CN114354726B - Nano material single crystal stress field coupling electrochemical testing device and method - Google Patents
Nano material single crystal stress field coupling electrochemical testing device and method Download PDFInfo
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Abstract
The invention provides a device and a method for testing the coupling electrochemistry of a single crystal stress field of a nano material, which solve the problem that the existing testing method can not realize the electrochemistry testing under the quantitative strain of a two-dimensional material. The testing device comprises an optical microscope, an electrochemical workstation, an electrochemical in-situ testing unit and a stress applying unit; the electrochemical in-situ test unit comprises a test main body and a test base which are arranged from top to bottom in a matched manner; the stress applying unit comprises a probe, a probe clamping assembly and a three-dimensional moving platform; the probe is vertically arranged on the three-dimensional moving platform through the probe clamping assembly, and under the regulation of the three-dimensional moving platform, the probe applies mechanical stress to the flexible substrate on the testing base, so that the nano material to be tested is strained; the optical microscope measures the strain quantity generated by the nano material to be measured through the small hole; and measuring the electrochemical performance of the nano material to be measured under the condition of measuring the strain capacity by the electrochemical workstation.
Description
Technical Field
The invention belongs to the technical field of micro device testing, and particularly relates to a nano material single crystal stress field coupling electrochemical testing device and method.
Background
Since the mechanical exfoliation method was reported in 2004 to obtain graphene from highly oriented cracked graphite and demonstrated its excellent electrical properties, two-dimensional materials represented by graphene have been rapidly developed. Because various two-dimensional materials have completely different energy band structures and electrical, optical, mechanical, magnetic and thermal properties, the two-dimensional materials have been widely studied by scientists.
In addition to graphene, other two-dimensional materials include single-element silylene, germylene, borolene, black phosphorus, and the like, transition metal chalcogenides such as MoS 2 、WS 2 WSe, WTe, etc., main group metal chalcogenides such as GaS, inSe, snS, etc., and other two-dimensional materials such as h-BN, crI3, niPS3, etc. These two-dimensional materials exhibit highly tunable bandgaps by controlling the number of layers, heterostructures, strain engineering, chemical dopingThe adjustment of the band gap can be realized by methods such as impurity, alloying and external electric field.
Strain engineering is a desirable approach to introduce novel and excellent physical properties by tuning the crystal lattice and electronic structure of ultra-thin two-dimensional materials. In particular, strain can effectively alter the interaction between the configuration of atomic bonds (i.e., bond length, bond angle, and bond strength) and electron orbitals, resulting in new phenomena and properties of ultra-thin two-dimensional materials, such as thermal, electrical, optical, and magnetic properties. Thus, the ability to change the intrinsic properties of ultra-thin two-dimensional materials through strain engineering creates a tremendous opportunity for their application in the fields of sensing, electronics, and opto-electronics, among others. However, the current method of applying mechanical stress to two-dimensional materials is to apply uniaxial strain to a sample by a bending device, and then to test the change of physical properties, such as: the device is large and complex to operate, and on the other hand, in-situ observation is difficult to realize in the liquid phase through the device. Therefore, an apparatus and a method for applying stress to a two-dimensional material to test its electrochemistry are still lacking.
Disclosure of Invention
The invention aims to solve the problem that the existing testing method can not realize in-situ electrochemical measurement when quantitative strain occurs to a nano material in an electrolyte environment, and provides a nano material single crystal stress field coupling electrochemical testing device and method.
