CN113189157B - Electrochemical reaction tank device suitable for scanning probe microscope - Google Patents

Abstract

An electrochemical reaction pool device suitable for a scanning probe microscope is composed of a reaction pool main body, a sealing ring, a reaction pool cover, a positioning iron block, a red copper electrode and a metal clamping ring. The front of the reaction tank main body is provided with a reaction tank cover insertion groove, a sample groove, a reference electrode groove and an electrode groove, and a sealing ring is used for preventing liquid from seeping and participating in guiding and fixing the reference electrode and the electrode wire. Block sample embedding reaction tank main part bottom sample groove, there is the electrode connecting hole sample groove bottom to switch on second working electrode circuit and help through inserting red copper electrode and take out the sample, and fixed position iron plate help fixed reaction tank is inhaled to cell body bottom embedding magnetism, inserts the metal snap ring that prevents the reaction tank deformation in the annular groove of reaction tank main part below. The invention has small volume, simple structure and high reliability, and can be perfectly matched with an electrochemical module of a scanning probe microscope, thereby solving the problem of matching of block samples in scanning in an SECM-AFM mode.

Description

An electrochemical reaction cell device suitable for scanning probe microscopy

technical field

The invention relates to an electrochemical reaction cell device suitable for scanning probe microscopes, belonging to the fields of electrochemistry and electrocatalysis.

Background technique

Scanning Probe Microscope (SPM) technology can analyze and measure the physical properties or nano-manipulation of various materials at the nanoscale in the atmosphere, liquid phase and ultra-high vacuum environment, and has become an important tool for nanoscience research. Scanning probe microscopy techniques can be performed on the micro- and nano-scale. According to the difference of the physical quantity detection signal between the probe and the sample, various functional modules can be refined, including mechanical atomic force microscopy (AFM), conductive force microscopy (c-AFM), piezoelectric response atomic force microscopy (PFM) ), Scanning Capacitance Atomic Force Microscopy (SCM), Electrostatic Force Atomic Force Microscopy (EFM), Kelvin Probe Microscopy (sKPFM), Magnetic Atomic Force Microscopy (MFM), and Scanning Electrochemical Atomic Force Microscopy (SECM-AFM). Among them, SECM-AFM technology combines the advantages of AFM and SECM. In the process of scanning the surface of the material, the substrate morphology, electrical conductivity and the electrochemical reaction signal at the interface between the substrate and the solution can be obtained at the same time. with broad application prospects.

Although SECM-AFM modules and probes for commercial applications have been developed, due to the different requirements of different researchers for samples and test conditions, there is currently no universal supporting electrochemical reaction cell device on the market.

SUMMARY OF THE INVENTION

The invention provides an electrochemical reaction cell device suitable for a scanning probe microscope, so that a potential can be applied to a substrate sample when the reaction cell is loaded with a sample, and at the same time, the probe can scan the interface between the sample and the solution to obtain the surface morphology of the sample information and detect electrochemical signals.

In order to solve the above-mentioned technical problems and realize the above-mentioned technical effects, the present invention is realized through the following technical solutions:

An electrochemical reaction cell device for scanning probe microscope is characterized in that: it is composed of a reaction cell main body, a sealing ring, a reaction cell cover, a positioning iron block, a red copper electrode and a metal snap ring; the front of the reaction cell main body is provided with a reaction cell The cell cover is embedded, the reference electrode and the counter electrode are inserted into the sample groove, and the sealing ring participates in the guidance and fixation of the reference electrode and the counter electrode wire while preventing liquid leakage; the block sample is embedded in the sample groove at the bottom of the main body of the reaction cell. There is an electrode connection hole at the bottom of the tank to conduct the second working electrode circuit and help to take out the sample by inserting a copper electrode. The bottom of the tank body is embedded with a magnetic fixed position iron block to help fix the reaction tank, and a ring groove under the main body of the reaction tank is inserted to prevent the deformation of the reaction tank. Metal snap ring. The main material of the reaction tank is polytetrafluoroethylene. The top of the reaction tank body includes a sample tank, a reaction tank cover insertion tank, a reference electrode tank and a counter electrode tank. The bottom of the sample tank has a copper electrode insertion hole that penetrates to the bottom surface; the bottom surface includes a metal snap ring embedding groove, and a positioning iron block embedding groove.

