Rapid detection equipment and method for fluorine-containing sludge in generic semiconductor industry
By designing a sample stage that can rotate and eccentrically rotate and an improved optical path component, the problems of low detection accuracy and large equipment volume in the prior art are solved, and the rapid and accurate detection of light elements in fluorine-containing sludge in the pan-semiconductor industry are achieved.
Patent Information
- Application Number
- CN202510213865.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-26
- Publication Date
- 2025-03-25
- Estimated Expiration
- 2045-02-26
AI Technical Summary
The prior art is difficult to quickly and accurately detect light elements such as fluorine-containing sludge in the pan-semiconductor industry, such as fluorine and calcium, resulting in low detection accuracy and high equipment price and large volume.
A rapid detection device is designed, which drives the first carrier to rotate about its central axis through the first driving member, and drives the first carrier to rotate eccentrically through the second driving member to realize multi-point irradiation on the surface of the sample to be detected. Combined with the improved optical path assembly and detection system, the detection accuracy is improved.
Quantitative detection of light elements in fluorine-containing sludge is achieved, the detection sensitivity and accuracy are improved, and the volume and cost of the equipment are reduced.
Smart Images

Figure CN119688754A_ABST
Abstract
Description
Technical Field
[0001] The present application relates to the technical field of treatment of fluorine-containing sludge in the pan-semiconductor industry, and in particular to a rapid detection device and method for fluorine-containing sludge in the pan-semiconductor industry. Background Art
[0002] In recent years, information technology, new energy industry, semiconductor, microelectronics, photovoltaic, optoelectronics and other pan-semiconductor industries have developed rapidly. In the pan-semiconductor industry, hydrofluoric acid (HF) is needed to etch, process and clean components, which generates a large amount of fluorine-containing wastewater. During the treatment of fluorine-containing wastewater, calcium ions and fluoride ions in the wastewater precipitate to form a large amount of fluorine-containing sludge. It has been identified that calcium fluoride (CaF2) accounts for a high proportion and is replaceable for natural fluorite ore.
[0003] Natural fluorite is a non-renewable resource. my country's current reserves can only meet the development needs for 10 years. As a by-product of a strategic emerging industry, on the one hand, with the development of emerging industries, the output of fluorine-containing sludge in the pan-semiconductor industry has increased year by year, and its quality recovery and resource utilization system is in urgent need of establishment. On the other hand, the industry has not yet established a basic quality identification method for fluorine-containing sludge in the pan-semiconductor industry. Because the composition of fluorine-containing sludge in the pan-semiconductor industry fluctuates greatly and the quality changes rapidly compared to natural fluorite, it has extremely high requirements for the frequency and timeliness of detection. 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 prices and large volumes. Therefore, a large amount of artificial fluorite cannot be effectively identified in terms of quality and is treated as ordinary solid waste, mainly through low-end disposal. Due to the large amount of sludge, landfill and other severe environmental incidents occur frequently.
[0004] X-ray fluorescence spectroscopy detection technology is increasingly used in the fields of geology, minerals, metallurgy, building materials, etc. It uses X-rays emitted by an X-ray tube to irradiate the sample surface. After the elements in the sample absorb the X-rays, they produce X-ray fluorescence of a specific wavelength. By measuring the wavelength and energy of these X-ray fluorescence, qualitative and quantitative analysis of the sample can be achieved.
[0005] However, X-ray fluorescence spectroscopy is not capable of analyzing light elements, and has low detection accuracy for light elements (C, N, O, F, etc.) in samples. Summary of the invention
[0006] The embodiments of the present application provide a rapid detection device and method for fluorine-containing sludge in the semiconductor industry, which can perform quantitative detection of light elements and has high detection sensitivity.
[0007] In a first aspect, the present application provides a rapid detection device for fluorine-containing sludge in the semiconductor industry, including:
[0008] case;
[0009] 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 movement within a preset range relative to the first central axis; wherein the preset range is 1° to 5°;
[0010] A detection system, wherein the detection system is arranged in the shell and is used to detect the light element content of the sample to be detected; wherein the detection system includes an optical path component, wherein 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 and the second bent crystal both include a first radius of curvature and a second radius of curvature, and the first radius of curvature is different from the second radius of curvature.
[0011] In a possible implementation, the bearing assembly further includes a third bearing member having a second installation chamber; the second bearing member is disposed in the second installation chamber, and the second driving member is at least partially accommodated in the second installation chamber.
[0012] Alternatively, the first curved crystal is used to detect the fluorine element in the fluorine-containing sludge, and the material of the first curved crystal includes lithium fluoride, thallium hydrogen phthalate or pentaerythritol;
[0013] The second bent crystal is used to detect calcium 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, 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;
[0015] The sample stage further includes a lifting device, which is connected to the inner wall of the shell 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 disposed in the carrying 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, wherein the light source is disposed on one side of the first optical element, the filter exchanger is disposed between the light source and the first optical element, and the filter exchanger includes an aluminum filter and a beryllium filter; the detector is disposed 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 to the sample to be detected by the first optical element; wherein, when the detection device is used to detect the fluorine element, the filter of the filter exchanger is a beryllium filter; when the detection device is used to detect the calcium element, the filter of the filter exchanger is an aluminum filter;
[0021] The X-rays excite the elements to be tested in the sample to be tested to form X-ray fluorescence;
[0022] The X-ray fluorescence is focused and reflected to the detector by the second optical element.
