CN105136822B - A kind of nano material transmission electron microscope in-situ test chip, chip preparation method and its application - Google Patents

Abstract

The invention discloses a nanomaterial transmission electron microscope in-situ testing chip, a chip preparation method and an application thereof, and belongs to the technical field of in-situ testing of nanomaterial performance. The chip of the present invention includes a silicon substrate, an insulating layer and a film window, and an insulating layer is formed on both sides of the silicon substrate; a metal film or device, or a semiconductor functional film or device is formed on the insulating layer on the front side of the chip, and various samples can be applied to the sample. Similar to physical and chemical effects; there is a film window in the center of the chip, and a large aspect ratio electron beam permeable long hole or electron beam long slot is opened in the film window area. Measurement, in addition to in-situ characterization of nanowire and nanotube samples, in-situ characterization of bulk samples and heterojunction interface samples can also be realized, and at the same time, it can be placed with a micromanipulator in the focused ion beam system and in the laboratory Samples can also be further processed using ion thinning equipment for samples that have been transferred and fixed on the chip.

Description

A nanometer material transmission electron microscope in-situ test chip, chip preparation method and its application

technical field

The invention relates to the technical field of in-situ testing of nanomaterial properties, more specifically, to a nanomaterial transmission electron microscope in-situ testing chip, a chip preparation method and an application thereof.

Background technique

In recent years, nanomaterials have attracted widespread attention in the field of scientific research due to their nanoscale properties such as small size effects, surface effects, quantum size effects, and macroscopic quantum tunneling effects. Transmission Electron Microscope (TEM) is a powerful modern material characterization method, which is used to analyze the fine structure smaller than 0.2 μm that cannot be seen clearly under the optical microscope. Today's TEM is capable of sub-Angstrom resolution and is a powerful tool for analyzing nanomaterials. Nanomaterials have peculiar effects in the fields of electricity, heat, mechanics, etc. With the development of microelectromechanical systems (MicroElectromechanical System, MEMS) and nanoelectromechanical systems (Nano Electromechanical System), the structure of materials is revealed from the nanometer scale and in the above fields The relationship between the various effects has become an urgent problem to be solved.

Obtaining material structure information with the help of transmission electron microscopy while detecting the corresponding electrical, thermal, and mechanical properties of the structure belongs to in-situ observation by transmission electron microscopy. At present, the tools for in-situ observation of TEM mainly include environmental transmission electron microscope (ETEM), in-situ sample rod for TEM, and in-situ MEMS chip, etc. Thanks to the development of MEMS technology, more and more physical and chemical functions can be integrated on existing in-situ MEMS chips. Moreover, the characteristics of the small size of the chip and the ability to work when it is powered on are well in line with the requirements for in-situ testing of the transmission electron microscope. However, the application of existing in-situ MEMS chips still has its limitations. Generally, only focused ion beam (FIB) systems can be used for sample transfer and fixation, which limits the conditions of use and greatly increases the cost of use. In addition, the focused ion beam system cannot avoid contamination of the sample during sample transfer and fixation, but the existing in-situ MEMS chip cannot process the sample after the transfer and fixation of the sample is completed. The above limitations limit the application of in-situ MEMS chips to a large extent, and there is no good solution at present.

Contents of the invention

1. The technical problem to be solved by the invention

The purpose of the present invention is to overcome the above-mentioned deficiencies in the prior art, provide a kind of nanomaterial transmission electron microscope in-situ test chip, chip preparation method and application thereof; Adopt the in-situ test chip of the present invention, can use focused ion beam (FIB) The system processes and transfers samples, and the micromanipulator (micromanipulator) can also be used to place samples outside the FIB, and the chip with the samples can be ion-cleaned or thinned in the ion thinning equipment, which can realize the In-situ TEM observation of a variety of samples including metals, low-dimensional materials, heterojunction interfaces, and bulk samples.

2. Technical solution

In order to achieve the above object, the technical scheme provided by the invention is:

A nanomaterial transmission electron microscope in-situ test chip of the present invention includes a silicon substrate, an insulating layer, and a thin film window. Both sides of the silicon substrate are provided with insulating layers, and the front side of the silicon substrate is provided with an insulating layer. The thin film window has a long hole or a long slot through which the electron beam passes through, and the width of the long hole through the electron beam or the long slot through the electron beam is 5-20 μm; the insulation on the front side of the silicon substrate Metal films or devices, or semiconductor functional films or devices that can apply various physical and chemical effects to the sample are arranged on the layer.

