Optical microscopic observation system and method

Abstract

The invention provides an optical microscopic observation system and method. 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 and method for observing high-temperature material preparation, chemical reaction and phase change process, and more specifically to an optical microscopic observation system and method. 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 deeply understanding 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, and real-time feedback on the state or change trend of materials is provided, 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 microscopic observation systems and applied to large-scale industrial manufacturing systems.

[0003] However, in-situ microscopic detection of high-temperature processes faces two major challenges: 1) The light (without valid information) generated by the thermal radiation (blackbody radiation) accompanying the high-temperature process will drown out the valid information and cause great interference to the observation; 2) To ensure the imaging quality, microscopic imaging requires a short working distance, while optical lenses cannot tolerate high-temperature environments, which puts extremely high demands on the heat preservation of high-temperature processes and short-distance thermal insulation. At present, there is an urgent need to develop high-quality imaging high-temperature optical microscopic observation systems and methods. Summary of the invention

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

[0005] Another object of the present application is to overcome at least one defect of the above-mentioned prior art, and to provide an optical microscopy observation method that can observe and clearly record high-temperature processes in real time, taking the in-situ observation of the high-temperature growth process of the material to be observed, graphene, as an example.

[0006] To achieve the above objectives, this application adopts the following technical solutions:

[0007] 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 comprises 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 to the surface of the material to be observed, and the material to be observed reflects the light and transmits it through the spectrometer. The first filter receives light that passes through the spectrometer. The imaging device receives light that passes through the first filter and images the material to be observed.

[0008] 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.

[0009] According to one embodiment of the present application, 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 shortwave pass filter or a bandpass filter, and the maximum wavelength of light allowed to pass through by the first filter does not exceed 550nm.

[0010] 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 wavelength range of light allowed to pass through by the second filter has a lower limit of 200-270nm and an upper limit of 280-350nm; the first filter is a shortwave pass filter or a bandpass filter, and the maximum wavelength of light allowed to pass through by the first filter does not exceed 550nm.

[0011] 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.

[0012] According to one embodiment of the present application, the material to be observed is graphene.

[0013] According to one embodiment of the present application, the growth device of 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.

[0014] 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.

[0015] 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.

[0016] According to one embodiment of the present application, the material growth device 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, and 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.

[0017] According to one embodiment of the present application, the device for growing the material to be observed further includes: a bracket, which is disposed in the inner cavity and supports the workbench, and the bracket can move three-dimensionally in the inner cavity.

[0018] According to one embodiment of the present application, the device for growing the material to be observed further includes a support tube, which is disposed between the workbench and the bracket.

[0019] 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 and drives the bracket to move three-dimensionally in the inner cavity to adjust the position of the workbench in the inner cavity.

[0020] According to one embodiment of the present application, the heater includes an electromagnetic induction heater, a resistance wire heater or a heating belt.

[0021] 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, and 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.

[0022] According to one embodiment of the present application, the material of the workbench is graphite, corundum, quartz or silicon carbide.

[0023] 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.

[0024] 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 reflected by the material to be observed and generated by the accompanying thermal radiation, an imaging device receives the light passing through the first filter and forms an image.

[0025] 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.

[0026] 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.

[0027] According to one embodiment of the present application, the material to be observed is graphene.

[0028] It can be seen from the above technical solutions that the advantages and positive effects of the optical microscopic observation system proposed in this application are:

[0029] The optical microscopic observation system proposed in the present application adopts a spectrometer and a first filter to observe the material to be observed through the observation window of the material growth device to be observed. 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 then passes through the spectrometer. The first filter receives the light that passes through the spectrometer, and the imaging device receives the light that passes through the first filter and images the material to be observed. It can be achieved that the material to be observed can be clearly observed under the high temperature state of the material to be observed, and the imaging process can be imaged on the imaging device. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] 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 attached drawings.

[0031] Figure 1 It is a schematic diagram of the structure of the optical part of the optical microscopic observation system of the present application.

[0032] Figure 2 It is a structural schematic diagram of the optical microscopic observation system of the present application.

[0033] Figure 3 yes Figure 2 Schematic diagram of the internal structure of the device for growing materials to be observed.

[0034] Figure 4 yes Figure 2 Schematic diagram of the structure of the material growth device to be observed after removing the end cover.

