A combined atmosphere annealing apparatus and method with reflux metering

Abstract

The application discloses a backflow quantitative combined atmosphere annealing device and method, and belongs to the technical field of thin film material preparation. The device can inject organic gas into gas through an organic vapor humidifier, mix the organic gas with original gas in a gas mixer, and obtain mixed gas meeting set conditions. The mixed gas is blown out towards a thin film supporting platform through a gas spray gun, and a heater heats the thin film supporting platform. Linear blowing and linear annealing are linked in the system, and the area of the thin film being blown and heated is always consistent, so that the organic atmosphere is fully utilized. The device avoids the problem of poor repeatability caused by unquantitative doping atmosphere and uneven atmosphere diffusion, the working environment of the whole system is room pressure and normal temperature, the atmosphere leakage problem of a high-pressure organic gas cylinder is avoided, and the experimental safety risk is reduced.

Description

Technical Field

[0001] This invention pertains to the field of thin film material preparation in semiconductor optoelectronics, photoelectrochemistry, electrocatalysis, and other related fields, and specifically relates to a combined atmosphere annealing apparatus and method with quantitative reflux. Background Technology

[0002] In the fabrication of battery devices, the quality of the perovskite light-absorbing layer typically determines the efficiency and stability of the entire device. The soft lattice properties of perovskite give it greater tolerance for defects compared to traditional inorganic semiconductors, making it an ideal material for solution-based optoelectronic device fabrication. However, perovskite liquid films prepared by spin-coating are highly sensitive during annealing and crystallization. Changes in external temperature and atmosphere can easily lead to inconsistent film quality, making it difficult to improve repeatability. Even when annealing is performed in a glove box, the atmosphere inside the box is difficult to control.

[0003] Some literature indicates that adding molecules of different polarities at different stages during perovskite layer preparation can significantly affect the quality of the thin film crystals. For example, in the synthesis of hybrid perovskite thin films, antisolvent engineering is a commonly used synthesis method. By adding a poorly polar organic solution during spin coating to assist nucleation, the crystal quality can be improved. However, the errors in artificially adding antisolvent (uncertainty in addition time, drop height, and drop amount) introduce many uncertainties to the film quality. In addition, some studies have shown that adding a trace amount of organic atmosphere during perovskite annealing can also help perovskite crystallize better. However, many studies on the participation of organic atmosphere in annealing are only qualitative analyses (e.g., adding a few drops of organic solvent on a heating stage, relying on solvent evaporation and diffusion to the film surface to participate in annealing). The optimal concentration of the atmosphere is still unknown. Furthermore, the uniformity of atmosphere diffusion to the film surface, the error in the amount added each time (drop position), and the influence of airflow caused by circulation in the glove box greatly reduce the repeatability of experimental results. Summary of the Invention

[0004] The purpose of this invention is to overcome the shortcomings of the prior art and provide a combined atmosphere annealing apparatus and method with quantitative reflux, so as to solve the problem that it is difficult to accurately control the annealing atmosphere in the perovskite annealing process, the experimental process is difficult to control the experimental precision, and thus it is difficult to control the quality of perovskite films.

[0005] To achieve the above objectives, the present invention employs the following technical solution:

[0006] A combined atmosphere annealing device with reflux metering includes a gas cylinder. The gas output pipeline of the gas cylinder is divided into a first type of gas pipeline and a second type of gas pipeline. The first type of gas pipeline is connected to a gas mixer. The second type of gas pipeline is connected to the gas mixer after passing through an organic vapor humidifier. The outlet of the gas mixer is connected to an atmosphere chamber.

[0007] The annealing atmosphere chamber is equipped with a thin film support platform. The atmosphere chamber has a second air inlet and an air outlet on both sides of the thin film support platform. A gas spray gun is installed on the thin film support platform. The upper end of the gas spray gun is connected to a gas conduit. A heater is installed at the lower end of the thin film support platform. The gas conduit and the heater are slidably connected to the atmosphere chamber.

[0008] The inlet of the gas duct is connected to the outlet of the gas mixer. The air outlet of the gas spray gun has two arc surfaces on both sides. The arc surface near the second air inlet has a smaller arc surface near the air outlet. The center of the two arc surfaces is on the side near the air outlet. The lower end of the two arc surfaces forms the air outlet.

