Optical microscopic observation system

Abstract

The utility model provides an optical microscopic observation system. The observation system comprises a light source, a to-be-observed material growth device, a beam splitter, a first filter and an imaging device. The to-be-observed material growth device comprises an observation window, a to-be-observed material is observed through the observation window, the beam splitter receives light emitted by the light source and reflects the light to the surface of the to-be-observed material, and the to-be-observed material reflects the light and then penetrates through the beam splitter. The first filter receives the light transmitted through the beam splitter. And the imaging device receives the light penetrating through the first filter and images the to-be-observed material.

Description

Technical Field

[0001] The present application relates to a device for observing high-temperature material preparation, chemical reaction, and phase change processes, and more specifically, to an optical microscopic observation system. Background Art

[0002] In recent years, in-situ microscopic observations involving high-temperature processes (such as metal heat treatment, high-temperature epitaxial growth and etching of thin film materials, high-temperature phase change processes of materials, high-temperature chemical reactions, etc.) have received widespread attention from the scientific research community and the industrial community. The reduction of these high-temperature processes through in-situ microscopic observations can effectively assist researchers in gaining a deeper understanding of the mechanisms, thereby developing new methods, new processes, and new materials. High-temperature microscopic observation technology is applied to online detection in industrial-grade continuous production processes, providing real-time feedback on the state or change trend of materials, thereby providing strong evidence for the setting and adjustment of reaction parameters, which will greatly improve production efficiency. The large amount of experimental data required for the AI ​​intelligent manufacturing technology that has emerged in recent years can also be obtained through high-temperature optical microscopy observation systems and applied to large-scale industrial manufacturing systems.

[0003] However, in-situ microscopic observation of high-temperature processes faces two major challenges: 1) The light (which carries no valid information) generated by the thermal radiation (blackbody radiation) accompanying high-temperature processes can overwhelm valid information, significantly interfering with observations; 2) To ensure image quality, microscopic imaging requires a short working distance, but optical lenses cannot tolerate high-temperature environments, placing extremely high demands on heat preservation during high-temperature processes and short-distance thermal insulation. Currently, there is an urgent need to develop high-quality high-temperature optical microscopic observation systems and methods. Utility Model Content

[0004] The main purpose of this application is to overcome at least one of the defects of the above-mentioned prior art, and to provide an optical microscopic observation system that can observe and clearly record the high-temperature process in real time, taking the in-situ observation of the high-temperature growth process of the material to be observed, graphene, as an example.

[0005] To achieve the above objectives, this application adopts the following technical solutions:

[0006] According to one aspect of the present application, an optical microscopic observation system is provided, comprising: a light source, a device for growing a material to be observed, a spectrometer, a first filter, and an imaging device. The device for growing a material to be observed includes an observation window through which the material to be observed is observed. The spectrometer receives light emitted by the light source and reflects the light onto the surface of the material to be observed. The material to be observed reflects the light and transmits it through the spectrometer. The first filter receives light transmitted through the spectrometer. The imaging device receives light transmitted through the first filter and images the material to be observed.

[0007] According to one embodiment of the present application, the light source is a full-spectrum light source, the first filter is a short-wave pass filter or a band-pass filter, and the maximum wavelength of light allowed to pass through the first filter does not exceed 550 nm.

[0008] According to one embodiment of the present application, the light source is an ultraviolet light source, and the wavelength of the light emitted by the ultraviolet light source is between 200nm and 350nm; the first filter is a shortwave pass filter or a bandpass filter, and the maximum wavelength of light allowed to pass through the first filter does not exceed 550nm.

[0009] According to one embodiment of the present application, the light source is a full-spectrum light source; a second filter is arranged between the light source and the spectrometer, the second filter is a bandpass filter, and the lower limit of the wavelength range of light allowed to pass through the second filter is between 200-270nm, and the upper limit is between 280-350nm; the first filter is a shortwave pass filter or a bandpass filter, and the maximum wavelength of light allowed to pass through the first filter does not exceed 550nm.

[0010] According to one embodiment of the present application, the first filter is a short-wave pass filter or a band-pass filter, and the maximum wavelength of light allowed to pass through the first filter does not exceed 550 nm.

[0011] According to one embodiment of the present application, the material to be observed is graphene.

[0012] According to one embodiment of the present application, the device for growing the material to be observed includes a shell, a workbench, a heater, an end cover, and a gas dispersion plate. The shell has an inner cavity; the shell has a first gas inlet, a first gas outlet, and a vacuum port. The workbench is arranged in the inner cavity, and the substrate required for the growth of the material to be observed is arranged on the workbench. The heater is arranged around the workbench and close to the substrate. The observation window is arranged to observe the end cover, and the end cover is arranged on the shell and closes the inner cavity; the orthographic projection of the substrate on the surface of the observation window is within the observation window. The gas dispersion plate is arranged between the heater and the end cover, and the gas dispersion plate has a through hole, and the workbench passes through the through hole; the gas dispersion plate is provided with a second gas inlet and a second gas outlet, the second gas inlet is connected to the first gas inlet, and the second gas outlet is connected to the first gas outlet.

[0013] According to one embodiment of the present application, the side wall of the shell is a double-layer hollow structure, and a first coolant inlet and a first coolant outlet are provided on the side wall. The coolant flows through the side wall to reduce the temperature of the inner cavity.

[0014] According to one embodiment of the present application, the gas dispersion plate includes two protrusions and a recessed portion, the through hole is located in the recessed portion, and the distance between the recessed portion and the inner surface of the end cover is greater than the distance between the protrusion and the inner surface of the end cover.

[0015] According to one embodiment of the present application, the device for growing the material to be observed also includes a heat insulating member, which is arranged between the workbench and the observation window and supported by the recessed portion. The heat insulating member has an observation hole, and the orthographic projection of the substrate on the surface of the observation window is located within the orthographic projection of the observation hole on the surface of the observation window.

