Precursor sublimation testing device and testing method thereof

Abstract

The invention relates to a precursor sublimation test device and a test method thereof. The device comprises a sublimation furnace with a sublimation cavity; a first heater configured to heat the sublimation furnace; the exhaust pipe is communicated with the sublimation cavity; the exhaust pipe is provided with a first exhaust valve; the vacuum mechanism is configured to adjust the vacuum degree in the sublimation furnace; the vacuum mechanism is connected with an exhaust pipe; the first vacuum meter is arranged on the exhaust pipe between the first exhaust valve and the vacuum mechanism; the flow limiter is arranged on the exhaust pipe between the first vacuum meter and the first exhaust valve; a flow restrictor configured to restrict a flow within the exhaust pipe; the first weightometer is configured to weigh the sublimation furnace; and the controller is electrically connected with the first heater, the first exhaust valve, the vacuum mechanism, the first vacuum meter and the first weightometer. According to the technical scheme, the reliable testing device and method capable of obtaining sublimation production parameters are provided.

Description

Technical Field

[0001] This application relates to the field of semiconductor manufacturing, and in particular to a precursor sublimation testing apparatus and its testing method. Background Technology

[0002] Precursors are crucial raw materials in the semiconductor industry, primarily used in semiconductor thin-film deposition processes, including chemical vapor deposition (CVD), physical vapor deposition (PVD), atomic layer deposition (ALD), and other derivative deposition technologies. Solid-state precursors used for vapor deposition require extremely high purity, such as 99.99999%. This necessitates reliable solid-state precursor sublimation technology and equipment.

[0003] Although the principle of sublimation is the same, under different conditions, such as different temperatures, pressures, and reaction vessels, even for the same material, the parameters such as temperature, pressure, carrier gas supply rate, and saturated vapor pressure required for stable sublimation may vary greatly. Therefore, it is urgent to measure the parameters such as temperature, pressure, carrier gas supply rate, and saturated vapor pressure required for stable sublimation of different solid precursors before sublimation production. However, there is currently no reliable testing method in the industry.

[0004] The information disclosed in this background section is intended only to enhance the understanding of the overall background of the invention and should not be construed as an admission or in any way implying that the information constitutes prior art known to those skilled in the art. Summary of the Invention

[0005] In view of this, this application provides a precursor sublimation testing apparatus and a testing method thereof to solve at least one problem existing in the prior art.

[0006] To achieve the above objectives, the technical solution of this application is implemented as follows: In a first aspect, embodiments of this application provide a precursor sublimation testing apparatus, comprising: A sublimation furnace has a sublimation chamber; A first heater is configured to heat the sublimation furnace; An exhaust pipe is connected to the sublimation chamber; the exhaust pipe is equipped with a first exhaust valve. A vacuum mechanism is configured to adjust the vacuum level inside the sublimation furnace; the vacuum mechanism is connected to the exhaust pipe. A first vacuum gauge is installed on the exhaust pipe between the first exhaust valve and the vacuum mechanism; A flow limiter is disposed on the exhaust pipe between the first vacuum gauge and the first exhaust valve; configured to limit the flow rate within the exhaust pipe. A first weighing meter is configured to weigh the sublimation furnace. The controller is electrically connected to the first heater, the first exhaust valve, the vacuum mechanism, the first vacuum gauge, and the first weighing gauge.

[0007] In an alternative embodiment, the apparatus further includes: A carrier gas cylinder is configured to provide carrier gas for the sublimation furnace. An air inlet pipe connects the sublimation chamber and the carrier gas cylinder; the air inlet pipe is equipped with a first air inlet valve.

[0008] In an alternative embodiment, the apparatus further includes: A second heater is configured to heat the gas flowing out of the carrier gas cylinder, and the second heater is located between the carrier gas cylinder and the first inlet valve.

[0009] In an alternative embodiment, the vacuum mechanism includes: Vacuum pump; A buffer tank is disposed between the sublimation furnace and the vacuum pump; the exhaust pipe includes a first exhaust pipe and a second exhaust pipe, the first exhaust pipe connecting the sublimation furnace and the buffer tank, and the second exhaust pipe connecting the buffer tank and the vacuum pump; the first exhaust pipe is provided with a first exhaust valve, and the second exhaust pipe is provided with a second exhaust valve; A second vacuum gauge is configured to monitor the vacuum level inside the buffer tank.

[0010] In an alternative embodiment, the apparatus further includes: A first connecting pipe connects the exhaust pipe and the inlet pipe outside the sublimation furnace, so that the exhaust pipe and the inlet pipe are connected. A first pipeline valve is installed in the first connecting pipe to control the connection between the exhaust pipe and the intake pipe.

[0011] Secondly, this application provides a precursor sublimation testing method, applied to the precursor sublimation testing apparatus described above; the method includes: The sublimation furnace is heated according to the sublimation temperature of the precursor to be tested, so that the temperature inside the sublimation chamber is adapted to the sublimation requirements. The suction process is repeated multiple times: the sublimation furnace is connected to the vacuum mechanism for a first duration, and then disconnected for a first duration, so that the sublimation gas is repeatedly suctioned by the vacuum mechanism. Record the vacuum level in the exhaust pipe, and adjust the suction pressure of the vacuum mechanism according to the changes in the vacuum level in the exhaust pipe until the saturated vapor pressure of the precursor to be tested is determined.

