Vacuum crystal making equipment

Abstract

The invention discloses vacuum crystal making equipment, and relates to the technical field of crystal growth equipment, the vacuum crystal making equipment comprises a vacuum cavity, the inner space of the vacuum cavity is used for vacuum crystal making; the constant-temperature bottom plate is fixedly connected to the bottom of the vacuum cavity in a sealed mode, and the constant-temperature bottom plate is externally connected with a constant-temperature device and used for maintaining the temperature of the constant-temperature bottom plate to a set value; the top cover is fixedly connected to the top of the vacuum cavity in a sealed mode, and the interior of the top cover is of a conical surface structure with the cross section area gradually reduced from bottom to top. A plurality of connectors are formed in the top cover and used for being connected with auxiliary equipment in a sealed mode. The vacuum crystal making equipment provided by the invention can improve the crystal growth stability and the airflow guide effect.

Description

Technical Field

[0001] This invention relates to the field of crystal growth equipment technology, and in particular to a vacuum crystallization device. Background Technology

[0002] In the field of crystal growth, the performance of vacuum crystallization equipment plays a decisive role in crystal quality and growth efficiency. Existing vacuum crystallization equipment mostly employs traditional planar or cylindrical designs, which presents numerous insurmountable problems.

[0003] From a temperature perspective, the uneven temperature distribution inside traditional equipment, especially the significant temperature differences in the substrate holder between different batches during verification, can affect experimental results. During crystal growth, temperature differences can easily lead to defects within the crystal, affecting its critical optical and electrical properties. Regarding energy utilization, the planar design of the top cover in vacuum crystallization equipment results in a relatively chaotic internal gas field, leading to high energy consumption and poor product quality in traditional equipment.

[0004] Existing equipment lacks effective means for bottom temperature control, resulting in large temperature fluctuations in the wet film on the substrate during nucleation, crystallization, and growth, further exacerbating the instability of crystal growth. Furthermore, the unreasonable design of the top structure also leads to poor airflow guidance. Therefore, there is an urgent need to design a technical solution that can improve crystal growth stability and airflow guidance. Summary of the Invention

[0005] The purpose of this invention is to provide a vacuum crystallization device to solve the problems existing in the prior art, and to improve the stability of crystal growth and the airflow guidance effect.

[0006] To achieve the above objectives, the present invention provides the following solution: This invention provides a vacuum crystallization apparatus, comprising: A vacuum chamber, the internal space of which is used for vacuum crystal formation; A constant temperature base plate is fixedly and sealed to the bottom of the vacuum chamber. A constant temperature device is connected to the outside of the constant temperature base plate to maintain the temperature of the constant temperature base plate to a set value. The top cover is fixedly and sealed to the top of the vacuum chamber. The interior of the top cover is a conical structure with a cross-sectional area that gradually decreases from bottom to top. The top cover has multiple interfaces for sealing and connecting auxiliary equipment.

[0007] Preferably, the vacuum chamber has a rectangular cross-section, and a gas equalization port is provided on the side wall of the vacuum chamber. The gas equalization port is connected to an inert gas input device through a pipeline with a valve.

[0008] Preferably, the constant temperature device includes a water tank, which is equipped with a heating device and a cooling device to maintain the water in the water tank at a set temperature; the constant temperature base plate has a spiral or serpentine flow channel, the inlet and outlet of the flow channel are respectively connected to the water tank through a circulating water pipe, and the circulating water pipe is equipped with a circulating water pump.

[0009] Preferably, the inclination angle of the side wall of the top cover is between 45° and 60°; the interface at the top of the top cover has a chamfer between it and the inner side wall of the top cover.

[0010] Preferably, a material inlet is provided on one side of the vacuum chamber, and a substrate holder is movably inserted through the material inlet. A door panel is fixedly connected to the outside of the substrate holder, and the door panel can be fixedly and sealingly abutted against the outer wall of the material inlet of the vacuum chamber; the bottom of the substrate holder contacts the top of the constant temperature base plate.

