Crystal growth raw material treatment equipment

Abstract

The utility model discloses crystal growth raw material treatment equipment and relates to the field of raw material treatment. The crystal growth raw material processing equipment comprises an electric heating furnace; the quartz tube is placed in the electric heating furnace, and the two ends of the quartz tube extend out of the electric heating furnace; an air inlet and an air outlet are respectively formed in two ends of the quartz tube; the air inlet vacuum valve is mounted at the air inlet of the quartz tube; the electric heating furnace, the quartz tube, the gas inlet vacuum valve, the gas exhaust vacuum valve, the gas extraction vacuum valve, the vacuum pump, the protective gas conveying tank and other components are matched for use, so that moisture and oxygen can be fully discharged from the rare earth halide when the rare earth halide is subjected to dehumidification and deoxygenation operation; the water oxygen content of the treated rare earth halide is smaller than 50 ppm, the risk that materials go bad is reduced, and the requirement for preparing single crystals is met.

Description

Technical Field

[0001] The utility model belongs to the technical field of raw material processing, and in particular relates to a crystal growth raw material processing device. Background Art

[0002] Rare earth halides are very important chemical raw materials and are widely used in catalysis, luminescence, functional materials and other fields. In particular, anhydrous and oxygen-free rare earth halides are important raw materials for the manufacture of scintillation crystals. However, due to their strong hygroscopicity and easy oxidation, rare earth halides are prone to material deterioration during storage, which may result in failure to produce qualified crystal materials. Therefore, before use, the water vapor and oxygen inside the rare earth halide raw materials need to be removed before crystal growth can be carried out.

[0003] In order to ensure that the rare earth halide raw materials after dehumidification and deoxygenation can meet the usage standards, technical personnel in this field have designed a crystal growth raw material processing equipment to perform sufficient dehumidification and deoxygenation operations on it, so that the water and oxygen content of the rare earth halide after treatment can be less than 50ppm, meeting the requirements for preparing single crystals. Utility Model Content

[0004] The technical problem to be solved by the utility model is to overcome the deficiencies of the prior art and provide a crystal growth raw material processing device which can overcome the above problems or at least partially solve the above problems.

[0005] In order to solve the above technical problems, the basic concept of the technical solution adopted by the utility model is: a crystal growth raw material processing equipment, including: an electric heating furnace; a quartz tube, placed in the electric heating furnace, and both ends of the electric heating furnace are extended out of the electric heating furnace; the two ends of the quartz tube are respectively provided with an air inlet and an air outlet; an air inlet vacuum valve, installed at the air inlet of the quartz tube; an exhaust vacuum valve, installed at the air outlet of the quartz tube; an exhaust port is opened on the side of the quartz tube close to the air outlet; an exhaust vacuum valve, installed at the exhaust port of the quartz tube; a vacuum pump, the exhaust port is connected to the exhaust port of the quartz tube; a protective gas delivery tank, installed on the side close to the air inlet of the quartz tube, and the gas delivery port is connected to the air inlet of the quartz tube.

[0006] Furthermore, the electric heating furnace includes a lower shell, an upper shell, a resistance wire type heating element and a temperature gauge. The lower shell and the upper shell are rotatably connected via a rotating shaft. The resistance wire of the resistance wire type heating element is spirally arranged in a cavity formed by the lower shell and the upper shell. The controller of the resistance wire type heating element is installed on the lower side of the lower shell. The temperature gauge is installed on the upper shell, and the detection end extends into the cavity formed by the lower shell and the upper shell.

[0007] In order to facilitate heating of the crystal growth raw materials at different temperatures, further, the heating range of the resistance wire type heating element is 50-900°C.

[0008] In order to improve the high stability of the quartz tube, further, the purity of the quartz tube is greater than 99.99%.

[0009] In order to ensure the stability of the use of the intake vacuum valve, the exhaust vacuum valve and the exhaust vacuum valve, the intake vacuum valve, the exhaust vacuum valve and the exhaust vacuum valve are all designed to have a limit pressure of less than 5×10 -5 Pa vacuum valve.

[0010] In order to facilitate the recycling and reuse of the protective gas, further, the gas outlet of the quartz tube is connected to a recovery tank, and a gas dehumidification and deoxygenation device is installed above the protective gas delivery tank. The gas suction port of the gas dehumidification and deoxygenation device is connected to the gas outlet of the recovery tank through a delivery pipe, and the gas outlet of the dehumidification and deoxygenation device is connected to the recovery port of the protective gas delivery tank. The delivery pipe is a three-way pipe, and the other air inlet end of the delivery pipe is connected to the air outlet end of the vacuum pump.