The sealing ring is made of nitrile rubber, and its inner and outer diameters closely fit the insertion groove of the reaction tank cover. Insert the sealing ring into the reaction tank cover above the main body of the reaction tank, punch holes in it, and introduce platinum wire as the counter electrode and The silver chloride wire is used as the reference electrode. The platinum wire is bent into a ring shape and embedded in the counter electrode groove after penetrating, and the silver chloride wire is directly embedded in the reference electrode groove.

The material of the reaction tank cover is acrylic, which is transparent as a whole, which is convenient to observe the scanning probe, the internal solution and the sample. Ring to meet the requirements of sealing against leakage of liquid.

The four positioning iron blocks on the back of the main body of the reaction tank are embedded in the grooves, and the positioning iron blocks are embedded in the groove. The material is Q235 steel. After the positioning iron block is embedded, the bottom surface is level with the bottom surface of the reaction tank. The metal snap ring is inserted into the metal snap ring on the back of the main body of the reaction tank. The material is Q235 steel, which is embedded by interference fit, and the interference amount is 0.05mm. After the metal snap ring is embedded, the bottom surface is flush with the bottom surface of the main body of the reaction tank. The red copper electrode is inserted into the red copper electrode insertion hole at the bottom of the reaction tank. The material is red copper, and it is embedded by interference fit. The interference amount is 0.03mm. The length of the red copper electrode is longer than the height of the copper electrode insertion hole by 0.2mm to ensure that it can be connected with the test sample and the upper test sample. The bottom chassis contacts at the same time.

The test sample is inserted from the sample slot above the main body of the reaction cell, and inserted by means of interference fit. The interference amount is 0.03mm. After insertion, the upper surface of the test sample is flush with the upper surface of the main body of the reaction cell. That is, the assembly of the cell body is completed.

During the experiment, the reaction cell is fixed by magnetic attraction through the positioning iron block embedded in the bottom surface and the magnet on the sample tray of the scanning probe microscope. The scanning probe enters from the circular hole above the reaction cell cover and gradually contacts the surface of the sample. A working electrode, a counter electrode and a reference electrode wire embedded in the cell body form a three-electrode system to realize the electrochemical scanning function; the copper electrode embedded at the bottom of the cell body is connected to the scanning probe microscope sample tray and the sample, which can realize the sample through the chassis. A potential is applied to form the second working electrode, which also forms a three-electrode system with the counter electrode and reference electrode wire embedded in the cell body, which can test the electrochemical reaction signal independently or in conjunction with the probe. After the test, the sample embedded in the cell body can be pushed out by pushing the copper electrode from the bottom up, and the reaction cell can be disassembled and cleaned.

The invention has the advantages of small size, simple structure and high reliability, and can be perfectly matched with the electrochemical module of the scanning probe microscope, thereby solving the problem of adaptation of the bulk sample scanned in the SECM-AFM mode.

Description of drawings

Fig. 1 is the schematic diagram of each component and assembly position of the reaction tank,

The components are: reaction tank cover 1, sample 2, sealing ring 3, reaction tank main body 4, red copper electrode 5, metal snap ring 6, positioning iron block 7;

Figure 2a is a schematic diagram of the top of the reaction tank body and each embedded groove,

Figure 2b is a schematic diagram of the bottom surface of the reaction tank body and each embedded groove,

The components in FIG. 2 are: sample tank 8, reaction tank cover insertion slot 9, reference electrode slot 10, counter electrode slot 11, copper electrode insertion hole 12, metal snap ring embedding slot 13, and positioning iron block embedding slot 14;

Figure 3a is the fitting diagram of the device and the SECM-AFM module of the Dimension Icon scanning probe microscope,

Figure 3b is the surface view of the sample seen by the software when the device is fitted with the SECM-AFM module of the Dimension Icon scanning probe microscope.

Detailed ways

An electrochemical reaction cell device for scanning probe microscope AFM-SECM module is characterized in that: it is composed of a reaction cell main body, a sealing ring, a reaction cell cover, a positioning iron block, a red copper electrode, and a metal snap ring; the reaction cell main body is composed of The front is equipped with a reaction cell cover embedded, a reference electrode and a counter electrode are inserted into the sample embedding groove, and the sealing ring participates in the guidance and fixation of the reference electrode and the counter electrode wire while preventing liquid extravasation; the block sample is embedded in the bottom of the main body of the reaction cell. The sample tank has an electrode connection hole at the bottom of the sample tank to conduct the second working electrode circuit and help to take out the sample by inserting a copper electrode. The bottom of the tank body is embedded with a magnetic fixed position iron block to help fix the reaction tank. Deformed metal snap ring of the reaction cell. The main material of the reaction tank is polytetrafluoroethylene, and the upper surface includes a sample tank, a reaction tank cover insertion tank, a reference electrode tank, and a counter electrode tank. The bottom of the sample tank has a copper electrode insertion hole that penetrates to the bottom surface; the bottom surface includes a metal card The ring is embedded in the groove, and the positioning iron block is embedded in the groove.

