Electronics grade polysilicon reduction furnace growth apparatus and deposition particle detection method
A particle size detection device combining dynamic light scattering and imaging methods has solved the problem of monitoring abnormally deposited particles in polycrystalline silicon reduction furnaces, enabling the detection of nano- and micron-sized particles, avoiding product degradation and production losses, and improving production quality.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-04-01
- Publication Date
- 2026-04-14
AI Technical Summary
Existing technologies cannot effectively monitor abnormal deposited particles in polysilicon reduction furnaces, leading to impaired product purity and production losses, and process parameters cannot be adjusted in a timely manner to avoid these losses.
A particle size detection device combining dynamic light scattering and imaging methods uses a first light source to emit laser light and acquire dynamic light scattering signals, a second light source to illuminate particles and acquire images, and an image processing unit to analyze particle size, covering particle detection at the nanometer and micrometer levels.
It enables timely detection and characterization of abnormal deposited particles in polysilicon reduction furnaces, and can improve production quality by adjusting process parameters to avoid product degradation and production losses.
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Figure CN118289766B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of polycrystalline silicon production technology, and in particular to an electronic-grade polycrystalline silicon reduction furnace growth equipment and a method for detecting deposited particles. Background Technology
[0002] In Siemens polysilicon production, abnormal deposition can occur due to factors such as high trichlorosilane ratios in the reaction gas, low trichlorosilane purity (high dichlorosilane content), and localized temperature differences in the reaction space or support caused by variations in gas flow rate. This abnormal deposition can result in the reduction furnace containing complex compounds ranging from silicon (amorphous to crystalline) to those with the general formula SixClyHz. Particles formed by abnormal deposition settle onto the silicon rod in a normal distribution throughout the reaction space, particularly on the reactor inner wall. During further deposition, these particles may be covered by newly formed layers, leading to product degradation and production losses. Therefore, it is crucial to employ advanced methods to detect the qualitative state of particles within the reduction furnace at points where polysilicon product purity is compromised, allowing for real-time monitoring of the furnace reaction and timely adjustments to process parameters to effectively prevent losses. Although process optimization can theoretically minimize the risk of abnormal deposition, it still occurs repeatedly. While related technologies monitor abnormal deposition within the furnace, they only monitor turbidity within the furnace chamber and cannot qualitatively detect the state of abnormal deposition. This makes it impossible to optimize process parameters in a timely and accurate manner based on the abnormal deposition status. Therefore, improvements are needed. Summary of the Invention
[0003] This invention proposes an electronic-grade polycrystalline silicon reduction furnace growth equipment, which can avoid product degradation and production losses caused by abnormally deposited particles.
[0004] The present invention also proposes a method for detecting deposited particles in the above-mentioned electronic-grade polycrystalline silicon reduction furnace growth equipment.
[0005] According to a first aspect of the present invention, an electronic-grade polycrystalline silicon reduction furnace growth apparatus includes: a furnace body having a furnace chamber, and an observation window provided on the outer peripheral wall of the furnace body; and a particle size detection device for detecting the particle size of a test particle in the furnace chamber, wherein the particle size detection device includes a first light source, a first image acquisition unit, a second light source, a second image acquisition unit, and an image processing unit. The first light source emits laser light towards the test particle in the furnace chamber through the observation window. The first image acquisition unit is used to acquire the dynamic light scattering signal of the test particle. The second light source illuminates the test particle in the furnace chamber through the observation window. The second image acquisition unit is used to acquire an image of the test particle. The image processing unit is used to receive the image information acquired by the first image acquisition unit and the second image acquisition unit and acquire the particle size of the test particle.
[0006] According to the first aspect of the present invention, the electronic-grade polysilicon reduction furnace growth equipment detects the particle size of the test particles by combining dynamic light scattering and imaging methods. This can effectively cover the particle size detection of nano- and micro-level test particles. As a result, abnormal deposited particles generated in the furnace chamber can be detected in a timely manner by measuring the particle size of the test particles and the type of abnormal deposited particles can be characterized. This allows for timely adjustment of process parameters and other methods to reduce the risk of abnormal deposition based on the type of abnormal deposited particles. Consequently, it can avoid product downgrading and production losses caused by abnormal deposited particles, thereby improving the production quality of the electronic-grade polysilicon reduction furnace growth equipment.
[0007] According to some embodiments of the present invention, the field of view of the first image acquisition unit in the furnace chamber at least partially overlaps with the field of view of the second image acquisition unit in the furnace chamber.
[0008] According to some embodiments of the present invention, the observation window is at least two, each corresponding to the first image acquisition unit and the second image acquisition unit respectively.
[0009] According to some embodiments of the present invention, the two observation windows, which correspond one-to-one with the first image acquisition unit and the second image acquisition unit, are arranged at intervals along the circumference of the furnace body and have the same height.
[0010] According to some embodiments of the present invention, the first light source and the first image acquisition unit share the same observation window; and / or, the second light source and the second image acquisition unit share the same observation window.
[0011] According to some embodiments of the present invention, the observation window is four, each corresponding to the first light source, the first image acquisition unit, the second light source, and the second image acquisition unit.