Furthermore, the length of the e-beam-transmitting long hole or electron-beam-transmitting slot is 100-400 μm.

Furthermore, the insulating layer includes a silicon dioxide layer grown on the silicon substrate and a silicon nitride layer grown on the silicon dioxide layer, since the silicon dioxide layer is too thin, it will affect the stress control of the silicon nitride And support ability and protection during etching process. If the silicon nitride layer is too thin, it will affect the supporting effect of the sample and the protective effect played in the etching process, so the thickness of the silicon dioxide layer is 200-1000nm, and the thickness of the silicon nitride layer is 5-200nm .

Furthermore, the part of the metal thin film or device, semiconductor functional thin film or device located on the film window is distributed along one side or both sides of the electron beam-transmitting long hole or the electron-beam-transmitting long groove.

Furthermore, the thickness of the silicon substrate is 100-400 μm.

A kind of preparation method of nanomaterial transmission electron microscope in-situ test chip of the present invention, its steps are:

Step 1, preparing a silicon substrate with a silicon dioxide layer on both sides, and growing a silicon nitride layer on both sides of the silicon substrate;

Step 2. Using a photolithography process, transfer the electrode pattern from the photolithography mask to the front side of the silicon substrate obtained in Step 1;

Step 3, using the micro-electromechanical processing technology to fabricate a metal film or device, or a semiconductor functional film or device on the front side of the silicon substrate obtained in step 2;

Step 4, using a photolithography process and a reactive ion etching process to etch a square window on the insulating layer on the back side of the silicon substrate obtained in step 3, and the square window is located on the central axis of the silicon substrate;

Step 5. Using photolithography and reactive ion etching to etch electron-beam-transmitting long holes or electron-beam-transmitting slots on the insulating layer on the front side of the silicon substrate obtained in step 4;

Step 6. Put the silicon substrate obtained in step 5 into a potassium hydroxide solution for wet etching until the silicon dioxide layer on the front side of the silicon substrate is etched to leave a film window, and take out the silicon substrate for cleaning;

Step seven, dicing the silicon substrate obtained in step six, and dividing it into independent chips.

The application of a nanometer material transmission electron microscope in-situ test chip of the present invention uses a micromanipulator to place a sample or utilizes a focused ion beam system to process and place a sample on the in-situ test chip, so that the sample and the metal film or device on the chip , or the semiconductor functional film or device is connected, and is located on the electron beam long hole or the electron beam long groove in the film window area; the test chip loaded with the sample is loaded into the sample rod and sent to the transmission electron microscope for observation, and the sample is applied Physical and chemical effects and receiving signals generated by the sample, and in-situ observation of the sample at atomic scale resolution.

Furthermore, after the transfer and fixation of the sample is completed on the in-situ test chip, the sample can be ion-cleaned and thinned in the ion thinning device.

3. Beneficial effect

Compared with the existing known technology, the technical solution provided by the invention has the following remarkable effects:

(1) A kind of in-situ testing chip of nanometer material transmission electron microscope of the present invention has adopted the long hole of electron beam of large aspect ratio or the long slot structure of electron beam at film window place, has given micromanipulator (micromanipulator) ) The needle tip has a large movable space along the direction of the electron beam long hole or the electron beam long slot, and at the same time allows the needle tip to move up and down through the electron beam long hole or the electron beam slot, so that the micromanipulator can be used to cooperate The optical microscope is used to transfer the sample, which reduces the use conditions and cost of the chip;

(2) A nanomaterial transmission electron microscope in-situ test chip of the present invention has a suitable aspect ratio of the electron beam slot or the electron beam slot, and is incident at a small angle along the electron beam slot or the electron beam slot direction. The ion beam can also be well transmitted, so the sample that has been transferred to the chip can be cleaned or thinned by using traditional ion thinning equipment, which can effectively remove the contamination caused by the sample transfer and fixation process, or cause damage to the sample. Continue processing to improve the effect of electron microscope observation.

