CN207232070U - It is a kind of to be used for the oxidation zirconium electrode that oxonium ion detects in high-temperature molten salt - Google Patents
It is a kind of to be used for the oxidation zirconium electrode that oxonium ion detects in high-temperature molten salt Download PDFInfo
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- CN207232070U CN207232070U CN201720922184.6U CN201720922184U CN207232070U CN 207232070 U CN207232070 U CN 207232070U CN 201720922184 U CN201720922184 U CN 201720922184U CN 207232070 U CN207232070 U CN 207232070U
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Abstract
The utility model belongs to high-temperature molten salt electrochemical analysis testing field, there is provided a kind of to be used for the oxidation zirconium electrode that oxonium ion detects in high-temperature molten salt, the oxidation zirconium electrode includes：Upper electrode fixing piece, electrode fix ball, lower electrode fixing piece, electrode body；The electrode body mainly includes：Silver electrode lead wires, upper sealing-plug, alundum tube, lower sealing-plug, tubular zirconium-oxide, interior reference fused salt.Used simple, easy to assembly, small, light-weight, suitable for various composition the high-temperature molten salt of zirconium oxide electrode structure in oxygen ion concentration, and laboratory condition, measurement result is accurate, be quick on the draw, range ability is big.
Description
Technical field
The utility model belongs to high-temperature molten salt electrochemical analysis testing field, more particularly to a kind of to be used for oxygen in high-temperature molten salt
The oxidation zirconium electrode of ion detection.
Background technology
High-temperature molten salt because its good conductivity, steam forces down, viscosity is low and thermal capacity is big the advantages that, be commonly used for metallurgical industry
In chemical reaction medium.Developed rapidly as fused salt is metallurgical, fused salt metallurgical technology there has also been higher to the quality of fused salt
It is required that the concentration of the oxonium ion wherein in fused salt is an important factor of molten salt nature, fused salt metallurgical technology is influenced very
Greatly.Therefore, the oxygen ion concentration dissolved in Accurate Determining fused salt is extremely important.
At present, in fused salt oxygen content measure, there has been no unified, general assay method at present.Analysed using oxygen part
Oxygen content in instrument (inert gas fusion infra-red sepectrometry) measure fused salt, but take such means can not reflect the oxygen in fused salt in real time
Ion concentration, and be predicted more difficult；Oxonium ion in fused salt can be measured in low concentration using square wave voltammetry to contain
Amount, but since the corrosion of metal anode, error are larger.Acid-base titration can with the oxonium ion content in off-line analysis fused salt, but
In low concentration, error is larger.
Usually adulterate some oxides as stabilizer by the use of zirconium oxide, the yttrium stable zirconium oxide material after sinter molding have compared with
Good oxonium ion selectivity.Solid electrolyte of yttrium oxide stabilized zirconium oxide to oxonium ion due to there are oxygen ion vacancy, having choosing
Selecting property.Side is poor there are oxygen ion concentration inside and outside oxidation zirconium electrode, produces oxonium ion concentration potential.Yttria-stabilized zirconia electricity
Oxygen ion concentration is kept certain in extremely interior interior reference fused salt, when oxygen ion concentration changes in fused salt to be measured, then in electrode
The oxonium ion concentration potential in outside also changes.Pass through surveyed potential relation corresponding from different oxygen ion concentrations, can measure
Oxygen ion concentration in fused salt.At present, the measuring cell of oxygen concentration in high temperature fluent metal is industrially measured with Mn/MnO2、Cr/
Cr2O3、Bi/Bi2O3For the oxidation zirconium electrode of interior reference, but these electrode measurement oxygen ranges are smaller and sufficiently bulky, no
Just it is used for the concentration of oxonium ion in a small amount of high-temperature molten salt of laboratory on-line checking.
The content of the invention
(1) purpose of innovation and creation
For overcome the deficiencies in the prior art, the utility model provide it is a kind of it is small, simple in structure, range is big, measurement
Accurately, suitable for the on-line checking high-temperature molten salt of laboratory oxonium ion oxidation zirconium electrode.