[0012] In an optional implementation, the aspiration process further includes: Before the sublimation furnace is connected to the vacuum mechanism for a first period of time, a carrier gas step is added: Disconnect the sublimation furnace from the vacuum mechanism for a second duration, and connect the sublimation furnace to the carrier gas cylinder for a first duration; Disconnect the sublimation furnace from the carrier gas cylinder for a first duration.

[0013] In an alternative implementation, the method further includes: The changes in vacuum within the exhaust pipe with and without the addition of a carrier gas step are compared to determine the saturated vapor pressure of the precursor to be tested.

[0014] In an alternative implementation, the method further includes: After determining the saturated vapor pressure of the precursor to be tested, the sublimation chamber is set to multiple vacuum levels lower than the saturated vapor pressure to perform sublimation tests on the precursor to be tested. The sublimation rates of the precursor under test were obtained at multiple different vacuum levels.

[0015] In an alternative implementation, the method further includes: The carrier gas cylinders were set to multiple carrier gas velocities, and the precursor to be tested was subjected to a sublimation test. Obtain the sublimation rate of the precursor under test at multiple different carrier gas velocities.

[0016] The precursor sublimation testing apparatus and method provided in this application include: a sublimation furnace having a sublimation chamber; a first heater configured to heat the sublimation furnace; an exhaust pipe connected to the sublimation chamber; a first exhaust valve provided on the exhaust pipe; a vacuum mechanism configured to adjust the vacuum level inside the sublimation furnace; the vacuum mechanism is connected to the exhaust pipe; a first vacuum gauge disposed on the exhaust pipe between the first exhaust valve and the vacuum mechanism; a flow limiter disposed on the exhaust pipe between the first vacuum gauge and the first exhaust valve; configured to limit the flow rate inside the exhaust pipe; a first weighing meter configured to weigh the sublimation furnace; and a controller electrically connected to the first heater, the first exhaust valve, the vacuum mechanism, the first vacuum gauge, and the first weighing meter. As can be seen, the precursor sublimation testing apparatus and method of this application, by setting a programmable valve, a vacuum gauge, a flow limiter, etc., in the exhaust pipe of the sublimation chamber, and recording the changes in the vacuum level inside the exhaust pipe during repeated suction of the sublimation chamber, adjusts the suction pressure of the vacuum mechanism until the saturated vapor pressure of the precursor to be tested is determined. By using a determined saturated vapor pressure, further testing can be conducted to obtain other parameters of sublimation production, exhibiting accuracy and reliability. Therefore, the precursor sublimation testing apparatus and method of this application embodiment provide a reliable testing apparatus and method capable of obtaining parameters of sublimation production.

[0017] Additional aspects and advantages of this application will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of this application. Attached Figure Description

[0018] The accompanying drawings, which are included to provide a further understanding of this application and form part of this application, illustrate exemplary embodiments and are used to explain this application, but do not constitute an undue limitation of this application. In the drawings: Figure 1 A schematic diagram of the precursor sublimation testing apparatus provided in the embodiments of this application; Figure 2 A schematic diagram of the precursor sublimation testing device provided in the embodiments of this application; Figure 3 A schematic flowchart of the precursor sublimation test method provided in the embodiments of this application; Figure 4 This is a graph showing experimental data obtained from the precursor sublimation testing apparatus provided in the embodiments of this application.

[0019] Explanation of reference numerals in the attached figures: 10. Sublimation furnace; 11. First heater; 12. First weighing gauge; 13. First connecting pipe; 131. First pipeline valve; 14. Second connecting pipe; 141. Second pipeline valve; 142. Third pipeline valve; 143. Fourth pipeline valve; 21. First exhaust pipe; 211. First exhaust valve; 212. Flow limiter; 213. First vacuum gauge; 214. Eighth pipeline valve; 22. Second exhaust pipe; 221. Second exhaust valve; 31. Vacuum pump; 3 2. Buffer tank; 321. Second vacuum gauge; 40. Carrier gas cylinder; 41. Second weighing gauge; 51. First inlet pipe; 511. Carrier gas purifier; 512. Pressure regulating valve; 513. Flow meter; 514. Pressure sensor; 515. First inlet valve; 52. Second inlet pipe; 521. Coil; 522. Second inlet valve; 53. Third connecting pipe; 54. Fifth pipeline valve; 55. Sixth pipeline valve; 56. Seventh pipeline valve; 60. Second heater. Detailed Implementation

[0020] To make the technical solutions and beneficial effects of this application more obvious and understandable, the technical solutions in the embodiments of this application are clearly and completely described below by listing specific embodiments. Obviously, the embodiments of this application are not exhaustive, and the described embodiments are only some embodiments of this application, not all embodiments.

[0021] The exemplary embodiments disclosed in this application will now be described in more detail with reference to the accompanying drawings, providing detailed structures and steps to illustrate the technical solution of this application. Note that the drawings are not necessarily drawn to scale, and local features may be enlarged or reduced to more clearly show the details of the local features.

[0022] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application pertains. The terminology used herein is for the purpose of describing particular embodiments only and should not be construed as limiting the technical solutions of this application.

[0023] The following description provides numerous specific details to offer a more thorough understanding of this application. However, it will be apparent to those skilled in the art that this application can be practiced without one or more of these details. To clearly define the inventive concept of this application and avoid confusion with its content, technical features well-known in the art and conventionally understood by those skilled in the art are not elaborated upon. Specifically, this document does not fully list all features of actual embodiments, nor does it provide a detailed description of well-known functions and structures.