[0012] According to some embodiments of the present invention, the first light source and the first image acquisition unit are respectively located on opposite sides of the furnace body; and / or, the second light source and the second image acquisition unit are respectively located on opposite sides of the furnace body.
[0013] According to some embodiments of the present invention, the centerline of the first image acquisition unit is perpendicular to the centerline of the furnace body and intersects with the centerline of the furnace body; and / or, the centerline of the second image acquisition unit is perpendicular to the centerline of the furnace body and intersects with the centerline of the furnace body.
[0014] According to some embodiments of the present invention, the particle size detection device further includes a converging lens disposed in front of the second light source to converge the light rays incident from the second light source into the furnace chamber.
[0015] According to a second aspect of the present invention, a method for detecting deposited particles in an electronic-grade polysilicon reduction furnace growth apparatus, wherein the electronic-grade polysilicon reduction furnace growth apparatus is as described above, the detection method includes: Step 1: A first light source emits a laser into a detection area within the furnace chamber, while a second light source illuminates the detection area within the furnace chamber; Step 2: A first image acquisition unit acquires the dynamic light scattering signal of the particles to be tested within the detection area, while a second image acquisition unit acquires an image of the particles to be tested within the detection area; Step 3: Based on the dynamic light scattering signal of the particles to be tested, it is determined whether there are particles to be tested within a first particle size range within the detection area, and based on the image of the particles to be tested, it is determined whether there are particles to be tested within a second particle size range within the detection area; Step 4: When particles to be tested within the first particle size range and / or the second particle size range are present within the detection area, abnormal deposited particles are present, and the process parameters are adjusted through an advanced control system, and steps 1 to 4 are repeated; when no particles to be tested within the first or second particle size range are present within the detection area, steps 1 to 4 are repeated.
[0016] According to the second aspect of the present invention, the method for detecting deposited particles in an electronic-grade polysilicon reduction furnace growth equipment combines dynamic light scattering and imaging methods to detect the particle size of the particles to be tested. This method can effectively cover the detection of particle sizes at both the nanometer and micrometer levels. By detecting the particle size of the particles to be tested, abnormal deposited particles generated in the furnace chamber can be identified in a timely manner, and the type of abnormal deposited particles can be characterized. Based on the type of abnormal deposited particles, the risk of abnormal deposition can be reduced in a timely manner by adjusting process parameters, thereby avoiding product degradation and production losses caused by abnormal deposited particles and improving the production quality of the electronic-grade polysilicon reduction furnace growth equipment.
[0017] According to some embodiments of the present invention, the first particle size range is 100 nm to 1 µm, and the second particle size range is 1 to 10 µm.
[0018] Additional aspects and advantages of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. Attached Figure Description
[0019] Figure 1 This is a schematic diagram of an electronic-grade polycrystalline silicon reduction furnace growth apparatus according to an embodiment of the present invention;
[0020] Figure 2 This is a schematic diagram of an electronic-grade polycrystalline silicon reduction furnace growth apparatus according to a specific embodiment of the present invention;
[0021] Figure 3 This is a schematic diagram of an electronic-grade polycrystalline silicon reduction furnace growth apparatus according to a specific embodiment two of the present invention;
[0022] Figure 4 This is a schematic diagram of an electronic-grade polycrystalline silicon reduction furnace growth apparatus according to a specific embodiment three of the present invention;
[0023] Figure 5 This is a flowchart of a deposition particle detection method according to an embodiment of the present invention.
[0024] Figure label:
[0025] 100 electronic-grade polycrystalline silicon reduction furnace growth equipment; 10 particles to be tested;
[0026] Furnace body 1; Furnace chamber 11; Observation window 12; Furnace cylinder 13; Cooling channel 131; Guide plate 132; Water inlet 133; Drain outlet 134; Chassis 14; Air inlet 141; Exhaust outlet 142;
[0027] Particle size detection device 2; first light source 21; first image acquisition unit 22; first microscope objective 221; first camera 222; second light source 23; second image acquisition unit 24; second microscope objective 241; second camera 242;
[0028] Electrode 3; Graphite base 4; Heating element 5. Detailed Implementation
[0029] Embodiments of the present invention are described in detail below, examples of which are illustrated in the accompanying drawings, wherein the same or similar reference numerals denote the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the accompanying drawings are exemplary and intended to explain the present invention, and should not be construed as limiting the present invention.
[0030] The following disclosure provides numerous different embodiments or examples for implementing various structures of the invention. To simplify the disclosure, specific examples of components and arrangements are described below. These are merely examples and are not intended to limit the invention. Furthermore, reference numerals and / or letters may be repeated in different examples. Such repetition is for simplification and clarity and does not in itself indicate a relationship between the various embodiments and / or arrangements discussed. Additionally, examples of various specific processes and materials are provided in this invention; however, those skilled in the art will recognize the applicability of other processes and / or the use of other materials.
[0031] The following description, with reference to the accompanying drawings, describes an electronic-grade polysilicon reduction furnace growth apparatus 100 according to a first aspect of the present invention.
