CN202512173U - Apparatus for measuring molten salt electrical conductivity by utilizing four-electrode method - Google Patents

Apparatus for measuring molten salt electrical conductivity by utilizing four-electrode method Download PDF

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Publication number
CN202512173U
CN202512173U CN2012200058992U CN201220005899U CN202512173U CN 202512173 U CN202512173 U CN 202512173U CN 2012200058992 U CN2012200058992 U CN 2012200058992U CN 201220005899 U CN201220005899 U CN 201220005899U CN 202512173 U CN202512173 U CN 202512173U
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China
Prior art keywords
electrode
fused salt
boiler tube
seal plug
potential electrode
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Expired - Fee Related
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CN2012200058992U
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Chinese (zh)
Inventor
周国治
陈志远
李丽芬
虞自由
刘俊昊
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University of Science and Technology Beijing USTB
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University of Science and Technology Beijing USTB
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Abstract

The utility model relates to an apparatus for measuring molten salt electrical conductivity by utilizing a four-electrode method. The apparatus comprises a heating sealing device including a molten salt temperature measurement thermocouple (1), an air outlet (2), a furnace upper sealing plug (3), a heating furnace main body (4), a furnace lower sealing plug (5), an air inlet (6), a heat insulation fireproofing material plate group (8) and a fireproof material lower holder (11) as well as a measurement electrode displacement clamp (7), a measurement electrode (9) and a crucible (10). And the measurement electrode has four leads that are connect to corresponding terminals of a digital electric bridge, wherein the corresponding terminals are voltage terminals and current terminals. According to the utility model, an improved square array is used to arrange four electrodes (15, 16, 17, and 18) and the digital electric bridge is also used for combination, so that the electrical conductivity of the molten salt is determined; besides, the length of the constant temperature zone needed by the apparatus is short, so that accurate control of the molten salt temperature can be realized; there is no need to calculate the density and the volume of the molten salt, thereby reducing an error caused by the calculation; and the depth of electrode insertion can be controlled conveniently and the electrode design is suitable for a small tubular furnace.