[0024] The applicant of this application discovered during the research and development that even for the same material, the parameters required for stable sublimation, such as temperature, pressure, carrier gas supply rate, and saturated vapor pressure, can vary significantly. For example, changing the type of sublimation furnace, or differences in pipe structure and diameter, can also lead to variations in these parameters, greatly affecting the efficiency of production (sublimation).

[0025] Therefore, based on further research and development by the applicant, the following technical solution was proposed.

[0026] To address the technical problems in related technologies, embodiments of this application provide a precursor sublimation testing apparatus. (Reference) Figure 1 and Figure 2 The precursor sublimation testing apparatus includes: Sublimation furnace 10 has a sublimation chamber; The first heater 11 is configured to heat the sublimation furnace 10; An exhaust pipe is connected to the sublimation chamber; the exhaust pipe is equipped with a first exhaust valve 211. A vacuum mechanism is configured to adjust the vacuum level inside the sublimation furnace 10; the vacuum mechanism is connected to the exhaust pipe. The first vacuum gauge 213 is installed on the exhaust pipe between the first exhaust valve 211 and the vacuum mechanism; A flow limiter 212 is disposed on the exhaust pipe between the first vacuum gauge 213 and the first exhaust valve 211; configured to limit the flow rate in the exhaust pipe. The first weighing scale 12 is configured to weigh the sublimation furnace 10; The controller is electrically connected to the first heater 11, the first exhaust valve 211, the vacuum mechanism, the first vacuum gauge 213, and the first weighing gauge 12.

[0027] Understandably, the sublimation furnace 10 is pre-filled with a sufficient amount of solid precursor to be tested for repeated testing during the sublimation test.

[0028] Understandably, the exhaust pipe is used to discharge the gas formed by sublimation in order to improve the vacuum level in the sublimation chamber, because the increase in gas after sublimation will reduce the original vacuum environment.

[0029] Understandably, the flow restrictor 212 can limit the flow rate of the airflow in the exhaust pipe, smooth out the changes in vacuum, and facilitate the vacuum measurement of the first vacuum gauge 213.

[0030] Specifically, the first heater 11 can use a high-precision heating element, such as a ceramic heating rod, which can achieve rapid and uniform heating and has a precise temperature control function. It can accurately control the temperature in the sublimation furnace 10 within a preset range of ±1℃ to meet the strict requirements of different precursors for sublimation temperature.

[0031] Specifically, the flow restrictor 212 can change the size and shape of the passage inside the exhaust pipe, for example, by setting a gasket with a small hole, which can be a conical hole, an arc hole, or other shapes.

[0032] Specifically, the flow restrictor 212 adopts a variable orifice structure, and its interior is equipped with a conical valve core driven by a stepper motor. The axial displacement of the conical valve core can adjust the effective flow area of ​​the exhaust pipe. The controller dynamically adjusts the opening of the conical valve core based on the weight change rate of the first weighing gauge 12, so that the exhaust pipe flow rate is always maintained within ±5% of the set value. For example, when the weight change rate exceeds the threshold, the controller increases the valve core opening to improve the suction efficiency; when approaching the saturated vapor pressure, it decreases the opening to stabilize vacuum fluctuations.

[0033] Understandably, a vacuum mechanism can simulate equipment that specifically uses precursors, such as a chemical vapor deposition (CVD) device. The preparation chamber of a CVD device is a vacuum environment, and during CVD, the precursor needs to be continuously used, i.e., the precursor in the exhaust pipe needs to be continuously pumped out. Therefore, this application embodiment uses a vacuum mechanism for simulation to conduct more accurate testing.

[0034] The first weighing gauge 12 can determine the progress of sublimation by weighing the sublimation furnace 10, i.e., how much weight has decreased, and thus how much mass of solid has been sublimated.

[0035] Specifically, the controller can be a PLC controller, which can quickly and programmatically control the opening and closing of the first exhaust valve 211, and can simultaneously notify the actions of multiple pipeline valves.

[0036] Specifically, the first exhaust valve 211 can be a double-acting cylinder + high-frequency solenoid valve: the high-frequency solenoid valve quickly switches the air path, and the double-acting cylinder works together to realize the rapid reciprocating motion of the valve core, so that the response time is <10ms.

[0037] Specifically, the first exhaust valve 211 can use a high-flow pneumatic head to increase the distance between cylinders and shorten the diaphragm stroke time.

[0038] Specifically, the first exhaust valve 211 can adopt a PFA (soluble polytetrafluoroethylene) diaphragm and a lightweight design.

[0039] Understandably, in addition to the first exhaust valve 211, other valves can be included in the device. This allows for rapid switching of valve states and more synchronized operation of each valve, thereby improving the accuracy of the measurement by the first vacuum gauge 213. It should be noted that synchronization does not necessarily mean simultaneous opening or closing. One valve can be open while the other is closed, or one can be open while the other waits a set time before opening, strictly adhering to the set time. The shorter the delay time, the higher the synchronization rate.

[0040] The precursor sublimation testing apparatus of this application embodiment, by installing programmable valves, vacuum gauges, flow restrictors 212, etc., in the exhaust pipe of the sublimation chamber, records the changes in the vacuum degree in the exhaust pipe during repeated suction cycles of the sublimation chamber, and adjusts the suction pressure of the vacuum mechanism until the saturated vapor pressure of the precursor to be tested is determined. By using the determined saturated vapor pressure, further testing can be conducted to obtain other parameters of sublimation production, exhibiting accuracy and reliability.