[0032] like Figures 1 to 4 As shown, the electronic-grade polysilicon reduction furnace growth apparatus 100 according to a first aspect embodiment of the present invention includes: a furnace body 1 and a particle size detection device 2. The furnace body 1 has a furnace chamber 11, and an observation window 12 is provided on the outer peripheral wall of the furnace body 1. The observation window 12 is light-transmitting, so that the polysilicon growth in the furnace chamber 11 can be observed from outside the furnace body 1 through the observation window 12, so as to promptly identify problems and adjust technical parameters, which is beneficial to ensuring the growth quality of polysilicon. In a specific example, the electronic-grade polysilicon reduction furnace growth apparatus 100 is a chemical vapor deposition reactor.
[0033] The particle size detection device 2 is used to detect the particle size of the test particle 10 in the furnace chamber 11. In the description of this application, the test particle 10 may be amorphous silicon or SixClyHz complex compounds caused by abnormal deposition due to factors such as high trichlorosilane ratio in the reaction gas, low trichlorosilane purity, local gas temperature differences in the reaction space caused by changes in gas flow rate, or local temperature differences in the support. The test particle 10 may also be carbon-containing methyl groups formed during the vapor deposition process from carbonaceous impurities in trichlorosilane. The test particle 10 may also be other impurities generated by side reactions during the vapor deposition process. It should be noted that the types of test particles 10 include, but are not limited to, the types mentioned above. The above are only examples of some of the types of test particles 10 and are not a limitation on the types of test particles 10 that the particle size detection device 2 can detect.
[0034] Therefore, the particle size of the particles to be tested 10 in the furnace chamber 11 can be obtained in a timely manner through the particle size detection device 2. Thus, it can be determined whether there are abnormal deposited particles in the furnace chamber 11 based on the particle size of the particles to be tested 10. It should be noted that abnormal deposited particles refer to deposited particles larger than a certain particle size that affect the quality of polycrystalline silicon growth. When there are abnormal deposited particles in the furnace chamber 11, the abnormal deposited particles generated later can be eliminated by adjusting process parameters, which is beneficial to improving the quality of polycrystalline silicon growth.
[0035] The particle size detection device 2 includes a first light source 21, a first image acquisition unit 22, a second light source 23, a second image acquisition unit 24, and an image processing unit. The first light source 21 emits laser light towards the particle to be tested 10 in the furnace chamber 11 through the observation window 12. The first image acquisition unit 22 is used to acquire the dynamic light scattering signal of the particle to be tested 10. The second light source 23 illuminates the particle to be tested 10 in the furnace chamber 11 through the observation window 12. The second image acquisition unit 24 is used to acquire the image of the particle to be tested 10. The image processing unit is used to receive the image information acquired by the first image acquisition unit 22 and the second image acquisition unit 24 and acquire the particle size of the particle to be tested 10.
[0036] It can be understood that when the laser emitted by the first light source 21 irradiates the particle 10 to be tested, if the particle 10 is a nanoparticle, the particle 10 suspended in a fluid such as the rising airflow in the furnace chamber 11 will be in constant Brownian motion due to the interaction between the particles and the molecules of the rising airflow. This will cause the laser light irradiated onto the nanoparticle to be tested to pulsate after scattering. The pulsation frequency of the particle 10 is related to the diffusion coefficient of the particle 10. The diffusion coefficient Dt is related to the particle size. The relationship between particle diffusion and particle size can be described by the Stocks-Einstein formula: In the formula, KB is the Boltzmann constant, T is the absolute temperature, η is the viscosity, and R is the radius of the particle 10 to be tested. That is, the Brownian motion speed of small particles 10 results in faster scattered light fluctuations, while the Brownian motion speed of large particles 10 results in slower scattered light fluctuations. Therefore, by analyzing the dynamic light scattering signal of the particle 10 to be tested acquired by the first image acquisition unit 22 through the image processing unit, the specific size of the nanoscale particle 10 to be tested can be accurately obtained based on the fluctuation speed of the scattered light of the particle 10 to be tested, that is, the particle size of the nanoscale particle 10 to be tested can be measured by the dynamic light scattering method.
[0037] When the particle size of the test particle 10 is large, such as at the micrometer level, Brownian motion no longer exists for particles larger than several micrometers, making it impossible to measure its size using dynamic light scattering. Therefore, the second image acquisition unit 24 can directly acquire an image of the illuminated test particle 10, and the image processing unit can obtain the particle size distribution and shape factor parameters of the test particle 10 based on the image information acquired by the second image acquisition unit 24. In other words, the particle size of the micrometer-level test particle 10 can be measured using an image method. It should be noted that the lower limit of the image method is approximately 1 micrometer, while the upper limit can reach several hundred micrometers.
[0038] Therefore, by combining dynamic light scattering and imaging methods to detect the particle size of the test particle 10, the detection of the particle size of the test particle 10 at both the nanometer and micrometer levels can be well covered. This allows for the timely detection of abnormal deposited particles generated in the furnace chamber 11 by measuring the particle size of the test particle 10 and identifying the type of abnormal deposited particles. Based on the type of abnormal deposited particles, the risk of abnormal deposition can be reduced in a timely manner by adjusting process parameters, thereby avoiding product downgrading and production losses caused by abnormal deposited particles and improving the production quality of the electronic-grade polysilicon reduction furnace growth equipment 100.
