Temperature control device for phosphorus cracking source, phosphorus cracking source and vacuum treatment system

By using a mixed temperature control device of fluid pipelines and cooling tanks in the phosphorus cracking source, combined with a closed-loop control system of temperature sensors and thermostats, the problem of difficulty in stably controlling the temperature of the white phosphorus area is solved, and the precise adjustment and stability of the white phosphorus pool temperature is achieved, and the phosphorus rotation efficiency and the stability of the phosphorus source beam flow are improved.

CN222961541UActive Publication Date: 2025-06-10FERMION INSTR (SHANGHAI) CO LTD
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Patent Information

Application Number
CN202421900394.1
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-08-07
Publication Date
2025-06-10
Estimated Expiration
2034-08-07

AI Technical Summary

Technical Problem

In the fields of optoelectronics and microelectronics, the white phosphorus steam used for the preparation of optoelectronic semiconductor devices needs to be very pure, but the prior art is difficult to stabilize the temperature of the white phosphorus region of the phosphorus cracking source, affecting the quality of the phosphide film.

Method used

A temperature control device including a fluid pipeline and a cooling pool is adopted, and the cooling fluid flows through the cooling pool for cooling and then enters the cooling zone. Combined with a closed-loop control system of a temperature sensor and a thermostat, the temperature of the white phosphorus tank is accurately adjusted.

Benefits of technology

It improves the cooling efficiency and temperature control range, ensures the stability of the white phosphorus tank temperature, improves the phosphorus transfer efficiency and the stability and repetition of the phosphorus source beam flow, and is suitable for obtaining phosphorus-containing films with good uniformity and repeatability.

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Abstract

The utility model relates to the technical field of vacuum equipment, and discloses a temperature control device for a phosphorus cracking source, the phosphorus cracking source and a vacuum treatment system. A temperature control device for a phosphorus cracking source comprises a fluid pipeline and a cooling pond. The fluid conduit is for permitting circulation of a cooling fluid into the cooling zone. The cooling pool is used for containing at least one part of the fluid pipeline so as to cool the cooling fluid in the fluid pipeline.
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Description

Technical Field

[0001] The present disclosure relates to the technical field of vacuum equipment, and particularly to a temperature control device for a phosphorus cracking source, a phosphorus cracking source, and a vacuum processing system. Background Art

[0002] Phosphorus-containing compound semiconductors have excellent electrical and optical properties and are of great value in the fields of optoelectronics and microelectronics. The white phosphorus vapor used for the preparation of various optoelectronic semiconductor devices must be very pure. However, there is no high-purity white phosphorus commercially available at present. The white phosphorus actually used in film coating is generally obtained by converting solid or gaseous phosphorus-containing compounds or elemental phosphorus. During the film coating process, a stable white phosphorus beam is a prerequisite for repeatedly obtaining high-quality and uniform phosphorus compound thin films. Therefore, a device capable of stably controlling the temperature of the white phosphorus region of the phosphorus cracking source is required. Summary of the Utility Model

[0003] The present disclosure provides a temperature control device for a phosphorus cracking source, comprising:

[0004] A fluid pipeline for allowing a cooling fluid to flow into a cooling area; and

[0005] A cooling pool for accommodating at least a part of the fluid pipeline to cool the cooling fluid in the fluid pipeline.

[0006] In some embodiments of the present disclosure, the fluid pipeline includes at least one coiled pipe located in the cooling pool to cool the cooling fluid through the cooling pool.

[0007] In some embodiments of the present disclosure, the temperature control device for a phosphorus cracking source further includes a temperature control unit, and the temperature control unit includes:

[0008] A temperature sensor disposed in the cooling area for measuring the temperature of the cooling area; and

[0009] A thermostat, the signal input end of which is connected to the temperature sensor, and the thermostat controls the flow rate of the cooling fluid in the fluid pipeline based on the temperature signal output by the temperature sensor.

[0010] In some embodiments of the present disclosure, the temperature control device for a phosphorus cracking source further includes a mass flow controller disposed on the fluid pipeline and connected to the thermostat. The mass flow controller is configured to receive a control signal from the thermostat and control the flow rate of the cooling fluid in the fluid pipeline based on the control signal.

