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CN117947410B - Solid source allowance detection device and detection method thereof - Google Patents

Solid source allowance detection device and detection method thereof
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Publication number
CN117947410B
CN117947410BCN202410249478.1ACN202410249478ACN117947410BCN 117947410 BCN117947410 BCN 117947410BCN 202410249478 ACN202410249478 ACN 202410249478ACN 117947410 BCN117947410 BCN 117947410B
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temperature
source
measured
sensor
weighing sensor
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CN117947410A (en
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陈志敏
姚立柱
国政
张丛
李英万
姜瑞英
陈帅
聂翔
陈祥龙
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Qingdao Sirui Intelligent Technology Co ltd
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Qingdao Sifang Sri Intelligent Technology Co ltd
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Abstract

The invention belongs to the technical field of electronics, and discloses a solid source allowance detection device and a detection method thereof, wherein the solid source allowance detection device comprises a first detection device, a second detection device and a controller, the first detection device and the second detection device are fixed above a source bottle and are arranged in a lifting way, the first detection device and the second detection device respectively comprise an annular shell, a weighing sensor and a temperature sensor on the annular shell, one annular shell is respectively connected with an air inlet pipe of the source bottle and an air outlet of a carrier gas source in a sealing way, the other annular shell is respectively and hermetically connected with the gas outlet pipe of the source bottle and the gas inlet of the reaction chamber, and the controller is respectively and electrically connected with the weighing sensor and the temperature sensor and is used for calculating a weight compensation coefficient K according to the temperature measured by the temperature sensor and the weight measured by the weighing sensor and calculating the allowance W of the solid source in the source bottle according to the measured temperature, the measured weight and the weight compensation coefficient K. The influence of temperature and hardware on the detection result is reduced, and the detection precision is improved.

Description

Solid source allowance detection device and detection method thereof
Technical Field
The invention relates to the technical field of electronics, in particular to a solid source allowance detection device and a detection method thereof.
Background
Currently, thin film deposition reaction systems and methods are widely used in devices in a variety of fields, such as: semiconductors, integrated circuits, solar panels, flat panel displays, microelectronics, light emitting diodes, and the like. Among them, chemical vapor deposition (Chemical Vapour Deposition, CVD) technique and atomic layer deposition (Atomic Layer Deposition, ALD) technique are common thin film deposition methods.
The preparation of gaseous reaction precursors for either CVD or ALD reactions is predominantly accomplished by introducing a carrier gas (typically an inert gas) into a source bottle and carrying the reaction source (including liquid and solid sources) with the carrier gas into a reaction chamber.
Taking hafnium oxide (HfO2) as an example, which is a ceramic material with a wide band gap and a high dielectric constant, attention has been paid to the electronic field in recent years, and the specific structure of the hafnium oxide is most likely to replace the silicon dioxide (SiO2) of the gate insulating layer of the oxide semiconductor field effect transistor (MOSFET) of the core device of the existing silicon-based integrated circuit, so that the problem of size limitation of SiO2 in the conventional MOSFET is solved.
The preparation of HfO2 is accomplished using ALD process technology, which involves reacting a solid source hafnium tetrachloride (molecular formula: hfCl4) with an oxygen-containing species. Under the general condition, hfCl4 is a powdery colorless and crystalline inorganic compound with a melting point of 320 ℃, and the colorless solid is a precursor of most organohafnium compounds, can react strongly with water, has strong hygroscopicity and is very easy to hydrolyze, hfCl4 is stored in a solid source bottle in the ALD process, an air inlet and an air outlet are formed in the upper side of the source bottle, carrier gas is introduced into the air inlet, and the solid source is brought into a reaction chamber in a gas carrying mode to react in the reaction chamber.
In order to make the gas fully carry the solid source into the reaction chamber for reaction, most of the solid source is adsorbed in the source bottle in the form of particles or powder, and the internal structure of the source bottle is provided with a plurality of groups of grooves for loading the solid source, as shown in fig. 1, fig. 1 is a schematic structural diagram of the existing solid source residue detection device, and the detection method is as follows: the source bottle 5 with the solid source is placed on a detection platform 7 with a weighing sensor at the bottom, the solid source in the source bottle 5 is volatilized into a gas state by heating through a heating sleeve 6 wrapped outside the source bottle 5, then carrier gas is introduced from the gas inlet pipe 1, the solid source is carried out of the gas outlet pipe 3 in a gas carrying mode, and the solid source is introduced into the reaction chamber. Along with the introduction of carrier gas, the number of solid sources in the source bottle 5 is gradually reduced, and after the reduction, the change value can be checked through the detection platform 7 and the detection value is transmitted to an upper computer for recording. In order to realize that the source bottle 5 floats up and down due to the loss of the solid source, a first corrugated pipe 8 is connected at the air inlet pipe 1, and a second corrugated pipe 9 is connected at the air outlet pipe 3 for adjustment; when the air inlet valve 2 and the air outlet valve 4 are opened in the process, the total mass of the source bottle, the heating jacket, the solid source, the air inlet pipe, the air outlet pipe, the air inlet valve and the air outlet valve is lightened along with the loss of the solid source, and gradually floats upwards, and the first corrugated pipe 8 and the second corrugated pipe 9 deform.
In the measurement process, the sizes of the first corrugated pipe 8 and the second corrugated pipe 9 are changed along with the reduction of the solid source, so that the numerical value detected by the bottom detection platform 7 is not the allowance of the actual solid source, besides, the actual temperature of the source bottle and the surrounding environment is not room temperature (exceeds the rated use temperature of the detection platform) due to the fact that the source bottle 5 is wrapped by the heating sleeve 6, the influence of temperature drift on the measurement result cannot be overcome by the detection platform, and the actual allowance of the solid source cannot be accurately detected by the detection mode due to the superposition of the two irresistible factors.