[0035] Figure 5 yes Figure 4 Schematic diagram of the structure of the growth device for the material to be observed with the thermal insulation removed.

[0036] Figure 6 yes Figure 5 Schematic diagram of the structure of the material growth device to be observed with the gas dispersion plate removed.

[0037] Figure 7 It is a schematic diagram of the structure of the gas dispersion plate of the device for growing the material to be observed in the present application.

[0038] Figure 8 This is the optical image of the 22um copper foil surface before pretreatment.

[0039] Fig. 9 This is the optical image of the 22um copper foil surface after pretreatment.

[0040] Fig.10 This is an optical image of the graphene film growing for 1 minute.

[0041] Fig.11 This is an optical image of the graphene film growing for 7 minutes.

[0042] Fig.12 This is an optical image of the graphene film growing for 14 minutes.

[0043] Fig.13 This is the Raman spectrum of graphene film.

[0044] Fig.14 This is a light microscope image of graphene film growth without using the optical microscopic observation system of the present application.

[0045] Fig.15 This is a light microscope image of graphene film growth using the optical microscopic observation system of the present application.

[0046] The reference numerals are described as follows:

[0047] 1- Optical part of the optical microscopy system;

[0048] 2-device for growing materials to be observed;

[0049] 10- Light source;

[0050] 20-beam splitter;

[0051] 30- Materials to be observed;

[0052] 40-a first filter;

[0053] 50- imaging device;

[0054] 60- a second filter;

[0055] 21-housing;

[0056] 22- workbench;

[0057] 23-heater;

[0058] 24-end cover;

[0059] 25-gas dispersion plate;

[0060] 26- thermal insulation;

[0061] 27-Stand;

[0062] 28-support tube;

[0063] 29- three-dimensional moving mechanism;

[0064] 210 - first gas inlet;

[0065] 211-first gas outlet;

[0066] 212-vacuum port;

[0067] 213 - side wall of the housing;

[0068] 214 - first coolant inlet;

[0069] 221-substrate;

[0070] 231-heater lead-out terminal;

[0071] 241-Observation window;

[0072] 242 - second coolant inlet;

[0073] 243 - second coolant outlet;

[0074] 244-Seal;

[0075] 250-through hole;

[0076] 251 - second gas inlet;

[0077] 252-second gas outlet;

[0078] 253- protrusion;

[0079] 254-depression;

[0080] 255-flow plate;

[0081] 261-Observation hole;

[0082] 291- bellows;

[0083] 300-base. DETAILED DESCRIPTION

[0084] Example embodiments will now be described more fully with reference to the accompanying drawings. However, example embodiments can be implemented in a variety of forms and should not be construed as limited to the embodiments set forth herein; rather, these embodiments are provided so that this application will be comprehensive and complete and fully convey the concepts of the example embodiments to those skilled in the art. The same reference numerals in the figures represent the same or similar structures, and thus their detailed description will be omitted.

[0085] 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 multiple 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. can be used in this specification to describe different exemplary features and elements of the present application, these terms are used herein only for convenience, such as according to the direction 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.

[0086] 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 device that includes a series of steps or units is not limited to the listed steps or units, but may optionally include steps or units that are not listed, or may optionally include other steps or components that are inherent to these processes, methods, products, or devices.

[0087] Relative terms such as "under" 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 one figure is turned over, the element described as being "under" or "bottom" of other elements will be oriented "on" or "top" of other elements. Therefore, the exemplary term "under" may include the orientations of "under" and "top", and the term "bottom" may include the orientations of "bottom" and "top", depending on the specific orientation of the figure. Similarly, if the device in one figure is turned over, the element described as being "under" or "bottom" of other elements will be oriented to be "on" or "top" of other elements. Therefore, the exemplary terms "bottom" or "below" may include the orientations of top and bottom.

[0088] like Figure 1 to Figure 2 As shown, the optical microscopic observation system of the present application is used to observe the growth process of the 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 and reflecting three-dimension beam splitter or a five-transmitting and reflecting five-dimension beam splitter. In other embodiments, the beam splitter can also use other types of beam splitters. The beam splitter 20 receives the light emitted by the light source 10 and reflects the light to the surface of the material to be observed 30. The material to be observed 30 reflects the light and then passes through the beam splitter 20. The first filter 40 receives the light passing through the beam splitter 20 and shields the stray light (mostly red light and infrared light) generated by the accompanying thermal radiation in the light passing through the beam splitter. The imaging device 50 receives the light passing through the first filter 40 and images the growth process of the material to be observed 30. The material to be observed 30 is arranged in the material to be observed growth device 2. The material to be observed growth device 2 includes an observation window 241, and the material to be observed is observed through the observation window 241.