[0009] The outlet of the gas spray gun and the inner end of the heater are on the same vertical plane;

[0010] The second air inlet is connected to the gas cylinder.

[0011] A further improvement of the present invention is that:

[0012] Preferably, the lower end of the second air inlet and the upper surface of the film support platform are on the same plane.

[0013] Preferably, the gas spray gun has a plate-like structure, and the lower end of the gas spray gun is inclined towards the air outlet direction.

[0014] Preferably, the atmosphere chamber is equipped with a guide rail, which is slidably connected to the gas conduit; the heater is slidably connected to the atmosphere chamber via a screw structure.

[0015] Preferably, the organic vapor humidifier includes a housing, a liquid chamber and a support platform are provided inside the housing, and an organic vapor humidification column is arranged between the liquid chamber and the support platform, with the upper end of the organic vapor humidification column inserted into the liquid chamber;

[0016] The housing has a first air inlet and an exhaust outlet on its two sides, respectively.

[0017] Preferably, both the first type of gas pipeline and the second type of gas pipeline are equipped with float flow meters.

[0018] Preferably, the gas mixer is provided with a tee at its inlet, and the first type of gas pipeline and the second type of gas pipeline are respectively connected to the inlet of the tee.

[0019] Preferably, a gas heat exchanger is provided between the gas mixer and the atmosphere chamber.

[0020] Preferably, the inlet portion of the gas conduit and the outer end of the heater are connected by a connecting rod.

[0021] An annealing method based on the above-mentioned combined atmosphere annealing apparatus with reflux metering involves placing the film to be heat-treated on a film support platform.

[0022] The gas cylinder feeds the gas into the first type of gas pipeline and the second type of gas pipeline respectively. The gas in the second type of gas pipeline is treated by an organic steam humidifier and carries organic gas. The first type of gas pipeline and the second type of gas pipeline are mixed in a gas mixer and then enter the gas conduit. The flow rates of the first type of gas pipeline and the second type of gas pipeline are adjusted to adjust the mixing ratio of the two types of gas in the gas mixer.

[0023] The gas conduit blows the mixed gas out toward the film support platform through the gas spray gun, the second air inlet blows air toward the film support platform, and the heater heats the film support platform.

[0024] During the heat treatment process, the gas spray gun and the heater move synchronously.

[0025] Compared with the prior art, the present invention has the following beneficial effects:

[0026] This invention discloses a combined atmosphere annealing apparatus and method with quantitative reflux. The apparatus outputs two types of gas pipelines from a gas cylinder. One type of gas pipeline injects organic gas through an organic vapor humidifier, which then mixes with the original gas in a gas mixer to obtain a mixed gas that meets set conditions. The mixed gas is blown towards a thin film support platform through a gas spray gun, while a heater simultaneously heats the thin film support platform. This structure can uniformly mix multiple gas sources (organic and inorganic) to provide an annealing atmosphere, and each atmosphere is quantitatively controllable, achieving thin film annealing under a specified atmosphere, with trace amounts of atmosphere being quantitatively controllable. During the heating process, while the gas spray gun injects the mixed gas, a second air inlet simultaneously blows air onto the thin film surface. Because the air outlet is designed with an arc surface, the air outlet is tilted towards the air outlet direction but exhausts towards the heated surface. In this system, linear atmosphere purging and linear annealing are linked, ensuring that the purged and heated areas of the thin film are always consistent, and the atmosphere is fully utilized under these experimental conditions. Unlike traditional heating platforms that simultaneously heat the entire battery, the thin film heating process in this method is directional and slow, matching the atmosphere purging process. Furthermore, the entire process requires no manual operation, avoiding the problems of deteriorated film quality caused by inconsistent doping atmosphere or uneven atmosphere diffusion. In addition, this film annealing process is more suitable for assembly line operations; the linkage control stabilizes the annealing process, improving film uniformity and repeatability. The entire system operates at room pressure and temperature, eliminating the atmosphere leakage issues associated with high-pressure organic gas cylinders and reducing experimental safety risks.

[0027] Furthermore, the upper surface of the second air inlet and the film support platform are on the same plane, so that the gas output from the second air inlet can be directed between the gas spray gun and the atmosphere chamber.

[0028] Furthermore, the gas spray gun has a plate-like structure, which allows synchronous purging to span the entire width of the film.