[0023] In a possible implementation, the detection device further includes a constant temperature system, the constant temperature system includes 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;
[0024] 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;
[0025] The constant temperature system further comprises at least one fan, wherein at least one fan is arranged on the housing and spaced apart from the temperature sensor;
[0026] At least one of the fans is connected to the thermostatic controller.
[0027] In a possible implementation, the shell includes 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;
[0028] The heating element is a resistance wire, which is wound on the first shell and accommodated in the chamber;
[0029] The temperature sensor is embedded in the first shell, and the fan is embedded in the second shell.
[0030] In a possible implementation, the detection device further includes a vacuum system, and the vacuum system includes a vacuum pressure sensor, a vacuum generator, and a vacuum controller; the vacuum pressure sensor is disposed on the housing and is used to detect the vacuum degree in the housing;
[0031] 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;
[0032] 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;
[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, and the control system is connected to the constant temperature controller and the vacuum controller respectively.
[0035] In a second aspect, an embodiment of the present application provides a method for rapid detection of fluorine-containing sludge in a pan-semiconductor industry, and the detection method is applied to the rapid detection device for fluorine-containing sludge in a pan-semiconductor industry as described in the first aspect; the detection method comprises:
[0036] Installing the sample to be tested on the sample stage of the testing device, and starting the telescopic fixing member of the testing device so that the telescopic fixing member fixes the transparent film of the sample to be tested;
[0037] Start the lifting device and the rotating device of the test equipment to put 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, so that the sample stage is in the test position; the second central axis is perpendicular to the first central axis;
[0038] 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 perform an eccentric movement within a preset range relative to the first central axis;
[0039] A detection system is started, wherein the detection system is used to test the content of light elements in the sample to be detected.
[0040] In a possible implementation manner, after the step of placing the sample stage in the testing position, the testing method further includes:
[0041] 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;
[0042] determining a temperature change rate according to a plurality of the first test temperatures and a plurality of the second test temperatures;
[0043] Inputting the plurality of the first test temperatures and the temperature change speeds 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;
[0044] 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;
[0045] 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;
[0046] 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.
[0047] In a possible implementation, the testing method further includes:
[0048] obtaining a first vacuum degree in the housing;
[0049] Inputting the first vacuum degree into a fuzzy inference algorithm model of a frequency converter, and outputting a target speed of the frequency converter through the fuzzy inference algorithm model to adjust the speed of a vacuum pump;
[0050] 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;
[0051] generating a third control instruction for PID control according to the error value and the target vacuum degree;
[0052] Based on the third control instruction, the frequency converter is adjusted, and then the rotation speed of the vacuum pump is adjusted so that the vacuum degree of the shell is 0.8Kpa to 1Kpa.
[0053] In a rapid detection device and method for fluorine-containing sludge in a pan-semiconductor industry provided in an embodiment of the present application, a first driving member can drive a first supporting member to rotate around its first central axis, and at the same time, a second driving member can drive the first supporting member to rotate eccentrically; in this way, during the detection process, while 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 impact of the surface morphology of the sample to be detected and the uneven distribution of internal particles on the test accuracy, thereby improving the detection accuracy of the test equipment. BRIEF DESCRIPTION OF THE DRAWINGS
[0054] The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the present application and, together with the description, serve to explain the principles of the present application.
[0055] Figure 1 A schematic diagram of the structure of a rapid detection device for fluorine-containing sludge in the pan-semiconductor industry provided in this application;
[0056] Figure 2 for Figure 1 A magnified schematic diagram of the middle A area;
[0057] Figure 3 A partial structural schematic diagram of the rapid detection equipment for fluorine-containing sludge in the pan-semiconductor industry provided in this application.
[0058] Description of reference numerals:
[0059] 100: housing; 110: first housing; 120: second housing; 130: chamber; 140: sealing end cover;
[0060] 200: sample stage; 210: bearing assembly; 211: first bearing member; 2111: bearing chamber; 212: second bearing member; 2121: first mounting chamber; 213: third bearing member; 2131: second mounting 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 curved crystal; 3112: second curved crystal; 3113: curved crystal support; 313: filter exchanger; 314: first collimator; 315: aperture; 316: second collimator;
[0066] 320: light source;
[0067] 330: detector;
[0068] 400: Sample to be tested;
[0069] 500: Constant temperature system;
[0070] 510: heating element; 520: temperature sensor; 530: thermostat 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] The above drawings have shown clear embodiments of the present application, which will be described in more detail later. These drawings and text descriptions are not intended to limit the scope 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 DESCRIPTION
[0075] As described in the background technology, the X-ray fluorescence spectroscopy technology in the related art is insufficient in its ability to analyze light elements, resulting in the problem of low detection accuracy of light elements (C, N, O, F, etc.) in the sample to be tested. The inventors have found that the reason for this problem is that the primary ray formed by the test equipment can only excite a specific area of the sample to be tested, and the test data obtained by the test equipment is affected by the morphology of the specific area, resulting in a technical problem of low detection accuracy.