[0041] In some embodiments, the apparatus further includes: Carrier gas cylinder 40 is configured to treat the sublimation furnace 10 with carrier gas. An air inlet pipe connects the sublimation chamber and the carrier gas cylinder 40; the air inlet pipe is equipped with a first air inlet valve 515.

[0042] Using a carrier gas can significantly increase the sublimation rate of the precursor.

[0043] Similarly, the first intake valve 515 can also be electrically connected to the controller and controlled by the controller. Furthermore, the first intake valve 515 can also use the same specifications and model as the first exhaust valve 211 to make the operation more synchronized.

[0044] Specifically, the carrier gas can be an inert gas, such as nitrogen.

[0045] Specifically, the device also includes a second weighing gauge 41, which can measure the weight of the gas cylinder 40 to determine the amount of gas used and whether gas needs to be added.

[0046] In some embodiments, the apparatus further includes: The second heater 60 is configured to heat the gas flowing out of the gas cylinder 40, and the second heater 60 is located between the gas cylinder 40 and the first inlet valve 515.

[0047] To reduce the impact of the carrier gas on the temperature inside the sublimation chamber, the gas entering the sublimation chamber needs to be heated to bring it close to the temperature inside the sublimation chamber. Specifically, the second heater 60 can also be electrically connected to the controller and controlled by the controller.

[0048] Specifically, the air inlet pipe includes a first air inlet pipe 51 and a second air inlet pipe 52. The first air inlet pipe 51 connects the carrier gas cylinder 40 and the second heater 60. The second air inlet pipe 52 connects the sublimation furnace 10 and the second heater 60. The first air inlet pipe 51 is provided with a first air inlet valve 515, and the second air inlet pipe 52 is provided with a second air inlet valve 522.

[0049] In some embodiments, the vacuum mechanism includes: Vacuum pump 31; A buffer tank 32 is disposed between the sublimation furnace 10 and the vacuum pump 31; the exhaust pipe includes a first exhaust pipe 21 and a second exhaust pipe 22, the first exhaust pipe 21 connecting the sublimation furnace 10 and the buffer tank 32, and the second exhaust pipe 22 connecting the buffer tank 32 and the vacuum pump 31; the first exhaust pipe 21 is provided with a first exhaust valve 211, and the second exhaust pipe 22 is provided with a second exhaust valve 221; The second vacuum gauge 321 is configured to monitor the vacuum level inside the buffer tank 32.

[0050] Understandably, by setting up the vacuum pump 31 and the buffer tank 32, the equipment using the precursor can be simulated more accurately. This is because equipment using precursors, such as chemical vapor deposition equipment, also has a vacuum preparation chamber and a vacuum pump 31 to maintain that vacuum. The buffer tank 32 in this embodiment is used to simulate the preparation chamber, making the test results more accurate.

[0051] In some embodiments, the apparatus further includes: The first connecting pipe 13 connects the exhaust pipe and the inlet pipe outside the sublimation furnace 10, so that the exhaust pipe and the inlet pipe are connected. A first pipeline valve 131 is installed in the first connecting pipe 13 to control the connection between the exhaust pipe and the intake pipe.

[0052] The first connecting pipe 13 allows the exhaust pipe and the intake pipe to be directly connected without passing through the sublimation furnace 10. This allows for better control of the vacuum level within the intake pipe. For example, when necessary, the intake pipe can be directly evacuated by a vacuum mechanism.

[0053] A first pipeline valve 131 is provided in the first connecting pipe 13 to facilitate the control of pipeline opening and closing.

[0054] Furthermore, the device also includes a second connecting pipe 14, which is configured based on the first connecting pipe 13. The second connecting pipe 14 also connects to the exhaust pipe and the inlet pipe outside the sublimation furnace 10, but is closer to the sublimation furnace 10 than the first connecting pipe 13. In this way, even when the first pipe valve 131 is open, i.e., when the vacuum mechanism directly draws in the inlet pipe, the second inlet pipe 52 and the first exhaust pipe 21 of the sublimation furnace 10 can still be connected to the outside of the sublimation furnace 10, but not to other external pipes, such as the vacuum mechanism, so that the sublimation furnace 10 can establish an internal circulation and accelerate the sublimation process.

[0055] Specifically, establishing an internal circulation system requires additional pipe valves. For example, in addition to the existing first exhaust valve 211 and first intake valve 515 outside the sublimation furnace 10, a second pipe valve 141, a third pipe valve 142, and a fourth pipe valve 143 are added. The second pipe valve 141 is located on the second connecting pipe 14, while the other two are located on the second intake pipe 52 and the first exhaust pipe 21 outside the first connecting pipe 13, respectively. During internal circulation, the first intake valve 515, the first exhaust valve 211, and the second pipe valve 141 are all open to achieve circulation; the third pipe valve 142 and the fourth pipe valve 143 are closed to prevent gas outflow.

[0056] Furthermore, the device also includes a third connecting pipe 53, which connects the first intake pipe 51 and the second intake pipe 52. In this way, the first intake pipe 51 and the second intake pipe 52 can be directly connected without passing through the second heater 60. This allows for better control of the vacuum level of the second intake pipe 52; that is, the second intake pipe 52 can directly pass through the first intake pipe 51 without passing through the second heater 60, and then directly connect to the vacuum mechanism through the first exhaust pipe 21 without passing through the sublimation furnace 10, thus receiving suction from the vacuum mechanism.