[0029] Furthermore, the organic atmosphere of the present invention is adsorbed onto the liquid adsorbent by an organic solvent, so that when the gas passes through, some of the gas can be adsorbed. At the same time, by controlling the temperature and the saturated vapor pressure of the organic atmosphere, the amount of organic gas adsorbed in the gas can be controlled.

[0030] Furthermore, this invention enables the addition of organic gases to the gas stream via an organic steam humidifier, which can save on the production costs of using high-pressure gas cylinders for organic sources with high boiling points (which are not easily manufactured into high-pressure gas cylinders). Attached Figure Description

[0031] Figure 1 This is a system structure diagram of the present invention;

[0032] Figure 2 This is a cross-sectional view of the organic steam humidifier of the present invention;

[0033] Figure 3 This is a perspective view of the atmosphere chamber of the present invention;

[0034] Figure 4 This is a two-dimensional side view of the atmosphere chamber of the present invention;

[0035] Figure 5 This is a simulation diagram of the gas flow direction when there is no second air inlet;

[0036] Figure 6 This is a simulation diagram of the gas flow rate during blowing in this invention;

[0037] The components include: 1. Gas cylinder; 2. First-class gas pipeline; 3. Second-class gas pipeline; 4. Gas mixer; 5. Shell; 6. Liquid inlet; 7. First air inlet; 8. Support platform; 9. Liquid outlet; 10. Organic vapor humidification column; 11. Exhaust outlet; 12. Liquid chamber; 13. T-junction; 14. Float flow meter; 15. Atmosphere chamber; 16. Gas heat exchanger; 17. Screw structure; 18. Thin-film support platform; 19. Second air inlet; 20. Guide rail; 21. Gas spray gun; 22. Gas conduit; 23. Connecting rod; 24. Heater; 25. Air outlet; 26. Groove; 27. Organic vapor humidifier; 28. Air outlet section; 29. ​​Air outlet; 30. Other gas sources; 31. Flow regulating valve. Detailed Implementation

[0038] The present invention will now be described in further detail with reference to the accompanying drawings:

[0039] In the description of this invention, it should be noted that the terms "center," "upper," "lower," "left," "right," "vertical," "horizontal," "inner," and "outer," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are used only for the convenience of describing the invention and for simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on the invention. The terms "first," "second," and "third" are used for descriptive purposes only and should not be construed as indicating or implying relative importance. Furthermore, unless otherwise explicitly specified and limited, the terms "installed," "connected," and "linked" should be interpreted broadly. For example, they can refer to a fixed connection or a detachable connection; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal connection of two elements. Those skilled in the art can understand the specific meaning of the above terms in this invention based on the specific circumstances.

[0040] This invention discloses a combined atmosphere annealing device with reflux quantitative flow, which is mainly divided into four parts, in order of gas path: main gas source section (usually inert gas N2 or air, supplied by gas pump or high pressure gas cylinder); organic vapor humidification section (used to carry other trace organic gases); gas mixing section (determining the final required flow rate); and purging annealing section (the thin film undergoes annealing and crystallization in this step).

[0041] The device includes a gas cylinder 1, which has two types of pipelines for outputting gas: a first type of gas pipeline 2 and a second type of gas pipeline 3. The first type of gas pipeline 2 is directly connected to a gas mixer 4, while the second type of gas pipeline 3 enters the gas mixer 4 after passing through an organic vapor humidifier 27. The outlet of the gas mixer 4 is connected to an atmosphere chamber 15, which is also connected to the gas cylinder 1. The gas cylinder 1 typically contains inert gas N2 or air, supplied by a gas pump or a high-pressure gas cylinder. A gas pump can be installed at the outlet of the gas cylinder 1 as needed.

[0042] Both the first type of gas pipeline 2 and the second type of gas pipeline of the present invention are equipped with flow regulating valves 31. The flow regulating valves 31 can adjust the flow rate of the two types of pipelines, thereby adjusting the volume of each gas entering the gas mixer 4, that is, adjusting the mixing ratio of the two gases.

