Perovskite single crystal crystallization device

Abstract

The utility model relates to the technical field of perovskite, and discloses a perovskite single crystal crystallization device which comprises a mixing machine, the mixing machine comprises a connector, the connector is respectively connected with a heating test tube and a condensing test tube, the interior of the connector is divided into two sections, one section, connected with the heating test tube, of the connector can drive the heating test tube to rotate through a built-in motor, the other section, connected with the condensation test tube, of the connector cannot rotate, and the two sections of the connector are in sealed connection through a sealing piece. Heating can be more uniform through a water bath heating mode, adverse effects of local overheating on a solution are avoided, flexible adjustment of the angles of a heating test tube and a condensation test tube is achieved through the design of a mixing machine rotating disc and a connector, different operation requirements are met, and the practicability is high. And through the inclined angle, steam generated by heating can enter the condensation cavity more conveniently for heat exchange and cooling.

Description

Technical Field

[0001] The utility model relates to the technical field of perovskite, in particular to a perovskite single crystal crystallization device. Background Art

[0002] Perovskites are generally cubic or octahedral in shape, shiny, and light to brown in color. They can be used to refine titanium, niobium and rare earth elements, but they are only worth mining when they are gathered in large quantities. Due to the special structure of perovskite materials, it has potential application prospects in high-temperature catalysis and photocatalysis. Research on perovskite structure-type materials at home and abroad mainly focuses on material structure, and there is relatively little research on their application in catalysis. In addition to crystalline silicon, perovskites can also be used to make alternative materials for solar cells. In 2009, solar cells made of perovskites had a solar energy conversion rate of 3.8%. By 2014, this figure had increased to 19.3%. Compared with the energy efficiency of traditional crystalline silicon cells of more than 20%. Scientists believe that the performance of this material is still likely to be improved. By optimizing the preparation conditions and process parameters, high-quality, high-performance perovskite crystals can be obtained to meet its application needs in solar cells, LEDs and other fields.

[0003] For example, the Chinese patent "CN217173938U" discloses a perovskite single crystal crystallization device, which proposes: the perovskite single crystal crystallization device includes a crystallization dish for accommodating a perovskite solution, and an opening is provided at the upper end of the crystallization dish; a lid is used to seal with the upper end opening of the crystallization dish, and a condensed solvent collection tank is circumferentially provided at the lower inner wall of the lid; a heating mechanism is used to heat the perovskite solution in the crystallization dish; and a heat preservation mechanism at least covers the outer wall of the lid and the crystallization dish. The perovskite single crystal crystallization device provided by the utility model is provided with a heat preservation mechanism and a condensed solvent collection tank, which can prevent the relatively low temperature solvent after condensation from dripping back into the crystallization solution, ensure the temperature stability of the crystallization solution, and effectively prevent the temperature-sensitive perovskite from producing multiple crystal types.

[0004] It can be seen from the above-mentioned device that although the above-mentioned device avoids the reflux of low-temperature solvent, the applicant believes that the following defects still exist:

[0005] Traditional devices often find it difficult to achieve precise temperature control during the reaction process. Since perovskite crystallization is sensitive to temperature, temperature fluctuations may lead to unstable crystallization rate, affecting crystal quality and yield. There is no stirring step in the process of heating and crystallizing the perovskite solution, which will cause problems of uneven heating and mixing. The steam generated by the heated crystallization is not effectively collected, resulting in environmental pollution and health risks for operators. In addition, the condensed solution formed after the steam is cooled can be heated again for crystallization operation. Utility Model Content

[0006] (I) Technical problems solved: In view of the deficiencies in the prior art, the utility model provides a perovskite single crystal crystallization device, which has the advantages of being able to fully stir the solution during heating and ensuring the stability of the solution temperature during the crystallization process. It solves the problem that traditional devices are often difficult to achieve precise control of temperature during the reaction process. Since perovskite crystallization is sensitive to temperature, temperature fluctuations may lead to unstable crystallization rate, affecting crystal quality and yield. There is no stirring step in the process of heating and crystallizing the perovskite solution, which will cause problems of uneven heating and mixing. The steam generated by the heated crystallization is not effectively collected, resulting in environmental pollution and health risks for operators.

[0007] (II) Technical solution: To achieve the above-mentioned purpose, the utility model provides the following technical solution: a perovskite single crystal crystallization device, comprising a mixer, the mixer comprising a chassis, the outer wall of the chassis is provided with a turntable, the outer wall of the turntable is fixedly connected with a connector, the connector is respectively connected to a heating test tube and a condensing test tube, the interior of the connector is divided into two sections, the section of the connector connected to the heating test tube can drive the heating test tube to rotate through a built-in motor, the other section of the connector connected to the condensing test tube cannot rotate, and the two sections of the connector are sealed and connected by a seal;

[0008] The heating test tube is arranged inside the heating furnace, water is arranged inside the heating furnace, and the water inside the heating furnace is heated by a heating plate arranged below.

