A rapid detection device and method for fluorine-containing sludge in the pan-semiconductor industry

Abstract

The present application provides a rapid detection device and method for fluorine-containing sludge in the pan-semiconductor industry. The device includes a housing, a sample stage, and a detection system. The sample stage includes a bearing assembly and a second driving member; the bearing assembly is movably connected inside the housing, and the bearing assembly includes a first bearing member having a bearing chamber and a second bearing member having a first installation chamber; the first bearing member is installed in the first installation chamber through a first driving member, and the first driving member is used to drive the first bearing member to rotate around its first central axis; the first central axis extends in a direction perpendicular to the second bearing member; the second driving member is disposed on the second bearing member, and the output end of the second driving member is connected to the first driving member; the second driving member is used to drive the first bearing member to perform an eccentric motion within 1° to 5° relative to the first central axis; the detection system is disposed inside the housing and is used to detect the light element content of the sample to be detected. The present application can perform quantitative detection of light elements and has high detection sensitivity.

Description

Technical Field

[0001] The present application relates to the technical field of treating fluorine-containing sludge in the pan-semiconductor industry, and particularly relates to a rapid detection device and method for fluorine-containing sludge in the pan-semiconductor industry. Background Art

[0002] In recent years, the information technology, new energy industries, and pan-semiconductor industries such as semiconductors, microelectronics, photovoltaics, and optoelectronics have developed rapidly. In the pan-semiconductor industry, hydrofluoric acid (HF) is required to etch, process, and clean components, resulting in a large amount of fluorine-containing wastewater. During the treatment of fluorine-containing wastewater, a large amount of fluorine-containing sludge is generated by the precipitation of calcium ions and fluoride ions in the wastewater. After identification, calcium fluoride (CaF2) accounts for a high proportion, and it has the replaceability of natural fluorite ore.

[0003] Natural fluorite ore is a non-renewable resource. The existing reserves in China can only meet the development needs for 10 years. As a by-product of strategic emerging industries, on the one hand, with the development of emerging industries, the output of fluorine-containing sludge in the pan-semiconductor industry increases year by year, and its fractional recovery and resource utilization system urgently needs to be established. On the other hand, the industry has not yet established a basic method for identifying the quality of fluorine-containing sludge in the pan-semiconductor industry. Due to the large fluctuations in the composition and rapid changes in the quality of fluorine-containing sludge in the pan-semiconductor industry compared to natural fluorite, and the extremely high requirements for the detection frequency and timeliness, the existing analysis methods for fluorine-containing sludge in the pan-semiconductor industry have problems such as cumbersome analysis steps, long detection time, high equipment price, and large volume. Therefore, a large amount of artificial fluorite cannot be effectively identified in terms of quality and is mainly disposed of through low-end disposal paths as ordinary solid waste. Due to the large amount of sludge, environmental protection incidents such as landfill occur frequently.

[0004] X-ray fluorescence spectroscopy detection technology is increasingly widely used in fields such as geology, minerals, metallurgy, and building materials. It uses X-rays emitted by an X-ray tube to irradiate the surface of a sample. Each element in the sample absorbs the X-rays and generates X-ray fluorescence with a specific wavelength. By measuring the wavelength and energy of these X-ray fluorescences, qualitative and quantitative analysis of the sample can be achieved.

[0005] However, X-ray fluorescence spectroscopy technology has insufficient analytical ability for light elements and low detection accuracy for light elements (such as C, N, O, F, etc.) in the sample. Summary of the Invention

[0006] The embodiments of the present application provide a rapid detection device and method for fluorine-containing sludge in the pan-semiconductor industry, which can perform quantitative detection of light elements and has high detection sensitivity.

[0007] In a first aspect, the embodiments of the present application provide a rapid detection device for fluorine-containing sludge in the pan-semiconductor industry, including:

[0008] A housing;

[0009] Sample stage, the sample stage includes a loading component and a second driving member; the loading component is movably connected to the inside of the housing, and the loading component includes a first loading member and a second loading member having a first installation chamber; the first loading member includes a loading chamber for fixing the sample to be detected; wherein, the first loading member is installed in the first installation chamber by a first driving member, and the first driving member is used to drive the first loading member to rotate around its first central axis; the first central axis extends in a direction perpendicular to the second loading member; the second driving member is arranged on the second loading member, and the output end of the second driving member is connected to the first driving member; the second driving member is used to drive the first loading member to perform eccentric motion within a preset range relative to the first central axis; wherein, the preset range is 1° to 5°.

[0010] Detection system, the detection system is arranged inside the housing and is used to detect the light element content of the sample to be detected; wherein, the detection system includes an optical path component, and the optical path component is arranged inside the housing; the optical path component includes a first optical element and a second optical element arranged at intervals; in a cross-section parallel to the housing, the orthographic projection of the sample stage is located on one side of the connection line of the orthographic projections of the first optical element and the second optical element; wherein, both the first optical element and the second optical element include a bent crystal support and a first bent crystal and a second bent crystal rotatably connected to the bent crystal support, the orientations of the first bent crystal and the second bent crystal are opposite, and the materials are different; both the first bent crystal and the second bent crystal include a first radius of curvature and a second radius of curvature, and the first radius of curvature and the second radius of curvature are different.

[0011] In a possible implementation manner, the loading component further includes a third loading member, and the third loading member has a second installation chamber; the second loading member is arranged in the second installation chamber, and at least part of the second driving member is accommodated in the second installation chamber.

[0012] Alternatively, the first bent crystal is used to detect the fluorine element in the fluorine-containing sludge, and the material of the first bent crystal includes lithium fluoride, thallium hydrogen phthalate or pentaerythritol;

[0013] The second bent crystal is used to detect the calcium element in the fluorine-containing sludge, and the material of the second bent crystal includes lithium fluoride or germanium.

[0014] In a possible implementation manner, the sample stage further includes a rotating device, and the rotating device is connected to the loading component and is used to drive the loading component to rotate along a second central axis; the second central axis is perpendicular to the first central axis;

[0015] The sample stage further includes a lifting device, which is connected to the inner wall of the housing and extends along the first central axis;

[0016] The rotating device of the sample stage is connected to the lifting device.

[0017] In a possible implementation, the sample to be detected includes a sample cup with an opening and a transparent film covering the opening; the inner diameter of the sample cup is 3 cm to 5 cm, and the height is 0.6 cm to 1.0 cm;

[0018] A telescopic fixing member is arranged in the bearing chamber, and the telescopic fixing member is configured to be connected to the sample cup and fix the transparent film.

[0019] In a possible implementation, the detection system further includes a light source, a filter exchanger, and a detector. The light source is arranged on one side of the first optical element, the filter exchanger is arranged between the light source and the first optical element, and the filter exchanger includes an aluminum filter and a beryllium filter; the detector is arranged on one side of the second optical element;

[0020] The X-rays emitted by the light source are filtered by the filter of the filter exchanger and then focused and reflected by the first optical element to the sample to be detected; wherein, when the detection device is used to detect fluorine element, the filter of the filter exchanger is a beryllium filter; when the detection device is used to detect calcium element, the filter of the filter exchanger is an aluminum filter;

[0021] The X-rays excite the element to be tested in the sample to be detected to form X-ray fluorescence;

[0022] The X-ray fluorescence is focused and reflected by the second optical element to the detector.

[0023] In a possible implementation, the detection device further includes a constant temperature system, which includes a heating element, at least one temperature sensor, and a constant temperature controller; the heating element and at least one of the temperature sensors are respectively arranged on the housing;

[0024] The constant temperature controller is respectively connected to the heating element and the temperature sensor; the constant temperature controller is used to control the working state of the heating element according to the temperature sensor;

[0025] The constant temperature system further includes at least one fan, and at least one fan is arranged on the housing and is spaced from the temperature sensor;

[0026] At least one of the fans is connected to the constant temperature controller.