Disclosure of Invention
Aiming at the defects of the prior art, the invention innovatively provides a solid source allowance detection device and a detection method thereof, which can effectively overcome measurement errors caused by temperature change and corrugated pipe deformation, and eliminate the influence of temperature on a weight detection result by utilizing a weight compensation coefficient; the weighing mode is changed into hoisting weighing, so that the corrugated pipe can be completely replaced, the influence of hardware on a detection result is reduced to the greatest extent, and the detection precision is improved; the detection device can be directly used on the existing source bottle, does not change the installation form of the existing source bottle and devices on the existing source bottle, and is simple and convenient to use.
To achieve the above technical object, a first aspect of the present invention discloses a solid source residue detecting device, comprising a first detecting device, a second detecting device and a controller,
The first detection device and the second detection device are fixed above the source bottle, the first detection device and the second detection device are arranged in a hoisting way,
The first detection device comprises a first annular shell, a first weighing sensor and a first temperature sensor, wherein the first weighing sensor and the first temperature sensor are fixed on the first annular shell, the first annular shell is respectively connected with an air inlet pipe of a source bottle and an air outlet of a carrier gas source in a sealing way,
The second detection device comprises a second annular shell, a second weighing sensor and a second temperature sensor, wherein the second weighing sensor and the second temperature sensor are fixed on the second annular shell, the second annular shell is respectively connected with an air outlet pipe of a source bottle and an air inlet of a reaction chamber in a sealing way,
The first weighing sensor and the second weighing sensor are used for detecting the weight of a source bottle, a heating sleeve, an air inlet pipe, an air outlet pipe, an air inlet valve, an air outlet valve and a solid source in the source bottle below the first weighing sensor and the second weighing sensor, the first temperature sensor and the second temperature sensor are respectively used for detecting the temperature of the position where the first temperature sensor and the second temperature sensor are positioned,
The controller is electrically connected with the first weighing sensor, the second weighing sensor, the first temperature sensor and the second temperature sensor respectively, and is used for calculating a weight compensation coefficient K according to the temperature measured by the first temperature sensor, the temperature measured by the second temperature sensor, the weight measured by the first weighing sensor and the weight measured by the second weighing sensor, and calculating the allowance W of the solid source in the source bottle according to the temperature measured by the first temperature sensor, the temperature measured by the second temperature sensor, the weight measured by the first weighing sensor, the weight measured by the second weighing sensor and the weight compensation coefficient K.
Further, the first annular shell is in sealing connection with an air outlet of the carrier air source through an air inlet pipeline, the second annular shell is in sealing connection with an air inlet of the reaction chamber through an air outlet pipeline, and the air inlet pipeline and the air outlet pipeline are both rigid pipelines.
Further, the controller is further configured to calculate a solid source usage amount W0 required by a process, and determine whether the current solid source allowance W in the source bottle meets the requirement of a next process.
Further, the device also comprises an alarm, wherein the alarm is electrically connected with the controller and is used for alarming when the solid source allowance W in the current source bottle cannot meet the next process.
Further, the method for calculating the weight compensation coefficient K by the controller according to the temperature measured by the first temperature sensor, the temperature measured by the second temperature sensor, the weight measured by the first weighing sensor and the weight measured by the second weighing sensor includes:
When a solid source is not added into a source bottle, gradually heating from room temperature to a first temperature which is larger than or equal to a process temperature, dividing a temperature interval between the first temperature and the room temperature into n equal divisions, wherein n is larger than or equal to 3 and n is an integer, acquiring the sum W1 and Wn of weights measured by the first weighing sensor and the second weighing sensor respectively when the room temperature and each equal division node temperature are respectively increased from the room temperature to the first temperature, wherein the node temperature is an average value of the temperatures measured by the first temperature sensor and the second temperature sensor or the temperature measured by the second temperature sensor, a weight compensation value DeltaW at a certain node temperature is obtained by a difference value W1 and Wn at the certain node temperature, and drawing a linear relation graph by taking the difference DeltaT of the node temperature and the room temperature as a horizontal coordinate and the weight compensation value DeltaW at the node temperature as a vertical coordinate, and the slope of the linear relation graph is a weight compensation coefficient K.
Further, the method for calculating the residual W of the solid source in the source bottle by the controller according to the temperature measured by the first temperature sensor, the temperature measured by the second temperature sensor, the weight measured by the first weighing sensor, the weight measured by the second weighing sensor and the weight compensation coefficient K comprises the following steps:
Obtaining the sum W1 of the weights measured by the first weighing sensor and the second weighing sensor when the solid source is not added in the source bottle at room temperature;
Acquiring the sum W2 of the weights measured by the first weighing sensor and the second weighing sensor at the current temperature in the process or after the process is finished; the current temperature is the average value of the temperatures measured by the first temperature sensor and the second temperature sensor or the temperature measured by the second temperature sensor;
Calculating a temperature difference DeltaT: Δt=t-T0, where T is the current temperature and T0 is room temperature;
Calculating the solid source allowance W in the source bottle: w=w2+K*△T-W1.
To achieve the above object, a second aspect of the present invention discloses a solid source balance detecting method using the above solid source balance detecting device, comprising the steps of:
calculating weight compensation coefficients K at different temperatures;
Obtaining the total mass W1 of a source bottle, a heating sleeve, an air inlet pipe, an air outlet pipe, an air inlet valve and an air outlet valve at room temperature;
Obtaining the sum W1 of the weights measured by the first weighing sensor and the second weighing sensor when the solid source is not added in the source bottle at room temperature;
acquiring the sum W2 of the weights measured by the first weighing sensor and the second weighing sensor at the current temperature in the process or after the process is finished, wherein the current temperature is the average value of the temperatures measured by the first temperature sensor and the second temperature sensor or the temperature measured by the second temperature sensor;
Calculating a temperature difference DeltaT: Δt=t-T0, where T is the current temperature and T0 is room temperature;
calculating the solid source allowance W in the source bottle: w=w2+K△T-W1.
