CN113252176A - Sapphire inoculation point high-precision sensing device and method based on radiation spectrum - Google Patents
Sapphire inoculation point high-precision sensing device and method based on radiation spectrum Download PDFInfo
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- 238000001228 spectrum Methods 0.000 title claims abstract description 63
- 238000011081 inoculation Methods 0.000 title claims abstract description 57
- 230000005855 radiation Effects 0.000 title claims abstract description 40
- 229910052594 sapphire Inorganic materials 0.000 title claims abstract description 32
- 239000010980 sapphire Substances 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000001514 detection method Methods 0.000 claims abstract description 9
- 238000005070 sampling Methods 0.000 claims abstract description 7
- 230000003595 spectral effect Effects 0.000 claims description 27
- 238000007405 data analysis Methods 0.000 claims description 22
- 239000000523 sample Substances 0.000 claims description 18
- 238000013459 approach Methods 0.000 claims description 9
- 239000000155 melt Substances 0.000 claims description 8
- 238000009826 distribution Methods 0.000 claims description 3
- 238000010899 nucleation Methods 0.000 claims description 3
- 238000005516 engineering process Methods 0.000 abstract description 4
- 239000007788 liquid Substances 0.000 abstract description 3
- 230000005540 biological transmission Effects 0.000 abstract description 2
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 description 17
- 239000002994 raw material Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000003745 diagnosis Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000008447 perception Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000002096 quantum dot Substances 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
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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
- G01J5/0003—Radiation pyrometry, e.g. infrared or optical thermometry for sensing the radiant heat transfer of samples, e.g. emittance meter
- G01J5/0007—Radiation pyrometry, e.g. infrared or optical thermometry for sensing the radiant heat transfer of samples, e.g. emittance meter of wafers or semiconductor substrates, e.g. using Rapid Thermal Processing
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B17/00—Single-crystal growth onto a seed which remains in the melt during growth, e.g. Nacken-Kyropoulos method
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/20—Aluminium oxides
-
- 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
- G01J5/10—Radiation pyrometry, e.g. infrared or optical thermometry using electric radiation detectors
- G01J5/20—Radiation pyrometry, e.g. infrared or optical thermometry using electric radiation detectors using resistors, thermistors or semiconductors sensitive to radiation, e.g. photoconductive devices
-
- 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
- G01J5/10—Radiation pyrometry, e.g. infrared or optical thermometry using electric radiation detectors
- G01J5/20—Radiation pyrometry, e.g. infrared or optical thermometry using electric radiation detectors using resistors, thermistors or semiconductors sensitive to radiation, e.g. photoconductive devices
- G01J2005/202—Arrays
- G01J2005/204—Arrays prepared by semiconductor processing, e.g. VLSI
Abstract
The invention provides a device and a method for sensing the high precision of a sapphire inoculation point based on a radiation spectrum, belonging to the technical field of safety positioning; the method aims to solve the problems of high misjudgment rate and low automation degree of the existing manual inoculation technology, and the detection of single relevant image characteristics and complex thermal field changes of an optimal inoculation point is not needed; the invention has the technical scheme and the technical effect that the invention utilizes the characteristic that the environment in the crucible is vacuum, greatly reduces the loss in the process of electromagnetic wave transmission, combines the high sensitivity characteristic of the wavelength emitted by the surface of the high-temperature melt to the temperature, judges the stability of the temperature field by analyzing the change characteristic of the spectrum in real time, and when the continuous spectrum curves gradually tend to be consistent, indicates that the liquid level temperature field is in a stable state at the moment, and can consider inoculation. The influence of system errors is effectively eliminated by comparing the spectrum curves of continuous time points, the misjudgment rate of prediction inoculation is low, the spectrum detection sampling period is short, and the requirements on detection real-time performance and automation are met.
Description
Technical Field
The invention belongs to the technical field of safety positioning, and particularly relates to a sapphire inoculation point high-precision sensing device and method based on a radiation spectrum.
Background
Sapphire is an important semiconductor material, has large forbidden band width and small mobility, and is widely applied to industrial production. At present, the method for producing the sapphire is mainly to artificially synthesize the sapphire by a kyropoulos method. Putting raw materials in a crucible, heating the raw materials in a high vacuum environment to melt the raw materials into melt, adjusting the temperature in the crucible, guiding seed crystals with lower temperature to contact the raw material melt under a proper condition, starting to grow crystals at the seed crystals at the inoculation point, and finally growing sapphire crystal ingots with complete shapes in the crucible by controlling the processes of seeding (inoculation), shouldering, constant diameter, ending, annealing and the like.
