CN109521069A - Multi-functional electrochemistry subtest case - Google Patents

Multi-functional electrochemistry subtest case Download PDF

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Publication number
CN109521069A
CN109521069A CN201811299515.0A CN201811299515A CN109521069A CN 109521069 A CN109521069 A CN 109521069A CN 201811299515 A CN201811299515 A CN 201811299515A CN 109521069 A CN109521069 A CN 109521069A
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light source
test
electrode
time relay
pin
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CN109521069B (en
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李靖
刘天宝
唐辉
王鹏
宋明
堵锡华
田林
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Xuzhou University of Technology
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/28Electrolytic cell components

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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Abstract

The invention discloses multi-functional electrochemistry subtest casees, including testing tank shell, transparent window and four buttons are distributed with counterclockwise on four angles of test box housing top surface, level meter, memory block and light source region, centre is equipped with ITO electro-conductive glass groove area, test box housing side is equipped with electrode connection mouth and power interface, it is test cabinet among light source region and transparent window, it tests in tank shell and is equipped with light source and the time relay with corresponding position above and below light source region, there is electro bath-lid fixed frame in test cabinet, electro bath-lid fixed frame inner bottom surface is fixed with electrolytic cell fixing clamp, have out electrode jack on electrolytic cell is opened flat electro bath-lid, infrared lamp is equipped in ITO electro-conductive glass groove area, the time relay, infrared lamp, light source and small fan circuit connection.The present invention, which can facilitate, prepares conductor photocatalysis working electrode, and preparation process is simple, at low cost, and accurate to the electrochemical property test of semiconductor catalyst working electrode, test result error is small, test process is easy to operate.