[0011] In some embodiments of the present disclosure, the cooling pool includes a cooling medium and / or a refrigerator; and / or the cooling fluid is a gas.

[0012] The present disclosure provides a phosphorus cracking source, comprising:

[0013] a white phosphorus pool; and

[0014] a temperature control device for the phosphorus cracking source according to any embodiment of the present disclosure, wherein a cooling zone surrounds the white phosphorus pool, and the temperature control device for the phosphorus cracking source can control the temperature of the white phosphorus pool through the cooling zone.

[0015] In some embodiments of the present disclosure, the phosphorus cracking source further comprises an encapsulation structure configured to surround the white phosphorus pool. A cooling zone is formed inside the encapsulation structure, and there is a gap between the outer wall of the white phosphorus pool and the inner wall of the encapsulation structure, forming a cavity sandwich surrounding the white phosphorus pool for allowing a cooling fluid to flow through.

[0016] In some embodiments of the present disclosure, the encapsulation structure further comprises at least one baffle for dividing the cavity sandwich into a plurality of sandwich chambers. The baffle comprises at least one through hole, and the cooling fluid flows through the at least one through hole among the plurality of sandwich chambers to cool the white phosphorus pool.

[0017] In some embodiments of the present disclosure, a fluid pipeline of the temperature control device for the phosphorus cracking source is communicated with a fluid inlet located at the top of the encapsulation structure for guiding the cooling fluid into the cooling zone, and the fluid pipeline is communicated with a fluid outlet located at the bottom of the encapsulation structure or extends into the bottom of the encapsulation structure for guiding the cooling fluid out of the cooling zone.

[0018] In some embodiments of the present disclosure, the phosphorus cracking source further comprises:

[0019] a red phosphorus pool communicated with the white phosphorus pool so that red phosphorus vapor generated by the red phosphorus pool can diffuse into the white phosphorus pool; and / or

[0020] a cracking zone communicated with the white phosphorus pool.

[0021] In some embodiments of the present disclosure, the phosphorus cracking source further comprises:

[0022] a needle valve disposed on the connecting pipeline between the cracking zone and the white phosphorus pool for controlling the flow rate of white phosphorus vapor flowing from the white phosphorus pool to the cracking zone; and

[0023] a stepper motor connected to the needle valve for adjusting the needle valve.

[0024] The present disclosure provides a vacuum processing system, comprising:

[0025] a vacuum processing chamber; and

[0026] a phosphorus cracking source according to any embodiment of the present disclosure, which is vacuum-sealed and connected to the vacuum processing chamber for providing a phosphorus source beam to the vacuum processing chamber.

[0027] The temperature control device for the phosphorus cracking source, the phosphorus cracking source, and the vacuum processing system according to some embodiments of the present disclosure can bring beneficial technical effects. For example, the temperature control device for the phosphorus cracking source, the phosphorus cracking source, and the vacuum processing system according to some embodiments of the present disclosure adopt a mixed temperature control method of a cooling fluid and a cooling pool. The cooling fluid flows through a part of the fluid pipeline located in the cooling pool, is cooled by the cooling pool, and then enters the cooling area through the fluid pipeline, improving the cooling efficiency and the temperature control range. For another example, the phosphorus cracking source and the vacuum processing system according to some embodiments of the present disclosure can control and adjust the phosphorus conversion efficiency and the stability of the phosphorus source beam by changing the temperatures of different regions (such as the white phosphorus pool and the red phosphorus pool). During the phosphorus conversion, although the white phosphorus pool is continuously irradiated by the high temperature of the red phosphorus pool, by using the temperature control device for the phosphorus cracking source according to some embodiments of the present disclosure, the mixed temperature control method increases the heat capacity of the cooling circulation, so the temperature of the white phosphorus pool can still remain stable at a low temperature, thereby improving the phosphorus conversion efficiency. For another example, in the phosphorus cracking source and the vacuum processing system according to some embodiments of the present disclosure, since the closed-loop temperature control device for the phosphorus cracking source according to some embodiments of the present disclosure can keep the temperature of the white phosphorus pool stable for a long time and is not affected by the indoor environmental temperature where the device is located, the generated white phosphorus source beam also has good stability and repeatability, providing a good basis for obtaining a phosphorus-containing thin film with good uniformity and repeatability in the process. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] In order to more clearly illustrate the technical solutions in the embodiments of the present disclosure or the prior art, the following will briefly introduce the drawings required for use in the description of the embodiments or the prior art. Obviously, the drawings in the following description are only one embodiment of the present disclosure. For those of ordinary skill in the art, without creative efforts, other drawings can also be obtained based on these drawings.