[0076] In response to the above technical problems, the embodiments of the present application provide a rapid detection device and method for fluorine-containing sludge in the semiconductor industry. The first driving member drives the first carrier to rotate around its first central axis. At the same time, the second driving member can drive the first carrier to rotate eccentrically. In this way, while ensuring that the parameters of the detection system remain unchanged during the detection process, the surface of the sample to be detected can be irradiated at multiple points, so that the detection system can obtain more test data, reduce the impact of the surface morphology of the sample to be detected and the uneven distribution of internal particles on the test accuracy, and thereby improve the detection accuracy of the test equipment.
[0077] In order to make the above-mentioned purposes, 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 in conjunction with the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without creative work belong to the scope of protection of this application.
[0078] Please refer to the attached Figure 1 The present application embodiment provides a rapid detection device for fluorine-containing sludge in the pan-semiconductor industry, which is used to detect fluorine-containing sludge in sludge; it should be noted that fluorine-containing sludge contains not only fluorine but also calcium or other elements, therefore, the present application embodiment refers to fluorine, calcium and other elements as hydrogen. It should be noted that other elements may include oxygen and / or carbon.
[0079] The detection device comprises a housing 100, which is a bearing component of the detection device and is used to provide a mounting carrier for the sample stage 200 and the detection system 300. It should be noted that the housing 100 may be a single-layer structure or a double-layer structure.
[0080] Exemplarily, the shell 100 includes a first shell 110 and a second shell 120, and the second shell 120 is mounted on the first shell 110 and encloses a chamber 130 together with the first shell 110; in this way, the shell 100 is a double-layer structure, and the chamber 130 can not only provide an installation area for some components of the detection equipment, but also play an isolation function. For example, the cavity can have a good heat insulation effect. When the test equipment is working in a high or low temperature environment, the chamber 130 can reduce heat transfer and maintain the internal temperature stable. This is particularly important for detection equipment that requires precise temperature control, and can ensure the accuracy and stability of the test results.
[0081] Among them, the sample stage 200 and the detection system 300 are installed in the shell 100. For example, the sample stage 200 and the detection system 300 can be installed in the first shell 110. In this embodiment, the shell 100 also includes a top opening and a sealing end cover 140 that covers the top opening. In this way, the sample to be tested can be easily installed in the shell 100 through the top opening. At this time, the sealing end cover 140 is used to seal the top opening to prevent the leakage of rays formed by the detection system during the test and maintain a constant temperature vacuum environment. It should be noted that when the shell 100 includes a first shell 110 and a second shell 120, the first shell 110 and the second shell 120 can both be cylindrical, and the first shell 110 and the second shell 120 both have a top opening.
[0082] The testing device further includes a sample stage 200 , wherein the sample stage 200 is disposed in the housing 100 . The sample stage 200 includes a bearing assembly 210 , which is movably connected in the housing 100 , that is, the bearing assembly 210 is movably connected in the first housing 110 .
[0083] The carrying assembly 210 includes a first carrying member 211 and a second carrying member 212 . The second carrying member 212 has a first mounting chamber 2121 . The first carrying member 211 includes a carrying chamber 2111 . The carrying chamber 2111 is used to accommodate a sample to be detected so as to fix the sample to be detected in the sample stage 200 .
[0084] It should be noted that there are multiple options for connecting the sample to be tested and the first carrier 211, which can be set according to the structure of the sample to be tested. Exemplarily, the sample to be tested includes a sample cup with an opening and a transparent film covering the opening; wherein the transparent film not only covers the opening, but also covers part of the outer circumference of the sample cup to reduce the risk of the transparent film falling off. The sample cup is cylindrical in shape, with an inner diameter of 3 cm to 5 cm and a height of 0.6 cm to 1.0 cm.
[0085] At this time, a telescopic fixing member 214 is provided in the carrying 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 toward or away from the center of the carrying chamber 2111 to clamp or release the sample to be tested. 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 preventing the sample to be tested from spilling, thereby improving the safety during the test.
[0086] In this example, there can be multiple options for the telescopic fixing member 214. For example, there can be multiple telescopic fixing members 214, and each telescopic fixing member 214 can also include a spring and a rubber fixing block, wherein 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] A plurality of telescopic fixing members 214 can enclose a space for accommodating the sample to be tested. When the sample to be tested is installed in the carrying chamber 2111, the sample to be tested 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 tested.
