composite electrolyte, bi-material does not react, and all keeps the original diffraction maximum of each material.Fig. 1 result shows, the feature that two-phase or multiphase of this material is compound.
As seen from Figure 2, the YSZ-SDC composite electrolyte is compared with the YSZ electrolyte, and open circuit voltage remains unchanged substantially, all more than 1.03V, yet but greatly improved the increase along with current density, output voltage descends rapidly the degradation problem, has improved fuel battery performance.
As seen from Figure 3, the YSZ-5%CeO2 compound electrolyte material is compared with YSZ, and conductivity obviously promotes, and for promoting battery performance, acts on fairly obvious.
Claims (5)
1. the composite electrolyte based on the zirconia base oxide is characterized in that, this composite electrolyte is after heat treatment fully to be ground and sintering forms by following component mixture:
Zirconia 50～99wt% that zirconia or oxide are stable
One or more inorganic salts 0～50wt%
One or more other oxides or doping oxide 1～50wt%.
2. composite electrolyte according to claim 1, it is characterized in that, oxide is scandium oxide, titanium oxide, vanadium oxide, yittrium oxide, niobium oxide, molybdenum oxide, lanthana in the stable zirconia of described oxide, and this oxide and zirconia form solid solution.
3. composite electrolyte according to claim 1, it is characterized in that described inorganic salts are: lithium metasilicate, sodium metasilicate, potassium silicate, magnesium silicate, calcium silicates, strontium silicate, barium silicate, lithium phosphate, sodium phosphate, potassium phosphate, magnesium phosphate, calcium phosphate, strontium phosphate, barium phosphate, lithium sulfate, sodium sulphate, potassium sulfate, magnesium sulfate, calcium sulfate, strontium sulfate, barium sulfate.
4. composite electrolyte according to claim 1, it is characterized in that, described other oxides are lithia, magnesium oxide, aluminium oxide, silica, calcium oxide, manganese oxide, iron oxide, cobalt oxide, nickel oxide, cupric oxide, zinc oxide, gallium oxide, germanium oxide, bismuth oxide, strontium oxide strontia, barium monoxide, lanthana, cerium oxide, praseodymium oxide, neodymia, samarium oxide, gadolinium oxide, dysprosia, and described doping oxide is the oxide that described other oxides form through ion doping.
5. composite electrolyte according to claim 1 is characterized in that, described sintering temperature is between 500-1500 ℃.
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Application publication date: 20131030 |