(3) A nanomaterial transmission electron microscope in-situ test chip of the present invention has a simple manufacturing process and is suitable for mass production. Compared with existing chips, the cost of a single chip is significantly reduced, and has a wide range of applications, good use effects, and is easy to promote.

Description of drawings

Fig. 1 is the front structure schematic diagram of in-situ test chip among the present invention;

Fig. 2 is a partial enlarged view of the film window position in Fig. 1;

Fig. 3 is a schematic diagram of the back structure of the in-situ test chip in the present invention.

Explanation of the labels in the schematic diagram:

1. Square window; 2. Metal electrode; 3. Thin film window; 4. Electron beam transmission area.

Detailed ways

In order to further understand the content of the present invention, the present invention will be described in detail in conjunction with the accompanying drawings and embodiments.

Example 1

Referring to FIG. 1 , FIG. 2 and FIG. 3 , a nanomaterial transmission electron microscope in-situ electrical test chip of this embodiment includes a silicon substrate, an insulating layer, a film window 3 and an electron beam transmission region 4 . Specifically: the silicon substrate is a rectangular sheet with a thickness of 400 μm, and there are insulating layers on both sides of the silicon substrate, and the insulating layer includes a silicon dioxide layer grown on the silicon substrate and a silicon dioxide layer on the silicon dioxide layer. For the grown silicon nitride layer, the thickness of the silicon dioxide layer is 900nm, and the thickness of the silicon nitride layer is 200nm. On the front insulating layer of the silicon substrate, it is necessary to set metal thin films or devices that can apply various physical and chemical effects to the sample, or semiconductor functional thin films or devices. Referring to Fig. There is a metal electrode 2 growing on it, and the thickness of the metal electrode 2 is 150nm. The metal electrode 2 is mainly used for connecting with the lead wire on the sample rod of the transmission electron microscope. A film window 3 made of an insulating layer is opened in the center of the front surface of the silicon substrate, and the film window 3 is obtained by performing wet etching on the back surface of the silicon substrate.

In this embodiment, an electron beam-transmitting area 4 is provided in the center of the film window 3, and the electron beam and ion beams can pass through the electron beam-transmitting area 4, allowing the tip of the micromanipulator (micromanipulator) to move up and down and back and forth. Electron beam permeable slots or slots. Specifically, there is a long electron beam slot in the center of the film window 3 in this embodiment, and the part of the metal electrode 2 located on the film window 3 is distributed along both sides of the electron beam slot, and the electron beam slot extends To the edge of the film window 3, the length is 300 μm, and the width is 10 μm, which is used to transmit electron beams and ion beams.

The electrical test chip of this embodiment provides a plurality of metal electrodes 2 available for sample connection near the long groove region of the electron beam, so it can be used for metals, nanowires, nanotubes, two-dimensional materials, heterojunction interfaces and In-situ electrical testing of various samples such as bulk samples.

In addition, this embodiment adopts a large aspect ratio e-beam permeable long slot structure at the film window 3, so that the chip can be processed in the FIB equipped with a micro-manipulator, and then the micro-manipulator in the FIB can be used to complete the sample processing. The sample is placed across the electron beam-transmitting slot of the chip and connected to the metal electrode 2 by depositing a certain thickness of platinum, and then the chip is taken out and put into the transmission electron microscope. It is also possible to transfer the sample to the desired position through the micromanipulator in the laboratory environment, and then process it in the FIB or directly enter the transmission electron microscope for observation, which is more economical than the transfer of the micromanipulator in the conventional FIB system.

The inventor pointed out that the function of the electron beam-transmitting long slot is to allow the electron beam to pass through, and if it is too wide, smaller samples cannot be placed on the electron beam-transmitting slot, and if it is too narrow, the area that the electron beam can pass through becomes smaller. Observe the effect. If it is too short, it cannot give the micromanipulator (micromanipulator) the required range of motion for the needle tip, and if it is too long, it will affect the strength of the film window. Traditional in-situ test chips use micron-sized diameter circular through-holes, elliptical through-holes, or silicon nitride films with a thickness of less than 50nm to pass through the electron beam in the film window area. If a micromanipulator (micromanipulator) is used to transfer the sample, it cannot The space to move up and down is provided, so the focused ion beam system can only be used to transfer the sample, which limits the conditions of use and greatly increases the cost of use. At the same time, the small hole or film will block the obliquely incident ion beam, and the traditional film window structure cannot penetrate the ion beam incident at a small angle. It is thin, and the focused ion beam system cannot avoid contamination of the sample during sample transfer and fixation, which directly affects the observation effect.

