CN108998761B - Molybdenum disulfide film and preparation method and preparation system thereof - Google Patents

Molybdenum disulfide film and preparation method and preparation system thereof Download PDF

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CN108998761B
CN108998761B CN201810936808.9A CN201810936808A CN108998761B CN 108998761 B CN108998761 B CN 108998761B CN 201810936808 A CN201810936808 A CN 201810936808A CN 108998761 B CN108998761 B CN 108998761B
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module
molybdenum disulfide
temperature
control module
chip microcomputer
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CN108998761A (en
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周仁龙
杨飒
周桓君
肖鹰翼
刘丹
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GUANGDONG UNIVERSITY OF EDUCATION
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GUANGDONG UNIVERSITY OF EDUCATION
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0623Sulfides, selenides or tellurides
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021Reactive sputtering or evaporation
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24Vacuum evaporation
    • C23C14/28Vacuum evaporation by wave energy or particle radiation
    • C23C14/30Vacuum evaporation by wave energy or particle radiation by electron bombardment
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/54Controlling or regulating the coating process

Abstract

The invention belongs to the technical field of molybdenum disulfide film preparation, and discloses a molybdenum disulfide film, a preparation method and a preparation system thereof, wherein the molybdenum disulfide film and the preparation system thereof comprise: the device comprises a video monitoring module, a temperature detection module, a sealing detection module, a single-chip microcomputer control module, an air exhaust module, a heating module, an adjusting module, a cooling module, an alarm module and a display module. The temperature and the tightness are detected in real time through the temperature detection module and the sealing detection module, and if the detection data is abnormal, the alarm module informs workers to take timely protective measures; meanwhile, the size of the electron beam current for molybdenum metal evaporation, the temperature for sulfur powder evaporation and the growth time are adjusted through the adjusting module, so that the uniform molybdenum disulfide film with controllable layer number is obtained.

Description

Molybdenum disulfide film and preparation method and preparation system thereof
Technical Field
The invention belongs to the technical field of molybdenum disulfide film preparation, and particularly relates to a molybdenum disulfide film, and a preparation method and a preparation system thereof.
Background
Molybdenum disulfide, the english name molybdenum disulfide, the main component of molybdenite. Black solid powder with metallic luster. The chemical formula MoS2, the melting point 1185 ℃, the density of 4.80g/cm3(14 ℃), and the Mohs hardness of 1.0-1.5. Molybdenum disulfide is an important solid lubricant, and is particularly suitable for high temperature and high pressure. It is also diamagnetic and can be used as a linear photoconductor and a semiconductor exhibiting P-type or N-type conductivity, having rectifying and transducing functions. Molybdenum disulfide is also useful as a catalyst for the dehydrogenation of complex hydrocarbons. However, in the existing molybdenum disulfide film preparation process, if the temperature or the sealing is abnormal, workers cannot be informed to adjust the molybdenum disulfide film in time; meanwhile, the prepared molybdenum disulfide film is not uniform and has low quality.
In summary, the problems of the prior art are as follows:
(1) if the temperature or the sealing is abnormal in the existing molybdenum disulfide film preparation process, workers cannot be informed to adjust the temperature or the sealing in time; meanwhile, the prepared molybdenum disulfide film is not uniform and has low quality.
(2) The existing molybdenum disulfide film preparation process has large sampling data volume and long sampling time in video processing.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a molybdenum disulfide film, a preparation method and a preparation system thereof.
