Probe testing auxiliary device for realizing in-situ micro electric field multifunction

Abstract

The application discloses a kind of in-situ micro electric field multifunctional probe test auxiliary device.The device includes hexagonal box body, U-shaped probe baffle and main base;Each side wall of the hexagonal box body is provided with U-shaped window;The U-shaped probe baffle is inserted into the U-shaped window;A pair of sealing sheets is provided on each U-shaped probe baffle, and the gap formed at the abutting place thereof is used as the entrance and exit of the probe;An objective lens sealing sliding element is provided on the top cover of the hexagonal box body, and the objective lens can move vertically through the central hole of the objective lens sealing sliding element;The hexagonal box body, U-shaped probe baffle, objective lens sealing sliding element and objective lens form a sealed cavity.The device can realize multiple probes to prick in micron scale sample at any position to apply voltage or current, and after being used with a microscopic Raman spectrometer, the sample can be in-situ collected Raman spectrum, and the microstructure change is analyzed.

Description

Technical Field

[0001] This invention relates to a probe testing auxiliary device for realizing multifunctional in-situ micro electric fields, belonging to the field of analytical testing equipment manufacturing. Background Technology

[0002] An electric field can affect the molecular orientation, phase transition, thermal effects, and virus capture of a sample, thus influencing changes in Raman spectra. Raman spectroscopy under a microscopic electric field can be used to analyze changes in molecular orientation or phase transitions in field-effect transistors, semiconductors, ceramic samples, etc., and can also be used to study surface-enhanced Raman spectroscopy (SERS), which is particularly suitable for studying graphene-like materials.

[0003] Taking graphene as an example, an electrostatic potential difference is created between graphene and the gate. By adjusting the gate voltage, the position of the Fermi level in graphene can be adjusted, thereby actively regulating the electron-phonon coupling degree. This can alter the Raman spectral characteristics of graphene, demonstrating the reversibility and controllability of graphene doping. The gate voltage can be converted into doping concentration using a formula. Excessive charge (defects) leads to lattice expansion (contraction). Therefore, changes in the Raman spectral characteristics of graphene can be used to qualitatively and quantitatively assess the effects of external doping and electric field effect doping on the carrier concentration of graphene, providing essential tools for the functional design and control of carbon materials.

[0004] However, there are currently no commercially available probe stations specifically designed for micro Raman instruments. The specifications and dimensions of existing probe stations are not suitable for installation on existing micro confocal laser Raman spectrometers, and their functions cannot fully meet the needs of researchers. Summary of the Invention

[0005] The purpose of this invention is to provide a probe testing auxiliary device. This device allows multiple probes to be inserted at arbitrary locations on a micrometer-scale sample to apply voltage or current. When used in conjunction with a micro Raman spectrometer, it enables in-situ acquisition of Raman spectra of the sample, allowing analysis of its microstructural changes.

[0006] To achieve the above objectives, the present invention adopts the following technical solution:

[0007] A probe testing auxiliary device includes an upper hexagonal box-shaped main body and a U-shaped probe baffle;

[0008] The hexagonal box-shaped main body is a hexagonal prism-shaped cavity; a U-shaped window is opened in the upper middle part of each side wall of the cavity; the U-shaped probe baffle is inserted into the U-shaped window and moves horizontally within the U-shaped window; a pair of abutting sealing plates are provided at the vertical center line of each U-shaped probe baffle, and the gap formed at the abutting part of each pair of sealing plates serves as the entrance and exit of the external device probe;

[0009] The top cover of the cavity is a concave hexagonal ring structure. A lens sealing slide with a central hole is provided at the center of the top cover. The lens moves vertically in the lens sealing slide through the central hole. A sealing gasket is also provided on the upper surface of the lens sealing slide.

[0010] The objective lens, together with the objective lens sealing slide, the sealing gasket, the U-shaped probe baffle, the sealing sheet, and the hexagonal box-shaped body, forms a sealed cavity;

[0011] The cavity is provided with a main body base at its lower part;

[0012] An X-axis micrometer and a Y-axis micrometer are provided on the outer side wall of the main body base, and the X-axis micrometer and the Y-axis micrometer extend into the interior of the main body base respectively;

[0013] The main body base contains a sample stage base for placing samples. The hexagonal box-shaped main body has a side length of 60-100mm and a height of 40-70mm.