[0043] In some embodiments of the present invention, the structural schematic diagram of the organic steam humidifier 27 is as follows: Figure 2 As shown, the organic vapor humidifier 27 is used to input into the second type of gas pipeline 3. The organic vapor humidifier 27 includes a housing 5, in which a support platform 8 and a liquid chamber 12 are disposed. The liquid chamber 12 is located at the upper end inside the gas mixer 4, and the support platform 8 is located at the lower end inside the housing 5. The liquid chamber 12 has a hollow structure to hold the organic solvent. Organic vapor humidification columns 10 are arranged in a rectangular array on the support platform 8. The upper ends of the organic vapor humidification columns 10 are inserted into the liquid chamber 12, and the insertion height is greater than the height of the liquid in the liquid chamber 12. The liquid chamber 12 is located above the organic vapor humidification columns 10 to better wet the humidification columns under the action of solvent gravity.

[0044] It should be noted that different organic vapor humidification columns 10 need to be matched with different organic solvents to make them have a large specific surface area structure, strong wettability to organic vapors, and will not react with organic vapors.

[0045] It should be understood that, Figure 2 This is one embodiment of the organic steam humidifier 27 of the present invention. In practical applications, the organic steam humidifier 27 can have other structural forms, as long as it can meet the condition of carrying organic gas in the steam and humidifying the organic steam to saturation. Figure 2The organic vapor humidification column 10 in the dashed box can be replaced with other structural forms.

[0046] This device utilizes the physical properties of organic vapor to quantitatively determine the content of organic atmosphere by controlling the temperature. Organic solvent enters the liquid chamber 12 through the inlet 6 and is adsorbed onto the organic vapor humidification column 10. The organic vapor humidification column 10 has a large specific surface area and low airflow resistance. Its main purpose is to ensure that the organic gas carried by the gas reaches saturation (i.e., the gas pressure reaches the saturated vapor pressure) when the gas flows to the end of the channel. When the gas can no longer draw in organic atmosphere, the internal atmosphere is controlled. The gas enters the interior of the housing 5 through the first inlet 7 and flows out from the exhaust port 11 after passing through the organic vapor humidification column 10. The liquid chamber 12 has a sealing structure at the contact point between the organic vapor humidification column 10 and the liquid chamber 12 to prevent liquid from leaking directly from the chamber into the channel. The organic solvent wets the organic vapor humidification column 10 and permeates downwards by gravity and capillary action, keeping the entire column completely wetted. This allows the gas to reach adsorption saturation as quickly as possible during flow. The advantage of this structure is that it allows the adsorption column to remain wetted for a longer period of time even as the liquid level decreases, ensuring the amount of gas adsorbed.

[0047] Furthermore, the saturated vapor pressure of the gas is calculated using this formula:

[0048] ln(P1 / P2)=(ΔH vap / R)((1 / T2)-(1 / T1)) (1)

[0049] In Formula 1, ΔH vap Let T1 be the enthalpy of vaporization of the liquid, R be the ideal gas constant (8.314 J / (K·mol)), T1 and P1 be the known temperatures and corresponding vapor pressures at those temperatures, and T2 be the actual temperature. Therefore, temperature is the primary factor determining vapor pressure.

[0050] Another point to note is that this component does not have a heating source; that is, the airflow temperature T2 at the inlet and outlet is the same, which is room temperature. No heating is performed because if the airflow were heated and discharged from the exhaust port 11, the external pipe temperature would be lower than the airflow temperature. This would cause the saturated vapor pressure in the output pipe containing the organic gas to drop, leading to the liquefaction of the supersaturated vapor and subsequent blockage of the gas pipe.

[0051] In addition, the upper surface of the support platform 8 is designed with a small-angle inclined structure (left is lower and right is higher in the figure). The height of the exhaust port 7 side is higher than the height of the first air inlet 7 to prevent the dripping liquid from accumulating at the bottom of the channel and affecting the adsorption effect of the airflow. A vertical downward drain port 9 is provided on the housing 5 so that excess liquid will flow in along the slope and then flow out through the drain port 9. There is a gap between the bottom of the support platform 8 and the housing 5 to give the liquid a certain buffer space.

[0052] The gas processed by the organic steam humidifier 27 contains organic gases. Under normal circumstances, the organic gases in the gas path can reach saturation. By adjusting the mixing ratio of the first type of gas pipeline 2 and the second type of gas pipeline 3, the organic gases in the second type of gas pipeline 3 can be diluted, thereby controlling the content of organic gases in the final gas, so that the gas ratio and atmosphere input to the atmosphere chamber 15 can meet the requirements.