[0027] In a possible implementation, the housing includes a first housing and a second housing. The second housing is sleeved on the first housing and encloses a chamber with the first housing;

[0028] The heating element is a resistance wire. The resistance wire is wound around the first housing and accommodated in the chamber;

[0029] The temperature sensor is embedded in the first housing, and the fan is embedded in the second housing.

[0030] In a possible implementation, the detection device further includes a vacuum system. The vacuum system includes a vacuum pressure sensor, a vacuum generator, and a vacuum controller; the vacuum pressure sensor is disposed on the housing for detecting the vacuum degree inside the housing;

[0031] The vacuum generator is communicated with the inner cavity of the housing; wherein, the vacuum generator includes a vacuum pump, an electromagnetic valve, a vacuum valve, a frequency converter, and a connecting pipeline; the vacuum pump, the electromagnetic valve, and the vacuum valve are all disposed on the connecting pipeline, and the frequency converter is connected to the vacuum pump;

[0032] The vacuum controller is respectively connected to the vacuum pressure sensor, the electromagnetic valve, the vacuum valve, the frequency converter, and the pressure relief valve;

[0033] The vacuum controller is used to control the working state of the vacuum generator and the working state of the pressure relief valve according to the vacuum pressure sensor.

[0034] In a possible implementation, the detection device further includes a control system. The control system is respectively connected to the temperature controller and the vacuum controller.

[0035] In a second aspect, an embodiment of the present application provides a rapid detection method for fluorine-containing sludge in the pan-semiconductor industry. The detection method is applied to the rapid detection device for fluorine-containing sludge in the pan-semiconductor industry as described in the first aspect; the detection method includes:

[0036] Install the sample to be detected on the sample stage of the detection device, and start the telescopic fixing member of the test device to fix the transparent film of the sample to be detected by the telescopic fixing member;

[0037] Start the lifting device and the rotating device of the test device to make the sample stage in the test position; wherein, the lifting device drives the bearing assembly of the sample stage to move along the first central axis; and the rotating device is connected to the bearing assembly and is used to drive the bearing assembly to rotate 180° along the second central axis to make the sample stage in the test position; the second central axis is perpendicular to the first central axis;

[0038] Start the first driving member and the second driving member. The first driving member is used to drive the rotation of the first central axis of the first carrier, and the second driving member is used to drive the first carrier to perform eccentric motion relative to the first central axis within a preset range.

[0039] Start the detection system, which is used to test the content of light elements in the sample to be detected.

[0040] In a possible implementation manner, after the step that the sample stage is in the test position, the test method further includes:

[0041] Obtain a plurality of first test temperatures at the current time node and a plurality of second test temperatures at the previous time node; wherein, the test temperature is the temperature inside the housing.

[0042] Determine the temperature change rate according to the plurality of first test temperatures and the plurality of second test temperatures.

[0043] Input the plurality of first test temperatures and the temperature change rate into the adaptive neuro-fuzzy inference algorithm model, and output the power adjustment value of the heating element and the speed adjustment value of the fan through the adaptive neuro-fuzzy inference algorithm model.

[0044] Based on the power adjustment value of the heating element and the current power of the heating element, determine the target power value of the heating element; and based on the speed adjustment value of the fan and the current value of the fan, determine the target speed of the fan.

[0045] Generate a first control instruction of the PID controller based on the difference between the target power value of the heating element and the current power of the heating element; and generate a second control instruction of the PID controller based on the difference between the target speed of the fan and the current value of the fan.

[0046] Adjust the power of the heating element based on the first control instruction; and adjust the speed of the fan based on the second control instruction so that the temperature inside the housing is 28.5°C to 30.5°C.

[0047] In a possible implementation manner, the test method further includes:

[0048] Obtain the first vacuum degree inside the housing.

[0049] Input the first vacuum degree into the fuzzy inference algorithm model of the frequency converter, and output the target speed of the frequency converter through the fuzzy inference algorithm model to adjust the speed of the vacuum pump.

[0050] Obtain the second vacuum degree inside the housing, where the second vacuum degree is the vacuum degree inside the housing after the vacuum pump operates at the target speed for a period of time; obtain an error value according to the second vacuum degree and the target vacuum degree;

[0051] Generate a third control instruction for PID control according to the error value and the target vacuum degree;

[0052] Based on the third control instruction, adjust the frequency converter, and then adjust the speed of the vacuum pump so that the vacuum degree of the housing is 0.8 Kpa to 1 Kpa.

[0053] In the rapid detection device and method for fluorine-containing sludge in the pan-semiconductor industry provided by the embodiments of the present application, the first driving member can drive the first carrier to rotate around its first central axis. At the same time, the second driving member can drive the first carrier to perform eccentric rotation; in this way, during the detection process, on the premise of ensuring that the parameters of the detection system remain unchanged, the surface of the sample to be detected can be irradiated at multiple points, so that the detection system can obtain more test data, reducing the influence of the unevenness of the surface morphology and internal particle distribution of the sample to be detected on the test accuracy, and further improving the detection accuracy of the test device. BRIEF DESCRIPTION OF THE DRAWINGS

[0054] The drawings here are incorporated into the specification and form a part of this specification, showing embodiments consistent with the present application and used together with the specification to explain the principles of the present application.

[0055] Figure 1 It is a schematic structural diagram of the rapid detection device for fluorine-containing sludge in the pan-semiconductor industry provided by the present application;

[0056] Figure 2 is Figure 1 an enlarged schematic diagram of area A in

[0057] Figure 3 It is a partial structural schematic diagram of the rapid detection device for fluorine-containing sludge in the pan-semiconductor industry provided by the present application.

[0058] Description of the reference numerals:

[0059] 100: housing; 110: first housing; 120: second housing; 130: chamber; 140: sealing end cover;

[0060] 200: sample stage; 210: carrier assembly; 211: first carrier; 2111: carrier chamber; 212: second carrier; 2121: first installation chamber; 213: third carrier; 2131: second installation chamber; 214: telescopic fixing member; 215: first driving member;

[0061] 220: Second driving member;

[0062] 230: Rotating device;

[0063] 240: Lifting device; 241: Transmission member; 242: Connecting member;

[0064] 300: Detection system;

[0065] 310: Optical path component; 311: First optical element; 312: Second optical element; 3111: First bent crystal; 3112: Second bent crystal; 3113: Bent crystal bracket; 313: Filter exchanger; 314: First collimator; 315: Diaphragm; 316: Second collimator;

[0066] 320: Light source;

[0067] 330: Detector;

[0068] 400: Sample to be detected;

[0069] 500: Constant temperature system;

[0070] 510: Heating member; 520: Temperature sensor; 530: Constant temperature controller; 540: Fan;

[0071] 600: Vacuum system;

[0072] 610: Vacuum pressure sensor; 620: Vacuum generator; 621: Vacuum pump; 622: Solenoid valve; 623: Vacuum valve; 624: Frequency converter; 625: Connecting pipeline; 630: Vacuum controller; 640: Pressure relief valve;

[0073] 700: Control system.

[0074] Through the above-mentioned drawings, specific embodiments of the present application have been shown, and there will be more detailed descriptions hereinafter. These drawings and textual descriptions are not intended to limit the scope of the concept of the present application in any way, but to illustrate the concept of the present application to those skilled in the art by referring to specific embodiments. Detailed implementation manners

[0075] As described in the background art, the X-ray fluorescence spectroscopy technology in the related art has insufficient ability to analyze light elements, resulting in the problem of low detection accuracy for light elements (such as C, N, O, F, etc.) in the sample to be detected. After research by the inventor, it is found that the reason for this problem is that the primary ray formed by the testing equipment can only excite a specific area of the sample to be detected, and the test data obtained by the testing equipment is affected by the morphology of the specific area, having the technical problem of low detection accuracy.