[0011] Preferably, the vacuum cavity has symmetrical strip tracks on two inner sidewalls perpendicular to the sidewall where the feed port is located, and the substrate holder is slidably disposed on both sides within the corresponding strip tracks.

[0012] Preferably, the auxiliary equipment includes a vacuum system, which is sealed to the interface at the top of the top cover via a vacuum pipeline with a valve; an inert gas branch is connected to the vacuum pipeline, the inert gas branch is externally connected to an inert gas input device, and a control valve and a flow meter are provided on the inert gas branch.

[0013] Preferably, the auxiliary device includes a digital resistance gauge, which is fixedly and sealed to an interface on the side wall of the top cover, and the digital resistance gauge can display the vacuum level inside the vacuum chamber in real time.

[0014] Preferably, a transparent plate is fixedly sealed at the interface on one of the side walls of the vacuum chamber, and a camera module is arranged on the outside of the transparent plate for acquiring images of the crystal growth process inside the vacuum chamber.

[0015] Preferably, a pressure relief valve is provided on the interface of the top cover sidewall.

[0016] Compared with the prior art, the present invention has achieved the following technical effects: This invention's constant-temperature substrate maintains a constant temperature at a set value, thereby precisely controlling the temperature at the bottom of the vacuum chamber and uniformly transferring heat or cold to the substrate. This ensures temperature consistency between the substrate and the bottom of the vacuum chamber, guaranteeing substrate temperature uniformity. The conical structure inside the top cover makes the gas field distribution in the upper and lower regions of the vacuum chamber more uniform, significantly reducing the probability of crystal defects caused by uneven internal gas field during evacuation, thus improving crystal quality. The rational conical design inside the top cover reduces airflow resistance during evacuation, lowering equipment energy consumption and saving production costs. The constant-temperature substrate ensures stable substrate temperature during nucleation, crystallization, and growth of the wet film. The guiding effect of the conical structure inside the top cover reduces the impact of airflow disturbance on crystal growth. Simultaneously, the uniform temperature environment ensures consistent crystal growth rate, making crystal shape and size easier to control, improving crystal growth stability and yield. Attached Figure Description

[0017] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0018] Figure 1 This is a schematic diagram of a vacuum cavity structure in one or more embodiments of the present invention; Figure 2 This is a front view of a vacuum cavity in one or more embodiments of the present invention; Figure 3 This is a top view schematic diagram of the top cover in one or more embodiments of the present invention; Figure 4 This is a left view of the top cover in one or more embodiments of the present invention; Figure 5 This is a schematic diagram of the constant temperature base plate structure in one or more embodiments of the present invention; Figure 6 This is a schematic diagram of the flow channel structure inside the constant temperature base plate in one or more embodiments of the present invention. Figure 7 This is a front view of the constant temperature base plate in one or more embodiments of the present invention; Figure 8 This is a schematic diagram of the overall structure of the vacuum crystallization equipment in one or more embodiments of the present invention; Figure 9 This is a top view of a door panel in one or more embodiments of the present invention; Figure 10 This is a right view of a door panel in one or more embodiments of the present invention.

[0019] In the diagram: 1-vacuum chamber, 101-feed port, 102-gas equalization port, 103-pressure relief port, 2-constant temperature base plate, 201-flow channel, 202-inlet, 203-outlet, 3-top cover, 301-interface, 302-observation window, 4-door panel, 5-substrate holder, 6-digital resistance gauge, 7-vacuum pump, 8-gas flow meter, 9-valve. Detailed Implementation

[0020] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0021] The purpose of this invention is to provide a vacuum crystallization device to solve the problems existing in the prior art, and to improve the stability of crystal growth and the airflow guidance effect.

[0022] To make the above-mentioned objects, features and advantages of the present invention more apparent and understandable, the present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.