[0057] Specifically, to enable the first intake pipe 51 and the second intake pipe 52 to be directly connected without passing through the second heater 60, the device further includes a fifth pipe valve 54, a sixth pipe valve 55, and a seventh pipe valve 56. The fifth pipe valve 54 is disposed on the third connecting pipe 53, and the sixth and seventh pipe valves 55 and 56 are respectively disposed on the intake and exhaust channels of the second heater 60, and are closer to the second heater 60 than the third connecting pipe 53. Thus, by opening the fifth pipe valve 54 and closing the sixth and seventh pipe valves 55 and 56, the goal of enabling the first intake pipe 51 and the second intake pipe 52 to be directly connected without passing through the second heater 60 can be achieved.

[0058] Furthermore, in order to better control the exhaust of the sublimation furnace 10, in addition to the first exhaust valve 211, an eighth pipeline valve 214 is also installed on the first exhaust pipe 21 near the buffer tank 32.

[0059] Furthermore, the device also includes a coil 521.

[0060] In this way, the spiral shape of the coil can prolong the passage time of nitrogen after heating, obtain a stable nitrogen output, reduce nitrogen flow fluctuations, and thus reduce the impact on the sublimation rate.

[0061] Furthermore, the apparatus also includes a carrier gas purifier 511 to remove impurities from the carrier gas. Specifically, when the carrier gas is nitrogen, the carrier gas purifier 511 is a nitrogen purifier. The carrier gas purifier 511 is located on the first inlet pipe 51 near the carrier gas cylinder 40 and before the first inlet valve 515. Here, "before" and "after" refer to the carrier gas cylinder 40 being in front and the sublimation furnace 10 being behind.

[0062] Furthermore, the device also includes a pressure regulating valve 512 for regulating the gas pressure of the first inlet pipe 51. It can be understood that regulating the gas pressure of the second inlet pipe 52 can also indirectly regulate the carrier gas velocity, thereby regulating the sublimation rate. The pressure regulating valve 512 is located on the second inlet pipe 52 between the carrier gas purifier 511 and the first inlet valve 515.

[0063] Specifically, the pressure regulating valve 512 is a back pressure type pressure regulating valve 512.

[0064] Furthermore, the device also includes a flow meter 513 for monitoring the carrier gas flow rate of the second intake pipe 52. The flow meter 513 is located between the pressure regulating valve 512 and the first intake valve 515.

[0065] Furthermore, the device also includes a pressure sensor 514 to monitor the air pressure within the first intake pipe 51. It is understood that the pressure sensor 514 and the pressure regulating valve 512 are used in combination for better performance. That is, the pressure regulating valve 512 adjusts the pressure based on the monitoring data from the pressure sensor 514. The pressure sensor 514 is located between the first intake valve 515 and the second heater 60.

[0066] This application also provides a precursor sublimation testing method, applied to the precursor sublimation testing apparatus described above; see reference. Figure 3 The method includes: Step 801: Heat the sublimation furnace 10 according to the sublimation temperature of the precursor to be tested, so that the temperature inside the sublimation chamber meets the requirements of sublimation. Step 802: Repeatedly perform the suction process: Connect the sublimation furnace 10 to the vacuum mechanism for a first duration, and then disconnect for a first duration, so that the sublimation gas is repeatedly suctioned by the vacuum mechanism; Step 803: Record the vacuum level in the exhaust pipe, and adjust the suction pressure of the vacuum mechanism according to the change in the vacuum level in the exhaust pipe until the saturated vapor pressure of the precursor to be tested is determined.

[0067] Understandably, in step 801, the sublimation temperature of each precursor to be tested has a certain reference range. Although it cannot be known precisely before the test, the approximate reference range can be known. The temperature is set according to this reference range.

[0068] Understandably, in step 802, only through repeated evacuation can the impact of sublimation on the vacuum level be understood more promptly.

[0069] Understandably, in step 803, if the vacuum level in the exhaust pipe does not change significantly during several adjacent suction processes, it can be said that the evaporation rate and the condensation rate have reached a dynamic equilibrium. The evaporation rate is the rate at which molecules on the solid surface continuously evaporate into the gas phase, and the condensation rate is the rate at which molecules in the gas phase continuously condense back into the solid phase.

[0070] Specifically, after each suction process, the controller calculates the rate of change of the vacuum degree of the exhaust pipe, ΔP / Δt. When the absolute value of ΔP / Δt is less than 0.1 Pa / s in three consecutive suction processes, and the weight change rate of the first weighing gauge 12 is less than 0.01 g / min, it is determined that evaporation and condensation have reached a dynamic equilibrium, and the vacuum degree recorded at this time can be determined as the saturated vapor pressure.

[0071] In the appendix Figure 2 In the specific embodiment shown, steps 802 and 803 above may include the following more specific steps: Step 8021: Control the third pipeline valve 142 and the second intake valve 522 to be normally closed; control the first exhaust valve 211 and the fourth pipeline valve 143 to be open for 6-12 seconds; control the first pipeline valve 131 and the second exhaust valve 221 to be closed for 6-12 seconds; control the eighth pipeline valve 214 to be open for 6-12 seconds. Note that the 6-12 seconds is a fixed value that can be set according to the actual situation, and all valves are the same. For example, according to the actual situation, if the first exhaust valve 211 and the fourth pipeline valve 143 are controlled to be open for 8 seconds, then the first pipeline valve 131 and the second exhaust valve 221 will also be controlled to be closed for 8 seconds.

