Plasma source pretreatment device

Abstract

The invention belongs to the technical field of plasma source equipment, and particularly relates to a plasma source pretreatment device. The plasma source is provided with a gas inlet and a gas outlet, and a precursor and reaction gas are introduced into the gas inlet; the particle collecting tank comprises a collecting tank gas inlet and a collecting tank gas outlet, and the collecting tank gas inlet is communicated with the gas outlet; the vacuum pump is communicated with the gas outlet of the collecting tank through an exhaust pipe; the heating system is arranged outside the exhaust pipe and the vacuum pump; the plasma source comprises an annular cavity and two groups of magnetic cores which are respectively arranged on the peripheral surface of the middle part of the annular cavity; the ignition head assembly is arranged on one side of the annular cavity, an ignition electrode is arranged in the ignition head assembly, and the ignition electrode is in a circular truncated cone shape. The invention aims to realize efficient and thorough decomposition of a TEMAZ precursor by using a high-density plasma technology, avoid formation of viscous byproducts so as to prevent TEMAZ gas phase condensation, improve MTBF of a pump, prevent blockage or burst of an exhaust pipeline, eliminate potential safety hazards, protect process equipment and improve environmental safety.

Description

Technical Field

[0001] This invention belongs to the field of plasma source equipment technology, and specifically relates to a plasma source pretreatment device. Background Technology

[0002] Plasma sources, as a highly efficient and controllable plasma generation technology, have wide applications in semiconductor manufacturing, material surface treatment, thin film deposition, and contaminant degradation. TEMAZ (tetra(ethylmethylamino)zirconium(IV)) is used as a precursor to deposit zirconium dioxide (ZrO2) thin films via chemical vapor deposition (CVD) or atomic layer deposition (ALD). ZrO2 thin films possess high dielectric constants, good thermal stability, and chemical stability, and are widely used in semiconductor devices (such as high-dielectric-constant gate dielectrics and capacitor dielectrics), optical coatings, and protective coatings.

[0003] TEMAZ condenses into a liquid state in the pumps and exhaust pipes connected to the plasma source structure, including incompletely broken-down viscous byproducts. This can easily reduce equipment lifespan and potentially cause pipe blockages or even ruptures, leading to safety accidents. Furthermore, TEMAZ reacts violently with air or moisture, potentially causing combustion and explosion; it is a hazardous gas requiring special management in the process. In practical industrial applications, existing plasma source structures are increasingly revealing design limitations in areas such as plasma excitation efficiency, airflow and thermal management, and long-term operational stability. Specifically, these include: First, existing plasma source structures are not efficient at activating and decomposing macromolecular metal-organic precursors such as TEMAZ, resulting in incomplete precursor decomposition. The configuration of the plasma reaction chamber and the design of the gas flow path lead to incomplete precursor decomposition, easily generating highly viscous byproducts. These incompletely decomposed neutral macromolecular fragments or polymers, due to their inherent adhesive properties, can easily reduce equipment lifespan and may cause pipeline blockage or even rupture, leading to safety accidents, frequent maintenance and cleaning requirements, and significantly reducing equipment uptime. Secondly, the heat dissipation efficiency of existing plasma and magnetic core component structures is poor. Under high-power, long-term continuous operation conditions, plasma excitation generates a large amount of heat energy, and the current thermal management design of the source has limitations, such as inadequate cooling paths or insufficient cooling area, leading to a cumulative increase in source temperature. This overheating state not only accelerates the deposition and solidification of the aforementioned viscous byproducts on the hot wall surface, but may also cause plasma discharge instability, affecting the uniformity and consistency of active group generation, and even causing damage to source components due to thermal stress, thus shortening the equipment lifespan. Finally, the existing structure has shortcomings in ignition performance. The existing cavity structure design is usually set to a fixed ignition voltage during the ignition process. When the gas type or gas pressure changes, the ignition breakdown voltage will also change. If the breakdown voltage needs to be increased, the originally set fixed ignition voltage is not sufficient, resulting in ignition failure and affecting the ignition success rate of the plasma source.

[0004] In summary, existing plasma source structures, while meeting the demands for efficient, clean, and stable plasma pretreatment, suffer from inherent deficiencies in decomposition efficiency, byproduct control, thermal management, and ignition reliability, making them insufficient to satisfy the increasingly sophisticated requirements of semiconductor manufacturing processes. These inherent deficiencies have become bottlenecks restricting further performance improvements in advanced semiconductor manufacturing processes.

