CN101771149A - Composite anode of magnesium-modified and nickel-based solid-oxide fuel cell and preparation and application thereof - Google Patents
Composite anode of magnesium-modified and nickel-based solid-oxide fuel cell and preparation and application thereof Download PDFInfo
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Abstract
The invention relates to a solid-oxide fuel cell, in particular to a composite anode of a solid-oxide fuel cell and a preparation method thereof. The composite anode comprises the following components by weight percent: 30-69.9 percent of nickel by nickel oxide, 0.01-30 percent of magnesium by magnesium oxide, doped zirconium oxide (zirconium oxide is doped with the yttrium oxide (YSZ)), the scandium oxide doped with the zirconium oxide (ScSZ) and/or the zirconium oxide (CeScSz), wherein the molar percent of the cerium oxide, the zirconium oxide and/or scandium oxide is 0.1-20 percent which accounts for 30-69.9 percent. The composite anode of the solid-oxide fuel cell has low polar polarization resistance, high activity and the like, and improves the output performance of the cell. The novel composite anode can be applied in solid-oxide fuel cells with flat plate type, pipe type and flat pipe type and other various structural modes.
Description
Technical field
The present invention relates to Solid Oxide Fuel Cell, specifically a kind of magnesium-modified nickel-based solid-oxide fuel cell composite anode, by adopting alkaline earth material magnesium mutually compound with traditional Ni-based anode material, the composite anode that obtains has and is evenly distributed, network connects characteristics such as tight between electrode material, reduce the polarization resistance of battery, improve the output performance of battery, the performance when improving battery and adopting hydrocarbon fuels such as methane.Directly the application for hydrocarbon fuels such as methane has great importance to the development of application technology for promoting the Solid Oxide Fuel Cell technology.
Background technology
Solid Oxide Fuel Cell is the energy conversion device that chemical energy is converted into electric energy, adopt structure of whole solid state, having the generating efficiency height, can directly adopting hydrocarbons such as natural gas is characteristics such as fuel, applied range, be desirable dispersion generating and concentrate power station technology, also can be applied to vehicle accessory power supply, compact power etc.Solid Oxide Fuel Cell mainly is made up of negative electrode, dielectric film, anode three parts.What anode mainly adopted at present is the Ni-YSZ porous metalloceramic, realizes the functions such as gas transfer, electrical conductivity, ionic conduction, catalytic reforming and electrocatalytic reaction of anode.Electrolyte adopts the zirconia (YSZ) of stabilized with yttrium oxide usually, also can be the zirconia (ScSZ) of doping of cerium oxide, scandia stabilized, the lanthanum gallate (LSGM) of mixing etc.Electrocatalyst for cathode generally adopts perovskite oxide and electrolyte to constitute composite cathode, as widely used LSM-YSZ composite cathode, also can be perovskites such as cobalt acid lanthanum, cobalt acid strontium samarium.
Have great importance for the application of hydrocarbon fuels such as natural gas development to the Solid Oxide Fuel Cell technical applicationization, therefore the various anode materials that are adapted to hydrocarbon fuels such as natural gas have obtained broad research, mainly comprise: Ni-based anode, copper base anode, cerium base anode, Ca-Ti ore type anode and precious metal anode etc.Though wherein copper base anode, cerium base anode and Ca-Ti ore type anode have anti-carbon effect preferably, there are problems such as activity is low, the difficult application development of realizing; Precious metal anode activity and anti-carbon aspect all have greatly improved, but its cost is very high, are not easy to use.Ni-based anode is the anode material that present Solid Oxide Fuel Cell generally adopts; but because battery needs high temperature sintering (＞1300 ℃ obtain fine and close dielectric film) in preparation process; cause the nickel-base catalyst sintering serious; and be difficult between nickel-base catalyst and the zirconia-based material soaking into; it is not strong to interact; cause in the high temperature reduction process nickel particle also can constantly grow up, thereby cause the anode activity lower, carbon distribution is comparatively serious.