[0076] In view of the above technical problems, the embodiments of the present application provide a rapid detection device and method for fluorine-containing sludge in the pan-semiconductor industry. The first driving member drives the first bearing member to rotate around its first central axis. At the same time, the second driving member can drive the first bearing member to perform eccentric rotation. In this way, during the detection process, on the premise of ensuring that the parameters of the detection system remain unchanged, the surface of the sample to be detected can be irradiated at multiple points, so that the detection system can obtain more test data, reducing the influence of the unevenness of the surface morphology and internal particle distribution of the sample to be detected on the test accuracy, and thus improving the detection accuracy of the test device.

[0077] In order to make the above objects, features, and advantages of the embodiments of the present application more obvious and understandable, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present application.

[0078] Please refer to the attached Figure 1 The embodiments of the present application provide a rapid detection device for fluorine-containing sludge in the pan-semiconductor industry, which is used to detect fluorine-containing sludge in the sludge; it should be noted that the fluorine-containing sludge not only contains fluorine elements, but also includes calcium elements or other elements. Therefore, in the embodiments of the present application, fluorine elements, calcium elements, and other elements are collectively referred to as hydrogen elements. It should be noted that other elements may include oxygen elements and / or carbon elements.

[0079] The detection device includes a housing 100. The housing 100 is a load-bearing component of the detection device and is used to provide an installation carrier for the sample stage 200 and the detection system 300. It should be noted that the housing 100 can be a single-layer structure or a double-layer structure.

[0080] Exemplarily, the housing 100 includes a first housing 110 and a second housing 120. The second housing 120 is sleeved on the first housing 110 and encloses a chamber 130 with the first housing 110; in this way, the housing 100 is a double-layer structure. The chamber 130 can not only provide an installation area for some components of the detection device, but also play an isolation function. For example, the cavity can have a good heat insulation effect. When the test device works in a high-temperature or low-temperature environment, the chamber 130 can reduce heat transfer and maintain the stability of the internal temperature, which is particularly important for a detection device that requires precise temperature control and can ensure the accuracy and stability of the detection results.

[0081] Among them, the sample stage 200 and the detection system 300 are installed inside the housing 100. For example, the sample stage 200 and the detection system 300 can be installed in the first housing 110. In this embodiment, the housing 100 further includes a top opening and a sealing end cap 140 that seals the top opening. In this way, it is convenient to install the sample to be detected inside the housing 100 through the top opening. At this time, the sealing end cap 140 is used to seal the top opening, prevent the rays formed by the detection system during testing from leaking, and maintain a constant temperature vacuum environment. It should be noted that when the housing 100 includes a first housing 110 and a second housing 120, both the first housing 110 and the second housing 120 can be cylindrical, and both the first housing 110 and the second housing 120 have top openings.

[0082] The testing device further includes a sample stage 200, among which, the sample stage 200 is arranged inside the housing 100. The sample stage 200 includes a loading component 210, and the loading component 210 is movably connected inside the housing 100, that is to say, the loading component 210 is movably connected inside the first housing 110.

[0083] The loading component 210 includes a first loading member 211 and a second loading member 212, and the second loading member 212 has a first installation chamber 2121; the first loading member 211 includes a loading chamber 2111, and the loading chamber 2111 is used to accommodate the sample to be detected to fix the sample to be detected in the sample stage 200.

[0084] It should be noted that there are various choices for the connection method between the sample to be detected and the first loading member 211. Specifically, it can be set according to the structure of the sample to be detected. Exemplarily, the sample to be detected includes a sample cup with an opening and a transparent film that seals the opening; among them, the transparent film not only seals the opening, but also can cover a part of the outer peripheral surface of the sample cup to reduce the risk of the transparent film falling off. Among them, the shape of the sample cup is cylindrical, the inner diameter is 3 cm to 5 cm, and the height is 0.6 cm to 1.0 cm.

[0085] At this time, a telescopic fixing member 214 is arranged inside the loading chamber 2111, and the telescopic fixing member 214 is configured to be connected to the sample cup and fix the transparent film. Exemplarily, the telescopic fixing member 214 can move in a direction towards or away from the center of the loading chamber 2111 to clamp or loosen the sample to be detected. Among them, in addition to fixing the sample cup, the telescopic fixing member also fixes the transparent film, which can prevent the transparent film from detaching from the sample cup, thereby avoiding the spillage of the sample to be detected and improving the safety during the testing process.

[0086] In this example, there are various options for the telescopic fixing member 214. For example, the number of telescopic fixing members 214 is multiple, and each telescopic fixing member 214 may further include a spring and a rubber fixing block. One end of the spring can be connected to the inner wall of the bearing chamber 2111, and the other end can be connected to the rubber fixing block.

[0087] The multiple telescopic fixing members 214 can enclose a space for accommodating the sample to be detected. When the sample to be detected is installed in the bearing chamber 2111, the sample to be detected will squeeze the rubber fixing block and compress the spring. In this way, the elastic force of the spring can be used to fix the sample to be detected.

[0088] For another example, the number of telescopic fixing members 214 is multiple, and each telescopic fixing member may include a driving member and a rubber fixing block. The driving member is fixed to the inner wall of the bearing chamber 2111, and the output shaft of the driving member is connected to the rubber fixing block, and is used to drive the rubber fixing block to move in a direction towards or away from the center of the bearing chamber 2111 to clamp or loosen the sample to be detected.

[0089] It should be noted that the surface shape of the rubber fixing block facing the center of the bearing chamber 2111 can be freely set according to the shape of the sample to be detected, which improves the design flexibility of the telescopic fixing member 214.

[0090] Please continue to refer to the appendix Figure 1 , the first carrier 211 is installed in the first installation chamber 2121 through the first driving member 215. The first driving member 215 is used to drive the first carrier 211 to rotate around its first central axis. Wherein, the first central axis extends in a direction perpendicular to the second carrier 212, that is, the dashed line S1 in the appendix Figure 1 in the figure.

[0091] As a possible implementation manner of the first driving member 215, the first driving member 215 includes a first motor, and its output end is directly connected to the first carrier 211. In this way, when the first motor is started, it will drive the first carrier 211 to rotate around its first central axis S1. Wherein, the first driving member 215 drives the first carrier 211 to rotate at a rotation rate in the range of 1 revolution per second to 2.5 revolutions per second.

[0092] The second driving member 220 is arranged on the second carrier 212, and the output end of the second driving member 220 is connected to the first driving member 215; the second driving member 220 is used to drive the first carrier 211 to perform eccentric motion within a preset range relative to the first central axis S1; wherein, the preset range is 1° to 5°. Wherein, the second driving member 220 can drive the first carrier 211 to perform eccentric rotation at a rotation rate in the range of 0.5 revolution per second to 1.5 revolutions per second.

[0093] It should be understood that the second driving member 220 can be arranged on the bottom surface of the second bearing member 212 or in the first installation chamber 2121.

[0094] As a possible implementation manner of the second driving member 220, the second driving member 220 may include a second motor and an eccentric wheel. The output end of the second motor is connected to the eccentric wheel, and the eccentric wheel is connected to the motor housing of the first driving member through a connecting shaft. In this way, when the first driving member 215 is started alone, it will directly drive the first bearing member 211 to rotate self - axially. When the second motor is started, it will drive the eccentric wheel to rotate. Since the eccentric wheel is connected to the first bearing member 211 (or indirectly to the first motor) through the connecting shaft, this rotation will cause the first bearing member 211 to perform eccentric motion relative to its first central axis. It should be noted that the connecting shaft here may be flexible (such as a universal joint) or rigid, depending on the required motion range and accuracy. And the second driving member 220 can also adopt the cooperation of an eccentric gear and a motor.