Further, calculating the weight compensation coefficient K includes:
When a solid source is not added into a source bottle, gradually heating from room temperature to a first temperature which is larger than or equal to a process temperature, dividing a temperature interval between the first temperature and the room temperature into n equal divisions, wherein n is larger than or equal to 3 and n is an integer, acquiring the sum W1 and Wn of weights measured by the first weighing sensor and the second weighing sensor respectively when the room temperature and each equal division node temperature are respectively increased from the room temperature to the first temperature, wherein the node temperature is an average value of the temperatures measured by the first temperature sensor and the second temperature sensor or the temperature measured by the second temperature sensor, a weight compensation value DeltaW at a certain node temperature is obtained by a difference value W1 and Wn at the certain node temperature, and drawing a linear relation graph by taking the difference DeltaT of the node temperature and the room temperature as a horizontal coordinate and the weight compensation value DeltaW at the node temperature as a vertical coordinate, and the slope of the linear relation graph is a weight compensation coefficient K.
Further, the method also comprises the step of judging whether the solid source allowance W in the current source bottle meets the requirement of the next process.
Further, the determining whether the solid source allowance W in the current source bottle meets the requirement of the next process includes:
obtaining the solid source dosage W0 required by the primary process at the process temperature;
And judging whether the difference value between the solid source allowance W and the solid source allowance W0 is larger than or equal to zero, if so, carrying out the next process, otherwise, giving an alarm.
The beneficial effects of the invention are as follows:
The solid source allowance detection device and the detection method thereof can effectively overcome measurement errors caused by temperature change and corrugated pipe deformation, and eliminate the influence of temperature on a weight detection result by using a weight compensation coefficient; the weighing mode is changed into hoisting weighing, so that the corrugated pipe can be completely replaced, the influence of hardware on a detection result is reduced to the greatest extent, and the detection precision is improved; the detection device can be directly used on the existing source bottle, does not change the installation form of the existing source bottle and devices on the existing source bottle, and is simple and convenient to use.
Drawings
Fig. 1 is a longitudinal sectional view of a conventional solid source residue detection device.
Fig. 2 is a longitudinal cross-sectional view of a solid-state source balance detection device according to an embodiment of the present invention.
Fig. 3 is a schematic structural diagram of a first detection device and a second detection device according to an embodiment of the present invention.
In the drawing the view of the figure,
1. An air inlet pipe; 2. an intake valve; 3. an air outlet pipe; 4. an air outlet valve; 5. a source bottle; 6. a heating jacket; 7. a detection platform; 8. a first bellows; 9. a second bellows; 10. a first detection device; 101. a first annular housing; 102. a first temperature sensor; 103. a first cable; 11. a second detection device; 111. a second annular housing; 112. a second temperature sensor; 113. a second cable; 12. an air intake line; 13. and an air outlet pipeline.
Detailed Description
The solid source balance detection device and the detection method thereof provided by the invention are explained and illustrated in detail below with reference to the accompanying drawings.
The source bottle 5 is used for holding solid source, and the outer parcel of source bottle 5 has heating jacket 6, and the top of source bottle 5 is connected with intake pipe 1 and outlet duct 3, is equipped with admission valve 2 on the intake pipe 1, is equipped with air outlet valve 4 on the outlet duct 3, and the solid source surplus detection device of this embodiment is installed on the top of intake pipe 1 and outlet duct 3 for detect the surplus of solid source in the source bottle 5. The above-described apparatus is typically housed within a source cabinet.
The embodiment specifically discloses a solid source allowance detection device, as shown in fig. 2-3, including a first detection device 10, a second detection device 11 and a controller, the first detection device 10 and the second detection device 11 are fixed above the source bottle 5, and the first detection device 10 and the second detection device 11 are lifted and arranged.
The first detection device 10 comprises a first annular shell 101, a first weighing sensor and a first temperature sensor 102, wherein the first weighing sensor and the first temperature sensor 102 are fixed on the first annular shell 101, and the first annular shell 101 is respectively and hermetically connected with the air inlet pipe 1 of the source bottle 5 and the air outlet of the carrier gas source. As shown in fig. 3, the first annular housing 101 includes a top plate, an inner ring and an outer ring, the top plate is annular and fixed at the top of the inner ring and the outer ring, the inner side of the top plate is fixedly connected with the inner ring, the outer side of the top plate is fixedly connected with the outer ring, the top plate and the inner ring and the outer ring enclose a U-shaped annular groove, the notch of the U-shaped annular groove faces downwards, the first temperature sensor 102 and the first weighing sensor are fixed in the U-shaped annular groove, the first weighing sensor is connected with the air inlet pipe 1 and used for detecting the weight of a device below the first weighing sensor, the lifting manner is adopted for weighing, and the detection result is accurate and is not influenced by other devices. The first temperature sensor 102 is in contact with the end part of the air inlet pipe 1 or is positioned in the air inlet of the air inlet pipe 1, the air inlet of the air inlet pipe 1 is communicated with the inner ring of the first annular shell 101, the air outlet of the carrier gas source is positioned above the first annular shell 101, the inner ring of the first annular shell 101 is communicated with the air outlet of the carrier gas source, and the carrier gas source enters the source bottle 5 through the inner ring of the first annular shell 101 and the air inlet pipe 1.
The second detection device 11 comprises a second annular shell 111, a second weighing sensor and a second temperature sensor 112, wherein the second weighing sensor and the second temperature sensor 112 are fixed on the second annular shell 111, and the second annular shell 111 is respectively and hermetically connected with the air outlet pipe 3 of the source bottle 5 and the air inlet of the reaction chamber. The structure of the second detection device 11 is the same as that of the first detection device 10, as shown in fig. 3, the second annular shell 111 comprises a top plate, an inner ring and an outer ring, the top plate is annular and fixed at the top of the inner ring and the outer ring, the inner side of the top plate is fixedly connected with the inner ring, the outer side of the top plate is fixedly connected with the outer ring, the top plate and the inner ring and the outer ring enclose a U-shaped annular groove, the notch of the U-shaped annular groove faces downwards, the second temperature sensor 112 and the second weighing sensor are fixed in the U-shaped annular groove, the second weighing sensor is connected with the air outlet pipe 3 and used for detecting the weight of a device below the second weighing sensor, the lifting manner is adopted for weighing, and the detection result is accurate and is not influenced by other devices. The second temperature sensor 112 is in contact with the end part of the air outlet pipe 3 or is positioned in the air outlet of the air outlet pipe 3, the air outlet of the air outlet pipe 3 is communicated with the inner ring of the second annular shell 111, the air inlet of the reaction chamber is positioned above the second annular shell 111, the inner ring of the second annular shell 111 is communicated with the air inlet of the reaction chamber, and the gas carrying solid source is discharged from the air outlet pipe, passes through the inner ring of the second annular shell 111 and enters the reaction chamber from the air inlet of the reaction chamber.
