Camera shooting observation device for combustion synthesis reaction kettle

Abstract

The invention provides a camera shooting observation device for a combustion synthesis reaction kettle. The camera shooting observation device comprises a shell; the shell comprises a cooling channel; a water inlet and a water outlet which are communicated with the cooling channel are formed in the shell; a camera device with adjustable focal length and contrast ratio is arranged in the shell; the camera shooting observation device further comprises a window sheet fixed on the shell through a connecting piece. The window sheet, the connecting piece and the shell are enclosed to form a closed space for accommodating and fixing the camera device; and the window sheet is correspondingly matched with the camera device. The camera shooting observation device can be installed in a silicon nitride powder combustion synthesis reaction kettle and can normally work in the environment with the environment temperature being 300 DEG C or above and the existence of ammonium-containing corrosion salt.

Description

Technical Field

[0001] The present invention relates to the technical field of silicon nitride powder combustion synthesis, and more specifically to a video observation device for a combustion synthesis reactor. Background Art

[0002] Silicon nitride powder combustion synthesis technology is regarded as an ideal method for preparing silicon nitride powder due to its significant advantages such as low cost and short cycle. As an important branch of combustion synthesis technology, gas-solid combustion synthesis has played an increasingly important role in the field of ceramic powder preparation. In addition to silicon nitride, this technology can also be used to prepare a variety of ceramic powders such as silicon carbide, boron nitride, aluminum nitride, and can even be used to synthesize high-quality graphene. Although gas-solid combustion synthesis technology has highlighted its potential value, there are still some technical problems that must be solved, the most notable of which is the problem of equipment and process matching.

[0003] Generally speaking, gas-solid combustion synthesis reaction needs to be carried out in a high-pressure combustion synthesis reactor, in which the high-pressure gas environment is a necessary condition to ensure that the reaction is carried out. At the same time, in order to ensure that the reaction is carried out according to the designed path, corrosive ammonium salts are also added to the raw materials. Such extreme conditions also greatly increase the difficulty of detecting the reaction process. With the continuous advancement of the combustion synthesis silicon nitride powder technology, many advances have been made in combustion synthesis equipment. However, the process monitoring of combustion synthesis has always remained at the temperature monitoring stage (CN200920046507.5). Video observation of the combustion propagation process is an effective means to study combustion propagation, but it is limited to the extreme environment of high temperature, high pressure and even corrosive gases in the reactor, and the difficulty of realizing this means is greatly increased. Therefore, a camera device with multiple protections is needed to achieve the purpose of recording the combustion propagation process. Summary of the invention

[0004] In view of the above problems, the present invention provides a video observation device for a combustion synthesis reactor which can be installed in the combustion synthesis reactor and can work normally in an environment with an ambient temperature of more than 300°C and the presence of ammonium corrosive salts.

[0005] To achieve the above object, the present invention adopts the following technical solutions:

[0006] The present invention provides a video observation device for a combustion synthesis reactor, comprising:

[0007] case;

[0008] The housing includes a cooling channel;

[0009] The shell is formed with a water inlet and a water outlet which are in communication with the cooling channel;

[0010] A camera device with adjustable focus and contrast is installed in the housing;

[0011] The video observation device also includes a window fixed to the shell through a connector; the window, the connector and the shell together form a closed space to accommodate and fix the video device; the window corresponds to the video device.

[0012] Preferably, the housing comprises an outer shell and an inner shell located inside the outer shell;

[0013] The cooling channel is located between the outer shell and the inner shell; the water inlet and the water outlet are formed on the outer shell;

[0014] The window piece is fixed on the inner shell through a connecting piece; the inner shell is fixed to the outer shell through the connecting piece; the window piece, the connecting piece and the inner shell are enclosed to form a closed space to accommodate a fixed camera device.

[0015] A preferred solution is that the window is located at the front side of the inner shell and corresponds to the front end of the lens of the camera device.

[0016] A preferred solution is that the window piece is made of quartz glass; and the thickness of the window piece is 20 to 30 mm.

