CN111006768A - Device and method for calibrating temperature of MOCVD (Metal organic chemical vapor deposition) equipment by utilizing alloy phase change - Google Patents
Device and method for calibrating temperature of MOCVD (Metal organic chemical vapor deposition) equipment by utilizing alloy phase change Download PDFInfo
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- 230000008859 change Effects 0.000 title claims description 37
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- 229910052751 metal Inorganic materials 0.000 title description 7
- 239000002184 metal Substances 0.000 title description 7
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- 239000012782 phase change material Substances 0.000 claims abstract description 66
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- 238000002488 metal-organic chemical vapour deposition Methods 0.000 claims abstract 8
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- XNRNVYYTHRPBDD-UHFFFAOYSA-N [Si][Ag] Chemical compound [Si][Ag] XNRNVYYTHRPBDD-UHFFFAOYSA-N 0.000 claims description 20
- MOFOBJHOKRNACT-UHFFFAOYSA-N nickel silver Chemical compound [Ni].[Ag] MOFOBJHOKRNACT-UHFFFAOYSA-N 0.000 claims description 20
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 claims description 19
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Images
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J5/00—Radiation pyrometry, e.g. infrared or optical thermometry
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/52—Controlling or regulating the coating process
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J5/00—Radiation pyrometry, e.g. infrared or optical thermometry
- G01J5/80—Calibration
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J5/00—Radiation pyrometry, e.g. infrared or optical thermometry
- G01J5/0044—Furnaces, ovens, kilns
Abstract
The utility model provides a utilize device of alloy phase transition calibration MOCVD equipment temperature includes: the temperature correcting sheet comprises a phase-change material layer, the phase-change material layer is provided with a preset phase-change temperature point, the temperature correcting sheet is arranged at a sample of the MOCVD equipment, and the real temperature of the sample is obtained through the surface laser reflectivity mutation of the temperature correcting sheet when the phase-change material layer generates a phase-change reaction. The method can correct the infrared temperature measurement curve under the conditions that no black body furnace exists and the emissivity parameter of the measured material is unknown, and solves the problem that the infrared temperature measurement curve in the MOCVD system deviates from the temperature of a real sample.
Description
Technical Field
The disclosure relates to the field of temperature measurement, and in particular relates to a device and a method for calibrating the temperature of Metal Organic Chemical Vapor Deposition (MOCVD) equipment by utilizing alloy phase change.
Background
MOCVD equipment usually adopts a non-contact infrared temperature measurement technology to monitor the temperature of a sample due to a special cavity structure and a material growth environment. The infrared thermometry technique is based on the blackbody radiation principle (planck's law). According to Planck's law, the infrared radiation spectrum of a black body is determined by its surface temperature, and the surface temperature of the black body can be determined by measuring the infrared radiation intensity of the black body. In practical application, a blackbody furnace device is usually used as a standard blackbody to calibrate and calibrate the infrared test system. The temperature measured by the infrared thermometer calibrated by the blackbody furnace is called the blackbody temperature of the object. Because the infrared radiation spectrum of the actual object and the blackbody has a certain difference, the temperature of the blackbody of the measured object and the real temperature of the surface of the object have a certain deviation, and emissivity parameters need to be introduced for correction. Different objects (even the same material) have different emissivity, and only if the correct emissivity parameter of the measured object is set in the infrared temperature measurement system, the temperature value obtained by infrared temperature measurement can be as close to the real temperature of the surface of the measured object as possible. Therefore, the current infrared temperature measurement system has two defects: firstly, expensive blackbody furnace equipment is required to be used; secondly, the emissivity parameters of the measured object need to be known. These two conditions, especially the emissivity parameter, are often difficult to meet.
Disclosure of Invention
Technical problem to be solved
The present disclosure provides an apparatus and method for calibrating the temperature of an MOCVD tool using alloy phase transition to at least partially solve the above-mentioned problems.
(II) technical scheme
According to one aspect of the present disclosure, there is provided an apparatus for calibrating the temperature of an MOCVD equipment by utilizing alloy phase transition, comprising:
the temperature correcting sheet comprises a phase-change material layer, the phase-change material layer is provided with a preset phase-change temperature point, the temperature correcting sheet is arranged at a sample of the MOCVD equipment, and the real temperature of the sample is obtained through the surface laser reflectivity mutation of the temperature correcting sheet when the phase-change material layer generates a phase-change reaction.
In some embodiments, the temperature calibration patch further comprises:
a base material on which the phase change material layer is deposited in the form of a thin film.
In some embodiments, the material of the phase change material layer is selected from the same material system, which includes aluminum germanium, aluminum silicon, silver germanium, silver silicon or silver nickel material systems, and the predetermined phase change temperature points are respectively 420 ℃, 577 ℃, 650 ℃, 848 ℃, 960 ℃.
In some embodiments, the phase change material layer includes an elemental thin film layer and/or an alloy material layer.
In some embodiments, the phase-change material layer includes at least one first simple substance thin film layer and at least one second simple substance thin film layer, and the materials of the first simple substance thin film layer and the second simple substance thin film layer are two different simple substance elements in the same material system.
In some embodiments, the first elemental thin film layer and the second elemental thin film layer are alternately deposited on the substrate material in any order, and the thickness of each elemental thin film layer is any value within a first predetermined thickness range.
