CN100508259C - Multiple phase electrocatalysis material and preparation method thereof - Google Patents

Multiple phase electrocatalysis material and preparation method thereof Download PDF

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CN100508259C
CN100508259C CNB2006101127772A CN200610112777A CN100508259C CN 100508259 C CN100508259 C CN 100508259C CN B2006101127772 A CNB2006101127772 A CN B2006101127772A CN 200610112777 A CN200610112777 A CN 200610112777A CN 100508259 C CN100508259 C CN 100508259C
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oxygen ion
conductor
ion conductor
volume fraction
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CN1921196A (en
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毛宗强
高瑞峰
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Tsinghua University
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Abstract

The invention relates to a multiple-phase electric catalyst material and preparation. Wherein, said material is formed at least three phases as oxygen ion conductor phase, oxygen ion-electron mixed conductor phase, or electron conductor phase, and gas phase; the oxygen ion-electron mixed conductor phase is A2BO4+delta, while A is one or several of Ca, Sr, Ba, Bi, Pb, Y, La, Ce, Pr, Nd, Sm, Eu and Gd, and 0<delta<=0.30. The electric catalyst material of said invention has high oxygen ion-electron mixed conductivity while the oxygen pressure is from 10-6 to 3MPa. And the cathode made from it in solid oxide fuel battery has better thermal stability and chemical stability at 400-700Deg. C, while its thermal expansion factor is near to Ce0.8Sm0.2O1.9, and it has better catalysis activity on the electric chemical reduction of oxygen.