Description

Multi-functional electrochemistry subtest case
Technical field
The invention belongs to electrochemical property test tool box manufacturing technology fields, are related to a kind of multi-functional electrochemistry auxiliary Test box.
Background technique
With the application of electrochemistry transient state technology, electrochemistry, optics and sufacing are interpenetrated, quickly the complicated electricity of analysis Chemical reaction, obtains electrode surface information, the electrochemistry branch developed using this principle and electrochemical test method are Through becoming the highly important characterization in laboratory and new high-tech enterprise and detection means;Electrochemical workstation can be used for test material Impedance, Schottky, photoelectricity current test, cyclic voltammetric performance etc., electric property, reaction invertibity, concentration for judgement material Detection etc..
Using semiconductor material as photochemical catalyst, natural light can carry out Photocatalitic Technique of Semiconductor at normal temperature as excitation, Save the energy;Special catalytic effect is realized by the interface interaction of contaminant molecule, makes oxygen and the hydrone excitation of surrounding At the free anion of great oxidizing force, to efficiently use sunlight as light source alleviating energy crisis, reach degradation environment The purpose of middle harmful organic substances or high oxidation number metal ion will not result in waste of resources, form additional pollution, and operate letter Single, catalyst can be used repeatedly, and be a kind of environmentally protective efficient process technology;The performance of semiconductor catalyst is partly to lead One of the key factor that body photocatalysis technology promotes and applies, the electrification of semiconductor catalyst is accurately tested using electrochemical workstation Learning performance also becomes the main means of testing of research.
Currently, needing to make using ITO electro-conductive glass and partly lead in the electrochemical property test to semiconductor catalysis material Body catalyst working electrode needs more preliminary preparation, cumbersome and time-consuming;During electrochemical property test, lack Fixed ancillary equipment causes electrode connection to be not fixed less, and the electrolytic cell for testing electrolyte is easy the disadvantages of toppling over, while photoelectricity External light source is needed when current test, is protected from light, switch lamp calendar scheduling operation repeatedly, error is easily occurred, is influenced the accurate of test result Degree and accuracy.
The present invention provides a kind of multi-functional supplementary instrument of assisted electrochemical work test, obtains more accurately test knot Fruit, to adapt to basic electro-chemical test.
Summary of the invention
In order to achieve the above object, the present invention provides a kind of multi-functional electrochemistry subtest case, solves the prior art Middle semiconductor catalyst working electrode preparation process is cumbersome, time-consuming, and electrode connection, electrolytic cell connect not during performance test The problems such as fixed, the timely switching light sources of energy, human error is small, and measurement result is accurate.
The technical scheme adopted by the invention is that multi-functional electrochemistry subtest case includes test tank shell, test box In a rectangular parallelepiped shape, transparent window and four buttons are distributed with counterclockwise, level meter, deposit shell for four angles of test box housing top surface Storage area and light source region, wherein transparent window and four buttons are located on the same angle, and four buttons are respectively: light source switch, red Outer lamp switch, locking press button and reset button are distributed with electrode on the side where the side that transparent window is closed on level meter and connect Line mouth and power interface, electrode connection mouth is close to transparent window, and power interface is close to level meter, the centre of test box housing top surface Test cabinet among light source region and transparent window equipped with ITO electro-conductive glass groove area, test tank shell in it is right above and below light source region Should place be provided with light source and the time relay, electro bath-lid fixed frame, electro bath-lid fixed frame inner bottom surface are fixed in test cabinet It is fixed with electrolytic cell fixing clamp, is sealed on electrolytic cell using being opened flat electro bath-lid, be opened flat on electro bath-lid and be provided with electrode jack, electricity Polar curve passes through electrode connection mouth and is connected on the electrode in electrode jack, the corresponding subtest case of ITO electro-conductive glass groove area Infrared lamp is equipped in shell;The time relay, infrared lamp, light source, small fan pass through circuit connection.
Further, after locking press button is in parallel with reset button one end with the pin of the time relayConnection, it is self-locking to press The other end of button and the pin of the time relayConnection, the other end of reset button and the pin of the time relayConnection; Infrared lamp one end is connected to the pin of the time relay after connecting with infrared lamp switchOn, other end turn-on time relay Pin, the pin of the time relay, pinPower interface is accessed after in parallel with small fan both ends, when light source one end is accessed Between relay pin, the other end is connected with light source switch accesses power interface.
The beneficial effects of the present invention are: the process that conductor photocatalysis working electrode is prepared in the present invention is simple, it is at low cost; When being tested for the property to semiconductor catalyst working electrode, the position of connection and electrolytic cell between electrode is fixed, and will not be gone out The problems such as now connecting deviation or electrolytic cell inclination, so that test result is accurate;The present invention connects the time relay with light source, Can accurate, timely switching light sources, reduce manually-operated error, so that the performance test results are accurate.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with It obtains other drawings based on these drawings.
Fig. 1 is the shell structure figure of multi-functional electrochemistry subtest case.
Fig. 2 is the internal structure chart of multi-functional electrochemistry subtest case.
Fig. 3 is the internal circuit diagram of multi-functional electrochemistry subtest case.
Fig. 4 is embodiment testing result schematic diagram.
In figure, 1. electrode connection mouths, 2. power interfaces, 3. level meters, 4.ITO electro-conductive glass groove area, 5. memory blocks, 6. Light source region, 7. test cabinets, 8. transparent windows, 9. infrared lamps, 10. light sources, 11. time relays, 12. electrode jacks, 13. electrolysis Slot, 14. electrolytic cell fixing clamps, 15. electro bath-lid fixed frames, 16. small fans, 17. are opened flat electro bath-lid, 18. light source switch, 19. infrared lamp switch, 20. locking press buttons, 21. reset button.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other Embodiment shall fall within the protection scope of the present invention.