[0023] Vacuum crystallization is a process in which target components are generated through phase transformation or chemical reactions of raw materials in a vacuum environment, allowing atoms / molecules to align along the crystal lattice structure of a seed crystal to form single or polycrystalline crystals. The principle and process are mature existing technologies. Generally, a substrate is placed inside a vacuum device, and a wet film on the substrate nucleates, crystallizes, and grows under set vacuum and temperature conditions, ultimately forming the desired crystal. However, existing vacuum crystallization equipment lacks effective means for bottom temperature control, resulting in large temperature fluctuations in the wet film on the substrate during nucleation, crystallization, and growth, further exacerbating the instability of crystal growth. Furthermore, the unreasonable design of the top structure of the vacuum crystallization equipment also leads to poor airflow guidance. To solve this problem, this invention provides a vacuum crystallization device, referencing... Figures 1-10As shown, the device includes a vacuum chamber 1, a constant-temperature base plate 2, and a top cover 3. The internal space of the vacuum chamber 1 is used for vacuum crystal formation. The constant-temperature base plate 2 is fixedly and sealed to the bottom of the vacuum chamber 1, and a constant-temperature device is connected to the outside of the constant-temperature base plate 2 to maintain the temperature of the constant-temperature base plate 2 at a set value. The top cover 3 is fixedly and sealed to the top of the vacuum chamber 1. The interior of the top cover 3 is a conical structure with a cross-sectional area that gradually decreases from bottom to top. The top cover 3 has multiple interfaces 301 for sealing and connecting auxiliary equipment. The constant-temperature base plate 2 of this invention can maintain a constant temperature at a set value, thereby accurately controlling the temperature at the bottom of the vacuum chamber 1 and uniformly transferring heat to the substrate, ensuring the consistency of the substrate temperature. The conical structure inside the top cover 3 makes the gas field distribution in the upper and lower regions inside the vacuum chamber 1 more uniform, greatly reducing the probability of defects in the crystal due to uneven internal gas field during evacuation, and improving the quality of the crystal. The bottom of the top cover 3 has a horizontally arranged outer edge, which can be fixedly and sealed to the top of the side wall of the vacuum chamber 1 to ensure the sealing performance of the vacuum chamber 1 after connection. The well-designed internal conical surface of the top cover 3 reduces airflow resistance during extraction, lowers equipment energy consumption, and saves production costs. The constant temperature base plate 2 ensures the stability of the substrate temperature during nucleation, crystallization, and growth of the wet film. The internal conical structure of the top cover 3 guides airflow, reducing the impact of airflow disturbance on crystal growth. At the same time, the uniform temperature environment ensures the consistency of crystal growth rate, making it easier to control the shape and size of the crystal, and improving the stability and yield of crystal growth.

[0024] In one embodiment, the vacuum chamber 1 has a rectangular cross-section and can be made of stainless steel or aluminum, with aluminum requiring surface treatment. Its shape is adapted to the bottom constant temperature plate and the internal conical structure of the top cover 3, providing a stable vacuum environment for crystal growth. Two symmetrically arranged gas equalization ports 102 are provided on the rear side wall of the vacuum chamber 1. Each gas equalization port 102 is connected to an inert gas input device via a pipe equipped with a valve 9. The valve 9 on the pipe is a solenoid valve or a needle valve, and a gas flow meter 8 is also provided on the pipe. The amount of inert gas entering during evacuation is controlled by the solenoid valve, needle valve, and gas flow meter 8. The inert gas input device includes an inert gas cylinder and a gas pump. The gas pump connects the outlet of the inert gas cylinder to the gas equalization port 102, and a control valve is also provided at the outlet of the inert gas cylinder.