Description

A kind of multiple phase electrocatalysis material and preparation method thereof
Technical field
The present invention relates to a kind of multiple phase electrocatalysis material and preparation method thereof, belong to the catalysis material technical field.This material can be used as the negative electrode of Solid Oxide Fuel Cell, the oxygen electrode of electrolytic tank of solid oxide, the composite cathode material of the intermediate temperature solid oxide fuel cell of especially a kind of high catalytic activity, high stability.
Background technology
The cathode material of Solid Oxide Fuel Cell must satisfy following basic demand:
(1) stability.In oxidizing atmosphere, in the scope from the room temperature to the working temperature, cathode material must be that sudden variation is stablized, do not had in stable performance, chemically stable, stable crystal form, overall dimension.
(2) conductivity.Under oxidizing atmosphere and working temperature, cathode material will have sufficiently high electronic conductivity, reduces ohmic polarization as far as possible.Preferably has oxygen ionic conductivity simultaneously.
(3) compatibility.Under operating temperature and making temperature, cathode material all should be compatible with other constituent element chemistry, and do not react with contiguous constituent element, thereby avoid second formation mutually, thermal coefficient of expansion variation and introduce electronic conductance etc. in electrolyte.
(4) thermal expansivity.From the room temperature to the operating temperature and in the scope of making temperature, cathode material all should be complementary with the thermal coefficient of expansion of other constituent elements, to avoid cracking, be out of shape and come off.
(5) porousness.Under from the room temperature to the operating temperature, cathode material should have loose structure.Consider to determine its porosity lower limit from the mass transfer aspect, consider to determine its porosity upper limit from mechanics of materials intensity aspect.
(6) catalytic performance.Good catalytic performance, the polarization in the time of can reducing oxygen reduction.
(7) other.Higher intensity and toughness, workability and low cost.
The composition general formula of the cathode material for solid-oxide fuel cell of Chinese patent CN1731607A (on February 8th, 2006 is open) invention is A 1+xA ' 1-xB 1-yB ' yO 4 ± δ, wherein A is the main group alkaline-earth metal, and A ' is a rare earth element, and B and B ' they are transiting group metal elements, 0＜x＜1,0≤y≤1, δ≤0.17.The feature of this invention is potassium fluoronickelate structure (A 2BO 4+ δ) single-phase pure cathode material, Sr for example 0.5Sm 1.5NiO 4Or Sr 0.5Sm 1.5Ni 0.8Co 0.2O 4In fact, 1. A bit element can also be selected other major elements, for example Bi, Pb etc. except selecting main group alkali earth metal, rare earth element; 2. A bit element is not limited to two, can carry out the multi-element doping of two above elements; 3. B bit element can also be selected major element, for example Li, Mg etc. except selecting transiting group metal elements; 4. the performance of single-phase pure cathode material is not as the complex phase cathode material, especially oxygen ionic conductivity, and the thermal expansion matching of electrolyte aspect.
At present for K 2NiF 4The La of structure 2-xNiO 4, Nd 2-xNiO 4And the single La that mixes in B position 2Ni 1-xCo xO 4Material is as the existing report of the research of the single-phase negative electrode of Solid Oxide Fuel Cell.
The present invention uses such material (A based on multi-element doping 2BO 4+ δ) oxonium ion calking characteristic, combination oxygen ion conductor, electronic conductor, pore creating material are prepared the multiple phase electrocatalysis material of superior performance.
Summary of the invention
The object of the present invention is to provide the multiple phase electrocatalysis material of a kind of high catalytic activity, high stability, can be used as the negative electrode of Solid Oxide Fuel Cell, the oxygen electrode of electrolytic tank of solid oxide.
Technical scheme of the present invention is to use to have higher oxonium ion-the electric A that leads of electronics mixing 2BO 4+ δThe type multivariant oxide, with oxygen-ion conduction mutually, pure electronic conductance phase, pore creating material combination, constitute multiple phase electrocatalysis material jointly.
A kind of multiple phase electrocatalysis material that the present invention proposes is characterized in that: described material is by three phase compositions: it is oxygen ion conductor phase, the oxonium ion of potassium fluoronickelate structure-electron mixed conductor phase, gas phase; The volume fraction of described oxygen ion conductor in whole material is 10～70%, the volume fraction of oxonium ion one electron mixed conductor in whole material of described potassium fluoronickelate structure is 10～85%, and the volume fraction of described electronic conductor in whole material is 0～50%.
A kind of multiple phase electrocatalysis material that the present invention proposes is characterized in that: described material is by four phase compositions: oxygen ion conductor phase, the oxonium ion of potassium fluoronickelate structure-electron mixed conductor phase, electronic conductor phase, gas phase; The volume fraction of described oxygen ion conductor in whole material is 10～70%, the volume fraction of oxonium ion one electron mixed conductor in whole material of described potassium fluoronickelate structure is 10～85%, the volume fraction of described electronic conductor in whole material is 0～50%, and the volume fraction of described gas phase in whole material is 5～50%.
In above-mentioned multiple phase electrocatalysis material, described oxygen ion conductor is selected from mutually: doping of cerium oxide series electrolyte, or the lanthanum gallate of mixing series electrolyte, or the zirconia that mixes series electrolyte.