[0016] According to one embodiment of the present application, the device for growing the material to be observed further includes: a bracket, which is arranged in the inner cavity and supports the workbench, and the bracket can move three-dimensionally in the inner cavity.

[0017] According to one embodiment of the present application, the device for growing the material to be observed further includes a support tube, which is arranged between the workbench and the bracket.

[0018] According to one embodiment of the present application, the device for growing the material to be observed further includes a three-dimensional moving mechanism, which is connected to the bracket. The three-dimensional moving mechanism drives the bracket to move three-dimensionally in the inner cavity to adjust the position of the workbench in the inner cavity.

[0019] According to one embodiment of the present application, the heater includes an electromagnetic induction heater, a resistance wire heater or a heating belt.

[0020] According to one embodiment of the present application, the observation window includes two layers of glass, with a space between the two layers of glass. A second coolant inlet and a second coolant outlet are provided on the end cover. The coolant enters the space through the second coolant inlet to cool the two layers of glass, and then flows out from the second coolant outlet.

[0021] According to one embodiment of the present application, the material of the workbench is graphite, corundum, quartz or silicon carbide.

[0022] According to one embodiment of the present application, a seal is provided between the end cover and the shell, and thermal insulation cotton is provided on the inner wall of the shell.

[0023] According to another aspect of the present application, the present application provides an optical microscopic observation method for observing the growth process of a material to be observed. Under the above optical microscopic observation system, light is irradiated onto the surface of the material to be observed, and the surface of the material to be observed reflects light to a first filter. After the first filter shields the red light and infrared light generated by thermal radiation in the light reflected by the material to be observed, an imaging device receives the light passing through the first filter and forms an image.

[0024] According to one embodiment of the present application, the light irradiated onto the surface of the material to be observed is full-spectrum light or ultraviolet light.

[0025] According to the third aspect of the present application, the present application provides an optical microscopic observation method for observing the growth process of a material to be observed. Under the above optical microscopic observation system, the light source is turned off and the growth process of the material to be observed is observed.

[0026] According to one embodiment of the present application, the material to be observed is graphene.

[0027] From the above technical solutions, it can be seen that the advantages and positive effects of the optical microscopic observation system proposed in this application are:

[0028] The optical microscopic observation system proposed in this application utilizes a beam splitter and a first filter to observe a material under observation through an observation window of a device for growing the material under observation. The beam splitter receives light from a light source and reflects it onto the surface of the material under observation. The material under observation then reflects the light and transmits it through the beam splitter. The first filter receives the light transmitted through the beam splitter, and an imaging device receives the light transmitted through the first filter and images the material under observation. This allows for clear observation of the material under observation while it is growing at high temperatures, and allows the imaging process to be captured on the imaging device. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] The above and other features and advantages of the present application will become more apparent by describing in detail example embodiments thereof with reference to the accompanying drawings.

[0030] Figure 1 It is a structural diagram of the optical part of the optical microscopic observation system of the present application.

[0031] Figure 2 It is a structural schematic diagram of the optical microscopic observation system of this application.

[0032] Figure 3 yes Figure 2 Schematic diagram of the internal structure of the device for growing the material to be observed.

[0033] Figure 4 yes Figure 2 Schematic diagram of the structure of the material growth device to be observed after removing the end cover.

[0034] Figure 5 yes Figure 4 Schematic diagram of the structure of the growth device of the material to be observed with the thermal insulation part removed.

[0035] Figure 6 yes Figure 5 Schematic diagram of the structure of the material growth device to be observed without the gas dispersion plate.

[0036] Figure 7 It is a structural schematic diagram of the gas dispersion plate of the device for growing the material to be observed in the present application.

[0037] Figure 8 This is the optical image of the 22um copper foil surface before pretreatment.

[0038] Figure 9 This is an optical image of the 22um copper foil surface after pretreatment.

[0039] Figure 10 This is an optical image of the graphene film growing for 1 minute.

[0040] Figure 11 This is an optical image of the graphene film growing for 7 minutes.

[0041] Figure 12 This is an optical image of the graphene film growing for 14 minutes.

[0042] Figure 13 This is the Raman spectrum of graphene film.

[0043] Figure 14 This is a light microscope image of graphene film growth without the optical microscopic observation system of the present application.

[0044] Figure 15 This is a light microscope image of graphene film growth using the optical microscopic observation system of the present application.

[0045] The description of the accompanying drawings is as follows:

[0046] 1- Optical part of the optical microscopy system;

[0047] 2-device for growing the material to be observed;

[0048] 10-light source;

[0049] 20-beam splitter;

[0050] 30- Materials to be observed;

[0051] 40-first filter;

[0052] 50- imaging device;

[0053] 60- second filter;

[0054] 21- housing;

[0055] 22- workbench;

[0056] 23-heater;

[0057] 24-end cover;

[0058] 25-gas dispersion plate;

[0059] 26- thermal insulation;

[0060] 27- bracket;

[0061] 28-support tube;

[0062] 29-three-dimensional moving mechanism;

[0063] 210 - first gas inlet;

[0064] 211-first gas outlet;

[0065] 212-vacuum port;

[0066] 213 - side wall of the housing;

[0067] 214-first coolant inlet;

[0068] 221-substrate;

[0069] 231-heater lead end;

[0070] 241-Observation window;

[0071] 242 - second coolant inlet;

[0072] 243-second coolant outlet;

[0073] 244-Seal;

[0074] 250-through hole;

[0075] 251-second gas inlet;

[0076] 252-second gas outlet;

[0077] 253-protrusion;

[0078] 254-depression;

[0079] 255-flow plate;

[0080] 261-Observation hole;

[0081] 291- bellows;

[0082] 300-base. DETAILED DESCRIPTION

[0083] Example embodiments will now be described more fully with reference to the accompanying drawings. However, example embodiments can be implemented in many forms and should not be construed as limited to the embodiments set forth herein; rather, these embodiments are provided so that this disclosure will be thorough and complete and will fully convey the concepts of the example embodiments to those skilled in the art. Like reference numerals in the figures represent like or similar structures, and thus their detailed description will be omitted.

