CN111893553A - Intelligent system for synthesizing new material by hydrothermal method and control method - Google Patents
Intelligent system for synthesizing new material by hydrothermal method and control method Download PDFInfo
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- CN111893553A CN111893553A CN202010779192.6A CN202010779192A CN111893553A CN 111893553 A CN111893553 A CN 111893553A CN 202010779192 A CN202010779192 A CN 202010779192A CN 111893553 A CN111893553 A CN 111893553A
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- 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
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/10—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by application of pressure, e.g. hydrothermal processes
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- 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
- C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
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Abstract
The invention belongs to the technical field of intelligent control, and mainly relates to an intelligent system and a control method for hydrothermal synthesis of a new material, which comprises the following steps: hydrothermal reaction system, high in the clouds database, front end webpage, hydrothermal reaction system comprises hydrothermal reaction system, real time monitoring module, data detection record module, the high in the clouds database comprises big data analysis module, experimental data processing module, the front end webpage is provided with experiment reservation page, experimental conditions and looks over the page, experimental data looks over the page, the page is looked over to the reaction process, stops the experiment page. The invention aims to provide an intelligent system and a control method for hydrothermal synthesis of a new material, and the intelligent setting of the system can effectively solve the problem of accurate analysis and processing of experimental data in the new material synthesis process, and effectively improve the experimental quality and the intelligent management level.
Description
Technical Field
The invention belongs to the technical field of intelligent control and Internet of things, and particularly relates to an intelligent system and a control method for hydrothermal synthesis of a new material.
Background
The hydrothermal reaction has obvious environment-friendly characteristic because the reaction medium is water. The hydrothermal method belongs to the category of liquid phase reaction, and is an effective method for carrying out inorganic synthesis and material treatment by adopting an aqueous solution as a reaction system and heating and pressurizing the reaction system in a specific closed reactor, and can realize the reaction under the hydrothermal condition, in the hydrothermal reaction, water can be used as a chemical component to react and participate in the reaction, can be used as a solvent and an expansion promoter, and can also be used as a pressure transfer medium, and the formation and improvement of an inorganic compound are realized by accelerating the permeation reaction and controlling the physicochemical factors of the process, so that the hydrothermal method has the following advantages in the aspect of synthesizing an inorganic nano functional material: obviously reducing the reaction temperature (100 ℃.); the formation and crystallization of the product can be completed in a single step, and the process is simple; the product ratio can be controlled; preparing a single-phase material; the cost is relatively low; crystals with good orientation and perfection are easy to obtain; in the grown crystal, the crystal can be uniformly doped; the atmosphere in which the crystals are formed can be adjusted.
At present, a hydrothermal reaction experiment synthesis process generally needs manual operation experiment, observation of an experiment process, data recording and experiment ending, the whole process has serious dependence on people, the labor intensity is high, the time is long, and large errors are easily caused by no intervention and real-time monitoring in the experiment process. Especially, the monitoring of experiment records and experiment process data is lost, so that the experiment synthesis management is not standard, the quality is not high, the experiment or synthesis effect cannot be achieved, and the experiment process is influenced. Meanwhile, real-time monitoring is not in place, potential safety hazards of experiments are easily caused due to the fact that reaction tanks need to be transferred manually, and the like, and damage risks are brought to experimenters and experiment platforms.
The purpose of the invention is: the intelligent system and the control method are used for solving the problems of intelligent data monitoring, cloud storage, big data analysis, intelligent operation of reaction equipment and the like in the hydrothermal reaction synthesis process of the new material.
In order to achieve the technical purpose, the technical scheme adopted by the invention is as follows:
an intelligent system for hydrothermal synthesis of new materials, comprising: hydrothermal reaction system, high in the clouds database, front end webpage, hydrothermal reaction system comprises hydrothermal reaction system, real time monitoring module, data detection record module, the high in the clouds database comprises big data analysis module, experimental data processing module, the front end webpage is provided with experiment reservation page, experimental conditions and looks over the page, experimental data looks over the page, the page is looked over to the reaction process, stops the experiment page.
Further, the front-end webpage also comprises a login page for identity recognition.