[0009] Preferably, the heating plate can adjust the heating temperature to adapt to perovskite solutions of different concentrations, and the maximum adjustable temperature of the heating plate is degrees Celsius.

[0010] Preferably, a supporting member is provided above the heating furnace to limit and clamp the heating test tube, the heating test tube includes a crystallization cavity, most of the crystallization cavity is arranged underwater inside the heating furnace, an extension tube is fixedly connected to the outer wall of the crystallization cavity, and the crystallization cavity is movably installed inside the clamping member above the heating furnace.

[0011] Preferably, a reflux cavity is provided on the outer wall of the extension tube, the extension tube extends into the reflux cavity, a connecting tube is provided on the outer wall of the reflux cavity, and the connecting tube is arranged inside the connector.

[0012] Preferably, the condensation test tube includes an adapter, which is arranged inside the connecting head, and the outer wall of the adapter is fixedly connected to a steam chamber, a condensation chamber is opened above the steam chamber, a spiral condensation tube is arranged inside the condensation chamber, and condensate is arranged inside the condensation tube.

[0013] Preferably, a pressure chamber is provided on the outer wall of the steam chamber, and a solvent tank is provided below the steam chamber.

[0014] Preferably, the turntable drives the connector to rotate so that the heating tube and the condensing tube are tilted upward, and the angles between the heating tube and the condensing tube and the horizontal plane are acute.

[0015] (III) Beneficial effects: Compared with the prior art, the utility model provides a perovskite single crystal crystallization device, which has the following beneficial effects:

[0016] 1. The perovskite single crystal crystallization device, through the cooperation between the mixer and the heating furnace, can make the heating more uniform through water bath heating when heating the perovskite solution, avoiding local overheating from causing adverse effects on the solution, and through the design of the mixer turntable and the connector, the angles of the heating test tube and the condensing test tube can be flexibly adjusted to meet different operating requirements, and the tilted angle makes it easier for the steam generated by the heating to enter the condensing chamber for heat exchange cooling.

[0017] 2. The perovskite single crystal crystallization device is configured to extend the extension tube in the reflux chamber. After the steam enters the condensation chamber for cooling, the formed liquid will slide down the inner wall. Since the whole is inclined, a small amount of liquid will slide along the test tube into the reflux chamber. Due to the extension of the extension tube, the refluxed liquid is effectively prevented from entering the crystallization chamber, ensuring the temperature of the crystallization solution to be stable, and effectively avoiding the temperature-sensitive perovskite from producing multiple crystal types. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 This is a schematic diagram of the crystal structure of the utility model;

[0019] Figure 2 This is a schematic diagram of the structure of the utility model in a state of waiting for heating;

[0020] Figure 3 This is a schematic diagram of the cross-sectional structure of the heating test tube of the utility model;

[0021] Figure 4 It is a schematic diagram of the cross-sectional structure of the condensation test tube of the utility model.

[0022] The numbers in the figure are:

[0023] 1. Heating plate; 2. Heating furnace; 3. Heating test tube; 31. Crystallization chamber; 32. Extension tube; 33. Reflux chamber; 34. Connecting tube; 4. Mixer; 41. Chassis; 42. Turntable; 43. Connector; 5. Condensation test tube; 51. Adapter; 52. Steam chamber; 53. Condensation chamber; 54. Condensation tube; 55. Pressure chamber; 56. Solvent tank. DETAILED DESCRIPTION

[0024] The following will be combined with the drawings in the embodiments of the utility model to clearly and completely describe the technical solutions in the embodiments of the utility model. Obviously, the described embodiments are only part of the embodiments of the utility model, not all of the embodiments. Based on the embodiments in the utility model, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the utility model.

[0025] See also Figure 1-2 A perovskite single crystal crystallization device includes a mixer 4, which includes a chassis 41. A turntable 42 is provided on the outer wall of the chassis 41. A connector 43 is fixedly connected to the outer wall of the turntable 42. The connector 43 is respectively connected to the heating tube 3 and the condensing tube 5. The interior of the connector 43 is divided into two sections. The section of the connector 43 connected to the heating tube 3 can drive the heating tube 3 to rotate through a built-in motor, and the other section of the connector 43 connected to the condensing tube 5 cannot rotate, and the two sections of the connector 43 are sealed and connected by a seal. The turntable 42 drives the connector 43 to rotate to form an upward inclination from the heating tube 3 to the condensing tube 5. The angles between the heating tube 3 and the condensing tube 5 and the horizontal plane are acute. The heating tube 3 is arranged inside the heating furnace 2. Water is arranged inside the heating furnace 2. The water inside the heating furnace 2 is heated by a heating plate 1 arranged below. The heating plate 1 can adjust the heating temperature to adapt to perovskite solutions of different concentrations. The maximum adjustable temperature of the heating plate 1 is 100 degrees Celsius.