[0039] According to the first aspect of the present invention, the electronic-grade polysilicon reduction furnace growth equipment 100 detects the particle size of the test particles 10 by combining dynamic light scattering and imaging methods. This can effectively cover the particle size detection of the test particles 10 at both the nanometer and micrometer levels. As a result, abnormal deposited particles generated in the furnace chamber 11 can be detected in a timely manner by measuring the particle size of the test particles 10 and the type of abnormal deposited particles can be characterized. This allows for timely adjustment of process parameters and other methods to reduce the risk of abnormal deposition based on the type of abnormal deposited particles. Consequently, it can avoid product downgrading and production losses caused by abnormal deposited particles, thereby improving the production quality of the electronic-grade polysilicon reduction furnace growth equipment 100.
[0040] In a specific example, the first image acquisition unit 22 includes a first microscope objective 221 and a first camera 222. The first microscope objective 221 is located between the corresponding observation window 12 and the first camera 222, and the observation window 12 corresponding to the first microscope objective 221 is located at the focal point of the first microscope objective 221. Therefore, the dynamic light scattering signal of the particle 10 under test can be amplified by the first microscope objective 221 for reception by the first camera 222. The second image acquisition unit 24 includes a second microscope objective 241 and a second camera 242. The second microscope objective 241 is located between the corresponding observation window 12 and the second camera 242, and the observation window 12 corresponding to the second microscope objective 241 is located at the focal point of the second microscope objective 241. The image of the particle 10 under test can be amplified by the second microscope objective 241 for reception by the second camera 242. This improves the accuracy of particle size detection by the particle size detection device 2. Both the first camera 222 and the second camera 242 are area array image sensors, such as CCD or CMOS devices.
[0041] In some embodiments, the first light source 21 is a semiconductor laser or a fiber laser.
[0042] In some embodiments, the second light source 23 is a light-emitting diode, a light bulb, or a fiber optic light source.
[0043] According to some embodiments of the present invention, the field of view of the first image acquisition unit 22 in the furnace chamber 11 at least partially overlaps with the field of view of the second image acquisition unit 24 in the furnace chamber 11. Therefore, the first image acquisition unit 22 can acquire the dynamic light scattering signal of the particle 10 to be tested in the overlapping area of the fields of view of the first image acquisition unit 22 and the second image acquisition unit 24 in the furnace chamber 11, and the second image acquisition unit 24 can also acquire the image of the particle 10 to be tested in the overlapping area of the fields of view of the first image acquisition unit 22 and the second image acquisition unit 24 in the furnace chamber 11. This allows the first image acquisition unit 22 and the second image acquisition unit 24 to acquire the image of the particle 10 to be tested in the same area, that is, to realize the synchronous detection of the particle 10 to be tested in the same area by the first image acquisition unit 22 and the second image acquisition unit 24, which is beneficial to improving the accuracy of the particle size detection device 2 in detecting the particle size of the particle 10 to be tested.
[0044] It should be noted that the first light source 21 only needs to ensure that the laser can be emitted onto the particle 10 to be tested in the overlapping area of the field of view of the first image acquisition unit 22 and the second image acquisition unit 24 in the furnace chamber 11, and the second light source 23 only needs to ensure that it illuminates the overlapping area of the field of view of the first image acquisition unit 22 and the second image acquisition unit 24 in the furnace chamber 11. Here, there is no specific limitation on the effective range of the first light source 21 and the second light source 23.
[0045] According to some embodiments of the present invention, there are at least two observation windows 12, each corresponding to a first image acquisition unit 22 and a second image acquisition unit 24. That is, the first image acquisition unit 22 can acquire the dynamic light scattering signal of the particle 10 to be tested within the furnace chamber 11 through one of its corresponding observation windows 12, and the second image acquisition unit 24 can acquire an image of the particle 10 to be tested within the furnace chamber 11 through its corresponding other observation window 12. This effectively avoids mutual obstruction between the first image acquisition unit 22 and the second image acquisition unit 24, while ensuring that both units have a wider field of view within the furnace chamber 11. For example, the first image acquisition unit 22 and the second image acquisition unit 24 can be positioned close to their respective observation windows 12, thereby enabling the particle size detection device 2 to more comprehensively and accurately detect the particle 10 to be tested within the furnace chamber 11, which helps to further reduce the risk of abnormally deposited particles affecting polysilicon growth.
[0046] According to some embodiments of the present invention, two observation windows 12, which correspond one-to-one with the first image acquisition unit 22 and the second image acquisition unit 24, are arranged at intervals along the circumference of the furnace body 1 and have the same height. Therefore, it is convenient to arrange the first image acquisition unit 22 and the second image acquisition unit 24 along the outer periphery of the furnace body 1, so that the first image acquisition unit 22 and the second image acquisition unit 24 can make full use of the space on the outer periphery of the furnace body 1. At the same time, the two observation windows 12 of the first image acquisition unit 22 and the second image acquisition unit 24 are the same, so that the field of view of the first image acquisition unit 22 in the furnace chamber 11 through its corresponding observation window 12 is at the same height as the field of view of the second image acquisition unit 24 in the furnace chamber 11 through its corresponding observation window 12. That is, the field of view of the first image acquisition unit 22 and the second image acquisition unit 24 in the furnace chamber 11 is at the same height, which can better ensure the consistency of the field of view of the first image acquisition unit 22 and the second image acquisition unit 24 in the furnace chamber 11. This enables the first image acquisition unit 22 and the second image acquisition unit 24 to synchronously detect the particles 10 to be tested in the same area, which is beneficial to improving the accuracy of the particle size detection device 2 in detecting the particle size of the particles 10 to be tested.
