Ultra-pure tellurium-zinc-cadmium polycrystalline material liquid-phase synthesis equipment and method

Abstract

The invention discloses liquid-phase synthesis equipment and method for an ultra-pure tellurium-zinc-cadmium polycrystalline material. The liquid-phase synthesis equipment comprises a synthesis tank, a tank cover is connected to the synthesis tank in a sealed mode, a heating furnace is arranged in the synthesis tank, a graphite crucible is placed in the heating furnace through a crucible lining, a graphite crucible cover is arranged on the graphite crucible, and a heating base is arranged at the lower end of the synthesis tank; a preset distance is formed between the synthesis tank and the heating furnace so as to obtain a heat exchange cavity therebetween; a liquid cooling heat dissipation mechanism I and an air cooling heat dissipation mechanism are fixedly mounted on the tank cover, and liquid cooling heat dissipation mechanisms II are arranged on the periphery and the bottom of the synthesis tank; an air valve communicated with the heat exchange cavity and the heating furnace is arranged in the center of the bottom of the synthesis tank. Compared with the prior art, the device has the following beneficial effects that multi-angle cooling of the device is achieved through the air cooling heat dissipation mechanism, the liquid cooling heat dissipation mechanism I and the liquid cooling heat dissipation mechanism II, and meanwhile the heat exchange cavity is used for conducting heat or isolating heat, so that the reaction temperature in the device can be better controlled, and smooth reaction is guaranteed.

Description

Technical Field

[0001] The invention belongs to the technical field of preparation and purification of cadmium zinc telluride polycrystals, and in particular relates to liquid phase synthesis equipment and a method for ultra-pure cadmium zinc telluride polycrystal materials. Background Art

[0002] At present, driven by the needs of military, civilian and scientific research fields, mercury cadmium telluride (HgCdTe, MCT) infrared detectors have developed to the third generation infrared focal plane array stage. 7N CdZnTe is very important. Among the excellent substrate materials of HgCdTe infrared detectors, CdZnTe and HgCdTe have good lattice adaptability, which can effectively reduce the misfit dislocation density of HgCdTe epitaxial layer. Therefore, the growth of HgCdTe materials on CdZnTe substrates has irreplaceable advantages over other heterogeneous substrates (such as GaAs). In addition, CdZnTe crystals also have broad application prospects in the preparation of X-ray and gamma-ray detectors, solar cells, optical modulators, laser windows, etc. Therefore, the preparation and research of high-quality CdZnTe crystals have always received widespread attention.

[0003] The core components of the cadmium zinc telluride (CZT) high-pressure liquid phase synthesis device include the furnace body, heating system, control system and vacuum / inert gas pressurization system. The research and development process mainly focuses on inert gas pressure control, internal structure design and temperature field design. According to the in-depth theoretical calculation results in the early stage, the design pressure of the high-pressure synthesis furnace needs to take into account the actual needs of the synthesis process and safety redundancy to ensure that there is a sufficient safety pressure range outside the upper limit of the process pressure. The internal structure and structural design of the high-pressure synthesis test device include a charging crucible, a graphite heating jacket tube wrapped around the crucible, and a crucible support device. The charging crucible needs to withstand a high temperature environment exceeding 1150°C. High-purity materials are selected for the material, and a combined crucible composed of a high-purity boron nitride crucible and a graphite set is considered to enhance the mechanical strength and increase the service life of the boron nitride crucible. The temperature field design of the high-pressure synthesis test equipment is carried out according to the raw material input and crucible size parameters. By planning the size specifications and spatial layout of each heater, a multi-stage temperature control technology is used to form a stable constant temperature area to ensure that the strict requirements of the CZT synthesis process for the temperature field are met.

[0004] However, most of the existing CdZnTe polycrystalline synthesis devices use a solid insulation layer inside to reduce heat loss during the reaction process. When the temperature inside the device reaches above the rated temperature of the reaction, the heat dissipation effect of the heat exchange cavity in the device cannot transfer the internal heat to the outside of the device in time. At the same time, the heat dissipation device outside the device uses a single water cooling cycle to cool down, so that the high temperature inside the device cannot be dissipated in time. If the temperature inside the device cannot be reduced to the experimental requirements in time, it will have a significant impact on the internal reaction process, causing the experimental results to be invalid or unable to proceed normally.

[0005] For example, patent application number CN118600548A discloses a method for synthesizing and purifying cadmium zinc telluride polycrystals and an integrated device for high-pressure synthesis and purification. The device is provided with a cooling water jacket on the shell, and the cooling water jacket is externally connected to a cold water tank to cool the entire device. At the same time, an insulation layer is provided inside the device to ensure that the experimental temperature is controlled within a predetermined range during the reaction process inside the device, thereby observing the reaction process of tellurium, zinc, and cadmium inside the device.

[0006] The above-mentioned devices all use traditional insulation and water cooling methods, and a physical insulation layer is used inside the device to insulate the inside of the device. However, in actual use, the physical insulation layer is attached to the inner wall of the device, and the insulation layer serves as a medium for transferring heat to the outside of the device. If the insulation effect of the insulation layer is weak, the temperature of the insulation layer is easily affected by the external water cooling jacket, which causes the internal temperature of the device to be easily affected, making it impossible for the temperature inside the device to be stably maintained within the temperature range required by the experiment; if the insulation effect of the insulation layer is strong, when the critical temperature value is reached inside the device, the reaction device cannot transfer the internal heat to the cooling water jacket through the insulation layer in time, and thus cannot achieve rapid cooling inside the device. Therefore, the device has major problems in controlling the insulation and heat dissipation of the internal temperature. Summary of the invention

[0007] An object of the present invention is to solve at least the above problems and / or disadvantages and to provide at least the advantages which will be described hereinafter.