At present, an artificial inoculation method is mainly adopted, workers judge the optimal inoculation time through past experiences, the method is high in misjudgment rate, the quality of grown crystals needs to be improved, informatization and digitization cannot be achieved, and the sapphire manufacturing quality is unstable and energy consumption is high. Therefore, the high-precision perception crystal growth diagnosis of the seed crystal inoculation point indicates that the scientific problem needs to be solved for the automation of sapphire crystal preparation by the kyropoulos method.
The existing method has low inoculation rate and low automation degree, cannot meet the current requirements for producing high-quality sapphire crystals at high speed, has incomplete scientific basis for high-precision perception of the position and the temperature of the inoculation point of the liquid level of the vacuum high-temperature alumina melt, and has the defect of a seed crystal inoculation and crystal growth criterion index system. The research kyropoulos method for preparing sapphire adopts a high-precision sensing diagnosis prediction method of seed crystal inoculation point radiation spectrum with strong identification capability and good noise resistance, and thoroughly breaks away from the urgent need of artificial experience inoculation.
Disclosure of Invention
The invention overcomes the defects of the prior art, provides a sapphire inoculation point high-precision sensing device and method based on a radiation spectrum, and aims to solve the problems of high misjudgment rate and low automation degree of the existing manual inoculation technology.
In order to achieve the above object, the present invention is achieved by the following technical solutions.
A sapphire inoculation point high-precision sensing device based on radiation spectrum comprises a crucible, a seed rod, a radiation acquisition probe, an observation window, a spectrum analyzer, a data analysis unit and a controller, wherein the crucible comprises a crucible body and a crucible cover, the crucible body is used for bearing high-temperature sapphire melt, and the crucible cover is provided with two through holes for respectively forming the observation window and a support hole of the seed rod; the radiation acquisition probe is fixedly arranged on the upper side of the observation window and is used for acquiring the spectral characteristics of the surface of the molten mass in real time; the spectrum analyzer is used for analyzing the spectrum signal, the display spectrum and the related spectral line information which are acquired by the radiation acquisition probe; the data analysis unit is connected with the spectrum analyzer and analyzes the spectrum analyzed by the spectrum analyzer; the controller is used for controlling the up-and-down movement of the seed rod according to the prediction result obtained by the data analysis unit.
Further, the photosensitive element of the radiation collecting probe is a CCD photosensitive element with 3648-point pixels, and spectral information collected by the CCD photosensitive element is analyzed and tested by a Φ 10mm cosine corrector.
A sapphire inoculation point high-precision sensing method based on a radiation spectrum is used for detection by using a sapphire inoculation point high-precision sensing device based on the radiation spectrum, and comprises the following steps:
the method comprises the following steps: the radiation acquisition probe acquires spectral information in real time, and the spectrum analyzer displays a corresponding spectral curve P (lambda), wherein the horizontal and vertical coordinates of the spectral curve are wavelength (nm) and radiation power (w) of a corresponding wavelength point respectively;
step two: the spectrum analyzer transmits the spectrum information to the data analysis unit according to the set sampling period, and the data analysis unit analyzes the spectrum informationA series of successive spectral analyses received, two spectral curves P successively acquired being continuously calculated1(λ)、 P2(λ) enclosed area | [ P ]1(λ)- P2(lambda) | d lambda, and fitting a curve to establish the relation between the area and time so as to judge the change trend of the area; the X axis of the fitting curve represents time, the Y axis represents area, when the fitting curve gradually approaches to the X axis and the slope approaches to 0, the area approaches to 0 and the spectral curve is more and more stable, the continuously acquired spectral curves tend to be consistent, the temperature field distribution on the surface of the melt is stable, and the optimal inoculation time can be predicted;
step three: and the controller controls the seed rod to reach a proper inoculation position for inoculation according to the optimal inoculation time predicted by the data analysis unit and by combining the distance between the seed rod and the surface of the melt and the movement speed of the seed rod.
Further, the area ^ P1(λ)- P2The integral range of (λ) | d λ is 350nm ultraviolet light to 950nm near infrared light, and the sampling period is freely selected between 0.5 μ s and 5 s.
Further, the data analysis unit empties the current data after completing the prediction of the optimal inoculation timing once, and performs the prediction of the optimal inoculation timing in the next cycle.
