A detection imaging device for a chemical reaction process, a preparation method thereof, and an application thereof

Abstract

The present invention relates to a detection imaging device for a chemical reaction process, a preparation method and an application thereof. The detection imaging device for the chemical reaction process includes an image transmission fiber rod and a light guiding fiber, and a plurality of light guiding fibers are annularly arranged on the outer periphery of the image transmission fiber rod. The detection imaging device for the chemical reaction process provided by the present invention has the advantages of dynamically monitoring the chemical reaction process, obtaining the morphology of products, and analyzing the particle size and quantity of reaction products based on the morphology pictures.

Description

Technical Field

[0001] The present invention belongs to the field of fiber optic detection imaging, and particularly relates to a detection imaging device for a chemical reaction process, a preparation method thereof, and an application thereof. Background Art

[0002] The essence of a chemical reaction is the disappearance of old substances and the generation of new substances, and energy changes also occur during the chemical reaction process. Currently, since some chemical reactions need to be carried out in a vacuum or a sealed environment, it is impossible to monitor the morphology and relative content of reaction products in real time to further master the progress of the reaction and optimize the reaction process. At present, in order to digitize the images of reaction products detected and recognized, only camera sampling can be used, and real-time monitoring cannot be achieved. Heat is released during the reaction process, and corrosive substances such as acids and alkalis may be generated, which not only puts higher requirements on the quality of the camera, but also the morphology and particle size of the reaction products cannot be continuously displayed. Therefore, there is an urgent need for a high-temperature resistant, corrosion resistant, explosion-prone environment adaptable device that can monitor the state and quantity of chemical reaction products and can realize real-time detection and imaging of the morphology of reaction products under vacuum or sealed conditions. Summary of the Invention

[0003] In view of this, the main object of the present invention is to provide a detection imaging device for a chemical reaction process, a preparation method thereof, and an application thereof. The technical problem to be solved is that it is not only high-temperature resistant, corrosion resistant, explosion-prone environment adaptable, can monitor the state and quantity of chemical reaction products, but also can realize real-time detection of the morphology of reaction products under vacuum or sealed conditions.

[0004] The object of the present invention and the technical problems to be solved are achieved by adopting the following technical solutions. A detection imaging device for a chemical reaction process proposed by the present invention, the detection imaging device includes an image transmission fiber optic rod and a light guiding fiber optic, and a plurality of light guiding fiber optics are annularly arranged on the outer periphery of the image transmission fiber optic rod.

[0005] Further, in the aforementioned detection imaging device for a chemical reaction process, the fiber optic image transmission rod is a conical or straight fiber optic image transmission rod.

[0006] Further, in the aforementioned detection imaging device for a chemical reaction process, the fiber optic image transmission rod is formed by fusing tens of millions of micron-scale optical fibers arranged regularly; the diameter of the optical fiber is 2.5 - 500 μm.

[0007] Further, in the aforementioned detection imaging device for a chemical reaction process, the fiber optic image transmission rod includes an image input end and an image output end. A plurality of grooves are provided on the outer periphery of the image input end of the fiber optic image transmission rod, and the light guiding fiber optics are embedded in the grooves, and the grooves and the light guiding fiber optics are cured and bonded by ultraviolet curing glue.

[0008] Further, in the aforementioned detection and imaging device for a chemical reaction process, a light-emitting light source and an image sensor are provided at the image output end of the fiber optic image transmitting rod.

[0009] Further, in the aforementioned detection and imaging device for a chemical reaction process, it further includes a fixing bracket, which includes an upper bracket surface and four supporting square columns connected to the upper bracket surface. The upper bracket surface is square, and a circular hole is provided at the center position of the upper bracket surface; the height of the fixing bracket is 1 / 3 to 1 / 2 of that of the fiber optic image transmitting rod, and the diameter of the circular hole is equal to the diameter of the fiber optic image transmitting rod at 1 / 3 to 1 / 2 of its length.

[0010] Further, in the aforementioned detection and imaging device for a chemical reaction process, the four supporting square columns are connected to the circuit board of the image sensor.

[0011] Further, in the aforementioned detection and imaging device for a chemical reaction process, the connection parts between the bracket and the fiber optic image transmitting rod and the circuit board are cured and bonded with an ultraviolet curable adhesive.

[0012] Further, in the aforementioned detection and imaging device for a chemical reaction process, the main component of the ultraviolet curable adhesive is polyurethane acrylate.

[0013] Further, in the aforementioned detection and imaging device for a chemical reaction process, it further includes a housing, which is composed of a protective cap and an end face protective shell connected to each other.

[0014] Further, in the aforementioned detection and imaging device for a chemical reaction process, a circular hole is provided at the bottom of the end face protective shell; the protective cap and the end face protective shell are connected by threads.

[0015] Further, in the aforementioned detection and imaging device for a chemical reaction process, the end face protective shell includes a first end face protective shell and a second end face protective shell spliced together. A semi-circular hole is provided at the center of the bottom of both, and a circular hole is formed after splicing.

[0016] Further, in the aforementioned detection and imaging device for a chemical reaction process, the housing is a metal housing; the protective cap is cylindrical.

[0017] Further, in the aforementioned detection and imaging device for a chemical reaction process, it further includes a computer, which includes a display device, and a chemical reaction particle statistics and analysis unit is provided in the display device.

[0018] The object of the present invention and the solution to its technical problems can also be achieved by adopting the following technical solutions. A preparation method of a detection and imaging device for a chemical reaction process proposed by the present invention includes the following steps:

[0019] Preparation and processing of fiber optic image bundles;

[0020] Processing of the bracket of the fiber optic image bundle;

[0021] Preparation of the encapsulating metal shell;

[0022] Removal of the protective window of the image sensor glass;

[0023] Coupling and curing;

[0024] Encapsulation of the fiber optic image bundle and the image sensor.