Summary of the invention
In order to overcome the shortcoming of conventional composite anode, the object of the present invention is to provide a kind of compound anode of solid-oxide fuel battery and preparation method thereof, by magnesium-modified preparation novel composite anode, improve the activity of anode, thereby improve the output performance of battery, improve the activity of anode, suppress carbon distribution hydrocarbon fuels such as methane.
For achieving the above object, the technical solution used in the present invention is:
A kind of compound anode of solid-oxide fuel battery, by weight percentage, the weight of composite anode consists of, nickel is calculated as 30-69.9% with nickel oxide, magnesium is calculated as 0.01-30% with magnesium oxide, the zirconia that mixes accounts for 30-69.9%, wherein the zirconia of Can Zaing can be the zirconia (YSZ) of Yttrium oxide doping, the zirconia (ScSZ) of scandium oxide doping and/or the zirconia (CeScSZ) of cerium oxide and scandium oxide doping, and the molar content of cerium oxide, yittrium oxide and/or scandium oxide is 0.1-20%.
Composite anode of the present invention has hypopolarization resistance, characteristics such as high electrode activity, thus improved the output performance of battery, and the output performance when having improved battery and adopting hydrocarbon fuels such as methane.
That this novel composite anode can be applicable to is plate, the Solid Oxide Fuel Cell of cast, flat-tube type and other various makes.
The preparation process of described composite anode is as follows:
1) A. can adopt earlier magnesium is compound with nickel oxide and then mix with the zirconia that mixes, must composite anode materials;
Being divided into of slaine, oxide and/or the hydroxide that the process that magnesium and nickel oxide is compound can be by nickel and slaine, oxide and/or the hydroxide of magnesium separated, co-precipitation, dipping, mechanical mixture and/or high temperature solid state reaction are finished, wherein slaine can be nitrate, carbonate, acetate and/or the oxalates of nickel or magnesium, and various organic complexs such as glycinate, citrate and/or edetate;
B. or earlier magnesium is compound with the zirconia of doping and then mix with nickel oxide, must composite anode materials;
The process that the zirconia of magnesium and doping is compound can adopt precipitation, dipping, mechanical mixture and/or high temperature solid state reaction to finish, wherein magnesium can be oxide, hydroxide, nitrate, carbonate, acetate and/or oxalates, and various organic complexs such as glycinate, citrate and/or edetate;
C. or directly that the zirconic mixture of magnesium and nickel oxide and doping is compound, must composite anode materials;
Directly the process that the zirconic mixture of magnesium and nickel oxide and doping is compound can adopt precipitation, dipping, mechanical mixture and/or high temperature solid state reaction to finish, wherein magnesium and nickel can be oxide, hydroxide, nitrate, carbonate, acetate and/or oxalates, and various organic complexs such as glycinate, citrate and/or edetate;
2) the preparation composite anode at 600 ℃ of-1700 ℃ of sintering 2-10h, obtains composite anode.
Described composite anode can adopt prepared in various methods moulding such as compression moulding, The tape casting, silk screen print method, and that the structure of applicable Solid Oxide Fuel Cell membrane electrode can adopt is plate, cast, flat-tube type and other various makes; Battery can adopt multiple structures such as dielectric film self-cradling type, cathode support type, anode support type; Solid oxide fuel battery electrolyte diaphram can adopt Zirconia electrolytic or doping of cerium oxide electrolyte or other Ca-Ti ore type electrolyte of doping.Electrolyte preparation method can adopt various preparation of inorganic methods such as high temperature sintering, vapour deposition, sol-gel, plasma spraying.
Adopt the battery of composite anode of the present invention to prepare according to the following procedure:
1) preparation method of compound anode of solid-oxide fuel battery for adopt earlier with alkaline earth material magnesium compound with nickel oxide and then in the zirconia that mixes mix or elder generation with alkaline earth material magnesium and then method that in nickel oxide mix compound with the zirconia of doping, also can adopt direct zirconia composite methods, the composite anode materials that obtains with alkaline earth material magnesium and nickel oxide and doping.
