CN103868962A - Test fixture of semi-sealing type solid oxide fuel cell cathode - Google Patents

Test fixture of semi-sealing type solid oxide fuel cell cathode Download PDF

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CN103868962A
CN103868962A CN201410100049.4A CN201410100049A CN103868962A CN 103868962 A CN103868962 A CN 103868962A CN 201410100049 A CN201410100049 A CN 201410100049A CN 103868962 A CN103868962 A CN 103868962A
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platinum
electrode
inner tube
test fixture
sample
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CN103868962B (en
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李箭
王方中
颜冬
池波
蒲健
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Huazhong University of Science and Technology
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Abstract

The invention discloses a test fixture of a semi-sealing type solid oxide fuel cell cathode. The test fixture comprises a fixing part, a movable part and a base, wherein the fixing part comprises an inner pipe for ventilation, an outer pipe for exhausting, a sleeve, and a first platinum wire and a first platinum net for collecting electric currents; the movable part comprises a connecting pipe which is arranged between the inner pipe and the outer pipe and is coaxial with the outer pipe; the base comprises a ceramic pipe, an end cover, a second platinum wire, a third platinum wire, a second platinum net and a third platinum net; and the second platinum wire is connected with the second platinum net, the third platinum wire is connected with the third platinum net, the first platinum net is connected with the cathode (working electrode) of a sample to be detected, the second platinum net is connected with a counter electrode of a sample to be detected, and a third platinum net is connected with a reference electrode of a sample to be detected; the test fixture is used for electrochemical testing of the electrode under a solid oxide fuel cell cathode atmosphere control condition, can reduce the complexity in an electrode sample assembling process, can ensure the assembling precision through a combined structure and achieve the effect of matching the sample in dilatation coefficient and having good atmosphere adjusting capability.

