CN117647300B - CVD online in-situ weighing system and method - Google Patents
CVD online in-situ weighing system and method Download PDFInfo
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- 238000005303 weighing Methods 0.000 title claims abstract description 99
- 238000000034 method Methods 0.000 title claims abstract description 56
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 49
- 239000010453 quartz Substances 0.000 claims abstract description 46
- 238000005259 measurement Methods 0.000 claims abstract description 34
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- 230000008569 process Effects 0.000 claims description 33
- 238000002474 experimental method Methods 0.000 claims description 28
- 238000000151 deposition Methods 0.000 claims description 20
- 230000008021 deposition Effects 0.000 claims description 20
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- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 4
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- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
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- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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Abstract
The application discloses a CVD online in-situ weighing system and a method, and belongs to the technical field of semiconductor manufacturing. According to the application, the sensor measurement value is calculated according to the moment principle by adopting the long cantilever to connect the weighing sensor and the sample carrier under the condition that the sensor cannot be applied to a high-temperature environment in the quartz tube, and meanwhile, the corresponding temperature-quality compensation curve and the corresponding barometric pressure compensation value are obtained in advance by considering the high-temperature low-pressure environment, and the corresponding temperature and barometric pressure compensation is carried out on the measurement value, so that a more accurate quality value is obtained, and the in-situ quality detection of a deposited sample in the deposition process is realized. Aiming at a high-temperature environment, the weighing system is provided with a sensor-connecting door-aviation plug integrated structure, so that the reliability of the structure is improved, the sealing performance is ensured, and the system structure is optimized.
Description
Technical Field
The invention relates to a CVD online in-situ weighing system and a method, and belongs to the technical field of semiconductor manufacturing.
Background
Chemical vapor deposition (Chemical Vapor Deposition, CVD) is a film forming technique widely used in semiconductor fabrication and in the preparation of thin film materials. The basic principle is that gaseous reactants are introduced into a reaction chamber, and the gaseous reactants reach the temperature and pressure conditions required by the reaction in the reaction chamber, so that the gaseous reactants react layer by layer on the solid surface, thereby forming a film and continuously growing.
In order to detect deposition, it is generally necessary to weigh the deposited sample, and the prior art generally takes the sample out of the reaction furnace after the reaction is completed and then weighs the sample to observe the reaction progress and the sample growth quality, so as to provide guidance for the subsequent film deposition parameters, but this method has the following problems:
Firstly, after the reaction is finished, waiting for the cooling of the reaction furnace, taking out the sample from the reaction furnace, and weighing, wherein on one hand, the sample mass increase condition in the reaction process cannot be obtained, and on the other hand, the time cost is high and the efficiency is low; second, when the sample is taken out from the reaction furnace and then weighed, impurities such as oxygen in the air may affect the reacted sample, and irreversible errors are caused to the result.
Disclosure of Invention
In order to achieve accurate mass detection of a sample in a chemical vapor deposition process, the invention provides a CVD online in-situ weighing system, which is applied to a horizontal tubular CVD device, and comprises: the device comprises a long cantilever, a weighing sensor, a temperature sensor and a mass compensation module;
The long cantilever and the weighing sensor are arranged in a quartz tube in the CVD equipment, wherein one end of the long cantilever is connected with the weighing sensor through a high-temperature-resistant connecting piece, and the other end of the long cantilever is used for placing a deposition sample; considering that a common weighing sensor cannot bear the high temperature of 800-1000 ℃ in a quartz tube, adopting a long cantilever structure to enable the weighing sensor to be far away from a direct heating area, and enabling a sample to be placed at the tail end of the long cantilever, and utilizing a moment principle to realize real-time mass measurement of a deposited sample in the high temperature area;
The weighing sensor is arranged at a sealing position at one end of the quartz tube, and transmits a measurement signal to the mass compensation module outside the quartz tube through the aviation connector; the aviation plug connector ensures that the data of the weighing sensor is smoothly transmitted and the tightness of the reaction environment is ensured;
the temperature sensor is arranged on the outer wall of the quartz tube at the position corresponding to the deposited sample and used for acquiring the temperature at the position of the deposited sample in real time;
The mass compensation module is used for carrying out temperature-mass compensation and air pressure-mass compensation on the measured value of the weighing sensor; the temperature-mass compensation compensates the difference between the measured value and the actual value of the deposition sample caused by the increase or decrease of the temperature, and the air pressure-mass compensation compensates the difference between the measured value and the actual value of the deposition sample caused by the difference of the air pressure.