[0025] In one embodiment, the constant temperature device includes a water tank equipped with a heating device such as a heating wire or heating element, and also includes existing mature refrigeration equipment. By turning on the heating or refrigeration equipment, the water in the water tank can be heated or cooled and maintained at a set temperature. The constant temperature base plate 2 has a spiral or serpentine flow channel 201 pre-set inside. The inlet 202 and outlet 203 of the flow channel 201 are respectively connected to the water tank through a circulating water pipe. A circulating water pump is installed on the circulating water pipe. Water heated or cooled to the set temperature is input into the flow channel 201 of the constant temperature base plate 2 to maintain the temperature value of the constant temperature base plate 2. The circulating water flows out through the outlet 203 of the flow channel 201 in the constant temperature base plate 2 and returns to the water tank for reheating or cooling. The temperature value of the constant temperature base plate 2 is kept constant by the circulating water. The constant temperature base plate 2 evenly transfers cold / heat to the bottom area of ​​the vacuum chamber 1, reduces the temperature fluctuation at the bottom, and ensures the temperature of the substrate holder 5 and the substrate in the vacuum chamber 1, providing a stable temperature environment for crystal growth.

[0026] The planar design of the top cover 3 in the prior art results in a relatively chaotic gas field inside the vacuum chamber 1, leading to high energy consumption and poor product quality in traditional equipment. To solve this problem, the side wall inclination angle of the top cover 3 in this invention is between 45° and 60°. The interface 301 at the top of the top cover 3 is a flange structure with a chamfer transition to the inside of the top cover 3. The height from the top of the top cover 3 to the vacuum chamber 1 adopts an inclined conical design to form a conical side wall. The conical side wall can also guide the airflow inside the vacuum chamber 1, reduce the impact of airflow disturbance on crystal growth, and improve the stability of crystal growth.

[0027] A material inlet 101 is provided on one side of the vacuum chamber 1, and a substrate holder 5 is movably inserted through the material inlet 101. A door panel 4 is fixedly connected to the outside of the substrate holder 5, and the door panel 4 can be fixedly and sealed against the outer wall of the material inlet 101 of the vacuum chamber 1. The bottom of the substrate holder 5 contacts the top of the constant temperature base plate 2, so that the substrate contacts the constant temperature base plate 2 to ensure the gas temperature. In order to make the substrate holder 5 enter and exit the vacuum chamber 1 more smoothly, in one embodiment, strip-shaped slides are symmetrically provided on the two inner side walls of the vacuum chamber 1 perpendicular to the side wall where the material inlet 101 is located. The two sides of the substrate holder 5 are slidably disposed in the strip-shaped slides on the corresponding sides. The contact surface between the door panel 4 and the outer wall of the vacuum chamber 1 is a sealing surface. The door panel 4 is designed as a drawer to assist the substrate coated with wet film to enter and exit the vacuum chamber 1. In another embodiment, the door panel 4 includes a vertical plate and two horizontally symmetrically arranged strip sliders. One end of the strip sliders is fixed to one side of the door panel 4. The vertical plate can be fixedly and sealed against or snapped against the outer wall of the vacuum chamber 1. The outer side of the strip sliders is slidably connected to the corresponding strip slide of the inner wall of the vacuum chamber. A support plate is connected between the two strip sliders. The support plate is used to snap onto the substrate holder 5 to fix the substrate holder 5.