In above-mentioned multiple phase electrocatalysis material, the composition general formula of the oxonium ion of described potassium fluoronickelate structure-electron mixed conductor phase is A 2BO 4+ δ, wherein A is the doping combination of one or more elements of Ca, Sr, Ba, Bi, Pb, Y, La, Ce, Pr, Nd, Sm, Eu, Gd; B is the doping combination of one or more elements of Li, Mg, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Zn; 0＜δ≤0.30.
In above-mentioned multiple phase electrocatalysis material, described electronic conductor is the combination of one or more metal materials of silver, platinum, rhodium, ruthenium, iridium, palladium, iron, cobalt, nickel, copper mutually.
In above-mentioned multiple phase electrocatalysis material, described gas phase refers to one or more the combination of the mixture of mixture, oxygen and inert gas of air, oxygen, oxygen and nitrogen or steam.
The preparation method of a kind of multiple phase electrocatalysis material that the present invention proposes, it is characterized in that: described method comprises following steps, the powder of the oxonium ion-electron mixed conductor phase of synthetic respectively oxygen ion conductor phase, potassium fluoronickelate structure, raw material, pore creating material, adhesive, plasticizer, solvent mix mutually mutually with metal, ball milling, sieve, prepare slurry; Utilize silk screen printing or rotation coating, spraying method slurry to be covered on the surface of dielectric substrate, then at 800～1300 ℃ of calcining 0.5～10h.
In the preparation of the method for above-mentioned multiple phase electrocatalysis material, it is characterized in that: the material of described method preparation has loose structure, and this loose structure prepares through using pore creating material, adhesive, plasticizer, solvent; Pore creating material is one or more of starch, graphite powder, polyethylene, polypropylene, active carbon or polyethylene glycol; Adhesive is one or more in polyvinyl alcohol, polyvinyl butyral resin, methylcellulose, ethyl cellulose, butyryl resin or the epoxy resin; Plasticizer is one or more of polyethylene glycol, glycerol, oleic acid, stearic acid, olein, the acid of phthalic acid fourth benzyl, repefral; Solvent is one or more of water, ethanol, isopropyl alcohol, n-butanol, terpinol, toluene, benzene, acetic acid, heptane and octane.
Multiple phase electrocatalysis material of the present invention has very high oxonium ion-electronics mixed conductivity in partial pressure of oxygen is 10-6 to 3MPa scope.With it is the negative electrode of Solid Oxide Fuel Cell, has good thermal stability, chemical stability at 400～700 ℃, its thermal coefficient of expansion and Ce 0.8Sm 0.2O 1.9Material is approaching, and its electrochemical reduction to oxygen has good catalytic activity.
The present invention uses has higher oxonium ion-the electric A that leads of electronics mixing 2BO 4+ δ type multivariant oxide, to lead phase (have identical with electrolyte or homologous series form) compound with electronic conductance phase, pure oxygen ion electricity, prepare the multiple phase electrocatalysis material of porous, can improve the oxygen-ion conduction of electrode, the stability of electrode structure, improve and electrolytical compatibility, increase the active region of electrode reaction, thereby reduce cathode overpotential, reduction cathode/electrolyte interface resistance, improve battery performance, have good effect.
Description of drawings
Fig. 1 is the La of glycine-nitrate process preparation 2Ni 0.8Fe 0.2O 4.19The XRD figure of powder.
Fig. 2 is the performance of monocell.The negative electrode of this monocell is Ce 0.8Sm 0.2O 1.9-La 2Ni 0.8Fe 0.2O 4.19Composite cathode, anode are Ni-Ce 0.8Sm 0.2O 1.9, electrolyte is Ce 0.8Sm 0.2O 1.9Solid legend is voltage-current characteristics among the figure; Hollow legend is power density-current characteristics.
Describe the present invention in detail with example below.
Embodiment
Said oxygen ion conductor is selected from mutually: 1) doping of cerium oxide series electrolyte; 2) the lanthanum gallate series electrolyte that mixes; 3) the zirconia series electrolyte that mixes.This electrolyte composition with fuel cell or electrolytic cell is identical, or selects isonomic electrolyte for use, for example, and Ce 0.8Sm 0.2O 1.9.Ce 0.9Gd 0.1O 1.95, La 0.9Sr 0.1Ga 0.8Mg 0.2O 2.85, ZrO 2-8%Sc 2O 3
Said electronic conductor is the combination of one or more metal materials of silver, platinum, rhodium, ruthenium, iridium, palladium, iron, cobalt, nickel, copper mutually.
Said gas phase refers to one or more the combination of " mixture of the mixture of air, oxygen, oxygen and nitrogen, oxygen and inert gas, steam ".That is, this multiple phase electrocatalysis material has loose structure.This loose structure prepares through using pore creating material, adhesive, plasticizer, solvent.Pore creating material is one or more of starch, graphite powder, polyethylene, polypropylene, active carbon or polyethylene glycol.Adhesive is one or more in polyvinyl alcohol, polyvinyl butyral resin, methylcellulose, ethyl cellulose, butyryl resin or the epoxy resin.Plasticizer is one or more of polyethylene glycol, glycerol, oleic acid, stearic acid, olein, the acid of phthalic acid fourth benzyl, repefral.Solvent is one or more of water, ethanol, isopropyl alcohol, n-butanol, terpinol, toluene, benzene, acetic acid, heptane and octane.
The preparation method of the said multiple phase electrocatalysis material of the present invention is:
1) preparation A 2BO 4+ δPowder can adopt solid reaction process, glycine-nitrate process, citric acid complex-decomposition method;
2) preparation electrolyte powder (oxygen-ion conduction phase) can adopt solid reaction process, coprecipitation, glycine-nitrate process;