Optionally, the high temperature resistant connector is used for connecting one end of the long cantilever to a fulcrum at one end of the weighing sensor, so that the weighing sensor can measure and obtain a mass measurement value M of the deposited sample placed at the other end of the long cantilever according to a moment calculation formula Measurement of ：M Measurement of =m Display device * Wherein m Display device represents the display value of the load cell, B represents the length of the load cell, A represents the length of the deposition sample placement position; l represents a long cantilever length.
Optionally, the temperature-mass compensation is determined according to a temperature-mass compensation curve, and the method for acquiring the temperature-mass compensation curve includes:
and (3) carrying out a standard experiment process, zeroing the weighing sensor under the condition that the quartz tube is empty, sequentially raising the temperature, maintaining the high temperature and reducing the temperature, reading and recording data of the temperature sensor and the weighing sensor, drawing a curve of the measured value of the weighing sensor along with the temperature change after the experiment is finished, and obtaining a symmetrical curve by taking the abscissa as a symmetrical axis, namely a temperature-quality compensation curve.
Optionally, the temperature-quality compensation curve includes a temperature-raising compensation curve and a temperature-lowering compensation curve, where the temperature-raising compensation curve is a temperature-quality compensation curve corresponding to a temperature-raising process in an experiment process, and the temperature-lowering compensation curve is a temperature-quality compensation curve corresponding to a temperature-lowering process in the experiment process.
Optionally, the air pressure-mass compensation is determined according to the buoyancy M Floating device of the long cantilever and the high temperature resistant connector under the atmospheric pressure, and the volume of the long cantilever and the high temperature resistant connector is V, then: m Floating device Wherein/>Representing air density,/>A gravitational constant.
The application also provides a CVD online in-situ weighing system, which is applied to vertical tubular CVD equipment and comprises: the device comprises a weighing sensor, a temperature sensor, a bearing tray, a high-temperature resistant support column, a sample placing tray, a sealing piece and a mass compensation module, wherein the bearing tray is placed on the weighing sensor, and the high-temperature resistant support column and the sample placing tray are sequentially placed on the weighing sensor; the temperature sensor is arranged on the outer wall of the quartz tube at the position corresponding to the deposited sample and used for acquiring the temperature at the position of the deposited sample in real time; the weighing sensor transmits a measurement signal to a mass compensation module outside the quartz tube through the aviation connector, and the mass compensation module is used for carrying out temperature-mass compensation and air pressure-mass compensation on the measurement value of the weighing sensor.
Since the measured values of the deposited samples can be directly read from the load cell in the vertical tube CVD apparatus, calculation from the moment is not required.
Optionally, the temperature-mass compensation is determined according to a temperature-mass compensation curve, and the method for obtaining the temperature-mass compensation curve includes:
and (3) carrying out a standard experiment process, zeroing the weighing sensor under the condition that the quartz tube is empty, sequentially raising the temperature, maintaining the high temperature and reducing the temperature, reading and recording data of the temperature sensor and the weighing sensor, drawing a curve of the measured value of the weighing sensor along with the temperature change after the experiment is finished, and obtaining a symmetrical curve by taking the abscissa as a symmetrical axis, namely a temperature-quality compensation curve.
Optionally, the temperature-quality compensation curve includes a temperature-raising compensation curve and a temperature-lowering compensation curve, where the temperature-raising compensation curve is a temperature-quality compensation curve corresponding to a temperature-raising process in an experiment process, and the temperature-lowering compensation curve is a temperature-quality compensation curve corresponding to a temperature-lowering process in the experiment process.