(2) technical solution
To solve the deficiencies in the prior art, the utility model is realized by following scheme：
A kind of to be used for the oxidation zirconium electrode that oxonium ion detects in high-temperature molten salt, the oxidation zirconium electrode mainly includes：On
Portion's electrode fixuture, electrode fix ball, lower electrode fixing piece, electrode body.
The upper electrode fixing piece is screw shaped structure, and upper electrode fixing piece, which is equipped with, runs through circular hole, and lower face is equipped with
Spherical groove；The lower electrode fixing piece is negative and positive screw shaped structure, and lower electrode fixing piece, which is equipped with, runs through circular hole, and top is cloudy
Threaded hole bottom is equipped with spherical groove；The upper electrode fixing piece is fixedly connected with lower electrode fixing piece；The electrode is consolidated
Determine ball and be equipped with the circular hole for running through the centre of sphere, Circularhole diameter is identical with corundum pipe outside diameter, and electrode fixes ball and is located at upper electrode fixing piece
With the inside of spherical groove of lower electrode fixing piece.
The electrode body mainly includes：It is silver electrode lead wires, upper sealing-plug, alundum tube, lower sealing-plug, tubular zirconium-oxide, interior
Reference fused salt；The upper sealing-plug, which is equipped with, runs through circular hole, and upper sealing-plug is fixedly connected with alundum tube upper end, upper sealing-plug and corundum
Pipe fixed connection place seals；The alundum tube fixes ball, lower electrode fixing piece through upper electrode fixing piece, electrode；It is described
Lower sealing-plug, which is equipped with, runs through circular hole, and lower sealing-plug is fixedly connected with tubular zirconium-oxide upper end, lower sealing-plug and tubular zirconium-oxide junction
Sealing；The tubular zirconium-oxide is mixed with 8%mol yittrium oxide, and end closure under tubular zirconium-oxide, tubular zirconium-oxide upper end is consolidated with alundum tube lower end
Fixed connection, tubular zirconium-oxide are sealed with alundum tube junction；The interior reference fused salt is located inside tubular zirconium-oxide；The silver electrode is drawn
For line through upper sealing-plug, alundum tube, lower sealing-plug, tubular zirconium-oxide, interior reference fused salt is submerged to tubular zirconium-oxide bottom, upper end in lower end
In stretching outside sealing-plug.
The interior reference fused salt is containing AgCl and indivisible Li2CO3Institute's pyrometry fused salt, wherein AgCl contents are 0.5-
0.8 mol/kg, Li2CO3Content is 0.03-0.1mol/kg, and interior reference fused salt addition is 0.5-1g.
The tubular zirconium-oxide thickness is 1-2mm.
The upper sealing-plug and alundum tube fixed connection place are to be wound upper sealing-plug using polytetrafluoro raw material band, and with high
Warm ceramic glue is applied to polytetrafluoro raw material band face seal.
The lower sealing-plug is sealed with the sealing of tubular zirconium-oxide fixed connection place using refractory ceramics glue.
The tubular zirconium-oxide is fixedly connected as be bonded with alundum tube.
The upper sealing-plug, lower sealing-plug material are heat-resisting material.
It is elastic material that the electrode, which fixes ball material,.
(3) beneficial effect
To overcome the problems such as prior art measuring apparatus volume is big, measurement range is small, poor accuracy, the utility model provides
A kind of oxidation zirconium electrode.Wherein oxidation zirconium electrode only includes main-body electrode, upper electrode fixing piece, electrode and fixes ball, lower part
Electrode fixuture, therefore simple, easy to assembly, small, light-weight, suitable for various composition the high-temperature molten salt of the electrode structure
Middle oxygen ion concentration, while be very suitable for using in laboratory；Ball, lower electrode are fixed with reference to upper electrode fixing piece, electrode
Fixing piece then fixes ball when tightening screw thread with the top and the bottom electrode fixuture that is fated to centre extruding electrode, and electrode is fixed ball and is subject to
Extruding then extrudes alundum tube to centre, achievees the purpose that fixed oxidation zirconium electrode；Zirconium electrode is aoxidized to use mixed with 8% yittrium oxide
Aoxidize zirconium electrode, thickness 1-2mm, interior equipped with AgCl contents is 0.5-0.8mol/kg, Li2CO3Content is 0.03-0.1mol/
The institute pyrometry fused salt 0.5-1g of kg, the sensitive and scope of the oxonium ion detection greatly increased.