[0088] For another example, there are multiple telescopic fixing members 214, each of which may include a driving member and a rubber fixing block. The driving member is fixed to the inner wall of the carrying chamber 2111, and the output shaft of the driving member is connected to the rubber fixing block to drive the rubber fixing block to move toward or away from the center of the carrying chamber 2111 to clamp or release the sample to be tested.
[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 tested, thereby improving the design flexibility of the telescopic fixing member 214.
[0090] Please continue to refer to the attached Figure 1 The first bearing member 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 bearing member 211 to rotate around its first central axis. The first central axis extends in a direction perpendicular to the second bearing member 212. Figure 1 Middle dashed line S1.
[0091] As a possible implementation of the first driving member 215, the first driving member 215 includes a first motor, whose output end is directly connected to the first bearing member 211. Thus, when the first motor is started, it drives the first bearing member 211 to rotate around its first central axis S1. The first driving member 215 drives the first bearing member 211 to rotate at a rotation rate ranging from 1 rpm to 2.5 rpm.
[0092] The second driving member 220 is disposed on the second bearing member 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 bearing member 211 to perform eccentric movement within a preset range relative to the first central axis S1; wherein the preset range is 1° to 5°. The second driving member 220 can drive the first bearing member 211 to perform eccentric rotation at a rotation rate of 0.5 rpm to 1.5 rpm.
[0093] It should be understood that the second driving member 220 can be disposed on the bottom surface of the second supporting member 212 , or can be disposed in the first installation chamber 2121 .
[0094] As a possible implementation of the second drive member 220, the second drive 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 drive member through a connecting shaft. In this way, when the first drive member 215 is started alone, it will directly drive the first bearing member 211 to rotate. 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 a connecting shaft, this rotation will cause the first bearing member 211 to produce eccentric motion relative to its first central axis. It should be noted that the connecting shaft here may be a flexible (such as a universal joint) or rigid, depending on the required range of motion and accuracy. And the second drive 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 disposed in the housing 100 and is used to detect the light element content of the sample to be detected. The detection system 300 is a conventional X-ray spectrometer.
[0096] In this embodiment, the sample stage 200 is improved so that the sample stage 200 can both rotate on its own and rotate eccentrically. For example, the first driving member 215 can drive the first supporting member 211 to rotate around its first central axis. At the same time, the second driving member can drive the first supporting member 211 to rotate eccentrically. In this way, during the detection process, combined with the structure of the sample cup, the surface of the sample to be detected can be irradiated at multiple points under the premise that the parameters of the detection system 300 remain unchanged, so that the detection system 300 can obtain more test data, reduce the impact of the surface morphology of the sample to be detected and the uneven distribution of internal particles on the test accuracy, and thus improve the detection accuracy of the test equipment.
[0097] It should be noted that the unchanged parameters of the detection system 300 may include but are not limited to the unchanged incident angle and the unchanged incident point of the primary ray (X-ray).
[0098] In a possible implementation, 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 disposed 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 of the device and making the entire device more compact and lightweight. In addition, the third bearing member 213 can also be a connecting member to facilitate the installation of the sample stage 200 in the housing 100.
[0099] The second driving member 220 is at least partially contained in the second installation chamber 2131, which helps to reduce vibration and noise during the driving process and improve driving efficiency. At the same time, this layout also helps to protect the second driving member 220 from interference and damage from the external environment, thereby extending its service life.
[0100] Please continue to refer to the attached Figure 1 and attached Figure 2 The sample stage 200 further includes a rotating device 230, which is connected to the bearing assembly 210 and is used to drive the bearing assembly to rotate along a second central axis; the second central axis is perpendicular to the first central axis. Figure 2 The dotted line S2.
[0101] Attach Figure 1 and attached Figure 2 Taking the position shown in the figure as an example, in the initial state, the opening of the carrying chamber 2111 faces upward. When the sample to be tested is installed in the carrying chamber 2111, the rotating device 230 is started, and the rotating device 230 drives the carrying component 210 to rotate around the second central axis. In other words, the rotating device 230 drives the carrying component 210 to rotate along the second central axis. Figure 2 The sample is rotated 180 degrees in the direction of the middle arrow so that the opening of the carrying chamber 2111 faces downward, so that the detection system 300 can detect the sample to be detected.
[0102] The rotating device 230 only needs to be able to drive the supporting assembly 210 to rotate. The structure of the rotating device 230 is prior art and will not be further described in detail in this embodiment.
[0103] In this embodiment, the provision of the rotating device 230 can facilitate the installation and removal of the sample to be tested, thereby improving the detection efficiency.
[0104] In a possible implementation, the sample stage 200 further includes a lifting device 240, which 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 bearing assembly 210) to reciprocate along the extension direction of the first central axis, thereby adjusting the relative position of the bearing assembly 210.
[0105] In this way, the introduction of the lifting device 240 enables the supporting assembly 210 to not only be rotated and adjusted on the horizontal plane through the rotating device 230, but also be positioned in the vertical direction. This position adjustment capability in three-dimensional space greatly enhances the flexibility of the sample stage, allowing the detection system 300 to more accurately locate the sample to be detected, thereby optimizing the detection effect.