In some embodiments, the first predetermined thickness ranges from 100nm to 1000 nm.
In some embodiments, the phase change material layer comprises at least one alloy material layer having a thickness within a second predetermined thickness range.
In some embodiments, the second predetermined thickness range is greater than 200 nm.
In some embodiments, the phase change material layer includes at least one elemental thin film layer and at least one alloy material layer, the materials in the elemental thin film layer and the alloy material layer are selected from two elements in the same material system, and the at least one elemental thin film layer and the at least one alloy material layer are arranged in any order and in any number of layers and are deposited on the substrate material.
In some embodiments, when aluminum germanium and aluminum silicon alloy are adopted, the aluminum accounts for preferably 2-98% by weight; when the Ag-Ge alloy is adopted, the weight ratio of Ag is 2-90%; when the silver-silicon alloy is adopted, the weight ratio of silver is 1-99 percent; when the silver-nickel alloy is adopted, the weight percentage of silver is 1 to 98 percent.
In some embodiments, when the phase change material layer is selected from any one of four material systems of aluminum germanium, aluminum silicon, silver germanium, silver silicon, the base material is silicon, sapphire or silicon carbide wafer;
when the phase change material layer is a silver-nickel material system, the substrate material is sapphire or silicon carbide wafer.
In some embodiments, when the substrate material is a silicon substrate, the phase change material layer includes an elemental thin film layer, and the elemental thin film layer forms the phase change material by cooperating with the silicon substrate.
In some embodiments, the single substance thin film layer is an aluminum single substance thin film layer or a silver single substance thin film layer.
In another embodiment of the present disclosure, a method for calibrating the temperature of an MOCVD equipment by utilizing alloy phase transition is provided, and the method adopts the device as described above, and comprises the following steps:
placing a sample into the system, heating the system at a constant heating rate of not higher than 1 ℃/min, and obtaining a corresponding relation between a set temperature T _ set of the system and an actual temperature T _ true of the surface of the sample by using an infrared temperature measuring device to be calibrated to obtain a set temperature-sample temperature curve of infrared temperature measurement of the system;
selecting one or more temperature correcting sheets of different material systems according to the actual temperature T _ true temperature zone range of the surface of the sample;
respectively testing by adopting the selected temperature correcting sheets, putting the selected temperature correcting sheets into the same sample position in the system, and monitoring the laser reflectivity of the surface of the temperature correcting sheets by adopting laser reflectivity monitoring equipment;
the initial temperature of the system is lower than the lowest phase change temperature of the temperature correcting sheet, and the system is heated at the constant heating rate consistent with that of infrared temperature measurement;
when the laser reflectivity is suddenly changed, the phase change temperature of the phase change material used by the temperature correcting sheet is the real temperature of the MOCVD system at the sample position at the moment, and set temperature-real temperature data is obtained;
and correcting a system set temperature-sample temperature curve obtained by the infrared temperature measuring device to be calibrated by using one or more set temperature-real temperature data obtained by the temperature correcting sheet.
In another embodiment of the present disclosure, a method for calibrating temperature field uniformity of an MOCVD equipment by utilizing alloy phase transition is provided, which employs the apparatus as described above, and includes:
selecting a plurality of temperature calibration sheets of a certain type of material system, and putting the temperature calibration sheets into a plurality of different positions to be calibrated in the system;
monitoring the laser reflectivity of the surface of each temperature correcting sheet;
setting the initial temperature of the system to be lower than the lowest phase change temperature of the temperature correcting sheet, and heating at a constant speed of not higher than 1 ℃/min;
and recording the corresponding system set temperature when the laser reflectivity of the surface of each temperature correcting sheet is suddenly changed, obtaining the set temperature values of the plurality of different positions to be temperature corrected in the system, and obtaining the relative distribution trend of the temperature of the system at different positions.
(III) advantageous effects
According to the technical scheme, the device and the method for calibrating the temperature of the MOCVD equipment by utilizing the alloy phase change have at least one of the following beneficial effects:
(1) the black body furnace adopted by the traditional MOCVD equipment black body-infrared temperature calibration method is expensive, and the temperature range of a sample required to be measured in the practical application process is often far away from a standard temperature point, so that the temperature measurement precision of an infrared thermometer cannot meet the requirement; compared with the traditional black body-infrared temperature correction method, the method has the advantages that the alloy phase change calibration device has more acquired real temperature points and low cost, and the calibrated infrared thermometer can keep smaller deviation between the measured temperature and the real temperature in a larger temperature interval;
(2) the alloy phase change calibration device is not influenced by the surface emissivity of the MOCVD tested sample, so that the surface of the MOCVD sample can be prevented from being interfered by a series of factors influencing the surface emissivity, such as high temperature, continuous deposition growth of homogeneous/heterogeneous materials, surface appearance change and the like, and the surface temperature of the sample measured by an infrared thermometer is prevented from drifting and deviating.
Drawings
FIG. 1 is a schematic structural diagram of a temperature calibration sheet for calibrating the temperature of a metal organic chemical vapor deposition apparatus by using alloy phase transition according to an embodiment of the present disclosure.
FIG. 2 is a schematic diagram of a phase-change material layer of a temperature calibration sheet using two elemental film layers according to an embodiment of the disclosure.