[0017] A preferred solution is that an opening corresponding to the window piece is formed at the front end of the shell; the connecting member is fixed at the opening position of the shell; the window piece is fixed on the connecting member and an avoidance opening corresponding to the window piece is formed on the connecting member.

[0018] A preferred solution is that a detachable outer rear cover is provided at the rear end of the housing, a rubber sealing protective sleeve is provided inside the outer rear cover, and the outer rear cover is threadedly connected to the housing;

[0019] A detachable inner rear cover is arranged at the rear end of the inner shell, a rubber sealing protective sleeve is arranged inside the inner rear cover, and the inner rear cover is threadedly connected to the inner shell.

[0020] A preferred solution is that the video observation device includes a water-cooling jacket located between the outer shell and the inner shell; the inner cavity of the water-cooling jacket forms the cooling channel.

[0021] The preferred solution is that it also includes a terminal penetrating the side wall of the reactor and an electromagnetic shielding wire for connecting a camera device; a polytetrafluoroethylene sealing ring is sleeved on the terminal; and the electromagnetic shielding wire extends to the outside of the reactor through the terminal.

[0022] A preferred solution is that the water outlet and the water inlet are both connected to external water pipes for cooling water circulation; the water pipes extend to the outside of the reactor through terminal posts.

[0023] The present invention further provides a combustion synthesis reactor, comprising the above-mentioned video observation device, wherein a through hole is provided on the side wall of the combustion synthesis reactor for accommodating the terminal of the video observation device.

[0024] The beneficial effects of the present invention are:

[0025] The invention provides a camera device which can work normally in a high-temperature and high-pressure combustion synthesis reactor. The external temperature can be well isolated by a shell. Cooling water is injected into a cooling channel through a water inlet. The cooling water circulates in the cooling channel and finally flows out from a water outlet, thereby achieving a water cooling effect. A closed space is formed by enclosing a window sheet, a connector and an inner shell to accommodate, fix and protect the camera device. The camera device is matched with a camera with adjustable focal length and contrast, so that the camera device can observe and record the image of the propagation of the combustion wave in the combustion process in the combustion synthesis reactor in real time in an environment of high temperature, high pressure and corrosive medium, thereby realizing the monitoring of the combustion propagation rate of silicon nitride powder and the analysis of the reaction process. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] The specific implementation modes of the present invention are further described in detail below in conjunction with the accompanying drawings.

[0027] Figure 1 It is a schematic diagram of the overall structure of the present invention.

[0028] Figure 2A-2D This is one of the combustion spread images observed using the camera device of the present invention.

[0029] Figure 3 This is the second image of the spread of combustion observed by using the camera device of the present invention. DETAILED DESCRIPTION

[0030] Various exemplary embodiments of the present invention will now be described in detail with reference to the accompanying drawings. It should be noted that the relative arrangement of components and steps, numerical expressions and numerical values ​​set forth in these embodiments do not limit the scope of the present invention unless otherwise specifically stated.

[0031] The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses.

[0032] Techniques and equipment known to ordinary technicians in the relevant art may not be discussed in detail, but where appropriate, the techniques and equipment should be considered part of the specification.

[0033] In all examples shown and discussed herein, any specific values ​​should be interpreted as merely exemplary and not limiting. Therefore, other examples of the exemplary embodiments may have different values.

[0034] It should be noted that like reference numerals and letters refer to similar items in the following figures, and therefore, once an item is defined in one figure, it need not be further discussed in subsequent figures.

[0035] If the combustion process cannot be monitored intuitively and dynamically, the understanding of the combustion process can only remain at the theoretical analysis stage, and the synthesis process cannot be precisely controlled, which will result in the quality and stability of the materials prepared by combustion synthesis being unguaranteed. Therefore, it is very important to develop a real-time monitoring device for the gas-solid combustion synthesis process and realize in-situ observation of the propagation of the combustion wave, in order to understand the combustion reaction process and improve the combustion synthesis equipment.