[0029] Figure 1 FIG. shows a schematic structural diagram of a temperature control device for a phosphorus cracking source according to some embodiments of the present disclosure.

[0030] Figure 2 FIG. shows a schematic structural diagram of a phosphorus cracking source according to some embodiments of the present disclosure.

[0031] Figure 3 FIG. shows a schematic structural diagram of a cooling area according to some embodiments of the present disclosure.

[0032] Figure 4 FIG. shows a curve graph of the temperature change of the white phosphorus pool during the phosphorus conversion process of a phosphorus cracking source according to some embodiments of the present disclosure.

[0033] Figure 5 FIG. shows a curve graph of the change in the stability of the phosphorus source beam of a phosphorus cracking source according to some embodiments of the present disclosure.

[0034] Figure 6 Shows a schematic structural diagram of a vacuum processing system according to some embodiments of the present disclosure.

[0035] In the above figures, each reference numeral represents respectively:

[0036] 10000 - Vacuum processing system

[0037] 1000 - Phosphorus cracking source

[0038] 100 - Temperature control device for the phosphorus cracking source

[0039] 110 - Fluid pipeline

[0040] 111 - Coiled pipe

[0041] 120 - Cooling pool

[0042] 130 - Temperature control unit

[0043] 131 - Temperature sensor

[0044] 132 - Thermostat

[0045] 140 - Mass flow controller

[0046] 150 - Cooling zone

[0047] 200 - White phosphorus pool

[0048] 300 - Encapsulation structure

[0049] 310 - Cavity sandwich

[0050] 320a, 320b, 320c, 320d - Baffle

[0051] 400 - Red phosphorus pool

[0052] 500 - Cracking zone

[0053] 600 - Needle valve

[0054] 2000 - Vacuum processing chamber Detailed implementation manners

[0055] Some embodiments of the present disclosure will be described below in conjunction with the accompanying drawings. Obviously, the described embodiments are only exemplary embodiments of the present disclosure, rather than all embodiments.

[0056] In the description of the present disclosure, it should be noted that the orientation or positional relationship indicated by the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", "top", "bottom", etc. is based on the orientation or positional relationship shown in the drawings. It is only for the convenience of describing the present disclosure and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be construed as a limitation to the present disclosure. In addition, the terms "first" and "second" are only used for descriptive purposes and should not be construed as indicating or implying relative importance. In the description of the present disclosure, it should be noted that unless otherwise clearly specified and defined, the terms "installed", "connected", "coupled" should be understood in a broad sense. For example, it can be a fixed connection or a detachable 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 communication inside two elements. In the description of the present disclosure, the distal end or the far side refers to the end or side that penetrates into the vacuum environment (for example, the vacuum chamber), and the proximal end or the near side is the end or side opposite to the distal end or the far side (for example, the end or side away from the vacuum chamber, or the end or side near the vacuum chamber wall inside the vacuum chamber, etc.). Or, the end or side close to the driving device is the proximal end or the near side, and the end or side away from the driving device is the distal end or the far side. For those of ordinary skill in the art, the specific meanings of the above terms in the present disclosure can be understood according to specific circumstances.

[0057] Figure 1 FIG. shows a schematic structural diagram of a temperature control device 100 for a phosphorus cracking source according to some embodiments of the present disclosure.

[0058] As Figure 1 shown, in some embodiments of the present disclosure, the temperature control device 100 for a phosphorus cracking source may include a fluid pipeline 110 and a cooling pool 120. The fluid pipeline 110 is used to allow the cooling fluid to flow into the cooling area 150. The cooling pool 120 is used to accommodate at least a part of the fluid pipeline 110 to cool the cooling fluid in the fluid pipeline.