[0005] Therefore, there is an urgent need in this field for an innovative plasma source structure design to overcome the many shortcomings of existing technologies and meet the needs of manufacturing next-generation high-performance, low-power semiconductor devices. Summary of the Invention

[0006] This invention provides a plasma source pretreatment device to solve the technical problems of existing plasma sources in practical industrial applications, such as limitations in plasma excitation efficiency, airflow and heat management, and long-term operational stability. The present invention includes: a plasma source having an inlet and an outlet, wherein the inlet is used to introduce a precursor and a reactant gas; A particle collection tank includes a collection tank inlet and a collection tank outlet, wherein the collection tank inlet and the collection tank outlet are connected. A vacuum pump, which is connected to the outlet of the collection tank via an exhaust pipe; A heating system is located outside the exhaust pipe and the vacuum pump; The plasma source includes: an annular cavity, the upper end of which is the air inlet, and the lower end of which is the air outlet; Two sets of magnetic cores are respectively disposed on the outer circumferential surface of the middle part of the annular cavity; An ignition head assembly is disposed on one side of the annular cavity, and an ignition electrode is disposed inside the ignition head assembly. The ignition electrode is frustoconical.

[0007] This invention modifies the structure of the ignition electrode, allowing it to provide different electrode spacings. Under constant voltage conditions, this broadens the range of pd values, thereby reducing the breakdown voltage V during plasma source ignition. bDuring ignition, discharge occurs along the electrode spacing d corresponding to the minimum breakdown voltage. In addition, the vacuum pump can maintain a low pressure state inside the plasma source. Under low pressure, collisions between gas molecules are reduced, which makes it more effective to excite gas molecules during plasma processing. It also promotes the stable generation and maintenance of plasma.

[0008] Furthermore, it also includes a gas scrubbing tank, which is connected to the outlet of the vacuum pump. The beneficial effect of this step is that the gas scrubbing tank, as an exhaust gas treatment device, can use the vacuum pump to pass the exhaust gas pollutants into it, so as to avoid the direct discharge of exhaust gas containing pollutants.

[0009] Furthermore, the outlet end of the vacuum pump is equipped with a gas composition detection device, which is connected in series or in parallel with the vacuum pump. The beneficial effect of this step is that the composition of the exhaust gas can be detected by the gas composition detection device, thereby determining whether the reaction in the plasma source is sufficient.

[0010] Furthermore, the plasma source also includes a cooling system located outside the annular cavity and the magnetic core. The beneficial effect of this step is that the cooling system is used to cool the annular cavity and the magnetic core, so as to ensure long-term controllable operation.

[0011] Furthermore: the plasma source is located inside a protective box, and the side wall of the protective box is provided with several sets of heat dissipation holes. Each set of heat dissipation holes is equipped with a fan on both sides. The beneficial effect of this step is that the protective box provides protection, and the fans provide auxiliary cooling.

[0012] Furthermore, this also includes a gas circuit control cabinet and a power supply control cabinet. The benefits of this step are: the gas circuit control cabinet controls the on / off and flow direction of gas through various pneumatic valves, achieving precise drive of pneumatic equipment; the output end of the gas circuit control cabinet is divided into two gas supply lines, namely the ignition head assembly gas supply line and the plasma source inlet gas supply line, providing sufficient gas to the ignition head assembly for ignition; the power supply control cabinet monitors electrical parameters (voltage, current, power) in real time through monitoring modules such as ammeters and voltmeters, and realizes power supply on / off control through circuit breakers and contactors, facilitating equipment start-up, shutdown, and maintenance.

[0013] Furthermore: the particle collection tank includes a cylindrical shell and a collection core; The cylindrical shell has an opening on one side, the collecting core is inserted through the opening and sealed to the opening, and the top surface of the cylindrical shell has an air inlet and an air outlet for the collecting tank. The collecting core includes a core shell, and the core shell is provided with a partition plate inside. The partition plate divides the core shell into a first chamber and a second chamber. The first chamber is also provided with a first partition plate, and the second chamber is also provided with a second partition plate. The collecting core is also equipped with an air duct, which passes through the first partition, the middle partition and the second partition; Both the first partition and the second partition have through holes at their bottom. The core shell corresponding to the first partition and the middle partition is in sealed communication with the air inlet of the collection tank, and the core shell corresponding to the second partition and the middle partition is in sealed communication with the air outlet of the collection tank. Several perforated plates are respectively disposed between the first partition and the middle partition, and between the second partition and the middle partition. The beneficial effect of this step is that the particle collection tank is mainly used to collect ZrO2 for recycling and reuse.

[0014] Furthermore, the perforated plate is set at an angle that mirrors the air duct, and the beneficial effect of this step is to improve the filtration and collection effect.

[0015] Furthermore: a frame is also provided, on which the plasma source and the control box are both mounted; The frame has an empty compartment underneath, which is adapted to the particle collection tank. The advantages of this step are that the device can be integrated and installed through the frame, making it more compact, saving space, and shortening the connecting pipes between the components, thereby reducing the amount of heating system used.

[0016] Furthermore, both the frame and the bottom of the particle collection tank are equipped with a moving platform. The advantage of this step is that it facilitates the overall movement of the device.