[0008] In order to achieve these purposes and other advantages according to the present invention, there is provided an ultra-pure cadmium zinc telluride polycrystalline material liquid phase synthesis equipment, comprising a synthesis tank, to which a tank cover is sealed, a heating furnace capable of heating a graphite crucible is arranged in the synthesis tank, the graphite crucible is placed in the heating furnace through a crucible liner, a graphite crucible cover abutting against the tank cover is arranged on the graphite crucible, and a heating base for bottom heating of the crucible liner and the graphite crucible is arranged at the lower end of the synthesis tank;

[0009] There is a predetermined distance between the synthesis tank and the heating furnace to obtain a heat exchange cavity therebetween, a fixed platform is arranged above the synthesis tank, an edge matching the fixed platform is arranged on the top of the heating furnace, and the heating furnace is fixedly connected to the fixed platform through the edge so that the heat exchange cavity is sealed;

[0010] A liquid-cooled heat dissipation mechanism I for dissipating heat from the top and periphery of the synthesis tank, and an air-cooled heat dissipation mechanism cooperating with the liquid-cooled heat dissipation mechanism I are fixedly installed on the tank cover; a liquid-cooled heat dissipation mechanism II for dissipating heat from the corresponding side walls of the synthesis tank is arranged on the periphery and bottom of the synthesis tank; the liquid-cooled heat dissipation mechanism I is connected to the liquid-cooled heat dissipation mechanism II through a conduit to cool the synthesis tank as a whole; an air valve connected to the heat exchange cavity and the heating furnace is arranged at the center of the bottom of the synthesis tank.

[0011] Preferably, the liquid cooling heat dissipation mechanism I comprises:

[0012] An annular heat dissipation base has a plurality of heat dissipation support plates connected to the tank cover equidistantly arranged at the bottom thereof, and a plurality of ventilation ducts are separated by the heat dissipation support plates. A heat dissipation layer I with a corrugated longitudinal section is provided inside the annular heat dissipation base. A connecting pipe matched with the conduit is provided on one side of the annular heat dissipation base. The heat dissipation layer I is connected with the liquid-cooled heat dissipation mechanism through the connecting pipe. A cold liquid outlet connected with a cold source is provided on the other side of the heat dissipation layer I.

[0013] Preferably, the air-cooling heat dissipation mechanism I comprises:

[0014] A heat dissipation cover, the bottom of which is fixedly connected to the upper end of the annular heat dissipation base, the outer periphery of the heat dissipation cover is provided with a heat dissipation ring surrounding the upper end of the synthesis tank and capable of guiding wind, and the connecting end passes through the heat dissipation ring;

[0015] A heat dissipation fan, which is fixedly arranged on the heat dissipation cover and faces the heat dissipation base;

[0016] A plurality of air ducts vertically penetrate the annular heat dissipation base;

[0017] Among them, the air outlet of each air duct is spatially connected with the corresponding ventilation duct.

[0018] Preferably, the liquid cooling heat dissipation mechanism II comprises:

[0019] A heat dissipation bottom plate, which serves as the bottom of the synthetic tank, wherein a heat dissipation layer II with a corrugated longitudinal section is provided in an annular direction inside the heat dissipation bottom plate, and a cold liquid inlet connected to the heat dissipation layer II is provided on one side of the heat dissipation bottom plate;

[0020] A plurality of water-cooling tubes with S-shaped cross-sections are spirally arranged on the periphery of the synthesis tank, the bottoms of the plurality of water-cooling tubes are simultaneously connected to the heat dissipation layer II, the upper ends of the plurality of water-cooling tubes are simultaneously connected to the water-cooling ring pipe and are thus mutually connected, and the water-cooling ring pipe is provided with a water outlet interface that matches the conduit, and the water-cooling ring pipe delivers the coolant to the heat dissipation layer I through the conduit.

[0021] Preferably, a heating platform for accommodating a graphite bushing is provided on the inner wall of the heating furnace, an upper end of the heating platform abuts against an end of the crucible bushing, and a heating graphite ring connected to an external power source is spirally provided inside the heating platform;

[0022] The heating platform is provided with a plurality of vent holes equidistantly arranged in a circular direction.

[0023] Preferably, a double-layer shock-absorbing ring is arranged between the heating furnace and the crucible liner, and a plurality of elastic elements are arranged in the gap between the double-layer shock-absorbing rings.

[0024] Preferably, the cross section of the air duct is funnel-shaped in space, and the larger end faces the fan side;

[0025] The cross section of the ventilation hole is spatially arranged in a corrugated and funnel-shaped structure, and the larger end of the funnel-shaped tube is close to the outer shock-absorbing ring and is spatially offset from the double-layer shock-absorbing ring to form a passage in the heating furnace that is connected to valve II.

[0026] Preferably, a heating couple is provided on one side of the synthesis tank, which passes through the heating furnace and performs heating treatment on the upper, middle and lower ends of the device respectively;

[0027] A pressure valve for controlling the internal pressure is arranged on the other side of the synthesis tank.

[0028] A method for liquid phase synthesis of ultrapure cadmium zinc telluride polycrystalline material comprises the following steps:

[0029] Step 1: introduce a predetermined amount of tellurium, zinc and cadmium into the unclosed graphite crucible, then cover the graphite crucible, and seal the tank cover with the synthesis tank. At this time, the heat exchange chamber and the heating furnace are evacuated through valves I and II on the gas valve to complete the preparation before the experiment.