[0059] The temperature control device 100 for a phosphorus cracking source in some embodiments of the present disclosure adopts a mixed temperature control method of a cooling fluid and a cooling pool 120. After the cooling fluid flowing through a part of the fluid pipeline 110 located in the cooling pool 120 is cooled, it then enters the cooling area 150 through the fluid pipeline 110, improving the cooling efficiency and the temperature control range. Figure 1 The arrow direction in [FIGURE] indicates the flow direction of the cooling fluid. Similarly, the arrow directions in other drawings also indicate the flow direction of the cooling fluid.

[0060] As Figure 1As shown, in some embodiments of the present disclosure, the fluid pipeline 110 may include at least one coiled pipe section 111, and at least one coiled pipe section 111 is located in the cooling pool 120 to cool the cooling fluid through the cooling pool 120.

[0061] Those skilled in the art can understand that although Figure 1 only the coiled pipe section 111 is shown to be located in the cooling pool 120, this is only exemplary. The non-coiled pipe section (such as a straight pipe section) of the fluid pipeline 110 can also be partially located in the cooling pool 120. Additionally, the coiled pipe section 111 should be understood broadly, and the coiled pipe section 111 can include any suitable coiled form, such as a serpentine pipe, a spiral pipe, etc. By using the coiled pipe section 111, the heat exchange efficiency of the cooling fluid can be improved, and the volume of the cooling pool 120 can also be reduced.

[0062] As Figure 1 shown, in some embodiments of the present disclosure, the temperature control device 100 for the phosphorus cracking source may further include a temperature control unit 130. The temperature control unit 130 may include a temperature sensor 131 and a temperature controller 132. The temperature sensor 131 is disposed in the cooling zone 150 for measuring the temperature of the cooling zone 150 (for example, Figure 2 the white phosphorus pool 200 shown to be located in the cooling zone 150). The signal input end of the temperature controller 132 is connected to the temperature sensor 131, and the temperature controller 132 controls the flow rate of the cooling fluid in the fluid pipeline 110 based on the temperature signal output by the temperature sensor 131.

[0063] As Figure 1 shown, in some embodiments of the present disclosure, the temperature control device 100 for the phosphorus cracking source may further include a mass flow controller (MFC) 140. The mass flow controller 140 may be disposed on the fluid pipeline 110 and connected to the temperature controller 132. The mass flow controller 140 can be used to receive a control signal from the temperature controller 132 and control the flow rate of the cooling fluid in the fluid pipeline 110 based on the control signal.

[0064] In some embodiments of the present disclosure, by combining the cooling fluid with the cooling medium in the cooling pool 120 for temperature control, a closed-loop control loop can be established between the temperature of the cooling zone 150 and the flow rate of the cooling fluid, improving the temperature control range and stability of the white phosphorus pool. In some embodiments, the temperature controller 132 may include a proportional-integral-derivative (PID) controller, and the temperature of the cooling zone 150 can be precisely adjusted through the temperature controller 132. The PID control relationship between the temperature of the cooling zone 150 and the cooling fluid is a negative feedback regulation, which can further improve the temperature stability of the cooling zone 150.

[0065] As Figure 1As shown, in some embodiments of the present disclosure, the cooling pool 120 may include a cooling medium (not shown in the figure). In some sets of embodiments, the cooling medium may include a cold source with a stable temperature, such as an ice-water bath.

[0066] As Figure 1 shown, in some embodiments of the present disclosure, the cooling pool 120 may include a refrigerator (not shown in the figure). For example, the refrigerator may include a water bath machine, etc., for providing a cooling medium with a stable temperature. As an alternative, the refrigerator may also directly cool the fluid pipeline 110.

[0067] In some embodiments of the present disclosure, using a cooling medium, for example, a cooling medium capable of providing a stable temperature, to cool the cooling fluid (such as a gas) can avoid large fluctuations in the temperature of the white phosphorus pool 200 caused by changes in the temperature of the cooling medium.

[0068] As Figure 1 shown, in some embodiments of the present disclosure, the cooling fluid is a gas. In some embodiments, the gas includes but is not limited to air, nitrogen, etc. Using a gas as the cooling fluid, its specific heat capacity is small and the temperature response is fast. For example, when the flow rate of the cooling fluid changes, the cooling zone 150 will quickly respond to the change in the gas flow rate.

[0069] In some embodiments of the present disclosure, the cooling fluid may be dry compressed gas (such as compressed gas with a pressure of 0.2 - 1 MPa).

