CN104835969B - Method for preparing porous electrode with high specific surface area - Google Patents

Method for preparing porous electrode with high specific surface area Download PDF

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CN104835969B
CN104835969B CN201510278697.3A CN201510278697A CN104835969B CN 104835969 B CN104835969 B CN 104835969B CN 201510278697 A CN201510278697 A CN 201510278697A CN 104835969 B CN104835969 B CN 104835969B
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thermochemical treatment
pulsed plasma
porous electrode
treatment stove
surface area
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CN104835969A (en
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张雁祥
闫牧夫
王祎雪
张华良
李怀旭
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Harbin Institute of Technology
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88—Processes of manufacture
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/8605—Porous electrodes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

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  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Inert Electrodes (AREA)

Abstract

A method for preparing a porous electrode with a high specific surface area relates to a preparation method of a porous electrode. The purpose of the invention is to solve the problem that a conventional nanostructured electrode, which is prepared by using a solution dipping method, needs to be dipped many times, and is low in preparation efficiency and repetitive rate, and the adopted chemical solution causes serious pollution to the environment. The method comprises the steps as follows: suspending a porous electrolyte/dielectric and a catalyst target on a sample holder of a pulse plasma multicomponent thermochemical furnace, vacuumizing, and maintaining pressure; and inflating hydrogen, then inflating hydrogen and argon, and keeping warm to obtain aporous electrode. In this way, the method for preparing the porous electrode with the high specific surface area is achieved. Compared with a conventional solution dipping method, the method of the invention can be used for forming the porous electrode with the high specific surface area within hours, is shortened more than ten times in preparation period, and therefore is reduced in cost. The invention provides the method that can prepare the porous electrode with the high specific surface area.

Description

A kind of method preparing high specific surface area porous electrode
Technical field
The present invention relates to a kind of preparation method of porous electrode.
Background technology
Porous media, especially inorganic non-metallic porous ceramic electrolyte/electrolyte has important application in numerous areas. Adulterated with Ca and Ti ore and stablize fluorite structure oxide in gas phase seperation film, oxygen permeable membrane, membrane reactor, solid fuel cell, solid Irreplaceable function is played on the devices such as body electrolyzer.The main source limiting these device performances has two：One is surface Process (as surface chemical reaction, interfacial charge transfer etc.), two is body phase process (as oxonium ion, the electronics biography in thin film Lead).By reducing film thickness, existing film preparing technology can reduce the resistance of body phase process to greatest extent.As The resistance what reduces surface process is the important topic that educational circles and industrial quarters face.
Surface process is concentrated mainly on the position that gas phase/electronic conductor/ion conductor intersects, that is, at three phase boundary.Mesh The method of front common electrolyte/electrolyte powder body and catalyst powder (such as NiO, CuO, Pt, perovskite etc.) mix grinding-co-sintering exists Prepare one layer of composite porous electrode on electrolyte/dielectric surface, three phase boundary is expanded to electrode interior, then pass through to increase The quantity of surface chemical reaction active sites reduces interface impedance.But how particle size is micro- in the electrode of mix grinding-sintering preparation Rice magnitude, three phase boundary density is usually 0.1～1 μm/μm3.Particle diameter is reduced to nano-scale certainly will increase three phase boundary Density.Nearly ten years, solution dipping method becomes laboratory and prepares nano structure electrode most common method.The method includes two Process：First catalyst pioneer's liquid (being often nitrate solution or fused solution) is impregnated in porous electrolyte skeleton, Ran Hou 800 DEG C～900 DEG C are fired into phase.The catalyst being formed is covered on skeleton surface with the form of nanoparticle.The method is produced Raw three phase boundary length is usually 1～100 μm/μm3, that is, hypergeometric surface area is 1～100 μm/μm3.Due to single impregnation-roasting Burn the catalytic amount being formed very limited, generally will repeatedly impregnate-roasting just can have the considerable pickup of comparison, lead to preparation effect Rate is low.Technological parameter is difficult to precise control, leads to repetitive rate low.In addition, chemical solution also can not be ignored to the pollution of environment.This It is the immediate cause that the method is not yet applied to industrial circle a bit.