[0036] In order to observe the reaction conditions in a high-temperature and high-pressure combustion synthesis reactor, the present invention provides a video observation device for a combustion synthesis reactor. Taking the synthesis reaction of silicon nitride powder as an example, combined with Figures 1 to 3 As shown, a video observation device for a combustion synthesis reactor is specifically described, including: a shell, the shell is made of 316 stainless steel, and has the characteristics of high temperature and high pressure resistance and corrosion resistance; the shell includes a cooling channel 12; the shell is formed with a water inlet and a water outlet connected to the cooling channel 12; the video observation device also includes a window 14 fixed to the shell by a connector 15; the window 14, the connector 15 and the shell are enclosed to form a closed space to accommodate a fixed video device 13, and the window 14 corresponds to the video device 13. The video device 13 is a miniature camera with adjustable focal length and adjustable contrast installed inside the shell. It should be noted that Figure 1 In the figure, the camera device 13 is located in a pressure vessel, which is a silicon nitride powder combustion synthesis reactor. The working gas medium in the reactor is a mixture of one or more of N2, Ar, CO2, and H2; the working pressure of the camera device 13 is 0 to 8 MPa; the working temperature of the camera device 13 is -20 to 350°C, and the above working pressure and working temperature refer to the pressure and temperature of the gas inside the reactor.

[0037] The outer shell of the video observation device is a stainless steel structure with a thickness of more than 5 mm, and the front of the camera is a quartz glass with a thickness of 20 to 30 mm. The above stainless steel structure and quartz glass can withstand a pressure of 0 to 10 MPa; the video observation device has a water cooling function, and the entire device can be cooled by external circulating water, so that it can work stably at a high temperature of 350°C.

[0038] In the above embodiment, the shell includes an outer shell 1 and an inner shell 2 located inside the outer shell 1; the cooling channel 12 is located between the outer shell 1 and the inner shell 2; the water inlet and the water outlet are formed on the outer shell 1; the window 14 is fixed to the inner shell 2 through a connector 15, and the window 14 and the outer shell 1 are sealed by the connector 15 and a rubber sealing ring; the inner shell 2 is combined and fixed to the outer shell 1 through the connector 15; the inner shell 2 is threadedly connected to the connector 15; the outer shell 1 is connected to the connector 15 by welding; the window 14, the connector 15 and the inner shell 2 enclose a closed space to accommodate and fix the camera device 13; the camera device 13 is fixed to the shell through a limiting sealing ring 16, specifically, it is fixed to the inner shell 2 through a limiting sealing ring 16 arranged outside the camera.

[0039] Furthermore, the window 14 is located at the front side of the inner shell 2 and corresponds to the front end of the lens of the camera device 13, ensuring that the camera device 13 can clearly and completely obtain the image of the propagation of the combustion wave and realize the observation of the interior of the reactor.

[0040] In a specific embodiment, the window 14 is made of quartz glass; the thickness of the window 14 is 20-30 mm, and the window 14 can effectively reduce the heat transfer during the heat transfer process and play a role in heat insulation. More specifically, quartz glass is made by melting various pure natural quartz (such as crystal, quartz sand, etc.), and has a very small linear expansion coefficient, which is one tenth to one twentieth of ordinary glass. It has good thermal shock resistance and high heat resistance. The regular use temperature is 1100-1200 degrees Celsius, and the short-term use temperature can reach 1400 degrees Celsius. Quartz glass is mainly used for laboratory equipment and special high-purity product refining equipment. Because it has high spectral transmittance, it will not be damaged by radiation.

[0041] In a specific embodiment, an opening corresponding to the window piece 14 is formed at the front end of the shell 1; the connecting member 15 is fixed at the opening position of the shell 1; the window piece 14 is fixed on the connecting member 15 and an avoidance opening corresponding to the window piece 14 is formed on the connecting member 15, thereby ensuring that the lens of the camera device 13 is not blocked, affecting the camera device 13 from obtaining a complete image.