[0072] Step 8022: Control the first exhaust valve 211 and the fourth pipeline valve 143 to close for 6-12 seconds; control the second exhaust valve 221 to open for 6-12 seconds.

[0073] Step 8023: Control the opening of the first pipeline valve 131 and the eighth pipeline valve 214 for 2-6 seconds.

[0074] Step 8024: Control the opening of the eighth pipeline valve 214 for 4-10 seconds.

[0075] Repeat the above steps and record the pressure curves of the first vacuum gauge 213 and the second vacuum gauge 321.

[0076] It should be noted that when a certain step is performed, all valves not involved in that step return to their initial state, i.e., the valves are closed.

[0077] In step 8023, without carrier gas, the pipes before the sublimation furnace, such as the second inlet pipe 52 and the first inlet pipe 51, are close to a vacuum state. The opening time of the first pipe valve 131 does not need to be too long, for example, 2 to 6 seconds, to achieve the required vacuum state.

[0078] The function of opening the first pipeline valve 131 is to increase the vacuum level in the pipeline between valve 56 and valve 142 and valve 131, thereby reducing the impact on the test.

[0079] In step 8024, since the pipeline between the outlet of sublimation furnace 10 and buffer tank 32 is relatively long, it takes a long time to evacuate the vacuum. Therefore, in step 8023, the eighth pipeline valve 214 is opened for 2-6 seconds, and in step 8024, the eighth pipeline valve 214 is opened for 4-10 seconds.

[0080] The precursor sublimation testing method of this application embodiment involves installing a programmable valve, vacuum gauge, and flow restrictor 212 in the exhaust pipe of the sublimation chamber. During repeated suction cycles of the sublimation chamber, the changes in vacuum level within the exhaust pipe are recorded, and the suction pressure of the vacuum mechanism is adjusted until the saturated vapor pressure of the precursor under test is determined. Based on the determined saturated vapor pressure, further testing is conducted to obtain other parameters for sublimation production.

[0081] In some embodiments, the aspiration process further includes: Before the sublimation furnace 10 is connected to the vacuum mechanism for a first period of time, a carrier gas addition step is performed: Disconnect the sublimation furnace 10 from the vacuum mechanism for a second duration, and connect the sublimation furnace 10 to the carrier gas cylinder 40 for a first duration; Disconnect the sublimation furnace 10 from the carrier gas cylinder 40 for a first duration.

[0082] Using a carrier gas can significantly increase the sublimation rate. Therefore, it is also necessary to test the relevant parameters of the carrier gas.

[0083] Specifically, a mass flow controller (MFC) is installed at the outlet of carrier gas cylinder 40. The target flow rate is dynamically adjusted by the controller based on the sublimation rate. For example, when the first weighing scale 12 shows that the weight is decreasing too quickly, the controller reduces the set flow rate of the MFC to prevent the precursor from being consumed too quickly; conversely, it increases the flow rate to accelerate sublimation. The flow accuracy of the MFC is ±1%FS, and the response time is ≤50ms. FS stands for full scale, meaning that the flow accuracy of the MFC is ±1% of the full scale.

[0084] In the appendix Figure 2 In the specific embodiment shown, after adding carrier gas, steps 802 and 803 above may include the following more specific steps: Step 80201: Control the third pipeline valve 142 and the second intake valve 522 to open for 6-12 seconds; control the first exhaust valve 211 and the fourth pipeline valve 143 to close for 6-12 seconds.

[0085] Step 80202: Control the first pipeline valve 131 to be normally closed, control the eighth pipeline valve 214 to be normally open; control the second exhaust valve 221 to be closed for 6-12 seconds.

[0086] Step 80203: Close the third pipeline valve 142 and the second intake valve 522 for 6-12 seconds.

[0087] Step 80204: Control the first exhaust valve 211 and the fourth pipeline valve 143 to open for 6-12 seconds.

[0088] Repeat the above steps and record the pressure curves of the first vacuum gauge 213 and the second vacuum gauge 321.

[0089] In some embodiments, the method further includes: The changes in vacuum within the exhaust pipe with and without the addition of a carrier gas step are compared to determine the saturated vapor pressure of the precursor to be tested.

[0090] This allows for a more accurate determination of the required saturated vapor pressure. Understandably, at the same temperature, the sublimation rate differs depending on whether there is a carrier gas or not. By adjusting the vacuum level, the time required for precursor sublimation at a fixed carrier gas rate can be determined. The test curves show that a lower vacuum level results in a shorter sublimation time for the same carrier gas rate. Therefore, the saturated vapor pressure obtained at this temperature is more meaningful for guiding production.

[0091] In some embodiments, the method further includes: After determining the saturated vapor pressure of the precursor to be tested, the sublimation chamber is set to multiple vacuum levels lower than the saturated vapor pressure to perform sublimation tests on the precursor to be tested. The sublimation rates of the precursor under test were obtained at multiple different vacuum levels.

[0092] In this way, an appropriate vacuum setting can be selected based on the test results to achieve a balance between sublimation rate and cost.

[0093] In some embodiments, the method further includes: The carrier gas cylinder 40 is set to multiple carrier gas velocities to perform a sublimation test on the precursor to be tested. Obtain the sublimation rate of the precursor under test at multiple different carrier gas velocities.

[0094] Similarly, based on the test results, an appropriate carrier gas velocity setting can be selected to achieve a balance between sublimation rate and cost.