The invention is realized in such a way that the preparation method of the molybdenum disulfide film comprises the following steps:
firstly, a video monitoring module, a temperature detection module and a sealing detection module send monitoring videos and detected data to a single chip microcomputer control module; the single chip microcomputer control module receives a video compression sensing model of the video monitoring module;
the video compression perception model is as follows:
Figure BDA0001768032980000021
Figure BDA0001768032980000022
in the formula (I), the compound is shown in the specification,
Figure BDA0001768032980000023
the total number of measurements per frame is
Figure BDA0001768032980000024
Figure BDA0001768032980000025
In order to dynamically measure the number of times,
Figure BDA0001768032980000026
for static measurement times, dynamic quantity observation matrix
Figure BDA0001768032980000027
Sum constant observation matrix
Figure BDA0001768032980000028
In order to measure the value dynamically,
Figure BDA0001768032980000029
for constant measurement values, sequence of measurement results ztAnd observation matrix phitFirst, by measuring the constant term
Figure BDA00017680329800000210
Estimating a sequence of states
Figure BDA00017680329800000211
And then reuse the dynamic measurement
Figure BDA00017680329800000212
And state sequence
Figure BDA00017680329800000213
Decalculation filterbank C ηtIs a systematic error; a is an element of Rd×dIs a state transition matrix; y istIs the video frame at time t, ztIs the observed value at time t;
step two, when the detection is normal, the single chip microcomputer control module starts the air extraction module to vacuumize the background of the cavity of the preparation container to 1 multiplied by 10-3Pa below; then, heating the preparation container to 300-600 ℃ by using a heating module of a heat conduction equation;
the heat conduction equation is:
Figure BDA00017680329800000214
wherein the content of the first and second substances,
Figure BDA00017680329800000215
k is the heat conduction coefficient, c is the specific heat capacity, ρ is the density, u is the temperature, t is the time, a is the temperature conduction coefficient, x, y, z are the paths of heat propagation; there is a heat source with intensity F (x, y, z, t) and the corresponding heat transfer equation is:
Figure BDA0001768032980000031
wherein the content of the first and second substances,
Figure BDA0001768032980000032
adjusting the size of an electron beam flow for molybdenum metal evaporation, the temperature for sulfur powder evaporation and the growth time through an adjusting module to obtain a uniform molybdenum disulfide film with controllable layer number; cooling the preparation container to room temperature by a cooling module;
checking data abnormity through a time series autoregressive model, sending an alarm sound through an alarm module, and finishing through a worker;
the time series autoregressive model is fitted to the state data through a first order AR model, and the formula is as follows:
Figure BDA0001768032980000033
in the formula, xtFor monitoring the time series of data online, etIs a normally distributed sequence, et~N(μe,λ2),xtObeying N (mu, sigma)2) Wherein μ and σ satisfy:
μ=μe/(1-α)
Figure BDA0001768032980000034
for each on-line monitoring state quantity, the corresponding limit value is not exceeded under the normal state, so the corresponding limit value is assumed to be matchedSome t, xtAll belong to the interval [ a, b],a≤xt≤b:
For all a is less than or equal to xt+kDerivation of ≦ b:
a-αkxt≤et+k+αet+k-1+…+αk-1et+1≤b-αkxt
and fifthly, displaying the monitoring video, the temperature detection data and the sealing detection data through a display module, and keeping the ratio of the brightness of each pixel before and after mapping to the local adaptive brightness around the pixel unchanged.
Further, the filter and the window size thereof for calculating the local adaptive brightness of each pixel of the original high dynamic range image by keeping the ratio of the brightness of each pixel before and after mapping to the local adaptive brightness around the pixel unchanged are selected according to a human visual system, and the local adaptive brightness of each pixel of the display image is obtained by mapping the local adaptive brightness of each pixel of the original high dynamic range image by identifying a threshold brightness value mapping curve:
Figure BDA0001768032980000041
wherein L isd(x, y) represents the luminance value of each pixel value of the mapped image, and L (x, y) represents the luminance value of the high dynamic range image; l isa(x, y) represents the locally adaptive luminance of the high dynamic range image; TM (L)a(x, y)) represents LaThe result of the mapping operation of (x, y) is the local adaptive luminance of each pixel of the display image, and TM () is the inverse function of the TVI curve.
Another object of the present invention is to provide a molybdenum disulfide thin film production system for implementing the molybdenum disulfide thin film production method, the molybdenum disulfide thin film production system including:
the device comprises a video monitoring module, a temperature detection module, a sealing detection module, a singlechip control module, an air extraction module, a heating module, an adjustment module, a cooling module, an alarm module and a display module;
the video monitoring module is connected with the single-chip microcomputer control module and is used for monitoring the preparation process in real time through the camera;
the temperature detection module is connected with the single chip microcomputer control module and is used for detecting the temperature of the preparation container in real time through the temperature sensor;
the sealing detection module is connected with the single chip microcomputer control module and is used for detecting the sealing degree of the container in real time through the sealing detector;
the singlechip control module is connected with the video monitoring module, the temperature detection module, the sealing detection module, the air extraction module, the heating module, the adjusting module, the cooling module, the alarm module and the display module and is used for controlling and scheduling each module to work normally;
the air pumping module is connected with the singlechip control module and is used for vacuumizing the background of the cavity of the preparation container to 1 x 10-3Pa below;
the heating module is connected with the single chip microcomputer control module and is used for heating the preparation container to 300-600 ℃;
the adjusting module is connected with the singlechip control module and is used for adjusting the electron beam flow of molybdenum metal evaporation, the temperature of sulfur powder evaporation and the growth time to obtain a uniform molybdenum disulfide film with controllable layer number;
the cooling module is connected with the single chip microcomputer control module and used for cooling the preparation container to room temperature after the growth is finished;
the alarm module is connected with the singlechip control module and used for sending out alarm sound through an alarm if temperature or sealing detection data are abnormal;
and the display module is connected with the single-chip microcomputer control module and used for displaying the monitoring video, the temperature detection data and the sealing detection data.