Compared with the prior art, the invention has the following beneficial effects: the invention breaks through the defects of high misjudgment rate and low automation degree of the existing manual inoculation technology, and does not have the problem of dependence on assumed conditions or some related radiation parameters; the invention utilizes the characteristic that the crucible environment is vacuum, greatly reduces the loss of electromagnetic waves in the transmission process, combines the high sensitivity characteristic of the wavelength emitted by the surface of the high-temperature melt to the temperature, judges the stability of the temperature field by analyzing the change characteristic of the continuous spectrum in real time, shows that the liquid level temperature field is in a stable state at the moment when the continuous spectrum curves gradually tend to be consistent, is most suitable for inoculation, does not need to detect the single relevant image characteristic of the optimal inoculation point and the change of a complex thermal field, has low misjudgment rate of the predicted inoculation, has short spectrum detection sampling period, and meets the requirements on detection real-time performance and automation.
Drawings
The invention is further described below with reference to the accompanying drawings;
FIG. 1 is a schematic diagram of a device for sensing the high precision of a sapphire inoculation point based on a radiation spectrum, provided by the invention;
FIG. 2 is a flowchart of a method for sensing the high precision of a sapphire inoculation point based on a radiation spectrum provided by the invention;
wherein, 1 is the crucible, 2 is the seed rod, 3 is the radiation acquisition probe, 4 is the observation window, 5 is the spectral analysis appearance, 6 is the data analysis unit, 7 is the controller, 101 is the crucible body, 102 is the crucible lid.
Detailed Description
In order to make the technical problems, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the embodiments and the accompanying drawings, it is to be understood that the specific embodiments described herein are merely illustrative of the present invention and are not intended to limit the present invention, and the technical solutions of the present invention are described in detail with reference to the embodiments and the accompanying drawings, but the scope of protection is not limited thereby.
As shown in figure 1, the sapphire inoculation point high-precision sensing device based on radiation spectrum comprises a crucible 1, a seed rod 2, a radiation acquisition probe 3, an observation window 4, a spectrum analyzer 5, a data analysis unit 6 and a controller 7, wherein the crucible 1 comprises a crucible body 101 and a circular crucible cover 102, the crucible body 101 is used for bearing high-temperature sapphire melt, two through holes are formed in the crucible cover 102 to respectively form a support hole of the observation window 4 and the purple crystal rod, the observation window 4 is arranged on the crucible cover 102 close to the circle center of the crucible cover 102 to ensure that a small-range view field around the inoculation point can be observed, the diameter of the through hole of the observation window 4 is equal to that of the probe of the radiation acquisition probe 3, the support hole is arranged at the circle center of the crucible cover, the aperture of the support hole is equal to or slightly larger than that of the seed rod 2, a seed crystal is arranged at the lower end of the seed rod 2, and an electric telescopic rod is arranged at the upper end, the electric telescopic rod is connected with the controller 7, but it should be understood that other suitable lifting devices can be adopted to replace the electric telescopic rod, the radiation collecting probe 3 is fixedly placed on the upper side of the observation window 4 and is used for collecting the spectral characteristics of the surface of the melt in real time, the photosensitive element of the radiation collecting probe 3 is a CCD photosensitive element with 3648-point pixels, and the spectral information collected by the CCD photosensitive element is analyzed and tested by a phi 10mm cosine corrector; the spectrum analyzer 5 is used for analyzing the spectrum signal, the display spectrum and the related spectral line information which are collected by the radiation collecting probe 3; the data analysis unit 6 is connected with the spectrum analyzer 5 and analyzes the spectrum analyzed by the spectrum analyzer 5; the controller 7 is used for controlling the up-and-down movement of the seed rod 2 through the electric telescopic rod according to the prediction result obtained by the data analysis unit 6.
As shown in fig. 2, the method for sensing the sapphire inoculation point high precision based on the radiation spectrum of the invention uses the sapphire inoculation point high precision sensing device based on the radiation spectrum for detection, and comprises the following steps:
the method comprises the following steps:
the radiation acquisition probe 3 acquires spectral information in real time, and the spectrum analyzer 5 displays a corresponding spectral curve P (lambda) and records a series of related parameters, wherein the horizontal and vertical coordinates of the spectral curve are respectively wavelength (nm) and nanodot radiation power (w).
Step two:
the spectrum analyzer 5 collects spectra every 0.01s, transmits a spectrum curve and related information to the data analysis unit 6, the data analysis unit 6 calculates and analyzes a series of received continuous spectrum curves, continuously calculates the area ^ P1 (lambda) -P2 (lambda) | d lambda enclosed by two continuously collected spectrum curves P1 (lambda) and P2 (lambda), the integral interval is set to be a wave band of 350nm-950nm, and the fitted curve judges the change trend of the area, the X axis of the fitted curve represents time and the Y axis represents area, when the fitted curve gradually approaches the X axis and the slope approaches 0, the area approaches 0 and the fitted curve becomes more and more stable, the continuously collected spectrum curves tend to be consistent, which shows that the temperature field distribution of the melt surface is stable, and the optimal inoculation time can be predicted.