In order to achieve the purpose, the technical solution provided by the invention is as follows:
the nanometer material single crystal stress field coupling electrochemical testing device is characterized in that: the device comprises an optical microscope, an electrochemical workstation, an electrochemical in-situ test unit and a stress applying unit;
the electrochemical in-situ test unit comprises a test main body and a test base which are arranged from top to bottom in a matched manner;
a first through hole is vertically arranged in the test main body, an annular groove which surrounds the first through hole and is not completely closed is arranged on the end face of the upper end of the test main body, the wall surface of the inner side of the annular groove is lower than the wall surface of the outer side of the annular groove, and a lead leading-out groove with a downward opening is axially arranged on the test main body where the ring is not completely closed; the upper end surface of the first through hole is hermetically provided with a transparent observation window with a small hole in the center;
the test main body is also provided with a first mounting hole and a second mounting hole which are communicated with the annular groove and used for respectively mounting a counter electrode and a reference electrode required by electrochemical test;
the test base is used for bearing and extending the flexible substrate and the nano material to be tested transferred onto the flexible substrate into the first through hole to be tightly pressed against the lower end face of the small hole of the observation window, so that the flexible substrate is matched with the wall of the small hole to form a cavity capable of containing electrolyte; when the electrolyte is filled, the electrolyte fills the cavity, overflows from the small hole of the observation window, flows into the annular groove, and is contacted with a counter electrode and a reference electrode required by electrochemical test through the first mounting hole and the second mounting hole, and at the moment, the nano material to be tested is also positioned in the observation area and is contacted with the electrolyte;
the test base is provided with a second through hole along the axial direction;
the stress applying unit comprises a probe, a probe clamping assembly and a three-dimensional moving platform; the probe is vertically arranged on the three-dimensional moving platform through the probe clamping assembly, extends into the second through hole under the regulation of the three-dimensional moving platform and applies mechanical stress to the flexible substrate arranged on the testing base, so that the nano material to be tested is strained;
the optical microscope measures the strain quantity generated by the nano material to be measured through the small hole; the optical microscope can read the strain amount by adopting a general high-power optical microscope, and meanwhile, the electrochemical test process can be accompanied with some special optical phenomena and structural changes, so the in-situ observation can also be carried out by adopting the optical microscope;
and the electrochemical workstation measures the electrochemical performance of the nano material to be measured under the strain.
Further, the test base comprises a base body and a support body;
the base main body comprises a bottom plate and a connecting section coaxially arranged on the bottom plate, and a third mounting hole for mounting a support body is formed in the base main body along the central shaft; the linkage segment is connected with test main part lower extreme structure looks adaptation, through adaptation between them, makes test base and test main part be connected, for example: the connecting section is provided with an external thread, the first through hole is internally provided with an internal thread, and the test base can be assembled into the test main body in a screwing mode, so that the flexible substrate is tightly propped against the lower end face of the small hole of the observation window; of course, other connection modes can be adopted;
the vertical section of the support body is T-shaped and comprises a supporting seat and a connecting rod which are coaxially arranged; the diameter of the supporting seat is larger than the aperture of the third mounting hole and smaller than the aperture of the first through hole, and the supporting seat is used for placing a sample; the connecting rod is inserted into the third mounting hole.
Further, in order to facilitate fine movement, the three-dimensional moving platform comprises a magnetic gauge stand, and a first mechanical cushion block, a second mechanical cushion block and a third mechanical cushion block which are sequentially arranged on the magnetic gauge stand from bottom to top and move towards an X axis, a Y axis and a Z axis respectively;
the three mechanical cushion blocks are adjusted to move through the adjusting screw assembly (the adjusting screw assembly adopts the existing structure), and the movement of the three mechanical cushion blocks is not completely independent, for example, when the movement is performed in the X-axis direction, the mechanical cushion blocks moving towards the Y axis and the Z axis can also move in the X-axis direction, and when the movement is performed in the Y-axis direction, the same principle is performed, but when the movement is performed in the Z axis, the movement is performed by the mechanical cushion blocks moving towards the Z axis.
Further, the probe is arranged on a third mechanical cushion block moving to the Z axis through a probe clamping assembly;
a fourth mounting hole is vertically formed in the third mechanical pad; a threaded hole vertical to the fourth mounting hole is formed in the wall of the fourth mounting hole;
the probe clamping assembly comprises an L-shaped supporting rod, a spring and a limiting block;
the L-shaped supporting rod comprises a vertical rod and a cross rod; the vertical rod is arranged in the fourth mounting hole through the matching of the fastening bolt and the threaded hole; the cross rod is provided with a mounting block and a third through hole; spring and stopper all overlap and establish on the horizontal pole, and the one end and the installation piece of spring are connected, and the other end is connected with the stopper, and the stopper can exert the effort to the probe of inserting the third through-hole under the effect of spring, fixes the position of probe in the third through-hole.