The invention also aims to provide the molybdenum disulfide film prepared by the preparation method of the molybdenum disulfide film, wherein the molybdenum element in the molybdenum disulfide film is Mo4+Sulfur element and S2-The form exists and the atomic ratio of Mo to S is confirmed to be close to 1: 2 by high resolution atomic percent.
Another object of the present invention is to provide a light-absorbing semiconductor prepared from the molybdenum disulfide thin film.
The invention has the advantages and positive effects that: the temperature and the tightness are detected in real time through the temperature detection module and the sealing detection module, and if the detection data is abnormal, the alarm module informs workers to take timely protective measures; meanwhile, the size of the electron beam current for molybdenum metal evaporation, the temperature for sulfur powder evaporation and the growth time are adjusted through the adjusting module, so that the uniform molybdenum disulfide film with controllable layer number is obtained. The video monitoring module of the invention fully utilizes the intra-frame sparsity and inter-frame correlation of the video under the framework of a compressed sensing theory, divides the video into a dynamic part and a static part, simultaneously samples and respectively processes the dynamic part and the static part, and obtains the key parameters of a first-order autoregressive moving average model of a video state space by using methods such as convex optimization and the like. The results of experiments under a plurality of groups of real scenes show that the model reduces the interframe redundancy and data acquisition quantity to a greater extent, and can still obtain a better reconstruction effect when the video acquisition compression ratio is 100-200. Conclusion combining with compressive sensing and linear prediction technology, a new video acquisition model is provided, the static part and the dynamic part of the video are processed respectively, and the using condition of the model is given. Experimental results show that the model has a good compression effect on videos with small interframe change. According to the invention, a numerical solution of the model is obtained through an online induction heating model based on MATALB, and the temperature field distribution characteristic of the molybdenum disulfide film in the heating process is analyzed through the numerical solution. The display module keeps the ratio of the brightness of each pixel before and after mapping to the local adaptive brightness around the pixel unchanged, thereby reducing the halo degree.
Drawings
FIG. 1 is a flow chart of a method for preparing a molybdenum disulfide film according to the present invention.
FIG. 2 is a schematic diagram of a system for preparing a molybdenum disulfide film according to the present invention;
in fig. 2: 1. a video monitoring module; 2. a temperature detection module; 3. a seal detection module; 4. a single chip microcomputer control module; 5. an air extraction module; 6. a heating module; 7. an adjustment module; 8. a cooling module; 9. an alarm module; 10. and a display module.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The application of the principles of the present invention will be further described with reference to the accompanying drawings and specific embodiments.
As shown in fig. 1, a method for preparing a molybdenum disulfide thin film according to an embodiment of the present invention includes the following steps:
s101: the video monitoring module, the temperature detection module and the sealing detection module send monitoring videos and detected data to the single-chip microcomputer control module;
s102: when the detection is normal, the singlechip control module starts the air extraction module to vacuumize the background of the cavity of the preparation container to 1 × 10-3Pa below; then heating the preparation container to 300-600 ℃ through a heating module;
s103: adjusting the size of an electron beam current for molybdenum metal evaporation, the temperature for sulfur powder evaporation and the growth time through an adjusting module to obtain a uniform molybdenum disulfide film with controllable layer number; cooling the preparation container to room temperature by a cooling module;
s104: if the inspection data is abnormal, an alarm sound is sent out through an alarm module, and the data is trimmed by workers;
s105: and displaying the monitoring video, the temperature detection data and the sealing detection data through the display module.