[0042] In a specific embodiment, a removable outer rear cover 4 is provided at the rear end of the outer shell 1, a rubber sealing protective sleeve is provided inside the outer rear cover 4, and the outer rear cover 4 is threadedly connected to the outer shell 1; a removable inner rear cover 9 is provided at the rear end of the inner shell 2, a rubber sealing protective sleeve is provided inside the inner rear cover 9, and the inner rear cover 9 is threadedly connected to the inner shell 2; the outer rear cover 4 and the inner rear cover 9 correspond in position; the above-mentioned rubber sealing protective sleeve can realize the extension of the circuit into the shell and electrically connected to the camera device 13 while ensuring that the interior of the shell is still a sealed environment.

[0043] In a specific embodiment, the video observation device includes a water-cooling jacket located between the outer shell 1 and the inner shell 2; the inner cavity of the water-cooling jacket forms the cooling channel 12, and the water temperature of the cooling water in the cooling channel 12 is constant at 20-25°C, thereby ensuring the cooling effect on the video device 13; the cooling water can continuously absorb heat, and by changing the flow rate of the cooling water, the efficiency of heat absorption can be changed, thereby flexibly absorbing heat according to the ambient temperature.

[0044] In order to enable the lines and pipelines to enter the reactor, the video observation device also includes a terminal 6 that passes through the side wall 8 of the reactor and an electromagnetic shielding wire 5 for connecting the camera 13, and the electromagnetic shielding wire 5 can avoid unstable signal transmission; a polytetrafluoroethylene sealing ring 7 is sleeved on the terminal 6 to ensure the sealing of the connection between the terminal 6 and the side wall 8 of the reactor; the electromagnetic shielding wire 5 extends to the outside of the reactor through the terminal 6; specifically, the electromagnetic shielding wire 5 and the water pipe are extended to the outside of the side wall 8 of the reactor through the terminal 7; further, the present invention also provides a combustion synthesis reactor, including the video observation device as described above, the side wall of the combustion synthesis reactor is provided with a through hole for accommodating the terminal 6 of the video observation device; a through hole is provided on the side wall 8 of the reactor for accommodating the terminal 6 of the video observation device, the through hole is generally designed on the side wall 8 of the reactor, mainly to facilitate the camera to observe the reaction process from the side or above of the material, and the terminal 6 is fastened to the side wall 8 of the reactor by a fastening nut 17 outside the reactor. It should be noted that a display can also be provided and electrically connected to the camera device 13, so as to realize real-time viewing of the videos and pictures taken by the camera remotely, which is convenient and quick.

[0045] In a specific embodiment, the water outlet and the water inlet are both connected to a water pipe for cooling water circulation; the water pipe extends to the outside of the reactor through a terminal. The water inlet pipe 11 injects cooling water into the cooling channel 12 through the water inlet, and the cooling water circulates inside the cooling channel 12 and finally flows out from the water outlet through the water outlet pipe 3, thereby achieving a water cooling effect.

[0046] In order to ensure the airtightness of the cooling channel 12 and prevent cooling water leakage, rubber sealing rings 10 are provided at the connection positions of the outer shell 1 and the inner shell 2. Through the above arrangement, it is also possible to ensure that the inner shell 2 is a sealed environment. The inner shell 2 includes a tool-retracting groove 18 for thread processing, and the assembly gap of the entire video observation device during assembly can be sealed by the rubber sealing ring.

[0047] Specifically, when the camera device 13 is used to monitor the spreading process of combustion synthesis silicon nitride powder, the nitrogen pressure is 5MPa, the working temperature range is 20-160°C, and the image screenshots obtained by the camera device 13 are as follows: Figure 2A-2DWhen the camera device 13 is used to monitor the spread of the combustion synthesis of silicon nitride powder, the nitrogen pressure is 3MPa, the operating temperature range is 20 to 120°C, and the image captured by the camera device 13 is as shown Figure 3 As shown, the measured propagation wave velocity is 0.57 mm / s and the combustion front width is 5 mm.

