Line heating equipment for perovskite material

Abstract

The utility model discloses a linear heating device for perovskite materials, which belongs to the technical field of perovskite material preparation and comprises a closed box body, a heating unit, a lifting platform, an infrared thermometer and a heating unit controller. According to the utility model, the closed box body is used for introducing inert protective gas, the lifting platform is provided with the working platform for placing the substrate, the temperature field is formed through the heating unit, the infrared thermometer is used for detecting the real-time temperature gradient in the temperature field, and the temperature field is driven to move slowly by utilizing the movement of the heating unit; the twin domain is driven to move in situ in the moving process, so that the crystal is normalized on the domain scale; the method can be used for the preparation process of various perovskite materials, is simple to operate and high in practicability, can improve the quality of crystals, and can be used for industrially obtaining high-quality perovskite crystals on a large scale.

Description

TECHNICAL FIELD

[0001] The utility model belongs to perovskite material preparation technical field, concretely relates to a kind of linear heating equipment applied to perovskite single crystal material. BACKGROUND

[0002] Perovskite materials are widely used in many fields, which is mainly due to the unique and excellent photoelectric properties of perovskite materials, such as high barrier ability, which is derived from its high atomic number elements and high mass density, efficient charge collection, high carrier mobility, long carrier lifetime and carrier diffusion length.

[0003] Material phase transition leads to lattice distortion, thereby generating spontaneous strain similar to spontaneous polarization in ferroelectric materials. This internal strain can be compensated by forming twin domains oriented along different crystal axes. These domains are formed during crystal growth due to alignment along different crystal axes, and the grain boundaries (twin boundaries) between two domains can affect the orientation of charge separation, transmission and recombination interface, which is due to the imperfect arrangement of atomic structure at the grain boundary, such as vacancies or other defects. Material phase transition inevitably produces large residual stress and forms many twin domains, which greatly limits the yield of high-quality crystals. Therefore, a linear heating device capable of obtaining domain normalized perovskite single crystal material is needed. SUMMARY

[0004] The utility model aims at overcoming that the prior art cannot obtain perovskite single crystal material with uniform domain size and low defect density, and provides a linear heating device for perovskite material.

[0005] The technical scheme adopted by the utility model is as follows:

[0006] A linear heating device for perovskite material, comprising: a sealed box body, a heating unit 1, a lifting platform 6, an infrared temperature measuring instrument 7 and a heating unit controller;

[0007] The heating unit 1 is connected by a plurality of heating devices, each heating device is connected with the heating unit controller, and the temperature of the heating device is detected in real time by the temperature sensor connected with the heating unit controller. At the same time, the heating temperature of each heating device is controlled by the heating unit controller, so that the heating unit 1 forms a temperature field with a specific temperature gradient around the set center temperature; in addition, the heating unit 1 is movably installed in the sealed box body;

[0008] The infrared temperature measuring instrument 7 is arranged above the heating unit 1, which is used to detect the temperature in the real-time temperature gradient field; the lifting platform 6 is arranged at the bottom of the sealed box body, and the upper part is provided with a working platform for placing the substrate; two air holes are formed on the shell of the sealed box body, which are used to introduce and exhaust the gas in the interior.

[0009] Preferably, the device further comprises a heating unit moving device, which is fixedly installed inside the closed box body; the heating unit moving device is connected with the heating unit 1 and is used for driving the heating unit 1 to move inside the closed box body.

[0010] Further preferably, the heating unit moving device comprises a screw nut pair and a servo motor, the heating unit 1 is connected with the screw nut 2, the screw rod 4 is installed on the side of the closed box body, the servo motor drives the screw rod 4 to rotate, and the screw nut 2 drives the heating unit 1 to move along the screw rod 4.

[0011] Further preferably, the heating unit moving device further comprises a light rod 5 and a sliding block 3, the light rod 5 is arranged in parallel with the screw rod 4 and is installed on the other side of the closed box body, the sliding block 3 is slidably installed on the light rod 5, and the sliding block 3 is connected with the heating unit 1.

[0012] Further preferably, the heating device is an electric heating coil, the electric heating coils are connected and arranged in parallel at equal intervals on the screw rod 4 and the light rod 5 of the heating unit moving device, and the electric heating coils at the ends are connected with the screw nut 2 and the sliding block 3.

[0013] Alternatively, the heating device is a heating rod, and the heating rod is connected with the screw nut 2 and the sliding block 3.

[0014] Preferably, the device further comprises a lifting platform moving device, which is fixedly installed inside the closed box body; the lifting platform moving device is connected with the lifting platform 6 and is used for driving the lifting platform 6 to move inside the closed box body.