[0047] According to some embodiments of the present invention, the first light source 21 and the first image acquisition unit 22 share the same observation window 12. That is, the first light source 21 emits laser light into the particle 10 to be tested in the furnace chamber 11 through an observation window 12 corresponding to the first image acquisition unit 22. Thus, while ensuring that the first light source 21 can emit laser light into the particle 10 to be tested in the furnace chamber 11, the number of observation windows 12 can be reduced, thereby reducing the production cost of the furnace body 1, and also reducing the difficulty and limitations of arranging the first light source 21 and the first image acquisition unit 22.
[0048] According to some embodiments of the present invention, the second light source 23 and the second image acquisition unit 24 share the same observation window 12. That is, the second light source 23 emits light into the furnace chamber 11 through another observation window 12 corresponding to the second image acquisition unit 24 to illuminate the particle 10 to be tested in the furnace chamber 11. Thus, while ensuring that the second light source 23 can illuminate the particle 10 to be tested in the furnace chamber 11, the number of observation windows 12 can be reduced, thereby reducing the production cost of the furnace body 1, and at the same time, it is beneficial to reduce the difficulty and limitations of arranging the second light source 23 and the second image acquisition unit 24.
[0049] In some embodiments, the first light source 21 and the first image acquisition unit 22 share the same observation window 12; and / or, the second light source 23 and the second image acquisition unit 24 share the same observation window 12. This reduces the number of observation windows 12 required, thereby lowering the production cost of the furnace body 1.
[0050] According to some embodiments of the present invention, there are four observation windows 12, each corresponding to a first light source 21, a first image acquisition unit 22, a second light source 23, and a second image acquisition unit 24. That is, the first light source 21 emits laser light into the particle 10 to be tested within the furnace chamber 11 through its corresponding and independent observation window 12; the first image acquisition unit 22 acquires the dynamic light scattering signal of the particle 10 to be tested within the furnace chamber 11 through its corresponding and independent observation window 12; the second light source 23 illuminates the particle 10 to be tested within the furnace chamber 11 through its corresponding and independent observation window 12; and the second image acquisition unit 24 acquires the particle 10 to be tested illuminated by the second light source 23 within the furnace chamber 11 through its corresponding and independent observation window 12. Therefore, the risk of mutual interference and occlusion between the first light source 21, the first image acquisition unit 22, the second light source 23, and the second image acquisition unit 24 can be better avoided. At the same time, it ensures that the first light source 21 and the second light source 23 have a larger illumination range in the furnace chamber 11, and the first image acquisition unit 22 and the second image acquisition unit 24 have a larger field of view in the furnace chamber 11. For example, the first light source 21, the second light source 23, the first image acquisition unit 22, and the second image acquisition unit 24 can be set close to the corresponding observation window 12, so that the particle size detection device 2 can detect the particles 10 to be tested in the furnace chamber 11 more comprehensively and accurately, which is conducive to further reducing the risk of abnormally deposited particles affecting the growth of polycrystalline silicon.
[0051] According to some embodiments of the present invention, the first light source 21 and the first image acquisition unit 22 are respectively located on opposite sides of the furnace body 1. That is, the first light source 21 is located on one side of the furnace body 1 and is adapted to emit laser light toward the other side of the furnace body 1, while the first image acquisition unit 22 is located on the other side of the furnace body 1 and its field of view extends toward the direction closer to the first light source 21. Therefore, the direction in which the first light source 21 emits laser light is opposite to the direction in which the first image acquisition unit 22 acquires signals, thereby reducing the difficulty for the first image acquisition unit 22 to acquire dynamic light scattering signals. In addition, the first light source 21 and the first image acquisition unit 22 can make full use of the installation space on the outer periphery of the furnace body 1 in the circumferential direction, which helps to reduce the difficulty of arranging the first light source 21 and the first image acquisition unit 22.
[0052] According to some embodiments of the present invention, the second light source 23 and the second image acquisition unit 24 are respectively located on opposite sides of the furnace body 1. That is, the second light source 23 is located on one side of the furnace body 1 and is adapted to emit illumination light toward the other side of the furnace body 1, while the second image acquisition unit 24 is located on the other side of the furnace body 1 and its field of view extends toward the direction close to the second light source 23. Therefore, the direction in which the second light source 23 emits illumination light is opposite to the direction in which the second image acquisition unit 24 acquires the image, thereby reducing the difficulty for the second image acquisition unit 24 to acquire the image of the particle 10 to be tested. In addition, the second light source 23 and the second image acquisition unit 24 can make full use of the installation space on the outer periphery of the furnace body 1 in the circumferential direction, which helps to reduce the difficulty of arranging the second light source 23 and the second image acquisition unit 24.