Content of the invention
The invention aims to the nano structure electrode solving existing use solution dipping method preparation needs repeatedly to impregnate, The problem that preparation efficiency is low, repetitive rate is low and the chemical solution of use is big for environment pollution, and provide one kind to prepare high-ratio surface The method of long-pending porous electrode.
A kind of method preparing high specific surface area porous electrode, completes according to the following steps：
First, porous electrolyte/electrolyte and catalyst target are suspended on the sample of pulsed plasma multicomponent thermochemical treatment stove On frame, then pulsed plasma multicomponent thermochemical treatment stove evacuation to vacuum is 10Pa～30Pa, then pulsed plasma is many First permeation stove is 10Pa～30Pa in vacuum and DC voltage is to keep 10min～30min under 500V～700V；
2nd, 1., in pulsed plasma multicomponent thermochemical treatment stove, it is passed through H2, more simultaneously to pulsed plasma multicomponent thermochemical treatment stove Evacuation, makes pressure in pulsed plasma multicomponent thermochemical treatment stove be 50Pa～100Pa, then pressure for 50Pa～100Pa and H2Atmosphere under by pulsed plasma multicomponent thermochemical treatment stove be incubated 10min～30min；
2., into pulsed plasma multicomponent thermochemical treatment stove, it is passed through hydrogen and argon, more simultaneously polynary to pulsed plasma Permeation stove evacuation, makes pressure in pulsed plasma multicomponent thermochemical treatment stove be 100Pa～1000Pa, temperature is 800 DEG C～900 DEG C, then it is incubated 2h～10h under conditions of pressure is 800 DEG C～900 DEG C for 100Pa～1000Pa and temperature；
Step 2 2. described in hydrogen and argon flow-rate ratio be 3:1；
3rd, stop being passed through argon, continue to be passed through hydrogen, by porous electrolyte/electrolyte and catalyst target in hydrogen gas Naturally cool to room temperature under atmosphere, obtain porous electrode；Complete a kind of method preparing high specific surface area porous electrode.
The principle and advantage of the present invention：
A kind of method preparing high specific surface area porous electrode of the first, present invention is easily operated, and preparation efficiency is high；
2nd, compared to solution dipping method, the present invention is oozed principle using thermal expansion and is directly formed nano-catalytic in porous electrode Oxidant layer, and technological parameter is accurately controlled, the accuracy controlling of achievable catalyst size and distribution；
3rd, the present invention reduces the directly contact of people and chemical reagent to greatest extent, safe and clean；
4th, the three phase boundary length using the porous electrode of method of the present invention preparation is 120 μm/μm3～130 μm/μm3 Suitable with the nanometer particle size of solution dipping method；
5th, the porous electrode prepared using the inventive method, can be within a few houres compared with using existing solution dipping method Form high-ratio surface porous electrode, compared with existing solution dipping method, manufacturing cycle shortens more than ten times, therefore also reduces into This；
6th, the present invention utilizes plasma glow discharge effect, ionized gaseous molecules, etching catalyst target, makes catalyst Atom is deposited with inside porous electrode, forms high-ratio surface porous electrode.
The present invention can obtain a kind of method preparing high specific surface area porous electrode.
Brief description
Fig. 1 is the SEM figure of the porous electrode of test one preparation；
Fig. 2 is XRD figure, and in Fig. 2,1 is porous electrolyte/dielectric XRD curve, and 2 is the porous electrode of test one preparation XRD curve, # be YSZ phase, $ be Ni3Fe phase,！For Fe0.64Ni0.36Phase, ＆ is NiO phase；
Fig. 3 is the SEM figure of the porous electrode inner hole wall of test one preparation；
Fig. 4 is the EDS scanning figure of the porous electrode inner hole wall of test one preparation, and in Fig. 4,1 is Zr Elemental redistribution, and 2 is Ni unit Element is distributed, 3 is Y element distribution, and 4 is O Elemental redistribution, and 5 is the Elemental redistribution of Fe.