Usually, after the position of the XY surface is adjusted, the third mechanical cushion block is driven, so that the probe moves along the Z-axis direction, the flexible substrate is jacked up to drive the nano material to be measured to generate strain, the strain of the nano material to be measured can be measured through an optical microscope, and the expected strain can be obtained by continuously adjusting the Z axis and observing.
Further, the inner walls of the first mounting hole and the second mounting hole are provided with internal threads and sealing rings, so that electrolyte is prevented from seeping out.
Further, the observation window is made of glass materials, such as: organic glass, quartz glass, silicate glass.
Further, the nano material to be detected is a single crystal, such as: the composite material is prepared from molybdenum disulfide, graphene, boron nitride and other single-crystal nanosheets.
Further, the optical microscope is replaced by a Raman device, the phase structure of the sample and the layer thickness of the crystal can be tested, and when stress is applied, the Raman characteristic peak of the material can be found to be regularly shifted.
Furthermore, the height of the lead leading-out groove is higher than the height of the bottom surface of the electrolytic bath, so that the lead is easier to contact with the area part of the electrode obtained by vapor deposition and connected with the nano material to be tested, and if the height of the lead leading-out groove of the working electrode is lower than the height of the bottom surface of the electrolytic bath, the lead is clamped between threads and is twisted off, and the lead is difficult to assemble.
Furthermore, the top of the test main body can be packaged with a top cover exposed out of the observation area, so that the electrolyte can be thinned to facilitate observation and Raman detection of in-situ electrochemical reaction, and volatilization of the electrolyte can be prevented.
Meanwhile, the invention also provides a testing method utilizing the nano material single crystal stress field coupling electrochemical testing device, which is characterized by comprising the following steps:
1) Respectively installing a counter electrode and a reference electrode in a first installation hole and a second installation hole of the testing device;
2) Fixing the flexible substrate transferred with the nano material to be tested on a test base of the test device, and enabling the nano material to be tested to face an observation window at the upper end of the test main body;
3) Fixing one end of a lead on an observation window of a testing device, aligning an area of an electrode obtained by vapor deposition and connected with a nano material to be tested with the lead, and enabling the lead to be in contact with the electrode of the nano material to be tested through extrusion of a testing base;
4) Connecting the other ends of the counter electrode, the reference electrode and the lead connected with the electrode of the nano material to be detected with the counter electrode, the reference electrode and the working electrode interface of the electrochemical workstation respectively;
5) Placing the testing device under an optical microscope and focusing the optical microscope on the surface of the nano material to be tested;
6) Injecting electrolyte into the testing device, and enabling the electrolyte to be in contact with the counter electrode, the reference electrode and the nano material area to be tested exposed from the small hole of the observation window;
7) Adjusting the three-dimensional moving platform, and aligning the probe to the flexible substrate through the second through hole of the test base;
8) Performing electrochemical scanning tests, such as performing Cyclic Voltammetry (CV);
9) After the hydrogen evolution of the nano material to be detected is stable, adjusting the position of a probe of the three-dimensional mobile platform to enable the probe to jack the flexible substrate upwards to deform, so that the nano material to be detected generates strain;
10 Optical microscopy is used to measure the amount of strain and the electrochemical performance at that amount of strain is measured by an electrochemical workstation. Therefore, different strains are generated on the sample by applying different stresses to the flexible substrate, so as to measure the electrochemical performance under different strains.
The counter electrode and the reference electrode can be a carbon rod electrode and a silver/silver chloride electrode respectively.
Further, in step 8), 0.4V to-0.9V scans were performed at a scan rate of 10 mV/s.
The invention has the beneficial effects that:
1. the invention can not only observe in situ, but also apply stress to the micro-nano device, quantitatively control and measure the material strain, and in addition, can perform physical property test and electrochemical performance test in situ after applying stress to the material.