Further, the real-time monitoring module is provided with an alarm module for early warning and reminding.
Further, the hydrothermal reaction system comprises: retort, the supporter that is provided with perception sensor, the arm and the manipulator that can realize X, Y, Z, A axle direction and remove to and be provided with the oven of gate electro-magnet.
Further, the hydrothermal reaction system further comprises: the system comprises an MCU controller for system control and an Ethernet interface for realizing communication between the MCU controller and the mechanical arm, wherein the MCU controller is in real-time communication connection with a cloud database and a front end webpage.
A control method of an intelligent system for synthesizing a new material by a hydrothermal method comprises the following steps:
s1, the laboratory technician opens the front end webpage to enter the reservation page to perform the experiment reservation and waits for the auditor to check;
s2, checking that the hydrothermal reaction system is started to start reaction when the checking is passed, and returning to the step S1 when the checking is not passed;
s3, the data detection recording module records and uploads various detection parameters in the reaction process to a cloud database;
s4, the monitoring module monitors abnormal parameters of the reaction process and uploads real-time data to a cloud database;
s5, executing the step S4 when the reaction process is monitored to be abnormal, and executing the step S6 when the reaction process is monitored to be abnormal;
s6, the real-time monitoring module sends out an early warning to remind experimenters, and the early warning is reminded to eliminate within the set time of the system and the step S5 is returned;
s7, if the early warning reminding is not eliminated within the set time of the system, automatically stopping the experiment;
and S8, when the whole reaction time reaches the preset time, ending the experiment, and if not, returning to the step S2.
Further, the step S1 is specifically as follows:
s101, the experimenter identifies the identity, sets the experiment name, the reaction temperature, the reaction duration and the position number of the to-be-reacted tank, and enters an appointment page through front-end webpage setting to submit and audit information.
Further, the method also comprises the following steps:
the following steps can be carried out by entering an experiment condition viewing page, an experiment data viewing page, a reaction process viewing page and an experiment stopping page through a front-end webpage:
s301, checking a webpage through experimental conditions, checking real-time reaction temperature and residual reaction duration data, and selecting a placement number for a reaction tank after the reaction is finished;
s302, searching a current reaction process or a historical reaction process according to the experiment name and the experiment date through a reaction process viewing page;
and S303, searching current reaction data or historical reaction data according to the experiment name and the experiment date through the experiment data viewing webpage.
Further, the method also comprises the following steps:
s401, the cloud database stores the reaction process and the experimental data, and performs big data analysis processing on the experimental data to provide experimental optimization data support.
Further, the method also comprises the following steps:
s501, receiving an instruction of front-end webpage control software by an MCU (microprogrammed control Unit) controller, sensing the working state of equipment, ignoring the control instruction when the equipment is in a busy state, detecting the states of a designated shelf position number and a designated oven position number when the equipment is in an idle state, and executing the instruction if both the equipment and the equipment are idle;
s502, resetting the reaction equipment, wherein the MCU controller controls the mechanical arm to move towards the directions of an A axis, an X axis, a Y axis and a Z axis so that the mechanical arm corresponds to a target shelf position number, the mechanical arm is used for grabbing the reaction tank for synthesizing materials, the reaction tank runs to a target oven position number, and the reaction tank is placed;
s503, the fixed reaction tank exits from the oven, and the door of the oven is closed through a door-controlled electromagnet, so that the equipment can automatically synthesize materials;
s504, after the synthesis is completed, resetting the A shaft of the mechanical arm and moving the A shaft to the target position of the oven, opening the door of the oven, coordinating the X shaft, the Y shaft and the Z shaft of the mechanical arm to the target position of the oven, clamping the synthesized reaction tank by matching with the mechanical arm, moving the X shaft, the Y shaft and the Z shaft of the mechanical arm to the corresponding position of the storage rack, and placing the reaction tank by using the mechanical arm;
and the data in the reaction process is uploaded to a cloud database in real time for storage and big data analysis, so that data support is provided for material synthesis optimization.