Optionally, the air pressure-mass compensation is determined according to buoyancy forces received by the bearing tray, the high-temperature resistant support column and the sample placing tray under the atmospheric pressure, and the volumes of the bearing tray, the high-temperature resistant support column and the sample placing tray are recorded asThen: m Floating device Wherein/>Representing air density,/>A gravitational constant.
The application also provides a CVD online in-situ weighing method, which is realized based on the system, and comprises the following steps:
The temperature-mass compensation curve is obtained in advance, and the obtaining method comprises the following steps: carrying out a standard experiment process, zeroing the weighing sensor under the condition that the quartz tube is empty, sequentially increasing the temperature, maintaining the high temperature and reducing the temperature, reading and recording data of the temperature sensor and the weighing sensor, drawing a curve of the measured value of the weighing sensor along with the temperature change after the experiment is finished, and obtaining a symmetrical curve by taking the abscissa as a symmetrical axis, namely a temperature-quality compensation curve; the temperature-quality compensation curve comprises a temperature rise compensation curve and a temperature reduction compensation curve, wherein the temperature rise compensation curve is a temperature-quality compensation curve corresponding to a temperature rise process in an experiment process, and the temperature reduction compensation curve is a temperature-quality compensation curve corresponding to a temperature reduction process in the experiment process;
acquiring a real-time measured value M Measurement of of a weighing sensor aiming at a deposited sample and a real-time temperature corresponding to a temperature sensor, and acquiring a compensation value corresponding to the real-time temperature according to a temperature-mass compensation curve Mass of deposited sample M Actual practice is that of =M Measurement of +Wherein/>The buoyancy of the connecting part is born in the quartz tube under the atmospheric pressure environment;
Aiming at horizontal tubular CVD equipment, the quartz tube inner bearing connecting part comprises a long cantilever and a high-temperature resistant connecting piece; for vertical tubular CVD equipment, bear connecting piece in the quartz capsule and include bearing tray, high temperature resistant support column and sample placement tray.
The invention has the beneficial effects that:
According to the application, the sensor measurement value is calculated according to the moment principle by adopting the long cantilever to connect the weighing sensor and the sample carrier under the condition that the sensor cannot be applied to a high-temperature environment in the quartz tube, and meanwhile, the corresponding temperature-mass compensation curve and the corresponding air pressure-mass compensation curve are obtained in advance by considering the high-temperature low-pressure environment, and the corresponding temperature and air pressure compensation is carried out on the measurement value, so that a more accurate quality value is obtained, and the in-situ quality detection of a deposited sample in the deposition process is realized. Aiming at a high-temperature environment, the weighing system is provided with a sensor-connecting door-aviation plug integrated structure, so that the reliability of the structure is improved, the sealing performance is ensured, and the system structure is optimized.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for the description of the embodiments will be briefly described below, and it is apparent that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of an in-situ weighing system applied to a horizontal tube CVD apparatus according to an embodiment of the present invention.
FIG. 2 is a schematic diagram of a CVD in-situ weighing system for integrated preparation of quartz boats and long cantilevers in accordance with one embodiment of the present invention.
FIG. 3 is a schematic diagram of an in-situ weighing system for use in a vertical tube CVD apparatus according to one embodiment of the present invention.
FIG. 4 is a graph of temperature-mass compensation for boron nitride growth experiments using a CVD in-situ weighing system according to one embodiment of the present invention.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, the embodiments of the present invention will be described in further detail with reference to the accompanying drawings.