Brief description of the drawings
Fig. 1 aoxidizes the structure diagram of zirconium electrode.
Fig. 2 aoxidizes the critical piece figure of zirconium electrode.
3 electrode fixuture top of sealing-plug, 4 electrode fixes 5 electrode fixuture lower part of ball wherein in 1 silver electrode lead wires 2
10 electrode body of reference fused salt in 6 sealing-plug of alundum tube 7 times, 8 tubular zirconium-oxide 9
Embodiment
The utility model is described in further detail in embodiment below in conjunction with the accompanying drawings：
As shown in Fig. 2, oxidation zirconium electrode mainly includes：Upper electrode fixing piece 3, electrode fix ball 4, lower electrode is fixed
Part 5, electrode body 10；Upper electrode fixing piece 3 is screw shaped structure, and upper electrode fixing piece 3, which is equipped with, runs through circular hole, lower end
Face is equipped with spherical groove；Lower electrode fixing piece 5 is negative and positive screw shaped structure, and lower electrode fixing piece 5, which is equipped with, runs through circular hole, pushes up
End female threaded hole bottom is equipped with spherical groove；Upper electrode fixing piece 3 is threadedly coupled with lower electrode fixing piece 5；Electrode is fixed
Ball 4 is equipped with the circular hole through the centre of sphere, and Circularhole diameter is identical with 6 outside diameter of alundum tube, and electrode fixes ball 4 and is located at upper electrode fixing piece
3 and the inside of spherical groove of lower electrode fixing piece 5；
As shown in Figure 1, electrode body 10 mainly includes：Silver electrode lead wires 1, upper sealing-plug 2, alundum tube 6, lower sealing-plug 7,
Tubular zirconium-oxide 8, interior reference fused salt 9；Upper sealing-plug 2, which is equipped with, runs through circular hole, and material is polytetrafluoroethylene (PTFE)；Twined outside upper sealing-plug 2
Polytetrafluoro raw material belt surface is applied to around polytetrafluoro raw material band, and with refractory ceramics glue, for clogging 6 upper port of alundum tube；On
Portion's electrode fixuture 3, electrode fix ball 4, lower electrode fixing piece 5 is sleeved on alundum tube 6；Lower sealing-plug 7 is equipped with through circle
Hole, material are quartz；Polytetrafluoro raw material band is wound outside lower sealing-plug 7, and polytetrafluoro raw material band table is applied to refractory ceramics glue
Face, for clogging 8 upper port of tubular zirconium-oxide；Tubular zirconium-oxide 8 is mixed with 8%mol yittrium oxide, 8 times end closures of tubular zirconium-oxide；Oxidation
8 upper end of zirconium pipe is Nian Jie with 6 lower end of alundum tube；Interior reference fused salt 9 is located at 8 bottom of tubular zirconium-oxide；Silver electrode lead wires 1 pass through upper close
Interior reference fused salt 9 is submerged to 9 bottom of tubular zirconium-oxide in blocking 2, alundum tube 6, lower sealing-plug 7, tubular zirconium-oxide 8, lower end, and upper end is stretched
Go out outside upper sealing-plug 2.
When wherein top terminal fixing piece 3 tightens screw thread with lower electrode fixing piece 5, it is located at spherical groove to centre extruding
Interior electrode fixes ball 4, forces electrode to fix ball 4 and fixes alundum tube 6 of the ball 4 in circular hole positioned at electrode to middle extruding,
Realize the effect of fixed oxidation zirconium electrode.
Zirconium oxide electrode assembling is completed according to aforesaid way, in order to good completion, the present embodiment will aoxidize zirconium electrode
It is used cooperatively with oxonium ion on-line system in a kind of high-temperature molten salt, so as to which the utility model is further described
A kind of high-temperature molten salt oxonium ion on-line system includes：Aoxidize zirconium electrode, reference electrode, thermocouple, moisture recorder,
Electrochemical workstation, computer, fixing device；Oxidation zirconium electrode, reference electrode, thermocouple are fixed by lower electrode fixing piece
On the securing means；Zirconium electrode, reference electrode and electrochemical workstation is aoxidized to connect；Thermocouple is connected with moisture recorder；Electricity
Chem workstation, moisture recorder are connected with computer.