[0095] The detection device further includes a detection system 300, which is arranged in the housing 100 and is used to detect the light element content of the sample to be detected. Among them, the detection system 300 is a conventional X - ray spectrometer.

[0096] In this embodiment, by improving the sample stage 200, the sample stage 200 can rotate self - axially and eccentrically. For example, the first driving member 215 can drive the first bearing member 211 to rotate around its first central axis. At the same time, the second driving member can drive the first bearing member 211 to perform eccentric rotation. In this way, during the detection process, combined with the structure of the sample cup, on the premise that the parameters of the detection system 300 remain unchanged, the surface of the sample to be detected can be irradiated at multiple points, so that the detection system 300 can obtain more test data, reducing the influence of the non - uniformity of the surface morphology and internal particle distribution of the sample to be detected on the test accuracy, and thus improving the detection accuracy of the test equipment.

[0097] It should be noted that the parameters of the detection system 300 remaining unchanged may include but are not limited to the incident angle and incident position of the primary ray (X - ray) remaining unchanged.

[0098] In a possible implementation manner, the bearing assembly 210 further includes a third bearing member 213, and the third bearing member 213 has a second installation chamber 2131; the second bearing member 212 is arranged in the second installation chamber 2131. In this way, the bearing assembly 210 can form a three - layer structure, allowing each component to be more effectively arranged in a limited space, thereby optimizing the space utilization rate of the equipment and making the entire equipment more compact and portable. In addition, the third bearing member 213 can also be a connecting component, which is convenient for installing the sample stage 200 in the housing 100.

[0099] Among them, the second driving member 220 is at least partially received in the second installation chamber 2131. In this way, it helps to reduce vibration and noise during driving and improve driving efficiency. At the same time, this layout also helps to protect the second driving member 220 from external environmental interference and damage, thereby extending its service life.

[0100] Please continue to refer to the appended Figure 1 and the appended Figure 2 , the sample stage 200 further includes a rotating device 230. The rotating device 230 is connected to the carrying component 210 and is used to drive the carrying component to rotate along the second central axis; the second central axis is perpendicular to the first central axis. Among them, the second central axis is the dotted line S2 in the appended Figure 2 .

[0101] Taking the orientation shown in the appended Figure 1 and the appended Figure 2 as an example, in the initial state, the opening of the carrying chamber 2111 faces upward. When the sample to be detected is to be installed into the carrying chamber 2111, the rotating device 230 is started. The rotating device 230 drives the carrying component 210 to rotate around the second central axis. That is to say, the rotating device 230 drives the carrying component 210 to rotate 180° in the direction of the arrow in the appended Figure 2 so that the opening of the carrying chamber 2111 faces downward, facilitating the detection system 300 to detect the sample to be detected.

[0102] Among them, the rotating device 230 only needs to be able to drive the carrying component 210 to rotate. Its structure is prior art and will not be elaborated here in this embodiment.

[0103] In this embodiment, through the setting of the rotating device 230, the installation and disassembly of the sample to be detected can be facilitated, thereby improving the detection efficiency.

[0104] In a possible implementation manner, the sample stage 200 further includes a lifting device 240. The lifting device 240 is connected to the inner wall of the housing 100 and extends along the first central axis; the rotating device 230 of the sample stage 200 is connected to the lifting device 240. In this way, the lifting device 240 can drive the rotating device (indirectly drive the carrying component 210) to perform reciprocating motion along the extension direction of the first central axis, thereby adjusting the relative position of the carrying component 210.

[0105] In this way, the introduction of the lifting device 240 enables the carrying component 210 to not only be rotationally adjusted on the horizontal plane through the rotating device 230 but also be positionally adjusted in the vertical direction. This ability to adjust positions in a three-dimensional space greatly enhances the flexibility of the sample stage, enabling the detection system 300 to more accurately position the sample to be detected, thereby optimizing the detection effect.

[0106] Among them, the structure of the lifting device 240 can have various choices. For example, the lifting device 240 can include a driving mechanism, a transmission member, and a connecting member. The output end of the driving mechanism is connected to the connecting member 242 through the transmission member 241. The end of the connecting member 242 facing away from the transmission member 241 is connected to the rotating device 230. In this way, the rotating device 230 and the carrying assembly 210 can be driven to reciprocate synchronously along the extension direction of the first central axis.

[0107] Among them, the type of the transmission member 241 is selected according to the driving mechanism. For example, if the driving mechanism is a motor, correspondingly, the transmission member 241 can include a lead screw and a nut threadedly connected to the lead screw; and the connecting member 242 can be a connecting rod.

[0108] Please refer to Appendix Figure 1 and Appendix Figure 3 , in a possible implementation manner, the detection system 300 includes an optical path assembly 310, and the optical path assembly 310 is disposed in the housing 100.

[0109] Among them, the optical path assembly 310 includes a first optical element 311 and a second optical element 312 arranged at intervals; in a cross-section parallel to the housing, the orthographic projection of the sample stage 200 is located on one side of the line connecting the orthographic projections of the first optical element 311 and the second optical element 312. In this way, it can be ensured that the rays formed by the detection system 300 can form a transmission path among the first optical element 311, the second optical element 312, and the sample 400 to be detected. This layout effectively utilizes the refraction, reflection, or transmission characteristics of the optical elements, enabling the light to be more efficiently directed and focused on the sample 400 to be detected.

[0110] It should be noted that the rays form a transmission path among the first optical element 311, the second optical element 312, and the sample 400 to be detected, which can be in a V shape or in the form of multiple broken lines, as long as it is ensured that the rays formed by the detection system 300 can be received by the detector 330.

[0111] In this embodiment, both the first optical element 311 and the second optical element 312 include a bent crystal bracket 3113, and a first bent crystal 3111 and a second bent crystal 3112 rotatably connected to the bent crystal bracket 3113. The orientations of the first bent crystal 3111 and the second bent crystal 3112 are opposite, and their materials are different.

[0112] For example, the first bent crystal 3111 is used to detect fluorine (F) element in sludge. The material of the first bent crystal includes lithium fluoride (LiF), thallium hydrogen phthalate (TAP), or pentaerythritol (PET). Among them, lithium fluoride and / or pentaerythritol also adopt specific crystal planes. For example, the material of the first bent crystal 3111 is lithium fluoride (200); or, the material of the first bent crystal 3111 is pentaerythritol (PET) (002). Among them, 200 in lithium fluoride (200) represents a specific direction or crystal plane of the crystal. The second bent crystal 3112 is used to detect calcium (Ca) element or other elements in sludge, and its material includes lithium fluoride (LiF) or germanium (Ge). Among them, the material of the second bent crystal 3112 is lithium fluoride (200) or lithium fluoride ((220); or, the material of the second bent crystal 3112 is germanium (111).

[0113] When it is necessary to detect the content of fluorine element in the sample to be detected 400, the first bent crystal 3111 can be rotated so that the curved surface of the first bent crystal 3111 faces the light source of the detection system 300. At the same time, when it is necessary to detect the content of calcium element in the sample to be detected 400, the second bent crystal 3112 can be rotated so that the curved surface of the second bent crystal 3112 faces the light source of the detection system 300. In this way, the same detection device can detect different elements, improving the flexibility of the detection device, reducing the detection cost, improving the detection efficiency, enhancing the detection accuracy, and simplifying the operation process.

[0114] It should be understood that the rotation of the first bent crystal 3111 and the second bent crystal 3112 can be realized by a conventional rotating device.