[0070] Figure 2 Shows a schematic structural diagram of a phosphorus cracking source 1000 according to some embodiments of the present disclosure.

[0071] As Figure 2 shown, in some embodiments of the present disclosure, the phosphorus cracking source 1000 may include a white phosphorus pool 200 and a temperature control device 100 for the phosphorus cracking source according to any one of the embodiments of the present disclosure. The cooling zone 150 surrounds the white phosphorus pool 200, and the temperature control device 100 for the phosphorus cracking source can control the temperature of the white phosphorus pool 200 through the cooling zone 150.

[0072] In some embodiments of the present disclosure, the temperature control device 100 for the phosphorus cracking source adjusts the temperature of the white phosphorus pool 200 by means of mixed temperature control, which can accurately and stably adjust the temperature of the white phosphorus pool 200 and expand the temperature control range of the white phosphorus pool 200. Therefore, during the phosphorus transfer process, the temperature difference between the red phosphorus pool and the white phosphorus pool can be increased, thereby improving the phosphorus transfer efficiency and providing a stable white phosphorus source beam. The stable white phosphorus vapor phosphorus source beam provided by accurately adjusting the temperature of the white phosphorus pool 200 can be easily used as a phosphorus source beam white phosphorus vapor source, such as for chemical vapor deposition, sputtering, vacuum deposition, and molecular beam epitaxy, etc.

[0073] As shown Figure 2 In some embodiments of the present disclosure, the phosphorus cracking source 1000 may further include a packaging structure 300. The packaging structure 300 is arranged to surround the white phosphorus pool 200, and a cooling zone 150 is formed inside the packaging structure 300. There is a gap between the outer wall of the white phosphorus pool 200 and the inner wall of the packaging structure 300, forming a cavity sandwich layer 310. The cavity sandwich layer 310 surrounds the white phosphorus pool 200 and is used to allow the cooling fluid to flow through, so as to cool the white phosphorus pool 200.

[0074] In some embodiments, the temperature sensor 131 may be installed outside the pool body of the white phosphorus pool 200. In some embodiments, as shown Figure 2 In some embodiments, the temperature sensor 131 may be installed outside the packaging structure 300. The temperature controller 132 receives the temperature signal of the temperature sensor 131, and based on the temperature signal output by the temperature sensor 131, controls the mass flow controller 140 to adjust the flow rate of the cooling fluid. In some embodiments, the temperature controller 132 adopts PID control, and the PID control will adjust the output of the controller through the change of the controlled object to form a closed-loop control loop. When the temperature sensor 131 senses the temperature of the white phosphorus pool 200 and feeds it back to the temperature controller 132, the temperature controller 132 will readjust the flow rate of the cooling fluid flowing through the mass flow controller 140 according to parameters such as the deviation between the temperature measurement value and the set value and the change trend of the measurement value. The adjustment of the cooling fluid flow rate changes the temperature of the white phosphorus pool 200, forming a negative feedback closed-loop control loop of "white phosphorus pool temperature - temperature controller - gas flow rate". This negative feedback regulation can enable the system to quickly respond to temperature changes, and at the same time can also adjust the temperature of the white phosphorus pool 200 to remain stable near the set value.

[0075] Figure 3 The structural schematic diagram of the packaging structure 300 according to some embodiments of the present disclosure is shown.

[0076] As shown Figure 3 In some embodiments of the present disclosure, the packaging structure 300 further includes at least one baffle (such as baffle 320a, baffle 320b, baffle 320c, baffle 320d) for separating the cavity sandwich layer 310 into multiple sandwich chambers. In some embodiments, baffle 320a and baffle 320b separate the packaging sandwich layer 310, and at least one through hole is provided on baffle 320b. Baffle 320c and baffle 320d separate the packaging sandwich layer 310, and at least one through hole is provided on baffle 320c. The cooling fluid can flow through at least one through hole on the baffle (such as baffle 320b, baffle 320c) between multiple sandwich chambers (for example, by flowing through different sandwich chambers in sequence) to cool the white phosphorus pool 200. Through the structural design of the baffle, the cooling fluid flows sufficiently in the cavity sandwich layer 310, improving the cooling efficiency and uniformity.