Multi-functional electrochemistry subtest case includes test tank shell, tests the surface texture of tank shell as shown in Figure 1, being in Transparent window 8 and four buttons, level meter 3, memory block is distributed in four angles of rectangular-shape, test box housing top surface counterclockwise 5 and light source region 6, wherein transparent window 8 and four buttons are located on the same angle, by transparent window 8 it can be observed that the time Time data on 11 display screen of relay facilitate the progress and control of electrochemical property test, and four buttons are respectively: light source Switch 18, infrared lamp switch 19, locking press button 20 and reset button 21, light source switch 18 can control unlatching and the pass of light source 10 It closes, infrared lamp switch 19 controls the open and close of infrared lamp 9, and reset button 21 makes the time relay 11 restart to count When, the electrochemical property test time can repeatedly, be accurately controlled, locking press button 20 promotes light environment or infrared lamp 9 to maintain to open The state for opening or closing reduces influence of the hand maloperation to test;Level meter 3 can be observed to judge whether test auxiliary tank In level, the position of test auxiliary tank can be adjusted in time, guarantee the accuracy of test, what transparent window 8 and level meter 3 closed on Electrode connection mouth 1 and power interface 2 are distributed on side where side, electrode connection mouth 1 is close to transparent window 8, for connecting Electrode, power interface 2 is close to level meter 3, and memory block 5 is for storing required tool and component, such as working electrode, reference electricity Pole, resistance meter, surface plate and cloth of real silk etc.;The centre of housing top surface is equipped with ITO electro-conductive glass groove area 4, for placing It is test cabinet 7 among ITO electro-conductive glass, light source region 6 and transparent window 8, test cabinet 7 passes through closed in space, closed shading, performance The light source of test is only provided by the light source 10 in multi-functional electrochemistry auxiliary, can timely switching light sources 10, and intensity of illumination Stablize, reduces test error;Subtest tank shell internal structure is as shown in Fig. 2, in subtest tank shell and light source region 6 Upper and lower corresponding position is provided with light source 10 and the time relay 11, and electro bath-lid fixed frame 15 is fixed in test cabinet 7 and is used to support Be opened flat electro bath-lid 17,15 inner bottom surface of electro bath-lid fixed frame is fixed with electrolytic cell fixing clamp 14, can with stationary electrolysis slot 13 with It keeps stablizing, using the sealing of electro bath-lid 17 is opened flat on electrolytic cell 13, is opened flat on electro bath-lid 17 and is provided with electrode jack 12, respectively It is working electrode jack, reference electrode reference electrode plug and auxiliary electrode jack, electrode wires pass through electrode connection mouth 1 and are connected to electrode jack On electrode in 12, infrared lamp 9 is equipped in the corresponding subtest tank shell of ITO electro-conductive glass groove area 4;The time relay 11, infrared lamp 9, light source 10, small fan 16 pass through circuit connection.
Circuit connection inside subtest tank shell is as shown in figure 3, locking press button 20 is in parallel with 21 one end of reset button Afterwards with the pin of the time relay 11Connection, the other end of locking press button 20 and the pin of the time relay 11Connection, it is multiple The other end of position button 21 and the pin of the time relay 11Connection;9 one end of infrared lamp connects after connecting with infrared lamp switch 19 Connect the pin in the time relay 11On, the pin of other end turn-on time relay 11, the pin of the time relay 11 , pinPower interface 2, the pin of 10 one end turn-on time relay 11 of light source are accessed after in parallel with 16 both ends of small fan, The other end is connected with light source switch 18 accesses power interface 2.
When preparing semiconductor catalyst working electrode, using high-power ultrasonic instrument, solid suspension is prepared, ITO conduction Glass is placed in the groove of ITO electro-conductive glass groove area 4, is dripped the suitable suspension of people, is opened infrared lamp switch 19, utilize light source 9 illumination of infrared lamp in area 6 is dried, until suspension forms thin film in ITO conductive glass surface, the ITO for having film Electro-conductive glass is placed in 100 DEG C of heat preservation 4h in baking oven, and fixed film layer obtains semiconductor catalyst working electrode;Semiconductor is catalyzed When the electrochemistry of agent working electrode can be carried out detection, Al is first used2O3Powder polishing, cleaning semiconductor catalyst working electrode, Auxiliary electrode and reference electrode;Then power supply is opened, electrochemical workstation is made to preheat 15min, opens the hatch door of test cabinet 7, Electrolyte is added in electrolytic cell 13, using 14 stationary electrolysis slot 13 of electrolytic cell fixing clamp, seals electricity using electro bath-lid 17 is opened flat Solve slot 13, semiconductor catalyst working electrode, auxiliary electrode and reference electrode are placed in electrode jack 12, connect each electrode with Electrode connection mouth 1 tests the performance of semiconductor catalyst working electrode.
When test, semiconductor catalyst working electrode is placed among auxiliary electrode and reference electrode, when photoelectricity current test Need to be arranged light source 10, testing impedance, Schottky test, cyclic voltammetry, electro-deposition test and charge-discharge test are not necessarily to Light source 10 is set;Multi-functional electrochemistry subtest case can satisfy the different of different electrochemical property tests and require, easy to be easy Operation, testing result accuracy is high, provides new thinking to application of the electrochemical workstation in terms of material characterization.
By the preparation of semiconductor catalyst working electrode and performance test together as one, semiconductor catalyst work electricity is simplified The preparation process of pole cooperates self-locking presses using the time relay 11 to light source and the accurate control of time progress in test process Button 20 reduces manually-operated error, also electrolytic cell 13 is fixed using electrolytic cell fixing clamp 14, so that test result Accuracy is higher, and electrochemical property test process is simple to operation.
Embodiment 1
The step of using present invention preparation and detection semiconductor catalyst working electrode, is as follows:
Step 1: preparing semiconductor catalyst working electrode
By appropriate semiconductor catalyst material SnO2/ PANI is placed in 10mL dehydrated alcohol, ultrasonic in 300W power Ultrasound Instrument Disperse 30min and conductor photocatalysis material suspension is made, ITO electro-conductive glass is placed in the groove of ITO electro-conductive glass groove area 4 It is interior, by the suspended drop-coated of the conductor photocatalysis material of preparation on ITO electro-conductive glass;
Infrared lamp switch 19 is pressed, the semiconductor catalyst suspension on ITO electro-conductive glass is dried using infrared lamp 9, forms one Layer film, is then placed in 100 DEG C of heat preservation 4h in baking oven for ITO electro-conductive glass, and fixed film layer obtains semiconductor catalyst work electricity Pole;
Step 2: using Al2O3Powder polishing, cleaning electrode, auxiliary electrode and reference electrode;
Step 3: connection electrode
The hatch door for opening test cabinet 7, is added appropriate 0.1mol/L Na in electrolytic cell 132SO4, use electrolytic cell fixing clamp 14 Stationary electrolysis slot 13 is opened flat 17 sealed electrolytic cell 13 of electro bath-lid, auxiliary electrode and reference electrode is accessed electrode jack 12, partly Conductor catalyst working electrode is located among auxiliary electrode and reference electrode, closes 7 hatch door of test cabinet, utilizes conductor grip connection three Electrode and electrochemical workstation;
Step 4: setting 10 opening time of light source as 40s using the time relay 11, shut-in time 20s is recycled;To the light of sample Current capability is tested, and reset button 21 can be pressed after the completion of test and repeats above-mentioned test process;
Step 5: after test, arrangement, cleaning electrode, instrument;
Testing result as shown in figure 4, with semiconductor catalyst quantity of material in suspension increase, the conductor photocatalysis of preparation The photocurrent curve amplitude of variation of agent working electrode first increases to be subtracted afterwards, when the load capacity of PANI is 3%, composite material SnO2/PANI With highest photo-current intensity, light induced electron separative efficiency is high in composite material, and the photoelectric current test curve of drafting understands, light It is sliding, it can accurately reflect the photoelectric current performance of semiconductor light-catalyst working electrode.
Each embodiment in this specification is all made of relevant mode and describes, same and similar portion between each embodiment Dividing may refer to each other, and each embodiment focuses on the differences from other embodiments.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the scope of the present invention.It is all Any modification, equivalent replacement, improvement and so within the spirit and principles in the present invention, are all contained in protection scope of the present invention It is interior.