[0015] The device has the advantages that:

[0016] The closed box body in the device is used for introducing inert protective gas, the lifting platform is provided with a working platform used for placing a substrate, a temperature field is formed by the heating unit, the infrared temperature detector 7 is used for detecting a real-time temperature gradient in the temperature field, the temperature field is driven to move slowly by the heating unit, and the movement of twin crystal domains is driven in situ during the movement, so that the crystal is normalized in the domain scale; the device can be used for the preparation process of various perovskite materials, has the advantages of simple operation and high practicability, can improve the quality of the crystal, and can be used for industrialized large-scale obtaining of high-quality perovskite crystals. BRIEF DESCRIPTION OF DRAWINGS

[0017] Figure 1 It is a schematic diagram of the linear heating device in Example 1;

[0018] Figure 2 It is a schematic diagram of the linear heating device in Example 2;

[0019] Figure 3This represents the gradient field formed under infrared thermal imaging.

[0020] Figure label:

[0021] 1 - Heating unit; 2 - Lead screw and nut; 3 - Slider; 4 - Lead screw; 5 - Optical bar; 6 - Lifting platform; 7 - Infrared thermometer. Detailed Implementation

[0022] The technical solution of this utility model is further illustrated below through specific embodiments.

[0023] Example 1

[0024] like Figure 1 As shown, the wire heating device for perovskite material in this embodiment includes: a sealed box, a heating unit 1, a heating unit moving device, a lifting platform 6, an infrared thermometer 7, and a heating unit controller;

[0025] The heating unit moving device is fixedly installed inside the sealed box; the heating unit moving device is connected to the heating unit 1 and is used to drive the heating unit 1 to move inside the sealed box; the heating unit 1 is composed of several heating devices connected together, each heating device is connected to the heating unit controller, and the temperature of the heating device is detected in real time by a temperature sensor connected to the heating unit controller. At the same time, the heating unit controller controls the heating temperature of each heating device individually, so that the heating unit 1 forms a temperature field with a specific temperature gradient according to the set center temperature and the surrounding area.

[0026] An infrared thermometer 7 is installed directly above the heating unit 1 to detect the temperature in the real-time temperature gradient field; the lifting platform 6 is located at the bottom of the sealed box, and a working platform for placing the base is installed on the top; the sealed box has two air holes on the shell, which are used to introduce and exhaust the internal gas respectively.

[0027] In this embodiment, the heating unit moving device includes a lead screw and nut pair, a servo motor, a guide bar 5, and a slider 3. The heating unit 1 is connected to the lead screw and nut 2. The lead screw 4 is installed on the side of the sealed box. The guide bar 5 is arranged parallel to the lead screw 4 and installed on the other side of the sealed box. The slider 3 is slidably installed on the guide bar 5 and is connected to the heating unit 1. The servo motor drives the lead screw 4 to rotate, and the lead screw and nut 2 drives the heating unit 1 to move along the plane formed by the lead screw 4 and the guide bar 5.

[0028] The heating device is composed of electric heating coils, which are interconnected and arranged side by side at equal intervals on the lead screw 4 and optical rod 5 of the heating unit moving device. The heating coils at the ends are connected to the lead screw nut 2 and the slider 3.

[0029] The lifting platform 6 is arranged at the bottom of the closed box body, and a working platform for placing a substrate is arranged at the upper portion; two air holes are formed in the shell of the closed box body, and are respectively used for introducing and discharging the gas in the closed box body.

[0030] Embodiment 2

[0031] As shown in the figure, the line heating device of the perovskite material in the embodiment comprises a closed box body, a heating unit 1, a heating unit moving device, a lifting platform 6, an infrared temperature measuring instrument 7 and a heating unit controller. Figure 2

[0032] The difference between the embodiment and the embodiment 1 is that the heating device is a heating rod, and the end of the heating rod is connected with the screw nut 2 and the sliding block 3.

[0033] The above embodiment is only a preferred embodiment of the utility model, in addition to the above embodiment, the heating unit moving device can also be composed of only the screw nut 2 pair and the servo motor, the heating unit 1 is connected with the screw nut 2, the screw rod 4 is installed in parallel on both sides of the closed box body, the servo motor drives the screw rod 4 to rotate, and the screw nut 2 drives the heating unit 1 to move along the plane formed by the two groups of screw rods 4.

[0034] In addition, the heating unit 1 can also be moved by manual operation, or the heating device can be fixedly installed in the closed box body and the slide rail is arranged at the bottom of the lifting platform 6, the lifting platform 6 is moved in the horizontal direction, or the corresponding driving device is arranged to drive the lifting platform 6 to move horizontally, and the same effect can be achieved.