2. According to the invention, by adjusting the position of the probe and applying stress to the flexible substrate with the sample through the second through hole on the test base for fixing the sample, the strain of the flexible substrate drives the sample to be tested to generate quantitative strain.
3. The invention carries out electrochemical test on a sample subjected to quantitative strain by virtue of an in-situ electrochemical test device of a nano device, and explores the influence of stress strain on the performance of a two-dimensional nano material.
4. According to the invention, the up-and-down movement of the probe is controlled by utilizing the built mechanical platform, and the deformation of the flexible substrate is driven, so that the micron-sized two-dimensional material attached to the flexible substrate is subjected to corresponding strain, the physical property change and the electrochemical property of a sample are tested, and the blank of electrochemical test of a micro-nano device under quantitative strain is filled.
5. The whole electrochemical in-situ test unit can be quickly obtained by a 3D printing technology without any metal material, is easy to realize and has low assembly technology content.
Drawings
FIG. 1 is a physical diagram of graphene transferred on a PDMS flexible substrate with different strains by applying stress to the graphene using the testing apparatus of the present invention; a: the graphene sample is not strained; b: the graphene sample was 8.86% strained; c: the graphene sample was 29.1% strained; d: the graphene sample was 40.6% strained;
FIG. 2 is a schematic view of a test apparatus according to example 2 of the present invention;
FIG. 3 is a first schematic view of a testing apparatus according to embodiment 3 of the present invention;
FIG. 4 is a second schematic view of a testing apparatus according to embodiment 3 of the present invention;
FIG. 5 is a third schematic view of a test apparatus according to embodiment 3 of the present invention;
FIG. 6 is a schematic structural view of a probe clamping assembly;
FIG. 7 is a schematic view of the mating of the test body with the test base;
FIG. 8 is a first schematic view of the structure of the test main body;
FIG. 9 is a second schematic structural view of a test subject;
FIG. 10 is a schematic structural view of a test base;
FIG. 11 is a schematic view of the structure of the base body in the test base;
FIG. 12 is a schematic view of the assembly of the test body with the test base;
FIG. 13 is a third schematic structural view of a test subject;
fig. 14 is a schematic structural diagram of a test main body.
The reference numbers are as follows:
1. a test subject; 2. an observation window; 3-1, a first mounting hole; 3-2, a second mounting hole; 3-3, conducting wires; 3-4, a counter electrode; 3-5, a reference electrode; 4. testing the base; 5. a second through hole; 6. a probe clamping assembly; 6-1, a spring; 6-2, adjusting bolts; 6-4, a limiting block; 6-5, mounting blocks; 6-6, a vertical rod; 6-7, a cross bar; 7. a probe; 8. a third mechanical pad; 9. a second mechanical pad; 10. a first mechanical cushion block; 11. a magnetic watch base; 12. a first through hole; 13. an annular groove; 14. a small hole; 15. a lead wire lead-out groove; 16. a base body; 17. a support body; 18. a sample; 19. and a third mounting hole.
Detailed Description
The invention is described in further detail below with reference to the following figures and specific examples:
as known from the background art, the testing device in the prior art has the problem that the in-situ electrochemical test cannot be carried out after stress is applied to the two-dimensional material.
In order to solve the above technical problem, the present invention provides a testing apparatus and a testing method, specifically comprising:
the nano material single crystal stress field coupling electrochemical testing device comprises an optical microscope, an electrochemical workstation, an electrochemical in-situ testing unit and a stress applying unit.