[0014] The length of the U-shaped window is 40-70mm, which is 2 / 3 of the side length of the cavity, and the height is 20-40mm, which is 1 / 2 of the height of the cavity.

[0015] The height of the entrance / exit is 20-30mm.

[0016] The main base has a length of 150-300mm and a height of 40-70mm.

[0017] The edge of the U-shaped window is provided with a groove, and the U-shaped probe baffle is inserted into the U-shaped window through the groove and moves horizontally; the length of the groove is 10-20mm and the depth is 3-6mm.

[0018] The U-shaped probe baffle is made of aluminum; the sealing sheet is made of rubber.

[0019] The objective lens sealing slider is an inverted frustum structure with a central hole; the outer diameter of the upper surface of the objective lens sealing slider is 50-65mm, the inner diameter is 25-30mm, and the height is 10-20mm.

[0020] The main base is equipped with an X-axis micrometer fixing plate, an X-axis micrometer sliding accessory, and a dovetail groove base X; the X-axis micrometer fixing plate is used to fix the X-axis micrometer; the X-axis micrometer moves the sample in the X direction through the X-axis micrometer fixing plate, the dovetail groove base, and the X-axis micrometer sliding accessory in sequence, with a movement range ≥5mm;

[0021] The main base is equipped with a Y-axis micrometer fixing plate, a Y-axis micrometer sliding accessory, and a dovetail groove base Y. The Y-axis micrometer fixing plate is used to fix the Y-axis micrometer. The Y-axis micrometer moves the sample in the Y direction through the Y-axis micrometer fixing plate, the dovetail groove base, and the Y-axis micrometer sliding accessory in sequence. The movement range is ≥5mm.

[0022] The main body base is equipped with an electrical connection assembly; the electrical connection assembly includes an electrical connection base, a sealed electrical connector, and a wire.

[0023] The electrical connector is located at the bottom of the main body base.

[0024] The sealed electrical connector is located on the lower part of the side wall inside the main body base.

[0025] The wire is used to connect the sample to the electrical connector, the sealed electrical connector, and the external high-precision power supply.

[0026] The side wall of the main base is provided with a gas input component that is connected to an external gas supply device; the gas input component includes an ambient gas port and a 1-to-4 gas conduit; the four gas outlets of the 1-to-4 gas conduit are fixed near the sample stage base by a gas conduit fixing base.

[0027] The sample stage base is equipped with high-temperature components.

[0028] The probe testing auxiliary device is used in in-situ microscopic electric field analysis coupled with a microscope. Preferably, the probe testing auxiliary device is used in in-situ spectroscopic analysis and in-situ mechanical analysis coupled with a microscope, such as in-situ Raman analysis.

[0029] The beneficial effects of this invention are as follows:

[0030] 1. The device described in this invention, through the combined use of the objective lens sealing slider, the U-shaped probe baffle and the sealing sheet, has certain airtightness and shielding characteristics. It can support the switching of multiple magnification objectives and enable multiple probes to be inserted at any position on the micron-scale sample to apply voltage or current. Thus, it can be used in conjunction with a micro Raman spectrometer to collect Raman spectra of the sample in situ and analyze its microstructural changes.

[0031] 2. The present invention, through the horizontal movement design of the U-shaped probe baffle, allows the probe to have a large range of movement (approximately 3cm) in both horizontal and vertical directions, providing greater convenience for testing applications.

[0032] 3. By designing the top of the hexagonal box-shaped main body as a hollow concave shape, the present invention forms a structure that gradually rises from the center outward, which not only provides sufficient operating space for the probe, but also makes the sealed cavity as small as possible, resulting in more accurate analysis results.

[0033] 4. This invention, through a precise micrometer design, enables precise movement of the sample in the X / Y directions, with a movement range ≥5mm and a movement accuracy better than 20μm.

[0034] 5. The main body base of the device described in this invention is also provided with an electrical connection component. The electrical connection component can be used to directly lead wires out from the sample to apply voltage or current to a fixed position on the sample.

[0035] 6. The main body base of the device described in this invention is also provided with a gas input component. Through the design of the atmospheric gas hole and the 1-to-4 gas conduit in the gas input component, the entire sample box and the area near the sample are purged, thereby ensuring that the entire device and the space near the sample are in an inert gas atmosphere.

