CN115274478B - Device and method for realizing interface chemical reaction between hard abrasive and substrate at nanoscale - Google Patents

Abstract

The invention discloses a device and a method for realizing interface chemical reaction of a hard abrasive and a substrate under a nanometer scale, wherein the device comprises a liquid-gas module, a temperature control module and a main shaft module, the liquid-gas module is used for containing different liquid-gas media in a liquid-gas tank, the temperature control module comprises a heating device and a cooling device, the main shaft module comprises a standard nanometer scratch device with pressure control, an optical lens, a conversion disc and a motion device, the optical lens is used for searching the scratch position on the substrate, the standard nanometer scratch device is used for applying different loads on the substrate and scratching, the conversion disc is used for switching the optical lens and a nanometer scratch pressure head, the temperature control module is used for controlling different temperatures, so that the nanometer scratch pressure head scratches on the surface of the substrate at a low speed under different temperatures, liquid-gas media and/or load conditions, the device is beneficial to observing the nanometer scale interface chemical reaction between the hard abrasive and the substrate under the action of different media, and the device has good application prospect in the field of ultra-precision processing of semiconductors.

Description

Device and method for realizing interface chemical reaction between hard abrasive and substrate at nanoscale

Technical Field

The invention relates to the field of ultra-precision processing of semiconductor wafers, in particular to a device and a method for realizing interface chemical reaction between hard abrasive and substrate at nanometer scale.

Background technique

The third-generation semiconductor materials have the characteristics of wide bandgap, high breakdown electric field, high thermal conductivity, high saturated electron mobility and smaller volume, and have huge application potential in high temperature, high frequency, high power, optoelectronics and radiation-resistant devices. Therefore, new semiconductor materials are also rapidly applied to emerging industries such as 5G communications, new energy vehicles, and smart grids. Among them, silicon carbide and gallium nitride are representatives of new semiconductor materials.

However, the new semiconductor material has extremely high hardness, very stable chemical properties, and overall great hardness and brittleness, which makes it extremely difficult to process semiconductor wafers ultra-precision. The traditional processing technology for processing new semiconductor materials has poor surface quality, low efficiency, and high cost. In addition, the chemical reagents used in the traditional process will also cause great pollution to the environment. In order to improve processing efficiency, improve the surface quality of wafers, and reduce environmental pollution, it is necessary to deeply analyze the interface process between nano-abrasives and wafers, which will help to master the abrasive polishing and removal mechanism of new semiconductor wafers, and then realize efficient, green, ultra-precision and damage-free processing of new semiconductor wafers.

Due to the high hardness, brittleness and chemical stability of hard and brittle materials, the processing surface is easily damaged and the interface reaction is difficult. The processing bottleneck can be broken through by studying the interface reaction process between abrasive grains and wafers. Existing literature searches have found that the current research on interface reaction is mainly aimed at the macroscopic level of materials. For example, the patent: "Device for realizing friction chemical reaction between abrasive and wafer substrate (CN214923387U)" proposes a device for realizing friction chemical reaction between abrasive grains and wafer substrates under high speed and lubricating medium. Although the interface action relationship between hard abrasive and wafer in the close processing process is revealed by scratching speed, lubrication state and load, the device cannot study the interface chemical action relationship at the nanoscale at low speed. "A vacuum high temperature reciprocating friction and wear test system (CN112945844A)" proposes a vacuum high temperature reciprocating friction and wear tester. Although the tribological properties of materials are tested under vacuum and high temperature environment with heavy load, it has certain limitations and cannot actually simulate the action of materials under various media, and cannot accurately study the chemical reaction at the nanoscale. There are also some that focus on the microscopic level of materials, such as "A Micro-Nano Scratch Instrument and Its Application Method (CN106840929A)", which proposes an observable micro-nano scratch instrument. Although it can accurately study the nanoscale performance of materials, it cannot study the interface effects under different liquid and gas media. Existing research methods use nanoindentation scratch instruments to explore nanoscale interface effects. However, due to the lack of sufficient processing conditions, such as different liquid and gas media conditions at different temperatures, it is difficult to achieve the effect of studying the interface effects at the nanoscale.

Summary of the invention

In view of the current difficulties in exploring the interfacial chemical reactions of substrate materials at nanoscale at extremely low speeds and exploring the properties of substrate materials under different environments (temperature, liquid phase, and gas phase combined), the embodiments of the present application propose a device and a method for realizing the interfacial chemical reactions between hard abrasives and substrates at nanoscale to solve the above problems.