[0077] Those skilled in the art can understand that Figure 3 Although only four baffles (baffle 320a, baffle 320b, baffle 320c, baffle 320d) are shown, this is only exemplary, and the encapsulation structure 300 may also include other numbers of baffles. In some embodiments, a single integral baffle may be employed to separate the encapsulation interlayer 310. Similarly, appropriate numbers of through holes may be provided at corresponding positions on the baffle according to the design of the flow path of the cooling fluid.

[0078] In some embodiments of the present disclosure, as Figure 3 shown, the fluid pipeline 110 of the temperature control device for the phosphorus cracking source is in communication with the fluid inlet located at the top of the encapsulation structure 300 to guide the cooling fluid into the cooling zone 150. Moreover, the fluid pipeline 110 extends into the bottom of the encapsulation structure 300 to guide the cooling fluid out of the cooling zone 150. In other embodiments of the present disclosure, the fluid pipeline 110 may be in communication with the fluid outlet located at the bottom of the encapsulation structure 300. By staggeredly arranging the inlet and outlet of the cooling fluid, the flow path of the cooling fluid can be effectively set, enabling the cooling fluid to flow sufficiently and improving the heat exchange and cooling efficiency.

[0079] As Figure 2 shown, in some embodiments of the present disclosure, the phosphorus cracking source 1000 may further include a red phosphorus pool 400. The red phosphorus pool 400 is in communication with the white phosphorus pool 200 so that the red phosphorus vapor generated by the red phosphorus pool 400 can diffuse into the white phosphorus pool 200.

[0080] As Figure 2 shown, in some embodiments of the present disclosure, the phosphorus cracking source 1000 may further include a cracking zone 500. The cracking zone 500 is in communication with the white phosphorus pool 200.

[0081] In the traditional technology, in order to accurately control the gas flow rate, a high-precision mass flow controller (MFC) is usually adopted, but the MFC is not suitable for white phosphorus (P 4 ) vapor with strong corrosiveness. Therefore, a threaded leak valve is used instead. However, the threaded leak valve has a delay in switching. When the white phosphorus vapor flux is too large and the threaded leak valve is closed, the white phosphorus vapor in the pipeline cannot be discharged, and an additional exhaust pipeline is required to discharge the excess white phosphorus vapor in the pipeline, resulting in a complex structure and unable to achieve fast and accurate beam current regulation.

[0082] As Figure 2As shown, in some embodiments of the present disclosure, the phosphorus cracking source 1000 may further include a needle valve 600 and a stepper motor (not shown in the figure). The needle valve 600 is arranged on the connecting pipeline between the cracking zone 500 and the white phosphorus pool 200, and is used to control the flow rate of white phosphorus steam from the white phosphorus pool 200 to the cracking zone 500. The stepper motor is connected to the needle valve 600, and the gas flow rate of the needle valve 600 can be controlled by controlling the stepper motor. For example, the power output shaft of the stepper motor can be connected to the valve stem of the needle valve 600, and the gas flow rate of the needle valve 600 can be controlled by controlling the stepper motor.

[0083] In some embodiments of the present disclosure, a needle valve 600 driven by a high-precision stepper motor is used to replace a traditional threaded leakage valve, which has the advantages of good switching repeatability, convenient control, rapid feedback, and high opening positioning accuracy.

[0084] like Figure 2 As shown, in some embodiments of the present disclosure, when the phosphorus cracking source 1000 is in the phosphorus conversion state: the needle valve 600 is closed, the red phosphorus pool 400 is heated (for example, 300-400° C.), and the temperature of the white phosphorus pool 200 is set to ≤40° C. (for example, 35° C., 30° C., 25° C., etc.) through the thermostat 132. The red phosphorus vapor generated by the high temperature of the red phosphorus pool 400 diffuses through the connecting pipe between the red phosphorus pool 400 and the white phosphorus pool 200, and condenses in the white phosphorus pool 200 to form a high-purity white phosphorus solid.

[0085] In some embodiments of the present disclosure, when the phosphorus cracking source 1000 is in a general process use state: the temperature of the red phosphorus pool 400 is lowered (always higher than the temperature of the white phosphorus pool 200, for example, 150-300° C.), the temperature of the white phosphorus pool 200 is adjusted (usually 40-80° C.) to generate white phosphorus steam, the needle valve 600 is opened to allow the white phosphorus steam to pass through the pipeline to the cracking zone 500, and the P is heated at a high temperature (usually > 900° C.) in the cracking zone 500. 4 Thermal cracking occurs, and the resulting phosphorus source beam enters the vacuum processing chamber (e.g., Figure 6 The vacuum processing chamber 2000 shown is used for deposition of phosphorus-containing thin films.