3) with A 2BO 4+ δPowder, electrolyte powder, metal phase raw material (for example silver oxide powder), pore creating material, adhesive, plasticizer, solvent mix (annotating: when adopting three phase compositions, do not add metal phase raw material) mutually, and ball milling sieves, the preparation electrode slurry; 4) utilize silk screen printing or rotation coating, spraying method that combination electrode is prepared in bath surface, the thickness of electrode is 10～100 μ m; According to the difference that electrode is formed, electrode is calcined 0.5～10h at 800～1300 ℃.
Embodiment one:
La 2Ni 0.8Fe 0.2O 4.19, adopt glycine-nitrate process preparation.According to La 2Ni 0.8Fe 0.2O 4.19Stoichiometric proportion, mix La (NO 3) 3, Ni (NO 3) 2, Fe (NO 3) 3The aqueous solution; Add glycine (its mol ratio with metal ion is 2:1), stirring, little heating (80 ℃).Then, solution is poured in the porcelain evaporating dishes, with the electric furnace heating, behind about 1h, spontaneous combustion gets black powder.Subsequently, this black powder is calcined decarburizations, one-tenth phase in 800 ℃.The X-ray diffraction pattern of this powder as shown in Figure 1.Powder and Ce that this glycine-nitrate process is synthetic 0.8Sm 0.2O 1.9Powder, starch, terpinol (this weight percentage is followed successively by 45%, 42%, 5%, 8%) mix, and (anode is Ni-Ce to the method by silk screen printing in anode-electrolyte double base 0.8Sm 0.2O 1.9Electrolyte is Ce 0.8Sm 0.2O 1.9) last preparation cathode thin film; 1200 ℃ of sintering are prepared monocell.Test the performance of this monocell, as shown in Figure 2 (hydrogen flowing quantity is 400ml/min, and air mass flow is 1400ml/min, and reaction gas pressure is 0.1MPa).The open circuit voltage of this monocell in the time of 600 ℃ is 0.64V, and peak power output density is 0.285W/cm 2
Embodiment two:
La 1.6Sr 0.4NiO 4.24, adopt the solid reaction process preparation.With La 2O 3, Ni (NO 3) 26H 2O, Sr (NO 3) 2According to La 1.6Sr 0.4NiO 4.24Stoichiometric proportion batching, be medium with ethanol, agate ball is an abrasive body, in the agate jar of packing into, ball milling is 6 hours on planetary ball mill.Slurry behind the ball milling is sieved in (120 order), drying, briquetting 1100 ℃ of calcinations 8 hours in air, cools to room temperature with the furnace.Grind, get the powder of solid reaction process preparation.With it and Ce 0.8Sm 0.2O 1.9Powder, starch, terpinol (this weight percentage is followed successively by 45%, 42%, 5%, 8%) mix, and (anode is Ni-Ce to the method by silk screen printing in anode-electrolyte double base 0.8Sm 0.2O 1.9Electrolyte is Ce 0.8Sm 0.2O 1.9) last preparation cathode thin film; 1150 ℃ of sintering are prepared monocell.
Embodiment three:
Bi 0.7La 0.7Sr 0.6NiO 4.19, adopting the solid reaction process preparation, raw material is La 2O 3, Bi 2O 3, Ni (NO 3) 26H 2O, Sr (NO 3) 2, all the other preparation processes are same as embodiment two.The solid phase reaction synthesis temperature is 1050 ℃.With it and Ce 0.8Sm 0.2O 1.9Powder, starch, terpinol (this weight percentage is followed successively by 45%, 42%, 5%, 8%) mix, and (anode is Ni-Ce to the method by silk screen printing in anode-electrolyte double base 0.8Sm 0.2O 1.9Electrolyte is Ce 0.8Sm 0.2O 1.9) last preparation cathode thin film; 1100 ℃ of sintering are prepared monocell.
Embodiment four:
Bi 0.5Sr 0.7La 0.5Y 0.3NiO 4.18, adopting glycine-nitrate process preparation, material solution is La (NO 3) 3, Bi (NO 3) 3, Ni (NO 3) 2, Sr (NO 3) 2, Y (NO 3) 3, all the other preparation processes are same as embodiment one.Powder that this glycine-nitrate process is synthetic and silver oxide powder, Ce 0.8Sm 0.2O 1.9Powder, starch, terpinol (this weight percentage is followed successively by 35%, 10%, 42%, 5%, 8%) mix, and (anode is Ni-Ce to the method by silk screen printing in anode-electrolyte double base 0.8Sm 0.2O 1.9Electrolyte is Ce 0.8Sm 0.2O 1.9) last preparation cathode thin film; 1050 ℃ of sintering are prepared monocell.
Embodiment five:
La 2Mg 0.2Ni 0.8O 4.20, adopting the solid reaction process preparation, raw material is La 2O 3, Ni (NO 3) 26H 2O, Mg (NO 3) 26H 2O, all the other preparation processes are same as embodiment two.The solid phase reaction synthesis temperature is 1100 ℃.With it and Ce 0.8Sn 0.2O 1.9Powder, starch, terpinol (this weight percentage is followed successively by 45%, 42%, 5%, 8%) mix, and (anode is Ni-Ce to the method by silk screen printing in anode-electrolyte double base 0.8Sm 0.2O 1.9Electrolyte is Ce 0.8Sm 0.2O 1.9) last preparation cathode thin film; 1100 ℃ of sintering are prepared monocell.
Embodiment six:
La 2Li 0.1Co 0.2Ni 0.7O 4.25, adopting the solid reaction process preparation, raw material is La 2O 3, LiNO 3, Ni (NO 3) 26H 2O, Co (NO 3) 26H 2O, all the other preparation processes are same as embodiment two.The solid phase reaction synthesis temperature is 1150 ℃.With it and Ce 0.8Sm 0.2O 1.9Powder, starch, terpinol (this weight percentage is followed successively by 45%, 42%, 5%, 8%) mix, and (anode is Ni-Ce to the method by silk screen printing in anode-electrolyte double base 0.8Sm 0.2O 1.9Electrolyte is Ce 0.8Sm 0.2O 1.9) last preparation cathode thin film; 1100 ℃ of sintering are prepared monocell.
Embodiment seven:
La 1.6Sr 0.4Mg 0.2Ni 0.8O 4.24, adopting glycine-nitrate process preparation, material solution is La (NO 3) 3, Mg (NO 3) 2, Ni (NO 3) 2, Sr (NO 3) 2, all the other preparation processes are same as embodiment one.Powder that this glycine-nitrate process is synthetic and silver oxide powder, Ce 0.8Sm 0.2O 1.9Powder, active carbon, ethyl cellulose, terpinol (this weight percentage is followed successively by 35%, 10%, 42%, 4.5%, 0.5%, 8%) mix, and (anode is Ni-Ce to the method by silk screen printing in anode-electrolyte double base 0.8Sm 0.2O 1.9Electrolyte is Ce 0.8Sm 0.2O 1.9) last preparation cathode thin film; 1050 ℃ of sintering are prepared monocell.