In order to achieve the above purpose, the technical solution of the present invention is:

A device for realizing interfacial chemical reaction between hard abrasive and substrate at nanoscale, comprising a liquid-gas module, a temperature control module and a spindle module, wherein the liquid-gas module comprises a liquid-gas box, a sealing cover, an air inlet, an air outlet, a water inlet and a water outlet, the sealing cover is arranged on the liquid-gas box and is sealed and connected to the liquid-gas box, a sample stage is arranged in the liquid-gas box, the air inlet, the air outlet, the water inlet and the water outlet are connected to the liquid-gas box so that different liquid-gas media exist in the liquid-gas box, the temperature control module comprises a heating device and a cooling device, the heating device is connected to the sample stage, the cooling device is connected to the heating device and the sample stage, the spindle module comprises a standard nano scratch device with pressure control, an optical lens, a conversion disk and a motion device, the motion device comprises an XY axis motion device and a Z axis motion device The invention discloses a device, a Z-axis motion device is connected with a sealing cover, an XY-axis motion device is connected with the Z-axis motion device, a standard nano scratch device and an optical lens are installed on a conversion disk, a nano scratch indenter is arranged on the standard nano scratch device, the conversion disk is fixed at the lower end of the XY-axis motion device, and the nano scratch indenter and the optical lens are moved in the XYZ direction, a substrate is fixed on a sample stage, the optical lens is used to find a scratching position on the substrate, the standard nano scratch device is used to apply different loads on the substrate and scratch it, the conversion disk is used to switch the optical lens and the nano scratch indenter, and a temperature control module is used to control different temperatures, and the nano scratch indenter is used to scratch the substrate surface at a low speed under different temperatures, liquid-gas media and/or load conditions.

Preferably, the liquid-gas module further comprises a sealing gasket and a fixing ring. The sealing gasket is arranged between the sealing cover and the liquid-gas box and between the sample table and the liquid-gas box. The fixing ring is fixed to the sealing cover with a hexagonal screw.

Preferably, the liquid-gas box is a closed container in the shape of a rectangular parallelepiped, with a length of 120 mm, a width of 100 mm, a height of 110 mm, and is made of stainless steel.

Preferably, the sample stage is connected to the liquid-gas box through a threaded seal, and the substrate is adhered to the sample stage by using hot melt adhesive.

Preferably, the air inlet and the air outlet are arranged above the water inlet and the water outlet, the air inlet is connected to an air inlet pipe to allow the gas medium to pass through, the water inlet is connected to a water inlet pipe to allow the liquid medium to pass through, the air outlet is connected to an air outlet pipe to extract gas, and the water outlet is connected to a water outlet pipe to discharge waste liquid.

Preferably, the liquid medium in the liquid-gas medium is a weakly acidic, weakly alkaline or neutral medium with a pH of 5-9, and the gas medium is air, oxygen and carbon dioxide.

Preferably, the heating device can heat the sample stage at a temperature of 40-80° C., and the cooling device uses liquid cooling to cool the heating device and the sample stage.

Preferably, a standard nano scratch device is fixed under the conversion disk and a load is applied, the load control accuracy is 0.1mN, and the range is 0.1mN-500mN. After loading, the nano scratch indenter forms scratches on the substrate in a constant direction at a scratching speed of 1-100μm/s through an XY axis motion device.

Preferably, the nano scratch indenter is a hard abrasive, the curvature of the nano scratch indenter is 1-50 μm, the hard abrasive includes diamond, aluminum oxide, cubic boron nitride or boron carbide, and the substrate is a hard and brittle material, including diamond, gallium nitride, gallium oxide, sapphire or silicon carbide.

A method for realizing the device for realizing the interface chemical reaction between the hard abrasive and the substrate at the nanoscale comprises the following steps:

1) Fix the sample stage with the substrate attached to it in the liquid-gas box through threaded connection, and fix the sealing gasket between the sample stage and the liquid-gas box;

2) Fix the spindle module on the sealing cover, fix the sealing cover on the liquid-gas tank through threads, fix the sealing gasket between the sealing cover and the liquid-gas tank, and fix the fixing ring on the sealing cover with hexagonal screws;

3) Using an optical lens to find a scratching position on the substrate, setting a certain load, speed, vacuum degree, gas medium, liquid medium and temperature at the scratching position, converting the optical lens into a nano scratch indenter through a conversion disk, and scratching the substrate surface with the nano scratch indenter;

4) Open the sealing cover, take out the sample stage, place the scratched substrate on an X-ray photoelectron spectrometer, observe the surface state of the scratched substrate, and detect the chemical composition of the scratched surface of the substrate.