[0028] In one embodiment, the auxiliary equipment includes a vacuum system, a digital resistance gauge 6, and a camera module. The vacuum system is sealed to the interface 301 on the top of the top cover 3 via a vacuum pipeline with a valve 9. The vacuum system in this embodiment includes a vacuum pump 7, a vacuum valve 9, and a vacuum measuring device. The vacuum pump 7 can pump the gas pressure inside the vacuum chamber 1 to the vacuum level required for crystal growth. The vacuum valve 9 is used to control the connection and disconnection of the pipeline between the vacuum chamber 1 and the vacuum pump 7. The vacuum measuring device uses an existing measuring instrument, which can monitor the vacuum level inside the vacuum chamber 1 in real time to ensure the stability of the vacuum environment. An inert gas branch is connected to the vacuum line, and an inert gas input device is connected to the inert gas branch. The inert gas branch is equipped with a control valve and a flow meter. During vacuuming, an adjustable flow rate of inert gas is introduced through the gas distribution port to carry the solvent in the wet film into the vacuum line for discharge. When the vacuum pump 7 evacuates the vacuum chamber 1, the pumping speed can reach 10 Pa in 3 seconds, and then continue until the ultimate vacuum is reached. By adjusting the inert gas intake in the vacuum line, the vacuum pump 7 increases the load on the branch while evacuating the vacuum chamber 1, which indirectly reduces the pumping speed. Thus, the evacuation effect of the vacuum pump 7 can be adjusted by introducing an adjustable flow rate of inert gas into the vacuum line through the inert gas branch. Each of the four side walls of the top cover 3 is equipped with an interface 301. One of the side wall interfaces 301 is sealed to a digital resistance gauge 6, which can display the vacuum level in the vacuum chamber 1 in real time. A transparent plate or transparent glass is fixedly sealed at interface 301 on another side wall of the vacuum chamber 1, serving as an observation window 302. A camera module is arranged on the outside of the transparent plate or transparent glass. The camera module is a video camera or a video recording camera, used to capture images of the crystal growth process inside the vacuum chamber 1. The video recording camera can record and present the color and morphological changes of the wet film during the nucleation-crystallization-growth process. A pressure relief valve is provided on the interface 301 of the remaining side wall of the top cover 3, or two symmetrical pressure relief ports 103 are opened in the middle of both sides of the vacuum chamber 1. A pressure relief valve is installed at the pressure relief port 103. In this embodiment, the pressure relief valve is a solenoid valve with a pressure relief button. The opening degree of the solenoid valve can be controlled by the pressure relief button, thereby controlling the pressure inside the vacuum chamber 1.

[0029] The constant-temperature base plate 2 of this invention can maintain a constant temperature at a set value, thereby precisely controlling the temperature at the bottom of the vacuum chamber 1 and uniformly transferring heat or cold to the substrate, ensuring the consistency of the substrate temperature. The conical structure inside the top cover 3 makes the gas field distribution in the upper and lower regions inside the vacuum chamber 1 more uniform, greatly reducing the probability of defects in the crystal caused by uneven internal gas field during evacuation, and improving the quality of the crystal. The reasonable conical design inside the top cover 3 reduces the airflow resistance during evacuation, reduces the energy consumption of the equipment, and saves production costs. The constant-temperature base plate 2 ensures the stability of the substrate temperature during nucleation, crystallization, and growth of the wet film. The conical structure inside the top cover 3 guides the airflow, reducing the impact of airflow disturbance on crystal growth. Simultaneously, the uniform temperature environment ensures consistent crystal growth rate, making the crystal shape and size easier to control, thus improving the stability and yield of crystal growth. When the vacuum pump 7 evacuates the vacuum chamber 1, the pumping speed can reach 10 Pa in 3 seconds, and then continue until the ultimate vacuum is reached. Adjusting the amount of inert gas introduced into the vacuum chamber 1 through the gas distribution port can remove the solvent from the wet film within the vacuum chamber 1, and simultaneously adjust the pressure within the vacuum chamber 1 to a fixed value (e.g., stabilized at 1 Pa). When the vacuum pump 7 evacuates the vacuum chamber 1, the pumping speed can... The process achieves a vacuum of 10 Pa in 3 seconds, continuing until the ultimate vacuum is reached. By adjusting the inert gas intake in the vacuum pipeline, the vacuum pump 7 effectively reduces the pumping speed by increasing the load on the branch while evacuating the vacuum chamber 1. The evacuation rate of the vacuum chamber 1 can be adjusted by regulating the inert gas intake at the gas distribution port and the inert gas intake at the exhaust port. The experimental process can be adjusted based on the recording effect through the observation window 302. The conical design inside the top cover 3 optimizes the film formation effect and avoids the formation of textures on the substrate surface. Experimental results show that the perovskite thin film grown using the equipment of this invention has more than 10% fewer internal defects than crystals grown using traditional equipment. The uniformity of grains and the uniformity of crystal growth rate are also significantly improved, greatly increasing production efficiency and product quality.