The electrochemical in-situ test unit comprises a test main body and a test base which are arranged from top to bottom in a matching way, and the whole electrochemical in-situ test unit is supported on a sample stage of the optical microscope. A first through hole is vertically arranged in the test main body, an annular groove (namely an electrolyte tank, preferably coaxially arranged with the first through hole) which surrounds the first through hole and is not completely closed is arranged on the end face of the upper end of the test main body, the wall surface of the inner side of the annular groove is lower than the wall surface of the outer side of the annular groove, and a lead leading-out groove with a downward opening is axially arranged on the test main body where the closed ring is not completely closed; an observation window with a small hole in the center is hermetically arranged on the upper end face of the first through hole, the small hole is positioned in the center of the observation window, and the observation window is made of transparent organic glass; the test main body is also provided with a first mounting hole and a second mounting hole which are communicated with the annular groove and used for respectively mounting a counter electrode and a reference electrode required by electrochemical test; the reference electrode and the counter electrode are respectively installed in the reference electrode connecting hole and the counter electrode connecting hole through waterproof threading bolts, and electrolyte is prevented from seeping. The test base is used for bearing and extending the flexible substrate and the nano material to be tested transferred onto the flexible substrate into the first through hole to be tightly pressed (namely, the contact is tight, and the electrolyte is prevented from seeping) on the lower end face of the small hole of the observation window, so that the flexible substrate and the wall of the small hole are matched to form a cavity capable of containing the electrolyte; when the electrolyte is filled, the electrolyte fills the cavity, overflows from the small hole of the observation window, flows into the annular groove, and contacts with a counter electrode and a reference electrode required by electrochemical test through the first mounting hole and the second mounting hole, and at the moment, the nano material to be tested is also positioned in the observation area and contacts with the electrolyte; the test base comprises a base main body and a support body; the base main body comprises a bottom plate and a connecting section coaxially arranged on the bottom plate, and a third mounting hole for mounting the support body is coaxially arranged in the base main body; the connecting section is provided with external threads, the first through hole is internally provided with internal threads, and the test base can be assembled into the test main body in a screwing mode; the vertical section of the support body is T-shaped, and a second through hole is arranged on the support body along the central shaft and comprises a support seat and a connecting rod which are coaxially arranged; the supporting seat is used for placing a sample, and the diameter of the supporting seat is larger than the aperture of the third mounting hole and smaller than the aperture of the first through hole; the connecting rod is inserted into the third mounting hole.
The stress applying unit comprises a probe, a probe clamping assembly and a three-dimensional moving platform. The three-dimensional moving platform comprises a magnetic gauge stand, and a first mechanical cushion block, a second mechanical cushion block and a third mechanical cushion block which are sequentially arranged on the magnetic gauge stand from bottom to top and respectively move towards an X axis, a Y axis and a Z axis; the three mechanical cushion blocks are all adjusted to move through adjusting the screw assemblies, and the movement of the three mechanical cushion blocks is not completely independent, for example, when the X-axis direction moves, the mechanical cushion blocks moving towards the Y axis and the Z axis simultaneously also can move in the X-axis direction, and when the Y-axis direction moves, the same is true, but when the Z-axis moves, the mechanical cushion blocks moving towards the Z axis only move. The probe is vertically (namely, vertical to the flexible substrate) arranged on a third mechanical cushion block moving to the Z axis through the probe clamping assembly; a fourth mounting hole is vertically formed in the third mechanical pad, and a threaded hole perpendicular to the fourth mounting hole is formed in the wall of the fourth mounting hole; the probe clamping assembly comprises an L-shaped supporting rod, a spring and a limiting block; the L-shaped supporting rod comprises a vertical rod and a cross rod; the vertical rod is arranged in the fourth mounting hole through the matching of the fastening bolt and the threaded hole; the cross rod is provided with a mounting block and a third through hole; spring and stopper are all established on the horizontal pole, and the one end and the installation piece of spring are connected, and the other end is connected with the stopper, and the stopper can exert the effort to the probe of inserting the third through-hole under the effect of spring, and the position of fixed probe in the third through-hole is with the probe chucking.
The optical microscope measures the strain quantity generated by the nano material to be measured through the small hole of the observation window; the optical microscope can read the strain capacity by adopting a general high-power optical microscope, and meanwhile, the electrochemical test process can be accompanied with some special optical phenomena and structural changes, so the in-situ observation can be carried out by adopting the optical microscope; and the electrochemical workstation measures the electrochemical performance of the nano material to be measured under the strain capacity, so that the electrochemical test of the nano material under the quantitative strain is realized.