[0048] In summary, the present invention provides a camera device that can work normally in a high-temperature and high-pressure combustion synthesis reactor. The shell can be well isolated from the external temperature, and cooling water is injected into the cooling channel through the water inlet. The cooling water circulates in the cooling channel and finally flows out from the water outlet, thereby achieving a water cooling effect; a closed space is formed by enclosing a window sheet, a connector and an inner shell to accommodate, fix and protect the camera device, and a camera with adjustable focal length and contrast is used, so that the camera device can observe and record the image of the propagation of the combustion wave during the combustion process in the combustion synthesis reactor in real time in an environment of high temperature, high pressure and corrosive media, thereby realizing the monitoring of the combustion propagation rate of silicon nitride powder and the analysis of the reaction process.

[0049] Obviously, the above embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not limitations on the implementation methods of the present invention. For ordinary technicians in the relevant field, other different forms of changes or modifications can be made based on the above description. It is impossible to list all the implementation methods here. All obvious changes or modifications derived from the technical solution of the present invention are still within the protection scope of the present invention.

Claims

1. A video observation device for a combustion synthesis reactor, characterized in that: include: case; The housing includes a cooling channel; The shell is formed with a water inlet and a water outlet which are in communication with the cooling channel; A camera device with adjustable focus and contrast is installed in the housing; The video observation device also includes a window fixed to the shell through a connector; the window, the connector and the shell together form a closed space to accommodate and fix the video device; the window corresponds to the video device.

2. The video observation device for a combustion synthesis reactor according to claim 1, characterized in that: The housing comprises an outer shell and an inner shell located inside the outer shell; The cooling channel is located between the outer shell and the inner shell; the water inlet and the water outlet are formed on the outer shell; The window piece is fixed on the inner shell through a connecting piece; the inner shell is fixed to the outer shell through the connecting piece; the window piece, the connecting piece and the inner shell are enclosed to form a closed space to accommodate a fixed camera device.

3. The video observation device for a combustion synthesis reactor according to claim 2, characterized in that: The window is located at the front side of the inner shell and corresponds to the front end of the lens of the camera device.

4. The video observation device for a combustion synthesis reactor according to claim 1, characterized in that: The material of the window piece is quartz glass; the thickness of the window piece is 20-30 mm.

5. The video observation device for a combustion synthesis reactor according to claim 2, characterized in that: The front end of the shell is formed with an opening corresponding to the window sheet; the connecting piece is fixed at the opening position of the shell; the window sheet is fixed on the connecting piece and an avoidance opening corresponding to the window sheet is formed on the connecting piece.

6. The video observation device for a combustion synthesis reactor according to claim 2, characterized in that: A detachable outer rear cover is disposed at the rear end of the housing, a rubber sealing protective sleeve is disposed inside the outer rear cover, and the outer rear cover is threadedly connected to the housing; A detachable inner rear cover is arranged at the rear end of the inner shell, a rubber sealing protective sleeve is arranged inside the inner rear cover, and the inner rear cover is threadedly connected to the inner shell.

7. The video observation device for a combustion synthesis reactor according to claim 2, characterized in that: The video observation device comprises a water cooling jacket located between the outer shell and the inner shell; the inner cavity of the water cooling jacket forms the cooling channel.

8. The video observation device for a combustion synthesis reactor according to claim 1, characterized in that: It also includes a terminal that passes through the side wall of the reactor and an electromagnetic shielding wire for connecting a camera device; a polytetrafluoroethylene sealing ring is sleeved on the terminal; and the electromagnetic shielding wire extends to the outside of the reactor through the terminal.

9. The video observation device for a combustion synthesis reactor according to claim 8, characterized in that: The water outlet and the water inlet are both connected to water pipes for cooling water circulation; the water pipes extend to the outside of the reactor through the terminal posts.

10. A combustion synthesis reactor, comprising the video observation device according to claim 1, characterized in that: The side wall of the self-propagation synthesis reactor is provided with a through hole for accommodating the terminal of the video observation device.

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