[0030] Step 2, start the power supplies connected to the heating graphite ring and the heating base respectively to heat the upper end and the bottom of the outer periphery of the graphite crucible respectively, when the internal temperature rises to a predetermined value, turn on the fan, and pass the cooling liquid into the cold liquid inlet until the liquid cooling heat dissipation mechanism I and the liquid cooling heat dissipation mechanism II are filled, and under the action of the fan, the wind flows into the outer periphery of the synthesis tank from the air duct and the ventilation duct on the air cooling heat dissipation mechanism, and flows to the bottom of the synthesis tank along the gap between the water cooling pipes, and flows out from the air supply holes on the outer shell of the bottom of the synthesis tank, and then cooperates with the liquid cooling heat dissipation mechanism I and the liquid cooling heat dissipation mechanism II to enhance the heat dissipation of the device;

[0031] Step 3: During the continuous reaction of tellurium, zinc and cadmium, a predetermined amount of inert gas is continuously introduced into the interior through valve II, and then the pressure and temperature of the internal gas are controlled by the pressure valve in combination with the heating couple group;

[0032] Step 4: After the reaction is completed, an inert gas is introduced into the heat exchange chamber through valve I to transfer the temperature inside the device out of the device, and finally the tank cover and the graphite crucible cover are separated to obtain the reaction product.

[0033] The present invention includes at least the following beneficial effects: Compared with the existing technology, the device can isolate the heat in the heating furnace through the heat exchange layer, so that the temperature inside the device can be well maintained, and at the same time, the liquid cooling heat dissipation mechanism can dissipate heat through the entire device as a heat transfer medium, so that the overall temperature of the device can be controlled. After the reaction in the device is completed, an inert gas can be introduced into the heat exchange cavity through the gas valve to achieve good gas transfer medium heat dissipation, and the temperature in the device can be timely transferred to the heat dissipation mechanism outside the device, so that the temperature in the device can be quickly reduced and controlled, which is convenient for the operator to open the device later to extract and detect the reactants inside the device.

[0034] Other advantages, objectives and features of the present invention will be embodied in part through the following description, and in part will be understood by those skilled in the art through study and practice of the present invention. BRIEF DESCRIPTION OF THE DRAWINGS

[0035] Figure 1 It is a liquid phase synthesis equipment for ultra-pure cadmium zinc telluride polycrystalline materials;

[0036] Figure 2 It is a side view of the equipment section;

[0037] Figure 3 This is the front view of the equipment section;

[0038] Figure 4 It is a tank cover and a liquid cooling heat dissipation mechanism I and an air cooling heat dissipation mechanism;

[0039] Figure 5 It is a cross-sectional view of the tank cover, liquid cooling heat dissipation mechanism I and air cooling heat dissipation mechanism.

[0040] Markings in the figure: 1. synthesis tank, 2. tank cover, 3. graphite crucible, 4. heating furnace, 41. heating table, 42. heating graphite ring, 43. vent, 44. heating couple, 5. crucible bushing, 6. graphite crucible cover, 7. heating base, 8. fixing table, 9. liquid cooling heat dissipation mechanism I, 91. annular heat dissipation base, 92. heat dissipation support plate, 92-1, ventilation duct, 93. heat dissipation layer I, 94. conduit, 95. connecting pipe, 97. cold liquid outlet, 10 0. Heat dissipation cover, 101. Heat dissipation ring, 102. Heat dissipation fan, 103. Air duct, 10. Air-cooled heat dissipation mechanism, 11. Liquid-cooled heat dissipation mechanism II, 110. Heat dissipation base plate, 111. Heat dissipation layer II, 112. Water-cooled pipe, 113. Water-cooled ring pipe, 114. Liquid outlet pipe, 115. Cold liquid inlet, 12. Air valve, 121. Valve I, 122. Valve II, 13. Heat exchange chamber, 16. Double-layer shock-absorbing ring, 17. Elastic element, 18. Pressure valve. DETAILED DESCRIPTION

[0041] The present invention is further described in detail below in conjunction with the accompanying drawings so that those skilled in the art can implement the invention with reference to the description.

[0042] It should be understood that the terms such as “having”, “including” and “comprising” used herein do not exclude the existence or addition of one or more other elements or combinations thereof.

[0043] It should be noted that in the description of the present invention, the orientation or positional relationship indicated by the term is based on the orientation or positional relationship shown in the drawings, which is only for the convenience of describing the present invention and simplifying the description, and does not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as limiting the present invention. In addition, the terms "first" and "second" are only used for descriptive purposes and cannot be understood as indicating or implying relative importance.

[0044] In the description of the present invention, unless otherwise clearly stipulated and limited, the terms "installed", "provided with", "mounted / connected", "connected", etc. should be understood in a broad sense. For example, "connected" can be a fixed connection, a detachable connection, or an integral connection. It can be a mechanical connection or an electrical connection. It can be a direct connection or an indirect connection through an intermediate medium. It can be the internal connection of two components. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0045] In addition, in the present invention, unless otherwise clearly specified and limited, a first feature being "above" or "below" a second feature may mean that the first and second features are in direct contact, or the first and second features are in indirect contact through an intermediate medium. Moreover, a first feature being "above", "above" or "above" a second feature may mean that the first feature is directly above or obliquely above the second feature, or simply means that the first feature is higher in level than the second feature. A first feature being "below", "below" or "below" a second feature may mean that the first feature is directly below or obliquely below the second feature, or simply means that the first feature is lower in level than the second feature.

[0046] like Figures 1 to 5 As shown, a liquid phase synthesis equipment for ultra-pure cadmium zinc telluride polycrystalline material comprises a synthesis tank 1, on which a tank cover 2 is sealed and connected, a heating furnace 4 capable of heating a graphite crucible 3 is arranged in the synthesis tank 1, the graphite crucible 3 is placed in the heating furnace 4 through a crucible liner 5, a graphite crucible cover 6 abutting against the tank cover 2 is arranged on the graphite crucible 3, and a heating base 7 for bottom heating the crucible liner 5 and the graphite crucible 3 is arranged at the lower end of the synthesis tank 1;

[0047] There is a predetermined distance between the synthesis tank 1 and the heating furnace 4 to obtain a heat exchange chamber 13 therebetween. A fixing platform 8 is disposed above the synthesis tank 1. An edge that matches the fixing platform 8 is disposed on the top of the heating furnace 4. The heating furnace 4 is fixedly connected to the fixing platform 8 through the edge so that the heat exchange chamber 13 is sealed.