Specific embodiment
Specific embodiment one：Present embodiment is a kind of method preparing high specific surface area porous electrode is by following step Suddenly complete：
First, porous electrolyte/electrolyte and catalyst target are suspended on the sample of pulsed plasma multicomponent thermochemical treatment stove On frame, then pulsed plasma multicomponent thermochemical treatment stove evacuation to vacuum is 10Pa～30Pa, then pulsed plasma is many First permeation stove is 10Pa～30Pa in vacuum and DC voltage is to keep 10min～30min under 500V～700V；
2nd, 1., in pulsed plasma multicomponent thermochemical treatment stove, it is passed through H2, more simultaneously to pulsed plasma multicomponent thermochemical treatment stove Evacuation, makes pressure in pulsed plasma multicomponent thermochemical treatment stove be 50Pa～100Pa, then pressure for 50Pa～100Pa and H2Atmosphere under by pulsed plasma multicomponent thermochemical treatment stove be incubated 10min～30min；
2., into pulsed plasma multicomponent thermochemical treatment stove, it is passed through hydrogen and argon, more simultaneously polynary to pulsed plasma Permeation stove evacuation, makes pressure in pulsed plasma multicomponent thermochemical treatment stove be 100Pa～1000Pa, temperature is 800 DEG C～900 DEG C, then it is incubated 2h～10h under conditions of pressure is 800 DEG C～900 DEG C for 100Pa～1000Pa and temperature；
Step 2 2. described in hydrogen and argon flow-rate ratio be 3:1；
3rd, stop being passed through argon, continue to be passed through hydrogen, by porous electrolyte/electrolyte and catalyst target in hydrogen gas Naturally cool to room temperature under atmosphere, obtain porous electrode；Complete a kind of method preparing high specific surface area porous electrode.
The principle and advantage of present embodiment：
A kind of method preparing high specific surface area porous electrode of the first, present embodiment is easily operated, and preparation efficiency is high；
2nd, compared to solution dipping method, present embodiment is oozed principle using thermal expansion and is directly formed nanometer in porous electrode Catalyst layer, and technological parameter is accurately controlled, the accuracy controlling of achievable catalyst size and distribution；
3rd, present embodiment reduces the directly contact of people and chemical reagent to greatest extent, safe and clean；
4th, the three phase boundary length using the porous electrode of method preparation of present embodiment is 120 μm/μm3～130 μ m/μm3Suitable with the nanometer particle size of solution dipping method；
5th, the porous electrode prepared using present embodiment method, can be several little compared with using existing solution dipping method When interior formation high-ratio surface porous electrode, compared with existing solution dipping method, manufacturing cycle shorten more than ten times, therefore also reduce Cost；
6th, present embodiment utilizes plasma glow discharge effect, ionized gaseous molecules, etching catalyst target, makes to urge Agent atom is deposited with inside porous electrode, forms high-ratio surface porous electrode.
Present embodiment can obtain a kind of method preparing high specific surface area porous electrode.
Specific embodiment two：The difference from specific embodiment one for the present embodiment is：Many described in step one Hole electrolyte/electrolyte is porous yttrium stable zirconium oxide, porous YSZ/NiO complex, porous samarium doping cerium oxide or porous Al2O3/SiO2Complex.Other are identical with specific embodiment one.
Porous YSZ/NiO complex described in present embodiment mix in any proportion for porous YSZ and porous NiO and Become；Described porous Al2O3/SiO2Complex is porous Al2O3With porous SiO2Mix in any proportion.
Specific embodiment three：Present embodiment with one of specific embodiment one or two difference is：Institute in step one The porous electrolyte stated/dielectric thickness is 0.5mm～1mm.Other steps are identical with specific embodiment one or two.