The above-mentioned problems greatly restrict the application of the in-situ MEMS chip. In this embodiment, the length of the beam-transmitting slot is designed to be 300 μm and the width is 10 μm, so that the aspect ratio is 30. The use of long slots with a large aspect ratio to pass through the electron beam gives the tip of the micro-manipulator (micromanipulator) a large space for movement along the direction of the long slot through the electron beam, and at the same time allows the needle tip to pass through the electron beam The long slot moves up and down, so that the micromanipulator can be used to transfer the sample with the optical microscope, which reduces the use conditions and cost of the chip. And because the length-to-width ratio of the beam-transmitting long slot is appropriate, the ion beam incident at a small angle along the direction of the electron-beam slot can also be transmitted well, so the samples that have been transferred to the chip can be processed using traditional ion thinning equipment. Ion cleaning or thinning can effectively remove the pollution caused by the sample transfer and fixation process, or continue to process the sample to improve the observation effect of the electron microscope.

For the thin film window with large aspect ratio electron-beam-transmitting long slots compared with small holes, it is easy to cause the film to rupture along the electron-beam-transmitting long slot direction due to stress concentration. In this embodiment, silicon dioxide film layer and nitrogen The composite layer of the silicon oxide film layer constitutes the thin film window, and the strength of the thin film window is effectively improved by using the good strength of the silicon dioxide film layer and the stress regulation effect on the silicon nitride, thus solving the problem that the film is easy to break along the long groove direction of the electron beam. The problem.

In this embodiment, the process of preparing a nanomaterial transmission electron microscope in-situ electrical test chip is as follows:

(1) Prepare a Si (100) wafer (i.e., a silicon substrate) with a silicon dioxide layer on both sides, the size of the wafer is 2 inches, the thickness is 400um, and the thickness of the silicon dioxide layer is 900nm. Using plasma enhanced chemical vapor deposition (PECVD) to grow silicon nitride layers with a thickness of 200nm on both sides of the wafer, the growth temperature is 300°C, the flow rate of N ₂ is 900 sccm, and the flow rate of SiH ₄ is 25 sccm;

(2) Put the wafer produced in step (1) into a muffle furnace for annealing at 500°C for 1 hour, and cool with the furnace;

(3) Using the photolithography process, expose for 7s in the hard contact mode of the ultraviolet lithography machine, transfer the electrode pattern from the photolithography mask to the front side of the wafer produced in step (2), and then develop it in 3038 developer 45s, the photoresist used is AZ5214;

(4) Utilize electron beam evaporation to vapor-deposit a layer of Cr with a thickness of 5nm on the front of the wafer produced in step (3), and then vapor-deposit a layer of Au with a thickness of 100nm, and then place the wafer with the front facing up. Ultrasonic cleaning in acetone and isopropanol solutions, and finally cleaning with deionized water to remove the photoresist and leave the metal electrodes;

(5) Using the photolithography process, expose in the hard contact mode of the ultraviolet lithography machine for 7s, transfer the square window pattern from the photolithography mask to the back of the wafer produced in step (4), and then expose it in 3038 developer solution Develop for 45s, the photoresist used is AZ5214;

(6) Using reactive ion etching (RIE), etch a square window on the silicon nitride layer and silicon dioxide layer on the back of the wafer produced in step (5), and then place the back of the wafer upwards into acetone and isopropanol solutions for ultrasonic cleaning, and finally with deionized water to remove the photoresist; the square window 5 of this embodiment is located on the central axis of the wafer, specifically determined according to the supporting transmission electron microscope sample rod of the chip . Due to the etching angle of silicon wet etching, if the square window is too small, it will form a pyramid-shaped pit when it is etched to a certain depth and cannot be etched to the front side. If the window is too large, the film window on the front side will be too large and affect the film window. strength and stability. According to different substrate thicknesses, the size of the square window is determined by being able to etch to the front of the substrate so that the front film window is not larger than 2mm*2mm;