FIG. 3 is a schematic diagram of a phase change material layer of a temperature calibration sheet using an alloy thin film layer according to an embodiment of the disclosure.
FIG. 4 is a schematic diagram of a phase change material layer of a temperature calibration sheet formed by mixing an alloy thin film layer and an elemental thin film layer according to an embodiment of the disclosure.
Fig. 5a is a schematic diagram of a method for calibrating an infrared temperature measurement temperature curve of an MOCVD apparatus by using a temperature calibration sheet according to an embodiment of the disclosure.
FIG. 5b is a flowchart of a method for calibrating an infrared temperature measurement temperature curve of an MOCVD apparatus using a temperature calibration sheet according to an embodiment of the disclosure.
FIG. 6a is a flowchart of a method for calibrating system temperature field uniformity using a temperature calibration patch according to an embodiment of the present disclosure.
FIG. 6b is a schematic diagram of an arrangement for calibrating a trend of a temperature distribution inside a system using a temperature calibration patch according to an embodiment of the present disclosure.
[ description of main reference numerals in the drawings ] of the embodiments of the present disclosure
10. A base material layer; 20. phase change material layer
200. A layer of alloy material;
201. a first elemental film layer; 202. second simple substance film layer
Detailed Description
Compared with the traditional MOCVD equipment black body-infrared temperature correction method, the device for correcting the temperature by using the alloy phase change has the advantages of multiple acquired real temperature points and low cost. At present, a blackbody furnace for commercial infrared temperature measurement calibration is expensive and generally has only one standard temperature point. Therefore, when the traditional blackbody-infrared temperature correction method is adopted, firstly, theoretical blackbody emissivity (and other related) parameters of a measured material (related parameters of part of common materials are built in a general infrared thermometer) are input into the infrared thermometer, and then temperature correction is carried out according to a standard temperature point provided by the blackbody furnace. According to the infrared thermometer corrected by the method, the farther the sample temperature is away from the temperature correction point of the black body furnace, the larger the deviation between the measured temperature and the real temperature of the surface of the sample is. However, in practical applications, the temperature range of the sample to be measured is often far from the standard temperature point, so that the temperature measurement precision of the infrared thermometer cannot meet the requirement.
The temperature calibration device utilizing alloy phase change adopts a series of temperature calibration sheets with specific phase change temperature points, specifically comprises five types of aluminum germanium, aluminum silicon, silver germanium, silver silicon and silver nickel, and obtains the real temperature of the measured position by utilizing the sudden change of the surface laser reflectivity of the phase change material layer on the surface of the temperature calibration sheet in the phase change process; and correcting an infrared temperature measurement temperature curve corresponding to the set temperature according to the corresponding relation between the set temperature and the real temperature. The cost of the temperature calibration device utilizing alloy phase change is very low compared with that of a blackbody furnace, and five different real temperature points can be arranged at 400-1000 ℃ (the temperature of most III-V group compounds grown by the MOCVD equipment is in the temperature interval). An infrared thermometer calibrated using five real temperature points can maintain a small deviation between the measured temperature and the real temperature over a larger temperature interval.
In addition, the temperature calibration device utilizing alloy phase change can not be influenced by the surface emissivity of the MOCVD detected sample. As mentioned above, the surface temperature of the sample measured by the infrared thermometer is related to the emissivity of the surface material of the sample, and in the practical application process, the surface of the MOCVD sample is interfered by a series of factors influencing the surface emissivity, such as high temperature, continuous deposition growth of homogeneous/heterogeneous materials, surface morphology change and the like, so that the surface temperature of the sample measured by the infrared thermometer drifts and deviates. In the blackbody-infrared temperature calibration method, the material emissivity parameter in the infrared thermometer is an experience parameter built in the system, that is, a standard temperature point during blackbody-infrared temperature calibration may have a certain deviation from the real temperature of the sample surface of the measured temperature point in practical application. The alloy phase change calibration device disclosed by the invention adopts the alloy phase change principle, and the real temperature of the position of a reacted sample is not influenced by the emissivity of the surface material of the sample.
Therefore, the infrared temperature measurement curve can be corrected under the conditions that no black body furnace exists and the emissivity parameter of the measured material is unknown, and the problem that the infrared temperature measurement curve deviates from the temperature of a real sample in an MOCVD system is solved.
For the purpose of promoting a better understanding of the objects, aspects and advantages of the present disclosure, reference is made to the following detailed description taken in conjunction with the accompanying drawings.
Certain embodiments of the present disclosure will now be described more fully hereinafter with reference to the accompanying drawings, in which some, but not all embodiments of the disclosure are shown. Indeed, various embodiments of the disclosure may be embodied in many different forms and should not be construed as limited to the embodiments set forth herein; rather, these embodiments are provided so that this disclosure will satisfy applicable legal requirements.
In an exemplary embodiment of the present disclosure, an apparatus for calibrating a temperature of a metal organic chemical vapor deposition device by using alloy phase transition is provided, the apparatus includes a temperature calibration sheet having a surface material layer with a specific phase transition temperature point, the temperature calibration sheet is placed at a position in an MOCVD system where temperature calibration is required when temperature calibration is performed, and a real temperature at a sample is obtained by a sudden change in a surface laser reflectivity of the temperature calibration sheet when a phase transition reaction occurs in the surface material layer.