[0025] The object of the present invention and the technical problems to be solved can also be achieved by the following technical solutions. A detection imaging method for a chemical reaction process proposed by the present invention includes the following steps:

[0026] Bring the substance to be detected close to the image input end of the fiber optic image bundle of the detection imaging device for the chemical reaction process. Then, the substance transmits the image in the form of photons to the image output end. Couple the image output end with the photosensitive surface of the chip of the image sensor, and perform digital conversion on the image. Then, the image can be seen at the chemical reaction particle statistics and analysis unit of the computer.

[0027] By means of the above technical solutions, the detection imaging device for the chemical reaction process and its preparation method and application according to the present invention at least have the following advantages:

[0028] The detection imaging device for the chemical reaction process of the present invention uses the coupling of the fiber optic image bundle and the image sensor to transmit the real-time situation of the reaction through the input end of the fiber optic image bundle to the small end face of the fiber optic image bundle, that is, photon input; the coupled image sensor forms an image on the display screen, that is, realizes the conversion of photons into electrons; then, the chemical reaction particle statistics and analysis unit analyzes and statistics the real-time image, and further obtains the morphology, quantity and size of the chemical reaction particles.

[0029] The detection imaging device for the chemical reaction process of the present invention has the advantages of dynamically monitoring the chemical reaction process, obtaining the morphology of the product, and analyzing the size and quantity of the reaction product particles based on the morphology pictures.

[0030] The actual inspection of the detection imaging device for the chemical reaction process of the present invention by the prototype also shows that the method is accurate, stable and effective.

[0031] The above description is only an overview of the technical solution of the present invention. In order to be able to understand the technical means of the present invention more clearly and implement it according to the content of the specification, the following will describe in detail with the preferred embodiments of the present invention as follows. Brief Description of the Drawings

[0032] Figure 1 Schematic diagram of the overall structure of the detection imaging device for chemical reaction processes according to the present invention;

[0033] Figure 2 Schematic diagram of the cross-sectional structure of the optical fiber of the detection imaging device for chemical reaction processes according to the present invention;

[0034] Figure 3 Schematic diagram of the fixed ring of the LED light source and the sleeve of the light guide fiber bundle according to the present invention;

[0035] Figure 4 Schematic diagram of the support structure of the fiber optic image transmission rod according to the present invention;

[0036] Figure 5A Schematic diagram of the end face protection shell of the metal shell according to the present invention;

[0037] Figure 5B Schematic diagram of the protective cap of the metal shell according to the present invention;

[0038] Figure 6A Resolution graph after coupling in Example 1 of the present invention;

[0039] Figure 6B Resolution graph after coupling in Example 2 of the present invention;

[0040] Figure 7A Morphology graph of chemical reaction particles detected in Example 1 of the present invention;

[0041] Figure 7B Morphology graph of chemical reaction particles detected in Example 2 of the present invention;

[0042] Figure 8A Gray-scale processing graph of chemical reaction particles detected in Example 1 of the present invention;

[0043] Figure 8B Gray-scale processing graph of chemical reaction particles detected in Example 2 of the present invention;

[0044] Figure 9A Statistical graph of the number of chemical reaction particles in Example 1 of the present invention;

[0045] Figure 9B Statistical graph of the number of chemical reaction particles in Example 1 of the present invention;

[0046] Figure 10A Statistical graph of the size measurement and statistics of chemical reaction particles detected in Example 1 of the present invention;

[0047] Figure 10B Statistical graph of the size measurement and statistics of chemical reaction particles detected in Example 2 of the present invention;

[0048] Wherein: 1 - Image input end; 2 - Light - guiding optical fiber; 3 - Image - transmitting fiber optic rod; 4 - Protective cap; 5 - First - end face protective shell; 6 - Second - end face protective shell; 7 - Image - transmitting fiber optic rod fixing bracket; 8 - LED light - source fixing ring; 9 - Light - emitting light source; 10 - Image output end; 11 - Photosensitive surface of the chip; 12 - Image sensor; 13 - Data line; 14 - Chemical - reaction particle statistics and analysis unit; 15 - Display device; 16 - Optical fiber; 17 - Groove; 18 - Sleeve; 19 - Circular hole; 20 - Upper end face of the bracket; 21 - Supporting square column; 22 - Screw; 23 - Bottom circular hole; 24 - External thread; 25 - Internal thread; 26 - Upper end face of the protective cap. Detailed implementation manners

[0049] To further elaborate on the technical means and effects adopted by the present invention to achieve the intended invention purpose, the following, in combination with preferred embodiments, details the specific implementation manners, structures, features, and effects of the detection and imaging device for chemical reaction processes proposed according to the present invention, its preparation method, and its applications. In the following description, different "one embodiment" or "embodiments" do not necessarily refer to the same embodiment. In addition, the specific features, structures, or characteristics in one or more embodiments can be combined in any suitable form.

[0050] The following materials or reagents are commercially available unless otherwise specified.

[0051] Currently, the method of obtaining images is by means of a camera. However, when detecting chemical reaction processes in a vacuum or sealed environment, the environment is harsh, the reactants are corrosive, the reaction process is intense and complex, the reaction time is long, the volume is large, and the liquid volume is large, which limits the use of the camera. Therefore, the detection inside the reaction process has become a bottleneck for researchers to conduct experiments.

[0052] For this reason, the applicant has solved the current problem by coupling an image - transmitting fiber optic rod with an image sensor such as a CMOS chip. The image - transmitting fiber optic rod is corrosion - resistant and high - temperature - resistant. The diameter of the optical fiber can be adjusted according to the size of the CMOS pixel used; the shape of the small end face can be adjusted according to the shape and size of the CMOS photosensitive surface; the length of the image - transmitting fiber optic rod can be customized according to the chemical reaction vessel.