[0053] See Figure 1 , Figure 3 and Figure 4 The atmosphere chamber 15 has an internal cavity, inside which a thin-film support platform 18 is mounted. The thin-film support platform 18 has a groove 26. A second air inlet 19 and an air outlet 25 are respectively located on two opposite side walls of the thin-film support platform 18. The lower end of the second air inlet 19 is flush with the plane of the thin-film support platform 18. A screw structure 17 is located below the thin-film support platform 18. One end of the screw structure 17 is connected to the side wall of the atmosphere chamber 15, and the other end is connected to a heater 24. The heater 24 and the lower side wall of the thin-film support platform 18 are slidably connected to the bottom of the atmosphere chamber 15, allowing the heater 24 to move below the thin-film support platform 18 to heat it. The outer end of the heater 24 is connected to a gas conduit 22 via a connecting rod 23. The inlet end of the gas conduit 22... The gas duct 22 is connected to the output end of the gas mixer 4. The gas duct 22 is parallel to the moving direction of the heater 24. The gas duct 22 is inserted into the atmosphere chamber 15 from the side wall where the gas outlet 25 is located. The gas duct 22 is connected to the end of the atmosphere chamber 15 by a gas spray gun 21. The gas spray gun 21 has a plate-shaped structure with a rectangular cavity inside for introducing gas. The upper two sides of the gas spray gun 21 are slidably connected to two guide rails 20. The two guide rails 20 are fixedly set on the upper surface inside the atmosphere chamber 15. The gas spray gun 21 is perpendicular to the gas duct 22. The lower end of the gas spray gun 21 is the air outlet. The air outlet 28 has two arc surfaces on both sides. The arc surface near the second air inlet 19 has a smaller arc surface than the arc surface near the air outlet 25. The center of the two arc surfaces is on the side near the air outlet 25. The lower end of the two arc surfaces forms the air outlet 28.

[0054] In some embodiments of the present invention, the gas conduit 22 is connected to the heater 24 via a connecting rod 23. To prevent the gas conduit 22 from getting heated, the connecting rod 23 is made of an insulating material.

[0055] In some embodiments of the present invention, the first type of gas pipeline and the second type of gas pipeline, each type of gas pipeline, can be configured with multiple gas pipelines in parallel as needed, and each gas pipeline is equipped with a float flowmeter 14. An air pump can provide a stable outlet air pressure. According to Bernoulli's principle, when the inlet and outlet air pressures are constant, the flow rate measured by the float flowmeter 14 is considered reliable. In outdoor environments, a gas cylinder and a pressure reducing valve are required to ensure the inlet pressure of the float flowmeter 14.

[0056] In some embodiments of the present invention, the first type of gas pipeline 2 and the second type of gas pipeline 3 are mixed via a tee 13 before entering the gas mixer 4. In the tee 13, the gases in the two pipelines are pre-mixed before entering the inlet section of the gas mixer 4. The gas mixer, with gas entering from the inlet end, contains staggered baffles to ensure thorough and uniform mixing of different types of gases before discharging from the outlet section.

[0057] In some embodiments of the present invention, a gas heat exchanger 16 is provided on the connecting pipeline between the gas mixer 4 and the atmosphere chamber 15 to control the temperature of the mixed gas at the inlet of the gas duct 22.

[0058] In some embodiments of the present invention, the gas mixer 4 can be supplied with other types of gas, which are determined according to the type of gas required for purging, and are other gas sources 30 in the figure.

[0059] The working process of the above device is as follows:

[0060] Gas cylinder 1 feeds gas into first-type gas pipeline 2 and second-type gas pipeline 3. The gas in second-type gas pipeline 3 is processed by organic steam humidifier 27, carrying organic gases; the amount carried is adjusted by the temperature in organic steam humidifier 27. The first-type gas pipeline 2 and second-type gas pipeline 3 are mixed in gas mixer 4. The mixed gas flow output from gas mixer 4 is connected to gas conduit 22 and gas gun 21 via gas heat exchanger 16, ultimately purging the film surface. Guide rail 20 limits the movement of gas gun 21, allowing it to move only back and forth. Furthermore, the gas purging position, the outlet 29 of gas gun 21, is positioned on the same vertical plane as the inner end of heater 24 to synchronize film heating with the atmosphere, ensuring the film is subjected to the mixed gas during growth. A spiral structure 17 is connected to the inner end of heater 24; the propulsion step size is controlled by a motor to control the movement speed of the spiral structure 17 and gas conduit 22. The thin-film support platform 18 has internal grooves 26 to secure the thin film and prevent it from shifting during atmosphere purging. A thinner platform is better to ensure efficient heat conduction. It is noteworthy that the airflow from the nozzle is at a certain angle to the thin film; its function is as follows... Figure 5 As shown: During purging, a negative pressure zone is formed on the left side of the nozzle. This negative pressure causes the atmosphere inside the chamber to move towards the nozzle (blue arrow). This structure is designed to prevent the unheated film from being affected by the doped atmosphere due to atmosphere diffusion (yellow arrow). Air inlet 3, the air source is also provided by an air pump, such as... Figure 6 As shown, the airflow enters through the air inlet and is horizontally swept to the nozzle. The air pump atmosphere replaces the atmosphere inside the chamber to protect the film on the unannealed part. At the same time, the airflow temperature is low, which weakens the influence of heat source through heat conduction during the flow process.

[0061] Thin film growth is a microscopic and sensitive process. Traditional gas purging processes involve purging the entire glass sheet before annealing. The purged portion of the film undergoes complex atmospheric disturbances before annealing, easily leading to inconsistent overall film quality. This invention aims to maximize the effect of the organic atmosphere by linking purging and annealing. The additional gas path ensures that the already crystallized portion is not disturbed by the external atmosphere, thus mitigating issues of uneven film quality and poor repeatability. Thin film annealing is a crystallization process accompanied by solvent evaporation. The main function of gas purging is to rapidly bring the precursor solution (wet film) on the film to a supersaturated state. At this point, most of the solvent in the wet film has evaporated with the high-pressure gas, forming numerous nucleation sites. These nucleation sites help the film form a high-quality, ordered crystal structure in the subsequent high-temperature annealing stage. During this period, the introduction of trace amounts of organic vapor affects the evaporation rate of the wet film. Selecting a suitable atmosphere can effectively control the mass transfer throughout the film nucleation and crystallization process. Furthermore, the dissolution characteristics of the vapor on the wet film during organic vapor treatment may lead to repeated dissolution / recrystallization processes. Crystallization is a process where the system gradually reaches a stable state, while dissolution makes the system more active. Therefore, the introduction of organic solvents affects both the mass transfer and energy transfer of the system. This atmosphere-controlled annealing apparatus not only makes it easy to control processing parameters, such as temperature, flow rate, and processing time, but more importantly, it optimizes the entire annealing process, improving crystal quality. In addition, this film annealing process is more suitable for assembly line operations. The linkage control can stabilize the film annealing process, improving the uniformity and repeatability of the film.

[0062] This invention has the following characteristics

[0063] (1) The content of organic gas is quantitatively controlled by the dynamic balance between the saturated vapor pressure of the organic source and the flow of a controllable inert atmosphere (N2) in a closed container.

[0064] (2) Through the combined action of capillary action and gravity, the humidifying component with a large specific surface area in the channel is completely wetted. When the gas flows through the humidifying component, the surface solvent evaporates quickly and the solvent vapor becomes saturated.

[0065] (3) In order to ensure that the gas is absorbed to saturation, the steam is pre-condensed in the pipeline (lower than the gas temperature) before entering the gas mixer. The pipeline temperature is manually controlled by the refrigeration equipment, and the condensed gas flows back to the vapor pressure saturation device.

[0066] (3) The annealing method is linear advance annealing (heating stage advance annealing), that is, the heating stage starts to contact the film from one end (the film starts to be heated from one end) until it is advanced to the other end of the film.

[0067] (4) The push-type hot stage is connected to the air knife through a connecting rod, so that the air knife and the hot stage act on the same position of the film.

[0068] (5) The curved shape of the nozzle makes the ejected airflow form an acute angle with the film.

[0069] (6) Another stream of N2 gas is supplied by a gas pump and blown horizontally from the other end of the annealing device (the other end of the film) to prevent the unheated film from being affected by the doped atmosphere due to atmospheric diffusion. At the same time, the gas flow temperature is low to minimize the effect of thermal diffusion.