The invention adopting the technical scheme has the advantages that:
1. the standardization and the quality of a hydrothermal reaction synthesis experimental process are effectively improved by combining the Internet of things cloud technology with the hydrothermal reaction system technology;
2. according to the invention, through cooperative control cooperation of the special mechanical mechanism and the control system, intelligent grabbing and transferring of the reaction equipment are realized, and the working efficiency and the intelligent level of experimental synthesis are greatly improved.
Drawings
The invention is further illustrated by the non-limiting examples given in the accompanying drawings;
FIG. 1 is a diagram of an intelligent system framework for hydrothermal synthesis of new materials in accordance with the present invention;
FIG. 2 is a schematic diagram of a hydrothermal reaction system for hydrothermal synthesis of new materials according to the present invention;
FIG. 3 is a flow chart illustrating the control of an intelligent system for hydrothermal synthesis of new materials according to the present invention;
FIG. 4 is a flow chart of the transfer process of the intelligent system reaction tank for hydrothermal synthesis of new materials according to the present invention.
Detailed Description
The present invention will be described in detail with reference to the drawings and specific embodiments, wherein like reference numerals are used for similar or identical parts in the drawings or the description, and implementations not shown or described in the drawings are known to those of ordinary skill in the art. In addition, directional terms, such as "upper", "lower", "top", "bottom", "left", "right", "front", "rear", and the like, used in the embodiments are only directions referring to the drawings, and are not intended to limit the scope of the present invention.
As shown in fig. 1, an intelligent system for hydrothermal synthesis of new materials comprises: hydrothermal reaction system, high in the clouds database, front end webpage, hydrothermal reaction system comprises hydrothermal reaction system, real time monitoring module, data detection record module, the high in the clouds database comprises big data analysis module, experimental data processing module, the front end webpage is provided with experiment reservation page, experimental conditions and looks over the page, experimental data looks over the page, the page is looked over to the reaction process, stops the experiment page. The front-end web page also includes a login page for identification. The real-time monitoring module is provided with an alarm module for early warning and reminding.
A hydrothermal reaction system: carrying out a nano material synthesis experiment by using hydrothermal reaction equipment; the real-time monitoring module records the reaction process in the experiment and uploads the record to the cloud, when abnormality occurs in the experiment process, the monitoring module automatically alarms to remind an experimenter, and if the experimenter does not return to the alarm within the alarm time set by the system to turn off the alarm, the experiment is automatically stopped; and the data detection recording module uploads the detected parameters to the cloud.
Cloud database: storing the reaction process and experimental data; carrying out big data analysis on experimental data; and (6) processing experimental data.
Front-end web page: experiment reservation (setting parameters such as experiment name, experiment temperature, duration and the like, placing a position number of a to-be-reacted tank, and waiting for a manager to pass the reservation); checking experimental conditions (data such as real-time reaction temperature, reaction residual time and the like can be seen, and selecting a placing position number for the reaction tank after the reaction is finished); checking the reaction process (the current reaction process can be seen, and the historical reaction process is searched by the experiment name and the experiment date); checking experimental data (current reaction data can be seen, and historical reaction data is searched through an experimental name and an experimental date); the experiment was stopped (only the administrator level users had this authority).
As shown in fig. 2, the hydrothermal reaction system includes: retort, the supporter that is provided with perception sensor, the arm and the manipulator that can realize X, Y, Z, A axle direction and remove to and be provided with the oven of gate electro-magnet. The hydrothermal reaction system further comprises: the system comprises an MCU controller for system control and an Ethernet interface for realizing communication between the MCU controller and the mechanical arm, wherein the MCU controller is in real-time communication connection with a cloud database and a front end webpage.