Compared with the prior art, the present invention has the following beneficial effects:

The present invention uses a heating device to conduct nano-scratch experiments on hard abrasive indenters and substrates under different liquid-gas medium environments, effectively making up for the shortcomings of existing nano-scratch instruments, and by combining heating, liquid, and gas, the temperature and liquid/gas medium conditions in the processing process are restored, which is consistent with the actual processing conditions, and helps to reveal the mechanism of the interface chemical reaction between the hard abrasive and the substrate at the nanoscale. Then, the scratch area on the sample surface is tested for chemical composition by an X-ray photoelectron spectrometer, so as to determine the interface chemical reaction mechanism at the nanoscale between the hard abrasive and the substrate. The implementation device is simple and easy to operate, effectively making up for the shortcomings of existing nano-scratch instruments, and by combining heating, liquid, and gas, it is consistent with the actual processing conditions, and helps to reveal the mechanism of the interface chemical reaction at the nanoscale between the hard abrasive and the substrate under the assistance of different media, and has good application prospects in the field of efficient ultra-precision processing of semiconductor wafer substrates.

BRIEF DESCRIPTION OF THE DRAWINGS

The accompanying drawings are included to provide a further understanding of the embodiments and are incorporated into and constitute a part of this specification. The accompanying drawings illustrate the embodiments and are used together with the description to explain the principles of the present invention. It will be easy to recognize other embodiments and many expected advantages of the embodiments because they become better understood by reference to the following detailed description. The elements of the accompanying drawings are not necessarily to scale with each other. The same reference numerals refer to corresponding similar parts.

FIG1 is a cross-sectional view of a device for realizing interfacial chemical reaction between a hard abrasive and a substrate at the nanoscale according to an embodiment of the present application;

FIG2 is a top view of a device for realizing interfacial chemical reaction between a hard abrasive and a substrate at the nanoscale according to an embodiment of the present application;

FIG3 is an exploded view of a device for realizing interfacial chemical reaction between a hard abrasive and a substrate at the nanoscale according to an embodiment of the present application;

FIG4 is a perspective view of a device for realizing interfacial chemical reaction between a hard abrasive and a substrate at the nanoscale according to an embodiment of the present application;

FIG5 is a schematic diagram and a physical diagram of a nano-scratch indenter of a device for realizing an interfacial chemical reaction between a hard abrasive and a substrate at the nanoscale according to an embodiment of the present application, wherein FIG5 (a) is a schematic diagram and FIG5 (b) is a physical diagram;

FIG6 is a schematic diagram of a nano scratch indenter of an apparatus for realizing an interface chemical reaction between a hard abrasive and a substrate at the nanoscale according to an embodiment of the present application scratching a substrate surface;

FIG7 is a first detection result of scratching the surface of a silicon carbide substrate by a nano-scratch indenter of the device for realizing the interface chemical reaction between a hard abrasive and a substrate at the nanoscale according to an embodiment of the present application;

FIG8 is a first diagram showing the scratch detection result of the nano scratch indenter of the device for realizing the interface chemical reaction between the hard abrasive and the substrate at the nanoscale according to the embodiment of the present application on the surface of the silicon carbide substrate.

Figure numerals: 1. Hexagon screw; 2. Fixing ring; 3. Hexagon nut; 4. First sealing gasket; 5. Sealing cover; 6. Z-axis motion device; 7. XY motion device housing; 8. X-axis motion device; 9. Y-axis motion device; 10. Spindle rod; 11. Bearing; 12. Conversion disk; 13. Second sealing gasket; 14. Sample table; 15. Condensation water inlet pipe; 16. Heating device; 17. Cooling device; 18. Temperature control device cover; 19. Hexagon screw and bolt; 20. Heat-resistant pipe; 23. Liquid-gas box; 21. Air inlet pipe; 24. Air outlet pipe; 22. Water inlet pipe; 25. Water outlet pipe; 26. Condensation water outlet pipe.