[0095] Figure 4 This test measures the sublimation time under various gas pressures and carrier gas velocities. Sublimation time refers to the time required for complete sublimation; the longer the sublimation time, the slower the sublimation rate.

[0096] from Figure 4 It can be seen that, in terms of gas pressure, the lower the pressure, i.e., the higher the vacuum, the faster the sublimation rate. In terms of carrier gas velocity, the higher the carrier gas velocity, the faster the sublimation rate. Therefore, through... Figure 4 Appropriate gas pressure and carrier gas velocity can be selected to achieve a balance between sublimation rate and cost.

[0097] Figure 4In this context, the unit of pressure, or atmospheric pressure, is TORR. 1 TORR is equal to the pressure produced by 1 millimeter of mercury (mmHg) under standard gravitational acceleration, with a precise value of 133.322 Pascals (Pa). The unit of carrier gas velocity is SCCM, where 1 SCCM = 1 cubic centimeter per minute.

[0098] It should be noted that the various embodiments or implementation methods in this document can be described in a progressive manner, with each embodiment focusing on the differences from other embodiments. Similar or identical parts between embodiments can be referred to mutually. It should be understood that in the various embodiments of this application, the embodiment numbers are merely for descriptive purposes and do not represent the superiority or inferiority of the embodiments.

[0099] Understandably, without conflict, the technical features in the technical solutions described in each embodiment can be arbitrarily combined to form new embodiments. For example, each structure in each embodiment can be implemented as an independent embodiment, and the structures can be arbitrarily combined; some or all of the structures in different embodiments can be arbitrarily combined. Each step in each embodiment can be implemented as an independent embodiment, and the steps can be arbitrarily combined; the order of the steps can be arbitrarily interchanged; some or all of the steps in different embodiments can be arbitrarily combined. Furthermore, regarding the table in the embodiments, each element, each row, or each column in the table can be implemented as an independent embodiment.

[0100] In this document, when the terms "embodiment," "implementation," or "example" are used, it means that the specific features described in connection with these implementations or examples are included in at least one implementation, embodiment, or example of this application. It should be noted that the illustrative expressions of the above terms do not necessarily refer to the same implementation, embodiment, or example. Furthermore, the specific features described, such as structures or steps, can be appropriately combined in any one or more implementations, embodiments, or examples.

[0101] In some embodiments, prefixes such as "first" and "second" are used merely to distinguish different descriptive objects and do not impose restrictions on the position, order, priority, or value of the descriptive objects. The description of the descriptive objects is based on the context of the claims or embodiments, and the use of prefixes does not constitute unnecessary limitations. For example, the numerical value of the descriptive object is not limited by ordinal numbers and can be one or more. For instance, in "first device," the numerical value of "device" can be one or more. Furthermore, objects modified by different prefixes can be the same or different. For example, if the descriptive object is "device," then "first device" and "second device" can be the same device or different devices, and their types can be the same or different. Describing "first" does not necessarily imply the existence of "second," and discussing "second" does not necessarily imply the existence of "first."

[0102] In some embodiments, unless otherwise stated, elements expressed in the singular form, such as “a,” “the,” “the,” “the,” “the,” “the,” etc., can mean “one and only one,” or “one or more,” “at least one,” etc. For example, when using articles such as “a,” “an,” “the,” etc. in translation, the noun following the article can be understood as either a singular or a plural expression. In some embodiments, “multiple” refers to two or more.

[0103] In some embodiments, the terms “at least one of”, “one or more”, “a plurality of”, “multiple”, etc., may be used interchangeably.

[0104] In some embodiments, the notation "at least one of A and B", "A and / or B", "A in one case, B in another", "A in one case, B in another", etc., may include the following technical solutions depending on the situation: in some embodiments, A (A is executed regardless of B); in some embodiments, B (B is executed regardless of A); in some embodiments, execution is selected from A and B (A and B are selectively executed); in some embodiments, both A and B are executed. The same applies when there are more branches such as A, B, C, etc.

[0105] In some embodiments, the notation "A or B" may include the following technical solutions, depending on the situation: in some embodiments, A (execution of A regardless of B); in some embodiments, B (execution of B regardless of A); in some embodiments, selective execution from A and B (A and B are selectively executed). The same applies when there are more branches such as A, B, and C.

[0106] In some embodiments, unless otherwise expressly defined, the terms "installation," "connection," "linking," "fixing," "setting," etc., should be interpreted broadly. For example, "connection" can be a fixed connection, a detachable connection, or an integral part; it can be a mechanical connection, an electrical connection, or a communication connection; it can be a direct connection or an indirect connection through an intermediate medium; it can also refer to the internal communication of two components or the interaction between two components. Those skilled in the art can understand the specific meaning of the above terms in this embodiment according to the specific circumstances.

[0107] In some embodiments, the terms “center,” “longitudinal,” “lateral,” “length,” “width,” “thickness,” “height,” “up,” “down,” “front,” “rear,” “left,” “right,” “vertical,” “horizontal,” “top,” “bottom,” “inner,” “outer,” “clockwise,” and “counterclockwise” indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only used for the purpose of simplifying the description of this application and do not indicate that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. That is, they should not be construed as limitations on this application.

[0108] In some embodiments, unless otherwise expressly defined, "above" or "below" the second feature can mean that the first and second features are in direct contact, or indirect contact via an intermediate medium, or that they are not in contact, but simply indicate that the horizontal level of the first feature is higher than that of the second feature. Furthermore, "above" or "below" the second feature can mean that the first feature is directly above or diagonally above, directly below, or diagonally below the second feature.