As shown in fig. 2, a system for preparing a molybdenum disulfide thin film according to an embodiment of the present invention includes: the device comprises a video monitoring module 1, a temperature detection module 2, a sealing detection module 3, a single-chip microcomputer control module 4, an air extraction module 5, a heating module 6, an adjusting module 7, a cooling module 8, an alarm module 9 and a display module 10.
The video monitoring module 1 is connected with the single chip microcomputer control module 4 and is used for monitoring the preparation process in real time through a camera;
the temperature detection module 2 is connected with the single chip microcomputer control module 4 and is used for detecting the temperature of the preparation container in real time through a temperature sensor;
the sealing detection module 3 is connected with the single chip microcomputer control module 4 and is used for detecting the sealing degree of the container in real time through a sealing detector;
the singlechip control module 4 is connected with the video monitoring module 1, the temperature detection module 2, the sealing detection module 3, the air extraction module 5, the heating module 6, the adjusting module 7, the cooling module 8, the alarm module 9 and the display module 10 and is used for controlling and scheduling each module to work normally;
an air pumping module 5 connected with the single chip microcomputer control module 4 and used for vacuumizing the background of the cavity of the preparation container to 1 x 10- 3Pa below;
the heating module 6 is connected with the single chip microcomputer control module 4 and is used for heating the preparation container to 300-600 ℃;
the adjusting module 7 is connected with the singlechip control module 4 and is used for adjusting the electron beam flow of molybdenum metal evaporation, the temperature of sulfur powder evaporation and the growth time to obtain a uniform molybdenum disulfide film with controllable layer number;
the cooling module 8 is connected with the single chip microcomputer control module 4 and is used for cooling the preparation container to room temperature after growth is finished;
the alarm module 9 is connected with the singlechip control module 4 and used for sending out alarm sound through an alarm if temperature or sealing detection data are abnormal;
and the display module 10 is connected with the single-chip microcomputer control module 4 and is used for displaying the monitoring video, the temperature detection data and the sealing detection data.
The application of the principles of the present invention will now be described in further detail with reference to specific embodiments.
The preparation method of the molybdenum disulfide film provided by the embodiment of the invention comprises the following steps:
firstly, a video monitoring module, a temperature detection module and a sealing detection module send monitoring videos and detected data to a single chip microcomputer control module; the single chip microcomputer control module receives a video compression sensing model of the video monitoring module;
the video compression perception model is as follows:
Figure BDA0001768032980000081
xt+1=Axtt
in the formula (I), the compound is shown in the specification,
Figure BDA0001768032980000082
the total number of measurements per frame is
Figure BDA0001768032980000083
Figure BDA0001768032980000084
In order to dynamically measure the number of times,
Figure BDA0001768032980000085
for static measurement times, dynamic quantity observation matrix
Figure BDA0001768032980000086
Sum constant observation matrix
Figure BDA0001768032980000087
Figure BDA0001768032980000088
In order to measure the value dynamically,
Figure BDA0001768032980000089
for constant measurement values, sequence of measurement results ztAnd observation matrix phitFirst, by measuring the constant term
Figure BDA00017680329800000810
Estimating a sequence of states
Figure BDA00017680329800000811
And then reuse the dynamic measurement
Figure BDA00017680329800000812
And state sequence
Figure BDA00017680329800000813
Decalculation filterbank C ηtIs a systematic error; a is an element of Rd×dIs a state transition matrix; y istIs the video frame at time t, ztIs the observed value at time t;
step two, when the detection is normal, the single chip microcomputer control module starts the air extraction module to vacuumize the background of the cavity of the preparation container to 1 multiplied by 10-3Pa below; then, heating the preparation container to 300-600 ℃ by using a heating module of a heat conduction equation;
the heat conduction equation is:
Figure BDA0001768032980000091
wherein the content of the first and second substances,
Figure BDA0001768032980000092
k is the heat conduction coefficient, c is the specific heat capacity, ρ is the density, u is the temperature, t is the time, a is the temperature conduction coefficient, x, y, z are the paths of heat propagation; there is a heat source with intensity F (x, y, z, t) and the corresponding heat transfer equation is:
Figure BDA0001768032980000093
wherein the content of the first and second substances,
Figure BDA0001768032980000094
adjusting the size of an electron beam flow for molybdenum metal evaporation, the temperature for sulfur powder evaporation and the growth time through an adjusting module to obtain a uniform molybdenum disulfide film with controllable layer number; cooling the preparation container to room temperature by a cooling module;
checking data abnormity through a time series autoregressive model, sending an alarm sound through an alarm module, and finishing through a worker;
the time series autoregressive model is fitted to the state data through a first order AR model, and the formula is as follows:
Figure BDA0001768032980000095
in the formula, xtFor monitoring the time series of data online, etIs a normally distributed sequence, et~N(μe,λ2),xtObeying N (mu, sigma)2) Wherein μ and σ satisfy:
μ=μe/(1-α)
Figure BDA0001768032980000096
for each on-line monitoring state quantity, the corresponding limit value should not be exceeded under normal conditions, so it is assumed that all t, xtAll belong to the interval [ a, b],a≤xt≤b:
For all a is less than or equal to xt+kDerivation of ≦ b:
a-αkxt≤et+k+αet+k-1+…+αk-1et+1≤b-αkxt
and fifthly, displaying the monitoring video, the temperature detection data and the sealing detection data through a display module, and keeping the ratio of the brightness of each pixel before and after mapping to the local adaptive brightness around the pixel unchanged.