Embodiment 1
Operating procedure is as noted above, and simply structural parameters are different, and design parameter is：Tubular zirconium-oxide size for 6mm,
Wall thickness 1mm, long 150mm；Interior reference fused salt is 0.75mol/kg silver chlorates and lithium chloride, the potassium chloride of 0.03mol/kg lithium carbonates
Eutectic salt powder, quality 1g；High-temperature molten salt temperature is 500 DEG C.
Zirconium oxide oxygen electrode is inserted into 500 DEG C of lithium chloride, in potassium chloride fused salt, hydrogen chloride gas is passed through into fused salt,
The electromotive force of oxidation zirconium electrode raises rapidly, and reaches again stable in 400s；Treat to stop being passed through chlorine after a period of stabilisation
Change hydrogen, and start to be passed through argon gas, the hydrogen chloride in fused salt is removed by bubbling, the current potential of electrode starts to reduce；Treat electricity
After kinetic potential is stablized, lithium carbonate is added into fused salt, electromotive force reduces rapidly, and reaches stable in 400S.Into fused salt repeatedly
Aforesaid operations 3 times, it is identical to survey potential change every time, record zirconium oxide oxygen determination ion electrode be passed through repeatedly hydrogen chloride gas with
The electrode potential of argon gas process, it is 5ppm to measure oxygen ion concentration in high-temperature molten salt.So as to understand oxonium ion detecting system to molten
Oxygen ion concentration response in salt is sensitive, and the measurement reappearance under the same conditions to oxonium ion is preferable.
Embodiment 2
Operate same as Example 1, its difference is：Tubular zirconium-oxide size is 6mm, wall thickness 2mm, long 150mm；It is interior
Reference fused salt is lithium chloride, the potassium chloride eutectic salt powder of 0.4mol/kg silver chlorates and 0.03mol/kg lithium carbonates, and quality is
0.5g；High-temperature molten salt temperature is 575 DEG C.
Zirconium electrode will be aoxidized and be inserted into 575 DEG C of sodium chloride, in calcium chloride fused salt.Lithium carbonate, electromotive force are added into fused salt
Reducing rapidly, after stablizing, hydrogen chloride gas is passed through into fused salt, the electromotive force of zirconium oxide oxygen electrode raises rapidly, and
Reach stable in 400s, it is 6ppm to measure oxygen ion concentration in high-temperature molten salt.
Embodiment 3
Operation embodiment 1 is identical, its difference is：Tubular zirconium-oxide size is 6mm, wall thickness 1mm, long 150mm；Internal reference
Lithium chloride, potassium chloride eutectic salt powder than fused salt for 0.8mol/kg silver chlorates and 0.1mol/kg lithium carbonates, quality are
0.75g；High-temperature molten salt temperature is 575 DEG C.
Zirconium electrode will be aoxidized and be inserted into 400 DEG C of lithium chloride, in potassium chloride fused salt.Lithium carbonate, electromotive force are added into fused salt
Reducing rapidly, after stablizing, hydrogen chloride gas is passed through into fused salt, the electromotive force of zirconium oxide oxygen electrode raises rapidly, and
Reach stable in 400s, it is 4ppm to measure oxygen ion concentration in high-temperature molten salt.