[0048] The tank cover 2 is fixedly provided with a liquid cooling heat dissipation mechanism Ⅰ9 for dissipating heat from the top and periphery of the synthesis tank 1, and an air cooling heat dissipation mechanism 10 cooperating with the liquid cooling heat dissipation mechanism Ⅰ9. The periphery and bottom of the synthesis tank 1 are provided with a liquid cooling heat dissipation mechanism Ⅱ11 for dissipating heat from the corresponding side walls of the synthesis tank 1. The liquid cooling heat dissipation mechanism Ⅰ9 is connected to the liquid cooling heat dissipation mechanism Ⅱ11 through a conduit 94 to cool down the synthesis tank 1 as a whole; the bottom center of the synthesis tank 1 is provided with an air valve 12 connected to the heat exchange chamber 13 and the heating furnace 4.

[0049] Working principle:

[0050] When the operator uses the device to perform polycrystalline liquid phase synthesis of tellurium, zinc and cadmium, the operator can put the reactants into the graphite crucible 3 in advance and cover it with the graphite crucible cover 6, and then seal the tank cover 2 and the synthesis tank 1. Then, the heat exchange chamber 13 and the heating furnace 4 are evacuated through the air valve 12. Then, the upper end and the bottom of the outer periphery of the crucible liner 5 can be heated by the heating furnace 4 and the heating base 7 through an external power supply, thereby indirectly heating the graphite crucible 3. At this time, the reactants begin to react and generate gas. By pressurizing the heating furnace 4 with inert gas, when the pressure on the system is increased, the interaction force between molecules is enhanced, making it more difficult for the molecules on the surface of the liquid to escape and become steam molecules, thereby reducing the volatilization of raw materials. The heat exchange chamber 13 separated by the fixed table 8 and the heating furnace 4 is isolated from the heat in the heating furnace 4 from being transferred to the outside of the device through the heat exchange chamber 13 by the operation of evacuating the inside of the device through the air valve 12, so that the environmental temperature change of the reaction inside the device tends to be stable, ensuring that the tellurium, zinc and cadmium in the graphite crucible 3 can react normally. At the same time, during the continuous heating process inside the device, the air-cooled heat dissipation mechanism 10 and the liquid-cooled heat dissipation mechanism Ⅰ9 located at the upper end of the synthesis tank 1 can be started to cool the tank cover 2 and the periphery of the synthesis tank 1, and at the same time cooperate with the liquid-cooled heat dissipation mechanism Ⅱ11 to complete the heat dissipation of the entire structure of the synthesis tank 1. At the same time, the bottom of the graphite crucible 3 and the crucible liner 5 in the device are formed in one step with a circular bottom, so that the internal stress of the structure is small, the mechanical strength is high, and it is not easy to be damaged during the synthesis process; a graphite cover is designed on the top of the crucible to reduce the loss of material volatilization.

[0051] Compared with the traditional single heat dissipation structure, the present device adopts air cooling and water cooling to dissipate heat simultaneously to ensure that the entire device is within the required range of the reaction. Finally, when the reaction is completed, the air valve 12 can pass inert gas into the heat exchange chamber 13 to realize air medium as a heat transfer medium to reduce the temperature in the device to a predetermined value.

[0052] In the above technical solution, the liquid cooling heat dissipation mechanism I9 includes:

[0053] The annular heat dissipation base 91 has a plurality of heat dissipation support plates 92 connected to the tank cover 2 equidistantly arranged at its bottom, and a plurality of ventilation ducts 92-1 are separated by the heat dissipation support plates 92. A heat dissipation layer I 93 with a corrugated longitudinal section is provided inside the annular heat dissipation base 91. A connecting pipe 95 matched with the conduit 94 is provided on one side of the annular heat dissipation base 91. The heat dissipation layer I 93 is connected to the liquid-cooled heat dissipation mechanism II 11 through the connecting pipe 95. A cold liquid outlet 97 connected to a cold source is provided on the other side of the heat dissipation layer I 93.

[0054] Through the above arrangement, when the coolant in the liquid cooling heat dissipation mechanism II11 flows into the heat dissipation layer I93 through the connecting pipe 95 and the conduit 94, the coolant begins to cover the heat dissipation layer I93 and begins to cool the tank cover 2. In this process, the air cooling heat dissipation mechanism 10 will also cooperate to cool the tank cover 2, and then the coolant will flow back to the cold source through the cold liquid outlet 97. Therefore, the wind generated by the air cooling heat dissipation device 10 will flow into the ventilation duct 92-1 along the through hole in the center of the annular heat dissipation base 91, and at the same time, under the action of the heat dissipation support plate 92, it will begin to flow toward the outer periphery of the top of the synthetic tank 1 in multiple directions. The setting of the corrugated cross section of the heat dissipation layer I93 increases the area for heat exchange between the coolant in the heat dissipation layer I93 and the heat, thereby effectively improving the cooling effect of the liquid cooling heat dissipation mechanism I9.

[0055] In the above technical solution, the air-cooling heat dissipation mechanism 10 includes:

[0056] The heat dissipation cover 100 has a bottom fixedly connected to the upper end of the annular heat dissipation base 91. The outer periphery of the heat dissipation cover 100 is provided with a heat dissipation ring 101 surrounding the upper end of the synthesis tank 1 and capable of guiding the wind. The connecting pipe 95 passes through the heat dissipation ring 101.