[0017] The beneficial effects of this invention are: 1. The ignition head assembly of this application can provide an ignition distance of a range to adapt to the minimum breakdown voltage required by the gas under different pressures, thereby ensuring the ignition success rate. In addition, the low-pressure environment created by the vacuum pump can promote the stable generation and maintenance of plasma. 2. The cooling system of this application can cool the annular cavity and the magnetic core simultaneously, instead of cooling them sequentially, so as to avoid the cooling water from affecting the cooling of the second heat source after it heats up through the first heat source. 3. Stable plasma allows the precursor to be fully pyrolyzed and heats the subsequent vacuum pump and exhaust pipe, which can prevent residual precursor from sticking together as decomposition products and improve service life. 4. Use gas composition detection equipment to detect and monitor the gas composition before and after the reaction to ensure that the reaction can proceed fully. Attached Figure Description

[0018] To more clearly illustrate the specific embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the specific embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0019] Figure 1 This is a schematic diagram of a plasma source pretreatment device provided by the present invention; Figure 2 A perspective view of a plasma source pretreatment device provided by the present invention; Figure 3 A perspective view of the plasma source in a plasma source pretreatment device provided by the present invention; Figure 4 for Figure 3 Cross-sectional view of AA in the middle; Figure 5 A cross-sectional view of an ignition head assembly in a plasma source pretreatment device provided by the present invention; Figure 6 A front perspective view of the cooling system in a plasma source pretreatment device provided by the present invention; Figure 7 A rear perspective view of the cooling system in a plasma source pretreatment device provided by the present invention; Figure 8 An exploded perspective view of the cooling system in a plasma source pretreatment device provided by the present invention; Figure 9 This is a schematic diagram of the structure of the annular cavity in a plasma source pretreatment device provided by the present invention; Figure 10 for Figure 9 Cross-sectional view of BB in the middle; Figure 11 for Figure 10 Cross-sectional view of CC in the middle; Figure 12 An exploded perspective view of the annular cavity in a plasma source pretreatment device provided by the present invention; Figure 13 An exploded perspective view of a magnetic core cooling water tray in a plasma source pretreatment device provided by the present invention; Figure 14 A perspective view of the magnetic core in a plasma source pretreatment device provided by the present invention; Figure 15 A cross-sectional view of the magnetic core cooling water tray in a plasma source pretreatment device provided by the present invention; Figure 16 A perspective view of a particle collection tank in a plasma source pretreatment device provided by the present invention; Figure 17 A cross-sectional perspective view of a particle collection tank in a plasma source pretreatment device provided by the present invention; Figure 18 This invention provides a schematic diagram of the process flow of a plasma source pretreatment device. Figure 19 The principle of a plasma source pretreatment device provided by the present invention Figure 1 ; Figure 20 The principle of a plasma source pretreatment device provided by the present invention Figure 2 ; Figure label: 1-Plasma source; 2-Particle collection tank; 3-Vacuum pump; 4-Exhaust pipe; 5-Gas scrubbing tank; 6-Gas composition detection equipment; 7-Gas circuit control cabinet; 8-Power control cabinet; 11-Annular cavity; 12-Magnetic core; 13-Heat sink; 14-Inlet pipe; 15-Outlet pipe; 16-Protective box; 17-Fan; 18-Ignition head assembly; 21-Cylindrical shell; 22-Collection core; 61-Dedicated pump; 111-Air inlet; 112-Air outlet; 113-Upper cavity; 114-Lower cavity; 115-Connecting cavity; 121-Magnetic core block; 122-Insulating partition; 123-Cooling water tray; 124-Connecting plate; 131-Cover plate; 132-Connecting block; 181-Ignition electrode; 211-Collection tank air inlet; 212-Collection tank air outlet; 221-Core outer shell; 222-Middle partition; 223-First partition; 224-Second partition; 225-Air duct; 226-Mesh plate; 1231 - Cooling water tray flow channel. Detailed Implementation

[0020] The embodiments of the technical solution of the present invention will now be described in detail with reference to the accompanying drawings. These embodiments are merely illustrative of the technical solution of the present invention and are therefore intended to limit the scope of protection of the present invention. It should be noted that, unless otherwise stated, the technical or scientific terms used in this application should have the ordinary meaning as understood by one of ordinary skill in the art to which this invention pertains.

[0021] In the description of this application, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential", etc., indicating the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings, are only for the convenience of describing the present invention and simplifying the description, and are not intended to indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of the present invention.

[0022] Furthermore, the terms "first," "second," etc., are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of technical features indicated. In the description of this invention, "a plurality of" means two or more, unless otherwise explicitly defined.

[0023] In this application, unless otherwise expressly 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.