[0086] It is generally believed that the greater the temperature difference between the white phosphorus pool 200 and the red phosphorus pool 400, the higher the white phosphorus collection efficiency. The more stable the temperature of the white phosphorus pool 200, the higher the stability of the white phosphorus source beam obtained. Therefore, there is a need for a phosphorus cracking source 1000 that can stably control the temperature of the white phosphorus pool 200 and increase the temperature difference between the red phosphorus pool 400 and the white phosphorus pool 200 as much as possible during phosphorus conversion. According to the phosphorus cracking source 1000 in some embodiments of the present disclosure, by changing the temperature of different regions (such as the white phosphorus pool 200 and the red phosphorus pool 400), the phosphorus conversion efficiency and phosphorus source beam stability can be controlled and adjusted.

[0087] Figure 4Shows the temperature change curve of the white phosphorus pool 200 during the 1000-turn phosphorus conversion process of the phosphorus cracking source according to some embodiments of the present disclosure.

[0088] In some embodiments of the present disclosure, a constant temperature water bath is used as the cold source of the cooling pool 120, the water bath temperature is set to a temperature between 0 - 20°C, and the temperature of the white phosphorus pool 200 is controlled at 30°C through the closed-loop control of the temperature controller 132 and the MFC140. The needle valve 600 is closed, the cracking zone 500 is raised to the cracking temperature (e.g., about 900 - 1000°C), and the red phosphorus pool is raised to the phosphorus conversion temperature (about 300 - 400°C) to start the phosphorus conversion. The temperature change of the white phosphorus pool 200 during the phosphorus conversion process is as Figure 4 shown. It can be seen that the temperature of the white phosphorus pool 200 is stably controlled within the range of 30 ± 0.1°C.

[0089] During the phosphorus conversion, although the white phosphorus pool 200 is continuously irradiated by the high temperature (about 300 - 400°C) of the red phosphorus pool 400, by using the temperature control device 100 for the phosphorus cracking source according to some embodiments of the present disclosure, the mixed temperature control method increases the heat capacity of the cooling circulation. Therefore, the temperature of the white phosphorus pool 200 can still remain stable at a low temperature (about 30°C), thereby improving the phosphorus conversion efficiency.

[0090] Figure 5 Shows the change curve of the phosphorus source beam stability of the phosphorus cracking source 1000 according to some embodiments of the present disclosure.

[0091] In some embodiments of the present disclosure, a constant temperature water bath is used as the cold source of the cooling pool 120, the water bath temperature is set to 0 - 20°C, the red phosphorus pool 400 is maintained at the standby temperature (about 200 - 300°C), the cracking zone 500 is raised to the cracking temperature (about 900 - 1000°C), the temperature of the white phosphorus pool 200 is controlled at 40 - 80°C through the closed-loop control of the temperature controller 132 and the MFC140, and the needle valve 600 is opened to a certain opening degree (e.g., the needle valve opening degree is 5% - 15%). At this time, a phosphorus source beam is generated from the outlet of the cracking zone 500, and the stability of the phosphorus source beam is tested by the beam current gauge (BFM) in the molecular beam epitaxy (MBE) chamber. As Figure 5 shown. It can be seen that the size of the phosphorus source beam is stably within the range of (2.75 ± 0.03)E-6 mbar within 60 minutes, and the beam fluctuation is better than ±1%.

[0092] Since the temperature control device 100 for the phosphorus cracking source according to some embodiments of the present disclosure can keep the temperature of the white phosphorus pool 200 stable for a long time, the finally obtained phosphorus source beam has good stability and high repeatability, providing a good basis for obtaining a phosphorus-containing thin film with good uniformity and repeatability in the process.

[0093] Figure 6 Shows the structural schematic diagram of the vacuum processing system 10000 according to some embodiments of the present disclosure.