2) adopt dry-pressing to prepare the thick composite anode substrate of 0.2-2mm,, obtain composite anode at 1000 ℃ of-1700 ℃ of sintering 2-10h; Apply one deck thereon and contain the slurry that thickness is 5-50 μ m YSZ.At 1200 ℃ of-1700 ℃ of sintering 2-10h, obtain the anode assembly;
Or, adopt dry-pressing to prepare the thick composite anode substrate of 0.2-2mm, apply one deck thereon and contain the slurry that thickness is 5-50 μ m YSZ; At 1200 ℃ of-1700 ℃ of sintering 2-10h, obtain the anode assembly;
3) after LSM eelctro-catalyst and YSZ mix (by weight 50: 50), adopt silk screen print method to prepare composite cathode, 1000 ℃ of-1300 ℃ of sintering 1-5h.
The test condition of battery: adopt hydrogen (80ml/min) or methane (20ml/min) as anode fuel gas at 800 ℃, oxygen (40ml/min) is as cathode gas.
Characteristics such as composite anode of the present invention has that electrode structure is evenly distributed, nickel contacts closely with interface between the YSZ, hypopolarization resistance, high activity.This composite anode and conventional anode have relatively obviously improved the output performance of battery.It can be applicable to the Solid Oxide Fuel Cell of plate, cast, flat-tube type and other various makes.
Embodiment
Embodiment is provided below, and the present invention will be further described:
Embodiment 1
Magnesium-modified compound anode of solid-oxide fuel battery is to the influence of battery performance
Adopt nitrate to be divided into solution (magnesium nitrate and nickel nitrate are in 800 ℃ of decomposition), obtain the nickel oxide that magnesium is modified.Select the nickel oxide that magnesium modifies (Ni: Mg=1 wherein: 0.01 for use, mol ratio) as anode catalysis material, wherein 20YSZ (molar content of yittrium oxide is 20% among the YSZ) accounts for 30% (weight ratio), adopt dry pressing to prepare the thick composite anode substrate of 0.7mm, at 1200 ℃ of sintering 5h, obtain composite anode; Apply one deck thereon and contain the slurry that thickness is 10 μ m YSZ.At 1450 ℃ of sintering 3h, obtain the anode assembly; After LSM eelctro-catalyst and YSZ mix (by weight 50: 50), adopt silk screen print method to prepare composite cathode, at 1100 ℃ of sintering 5h.
Traditional Ni-YSZ anode cell battery as a comparison.When being fuel gas with hydrogen, the battery performance that magnesium is modified and traditional Ni-YSZ anode cell performance relatively, when 800 ℃ of operations battery performance improve about 15%, 700 ℃ of performances raisings about 10%.When adopting methane to be fuel gas, the nickel oxide anode cell that magnesium is modified in the time of 800 ℃ improves about 30% than traditional Ni-YSZ anode cell performance, and the nickel oxide anode cell of modifying at 700 ℃ of magnesium improves about 20% than traditional Ni-YSZ anode cell performance.
Embodiment 2
Directly the compound anode of solid-oxide fuel battery that magnesium oxide and nickel oxide and YSZ are mixed with is to the influence of battery performance
Adopt the method for directly magnesium oxide, nickel oxide and 8YSZ (molar content of yittrium oxide is 8% among the YSZ) being mixed to prepare composite anode, the preparation battery, the modification of battery the results are shown in Table 1.With traditional Ni-YSZ anode cell battery as a comparison.
Table 1
As can be seen from Table 1, increased gradually before this, but battery performance improves little when the content of magnesium is higher at increase battery performance along with content of magnesium.