Embodiment one:
The embodiment provides a CVD online in-situ weighing system, which is applied to a horizontal tubular CVD device, wherein one end of a quartz tube in the horizontal tubular CVD device is provided with a sealing component with a handle, as shown in FIG. 1; the CVD in-situ weighing system comprises a long cantilever 2 with the length of L, a weighing sensor 1, a temperature sensor and a mass compensation module; one end of the long cantilever 2 is connected with the weighing sensor 1 through a high-temperature-resistant connecting piece 5, and the other end of the long cantilever 2 is used for placing a deposition sample; the weighing sensor 1 is arranged at a sealing part of the quartz tube with a handle, the weighing sensor 1 transmits a measurement signal to a mass compensation module outside the quartz tube through an aviation connector 4, and the mass compensation module performs mass compensation to obtain the accurate mass of a deposited sample; the temperature sensor is arranged on the outer wall of the quartz tube at the position corresponding to the deposited sample and used for acquiring the temperature at the position of the deposited sample in real time; the temperature sensor is not shown in fig. 1.
In fig. 1, to show the place where the deposition sample is placed, the other end of the long cantilever 2 is shown by reference numeral 6, the deposition sample is placed in a quartz boat and then placed in a quartz tube in a general deposition process, the length of the place where the deposition sample is placed is denoted by a, and generally the length of the quartz boat, the high temperature resistant connecting piece 5 can be made of high temperature resistant stainless steel or other high temperature resistant materials, meanwhile, the high temperature resistant connecting piece 5 has a heat insulation effect, so that the weighing sensor 1 is furthest ensured to be far away from a high temperature area, and the avionics connector 4 can ensure that a measurement signal transmitted by the sensor is not influenced by an external electromagnetic signal.
The mass compensation module is mainly used for compensating mass measurement errors caused by high-temperature low-pressure environments in the quartz tube, wherein the temperature-mass compensation value can compensate corresponding temperature according to a temperature compensation curve acquired in advance; the air pressure-mass compensation value is the buoyancy compensation value of the part connected with the weighing sensor 1 under the vacuum condition.
In the deposition process, the accurate quality of the deposition sample is obtained after corresponding temperature and air pressure compensation values are carried out on the obtained measured value of the weighing sensor 1.
The measured value M Measurement of obtained by the weighing sensor 1 can be obtained according to the moment calculation formula: m Measurement of =m Display device * Wherein, the initial end of the weighing sensor 1 is used as a fulcrum for calculation, m Display device represents the display value of the weighing sensor 1, B represents the length of the weighing sensor 1, A represents the length of the deposition sample placement position; l denotes the length of the long cantilever 2.
The mass of the deposited sample is the sum of the measured value M Measurement of of the load cell 1, the temperature-mass compensation value and the air pressure-mass compensation value.
In practical applications, the quartz boat and the long cantilever 2 may be manufactured as an integrated structure, as shown in fig. 2.
It should be noted that, for convenience of installation, the high temperature resistant connector 5 may include a plurality of connectors, and the connectors are connected by a suitable connection manner.
Example two
The embodiment provides a CVD online in-situ weighing method, which comprises the following steps:
The temperature-mass compensation curve and the air pressure-mass compensation curve are obtained in advance, and the obtaining method comprises the following steps:
1) Temperature-mass compensation curve: and (3) carrying out a standard experiment process, zeroing the weighing sensor under the condition that the quartz tube is empty, sequentially raising the temperature, maintaining the high temperature and lowering the temperature, reading and recording the data of the temperature sensor and the weighing sensor, drawing a curve of the measured value of the weighing sensor along with the temperature change after the experiment is finished, and inverting the curve to obtain the temperature compensation curve. In the later experiments, the final result can be output by only adding the temperature compensation value of the corresponding temperature to the result in the program.
And inverting the curve, namely taking the abscissa as the symmetry axis to obtain the symmetry curve.
The relation between the measured value and the display value of the weighing sensor is as follows: m Measurement of =m Display device * Wherein, the initial end of the weighing sensor 1 is used as a fulcrum for calculation, m Display device represents the display value of the weighing sensor 1, B represents the length of the weighing sensor 1, A represents the length of the deposition sample placement position; l denotes the length of the long cantilever 2.