[0089] The optical microscopic observation system of the present application adopts a beam splitter 20 and a first filter 40. The beam splitter 20 receives the light emitted by the light source 10 and reflects the light to 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 shields the stray light (mostly red light and infrared light) generated by the accompanying 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 the growth process of the graphene film to be clearly observed under the high temperature state of the graphene film growth.

[0090] The optical microscopic observation system of the present application can shield the thermal radiation generated by the high temperature during the growth of graphene films, and utilizes the different transmittances of graphene films with different numbers of layers in the UV band, selects a camera with excellent imaging capabilities in the visible light and UV bands, and uses a metallographic microscope to observe the growth of graphene, with clear images. It can also clearly observe the growth process of graphene films with a size exceeding 1cm×1cm in real time.

[0091] In the present embodiment, the light source 10 is a full-spectrum light source, the first filter 40 is a short-wave pass filter or a band-pass filter, and the maximum wavelength of the light allowed to pass through the first filter 40 does not exceed 550nm. Specifically, it can be a short-wave pass filter with a cut-off wavelength of 532nm, a band-pass filter of 330nm-410nm, a band-pass filter of 380nm-435nm, a band-pass filter of 400nm-495nm, etc. The first filter can shield the stray light (mostly red light and infrared light) generated by thermal radiation, so that the imaging is clear. In the present embodiment, the light source 10 is a full-spectrum light source, and a second filter 60 is arranged between the light source 10 and the spectrometer 20. The second filter 60 is a band-pass filter. The lower limit of the wavelength range of the light allowed to pass through by the second filter 60 is between 200nm-270nm, for example, 250nm, 260nm, and the upper limit is between 280nm-350nm, for example, 290nm, 300nm. Can further improve the clarity of the observation system.

[0092] In some other embodiments, the light source 10 is an ultraviolet light source, so that the light received by the spectrometer 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 shortwave pass filter or a bandpass filter, and the maximum wavelength of light allowed to pass through the first filter 40 does not exceed 550nm, specifically, it can be a shortwave pass filter with a cut-off wavelength of 532nm, a bandpass filter of 330nm-410nm, a bandpass filter of 380nm-435nm, a bandpass filter of 400nm-495nm, etc., which can shield the stray light (mostly red light and infrared light) generated by thermal radiation, so that the imaging is clear.

[0093] 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 550 nm.

[0094] In this embodiment, the direction in which the beam splitter 20 receives the light emitted by the light source 10 is at an angle of 45° to the normal direction of the beam splitter 20. In this way, the beam splitter 20 can completely reflect the light transmitted by the light source 10. In this embodiment, the beam splitter 20 is a seven-transmitting and five-reflecting beam splitter or a five-transmitting and five-reflecting beam splitter, which has a good light processing effect.

[0095] In this embodiment, the material to be observed 30 is a graphene film. The optical microscopic observation system of the present application takes the observation of the in-situ growth of a graphene film as an example, and the observation system of the present application is not limited to the observation of the growth of a graphene film, but can also observe the growth of other materials to be observed.

[0096] In this embodiment, the imaging device 50 can be an ultraviolet camera, a tube lens can be arranged between the imaging device 50 and the first filter 40, an aperture stop can be arranged between the beam splitter 20 and the first filter 40, and an objective lens can be arranged between the material to be observed 30 and the beam splitter 20.

[0097] In this embodiment, if Figure 2 , Figure 3 , Figure 5 and Figure 7 As shown, the optical microscopic observation system also includes a growth device 2 for the material to be observed, wherein the growth device 2 for the material 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 positive 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 directly opposite to 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.

[0098] 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 inner cavity of the shell 21 close to the observation window 241 being too high, thereby affecting the clarity of the picture of the growth of the graphene film taken by the observation window 241.