[0053] In some embodiments, the first light source 21 and the first image acquisition unit 22 are located on opposite sides of the furnace body 1, and the second light source 23 and the second image acquisition unit 24 are located on opposite sides of the furnace body 1. This reduces the difficulty for the first image acquisition unit 22 to acquire dynamic light scattering signals and for the second image acquisition unit 24 to acquire images of the particles 10 under test. Simultaneously, it reduces the difficulty of arranging the first light source 21 and the first image acquisition unit 22, the second light source 23, and the second image acquisition unit 24.
[0054] According to some embodiments of the present invention, the centerline of the first image acquisition unit 22 is perpendicular to and intersects the centerline of the furnace body 1. It should be noted that the centerline here refers to the centerline of the field of view of the first image acquisition unit 22. Therefore, the field of view of the first image acquisition unit 22 within the furnace chamber 11 can be better guaranteed, enabling the first image acquisition unit 22 to acquire the dynamic light scattering signal of the particles 10 to be tested within the furnace chamber 11 more comprehensively and accurately, thus avoiding the risk of missing detection areas and failing to detect abnormal deposited particles in a timely manner.
[0055] According to some embodiments of the present invention, the centerline of the second image acquisition unit 24 is perpendicular to and intersects the centerline of the furnace body 1. It should be noted that the centerline here refers to the centerline of the field of view of the second image acquisition unit 24. This ensures a better view of the second image acquisition unit 24 within the furnace chamber 11, allowing it to acquire images of the particles 10 to be tested within the furnace chamber 11 more comprehensively and accurately, thus avoiding the risk of missing detection areas and failing to detect abnormally deposited particles in a timely manner.
[0056] In some embodiments, the centerline of the first image acquisition unit 22 is perpendicular to and intersects the centerline of the furnace body 1, and the centerline of the second image acquisition unit 24 is perpendicular to and intersects the centerline of the furnace body 1. Therefore, the particle size detection device 2 can more comprehensively and accurately detect abnormal deposited particles within the furnace chamber 11, which helps to further reduce the risk of abnormal deposited particles affecting polysilicon growth.
[0057] According to some embodiments of the present invention, the particle size detection device 2 further includes a converging lens, which is disposed in front of the second light source 23 to converge the light emitted by the second light source 23 into the furnace chamber 11. Thus, the converging lens can effectively concentrate the light emitted by the second light source 23 before it enters the furnace chamber 11 to illuminate the particles 10 to be tested, thereby enabling the converging lens to focus and illuminate the area to be tested within the furnace chamber 11, which helps to improve the accuracy of the particle size detection device 2.
[0058] The following is for reference. Figures 1-4 This invention describes an electronic-grade polycrystalline silicon reduction furnace growth apparatus 100 according to a specific embodiment of the present invention. It is to be understood that the following description is merely exemplary and intended to explain the invention, and should not be construed as limiting the invention.
[0059] Example 1
[0060] like Figure 2 As shown, the electronic-grade polycrystalline silicon reduction furnace growth equipment 100 includes a furnace body 1 and a particle size detection device 2. The furnace body 1 includes a furnace cylinder 13 and a chassis 14 located at the bottom of the furnace cylinder 13. The chassis 14 is used to seal the bottom opening of the furnace cylinder 13. A cooling channel 131 is formed inside the side wall of the furnace cylinder 13. A guide plate 132 is provided inside the cooling channel 131. A water inlet 133 and a water outlet 134 communicating with the cooling channel 131 are formed on the outer side of the furnace cylinder 13. The water inlet 133 is located near the bottom of the furnace cylinder 13, and the water outlet 134 is formed at the top of the furnace cylinder 13. The furnace cylinder 13 and the chassis 14 together define the furnace chamber 11. The chassis 14 has an air inlet 141 and an exhaust outlet 142 that communicate with the furnace chamber 11. An electrode 3 is provided on the upper side of the chassis 14. A heating element 5 extending in the vertical direction is electrically connected to the electrode 3. The heating element 5 includes two silicon cores and a crossbeam connected by the silicon cores. The whole is in the shape of an inverted "U". The bottom end of the silicon core is connected to the electrode 3 of the chassis 14 through a graphite seat 4. The silicon rod is generated by chemical vapor deposition reaction in the reduction furnace. An observation window 12 is also formed on the furnace cylinder 13. The observation window 12 is located between the two ends of the heating element 5 in the vertical direction.
[0061] The particle size detection device 2 is located outside the furnace body 1 and includes a first light source 21, a first image acquisition unit 22, a second light source 23, a second image acquisition unit 24, and an image processing unit. There are four observation windows 12, which correspond one-to-one with the first light source 21, the first image acquisition unit 22, the second light source 23, and the second image acquisition unit 24. The four observation windows 12 are evenly spaced along the circumference of the furnace body 1 and are located at the same height. The first light source 21 and the first image acquisition unit 22 are located on opposite sides of the furnace body 1 and are arranged opposite to each other. The second light source 23 and the second image acquisition unit 24 are located on opposite sides of the furnace body 1 and are arranged opposite to each other.