Embodiment 3
When magnesium-modified composite anode is used for tubular solid oxide fuel cells to the influence of battery performance
Adopt nitrate to be divided into the method (magnesium nitrate and nickel nitrate are in 800 ℃ of decomposition) of separating, obtain the nickel oxide that magnesium is modified.Adopt nickel oxide that magnesium modifies as anode catalysis material (Ni: Mg=1 wherein: 0.04, mol ratio), mix (by weight 50: 50) with 2YSZ (molar content of yittrium oxide is 2% among the YSZ), adopt the inoranic membrane technology to prepare the cast anode support, apply one deck thereon and contain the slurry that thickness is 50 μ m YSZ.After the drying,, obtain the anode assembly at 1600 ℃ of sintering 2h.After LSM eelctro-catalyst and YSZ mix (weight ratio 50: 50), preparation composite cathode, 1200 ℃ of sintering 3h.Traditional Ni-YSZ anode tubular cells battery as a comparison.When being fuel gas with hydrogen, the battery performance that magnesium is modified and traditional Ni-YSZ anode cell performance relatively, when 800 ℃ of operations battery performance improve about 25%, 700 ℃ of performances raisings about 20%.When adopting methane to be fuel gas, the nickel oxide anode cell that magnesium is modified in the time of 800 ℃ improves about 50% than traditional Ni-YSZ anode cell performance, and the nickel oxide anode cell of modifying at 700 ℃ of magnesium improves about 30% than traditional Ni-YSZ anode cell performance.
Embodiment 4
Earlier mix the influence of the compound anode of solid-oxide fuel battery that obtains in nickel oxide again with magnesium and YSZ are compound to battery performance
Adopt the method (600 ℃ of decomposition) of magnesium nitrate dipping, compound with magnesium and 8YSZ (molar content of yittrium oxide is 8% among the YSZ), then this material is mixed (by weight percentage with nickel oxide, nickel oxide accounts for 40%, magnesium oxide accounts for 10%, YSZ accounts for 50%), adopt dry pressing to prepare the thick composite anode substrate of 1mm, apply one deck thereon and contain the slurry that thickness is 20 μ m YSZ; At 1300 ℃ of sintering 10h, obtain the anode assembly; After LSM eelctro-catalyst and YSZ mix (by weight 50: 50), adopt silk screen print method to prepare composite cathode, 1100 ℃ of sintering 5h.
Traditional Ni-YSZ anode cell battery as a comparison.When being fuel gas with hydrogen, magnesium-modified battery performance and traditional Ni-YSZ anode cell performance relatively, battery performance improves approximately 12% when 800 ℃ of operations, improves about 8% 650 ℃ of performances.When adopting methane to be fuel gas, magnesium-modified battery improves approximately 50% than traditional Ni-YSZ anode cell performance in the time of 800 ℃, and improves about 30% at 650 ℃ of magnesium-modified batteries than traditional Ni-YSZ anode cell performance.
Embodiment 5
Directly with magnesium and YSZ and the compound influence of nickel oxide to solid-oxide fuel battery performance
Adopt the method (800 ℃ of decomposition) of magnesium nitrate dipping, magnesium and 10YSZ (molar content of yittrium oxide is 10% among the 10YSZ) and nickel oxide is compound (by weight percentage, nickel oxide accounts for 30%, magnesium oxide accounts for 5%, YSZ accounts for 65%), adopt dry pressing to prepare the thick composite anode substrate of 1.5mm, apply one deck thereon and contain the slurry that thickness is 20 μ m YSZ; At 1300 ℃ of sintering 10h, obtain the anode assembly; After LSM eelctro-catalyst and YSZ mix (by weight 50: 50), adopt silk screen print method to prepare composite cathode, 1100 ℃ of sintering 5h.
Traditional Ni-YSZ anode cell battery as a comparison.When being fuel gas with hydrogen, magnesium-modified battery performance and traditional Ni-YSZ anode cell performance relatively, battery performance improves approximately 20% when 800 ℃ of operations, improves about 15% 650 ℃ of performances.When adopting methane to be fuel gas, magnesium-modified battery improves approximately 50% than traditional Ni-YSZ anode cell performance in the time of 800 ℃, and improves about 30% at 650 ℃ of magnesium-modified batteries than traditional Ni-YSZ anode cell performance.