[0099] In this embodiment, see Figure 3The side wall 213 of the housing 21 is a double-layer hollow structure, and a first coolant inlet 214 and a first coolant outlet (not shown in the figure) are provided on the side wall 213. The coolant flows through the side wall 213 to reduce the temperature of the inner cavity. The side wall 213 of the housing 21 is designed as a hollow liquid cooling mode, which can timely reduce the temperature of the inner cavity and further reduce the high temperature effect on the observation window 241 during the growth of the graphene film.

[0100] 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 to have a recessed portion 254 between the two protrusions 253, so that the gas can be gathered around the substrate 221 where the graphene film is grown, which can reduce the amount of gas used and reduce costs. Figure 7 As shown, a flow plate 255 is further provided between the second gas inlet 251 on the recess 254 and the through hole 250 to evenly 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.

[0101] In this embodiment, if Figure 3 , Figure 4 and Figure 5 As shown, the material growth device 2 to be observed also includes a heat insulating member 26, which is arranged between the workbench 22 and the observation window 241 and supported by the recessed portion 254. The heat insulating member 26 has an observation hole 261. 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 to the substrate 221. The setting 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 heat 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 by the recessed portion 254 of the gas dispersion plate 25, and the heat insulating member 26 is suspended above the substrate 221.

[0102] In this embodiment, see Figure 3 and Figure 6 The device 2 for growing materials to be observed further includes a support 27, which is arranged in the inner cavity and supports the workbench 22. The support 27 can move three-dimensionally (in the XYZ direction) in the inner cavity. The setting of the support 27 can adjust the position of the workbench 22 in the inner cavity according to actual conditions, so that the device 2 for growing materials to be observed can be applied to different materials 30 to be observed.

[0103] In this embodiment, the growth device 2 for the material to be observed 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.

[0104] In this embodiment, the growth device 2 of the material to be observed further includes a three-dimensional moving mechanism 29, which is connected to the bracket 27. The three-dimensional moving mechanism 29 drives the bracket 27 to move three-dimensionally in the inner cavity to adjust the position of the workbench 22 in the inner cavity. A bellows 291 is provided between the three-dimensional moving mechanism 29 and the shell 21. The bracket 27 includes a crossbeam in contact with the support tube 28, a vertical beam connected to the end of the crossbeam, and a connecting piece connected to the end of the vertical beam. The connecting piece passes through the bellows 291 to connect the three-dimensional moving mechanism 29.

[0105] 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) 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.

[0106] When the carbon source for preparing graphene is a liquid carbon source, such as ethanol, a hole can be opened at an appropriate position on the side wall 213 of the housing 21 of the material growth device 2 to be observed in the present application, and a front heating chamber is connected through the hole, and the front heating chamber can sublime the liquid carbon source such as ethanol. This is a dual-temperature zone series structure. A multi-temperature zone series structure can also be used.

[0107] In this embodiment, see Figure 2 The observation window 241 includes two layers of glass with a space between the two layers of glass. The end cover 24 is provided with a second coolant inlet 242 and a second coolant outlet 243. The coolant enters the space through the second coolant inlet 242 to cool the two layers of glass, and then flows out through the second coolant outlet 243. This design is a cooling design for the glass of the observation window 241, which is conducive to taking clear pictures through the observation window 241.

[0108] In this embodiment, a seal 244 is provided between the end cover 24 and the housing 21 , and a 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 .

[0109] It should be noted that the optical microscopic observation systems shown in the drawings and described in this specification are only a few examples of the many optical microscopic observation systems that can employ the principles of the present application. It should be clearly understood that the principles of the present application are by no means limited to any details of the optical microscopic observation systems shown in the drawings or described in this specification or any components of the optical microscopic observation systems.

[0110] The above is a detailed description of several exemplary embodiments of the optical microscopic observation system proposed in the present application. The following is an exemplary description of the use process of the optical microscopic observation system of the present application.

[0111] Combined with Figures 1 to 7 The optical microscopic observation system proposed in the present 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 the present application, and the growth process is:

[0112] This embodiment is described using a copper foil with a thickness of 22 um as the substrate 221. The substrate 221 may also be other metal foils, or fiber fabrics, etc. The thickness may be 10 um-100 um.

