Anti-solvent vapor assisted crystallization method single crystal growth device

Abstract

The utility model belongs to the technical field of crystal growth, specifically disclose a kind of anti-solvent vapor assisted crystallization method single crystal growth device, including container, inner container, heating tube group and gas pipe group. The inside of container has two parallel distribution cavities. Two inner containers are respectively one-to-one corresponding to be arranged in two cavities and constitute two placing cavities, and two placing cavities are communicated by connecting pipe. Heating tube group includes two distribution heating tubes in placing cavity, and two ends of heating tube are through container for with external heat source equipment constitutes heat supply circuit. Gas pipe group includes first gas pipe and second gas pipe, and first gas pipe is used to be connected with external inert gas source, and external inert gas source is used to provide inert gas to first gas pipe. The utility model can flexibly adjust the growth temperature of single crystal and the volatilization speed of anti-solvent vapor according to the growth condition of single crystal, so as to ensure that single crystal grows under the best growth condition.

Description

Technical Field

[0001] This invention belongs to the field of crystal growth technology, and specifically relates to a single crystal growth apparatus for antisolvent vapor-assisted crystallization. Background Technology

[0002] Antisolvent vapor-assisted crystallization is one of the most common methods for preparing metal halide single crystals.

[0003] The antisolvent vapor-assisted crystallization method requires auxiliary equipment. The traditional auxiliary equipment is a combination of a "large bottle inside a small bottle" and a heating device. That is, a large bottle contains a small bottle and the large bottle is heated by the heating device. The small bottle is used to hold the precursor solution, and the large bottle is used to hold the antisolvent, so as to achieve crystallization at the optimal growth temperature of single crystal.

[0004] However, because the auxiliary equipment is designed with the small vial inside the large vial, the temperature environment of the small vial and the large vial is the same. This results in the precursor solution in the small vial and the antisolvent in the large vial being heated at essentially the same temperature. Since the evaporation temperature of the antisolvent is different from the optimal growth temperature of the single crystal, it is impossible to simultaneously satisfy both the temperature environment and the evaporation temperature of the antisolvent and the optimal growth temperature of the single crystal, thus leading to low production efficiency. Utility Model Content

[0005] To address the aforementioned problems, the purpose of this invention is to provide a single crystal growth apparatus for antisolvent vapor-assisted crystallization.

[0006] The technical solution of this utility model is: a single crystal growth apparatus for antisolvent vapor-assisted crystallization, comprising a container, an inner liner, a heating tube assembly, and a gas supply pipe assembly. The container has two parallel cavities inside. There are two inner liners, each corresponding to one of the two cavities to form two placement chambers. One placement chamber is used to hold the antisolvent, and the other is used to hold the precursor solution. The two placement chambers are connected by a connecting pipe. The heating tube assembly includes two heating tubes corresponding to each of the two placement chambers. The middle section of the heating tube is embedded in the inner liner, and both ends of the heating tube penetrate the container to form a heating circuit with an external heat source device, which provides a heat medium to the heating tube. The gas supply pipe assembly includes a first gas supply pipe and a second gas supply pipe. A first gas delivery pipe is installed on the placement chamber for the antisolvent, with its inlet end located outside the placement chamber and its outlet end located inside the placement chamber. A first valve is installed on the inlet end of the first gas delivery pipe. The first gas delivery pipe is used to connect to an external inert gas source, which supplies inert gas to the first gas delivery pipe. A second gas delivery pipe is installed on the placement chamber for the precursor solution, with its inlet end located inside the placement chamber and its outlet end located outside the placement chamber. A second valve is installed on the outlet end of the second gas delivery pipe.

[0007] Furthermore, it also includes a heat insulation layer that wraps around the outside of the two cavities.

[0008] Furthermore, the insulation layer is made of asbestos.

[0009] Furthermore, the inner liner is made of polytetrafluoroethylene.

[0010] Furthermore, the inlet end of the connecting tube is located above the placement chamber where the antisolvent is placed, and the outlet end of the connecting tube is located above another placement chamber. The connecting tube is used to connect the upper interiors of the two placement chambers.

[0011] Furthermore, the connecting pipe is made of glass.

[0012] Furthermore, the outlet end of the first gas supply pipe is located inside the placement cavity at the bottom.

[0013] Furthermore, the heat transfer medium is water.

[0014] Compared with the prior art, the beneficial effects of this utility model are as follows: This utility model is based on two different placement chambers connected by a connecting pipe, which can establish different temperature environments in the two placement chambers. One placement chamber is used to place the antisolvent, and the other placement chamber is used to place the precursor solution. This realizes the separation of the antisolvent and the precursor solution in terms of temperature control. The growth temperature of the single crystal and the evaporation rate of the antisolvent vapor can be flexibly adjusted according to the growth of the single crystal, thereby ensuring that the single crystal grows under the optimal growth conditions and effectively improving the production efficiency of the single crystal. Attached Figure Description

[0015] Figure 1 This is a schematic diagram of the structure of this utility model.