[0084] In the following description of different exemplary embodiments of the present application, reference is made to the accompanying drawings, which form a part of the present application and in which different exemplary structures, systems and steps that can implement various aspects of the present application are shown by way of example. It should be understood that other specific schemes of components, structures, exemplary devices, systems and steps can be used, and structural and functional modifications can be made without departing from the scope of the present application. Moreover, although the terms "above", "between", "within", etc. may be used in this specification to describe different exemplary features and elements of the present application, these terms are used herein for convenience only, for example, according to the directions of the examples described in the accompanying drawings. Nothing in this specification should be construed as requiring a specific three-dimensional orientation of the structure to fall within the scope of the present application.

[0085] It is understood that the terms "including" and "having" and any variations thereof in the embodiments of the present application are intended to cover non-exclusive inclusions. For example, a process, method, system, product, or apparatus comprising a series of steps or units is not limited to the listed steps or units, but may optionally include steps or units not listed, or may optionally include other steps or components inherent to the process, method, product, or apparatus.

[0086] Relative terms such as "lower" or "bottom" and "upper" or "top" may be used herein to describe the relationship of one element to another element, as shown in the figures. It should be understood that relative terms are intended to include different orientations of the device in addition to the orientation shown in the figures. For example, if the device in a figure is turned over, the element described as being "lower" or "bottom" of other elements will be oriented "upper" or "top" of the other elements. Thus, the exemplary term "lower" can include both "lower" and "top" orientations, and the term "bottom" can include both "bottom" and "top" orientations, depending on the particular orientation of the figure. Similarly, if the device in a figure is turned over, the element described as being "lower" or "bottom" of other elements will be oriented as being "upper" or "top" of the other elements. Thus, the exemplary terms "bottom" or "below" can include both "upper" and "lower" orientations.

[0087] like Figures 1 to 2As shown, the optical microscopic observation system of the present application is used to observe the growth process of a material to be observed 30. The optical part 1 of the optical microscopic observation system includes: a light source 10, a beam splitter 20, a first filter 40, and an imaging device 50. In this embodiment, the beam splitter 20 is a seven-transmitting, three-reflecting beam splitter or a five-transmitting, five-reflecting beam splitter. In other embodiments, the beam splitter may also be of other types. The beam splitter 20 receives light emitted by the light source 10 and reflects the light onto the surface of the material to be observed 30. The material to be observed 30 reflects the light and then transmits it through the beam splitter 20. The first filter 40 receives the light transmitted through the beam splitter 20 and blocks stray light (mostly red and infrared light) generated by thermal radiation in the light transmitted through the beam splitter. The imaging device 50 receives the light transmitted through the first filter 40 and images the growth process of the material to be observed 30. The material to be observed 30 is disposed in a material to be observed growth device 2. The material to be observed growth device 2 includes an observation window 241 through which the material to be observed is observed.

[0088] The optical microscopic observation system of the present application utilizes a beam splitter 20 and a first filter 40. The beam splitter 20 receives light emitted by a light source 10 and reflects the light onto the surface of a material to be observed 30. The material to be observed 30 then reflects the light and transmits it through the beam splitter 20. The first filter 40 receives the light transmitted through the beam splitter 20 and shields the stray light (mostly red and infrared light) generated by thermal radiation in the light transmitted through the beam splitter. The imaging device 50 receives the light transmitted through the first filter 40 and images the growth process of the material to be observed 30. This design enables clear observation of the growth process of graphene films even at high temperatures during their growth.

[0089] The optical microscopic observation system of this application can shield the thermal radiation generated by the high temperature during graphene film growth. By utilizing the different UV transmittances of graphene films with different numbers of layers, a camera with excellent imaging capabilities in the visible and UV bands is selected to observe graphene growth using a metallographic microscope, resulting in clear images. It can also provide real-time and clear observation of the growth process of graphene films exceeding 1 cm x 1 cm in size.

[0090] In this embodiment, the light source 10 is a full-spectrum light source, and the first filter 40 is a short-wave pass filter or a band-pass filter. The maximum wavelength of light allowed to pass through the first filter 40 does not exceed 550 nm. Specifically, it can be a short-wave pass filter with a cutoff wavelength of 532 nm, a band-pass filter with a wavelength range of 330 nm to 410 nm, a band-pass filter with a wavelength range of 380 nm to 435 nm, a band-pass filter with a wavelength range of 400 nm to 495 nm, etc. The first filter can shield stray light (mostly red light and infrared light) generated by thermal radiation, thereby ensuring clear imaging. In this embodiment, the light source 10 is a full-spectrum light source, and a second filter 60 is provided between the light source 10 and the spectrometer 20. The second filter 60 is a band-pass filter. The wavelength range of light allowed to pass through the second filter 60 has a lower limit of 200 nm to 270 nm, such as 250 nm, 260 nm, etc., and an upper limit of 280 nm to 350 nm, such as 290 nm, 300 nm, etc. It can further improve the clarity of the observation system.

[0091] In some other embodiments, the light source 10 is an ultraviolet light source, so that the light received by the beam splitter 20 is ultraviolet light, and the wavelength of the light emitted by the ultraviolet light source is between 200nm and 350nm; the first filter 40 is a short-wave pass filter or a band-pass filter, and the maximum wavelength of light allowed to pass through the first filter 40 does not exceed 550nm. Specifically, it can be a short-wave pass filter with a cutoff wavelength of 532nm, a band-pass filter with a range of 330nm to 410nm, a band-pass filter with a range of 380nm to 435nm, a band-pass filter with a range of 400nm to 495nm, etc., which can shield the red light and infrared light generated by thermal radiation, thereby ensuring clear imaging. In some other embodiments, the first filter 40 is a short-wave pass filter or a band-pass filter, and the maximum wavelength of light allowed to pass through the first filter 40 does not exceed 550nm.