[0109] In some embodiments, spatial relation terms such as “upper” and “lower” may be used for convenience of description to describe the relationship of one element or feature shown in the figures to other elements or features. It should be understood that, in addition to the orientation shown in the figures, spatial relation terms are intended to also include different orientations of the device in use and operation. For example, if the device in the figures is flipped, the description of an element or feature “below” other elements or features will change it to “upper” other elements or features. Therefore, the exemplary terms “upper” and “lower” can include both upper and lower orientations. The device may also be otherwise oriented (rotated 90 degrees or otherwise), and the spatial descriptive terms used herein will be interpreted accordingly.

[0110] It should be understood that the above embodiments are exemplary and are not intended to encompass all possible implementations of the technical solutions of this application. Various modifications and changes can be made to the above embodiments without departing from the scope of this application. Similarly, the various technical features of the above embodiments can be arbitrarily combined to form other embodiments of this application that may not be explicitly described. Therefore, the above embodiments only illustrate several implementations of this application and do not limit the scope of protection of this patent application. All other embodiments obtained by those skilled in the art based on the embodiments of this application without inventive effort are within the scope of protection of this application.

Claims

1. A precursor sublimation testing device, characterized in that, include: A sublimation furnace has a sublimation chamber; A first heater is configured to heat the sublimation furnace; The exhaust pipe is connected to the sublimation chamber; The exhaust pipe is equipped with a first exhaust valve; A vacuum mechanism is configured to adjust the vacuum level inside the sublimation furnace; the vacuum mechanism is connected to the exhaust pipe. A first vacuum gauge is installed on the exhaust pipe between the first exhaust valve and the vacuum mechanism; A flow limiter is installed on the exhaust pipe between the first vacuum gauge and the first exhaust valve; Configured to limit the flow rate within the exhaust pipe; A first weighing meter is configured to weigh the sublimation furnace. The controller is electrically connected to the first heater, the first exhaust valve, the vacuum mechanism, the first vacuum gauge, and the first weighing gauge.

2. The precursor sublimation testing apparatus according to claim 1, characterized in that, The device further includes: A carrier gas cylinder is configured to provide carrier gas for the sublimation furnace. An air inlet pipe connects the sublimation chamber and the carrier gas cylinder; the air inlet pipe is equipped with a first air inlet valve.

3. The precursor sublimation testing apparatus according to claim 2, characterized in that, The device further includes: A second heater is configured to heat the gas flowing out of the carrier gas cylinder, and the second heater is located between the carrier gas cylinder and the first inlet valve.

4. The precursor sublimation testing apparatus according to claim 2, characterized in that, The vacuum mechanism includes: Vacuum pump; A buffer tank is disposed between the sublimation furnace and the vacuum pump; the exhaust pipe includes a first exhaust pipe and a second exhaust pipe, the first exhaust pipe connecting the sublimation furnace and the buffer tank, and the second exhaust pipe connecting the buffer tank and the vacuum pump; the first exhaust pipe is provided with a first exhaust valve, and the second exhaust pipe is provided with a second exhaust valve; A second vacuum gauge is configured to monitor the vacuum level inside the buffer tank.

5. The precursor sublimation testing apparatus according to claim 4, characterized in that, The device further includes: A first connecting pipe connects the exhaust pipe and the inlet pipe outside the sublimation furnace, so that the exhaust pipe and the inlet pipe are connected. A first pipeline valve is installed in the first connecting pipe to control the connection between the exhaust pipe and the intake pipe.

6. A precursor sublimation testing method, applied to the precursor sublimation testing apparatus according to any one of claims 1-5; characterized in that, The method includes: The sublimation furnace is heated according to the sublimation temperature of the precursor to be tested, so that the temperature inside the sublimation chamber is adapted to the sublimation requirements. The suction process is repeated multiple times: the sublimation furnace is connected to the vacuum mechanism for a first duration, and then disconnected for a first duration, so that the sublimation gas is repeatedly suctioned by the vacuum mechanism. Record the vacuum level in the exhaust pipe, and adjust the suction pressure of the vacuum mechanism according to the changes in the vacuum level in the exhaust pipe until the saturated vapor pressure of the precursor to be tested is determined.

7. The precursor sublimation test method according to claim 6, characterized in that, The suction process also includes: Before the sublimation furnace is connected to the vacuum mechanism for a first period of time, a carrier gas step is added: Disconnect the sublimation furnace from the vacuum mechanism for a second duration, and connect the sublimation furnace to the carrier gas cylinder for a first duration; Disconnect the sublimation furnace from the carrier gas cylinder for a first duration.

8. The precursor sublimation test method according to claim 7, characterized in that, The method further includes: The changes in vacuum within the exhaust pipe with and without the addition of a carrier gas step are compared to determine the saturated vapor pressure of the precursor to be tested.

9. The precursor sublimation test method according to claim 6, characterized in that, The method further includes: After determining the saturated vapor pressure of the precursor to be tested, the sublimation chamber is set to multiple vacuum levels lower than the saturated vapor pressure to perform sublimation tests on the precursor to be tested. The sublimation rates of the precursor under test were obtained at multiple different vacuum levels.

10. The precursor sublimation test method according to claim 7, characterized in that, The method further includes: The carrier gas cylinders were set to multiple carrier gas velocities, and the precursor to be tested was subjected to a sublimation test. Obtain the sublimation rate of the precursor under test at multiple different carrier gas velocities.

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