[0057] A heat dissipation fan 102, which is fixedly disposed on the heat dissipation cover 100, and the heat dissipation fan 102 is directly facing the annular heat dissipation base 91;

[0058] A plurality of air ducts 103, which are vertically arranged on the annular heat dissipation base 91;

[0059] Among them, the air outlet of each air duct is spatially connected with the corresponding ventilation duct 92-1.

[0060] Through the above arrangement, when the air-cooled heat dissipation mechanism 10 dissipates heat for the device, the wind generated by the heat dissipation fan 102 will flow into the multiple ventilation ducts 92-1 through multiple air ducts 103. At the same time, multiple air ducts 103 can be arranged in multiple annular directions along the annular heat dissipation base 91, and the distance between two adjacent air ducts 103 is equidistant, so that the wind can pass through multiple air ducts 103 evenly, thereby realizing efficient heat dissipation of the tank cover 2, and flow into the heat dissipation ring 101 under the action of the heat dissipation support plate 92. The heat dissipation ring 101 can guide the wind here to the liquid-cooled heat dissipation mechanism II 11 on the periphery of the synthesis tank 1, so as to cooperate with the liquid-cooled heat dissipation mechanism II 11 to double cool the periphery of the synthesis tank 1. The connecting pipe 95 is set through the heat dissipation ring 101, so that the overall structure of the device is more reasonably set, and it is convenient for the operator to connect the connecting pipe 95 with the liquid-cooled heat dissipation mechanism II. In the above process, the heat dissipation cover 100 ensures that the heat dissipation fan 102 can be vertically facing the multiple air ducts 103 on the annular heat dissipation base 91 to ensure the heat dissipation effect.

[0061] In the above technical solution, the liquid cooling heat dissipation mechanism II11 includes:

[0062] A heat dissipation bottom plate 110, which serves as the bottom of the synthesis tank 1, wherein a heat dissipation layer II 111 with a corrugated longitudinal section is provided in an annular direction inside the heat dissipation bottom plate 110, and a cold liquid inlet 115 connected to the heat dissipation layer II 111 is provided on one side of the heat dissipation bottom plate 110;

[0063] A plurality of water-cooling tubes 112 with S-shaped cross-sections are spirally arranged on the periphery of the synthesis tank 1, the bottoms of the plurality of water-cooling tubes 112 are simultaneously connected to the heat dissipation layer II 111, the upper ends of the plurality of water-cooling tubes 112 are simultaneously connected to the water-cooling loop pipe 113 and are thus interconnected, and the water-cooling loop pipe 113 is provided with a liquid outlet pipe 114 that cooperates with the conduit 94, and the water-cooling loop pipe 113 delivers the coolant to the heat dissipation layer I 93 through the conduit 94.

[0064] Through the above arrangement, the coolant can flow from the coolant inlet 115 into the heat dissipation layer II 111 in the heat dissipation base plate 110, and then the coolant continues to spread upward along the water-cooling tube 112 until it flows into the water-cooling ring tube 113, so that the upper ends of multiple water-cooling tubes 112 are connected to simultaneously perform wrap-type heat dissipation on the periphery and bottom of the synthesis tank 1, and then the coolant flows into the heat dissipation layer I 93 through the liquid outlet pipe 114 and the conduit 94, so as to achieve the connection and coordination between multiple heat dissipation mechanisms. Among them, the cross-sections of the water-cooling tube 112 and the heat dissipation layer II 111 are both S-shaped, which increases the area for heat exchange between the heat in the device and the coolant, and further improves the heat dissipation effect inside the device.

[0065] In the above technical solution, the inner wall of the heating furnace 4 is provided with a heating platform 41 for accommodating the crucible liner 5, the upper end of the heating platform 41 is in contact with the end of the crucible liner 5, and a heating graphite ring 42 connected to an external power source is spirally provided inside the heating platform 41;

[0066] The heating platform 41 is provided with a plurality of vent holes 43 equidistantly arranged in an annular direction.

[0067] Through the above arrangement, when the internal environment of the device is heated, the heating graphite ring 42 in the heating platform 41 is heated by an external power supply, and the heating graphite ring 42 is arranged in a threaded shape to ensure that the generated heat can surround the crucible liner 5 and the graphite crucible 3, thereby ensuring the heating effect of the reaction vessel inside the device, and realizing the heat conduction of the graphite crucible 3 by the crucible liner 5 to achieve the required environmental temperature of the reaction material. When the reaction occurs, the gas valve 12 will pass inert gas into the heating furnace 4, and the inert gas can flow to the upper end of the heating furnace 4 through multiple vents 43, and cover the tank cover 2 and the graphite crucible cover 6. By adding inert gas to increase the pressure, when the pressure on the system is increased, the interaction force between molecules is enhanced, making it more difficult for the molecules on the surface of the liquid to escape into steam molecules, thereby reducing the volatilization of raw materials.

[0068] In the above technical solution, a double-layered shock-absorbing ring 16 is arranged between the heating furnace 4 and the crucible liner 5 , and a plurality of elastic elements 17 are arranged in the gap between the double-layered shock-absorbing rings 16 .

[0069] Through the above arrangement, when the inert gas is introduced into the heating furnace 4, since the inside of the device is in a vacuum state, the inert gas flowing in at this time will generate a large impact force. When the inert gas flows into the upper end of the heating platform 41, it will flow in the cavity in the heating furnace 4, which may cause the graphite crucible cover 6 to be impacted. By clamping the inner ring of the heating furnace 4 with the outer ring of the double-layer shock-absorbing ring 16, and the upper end of the crucible liner 5 with the inner ring of the double-layer shock-absorbing ring 16, when the inert gas impacts the crucible liner 5 and the graphite crucible cover 6, the impact force can be absorbed by the double-layer shock-absorbing ring 16 through multiple elastic elements 17, thereby ensuring the structural stability of the crucible liner 5 and the graphite crucible 3 and reducing the influence of the gas on the internal reaction.