Embodiment 6
Directly with magnesium and YSZ and the compound influence of nickel oxide to solid-oxide fuel battery performance
Adopt infusion process that magnesium nitrate and 8YSZ (molar content of yittrium oxide is 8% among the YSZ) and nickel oxide is compound (by weight percentage, nickel oxide accounts for 65%, magnesium oxide accounts for 5%, YSZ accounts for 30%) 800 ℃ of roastings, obtain magnesium-modified composite anode materials, adopt dry pressing to prepare the thick composite anode substrate of 1.5mm, apply one deck thereon and contain the slurry that thickness is 20 μ m YSZ; At 1300 ℃ of sintering 10h, obtain the anode assembly; After LSM eelctro-catalyst and YSZ mix (by weight 50: 50), adopt silk screen print method to prepare composite cathode, 1100 ℃ of sintering 5h.
Traditional Ni-YSZ anode cell battery as a comparison.When being fuel gas with hydrogen, magnesium-modified battery performance and traditional Ni-YSZ anode cell performance relatively, battery performance improves approximately 20% when 800 ℃ of operations, improves about 15% 650 ℃ of performances.When adopting methane to be fuel gas, magnesium-modified battery improves approximately 40% than traditional Ni-YSZ anode cell performance in the time of 800 ℃, and improves about 25% at 650 ℃ of magnesium-modified batteries than traditional Ni-YSZ anode cell performance.
Embodiment 7
Directly with magnesium and ScSZ and the compound influence of nickel oxide to solid-oxide fuel battery performance
Adopt infusion process that magnesium nitrate and 10ScSZ (molar content of scandium oxide is 10% among the ScSZ) and nickel oxide is compound (by weight percentage, nickel oxide accounts for 65%, magnesium oxide accounts for 5%, ScSZ accounts for 30%) 800 ℃ of roastings, obtain magnesium-modified composite anode materials, adopt dry pressing to prepare the thick composite anode substrate of 1.5mm, apply one deck thereon and contain the slurry that thickness is 20 μ m ScSZ; At 1300 ℃ of sintering 10h, obtain the anode assembly; After LSM eelctro-catalyst and YSZ mix (by weight 50: 50), adopt silk screen print method to prepare composite cathode, 1100 ℃ of sintering 5h.
Traditional Ni-ScSZ anode cell battery as a comparison.When being fuel gas with hydrogen, magnesium-modified battery performance and traditional Ni-ScSZ anode cell performance relatively, battery performance improves approximately 30% when 800 ℃ of operations, improves about 20% 650 ℃ of performances.When adopting methane to be fuel gas, magnesium-modified battery improves approximately 50% than traditional Ni-ScSZ anode cell performance in the time of 800 ℃, and improves about 30% at 650 ℃ of magnesium-modified batteries than traditional Ni-ScSZ anode cell performance.
Embodiment 8
Directly with magnesium and CeScSZ and the compound influence of nickel oxide to solid-oxide fuel battery performance
(molar content of scandium oxide is 10% among the 1Ce10ScSZ with magnesium nitrate and 1Ce10ScSZ to adopt infusion process, the molar content of cerium oxide is 1%) and nickel oxide compound (by weight percentage, nickel oxide accounts for 65%, magnesium oxide accounts for 5%, 1Ce10ScSZ accounts for 30%) 800 ℃ of roastings, obtain magnesium-modified composite anode materials, adopt dry pressing to prepare the thick composite anode substrate of 1.5mm, apply one deck thereon and contain the slurry that thickness is 20 μ m ScSZ; At 1300 ℃ of sintering 10h, obtain the anode assembly; After LSM eelctro-catalyst and YSZ mix (by weight 50: 50), adopt silk screen print method to prepare composite cathode, 1100 ℃ of sintering 5h.
Traditional Ni-1Ce10ScSZ anode cell battery as a comparison.When being fuel gas with hydrogen, magnesium-modified battery performance and traditional Ni-1Ce10ScSZ anode cell performance relatively, battery performance improves approximately 15% when 800 ℃ of operations, improves about 10% 650 ℃ of performances.When adopting methane to be fuel gas, magnesium-modified battery improves approximately 30% than traditional Ni-1Ce10ScSZ anode cell performance in the time of 800 ℃, and improves about 15% at 650 ℃ of magnesium-modified batteries than traditional Ni-1Ce10ScSZ anode cell performance.