Detailed ways

The present application will be further described in detail below in conjunction with the accompanying drawings and embodiments. It is to be understood that the specific embodiments described herein are only used to explain the relevant invention, rather than to limit the invention. It should also be noted that, for ease of description, only the parts related to the relevant invention are shown in the accompanying drawings.

It should be noted that, in the absence of conflict, the embodiments and features in the embodiments of the present application can be combined with each other. The present application will be described in detail below with reference to the accompanying drawings and in combination with the embodiments.

Referring to FIGS. 1-4 , an embodiment of the present invention provides a device for realizing the interfacial chemical reaction between a hard abrasive and a substrate at the nanoscale, comprising a liquid-gas module, a temperature control module and a spindle module, wherein the liquid-gas module comprises a liquid-gas box 23, a sealing cover 5, an air inlet, an air outlet, a water inlet and a water outlet, the sealing cover 5 being arranged on the liquid-gas box 23 and being sealedly connected to the liquid-gas box 23, the liquid-gas box 23 being provided with an inner sample stage 14, the air inlet, the air outlet, the water inlet and the water outlet being connected to the liquid-gas box 23 so that different liquid-gas media exist in the liquid-gas box 23, and the temperature control module comprises a heating device 16 and a cooling device 17, the heating device 16 is connected to the sample stage 14, the cooling device 17 is connected to the heating device 16 and the sample stage 14, the spindle module includes a standard nano scratch device with pressure control, an optical lens, a conversion disk 12 and a motion device, the motion device includes an XY axis motion device and a Z axis motion device 6, the XY axis motion device includes an X axis motion device 8 and a Y axis motion device 9, the X axis motion device 8 is connected to the Y axis motion device 9 and is connected to the Z axis motion device 6, so as to realize the movement of the standard nano scratch device and the optical lens within a certain range in the XYZ direction. The Z-axis motion device 6 is connected to the sealing cover 5, and the standard nano-scratch device and the optical lens are installed on the conversion disk 12. The standard nano-scratch device is provided with a nano-scratch indenter. The conversion disk 12 is fixed to the lower end of the XY-axis motion device to realize the movement of the nano-scratch indenter and the optical lens in the XYZ direction. The substrate is fixed on the sample stage 14. The optical lens is used to find the scratching position on the substrate. The standard nano-scratch device is used to apply different loads on the substrate and scratch it. The conversion disk 12 is used to switch the optical lens and the nano-scratch indenter. The temperature control module is used to control different temperatures to realize the nano-scratch indenter scratching the substrate surface at low speed under different temperatures, liquid-gas media and/or load conditions. By adjusting different temperatures, liquid-gas media, and loads, the substrate surface of the hard and brittle material can be scratched with hard abrasive at low speed, and then the scratched substrate is taken out and placed on an X-ray photoelectron spectrometer to observe the chemical state changes at the scratches on the substrate surface.

In a specific embodiment, the liquid-gas module further includes a sealing gasket and a fixing ring 2, which are arranged between the sealing cover 5 and the liquid-gas box 23 and between the sample stage 14 and the liquid-gas box 23 to ensure the sealing of the liquid-gas box 23. The sealing gasket is made of polytetrafluoroethylene filled with carbon fiber. The fixing ring 2 is fixed to the sealing cover 5 with a hexagonal screw 1. The liquid-gas box 23 is a closed container in the shape of a rectangular parallelepiped, with a length of 120 mm, a width of 100 mm, and a height of 110 mm. The material is stainless steel, and the standard nano scratch device and the sample stage 14 can be sealed in a normal liquid-gas environment or a vacuum liquid-gas environment.

In a specific embodiment, the sample stage 14 is connected to the liquid-gas box 23 by threaded sealing, and the substrate is adhered to the sample stage 14 by hot melt adhesive. The heating device 16 can heat the sample stage 14. The heating device 16 adopts a laser heating module, and the heating temperature is 40-80°C. The cooling device 17 uses liquid cooling to cool the heating device 16 and the sample stage 14. The laser heating peripheral cooling device 17 is externally connected to the condensation water outlet pipe 26. Deionized water is used as the coolant. The condensation water inlet pipe 15 is passed through the deionized water, and the water outlet pipe 25 discharges the deionized water, forming a condensation water reflux to achieve cooling.