[0024] In this application, unless otherwise expressly specified and limited, "above" or "below" the second feature can mean that the first feature is in direct contact with the second feature, or that the first feature is in indirect contact with the second feature through an intermediate medium. Furthermore, "above," "on top of," and "over" the second feature can mean that the first feature is directly above or diagonally above the second feature, or simply that the first feature is at a higher horizontal level than the second feature. "Below," "below," and "under" the second feature can mean that the first feature is directly below or diagonally below the second feature, or simply that the first feature is at a lower horizontal level than the second feature.

[0025] Example First, the basic principles related to this application will be explained, including the specific composition of the products at different degrees of pyrolysis during the thermal decomposition of TEMAZ, and the effect of gas pressure p and electrode spacing d on the breakdown voltage V. b Relationship diagram; like Figure 19 As shown, the specific chemical reaction of the precursor TEMAZ is as follows: Zr[N(CH3)(C2H5)]4→Zr+NCH3C2H5→Zr+N+C+2H2(1); The first and second stage decompositions produce residual TEMAZ and amine compounds. The intermediate state of the precursor during pyrolysis is also oxidized to generate byproducts (CH3(CH2)). 16 The carboxylic acid (-COOH) can condense into a liquid state in pumps and exhaust pipes, forming viscous byproducts that reduce equipment life (MTBF, mean time between failures) and may cause pipe blockage or even rupture. Oxidation reaction: Zr + O2 → ZrO2 (white powder) (2); C+O2→CO2(3; N+N→N2(4) 4H + O2 → 2H2O (5); Byproduct reactions: Zr + N → ZrN (brown powder) (6); Zr + C → ZrC (black powder) (7); Among them, ZrO2 is the final deposited zirconium oxide film, as shown in formulas (6) and (7). The process of preparing zirconium oxide (ZrO2) by decomposing Zr[N(CH3)(C2H5)]4 will produce byproducts ZrN or ZrC. These two byproducts are unstable and will undergo oxidation reaction with oxygen when heated. The Zr-N bond (564±25 kJ / mol) is rapidly broken under the action of high-density plasma. At the same time, carbon (C), hydrogen (H) and nitrogen (N) react with oxygen to form stable and non-toxic gaseous products such as CO2, H2O and N2. The solid by-product is pure ZrO2 micro powder, which is dry and non-sticky, making it easy to discharge and collect.

[0026] During plasma ignition, when the gas is not ionized, the system is approximately open-circuited and exhibits high impedance, requiring a sufficient breakdown voltage to trigger ionization. The breakdown voltage is described by Paschen's law: (8); p is the gas pressure; d is the electrode spacing; A and B are constants related to the type of gas (e.g., for argon: A≈13.6cm). −1 Torr −1 B≈176V·cm −1 Torr −1 ); γ is the secondary electron emission coefficient; The voltage needs to reach V b Only when the breakdown condition is met can discharge be triggered. Impedance and voltage are not directly proportional.

[0027] According to Pascal's law, the breakdown voltage does not change linearly with d, but rather has a minimum value. When d is very small, a very high voltage is required for breakdown because the electrons accelerate over a short distance and the number of collisions is insufficient. Conversely, if d is too large, although the energy of a single collision is high, the number of collisions decreases, and a higher voltage is still needed to maintain sufficient ionization. Therefore, a certain value of d corresponds to the lowest breakdown voltage. like Figure 20 As shown, under different gases, the gas pressure p and electrode spacing d affect the breakdown voltage V. b Impact diagram; For any given gas, there exists a specific pd value such that the breakdown voltage V b Reaching the minimum value V b The minimum breakdown voltage V corresponding to min, (pd)min b min depends on the type of gas.

[0028] Based on the above, this application provides a plasma source pretreatment device.