[0053] As Figures 1 - 5B shown, some embodiments of the present invention provide a detection and imaging device for chemical reaction processes. The detection and imaging device includes an image - transmitting fiber optic rod 3 and a light - guiding optical fiber 2, and a plurality of light - guiding optical fibers 2 are annularly arranged around the outer periphery of the image - transmitting fiber optic rod 3.

[0054] In some embodiments, optionally, the fiber optic image transmitting rod 3 is a conical or straight fiber optic image transmitting rod. To increase the detection field of view, a conical fiber optic image transmitting rod can be considered. It is formed by reheating and softening the blank plate and then stretching it on the basis of a straight fiber optic image transmitting rod, which can achieve image magnification or reduction transmission, thereby achieving the purpose of increasing the detection field of view. The detection end is the image input end 1 of the fiber optic image transmitting rod, and the maximum operating temperature can reach 550 °C; the glass acid resistance grade meets Class A1, and the detection end can be reused, greatly reducing the usage cost. The detection end refers to the end for detecting chemical reactions, that is, the image input end of the fiber optic image transmitting rod.

[0055] In some embodiments, optionally, the fiber optic image transmitting rod 3 is formed by fusing tens of millions of micron-scale optical fibers 16 arranged regularly; the diameter of the optical fiber 16 is 2.5 - 500 μm. It can be adjusted according to the photosensitive element size of the photosensitive surface 11 of the chip. If the size of the photosensitive surface 11 of the chip of the image sensor 12 used is small, resulting in a small effective area at the input end (image input end 1) of the fiber optic image transmitting rod, the fiber optic image transmitting rod 3 can be considered to be made into a conical shape, that is, a long light cone, and the magnification ratio can be adjusted according to the usage requirements (for example: when the magnification ratio is 2:1, the fiber optic image transmitting rod has the function of magnifying the image by 2 times). The above-mentioned effective area refers to the area at the input end that can transmit images. If the image transmitting rod has no magnification, the image transmitting areas at the input end and the output end are equal. If the magnification ratio is 2, the image transmitting area at the input end is 2 times that of the output end.

[0056] In some embodiments, optionally, the fiber optic image transmitting rod 3 includes an image input end 1 and an image output end 10. A plurality of grooves 17 are provided on the outer periphery of the image input end 1 of the fiber optic image transmitting rod 3, and the light guiding optical fibers 2 are embedded in the grooves 17 for supplementary lighting when detecting a dark environment. The grooves 17 and the light guiding optical fibers 2 are filled and cured with ultraviolet curing glue for bonding. The setting of the grooves 17 can avoid using fixing rings made of other materials (such as metal, plastic) to fix the light guiding optical fibers, improving the heat resistance and corrosion resistance of the detection device.

[0057] In some embodiments, optionally, the image output end 10 of the fiber optic image transmitting rod is coupled to the photosensitive surface 11 of the chip of the image sensor 12 for converting photons into digital signals. In specific implementation, the image sensor 12 may be a CMOS chip, for example, a commercially available back-illuminated CMOS chip. Currently, most of the CMOSs coupled with fiber optic image transmitting elements are front-illuminated. Compared with the traditional front-illuminated CMOS, the arrangement order of the structure is different. For the back-illuminated CMOS, the circuit layer is located behind the photosensitive diode, and the light will not be blocked and reflected by the circuit layer, and the light reaching the photodiode reduces the loss by 30%, improving the light utilization rate. And in low-light environments, the back-illuminated sensor can improve the photosensitive ability by 30% - 50%.

[0058] It should be noted that the fiber optic image transmitting rod needs to detect the real-time situation of chemical reactions in a vacuum or sealed environment where there is no light, which will affect the clarity of the detection and imaging of the fiber optic image transmitting rod. Therefore, the light-emitting light source and the light guiding fiber need to cooperate with each other.

[0059] Furthermore, the light-emitting light source 9 is arranged near the image output end 10 to provide a light source for the light guiding fiber and should be far away from the image input end 1 because the light-emitting light source 9 is fixed by a metal ring and should be far away from high-temperature and corrosive environments. The light-emitting light source 9 is composed of four LED light sources, which can evenly provide a light source for the light guiding fiber 2. The light-emitting light source 9 is installed on the LED light source fixing ring 8, and the fixing ring is made of a metal material and is located in the four directions of up, down, left, and right. And there is a sleeve with a height of 5 mm at the upper end of the light source, which is beneficial to the fixation of the light guiding fiber 2. The light guiding fiber 2 is divided into four areas: upper left, lower left, upper right, and lower right. The fiber bundle in the upper left area is inserted into the sleeve of the LED light source in the left direction, the fiber bundle in the lower left area is inserted into the sleeve 18 of the LED light source in the lower direction, the fiber bundle in the upper right area is inserted into the sleeve 18 of the LED light source in the upper direction, and the fiber bundle in the lower right area is inserted into the sleeve of the LED light source in the right direction, and is filled and cured with ultraviolet curing glue. The brightness of the four lamps is controlled externally.

[0060] In some embodiments, considering that the fiber optic image transmission rod 3 is relatively long and thin, with a length of about 0.2 to 1 m, and the diameter of the output end 10 of the fiber optic image transmission rod coupled to the photosensitive surface 11 of the chip is 12 mm to 200 mm. To avoid the situation where the image output end 10 of the fiber optic image transmission rod is detached from the photosensitive surface 11 of the chip of the image sensor during use, a fiber optic image transmission rod fixing bracket 7 is introduced during coupling; optionally, the detection imaging device for the chemical reaction process further includes a fixing bracket 7, which serves to fix the fiber optic image transmission rod and the image sensor. The fixing bracket includes a bracket upper end surface 20 and four support square columns 21 connected to the bracket upper end surface 20. The bracket upper end surface 20 is square, and a circular hole 19 is provided at the center position of the bracket upper end surface 20; the height of the fixing bracket is about 1 / 3 to 1 / 2 of that of the fiber optic image transmission rod, and the diameter of the circular hole is equal to the diameter of the fiber optic image transmission rod at 1 / 3 to 1 / 2 of its length.