In a specific embodiment, the air inlet and the air outlet are arranged above the water inlet and the water outlet, the air inlet is connected to an air inlet pipe 21, through which a gas medium can be introduced, the water inlet is connected to an water inlet pipe 22, through which a liquid medium can be introduced, the air outlet is connected to an air outlet pipe 24, for extracting gas, and the water outlet is connected to an outlet pipe 25, for discharging waste liquid. Referring to Figures 5 and 6, the liquid medium in the liquid-gas medium is a weakly acidic, weakly alkaline or neutral medium, with a pH of 5-9, and the gas medium is air, oxygen and carbon dioxide. A certain vacuum degree can also be set, such as a vacuum degree set to ^10-3 Pa, with an accuracy of ± ^10-5 Pa. Therefore, different liquid-gas media can be provided, so that the nano scratch indenter can be scratched under different liquid-gas media.

In a specific embodiment, the nano scratch indenter is fixed on a standard nano scratch device with a pressure sensor, which can control the load with an accuracy of 0.1mN and a range of 0.1mN-500mN. After loading, the nano scratch indenter forms scratches on the substrate at a certain speed in a constant direction through an XY axis motion device 9. Specifically, the nano scratch indenter is a hard abrasive, and the curvature of the nano scratch indenter is 1-50μm. The hard abrasive includes diamond, aluminum oxide, cubic boron nitride or boron carbide. The load applied to the nano scratch indenter is 0.1-500mN, and the scratching speed is 1-100μm/s. The substrate is a hard and brittle material, and the substrate includes diamond, gallium nitride, gallium oxide, sapphire or silicon carbide. The substrate can be irregular in shape, with a fixed circular size of 5-30mm. The brand of the X-ray photoelectron spectrometer is: PHI Quantera II, which is a device that can characterize the information of different elements with information of binding energy, and can realize the chemical state detection of the metamorphic layer at the scratch.

The installation process of the device for realizing the interface chemical reaction between the hard abrasive and the substrate at the nanoscale in the embodiment of the present application is as follows:

First, install the bearing 11 in the conversion disk 12, install the spindle rod 10 on the conversion disk 12, install the X-axis motion device 8, the Y-axis motion device 9, and the XY motion device housing 7 on the spindle rod 10, install the Z-axis motion device 6 on the XY motion device housing 7, and install the sealing cover 5 on the Z-axis motion device 6.

First, place the second sealing gasket 13 in the groove of the sample table 14, fix the sample table 14 on the liquid-gas box 23 by bolt sealing connection, and use hot melt adhesive to stick the substrate on the sample table 14; fix the heating device 16 under the sample table 14, connect the cooling device 17 to the heating device 16, connect the condensation water inlet pipe 15 and the condensation water outlet pipe 26 to the cooling device 17, connect the heat-resistant pipe 20 to the heating device 16, and connect the temperature control device cover 18 to the liquid-gas box 23 by hexagonal screws and bolts 19.

Install the sealing cover 5 on the liquid-gas tank 23, place the first sealing gasket 4 in the groove of the sealing cover 5, connect the fixing ring 2 to the liquid-gas tank 23 through the hexagonal screw bolt 19, fix the hexagonal nut 3 under the hexagonal screw 1, and then install the air inlet pipe 21 and the air outlet pipe 24 on the liquid-gas tank 23, and install the water inlet pipe 22 and the water outlet pipe 25 on the liquid-gas tank 23; after installing the spindle module, the temperature control module, and the liquid-gas module, fix the nano scratch indenter and the optical lens on the conversion disk 12.

The embodiment of the present application further proposes a method for realizing the device for realizing the interfacial chemical reaction between the hard abrasive and the substrate at the nanoscale, comprising the following steps:

1) The sample stage 14 with the substrate attached thereto is fixed in the liquid-gas box 23 by threaded connection, and a sealing gasket is fixed between the sample stage 14 and the liquid-gas box 23;

2) Fix the spindle module on the sealing cover 5, fix the sealing cover 5 on the liquid-gas tank 23 through threads, fix the sealing gasket between the sealing cover 5 and the liquid-gas tank 23, and fix the fixing ring 2 on the sealing cover 5 with the hexagonal screw 1;

3) Using an optical lens to find a scratching position on the substrate, setting a certain load, speed, vacuum degree, gas medium, liquid medium and temperature at the scratching position, converting the optical lens into a nano scratch indenter through a conversion disk 12, and scratching the substrate surface with the nano scratch indenter;

4) Open the sealing cover 5, take out the sample stage 14, place the scratched substrate on an X-ray photoelectron spectrometer, observe the surface state of the scratched substrate, and detect the chemical composition of the scratched surface of the substrate.