[0036] 7. The sample stage base provided by the present invention adopts a high temperature adaptability design, and reserves mounting holes and fixing positions for high temperature optional components. It can be upgraded with high temperature optional components in the future, thereby realizing a wide range of testing applications from room temperature to 200℃. Attached Figure Description

[0037] Figure 1 This is a schematic diagram of the overall structure of the probe testing auxiliary device provided by the present invention.

[0038] Figure 2 This is a schematic diagram of the objective lens sealing part in the probe testing auxiliary device provided by the present invention.

[0039] Figure 3 This is a schematic diagram of the objective lens sealing part and the hexagonal box-shaped main body in use in the probe testing auxiliary device provided by the present invention.

[0040] Figure 4 This is a schematic diagram of the sample displacement stage in the probe testing auxiliary device provided by the present invention.

[0041] Figure 5 This is a schematic diagram of the internal space of the probe testing auxiliary device provided by the present invention.

[0042] Figure 6 A 3D model diagram of the probe testing auxiliary device provided by the present invention in its usage state.

[0043] Figure 7 The images show two probe needles of a 1000Ω resistance sample obtained by analysis using the probe testing auxiliary device provided by this invention.

[0044] Figure 8 The present invention provides a probe testing auxiliary device for analyzing the voltage and current changes of a 1000Ω resistor sample under microscopic conditions after applying a voltage.

[0045] In the figure: 1-Objective lens; 2-Top cover of hexagonal box-shaped body; 3-Hexagonal box-shaped body; 4-Main body base; 5-X-axis micrometer fixing plate; 6-X-axis micrometer; 7-Y-axis micrometer fixing plate; 8-Y-axis micrometer; 9-Objective lens sealing sliding component; 10-U-shaped probe baffle; 10-1 rubber sealing sheet; 11-Electrical connection seat; 12-Sealed electrical connector; 13-Atmosphere gas port; 14-High temperature element; 15-1 / 4 gas conduit; 16-Gas conduit fixing base; 17-X-axis micrometer sliding accessory; 18-Dovetail groove base Y; 19-Dovetail groove base X; 20-Y-axis micrometer sliding accessory; 21-Sample; 22-High-precision moving needle seat; 23-Rubber sealing gasket; 24-Sample stage base. Detailed Implementation

[0046] The present invention will be further described in detail below with reference to specific embodiments. The embodiments given are only for illustrating the present invention and are not intended to limit the scope of the present invention.

[0047] This invention specifically provides a probe testing auxiliary device, including a hexagonal box-shaped main body 3, a U-shaped probe baffle 10, and other components, with the following specific structure:

[0048] The hexagonal box-shaped main body 3 is a hexagonal prism-shaped cavity, such as... Figure 1 As shown, its side length is 60-100mm and its height is 40-70mm; a U-shaped window is opened in the upper middle part of each side wall of the cavity, the length of the U-shaped window is 40-70mm (about 2 / 3 of the side length of the cavity) and the height is 20-40mm (about 1 / 2 of the height of the cavity); a groove is provided at the edge of each U-shaped window, the width of the groove is 10-20mm and the depth is 3-6mm.

[0049] The U-shaped probe baffle 10 is inserted into the U-shaped window and moves horizontally within the U-shaped window, such as... Figure 1 As shown; the U-shaped probe baffle, 10 is made of aluminum.

[0050] A pair of mating rubber sealing sheets 10-1 are also provided at the vertical center line of each U-shaped probe baffle 10, such as... Figure 1 As shown, the gap formed at the point where each pair of rubber sealing sheets touches can serve as the entrance and exit of an external device probe, with the height of the entrance and exit being 20-30mm. The rubber sealing sheets not only provide a certain degree of sealing for the hexagonal box-shaped body 3, but also ensure the vertical movement of the probe through the entrance and exit. The material of the rubber sealing sheets is acetonitrile rubber.

[0051] A hexagonal box-shaped top cover 2 is provided at the top of the aforementioned cavity. This top cover has a concave hexagonal annular structure, such as... Figure 1As shown, the concave structure with a low center and high sides allows the probe to have sufficient room to move within the hexagonal box-shaped body 3, while also minimizing the sealed space of the cavity; the top cover 2 can be fixed to the hexagonal box-shaped body through screw holes.