Claims (9)
1. magnesium-modified nickel-based solid-oxide fuel cell composite anode, it is characterized in that: the weight percent of composite anode consists of: nickel is counted 30-69.9% with nickel oxide, and magnesium is counted 0.01-30% with magnesium oxide, and the zirconia of doping accounts for 30-69.9%.
2. according to the described composite anode of claim 1, it is characterized in that: the zirconia of described doping is one or more in the zirconia (CeScSZ) that mixes of zirconia (ScSZ), cerium oxide and scandium oxide that the zirconia (YSZ), scandium oxide of Yttrium oxide doping mixes, and wherein cerium oxide, yittrium oxide, the molar content of scandium oxide in the zirconia that mixes are respectively 0.1-20%.
3. according to the described composite anode of claim 1, it is characterized in that: the weight percentage of described magnesium oxide in composite anode is 0.1-25%.
4. according to the described composite anode of claim 1, it is characterized in that: the weight percent of composite anode consists of: nickel is counted 30-69.5% with nickel oxide, and magnesium is counted 0.5-15% with magnesium oxide, and the zirconia of doping accounts for 30-69.5%.
5. the preparation method of claims 1 described composite anode is characterized in that:
1) can adopt earlier magnesium is compound with nickel and then mix with the zirconia that mixes, must composite anode materials;
Or earlier that magnesium is compound with the zirconia of doping and then mix with nickel, must composite anode materials;
Or directly that the zirconic mixture of magnesium and nickel and doping is compound, get composite anode materials;
2) with composite anode materials at 600 ℃ of-1700 ℃ of sintering 2-10h, obtain composite anode.
6. according to the preparation method of the described composite anode of claim 5, it is characterized in that:
Being divided into of slaine, hydroxide or the oxide that the compound process of described magnesium and nickel can be by nickel element and slaine, hydroxide or the oxide of magnesium elements separated, co-precipitation, dipping, mechanical mixture or high temperature solid state reaction are finished, and wherein slaine can be one or more in the nitrate, carbonate, acetate, oxalates, glycinate, citrate, edetate of nickel or magnesium;
The process that the zirconia of magnesium and doping is compound can adopt precipitation, dipping, mechanical mixture or high temperature solid state reaction to finish, and wherein magnesium is one or more in the oxide, hydroxide, nitrate, carbonate, acetate, oxalates, glycinate, citrate, edetate of magnesium elements;
The process that the zirconic mixture of magnesium and nickel and doping is compound can adopt precipitation, dipping, mechanical mixture or high temperature solid state reaction to finish, and wherein magnesium and nickel are one or more in the oxide, hydroxide, nitrate, carbonate, acetate, oxalates, glycinate, citrate, edetate of nickel or magnesium.
7. the application of the described composite anode of claim 1 is characterized in that: described composite anode can adopt compression moulding, The tape casting or silk screen print method to prepare moulding; It is applicable to the Solid Oxide Fuel Cell membrane electrode of plate, cast, flat-tube type and other various makes.
8. according to the application of the described composite anode of claim 7, it is characterized in that: described membrane electrode can adopt the structure of dielectric film self-cradling type, cathode support type, anode support type or metallic support type.
9. according to the application of the described composite anode of claim 8, it is characterized in that: the electrolyte membrance that described dielectric film can adopt the Zirconia electrolytic of doping or doping of cerium oxide electrolyte or other Ca-Ti ore type electrolyte to make.
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| CN102544528A (en) * | 2010-12-14 | 2012-07-04 | 中国科学院大连化学物理研究所 | Battery anode catalytic material containing magnesium and rare earth element, preparation method and application thereof |
| CN102569823A (en) * | 2010-12-14 | 2012-07-11 | 中国科学院大连化学物理研究所 | Ni-based composite anode co-modified by Mg and rare earth elements of solid oxide fuel cell |
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| CN106159288B (en) * | 2015-04-22 | 2019-03-08 | 中国科学院物理研究所 | A kind of Ni base anode material, preparation method and the purposes of anti-carbon |
| CN106450352A (en) * | 2016-12-08 | 2017-02-22 | 常熟理工学院 | Carbon deposition-resistant solid oxide fuel cell anode and preparation method thereof |
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