The first weighing sensor and the second weighing sensor are used for detecting the weight of the source bottle 5, the heating jacket 6, the air inlet pipe 1, the air outlet pipe 3, the air inlet valve 2, the air outlet valve 4 and the solid source in the source bottle 5, a hoisting weighing mode is adopted, only the source bottle 5, the heating jacket 6, the air inlet pipe 1, the air outlet pipe 3, the air inlet valve 2, the air outlet valve 4 and the solid source in the source bottle 5 are arranged below the weighing sensors, the weight of the devices is measured every time, the influence of measuring errors caused by deformation of a corrugated pipe and other devices on a measuring result is effectively overcome, and the measuring precision is higher. The first temperature sensor 102 and the second temperature sensor 112 are respectively used for detecting the temperature of the place where they are located. The controller is electrically connected with the first weighing sensor, the second weighing sensor, the first temperature sensor 102 and the second temperature sensor 112 respectively, and is used for receiving and processing data measured by the first weighing sensor, the second weighing sensor, the first temperature sensor 102 and the second temperature sensor 112, calculating a weight compensation coefficient K according to the temperature measured by the first temperature sensor 102, the temperature measured by the second temperature sensor 112, the weight measured by the first weighing sensor and the weight measured by the second weighing sensor, and calculating the allowance W of the solid source in the source bottle 5 according to the temperature measured by the first temperature sensor 102, the temperature measured by the second temperature sensor 112, the weight measured by the first weighing sensor, the weight measured by the second weighing sensor and the weight compensation coefficient K.
The first temperature sensor, the second temperature sensor, the first weighing sensor, the second weighing sensor, the first annular shell and the second annular shell are all fixed in the source cabinet together with the source bottle, the controller is fixed outside the source cabinet, the first temperature sensor 102 and the first weighing sensor are connected with the controller outside the source cabinet through a first cable 103 penetrating through the outer ring of the first annular shell 101, the second temperature sensor 112 and the second weighing sensor are connected with the controller outside the source cabinet through a second cable 113 penetrating through the outer ring of the second annular shell 111, the first cable 103 and the second cable 113 adopt high-temperature flexible cables, detected temperature signals and weight signals are transmitted to the controller, and the controller performs operation processing.
The first weighing sensor and the second weighing sensor of the embodiment are of a high temperature resistant type, and can normally work in a high temperature environment.
The data transmission and processing method of the conventional solid-state source balance detection device shown in fig. 1 is as follows:
The weighing controller of the detection platform 7 measures the total weight of substances borne above the weighing sensor (including the weight of a solid source, a source bottle, a heating jacket, an air inlet valve, an air outlet valve and the soft connection weight of the first corrugated pipe and the second corrugated pipe), and transmits the measurement result to the main controller in a signal form through operation; meanwhile, as the weighing controller needs to calculate the measurement data and then send the measurement data to the main controller, the time factors of data sending and sampling are considered, so that the numerical value on the weighing sensor acquired by the main controller is delayed; greatly reduces the utilization rate of the equipment.
The data transmission and processing method of the application comprises the following steps:
the weighing sensor of the application is of a high temperature resistant type, can normally work in a high temperature environment, cancels the original weighing controller, directly collects initial signals to the controller, collects weight and temperature signals through the controller, the method has the advantages that the method can directly collect and process the signals, reduce the communication processing time of the equipment, at the moment, the data collected by the controller is the current value of the weighing sensor, and the weight compensation of the collected value is completed due to the addition of the temperature signals, so that the measurement accuracy is improved; in addition, the controller is not arranged in the source cabinet, so that the damage to the controller caused by high temperature is reduced; the utilization rate of the equipment is improved.
The embodiment introduces the weight compensation coefficient K to eliminate the influence of temperature change on the weight detection result, and the detection result is more accurate.
The detection device provided by the application has a simple structure, can be directly installed on the structure of the existing source bottle 5, does not need to change the installation form of the existing source bottle 5 and devices thereon, and is simple and convenient to use.
Optionally, the first annular housing 101 is connected with the gas outlet of the carrier gas source in a sealing manner through a gas inlet pipeline 12, the second annular housing 111 is connected with the gas inlet of the reaction chamber in a sealing manner through a gas outlet pipeline 13, and the gas inlet pipeline 12 and the gas outlet pipeline 13 are both rigid pipelines. The air inlet pipeline 12 is fixed above the first annular shell 101, the bottom end of the air inlet pipeline 12 is in sealing connection with the first annular shell 101, the air inlet pipeline 12 is communicated with the inner ring of the first annular shell 101, and the top end of the air inlet pipeline 12 is in sealing connection with the air outlet of the carrier gas source; the air outlet pipeline 13 is fixed above the second annular shell 111, the bottom end of the air outlet pipeline 13 is connected with the second annular shell 111 in a sealing way, the air outlet pipeline 13 is communicated with the inner ring of the second annular shell 111, and the top end of the air outlet pipeline 13 is connected with the air inlet of the reaction chamber in a sealing way. In the prior art, the residual solid source can appear between the gaps of the corrugated pipes in the long-term use process due to the introduction of the corrugated pipes, and part of particles can be inevitably caused to enter the reaction chamber during the passing of carrier gas, so that the problem of indistinguishable particles is caused. The air outlet pipeline 13 and the air inlet pipeline 12 are rigid pipelines, so that the condition that particles at the joint part enter the reaction chamber due to deformation is avoided. Preferably, both the inlet pipe 12 and the outlet pipe 13 are smooth surfaces.