[0052] An objective lens sealing slider 9 is provided at the center of the top cover 2, such as Figure 1 As shown; the objective lens sealing slider 9 is an inverted frustum-shaped structure with a central hole, as shown. Figure 2 As shown, a rubber sealing gasket 23 is also provided on the upper surface of the objective lens sealing slider 9. The diameter of the central hole of the objective lens sealing slider and the inner diameter of the sealing gasket are matched with the size of the objective lens. The objective lens 1 moves vertically through the central hole and the rubber sealing gasket 23. As long as the objective lens 1 does not touch the probe, the objective lens can get infinitely close to the sample, thus enabling high-magnification objective lens analysis. The outer diameter of the upper surface of the objective lens sealing slider 9 is 50-65 mm, the overall height is 10-20 mm, and the material is metal. The diameter of the central hole of the objective lens sealing slider 9 is 25-30 mm.

[0053] like Figure 3 As shown, a sealed space can be formed by the cooperation design of objective lens 1, objective lens sealing slider 9, rubber sealing gasket 23, U-shaped probe baffle 10, rubber sealing sheet 10-1 and hexagonal box-shaped body 3.

[0054] Furthermore, a main body base 4 is provided at the bottom of the cavity, such as... Figure 1 As shown; the length of the main body base 4 is 150-300mm and the height is 40-70mm.

[0055] An X-axis micrometer 6 and a Y-axis micrometer 8 are provided on the outer side wall of the aforementioned main base, such as... Figure 1 As shown, the X-axis micrometer and the Y-axis micrometer extend into the interior of the main body base and are connected to the sample stage base 24.

[0056] Inside the main base, there are also X-axis micrometer fixing plates 5, X-axis micrometer sliding fittings 17, and dovetail groove bases X18 for fixing the X-axis micrometer 6, such as... Figure 4 As shown, the X-axis micrometer 6 moves the sample in the X direction through the X-axis micrometer fixing plate 5, the dovetail groove base X18 and the X-axis micrometer sliding accessory 17 in sequence, with a movement range ≥5mm.

[0057] Inside the main base, there are also Y-axis micrometer fixing plates 7, Y-axis micrometer sliding fittings 19, and dovetail groove bases Y 20 for fixing the Y-axis micrometer 8, such as... Figure 4 As shown, the Y-axis micrometer 8 moves the sample in the Y direction through the Y-axis micrometer fixing plate 7, the dovetail groove base Y 20 and the Y-axis micrometer sliding accessory 19 in sequence, with a movement range ≥5mm.

[0058] A sample stage base 24 is also provided inside the main body base, such as Figure 5 As shown; wherein, a high-temperature element 14 is configured on the sample stage base 24, which can perform high-temperature tests from room temperature to 200℃.

[0059] An electrical connection assembly is also provided within the main base; the electrical connection assembly includes an electrical connector 11, a sealed electrical connector 12, and wires, such as... Figure 5 As shown; the electrical connector 11 is located at the bottom of the main body base, and the sealed electrical connector 12 is located at the lower part of the side wall inside the main body base. The sample on the sample stage base 24 is connected to the electrical connector 11, the sealed electrical connector 12 and the external high-precision power supply in sequence through wires, so that voltage or current can be applied directly to the sample without the need to apply it through a probe; a maximum of 4 wires can be set to connect to the sample.

[0060] A gas input assembly for connection to an external gas supply device is provided on the side wall of the main base 4; the gas input assembly includes an ambient gas port 13 and a 1 / 4-way gas conduit 15, such as... Figure 5 As shown; the inlet of the atmosphere gas port 13 and the inlet of the 1-to-4 gas conduit 15 are respectively connected to external gas supply equipment (such as gas cylinders or gas bags); the four outlets of the 1-to-4 gas conduit 15 are fixed near the sample stage base 24 through the gas conduit fixing base 16; the atmosphere gas port 13 can be used to fill the inside of the device, replacing the internal air and making the sample in the atmosphere gas; the 1-to-4 gas conduit 15 can make the atmosphere gas near the sample, ensuring that the sample is in the atmosphere gas.