Further, the application respectively draws a temperature rise compensation curve and a temperature reduction compensation curve aiming at the temperature rise process and the temperature reduction process, wherein the temperature rise compensation curve is a temperature-quality compensation curve corresponding to the temperature rise process in the experimental process, and the temperature reduction compensation curve is a temperature-quality compensation curve corresponding to the temperature reduction process in the experimental process, as shown in fig. 4.
2) Barometric-mass compensation:
The air pressure in the reactor was close to vacuum (typically 1.5 kPa) and thus can be calculated as vacuum. Therefore, the mass of the part connected with the weighing sensor due to the reduced buoyancy at the atmospheric pressure is the air pressure compensation value, namely the mass obtained under the vacuum condition is more than M Floating device than the mass obtained under the atmospheric pressure condition, and the measured value obtained by the application needs to be subtracted by M Floating device ：M Floating device
Wherein V refers to the volume of the part connected with the weighing sensor, and for horizontal tubular CVD equipment, the part connected with the weighing sensor comprises a long cantilever 2, a high-temperature resistant connecting piece 5 and other parts, and if a separate quartz boat is used for bearing a deposition sample, the part also comprises the volume of the quartz boat; Representing air density,/> A gravitational constant.
Taking the component shown in fig. 2 actually prepared by the application as an example, the volumes of the long cantilever 2 and the high temperature resistant connecting piece 5 are 29031.48L, the buoyancy value of air pressure compensation is:
M Floating device
For vertical tubular CVD equipment, the part connected with the weighing sensor comprises a bearing tray 7, a high-temperature resistant supporting column 11 and a sample placing tray 6, as shown in FIG. 3, M Floating device ，/>The volumes of the carrying tray 7, the high temperature resistant support column 11 and the sample placement tray 6 are shown.
And acquiring and recording data of the weighing sensor and the temperature sensor in real time in the deposition process, and correspondingly compensating the data of the weighing sensor acquired in real time according to the temperature-mass compensation curve and the air pressure compensation to obtain the accurate quality of the deposited sample.
For example, the measurement value of the weighing sensor at a certain time during the deposition process is M Measurement of , the corresponding temperature at the moment is X 1 ℃, and the corresponding temperature-mass compensation value of X 1 ℃ read according to the temperature-mass compensation curve isAir pressure-mass compensation value/>The mass of the deposited sample corresponding to this moment is M Actual practice is that of =M Measurement of +/>-/>，/>And/>The units of (a) are the same as M Measurement of .
Embodiment III:
The embodiment provides a CVD online in-situ weighing system and a method, the system is applied to a vertical tubular CVD device, the vertical tubular CVD device does not need to calculate a measured value according to moment, and the measured value can be directly read from a weighing sensor, as shown in figure 3, the system comprises a weighing sensor 1, a temperature sensor, a bearing tray 7, a high temperature resistant supporting column 11, a sample placing tray 6, a sealing element 10, a flange 8 and a mass compensation module, wherein the weighing sensor 1 transmits a measuring signal to the mass compensation module outside a quartz tube through an aviation connector 4; a temperature sensor, which is not shown in fig. 3, is provided on the outer wall of the quartz tube at a position corresponding to the deposition sample for acquiring the temperature at the deposition sample position in real time. The mass compensation module is used for carrying out temperature-mass compensation and air pressure-mass compensation on the measured value of the weighing sensor.
The sealing element 10 can be made of materials with poor heat conduction performance, and is used for realizing heat insulation, such as aluminum oxide, aluminum silicate and other materials, and meanwhile, the sealing element 10 can fix the quartz tube 9 to realize gravity bearing; the high-temperature-resistant support column 11 can be made of high-temperature-resistant stainless steel, meanwhile, the high-temperature-resistant support column 11 has a heat insulation function, and the flange 8 is used for sealing the lower port of the quartz tube 9.
When mass measurement of the deposited sample is realized, final mass is obtained after measurement and corresponding temperature-mass compensation and air pressure-mass compensation are performed by adopting the method provided in the second embodiment.