[0062] Example 2
[0063] This embodiment has a largely the same structure as Embodiment 1, with identical components using the same reference numerals. Figure 3 The difference between Embodiment 2 and Embodiment 1 is that there are two observation windows 12. The two observation windows 12 are evenly spaced along the circumference of the furnace body 1 and are located at the same height. The first light source 21 and the first image acquisition unit 22 are located on the same side of the furnace body 1 and share the same observation window 12. The second light source 23 and the second image acquisition unit 24 are located on the other side of the furnace body 1 and share another observation window 12.
[0064] Example 3
[0065] This embodiment has a largely the same structure as Embodiment 1, with identical components using the same reference numerals. Figure 4 The difference between Embodiment 3 and Embodiment 1 is that there are three observation windows 12. The three observation windows 12 are arranged at intervals along the circumference of the furnace body 1 and are located at the same height. The first image acquisition unit 22 and the second image acquisition unit 24 correspond to independent observation windows 12 respectively. The first light source 21 and the second light source 23 share the same observation window 12.
[0066] The following describes a method for detecting deposited particles in an electronic-grade polysilicon reduction furnace growth apparatus 100 according to a second aspect of the present invention, with reference to the accompanying drawings, wherein the electronic-grade polysilicon reduction furnace growth apparatus 100 is the aforementioned electronic-grade polysilicon reduction furnace growth apparatus 100.
[0067] like Figure 5As shown, a method for detecting deposited particles in an electronic-grade polysilicon reduction furnace growth apparatus 100 according to a second aspect embodiment of the present invention includes: Step 1: A first light source 21 emits a laser into a detection area within the furnace chamber 11, while a second light source 23 illuminates the detection area within the furnace chamber 11. Thus, by emitting a laser into the detection area, the nanoscale test particles 10 within the detection area can generate dynamic light scattering, and the second light source 23 can effectively enhance the brightness of the detection area within the furnace chamber 11 to facilitate the acquisition of visible light images of the micron-scale test particles 10 within the detection area.
[0068] Step 2: The first image acquisition unit 22 acquires the dynamic light scattering signal of the test particle 10 within the detection area, and the second image acquisition unit 24 acquires an image of the test particle 10 within the detection area. Therefore, by acquiring the dynamic light scattering signal of the test particle 10, the specific particle size of the test particle 10 at the nanometer level within the detection area can be obtained through analysis. By acquiring the image of the test particle 10 within the detection area, the specific particle size of the test particle 10 at the micrometer level within the detection area can be obtained through analysis. In other words, the specific particle sizes of the test particle 10 at both the nanometer and micrometer levels within the detection area can be acquired simultaneously.
[0069] Step 3: Based on the dynamic light scattering signal of the test particle 10, determine whether there are test particles 10 within the first particle size range in the detection area. Simultaneously, based on the image of the test particle 10, determine whether there are test particles 10 within the second particle size range in the detection area. The first particle size range is the particle size range of abnormally deposited particles among the test particles 10 that can be detected by the first image acquisition unit 22. The second particle size range is the particle size range of abnormally deposited particles among the test particles 10 that can be detected by the second image acquisition unit 24. In other words, the particle size range of abnormally deposited particles is the union of the first and second particle size ranges. Therefore, it is possible to accurately determine whether the test particles 10 within the detection area are located within the first or second particle size range, thus determining whether abnormally deposited particles exist within the detection area.
[0070] Step 4: When test particles 10 within the first and / or second particle size range are present in the detection area, abnormal deposited particles are identified. The process parameters are adjusted using the advanced control system, and steps one through four are repeated. When no test particles 10 within the first or second particle size range are present in the detection area, steps one through four are repeated. Therefore, continuous monitoring of the detection area can be achieved, and when abnormal deposited particles are present in the detection area, adjusting the process parameters can prevent the continued generation of abnormal deposited particles.
[0071] Therefore, by combining dynamic light scattering and imaging methods to detect the particle size of the test particle 10, the detection of particle size at both the nanometer and micrometer levels can be effectively covered. This allows for the timely detection of abnormal deposited particles generated in the furnace chamber 11 and the qualitative identification of the type of abnormal deposited particles. Based on the type of abnormal deposited particles, the risk of abnormal deposition can be reduced in a timely manner by adjusting process parameters, thereby avoiding product downgrading and production losses caused by abnormal deposited particles and improving the production quality of the electronic-grade polysilicon reduction furnace growth equipment 100.
[0072] According to the second aspect of the present invention, the deposition particle detection method for an electronic-grade polysilicon reduction furnace growth equipment 100 detects the particle size of the test particle 10 by combining dynamic light scattering method and image method. It can better cover the particle size detection of the test particle 10 at the nanometer and micrometer levels. Thus, it can promptly detect abnormal deposition particles generated in the furnace chamber 11 by detecting the particle size of the test particle 10 and characterize the type of abnormal deposition particles. In order to reduce the risk of abnormal deposition in a timely manner by adjusting process parameters according to the type of abnormal deposition particles, it can avoid product downgrading and production loss caused by abnormal deposition particles, and improve the production quality of the electronic-grade polysilicon reduction furnace growth equipment 100.