[0061] like Figure 6 As shown, through the design of the above-mentioned probe testing auxiliary device, the high-precision moving needle holder can enter the hexagonal box-shaped body 3 through the rubber sealing sheet 10-1 of the U-shaped probe baffle 10, and make contact with the sample, and apply voltage or current to the sample through an external high-precision power supply; using the above-mentioned probe testing auxiliary device provided by the present invention, up to 6 high-precision moving needle holders can be used at the same time, that is, up to 6 electrodes can be set on the sample at the same time.

[0062] The probe testing auxiliary device provided by this invention can be used according to the following steps:

[0063] S1. Place the above-mentioned probe testing auxiliary device, except for the top cover 2 of the hexagonal box-shaped main body, the objective lens sealing sliding part 9 and the rubber sealing gasket 23, on the sample base of the micro Raman instrument, and place the sample on the sample stage base 24 inside the probe testing auxiliary device.

[0064] S2. Place multiple high-precision movable needle holders 22 near each side wall of the hexagonal box-shaped main body, and insert the multiple probes configured thereon into the inside of the probe testing auxiliary device through the gaps between the rubber sealing sheets 10-1 of the U-shaped probe baffles 10 on each side wall, and adjust the position of the probes so that they are directly above the sample.

[0065] S3. First, focus the sample using the 10X objective lens (low-power objective lens) of the Raman spectrometer, and move the sample using the X-axis micrometer and Y-axis micrometer to find a suitable field of view; then place one of the probes below the focusing spot of the 10X objective lens and away from the sample, and then gradually lower the height of the probe to bring it closer to the sample while focusing the probe; finally, without the probe touching the sample, slowly move the position and pitch angle of the probe in the XY direction so that the probe falls within the specific field of view of the sample; use the same method to focus and adjust the remaining probes; after all probes have been adjusted, install the top cover 2 of the hexagonal box-shaped main body, the objective lens sealing slider 9, and the rubber sealing gasket 23;

[0066] S4. Connect the high-precision moving needle holder 22 to an external high-precision power supply, and apply voltage or current to the probe carried by the high-precision moving needle holder 22 through software.

[0067] If the sample testing needs to be carried out in an inert atmosphere, connect the inlet of the atmospheric gas port 13 and the inlet of the 1-to-4 gas conduit 15 to the external gas supply equipment respectively, and introduce inert gas to purge the internal space of the probe testing auxiliary device and the space near the sample.

[0068] S5. Replace with a high-power objective lens (such as a 50X or 100X objective lens) and use a micro Raman spectrometer to perform Raman analysis on the sample.

[0069] Application examples

[0070] Taking a 1000Ω resistive material as a sample for Raman analysis as an example, the steps for using the above-mentioned probe testing auxiliary device are as follows:

[0071] (1) Place the above-mentioned probe testing auxiliary device, except for the top cover 2 of the hexagonal box-shaped main body, the objective lens sealing sliding part 9 and the rubber sealing gasket 23, on the sample base of the micro Raman instrument, and then place the 1000Ω resistance material sample on the sample stage base 24 inside the probe testing auxiliary device.

[0072] (2) Adjust the probe position according to steps S2 and S3 above;

[0073] (3) Following step S4 above, use two probes to poke the ends of the 1000Ω resistor, as follows: Figure 7As shown, the probe has made full contact with the resistor sample; by changing different voltages, voltage and current curves are plotted to observe whether a voltage is applied across the resistor. The results show that, as... Figure 8 As shown, a voltage has been applied to the microscale of the resistive sample, thus enabling in-situ acquisition of Raman spectra to analyze changes in its microstructure.

[0074] The probe testing auxiliary device provided by this invention, as a microscope analysis auxiliary device, can be used not only with micro Raman instruments, but also with various other analytical devices that need to be used in conjunction with microscopes, such as mechanical testing devices and spectroscopic analysis devices.

[0075] When used as a probe testing auxiliary device for Raman analysis, the probe testing auxiliary device provided by this invention is suitable for a variety of samples, such as graphene materials, field-effect transistors, semiconductors, ceramics, etc.

[0076] Although the present invention has been described in detail above with general descriptions and specific embodiments, modifications or improvements can be made to it, which will be obvious to those skilled in the art. Therefore, all such modifications or improvements made without departing from the spirit of the present invention fall within the scope of protection claimed by the present invention.