The sealing ring is made of nitrile rubber, and its inner and outer diameters closely fit the insertion groove of the reaction tank cover. Insert the sealing ring into the reaction tank cover above the main body of the reaction tank, punch holes in it, and introduce platinum wire as the counter electrode and The silver chloride wire is used as the reference electrode. The platinum wire is bent into a ring shape and embedded in the counter electrode groove after penetrating, and the silver chloride wire is directly embedded in the reference electrode groove.

The material of the reaction tank cover is acrylic, which is transparent as a whole, which is convenient to observe the scanning probe, the internal solution and the sample. Sealing ring to meet the requirements of sealing against leakage of liquid.

The four positioning iron blocks on the back of the main body of the reaction tank are embedded in the grooves, and the positioning iron blocks are embedded in the groove. The material is Q235 steel. After the positioning iron block is embedded, the bottom surface is level with the bottom surface of the reaction tank. The metal snap ring is inserted into the metal snap ring on the back of the main body of the reaction tank. The material is Q235 steel, which is embedded by interference fit, and the interference amount is 0.05mm. After the metal snap ring is embedded, the bottom surface is flush with the bottom surface of the main body of the reaction tank. The copper electrode is inserted into the copper electrode insertion hole at the bottom of the reaction tank. The material is red copper, which is embedded by interference fit. The interference is 0.03mm. The length of the copper electrode is longer than the height of the copper electrode insertion hole by 0.2mm to ensure that it can be connected with the test sample and the upper test sample. The bottom chassis contacts at the same time.

The test sample is inserted from the sample slot above the main body of the reaction cell, and inserted by means of interference fit. The interference amount is 0.03mm. After insertion, the upper surface of the test sample is flush with the upper surface of the main body of the reaction cell. That is, the assembly of the cell body is completed.

During the experiment, the reaction cell is fixed by magnetic attraction through the positioning iron block embedded in the bottom surface and the magnet on the sample tray of the scanning probe microscope. The scanning probe enters from the circular hole above the reaction cell cover and gradually contacts the surface of the sample. A working electrode, a counter electrode and a reference electrode wire embedded in the cell body form a three-electrode system to realize the electrochemical scanning function; the copper electrode embedded at the bottom of the cell body is connected to the scanning probe microscope sample tray and the sample, which can realize the sample through the chassis. A potential is applied to form the second working electrode, which also forms a three-electrode system with the counter electrode and reference electrode wire embedded in the cell body, which can test the electrochemical reaction signal independently or in conjunction with the probe. After the test, the sample embedded in the cell body can be pushed out by pushing the copper electrode from the bottom up, and the reaction cell can be disassembled and cleaned.

Applications

When this device is matched with the SECM-AFM module of the Dimension Icon scanning probe microscope produced by Bruker, a perfect fit can be achieved, and the surface of the sample after needle insertion can be clearly seen on the scanning probe microscope control software end.

Claims (10)

1. The utility model provides an electrochemical reaction pond device suitable for scanning probe microscope which characterized in that: the device is formed by assembling a reaction tank main body (4), a sealing ring (3), a reaction tank cover (1), a positioning iron block (7), a red copper electrode (5) and a metal clamping ring (6); the front surface of the reaction tank main body (4) is provided with a reaction tank cover insertion groove (9), a sample groove (8), a reference electrode groove (10) and a counter electrode groove (11), the inner diameter and the outer diameter of the sealing ring (3) are tightly attached to the reaction tank cover insertion groove (9), the sealing ring is embedded into the reaction tank cover insertion groove on the reaction tank main body, then a hole is punched in the sealing ring and a platinum wire is introduced to serve as a counter electrode and a silver chloride wire as a reference electrode, the platinum wire is bent into a ring shape after penetrating into the counter electrode groove (11), the silver chloride wire is directly embedded into the reference electrode groove (10), and the sealing ring (3) is used for guiding and fixing the reference electrode and the electrode wire while preventing liquid from leaking; block sample (2) embedding reaction tank main part (4) bottom sample groove, there is the electrode connecting hole sample groove bottom to switch on second working electrode circuit and help and take out the sample through inserting red copper electrode (5), and fixed position iron plate (7) help fixed reaction tank is inhaled to cell body bottom embedding magnetism, inserts in reaction tank main part (4) below annular groove and prevents metal snap ring (6) that the reaction tank warp.