The technical solution of the present invention is further explained below through specific embodiments.

Example 1

(1) First, prepare a group of 10mm×10mm single crystal silicon carbide samples, load the samples into the implementation device, observe the samples through the optical lens, set five groups of scratching positions, and the scratching parameters are all set to set the load applied by the nano scratch indenter to 45mN, the speed of the nano scratch indenter to 1μm/s, select deionized water as the lubricant, PH=7, and set the air to flow; connect the temperature control device on the sample stage, set the sample stage to 35℃ for the first group, 40℃ for the second group, 60℃ for the third group, 80℃ for the fourth group, and 85℃ for the fifth group, with a temperature control accuracy of ±0.5℃. After the scratching parameters are set, the conversion disk turns the nano scratch indenter to the sample, and the force sensor automatically contacts the scratching position. When the pressure reaches the set value, the system starts to operate. After completing the experiment according to the set parameters, take out the sample.

(2) The five groups of scratches obtained in step (1) were subjected to chemical composition detection of the scratched areas on the surface of silicon carbide using an X-ray photoelectron spectrometer. The scratch results of the first and fifth groups are shown in FIG7 . The XPS fine spectrum was peaked. There were two peaks in the Si2p peak diagram of FIG7 , where 100.3 eV corresponds to the peak position of silicon carbide, and 101.6 eV corresponds to the peak position of Si-N. The scratch results of the second, third, and fourth groups are shown in FIG8 . There were three peaks in the Si2p peak diagram of FIG8 , where 100.2 eV corresponds to the peak position of silicon carbide, 101.5 eV corresponds to the peak position of Si-N, and 102.7 eV corresponds to the peak position of silicon dioxide. When the temperature is lower than 40℃, single crystal silicon carbide does not react. However, between 40℃ and 80℃, deionized water induces single crystal silicon carbide to undergo interfacial chemical reaction through mechanical force. When the temperature is higher than 80℃, deionized water easily vaporizes to form water vapor and cannot react. This indicates that the diamond abrasive and silicon carbide wafer undergo interfacial chemical reaction induced by mechanical force in the presence of deionized water as lubricant, at a temperature between 40℃ and 80℃, and in an air environment. Single crystal silicon carbide undergoes amorphization transformation under stress, and then amorphous silicon carbide undergoes interfacial chemical reaction with high-temperature water molecules to generate amorphous silicon oxide.

Example 2

(1) First, prepare a group of 10mm×10mm single crystal silicon carbide samples, load the samples into the implementation device, observe the samples through the optical lens, set three groups of scratching positions, and the scratching parameters are all set to set the load applied by the nano scratch indenter to 45mN, the speed of the nano scratch indenter to 1μm/s, the first group selects HCl solution as the lubricant, PH=5; the second group selects _H2O2 solution as the lubricant, PH=9; the third group selects _deionized water as the lubricant, PH=7; set the air to flow, connect the temperature control device on the sample stage, and set the sample stage to 25℃ for the first, second and third groups, with a temperature control accuracy of ±0.5℃. After the scratching parameters are set, the conversion disk turns the nano scratch indenter to the sample, and the force sensor automatically contacts the scratching position. When the pressure reaches the set value, the system starts to operate. After completing the experiment according to the set parameters, take out the sample.

(2) The three groups of scratches obtained in step (1) were used to detect the chemical composition of the scratched area on the silicon carbide surface using an X-ray photoelectron spectrometer. The scratch results of the third group are shown in Figure 7. The XPS fine spectrum was peaked. There were two peaks in the Si2p peak diagram of Figure 7, of which 100.3eV corresponds to the peak position of silicon carbide, and 101.6eV corresponds to the peak position of Si-N. The scratch results of the first and second groups are shown in Figure 8. There are three peaks in the Si2p peak diagram of Figure 8, of which 100.2eV corresponds to the peak position of silicon carbide, 101.5eV corresponds to the peak position of Si-N, and 102.7eV corresponds to the peak position of silicon dioxide. At 25°C, deionized water cannot react with single-crystal silicon carbide, while single-crystal silicon carbide obviously reacts to generate silicon dioxide under HCl solution and H ₂ O ₂ solution. It shows that the diamond abrasive and the silicon carbide wafer react with each other at an interface chemical reaction at 25°C in an air environment under the action of a weak acid or weak base medium. The single-crystal silicon carbide undergoes an amorphous transformation after being subjected to force, and then the amorphous silicon carbide in the weak acid medium reacts with the H+ and _H2O in the HCl solution at 25°C to generate amorphous silicon oxide, while the amorphous silicon carbide in the weak base medium reacts with the OH- _{and O2} in the _H2O2 solution to generate amorphous silicon oxide.