[0092] In this embodiment, the direction in which the beam splitter 20 receives light emitted by the light source 10 is at a 45° angle to the normal direction of the beam splitter 20. This allows the beam splitter 20 to completely reflect the light transmitted from the light source 10. In this embodiment, the beam splitter 20 is a seven-transmitting, five-reflecting beam splitter or a five-transmitting, five-reflecting beam splitter, which provides excellent light processing effects.

[0093] In this embodiment, the material to be observed 30 is a graphene film. The optical microscopic observation system of this application takes the observation of the in-situ growth of a graphene film as an example. The observation system of this application is not limited to observing the growth of graphene films, but can also observe the growth of other materials to be observed.

[0094] In this embodiment, the imaging device 50 can be an ultraviolet camera. A tube lens can be provided between the imaging device 50 and the first filter 40. An aperture stop can be provided between the beam splitter 20 and the first filter 40. An objective lens can be provided between the material to be observed 30 and the beam splitter 20.

[0095] In this embodiment, if Figure 2 、 Figure 3 、 Figure 5 and Figure 7 As shown, the optical microscopic observation system also includes a material growth device 2 to be observed, wherein the material growth device 2 to be observed includes a shell 21, a workbench 22, a heater 23, an end cover 24 and a gas dispersion plate 25. The shell 21 has an inner cavity; the shell 21 has a first gas inlet 210, a first gas outlet 211 and a vacuum port 212. The workbench 22 is arranged in the inner cavity, and a substrate 221 required for the growth of the material 30 to be observed is arranged on the workbench 22. The heater 23 is arranged around the workbench 22 and is close to the substrate 221. The observation window 241 is arranged on the end cover 24, and the end cover 24 is covered on the shell 21 and closes the inner cavity; the orthographic projection of the substrate 221 on the surface of the observation window 241 is in the observation window 241, that is, the observation window 241 is facing the substrate 221. The gas dispersion plate 25 is arranged between the heater 23 and the end cover 24. The gas dispersion plate 25 has a through hole 250, and the workbench 22 passes through the through hole 250; the gas dispersion plate 25 is provided with a second gas inlet 251 and a second gas outlet 252. The second gas inlet 251 is connected to the first gas inlet 210, and the second gas outlet 252 is connected to the first gas outlet 211.

[0096] The device 2 for growing the material to be observed of the present application can concentrate the gas required for the growth of the graphene film around the substrate 221 by setting a gas dispersion plate 25 between the heater 23 and the observation window 241 of the end cover 24, and can reduce the gas overflow to the vicinity of the heater 23, thereby avoiding the temperature of the part of the inner cavity of the shell 21 close to the observation window 241 being too high, thereby affecting the clarity of the picture of the graphene film growth taken by the observation window 241.

[0097] In this embodiment, see Figure 3 The sidewall 213 of the housing 21 has a double-layer hollow structure. A first coolant inlet 214 and a first coolant outlet (not shown) are provided on the sidewall 213. Coolant flows through the sidewall 213 to reduce the temperature of the inner cavity. The hollow liquid cooling design of the sidewall 213 of the housing 21 can effectively reduce the temperature of the inner cavity and further reduce the impact of high temperatures on the observation window 241 during the graphene film growth process.

[0098] In this embodiment, see Figure 7 The gas dispersion plate 25 includes two protrusions 253 and a recessed portion 254. The through hole 250 is located in the recessed portion 254. The distance between the recessed portion 254 and the inner surface of the end cap 24 is greater than the distance between the protrusion 253 and the inner surface of the end cap 24. The gas dispersion plate 25 is designed with a recessed portion 254 between the two protrusions 253. This can gather gas around the substrate 221 where the graphene film is grown, thereby reducing gas consumption and lowering costs. Figure 7 As shown, a flow plate 255 is provided between the second gas inlet 251 on the recess 254 and the through hole 250 to uniformly disperse the gas entering from the second gas inlet 251 to the vicinity of the substrate 221 in the through hole 250. Both the gas dispersion plate 25 and the flow plate 255 can be made of stainless steel.

[0099] In this embodiment, if Figure 3 、 Figure 4 and Figure 5 As shown, the material growth device 2 to be observed further includes a heat insulating member 26, which is disposed between the workbench 22 and the observation window 241 and supported on the recessed portion 254. The heat insulating member 26 has an observation hole 261, and the orthographic projection of the substrate 221 on the surface of the observation window 241 is located within the orthographic projection of the observation hole 261 on the surface of the observation window 241, that is, the observation hole 261 is directly opposite the substrate 221. The provision of the heat insulating member 26 can prevent the copper of the copper foil substrate 221 from volatilizing and blocking the observation window 241, and can shield and isolate the thermal radiation during the growth of the graphene film. The heat insulating member 26 can be a square plate with an observation hole 261 in the middle. The four corners of the heat insulating member 26 can be supported on the recessed portion 254 of the gas dispersion plate 25, and the heat insulating member 26 is suspended above the substrate 221.

[0100] In this embodiment, see Figure 3 and Figure 6 The device 2 further includes a support 27 disposed within the inner chamber and supporting the workbench 22. The support 27 is capable of three-dimensional movement (X, Y, and Z directions) within the inner chamber. The support 27 allows the position of the workbench 22 within the inner chamber to be adjusted according to actual conditions, allowing the device 2 to be applied to different materials 30 to be observed.

[0101] In this embodiment, the device for growing the material to be observed 2 further includes a support tube 28, which is disposed between the workbench 22 and the bracket 27. The support tube 28 can be made of corundum or stainless steel.

