CN106645358A - Inert atmosphere-based electrochemical testing device and method of high-temperature molten salt - Google Patents
Inert atmosphere-based electrochemical testing device and method of high-temperature molten salt Download PDFInfo
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- CN106645358A CN106645358A CN201611180683.9A CN201611180683A CN106645358A CN 106645358 A CN106645358 A CN 106645358A CN 201611180683 A CN201611180683 A CN 201611180683A CN 106645358 A CN106645358 A CN 106645358A
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- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
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Abstract
The invention relates to the technical field of electrochemical property testing in a high-temperature inert atmosphere, and discloses an inert atmosphere-based electrochemical testing device and method of a high-temperature molten salt. The device comprises an inert atmosphere circulation system, a high-temperature molten salt testing system and an electrochemical work station, wherein the inert atmosphere circulation system comprises a sealed box body and an inert atmosphere circulation device which is arranged outside the sealed box body and connected with the sealed box body; the high-temperature molten salt testing system comprises a heating device arranged in the sealed box body and a testing device arranged in the heating device; and the electrochemical work station is electrically connected with the testing device, and the heating device is used for providing the testing device with a temperature for electrochemical testing. According to the inert atmosphere-based electrochemical testing device and method, direct electrochemical testing of the battery after being assembled in the inert atmosphere circulation system can be achieved, the inert atmosphere-based electrochemical testing device and method are suitable for electrochemical property testing of a thermal battery and a high-temperature molten salt electrolyte, interference of other factors is reduced, the reliability of the test result is improved and the testing step is simplified.
Description
Technical field
The present invention relates to electrochemical property test technical field in high temperature inert atmosphere, and in particular to one kind is based on indifferent gas
The high-temperature molten salt electrochemical testing device of atmosphere and method.
Background technology
The inert atmosphere circulatory system is mainly used in the assembling of battery in electrochemical field, and it can be various scientific researches and life
Produce and anhydrous, anaerobic experimental situation is provided, while security protection can also be provided to researcher.Heating system is in electrochemistry
Field can provide specific hot environment for the electro-chemical test of high temperature fused salt electrolysis plastidome.
Thermal cell etc. needs to carry out chemical property survey in hot environment using the battery of high temperature fused salt electrolysis plastidome
Examination, but, the technique such as activation, heating and sealing system needed for test is more more complicated.
The assembling of current battery is more to be carried out in glove box, and the electrochemical property test of high-temperature molten salt system battery is main
Carry out in tube furnace, this sealing requirements to battery is higher, and assembling is separated so that step is more with test process, is operated
Complexity, is unfavorable for the raising of laboratory scientific research efficiency and the simplification of experimentation.
The content of the invention
In order to overcome above-mentioned deficiency present in prior art, the invention provides a kind of high temperature melting based on inert atmosphere
Salt electrochemical testing device and method, can realize high-temperature molten salt and related system battery high-temperature electrochemistry in an inert atmosphere
Test, and it is simple to operate.
According to the first aspect of the invention, the invention provides a kind of high-temperature molten salt electro-chemical test based on inert atmosphere
Device, the device includes：
The inert atmosphere circulatory system, it includes seal case and is arranged at outer and coupled lazy of the seal case
Property atmosphere circulator；
High-temperature molten salt test system, it includes the heater being built in the seal case and is built in described adding
Test device in thermal；
And electrochemical workstation, it is with the test device is by copper conductor and is embedded in the seal box body sidewall
Multifunctional socket is electrically connected；
Wherein, the heater carries out the temperature of electro-chemical test for providing the test device.
According to the second aspect of the invention, the invention provides a kind of using the high-temperature molten salt electrochemical testing device
Method of testing, the method for testing is comprised the following steps：
Step 1, determinand is placed in test device, is connected as test mode；
Step 2, starts heater, is heated to test temperature；
Step 3, is tested, and by electrochemical workstation gathered data.
The high-temperature molten salt electrochemical testing device of the present invention has following technique effect：
1st, can realize that high-temperature molten salt and related system battery are carried out in an inert atmosphere plus Thermal test：Inert atmosphere is circulated
System provides the inert atmosphere needed for the test of high temperature fused salt electrolysis plastidome, while high-temperature molten salt test system provides high-temperature molten salt
High temperature needed for melting work, realizes the high temperature fused salt electrolysis matter and related system battery operational group in the inert atmosphere circulatory system
Electro-chemical test after dress, it is adaptable to experimental study.