[0073] According to some embodiments of the present invention, the first particle size range is 100 nm to 1 µm, and the second particle size range is 1 to 10 µm. Specifically, the particle size range of the abnormally deposited particles is 100 nm to 10 µm. When the dynamic light scattering signal acquired by the first image acquisition unit 22 contains test particles 10 with a particle size of 100 nm to 1 µm, abnormally deposited particles are present in the detection area. Similarly, when the image acquired by the second image acquisition unit 24 contains test particles 10 with a particle size of 1 to 10 µm, abnormally deposited particles are present in the detection area.
[0074] In this invention, unless otherwise explicitly specified and limited, the terms "installation," "connection," "linking," and "fixing," etc., should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral part; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal communication of two components or the interaction between two components. Those skilled in the art can understand the specific meaning of the above terms in this invention according to the specific circumstances.
[0075] In the description of this specification, the references to terms such as "one embodiment," "some embodiments," "example," "specific example," or "some examples," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the present invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples. Moreover, without contradiction, those skilled in the art can combine and integrate the different embodiments or examples described in this specification, as well as the features of different embodiments or examples.
[0076] Although embodiments of the invention have been shown and described, those skilled in the art will understand that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the claims and their equivalents.
Claims
1. An electronic-grade polycrystalline silicon reduction furnace growth apparatus, characterized in that, include: The furnace body has a furnace chamber inside, and an observation window is provided on the outer peripheral wall of the furnace body; A particle size detection device is provided for detecting the particle size of a test particle in a furnace chamber. The device includes a first light source, a first image acquisition unit, a second light source, a second image acquisition unit, and an image processing unit. The first light source emits laser light towards the test particle in the furnace chamber through an observation window. The first image acquisition unit acquires the dynamic light scattering signal of the test particle. The second light source illuminates the test particle in the furnace chamber through the observation window, and the second image acquisition unit acquires an image of the test particle. The image processing unit receives the image information acquired by the first and second image acquisition units and acquires the particle size of the test particle.
2. The electronic-grade polycrystalline silicon reduction furnace growth equipment according to claim 1, characterized in that, The field of view of the first image acquisition unit in the furnace chamber at least partially overlaps with the field of view of the second image acquisition unit in the furnace chamber.
3. The electronic-grade polycrystalline silicon reduction furnace growth equipment according to claim 1, characterized in that, The observation window is at least two, each corresponding to the first image acquisition unit and the second image acquisition unit respectively.
4. The electronic-grade polycrystalline silicon reduction furnace growth equipment according to claim 3, characterized in that, The two observation windows, which correspond one-to-one with the first image acquisition unit and the second image acquisition unit, are arranged at intervals along the circumference of the furnace body and have the same height.
5. The electronic-grade polycrystalline silicon reduction furnace growth equipment according to claim 3, characterized in that, The first light source and the first image acquisition unit share the same observation window; and / or, the second light source and the second image acquisition unit share the same observation window.
6. The electronic-grade polycrystalline silicon reduction furnace growth equipment according to claim 3, characterized in that, The observation windows are four in total, each corresponding to one of the first light source, the first image acquisition unit, the second light source, and the second image acquisition unit.
7. The electronic-grade polycrystalline silicon reduction furnace growth equipment according to claim 6, characterized in that, The first light source and the first image acquisition unit are located on opposite sides of the furnace body; and / or, the second light source and the second image acquisition unit are located on opposite sides of the furnace body.
8. The electronic-grade polycrystalline silicon reduction furnace growth equipment according to claim 1, characterized in that, The centerline of the first image acquisition unit is perpendicular to the centerline of the furnace body and intersects with the centerline of the furnace body; and / or, the centerline of the second image acquisition unit is perpendicular to the centerline of the furnace body and intersects with the centerline of the furnace body.
9. The electronic-grade polycrystalline silicon reduction furnace growth equipment according to claim 1, characterized in that, The particle size detection device also includes a converging lens, which is disposed in front of the second light source to converge the light emitted by the second light source into the furnace chamber.
10. A method for detecting deposited particles in an electronic-grade polycrystalline silicon reduction furnace growth equipment, characterized in that, The electronic-grade polysilicon reduction furnace growth equipment is the electronic-grade polysilicon reduction furnace growth equipment according to any one of claims 1-9, and the detection method includes: Step 1: The first light source emits a laser into the detection area inside the furnace, while the second light source illuminates the detection area inside the furnace. Step 2: The dynamic light scattering signal of the particles to be tested in the detection area is acquired by the first image acquisition unit, and the image of the particles to be tested in the detection area is acquired by the second image acquisition unit. Step 3: Determine whether there are particles within the first particle size range in the detection area based on the dynamic light scattering signal of the particles to be tested, and at the same time determine whether there are particles within the second particle size range in the detection area based on the image of the particles to be tested. Step 4: When there are test particles in the detection area that are within the first particle size range and / or the second particle size range, there are abnormal deposited particles. Adjust the process parameters through the advanced control system and repeat steps 1 to 4. When there are no test particles in the detection area that are within the first particle size range and the second particle size range, repeat steps 1 to 4.
11. The method for detecting sedimentary particles according to claim 10, characterized in that, The first particle size range is 100 nm to 1 µm, and the second particle size range is 1 to 10 µm.
Citation Information
Patent Citations
Particle-size measuring instrument
CN102207443A
Multi-parameter online monitoring and optimizing control device and method of polycrystalline silicon reduction furnace
CN102795627A