The first detection device 10 and the second detection device 11 can be hung in the source cabinet through a hanging rope, and can be hung below the carrier gas source and the reaction chamber through the gas inlet pipeline 12 and the gas outlet pipeline 13, and the hanging of the first detection device 10, the second detection device 11 and the source bottle 5, the gas inlet pipe 1, the gas inlet valve 2, the gas outlet pipe 3, the gas outlet valve 4 and the heating jacket 6 below the first detection device and the second detection device can be realized through the gas inlet pipeline 12 and the gas outlet pipeline 13, so that hanging weighing is realized, weighing is more accurate, and the influence of other devices is avoided.
Further, the method for calculating the weight compensation coefficient K by the controller according to the temperature measured by the first temperature sensor 102, the temperature measured by the second temperature sensor 112, the weight measured by the first load cell and the weight measured by the second load cell includes:
When a solid source is not added into the source bottle 5, gradually heating from room temperature to a first temperature, wherein the first temperature is greater than or equal to a process temperature, dividing a temperature interval between the first temperature and the room temperature into n equal divisions, wherein n is greater than or equal to 3 and n is an integer, respectively obtaining the sum W1 and Wn of weights measured by a first weighing sensor and a second weighing sensor when the room temperature is heated to the first temperature and each equal division node temperature, wherein the node temperature is the average value of the temperatures measured by the first temperature sensor 102 and the second temperature sensor 112 or the temperature measured by the second temperature sensor 112, the difference between W1 and Wn at a certain node temperature is obtained, the weight compensation value DeltaW at the node temperature is drawn by taking the difference DeltaT between the node temperature and the room temperature as an abscissa, the weight compensation value DeltaW at the node temperature as a longitudinal linear relation graph, and the slope of the linear relation graph is a weight compensation coefficient K.
Preferably, n is 5, so that the result of the calculation is more accurate.
The process temperatures of different solid sources are different, taking the highest process temperature as 200 ℃ as an example, the first temperature can be set to 220 ℃, when the solid source is not added in the source bottle 5, the temperature is gradually increased to 220 ℃ from the room temperature of 20 ℃, the sum of the weights measured by the first weighing sensor and the second weighing sensor is recorded at the room temperature, 60 ℃,100 ℃, 140 ℃, 180 ℃ and 220 ℃ respectively in the heating process, the difference between the sum of the weights measured by the two weighing sensors at the room temperature and the sum of the weights measured by the two weighing sensors at the node temperature is the weight compensation value DeltaW of the node temperature, the node temperature is based on the average value of the temperatures measured by the first temperature sensor 102 and the second temperature sensor 112 or the temperature measured by the second temperature sensor 112, a linear relation graph is drawn by taking the difference DeltaT between the node temperature and the room temperature as an abscissa and the weight compensation value DeltaW at the node temperature as an ordinate, and the slope of the linear relation graph is the weight compensation coefficient K.
Further, the method for calculating the residual W of the solid source in the source bottle 5 according to the temperature measured by the first temperature sensor 102, the temperature measured by the second temperature sensor 112, the weight measured by the first weighing sensor, the weight measured by the second weighing sensor and the weight compensation coefficient K by the controller comprises the following steps:
Obtaining the sum W1 of the weights measured by the first weighing sensor and the second weighing sensor when the solid source is not added in the source bottle at room temperature, namely the total mass W1 of the source bottle 5, the heating jacket 6, the air inlet pipe 1, the air outlet pipe 3, the air inlet valve 2 and the air outlet valve 4 at room temperature;
After the temperature is raised to the process temperature, an air inlet valve 2 is opened, carrier gas is continuously introduced into a source bottle 5, an air outlet valve 4 is opened, and a solid source carried by the carrier gas is continuously introduced into a reaction chamber for processing; acquiring the sum W2 of the weights measured by the first weighing sensor and the second weighing sensor at the current temperature in the process or after the process is finished; wherein the current temperature is an average value of temperatures measured by the first temperature sensor 102 and the second temperature sensor 112 or a temperature measured by the second temperature sensor 112;
Calculating a temperature difference DeltaT: Δt=t-T0, where T is the current temperature and T0 is room temperature;
Calculating the solid source allowance W in the source bottle 5: w=w2+K△T-W1.
And a weight compensation coefficient K is introduced, the influence of temperature on a weight detection result is eliminated, the measured W is the actual allowance of the solid source, and the detection result is more accurate.
In some embodiments, the controller is further configured to calculate the amount of solid source W0 required for one process and determine whether the remaining amount of solid source W in the current source bottle 5 meets the requirement for the next process. If W is greater than or equal to W0, then the next process requirements are met, and the process may continue.
Further, the device also comprises an alarm electrically connected with the controller and used for alarming when the residual quantity W of the solid source in the current source bottle 5 cannot meet the requirement of the next process, namely, when the W is smaller than W0, the process is stopped, and the risk of influencing the process result due to insufficient solid source is reduced before the process.
The application also discloses a solid source residue detection method using the solid source residue detection device, which comprises the following steps:
s1, calculating a weight compensation coefficient K; the method specifically comprises the following steps:
When a solid source is not added into the source bottle 5, gradually heating from room temperature to a first temperature, wherein the first temperature is greater than or equal to a process temperature, dividing a temperature interval between the first temperature and the room temperature into n equal divisions, wherein n is greater than or equal to 3 and n is an integer, respectively obtaining the sum W1 and Wn of weights measured by a first weighing sensor and a second weighing sensor when the room temperature is heated to the first temperature and each equal division node temperature, wherein the node temperature is the average value of the temperatures measured by the first temperature sensor 102 and the second temperature sensor 112 or the temperature measured by the second temperature sensor 112, the difference between W1 and Wn at a certain node temperature is obtained, the weight compensation value DeltaW at the node temperature is drawn by taking the difference DeltaT between the node temperature and the room temperature as an abscissa, the weight compensation value DeltaW at the node temperature as a longitudinal linear relation graph, and the slope of the linear relation graph is a weight compensation coefficient K.
S2, obtaining the sum W1 of the weights measured by the first weighing sensor and the second weighing sensor when the solid source is not added in the source bottle at room temperature, namely obtaining the total mass W1 of the source bottle 5, the heating jacket 6, the air inlet pipe 1, the air outlet pipe 3, the air inlet valve 2 and the air outlet valve 4 at room temperature.