2nd, operating procedure is simplified while operability is ensured：For thermal cell, assembling and test can be same
Carry out in device, eliminate battery and the transfer of required device and the process for vacuumizing repeatedly；For electrode or high-temperature molten salt electricity
Xie Zhi, can connect peripheral hardware and directly test chemical property, letter by electrochemical workstation using three-electrode system by device
Change testing process.
Description of the drawings
Fig. 1：The structural representation of high-temperature molten salt electrochemical testing device of the present invention.
Fig. 2：The structural representation of high-temperature molten salt test system of the present invention.
Fig. 3：The electrical block diagram of high-temperature molten salt test system of the present invention.
Description of reference numerals：
1st, electrochemical workstation；2nd, copper conductor；3rd, electric cabinet is heated；4th, Multifunctional socket；5th, heater；6th, test
Device；7th, seal case；8th, inert atmosphere EGR；9th, apparatus for controlling of lifting；10th, heat-insulation layer housing；11st, heating module；
12nd, thermocouple；13rd, insulated thermal insulating layer；14th, insulated heat top cover；15th, insulation board；16th, insulated heat block；17th, pallet connection
Bar；18th, can adjust electrode；19th, pallet；20th, collets.
Specific embodiment
To make the present invention easier to understand, below in conjunction with embodiment and accompanying drawing the present invention is described in detail, these
Embodiment only plays illustrative effect, is not limited to the present invention.
According to the first aspect of the invention, the invention provides a kind of high-temperature molten salt electro-chemical test based on inert atmosphere
Device, as shown in figure 1, the device includes：
The inert atmosphere circulatory system, it includes seal case 7 and is arranged at outside the seal case 7 and coupled
Inert atmosphere EGR 8；
High-temperature molten salt test system, it includes the heater 5 being built in the seal case 7 and is built in described
Test device 6 in heater 5；
And electrochemical workstation 1, it is with the test device 6 is by copper conductor 2 and is embedded in the side of the seal case 7
The Multifunctional socket 4 of wall is electrically connected；
Wherein, the heater 5 carries out the temperature of electro-chemical test for providing the test device 6.
According to the present invention, the height being made up of the inert atmosphere circulatory system, high-temperature molten salt test system and electrochemical workstation 1
Temperature molten salt electrochemical testing device, realizes the On-line Control of inert atmosphere high temperature fused salt test.
According to the present invention, the device further preferably includes：Heating electric cabinet 3, outside it the side wall of the seal case 7 is hung on, and is used
In the control heater 5.
In one embodiment of the present invention, the seal case 7 has handle hole and visual panel, and the handle hole is by resistance to
Soda acid PPS material seals, easily can be operated by the handle hole to test device；Post the visual panel inner side
Anti-corrosion protective film.
As shown in Fig. 2 in the present invention, the heater 5 is preferably included：Top end opening and madial wall be sticked have insulation every
The heat-insulation layer housing 10 of thermosphere 13, the insulated heat top cover 14 being located at the opening, heating module 11 and thermocouple 12；
The heating module 11 is sticked in the insulated thermal insulating layer 13；
The thermocouple 12 is sequentially passed through heat-insulation layer housing 10, insulated thermal insulating layer 13 by the lateral wall of heat-insulation layer housing 10 and is added
Thermal modules 11 to heater 5, for detecting test temperature；
The insulated heat top cover 14 is made up of insulated heat block 16 and insulation board 15.
Wherein, the above-mentioned setting of the heating module 11, can make temperature in the heater 5 uniform, and add thermal effect
Rate is high.
One end of the thermocouple 12 is placed in temperature sensor in heater 5, and is located at the other end outside heater
It is connected with heating electric cabinet 3, records and displays temperature numerical value.
The insulated heat block 16 matches with the top end opening, can realize the sealing of heater 5, the insulation
Plate 15 is fixed on the lateral wall of the insulated heat block 16, and its cross section more than the cross section of the insulated heat block 16.
According to the present invention, by the heat-insulation layer housing 10, heating module 11, insulated thermal insulating layer 13 and insulated heat top cover
14 setting causes controllable temperature of the heater 5 in 80 minutes to may range from RT～500 DEG C.