[0011] After adopting the above technical scheme, the utility model has the following beneficial effects compared with the prior art: the utility model uses an electric heating furnace, a quartz tube, an air intake vacuum valve, an exhaust vacuum valve, an exhaust vacuum valve, a vacuum pump, a protective gas delivery tank and other components in coordination, and when dehumidifying and deoxygenating rare earth halides, moisture and oxygen can be discharged more fully from the rare earth halides, so that the water and oxygen content of the rare earth halides after treatment is less than 50ppm, reducing the risk of material deterioration and meeting the requirements for preparing single crystals.

[0012] The specific implementation of the utility model is further described in detail below with reference to the accompanying drawings. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] In the attached picture:

[0014] Figure 1 This is a schematic diagram of the structure of a crystal growth raw material processing device proposed by the utility model Figure 1 ;

[0015] Figure 2 This is a schematic diagram of the structure of a crystal growth raw material processing device proposed by the utility model Figure 2 ;

[0016] Figure 3 The utility model is a schematic structural diagram of a crystal growth raw material processing device when the upper shell is opened.

[0017] In the figure: 1. electric heating furnace; 101. lower shell; 102. upper shell; 103. resistance wire heating element; 104. thermometer; 2. quartz tube; 201. air inlet vacuum valve; 202. exhaust vacuum valve; 203. exhaust vacuum valve; 204. vacuum pump; 3. protective gas delivery tank; 301. recovery tank; 302. gas dehumidification and deoxygenation equipment; 303. delivery pipe. DETAILED DESCRIPTION

[0018] In order to make the purpose, technical solutions and advantages of the embodiments of the utility model clearer, the technical solutions in the embodiments will be clearly and completely described below in conjunction with the drawings in the embodiments of the utility model. The following embodiments are used to illustrate the utility model but are not used to limit the scope of the utility model.

[0019] Embodiment 1:

[0020] Reference Figure 1-Figure 3 A crystal growth raw material processing equipment includes: an electric heating furnace 1; a quartz tube 2, which is placed in the electric heating furnace 1 and has both ends extending out of the electric heating furnace 1; an air inlet and an air outlet are respectively provided at both ends of the quartz tube 2; an air inlet vacuum valve 201 is installed at the air inlet of the quartz tube 2; an exhaust vacuum valve 202 is installed at the air outlet of the quartz tube 2; an exhaust port is provided on the side of the quartz tube 2 close to the air outlet; an exhaust vacuum valve 203 is installed at the exhaust port of the quartz tube 2; a vacuum pump 204, whose exhaust port is connected to the exhaust port of the quartz tube 2; a protective gas delivery tank 3 is installed on the side close to the air inlet of the quartz tube 2, and the gas delivery port is connected to the air inlet of the quartz tube 2.

[0021] The electric heating furnace 1 includes a lower shell 101, an upper shell 102, a resistance wire heating element 103 and a temperature gauge 104. The lower shell 101 and the upper shell 102 are rotatably connected via a rotating shaft. The resistance wire of the resistance wire heating element 103 is spirally arranged in a cavity formed by the lower shell 101 and the upper shell 102. The controller of the resistance wire heating element 103 is installed on the lower side of the lower shell 101. The temperature gauge 104 is installed on the upper shell 102, and the detection end extends into the cavity formed by the lower shell 101 and the upper shell 102.

[0022] When it is necessary to dehumidify and deoxygenate the rare earth halide raw material of the scintillation crystal, the staff first fills the rare earth halide into the quartz tube 2, then opens the upper shell 102, places the quartz tube 2 into the spirally arranged resistance wire, and then respectively connects the air inlet vacuum valve 201, the exhaust vacuum valve 202 and the exhaust vacuum valve 203 at the air inlet, exhaust port and exhaust port of the quartz tube 2, and then respectively connects the protective gas delivery tank 3 and the vacuum pump 204 to the air inlet and exhaust port of the quartz tube 2, and finally covers the upper shell 102, and connects the electrical equipment to the power supply before it can be put into use.