(7) Using the photolithography process, expose for 7s in the hard contact mode of the ultraviolet lithography machine, transfer the long groove pattern of the electron beam from the photolithography mask to the front side of the wafer produced in step (6), and then Develop in 3038 developer solution for 45s, the photoresist used is AZ5214;

(8) Utilize the reactive ion etching process (RIE), etch the electron beam-transmitting long slots on the silicon nitride layer and silicon dioxide layer on the front side of the wafer produced in step (7), and then place the front side of the wafer on the silicon nitride layer and silicon dioxide layer. Put it into acetone and isopropanol solution successively for ultrasonic cleaning, and finally clean it with deionized water to remove the photoresist;

(9) Put the back of the wafer produced in step (8) upward into a potassium hydroxide solution with a mass percentage concentration of 20% for wet etching. Leaving the film window, remove the wafer for cleaning.

(10) Scribing the wafer produced in step (9) into individual chips.

In this embodiment, the process of manufacturing nanomaterial TEM in-situ electrical test chips is simple, suitable for mass production, the cost of a single chip is significantly lower than that of existing chips, and it has a wide range of applications. The sample can be placed using a micromanipulator in a laboratory environment, or it can be processed and placed using a focused ion beam system so that the sample is connected to the electrodes on the chip and located in the thin film window area that is transparent to the electron beam. Install the sample-loaded chip into the sample rod that can provide multiple electrical channels and send it to the transmission electron microscope for observation. By applying electrical action to the sample or receiving the electrical signal of the sample, the electrical in-situ observation of the sample can be realized at atomic scale resolution. At the same time, after the transfer and fixation of the sample is completed, the chip can perform ion cleaning and thinning on the sample in the ion thinning equipment, which can effectively reduce the pollution of the sample during the processing and improve the observation effect of the electron microscope.

The following describes the specific process of preparing and transferring heterojunction interface samples using the focused ion beam system (FIB) and further processing the samples using ion thinning equipment:

(1) Put the grown substrate with heterojunction structure, the half sub-carrier grid and the chip prepared in this embodiment into the cavity of the focused ion beam system, and cut out a size on the substrate with the focused ion beam. The prototype of the heterojunction interface sample is about 20 μm × 10 μm × 3 μm.

(2) Use the micromanipulator needle tip in the FIB to connect the sample prototype by depositing a certain thickness of platinum, lift the sample prototype and transfer it to the half-split net, and deposit a certain thickness of platinum to connect the sample prototype to the half-split net, Then use the focused ion beam to desolder the tip of the micromanipulator from the prototype of the sample. Focused ion beam thinning is performed on the prototype of the sample on a half-split grid to obtain a heterojunction interface sample with a thin region.

(3) Connect the tip of the micromanipulator with the thinned sample by depositing a certain thickness of platinum, and then use the focused ion beam to desolder the sample from the half-divided carrier net, and transfer the sample to the electron beam of the chip through the micromanipulator The position of the long groove is in contact with the required electrodes, and the sample is desoldered from the tip of the micromanipulator through the focused ion beam. A certain thickness of platinum is deposited at the contact position between the sample and the electrode for welding, which can not only fix the sample, but also ensure a good electrical connection between the sample and the electrode.

(4) Take out the chip containing the sample from the FIB system, put it into the ion thinning equipment (such as PIPS), adjust the relative angle between the chip and the upper ion gun until the incident direction of the ion beam is consistent with the direction of the long groove of the electron beam, and the ions The beam can bombard the sample from above at a small angle. Since the ion beam enters the sample position from above at a small angle (1 to 5°), the ion beam spot on the sample plane is actually a long strip, which will fall on the long slot of the electron beam, so that the ions that have not irradiated the sample can be seen. Pass through the long slot for the electron beam to avoid damage to the film window of the chip. Fix the position of the chip, turn off the lower ion gun, select an appropriate beam size, and turn on the upper ion gun to clean the sample with ions.

(5) After the ion cleaning is completed, take out the chip from the ion thinning equipment, put it into the sample rod of the transmission electron microscope, connect it with the electrical measurement equipment, and then enter the transmission electron microscope for in-situ observation and testing.