[0061] In some embodiments, optionally, the four support square columns 21 are connected to the circuit board of the image sensor 12, so that the fiber optic image transmission rod and the image sensor are integrated and do not move relative to each other.

[0062] In some embodiments, optionally, the connection between the fiber optic image transmission rod fixing bracket 7 and the fiber optic image transmission rod 3 and the circuit board is cured and bonded with an ultraviolet curable adhesive, making the two more firmly fixed.

[0063] In some embodiments, optionally, the ultraviolet curable adhesive is composed of 60% polyurethane acrylate, 20% acrylate monomer, 15% methacrylate monomer, and 5% photoinitiator by weight percentage. This ultraviolet curable adhesive has the maximum absorption for ultraviolet light in the wavelength range of 350 to 395 nm, can be cured by irradiation for 10 to 30 s, has a refractive index of 1.60, a hardness of 70 to 80 Shore D, a tensile strength > 18 MPa, a shear strength > 20 MPa, and a visible light transmittance > 90%. This ultraviolet curable adhesive can ensure the relative stability of the fiber optic image transmission rod and the image sensor after curing.

[0064] Furthermore, in the aforementioned detection imaging device for the chemical reaction process, in order to avoid the fiber optic image transmission rod 3 and the image sensor 12 from being knocked during later use, the fiber optic rod 3 and the image sensor 12 need to be protected. Therefore, the detection imaging device may further include a housing, which is composed of a protective cap 4 and an end face protective shell connected to each other. The end face protective shell serves to protect the LED light source, the image sensor, and the position where it is coupled to the fiber optic image transmission rod; when the detection imaging device is in a non-working state, the protective cap is used to protect the detection end of the fiber optic image transmission rod to avoid scratching and corrosion.

[0065] In some embodiments, optionally, the outer shell is a metal shell; the end face protection shell includes a first end face protection shell 5 and a second end face protection shell 6 that are spliced together. Both have a semi-circular hole at the center of the bottom. After splicing, a circular hole 23 is formed, allowing the power control line of the light-emitting light source 9 and the power line of the image sensor 12 to lead from the inside of the detection imaging device to the outside.

[0066] In some embodiments, optionally, the protective cap 4 and the end face protection shell are connected by threads. The protective cap 4 is cylindrical in shape to match the shape of the fiber optic image transmission rod. The upper end face 26 of the protective cap is used to protect the detection end of the fiber optic image transmission rod.

[0067] In some embodiments, optionally, a computer is further included, which includes a display device 15 and a central processing unit. The image sensor 12 is connected to the central processing unit through a data line 13. The display device 15 can be a display. A chemical reaction particle statistics and analysis unit 14 is provided inside the central processing unit. The chemical reaction particle statistics and analysis unit 14 can satisfy the dynamic real-time monitoring of the morphology of reaction products in a vacuum or sealed environment and can count the quantity and size of chemical products in different regions.

[0068] In the above detection imaging device for the chemical reaction process, the working principle of the fiber optic image transmission rod 3 and the image sensor 12, such as a CMOS chip, for coupled detection imaging is as follows: The detection end adopts a structure of "fiber optic image transmission rod + photosensitive surface (CMOS) of the chip". The morphology inside the vacuum or sealed environment is imaged on the output end face 10 of the fiber optic image transmission rod. The end face is directly coupled with the photosensitive surface 11 of an image sensor such as a CMOS chip to digitalize the image. The digitalized image is recognized and processed by the chemical reaction particle statistics and analysis unit to obtain the real-time reaction morphology, and the real-time reaction product particle size, quantity, and shape can be analyzed based on the morphology picture.

[0069] Some embodiments of the present invention also provide a preparation method for a detection imaging device for a chemical reaction process, including the following steps:

[0070] 1) Preparation work:

[0071] a) Preparation and processing of the fiber optic image transmission rod: A fiber optic preform is obtained by nesting a fiber optic core glass rod with a diameter of 29.3 - 29.8 mm and a fiber optic cladding glass tube with a diameter of 33.8 - 34.3 mm. The fiber optic preform undergoes three drawing processes. First, at 750 - 850 °C, the fiber optic preform is drawn into a single fiber with a diameter of 2.95 - 3.15 mm. The single fibers are stacked in a hexagonal closest packing pattern, and light absorption fibers are inserted into the gaps between the single fibers. After the arrangement is completed, they are bundled into a primary multifilament rod. Then, at 750 - 850 °C, the primary multifilament rod is drawn into a primary multifilament with an opposite side dimension of 1.25 - 1.30 mm. Then, the primary multifilaments are arranged in a hexagonal shape to obtain a secondary multifilament rod, and at 750 - 850 °C, the secondary multifilament rod is drawn into a secondary multifilament with an opposite side dimension of 1.20 mm. The secondary multifilaments are arranged in a hexagonal shape again, with an opposite side dimension of 32 - 33 mm. The formed hexagonal plate segment is placed in a hot pressing furnace, and the hot pressing temperature is controlled at 650 - 700 °C. Mechanical vacuum hot pressing is carried out to melt and form the fiber bundle into a plate segment with an opposite side dimension of 26 - 29 mm. Then, the blank plate is cut according to the required length; (if a fiber optic image transmission rod with an amplifying function is to be made, secondary heating and stretching are also required in a stretching furnace, with the outer furnace temperature controlled at 540 - 550 °C and the inner furnace temperature controlled at 790 - 800 °C). One end of the blank plate is processed with a square groove profile on a precision engraving machine, with the side length of the square groove being 0.3 - 1 mm, and the other end of the fiber optic image transmission rod is processed to have the same length and width as the CMOS photosensitive surface. After that, the blank plate undergoes optical precision processing such as milling, grinding, and polishing, so that the surface roughness of the fiber optic image transmission rod is less than 5 nm, the surface shape accuracy reaches 0.1000 ± 0.0500 wave, and the parallelism is less than 0.2 mm, obtaining a straight or tapered fiber optic image transmission rod.