Example 3

(1) First, prepare a group of 10mm×10mm single crystal silicon carbide samples, load the samples into the realization device, observe the samples through the optical lens, set three groups of scratching positions, and the scratching parameters are all set to set the load applied by the nano scratch indenter to 45mN, the indenter speed to 1μm/s, and no coolant is added. The vacuum degree of the first group is set to 10-3Pa, with an accuracy of ±10-5Pa, and then carbon dioxide is introduced to keep the pressure inside and outside the realization device consistent; the vacuum degree of the second group is set to 10-3Pa, with an accuracy of ±10-5Pa, and then oxygen is introduced to keep the pressure inside and outside the realization device consistent; the third group is set to introduce air. Turn on the temperature control device on the sample stage, and set the sample stage to 25℃ for the first, second, and third groups, with a temperature control accuracy of ±0.5℃. After the scratching parameters are set, the conversion disk turns the nano scratch indenter to the sample, and the force sensor automatically contacts the scratching position. When the pressure reaches the set value, the system starts to operate. After completing the experiment according to the set parameters, take out the sample.

(2) The three groups of scratches obtained in step (1) were used to detect the chemical composition of the scratched area on the surface of silicon carbide using an X-ray photoelectron spectrometer. The scratch results of the first and third groups are shown in Figure 7. The XPS fine spectrum was peaked. There were two peaks in the Si2p peak diagram of Figure 7, of which 100.3eV corresponded to the peak position of silicon carbide, and 101.6eV corresponded to the peak position of Si-N. The second group of scratch results are shown in Figure 8. There were three peaks in the Si2p peak diagram of Figure 8, of which 100.2eV corresponded to the peak position of silicon carbide, 101.5eV corresponded to the peak position of Si-N, and 102.7eV corresponded to the peak position of silicon dioxide. At 25°C, single-crystal silicon carbide did not react to stress under the action of carbon dioxide or air medium, but reacted to stress under the action of oxygen. It shows that diamond abrasive and silicon carbide wafer can undergo interfacial chemical reaction induced by mechanical force in an oxygen environment at a temperature of 25°C in the absence of liquid medium. Single-crystal silicon carbide undergoes amorphous transformation under force, and then amorphous silicon carbide reacts chemically with oxygen to generate amorphous silicon oxide.

The above describes the specific implementation of the present application, but the protection scope of the present application is not limited thereto. Any technician familiar with the technical field can easily think of changes or substitutions within the technical scope disclosed in the present application, which should be included in the protection scope of the present application. Therefore, the protection scope of the present application should be based on the protection scope of the claims.

In the description of the present application, it should be understood that the terms "upper", "lower", "inside", "outside", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, which are only for the convenience of describing the present application and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the present application. The word "comprising" does not exclude the presence of elements or steps not listed in the claims. The word "one" or "an" preceding an element does not exclude the presence of multiple such elements. The simple fact that certain measures are recorded in mutually different dependent claims does not indicate that a combination of these measures cannot be used for improvement. Any reference symbols in the claims should not be interpreted as limiting the scope.

Claims (8)