Fig. 1 is a schematic structural diagram of a temperature calibration sheet for calibrating a temperature of a metal organic chemical vapor deposition apparatus by using alloy phase transition according to an embodiment of the disclosure. As shown in fig. 1, the temperature calibration sheet of the present embodiment includes a base material 10 and a phase change material layer 20. Preferably, the phase-change material layer 20 independently selects any one of five material systems of aluminum germanium, aluminum silicon, silver germanium, silver silicon and silver nickel, but is not limited to the above-mentioned preferred types, and those skilled in the art can reasonably design the above-mentioned type of phase-change material 20 according to the needs.
Because the corresponding phase transition temperature points of the aluminum germanium, aluminum silicon, silver germanium, silver silicon and silver nickel material systems are respectively 420 ℃, 577 ℃, 650 ℃, 848 ℃ and 960 ℃, the temperature range completely covers the material epitaxy requirement, and the problem of inconsistent deviation between the set temperature and the actual temperature under different temperature regions is solved.
Further, the alloy component range parameters of the phase change material layer with the same phase change temperature of the five preferred material systems are as follows: the weight ratio of aluminum in the aluminum germanium and aluminum silicon alloy is 2 to 98 percent; the weight ratio of silver in the silver-germanium alloy is 2-90 percent; the weight of silver in the silver-silicon alloy accounts for 1-99 percent; the weight ratio of silver in the silver-nickel alloy is 1-98%.
Specifically, the phase change material layer alloy may adopt a combination of two simple substance thin film layers, or an alloy thin film layer of two simple substance elements, or a combination of a simple substance thin film layer and an alloy thin film layer. The combination of the two simple substance thin film layers and the components of the elements in the alloy thin film layers of the two simple substance elements both meet the range of the alloy components of the phase-change material layer; when the combination of the simple substance thin film layer and the alloy thin film layer is used as the phase-change material layer, the two elements in the simple substance thin film layer and the alloy thin film layer respectively meet the alloy component range of the phase-change material layer, and the total proportion also meets the component range.
In this embodiment, when the phase-change material layer 20 adopts an aluminum-germanium, aluminum-silicon, silver-germanium, silver-silicon alloy system, silicon, sapphire, and silicon carbide can be selected as the base material 10 as required; however, when the phase-change material layer 20 is made of silver-nickel material, silicon should not be used as the material of the substrate 10, because the phase-change process of silver-nickel alloy is affected when silver-silicon or nickel-silicon is contacted.
Further, in selecting the base material 10 of the temperature correcting chip of the present disclosure, a high purity type of wafer material is preferred to avoid possible interference of the base material with the phase transition temperature of the phase change material layer alloy.
As an embodiment of the present disclosure, in the preparation of the phase-change material layer 20 of the temperature calibration sheet of the present disclosure, an alloy form of a simple substance film layer combination may be selected. FIG. 2 is a schematic diagram of a phase-change material layer of a temperature calibration sheet using two elemental film layers according to an embodiment of the disclosure.
As shown in fig. 2, 201 represents a first elemental material in a material system, and 202 represents a second elemental material in the same material system, that is, the phase-change material layer 20 at least includes a first elemental thin film layer 201 and a second elemental thin film layer 202, and the first elemental thin film layer 201 and the second elemental thin film layer 202 are alternately deposited on the substrate material 10 in any order. When the phase-change material layer 20 includes a plurality of first elemental film layers 201 and/or second elemental film layers 202, any one of the first elemental film layers 201 or the second elemental film layers 202 may be selected as the outermost surface layer.
Further, when the elemental thin film material combination is used, as shown in fig. 2, the first elemental thin film layer 201 may be any one of two materials of the material system, and the second elemental thin film layer 202 is another material of the material system. Taking an aluminum-germanium alloy system as an example, when the first elemental film layer 201 is an aluminum elemental film layer, the second elemental film layer 202 is a germanium elemental film layer; when the first elemental substance thin film layer 201 is a germanium elemental substance thin film layer, the second elemental substance thin film layer 202 is an aluminum elemental substance thin film layer. The same applies to other alloy systems. In fig. 2, the first simple substance film layer 201 and the second simple substance film layer 202 are arranged in sequence, but it should be noted that the stacking sequence of the simple substance film layers does not affect the effect of the temperature correcting sheet in this embodiment, that is, the first and last simple substance films from the substrate material 10 to the top can be any of two elements of the material system.
Further, in the phase change material layer 20 system of the present disclosure, the thicknesses of the first simple substance film layer 201 and the second simple substance film layer 202 are preferably between 100nm and 1000nm, and the phase change material layer 20 includes a plurality of first simple substance film layers 201, the film thickness of each first simple substance film layer 201 can be arbitrarily selected, and the second simple substance film layer 202 is the same. However, it should be noted that in the present disclosure, too thick a single thin film layer may cause a time of a method surface reflectivity abrupt change process to be lengthened in an alloy phase change process, thereby affecting the accuracy of temperature calibration.
Further, in the phase change material layer system of the present disclosure, in addition to the structure shown in fig. 2, in the aluminum-silicon-silver-silicon system, when a silicon wafer is used as the base material 10, only one aluminum or silver simple substance thin film layer may be deposited on the silicon substrate to perform the preparation of the temperature calibration sheet. In the temperature correction sheet of such a structure, the silicon constituting the phase change material layer 20 is replaced with a base silicon material. The thickness of the aluminum or silver simple substance thin film layer is preferably between 100nm and 1000 nm.