According to the invention, the probe jacks up the flexible substrate by adjusting the position of the probe, the deformed substrate drives the sample, so that the sample is strained, and the strain of the micro-nano sample can be directly read by the optical microscope. The electrochemical test can be carried out while generating strain, and the change of the electrochemical performance of the micro-nano material under different strains can be explored. Usually, after the position of the XY surface is adjusted, the third mechanical cushion block is driven, so that the probe moves along the Z-axis direction, the flexible substrate is jacked up to drive the nano material to be measured to generate strain, the strain of the nano material to be measured is measured through an optical microscope, and the expected strain can be obtained by continuously adjusting the Z axis and observing.
The nanomaterial to be tested may be a single crystal, such as: the composite material is prepared from molybdenum disulfide, graphene, boron nitride and other single-crystal nanosheets.
According to the test requirements, the optical microscope can be replaced by a Raman device for testing the phase structure and the layer thickness of the crystal of the sample, and when stress is applied, the Raman characteristic peak of the material can be regularly shifted.
According to the invention, the flexible substrate is fixed in the in-situ observation device, the probe is contacted with the flexible substrate by adjusting the position of the probe, the flexible substrate can deform from small to large in the upward process of the probe, and the deformation of the flexible substrate drives the sample, so that the sample generates strain.
Referring to fig. 1 to 3, schematic structural diagrams and physical diagrams of the testing device according to the embodiment of the present invention are shown. Fig. 1 is a physical diagram of graphene transferred on a PDMS flexible substrate and subjected to different strains by the device, fig. 2 is a structural diagram of a raman spectrum obtained by applying different strains to molybdenum disulfide transferred on the PDMS flexible substrate by the device, and fig. 3-4 are schematic diagrams of electrochemical properties obtained by applying different strains to molybdenum disulfide transferred on the PDMS flexible substrate by the device.
Example one
Different stresses are applied to the graphene transferred on the PDMS flexible substrate by using part of the components (excluding the electrochemical workstation) of the testing device to generate different strains, and a specific physical diagram is shown in FIG. 1, which can be derived from the physical diagram that the graphene generates strains of 0%, 8.86%, 29.1% and 40.6%. This indicates that it is indeed possible to apply stress to the sample with this apparatus and method, causing it to become strained.
Example two
Fig. 2 is an example of a testing device of the present invention, which is a study of in situ observation of the influence of stress strain on raman effect of molybdenum disulfide.
The difference from the testing apparatus used in the first embodiment is that after the strain condition is observed, the optical microscope is replaced with a raman device, and the nano-material molybdenum disulfide to be tested is on the flexible substrate PDMS.
Adjusting the position of the probe to enable the probe to jack PDMS upwards so that PDMS is deformed, and the deformation of PDMS causes the strain of molybdenum disulfide; by adjusting the position of the probe, 0%, 1%, 2%, 3% and 4% stress strain is introduced into the molybdenum disulfide, and the strain generated by the molybdenum disulfide can be quantitatively measured by a microscope. The raman properties of molybdenum disulphide at different strains can be measured by raman equipment.
EXAMPLE III
As shown in fig. 3 to 14, this example is a study of the effect of stress strain on hydrogen evolution by molybdenum disulfide.
The embodiment adopts the whole testing device, namely comprises an optical microscope, a DH7003 electrochemical workstation, an electrochemical in-situ testing unit and a stress applying unit, wherein the nano material to be tested is a molybdenum disulfide micro device (substrate PDMS) and is tested according to the following steps:
1) The carbon rod electrode and the silver/silver chloride electrode are respectively arranged in a first mounting hole and a second mounting hole of the testing device, and the porous screw for fixing the electrode head and the rubber ring positioned between the electrode and the screw hole are screwed down to prevent the electrolyte from seeping.