[0072] b) Processing of the fiber optic image transmission rod fixing bracket 7: The height of the fiber optic image transmission rod fixing bracket 7 is approximately 1 / 3 - 1 / 2 of the length of the fiber optic image transmission rod 3. The fiber optic image transmission rod fixing bracket 7 is made of acrylic plate. Measure the diameter of the fiber optic image transmission rod 3 at the contact position between the fiber optic image transmission rod fixing bracket 7 and the fiber optic image transmission rod 3, and at the exact center of the end face of the fixing bracket, use a precision engraving machine to engrave a circular hole with a diameter 1 mm larger than the diameter of the fiber optic image transmission rod at the contact position, so that the output end 10 of the fiber optic image transmission rod can pass through the circular hole 19 and can be fixed at the 1 / 3 - 1 / 2 position of the fiber optic image transmission rod 3. The upper end face 20 of the processed fiber optic image transmission rod fixing bracket has a circular hole 19, and the side has four support square columns 21, similar to the shape of a table.

[0073] c) Preparation of the encapsulated metal housing: The metal housing includes a protective cap 4, a first end-face protective housing 5, and a second end-face protective housing 6. The protective cap 4 has an internal thread 25 at the lower end of its interior. The upper ends of the first end-face protective housing 5 and the second end-face protective housing 6 have external threads 24, and the internal and external threads can be screwed together. The height of the end-face protective housing is 2 / 3 to 3 / 4 of the total height of the fiber optic image transmission rod 3 and the image sensor 12, and the height of the protective cap 4 is 1 / 4 to 1 / 3 of the total height of the fiber optic image transmission rod 3 and the image sensor 12.

[0074] d) Removal of the CMOS glass protective window: Since the chip of the image sensor is protected by a glass window to prevent contamination or scratching of the photosensitive surface of the chip, the glass protective window needs to be removed before coupling the fiber optic image transmission rod 3 with the photosensitive surface 11 of the chip. The glass protective window of the COMS is removed by means of laser windowing. The image sensor 12 is placed on the workbench of the laser marking machine, and the range of laser output is adjusted. The adjustment basis is to irradiate only the optical glue at the connection part between the glass and the CMOS. The size of the laser frame is set, the laser power is adjusted to 80 - 100, the speed is 60 - 80, and then the laser is continuously irradiated for 20 - 25 s to carbonize the optical glue and make it lose its activity. The glass protective window is pried open with a blade, and thus the glass protective window is removed.

[0075] 2) Coupling and curing:

[0076] The fiber optic image transmission rod 3 and the image sensor 12 are coupled on the coupling device. The camera on the coupling device is used to take pictures of the photosensitive surface 11 of the chip for positioning and monitoring of the coupling position, and the image is transmitted to the terminal display screen of the coupling device. The fiber optic image transmission rod 3 passes through the circular hole 19 of the fiber optic image transmission rod fixing bracket 7 and the LED light source fixing ring 8, and the fiber optic image transmission rod is fixed by the clamping unit. The computer control software of the coupling device is used to roughly adjust the combination of the fiber optic image transmission rod 3, the fiber optic image transmission rod fixing bracket 7, and the light emitting light source 9, so that the distance between the image output end 10 of the fiber optic image transmission rod and the photosensitive surface 11 of the CMOS chip is 5 - 10 mm. At this time, ultraviolet curing glue is evenly coated on the image output surface of the fiber optic image transmission rod and the end faces of the four supporting square columns of the bracket, and the coating thickness does not exceed 20 μm. Then, with the help of the computer control terminal, the distance between the output surface of the fiber optic image transmission rod and the photosensitive surface of the CMOS chip is finely adjusted to 1 - 2 mm. When observing the image at the coupling position on the display screen and obtaining the most ideal coupling position, the image output end 10 of the fiber optic image transmission rod is brought into contact with the photosensitive surface 11 of the chip. Then, the ultraviolet lamp with a wavelength of 365 nm is turned on, and the ultraviolet light can pass through the fiber optic image transmission rod to irradiate the ultraviolet curing glue to achieve rapid curing. Then, ultraviolet curing glue with a thickness less than 0.25 mm is coated at the contact part between the side wall of the circular hole 19 at the upper end face of the fiber optic image transmission rod and the neck of the fiber optic image transmission rod for curing and bonding. Finally, the LED light source fixing ring 8 is bonded to the side wall of the fiber optic image transmission rod.

[0077] 3) Encapsulation of the fiber optic image transmission rod and the CMOS:

[0078] After the curing is completed, a first end face protective case 5 and a second end face protective case 6 are encapsulated outside the fiber optic image transmission rod 3 and the image sensor 12. The light source control line and the CMOS power supply line lead to the outside through the bottom circular hole 23, and the screw 22 is screwed on to avoid loosening. The protective cap is screwed onto the external thread 24 of the end face protective case through the internal thread 25 and unscrewed when the detector is in use for image detection.