In the present invention, the test device 6 includes：
Apparatus for controlling of lifting 9, for controlling the direction switch of insulated heat top cover 14；
Pallet connecting rod 17, its top is connected with the insulation board 15；
Adjustable electrode 18, its top is arranged on the insulation board 15 and can be relative to moving down on the insulation board 15
Dynamic, Multifunctional socket 4 is electrically connected with electrochemical workstation 1 described in the Jing of top；
Pallet 19, is fixed on the bottom of pallet connecting rod 17, for placing determinand；
Collets 20, it is arranged at the junction of pallet 19 and pallet connecting rod 17, with pallet 19, insulated heat top cover
14th, insulation board 15 is used to ensure the lateral isolation of the test device together；The pallet connecting rod 17 and adjustable electrode 18
The longitudinal direction for being ensured is conductive.
Wherein, the apparatus for controlling of lifting 9 can be come by being connected with the insulation board 15 of the insulated heat top cover 14
Realize the elevating control to insulated heat top cover 14.
The top of the pallet connecting rod 17 can be connected with the insulation board 15 by screw thread, and it is relative to insulation board
17 can move up and down.
A preferred embodiment of the invention, the bottom of pallet connecting rod 17 is provided with screw thread, the pallet
19 are connected with the pallet connecting rod 17 by screw nut, and the collets 20 are arranged at the through hole of pallet 19 and pallet 19
With nut contact position.
A preferred embodiment of the invention, the apparatus for controlling of lifting 9 includes foot controller and cylinder, leads to
Cross the direction switch of pneumatic control insulated heat top cover 14.
According to the present invention, the pallet connecting rod 17 includes two copper bars, and its bottom is connected to the pallet 19
Two relative edges；
The adjustable electrode 18 is made up of two copper electrode rods；
The pallet 19 can be ceramic tray.
As shown in figure 3, the circuit structure of high-temperature molten salt test system of the present invention includes heater circuit module and test circuit
Module.
Specifically, heater circuit module includes the control circuit of heating module (heater) and thermocouple；Test circuit mould
Block includes elevating control circuit and test control circuit.
According to the second aspect of the invention, the invention provides a kind of using the high-temperature molten salt electrochemical testing device
Method of testing, the method for testing is comprised the following steps：
Step 1, determinand is placed in test device 6, is connected as test mode；
Step 2, starts heater 5, is heated to test temperature；
Step 3, is tested, and by the gathered data of electrochemical workstation 1.
Specifically, following operation is carried out by the handle hole of seal case 7：Determinand is placed in into the pallet of test device 5
On 19, adjustment controllable electrode 18 so as to which the bottom of two copper electrode rods is connected respectively with the both positive and negative polarity of determinand；By lifting
Control device 9 closes the insulated heat top cover 14 of heater 5, while also just determinand has been placed in heater 5, by adding
The control of hot electric cabinet 3 starts heater 5, is heated to required test temperature；Tested, and by electrochemical workstation 1
Gathered data.
Present invention explanation will be described in detail by embodiment below.
Embodiment 1
The present embodiment is used to illustrate the high-temperature molten salt electrochemical testing device based on inert atmosphere and method of the present invention.
As shown in Figure 1 and Figure 2, the high-temperature molten salt electrochemical testing device includes：The inert atmosphere circulatory system, high temperature melting
Salt test system, and electrochemical workstation 1.
The inert atmosphere circulatory system is by seal case 7 and is arranged at the outer and coupled inertia of the seal case 7
Atmosphere circulator 8 is constituted, and the seal case 7 posts anti-corrosion protection with the handle hole by PPS material seals and inner side
The visual panel of film, can realize the operation of seal case build-in test device.
High-temperature molten salt test system includes the heater 5 being built in the seal case 7 and is built in described adding
Test device 6 in thermal 5, the heater 5 is controlled by the heating electric cabinet 3 for being hung on the side wall of the seal case 7 outward
Heating, is that the test device 6 provides the temperature for carrying out electro-chemical test.
Wherein, the heater 5 includes：Top end opening and madial wall is sticked and has the heat-insulation layer housing of insulated thermal insulating layer 13
10th, insulated heat top cover 14 at the opening, heating module 11 and thermocouple 12 are located at；The heating module 11 is sticked
In the insulated thermal insulating layer 13；The thermocouple sequentially passes through heat-insulation layer housing 10, insulation by the lateral wall of heat-insulation layer housing 10
Thermal insulation layer 13 and heating module 11 to heater 5, for detecting test temperature；The insulated heat top cover 14 by insulation every
Hot block 16 is constituted with the insulation board 15 for being fixed on the lateral wall of insulated heat block 16, and the cross section of the insulation board 15 is more than institute
State the cross section of insulated heat block 16；The heater 5 can be heated to 500 DEG C in 80 minutes.