Description

A kind of four electrode method is measured the device of fused salt conductivity
Technical field
The utility model belongs to the experimental facilities field, relates to a kind of device with four electrode method measurement fused salt conductivity, and a kind of measuring head that is easy to realize a kind of easy and simple to handle that utilizes bridge measurement fused salt electricity to lead that meets particularly is provided.
Background technology
The conductivity of high-temperature molten salt is difficult with respect to the measurement of normal temperature liquid, and influence factor is more with restriction.This always is the conductance cell of the own assembling design of experimenter do not have the appearance of commercialization conductance cell with regard to the conductivity measuring apparatus that has caused high-temperature molten salt.Reason is the following aspects:
(1) high temperature has proposed stricter requirement for the conductance cell material, and normal temperature measures down with material or electrode structural designs because problem such as the material deformation that causes with fused salt interphase interaction, temperature variation and can not adapt to measurement requirement;
(2) the conductivity variations scope of fused salt is bigger, and what have far exceeds commercialization conductivity meter measurement range;
(3) owing to obtain high-temperature service flat-temperature zone size restriction is provided, the means that make some can improve measuring accuracy can not reach, and measure the length between the utmost point such as increasing conductance cell;
(4) firing equipment is for electromagnetic interference (EMI) of conductivity measurement or the like.
Therefore, a kind of conductivity measurement equipment simple, that adapt to the laboratory hot environment is necessary.
The utility model content
The purpose of the utility model is to invent the device that a kind of four electrode method is measured the fused salt conductivity, can under most laboratory conditions, realize the surveying work to the fused salt conductivity easily through the logotype of digital electric bridge and this device.
The device that a kind of four electrode method is measured the fused salt conductivity comprises measuring head, sealing tubular heater; Wherein measuring head comprises potential electrode displacement anchor clamps, crucible and by potential electrode, temperature thermocouple, fireclay insulating refractory plate group, gas outlet and boiler tube top seal plug; Fireclay insulating refractory plate group is fixed on boiler tube top seal plug bottom; Potential electrode moves up and down through potential electrode displacement anchor clamps, after potential electrode is passed boiler tube top seal plug and fireclay insulating refractory plate group, is positioned at the crucible top; Temperature thermocouple is fixed on boiler tube top seal plug and the fireclay insulating refractory plate group, and the temperature thermocouple lower end is submerged in the fused salt of crucible; Open in the boiler tube top seal beyond the Great Wall the gas outlet;
The sealing tubular heater comprises holder under heating furnace main body, boiler tube lower seal plug, air intake opening and the fire resistive material; Hot furnace main body heats crucible, and on crucible placed and holds in the palm under the fire resistive material, boiler tube lower seal plug and boiler tube top seal plug laid respectively at the bottom and the top of heating furnace main body; Air intake opening passes boiler tube lower seal plug and fire resistive material holds in the palm down in the entering heating furnace main body.
Potential electrode has four external lead wires, receives the digital electric bridge corresponding end, is respectively voltage end and current terminal; The potential electrode outside is surrounded by fixed bar, and fixed bar is connected to the insulation fixed block, and four external lead wires of described potential electrode are connected respectively to voltage end electrode and current terminal electrode; Voltage end electrode and current terminal electrode place fused salt.
A kind of four electrode method is measured the device of fused salt conductivity, and be made up of following part: measuring head comprises potential electrode, temperature thermocouple, fireclay insulating refractory plate group, gas outlet and boiler tube top seal plug; Potential electrode displacement anchor clamps; Crucible and heating furnace main body and other auxiliary equipment comprise air intake opening and boiler tube lower seal plug.
The sealing tubular heater that measuring head of forming by potential electrode displacement anchor clamps, crucible and by potential electrode, temperature thermocouple, fireclay insulating refractory plate group, gas outlet and boiler tube top seal plug and heating furnace main body, boiler tube lower seal plug, air intake opening are formed.Through rubber seal, potential electrode can move up and down between potential electrode and the boiler tube top seal plug.Temperature thermocouple be fixed on the boiler tube top seal beyond the Great Wall and its lower end be submerged in the fused salt.Fireclay insulating refractory plate group is fixed on boiler tube top seal plug bottom, utilizes the corundum disk to process, and wears with alumina tube and heat-resisting alloy line to turn to.Potential electrode has four lead-in wires, receives the digital electric bridge corresponding end, is respectively voltage end and current terminal; Its fixed bar is four hole alundum tubes, is connected to the insulation fixed block, and lead-in wire wherein is connected respectively to voltage end electrode and current terminal electrode.Potential electrode is clamped on the potential electrode displacement anchor clamps, moves up and down the electrode measurement electrode, can turned crosses the scale of potential electrode displacement anchor clamps and observes the degree of depth that electrode inserts fused salt.Be lined with heat-resisting alloy pipe or graphite-pipe in the burner hearth of heating furnace main body, be used to shield the electromagnetic interference (EMI) of external heating element, especially avoid the influence of the induced potential that heater coil produces of Fe-Cr-Al wire heating material high temperature furnace measuring.There is screen layer the lead-in wire outside that potential electrode is connected to digital electric bridge, and the fixed bar skin is coated with one deck screen layer.Two voltage end electrodes and current terminal electrode are 2 * 2 arranged in arrays.External lead wire connect is the ac digital electric bridge, and parameters such as its frequency of operation, ac voltage are relevant with molten salt nature.