[0106] Among them, the structure of the lifting device 240 can have multiple options. 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, and the end of the connecting member 242 away from the transmission member 241 is connected to the rotating device 230. In this way, the rotating device 230 and the supporting assembly 210 can be driven to reciprocate synchronously along the extension direction of the first center axis.
[0107] The type of the transmission member 241 is selected according to the driving mechanism. For example, the driving mechanism is a motor. Accordingly, the transmission member 241 may include a lead screw and a nut threadedly connected to the lead screw; and the connecting member 242 may be a connecting rod.
[0108] Please refer to the attached Figure 1 and attached Figure 3 In a possible implementation, the detection system 300 includes an optical path component 310 , and the optical path component 310 is disposed in the housing 100 .
[0109] The optical path assembly 310 includes a first optical element 311 and a second optical element 312 arranged at intervals; on a cross section parallel to the shell, the orthographic projection of the sample stage 200 is located on one side of the line connecting the orthographic projection of the first optical element 311 and the orthographic projection of 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 between 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, so that the light can be more efficiently guided and focused on the sample 400 to be detected.
[0110] It should be noted that the transmission path formed by the rays between the first optical element 311 , the second optical element 312 and the sample to be detected 400 can be V-shaped or in the form of multiple broken lines, as long as the rays formed by the detection system 300 can be received by the detector 330 .
[0111] In this embodiment, the first optical element 311 and the second optical element 312 both include a bent crystal support 3113 and a first bent crystal 3111 and a second bent crystal 3112 rotatably connected to the bent crystal support 3113. The orientation of the first bent crystal 3111 and the orientation of the second bent crystal 3112 are opposite and made of different materials.
[0112] For example, the first curved crystal 3111 is used to detect the fluorine (F) element in the sludge, and the material of the first curved crystal includes lithium fluoride (LiF), thallium phthalate (TAP) or pentaerythritol (PET). Wherein, lithium fluoride and / or pentaerythritol also use specific crystal planes, for example, the material of the first curved crystal 3111 is lithium fluoride (200); or, the material of the first curved crystal 3111 is pentaerythritol (PET) (002). Wherein, 200 in lithium fluoride (200) represents a specific direction or crystal plane of the crystal. The second curved crystal 3112 is used to detect calcium (Ca) elements or other elements in the sludge, and its material includes lithium fluoride (LiF) or germanium (Ge). Wherein, the material of the second curved crystal 3112 is lithium fluoride (200) or lithium fluoride ((220); or, the material of the second curved crystal 3112 is germanium (111).
[0113] When it is necessary to detect the content of fluorine in the sample 400 to be detected, the first curved crystal 3111 can be rotated so that the curved surface of the first curved 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 in the sample 400 to be detected, the second curved crystal 3112 can be rotated so that the curved surface of the second curved crystal 3112 faces the light source of the detection system 300. In this way, the same detection device can detect different elements, which improves the flexibility of the detection device, reduces the detection cost, improves the detection efficiency, enhances the detection accuracy and simplifies the operation process.
[0114] It should be understood that the rotation of the first curved crystal 3111 and the second curved crystal 3112 may be achieved by a conventional rotating device.
[0115] The first curved crystal 3111 and the second curved crystal 3112 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 first radius of curvature is R, and the second radius of curvature is r. The first curved crystal 3111 and the second curved crystal 3112 have an area of 30-45 mm×15-30 mm and a thickness of 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 curved crystal can monochromatize the X-rays irradiated on the first curved crystal 3111 and fully focus them to a focal position with the curvature radius R as the center, focusing on the detection surface of the sample to be detected 400, so as to better excite the fluorine element. By utilizing the spatial layout of multiple hyperbolic curved crystals, a fixed channel energy spectrum for monochromatic single-channel excitation and reception of the element to be detected is formed, the particle size effect and mineral effect of photovoltaic sludge are eliminated, the detection limit of the X-ray fluorescence spectrum for the F element is improved, and the resolution of the test equipment is improved.
[0117] Particle size effect: The intensity of X-rays may vary with the sample size and sample heterogeneity. Mineral effect: The intensity of X-rays varies with the chemical structure of the analyzed component and the mineral crystal morphology.
[0118] In order to better describe the first curvature radius R and the second curvature radius 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 to the sample 400 by the first optical element 311 ; the X-rays excite the elements to be tested in the sample 400 to form X-ray fluorescence; the X-ray fluorescence is focused and reflected to the detector 330 by the second optical element 312 .
[0121] This embodiment ensures the precision and accuracy of the analysis of F and Ca elements in photovoltaic sludge by improving the sample stage 200, the first optical element 311 and the second optical element 312 that carry the sample 400 to be detected, and the detection limit reaches 0.001%, thereby promoting the development of photovoltaic sludge to replace natural fluorite ore.