Step three:
the controller 7 controls the seed rod 2 to reach a proper inoculation position for inoculation according to the inoculation time predicted by the data analysis unit 6 and by combining the distance between the seed rod 2 and the melt surface and the movement speed of the seed rod 2.
The data analysis unit 6 empties the current data after completing the prediction of the optimal inoculation timing once, and predicts the optimal inoculation timing in the next cycle.
The working principle of the invention is that the invention does not depend on related hypothesis or critical environment parameters, does not analyze related physicochemical characteristics of isolated spectral curves, but directly judges the variation trend of the consistency of continuously acquired spectral curves according to a certain sampling period, and when the area enclosed by the two continuously acquired spectral curves is smaller and smaller until the area is close to 0, the optimal inoculation point can be predicted; and after the first prediction is finished, clearing the current data and carrying out inoculation prediction in the next period. The invention establishes the sapphire seed crystal inoculation crystal growth high-resolution and noise-resistant semiconductor material preparation automatic detection model, ensures the scientific growth of the sapphire seed crystal, improves the sapphire production efficiency and improves the yield.
The invention is not the best known technology.
While the invention has been described in further detail with reference to specific preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (5)
1. The sapphire inoculation point high-precision sensing device based on radiation spectrum is characterized by comprising a crucible, a seed rod, a radiation acquisition probe, an observation window, a spectrum analyzer, a data analysis unit and a controller, wherein the crucible comprises a crucible body and a crucible cover, the crucible body is used for bearing high-temperature sapphire melt, and the crucible cover is provided with two through holes which respectively form the observation window and a support hole of the seed rod; the radiation acquisition probe is fixedly arranged on the upper side of the observation window and is used for acquiring the spectral characteristics of the surface of the melt in real time; the spectrum analyzer is used for analyzing the spectrum signal, the display spectrum and the related spectral line information which are acquired by the radiation acquisition probe; the data analysis unit is connected with the spectrum analyzer and analyzes the spectrum analyzed by the spectrum analyzer; the controller is used for controlling the up-and-down movement of the seed rod according to the prediction result obtained by the data analysis unit.
2. The device for sensing the sapphire inoculation point high-precision based on the radiation spectrum according to claim 1, wherein the photosensitive element of the radiation collection probe is a CCD photosensitive element with 3648 points in pixel, and spectral information collected by the CCD photosensitive element is analyzed and tested by a phi 10mm cosine corrector.
3. A radiation spectrum-based sapphire inoculation point high-precision sensing method, which is used for detection by the radiation spectrum-based sapphire inoculation point high-precision sensing device according to claims 1-2, and is characterized by comprising the following steps:
the method comprises the following steps: the radiation acquisition probe acquires spectral information in real time, and the spectrum analyzer displays a corresponding spectral curve P (lambda), wherein the horizontal and vertical coordinates of the spectral curve are wavelength (nm) and radiation power (w) of a corresponding wavelength point respectively;
step two: the spectrum analyzer transmits the spectrum information to the data analysis unit according to the set sampling period, and the data analysis unit analyzes a series of received continuous spectrums and continuously calculates two continuously acquired spectrum curves P1(λ)、 P2(λ) enclosed area | [ P ]1(λ)- P2(lambda) | d lambda, and fitting a curve to establish the relation between the area and time so as to judge the change trend of the area; the X axis of the fitting curve represents time, the Y axis represents area, when the fitting curve gradually approaches to the X axis and the slope approaches to 0, the area approaches to 0 and the spectral curve is more and more stable, the continuously acquired spectral curves tend to be consistent, the temperature field distribution on the surface of the melt is stable, and the optimal inoculation time can be predicted;
step three: and the controller controls the seed rod to reach a proper inoculation position for inoculation according to the optimal inoculation time predicted by the data analysis unit and by combining the distance between the seed rod and the surface of the melt and the movement speed of the seed rod.
4. The method for sensing the high accuracy of the sapphire inoculation point based on radiation spectrum according to claim 3, wherein the area ^ PjP1(λ)- P2The integral range of (λ) | d λ is 350nm ultraviolet light to 950nm near infrared light, and the sampling period is freely selected between 0.5 μ s and 5 s.
5. The method as claimed in claim 3, wherein the data analysis unit empties the current data after completing one prediction of the optimal seeding time, and predicts the optimal seeding time in the next cycle.
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