Embodiment four:
the embodiment provides a CVD online in-situ weighing method, which takes a boron nitride growth experiment as an example to verify the effectiveness of the method, and specifically, the conditions of the boron nitride growth experiment are as follows: the reaction temperature was 1075℃and the reaction pressure was 600Pa, and the environment was 300sccm Ar+H 2.
The method is adopted to firstly obtain a corresponding temperature-quality compensation curve as shown in fig. 4, and the corresponding quality compensation value at each temperature can be inquired according to the temperature-quality compensation curve. And in the subsequent deposition experiment process, the measured value of the quality sensor 1 is obtained in real time, and then the corresponding compensation value is inquired and added to obtain the quality corresponding to each deposition moment.
The initial mass, the mass after growth at each time point, and the loss mass obtained by the above method are shown in table 1 below as a function of BN growth time:
Table 1: boron nitride growth experimental data
In addition, after changing the experimental conditions, the test was carried out at 1000 ℃, 1050 ℃, 1100 ℃ and 500Pa, 550Pa and 650Pa, respectively, to obtain more reliable results.
In order to verify the quality error obtained by the application, quartz balls with known quality are put into a long cantilever of a quartz tube, high-temperature experiments at different temperatures are carried out, and the error verification of the obtained weighing result is within +/-1 mg. The quartz ball is selected because the quartz glass does not react in high-temperature low-pressure environment and corresponding reaction atmosphere, and the quality of the quartz glass is not changed when the quartz glass is placed in a long cantilever of a quartz tube.
Some steps in the embodiments of the present invention may be implemented by using software, and the corresponding software program may be stored in a readable storage medium, such as an optical disc or a hard disk.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (4)
1. A CVD online in-situ weighing system for use with a horizontal tube CVD apparatus, the system comprising: the device comprises a long cantilever, a weighing sensor, a temperature sensor and a mass compensation module, wherein the long cantilever and the weighing sensor are arranged in a quartz tube in a CVD device, one end of the long cantilever is connected with the weighing sensor through a high-temperature-resistant connecting piece, and the other end of the long cantilever is used for placing a deposition sample; the weighing sensor is arranged at a sealing position at one end of the quartz tube, and transmits a measurement signal to the mass compensation module outside the quartz tube through the aviation connector; the temperature sensor is arranged on the outer wall of the quartz tube at the position corresponding to the deposited sample and used for acquiring the temperature at the position of the deposited sample in real time; the mass compensation module is used for carrying out temperature-mass compensation and air pressure-mass compensation on the measured value of the weighing sensor; the temperature-mass compensation is determined according to a temperature-mass compensation curve; the temperature-quality compensation curve comprises a temperature rise compensation curve and a temperature reduction compensation curve;
the method for acquiring the temperature-mass compensation curve comprises the following steps:
Carrying out a standard experiment process, zeroing the weighing sensor under the condition that the quartz tube is empty, sequentially increasing the temperature, maintaining the high temperature and reducing the temperature, reading and recording data of the temperature sensor and the weighing sensor, drawing a curve of the measured value of the weighing sensor along with the temperature change after the experiment is finished, and obtaining a symmetrical curve by taking the abscissa as a symmetrical axis, namely a temperature-quality compensation curve;
The temperature rise compensation curve is a temperature-quality compensation curve corresponding to a temperature rise process in the experimental process, and the temperature reduction compensation curve is a temperature-quality compensation curve corresponding to a temperature reduction process in the experimental process;
The air pressure-mass compensation is determined according to the buoyancy M Floating device born by the long cantilever and the high-temperature-resistant connecting piece under the atmospheric pressure, and the volumes of the long cantilever and the high-temperature-resistant connecting piece are V, so that: m Floating device Wherein/>Representing air density,/>A gravitational constant.
2. The system of claim 1, wherein the high temperature resistant connector is configured to connect one end of the long cantilever to a fulcrum at one end of the load cell, such that the load cell measures a mass measurement M of the deposited sample placed at the other end of the long cantilever according to a moment calculation formula Measurement of ：M Measurement of =m Display device * Wherein m Display device represents the display value of the load cell, B represents the length of the load cell, A represents the length of the deposition sample placement position; l represents a long cantilever length.