Specific embodiment four：Present embodiment with one of specific embodiment one to three difference is：Institute in step one The catalyst target stated is Ni target, Fe target or Cu target.Other steps are identical with specific embodiment one to three.
Specific embodiment five：Present embodiment with one of specific embodiment one to four difference is：Institute in step one The catalyst target stated is bulk catalyst target, sheet catalyst target, netted catalyst target or cystose catalyst target Material.Other steps are identical with specific embodiment one to four.
Specific embodiment six：Present embodiment with one of specific embodiment one to five difference is：Will in step one Porous electrolyte/electrolyte and catalyst target are suspended on the specimen mounting of pulsed plasma multicomponent thermochemical treatment stove, then by pulse Plasma multicomponent thermochemical treatment stove evacuation to vacuum is 10Pa, then pulsed plasma multicomponent thermochemical treatment stove in vacuum is 10Pa and DC voltage are to keep 30min under 600V.Other steps are identical with specific embodiment one to five.
Specific embodiment seven：Present embodiment with one of specific embodiment one to six difference is：Step 2 1. in It is passed through H in pulsed plasma multicomponent thermochemical treatment stove2, more simultaneously to pulsed plasma multicomponent thermochemical treatment stove evacuation, make pulse Pressure in plasma multicomponent thermochemical treatment stove is 80Pa～100Pa, then is 80Pa～100Pa and H in pressure2Atmosphere under by arteries and veins Rush plasma multicomponent thermochemical treatment stove insulation 30min.Other steps are identical with specific embodiment one to six.
Specific embodiment eight：Present embodiment with one of specific embodiment one to seven difference is：Step 2 2. in It is passed through hydrogen and argon into pulsed plasma multicomponent thermochemical treatment stove, then pulsed plasma multicomponent thermochemical treatment stove is taken out very simultaneously Sky, makes in pulsed plasma multicomponent thermochemical treatment stove pressure be 100Pa, temperature is 900 DEG C, then is 100Pa in pressure and temperature is It is incubated 2h under conditions of 900 DEG C.Other steps are identical with specific embodiment one to seven.
Specific embodiment nine：Present embodiment with one of specific embodiment one to eight difference is：Step 2 1. in The purity of described hydrogen is 99.999%；Step 2 2. described in the purity of hydrogen be 99.999%, described argon Purity is 99.999%.Other steps are identical with specific embodiment one to eight.
Specific embodiment ten：Present embodiment with one of specific embodiment one to nine difference is：Institute in step one The porous electrolyte stated/dielectric aperture is 0.5 μm～1 μm.Other steps are identical with specific embodiment one to nine.
Advantages of the present invention is verified using tests below：
Test one：A kind of method preparing high specific surface area porous electrode completes according to the following steps：
First, porous electrolyte/electrolyte and catalyst target are suspended on the sample of pulsed plasma multicomponent thermochemical treatment stove On frame, then pulsed plasma multicomponent thermochemical treatment stove evacuation to vacuum is 10Pa, then by pulsed plasma multicomponent thermochemical treatment Stove is 10Pa in vacuum and DC voltage is to keep 30min under 600V；
Porous electrolyte/electrolyte described in step one is porous YSZ/NiO complex；Described porous YSZ/NiO In complex, the weight fraction for 60%, NiO for the weight fraction of YSZ is 40%；
The thickness of described porous YSZ/NiO complex is 0.5mm, a diameter of 10mm, and aperture is 1 μm；
Catalyst target described in step one is cystose Ni target；
2nd, 1., in pulsed plasma multicomponent thermochemical treatment stove, it is passed through H2, more simultaneously to pulsed plasma multicomponent thermochemical treatment stove Evacuation, makes the pressure in pulsed plasma multicomponent thermochemical treatment stove be 80Pa, then is 80Pa and H in pressure2Atmosphere under by arteries and veins Rush plasma multicomponent thermochemical treatment stove insulation 30min；
Step 2 1. described in hydrogen purity be 99.999%；
2., into pulsed plasma multicomponent thermochemical treatment stove, it is passed through hydrogen and argon, more simultaneously polynary to pulsed plasma Permeation stove evacuation, makes pressure in pulsed plasma multicomponent thermochemical treatment stove be 100Pa, temperature is 900 DEG C, then in pressure is 100Pa and temperature are for being incubated 2h under conditions of 900 DEG C；
Step 2 2. described in hydrogen and argon flow-rate ratio be 3:1；
Step 2 2. described in the purity of hydrogen be 99.999%, the purity of described argon is 99.999%；
3rd, stop being passed through argon, continue to be passed through hydrogen, by porous electrolyte/electrolyte and catalyst target in hydrogen gas Naturally cool to room temperature under atmosphere, obtain porous electrode；Complete a kind of method preparing high specific surface area porous electrode.