As another embodiment of the present disclosure, the phase-change material layer 20 may also be an alloy thin film layer, and an alloy material system of the alloy thin film layer should have the same phase-change temperature within a larger composition range, and the phase-change temperature point should have two basic characteristics within a typical application temperature range of MOCVD equipment. According to the phase diagram, five alloy systems of aluminum germanium, aluminum silicon, silver germanium, silver silicon and silver nickel are preferred.
FIG. 3 is a schematic diagram of a phase change material layer of a temperature calibration sheet using an alloy thin film layer according to an embodiment of the disclosure. As shown in fig. 3, the phase change material layer 20 is formed by depositing the temperature correcting plate directly on the base material 10 as the alloy material layer 200 in the form of the alloy material. Wherein the thickness of the alloy material layer 200 is preferably greater than 200 nm.
Further, as shown in fig. 3, for the alloy material layer 200, the preferred weight ratio parameters of the two-phase materials in each alloy system are as follows: the weight ratio of aluminum in the aluminum germanium and aluminum-silicon alloy is preferably 10-90 percent; the weight ratio of silver in the silver-germanium alloy is preferably 10-80%; the weight proportion of silver in the silver-silicon alloy is preferably 10-90 percent; the weight ratio of silver in the silver-nickel alloy is preferably 10-90%.
As another embodiment of the present disclosure, the alloy material layer 200 may further be combined with the first simple substance film layer 201 and the second simple substance film layer 202 of the material system to form the phase change material layer 20. FIG. 4 is a schematic diagram of a phase change material layer of a temperature calibration sheet formed by mixing an alloy thin film layer and an elemental thin film layer according to an embodiment of the disclosure. As shown in fig. 4, in this structure, an alloy material layer 200 may be deposited on a substrate, and then a first elemental thin film layer 201 and a second elemental thin film layer 202 of the same material system may be deposited in any number of layers.
Further, in addition to the structure shown in fig. 4, an arbitrary number of first simple substance thin film layer 201 and second simple substance thin film layer 202 of a certain material system may be deposited on the substrate, and then an alloy material layer 200 of the same material system may be deposited.
Furthermore, the phase change material layer 20 of the method may be formed by combining an alloy material layer 200 of a certain material system and two simple substance film layers of the system, i.e., a first simple substance film layer 201 and a second simple substance film layer 202, in any number of layers and in any order.
The first simple substance film layer 201, the second simple substance film layer 202 and the alloy material layer 200 are preferably deposited on the substrate by adopting a magnetron sputtering or electron beam evaporation method, and the deposition rate is controlled below 1000nm/h so as to obtain a surface which is as bright as possible. In the present disclosure, the phase transition temperature point of the phase change material is closely related to the material purity, and therefore, the raw material should be a high-purity material having a purity of more than 99.99%.
In a second exemplary embodiment of the present disclosure, a method for calibrating a temperature of a metal organic chemical vapor deposition apparatus using an alloy phase transition calibration device is provided.
Fig. 5a is a schematic diagram of a method for calibrating an infrared temperature measurement temperature curve of an MOCVD apparatus by using a temperature calibration sheet according to an embodiment of the disclosure. As shown in fig. 5a, in this embodiment, an alloy material is used as a phase change material layer of the temperature calibration sheet, and infrared temperature measurement is calibrated by the temperature calibration sheet.
Fig. 5b is a flowchart of a method for calibrating an infrared temperature measurement temperature curve of an MOCVD device by using a temperature calibration strip according to an embodiment of the present disclosure, and as shown in fig. 5b, the method for calibrating the temperature of the MOCVD device by using the temperature calibration strip according to the first embodiment includes the steps of:
s11, placing the normal sample into the system, using an infrared temperature measuring device which is self-carried by the system or is externally arranged, heating the system at a constant heating rate which is not higher than 1 ℃/min, obtaining the corresponding relation between the set temperature T _ set of the system and the actual temperature T _ true of the surface of the sample, and obtaining the set temperature-sample temperature curve of the infrared temperature measurement of the system. For a general system, T _ true and T _ set can be generally fitted with a quadratic or cubic function;
s12, selecting one or more of aluminum germanium, aluminum silicon, silver germanium, silver silicon and silver nickel temperature correcting sheets according to the T _ true temperature zone range;
s13, adopting the selected temperature correcting sheets to respectively carry out tests, putting the selected temperature correcting sheets into the same sample position in the system, and monitoring the laser reflectivity of the surface of the temperature correcting sheets by using laser reflectivity monitoring equipment which is arranged on the system or is externally arranged;
s14, setting the initial temperature of the system to be lower than the lowest phase change temperature of the temperature correcting sheet, and heating at the constant temperature rise rate consistent with that during infrared temperature measurement;
s15, when the laser reflectivity is suddenly changed, the phase change temperature of the phase change material used by the temperature correcting sheet is the real temperature of the MOCVD system at the sample position at the moment, and set temperature-real temperature data are obtained;
and S16, correcting the system set temperature-sample temperature curve obtained by infrared temperature measurement by using one or more set temperature-real temperature data obtained by the temperature correcting sheet.