3. A CVD online in-situ weighing system for use with a vertical tube CVD apparatus, the system comprising: the device comprises a weighing sensor, a temperature sensor, a bearing tray, a high-temperature resistant support column, a sample placing tray, a sealing piece and a mass compensation module, wherein the bearing tray is placed on the weighing sensor, and the high-temperature resistant support column and the sample placing tray are sequentially placed on the weighing sensor; the temperature sensor is arranged on the outer wall of the quartz tube at the position corresponding to the deposited sample and used for acquiring the temperature at the position of the deposited sample in real time; the weighing sensor transmits a measurement signal to a mass compensation module outside the quartz tube through the aviation connector, and the mass compensation module is used for carrying out temperature-mass compensation and air pressure-mass compensation on the measurement value of the weighing sensor; the temperature-mass compensation is determined according to a temperature-mass compensation curve, and the temperature-mass compensation curve comprises a temperature rise compensation curve and a temperature reduction compensation curve;
the method for acquiring the temperature-mass compensation curve comprises the following steps:
Carrying out a standard experiment process, zeroing the weighing sensor under the condition that the quartz tube is empty, sequentially increasing the temperature, maintaining the high temperature and reducing the temperature, reading and recording data of the temperature sensor and the weighing sensor, drawing a curve of the measured value of the weighing sensor along with the temperature change after the experiment is finished, and obtaining a symmetrical curve by taking the abscissa as a symmetrical axis, namely a temperature-quality compensation curve;
The temperature-rise compensation curve is a temperature-quality compensation curve corresponding to a temperature-rise process in the experimental process, and the temperature-reduction compensation curve is a temperature-quality compensation curve corresponding to a temperature-reduction process in the experimental process;
the air pressure-mass compensation is determined according to the buoyancy force of the bearing tray, the high-temperature resistant support column and the sample placing tray under the atmospheric pressure, and the volumes of the bearing tray, the high-temperature resistant support column and the sample placing tray are recorded as follows Then: m Floating device />Wherein/>Representing air density,/>A gravitational constant.
4. A CVD online in-situ weighing method, characterized in that it is implemented on the basis of the system according to claims 1-2 and 3, the method comprising:
The temperature-mass compensation curve is obtained in advance, and the obtaining method comprises the following steps: carrying out a standard experiment process, zeroing the weighing sensor under the condition that the quartz tube is empty, sequentially increasing the temperature, maintaining the high temperature and reducing the temperature, reading and recording data of the temperature sensor and the weighing sensor, drawing a curve of the measured value of the weighing sensor along with the temperature change after the experiment is finished, and obtaining a symmetrical curve by taking the abscissa as a symmetrical axis, namely a temperature-quality compensation curve; the temperature-quality compensation curve comprises a temperature rise compensation curve and a temperature reduction compensation curve, wherein the temperature rise compensation curve is a temperature-quality compensation curve corresponding to a temperature rise process in an experiment process, and the temperature reduction compensation curve is a temperature-quality compensation curve corresponding to a temperature reduction process in the experiment process;
acquiring a real-time measured value M Measurement of of a weighing sensor aiming at a deposited sample and a real-time temperature corresponding to a temperature sensor, and acquiring a compensation value corresponding to the real-time temperature according to a temperature-mass compensation curve Mass of deposited sample M Actual practice is that of =M Measurement of +Wherein/>The buoyancy of the connecting part is born in the quartz tube under the atmospheric pressure environment.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202410122781.5A CN117647300B (en) | 2024-01-30 | 2024-01-30 | CVD online in-situ weighing system and method |
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| CN202410122781.5A CN117647300B (en) | 2024-01-30 | 2024-01-30 | CVD online in-situ weighing system and method |
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| CN117647300A CN117647300A (en) | 2024-03-05 |
| CN117647300B true CN117647300B (en) | 2024-04-23 |
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