[0113] The pretreatment process of the substrate 221 is as follows: the copper foil is placed in the material growth device 2 to be observed, the vacuum control device is turned on, and the inside of the shell 21 is evacuated from the vacuum port 212 to make the pressure in the inner cavity of the shell 21 in a low vacuum state, for example, 1-20 kPa. After the pressure is stable, the optical part 1 of the optical microscope observation system is turned on to observe the surface of the copper foil. Figure 8 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.

[0114] The heater 23 is turned on for heating, and an appropriate amount of argon (20sccm-2000sccm) and diluted oxygen (2sccm-200sccm) 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. Then, the argon and diluted oxygen are turned off, and hydrogen (3sccm-600sccm) is introduced for the first annealing for 3-20min. After the first annealing is completed, hydrogen (3sccm-600sccm) and diluted oxygen (2sccm-200sccm) are introduced for the second annealing for 2-100min until the surface of the copper foil becomes relatively flat, such as Fig. 9 shown.

[0115] After the substrate 221 is pretreated, the graphene film is grown at the target temperature (100°C-3000°C). The gases introduced at this time include but are not limited to argon, diluted oxygen, methane, diluted methane, acetylene, diluted acetylene, hydrogen, etc., and an ultraviolet camera (ULTRAVIOLET CAMERA) is used to observe the growth of graphene films with different numbers of layers. Fig.10 This is an optical image of the graphene film growing for 1 minute. Fig.11 This is an optical image of the graphene film growing for 7 minutes. Fig.12 This is an optical image of the graphene film growing for 14 minutes.

[0116] After the growth is completed, only argon gas (20sccm-2000sccm) is introduced to cool down. After it drops to room temperature, the copper foil is taken out to characterize the graphene film. Fig.13 is the Raman spectrum of graphene film.

[0117] The optical microscopic observation system of the present application can observe the growth process of the material 30 to be observed, and can also observe the growth process of the graphene film grown on the copper foil under high temperature conditions, and can realize the visualization of the growth process of the graphene film using a metallographic microscope, thereby reducing costs, having high imaging resolution, and providing clear images. The optical microscopic observation system of the present application can observe the changes in the surface of the substrate 221 during the entire growth process of the graphene film.

[0118] In order to further understand the content of this application, this application is now described in detail in conjunction with specific embodiments. It should be noted that due to limited space here, only some embodiments are listed below, in which the optical microscopic observation system and various parameters during the growth of the material 30 to be observed are not limited to the following specific embodiments.

[0119] Embodiment 1

[0120] Place the copper foil in the material growth device 2 to be observed, turn on the vacuum control device, and evacuate the inside of the shell 21 from the vacuum port 212 to make the pressure in the inner cavity of the shell 21 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.

[0121] 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. Subsequently, 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.

[0122] After the substrate 221 is pretreated, the graphene film is 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.

[0123] After the growth is completed, only 100 sccm of argon gas is introduced to cool down. After it drops to room temperature, the copper foil is taken out to characterize the graphene film.

[0124] Embodiment 2

[0125] Place the copper foil in the material growth device 2 to be observed, turn on the vacuum control device, and evacuate the inside of the shell 21 from the vacuum port 212 to make the pressure in the inner cavity of the shell 21 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.

[0126] 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, so that the temperature in the inner cavity of the shell 21 rises to 900°C and is maintained, 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.

[0127] After the substrate 221 is pretreated, the graphene film is grown at 900° 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.

[0128] After the growth is completed, only 100 sccm of argon gas is introduced to cool down. After it drops to room temperature, the copper foil is taken out to characterize the graphene film.

[0129] Embodiment 3

[0130] Place the copper foil in the material growth device 2 to be observed, turn on the vacuum control device, and evacuate the inside of the shell 21 from the vacuum port 212 to make the pressure in the inner cavity of the shell 21 in a low vacuum state, for example, 15 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.

[0131] 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, so that the temperature in the inner cavity of the shell 21 rises to 1000°C and is maintained. Subsequently, 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.

[0132] After the substrate 221 is pretreated, the graphene film is 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.

[0133] After the growth is completed, only 1000 sccm of argon gas is introduced to cool down. After it drops to room temperature, the copper foil is taken out to characterize the graphene film.

[0134] Embodiment 4

[0135] Place the copper foil in the material growth device 2 to be observed, turn on the vacuum control device, and evacuate the inside of the shell 21 from the vacuum port 212 to make the pressure in the inner cavity of the shell 21 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.