Description

A kind of test fixture of half-sealed cathode of solid oxide fuel cell
Technical field
The invention belongs to Solid Oxide Fuel Cell technical field, more specifically, relate to a kind of test fixture of half-sealed cathode of solid oxide fuel cell.
Background technology
Solid Oxide Fuel Cell is generally operational in higher temperature, comprise that its general design effort of intermediate temperature solid oxide fuel cell of development in recent years, more than 600 DEG C, therefore also needs to be adapted to accordingly the equipment of its temperature range for the research of its critical material.Because cathode of solid oxide fuel cell is operated in the environment with oxygen, therefore generally directly make it be exposed in the middle of air and do not seal, but for the dynamic (dynamical) test process General Requirements of electrode reaction, the atmosphere of electrode is regulated.Therefore generally copy the encapsulating method of anode, the sample specimens of sheet, directly by contacting, seal and realize with tubulose test fixture, also can directly be become the sample preparation of test to the U-shaped sealing difficulty of simplifying, increase reliability.
The material of test fixture is often corundum, its thermal expansivity is larger with the electrolyte difference of test sample, in test, easily there is the excessive problem that causes sample Cracking Failure of stress, if prepare the fixture close with electrolyte thermal expansivity, cost is difficult to control and need to frequently change fixture according to the difference of test material; And prepare the cost of U-shaped sample and technical difficulty is higher and length is restricted, be unfavorable for that long-term, a large amount of tests is used.
Summary of the invention
For the defect of prior art, the invention provides a kind of test fixture of half-sealed cathode of solid oxide fuel cell, object is to reduce the complexity in electrode sample assembling process, ensures the precision of assembling by knockdown structure.
The invention provides a kind of test fixture of half-sealed cathode of solid oxide fuel cell, comprise fixed part, movable part and base; Described fixed part comprises the inner tube for ventilating, the outer tube for exhaust, sleeve and the first platinum line and the first platinum guaze for collected current; Described inner tube is the pipeline with two parallel inner chambers, between the top, side of described inner tube and boss, be provided with two the first perforates, side in described inner tube is provided with two the second perforates near the first platinum guaze place, and described the first platinum line enters and is connected with the first platinum guaze that is arranged on described inner tube bottom by the inner chamber of described inner tube from described the first perforate; The second perforate is used for the excess air conducting of the interior tube cavity of flowing through to the cavity between inner tube and connecting pipe; Described sleeve is rotation body structure, comprises that annular boss, inside have the right cylinder of three grades of stepped holes and air hole; Described three grades of stepped holes comprise one-level through hole, secondary through holes and the three grades of through holes that aperture reduces successively; Described air hole is arranged on the hole wall of secondary through holes, for being communicated with secondary through holes and external environment; The aperture of described three grades of through holes is suitable with the external diameter of described inner tube, and described three grades of through holes are for fixing inner tube; The aperture of described one-level through hole is suitable with the external diameter of described outer tube, and described one-level through hole is for fixing described outer tube; Described outer tube and described inner tube coaxially arrange; Described movable part comprises connecting pipe, for connecting testing sample, between inner tube and outer tube, and with described outer coaxial tube setting; Described testing sample is sheet, is provided with working electrode at upper surface center, i.e. negative electrode is provided with electrode at lower surface center, is provided with contrast electrode in lower surface outer rim; Described base comprises ceramic pipe, is fixed on the end cap on described ceramic pipe, the second platinum line, the 3rd platinum line, the second platinum guaze and the 3rd platinum guaze for collected current; The second platinum line is connected with the second platinum guaze, the 3rd platinum line is connected with the 3rd platinum guaze, the first platinum guaze is connected with the working electrode of described testing sample, the second platinum guaze be arranged on end cap and with described testing sample electrode is connected, the 3rd platinum guaze is arranged on end cap and with the contrast electrode of described testing sample and is connected; The second platinum line has two lead-in wires, and a lead-in wire is for collecting electrode surface voltage signal, and another lead-in wire is for collecting electrode surface current signal; The 3rd platinum line is used for collecting contrast electrode surface voltage signal.
Wherein, the external diameter Φ 1 of described inner tube and the equal diameters of the working electrode of described testing sample.
Wherein, the external diameter Φ 12 of described connecting pipe is greater than the internal diameter of described outer tube
Figure BDA0000478397080000021
0.8 times.
Wherein, the length L 12 of described connecting pipe is greater than the gap width between itself and outer tube 20 times.
Wherein, the electrolyte thermal expansivity of the material of described connecting pipe and the electrolyte thermal expansivity of described testing sample are similar.
The present invention can reduce the complexity in electrode sample assembling process, ensures the precision of assembling by knockdown structure; And obtain matched coefficients of thermal expansion and sealing effectiveness meets the requirements of result by the sample of simple shape.
Brief description of the drawings