[0029] like Figures 1-18 As shown, this application includes: a plasma source 1, which is provided with an inlet 111 and an outlet 112. The inlet 111 is used to introduce a precursor and a reaction gas. The reaction gas includes an oxidizing gas O2 / O3 and a purge gas N2. The particle collection tank 2 includes a collection tank inlet 211 and a collection tank outlet 212, with the collection tank inlet 211 and outlet 212 connected. Vacuum pump 3 is connected to the gas outlet 212 of the collection tank through exhaust pipe 4. Vacuum pump 3 is used to extract gas from the particle collection tank 2. The heating system is located outside the exhaust pipe 4 and the vacuum pump 3. The heating system generally includes a heater and a thermocouple. The thermocouple is used to detect the temperature of the vacuum pump 3 and the exhaust pipe 4 so as to adjust the heating power of the heater and achieve the purpose of temperature control. The heater is preferably an electric heating tape. The electric heating tape is wound around the exhaust pipe 4 and the vacuum pump 3. The heating system can continuously maintain the temperature of the exhaust pipe 4 and the vacuum pump 3 above the TEMAZ gas temperature (≥348℃) to avoid condensation on the exhaust pipe 4 and the vacuum pump 3, which would cause adverse consequences. The plasma source 1 includes an annular cavity 11, which comprises an upper cavity 113, a lower cavity 114, and a connecting cavity 115. The connecting cavity 115 is used to seal and connect the upper cavity 113 and the lower cavity 114. The upper end of the upper cavity 113 is an inlet 111, and the side of the inlet 111 is also provided with at least two through holes, which are respectively connected to the pipeline of oxidizing gas and the pipeline of purging gas. The lower end of the lower cavity 114 is an outlet 112. The connection points of the connecting chamber 115 and the connection points of the lower chamber 114 and the connecting chamber 115 are equipped with matching ceramic rings and sealing rings for sealing connection to ensure no leakage. In addition, the interior of the annular chamber 11 forms an annular gas passage from the upper chamber 113, through the two connecting chambers 115, to the lower chamber 114 where the gas flows out. The ports of the upper chamber 113 and the lower chamber 114 are also equipped with ISO-K flanges for sealing connection of the gas pipelines connected to them. Two sets of magnetic cores 12 are respectively disposed on the outer peripheral surface of the middle part of the annular cavity 11, that is, on the outer peripheral surface of the connecting cavity 115; The ignition head assembly 18 is located on one side of the annular cavity 11. The ignition head assembly 18 contains an ignition electrode 181, which is frustoconical in shape. Specifically, the ignition head assembly 18 is located on the side of the upper cavity 113. The ignition head assembly 18 has a gas supply hole for supplying plasma gas, such as argon or nitrogen trifluoride.

[0030] This invention, by changing the structure of the ignition electrode 181, allows the ignition electrode 181 to provide different electrode spacings, such as... Figure 5 As shown, the electrode spacing d1 is 10mm, d3 is 5mm, D is 40mm, and l is 81.9mm. Under constant voltage conditions, it can be widened. pd The range of values ​​for this value is used to reduce the breakdown voltage during plasma source ignition. V b During ignition, the electrode spacing that satisfies the minimum breakdown voltage at this time is... d Discharge; in addition, the vacuum pump 3 can keep the plasma source 1 in a low-pressure state. Under low pressure, the collision between gas molecules is reduced, which makes it more effective to excite gas molecules during plasma processing; it also promotes the stable generation and maintenance of plasma.

[0031]

[0032] Table 1 shows the pd range corresponding to gas pressure and electrode spacing. As shown in Table 1, the structure of the ignition electrode 181 can satisfy the value range of d from 0.5 to 1 cm. According to Paschen's law, when the gas pressure p in this application is in the range of 0.15 to 3 Torr, the value range of pd is between 0.075 and 3, which can meet the minimum ignition voltage requirements of most gases and can also promote the stable generation of plasma.

[0033] Based on the above technical solution, it also includes a gas scrubbing tank 5, which is connected to the outlet of the vacuum pump 3. As an exhaust gas treatment device, the gas scrubbing tank 5 can use the vacuum pump 3 to pass the exhaust gas pollutants into it and remove the pollutants (parts and harmful gases) through technologies such as filtration, catalysis and adsorption, so as to avoid the direct discharge of exhaust gas containing pollutants.

[0034] Based on the above technical solution, a gas composition detection device 6 is provided at the outlet end of the vacuum pump 3. The gas composition detection device 6 is connected in series or in parallel with the vacuum pump 3. The composition of the exhaust gas can be detected by the gas composition detection device 6, thereby determining whether the reaction in the plasma source 1 is sufficient.

[0035] Specifically, the gas composition detection device 6 is a Fourier transform infrared spectrometer (FT-IR) that can detect the gas composition before and after the reaction online. It pays special attention to the removal effect of Zr precursor and amine gas. The test results showed that no unreacted TEMAZ and amine substances were detected, proving that the decomposition was complete.

[0036] The operating steps are as follows: Step S1: Turn on the special pump 61 of the Fourier transform infrared spectrometer to extract the residual reaction products and gas. Heat the connecting pipeline between the Fourier transform infrared spectrometer and the outlet of the vacuum pump 3 at 150°C to prevent TEMAZ from condensing. Step S2: First, infrared spectra of TEMAZ with different contents and CO, NO2, NO and O3 with different concentrations are collected by Fourier transform infrared spectrometer, and an infrared spectral database calibrated with characteristic spectral peaks and different concentrations of residual gas is established. Step S3: Data preprocessing: Data preprocessing can eliminate the influence of factors such as offset and baseline changes, reduce the influence of unimportant features on infrared spectral curves, retain and highlight effective information, and ensure a good correlation between spectral data and output dissociation rate; Step S4: After data preprocessing, a support vector machine regression algorithm is used to establish a plasma source ionization identification model using infrared spectral data of different contents of TEMAZ and different concentrations of gas. Step S5: Using the same infrared spectral acquisition conditions, sample the infrared spectrum (TEMAZ, CO, NO2, NO, O3) of the plasma source to be detected. Calculate the spectral characteristic peaks of the unknown sample based on the support vector machine model and compare them with the characteristic spectral peaks in the database. Compare the deviation value with 0.5. If the deviation value > 0.5, the sample is determined not to belong to this category; if the deviation value < 0.4, the sample is determined to belong to this category; if 0.4 <= deviation value <= 0.5, the determination is unstable or cannot be determined. Step S6: Obtain the compositional state of the current residual gas or precursor based on the calibration database.