[0136] 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.

[0137] After the substrate 221 is pretreated, the graphene film is grown at 1500° C., and 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.

[0138] After the growth is completed, only 1500 sccm of argon gas is introduced to cool down. After it drops to room temperature, the copper foil is taken out for characterization of the graphene film.

[0139] Through the description of the optical part 1 and the growth device 2 of the material to be observed of the optical microscopic observation system of the present application, it can be concluded that the optical microscopic observation system of the present application adopts a beam splitter 20 and a first filter 40, wherein the beam splitter 20 receives the light emitted by the light source 10 and reflects the light to the surface of the material to be observed 30, and the material to be observed 30 reflects the light and then transmits 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 can clearly observe the growth process of the graphene film under the high temperature state of the growth of the graphene film.

[0140] The optical microscopic observation method for observing the growth process of the material to be observed in the present application is as follows: Figure 1 As shown, after the light is irradiated to the surface of the material to be observed 30, the material to be observed 30 reflects the light (including the light generated by the thermal radiation of the material to be observed) to the first filter 40. After the first filter 40 shields the red light and infrared light generated by the thermal radiation in the light reflected by the material to be observed 30, the imaging device 50 receives the light passing through the first filter 40 and forms an image. The above method can shield the thermal radiation generated by the high temperature during the growth of the graphene film. By using the different transmittance of graphene films with different numbers of layers in the UV band, a camera with excellent imaging capabilities in the visible light and UV bands is selected, and the graphene growth is observed using a metallographic microscope, and the image is clear. It is also possible to clearly observe the growth process of graphene films with a size exceeding 1cm×1cm in real time.

[0141] In this embodiment, the light irradiated to the surface of the material to be observed 30 is ultraviolet light, and a second filter 60 can be provided between the full-spectrum light source and the spectrometer, so that the light irradiated to the surface of the material to be observed 30 is ultraviolet light. In some other embodiments, the light irradiated to the surface of the material to be observed 30 is full-spectrum light.

[0142] The optical microscopic observation method for observing the growth process of the material to be observed in the present application is to turn off the light source 10 under the above optical microscopic observation system and observe the growth process of the material to be observed 30. In this observation method, the light source 10 is not set, and the different infrared radiation capabilities of the graphene film and the substrate 221 (copper foil) under high temperature heating can be used for imaging.

[0143] In this embodiment, the material to be observed 30 is graphene, or may be silicon carbide or the like.

[0144] 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:

[0145] See also Fig.14 , Fig.14This is a light microscope image of graphene film growth without using the optical microscopic observation system of the present application. Fig.14 It can be seen from the optical microscope image of graphene film growth without the optical microscope observation system of the present application that the image is blurred and has a low resolution.

[0146] In comparison, Fig.15 This is a light microscope image of graphene film growth using the optical microscopic observation system of the present application, Fig.15 It can be seen that the graphene film growth picture observed by the optical microscope observation system of the present application has a clear image and a high resolution.

[0147] 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 transmitted through the spectrometer. The imaging device receives the light transmitted 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 growth of the graphene film. And the size of the heater will not be reduced. For graphene films with a size exceeding 1cm×1cm, pictures of the growth process of the graphene film can still be clearly taken.

[0148] The optical microscopic observation method for observing the growth process of the material to be observed in the present application, after light is irradiated to the surface of the material to be observed, the material to be observed reflects light to the first filter, and after the first filter shields the red light and infrared light generated by the accompanying thermal radiation in the light reflected by the material to be observed, the imaging device receives the light passing through the first filter and forms an image. The above method can shield the thermal radiation generated by the high temperature during the growth of the graphene film, and utilizes the different transmittance of graphene films with different numbers of layers in the UV band, selects a camera with excellent imaging capabilities in the visible light and UV bands, and uses a metallographic microscope to observe the growth of graphene, and the image is clear. It can also clearly observe the growth process of graphene films with a size exceeding 1cm×1cm in real time.

[0149] 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.

[0150] It is understandable that the various embodiments / implementations provided in the present application can be combined with each other without causing any contradiction, and will not be illustrated one by one here.