[0102] In this embodiment, the observed material growth apparatus 2 further includes a three-dimensional motion mechanism 29, which is connected to the bracket 27. The three-dimensional motion mechanism 29 drives the bracket 27 to move three-dimensionally within the inner cavity to adjust the position of the worktable 22 within the inner cavity. A bellows 291 is disposed between the three-dimensional motion mechanism 29 and the housing 21. The bracket 27 includes a horizontal beam that contacts the support tube 28, a vertical beam connected to the end of the horizontal beam, and a connector connected to the end of the vertical beam. The connector passes through the bellows 291 and connects to the three-dimensional motion mechanism 29.

[0103] In this embodiment, the heater 23 is an electromagnetic induction heater. Figure 2 、 Figure 4 、 Figure 5 and Figure 6 The heater 23 is connected to an external electromagnetic induction heating controller (not shown in the figure) through the heater lead-out terminal 231. In some other embodiments, the heater 23 can also be a resistance wire heater or a heating belt. The material of the workbench 22 is graphite, corundum, quartz or silicon carbide. The heater 23 is mainly used to heat the gas in the inner cavity reactor of the material growth device 2 to be observed, so that it decomposes at high temperature to produce a chemical reaction. Taking the preparation of graphene from methane as an example, an electromagnetic induction heater heating method is used. The heating temperature is 1000°C.

[0104] When the carbon source for graphene production is a liquid carbon source, such as ethanol, a hole can be provided at an appropriate location on the sidewall 213 of the housing 21 of the apparatus for growing the material to be observed 2. This hole connects to a front heating chamber, which can sublime the liquid carbon source, such as ethanol. This is a dual-temperature zone series configuration. A multi-temperature zone series configuration can also be used.

[0105] In this embodiment, see Figure 2 Observation window 241 comprises two layers of glass with a space between them. End cap 24 is provided with a second coolant inlet 242 and a second coolant outlet 243. Coolant enters the space through second coolant inlet 242 to cool both layers of glass before exiting through second coolant outlet 243. This design cools the glass of observation window 241, facilitating clear images captured through observation window 241.

[0106] In this embodiment, a seal 244 is provided between the end cap 24 and the housing 21 , and heat-insulating cotton is provided on the inner wall of the housing 21 . The growth device 2 for the material to be observed further includes a base 300 .

[0107] It should be noted that the optical microscopy systems shown in the drawings and described in this specification are merely examples of a wide variety of optical microscopy systems that can employ the principles of the present application. It should be clearly understood that the principles of the present application are in no way limited to any detail of the optical microscopy systems shown in the drawings or described in this specification, or to any component of the optical microscopy systems.

[0108] The above is a detailed description of several exemplary embodiments of the optical microscopic observation system proposed in this application. The following is an exemplary description of the use process of the optical microscopic observation system of this application.

[0109] Combined with attachment Figures 1 to 7 The optical microscopic observation system proposed in this application is used for in-situ growth observation of the material to be observed 30, wherein the in-situ growth of the material to be observed 30 is carried out in the material to be observed growth device 2 of this application, and the growth process is:

[0110] This embodiment is described using a copper foil with a thickness of 22 μm as the substrate 221. The substrate 221 may also be other metal foils or fiber fabrics, etc. The thickness may be between 10 μm and 100 μm.

[0111] Pretreatment process of substrate 221: Place the copper foil in the material growth device 2 to be observed, turn on the vacuum control device, and evacuate the interior of the housing 21 from the vacuum port 212 to make the pressure in the inner cavity of the housing 21 in a low vacuum state, for example, 1-20kPa. After the pressure stabilizes, turn on the optical part 1 of the optical microscope observation system to observe the surface of the copper foil. Figure 8 It is the optical image of the copper foil surface before pretreatment. Figure 8 It can be seen that the surface of the copper foil without pretreatment is rough and uneven, which is not conducive to the growth of graphene film.

[0112] The heater 23 is turned on for heating, and an appropriate amount of argon (20 sccm-2000 sccm) and diluted oxygen (2 sccm-200 sccm) are introduced into the inner cavity of the shell 21 to raise the temperature in the inner cavity of the shell 21 to the target temperature (100°C-3000°C) and maintain it. Subsequently, the argon and diluted oxygen are turned off, and hydrogen (3 sccm-600 sccm) is introduced for the first annealing for 3-20 minutes. After the first annealing is completed, hydrogen (3 sccm-600 sccm) and diluted oxygen (2 sccm-200 sccm) are introduced for the second annealing for 2-100 minutes until the surface of the copper foil becomes relatively flat, as shown in FIG. Figure 9 shown.

[0113] After the substrate 221 is pretreated, the graphene film is grown at a target temperature (100°C-3000°C). The gases introduced include but are not limited to argon, diluted oxygen, methane, diluted methane, acetylene, diluted acetylene, hydrogen, etc., and an ultraviolet camera is used to observe the growth of graphene films with different numbers of layers. Figure 10 This is an optical image of the graphene film growing for 1 minute. Figure 11 This is an optical image of the graphene film growing for 7 minutes. Figure 12 This is an optical image of the graphene film growing for 14 minutes.

[0114] After the growth is completed, only argon gas (20 sccm-2000 sccm) is introduced to cool the film down to room temperature, and the copper foil is removed for graphene film characterization. Figure 13 is the Raman spectrum of graphene film.

[0115] The optical microscopic observation system of the present application can observe the growth process of the observed material 30, and can also observe the growth process of the graphene film growing on copper foil under high temperature conditions. This can realize the visualization of the graphene film growth process using a metallographic microscope, reducing costs, and providing high imaging resolution and clear images. The optical microscopic observation system of the present application can observe the changes in the surface of the substrate 221 throughout the growth process of the graphene film.