Example 2

A nanomaterial transmission electron microscope in-situ electrical test chip and its preparation method in this embodiment are basically the same as in Embodiment 1, except that the thickness of the silicon substrate in this embodiment is 300 μm, and the metal electrodes are located on the film window. Some are distributed along one side of the electron beam-transmitting long groove, the length of the electron-beam transmitting long groove is 300 μm, and the width is 10 μm. The thickness of the metal electrode is 50nm, the thickness of the silicon dioxide layer in the insulating layer is 200nm, and the thickness of the silicon nitride layer is 5nm.

In this embodiment, the process of using the in-situ electrical test chip to transfer the nanowire sample in the laboratory using a micromanipulator (micromanipulator) is as follows:

(1) Under an optical microscope, a nanowire sample with a length of about 20 microns is picked up with the tip of a micromanipulator. Since the micromanipulator is made of glass, the sample can be stably attached to the tip of the micromanipulator through the van der Waals force between the sample and the sample after being picked up. The micromanipulator only needs an optical microscope and a manual micromanipulator system to work. Compared with the focused ion beam system, it has the characteristics of convenient operation, easy equipment, and low cost of use.

(2) Move the needle tip of the micromanipulator to the top of the long electron beam slot on the chip so that the needle tip of the micromanipulator is flush with the long slot of the electron beam. The angle between the micromanipulator and the upper surface of the chip is 10 to 45° (micro manipulation good working angle of the hand).

(3) Move the needle tip of the micromanipulator along the direction of the electron beam long groove to the position where there are electrodes on both sides of the electron beam long groove. Since the diameter of the micromanipulator needle tip is only a few microns, which is smaller than the 10 μm diameter of the electron beam long groove Width, so the height of the tip of the micromanipulator can be reduced so that the tip passes through the long slot through which the electron beam passes. Traditional chips only have circular or elliptical through-holes or no through-holes in the film window area, and use silicon nitride films below 50nm to transmit electron beams, so they cannot allow the needle tip of the micro-manipulator to pass through, so it cannot be completed by the micro-manipulator. Sample transfer.

(4) The nanowire sample attached to the needle tip of the micromanipulator will be blocked by the long slot of the electron beam because the length is greater than the width of the long slot of the electron beam, so that it remains on the electrode of the chip and is connected to the chip by van der Waals force.

(5) Put the sample into the sample rod, and then enter the transmission electron microscope for in-situ observation and testing.

Example 3

A nanomaterial transmission electron microscope in-situ electrical test chip and its preparation method in this embodiment are basically the same as in Embodiment 1, except that the thickness of the silicon substrate in this embodiment is 200 μm, and the metal electrodes are located on the film window. Parts are distributed along both sides of the electron beam-transmitting long groove, the length of the electron-beam transmitting long groove is 320 μm, and the width is 8 μm. The thickness of the metal electrode is 200nm, the thickness of the silicon dioxide layer in the insulating layer is 1000nm, and the thickness of the silicon nitride layer is 150nm.

Example 4

A nanomaterial transmission electron microscope in-situ electrical test chip and its preparation method in this embodiment are basically the same as in Embodiment 1, the difference is that the thickness of the silicon substrate in this embodiment is 300 μm, and the film window has a transparent electron For beam slots, the part of the metal electrode located on the film window is distributed along one side of the electron beam slots. The length of the slots for electron beam slots is 400 μm and the width is 20 μm. The thickness of the metal electrode is 150nm, the thickness of the silicon dioxide layer in the insulating layer is 800nm, and the thickness of the silicon nitride layer is 120nm.

Example 5

A nanomaterial transmission electron microscope in-situ electrical test chip and its preparation method in this embodiment are basically the same as in Embodiment 1, the difference is that in this embodiment, there are long holes through the electron beam in the film window, and the electron beam through The length of the long hole is 100 μm, the width is 5 μm, the thickness of the silicon dioxide layer in the insulating layer is 900 nm, and the thickness of the silicon nitride layer is 160 nm.