The test device 6 includes：Apparatus for controlling of lifting 9, it includes foot controller and cylinder, cylinder and the insulation
The insulation board 15 of heat-insulated top cover 14 is connected, by the direction switch of pneumatic control insulated heat top cover 14；Pallet connecting rod 17,
It includes two copper bars, and the top of two copper bars is connected with the insulation board 15 by screw thread, can be relative on insulation board 17
Lower movement, the bottom of two copper bars is provided with screw thread, by screw nut be connected to two of the pallet 19 it is relative
Edge；Adjustable electrode 18, is made up of two copper electrode rods, the top of two electrode bars be arranged on the insulation board 15 and
Can move up and down relative to the insulation board 15, top Jing wires and be embedded in the multifunctional access of the side wall of the seal case 7
Line plate 4 is electrically connected with electrochemical workstation 1；Pallet 19, it is ceramic tray, is fixed on the bottom of pallet connecting rod 17, is used for
Place determinand；Collets 20, are arranged at the through hole of pallet 19 and pallet 19 and nut contact position, with pallet 19, insulated heat
Top cover 14, insulation board 15 are used to ensure the lateral isolation of the test device together.
Using above-mentioned high-temperature molten salt electrochemical testing device, the electrochemistry of self-control positive pole is tested by three-electrode system
Can, with low melting point LiF-LiBr-KBr as electrolyte, using CHI-660E type electrochemical workstations (electrochemical workstation 1), if
Put resistant to elevated temperatures to electrode and reference electrode, method of testing is comprised the following steps：
Step 1：Positive pole (working electrode) will be made by oneself, LiF-LiBr-KBr eutectics will be loaded with to electrode and reference electrode insertion
In the ceramic vessel of point electrolyte, it is ensured that can not have electrode after electrolyte melting, ceramic vessel is placed on pallet 19, and adjust
Whole controllable electrode 18 so as in the bottom of a copper electrode rod be connected with the positive pole of tested systems, another copper electrode rod
Bottom be connected with the negative pole of tested systems；
Step 2：By the insulated heat top cover 14 of foot controller closed pneumatic heater 5, start heater 5 to
Test temperature；
Step 3：Tested, and by CHI-660E type electrochemical workstation gathered datas.
It is described above embodiments of the invention, described above is exemplary, and non-exclusive, and also not
It is limited to disclosed embodiment.In the case of the scope and spirit without departing from illustrated embodiment, for the art
Many modifications and changes will be apparent from for those of ordinary skill.
Claims (10)
1. a kind of high-temperature molten salt electrochemical testing device based on inert atmosphere, it is characterised in that：The device includes：
The inert atmosphere circulatory system, it includes seal case (7) and to be arranged at the seal case (7) outward and coupled
Inert atmosphere EGR (8)；
High-temperature molten salt test system, it includes the heater (5) being built in the seal case (7) and is built in described
Test device (6) in heater (5)；
And electrochemical workstation (1), it is with the test device (6) is by copper conductor (2) and is embedded in the seal case
(7) Multifunctional socket (4) of side wall is electrically connected；
Wherein, the heater (5) carries out the temperature of electro-chemical test for providing the test device (6).
2. high-temperature molten salt electrochemical testing device according to claim 1, wherein, the device includes：Heating electric cabinet
(3), the seal case (7) side wall is hung on outside it, for controlling the heater (5).
3. high-temperature molten salt electrochemical testing device according to claim 1, wherein,
The seal case (7) with handle hole and visual panel, the handle hole by acid and alkali-resistance PPS material seals, it is described can
Anti-corrosion protective film is posted depending on panel inner side.
4. high-temperature molten salt electrochemical testing device according to claim 1, wherein,
The heater (5) includes：Top end opening and madial wall be sticked have the heat-insulation layer housing (10) of insulated thermal insulating layer (13),
It is located at insulated heat top cover (14) at the opening, heating module (11) and thermocouple (12)；
The heating module (11) is sticked in the insulated thermal insulating layer (13)；
The thermocouple (12) sequentially passes through heat-insulation layer housing (10), insulated thermal insulating layer (13) by heat-insulation layer housing (10) lateral wall
In heating module (11) to heater (5), for detecting test temperature；
The insulated heat top cover (14) is made up of insulated heat block (16) and insulation board (15).