[0115] Among them, both the first bent crystal 3111 and the second bent crystal 3112 include a first radius of curvature and a second radius of curvature, and the first radius of curvature and the second radius of curvature are different. The first radius of curvature is R, and the second radius of curvature is r; among them, the areas of the first bent crystal 3111 and the second bent crystal 3112 are 30 - 45 mm × 15 - 30 mm, and the thickness is 0.2 - 0.4 mm. The first radius of curvature R = 60 - 150 mm; the second radius of curvature r = 30 - 90 mm.

[0116] In this way, the design of the hyperbolic bent crystal can monochromatize the X-rays irradiated on the first bent crystal 3111 and fully focus them on the focal position with the radius of curvature R as the center, focusing on the detection surface of the sample to be detected 400, and better exciting the fluorine element. Using the spatial layout of multiple hyperbolic bent crystals, a fixed-channel energy spectrum for monochromatic single-channel excitation and reception of the element to be measured is formed, eliminating the particle size effect and mineral effect of photovoltaic sludge, improving the detection limit of X-ray fluorescence spectroscopy for F element, and improving the resolution of the testing equipment.

[0117] Particle size effect: The intensity of X-rays may vary with the particle size of the sample and the inhomogeneity of the sample. This phenomenon; Mineral effect: The phenomenon that the intensity of X-rays varies with the chemical structure of the analyzed component and the crystal form of the mineral.

[0118] To better describe the first radius of curvature R and the second radius of curvature r, this embodiment is explained by a light source and a detector.

[0119] Exemplarily, the detection system 300 further includes a light source 320 and a detector 330. The light source 320 is disposed on one side of the first optical element 311, and the detector 330 is disposed on one side of the second optical element 312.

[0120] The X-rays emitted by the light source 320 are focused and reflected by the first optical element 311 to the sample 400 to be detected; the X-rays excite the elements to be tested in the sample 400 to be detected to form X-ray fluorescence; the X-ray fluorescence is focused and reflected by the second optical element 312 to the detector 330.

[0121] In this embodiment, by improving the sample stage 200 for carrying the sample 400 to be detected, the first optical element 311 and the second optical element 312, the accuracy and precision of the analysis of F element and Ca element in photovoltaic sludge can be ensured, and the detection limit reaches 0.001%, which promotes the development process of replacing natural fluorite ore with photovoltaic sludge.

[0122] Among them, the X target material of the light source 320 is molybdenum (Mo), silver (Ag), rhodium (Rh) or chromium (Cr), the power is 15 - 80 W, and the diffraction energy is 5.40 - 22.16 keV. The detector 330 uses a solid-state detector, which is not limited to a silicon drift detector (SSD), an SDD high-purity silicon detector, a high-purity germanium detector, etc.

[0123] In the embodiment of the present application, the sample stage 200 is located on the center line of the connection line between the light source 320 and the detector 330, and the linear distances from the light source 320 and the detector 330 are equal. Thus, the sample stage 200, the light source 320 and the detector 330 form an isosceles triangle.

[0124] The centers of the light source 320, the first optical element 311 and the sample stage 200 are on a circle with a radius of R; the centers of the detector 330, the second optical element 312 and the sample stage 200 are on another circle with a radius of R. The X-rays formed by the light source 320 are refracted by the first optical element 311 at an incident angle θ to the sample stage 200, and the excited X-ray fluorescence can enter the second optical element 312 at an angle θ and then be refracted to the detector 330.

[0125] Among them, the first radius of curvature is R, and the second radius of curvature r is the radius of the circle obtained by rotating the first optical element 311 with the center of the line connecting the light source 320 to the sample stage 200 as the center of the circle; the radius of curvature R and the rotation radius r satisfy r = R - R COS2θ. In this embodiment, the value range of the incident angle θ is 20° to 30°.

[0126] It should be noted that the optical path component 310 provided in the embodiment of the present application further includes a filter exchanger 313, a first collimator 314, a diaphragm 315, and a second collimator 316; the filter exchanger 313, the first collimator 314, and the first optical element 311 are arranged on the transmission path of the X-rays formed by the light source 320, and the filter exchanger 313 is arranged between the light source 320 and the first collimator 314;

[0127] The diaphragm 315, the second collimator 316, and the detector 330 are arranged on the transmission path of the X-ray fluorescence, and the diaphragm 315 is located between the second collimator 316 and the second optical element 312.

[0128] Among them, the filter exchanger 313 includes an aluminum filter and a beryllium filter. When detecting the F element, the beryllium filter is selected; when detecting the Ca element and other impurity elements, the aluminum filter is selected.

[0129] The first collimator 314 is arranged on the side of the filter exchanger 313 away from the light source 320, and the distance between the light source 320 and the first collimator 314 is 15 - 25 mm.

[0130] The aperture of the diaphragm 315 is 1 - 5 mm. Both the first collimator 314 and the second collimator 316 are mainly made of copper with an aluminum lining, and the aperture is 3 - 5 mm, reducing stray lines and reducing the interference introduced by the collimator material.

[0131] In a possible implementation manner, the detection device further includes a constant temperature system 500, and the constant temperature system 500 includes a heating element 510, at least one temperature sensor 520, and a constant temperature controller 530; the heating element 510 and at least one temperature sensor 520 are respectively arranged on the housing 100; it should be understood that the positions where the heating element 510 and the temperature sensor 520 are arranged on the housing 100 are related to the structure of the housing 100 itself.

[0132] For example, when the housing 100 includes a first housing 110 and a second housing 120, the heating element 510 is a resistance wire, and the resistance wire is wound around the first housing 110 and accommodated in the chamber 130; at this time, the chamber 130 provides an installation space for the layout of the resistance wire. At the same time, the temperature sensor 520 is embedded in the first housing 110, and can better detect the temperature of the inner cavity of the first housing 110.

[0133] The constant temperature controller 530 is respectively connected to the heating element 510 and the temperature sensor 520; the constant temperature controller 530 is used to control the working state of the heating element 510 according to the temperature sensor 520.

[0134] Given that the first optical element 311 and the second optical element 312 have a certain coefficient of thermal expansion, the temperature change in the first housing 110 will cause a change in the surface spacing between the first optical element 311 and the second optical element 312, thereby causing a change in the detection angle and bringing errors to the measurement.

[0135] Therefore, in this embodiment, through the setting of the constant temperature system 500, the constant temperature controller 530 is used to control the working state of the heating element 510 according to the temperature sensor 520; for example, when the temperature in the first housing 110 is lower than the appropriate temperature, the constant temperature controller 530 can control the heating element 510 to work, and then heat the first housing 110. For another example, when the temperature in the first housing 110 is higher than the appropriate temperature, the constant temperature controller 530 can control the heating element 510 to stop working. In this way, it helps to keep the surface spacing between the first optical element 311 and the second optical element 312 stable, thereby ensuring the accuracy of the detection angle and improving the overall measurement accuracy.

[0136] Please continue to refer to the appendix Figure 1 The constant temperature system 500 further includes at least one fan 540. The at least one fan 540 is disposed on the housing and is spaced apart from the temperature sensor 520. The at least one fan 540 is also connected to the constant temperature controller 530. Exemplarily, the fan 540 is embedded in the second housing 120.

[0137] The constant temperature controller 530 can control the start and stop of the fan 540 and the rotation speed of the fan 540. In this way, the housing 100 can be evenly heated by means of the fan 540, which helps to accelerate heat transfer and improve the effect of uniform temperature. Furthermore, it helps to further reduce the measurement error caused by uneven temperature distribution and improve the measurement accuracy.