Fig. 1 is the SEM figure of the porous electrode of test one preparation；It can be seen from figure 1 that Ni nanoparticle granule is evenly distributed on YSZ bone On frame surface, the average diameter of Ni is 48nm, suitable with the nanometer particle size of the 50nm～100nm of solution dipping method；YSZ skeleton Mean diameter is 1.6 μm；Expand and there is no three phase boundary before oozing, expand and ooze rear three phase boundary length for 125 μm/μm3.
Fig. 2 is XRD figure, and in Fig. 2,1 is porous electrolyte/dielectric XRD curve, and 2 is the porous electrode of test one preparation XRD curve, # be YSZ phase, $ be Ni3Fe phase,！For Fe0.64Ni0.36Phase, ＆ is NiO phase；
The XRD diffraction maximum of the porous YSZ/NiO Composite Scaffolds before plating is oozed as can be seen from Figure 2 substantially, does not have other dephasigns；From Not there is chemical reaction in the YSZ that the XRD diffraction maximum of the porous electrode that plating obtains after oozing can be seen that in electrode skeleton, and NiO Reducing atmosphere during being oozed due to plating, is Ni by Restore All3Fe and Fe0.64Ni0.36, Fe therein is from stove inwall quilt The Fe that plasma bombardment gets off；Chemically stable under hydrocarbon fuel for the porous electrode can be increased after forming Fe-Ni compound Property.
Fig. 3 is the SEM figure of the porous electrode inner hole wall of test one preparation；Fig. 4 is the porous electrode endoporus of test one preparation The EDS scanning figure of wall, in Fig. 4,1 is Zr Elemental redistribution, and 2 is Ni Elemental redistribution, 3 is Y element distribution, and 4 is O Elemental redistribution, and 5 are The Elemental redistribution of Fe；
Knowable to Fig. 3 and Fig. 4, the granule that porous electrode YSZ skeleton inner surface is formed contains Ni element and Fe element, with XRD diffraction patterns always, and confirm that the granule on skeleton is to ooze formation by plating, and in non-porous YSZ/NiO skeleton Original Ni.