[0026] The mixer 4 is responsible for mixing and stirring the solution, the chassis 41 provides a stable working environment for the mixer, and the turntable 42 is connected to the heating tube 3 and the condensing tube 5 through the connector 43. The turntable 42 can adjust the angle of the connector 43 to control the inclination angle of the heating tube 3 and the condensing tube 5, forming a complete solution processing process. A water bath is provided inside the heating furnace 2, which is heated by the heating plate 1. This water bath heating method can make the heating more uniform and avoid local overheating from causing adverse effects on the solution. The temperature of the heating plate 1 can be adjusted according to the concentration of the perovskite solution, up to 100 degrees Celsius, meeting the needs of different crystallization conditions.

[0027] See also Figure 1-3 A supporting member is provided above the heating furnace 2 to limit and clamp the heating test tube 3. The heating test tube 3 includes a crystallization chamber 31. Most of the crystallization chamber 31 is arranged underwater inside the heating furnace 2. An extension tube 32 is fixedly connected to the outer wall of the crystallization chamber 31. The crystallization chamber 31 is movably installed inside the clamping member above the heating furnace 2. A reflux chamber 33 is provided on the outer wall of the extension tube 32. The extension tube 32 extends inside the reflux chamber 33. A connecting tube 34 is provided on the outer wall of the reflux chamber 33. The connecting tube 34 is arranged inside the connecting head 43.

[0028] The support member arranged above the heating furnace 2 is to limit and clamp the heating test tube 3 to ensure its stability during the heating process. The design of the support member not only ensures the fixation of the heating test tube 3, but also allows it to be fine-tuned or replaced when necessary to adapt to different experimental needs. The heating test tube 3 is the core part of the crystallization process, and the crystallization chamber 31 therein is the main place for the crystallization of the perovskite solution. Most of the crystallization chamber 31 is arranged underwater inside the heating furnace 2, so that it can ensure that the solution is heated evenly and stably, which is conducive to the formation of single crystals. The reflux chamber 33 is located on the outer wall of the extension tube 32, and its function is to collect and guide part of the liquid in the solution to reflux, and the extension tube 32 extends and protrudes inside the reflux chamber 33 to prevent the solution inside the reflux chamber 33 from flowing into the crystallization chamber 31.

[0029] See also Figure 2 , Figure 4 The condensation test tube 5 includes an adapter 51, which is arranged inside the connecting head 43. The outer wall of the adapter 51 is fixedly connected to a steam chamber 52. A condensation chamber 53 is opened above the steam chamber 52. A spiral condensation tube 54 is arranged inside the condensation chamber 53. Condensate is arranged inside the condensation tube 54. A pressure chamber 55 is opened on the outer wall of the steam chamber 52. A solvent tank 56 is opened below the steam chamber 52.

[0030] The adapter 51 is arranged inside the connector 43, and serves to connect the condensation tube 5 and the heating tube 3. Its design ensures that the steam can be smoothly transferred from the heating tube 3 to the condensation tube 5, while maintaining the sealing of the entire system. The steam chamber 52 is located on the outer wall of the adapter 51, and its main function is to receive the steam rising from the heating tube 3. The steam gathers in the steam chamber 52, providing the necessary conditions for the subsequent condensation process. The condensation chamber 53 is located above the steam chamber 52, and a spiral condensation tube 54 is arranged inside. The condensation tube 54 is filled with condensate. When the steam enters the condensation chamber 53, it contacts the condensate in the condensation tube 54, thereby realizing the condensation of the steam. This spiral design increases the condensation area and improves the condensation efficiency. The outer wall of the steam chamber 52 opens a pressure chamber 55. The pressure chamber 55 can monitor the pressure changes in the steam chamber 52 to ensure the stability of the pressure of the steam during the condensation process. This is very important for controlling the condensation speed and effect.