[0116] To further understand the content of this application, the present application is now described in detail in conjunction with specific embodiments. It should be noted that due to limited space, only some embodiments are listed below, and the optical microscopic observation system and various parameters during the growth of the material 30 to be observed are not limited to the specific embodiments described below.

[0117] Example 1

[0118] Place the copper foil in the material growth device 2 to be observed, turn on the vacuum control device, and evacuate the interior of the shell 21 from the vacuum port 212 so that the pressure in the inner cavity of the shell 21 is in a low vacuum state, for example, 2 kPa. After the pressure stabilizes, turn on the optical part 1 of the optical microscope observation system to observe the surface of the copper foil.

[0119] The heater 23 is turned on for heating, and 100 sccm of argon and 100 sccm of diluted oxygen are introduced into the inner cavity of the shell 21 to raise the temperature in the inner cavity of the shell 21 to 500°C and maintain it. Then, the argon and diluted oxygen are turned off, and 100 sccm of hydrogen is introduced for the first annealing for 10 minutes. After the first annealing is completed, 100 sccm of hydrogen and 60 sccm of diluted oxygen are introduced for the second annealing for 15 minutes until the surface of the copper foil becomes relatively flat.

[0120] After the substrate 221 is pretreated, graphene films are grown at 500° C. The gases introduced at this time are argon, diluted oxygen, methane, diluted methane and hydrogen. At the same time, an ultraviolet camera (ULTRAVIOLET CAMERA) is used to observe the growth of graphene films with different numbers of layers.

[0121] After the growth is completed, only 100 sccm of argon gas is introduced to cool the film. After the temperature drops to room temperature, the copper foil is taken out for characterization of the graphene film.

[0122] Example 2

[0123] Place the copper foil in the material growth device 2 to be observed, turn on the vacuum control device, and evacuate the interior of the shell 21 from the vacuum port 212 so that the pressure in the inner cavity of the shell 21 is in a low vacuum state, for example, 10 kPa. After the pressure stabilizes, turn on the optical part 1 of the optical microscope observation system to observe the surface of the copper foil.

[0124] The heater 23 is turned on for heating, and 500 sccm of argon and 600 sccm of diluted oxygen are introduced into the inner cavity of the shell 21 to raise the temperature in the inner cavity of the shell 21 to 900°C and maintain it. Then, the argon and diluted oxygen are turned off, and 80 sccm of hydrogen is introduced for the first annealing for 15 minutes. After the first annealing is completed, 200 sccm of hydrogen and 100 sccm of diluted oxygen are introduced for the second annealing for 30 minutes until the surface of the copper foil becomes relatively flat.

[0125] After the substrate 221 is pretreated, graphene film is grown at 900° C., with argon, diluted oxygen, methane, diluted methane and hydrogen being introduced. An ultraviolet camera is used to observe the growth of graphene films with different numbers of layers.

[0126] After the growth is completed, only 100 sccm of argon gas is introduced to cool the film. After the temperature drops to room temperature, the copper foil is taken out for characterization of the graphene film.

[0127] Example 3

[0128] Place the copper foil in the material growth device 2 to be observed, turn on the vacuum control device, and evacuate the interior of the shell 21 from the vacuum port 212 so that the pressure in the inner cavity of the shell 21 is in a low vacuum state, for example, 15kPa. After the pressure stabilizes, turn on the optical part 1 of the optical microscope observation system to observe the surface of the copper foil.

[0129] The heater 23 is turned on for heating, and 1000 sccm of argon and 500 sccm of diluted oxygen are introduced into the inner cavity of the shell 21 to raise the temperature in the inner cavity of the shell 21 to 1000°C and maintain it. Then, the argon and diluted oxygen are turned off, and 200 sccm of hydrogen is introduced for the first annealing for 10 minutes. After the first annealing is completed, 300 sccm of hydrogen and 200 sccm of diluted oxygen are introduced for the second annealing for 30 minutes until the surface of the copper foil becomes relatively flat.

[0130] After the substrate 221 is pretreated, graphene films are grown at 1000° C. The gases introduced at this time are argon, diluted oxygen, acetylene, diluted acetylene and hydrogen. At the same time, an ultraviolet camera (ULTRAVIOLET CAMERA) is used to observe the growth of graphene films with different numbers of layers.

[0131] After the growth is completed, only 1000 sccm of argon gas is introduced to cool the film. After the temperature drops to room temperature, the copper foil is taken out for characterization of the graphene film.

[0132] Example 4

[0133] Place the copper foil in the material growth device 2 to be observed, turn on the vacuum control device, and evacuate the interior of the shell 21 from the vacuum port 212 so that the pressure in the inner cavity of the shell 21 is in a low vacuum state, for example, 18 kPa. After the pressure stabilizes, turn on the optical part 1 of the optical microscope observation system to observe the surface of the copper foil.

[0134] The heater 23 is turned on for heating, and 1500 sccm of argon and 100 sccm of diluted oxygen are introduced into the inner cavity of the shell 21 to raise the temperature in the inner cavity of the shell 21 to 1500°C and maintain it. Subsequently, the argon and diluted oxygen are turned off, and 300 sccm of hydrogen is introduced for the first annealing for 10 minutes. After the first annealing is completed, 300 sccm of hydrogen and 100 sccm of diluted oxygen are introduced for the second annealing for 40 minutes until the surface of the copper foil becomes relatively flat.

[0135] After the substrate 221 is pretreated, graphene films are grown at 1500° C. The gases introduced at this time are argon, diluted oxygen, acetylene, diluted acetylene and hydrogen. At the same time, an ultraviolet camera (ULTRAVIOLET CAMERA) is used to observe the growth of graphene films with different numbers of layers.

[0136] After the growth is completed, only 1500 sccm of argon gas is introduced to cool the film. After it reaches room temperature, the copper foil is taken out for characterization of the graphene film.