2) Fixing the flexible substrate PDMS transferred with the nano material to be tested on a test base of the in-situ test device, and enabling the nano material to be tested to face an observation window at the upper end of the test main body;
3) Fixing one end of a lead on an observation window of a testing device, aligning an area of an electrode obtained by vapor deposition and connected with a nano material to be tested with the lead, and enabling the lead to be in good contact with the electrode of the nano material to be tested through extrusion of a testing base;
4) Respectively connecting the carbon rod electrode, the silver/silver chloride electrode and the other end of a lead (the other end of the lead is led out from a lead leading-out groove) connected with the electrode of the nano material to be detected with a counter electrode, a reference electrode and a working electrode of an electrochemical workstation;
5) Placing the testing device under an optical microscope and focusing the optical microscope on the surface of the nano material to be tested;
6) 0.5M H 2 SO 4 Injecting the electrolyte into the testing device to expose the electrolyte, the silver/silver chloride electrode, the carbon rod electrode and the observation window aperture 2 A region contact;
7) Adjusting the three-dimensional moving platform, and aligning the probe to the flexible substrate PDMS through a second through hole of the test base;
8) Performing an electrochemical scan test, such as performing Cyclic Voltammetry (CV), performing a 0.4V to-0.9V scan at a scan rate of 10 mV/s;
9) After the hydrogen evolution of the nano material to be detected is stable, adjusting the position of a probe of the three-dimensional mobile platform to enable the probe to jack up the flexible substrate PDMS upwards, so that the flexible substrate PDMS is deformed, and the deformation of the PDMS causes the strain of molybdenum disulfide;
10 By adjusting the probe position, 0%, 1%, 2%, 3%, and 4% stress strain is introduced to the molybdenum disulfide; and testing the strain capacity under different stresses by adopting an optical microscope, and testing the corresponding electrochemical hydrogen evolution performance under different strain capacities by using an electrochemical workstation.
In conclusion, the mechanical device is combined with the in-situ observation device, so that the electrochemical test can be performed on the micro-nano two-dimensional material while stress is applied; in addition, under the condition of not applying stress, the device can also be used for carrying out in-situ electrochemical reaction, in-situ electrical reaction, in-situ optical reaction or other combined tests on the material to be tested.
While the invention has been described with reference to specific embodiments, the invention is not limited thereto, and various equivalent modifications or substitutions can be easily made by those skilled in the art within the technical scope of the present disclosure.
Claims (9)
1. The nano material single crystal stress field coupling electrochemical testing device is characterized in that: the device comprises an optical microscope, an electrochemical workstation, an electrochemical in-situ test unit and a stress applying unit;
the electrochemical in-situ test unit comprises a test main body and a test base which are arranged from top to bottom in a matched manner;
a first through hole is vertically arranged in the test main body, an annular groove which surrounds the first through hole and is not completely closed is arranged on the end face of the upper end of the test main body, the wall surface of the inner side of the annular groove is lower than the wall surface of the outer side of the annular groove, and a lead leading-out groove with a downward opening is axially arranged on the test main body where the ring is not completely closed; an observation window with a small hole in the center is hermetically arranged on the upper end surface of the first through hole;
the test main body is also provided with a first mounting hole and a second mounting hole which are communicated with the annular groove and used for respectively mounting a counter electrode and a reference electrode required by electrochemical test;
the test base is used for bearing and extending the flexible substrate and the nano material to be tested transferred onto the flexible substrate into the first through hole to be tightly pressed against the lower end face of the small hole of the observation window, so that the flexible substrate and the wall of the small hole are matched to form a cavity capable of containing electrolyte;
the test base is provided with a second through hole along the axial direction;
the stress applying unit comprises a probe, a probe clamping assembly and a three-dimensional moving platform; the probe is vertically arranged on the three-dimensional moving platform through the probe clamping assembly, extends into the second through hole under the adjustment of the three-dimensional moving platform and applies mechanical stress to the flexible substrate arranged on the testing base, so that the nano material to be tested is strained;
the optical microscope measures the strain quantity generated by the nano material to be measured through the small hole;
the electrochemical workstation measures the electrochemical performance of the nano material to be measured under the strain;