1. The device for realizing the interface chemical reaction of the hard abrasive and the substrate under the nano scale is characterized by comprising a liquid-gas module, a temperature control module and a main shaft module, wherein the liquid-gas module comprises a liquid-gas box, a sealing cover, an air inlet, an air outlet, a water inlet and a water outlet, the sealing cover is arranged on the liquid-gas box and is in sealing connection with the liquid-gas box, a sample table is arranged in the liquid-gas box, the air inlet, the air outlet, the water inlet and the water outlet are connected with the liquid-gas box so that different liquid-gas media exist in the liquid-gas box, the temperature control module comprises a heating device and a cooling device, the heating device is connected with the sample table, the cooling device is connected with the heating device and the sample table, the main shaft module comprises a standard nano scratch device with pressure control, an optical lens, a conversion disc and a movement device, the motion device comprises an XY axis motion device and a Z axis motion device, the Z axis motion device is connected with the sealing cover, the XY axis motion device is connected with the Z axis motion device, the standard nanometer scratch device and the optical lens are arranged on the conversion disc, the standard nanometer scratch device is provided with a nanometer scratch pressure head, the conversion disc is fixed at the lower end of the XY axis motion device to realize the movement of the nanometer scratch pressure head and the optical lens in the XYZ direction, the substrate is fixed on the sample table, the optical lens is used for searching the scratching position on the substrate, the standard nanometer scratch device is used for applying different loads on the substrate and scratching, the conversion disc is used for switching the optical lens and the nanometer scratch pressure head, the temperature control module is used for controlling different temperatures, the method is characterized in that the nano scratch pressure head scratches on the surface of a substrate at low speed under different temperature, liquid-gas medium and/or load conditions, wherein the liquid medium in the liquid-gas medium is weak acid, weak alkaline or neutral medium, the PH is 5-9, the gas medium is air, oxygen and carbon dioxide, the standard nano scratch device is fixed under a conversion disc and applies load, the load control precision is 0.1mN and ranges from 0.1mN to 500mN, and the nano scratch pressure head forms scratching on the substrate at the scratching speed of 1-100 mu m/s in a constant direction through the XY axis movement device after loading.

2. The apparatus according to claim 1, wherein the liquid-gas module further comprises a sealing gasket, a fixing ring, wherein the sealing gasket is disposed between the sealing cover and the liquid-gas tank and between the sample stage and the liquid-gas tank, and the fixing ring is fixed on the sealing cover by a hexagonal screw.

3. The device for realizing the interfacial chemical reaction between the hard abrasive and the substrate under the nano scale according to claim 1, wherein the liquid-gas box is a closed container with a cuboid shape, the length is 120mm, the width is 100mm, the height is 110mm, and the material is stainless steel.

4. The device for realizing the interfacial chemical reaction between the hard abrasive and the substrate under the nano scale according to claim 1, wherein the sample stage is connected in the liquid-gas box through screw thread sealing, and the substrate is stuck on the sample stage by adopting hot melt adhesive.

5. The device for realizing the interface chemical reaction between the hard abrasive and the substrate under the nano scale according to claim 1, wherein the air inlet and the air outlet are arranged above the water inlet and the water outlet, the air inlet is externally connected with an air inlet pipe, a gas medium can be introduced, the water inlet is externally connected with a water inlet pipe, a liquid medium can be introduced, the air outlet is externally connected with an air outlet pipe for extracting gas, and the water outlet is externally connected with an air outlet pipe for discharging waste liquid.

6. The device for realizing the interfacial chemical reaction between the hard abrasive and the substrate under the nano-scale according to claim 1, wherein the heating device can heat the sample stage at a heating temperature of 40-80 ℃, and the cooling device cools the heating device and the sample stage in a liquid cooling mode.

7. The apparatus for realizing chemical reaction between a hard abrasive and a substrate at a nanoscale according to claim 1, wherein the nano-scratch indenter is a hard abrasive, the curvature of the nano-scratch indenter is 1-50 μm, the hard abrasive comprises diamond, aluminum oxide, cubic boron nitride or boron carbide, the substrate is a hard brittle material, and the substrate comprises diamond, gallium nitride, gallium oxide, sapphire or silicon carbide.

8. A method of implementing a device for implementing interfacial chemical reactions between a hard abrasive and a substrate at the nanoscale according to any one of claims 1-7, comprising the steps of:

1) The sample platform adhered with the substrate is fixed in the liquid-gas box through threaded connection, and the sealing gasket is fixed between the sample platform and the liquid-gas box;

2) The main shaft module is fixed on the sealing cover, the sealing cover is fixed on the liquid-gas tank through threads, the sealing gasket is fixed between the sealing cover and the liquid-gas tank, and the fixing ring is fixed on the sealing cover through hexagonal screws;

3) Searching a scratching position on the substrate by using an optical lens, setting a certain load, speed, vacuum degree, gas medium, liquid medium and temperature at the scratching position, converting the optical lens into a nano scratching pressure head by using a conversion disc, and scratching the nano scratching pressure head on the surface of the substrate;

4) And opening the sealing cover, taking out the sample stage, placing the scratched substrate on an X-ray photoelectron spectrometer, observing the surface state of the scratched substrate, and detecting chemical components at the scratch position of the surface of the substrate.