[0137] Based on the above description of the optical portion 1 and the device for growing the material to be observed 2 of the optical microscopic observation system of the present application, it can be concluded that the optical microscopic observation system of the present application utilizes a beam splitter 20 and a first filter 40. The beam splitter 20 receives light emitted by the light source 10 and reflects the light onto the surface of the material to be observed 30. The material to be observed 30 then reflects the light and transmits it through the beam splitter 20. The first filter 40 receives the light transmitted through the beam splitter 20 and forms an image on the imaging device 50. The optical microscopic observation system of the present application enables clear observation of the growth process of the graphene film even under high-temperature conditions during the growth of the graphene film.

[0138] The optical microscopic observation method of the present application for observing the growth process of the material to be observed is as follows: Figure 1 As shown, after light irradiates the surface of the material to be observed 30, the material 30 reflects the light (including light generated by thermal radiation from the material to be observed) to the first filter 40. The first filter 40 then blocks the red and infrared light generated by the thermal radiation from the light reflected by the material 30. The imaging device 50 then receives the light transmitted through the first filter 40 and forms an image. This method can shield the thermal radiation generated by the high temperatures during graphene film growth. By utilizing the different UV transmittances of graphene films with different numbers of layers, a camera with excellent imaging capabilities in the visible and UV bands is selected, and graphene growth observations using a metallographic microscope produce clear images. This method also enables real-time, clear observation of the growth process of graphene films exceeding 1 cm x 1 cm.

[0139] In this embodiment, the light irradiated onto the surface of the material to be observed 30 is ultraviolet light. A second filter 60 can be provided between the full-spectrum light source and the spectrometer to ensure that ultraviolet light is irradiated onto the surface of the material to be observed 30. In other embodiments, the light irradiated onto the surface of the material to be observed 30 is full-spectrum light.

[0140] The optical microscopic observation method of the present application for observing the growth process of a material to be observed is to observe the growth process of the material to be observed 30 by turning off the light source 10 under the above optical microscopic observation system. In this observation method, the light source 10 is not provided, and imaging can be performed by utilizing the difference in infrared radiation capacity between the graphene film and the substrate 221 (copper foil) under high temperature heating.

[0141] In this embodiment, the material to be observed 30 is graphene, but may also be silicon carbide or the like.

[0142] The above is an explanation of the use process and method of the optical microscopic observation system of the present application. <111> Take copper single crystal as an example for comparison:

[0143] See also Figure 14 , Figure 14This is a light microscope image of graphene film growth without using the optical microscopic observation system of this application. Figure 14 It can be seen from the figure that the optical microscope image of the graphene film growth without the optical microscope observation system of the present application is blurred and has a low resolution.

[0144] In comparison, Figure 15 This is a light microscope image of graphene film growth using the optical microscopic observation system of the present application, Figure 15 It can be seen that the graphene film growth images observed using the optical microscopy observation system of the present application have clear images and high resolution.

[0145] In summary, the optical microscopic observation system proposed in the present application includes a light source, a spectrometer, a growth device for the material to be observed, a first filter, and an imaging device. The spectrometer receives the light emitted by the light source and reflects the light to the surface of the material to be observed. The material to be observed reflects the light and passes it through the spectrometer. The first filter receives the light that passes through the spectrometer. The imaging device receives the light that passes through the first filter and images the growth process of the material to be observed. The optical microscopic observation system of the present application can clearly observe the growth process of the graphene film under the high-temperature state of the graphene film growth. And the size of the heater will not be reduced. For graphene films with a size exceeding 1cm×1cm, it is still possible to clearly capture pictures of the growth process of the graphene film.

[0146] The present application discloses an optical microscopic observation method for observing the growth process of a material to be observed. After light is irradiated onto the surface of the material to be observed, the material to be observed reflects light onto a first filter. The first filter shields the red and infrared light reflected by the material to be observed. Then, an imaging device receives the light transmitted through the first filter and forms an image. This method can shield the thermal radiation generated by the high temperature during graphene film growth. By utilizing the different UV transmittances of graphene films with different numbers of layers, a camera with excellent imaging capabilities in the visible and UV bands is selected. Graphene growth is observed using a metallographic microscope, resulting in clear images. This method can also provide real-time, clear observation of the growth process of graphene films exceeding 1 cm x 1 cm in size.

[0147] The optical microscopic observation method of the present application for observing the growth process of the material to be observed is to turn off the light source and observe the growth process of the material to be observed under the above optical microscopic observation system.

[0148] It is understandable that the various embodiments / implementations provided in this application can be combined with each other without causing any contradiction, and they will not be illustrated one by one here.

[0149] In the exemplary embodiments described above, the optical microscopic observation system proposed in this application is described using the example of its application to observing graphene films. Those skilled in the art will readily appreciate that various modifications, additions, substitutions, deletions, or other changes to the specific embodiments may be made to apply the relevant designs of this application to other types of materials to be observed, and such modifications remain within the scope of the principles of the optical microscopic observation system proposed in this application.

[0150] It should be noted that the optical microscopy systems shown in the drawings and described in this specification are only a few examples of the many optical microscopy systems that can employ the principles of the present application. It should be clearly understood that the principles of the present application are in no way limited to any detail or component of the optical microscopy systems shown in the drawings or described in this specification.

[0151] In the application examples, the terms "first", "second", and "third" are used for descriptive purposes only and are not to be understood as indicating or implying relative importance; the term "plurality" refers to two or more, unless otherwise expressly defined. Terms such as "installed", "connected", "connected", and "fixed" should be understood in a broad sense. For example, "connected" can mean a fixed connection, a detachable connection, or an integral connection; "connected" can mean a direct connection or an indirect connection through an intermediate medium. For those skilled in the art, the specific meanings of the above terms in the application examples can be understood according to the specific circumstances.