In a third exemplary embodiment of the present disclosure, a method for calibrating system temperature field uniformity using an alloy phase change calibration device is provided.
FIG. 6a is a flowchart of a method for calibrating system temperature field uniformity using a temperature calibration patch according to an embodiment of the present disclosure. As shown in fig. 6a, the method for calibrating the uniformity of the temperature field of the system by using the temperature calibration sheet in this embodiment includes the following specific steps:
s21, selecting a certain type of temperature correcting sheet, and placing the temperature correcting sheet into a plurality of different positions to be temperature corrected in the system (FIG. 6b is a schematic layout diagram of the temperature distribution trend in the system calibrated by using the temperature correcting sheet in the embodiment of the disclosure, and FIG. 6b schematically depicts 4 position points);
s22, monitoring the laser reflectivity of the surface of each temperature correcting sheet;
s23, setting the initial temperature of the system to be lower than the lowest phase change temperature of the temperature correcting sheet, and heating at a constant speed of not higher than 1 ℃/min;
and S24, recording the corresponding system set temperature when the laser reflectivity of the surface of each temperature correcting sheet changes suddenly, and obtaining four set temperature values of T1, T2, T3 and T4.
The four temperature values of T1, T2, T3 and T4 reflect the relative distribution trend of the temperature at the 4 positions of the system. When a plurality of temperature measuring positions are not positioned on the same laser light path for monitoring the reflectivity, the process can be repeated for a plurality of times.
The method for calibrating temperature by alloy transformation according to the present disclosure is further explained with reference to the following embodiments.
Example 1
The preparation method and the application method of the temperature correcting sheet using the alloy phase transition temperature calibration provided by the embodiment comprise the following steps:
the method comprises the steps of sequentially depositing 2 periods of a 500 nm-thick germanium simple substance film and a 500 nm-thick aluminum simple substance film on a sapphire wafer substrate by adopting an electron beam evaporation technology to prepare the aluminum germanium film.
The same method is adopted to prepare aluminum silicon, silver germanium, silver silicon and silver nickel. The structure of each temperature correcting sheet is as follows:
aluminum silicon: sapphire substrate \500nm silicon \500nm aluminum;
silver and germanium: sapphire substrate \500nm germanium \500nm silver;
silver silicon: sapphire substrate \500nm silicon \500nm silver;
silver nickel: sapphire substrate \500nm nickel \500nm silver.
The method is used for correcting the temperature curve of a certain MOCVD system between 400 ℃ and 1000 ℃, and comprises the following steps:
s101, heating at a constant heating rate of 1 ℃/min by using a system infrared temperature measuring device to obtain a corresponding relation between a system set temperature T _ set (x) and an actual temperature T _ true (y) of the surface of the sapphire sample. Fitting T _ true (y) and T _ set (x) by a cubic function to obtain a function of y ═ f (x);
s102, the five temperature correcting pieces of aluminum germanium, aluminum silicon, silver germanium, silver silicon and silver nickel are respectively placed at the same sample position in the system, and the reflectivity of the surface of each temperature correcting piece is monitored by using laser reflectivity equipment which is arranged in the system or is externally arranged;
s103, setting the initial temperature of the system as room temperature, and heating at a constant heating rate which is consistent with that during infrared temperature measurement, namely 1 ℃/min;
s104, when the laser reflectivity is suddenly changed, the phase change temperature of the phase change material used by the temperature correcting sheet is the real temperature of the system at the temperature correcting sheet, and when the laser reflectivity of the surfaces of the aluminum germanium, aluminum silicon, silver germanium, silver silicon and silver nickel is gradually changed, the temperature correcting process is finished;
s105, 5 pieces of real temperature point data are obtained, and y ═ f (x) functions obtained by infrared temperature measurement are corrected by using the five pieces of temperature data.
Specifically, the 5 real temperature point data were aluminum germanium T _ set (x1) 420 ℃, aluminum silicon T _ set (x2) 577 ℃, silver germanium T _ set (x3) 650 ℃, silver silicon T _ set (x4) 848 ℃, silver nickel T _ set (x5) 960 ℃, respectively; therefore, in the function y ═ f (x) obtained by infrared temperature measurement, the true temperatures corresponding to the set temperatures x1 to x5 were 420 ℃, 577 ℃, 650 ℃, 848 ℃, 960 ℃, respectively; these five temperature data are used to correct the infrared thermometry resulting in y ═ f (x) function.
Example 2
The method for implementing the temperature field uniformity of the temperature calibration system by using the temperature calibration sheet provided by the embodiment comprises the following steps:
s201, sequentially depositing 2 periods of a 500 nm-thick germanium simple substance film and a 500 nm-thick aluminum simple substance film on a sapphire wafer substrate by adopting an electron beam evaporation technology to prepare an aluminum-germanium temperature correcting sheet;
s202, placing five aluminum-germanium temperature correcting sheets at different positions in the system respectively, and monitoring the reflectivity of the surface of the temperature correcting sheet by using laser reflectivity monitoring equipment which is arranged in the system or is externally arranged;
s203, setting the initial temperature of the system as room temperature, and heating at a constant heating rate of 1 ℃/min;
s204, when the laser reflectivity of a certain aluminum germanium temperature correcting sheet changes suddenly, recording the system set temperature T corresponding to the position;
s205, when the laser reflectivity of the five aluminum-germanium temperature correcting sheets all changes suddenly, ending the temperature correcting process to obtain the set temperature T1-T5 of five points, wherein the T1-T5 reflect the relative height of the actual temperature of the five points.