[0138] It should be noted that the number of the temperature sensors 520 and the fans 540 can be multiple or one. Exemplarily, the number of the temperature sensors 520 and the number of the fans 540 are both multiple; each temperature sensor 520 is spaced apart from each fan 540. Or rather, the multiple temperature sensors 520 and the multiple fans 540 are alternately arranged. For example, one temperature sensor 520 is embedded every 4 - 8 cm 2 and one fan 540 is embedded every 6 - 10 cm 2

[0139] ​In this way, multiple temperature sensors 520 can achieve multi-point and multi-frequency data acquisition. The adaptive neuro-fuzzy inference system (ANFIS) is adopted. The model takes multi-point temperature information and the temperature change rate as inputs, and outputs the power adjustment value of the heating element 510 and the speed regulation value of the fan 540. At the same time, to efficiently train the algorithm, the particle swarm optimization algorithm is used to globally search the parameter space of the ANFIS model. After obtaining the target control value, specific parameter control is realized through the PID algorithm, so as to adjust the calorific value of the heating element 510 and the start-up and ventilation rates of the fan 540, effectively control the temperature fluctuation, and the temperature control accuracy is ±0.1 °C.

[0140] In a possible implementation manner, the detection device further includes a vacuum system 600. The vacuum system 600 includes a vacuum pressure sensor 610, a vacuum generator 620, a vacuum controller 630, and a pressure relief valve 640. The vacuum pressure sensor 610 is disposed on the housing 100 and is used to detect the vacuum degree inside the housing 100. The pressure relief valve 640 is installed on the housing 100 and is connected to the vacuum controller 630. When the housing 100 includes a first housing 110 and a second housing 120, the pressure relief valve 640 is installed on the first housing 110.

[0141] Among them, the vacuum pressure sensor 610 can be a resistive vacuum gauge tube. The resistive vacuum gauge tube affects the temperature of the element by the heat conduction ability of the space gas, changes the resistivity of the sensitive element with the vacuum degree, and can then convert and measure the vacuum degree. Combined with the precise cavity temperature, it can accurately control the detection performance of the detection device.

[0142] The vacuum generator 620 is communicated with the inner cavity of the housing 100 and is connected to the vacuum generator 620. The vacuum pressure sensor 610 provides a theoretical basis for controlling the working state of the vacuum generator 620, so as to facilitate adjusting the vacuum degree inside the housing 100. It should be noted that when the housing 100 includes a first housing 110 and a second housing 120, the vacuum pressure sensor 610 is disposed on the first housing 110 and is used to detect the vacuum degree inside the first housing 110. The vacuum generator 620 is communicated with the inner cavity of the first housing 110 and is used to adjust the vacuum degree inside the first housing 110.

[0143] Among them, the vacuum generator 620 includes a vacuum pump 621, a solenoid valve 622, a vacuum valve 623, an inverter 624, and a connecting pipeline 625. The vacuum pump 621, the solenoid valve 622, and the vacuum valve 623 are all disposed on the connecting pipeline 625. The inverter 624 is connected to the vacuum pump 621 and is used to adjust the rotation speed of the vacuum pump 621.

[0144] The vacuum controller 630 is respectively connected to the vacuum pressure sensor 610, the solenoid valve 622, the vacuum valve 623, the inverter 624, and the pressure relief valve 640.

[0145] When the vacuum pressure sensor 610 measures that the vacuum degree reaches the set value, the vacuum controller 630 receives the test signal of the vacuum pressure sensor 610 and processes it to form corresponding action instructions. For example, the vacuum controller 630 can control the solenoid valve 622 to regulate the start and stop of the vacuum pump 621; it can also adjust the rotation speed of the vacuum pump 621 through the frequency converter 624, so as to meet the pressure value in the first housing 110 and apply different strategies in different stages. In the vacuum pumping stage, the frequency converter adopts a fuzzy inference algorithm to quickly respond to the target rotation speed according to the current pressure value; when approaching the target vacuum value, it is dynamically adjusted through the PID algorithm to avoid overshoot or oscillation; in the vacuum holding stage, it runs at a low speed to reduce energy consumption and maintain a stable vacuum degree. In this way, it can ensure that there is an appropriate vacuum degree in the first housing 110, and the appropriate vacuum degree can reduce the absorption of X-rays by air, and avoid the fluorescence generated by water vapor and carbon dioxide in the air under the action of X-rays, so as to avoid interfering with the X-ray fluorescence signal of the sample 400 to be detected.

[0146] After the detection is completed, the vacuum controller 630 can also control the opening of the pressure relief valve 640 to relieve the pressure of the housing.

[0147] In a possible implementation, the detection device further includes a control system 700, and the control system 700 is respectively connected to the constant temperature controller 530 and the vacuum controller 630. Among them, the signal calculation and processing of the constant temperature controller 530 and the vacuum controller 630 and the control system 700 are located in the same host. In this way, the test equipment can be simplified.

[0148] The control system 700 uses a high-performance processing unit combined with a variety of optimization algorithms to achieve precise analysis and processing of the signals collected by the detector 330. First, an adaptive filtering algorithm is used to remove signal noise, and calibration is performed using a standard sample calibration curve to ensure the accurate correspondence between the signal intensity and the element content. Subsequently, the spectral characteristic peaks are extracted through principal component analysis to achieve quantitative analysis of F and Ca elements. In addition, to improve the adaptability of complex samples, the system uses particle swarm optimization to globally optimize the model parameters, and combines the PID algorithm to control the constant temperature and vacuum modules to ensure environmental stability, and finally generates reliable detection results and analysis reports.

[0149] The embodiment of the present application also provides a rapid detection method for fluorine-containing sludge in the pan-semiconductor industry, and the detection method is applied to a rapid detection device for fluorine-containing sludge in the pan-semiconductor industry described in any of the above embodiments.

[0150] The detection method includes:

[0151] Step S100: Install the sample to be detected on the sample stage of the detection device, and start the telescopic fixing member of the test device so that the telescopic fixing member fixes the transparent film of the sample to be detected.

[0152] Among them, the preparation of the sample to be detected also needs to be carried out in a certain way. For example, weigh 3g - 3.5g of sludge sample and place it in a sample cup. Then, compact it using a press, where the pressure of the press is 20Mpa - 30Mpa.

[0153] Step S200: Start the lifting device and the rotating device of the testing equipment so that the sample stage is in the testing position; among them, the lifting device drives the bearing component of the sample stage to move along the first central axis; and the rotating device is connected to the bearing component and is used to drive the bearing component to rotate 180° along the second central axis; the second central axis is perpendicular to the first central axis.

[0154] In this embodiment, first start the lifting device, and use the lifting device to drive the bearing component of the sample stage to move along the first central axis to be in the testing position; or rather, the lifting device can adjust the height of the bearing component.

[0155] After that, start the rotating device of the testing equipment. The rotating device is connected to the bearing component and is used to drive the bearing component to rotate 180° along the second central axis so that the opening of the sample to be detected faces downward; among them, the second central axis is perpendicular to the first central axis.

[0156] Step S300: Start the first driving member and the second driving member. The first driving member is used to drive the first central axis of the first bearing member to rotate, and the second driving member is used to drive the first bearing member to perform eccentric motion within a preset range relative to the first central axis.

[0157] After that, adjust the test parameters inside the housing of the testing equipment so that the test parameters reach the test conditions; among them, the test parameters include test temperature and vacuum degree. Exemplarily, through the constant temperature system 500 and the vacuum system 600, adjust the test parameters. For example, make the test temperature inside the housing 100 be 28.5°C - 30.5°C; the vacuum degree is 0.8Kpa - 1Kpa.

[0158] Step 400: Start the detection system. The detection system is used to test the content of light elements in the sample to be detected.

[0159] In order to improve the detection accuracy of the detection system, in this embodiment, the environment inside the housing is also controlled before starting the detection system.