[0079] Some embodiments of the present invention also provide a detection imaging method for a chemical reaction process, including the following steps:

[0080] The substance to be detected is brought close to the image input end 1 of the fiber optic image transmission rod. Then, the substance transmits the image in the form of photons to the image output end 10. The image output end 10 is coupled with the photosensitive surface 11 of the chip of the image sensor, and the image is digitally converted, so that the image can be seen at the chemical reaction particle statistics and analysis unit 14 of the computer.

[0081] The present invention will be further described below in conjunction with specific embodiments.

[0082] Embodiment 1:

[0083] A straight fiber optic image transmission rod is coupled with a CMOS camera to prepare a detection imaging device for a chemical reaction process.

[0084] The photosensitive element of the CMOS camera chip is 2.9×2.9 μm, the photosensitive surface is 12.493×9.994 mm, and the resolution is 3864×2176.

[0085] Preparation of a straight fiber optic image bundle: A core layer glass rod with a diameter of 29.5 mm and an optical fiber cladding glass tube with a diameter of 34.7 mm are nested with each other to obtain an optical fiber preform. The optical fiber preform is drawn into a single filament with a diameter of 2.95 mm at 800 °C. The single filaments are stacked in a hexagonal close-packed manner, and light absorption filaments are inserted into the gaps between the single filaments to absorb stray light. After the arrangement is completed, they are bundled into a primary multifilament rod, and the primary multifilament rod is drawn into a primary multifilament with an opposite side dimension of 1.30 mm at 800 °C. Then, the primary multifilaments are arranged in a hexagonal shape to obtain a secondary multifilament rod, and the secondary multifilament rod is drawn into a secondary multifilament with an opposite side dimension of 1.20 mm at 790 °C. The secondary multifilaments are arranged in a hexagonal shape again, with an opposite side dimension of 32.34 mm. The formed hexagonal plate segment is placed in a hot pressing furnace, and the hot pressing temperature is controlled at 680 °C. Mechanical vacuum hot pressing is carried out to melt and form the fiber bundle into a plate segment with an opposite side dimension of 27 mm. Then, the length of the blank plate is cut to 210 mm. Square grooves with a side length of 0.3 mm are opened on the outer edge of one end of the blank plate, and the number of square grooves is 16. The other end of the fiber optic image bundle is processed to be 12.4 mm long and 9.9 mm wide. After that, the blank plate is subjected to optical precision machining such as milling, grinding, and polishing, so that the surface roughness of the fiber optic image bundle reaches 5 nm, the surface shape accuracy reaches 0.1000 wave, and the parallelism reaches 0.2 mm. Finally, a straight fiber optic image bundle with a height of 200 mm and a fiber unit filament diameter of 3 μm is obtained. The fiber optic image bundle is composed of more than 16 million optical fibers approximately.

[0086] LED light source fixing ring and light guide fiber bundle sleeve: The light source fixing ring is made of metal, with an inner diameter of 16 mm and an outer diameter of 25 mm. The LED light sources are located in the upper, lower, left, and right four directions of the ring respectively. There are metal sleeves with a diameter of 5 mm and a height of 5 mm above each light source, which can both gather the light source and fix the light guide fiber.

[0087] Fixed light - guiding optical fiber: The diameter of the light - guiding optical fiber is 0.25 mm and the length is 190 mm. Embed the light - guiding optical fiber into the groove of the fiber optic image bundle. The end face of the light - guiding optical fiber and the input end of the fiber optic image bundle are in the same plane. Pour ultraviolet - curable glue into the groove with a thickness less than 25 μm. Turn on the ultraviolet lamp with a wavelength of 365 nm and irradiate for 25 s for curing. After the embedding of the light - guiding optical fiber is completed, divide all the light - guiding optical fibers into four areas: upper - left, lower - left, upper - right, and lower - right. Each area consists of 4 optical fibers. The optical fiber bundle in the upper - left area is inserted into the sleeve 18 of the LED light source located on the left. The optical fiber bundle in the lower - left area is inserted into the sleeve of the LED light source located below. The optical fiber bundle in the upper - right area is inserted into the sleeve 18 of the LED light source located above. The optical fiber bundle in the lower - right area is inserted into the sleeve 18 of the LED light source located on the right. And pour liquid ultraviolet - curable glue into the sleeve so that the height of the ultraviolet - curable glue liquid is flush with the height of the sleeve. Turn on the ultraviolet lamp with a wavelength of 365 nm and irradiate for 25 s for curing.

[0088] Specifications of the fiber optic image bundle support: The height of the support is 1 / 3 of the fiber optic image bundle, so its height is 67 mm. The length and width of the upper end face of the support are 35 mm. The diameter of the fiber optic image bundle at 67 mm is 16 mm, and the diameter of the circular hole is 16.5 mm.

[0089] Specifications of the encapsulated metal shell: The height of the first - end face protective shell is 125 mm, the height at the external - thread part is 5 mm. The bottom is a semi - circle with a diameter of 50 mm, and there is a semi - circular hole with a diameter of 10 mm at the center of the semi - circle. The second - end face protective shell is symmetric with the first - end face protective shell, and the two are fixed with screws, finally forming a cylindrical protective shell. The bottom is a circle with a diameter of 50 mm, and there is a circular hole with a diameter of 10 mm at the center of the bottom. The protective cap is similar to a cylinder, with a circular top with a diameter of 50 mm, a height of 80 mm, and an internal thread of 5 mm on the bottom cylindrical surface.

[0090] Through the above - mentioned detection and imaging device for the chemical reaction process, the morphology, quantity, and size of chemical reaction particles can be obtained through the chemical reaction particle statistics and analysis unit.

[0091] Coupling resolution: 50.8 lp / mm. The resolution after coupling is as Figure 6A shown. As can be seen from Figure 6A 5 - 5 (marked by the black oval) can be seen, representing 50.8 lp / mm, that is, horizontal line pairs and vertical line pairs (a line pair consists of a black line and a white line), and each line pair contains 3 lines.