Example 6

A nanomaterial transmission electron microscope in-situ thermal test chip and its preparation method in this embodiment are basically the same as in Embodiment 1, except that the thickness of the silicon substrate in this embodiment is 200 μm, and a layer of 50 nm is grown on the film window. Thick silicon carbide (SiC) layer, this embodiment grows a layer of silicon carbide (SiC) film on the insulating layer (specifically on the film window). Since silicon carbide (SiC) is a semiconductor, it can generate heat by providing an electric current. Therefore, the sample placed on it can be heated, and the heating temperature can be changed by adjusting the current input to the silicon carbide film to heat the sample.

The above schematically describes the present invention and its implementation, which is not restrictive, and what is shown in the drawings is only one of the implementations of the present invention, and the actual structure is not limited thereto. Therefore, if a person of ordinary skill in the art is inspired by it, without departing from the inventive concept of the present invention, without creatively designing a structural mode and embodiment similar to the technical solution, it shall all belong to the protection scope of the present invention .

Claims (6)

1. a nanometer material transmission electron microscope in-situ testing chip, comprises silicon substrate and insulating layer, is characterized in that: also comprises film window (3), and described silicon substrate both sides is all provided with insulating layer, and described insulating layer The layer comprises a silicon dioxide layer grown on a silicon substrate and a silicon nitride layer grown on the silicon dioxide layer, the thickness of the silicon dioxide layer is 200-1000nm, and the thickness of the silicon nitride layer is 5-200nm; and the silicon The front side of the substrate is provided with a thin film window (3) made of an insulating layer, and the thin film window (3) is provided with a long hole for transmitting electron beams or a long slot for transmitting electron beams. The width is 5-20 μm, and the length of the electron beam-transmitting long hole or the electron-beam-transmitting slot is 100-400 μm; the insulating layer on the front side of the silicon substrate is provided with a metal film or device, or a semiconductor functional film or device. 2. A kind of in-situ test chip of nanometer material transmission electron microscope according to claim 1, it is characterized in that: the part of described metal thin film or device, semiconductor functional thin film or device is located on the thin film window (3) passes through electron beam Distributed on one or both sides of the long hole or the long slot through the electron beam. 3. A nanomaterial transmission electron microscope in-situ test chip according to claim 2, characterized in that: the thickness of the silicon substrate is 100-400 μm. 4. a preparation method of nanomaterial transmission electron microscope in-situ test chip as claimed in claim 3, its steps are: Step 1, preparing a silicon substrate with a silicon dioxide layer on both sides, and growing a silicon nitride layer on both sides of the silicon substrate; Step 2. Using a photolithography process, transfer the electrode pattern from the photolithography mask to the front side of the silicon substrate obtained in Step 1; Step 3, using the micro-electromechanical processing technology to fabricate a metal film or device, or a semiconductor functional film or device on the front side of the silicon substrate obtained in step 2; Step 4. Using the photolithography process and reactive ion etching process, etch a square window (1) on the insulating layer on the back side of the silicon substrate obtained in step 3, the square window (1) is located on the central axis of the silicon substrate ; Step 5. Using photolithography and reactive ion etching to etch electron-beam-transmitting long holes or electron-beam-transmitting slots on the insulating layer on the front side of the silicon substrate obtained in step 4; Step 6. Put the silicon substrate obtained in step 5 into a potassium hydroxide solution for wet etching until the silicon dioxide layer on the front side of the silicon substrate is etched to leave a film window (3), take out the silicon substrate and clean it ; Step seven, dicing the silicon substrate obtained in step six, and dividing it into independent chips. 5. An application of nanomaterial transmission electron microscope in-situ test chip as claimed in claim 3, characterized in that: use a micromanipulator to place a sample or utilize a focused ion beam system to process and place a sample on a test chip, so that the sample It is connected to the metal thin film or device on the chip, or the semiconductor functional thin film or device, and is located on the long hole through the electron beam or the long slot through the electron beam in the area of the film window (3); the test chip loaded with the sample is loaded into the sample rod The transmission electron microscope is sent to the sample for observation, the sample is subjected to physical and chemical effects and the signal generated by the sample is received, and the sample is observed in situ under atomic scale resolution. 6. The application of a nanomaterial transmission electron microscope in-situ test chip according to claim 5, characterized in that: after the in-situ test chip completes the transfer and fixation of the sample, the sample can be ion-cleaned and cleaned in the ion thinning device. thinning.