Claims (8)

1. a kind of method preparing high specific surface area porous electrode is it is characterised in that a kind of prepare high specific surface area porous electrode Method completes according to the following steps：
First, electrolyte and catalyst target are suspended on the specimen mounting of pulsed plasma multicomponent thermochemical treatment stove, then by pulse etc. Gas ions multicomponent thermochemical treatment stove evacuation to vacuum is 10Pa～30Pa, then by pulsed plasma multicomponent thermochemical treatment stove in vacuum Be 10Pa～30Pa and DC voltage be under 500V～700V, to keep 10min～30min；
Electrolyte described in step one is porous yttrium stable zirconium oxide, porous YSZ/NiO complex, porous samarium doping cerium oxide Or porous Al2O3/SiO2Complex；
Catalyst target described in step one is Ni target, Fe target or Cu target；
2nd, 1., in pulsed plasma multicomponent thermochemical treatment stove, it is passed through H2, then pulsed plasma multicomponent thermochemical treatment stove is taken out very simultaneously Sky, makes the pressure in pulsed plasma multicomponent thermochemical treatment stove be 50Pa～100Pa, then is 50Pa～100Pa and H in pressure2's Under atmosphere, pulsed plasma multicomponent thermochemical treatment stove is incubated 10min～30min；
2., into pulsed plasma multicomponent thermochemical treatment stove, it is passed through hydrogen and argon, more simultaneously to pulsed plasma multicomponent thermochemical treatment Stove evacuation, makes pressure in pulsed plasma multicomponent thermochemical treatment stove be 100Pa～1000Pa, temperature is 800 DEG C～900 DEG C, then It is incubated 2h～10h under conditions of pressure is 800 DEG C～900 DEG C for 100Pa～1000Pa and temperature；
Step 2 2. described in hydrogen and argon flow-rate ratio be 3:1；
3rd, stop being passed through argon, continue to be passed through hydrogen, electrolyte and catalyst target are naturally cooled to room in a hydrogen atmosphere Temperature, obtains porous electrode；Complete a kind of method preparing high specific surface area porous electrode.
2. a kind of method preparing high specific surface area porous electrode according to claim 1 is it is characterised in that in step one The thickness of described electrolyte is 0.5mm～1mm.
3. a kind of method preparing high specific surface area porous electrode according to claim 1 is it is characterised in that in step one Described catalyst target is bulk catalyst target, sheet catalyst target, netted catalyst target or cystose catalyst Target.
4. a kind of method preparing high specific surface area porous electrode according to claim 1 is it is characterised in that in step one Electrolyte and catalyst target are suspended on the specimen mounting of pulsed plasma multicomponent thermochemical treatment stove, then pulsed plasma is many First permeation stove evacuation to vacuum is 10Pa, then pulsed plasma multicomponent thermochemical treatment stove is 10Pa and unidirectional current in vacuum Press as keeping 30min under 600V.
5. a kind of method preparing high specific surface area porous electrode according to claim 1 it is characterised in that step 2 1. It is passed through H in the middle multicomponent thermochemical treatment stove to pulsed plasma2, more simultaneously to pulsed plasma multicomponent thermochemical treatment stove evacuation, make arteries and veins The pressure rushing in plasma multicomponent thermochemical treatment stove is 80Pa～100Pa, then is 80Pa～100Pa and H in pressure2Atmosphere under will Pulsed plasma multicomponent thermochemical treatment stove is incubated 30min.
6. a kind of method preparing high specific surface area porous electrode according to claim 1 it is characterised in that step 2 2. It is passed through hydrogen and argon in the middle multicomponent thermochemical treatment stove to pulsed plasma, then pulsed plasma multicomponent thermochemical treatment stove is taken out very simultaneously Sky, makes in pulsed plasma multicomponent thermochemical treatment stove pressure be 100Pa, temperature is 900 DEG C, then is 100Pa in pressure and temperature is It is incubated 2h under conditions of 900 DEG C.
7. a kind of method preparing high specific surface area porous electrode according to claim 1 it is characterised in that step 2 1. Described in hydrogen purity be 99.999%；Step 2 2. described in the purity of hydrogen be 99.999%, described argon Purity be 99.999%.
8. a kind of method preparing high specific surface area porous electrode according to claim 1 is it is characterised in that in step one The aperture of described electrolyte is 0.5 μm～1 μm.
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JP2002014076A (en) * 2000-06-30 2002-01-18 Tokyo Gas Co Ltd Solid electrolyte type micro gas sensor and its manufacturing method
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002014076A (en) * 2000-06-30 2002-01-18 Tokyo Gas Co Ltd Solid electrolyte type micro gas sensor and its manufacturing method
CN103390739A (en) * 2012-05-11 2013-11-13 中国科学院大连化学物理研究所 Solid oxide fuel cell cerium-oxide-based electrolyte barrier layer and preparation method thereof

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