The inner chamber of body of heater is an electro-magnetic screen layer with high temperature heat-resisting or graphite internal lining pipe, to prevent external electromagnetic interference.Inner chamber feeds inert atmosphere.The electrode of measuring head partly is clamped on the potential electrode displacement anchor clamps that indicate scale.Contain fused salt in the crucible, and voltage end, current terminal electrode and temperature thermocouple are put into fused salt.Four external shielded leads of electrode link to each other with digital electric bridge.
Adopt said apparatus, Sheng is put into burner hearth after going into an amount of testing sample in crucible, assembles device feature, at first feeds high purity inert gas, is 573K in heat temperature raising to the crucible slowly, and insulation a period of time continued slowly is warming up to temperature required.The potential electrode lead-in wire is connected to digital electric bridge, and makes electrode drop to the fused salt liquid level through mobile measuring electrode displacement anchor clamps.When four electrode contact fused salts, the digital electric bridge measured resistance value can descend rapidly, writes down scale shown in the potential electrode displacement anchor clamps this moment.The electrode certain distance that descends afterwards can be measured the resistance value of fused salt.Through measuring the cell constant of conductometric vessel that normal temperature records with the KCl standard solution down, finally calculate the conductivity value of fused salt.
The utlity model has following principal feature:
1, this device provides a cover complete easy fused salt conductance measurement scheme.
2, the current terminal electrode of this device and voltage end electrode are 2 * 2 arranged in arrays, the characteristics that to adapt to general accurate temperature controlling firing equipment be the tubular type burner hearth.Help the measurement operation in less furnace cavity and shorter zone of constant temperature.
3, the fireclay insulating refractory plate group that corundum disk is processed is adopted on this device top, prevents that the top furnace temperature is too high, and the general lightweight refracrory that adopts in top scrapes the pollution testing sample that drops during effectively anti-upper member loading and unloading.
4, this device can accurately be located four electrodes and inserted the fused salt degree of depth, and under the suitable operation situation, the conductivity of surveying receives to measure crucible shape error, testing sample at every turn, and to put into the influence of quantitative changeization, electrode pair little." crucible-central electrode method " need be known fused salt volume when measuring temperature; Be easy to generate the measurement data error when measuring fused salt density etc.; Need not during this measurement device accurately to control the fused salt volume, reduced requirement, thereby reduced the error of measurement result fused salt addition degree of accuracy.
5, this device has adopted electromagnetic shielding measure, the influence of electromagnetic interference (EMI) to installing of effectively having avoided high-temperature service often to have.
Below, in conjunction with accompanying drawing the utility model is done further to describe in detail.
Description of drawings
Fig. 1 implements illustration for the utility model.
The holder (11) down of fused salt temperature thermocouple (1), gas outlet (2), boiler tube top seal plug (3), heating furnace main body (4), boiler tube lower seal plug (5), air intake opening (6), potential electrode displacement anchor clamps (7), fireclay insulating refractory plate group (8), potential electrode (9), crucible (10), fire resistive material.
Fig. 2 is potential electrode (a 9) detail drawing.
External lead wire (12), four hole alundum tube fixed bars (13), insulation fixed block (14), voltage end electrode (15), (16), current terminal (17), (18).
Fig. 3 is the measuring head detail drawing.
Embodiment
Measurement mechanism shown in Figure 1 asks 11 to form down by fused salt temperature thermocouple 1, gas outlet 2, boiler tube top seal plug 3, heating furnace main body 4, boiler tube lower seal plug 5, air intake opening 6, potential electrode displacement anchor clamps 7, fireclay insulating refractory plate group 8, potential electrode 9, crucible 10, fire resistive material.Wherein potential electrode 9, temperature thermocouple 1, fireclay insulating refractory plate group 8, gas outlet 2 and boiler tube top seal plug 3 are formed measuring head.
Testing sample is contained in the crucible 10, and the temperature thermocouple 1 of measuring head is indicated the measurement temperature of fused salt in the burner hearth in fused salt.Under inert atmosphere,, utilize potential electrode displacement anchor clamps 7 that four electrodes 15~18 are put into the fixing degree of depth of fused salt through specific heating step to temperature to be measured.Set the electric bridge parameter, after insulation a period of time, the resistance value that can read this sample through digital electric bridge.Through the resistance value of measurement standard KCl solution under assigned temperature, calculate cell constant of conductometric vessel, can calculate the conductivity value of measuring fused salt.