[0122] The X-target material of the light source 320 is molybdenum (Mo), silver (Ag), rhodium (Rh) or chromium (Cr), the power is 15-80W, and the diffraction energy is 5.40-22.16 keV. The detector 330 uses a solid-state detector, including but not limited to a silicon drift detector (SSD), an SDD high-purity silicon detector, a high-purity germanium detector, and the like.
[0123] In the embodiment of the present application, the sample stage 200 is located on the center line of the line connecting the light source 320 and the detector 330, and is equidistant from the light source 320 and the detector 330. 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 generated by the light source 320 are refracted to the sample stage 200 through the first optical element 311 at an incident angle θ, and the excited X-ray fluorescence can be incident on the second optical element 312 at an angle θ and then refracted to the detector 330.
[0125] The first curvature radius is R, and the second curvature radius 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 and the sample stage 200 as the center; the curvature radius R and the rotation radius r satisfy r=RR*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, an aperture 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-ray 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 aperture 315 , the second collimator 316 and the detector 330 are arranged on the transmission path of the X-ray fluorescence, and the aperture 315 is located between the second collimator 316 and the second optical element 312 .
[0128] 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 disposed on a 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 aperture 315 is 1-5 mm. The first collimator 314 and the second collimator 316 are both made of copper as the main material and aluminum as the outer lining, with an aperture of 3-5 mm, which can reduce stray lines and reduce interference introduced by the collimator material.
[0131] In a possible embodiment, the detection device also includes a constant temperature system 500, which includes a heating element 510, at least one temperature sensor 520 and a constant temperature controller 530; the heating element 510 and the at least one temperature sensor 520 are respectively arranged on the shell 100; it should be understood that the position at which the heating element 510 and the temperature sensor 520 are arranged on the shell 100 is related to the structure of the shell 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, which is wound around the first housing 110 and accommodated in the chamber 130; in this case, 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, which can better detect the temperature of the inner cavity of the first housing 110.
[0133] The thermostatic controller 530 is connected to the heating element 510 and the temperature sensor 520 respectively; the thermostatic controller 530 is used to control the working state of the heating element 510 according to the temperature sensor 520.
[0134] Since the first optical element 311 and the second optical element 312 have certain thermal expansion coefficients, temperature changes in the first housing 110 may cause changes in the inter-surface distance between the first optical element 311 and the second optical element 312, thereby causing changes in the detection angle, which may cause errors in 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 shell 110 is lower than the appropriate temperature, the constant temperature controller 530 can control the heating element 510 to work, thereby heating the first shell 110. For another example, when the temperature in the first shell 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 is helpful 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 attached Figure 1 The constant temperature system 500 further includes at least one fan 540, which is disposed on the housing and 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 thermostat controller 530 can control the start and stop of the fan 540 and the speed of the fan 540, so that the housing 100 can be evenly heated by the fan 540, which helps to speed up heat transfer and improve the temperature equalization effect. This 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 temperature sensors 520 and fans 540 can be multiple or one. Exemplarily, the number of temperature sensors 520 and the number of fans 540 are both multiple; each temperature sensor 520 is arranged at intervals from each fan 540. In other words, multiple temperature sensors 520 and multiple fans 540 are arranged alternately. For example, one temperature sensor 520 is embedded in every 4-8 cm2, and one fan 540 is embedded in every 6-10 cm2.
[0139] In this way, multiple temperature sensors 520 can collect data at multiple points and frequencies. Adopting the adaptive neural fuzzy inference algorithm (ANFIS), the model inputs multi-point temperature information and temperature change rate, and outputs the power adjustment value of the heating element 510 and the speed adjustment value of the fan 540. At the same time, in order to efficiently train the algorithm, the particle swarm optimization algorithm is used to perform a global search on the parameter space of the ANFIS model. After obtaining the target control value, the specific parameter control is realized through the PID algorithm, thereby adjusting the heat generation of the heating element 510 and the start-up and ventilation rate of the fan 540, which can effectively control the temperature fluctuation, and the temperature control accuracy is ±0.1°C.
[0140] In a possible implementation, the detection device further includes a vacuum system 600, which 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 in the housing 100. The pressure relief valve 640 is installed on the housing 100 and 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] The vacuum pressure sensor 610 may be a resistive vacuum gauge, which uses the thermal conductivity of the space gas to affect the temperature of the component, and changes the resistivity of the sensitive component with the vacuum degree, thereby converting and measuring the vacuum degree. Combined with the precise cavity temperature, the detection performance of the detection equipment can be accurately controlled.
[0142] The vacuum generator 620 is in communication 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 adjust the vacuum degree in 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 to detect the vacuum degree in the first housing 110. The vacuum generator 620 is in communication with the inner cavity of the first housing 110 to adjust the vacuum degree in the first housing 110.