[0070] In the above scheme, the gas valve 12 is arranged at the bottom center of the synthesis tank 1, and the gas valve 12 is provided with valve I 121 and valve II 122. The valve I 121 passes through the bottom of the synthesis tank 1 and is connected with the heat exchange chamber 13, and the valve II 122 passes through the heating furnace 4 and is located directly below the heating base 7.

[0071] Through the above arrangement, when it is necessary to maintain the heat in the reaction process, the gas valve 12 evacuates the heat exchange chamber 13 through the valve I 121, so that the heat inside the device is mainly transferred out by heat radiation, and a small amount of heat can be transmitted through the internal container itself. The setting of the heat exchange chamber 13 can largely isolate the heat transfer in the heating furnace 4. When the device is finished, the heat exchange chamber 13 can be filled with inert gas, and then the heat exchange chamber 13 and the inert gas can be used as heat transfer media to transfer the heat to the water cooling pipe 112 in time. Valve II 122 is used to ensure the vacuum in the reaction device to prevent the residual oxygen from affecting the reaction in the device. At the same time, inert gas can be introduced to maintain the effectiveness of the reaction in the device. When the pressure on the system is increased, the interaction force between molecules is enhanced, making it more difficult for the molecules on the surface of the liquid to escape and become steam molecules, thereby reducing the volatilization of raw materials. The setting of valve II 122 directly facing the heating base 7 reduces the impact of the inert gas introduced on the internal structure of the device and ensures the stability of the internal structure.

[0072] In the above solution, the cross section of the air duct 103 is funnel-shaped in space, and the larger end faces the fan side;

[0073] The cross section of the ventilation hole 43 is spatially arranged in a corrugated and funnel-shaped structure, and the larger end of the funnel-shaped tube is close to the outer shock-absorbing ring, and is spatially offset from a portion of the double-layer shock-absorbing ring 16 to form a passage in the heating furnace 4 that is connected to the valve II 122.

[0074] Through the above arrangement, when the wind flow generated by the heat dissipation fan 102 passes through the air duct 103, due to the structural arrangement of the air duct 103, the wind speed becomes faster and more concentrated, and therefore the pressure at the smaller end of the air duct 103 is smaller, so that a pressure difference is formed on the two sides of the air duct 103, thereby driving more air to flow into the air duct 103. The cross-sectional arrangement of the ventilation hole 43 alleviates the turbulence of the inert gas when it flows through multiple bellows, and at the same time, the funnel-shaped structure at the upper end of the ventilation hole 43 ensures that the inert gas can stably flow out of the ventilation hole, and reduces the impact on the staggered double-layer shock-absorbing ring 16, making the overall structure inside the device more stable.

[0075] In the above scheme, a heating furnace 4 is provided on one side of the synthesis tank 1, and a heating couple group 44 is provided to heat the upper, middle and lower ends of the device respectively; a pressure valve 18 for controlling the internal pressure is provided on the other side of the synthesis tank 1.

[0076] Through the above arrangement, the operator can use multiple heating couple groups 44 and combine with an external temperature control monitoring system to detect the changes in the temperature inside the device in real time, and then control the amount and rate of the inert gas introduced by the gas valve 12 to control the pressure and temperature within the predetermined reaction range. When the volume of the gas generated by the reaction process inside the device and the inert gas introduced is too large, the pressure valve 18 can timely discharge part of the gas in the heating furnace 4 to the outside of the synthesis tank 1 to keep the pressure inside the device stable. The heating couple group 44 uses a high-precision high-pressure resistant platinum-rhodium-platinum temperature control thermocouple in conjunction with the heating base 7 external DC heating power supply module, so that the furnace temperature can be heated and cooled according to the designed temperature curve to meet the strict temperature requirements of the synthesis process.

[0077] Embodiment 1:

[0078] A method for liquid phase synthesis of ultrapure cadmium zinc telluride polycrystalline material comprises the following steps:

[0079] Step 1: introduce a predetermined amount of tellurium, zinc and cadmium into the unclosed graphite crucible 3, then cover the graphite crucible cover 6, and seal the tank cover 2 to the synthesis tank 1. At this time, the valve Ⅰ121 and valve Ⅱ122 on the gas valve 12 are used to evacuate the heat exchange chamber 13 and the heating furnace 4 respectively, so that the heat exchange chamber 13 can be isolated from the high temperature in the heating furnace 4, and at the same time, the oxygen in the heating furnace 4 is prevented from affecting the reaction process. By adding inert gas to increase the pressure on the system, the interaction force between molecules is enhanced, making it more difficult for the molecules on the surface of the liquid to escape and become steam molecules, thereby reducing the volatilization of raw materials. At the same time, the heating couple group 44 is connected to the detection system in advance, and it is ensured that the liquid cooling and heat dissipation mechanism Ⅰ9 and the liquid cooling and heat dissipation mechanism Ⅱ11 have been connected to the cold liquid system in advance to complete the preparations before the experiment begins;