Claims (7)

1. a four electrode method is measured the device of fused salt conductivity, it is characterized in that: device comprises measuring head, seals tubular heater; Wherein measuring head comprises potential electrode displacement anchor clamps (7), crucible (10) and by potential electrode (9), temperature thermocouple (1), fireclay insulating refractory plate group (8), gas outlet (2) and boiler tube top seal plug (3); Fireclay insulating refractory plate group (8) is fixed on boiler tube top seal plug (3) bottom; Potential electrode (9) moves up and down through potential electrode displacement anchor clamps (7), after potential electrode (9) is passed boiler tube top seal plug (3) and fireclay insulating refractory plate group (8), is positioned at crucible (10) top; Temperature thermocouple (1) is fixed on boiler tube top seal plug (3) and the fireclay insulating refractory plate group (8), and temperature thermocouple (1) lower end is submerged in the fused salt of crucible (10); Open on boiler tube top seal plug (3) gas outlet (2);
The sealing tubular heater comprises holder (11) under heating furnace main body (4), boiler tube lower seal plug (5), air intake opening (6) and the fire resistive material; Hot furnace main body (4) heats crucible (10), and crucible (4) places and holds in the palm under the fire resistive material on (11), and boiler tube lower seal plug (5) and boiler tube top seal plug (3) lay respectively at the bottom and the top of heating furnace main body (4); Air intake opening (6) passes boiler tube lower seal plug (5) and fire resistive material asks (11) to get in the heating furnace main body (4) down;
Potential electrode (9) has four external lead wires, receives the digital electric bridge corresponding end, is respectively voltage end and current terminal; Potential electrode (9) outside is surrounded by fixed bar (13); Fixed bar (13) is connected to insulation fixed block (14), and four external lead wires of described potential electrode (9) are connected respectively to voltage end electrode (15), (16) and current terminal electrode (17), (18); Voltage end electrode (15), (16) and current terminal electrode (17), (18) place fused salt.
2. four electrode method as claimed in claim 1 is measured the device of fused salt conductivity, and it is characterized in that: described fixed bar (13) is four hole alundum tubes.
3. four electrode method as claimed in claim 2 is measured the device of fused salt conductivity, it is characterized in that: on the described potential electrode displacement anchor clamps (7) scale is arranged, measuring voltage termination electrode (15,16) and current terminal electrode (17,18) insert the degree of depth of fused salt.
4. four electrode method as claimed in claim 1 is measured the device of fused salt conductivity, it is characterized in that: be lined with heat-resisting alloy pipe or graphite-pipe in the burner hearth of described heating furnace main body (4).
5. four electrode method as claimed in claim 1 is measured the device of fused salt conductivity, and it is characterized in that: there is screen layer the lead-in wire outside that described potential electrode (9) is connected to digital electric bridge, and fixed bar (13) skin is coated with one deck screen layer.
6. four electrode method as claimed in claim 3 is measured the device of fused salt conductivity, and it is characterized in that: described voltage end electrode (15), (16) and current terminal electrode (17), (18) are 2 * 2 arranged in arrays.
7. four electrode method as claimed in claim 2 is measured the device of fused salt conductivity, and it is characterized in that: described external lead wire (12) connect is the ac digital electric bridge.
CN2012200058992U 2012-01-06 2012-01-06 Apparatus for measuring molten salt electrical conductivity by utilizing four-electrode method Expired - Fee Related CN202512173U (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103076500A (en) * 2012-12-31 2013-05-01 中国电子科技集团公司第四十九研究所 Conductivity sensor in cofiring structure and manufacturing method thereof
CN104749445A (en) * 2013-12-25 2015-07-01 湖南创元铝业有限公司 Molten salt and molten slag conductivity detection equipment and detection method
CN105334394A (en) * 2015-10-23 2016-02-17 国联汽车动力电池研究院有限责任公司 Online monitoring system for conductivity of high-temperature fused salt
CN105606901A (en) * 2015-12-24 2016-05-25 河海大学 MEMS seawater conductivity sensor with filtering device
WO2016095769A1 (en) * 2014-12-19 2016-06-23 中国科学院大连化学物理研究所 Ionic conductivity test device, and test method using same
CN105759123A (en) * 2014-12-19 2016-07-13 中国科学院大连化学物理研究所 Ion conductivity test apparatus and test method employing same
CN106824833A (en) * 2017-02-28 2017-06-13 中国振华集团云科电子有限公司 Resistor screening technology method
CN107478905A (en) * 2017-08-03 2017-12-15 天津中环电炉股份有限公司 A kind of conductivity measurement
CN113237827A (en) * 2021-06-25 2021-08-10 清华大学 Electrochemical test system for molten salt corrosion experiment

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103076500A (en) * 2012-12-31 2013-05-01 中国电子科技集团公司第四十九研究所 Conductivity sensor in cofiring structure and manufacturing method thereof
CN104749445A (en) * 2013-12-25 2015-07-01 湖南创元铝业有限公司 Molten salt and molten slag conductivity detection equipment and detection method
CN105759123B (en) * 2014-12-19 2017-11-14 中国科学院大连化学物理研究所 A kind of ionic conductivity test device and use its method of testing
US10054561B2 (en) 2014-12-19 2018-08-21 Dalian Institute Of Chemical Physics, Chinese Academy Of Sciences Device for detection of ionic conductivity and its applied measurement
WO2016095769A1 (en) * 2014-12-19 2016-06-23 中国科学院大连化学物理研究所 Ionic conductivity test device, and test method using same
CN105759123A (en) * 2014-12-19 2016-07-13 中国科学院大连化学物理研究所 Ion conductivity test apparatus and test method employing same
CN105334394A (en) * 2015-10-23 2016-02-17 国联汽车动力电池研究院有限责任公司 Online monitoring system for conductivity of high-temperature fused salt
CN105606901B (en) * 2015-12-24 2018-02-23 河海大学 A kind of MEMS sea water conductivity sensors with filter
CN105606901A (en) * 2015-12-24 2016-05-25 河海大学 MEMS seawater conductivity sensor with filtering device
CN106824833A (en) * 2017-02-28 2017-06-13 中国振华集团云科电子有限公司 Resistor screening technology method
CN106824833B (en) * 2017-02-28 2023-07-18 中国振华集团云科电子有限公司 Resistor screening process
CN107478905A (en) * 2017-08-03 2017-12-15 天津中环电炉股份有限公司 A kind of conductivity measurement
CN113237827A (en) * 2021-06-25 2021-08-10 清华大学 Electrochemical test system for molten salt corrosion experiment
CN113237827B (en) * 2021-06-25 2022-08-23 清华大学 Electrochemical test system for molten salt corrosion experiment

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CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20121031

Termination date: 20160106