[0030] The present invention uses specific examples to illustrate the principles and implementation methods of the present invention. The above examples are only intended to help understand the method and core concept of the present invention. At the same time, those skilled in the art will find that the specific implementation methods and application scopes may vary based on the concept of the present invention. In summary, the contents of this specification should not be construed as limiting the present invention.

Claims

1. A vacuum crystallization apparatus, characterized in that: include: A vacuum chamber, the internal space of which is used for vacuum crystal formation; A constant temperature base plate is fixedly and sealed to the bottom of the vacuum chamber. A constant temperature device is connected to the outside of the constant temperature base plate to maintain the temperature of the constant temperature base plate to a set value. The top cover is fixedly and sealed to the top of the vacuum chamber. The interior of the top cover is a conical structure with a cross-sectional area that gradually decreases from bottom to top. The top cover has multiple interfaces for sealing and connecting auxiliary equipment.

2. The vacuum crystallization equipment according to claim 1, characterized in that: The vacuum chamber has a rectangular cross-section, and a gas equalization port is provided on the side wall of the vacuum chamber. The gas equalization port is connected to an inert gas input device through a pipeline with a valve.

3. The vacuum crystallization equipment according to claim 1, characterized in that: The constant temperature device includes a water tank, which is equipped with a heating device and a cooling device to maintain the water in the water tank at a set temperature; the constant temperature base plate has a spiral or serpentine flow channel, and the inlet and outlet of the flow channel are connected to the water tank through a circulating water pipe, which is equipped with a circulating water pump.

4. The vacuum crystallization equipment according to claim 2, characterized in that: The side wall of the top cover has an inclination angle between 45° and 60°; the interface at the top of the top cover has a chamfer between it and the inner side wall of the top cover.

5. The vacuum crystallization apparatus according to claim 1, characterized in that: The vacuum chamber has a material inlet on one side, and a substrate holder is movably inserted through the material inlet. A door panel is fixedly connected to the outside of the substrate holder, and the door panel can be fixedly and sealed against the outer wall of the material inlet of the vacuum chamber. The bottom of the substrate holder is in contact with the top of the constant temperature base plate.

6. The vacuum crystallization apparatus according to claim 5, characterized in that: The vacuum chamber has symmetrical strip tracks on its two inner sidewalls that are perpendicular to the sidewall where the feed port is located, and the substrate holder is slidably disposed in the corresponding strip tracks on both sides.

7. The vacuum crystallization apparatus according to claim 1, characterized in that: The auxiliary equipment includes a vacuum system, which is sealed to the interface at the top of the top cover via a vacuum pipeline with a valve; an inert gas branch is connected to the vacuum pipeline, and an inert gas input device is connected to the inert gas branch, which is equipped with a control valve and a flow meter.

8. The vacuum crystallization apparatus according to claim 1, characterized in that: The auxiliary equipment includes a digital resistance gauge, which is fixedly and sealed to an interface on the side wall of the top cover. The digital resistance gauge can display the vacuum level inside the vacuum chamber in real time.

9. The vacuum crystallization apparatus according to claim 1, characterized in that: A transparent plate is fixedly sealed at the interface on one of the side walls of the vacuum chamber, and a camera module is arranged on the outside of the transparent plate to collect images of the crystal growth process inside the vacuum chamber.

10. The vacuum crystallization apparatus according to claim 1, characterized in that: A pressure relief valve is provided on the interface of the top cover side wall.

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