Claims (7)
1. a kind of be used for the oxidation zirconium electrode that oxonium ion detects in high-temperature molten salt, it is characterised in that the oxidation zirconium electrode master
Including：Upper electrode fixing piece (3), electrode fix ball (4), lower electrode fixing piece (5), electrode body (10)；
The upper electrode fixing piece (3) is screw shaped structure, and upper electrode fixing piece (3), which is equipped with, runs through circular hole, and lower face is set
There is spherical groove；The lower electrode fixing piece (5) is negative and positive screw shaped structure, and lower electrode fixing piece (5) is equipped with through circle
Hole, top female threaded hole bottom are equipped with spherical groove；The upper electrode fixing piece (3) is fixed with lower electrode fixing piece (5)
Connection；The electrode fixes ball (4) and is equipped with the circular hole for running through the centre of sphere, and Circularhole diameter is identical with alundum tube (6) outside diameter, and electrode is fixed
Ball (4) is located at the inside of spherical groove of upper electrode fixing piece (3) and lower electrode fixing piece (5)；
The electrode body (10) mainly includes：Silver electrode lead wires (1), upper sealing-plug (2), alundum tube (6), lower sealing-plug (7),
Tubular zirconium-oxide (8), interior reference fused salt (9)；The upper sealing-plug (2), which is equipped with, runs through circular hole, upper sealing-plug (2) and alundum tube (6)
Upper end is fixedly connected, and upper sealing-plug (2) seals with alundum tube (6) fixed connection place；The alundum tube (6) is consolidated through upper electrode
Determine part (3), electrode fixes ball (4), lower electrode fixing piece (5)；The lower sealing-plug (7), which is equipped with, runs through circular hole, lower sealing-plug
(7) it is fixedly connected with tubular zirconium-oxide (8) upper end, lower sealing-plug (7) seals with tubular zirconium-oxide (8) junction；The tubular zirconium-oxide
(8) end closure under, tubular zirconium-oxide (8) upper end are fixedly connected with alundum tube (6) lower end, and tubular zirconium-oxide (8) is connected with alundum tube (6)
Place's sealing；It is internal that the interior reference fused salt (9) is located at tubular zirconium-oxide (8)；The silver electrode lead wires (1) through upper sealing-plug (2),
Interior reference fused salt (9) is submerged to tubular zirconium-oxide (8) bottom, upper end in alundum tube (6), lower sealing-plug (7), tubular zirconium-oxide (8), lower end
Sealing-plug (2) is outside in stretching.
A kind of 2. oxidation zirconium electrode for being used for oxonium ion detection in high-temperature molten salt according to claim 1, it is characterised in that
Tubular zirconium-oxide (8) thickness is 1-2mm.
A kind of 3. oxidation zirconium electrode for being used for oxonium ion detection in high-temperature molten salt according to claim 1, it is characterised in that
The upper sealing-plug (2) is to be wound upper sealing-plug (2) using polytetrafluoro raw material band with alundum tube (6) fixed connection place, is used in combination
Refractory ceramics glue is applied to polytetrafluoro raw material band face seal.
A kind of 4. oxidation zirconium electrode for being used for oxonium ion detection in high-temperature molten salt according to claim 1, it is characterised in that
The lower sealing-plug (7) is sealed with the sealing of tubular zirconium-oxide (8) fixed connection place using refractory ceramics glue.
A kind of 5. oxidation zirconium electrode for being used for oxonium ion detection in high-temperature molten salt according to claim 1, it is characterised in that
The tubular zirconium-oxide (8) is fixedly connected as be bonded with alundum tube (6).
A kind of 6. oxidation zirconium electrode for being used for oxonium ion detection in high-temperature molten salt according to claim 1, it is characterised in that
The upper sealing-plug (2), lower sealing-plug (7) material are heat-resisting material.
A kind of 7. oxidation zirconium electrode for being used for oxonium ion detection in high-temperature molten salt according to claim 1, it is characterised in that
It is elastic material that the electrode, which fixes ball (4) material,.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201720922184.6U CN207232070U (en) | 2017-07-27 | 2017-07-27 | It is a kind of to be used for the oxidation zirconium electrode that oxonium ion detects in high-temperature molten salt |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201720922184.6U CN207232070U (en) | 2017-07-27 | 2017-07-27 | It is a kind of to be used for the oxidation zirconium electrode that oxonium ion detects in high-temperature molten salt |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107515238A (en) * | 2017-07-27 | 2017-12-26 | 中国原子能科学研究院 | It is a kind of to be used for the oxidation zirconium electrode that oxonium ion detects in high-temperature molten salt |
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2017
- 2017-07-27 CN CN201720922184.6U patent/CN207232070U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107515238A (en) * | 2017-07-27 | 2017-12-26 | 中国原子能科学研究院 | It is a kind of to be used for the oxidation zirconium electrode that oxonium ion detects in high-temperature molten salt |
| CN107515238B (en) * | 2017-07-27 | 2019-09-13 | 中国原子能科学研究院 | A kind of oxidation zirconium electrode detected for oxonium ion in high-temperature molten salt |
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