[0151] In the above exemplary embodiments, the optical microscopic observation system proposed in the present application is described by taking the application to observe graphene film as an example. It is easy for those skilled in the art to understand that in order to apply the relevant design of the present application to other types of materials to be observed, various modifications, additions, substitutions, deletions or other changes are made to the specific embodiments, and these changes are still within the scope of the principle of the optical microscopic observation system proposed in the present application.

[0152] It should be noted that the optical microscopic observation systems shown in the drawings and described in this specification are only a few examples of the many optical microscopic observation systems that can adopt the principles of the present application. It should be clearly understood that the principles of the present application are by no means limited to any details or any components of the optical microscopic observation systems shown in the drawings or described in this specification.

[0153] In the application embodiments, 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. The terms "installed", "connected", "connected", "fixed", etc. should be understood in a broad sense. For example, "connected" can be a fixed connection, a detachable connection, or an integral connection; "connected" can be a direct connection or an indirect connection through an intermediate medium. For those of ordinary skill in the art, the specific meanings of the above terms in the application embodiments can be understood according to the specific circumstances.

[0154] In the description of the application embodiments, it should be understood that the terms "up", "down", "left", "right", "front", "back", "top", "bottom", etc. indicate directions or positional relationships based on the directions or positional relationships shown in the accompanying drawings. They are only for the convenience of describing the application embodiments and simplifying the description, and do not indicate or imply that the device or unit referred to must have a specific direction, be constructed and operated in a specific orientation. Therefore, they should not be understood as limitations on the application embodiments.

[0155] In the description of this specification, the description of the terms "one embodiment", "some embodiments", "specific embodiments", etc. means 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 may be combined in any one or more embodiments or examples in a suitable manner.

[0156] The above are only preferred embodiments of the application embodiments and are not intended to limit the application embodiments. For those skilled in the art, the application embodiments may have various modifications and changes. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the application embodiments shall be included in the protection scope of the application embodiments.

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 receives the light emitted by the light source and reflects the light to the surface of the material to be observed, and the material to be observed reflects the light and then passes through 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, characterized in that: 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, characterized in that: 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, characterized in that: 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 is a bandpass filter, and the wavelength range of light allowed to pass through by the second filter has a lower limit of 200nm-270nm and an upper limit of 280nm-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.

5. The optical microscopic observation system according to claim 1, characterized in that: 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, characterized in that: 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 shell having an inner cavity; the shell having a first gas inlet, a first gas outlet and a vacuum port; A workbench, arranged in the inner cavity, wherein the workbench is provided with a substrate required for the growth of the material to be observed; a heater, the heater being arranged around the workbench and close to the substrate; an end cover, the observation window is arranged on the end cover, 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; 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 arranged 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, characterized in that: The side wall of the shell is a double-layer hollow structure. A first coolant inlet and a first coolant outlet are arranged 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, characterized in that: 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, characterized in that: The device for growing the material to be observed further comprises: A 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, characterized in that: The device for growing the material to be observed further comprises: A support is arranged in the inner cavity and supports the workbench, and the support can move three-dimensionally in the inner cavity.

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

13. The optical microscopic observation system according to claim 11 or 12, characterized in that: The device for growing the material to be observed further comprises 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, characterized in that: 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, characterized in that: 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, characterized in that: The material of the workbench is graphite, corundum, quartz or silicon carbide.

17. The optical microscopic observation system according to claim 7, characterized in that: A seal is arranged between the end cover and the shell, and a heat-insulating cotton is arranged on the inner wall of the shell.

18. An optical microscopic observation method for observing the growth process of a material to be observed, characterized in that: In the optical microscopic observation system of any one of claims 1 to 4, light is irradiated onto the surface of the material to be observed, and the surface of the material to be observed reflects the light to the first filter. After the first filter shields the red light and infrared light reflected by the material to be observed and generated by the accompanying thermal radiation, the imaging device receives the light passing through the first filter and forms an image.

19. The optical microscopic observation method according to claim 18, characterized in that: The light irradiated onto the surface of the material to be observed is full-spectrum light or ultraviolet light.

20. An optical microscopic observation method for observing the growth process of a material to be observed, characterized in that: In the optical microscopic observation system as described in claim 1 or 5, the light source is turned off and the growth process of the material to be observed is observed.

21. The optical microscopic observation method according to any one of claims 18 to 20, characterized in that: The material to be observed is graphene.

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