Claims (2)

1. multi-functional electrochemistry subtest case, which is characterized in that including test tank shell, test tank shell in a rectangular parallelepiped shape, Four angles of test box housing top surface be distributed with counterclockwise transparent window (8) and four buttons, level meter (3), memory block (5) and Light source region (6), wherein transparent window (8) and four buttons are located on the same angle, and four buttons are respectively: light source switch (18), infrared lamp switch (19), locking press button (20) and reset button (21), the side that transparent window (8) is closed on level meter (3) Electrode connection mouth (1) and power interface (2) are distributed on the side at place, electrode connection mouth (1) is close to transparent window (8), electricity Source interface (2) is equipped with ITO electro-conductive glass groove area (4), light source region (6) close to level meter (3), the centre of test box housing top surface Intermediate with transparent window (8) is test cabinet (7), and corresponding position is provided with light source (10) up and down with light source region (6) in test tank shell With the time relay (11), test cabinet (7) is interior to be fixed with electro bath-lid fixed frame (15), electro bath-lid fixed frame (15) inner bottom surface It is fixed with electrolytic cell fixing clamp (14), using electro bath-lid (17) sealing is opened flat on electrolytic cell (13), is opened flat electro bath-lid (17) On be provided with electrode jack (12), electrode wires pass through electrode connection mouth (1) be connected on the electrode in electrode jack (12), ITO is led Infrared lamp (9) are equipped in the corresponding subtest tank shell of electric glass groove area (4);The time relay (11), infrared lamp (9), Circuit connection between light source (10) and small fan (16).
2. multi-functional electrochemistry subtest case according to claim 1, which is characterized in that the locking press button (20) with Pin after reset button (21) one end is in parallel with the time relay (11)Connection, the other end of locking press button (20) and time The pin of relay (11)Connection, the other end of reset button (21) and the pin of the time relay (11)Connection;Infrared lamp (9) one end is connected to the pin of the time relay (11) after connecting with infrared lamp switch (19)On, other end turn-on time after The pin of electric appliance (11), the pin of the time relay (11), pinPower supply is accessed after in parallel with small fan (16) both ends to connect Mouth (2), the pin of light source (10) one end turn-on time relay (11), the other end is connected with light source switch (18) accesses power supply Interface (2).
CN201811299515.0A 2018-11-02 2018-11-02 Multifunctional electrochemical auxiliary test box Active CN109521069B (en)

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CN111458623A (en) * 2020-04-17 2020-07-28 全球能源互联网研究院有限公司 Semiconductor chip's testing arrangement

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CN111458623B (en) * 2020-04-17 2022-03-11 全球能源互联网研究院有限公司 Semiconductor chip's testing arrangement

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