[0037] Based on the above technical solution, the plasma source 1 also includes a cooling system located outside the annular cavity 11 and the magnetic core 12. The cooling system is used to cool the annular cavity 11 and the magnetic core 12 to ensure long-term controllable operation.

[0038] The specific implementation method of the cooling system is as follows: Figures 6-9 , Figure 13 and Figure 15 As shown, it specifically includes: an inlet pipe 14 and an outlet pipe 15, which are respectively located on both sides of the annular cavity 11, and the corresponding inlet end and outlet end are both below the annular cavity 11. The cooling system includes two sets of cooling channels: an annular cavity channel and a magnetic core channel. The annular cavity flow channel includes four heat sinks 13, located on both sides of the upper cavity 113 and both sides of the lower cavity 114. The heat sink 13 corresponding to the ignition head assembly 18 position on one side of the upper cavity 113 also has a clearance groove. Two independent flow channels are formed on the outer side of the heat sink 13, and two independent flow channels are also formed on both sides of the connecting cavity 115. The flow channels of the heat sink 13 and the connecting cavity 115 are M-shaped, S-shaped, or spiral-shaped, etc. The configuration of the flow channels can be set according to the actual heat generation to meet the heat dissipation area and achieve the best heat dissipation effect. The flow channel positions on the heat sink 13 and the connecting cavity 115 are provided with... The corresponding cover plate 131; taking one side of the annular cavity 11 as an example, the flow channel on the left side of the heat sink 13 at the position of the upper cavity 113 and the flow channel of the left connecting cavity 115 are connected by the connecting block 132, and the flow channel on the left side of the heat sink 13 at the position of the lower cavity 114 and the flow channel of the left connecting cavity 115 are also connected by the connecting block 132; the same applies to the right side. In this way, one side of the annular cavity 11 will form a double independent flow channel (the left flow channel and the right flow channel, which are not interconnected), which can be called the first flow channel; similarly, the other side of the annular cavity 11 is also a double independent flow channel, which can be called the second flow channel. The first flow channel and the second flow channel are also connected by the connecting block 132. The magnetic core flow channel is formed inside the heat dissipation plate 123. This flow channel includes several transverse through holes, with adjacent transverse through holes connected end to end, or a vertical blind hole is set at each end of several transverse through holes, and the blind hole is connected to the transverse through holes respectively. Regardless of the configuration, the flow channel has an inlet and an outlet, which are used to connect to the water inlet pipe 14 and the water outlet pipe 15 respectively. The two heat dissipation plates 123 are respectively set on both sides of the connecting cavity 115 of the annular cavity 11 and cover the magnetic core 12. The specific connection method of water inlet pipe 14 and water outlet pipe 15 is as follows: Figure 6 and Figure 7 As shown, the inlet pipe 14 is first split into two paths through a tee. One path is connected to the inlet of the cooling water tray 123, and the outlet of the cooling water tray 123 is connected to the inlet of the cooling water tray 123 on the other side through a pipe. The other path of the inlet pipe 14 is split into two paths again through a tee. The ends of both paths are connected to the connecting block 132 with the tee function. This is equivalent to having four inlets, which are respectively connected to the top of the first flow channel and the second flow channel on both sides of the annular cavity 11. Similarly, the outlet pipe 15 is set in a way that is a mirror image of the structure of the inlet pipe 14.

[0039] The cooling system can simultaneously supply water to cool the annular cavity 11 and the magnetic core 12. In particular, the flow channels of the annular cavity 11 and the magnetic core 12 are separated, unlike the traditional cooling system that cools the annular cavity 11 and the magnetic core 12 sequentially. This avoids the cooling water being heated by the annular cavity 11 before cooling the magnetic core 12, thus not affecting the cooling effect.

[0040] In addition, in the above content, except for the heat sink 13 and the flow channel of the connecting cavity 115 which are open structures, the flow channels of the other heat sink 123 and the connecting block 132 are all machined with holes, and the holes are sealed after the holes are machined.

[0041] Based on the above technical solution, the plasma source 1 is installed inside the protective box 16. The side wall of the protective box 16 is provided with several sets of heat dissipation holes. Each set of heat dissipation holes is provided with a fan 17 on both sides. The protective box plays a protective role, and the fan plays an auxiliary cooling role.