S3, acquiring the sum W2 of the weights measured by the first weighing sensor and the second weighing sensor at the current temperature in the process or after the process is finished, wherein the current temperature is the average value of the temperatures measured by the first temperature sensor 102 and the second temperature sensor 112 or the temperature measured by the second temperature sensor 112; the air inlet pipe 1 of the source bottle 5 is opened, carrier gas is continuously introduced into the source bottle 5, the air outlet pipeline 13 is opened, a solid source carried by the carrier gas is continuously introduced into the reaction chamber for processing, and the current weight W2 can be measured in real time in the process or at the end of one process.
S4, calculating a temperature difference value delta T: Δt=t-T0, where T is the current temperature and T0 is room temperature.
S5, calculating the solid source allowance W in the source bottle 5: w=w2+K△T-W1.
A plurality of source bottles are fixed in the source cabinet, the process temperatures of the same solid source are the same, the amount of the solid source in the same source bottle can possibly be processed for a plurality of times, and when the same source bottle is processed for a plurality of times, the amount of the solid source consumed by each work can be different due to different flow of the carrier gas source, so that whether the residual amount of the solid source meets the requirement of the next process is calculated.
Further, the solid source allowance detection method of the present application further includes step S6 of determining whether the solid source allowance W in the current source bottle 5 meets the requirement of the next process. The method specifically comprises the following steps:
S61, obtaining the solid source dosage W0 required by the primary process at the process temperature; specifically, the solid source dosage W0 of the first process after the solid source is introduced is obtained. After the temperature is raised to the process temperature, before carrier gas is introduced, the sum of the weights measured by the first weighing sensor and the second weighing sensor is read, namely the total weight of the source bottle 5, the heating jacket 6, the air inlet pipe 1, the air outlet pipe 3, the air inlet valve 2, the air outlet valve 4 and the solid source in the source bottle 5 before the process; the air inlet valve of the source bottle 5 is opened, the carrier gas is continuously introduced into the source bottle 5, the air outlet valve is opened, the solid source carried by the carrier gas is continuously introduced into the reaction chamber, the sum of the weights measured by the first weighing sensor and the second weighing sensor is read after the process is finished, and the difference + (process temperature-room temperature) K of the sum of the weights before and after the process is the solid source dosage W0 required by one process.
S62, judging whether the difference value between the solid source allowance W and the solid source allowance W0 is larger than or equal to zero, if so, carrying out the next process, otherwise, giving an alarm. The controller is electrically connected with the air inlet valve 2 and the air outlet valve 4, and if the difference value between W and W0 is larger than or equal to zero, the opening state of the air inlet valve 2 and the air outlet valve 4 is kept, and the next process is carried out; if the difference between W and W0 is smaller than zero, the controller closes the air inlet valve 2 and the air outlet valve 4, stops introducing carrier gas, and controls the alarm to alarm.
And from the second process, judging once before each process is started, so that the risk of influencing the process result due to insufficient solid source is reduced.
The detection method is simple, can overcome the influence of temperature on the detection structure, and further obtains relatively stable and accurate solid source allowance, and has high detection precision. And a judging and alarming step is introduced, so that the utilization rate of the solid source is improved, and the cost is saved.
The application introduces the weight compensation coefficient K, and can calculate the weight compensation value DeltaW under different process temperatures according to the weight compensation coefficient K, and the detection device can be suitable for all source bottles.
In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a specific orientation, be configured and operated in a specific orientation, and therefore should not be construed as limiting the present invention.
In the present invention, unless explicitly specified and limited otherwise, the terms "mounted," "connected," "secured," and the like are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; either directly or indirectly, through intermediaries, or both, may be in communication with each other or in interaction with each other, unless expressly defined otherwise. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
In the description of the present specification, a description referring to the terms "present embodiment," "one embodiment," "some embodiments," "example," "specific example," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any at least one embodiment or example. Furthermore, the features of the different embodiments or examples described in the present specification and their different embodiments or examples may be combined and combined by those skilled in the art without contradiction.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. In the description of the present invention, the meaning of "plurality" means at least two, for example, two, three, etc., unless specifically defined otherwise.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the invention, but any modifications, equivalents, and simple improvements made within the spirit of the present invention should be included in the scope of the present invention.