[0092] The morphology diagram of the detected chemical reaction particles is as Figure 7A shown. As can be seen from Figure 7A it, through the detection and imaging device for the chemical reaction process, the image of the chemical reaction particles can be clearly seen, and the quantity of the particles can be counted.

[0093] The grayscale processing diagram of the detected chemical reaction particles is as Figure 8A shown. It can be seen from Figure 8A that all pixel points in the digital image of the chemical reaction particle morphology diagram are grayscaled, and each pixel point has only one value (0 - 255) representing the color depth.

[0094] The statistical count of chemical reaction particles is as Figure 9A shown. It can be seen from Figure 9A that according to the size range of the particles to be analyzed, that is, removing too small impurity particles, the grayscaled image is statistically analyzed for particles, and 110 particles are obtained.

[0095] The measurement and statistics of the sizes of the detected chemical reaction particles are as Figure 10A shown. It can be seen from Figure 10A that the sizes of the chemical reaction particles are measured, and the size of particle a is 0.810 mm, the size of particle b is 0.457 mm, the size of particle c is 0.437 mm, the size of particle d is 0.425 mm, and the size of particle e is 0.415 mm.

[0096] Example 2

[0097] A cone fiber image transmission rod is coupled with a CMOS camera to prepare a detection imaging device for the chemical reaction process.

[0098] The photosensitive element of the CMOS camera chip is 2.4×2.4 μm, the photosensitive surface is 15.86×15.86 mm, and the resolution is 5472×3648.

[0099] Preparation of tapered fiber optic image guide rod: To increase the detection field of view, the fiber optic image guide rod can be made tapered, i.e., a long light cone. A core layer glass rod with a diameter of 29.5 mm and a fiber optic cladding glass tube with a diameter of 35.2 mm are nested with each other to obtain a fiber preform. The fiber preform is drawn at 820 °C into a single filament with a diameter of 3.195 mm. The single filaments are stacked in a hexagonal close-packed manner, and light-absorbing filaments are inserted into the gaps between the single filaments. After the arrangement is completed, they are bundled into a primary multifilament rod. The primary multifilament rod is drawn at 820 °C into a primary multifilament with an opposite side dimension of 1.26 mm. Then, the primary multifilaments are arranged in a hexagonal shape to obtain a secondary multifilament rod, and the secondary multifilament rod is drawn at 810 °C into a secondary multifilament with an opposite side dimension of 1.192 mm. The secondary multifilaments are arranged in a hexagonal shape again, with an opposite side dimension of 31.28 mm. The formed hexagonal plate segment is placed in a hot pressing furnace, and the hot pressing temperature is controlled at 680 °C. Mechanical vacuum hot pressing is carried out to melt and form the fiber bundle into a plate segment with an opposite side dimension of 26.5 mm. Then, the length of the blank plate is cut to 400 mm. The blank plate segment of the tapered fiber optic rod is placed in a high-temperature stretching furnace for stretching. The temperature of the outer furnace is controlled at 550 °C, the temperature of the inner furnace is controlled at 800 °C, and the stretching length is controlled at 35 mm, so as to obtain a blank of the tapered fiber optic image guide rod with a magnification of 2:1. A square groove with a side length of 0.3 mm is opened on the outer edge at one end of the blank plate, and the number of square grooves is 16. The other end of the fiber optic image guide rod is processed to be 15.8 mm long and 15.8 mm wide. Then, the blank plate is subjected to optical precision processing such as milling, grinding, and polishing, so that the surface roughness of the fiber optic image guide rod reaches 5 nm, the surface shape accuracy reaches 0.1000 wave, and the parallelism reaches 0.2 mm. Finally, a tapered fiber optic image guide rod with a height of 200 mm, a filament diameter of 5 μm for the input end fiber unit, a filament diameter of 2.5 μm for the output end fiber unit, and a magnification ratio of 2:1 is obtained. The fiber optic image guide rod is composed of more than 39 million fibers. The height L1 (tapered part) is 70 mm, the height L2 (straight rod part) is 130 mm, and the diameter of the input end face is about 50 mm.

[0100] The above-mentioned tapered fiber optic image guide rod, i.e., a long light cone, has the function of magnifying or reducing the transmission of images because the fiber filament diameters at the image input end and the output end are 2:1 (for example, when the magnification ratio is 2:1, the fiber optic image guide rod has the function of magnifying the image by 2 times).

[0101] Specifications of the fiber optic image guide rod bracket: The height of the bracket is 1 / 3 of the height of the fiber optic image guide rod, so its height is 67 mm. The length and width of the upper end face of the bracket are 40 mm. The diameter of the fiber optic image guide rod at 67 mm is 21 mm, and the diameter of the circular hole is 21.5 mm.

[0102] The specifications of the encapsulated metal shell: The height of the first-end face protective shell is 125 mm, the height at the external thread is 5 mm, the bottom is a semi-circle with a diameter of 60 mm, and there is a semi-circular hole with a diameter of 10 mm at the center of the semi-circle. The first-end face protective shell is symmetrical to the second-end face protective shell, and the two are fixed with screws, finally forming a cylindrical protective shell. The bottom is a circle with a diameter of 60 mm, and there is a circular hole with a diameter of 10 mm at the center of the bottom. The protective cap is similar to a cylinder, with a circular top with a diameter of 60 mm and a height of 80 mm, and there is an internal thread of 5 mm on the bottom cylindrical surface.

[0103] Through the above-mentioned detection and imaging device for the chemical reaction process, the morphology, quantity, and size of chemical reaction particles can be obtained through the chemical reaction particle statistics and analysis unit.