[0023] Among them, the protective gas stored in the protective gas delivery tank 3 can be argon or nitrogen (both nitrogen and argon can be used as protective gases. Although argon has a better protective effect, the cost of using argon is higher. Although the protective effect of nitrogen is weaker than that of argon, nitrogen is cheaper. Therefore, when using, the manufacturer can choose one of them as the protective gas according to demand).

[0024] When argon is used as the protective gas, the staff first opens the air intake vacuum valve 201 and the exhaust vacuum valve 202, and closes the exhaust vacuum valve 203, and then uses the protective gas delivery tank 3 to pass argon with a purity greater than 99.999% into the quartz tube 2 at a speed of 10L / min, and maintains it for 30 minutes. When the water vapor and oxygen filled in the quartz tube 2 are taken away by the argon, and there is a lot of argon in the quartz tube 2 to wrap the rare earth halide, the staff can raise the temperature in the electric heating furnace 1 to 280°C at a heating rate of 5°C / min by observing the thermometer 104, and maintain it for 3 hours. In the process of heating, the moisture and oxygen in the rare earth halide can be precipitated. When the heating is completed, the electric heating furnace 1, the air intake vacuum valve 201, the exhaust vacuum valve 202 can be closed, and the vacuum pump 204 can be started, and the exhaust vacuum valve 203 can be opened until the pressure inside the quartz tube 2 is evacuated to 5×10 -5 Pa, and finally close the vacuum pump 204 and the vacuum valve 203 to complete the dehumidification and deoxygenation process of the rare earth halide.

[0025] When nitrogen is used as the protective gas, the staff first opens the air intake vacuum valve 201 and the exhaust vacuum valve 202, and closes the exhaust vacuum valve 203, and then uses the protective gas delivery tank 3 to pass nitrogen with a purity greater than 99.99% into the quartz tube 2 at a rate of 5L / min, and maintains it for 1 hour. When the water vapor and oxygen filled in the quartz tube 2 are taken away by the argon gas, and there is a lot of argon gas in the quartz tube 2 to wrap the rare earth halide, the staff can raise the temperature of the electric heating furnace 1 to 500℃ at a heating rate of 5℃ / min by observing the thermometer 104, and maintain it for 1 hour. In the process of heating, the moisture and oxygen in the rare earth halide can be precipitated. When the heating is completed, the electric heating furnace 1, the air intake vacuum valve 201, the exhaust vacuum valve 202 can be closed, and the vacuum pump 204 can be started, and the exhaust vacuum valve 203 can be opened until the pressure inside the quartz tube 2 is evacuated to 5×10 -5 Pa, and finally close the vacuum pump 204 and the vacuum valve 203 to complete the dehumidification and deoxygenation process of the rare earth halide.

[0026] Embodiment 2:

[0027] Reference Figure 1-Figure 3, a crystal growth raw material processing equipment, is basically the same as Example 1, and further: the heating range of the resistance wire heating element 103 is 50-900°C. By increasing the heating range of the resistance wire heating element 103, the crystal growth raw material can be heated at different temperatures according to different protective gases, which effectively improves the applicability of the equipment.

[0028] The purity of the quartz tube 2 is greater than 99.99%, and the diameter is 50-100mm, the length is 100-1200mm, and the wall thickness is 1-5mm. By making the quartz tube 2 made of quartz stone with higher purity, the hardness, fire resistance and flame retardancy of the quartz tube 2 can be guaranteed, and the high stability of the quartz tube 2 during use is effectively guaranteed.

[0029] The intake vacuum valve 201, the exhaust vacuum valve 202 and the exhaust vacuum valve 203 all have a limit pressure of less than 5×10 -5 The vacuum valve of Pa can prevent the vacuum pump 204 from pumping the pressure inside the quartz tube 2 to 5×10 -5 Pa, the intake vacuum valve 201, the exhaust vacuum valve 202 and the exhaust vacuum valve 203 will not be damaged or conductive due to the large negative pressure value, which effectively ensures the stability of the use of the intake vacuum valve 201, the exhaust vacuum valve 202 and the exhaust vacuum valve 203.