[0094] As Figure 6 shown, in some embodiments of the present disclosure, the vacuum processing system 10000 may include a vacuum processing chamber 2000 and a phosphorus cracking source 1000 according to any one of the embodiments of the present disclosure. The phosphorus cracking source 1000 is vacuum-sealedly connected to the vacuum processing chamber 2000 and is configured to provide a phosphorus source beam to the vacuum processing chamber 2000.

[0095] It should be noted that the above are only exemplary embodiments of the present disclosure and are not intended to limit the present disclosure. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present disclosure shall be included within the protection scope of the present disclosure.

Claims

1. A temperature control device for a phosphorus cracking source, characterized in that: include: a fluid conduit for allowing a cooling fluid to flow into the cooling zone; as well as A cooling pool is used to accommodate at least a portion of the fluid pipeline to cool the cooling fluid in the fluid pipeline.

2. The temperature control device for a phosphorus cracking source according to claim 1, characterized in that: The fluid pipeline includes at least one section of coiled pipe, and the at least one section of coiled pipe is located in the cooling pool to cool the cooling fluid through the cooling pool.

3. The temperature control device for a phosphorus cracking source according to claim 1, characterized in that: Also included is a temperature control unit, the temperature control unit comprising: a temperature sensor, the temperature sensor being disposed in the cooling zone and configured to measure a temperature of the cooling zone; and A temperature controller, wherein a signal input end of the temperature controller is connected to the temperature sensor, and the temperature controller controls the flow rate of the cooling fluid in the fluid pipeline based on the temperature signal output by the temperature sensor.

4. The temperature control device for a phosphorus cracking source according to claim 3, characterized in that: It also includes a mass flow controller, which is arranged on the fluid pipeline and connected to the temperature controller. The mass flow controller is used to receive a control signal from the temperature controller and control the flow of the cooling fluid in the fluid pipeline based on the control signal.

5. The temperature control device for a phosphorus cracking source according to claim 1, characterized in that: The cooling pool comprises a cooling medium and / or a refrigerator; and / or The cooling fluid is a gas.

6. A phosphorus cracking source, characterized in that: include: white phosphorus pond; as well as According to the temperature control device for a phosphorus cracking source according to any one of claims 1 to 5, the cooling zone surrounds the white phosphorus pool, and the temperature control device for a phosphorus cracking source can control the temperature of the white phosphorus pool through the cooling zone.

7. The phosphorus cracking source according to claim 6, characterized in that: It also includes a packaging structure, which is configured to surround the white phosphorus pool. The interior of the packaging structure forms the cooling zone, and there is a gap between the outer wall of the white phosphorus pool and the inner wall of the packaging structure to form a cavity interlayer surrounding the white phosphorus pool for allowing cooling fluid to flow.

8. The phosphorus cracking source according to claim 7, characterized in that: The packaging structure also includes at least one baffle for dividing the cavity sandwich into a plurality of sandwich chambers. The baffle includes at least one through hole, and a cooling fluid flows through the at least one through hole between the plurality of sandwich chambers to cool the white phosphorus pool.

9. The phosphorus cracking source according to claim 7, characterized in that: The fluid pipeline of the temperature control device for the phosphorus cracking source is connected to the fluid inlet located at the top of the packaging structure, which is used to guide the cooling fluid to flow into the cooling zone, and the fluid pipeline is connected to the fluid outlet located at the bottom of the packaging structure or extends into the bottom of the packaging structure, which is used to guide the cooling fluid to flow out of the cooling zone.

10. The phosphorus cracking source according to claim 6, characterized in that: Also includes: a red phosphorus pool, the red phosphorus pool being connected to the white phosphorus pool so that the red phosphorus vapor generated by the red phosphorus pool can diffuse into the white phosphorus pool; and / or A cracking zone is connected to the white phosphorus pool.

11. The phosphorus cracking source according to claim 10, characterized in that: Also includes: A needle valve, disposed on the connecting pipeline between the cracking zone and the white phosphorus pool, for controlling the flow rate of white phosphorus steam flowing from the white phosphorus pool to the cracking zone; as well as A stepper motor is connected to the needle valve and is used to adjust the needle valve.

12. A vacuum processing system, characterized in that: include: Vacuum processing chamber; as well as The phosphorus cracking source according to any one of claims 6 to 11 is vacuum-sealed and connected to the vacuum processing chamber to provide a phosphorus source beam to the vacuum processing chamber.