Claims

1. A probe testing auxiliary device, comprising an upper hexagonal box-shaped main body and a U-shaped probe baffle; The hexagonal box-shaped main body is a hexagonal prism-shaped cavity; a U-shaped window is opened in the upper middle part of each side wall of the cavity; the U-shaped probe baffle is inserted into the U-shaped window and moves horizontally within the U-shaped window; a pair of abutting sealing plates are provided at the vertical center line of each U-shaped probe baffle, and the gap formed at the abutting part of each pair of sealing plates serves as the entrance and exit of the external device probe; The top cover of the cavity is a concave hexagonal ring structure. A lens sealing slide with a central hole is provided at the center of the top cover. The lens moves vertically in the lens sealing slide through the central hole. A sealing gasket is also provided on the upper surface of the lens sealing slide. The objective lens, together with the objective lens sealing slide, the sealing gasket, the U-shaped probe baffle, the sealing sheet, and the hexagonal box-shaped body, forms a sealed cavity; The cavity is provided with a main body base at its lower part; An X-axis micrometer and a Y-axis micrometer are provided on the outer side wall of the main body base, and the X-axis micrometer and the Y-axis micrometer extend into the interior of the main body base respectively; The main body base contains a sample stage base.

2. The probe testing auxiliary device according to claim 1, characterized in that: The hexagonal box-shaped main body has a side length of 60-100mm and a height of 40-70mm; The length of the U-shaped window is 40-70mm, and the height is 20-40mm; The height of the entrance / exit is 20-30mm; The main base has a length of 150-300mm and a height of 40-70mm.

3. The probe testing auxiliary device according to claim 1 or 2, characterized in that: The edge of the U-shaped window is provided with a groove, and the U-shaped probe baffle is inserted into the U-shaped window through the groove and moves horizontally. The groove is 10-20mm long and 3-6mm deep.

4. The probe testing auxiliary device according to any one of claims 1-3, characterized in that: The U-shaped probe baffle is made of aluminum. The sealing sheet is made of rubber.

5. The probe testing auxiliary device according to any one of claims 1-4, characterized in that: The objective lens sealing slider is an inverted frustum structure with a central hole; The outer diameter of the upper surface of the objective lens sealing slider is 50-65mm, the inner diameter is 25-30mm, and the height is 10-20mm.

6. The probe testing auxiliary device according to any one of claims 1-5, characterized in that: The main base is equipped with an X-axis micrometer fixing plate, an X-axis micrometer sliding fitting, and a dovetail groove base X. The X-axis micrometer fixing plate is used to fix the X-axis micrometer; the X-axis micrometer moves the sample in the X direction through the X-axis micrometer fixing plate, the dovetail groove base and the X-axis micrometer sliding accessory in sequence, with a movement range ≥5mm; The main base is equipped with a Y-axis micrometer fixing plate, a Y-axis micrometer sliding accessory, and a dovetail groove base Y; the Y-axis micrometer fixing plate is used to fix the Y-axis micrometer. The Y-axis micrometer moves the sample in the Y direction sequentially through the Y-axis micrometer fixing plate, the dovetail groove base, and the Y-axis micrometer sliding accessory; the movement range is ≥5mm.

7. The probe testing auxiliary device according to any one of claims 1-6, characterized in that: The main body base is equipped with an electrical connection assembly; the electrical connection assembly includes an electrical connection base, a sealed electrical connector, and a wire; The electrical connector is located at the bottom of the main body base; The sealed electrical connector is located on the lower part of the side wall inside the main body base; The wire is used to connect the sample to the electrical connector, the sealed electrical connector, and the external high-precision power supply.

8. The probe testing auxiliary device according to any one of claims 1-7, characterized in that: The main base is provided with a gas input component on its side wall for connection to an external gas supply device; the gas input component includes an ambient gas port and a 1-to-4 gas conduit. The four gas outlets of the 1-to-4 gas conduit are fixed near the sample stage base by the gas conduit fixing base.

9. The probe testing auxiliary device according to any one of claims 1-8, characterized in that: The sample stage base is equipped with high-temperature components.

10. The application of the probe testing auxiliary device according to any one of claims 1-9 in in-situ microscopic electric field analysis in conjunction with a microscope.

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