Fig. 1 is the fixed part of electrode test fixture;
Fig. 2 is the movable part of electrode test fixture and the assembling schematic diagram with fixed part thereof;
Test electrode and voltage difference to electrode under different temperatures when Fig. 3 (a) is 10kPa for partial pressure of oxygen;
Fig. 3 (b) is 800 DEG C of test electrode and the voltage differences to electrode in different partial pressure of oxygen situations.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
In Solid Oxide Fuel Cell, due to the negative electrode atmosphere inflammable articles not identical, not dangerous with anode atmosphere, therefore the fixture of cathode material test does not need identical with anode material.In line with simplifying the installation process of fixture and ensureing under the condition of measuring accuracy, can use a kind of nested fixture of half-sealed.The invention provides a kind of electrode test fixture, for the electrode electro Chemical test under cathode of solid oxide fuel cell atmosphere controlled condition.
The cell cathode sample test fixture of half-sealed provided by the invention can reduce the complexity in electrode sample assembling process, ensures the precision of assembling by knockdown structure; And obtain matched coefficients of thermal expansion and sealing effectiveness meets the requirements of result by the sample of simple shape.
The test fixture of the half-sealed cathode of solid oxide fuel cell that as depicted in figs. 1 and 2, the embodiment of the present invention provides comprises fixed part, movable part and base; The center line of 3 parts overlaps and is perpendicular to the ground, is fixed part, movable part, base from top to bottom.
Fixed part comprises the inner tube 1 for ventilating, the outer tube 3 for exhaust, sleeve 2 and the first platinum line 4 and the first platinum guaze 7 for collected current.
Sleeve 2 can select to be convenient to the metal material preparation of machining, to boss lower edge, processes the upper, middle and lower segment formula through hole 221,222,223 of aperture Φ 221 < Φ 222 < Φ 223 from plate-like upper surface.
Sleeve 2 is rotation body structure, comprises annular boss 21 and the inner right cylinder with three grades of stepped holes 22 and air hole 23; Three grades of stepped holes 22 comprise one-level through hole 221, secondary through holes 222 and the three grades of through holes 223 that aperture reduces successively; Air hole 23 is arranged on the hole wall of secondary through holes 222, for being communicated with secondary through holes 222 and external environment; The external diameter of the aperture of three grades of through holes 223 and inner tube 1 is suitable, and three grades of through holes 223 are for fixing inner tube 1; One-level through hole 221 is for fixing outer tube 3.
Wherein Φ 221 is slightly larger than inner tube 1 external diameter Φ 1, and Φ 223 is slightly larger than outer tube 3 external diameter Φ 3, is convenient to two pipes and is inserted in.The size of middle aperture Φ 222 is between Φ 1 and Φ 3, and middle part exists and lead to the vent port of sleeve 2 external environments, is convenient to the discharge of fixture internal gas flow.Inner tube 1 and outer tube 3 ensure the coincidence of center line by being inserted in sleeve 2, two pipes can use rubber ring to reach the effect of sealing with the contact portion of sleeve 2.
Inner tube 1 is for having the refractory ceramics tubing pipeline of two parallel inner chambers, its external diameter Φ 1 and working electrode are that the diameter of negative electrode is identical, between the top, side of described inner tube 1 and boss 21, be provided with two the first perforates 100, be provided with two the second perforates 200 in the side of described inner tube 1 near the place at the first platinum guaze 7 places (about 1cm).Described the first platinum line 4 enters and passes through the inner chamber of inner tube 1 from described the first perforate 100, the first perforate 100 use sealing silica gel sealings, prevent possible gas leak afterwards.The first platinum line 4 by inner tube 1 inner chamber is connected with the first platinum guaze 7 that is arranged on inner tube 1 bottom, plays the effect of collection work electrode current when test.
Test required gas and flow into bottom rear portion bottom the first platinum guaze 7 of flowing through from two, the top inner chamber of inner tube 1 and reach working electrode surface, a part is circulated in the cavity between inner tube 1 and connecting pipe 12 by the second perforate 200 of bottom end vicinity.Such design has ensured that the gas of working electrode surface under test condition can upgrade at any time on the one hand; on the other hand; flow into the gas in cavity between inner tube 1 and connecting pipe 12 by the second perforate 200 and can protect the stable of working electrode surrounding environment atmosphere, get rid of the interference that ambient atmos causes.
Outer tube 3 is high temperature resistant hollow ceramic pipe, discharge the passage of fixture as gas, flow through the gas part of testing sample 11 by upwards flow through sleeve 2 flow out to external environment through air hole 23 of outer tube 3, another part by the interstitial diffusion between outer tube 3 and connecting pipe 12 in external environment.When work, should there be certain distance (as 5mm) bottom of outer tube 3 with the upper surface of sample 11.
Movable part is made up of connecting pipe 12, its internal diameter
Figure BDA0000478397080000051
be greater than inner tube 1 external diameter Φ 1, the internal diameter of external diameter Φ 12 and outer tube 3 meet such design is gas in order to reduce outer tube 3 inner chambers and the contact area of external environment gas, prevents the pollution of external environment gas to fixture internal gas composition.After using high-temperature seal adhesive 10 that connecting pipe 12 and sample 11 are sealed when work, being inserted in fixed part uses.The cathode center to be measured that need to ensure sample when sealing-in is positioned on connecting pipe 12 center lines.