[0152] In the description of the application embodiments, it should be understood that the terms "up", "down", "left", "right", "front", "back", "top", "bottom", etc., indicating the orientation or position relationship, are based on the orientation or position relationship shown in the accompanying drawings, and are only for the convenience of describing the application embodiments and simplifying the description, rather than indicating or implying that the device or unit referred to must have a specific direction, be constructed and operated in a specific orientation. Therefore, it cannot be understood as a limitation on the application embodiments.

[0153] In the description of this specification, the terms "one embodiment", "some embodiments", "specific embodiments", etc. mean that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the application embodiment. When introducing the elements / components / etc. described and / or illustrated herein, the terms "one", "an", and "above" are used to indicate the presence of one or more elements / components / etc. In this specification, the schematic representations of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any appropriate manner in any one or more embodiments or examples.

[0154] The above are merely preferred embodiments of the present invention and are not intended to limit the present invention. Those skilled in the art will readily appreciate that various modifications and variations of the present invention are possible. Any modifications, equivalent substitutions, or improvements made within the spirit and principles of the present invention shall be included within the scope of protection of the present invention.

Claims

1. An optical microscopic observation system, characterized in that: include: light source; A device for growing a material to be observed, comprising an observation window through which the material to be observed is observed; a beam splitter, the beam splitter receiving the light emitted by the light source and reflecting the light onto the surface of the material to be observed, and the material to be observed reflects the light and then transmits the beam splitter; a first filter, receiving light transmitted through the beam splitter; An imaging device receives the light transmitted through the first filter and images the material to be observed.

2. The optical microscopic observation system according to claim 1, wherein: The light source is a full-spectrum light source, the first filter is a short-wave pass filter or a band-pass filter, and the maximum wavelength of light allowed to pass through the first filter does not exceed 550 nm.

3. The optical microscopic observation system according to claim 1, wherein: The light source is an ultraviolet light source, and the wavelength of light emitted by the ultraviolet light source is between 200nm and 350nm; The first filter is a short-wave pass filter or a band-pass filter, and the maximum wavelength of light allowed to pass through the first filter does not exceed 550 nm.

4. The optical microscopic observation system according to claim 1, wherein: The light source is a full-spectrum light source; A second filter is provided between the light source and the beam splitter, the second filter being a bandpass filter, and the wavelength range of light allowed to pass through the second filter has a lower limit of 200-270 nm and an upper limit of 280-350 nm; The first filter is a short-wave pass filter or a band-pass filter, and the maximum wavelength of light allowed to pass through the first filter does not exceed 550 nm.

5. The optical microscopic observation system according to claim 1, wherein: The first filter is a short-wave pass filter or a band-pass filter, and the maximum wavelength of light allowed to pass through the first filter does not exceed 550 nm.

6. The optical microscopic observation system according to any one of claims 1 to 5, wherein: The material to be observed is graphene.

7. The optical microscopic observation system according to any one of claims 1 to 5, characterized in that: The device for growing the material to be observed comprises: A housing having an inner cavity; the housing having a first gas inlet, a first gas outlet, and a vacuum port; A workbench, disposed in the inner cavity, wherein a substrate required for the growth of the material to be observed is disposed on the workbench; a heater, the heater being disposed around the workbench and close to the substrate; an end cover, wherein the observation window is provided on the end cover, the end cover is provided on the housing, and closes the inner cavity; the orthographic projection of the substrate on the surface of the observation window is within the observation window; A gas dispersion plate is arranged between the heater and the end cover, the gas dispersion plate has a through hole, and the workbench passes through the through hole; a second gas inlet and a second gas outlet are provided on the gas dispersion plate, the second gas inlet is connected to the first gas inlet, and the second gas outlet is connected to the first gas outlet.

8. The optical microscopic observation system according to claim 7, wherein: The side wall of the shell is a double-layer hollow structure. A first coolant inlet and a first coolant outlet are provided on the side wall. The coolant flows through the side wall to reduce the temperature of the inner cavity.

9. The optical microscopic observation system according to claim 7, wherein: The gas dispersion plate includes two protrusions and a recessed portion, the through hole is located in the recessed portion, and the distance between the recessed portion and the inner surface of the end cover is greater than the distance between the protrusion and the inner surface of the end cover.

10. The optical microscopic observation system according to claim 7, wherein: The device for growing the material to be observed further comprises: The heat insulating member is arranged between the workbench and the observation window and supported by the recessed portion. The heat insulating member has an observation hole. The orthographic projection of the substrate on the surface of the observation window is located within the orthographic projection of the observation hole on the surface of the observation window.

11. The optical microscopic observation system according to claim 7, wherein: The device for growing the material to be observed further comprises: The support is arranged in the inner cavity and supports the workbench. The support can move three-dimensionally in the inner cavity.

12. The optical microscopic observation system according to claim 11, wherein: The device for growing the material to be observed further includes a support tube, which is arranged between the workbench and the bracket.

13. The optical microscopic observation system according to claim 11 or 12, wherein: The device for growing the material to be observed further includes a three-dimensional moving mechanism, which is connected to the bracket and drives the bracket to move three-dimensionally in the inner cavity to adjust the position of the workbench in the inner cavity.

14. The optical microscopic observation system according to claim 7, wherein: The heater includes an electromagnetic induction heater, a resistance wire heater or a heating belt.

15. The optical microscopic observation system according to claim 7, wherein: The observation window includes two layers of glass with a space between the two layers of glass. The end cover is provided with a second coolant inlet and a second coolant outlet. The coolant enters the space through the second coolant inlet to cool the two layers of glass, and then flows out from the second coolant outlet.

16. The optical microscopic observation system according to claim 7, wherein: The material of the workbench is graphite, corundum, quartz or silicon carbide.

17. The optical microscopic observation system according to claim 7, wherein: A seal is provided between the end cover and the shell, and the inner wall of the shell is provided with heat-insulating cotton.

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