[0042] Based on the above technical solution, it also includes a gas circuit control cabinet 7 and a power control cabinet 8. The gas circuit control cabinet 7 controls the on / off and flow direction of gas through various valves (flow regulating valves, shut-off valves, and reversing valves, etc.) to achieve precise drive of pneumatic equipment. The output end of the gas circuit control cabinet is divided into two gas supply pipelines, namely the ignition head assembly gas supply pipeline and the plasma source inlet gas supply pipeline, to provide sufficient gas to the ignition head assembly 18 for ignition. The power control cabinet 8 monitors power parameters (voltage, current, power) in real time through monitoring modules such as ammeters and voltmeters, and realizes power supply on / off control through circuit breakers and contactors, which facilitates the start-up, shutdown and maintenance of equipment.

[0043] Based on the above technical solution, the particle collection tank 2 includes a cylindrical shell 21 and a collection core 22; The cylindrical shell 21 has an opening on one side, and the collecting core 22 is inserted into the opening and sealed to the opening. The top surface of the cylindrical shell 21 is provided with a collecting tank inlet 211 and a collecting tank outlet 212. The collecting core 22 includes a core shell 221. The core shell 221 is provided with a middle partition 222 inside. The middle partition 222 divides the core shell 221 into a first chamber and a second chamber. The first chamber is also provided with a first partition 223, and the second chamber is also provided with a second partition 224. The collecting core 22 is also equipped with an air duct 225, which passes through the first partition 223, the middle partition 222 and the second partition 224; Both the first partition 223 and the second partition 224 have through holes at their bottoms; The core shell 221 between the first partition 223 and the middle partition 222 is sealed and connected to the air inlet 211 of the collection tank, and the core shell 221 between the second partition 224 and the middle partition 222 is sealed and connected to the air outlet 212 of the collection tank. Several perforated plates 226 are respectively disposed between the first partition 223 and the middle partition 222, and between the second partition 224 and the middle partition 222. The particle collection tank 2 is mainly used to collect ZrO2 for recycling and reuse.

[0044] The specific gas flow path is as follows: the gas enters from the inlet 211 of the collection tank into the space between the middle partition 222 and the first partition 223 of the first chamber, then enters one end of the air duct 225 through the through hole of the first partition 223, and exits from the other end of the air duct 225 into the second chamber, and enters the space between the middle partition 222 and the second partition 224 through the through hole of the second partition 224, and finally exits from the outlet 212 of the collection tank. The gas will pass through the perforated plate 226 in the flow path. The perforated plate 226 can reduce the gas flow rate, allowing the ZrO2 particles carried in the gas flow to be deposited at the bottom of the first chamber and the second chamber under the action of gravity. In particular, after the gas flow reaches the second chamber, the flow rate will be further reduced, and more ZrO2 particles will be deposited at the bottom. The collected ZrO2 particles achieve the purpose of recycling and reuse.

[0045] Based on the above technical solutions, such as Figure 17 As shown, the perforated plate 226 is arranged at an angle mirroring the air duct 225. One end of the perforated plate 226 is sealed to the air duct 225, and the other end is sealed to the core housing 221 to ensure that airflow can only pass through the perforated plate 226, thereby improving the filtration and collection effect. Furthermore, the tilt angle and number of layers of the perforated plate 226 can be adjusted according to actual production conditions; the mesh diameter of the perforated plate 226 is generally within the range of 7.5±1mm.

[0046] Based on the above technical solution, a rack is also provided, on which plasma source 1 and control box are both located; The frame has an empty compartment at the bottom, which is compatible with the pellet collection tank 2. The frame allows for integrated installation of the device, making it more compact, saving space, and shortening the connecting pipes between components to reduce the amount of heating system required.

[0047] Based on the above technical solution, both the frame and the bottom of the particle collection tank 2 are equipped with a mobile platform, which can be a distributed caster to facilitate the overall movement of the device.

[0048] like Figure 13 and Figure 14 As shown, the magnetic core 12 is composed of several magnetic core blocks 121, and the magnetic core blocks 121 can be... Figure 14 The entire structure can also be a modular design (dividing the entire magnetic core 121 into multiple smaller pieces), which are then assembled into a unified magnetic circuit structure through an interlaced splicing method. Dividing the magnetic core 121 into smaller segments not only increases the surface area and volume ratio of the magnetic core 121, facilitating heat dissipation and improving heat dissipation efficiency, but also makes it easier to manufacture, process, and assemble. The magnetic core 121 has an insulating partition 122 in the middle, and a frame formed by a cooling water tray 123 and a connecting plate 124 on the outside, serving as a protective and cooling mechanism. Heat-conducting plates are also provided between the magnetic core 121 and the cooling water tray 123, and between the connecting plate 124 and the insulating partition 122.