[0016] Among them, 1-container, 10-cavity, 11-connecting pipe, 2-inner liner, 3-heating tube assembly, 30-heating tube, 4-gas supply pipe assembly, 41-first gas supply pipe, 410-first valve, 42-second gas supply pipe, 420-second valve, 5-insulation layer. Detailed Implementation

[0017] The following is combined with Figure 1 The specific embodiments of this utility model will be described in detail below. In the description of this utility model, it should be understood that the terms "center", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc., indicating the orientation or positional relationship are based on the orientation or positional relationship shown in the accompanying drawings, and are only for the convenience of describing this utility model and 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, and therefore should not be construed as a limitation of this utility model.

[0018] The terms "first" and "second" 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. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature; in the description of this utility model, unless otherwise stated, "a plurality of" means two or more.

[0019] Traditional auxiliary equipment uses a combination of a large bottle containing a smaller bottle, along with a heating device. When using this equipment for antisolvent vapor-assisted crystallization, the antisolvent evaporation rate depends on the single crystal growth temperature, and the supersaturation of the precursor solution cannot be independently controlled. When the optimal growth temperature of the single crystal is high, the antisolvent evaporation and intrusion into the precursor solution are too rapid, leading to a rapid increase in the supersaturation of the precursor solution and a surge in the number of single crystal nuclei. However, the solute in the precursor solution is limited, and the growth potential of the single crystal cannot be fully realized. When the optimal growth temperature of the single crystal is low, the antisolvent diffusion rate is very slow, prolonging the single crystal growth time and reducing production efficiency.

[0020] It should be noted that the circuit connections involved in this utility model are all conventional circuit connection methods and do not involve any innovation.

[0021] Example like Figure 1 The apparatus shown is a single crystal growth device using an antisolvent vapor-assisted crystallization method, comprising: a container 1, an inner liner 2, a heating tube assembly 3, and a gas supply pipe assembly 4. The container 1 has two parallel cavities 10 inside. There are two inner liners 2, each corresponding to one of the two cavities 10, forming two placement chambers. One placement chamber is used to hold the antisolvent, and the other is used to hold the precursor solution. The two placement chambers are connected by a connecting pipe 11. The heating tube assembly 3 includes two heating tubes 30 corresponding to each other in the two placement chambers. The middle section of the heating tube 30 is embedded in the inner liner 2, and both ends of the heating tube 30 penetrate the container 1 to form a heating circuit with an external heat source device, which provides a heat medium to the heating tube 30. The gas supply pipe assembly 4 includes a first gas supply pipe 41 and a second gas supply pipe 42. A first gas supply pipe 41 is installed on the placement chamber for the antisolvent. The inlet end of the first gas supply pipe 41 is located outside the placement chamber, and the outlet end of the first gas supply pipe 41 is located inside the placement chamber. A first valve 410 is installed on the inlet end of the first gas supply pipe 41. The first gas supply pipe 41 is used to connect to an external inert gas source, which provides inert gas to the first gas supply pipe 41. A second gas supply pipe 42 is installed on the placement chamber for the precursor solution. The inlet end of the second gas supply pipe 42 is located inside the placement chamber, and the outlet end of the second gas supply pipe 42 is located outside the placement chamber. A second valve 420 is installed on the outlet end of the second gas supply pipe 42.

[0022] Preferably, it also includes a heat insulation layer 5, which wraps around the outside of the two cavities 10.

[0023] Preferably, the insulation layer 5 is made of asbestos.

[0024] Preferably, the inner liner 2 is made of polytetrafluoroethylene.

[0025] Preferably, the inlet end of the connecting tube 11 is located above the placement chamber where the antisolvent is placed, and the outlet end of the connecting tube 11 is located above another placement chamber. The connecting tube 11 is used to connect the upper interior of the two placement chambers.

[0026] Preferably, the connecting pipe 11 is made of glass.

[0027] Preferably, the first gas supply pipe 41 has an L-shaped structure, and the outlet end of the first gas supply pipe 41 is located inside the lower part of the placement cavity.

[0028] Preferably, the heat transfer medium is water or dimethyl silicone oil, and water is preferred in this embodiment.

[0029] Preferably, the inert gas is nitrogen or argon, and in this embodiment, argon is preferred.

[0030] Preferably, the heating element 30 is made of stainless steel, and the first valve 410 and the second valve 420 are both stainless steel gas flow valves.

[0031] Preferably, the system also includes a temperature monitoring system and a control system. The temperature monitoring system includes thermocouple temperature probes and a temperature conversion device. There are two thermocouple temperature probes, one-to-one installed in two corresponding cavities 10, used to convert the temperature data within the cavities 10 into electrical signals. The temperature conversion device is electrically connected to the thermocouple temperature probes and is used to convert the electrical signals into temperature data. The control system is used to connect to an external heat source device. The heating rod is used to heat the heat medium. The control system is electrically connected to the heating rod and the temperature conversion device respectively. The temperature conversion device transmits the actual temperature data to the control system, and the control system interacts with the external heat source device, which controls the temperature of the heat medium. In this embodiment, the thermocouple temperature probe uses a WRGKK-100-3-120 thermocouple, the temperature conversion device uses an E5CC-RX2ASM-800 temperature controller, and the control system uses a PIC18F45K22 microcontroller. The external heat source device is a container with a heating rod, which is connected to the heating tube 30 via a pump body. The heating rod is connected to the control system. It should be noted that the temperature monitoring system and control system can be selectively adapted according to actual needs, and the specific model is not limited.