[0080] Step 2, at this time, start the power supplies connected to the heating graphite ring 42 and the heating base 7 respectively, so as to heat the upper end and the bottom of the periphery of the graphite crucible 3 and the crucible liner 5 respectively. When the internal temperature rises to a predetermined value, turn on the cooling fan 102, and start to let the cooling liquid into the cold liquid inlet 115 until the liquid cooling heat dissipation mechanism I9 and the liquid cooling heat dissipation mechanism II11 are filled. Under the action of the cooling fan 102, the wind flows into the periphery of the synthesis tank 1 from the air duct 103 and the ventilation duct 92-1 on the air cooling heat dissipation mechanism 10, and flows to the bottom of the synthesis tank 1 along the gap between the air ducts, so as to flow out from the air supply holes on the bottom outer shell of the synthesis tank 1. In this process, the heat dissipation layer II 111 on the synthesis tank 1 is configured to be corrugated to increase the area of ​​heat exchange between the coolant in the device and the high temperature inside the device, and the cross-section of the water-cooling tube 112 is configured to be corrugated to further increase the contact area with the air and the wind generated by the air-cooling heat dissipation mechanism 10 and sent to the periphery of the synthesis tank 1, so that the periphery of the synthesis tank 1 can better dissipate heat inside the device, and at the same time, the heat dissipation layer II 111 can spread upward along the water-cooling tube 112 until it flows into the water-cooling ring pipe 113, thereby realizing the connection between the upper ends of multiple water-cooling tubes 112, and flowing into the liquid-cooling heat dissipation mechanism I 9 through the liquid outlet pipe 114 and the conduit 94 on the water-cooling ring pipe 113, thereby realizing The connection and coordination between multiple heat dissipation mechanisms, at this time, the coolant can start to fill in the heat dissipation layer I 93 to take away the heat from the top of the device near the tank cover 2. At the same time, under the action of the air-cooled heat dissipation mechanism 10, the wind flows through the air duct 103 that runs through the annular heat dissipation base 91 to take away the heat of the coolant in the heat dissipation layer I 93. At the same time, the wind flows out along the ventilation duct 92-1 formed by the intervals of the heat dissipation support plate 92, further taking away the heat on both sides of the annular heat dissipation base 91, thereby achieving the cooling of the air-cooled heat dissipation mechanism 10 and the liquid-cooled heat dissipation mechanism I 9. Finally, the coolant flows back to the cold source from the cold liquid outlet 97, thereby achieving the circulation cooling of the entire tank 1. The above-mentioned air-cooled heat dissipation mechanism 10 cooperates with the liquid-cooled heat dissipation mechanism I 9 and the liquid-cooled heat dissipation mechanism II 11 to enhance the heat dissipation of the device.

[0081] Step three, during the continuous reaction of tellurium, zinc and cadmium, a predetermined amount of inert gas is continuously introduced into the interior through valve II122, and the pressure is increased by adding inert gas. When the pressure of the system is increased, the interaction force between molecules is enhanced, making it more difficult for molecules on the surface of the liquid to escape and become steam molecules, thereby reducing the volatilization of raw materials. According to the saturated vapor pressure curves of tellurium, zinc and cadmium in the prior art, it is planned to increase the pressure in stages during the synthesis process to suppress the volatilization of raw materials, and then the pressure valve 30 is combined with the heating couple group 44 and the temperature of the internal gas to achieve precise temperature control inside the device, and the temperature control accuracy reaches ±1°C to prevent the temperature in the heating furnace 4 from affecting the device structure or reaction results;

[0082] Step 4: After the reaction is completed, an inert gas is introduced into the heat exchange chamber 13 through valve I121 to convert the heat exchange chamber 13 into a heat-conducting layer for transferring temperature, and the high temperature inside the device is transferred to the outside of the device through the heat exchange chamber 13 and the inert gas in the heat exchange chamber 13. Finally, the temperature is taken away by the cooling effect of the water-cooling pipe 112 and the wind generated by the air-cooling heat dissipation mechanism 10, so as to achieve rapid cooling of the device. Finally, the tank cover 2 and the graphite crucible cover 6 are removed to obtain the reaction product. If the experiment needs to be carried out again, the heat exchange chamber 13 can be evacuated again through valve I121, and then the heat exchange chamber 13 in the device can be converted into a heat-insulating structure with a heat-insulating effect to achieve heat insulation of the device.

[0083] Although the embodiments of the present invention have been disclosed as above, they are not limited to the applications listed in the specification and the implementation modes, and they can be fully applied to various fields suitable for the present invention. For those familiar with the art, additional modifications can be easily implemented. Therefore, without departing from the general concept defined by the claims and the scope of equivalents, the present invention is not limited to the specific details and the illustrations shown and described herein.

Claims

1. An ultrapure cadmium zinc telluride polycrystalline material liquid phase synthesis equipment, comprising a synthesis tank, on which a tank cover is sealed, a heating furnace capable of heating a graphite crucible is arranged in the synthesis tank, the graphite crucible is placed in the heating furnace through a crucible liner, a graphite crucible cover abutting against the tank cover is arranged on the graphite crucible, and a heating base for bottom heating of the crucible liner and the graphite crucible is arranged at the lower end of the synthesis tank, characterized in that: There is a predetermined distance between the synthesis tank and the heating furnace to obtain a heat exchange cavity therebetween, a fixed platform is arranged above the synthesis tank, an edge matching the fixed platform is arranged on the top of the heating furnace, and the heating furnace is fixedly connected to the fixed platform through the edge so that the heat exchange cavity is sealed; A liquid-cooled heat dissipation mechanism I for dissipating heat from the top and periphery of the synthesis tank, and an air-cooled heat dissipation mechanism cooperating with the liquid-cooled heat dissipation mechanism I are fixedly installed on the tank cover; a liquid-cooled heat dissipation mechanism II for dissipating heat from the corresponding side walls of the synthesis tank is arranged on the periphery and bottom of the synthesis tank; the liquid-cooled heat dissipation mechanism I is connected to the liquid-cooled heat dissipation mechanism II through a conduit to cool the synthesis tank as a whole; an air valve connected to the heat exchange cavity and the heating furnace is arranged at the center of the bottom of the synthesis tank.