5. the high-temperature molten salt electrochemical testing device according to claim 1 or 4, wherein,
Controllable temperature scope of the heater (5) in 80 minutes is RT～500 DEG C.
6. high-temperature molten salt electrochemical testing device according to claim 4, wherein, the test device (6) includes：
Apparatus for controlling of lifting (9), for controlling the direction switch of insulated heat top cover (14)；
Pallet connecting rod (17), its top is connected with the insulation board (15)；
Adjustable electrode (18), its top is arranged on the insulation board (15) and can be relative to the insulation board (15) up and down
Mobile, Multifunctional socket (4) is electrically connected with electrochemical workstation (1) described in the Jing of top；
Pallet (19), is fixed on the bottom of pallet connecting rod (17), for placing determinand；
Collets (20), it is arranged at the junction of pallet (19) and pallet connecting rod (17), with pallet (19), insulated heat top
Lid (14), insulation board (15) are used to ensure the lateral isolation of the test device together.
7. high-temperature molten salt electrochemical testing device according to claim 6, wherein,
Pallet connecting rod (17) bottom is provided with screw thread, and the pallet (19) is with the pallet connecting rod (17) by screw thread
Nut is connected, and the collets (20) are arranged at pallet (19) through hole and pallet (19) and nut contact position.
8. high-temperature molten salt electrochemical testing device according to claim 6, wherein,
The apparatus for controlling of lifting (9) includes foot controller and cylinder, by the liter of pneumatic control insulated heat top cover (14)
Drop switch.
9. high-temperature molten salt electrochemical testing device according to claim 6, wherein,
Including two copper bars, its bottom is connected to two relative sides of the pallet (19) to the pallet connecting rod (17)
At edge；
The adjustable electrode (18) is made up of two copper electrode rods；
The pallet (19) is ceramic tray.
10. in a kind of employing claim 1-9 arbitrary described high-temperature molten salt electrochemical testing device method of testing, the test
Method is comprised the following steps：
Step 1, determinand is placed in test device (6), is connected as test mode；
Step 2, starts heater (5), is heated to test temperature；
Step 3, is tested, and by electrochemical workstation (1) gathered data.
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| CN201611180683.9A CN106645358B (en) | 2016-12-19 | 2016-12-19 | A kind of high-temperature molten salt electrochemical testing device and method based on inert atmosphere |
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| CN201611180683.9A CN106645358B (en) | 2016-12-19 | 2016-12-19 | A kind of high-temperature molten salt electrochemical testing device and method based on inert atmosphere |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109298338A (en) * | 2018-09-19 | 2019-02-01 | 沈阳君威新能科技有限公司 | A kind of single cell of thermo battery test device and single battery test method |
| CN110102235A (en) * | 2019-05-07 | 2019-08-09 | 北京缔森科技发展有限公司 | A kind of high-temperature and high pressure electrochemistry reactor |
| CN110212209A (en) * | 2019-06-03 | 2019-09-06 | 中国工程物理研究院电子工程研究所 | A kind of constant temperature and pressure formula thermal cell electric performance test system and its test method |
| CN110304632A (en) * | 2018-03-20 | 2019-10-08 | 中国科学院金属研究所 | Sheet MXene material and preparation method thereof and energy storage material |
| CN112903950A (en) * | 2021-01-11 | 2021-06-04 | 北京科技大学 | Device suitable for high-temperature in-situ nondestructive testing of liquid metal battery |
| CN115494339A (en) * | 2022-11-15 | 2022-12-20 | 陕西华秦科技实业股份有限公司 | High-precision atmosphere controllable temperature-changing electrical testing system |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110304632A (en) * | 2018-03-20 | 2019-10-08 | 中国科学院金属研究所 | Sheet MXene material and preparation method thereof and energy storage material |
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| CN110102235A (en) * | 2019-05-07 | 2019-08-09 | 北京缔森科技发展有限公司 | A kind of high-temperature and high pressure electrochemistry reactor |
| CN110212209A (en) * | 2019-06-03 | 2019-09-06 | 中国工程物理研究院电子工程研究所 | A kind of constant temperature and pressure formula thermal cell electric performance test system and its test method |
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| CN112903950A (en) * | 2021-01-11 | 2021-06-04 | 北京科技大学 | Device suitable for high-temperature in-situ nondestructive testing of liquid metal battery |
| CN115494339A (en) * | 2022-11-15 | 2022-12-20 | 陕西华秦科技实业股份有限公司 | High-precision atmosphere controllable temperature-changing electrical testing system |
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