Testing sample 11 is disc-shaped, is provided with working electrode at upper surface center, is provided with electrode at lower surface center, is provided with contrast electrode in lower surface outer rim.The material of connecting pipe 12 should approach with the electrolyte thermal expansivity of sample 11 (as difference is less than 10%), and during such as sample 11 selective oxidation zirconium, connecting pipe 12 also uses zirconia, and the 11st, during with cerium oxide, connecting pipe 12 can use aluminium oxide.
The length L 12 of connecting pipe 12 need to be than the gap width between itself and outer tube 3
Figure BDA0000478397080000054
long more than 20 times, and the external diameter Φ 12 of connecting pipe 12 is greater than the internal diameter of outer tube 3
Figure BDA0000478397080000055
0.8 times.Such design one is that the distance between working electrode and top, gap is extended, the 2nd, the distance of top, gap and low side is extended, and the 3rd, reduce gap width.This structure can increase ambient atmos and diffuse into by gap the difficulty of outer tube 3 inside, adds the renewal at any time of working electrode ambient gas, has reached maintenance work electrode stable object of atmosphere under test condition.
Base is made up of ceramic pipe 13 and end cap, the second platinum line 5, the 3rd platinum line 6, the second platinum guaze 8 and the 3rd platinum guaze 9 fixed thereon.
Ceramic pipe 13 positions are fixed, and diameter is greater than the external diameter of sample 11, its interface, top level, on the end cap that diameter is identical is installed, and by fluid sealant bond, fixing, on end cap, hole, facilitate the second platinum line 5, the 3rd platinum line 6 to pass.The second platinum line 5 is connected with the second platinum guaze 8, and the 3rd platinum line 6 is connected with the 3rd platinum guaze 9.The second platinum guaze 8 be arranged on end cap and with described testing sample 11 electrode is connected, the 3rd platinum guaze 9 is arranged on end cap and with the contrast electrode of described testing sample 11 and is connected, and the 3rd platinum guaze 9 equals the distance of contrast electrode apart from sample center apart from the position of ceramic pipe 13 center lines.The second platinum line 5 has two lead-in wires, and a lead-in wire is for collecting electrode surface voltage signal, and another lead-in wire is for collecting electrode surface current signal; The 3rd platinum line 6 is for collecting contrast electrode surface voltage signal.
In embodiments of the present invention, details are as follows as example to adopt following material taking movable part:
Sample 11 uses the zirconia (YSZ) of stabilized with yttrium oxide as electrolyte, and working electrode uses La 0.8sr 0.2mnO 3material preparation, is used platinum slurry sintering to form to electrode and contrast electrode.Connecting pipe 12 uses tubular zirconium-oxide, and internal diameter, external diameter and length are respectively 9mm, 11mm and 45mm.Use glazing compound as high-temperature agglomerant, connecting pipe 12 centerings to be bonded on sample 11, after sintering, obtain having at a certain temperature the movable part of some strength.
When test, will after movable part and sample sealing-in, be inserted in fixed part, the first platinum guaze 7 of at this moment inner tube 1 lower surface laminating fully contacts with the working electrode of sample 11, due to reasons in structure, 1,3,11,12 center all point-blank.Sample 11 is supported on pedestal 13, because gravity reason end cap exists certain pressure to contrast electrode with to electrode, ensures working electrode, electrode, contrast electrode are contacted well with the first platinum guaze 7, the second platinum guaze 8, the 3rd platinum guaze 9 respectively with this.
Gap between connecting pipe 12 and outer tube 3 is another passage that fixture is inner and the external world communicates.Diffusion coefficient D=2 × 10 of airborne oxygen under standard state -5cm 2/ s, supposes Φ 12=12mm,
Figure BDA0000478397080000061
l12=20mm.Connecting pipe 12 inside are nitrogen, and outside is under the condition of air, and the speed that 25 DEG C of oxygen diffuses into connecting pipe 12 inside under equilibrium condition is 1.2 × 10 -5ml/s, 800 DEG C is 8.3 × 10 -5ml/s.Show according to above simple estimation, it is very slow that extraneous gas enters inner speed by this gap, fixture is inner continue supply gas in, can think that extraneous gas can not enter inside, internal gas is also very little to the speed of external diffusion simultaneously.
Speed with 30ml/min passes into desired gas, and the voltage difference of different temperatures test job electrode and contrast electrode is set, and is considered as the open-loop voltage OCV of battery.And judge by the calculated value of contrast Nernst equation whether near partial pressure of oxygen working electrode is consistent with the partial pressure of oxygen that passes into gas.
The voltage difference (OCV) of working electrode and contrast electrode under different temperatures when Fig. 3 (a) is 10kPa for partial pressure of oxygen.Along with the rising of temperature, the linear downward trend of OCV, its rule is consistent with theoretical value.Test data and theoretical value Error Absolute Value are between 0.1～0.2mV, and relative value is approximately 1%, consider other the influence factor such as temperature, can think that the measuring accuracy of this fixture meets experiment demand.
Fig. 3 (b) is the voltage difference (OCV) of working electrode and contrast electrode under different partial under 800 DEG C of isothermys.Along with reducing of working electrode surrounding environment partial pressure of oxygen, the absolute value of OCV is in rising trend.Its rule and theoretical value are also consistent, and error is about 1%, can think that the measuring accuracy of this fixture meets the demand of experiment test.
Those skilled in the art will readily understand; the foregoing is only preferred embodiment of the present invention; not in order to limit the present invention, all any amendments of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.