[0032] The working method of the above embodiment is as follows: First, the antisolvent is placed in a placement cavity with a first gas supply pipe 41, wherein the first gas supply pipe 41 has an L-shaped structure; the precursor solution is placed in another placement cavity.

[0033] The two placement chambers are heated by introducing a heat medium into the heating tube 30, and the different temperatures of the two placement chambers are achieved by controlling the flow rate of the heat medium in the two heating tubes 30.

[0034] An inert gas is introduced into the placement chamber containing the antisolvent via the first gas supply pipe 41. The antisolvent is heated and vaporized, and the vaporized antisolvent is carried by the inert gas through the connecting pipe 11 into another placement chamber. The flow rate of the vaporized antisolvent gas is controlled by the flow rate of the inert gas.

[0035] The single crystal growth temperature is maintained at an optimal level by a temperature monitoring and control system. At this temperature, due to the intrusion of the antisolvent gas, the solubility of the mixed solvent in the precursor solution gradually decreases, and the supersaturation of the solution increases, thereby promoting the nucleation and growth of the solute single crystal. During this process, the inert carrier gas can prevent the oxidation of metal ions in the single crystal growth chamber, ensuring the continuous and stable progress of the single crystal growth process.

[0036] The specific models of the above electronic components are not specifically specified; any commercially available ordinary products can be selected, as long as they meet the usage requirements of this utility model.

[0037] The specific embodiments described above further illustrate the purpose, technical solution, and beneficial effects of this utility model. It should be understood that the above description is only a specific embodiment of this utility model and does not limit this utility model. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of this utility model are included within the protection scope of this utility model.

Claims

1. A single crystal growth apparatus for anti-solvent vapor-assisted crystallization, characterized in that, include: The container (1) has two parallel cavities (10) inside. There are two inner liner (2), and the two inner liner (2) are respectively set in the two cavities (10) to form two placement cavities. One placement cavity is used to place the antisolvent, and the other placement cavity is used to place the precursor solution. The two placement cavities are connected by a connecting pipe (11). The heating tube assembly (3) includes two heating tubes (30) that are distributed one-to-one in the two placement cavities. The middle section of the heating tube (30) is embedded in the inner liner (2). The two ends of the heating tube (30) pass through the container (1) to form a heating circuit with the external heat source equipment. The external heat source equipment is used to provide heat medium to the heating tube (30). The gas delivery pipe assembly (4) includes: a first gas delivery pipe (41), which is disposed on the placement chamber for placing the antisolvent, with the inlet end of the first gas delivery pipe (41) located outside the placement chamber and the outlet end of the first gas delivery pipe (41) located inside the placement chamber; a first valve (410) is provided on the inlet end of the first gas delivery pipe (41); the first gas delivery pipe (41) is used to connect to an external inert gas source, which is used to supply inert gas to the first gas delivery pipe (41); a second gas delivery pipe (42), which is disposed on the placement chamber for placing the precursor solution, with the inlet end of the second gas delivery pipe (42) located inside the placement chamber and the outlet end of the second gas delivery pipe (42) located outside the placement chamber; a second valve (420) is provided on the outlet end of the second gas delivery pipe (42).

2. The anti-solvent vapor-assisted crystallization single crystal growth apparatus as described in claim 1, characterized in that, It also includes a heat insulation layer (5), which wraps around the outside of the two cavities (10).

3. The anti-solvent vapor-assisted crystallization single crystal growth apparatus as described in claim 2, characterized in that, The insulation layer (5) is made of asbestos.

4. The anti-solvent vapor-assisted crystallization single crystal growth apparatus as described in claim 1, characterized in that, The inner liner (2) is made of polytetrafluoroethylene.

5. The anti-solvent vapor-assisted crystallization single crystal growth apparatus as described in claim 1, characterized in that, The inlet end of the connecting tube (11) is located above the placement chamber where the antisolvent is placed, and the outlet end of the connecting tube (11) is located above another placement chamber. The connecting tube (11) is used to connect the upper interior of the two placement chambers.

6. The anti-solvent vapor-assisted crystallization single crystal growth apparatus as described in claim 5, characterized in that, The connecting pipe (11) is made of glass.

7. The anti-solvent vapor-assisted crystallization single crystal growth apparatus as described in claim 1, characterized in that, The first gas supply pipe (41) has an L-shaped structure, and the outlet end of the first gas supply pipe (41) is located inside the lower part of the placement cavity.

8. The anti-solvent vapor-assisted crystallization single crystal growth apparatus as described in claim 1, characterized in that, The heat transfer medium is water.

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