[0035] The principle of the utility model will be described in combination with a specific experimental method, and the specific method is as follows:

[0036] Taking the tempering treatment of a methylamine lead iodine perovskite single crystal as an example, the tempering treatment method of the perovskite single crystal based on the equipment is as follows:

[0037] 1) A methylamine lead iodine perovskite precursor solution with a concentration of 1.5 mol·L -1 -1 is prepared, stirred at 70 DEG C for 4 h, and the glass substrate is preheated on a hot stage at 75 DEG C; the precursor solution is quickly injected into the middle of the two substrates; the temperature of the hot stage is gradually increased to 120 DEG C, and the growth is carried out for 10 h.

[0038] 2) The surface of the perovskite single crystal grown in step 1) is polished with silk, and the large particles and uneven impurities are removed to obtain a smooth and flat crystal surface.

[0039] 3) The methylamine lead iodine perovskite single crystal is placed on the working platform on the lifting platform 6, and the height is adjusted to make the crystal close to the heating unit.

[0040] ​4) High purity nitrogen is continuously injected into the sealed box through one gas hole, and air is discharged from another gas hole, so that a protective atmosphere is formed in the box to avoid material oxidation.

[0041] 5) Adjust the heating unit controller to control the temperature rise of the heating coil, and form a temperature field with gradient on both sides of the heated area, the center temperature of the temperature field is above the tetragonal-cubic phase transition temperature, and there is a temperature gradient of 20 Kcm -1 between the center temperature and the periphery;

[0042] 6) The heating coil is scanned over the perovskite single crystal at a speed of 300 μm s -1 , so that the temperature gradient field is scanned on the perovskite single crystal at the same speed, the perovskite single crystal is heated to above the tetragonal-cubic phase transition temperature, and the micro-stress generated by the phase transition drives the elimination of the perovskite single crystal domain wall in the slow movement of the temperature gradient field, completes the tempering treatment, and obtains a single crystal with uniform domain size.

Claims

1. A linear heating apparatus for perovskite material, characterized by, The device comprises a sealed box, a heating unit (1), a lifting platform (6), an infrared temperature detector (7) and a heating unit controller. The heating unit (1) is connected by several heating devices, each of which is connected to the heating unit controller and detects the temperature of the heating device in real time through the temperature sensor connected to the heating unit controller. Meanwhile, the heating temperature of each heating device is controlled by the heating unit controller, so that the heating unit (1) forms a temperature field with a specific temperature gradient around the center temperature. In addition, the heating unit (1) is movably installed in the sealed box. The infrared temperature detector (7) is arranged above the heating unit (1) to detect the temperature in the real-time temperature gradient field. The lifting platform (6) is arranged at the bottom of the sealed box and has a working platform at the upper part for placing the substrate. Two air holes are formed on the shell of the sealed box for introducing and discharging the gas inside.

2. The linear heating apparatus for perovskite material according to claim 1, characterized by, The device further comprises a heating unit moving device, which is fixedly installed in the sealed box. The heating unit moving device is connected to the heating unit (1) to drive the heating unit (1) to move inside the sealed box.

3. The linear heating apparatus for perovskite material according to claim 2, characterized by, The heating unit moving device comprises a screw nut pair and a servo motor. The heating unit (1) is connected to the screw nut (2), the screw rod (4) is installed on the side of the sealed box, the servo motor drives the screw rod (4) to rotate, and the screw nut (2) drives the heating unit (1) to move along the screw rod (4).

4. The linear heating apparatus for perovskite material according to claim 3, characterized by, The heating unit moving device further comprises a light rod (5) and a sliding block (3). The light rod (5) is arranged in parallel with the screw rod (4) and is installed on the other side of the sealed box. The sliding block (3) is slidably installed on the light rod (5) and is connected to the heating unit (1).

5. The linear heating apparatus for perovskite material according to claim 4, characterized by, The heating device is an electric heating coil. The electric heating coils are connected and arranged in parallel on the screw rod (4) and the light rod (5) of the heating unit moving device at equal intervals. The end electric heating coils are connected to the screw nut (2) and the sliding block (3).

6. The linear heating apparatus for perovskite material according to claim 4, characterized by, The heating device is a heating rod, which is connected to the screw nut (2) and the sliding block (3).

7. The linear heating apparatus for perovskite material according to claim 1, characterized by, The heating unit (1) is fixedly installed in the sealed box, and the lifting platform (6) is provided with a sliding rail below to enable the lifting platform (6) to move horizontally.

8. The linear heating apparatus for perovskite material according to claim 7, characterized by, The device further comprises a lifting platform moving device, which is fixedly installed in the sealed box. The lifting platform moving device is connected to the lifting platform (6) to drive the lifting platform (6) to move inside the sealed box.

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