So far, the embodiments of the present disclosure have been described in detail with reference to the accompanying drawings. It is to be noted that, in the attached drawings or in the description, the implementation modes not shown or described are all the modes known by the ordinary skilled person in the field of technology, and are not described in detail. Further, the above definitions of the various elements and methods are not limited to the various specific structures, shapes or arrangements of parts mentioned in the examples, which may be easily modified or substituted by those of ordinary skill in the art.
And the shapes and sizes of the respective components in the drawings do not reflect actual sizes and proportions, but merely illustrate the contents of the embodiments of the present disclosure. Furthermore, in the claims, any reference signs placed between parentheses shall not be construed as limiting the claim.
Unless otherwise indicated, the numerical parameters set forth in the specification and attached claims are approximations that can vary depending upon the desired properties sought to be obtained by the present disclosure. In particular, all numbers expressing quantities of ingredients, reaction conditions, and so forth used in the specification and claims are to be understood as being modified in all instances by the term "about". Generally, the expression is meant to encompass variations of ± 10% in some embodiments, 5% in some embodiments, 1% in some embodiments, 0.5% in some embodiments by the specified amount.
Furthermore, the word "comprising" does not exclude the presence of elements or steps not listed in a claim. The word "a" or "an" preceding an element does not exclude the presence of a plurality of such elements.
The use of ordinal numbers such as "first," "second," "third," etc., in the specification and claims to modify a corresponding element does not by itself connote any ordinal number of the element or any ordering of one element from another or the order of manufacture, and the use of the ordinal numbers is only used to distinguish one element having a certain name from another element having a same name.
In addition, unless steps are specifically described or must occur in sequence, the order of the steps is not limited to that listed above and may be changed or rearranged as desired by the desired design. The embodiments described above may be mixed and matched with each other or with other embodiments based on design and reliability considerations, i.e., technical features in different embodiments may be freely combined to form further embodiments.
The algorithms and displays presented herein are not inherently related to any particular computer, virtual machine, or other apparatus. Various general purpose systems may also be used with the teachings herein. The required structure for constructing such a system will be apparent from the description above. Moreover, this disclosure is not directed to any particular programming language. It is appreciated that a variety of programming languages may be used to implement the present disclosure as described herein, and any descriptions above of specific languages are provided for disclosure of enablement and best mode of the present disclosure.
The disclosure may be implemented by means of hardware comprising several distinct elements, and by means of a suitably programmed computer. Various component embodiments of the disclosure may be implemented in hardware, or in software modules running on one or more processors, or in a combination thereof. Those skilled in the art will appreciate that a microprocessor or Digital Signal Processor (DSP) may be used in practice to implement some or all of the functionality of some or all of the components in the relevant apparatus according to embodiments of the present disclosure. The present disclosure may also be embodied as apparatus or device programs (e.g., computer programs and computer program products) for performing a portion or all of the methods described herein. Such programs implementing the present disclosure may be stored on a computer-readable medium or may be in the form of one or more signals. Such a signal may be downloaded from an internet website or provided on a carrier signal or in any other form.
Those skilled in the art will appreciate that the modules in the device in an embodiment may be adaptively changed and disposed in one or more devices different from the embodiment. The modules or units or components of the embodiments may be combined into one module or unit or component, and furthermore they may be divided into a plurality of sub-modules or sub-units or sub-components. All of the features disclosed in this specification (including any accompanying claims, abstract and drawings), and all of the processes or elements of any method or apparatus so disclosed, may be combined in any combination, except combinations where at least some of such features and/or processes or elements are mutually exclusive. Each feature disclosed in this specification (including any accompanying claims, abstract and drawings) may be replaced by alternative features serving the same, equivalent or similar purpose, unless expressly stated otherwise. Also in the unit claims enumerating several means, several of these means may be embodied by one and the same item of hardware.
Similarly, it should be appreciated that in the foregoing description of exemplary embodiments of the disclosure, various features of the disclosure are sometimes grouped together in a single embodiment, figure, or description thereof for the purpose of streamlining the disclosure and aiding in the understanding of one or more of the various disclosed aspects. However, the disclosed method should not be interpreted as reflecting an intention that: that is, the claimed disclosure requires more features than are expressly recited in each claim. Rather, as the following claims reflect, disclosed aspects lie in less than all features of a single foregoing disclosed embodiment. Thus, the claims following the detailed description are hereby expressly incorporated into this detailed description, with each claim standing on its own as a separate embodiment of this disclosure.
The above-mentioned embodiments are intended to illustrate the objects, aspects and advantages of the present disclosure in further detail, and it should be understood that the above-mentioned embodiments are only illustrative of the present disclosure and are not intended to limit the present disclosure, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present disclosure should be included in the scope of the present disclosure.
Claims (16)
1. A device for calibrating the temperature of MOCVD equipment by utilizing alloy phase change is characterized by comprising the following components:
the temperature correcting sheet comprises a phase change material layer (20), the phase change material layer (20) is provided with a preset phase change temperature point, the temperature correcting sheet is arranged at a sample of the MOCVD equipment, and the real temperature of the sample is obtained through the surface laser reflectivity mutation of the temperature correcting sheet when the phase change material layer (20) is subjected to phase change reaction.