the method for testing the nano material single crystal stress field coupling electrochemical testing device comprises the following steps:
1) Respectively mounting a counter electrode and a reference electrode in a first mounting hole and a second mounting hole of the testing device;
2) Fixing the flexible substrate transferred with the nano material to be tested on a test base of the test device, and enabling the nano material to be tested to face an observation window at the upper end of the test main body;
3) Fixing one end of a lead on an observation window of a testing device, aligning an area of an electrode obtained by vapor deposition and connected with a nano material to be tested with the lead, and enabling the lead to be in contact with the electrode of the nano material to be tested through extrusion of a testing base;
4) Connecting the other ends of the counter electrode, the reference electrode and the lead connected with the electrode of the nano material to be detected with the counter electrode, the reference electrode and the working electrode interface of the electrochemical workstation respectively;
5) Placing the testing device under an optical microscope and focusing the optical microscope on the surface of the nano material to be tested;
6) Injecting electrolyte into the testing device, and enabling the electrolyte to be in contact with the counter electrode, the reference electrode and the nano material area to be tested exposed from the small hole of the observation window;
7) Adjusting the three-dimensional moving platform, and enabling the probe to penetrate through the second through hole of the test base to be aligned with the flexible substrate;
8) Performing an electrochemical scanning test;
9) After the electrochemical signal of the nano material to be detected is stable, adjusting the position of a probe of the three-dimensional moving platform to enable the probe to jack the flexible substrate upwards to deform, so that the nano material to be detected generates strain;
10 Optical microscopy is used to measure the amount of strain and the electrochemical performance at that amount of strain is measured by an electrochemical workstation.
2. The nanomaterial single crystal stress field coupled electrochemical test device of claim 1, wherein:
the test base comprises a base main body and a supporting body;
the base main body comprises a bottom plate and a connecting section coaxially arranged on the bottom plate, and a third mounting hole for mounting the support body is vertically arranged in the base main body; the connecting section is matched with the lower end structure of the test main body, and the test base is connected with the test main body through the adaptive connection of the connecting section and the test main body;
the vertical section of the support body is T-shaped and comprises a coaxial support seat and a connecting rod; the diameter of the supporting seat is larger than the aperture of the third mounting hole, and the connecting rod is inserted into the third mounting hole.
3. The nanomaterial single crystal stress field coupling electrochemical test device according to claim 1 or 2, characterized in that:
the three-dimensional moving platform comprises a magnetic gauge stand, and a first mechanical cushion block, a second mechanical cushion block and a third mechanical cushion block which are sequentially arranged on the magnetic gauge stand from bottom to top and move towards an X axis, a Y axis and a Z axis respectively;
the three mechanical cushion blocks are adjusted to move through adjusting screw assemblies.
4. The nano-material single crystal stress field coupling electrochemical test device of claim 3, wherein:
the probe is arranged on a third mechanical cushion block moving to the Z axis through a probe clamping assembly;
a fourth mounting hole is vertically formed in the third mechanical pad;
the probe clamping assembly comprises an L-shaped supporting rod, a spring and a limiting block;
the L-shaped supporting rod comprises a vertical rod and a cross rod; the vertical rod is installed in the fourth installation hole through a fastening bolt; the cross rod is provided with a mounting block and a third through hole; spring and stopper all overlap and establish on the horizontal pole, and the one end and the installation piece of spring are connected, and the other end is connected with the stopper, and the stopper can exert the effort to the probe of inserting the third through-hole under the effect of spring, fixes the position of probe in the third through-hole.
5. The nanomaterial single crystal stress field coupled electrochemical test device of claim 4, wherein:
the inner walls of the first mounting hole and the second mounting hole are provided with internal threads and sealing rings.
6. The nanomaterial single crystal stress field coupled electrochemical test device of claim 5, wherein:
the observation window is made of glass.
7. The nanomaterial single crystal stress field coupled electrochemical test device of claim 1, wherein:
the nano material to be detected is prepared from a single crystal.
8. The nanomaterial single crystal stress field coupled electrochemical test device of claim 1, wherein:
the optical microscope is replaced by a Raman device.
9. The nanomaterial single crystal stress field coupled electrochemical test device of claim 1, wherein:
in the step 8), scanning is carried out at a scanning speed of 10mV/s from 0.4V to-0.9V.
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