[0030] Embodiment 3:

[0031] Reference Figure 1-Figure 3 , a crystal growth raw material processing equipment, which is basically the same as Example 2, and further: the gas outlet of the quartz tube 2 is connected to a recovery tank 301, and a gas dehumidification and deoxygenation device 302 is installed above the protective gas delivery tank 3, and the gas extraction port of the gas dehumidification and deoxygenation device is connected to the gas outlet of the recovery tank 301 through a delivery pipe 303, and the gas outlet of the dehumidification and deoxygenation device 302 is connected to the recovery port of the protective gas delivery tank 3, and the delivery pipe 303 is a three-way pipe, and the other air inlet end of the delivery pipe 303 is connected to the air outlet end of the vacuum pump 204. When the air inlet vacuum valve 201 and the exhaust vacuum valve 202 are opened to allow the protective gas to flow in the quartz tube 2, the stone is discharged at this time. The protective gas in the quartz tube 2 can be recovered into the recovery tank 301, and then the gas dehumidification and deoxygenation equipment 302 can be started, and the protective gas stored in the recovery tank 301 can be pumped into the gas dehumidification and deoxygenation equipment 302 through the delivery pipe 303 for dehumidification and deoxygenation. When the protective gas filled with moisture and oxygen inside is dehumidified and deoxygenated, it can flow back into the protective gas delivery tank 3 for recycling and reuse. When the vacuum pump 204 starts to evacuate the quartz tube 2, the gas dehumidification and deoxygenation equipment 302 can be started again, so that the protective gas can be fully recovered, which is convenient for recycling the protective gas and reducing the cost of processing crystal growth raw materials.

[0032] Among them, the gas dehumidification and deoxygenation equipment 302 can adopt common equipment on the market that can remove moisture and oxygen from the gas. Its structure and principle can be known to technicians through technical manuals or through conventional experimental methods, so as to facilitate the processing of the protective gas into pure and dry gas.

[0033] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any form. Although the present invention has been disclosed as a preferred embodiment, it is not intended to limit the present invention.

Claims

1. A crystal growth raw material processing device, characterized in that: include: Electric heating furnace (1); A quartz tube (2) is placed in the electric heating furnace (1), and both ends of the quartz tube extend out of the electric heating furnace (1); The two ends of the quartz tube (2) are respectively provided with an air inlet and an air outlet; An air inlet vacuum valve (201) installed at the air inlet of the quartz tube (2); An exhaust vacuum valve (202) installed at the gas outlet of the quartz tube (2); The quartz tube (2) is provided with an air extraction port on one side close to the air outlet; An exhaust vacuum valve (203) installed at the exhaust port of the quartz tube (2); A vacuum pump (204), the air suction port of which is connected to the air suction port of the quartz tube (2); The protective gas delivery tank (3) is installed on a side close to the gas inlet of the quartz tube (2), and the gas delivery port is connected to the gas inlet of the quartz tube (2).

2. A crystal growth raw material processing equipment according to claim 1, characterized in that: The electric heating furnace (1) comprises a lower shell (101), an upper shell (102), a resistance wire type heating element (103) and a temperature gauge (104); the lower shell (101) and the upper shell (102) are rotatably connected via a rotating shaft; the resistance wire of the resistance wire type heating element (103) is spirally arranged in a cavity formed by the lower shell (101) and the upper shell (102); the controller of the resistance wire type heating element (103) is installed on the lower side of the lower shell (101); the temperature gauge (104) is installed on the upper shell (102), and the detection end extends into the cavity formed by the lower shell (101) and the upper shell (102).

3. A crystal growth raw material processing device according to claim 2, characterized in that: The heating range of the resistance wire heating element (103) is 50-900°C.

4. The crystal growth material processing equipment according to claim 1, characterized in that: The purity of the quartz tube (2) is greater than 99.99%.

5. The crystal growth material processing equipment according to claim 1, characterized in that: The intake vacuum valve (201), the exhaust vacuum valve (202) and the exhaust vacuum valve (203) all have a limit pressure of less than 5×10 -5 Pa vacuum valve.

6. The crystal growth material processing equipment according to claim 1, characterized in that: The gas outlet of the quartz tube (2) is connected to a recovery tank (301), and a gas dehumidification and deoxygenation device (302) is installed above the protective gas protective gas delivery tank (3). The gas extraction port of the gas dehumidification and deoxygenation device is connected to the gas outlet of the recovery tank (301) through a delivery pipe (303), and the gas outlet of the dehumidification and deoxygenation device (302) is connected to the recovery port of the protective gas delivery tank (3). The delivery pipe (303) is a three-way pipe, and the other gas inlet end of the delivery pipe (303) is connected to the gas outlet end of the vacuum pump (204).

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