Claims (5)

1. a test fixture for half-sealed cathode of solid oxide fuel cell, is characterized in that, comprises fixed part, movable part and base;
Described fixed part comprises the inner tube (1) for ventilating, the outer tube (3) for exhaust, sleeve (2) and the first platinum line (4) and the first platinum guaze (7) for collected current; Described inner tube (1) is for having the pipeline of two parallel inner chambers, between the top, side of described inner tube (1) and boss (21), be provided with two the first perforates (100), two the second perforates (200) are located to be provided with near the first platinum guaze (7) in side in described inner tube (1), and described the first platinum line (4) enters and is connected with the first platinum guaze (7) that is arranged on described inner tube (1) bottom by the inner chamber of described inner tube (1) from described the first perforate (100); The second perforate (200) for the excess air conducting of inner tube (1) inner chamber of flowing through to the cavity between inner tube (1) and connecting pipe (12);
Described sleeve (2) is rotation body structure, comprises that annular boss (21), inside have the right cylinder of three grades of stepped holes (22) and air hole (23); Described three grades of stepped holes (22) comprise one-level through hole (221), secondary through holes (222) and the three grades of through holes (223) that aperture reduces successively; Described air hole (23) is arranged on the hole wall of secondary through holes (222), for being communicated with secondary through holes (222) and external environment; The external diameter of the aperture of described three grades of through holes (223) and described inner tube (1) is suitable, and described three grades of through holes (223) are for fixing inner tube (1); The external diameter of the aperture of described one-level through hole (221) and described outer tube (3) is suitable, and described one-level through hole (221) is for fixing described outer tube (3);
Described outer tube (3) coaxially arranges with described inner tube (1);
Described movable part comprises connecting pipe (12), for connecting testing sample (11), between inner tube and outer tube, and coaxially arranges with described outer tube (3); Described testing sample (11) is sheet, is provided with working electrode at upper surface center, i.e. negative electrode is provided with electrode at lower surface center, is provided with contrast electrode in lower surface outer rim;
Described base comprises ceramic pipe (13), is fixed on the end cap on described ceramic pipe (13), the second platinum line (5), the 3rd platinum line (6), the second platinum guaze (8) and the 3rd platinum guaze (9) for collected current; The second platinum line (5) is connected with the second platinum guaze (8), the 3rd platinum line (6) is connected with the 3rd platinum guaze (9), the first platinum guaze (7) is connected with the working electrode of described testing sample (11), the second platinum guaze (8) be arranged on end cap and with described testing sample (11) electrode is connected, the 3rd platinum guaze (9) is arranged on end cap and with the contrast electrode of described testing sample (11) and is connected; The second platinum line (5) has two lead-in wires, and a lead-in wire is for collecting electrode surface voltage signal, and another lead-in wire is for collecting electrode surface current signal; The 3rd platinum line (6) is for collecting contrast electrode surface voltage signal.
2. test fixture as claimed in claim 1, is characterized in that, the external diameter Φ 1 of described inner tube (1) and the equal diameters of the working electrode of described testing sample (11).
3. test fixture as claimed in claim 1, is characterized in that, the external diameter Φ 12 of described connecting pipe (12) is greater than the internal diameter of described outer tube (3)
Figure FDA0000478397070000021
0.8 times.
4. test fixture as claimed in claim 1, is characterized in that, the length L 12 of described connecting pipe (12) is greater than the gap width between itself and outer tube (3)
Figure FDA0000478397070000022
20 times.
5. test fixture as claimed in claim 1, is characterized in that, the electrolyte thermal expansivity of the material of described connecting pipe (12) is similar to the electrolyte thermal expansivity of described testing sample (11).
CN201410100049.4A 2014-03-18 2014-03-18 A kind of test fixture of half-sealed cathode of solid oxide fuel cell Expired - Fee Related CN103868962B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105866214A (en) * 2016-03-29 2016-08-17 华中科技大学 Electrochemical test clamp system of chromium poisoning effect of solid oxide fuel cell
CN110186967A (en) * 2019-05-17 2019-08-30 超威电源有限公司 Three electrode inspectors
CN111912777A (en) * 2020-07-15 2020-11-10 中国核动力研究设计院 Sample fixing device for high-temperature and high-pressure electrochemical experiment and mounting method thereof
CN113049653A (en) * 2021-04-01 2021-06-29 南京理工大学 Integrated evaluation device and method for gas impurity poisoning of fuel cell material
US11296342B2 (en) * 2017-07-25 2022-04-05 Kent State University Universal tubular solid oxide fuel cell testing kit