[0143] Among them, the vacuum generator 620 includes a vacuum pump 621, a solenoid valve 622, a vacuum valve 623, a frequency converter 624 and a connecting pipe 625; the vacuum pump 621, the solenoid valve 622 and the vacuum valve 623 are all arranged on the connecting pipe 625, and the frequency converter 624 is connected to the vacuum pump 621 for adjusting the rotation speed of the vacuum pump 621.
[0144] The vacuum controller 630 is respectively connected to the vacuum pressure sensor 610 and the solenoid valve 622 , the vacuum valve 623 , the frequency converter 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 a corresponding action instruction. For example, the vacuum controller 630 can control the solenoid valve 622 to adjust the start and stop of the vacuum pump 621; it can also adjust the speed of the vacuum pump 621 through the frequency converter 624, so as to meet the pressure value in the first shell 110 and apply different strategies in different stages. In the vacuum stage, the frequency converter adopts a fuzzy reasoning algorithm to quickly respond to the current pressure value to obtain the target speed; 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 be ensured that there is a suitable vacuum degree in the first shell 110. The suitable vacuum degree can reduce the absorption of X-rays by air, avoid the water vapor and carbon dioxide in the air to produce fluorescence under the action of X-rays, and thus 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 in the shell.
[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. The signal calculation processing and control system 700 of the constant temperature controller 530 and the vacuum controller 630 are located in the same host. In this way, the test device can be simplified.
[0148] The control system 700 uses a high-performance processing unit combined with a variety of optimization algorithms to achieve accurate analysis and processing of the signals collected by the detector 330. First, an adaptive filtering algorithm is used to remove signal noise, and a standard sample calibration curve is used for calibration to ensure the accurate correspondence between signal intensity and element content. Subsequently, the spectral characteristic peaks are extracted through principal component analysis to achieve quantitative analysis of F and Ca elements. In addition, in order 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 test results and analysis reports.
[0149] An embodiment of the present application also provides a method for rapid detection of fluorine-containing sludge in the pan-semiconductor industry. The detection method is applied to a rapid detection device for fluorine-containing sludge in the pan-semiconductor industry as described in any of the above embodiments.
[0150] Detection methods include:
[0151] Step S100: Install the sample to be tested on the sample stage of the testing equipment, and start the telescopic fixing member of the testing equipment so that the telescopic fixing member fixes the transparent film of the sample to be tested.
[0152] The sample to be tested also needs to be prepared in a certain way. For example, 3g-3.5g of sludge sample is weighed and placed in a sample cup. After that, it is compacted 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 test equipment to place the sample stage in the test position; wherein the lifting device drives the supporting assembly of the sample stage to move along the first central axis; and the rotating device is connected to the supporting assembly to drive the supporting assembly to rotate 180° along the second central axis; the second central axis is perpendicular to the first central axis.
[0154] In this embodiment, the lifting device is first started, and the lifting device is used to drive the carrying component of the sample stage to move along the first central axis to be in the testing position; in other words, the lifting device can adjust the height of the carrying component.
[0155] Afterwards, the rotating device of the test equipment is started, and the rotating device is connected to the supporting assembly to drive the supporting assembly to rotate 180° along the second central axis so that the opening of the sample to be tested faces downward; wherein the second central axis is perpendicular to the first central axis.
[0156] Step S300: start the first driving member and the second driving member, wherein the first driving member is used to drive the first central axis of the first supporting member to rotate, and the second driving member is used to drive the first supporting member to perform eccentric movement within a preset range relative to the first central axis.
[0157] Afterwards, the test parameters in the shell of the test equipment are adjusted so that the test parameters reach the test conditions; wherein the test parameters include the test temperature and the vacuum degree. Exemplarily, the test parameters are adjusted by the constant temperature system 500 and the vacuum system 600, for example, so that the test temperature in the shell 100 is 28.5°C to 30.5°C; the vacuum degree is 0.8Kpa to 1Kpa.
[0158] Step 400: Start the detection system, which 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, this embodiment also controls the environment inside the shell before starting the detection system.
[0160] In a possible implementation, the testing method further includes:
[0161] Acquire multiple first test temperatures at the current time node and multiple second test temperatures at the previous time node; wherein the test temperature is the temperature inside the shell.
[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 a collection of temperatures obtained at multiple different test points.
[0163] A temperature change rate is determined based on the plurality of first test temperatures and the plurality of second test temperatures.
[0164] A plurality of first test temperatures and temperature change speeds are input into an adaptive neural fuzzy inference algorithm model, and a power adjustment value of the heating element and a speed adjustment value of the fan are output through the adaptive neural fuzzy inference algorithm model.
[0165] Based on the power adjustment value of the heating element and the current power of the heating element, a target power value of the heating element is determined; and based on the speed adjustment value of the fan and the current value of the fan, a target speed of the fan is determined.
[0166] A first control instruction of the PID controller is generated based on a difference between a target power value of the heating element and a current power of the heating element; and a second control instruction of the PID controller is generated based on a difference between a target speed of the fan and a current speed of the fan.
[0167] 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 in the housing is 28.5°C to 30.5°C.