[0031] Working principle: First, the constituent elements of perovskite are dissolved in a suitable solvent according to a specific molar ratio to prepare a solution. The solution is introduced into the crystallization chamber 31 below the heating test tube 3. The heating plate 1 heats the water in the heating furnace 2. During the heating process, the temperature and concentration of the solution are precisely regulated to promote the crystallization of perovskite crystals. The perovskite solution inside the crystallization chamber 31 is heated by the heat of water. This water bath heating method can make the heating more uniform and avoid local overheating from causing adverse effects on the solution. During the heating process, the heating test tube 3 is driven to rotate by the built-in motor of the connector 43. The crystallization chamber 31 rotates in the water to make the whole body more uniformly heated. Under appropriate conditions, atoms or ions will gather in the solution to form tiny crystal nuclei. These crystal nuclei are the starting points of new crystals. Subsequently, the crystal nuclei will grow further, adsorb the solute in the solution, and gradually form large crystals. During the crystal growth process, the shape and size of the crystal can be adjusted by controlling the crystallization conditions, and by continuously heating the perovskite solution, most of the water in the solution will produce steam. Since the heating test tube 3 is connected to the condensation test tube 5 through the connector 43 to form an upward tilt, since the density of the steam is lower than that of the surrounding cold air, the steam molecules will be subjected to an upward force in the space, and through the inclined setting, the steam is more convenient to enter the steam chamber 52. After the steam gathers in the steam chamber 52, it floats to the upper condensation chamber 53. The steam is cooled by the spiral condenser tube for heat exchange, so that the steam is converted into condensed water and falls into the solvent tank below by gravity. Some solvent flows into the reflux chamber 33 from the adapter 51. The reflux chamber 33 effectively prevents the refluxed solvent from entering the crystallization chamber 31 through the extension setting of the internal extension tube 32, thereby ensuring the stability of the heating temperature in the crystallization chamber 31. Finally, after a certain period of time, most of the solutes in the solution are adsorbed by the crystals to form relatively pure perovskite crystals, and the solvent with a lower concentration after evaporation can be recycled.

[0032] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device. In the absence of further restrictions, the elements defined by the sentence "comprise a ..." do not exclude the existence of other identical elements in the process, method, article or device including the elements.

[0033] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A perovskite single crystal crystallization device, comprising a mixer (4), characterized in that: The mixer (4) comprises a chassis (41), the outer wall of the chassis (41) being provided with a turntable (42), the outer wall of the turntable (42) being fixedly connected with a connector (43), the connector (43) being respectively connected to the heating test tube (3) and the condensing test tube (5), the interior of the connector (43) being divided into two sections, the section of the connector (43) connected to the heating test tube (3) being able to drive the heating test tube (3) to rotate via a built-in motor, the other section of the connector (43) being unable to rotate, and the two sections of the connector (43) being sealed and connected via a sealing member; The heating test tube (3) is arranged inside the heating furnace (2), water is arranged inside the heating furnace (2), and the water inside the heating furnace (2) is heated by a heating plate (1) arranged below.

2. A perovskite single crystal crystallization device according to claim 1, characterized in that: The heating plate (1) can adjust the heating temperature to adapt to perovskite solutions of different concentrations, and the maximum adjustable temperature of the heating plate (1) is 100 degrees Celsius.

3. A perovskite single crystal crystallization device according to claim 1, characterized in that: A supporting member is provided above the heating furnace (2) to limit and clamp the heating test tube (3); the heating test tube (3) comprises a crystallization chamber (31); most of the crystallization chamber (31) is arranged underwater inside the heating furnace (2); an extension tube (32) is fixedly connected to the outer wall of the crystallization chamber (31); and the crystallization chamber (31) is movably installed inside the clamping member above the heating furnace (2).

4. A perovskite single crystal crystallization device according to claim 3, characterized in that: The outer wall of the extension tube (32) is provided with a reflux chamber (33), the extension tube (32) extends into the reflux chamber (33), the outer wall of the reflux chamber (33) is provided with a connecting tube (34), and the connecting tube (34) is arranged inside the connecting head (43).

5. The perovskite single crystal crystallization device according to claim 1, characterized in that: The condensation test tube (5) comprises an adapter (51), the adapter (51) being arranged inside the connector (43), the outer wall of the adapter (51) being fixedly connected to a steam chamber (52), a condensation chamber (53) being provided above the steam chamber (52), a spiral condensation tube (54) being provided inside the condensation chamber (53), and condensate being provided inside the condensation tube (54).

6. A perovskite single crystal crystallization device according to claim 5, characterized in that: A pressure chamber (55) is provided on the outer wall of the steam chamber (52), and a solvent tank (56) is provided below the steam chamber (52).

7. A perovskite single crystal crystallization device according to claim 1, characterized in that: The rotating disk (42) drives the connecting head (43) to rotate so that the heating test tube (3) and the condensing test tube (5) are tilted upward, and the angle between the heating test tube (3) and the condensing test tube (5) and the horizontal plane is an acute angle.

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