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CN101122577A (en) * 2007-09-14 2008-02-13 清华大学 Solid oxide electrolytic cell high temperature electrochemical property test device
CN101216445A (en) * 2007-12-29 2008-07-09 清华大学 High-temperature solid oxide single electrolytic cell fixing test bracket
CN101980009A (en) * 2010-09-10 2011-02-23 清华大学 Solid oxide electrolytic cell testing bracket
CN102967733A (en) * 2012-10-19 2013-03-13 华中科技大学 Solid oxide fuel cell (SOFC) button type cell testing clamp and assembling method thereof

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Publication number Priority date Publication date Assignee Title
CN101122577A (en) * 2007-09-14 2008-02-13 清华大学 Solid oxide electrolytic cell high temperature electrochemical property test device
CN101216445A (en) * 2007-12-29 2008-07-09 清华大学 High-temperature solid oxide single electrolytic cell fixing test bracket
CN101980009A (en) * 2010-09-10 2011-02-23 清华大学 Solid oxide electrolytic cell testing bracket
CN102967733A (en) * 2012-10-19 2013-03-13 华中科技大学 Solid oxide fuel cell (SOFC) button type cell testing clamp and assembling method thereof

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105866214A (en) * 2016-03-29 2016-08-17 华中科技大学 Electrochemical test clamp system of chromium poisoning effect of solid oxide fuel cell
US11296342B2 (en) * 2017-07-25 2022-04-05 Kent State University Universal tubular solid oxide fuel cell testing kit
CN110186967A (en) * 2019-05-17 2019-08-30 超威电源有限公司 Three electrode inspectors
CN110186967B (en) * 2019-05-17 2021-06-18 超威电源集团有限公司 Three-electrode detection device
CN111912777A (en) * 2020-07-15 2020-11-10 中国核动力研究设计院 Sample fixing device for high-temperature and high-pressure electrochemical experiment and mounting method thereof
CN111912777B (en) * 2020-07-15 2022-03-01 中国核动力研究设计院 Sample fixing device for high-temperature and high-pressure electrochemical experiment and mounting method thereof
CN113049653A (en) * 2021-04-01 2021-06-29 南京理工大学 Integrated evaluation device and method for gas impurity poisoning of fuel cell material
CN113049653B (en) * 2021-04-01 2023-10-31 南京理工大学 Integrated evaluation device and method for fuel cell material gas impurity poisoning

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