Claims (8)

Translated fromChinese
1.一种固态源余量检测装置,其特征在于,包括第一检测装置(10)、第二检测装置(11)和控制器,1. A solid-state source residual detection device, characterized in that it comprises a first detection device (10), a second detection device (11) and a controller,所述第一检测装置(10)和所述第二检测装置(11)固定在源瓶(5)的上方,所述第一检测装置(10)和所述第二检测装置(11)吊装设置,The first detection device (10) and the second detection device (11) are fixed above the source bottle (5), and the first detection device (10) and the second detection device (11) are hoisted.所述第一检测装置(10)包括第一环形壳体(101)、第一称重传感器和第一温度传感器(102),所述第一称重传感器和所述第一温度传感器(102)固定在所述第一环形壳体(101)上,所述第一环形壳体(101)分别与源瓶(5)的进气管(1)和载气源的出气口密封连接,The first detection device (10) comprises a first annular housing (101), a first weighing sensor and a first temperature sensor (102); the first weighing sensor and the first temperature sensor (102) are fixed on the first annular housing (101); the first annular housing (101) is sealedly connected to the air inlet pipe (1) of the source bottle (5) and the air outlet of the carrier gas source, respectively.所述第二检测装置(11)包括第二环形壳体(111)、第二称重传感器和第二温度传感器(112),所述第二称重传感器和所述第二温度传感器(112)固定在所述第二环形壳体(111)上,所述第二环形壳体(111)分别与源瓶(5)的出气管(3)和反应腔室的进气口密封连接,The second detection device (11) comprises a second annular housing (111), a second weighing sensor and a second temperature sensor (112), wherein the second weighing sensor and the second temperature sensor (112) are fixed on the second annular housing (111), and the second annular housing (111) is sealedly connected to the gas outlet pipe (3) of the source bottle (5) and the gas inlet of the reaction chamber, respectively.所述第一称重传感器和所述第二称重传感器用于检测其下方的源瓶(5)、加热套(6)、进气管(1)、出气管(3)、进气阀(2)、出气阀(4)以及源瓶(5)内固态源的重量,所述第一温度传感器(102)和所述第二温度传感器(112)分别用于检测其所在处的温度,The first weighing sensor and the second weighing sensor are used to detect the weight of the source bottle (5), the heating jacket (6), the air inlet pipe (1), the air outlet pipe (3), the air inlet valve (2), the air outlet valve (4) and the solid source in the source bottle (5) below them, and the first temperature sensor (102) and the second temperature sensor (112) are used to detect the temperature at their locations, respectively.所述控制器分别与所述第一称重传感器、所述第二称重传感器、所述第一温度传感器(102)和所述第二温度传感器(112)电连接,用于根据所述第一温度传感器(102)测得的温度、所述第二温度传感器(112)测得的温度、所述第一称重传感器测得的重量和所述第二称重传感器测得的重量计算重量补偿系数K,以及根据所述第一温度传感器(102)测得的温度、所述第二温度传感器(112)测得的温度、所述第一称重传感器测得的重量、所述第二称重传感器测得的重量和所述重量补偿系数K计算源瓶(5)内固态源的余量W;The controller is electrically connected to the first weighing sensor, the second weighing sensor, the first temperature sensor (102) and the second temperature sensor (112) respectively, and is used to calculate a weight compensation coefficient K according to the temperature measured by the first temperature sensor (102), the temperature measured by the second temperature sensor (112), the weight measured by the first weighing sensor and the weight measured by the second weighing sensor, and to calculate a residual amount W of the solid source in the source bottle (5) according to the temperature measured by the first temperature sensor (102), the temperature measured by the second temperature sensor (112), the weight measured by the first weighing sensor, the weight measured by the second weighing sensor and the weight compensation coefficient K;所述控制器根据所述第一温度传感器(102)测得的温度、所述第二温度传感器(112)测得的温度、所述第一称重传感器测得的重量和所述第二称重传感器测得的重量计算重量补偿系数K的方法包括:The method in which the controller calculates a weight compensation coefficient K according to the temperature measured by the first temperature sensor (102), the temperature measured by the second temperature sensor (112), the weight measured by the first weighing sensor, and the weight measured by the second weighing sensor comprises:源瓶(5)内未加入固态源时,从室温逐渐升温至第一温度,所述第一温度大于或等于工艺温度,将第一温度与室温之间的温度区间划分为n等分,其中n大于或等于3且n为整数,从室温升温至第一温度的过程中,分别在室温和每个等分节点温度时获取所述第一称重传感器和所述第二称重传感器测得的重量之和W1和Wn,其中节点温度为所述第一温度传感器(102)和所述第二温度传感器(112)测得的温度的平均值或所述第二温度传感器(112)测得的温度,W1与某节点温度下的Wn的差值得到该节点温度下的重量补偿值△W,以节点温度与室温的差值△T为横坐标、节点温度下的重量补偿值△W为纵坐标绘制线性关系图,所述线性关系图的斜率为重量补偿系数K;When no solid source is added to the source bottle (5), the temperature is gradually raised from room temperature to a first temperature, the first temperature is greater than or equal to the process temperature, the temperature interval between the first temperature and room temperature is divided into n equal parts, wherein n is greater than or equal to 3 and n is an integer, and in the process of raising the temperature from room temperature to the first temperature, the sum of the weightsW1 andWn measured by the first weighing sensor and the second weighing sensor are obtained at room temperature and at each equal part node temperature, respectively, wherein the node temperature is the average value of the temperatures measured by the first temperature sensor (102) and the second temperature sensor (112) or the temperature measured by the second temperature sensor (112), the difference betweenW1 andWn at a certain node temperature is used to obtain the weight compensation value △W at the node temperature, and a linear relationship diagram is drawn with the difference △T between the node temperature and the room temperature as the horizontal coordinate and the weight compensation value △W at the node temperature as the vertical coordinate, and the slope of the linear relationship diagram is the weight compensation coefficient K;所述控制器根据所述第一温度传感器(102)测得的温度、所述第二温度传感器(112)测得的温度、所述第一称重传感器测得的重量、所述第二称重传感器测得的重量和所述重量补偿系数K计算源瓶(5)内固态源的余量W的方法包括:The method in which the controller calculates the remaining amount W of the solid source in the source bottle (5) according to the temperature measured by the first temperature sensor (102), the temperature measured by the second temperature sensor (112), the weight measured by the first weighing sensor, the weight measured by the second weighing sensor and the weight compensation coefficient K comprises:获取室温下源瓶内未加入固态源时第一称重传感器和所述第二称重传感器测得的重量之和W1Obtaining the sum W1 of the weights measured by the first weighing sensor and the second weighing sensor when no solid source is added to the source bottle at room temperature;获取进行工艺过程中或工艺结束后,当前温度下第一称重传感器和第二称重传感器测得的重量之和W2;其中,当前温度为第一温度传感器(102)和第二温度传感器(112)测得的温度的平均值或第二温度传感器(112)测得的温度;Obtaining the sum W2 of the weights measured by the first weighing sensor and the second weighing sensor at the current temperature during or after the process; wherein the current temperature is the average of the temperatures measured by the first temperature sensor (102) and the second temperature sensor (112) or the temperature measured by the second temperature sensor (112);计算温度差值△T:△T=T-T0,其中,T为当前温度,T0为室温;Calculate the temperature difference △T: △T=TT0 , where T is the current temperature and T0 is the room temperature;计算源瓶(5)内固态源余量W:W=W2+K*△T-W1Calculate the solid source residual amount W in the source bottle (5): W = W2 + K* ΔTW1 .2.