[0070] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A reflow and dosing combined atmosphere annealing apparatus, characterized by, The gas cylinder (1) is provided with a first type gas pipeline (2) and a second type gas pipeline (3), the first type gas pipeline (2) is connected with a gas mixer (4), the second type gas pipeline (3) is connected to the gas mixer (4) through an organic vapor humidifier (27), and the outlet of the gas mixer (4) is connected with an atmosphere warehouse (15); A film supporting platform (18) is arranged in the atmosphere warehouse (15), and a second gas inlet (19) and a gas outlet (25) are arranged on the two sides of the film supporting platform (18); a gas spray gun (21) is arranged on the film supporting platform (18), the upper end of the gas spray gun (21) is connected with a gas pipeline (22), and the lower end of the film supporting platform (18) is provided with a heater (24); the gas pipeline (22) and the heater (24) are both in sliding connection with the atmosphere warehouse (15); The inlet of the gas pipeline (22) is connected with the outlet of the gas mixer (4), the gas spray gun (21) is provided with two arc surfaces on the two sides of the air outlet part (28), the arc surface close to the second gas inlet (19) has a smaller curvature than the arc surface close to the gas outlet (25), the centers of the two arc surfaces are on the side close to the gas outlet (25), and the lower ends of the two arc surfaces form the air outlet (28); The outlet of the gas spray gun (21) and the inner end of the heater (24) are in the same vertical plane; The second gas inlet (19) is connected with the gas cylinder (1); The lower end of the second gas inlet (19) and the upper surface of the film supporting platform (18) are in the same plane; The gas spray gun (21) is in a plate structure, and the lower end air outlet of the gas spray gun (21) is inclined towards the gas outlet (25); A guide rail (20) is arranged in the atmosphere warehouse (15), the guide rail (20) and the gas pipeline (22) are in sliding connection, and the heater (24) is in sliding connection with the atmosphere warehouse (15) through a screw rod structure (17).

2. A reflow and quantitative atmosphere annealing apparatus according to claim 1, wherein The organic vapor humidifier (27) comprises a shell (5), a liquid cavity (12) and a supporting table (8) are arranged in the shell (5), a plurality of organic vapor humidifying columns (10) are arranged between the liquid cavity (12) and the supporting table (8), and the upper ends of the organic vapor humidifying columns (10) are inserted into the liquid cavity (12). First gas inlets (7) and exhaust outlets (11) are arranged on the two sides of the shell (5).

3. A reflow and quantitative atmosphere annealing apparatus according to claim 1, wherein Float flowmeters (14) are arranged on the first type gas pipeline (2) and the second type gas pipeline (3).

4. The reflow and quantitative atmosphere annealing apparatus according to claim 1, wherein A three-way joint (13) is arranged at the inlet of the gas mixer (4), and the first type gas pipeline (2) and the second type gas pipeline (3) are connected with the inlet of the three-way joint (13).

5. The reflow and quantitative atmosphere annealing apparatus according to claim 1, wherein A gas heat exchanger (16) is arranged between the gas mixer (4) and the atmosphere warehouse (15).

6. The reflow and quantitative atmosphere annealing apparatus according to claim 1, wherein The input part of the gas pipeline (22) and the outer end of the heater (24) are connected through a connecting rod (23).

7. An annealing method of a combined atmosphere annealing apparatus based on the backflow quantification of claim 1, characterized by, The film to be heat treated is placed on the film supporting platform (18). The gas cylinder (1) inputs gas to the first type gas pipeline (2) and the second type gas pipeline (3) respectively, the gas in the second type gas pipeline (3) is treated by the organic vapor humidifier (27) and carries organic gas; the first type gas pipeline (2) and the second type gas pipeline (3) are mixed in the gas mixer (4) and then enter the gas pipeline (22); the flow of the first type gas pipeline (2) and the second type gas pipeline (3) is adjusted to adjust the mixing ratio of the two types of gas in the gas mixer (4); The mixed gas is blown out by the gas spray gun (21) toward the film supporting platform (18) through the gas pipeline (22), the second gas inlet (19) blows gas toward the film supporting platform (18), and the heater (24) heats the film supporting platform (18); During the heat treatment process, the gas spray gun (21) and the heater (24) move synchronously.

Images