[0168] In this way, by optimizing the power of the heating element and the speed of the fan through various 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, the testing method further includes:
[0170] A first vacuum degree is obtained in the shell.
[0171] The first vacuum degree is input into a fuzzy inference algorithm model, and the target rotation speed of the frequency converter is output through the fuzzy inference algorithm model.
[0172] Adjust the speed of the vacuum pump according to the target speed.
[0173] A second vacuum degree in the shell is obtained, 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.
[0174] Based on the second vacuum degree and the target vacuum degree, an error value is obtained.
[0175] A third control instruction for PID control is generated 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 by the frequency converter so that the vacuum degree of the shell is 0.8Kpa to 1Kpa.
[0177] In this way, the advantages of fuzzy reasoning algorithm and PID algorithm are combined. The fuzzy reasoning algorithm can quickly calculate the target speed according to the current vacuum degree, so that the system can quickly approach the target vacuum degree range (0.8Kpa~1Kpa) and shorten the response time; while the PID algorithm eliminates steady-state errors through fine adjustment of the error value, suppresses oscillations through the differential link, ensures that the vacuum degree is stable within the target range, and improves control accuracy.
[0178] In this embodiment, particle swarm optimization can be used to optimize the adaptive neural fuzzy reasoning algorithm model and the fuzzy reasoning algorithm model respectively to improve the accuracy of the above models.
[0179] During the entire testing process, the test data is optimized, for example:
[0180] Acquire a detection signal; wherein the detection signal is acquired through a detector.
[0181] The detection signal is input into the adaptive filtering algorithm model, and the noise-removed detection signal is output.
[0182] The de-noised detection signal is calibrated using the calibration curve of the standard sample to form a calibrated detection signal, thereby ensuring an accurate correspondence between the signal intensity and the light element content.
[0183] The principal component analysis was performed on the calibrated detection signal to extract the spectral characteristic peaks.
[0184] Light elements are quantitatively analyzed based on spectral characteristic peaks.
[0185] In this embodiment, the adaptive filtering algorithm model may be optimized using particle swarm optimization to improve the accuracy of the adaptive filtering algorithm model.
[0186] This embodiment uses the above-mentioned detection equipment to detect sludge of different qualities.
[0187] Example 1
[0188] The sludge of higher quality and different batches was tested, and the CaF2 content in the sludge was more than 80%. The specific test data is shown in Table 1: Table 1 Test results of sludge of higher quality and different batches
[0189]
[0190] Example 2
[0191] The sludge of lower quality and different batches was tested, among which the CaF2 content in the sludge was less than 40%. The specific test data is shown in Table 2: Table 2 Test results of different batches of sludge with lower quality
[0192]
[0193] It can be clearly seen from Tables 1 and 2 that both high-quality and low-quality sludge can accurately detect light elements in the sludge, thereby providing a scientific basis and optimization plan for sludge treatment, utilization and disposal, which helps to improve resource utilization efficiency and promote environmental sustainable development.
[0194] The various embodiments or implementation methods in this specification are described in a progressive manner. Each embodiment focuses on the differences from other embodiments, and the same or similar parts between the various embodiments can be referenced to each other.
[0195] It should be noted that the phrases "one embodiment", "an embodiment", "an exemplary embodiment", "some embodiments", etc. mentioned in the specification indicate that the described embodiments may include certain features, structures or characteristics, but not every embodiment may include the certain features, structures or characteristics. In addition, such phrases do not necessarily refer to the same embodiment. In addition, when describing certain features, structures or characteristics in conjunction with an embodiment, it is within the knowledge of those skilled in the art to implement such features, structures or characteristics in conjunction with other embodiments, whether explicitly or not explicitly described.
[0196] 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 it. Although the present application has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to 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 movement within a preset range relative to the first central axis; wherein the preset range is 1° to 5°; A detection system, wherein 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, which 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 and the second bent crystal both include a first radius of curvature and a second radius of curvature, and the first radius of curvature is different from the second radius of curvature.
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 first curved crystal is used to detect the fluorine element in the fluorine-containing sludge, and the material of the first curved crystal includes lithium fluoride, thallium hydrogen phthalate, and pentaerythritol; The second bent crystal is used to detect calcium in the fluorine-containing sludge, and 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 includes a rotating device, which is connected to the bearing assembly and is used to drive the bearing assembly to rotate along a second central axis; the second central axis is perpendicular to the first central axis; 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 detection device is used to detect the fluorine element, the filter of the filter exchanger is a beryllium filter; when the 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 detection device further comprises a constant temperature system, wherein the constant temperature system 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 detection device further 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 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 testing device, and starting the telescopic fixing member of the testing device so that the telescopic fixing member fixes the transparent film of the sample to be tested; Start the lifting device and the rotating device of the test equipment 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 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 perform an eccentric movement 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 placing the sample stage in the testing position, the testing 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 speeds 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 test method also includes: 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.
Citation Information
Patent Citations
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