[0104] Coupling resolution: 32 lp / mm. The resolution after coupling is as Figure 6B shown. As can be seen from Figure 6B 5-1 (marked by the black oval) represents 32 lp / mm, that is, horizontal line pairs and vertical line pairs (a line pair consists of a black line and a white line), and each line pair contains 3 lines.

[0105] The morphology diagram of the detected chemical reaction particles is as Figure 7B shown. As can be seen from Figure 7B it, through the detection and imaging device for the chemical reaction process, the image of chemical reaction particles can be clearly seen, and the quantity of particles can be counted.

[0106] The gray-scale processing diagram of the detected chemical reaction particles is as Figure 8B shown. As can be seen from Figure 8B it, all pixel points in the digital image of the morphology diagram of chemical reaction particles are subjected to gray-scale processing, and each pixel point has only one value (0 - 255) representing the color depth.

[0107] The statistics of the quantity of chemical reaction particles is as Figure 9B shown. As can be seen from Figure 9B it, according to the size range of the particles to be analyzed, that is, removing too small impurity particles, the gray-scale image is subjected to particle statistics, and 195 particles are obtained.

[0108] The measurement and statistics of the size of the detected chemical reaction particles are as Figure 10B shown. As can be seen from Figure 10B it, the sizes of chemical reaction particles are measured, and the size of particle a is 0.201 mm, the size of particle b is 0.356 mm, the size of particle c is 0.179 mm, the size of particle d is 0.185 mm, and the size of particle e is 0.179 mm.

[0109] The other content of this embodiment is the same as the description of the previous embodiment 1.

[0110] In the above embodiments, the descriptions of the respective embodiments have their own emphases. For parts not detailed in a certain embodiment, reference may be made to the relevant descriptions of other embodiments.

[0111] The numerical ranges described in the present invention include all the numerical values within this range, and also include the range values composed of any two numerical values within this range. Different numerical values of the same index appearing in all embodiments of the present invention can be arbitrarily combined to form range values.

[0112] The technical features in the claims and / or the specification of the present invention can be combined, and the combination methods are not limited to the combinations obtained through the citation relationship in the claims. The technical solutions obtained by combining the technical features in the claims and / or the specification also fall within the protection scope of the present invention.

[0113] The above is only a preferred embodiment of the present invention, and does not impose any form of limitation on the present invention. Any simple modification, equivalent change and modification made to the above embodiments based on the technical essence of the present invention still fall within the scope of the technical solutions of the present invention.

Claims

1. A detection imaging method for a chemical reaction process, characterized in that, It includes the following steps: Bring the substance to be detected close to the image input end of the fiber optic image transmitting rod of the detection imaging device for the chemical reaction process. Then, the substance transmits the image in the form of photons to the image output end. Couple the image output end with the photosensitive surface of the chip of the image sensor, and perform digital conversion on the image. Then, the image can be seen at the chemical reaction particle statistics and analysis unit of the computer. The detection imaging device for the chemical reaction process includes a fiber optic image transmitting rod and light guiding optical fibers. A plurality of light guiding optical fibers are arranged in a ring around the outer periphery of the fiber optic image transmitting rod. The fiber optic image transmitting rod is a conical fiber optic image transmitting rod. The fiber optic image transmitting rod is formed by fusing tens of millions of micron-level optical fibers arranged regularly. The diameter of the optical fiber is 2.5 - 500 μm. The fiber optic image transmitting rod includes an image input end and an image output end. The maximum operating temperature at the image input end reaches 550 °C. A light emitting light source and an image sensor are arranged at the image output end of the fiber optic image transmitting rod. The image sensor is a back-illuminated CMOS chip.

2. The detection imaging method for a chemical reaction process according to claim 1, characterized in that, There are a plurality of grooves on the outer periphery of the image input end of the fiber optic image transmitting rod. The light guiding optical fibers are embedded in the grooves, and the grooves and the light guiding optical fibers are fixedly bonded with ultraviolet curable glue.

3. The detection imaging method for a chemical reaction process according to claim 1, characterized in that, It also includes a fixing bracket. The fixing bracket includes an upper bracket surface and four supporting square columns connected to the upper bracket surface. The upper bracket surface is square, and there is a circular hole at the center position of the upper bracket surface. The height of the fixing bracket is 1 / 3 - 1 / 2 of the fiber optic image transmitting rod. The diameter of the circular hole is equal to the diameter of the fiber optic image transmitting rod at 1 / 3 - 1 / 2. The four supporting square columns are connected to the circuit board of the image sensor. The connections between the fixing bracket and the fiber optic image transmitting rod and the circuit board are fixedly bonded with ultraviolet curable glue.

4. The detection imaging method for a chemical reaction process according to claim 1, characterized in that, The detection imaging device for the chemical reaction process also includes a housing. The housing is composed of a protective cap and an end face protective shell connected to each other. There is a circular hole at the bottom of the end face protective shell. The protective cap and the end face protective shell are connected by threads. The end face protective shell includes a first end face protective shell and a second end face protective shell spliced with each other. There are semi-circular holes at the centers of their bottoms, and a circular hole is formed after splicing.

5. The detection imaging method for a chemical reaction process according to claim 4, characterized in that, The housing is a metal housing. The protective cap is cylindrical.

6. The detection imaging method for a chemical reaction process according to claim 1, characterized in that, It also includes a computer, which includes a display device. A chemical reaction particle statistics and analysis unit is arranged in the display device.

7. The detection imaging method for a chemical reaction process according to claim 1, characterized in that, The detection imaging device for the chemical reaction process is obtained through the following steps: Preparation and processing of the fiber optic image transmitting rod; Processing of the bracket of the fiber optic image transmitting rod; Preparation of the encapsulated metal housing; Removal of the protective window of the image sensor glass; Coupling and curing; Encapsulation of the fiber optic image transmitting rod and the image sensor.

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