Further, the filter and the window size thereof for calculating the local adaptive brightness of each pixel of the original high dynamic range image by keeping the ratio of the brightness of each pixel before and after mapping to the local adaptive brightness around the pixel unchanged are selected according to a human visual system, and the local adaptive brightness of each pixel of the display image is obtained by mapping the local adaptive brightness of each pixel of the original high dynamic range image by identifying a threshold brightness value mapping curve:
Figure BDA0001768032980000101
wherein,Ld(x, y) represents the luminance value of each pixel value of the mapped image, and L (x, y) represents the luminance value of the high dynamic range image; l isa(x, y) represents the locally adaptive luminance of the high dynamic range image; TM (L)a(x, y)) represents LaThe result of the mapping operation of (x, y) is the local adaptive luminance of each pixel of the display image, and TM () is the inverse function of the TVI curve.
According to the molybdenum disulfide film prepared by the invention, the molybdenum element in the molybdenum disulfide film is Mo4+Sulfur element and S2-The form exists and the atomic ratio of Mo to S is confirmed to be close to 1: 2 by high resolution atomic percent.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (4)

1. A preparation method of a molybdenum disulfide film is characterized by comprising the following steps:
firstly, a video monitoring module, a temperature detection module and a sealing detection module send monitoring videos and detected data to a single chip microcomputer control module; the single chip microcomputer control module receives a video compression sensing model of the video monitoring module;
the video compression perception model is as follows:
Figure FDA0002365236500000011
xt+1=Axtt
in the formula (I), the compound is shown in the specification,
Figure FDA0002365236500000012
the total number of measurements per frame is
Figure FDA0002365236500000013
Figure FDA0002365236500000014
In order to dynamically measure the number of times,
Figure FDA0002365236500000015
for static measurement times, dynamic quantity observation matrix
Figure FDA0002365236500000016
Sum constant observation matrix
Figure FDA0002365236500000017
Figure FDA0002365236500000018
In order to measure the value dynamically,
Figure FDA0002365236500000019
for constant measurement values, sequence of measurement results ztAnd observation matrix phitFirst, by measuring the constant term
Figure FDA00023652365000000110
Estimating a sequence of states
Figure FDA00023652365000000111
And then reuse the dynamic measurement
Figure FDA00023652365000000112
And state sequence
Figure FDA00023652365000000113
Decalculation filterbank C ηtIs a systematic error; a is an element of Rd×dIs a state transition matrix; y istIs the video frame at time t, ztIs the observed value at time t;
step two, when the detection is normal, the single chip microcomputer control module starts the air extraction module to vacuumize the background of the cavity of the preparation container to 1 multiplied by 10-3Pa below; followed byHeating the preparation container to 300-600 ℃ by using a heating module of a heat conduction equation;
the heat conduction equation is:
Figure FDA00023652365000000114
wherein the content of the first and second substances,
Figure FDA0002365236500000021
k is the heat conduction coefficient, c is the specific heat capacity, ρ is the density, u is the temperature, t is the time, a is the temperature conduction coefficient, x, y, z are the paths of heat propagation; there is a heat source with intensity F (x, y, z, t) and the corresponding heat transfer equation is:
Figure FDA0002365236500000022
wherein the content of the first and second substances,
Figure FDA0002365236500000023
adjusting the size of an electron beam flow for molybdenum metal evaporation, the temperature for sulfur powder evaporation and the growth time through an adjusting module to obtain a uniform molybdenum disulfide film with controllable layer number; cooling the preparation container to room temperature by a cooling module;
checking data abnormity through a time series autoregressive model, sending an alarm sound through an alarm module, and finishing through a worker;
the time series autoregressive model is fitted to the state data through a first order AR model, and the formula is as follows:
Figure FDA0002365236500000024
in the formula, xtFor monitoring the time series of data online, etIs a normally distributed sequence, et~N(μe,λ2),xtObeying N (mu, sigma)2) Is turning toA state distribution in which μ and σ satisfy:
μ=μe/(1-α)
Figure FDA0002365236500000025
for each on-line monitoring state quantity, the corresponding limit value should not be exceeded under normal conditions, so it is assumed that all t, xtAll belong to the interval [ a, b],a≤xt≤b:
For all a is less than or equal to xt+kDerivation of ≦ b:
a-αkxt≤et+k+αet+k-1+…+αk-1et+1≤b-αkxt
displaying the monitoring video, the temperature detection data and the sealing detection data through a display module, and keeping the ratio of the brightness of each pixel before and after mapping to the local adaptive brightness around the pixel unchanged;
the filter and the window size thereof used for calculating the local adaptive brightness of each pixel of the original high dynamic range image are selected according to a human visual system, and the local adaptive brightness of each pixel of the display image is obtained by mapping the local adaptive brightness of each pixel of the original high dynamic range image by identifying a threshold value brightness value mapping curve:
Figure FDA0002365236500000031
wherein L isd(x, y) represents the luminance value of each pixel value of the mapped image, and L (x, y) represents the luminance value of the high dynamic range image; l isa(x, y) represents the locally adaptive luminance of the high dynamic range image; TM (L)a(x, y)) represents LaThe result of the mapping operation of (x, y) is the local adaptive luminance of each pixel of the display image, and TM () is the inverse function of the TVI curve.
2. A molybdenum disulfide thin film production system for implementing the molybdenum disulfide thin film production method according to claim 1, wherein the molybdenum disulfide thin film production system comprises:
the device comprises a video monitoring module, a temperature detection module, a sealing detection module, a singlechip control module, an air extraction module, a heating module, an adjustment module, a cooling module, an alarm module and a display module;
the video monitoring module is connected with the single-chip microcomputer control module and is used for monitoring the preparation process in real time through the camera;
the temperature detection module is connected with the single chip microcomputer control module and is used for detecting the temperature of the preparation container in real time through the temperature sensor;
the sealing detection module is connected with the single chip microcomputer control module and is used for detecting the sealing degree of the container in real time through the sealing detector;
the singlechip control module is connected with the video monitoring module, the temperature detection module, the sealing detection module, the air extraction module, the heating module, the adjusting module, the cooling module, the alarm module and the display module and is used for controlling and scheduling each module to work normally;
the air pumping module is connected with the singlechip control module and is used for vacuumizing the background of the cavity of the preparation container to 1 x 10-3Pa below;
the heating module is connected with the single chip microcomputer control module and is used for heating the preparation container to 300-600 ℃;
the adjusting module is connected with the singlechip control module and is used for adjusting the electron beam flow of molybdenum metal evaporation, the temperature of sulfur powder evaporation and the growth time to obtain a uniform molybdenum disulfide film with controllable layer number;
the cooling module is connected with the single chip microcomputer control module and used for cooling the preparation container to room temperature after the growth is finished;
the alarm module is connected with the singlechip control module and used for sending out alarm sound through an alarm if temperature or sealing detection data are abnormal;
and the display module is connected with the single-chip microcomputer control module and used for displaying the monitoring video, the temperature detection data and the sealing detection data.
3. The molybdenum disulfide thin film prepared by the method for preparing a molybdenum disulfide thin film according to claim 1, wherein the molybdenum element in the molybdenum disulfide thin film is Mo4+Sulfur element and S2-The form exists and the atomic ratio of Mo to S is confirmed to be close to 1: 2 by high resolution atomic percent.
4. A light absorbing semiconductor made from the molybdenum disulfide film of claim 3.
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