2. The ultrapure cadmium zinc telluride polycrystalline material liquid phase synthesis equipment according to claim 1, characterized in that: The liquid cooling heat dissipation mechanism I comprises: An annular heat dissipation base has a plurality of heat dissipation support plates connected to the tank cover equidistantly arranged at the bottom thereof, and a plurality of ventilation ducts are separated by the heat dissipation support plates. A heat dissipation layer I with a corrugated longitudinal section is provided inside the annular heat dissipation base. A connecting pipe matched with the conduit is provided on one side of the annular heat dissipation base. The heat dissipation layer I is connected with the liquid-cooled heat dissipation mechanism through the connecting pipe. A cold liquid outlet connected with a cold source is provided on the other side of the heat dissipation layer I.

3. The ultrapure cadmium zinc telluride polycrystalline material liquid phase synthesis equipment according to claim 2, characterized in that: The air-cooling heat dissipation mechanism I comprises: A heat dissipation cover, the bottom of which is fixedly connected to the upper end of the annular heat dissipation base, the outer periphery of the heat dissipation cover is provided with a heat dissipation ring surrounding the upper end of the synthesis tank and capable of guiding wind, and the connecting end passes through the heat dissipation ring; A heat dissipation fan, which is fixedly arranged on the heat dissipation cover, and the heat dissipation fan is directly facing the annular heat dissipation base; A plurality of air ducts vertically penetrate the annular heat dissipation base; The air outlet of each air duct is spatially connected with the corresponding ventilation duct.

4. The ultrapure cadmium zinc telluride polycrystalline material liquid phase synthesis equipment according to claim 3, characterized in that: The liquid cooling heat dissipation mechanism II comprises: A heat dissipation bottom plate, which serves as the bottom of the synthetic tank, wherein a heat dissipation layer II with a corrugated longitudinal section is provided in an annular direction inside the heat dissipation bottom plate, and a cold liquid inlet connected to the heat dissipation layer II is provided on one side of the heat dissipation bottom plate; A plurality of water-cooling tubes with S-shaped cross-sections are spirally arranged on the periphery of the synthesis tank, the bottoms of the plurality of water-cooling tubes are simultaneously connected to the heat dissipation layer II, the upper ends of the plurality of water-cooling tubes are simultaneously connected to the water-cooling ring pipe and are thus mutually connected, and the water-cooling ring pipe is provided with a water outlet interface that matches the conduit, and the water-cooling ring pipe delivers the coolant to the heat dissipation layer I through the conduit.

5. The ultrapure cadmium zinc telluride polycrystalline material liquid phase synthesis equipment according to claim 4, characterized in that: The inner wall of the heating furnace is provided with a heating platform for accommodating a graphite bushing, the upper end of the heating platform abuts against the end of the crucible bushing, and a heating graphite ring connected to an external power source is spirally provided inside the heating platform; The heating platform is provided with a plurality of vent holes equidistantly in an annular direction.

6. The ultrapure cadmium zinc telluride polycrystalline material liquid phase synthesis equipment according to claim 5, characterized in that: A double-layer shock-absorbing ring is arranged between the heating furnace and the crucible liner, and a plurality of elastic elements are arranged in the gap between the double-layer shock-absorbing rings.

7. The ultrapure cadmium zinc telluride polycrystalline material liquid phase synthesis equipment according to claim 8, characterized in that: The air valve is arranged at the bottom center of the synthesis tank, and valve I and valve II are arranged on the air valve. Valve I passes through the bottom of the synthesis tank and is connected with the heat exchange cavity, and valve II passes through the heating furnace and is located directly below the heating base.

8. The ultrapure cadmium zinc telluride polycrystalline material liquid phase synthesis equipment according to claim 7, characterized in that: The cross section of the air duct is funnel-shaped in space, and the larger end faces the fan side; The cross section of the ventilation hole is spatially arranged in a corrugated and funnel-shaped structure, and the larger end of the funnel-shaped tube is close to the outer shock-absorbing ring and is spatially offset from the double-layer shock-absorbing ring to form a passage in the heating furnace that is connected to valve II.

9. The ultrapure cadmium zinc telluride polycrystalline material liquid phase synthesis equipment according to claim 8, characterized in that: One side of the synthesis tank is provided with a heating couple that penetrates the heating furnace and performs temperature treatment on the upper, middle and lower ends of the device respectively; A pressure valve for controlling the internal pressure is arranged on the other side of the synthesis tank.

10. A method for liquid phase synthesis of ultrapure cadmium zinc telluride polycrystalline material using any one of claims 1 to 4, characterized in that: The following steps are involved: Step 1: introduce a predetermined amount of tellurium, zinc and cadmium into the unclosed graphite crucible, then cover the graphite crucible, and seal the tank cover with the synthesis tank. At this time, the heat exchange chamber and the heating furnace are evacuated through valves I and II on the gas valve to complete the preparation before the experiment. Step 2, start the power supplies connected to the heating graphite ring and the heating base respectively to heat the upper end and the bottom of the outer periphery of the graphite crucible respectively, when the internal temperature rises to a predetermined value, turn on the fan, and pass the cooling liquid into the cold liquid inlet until the liquid cooling heat dissipation mechanism I and the liquid cooling heat dissipation mechanism II are filled, and under the action of the fan, the wind flows into the outer periphery of the synthesis tank from the air duct and the ventilation duct on the air cooling heat dissipation mechanism, and flows to the bottom of the synthesis tank along the gap between the water cooling pipes, and flows out from the air supply holes on the outer shell of the bottom of the synthesis tank, and then cooperates with the liquid cooling heat dissipation mechanism I and the liquid cooling heat dissipation mechanism II to enhance the heat dissipation of the device; Step 3: During the continuous reaction of tellurium, zinc and cadmium, a predetermined amount of inert gas is continuously introduced into the interior through valve II, and then the pressure and temperature of the internal gas are controlled by the pressure valve in combination with the heating couple group; Step 4: After the reaction is completed, an inert gas is introduced into the heat exchange chamber through valve I to transfer the temperature inside the device out of the device, and finally the tank cover and the graphite crucible cover are separated to obtain the reaction product.

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