Claims (5)

1, a kind of multiple phase electrocatalysis material is characterized in that: containing the composition general formula is A 2BO 4+ δThe oxonium ion-electron mixed conductor phase of potassium fluoronickelate structure, wherein A is the doping combination of one or more elements of Ca, Sr, Ba, Bi, Pb, Y, La, Ce, Pr, Nd, Sm, Eu, Gd; B is the doping combination of one or more elements of Li, Mg, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Zn; 0.18≤δ≤0.30; Also contain oxygen ion conductor mutually or contain oxygen ion conductor and electronic conductor simultaneously mutually.
2, according to the described multiple phase electrocatalysis material of claim 1, it is characterized in that: described material is by three phase compositions: it is oxygen ion conductor phase, A 2BO 4+ δPhase, gas phase; The volume fraction of described oxygen ion conductor in whole material is 10～70%, described A 2BO 4+ δVolume fraction in whole material is 10～85%.
3, according to the described multiple phase electrocatalysis material of claim 1, it is characterized in that: described material is by four phase compositions: oxygen ion conductor phase, A 2BO 4+ δPhase, electronic conductor phase, gas phase; The volume fraction of described oxygen ion conductor in whole material is 10～70%, described A 2BO 4+ δVolume fraction in whole material is 10～85%, and the volume fraction of described electronic conductor in whole material is 0～50%, and the volume fraction of described gas phase in whole material is 5～50%.
4, according to the described multiple phase electrocatalysis material of claim 1, it is characterized in that: described oxygen ion conductor is selected from mutually: doping of cerium oxide series electrolyte, or the lanthanum gallate of mixing series electrolyte, or the zirconia that mixes series electrolyte.
5, a kind of method for preparing multiple phase electrocatalysis material as claimed in claim 1, it is characterized in that: described method comprises following steps, synthetic respectively oxygen ion conductor phase, A 2BO 4+ δThe powder of phase, with metal mutually raw material, pore creating material, adhesive, plasticizer, solvent mix mutually, ball milling sieves, and prepares slurry; Utilize silk screen printing or rotation coating, spraying method slurry to be covered on the surface of dielectric substrate, then at 800～1300 ℃ of calcining 0.5～10h.
CNB2006101127772A 2006-09-01 2006-09-01 Multiple phase electrocatalysis material and preparation method thereof Expired - Fee Related CN100508259C (en)

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CN101295791B (en) * 2007-04-24 2011-01-26 中国科学院大连化学物理研究所 Ternary complex cathode material of intermediate/low temperature solid-oxide fuel battery
CN102109485B (en) * 2009-12-29 2013-10-02 比亚迪股份有限公司 Oxygen sensor electrode slurry and oxygen sensor sensing layer and preparation methods thereof
CN104934613B (en) * 2014-03-18 2018-04-06 中国科学院大连化学物理研究所 A kind of high-temperature solid oxide electrolytic cell anode material and composite anode materials
CN106410245B (en) * 2016-04-21 2018-03-13 重庆科技学院 A kind of preparation method of cathode of solid oxide fuel cell catalyst and catalytic cathode
CN110642375B (en) * 2019-11-05 2021-03-19 南京大学 Photocatalysis coupling autotrophic denitrification reactor
CN111403753A (en) * 2020-03-23 2020-07-10 武汉理工大学 La1.8Sr0.2NiO4+-Ce0.8Sm0.2O1.9Preparation method of composite cathode powder

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