2. The electrochemical reaction cell device suitable for a scanning probe microscope according to claim 1, wherein: all parts are assembled and disassembled in an interference fit manner, and the solution in the device is not leaked.

3. The electrochemical reaction cell device suitable for a scanning probe microscope according to claim 1, wherein: the reference electrode and the counter electrode wire are led into the system by penetrating into the sealing ring (3) and being embedded into the groove of the reaction tank main body (4).

4. The electrochemical reaction cell device suitable for a scanning probe microscope according to claim 1, wherein: after the test sample (2) is embedded into the sample groove, a potential and a conducting current are applied through the red copper electrode (5) below, and the tested sample (2) can be pushed out from the red copper electrode (5).

5. The electrochemical reaction cell device suitable for a scanning probe microscope according to claim 1, wherein: the positioning iron block (7) embedded at the bottom is adsorbed on a sample table of the scanning probe microscope to realize fixation.

6. The electrochemical reaction cell device suitable for a scanning probe microscope according to claim 1, wherein: the upper surface of the reaction tank main body comprises a sample tank (8), a reaction tank cover insertion groove (9), a reference electrode tank (10) and a counter electrode tank (11), wherein the bottom of the sample tank is provided with a red copper electrode insertion hole (12) which penetrates to the bottom surface; the bottom surface of the positioning iron block comprises a metal snap ring embedded groove (13) and a positioning iron block embedded groove (14).

7. The electrochemical reaction cell device suitable for a scanning probe microscope according to claim 1, wherein: the sealing ring is made of nitrile rubber.

8. The electrochemical reaction cell device suitable for a scanning probe microscope according to claim 1, wherein: the reaction tank cover is made of acrylic materials, is transparent as a whole, facilitates observation of scanning probes, internal solution and sample conditions, is embedded into the reaction tank cover insertion groove (9) in the reaction tank main body in an interference fit mode, has the interference magnitude of 0.05mm, and compresses the sealing ring after being embedded so as to achieve the requirement of sealing and not enabling liquid to leak.

9. The electrochemical reaction cell device suitable for a scanning probe microscope according to claim 1, wherein: positioning iron blocks are embedded into four positioning iron block embedding grooves (14) in the back of the reaction tank main body, the positioning iron blocks are made of Q235 steel and are embedded in an interference fit mode, and the interference magnitude is 0.05 mm; the bottom surface of the embedded positioning iron block is level to the bottom surface of the reaction tank; the metal snap ring is embedded into the metal snap ring embedding groove (13) on the back of the reaction tank main body; the metal clamping ring is made of Q235 steel and is embedded in an interference fit mode, and the interference magnitude is 0.05 mm; the bottom surface of the embedded metal snap ring is level with the bottom surface of the reaction tank main body; the red copper electrode is inserted into the red copper electrode insertion hole (12) at the bottom of the reaction tank, the red copper electrode is made of red copper and is embedded in an interference fit mode, the interference magnitude is 0.03mm, and the length of the red copper electrode is longer than the height of the red copper electrode insertion hole (12) by 0.2mm so as to ensure that the red copper electrode can be simultaneously contacted with an upper test sample and a lower bottom plate.

10. The method for using the electrochemical reaction cell device suitable for the scanning probe microscope as claimed in claim 1, wherein in the experiment process, the reaction cell is fixed with the magnet on the sample tray of the scanning probe microscope through the positioning iron block embedded in the bottom surface by magnetic attraction, the scanning probe enters from the round hole above the reaction cell cover and gradually contacts with the surface of the sample, and the probe as the first working electrode and the counter electrode and the reference electrode wire embedded in the cell body form a three-electrode system to realize the electrochemical scanning function; the red copper electrode embedded in the bottom of the cell body is communicated with the sample tray of the scanning probe microscope and a sample, so that a potential can be applied to the sample through the chassis to form a second working electrode, and the second working electrode, the counter electrode and the reference electrode wire embedded in the cell body form a three-electrode system which can independently or in linkage with the probe to test an electrochemical reaction signal; after the test, the sample embedded in the cell body can be pushed out by pushing the red copper electrode upwards from the lower part, and the reaction cell can be detached and cleaned.

Images