[0049] Finally, as Figure 18 As shown, to achieve complete decomposition during the use of this device, the following process cycle (zirconia ZrO2 deposition process flow) is adopted: Step P1: TEMAZ gas flows into the annular cavity 11 and is ignited to generate plasma for thermal decomposition. Step P2: Purge the reaction using high-purity N2 to remove reaction products and residual gases; Step P3: Removal of precursor molecule residues: Introduce active gas O2 or O3 for further oxidation reaction via plasma excitation; the gas after plasma reaction enters the catalytic reaction zone, and the catalyst is a metal oxide (such as palladium or platinum) catalyst; these catalysts effectively promote the oxidation reaction of harmful components in the gas at lower temperatures (such as 150°C to 250°C); using the precursor TEMAZ (Zr[N(CH3)(C2H5)]4) with the reaction gas ozone (O3) to form an oxide film (such as ZrO2), the purified gas and the carrier gas N2 undergo atomic layer deposition (ALD).

[0050] Step 4: Purge the reaction chamber again with N2 to purify it. Repeat the above steps to ensure complete decomposition.

[0051] The process conditions are controlled as follows: Operating frequency: 400 kHz; Plasma density: ≥10 11 / cm 3 ; Reaction temperature: Ensure that the temperature control in the exhaust pipe 4 and vacuum pump 3 area is higher than the TEMAZ vapor condensation point (approximately 348°C).

[0052] Numerous specific details are set forth in this specification. However, it will be understood that embodiments of the invention may be practiced without these specific details. In some instances, well-known methods, structures, and techniques have not been shown in detail so as not to obscure the understanding of this specification. In the description of this specification, 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 invention. In this specification, illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples. Furthermore, those skilled in the art can combine and integrate the different embodiments or examples described in this specification and the features of the different embodiments or examples without contradiction.

[0053] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. Such modifications or substitutions 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 invention, and they should all be covered within the scope of the claims and specification of the present invention.

Claims

1. A plasma source pretreatment device, characterized in that, include: The plasma source is provided with an inlet and an outlet, wherein the inlet is used to introduce the precursor and the reactant gas; A particle collection tank includes a collection tank inlet and a collection tank outlet, wherein the collection tank inlet and the collection tank outlet are connected. A vacuum pump, which is connected to the outlet of the collection tank via an exhaust pipe; A heating system is located outside the exhaust pipe and the vacuum pump; The plasma source includes: an annular cavity, the upper end of which is the air inlet, and the lower end of which is the air outlet; Two sets of magnetic cores are respectively disposed on the outer circumferential surface of the middle part of the annular cavity; An ignition head assembly is disposed on one side of the annular cavity, and an ignition electrode is disposed inside the ignition head assembly. The ignition electrode is frustoconical.

2. The plasma source pretreatment apparatus according to claim 1, characterized in that, It also includes a gas scrubbing tank, which is connected to the outlet of the vacuum pump.

3. The plasma source pretreatment apparatus according to claim 1 or 2, characterized in that, The outlet end of the vacuum pump is equipped with a gas composition detection device, which is connected in series or in parallel with the vacuum pump.

4. The plasma source pretreatment apparatus according to claim 1, characterized in that, The plasma source also includes a cooling system located outside the annular cavity and the magnetic core.

5. The plasma source pretreatment apparatus according to claim 1 or 4, characterized in that, The plasma source is located inside a protective enclosure, and the side wall of the protective enclosure has several sets of heat dissipation holes, with a fan on both sides of each set of heat dissipation holes.

6. The plasma source pretreatment apparatus according to claim 3, characterized in that, It also includes the gas circuit control cabinet and the power supply control cabinet.

7. The plasma source pretreatment apparatus according to claim 1, characterized in that, The particle collection tank includes a cylindrical shell and a collection core; The cylindrical shell has an opening on one side, the collecting core is inserted through the opening and sealed to the opening, and the top surface of the cylindrical shell has an air inlet and an air outlet for the collecting tank. The collecting core includes a core shell, and the core shell is provided with a partition plate inside. The partition plate divides the core shell into a first chamber and a second chamber. The first chamber is also provided with a first partition plate, and the second chamber is also provided with a second partition plate. The collecting core is also equipped with an air duct, which passes through the first partition, the middle partition and the second partition; Both the first partition and the second partition have through holes at their bottom. The core shell corresponding to the first partition and the middle partition is in sealed communication with the air inlet of the collection tank, and the core shell corresponding to the second partition and the middle partition is in sealed communication with the air outlet of the collection tank. Several perforated plates are respectively disposed between the first partition and the middle partition, and between the second partition and the middle partition.

8. The plasma source pretreatment apparatus according to claim 7, characterized in that, The perforated plate is tilted in a mirror image with respect to the air duct as the center.

9. The plasma source pretreatment apparatus according to claim 6, characterized in that, A frame is also provided, on which the plasma source and the control box are both mounted; The frame has an empty compartment underneath, which is adapted to the particle collection tank.

10. The plasma source pretreatment apparatus according to claim 9, characterized in that, Both the frame and the bottom of the particle collection tank are equipped with a moving platform.

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