[0160] In one possible implementation, the test method further includes:

[0161] Obtain multiple first test temperatures at the current time node and multiple second test temperatures at the previous time node; among them, the test temperature is the temperature inside the housing.

[0162] In this embodiment, the first test temperature and the second test temperature are obtained by a temperature sensor. It should be noted that the multiple first test temperatures refer to the set of temperatures obtained at multiple different test points.

[0163] Determine the temperature change rate according to the multiple first test temperatures and the multiple second test temperatures.

[0164] Input the multiple first test temperatures and the temperature change rate into the adaptive neuro-fuzzy inference algorithm model, and output the power adjustment value of the heating element and the speed adjustment value of the fan through the adaptive neuro-fuzzy inference algorithm model.

[0165] Based on the power adjustment value of the heating element and the current power of the heating element, determine the target power value of the heating element; and, based on the speed adjustment value of the fan and the current value of the fan, determine the target speed of the fan.

[0166] Generate the first control instruction of the PID controller based on the difference between the target power value of the heating element and the current power of the heating element; and, generate the second control instruction of the PID controller based on the difference between the target speed of the fan and the current value of the fan.

[0167] Adjust the power of the heating element based on the first control instruction; and adjust the speed of the fan based on the second control instruction so that the temperature inside the housing is 28.5°C to 30.5°C.

[0168] In this way, by reasonably optimizing the power of the heating element and the speed of the fan through multiple algorithms, it is possible to ensure that the temperature inside the housing is always within a reasonable range, and the temperature inside the housing is 28.5°C to 30.5°C.

[0169] In a possible implementation manner, the test method further includes:

[0170] Obtain the first vacuum degree inside the housing.

[0171] Input the first vacuum degree into the fuzzy inference algorithm model, and output the target speed of the frequency converter through the fuzzy inference algorithm model.

[0172] Adjust the speed of the vacuum pump according to the target speed.

[0173] Obtain the second vacuum degree inside the housing, where the second vacuum degree is the vacuum degree inside the housing after the vacuum pump operates at the target speed for a period of time.

[0174] Obtain the error value based on the second vacuum degree and the target vacuum degree.

[0175] Generate the third control instruction of the PID control according to the error value and the target vacuum degree.

[0176] Based on the third control instruction, the actual rotation speed of the vacuum pump is adjusted through a frequency converter so that the vacuum degree of the housing is 0.8 Kpa to 1 Kpa.

[0177] In this way, combining the advantages of the fuzzy inference algorithm and the PID algorithm, the fuzzy inference algorithm can quickly calculate the target rotation speed according to the current vacuum degree, enabling the system to quickly approach the target vacuum degree range (0.8 Kpa to 1 Kpa) and shortening the response time; while, the PID algorithm eliminates the steady-state error through the fine adjustment of the error value and suppresses oscillations through the differential link to ensure that the vacuum degree is stable within the target range and improve the control accuracy.

[0178] In this embodiment, particle swarm optimization can be used to optimize the adaptive neuro-fuzzy inference algorithm model and the fuzzy inference algorithm model respectively to improve the accuracy of the above models.

[0179] And during the whole detection process, that is, the detection data is optimized. Exemplarily:

[0180] Obtain the detection signal; the detection signal is obtained through a detector.

[0181] Input the detection signal into the adaptive filtering algorithm model to output the de-noised detection signal.

[0182] Calibrate the de-noised detection signal using the calibration curve of the standard sample to form the calibrated detection signal. In this way, the accurate correspondence between the signal fullness and the light element content can be ensured.

[0183] Perform principal component analysis on the calibrated detection signal to extract the spectral characteristic peaks.

[0184] Based on the spectral characteristic peaks, perform quantitative analysis on the light elements.

[0185] In this embodiment, particle swarm optimization can be used to optimize the adaptive filtering algorithm model to improve the accuracy of the adaptive filtering algorithm model.

[0186] This embodiment uses the above detection equipment to detect sludge of different qualities.

[0187] Example 1

[0188] Detect sludge of higher quality and different batches, where the CaF2 content in the sludge is more than 80%. The specific test data is shown in Table 1:

[0189] Table 1 Detection results of sludge of higher quality and different batches

[0190]

[0191] Example 2

[0192] The sludge of lower quality and different batches was tested, and the content of CaF2 in the sludge was below 40%. The specific test data are shown in Table 2:

[0193] Table 2 Test results of sludge of lower quality and different batches

[0194]

[0195] It can be clearly seen from Table 1 and Table 2 that whether it is high-quality sludge or low-quality sludge, it can accurately detect the light elements in the sludge, thereby providing a scientific basis and optimization plan for sludge treatment, utilization and disposal, and helping to improve the resource utilization efficiency and promote environmental sustainable development.

[0196] In this specification, the embodiments or implementation manners are described in a progressive manner. Each embodiment focuses on the differences from other embodiments. The same or similar parts among the embodiments can be referred to each other.

[0197] It should be noted that the phrases such as "an embodiment", "embodiment", "exemplary embodiment", "some embodiments" mentioned in the specification mean that the described embodiments may include specific features, structures or characteristics, but not necessarily every embodiment includes such specific features, structures or characteristics. In addition, such phrases do not necessarily refer to the same embodiment. Moreover, when combining a specific feature, structure or characteristic with an embodiment, implementing such a feature, structure or characteristic in combination with other embodiments, whether explicitly or implicitly described, is within the knowledge scope of those skilled in the art.

[0198] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present application, rather than to limit them; although the present application has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that they can still modify the technical solutions recorded in the foregoing embodiments, or perform equivalent replacements on some or all of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present application.

Claims

1. A rapid detection device for fluorine-containing sludge in the semiconductor industry, characterized in that: include: case; A sample stage, the sample stage comprising a bearing assembly and a second driving member; the bearing assembly is movably connected in the shell, and the bearing assembly comprises a first bearing member and a second bearing member having a first mounting chamber; the first bearing member comprises a bearing chamber, and the bearing chamber is used to fix a sample to be detected; wherein, the first bearing member is installed in the first mounting chamber by a first driving member, and the first driving member is used to drive the first bearing member to rotate around its first central axis; the first central axis extends in a direction perpendicular to the second bearing member; the second driving member is arranged on the second bearing member, and the output end of the second driving member is connected to the first driving member; the second driving member is used to drive the first bearing member to perform eccentric rotation within a preset range relative to the first central axis; wherein the preset range is 1° to 5°, and the rotation rate of the eccentric rotation of the first bearing member is 0.5 rev / sec to 1.5 rev / sec; A detection system, the detection system is arranged in the shell, and is used to detect the light element content of the sample to be detected; the detection system includes an optical path component, a light source and a detector, and the optical path component is arranged in the shell; the optical path component includes a first optical element and a second optical element arranged at intervals; on a cross section parallel to the shell, the orthographic projection of the sample stage is located on one side of a line connecting the orthographic projection of the first optical element and the orthographic projection of the second optical element; wherein the first optical element and the second optical element both include a bent crystal bracket and a first bent crystal and a second bent crystal rotatably connected to the bent crystal bracket, the orientation of the first bent crystal is opposite to that of the second bent crystal, and the materials are different; the first bent crystal is used to detect the fluorine element in the fluorine-containing sludge, and the second bent crystal is used to detect the calcium element in the fluorine-containing sludge; the first bent crystal and the second bent crystal both include a first radius of curvature and a second radius of curvature, and the first radius of curvature and the second radius of curvature are different; The centers of the light source, the first optical element, and the sample stage are on a circle with a radius of R, and the centers of the detector, the second optical element, and the sample stage are on another circle with a radius of R. The X-rays formed by the light source are refracted to the sample stage through the first optical element at an incident angle θ, and the excited X-ray fluorescence is incident on the second optical element at an angle θ and then refracted to the detector; the first curvature radius is R, and the second curvature radius r is the radius of a circle obtained by rotating the first optical element with the center of the line connecting the light source to the sample stage as the center of the circle, and the first curvature radius R and the second curvature radius r satisfy ; The sample stage further comprises a rotating device, which is connected to the carrying assembly and is used to drive the carrying assembly to rotate along a second central axis; the second central axis is perpendicular to the first central axis.