根据权利要求1所述的固态源余量检测装置,其特征在于,所述第一环形壳体(101)通过进气管路(12)与载气源的出气口密封连接,所述第二环形壳体(111)通过出气管路(13)与反应腔室的进气口密封连接,所述进气管路(12)和所述出气管路(13)均为刚性管路。2. The solid-state source residual detection device according to claim 1 is characterized in that the first annular shell (101) is sealedly connected to the air outlet of the carrier gas source through an air inlet pipeline (12), and the second annular shell (111) is sealedly connected to the air inlet of the reaction chamber through an air outlet pipeline (13), and the air inlet pipeline (12) and the air outlet pipeline (13) are both rigid pipelines.3.根据权利要求1所述的固态源余量检测装置,其特征在于,所述控制器还用于计算一次工艺所需固态源用量W0,并判断当前源瓶(5)内固态源余量W是否满足下次工艺所需。3. The solid source residual amount detection device according to claim 1, characterized in that the controller is also used to calculate the solid source amount W0 required for one process and determine whether the solid source residual amount W in the current source bottle (5) meets the requirements of the next process.4.根据权利要求3所述的固态源余量检测装置,其特征在于,还包括报警器,所述报警器与所述控制器电连接,用于在当前源瓶(5)内固态源余量W无法满足下次工艺时报警。4. The solid-state source remainder detection device according to claim 3 is characterized in that it also includes an alarm, which is electrically connected to the controller and is used to alarm when the solid-state source remainder W in the current source bottle (5) cannot meet the next process.5.一种使用权利要求1-4任一项所述的固态源余量检测装置的固态源余量检测方法,其特征在于,包括如下步骤:5. A solid-state source residual detection method using the solid-state source residual detection device according to any one of claims 1 to 4, characterized in that it comprises the following steps:计算重量补偿系数K;Calculate the weight compensation coefficient K;获取室温下源瓶内未加入固态源时第一称重传感器和第二称重传感器测得的重量之和W1Obtaining the sum W1 of the weights measured by the first weighing sensor and the second weighing sensor when no solid source is added to the source bottle at room temperature;获取进行工艺过程中或工艺结束后,当前温度下第一称重传感器和第二称重传感器测得的重量之和W2,其中,当前温度为第一温度传感器(102)和第二温度传感器(112)测得的温度的平均值或第二温度传感器(112)测得的温度;Obtaining the sum W2 of the weights measured by the first weighing sensor and the second weighing sensor at the current temperature during or after the process, wherein the current temperature is the average of the temperatures measured by the first temperature sensor (102) and the second temperature sensor (112) or the temperature measured by the second temperature sensor (112);计算温度差值△T:△T=T-T0,其中,T为当前温度,T0为室温;Calculate the temperature difference △T: △T=TT0 , where T is the current temperature and T0 is the room temperature;计算源瓶(5)内固态源余量W:W=W2+K△T-W1Calculate the solid source residual W in the source bottle (5): W = W2 + KΔTW1 .6.根据权利要求5所述的固态源余量检测方法,其特征在于,计算重量补偿系数K,包括:6. The solid-state source residual detection method according to claim 5, characterized in that the weight compensation coefficient K is calculated, comprising:源瓶(5)内未加入固态源时,从室温逐渐升温至第一温度,所述第一温度大于或等于工艺温度,将第一温度与室温之间的温度区间划分为n等分,其中n大于或等于3且n为整数,从室温升温至第一温度的过程中,分别在室温和每个等分节点温度时获取所述第一称重传感器和所述第二称重传感器测得的重量之和W1和Wn,其中节点温度为所述第一温度传感器(102)和所述第二温度传感器(112)测得的温度的平均值或所述第二温度传感器(112)测得的温度,W1与某节点温度下的Wn的差值得到该节点温度下的重量补偿值△W,以节点温度与室温的差值△T为横坐标、节点温度下的重量补偿值△W为纵坐标绘制线性关系图,所述线性关系图的斜率为重量补偿系数K。When no solid source is added to the source bottle (5), the temperature is gradually raised from room temperature to a first temperature, the first temperature is greater than or equal to the process temperature, the temperature interval between the first temperature and room temperature is divided into n equal parts, wherein n is greater than or equal to 3 and n is an integer, and in the process of raising the temperature from room temperature to the first temperature, the sum of the weightsW1 andWn measured by the first weighing sensor and the second weighing sensor are obtained at room temperature and each equal part node temperature, respectively, wherein the node temperature is the average value of the temperatures measured by the first temperature sensor (102) and the second temperature sensor (112) or the temperature measured by the second temperature sensor (112), the difference betweenW1 andWn at a certain node temperature is used to obtain the weight compensation value △W at the node temperature, and a linear relationship diagram is drawn with the difference △T between the node temperature and the room temperature as the horizontal coordinate and the weight compensation value △W at the node temperature as the vertical coordinate, and the slope of the linear relationship diagram is the weight compensation coefficient K.7.根据权利要求5所述固态源余量检测方法,其特征在于,所述方法还包括判断当前源瓶(5)内固态源余量W是否满足下次工艺所需。7. The solid source residual detection method according to claim 5 is characterized in that the method also includes judging whether the solid source residual W in the current source bottle (5) meets the requirements of the next process.8.根据权利要求7所述固态源余量检测方法,其特征在于,判断当前源瓶(5)内固态源余量W是否满足下次工艺所需,包括:8. The solid source residual quantity detection method according to claim 7 is characterized in that judging whether the solid source residual quantity W in the current source bottle (5) meets the requirements of the next process comprises:获取工艺温度下一次工艺所需的固态源用量W0Obtain the solid source amount W0 required for the previous process at the process temperature;判断固态源余量W与W0的差值是否大于或等于零,如果是,则进行下一次工艺,否则报警。Determine whether the difference between the solid source remainder W andW0 is greater than or equal to zero. If so, proceed to the next process, otherwise an alarm is issued.
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Country or region after:China

Address before:Room 205-5-7, 2nd Floor, East Office Building, No. 45 Beijing Road, Qianwan Bonded Port Area, Qingdao Pilot Free Trade Zone, Shandong Province (A)

Patentee before:QINGDAO SIFANG SRI INTELLIGENT TECHNOLOGY Co.,Ltd.

Country or region before:China

CP03Change of name, title or address

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