2. The apparatus of claim 1, wherein the temperature calibration patch further comprises:
a base material (10), the phase change material layer (20) being deposited in a thin film on the base material (10).
3. The device according to claim 2, characterized in that the material of the phase change material layer (20) is selected from the same material system comprising an aluminum germanium, aluminum silicon, silver germanium, silver silicon or silver nickel material system, corresponding to predetermined phase change temperature points of 420 ℃, 577 ℃, 650 ℃, 848 ℃, 960 ℃, respectively.
4. The device according to claim 2, wherein the phase change material layer (20) comprises an elemental thin film layer and/or an alloy material layer.
5. The device according to claim 4, wherein the phase-change material layer (20) comprises at least one first elemental film layer (201) and at least one second elemental film layer (202), and the materials of the first elemental film layer (201) and the second elemental film layer (202) are two different elemental elements in the same material system.
6. The apparatus of claim 5, wherein the first elemental thin film layer (201) and the second elemental thin film layer (202) are alternately deposited on the substrate material (10) in any order and the thickness of each elemental thin film layer is any value within a first predetermined thickness range.
7. The device of claim 6, wherein the first predetermined thickness is in a range of 100nm to 1000 nm.
8. The device according to claim 4, wherein the phase change material layer (20) comprises at least one layer (200) of an alloy material, the alloy material layer (200) having a thickness within a second predetermined thickness range.
9. The apparatus of claim 8, wherein the second predetermined thickness range is greater than 200 nm.
10. The device according to claim 4, wherein the phase change material layer (20) comprises at least one elemental thin film layer and at least one alloy material layer (200), the materials in the elemental thin film layer and the alloy material layer (200) are selected from two elements in the same material system, and the at least one elemental thin film layer and the at least one alloy material layer (200) are arranged in any sequence and number of layers and are deposited on the substrate material (10).
11. The device according to claim 3, characterized in that the phase change material layer (20), when aluminum germanium, aluminum silicon alloy is used, the aluminum accounts for preferably 2-98% by weight; when the Ag-Ge alloy is adopted, the weight ratio of Ag is 2-90%; when the silver-silicon alloy is adopted, the weight ratio of silver is 1-99 percent; when the silver-nickel alloy is adopted, the weight percentage of silver is 1 to 98 percent.
12. The apparatus of claim 3,
when the phase change material layer (20) is selected from any one of four material systems of aluminum germanium, aluminum silicon, silver germanium and silver silicon, the substrate material (10) is silicon, sapphire or silicon carbide wafer;
when the phase change material layer (20) is a silver-nickel material system, the substrate material (10) is a sapphire or silicon carbide wafer.
13. The device according to claim 2, wherein when the substrate material (10) is a silicon substrate, the phase change material layer (20) comprises an elemental thin film layer, and the elemental thin film layer forms the phase change material by cooperating with the silicon substrate.
14. The device of claim 13, wherein the single thin film layer is an elemental aluminum thin film layer or an elemental silver thin film layer.
15. A method for calibrating the temperature of MOCVD equipment using alloy phase transition, using the apparatus of any one of claims 1 to 14, the method comprising:
placing a sample into the system, heating the system at a constant heating rate of not higher than 1 ℃/min, and obtaining a corresponding relation between a set temperature T _ set of the system and an actual temperature T _ true of the surface of the sample by using an infrared temperature measuring device to be calibrated to obtain a set temperature-sample temperature curve of infrared temperature measurement of the system;
selecting one or more temperature correcting sheets of different material systems according to the actual temperature T _ true temperature zone range of the surface of the sample;
respectively testing by adopting the selected temperature correcting sheets, putting the selected temperature correcting sheets into the same sample position in the system, and monitoring the laser reflectivity of the surface of the temperature correcting sheets by adopting laser reflectivity monitoring equipment;
setting the initial temperature of the system to be lower than the lowest phase change temperature of the temperature correcting sheet, and heating at the constant temperature rise rate consistent with that during infrared temperature measurement;
when the laser reflectivity is suddenly changed, the phase change temperature of the phase change material used by the temperature correcting sheet is the real temperature of the MOCVD system at the sample position at the moment, and set temperature-real temperature data is obtained;
and correcting a system set temperature-sample temperature curve obtained by the infrared temperature measuring device to be calibrated by using one or more set temperature-real temperature data obtained by the temperature correcting sheet.
16. A method for calibrating temperature field uniformity of MOCVD equipment using alloy phase transformation, using the apparatus of any one of claims 1-14, the method comprising:
selecting a plurality of temperature calibration sheets of a certain type of material system, and putting the temperature calibration sheets into a plurality of different positions to be calibrated in the system;
monitoring the laser reflectivity of the surface of each temperature correcting sheet;
setting the initial temperature of the system to be lower than the lowest phase change temperature of the temperature correcting sheet, and heating at a constant speed of not higher than 1 ℃/min;
and recording the corresponding system set temperature when the laser reflectivity of the surface of each temperature correcting sheet is suddenly changed, obtaining the set temperature values of the plurality of different positions to be temperature corrected in the system, and obtaining the relative distribution trend of the temperature of the system at different positions.
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