2. The rapid detection device for fluorine-containing sludge in the pan-semiconductor industry according to claim 1 is characterized in that: The bearing assembly further includes a third bearing member, the third bearing member having a second mounting chamber; the second bearing member is disposed in the second mounting chamber, and the second driving member is at least partially accommodated in the second mounting chamber; or, The material of the first bent crystal includes lithium fluoride, thallium hydrogen phthalate, and pentaerythritol; The material of the second bent crystal includes lithium fluoride or germanium.

3. The rapid detection device for fluorine-containing sludge in the pan-semiconductor industry according to claim 2 is characterized in that: The sample stage further comprises a lifting device, which is connected to the inner wall of the shell and extends along the first central axis; the rotating device of the sample stage is connected to the lifting device.

4. The rapid detection device for fluorine-containing sludge in the pan-semiconductor industry according to claim 3 is characterized in that: The sample to be detected includes a sample cup with an opening and a transparent film covering the opening; the inner diameter of the sample cup is 3 cm to 5 cm, and the height is 0.6 cm to 1.0 cm; A telescopic fixing member is disposed in the carrying chamber, and the telescopic fixing member is configured to be connected to the sample cup and fix the transparent film.

5. The rapid detection device for fluorine-containing sludge in the pan-semiconductor industry according to any one of claims 1 to 4, characterized in that: The detection system further comprises a light source, a filter exchanger and a detector, wherein the light source is arranged at one side of the first optical element, the filter exchanger is arranged between the light source and the first optical element, and the filter exchanger comprises an aluminum filter and a beryllium filter; the detector is arranged at one side of the second optical element; The X-rays emitted by the light source are filtered by the filter of the filter exchanger, and then focused and reflected to the sample to be detected by the first optical element; wherein, when the rapid detection device is used to detect the fluorine element, the filter of the filter exchanger is a beryllium filter; when the rapid detection device is used to detect the calcium element, the filter of the filter exchanger is an aluminum filter; The X-rays excite the elements to be tested in the sample to be tested to form X-ray fluorescence; The X-ray fluorescence is focused and reflected to the detector by the second optical element.

6. The rapid detection device for fluorine-containing sludge in the pan-semiconductor industry according to claim 5 is characterized in that: The rapid detection device further comprises a constant temperature system, which comprises a heating element, at least one temperature sensor and a constant temperature controller; the heating element and at least one temperature sensor are respectively arranged on the housing; The thermostatic controller is connected to the heating element and the temperature sensor respectively; the thermostatic controller is used to control the working state of the heating element according to the temperature sensor; The constant temperature system further comprises at least one fan, wherein the at least one fan is arranged on the housing and spaced apart from the at least one temperature sensor; and the at least one fan is connected to the constant temperature controller.

7. The rapid detection device for fluorine-containing sludge in the pan-semiconductor industry according to claim 6 is characterized in that: The shell comprises a first shell and a second shell, wherein the second shell is sleeved on the first shell and encloses a chamber with the first shell; The heating element is a resistance wire, which is wound on the first shell and accommodated on the chamber; the temperature sensor is embedded in the first shell, and the fan is embedded in the second shell.

8. The rapid detection device for fluorine-containing sludge in the pan-semiconductor industry according to claim 6 or 7, characterized in that: The rapid detection device also includes a vacuum system, which includes a vacuum pressure sensor, a vacuum generator, a vacuum controller and a pressure relief valve; the vacuum pressure sensor is arranged on the housing and is used to detect the vacuum degree in the housing; The vacuum generator is in communication with the inner cavity of the housing; wherein the vacuum generator comprises a vacuum pump, a solenoid valve, a vacuum valve, a frequency converter and a connecting pipeline; the vacuum pump, the solenoid valve and the vacuum valve are all arranged on the connecting pipeline, and the frequency converter is connected to the vacuum pump; The vacuum controller is respectively connected to the vacuum pressure sensor and the solenoid valve, the vacuum valve, the frequency converter and the pressure relief valve; The vacuum controller is used to control the working state of the vacuum generator and the working state of the pressure relief valve according to the vacuum pressure sensor.

9. The rapid detection device for fluorine-containing sludge in the pan-semiconductor industry according to claim 8, characterized in that: The rapid detection device also includes a control system, which is connected to the constant temperature controller and the vacuum controller respectively.

10. A rapid detection method for fluorine-containing sludge in the semiconductor industry, characterized in that: The detection method is applied to the rapid detection device for fluorine-containing sludge in the pan-semiconductor industry as claimed in any one of claims 1 to 9; the detection method comprises: Installing the sample to be tested on the sample stage of the rapid testing device, and starting the telescopic fixing member of the rapid testing device so that the telescopic fixing member fixes the transparent film of the sample to be tested; The lifting device and the rotating device of the rapid detection device are started to place the sample stage in the test position; wherein the lifting device drives the bearing assembly of the sample stage to move along the first central axis; and the rotating device is connected to the bearing assembly to drive the bearing assembly to rotate 180° along the second central axis; the second central axis is perpendicular to the first central axis; Start a first driving member and a second driving member, wherein the first driving member is used to drive the first central axis of the first bearing member to rotate, and the second driving member is used to drive the first bearing member to rotate eccentrically within a preset range relative to the first central axis; A detection system is started, wherein the detection system is used to test the content of light elements in the sample to be detected.

11. The rapid detection method for fluorine-containing sludge in the pan-semiconductor industry according to claim 10, characterized in that: After the step of the sample stage being in the test position, the detection method further comprises: Acquire multiple first test temperatures at a current time node and multiple second test temperatures at a previous time node; wherein the test temperature is the temperature inside the shell; determining a temperature change rate according to a plurality of the first test temperatures and a plurality of the second test temperatures; Inputting the plurality of the first test temperatures and the temperature change rates into an adaptive neural fuzzy inference algorithm model, and outputting a power adjustment value of the heating element and a speed adjustment value of the fan through the adaptive neural fuzzy inference algorithm model; Determining a target power value of the heating element based on the power adjustment value of the heating element and the current power of the heating element; and determining a target speed of the fan based on the speed adjustment value of the fan and the current value of the fan; generating a first control instruction of the PID controller based on a difference between a target power value of the heating element and a current power of the heating element; and generating a second control instruction of the PID controller based on a difference between a target speed of the fan and a current value of the fan; Based on the first control instruction, the power of the heating element is adjusted; and based on the second control instruction, the speed of the fan is adjusted so that the temperature inside the housing is 28.5° C. to 30.5° C.

12. The rapid detection method for fluorine-containing sludge in the pan-semiconductor industry according to claim 11, characterized in that: The detection method further comprises: obtaining a first vacuum degree in the housing; Inputting the first vacuum degree into a fuzzy inference algorithm model, and outputting a target speed of the frequency converter through the fuzzy inference algorithm model; adjusting the speed of the vacuum pump according to the target speed; Obtaining a second vacuum degree in the shell, wherein the second vacuum degree is the vacuum degree in the shell after the vacuum pump runs at a target speed for a period of time; and obtaining an error value according to the second vacuum degree and the target vacuum degree; generating a third control instruction for PID control according to the error value and the target vacuum degree; Based on the third control instruction, the actual rotation speed of the vacuum pump is adjusted by the frequency converter so that the vacuum degree of the shell is 0.8 Kpa to 1 Kpa.

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