As shown in fig. 3, a control method of an intelligent system for hydrothermal synthesis of new materials includes the following steps:
s1, the laboratory technician opens the front end webpage to enter the reservation page to perform the experiment reservation and waits for the auditor to check;
s2, checking that the hydrothermal reaction system is started to start reaction when the checking is passed, and returning to the step S1 when the checking is not passed;
s3, the data detection recording module records and uploads various detection parameters in the reaction process to a cloud database;
s4, the monitoring module monitors abnormal parameters of the reaction process and uploads real-time data to a cloud database;
s5, executing the step S4 when the reaction process is monitored to be abnormal, and executing the step S6 when the reaction process is monitored to be abnormal;
s6, the real-time monitoring module sends out an early warning to remind experimenters, and the early warning is reminded to eliminate within the set time of the system and the step S5 is returned;
s7, if the early warning reminding is not eliminated within the set time of the system, automatically stopping the experiment;
and S8, when the whole reaction time reaches the preset time, ending the experiment, and if not, returning to the step S2.
The step of S1 is as follows:
s101, the experimenter identifies the identity, sets the experiment name, the reaction temperature, the reaction duration and the position number of the to-be-reacted tank, and enters an appointment page through front-end webpage setting to submit and audit information.
In order to further optimize the experimental management, the method also comprises the following steps:
the following steps can be carried out by entering an experiment condition viewing page, an experiment data viewing page, a reaction process viewing page and an experiment stopping page through a front-end webpage:
s301, checking a webpage through experimental conditions, checking real-time reaction temperature and residual reaction duration data, and selecting a placement number for a reaction tank after the reaction is finished;
s302, searching a current reaction process or a historical reaction process according to the experiment name and the experiment date through a reaction process viewing page;
and S303, searching current reaction data or historical reaction data according to the experiment name and the experiment date through the experiment data viewing webpage.
S401, the cloud database stores the reaction process and the experimental data, and performs big data analysis processing on the experimental data to provide experimental optimization data support.
As shown in fig. 4, the specific transfer process of the reaction tank in the hot water reaction system is as follows:
s501, receiving an instruction of front-end webpage control software by an MCU (microprogrammed control Unit) controller, sensing the working state of equipment, ignoring the control instruction when the equipment is in a busy state, detecting the states of a designated shelf position number and a designated oven position number when the equipment is in an idle state, and executing the instruction if both the equipment and the equipment are idle;
s502, resetting the reaction equipment, wherein the MCU controller controls the mechanical arm to move towards the directions of an A axis, an X axis, a Y axis and a Z axis so that the mechanical arm corresponds to a target shelf position number, the mechanical arm is used for grabbing the reaction tank for synthesizing materials, the reaction tank runs to a target oven position number, and the reaction tank is placed;
s503, the fixed reaction tank exits from the oven, and the door of the oven is closed through a door-controlled electromagnet, so that the equipment can automatically synthesize materials;
s504, after the synthesis is completed, resetting the A shaft of the mechanical arm and moving the A shaft to the target position of the oven, opening the door of the oven, coordinating the X shaft, the Y shaft and the Z shaft of the mechanical arm to the target position of the oven, clamping the synthesized reaction tank by matching with the mechanical arm, moving the X shaft, the Y shaft and the Z shaft of the mechanical arm to the corresponding position of the storage rack, and placing the reaction tank by using the mechanical arm;
and the data in the reaction process is uploaded to a cloud database in real time for storage and big data analysis, so that data support is provided for material synthesis optimization.
There is 16 bit numbers on the supporter, has put a photoelectric sensor on the first bit number for the state of perception bit number, when having the retort to place on the bit number, photoelectric sensor output high level signal to the GPIO mouth of MCU controller, and so on, can count the state of sixteen bit numbers on the supporter, for control provides the condition. The gated electromagnet is used for adsorbing the oven door to be tightly closed, and mainly outputs high and low level signals through a GPIO port of the MCU controller, so that the gated electromagnet detects a limit switch signal of the oven door through matching, and the GPIO port of the MCU controller is also used for controlling the opening and closing of the oven door.
The intelligent system and the control method for synthesizing the new material by the hydrothermal method are described in detail above. The description of the specific embodiments is only intended to facilitate an understanding of the method of the invention and its core ideas. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
Claims (10)
1. An intelligent system for hydrothermal synthesis of new materials, comprising: hydrothermal reaction system, high in the clouds database, front end webpage, hydrothermal reaction system comprises hydrothermal reaction system, real time monitoring module, data detection record module, the high in the clouds database comprises big data analysis module, experimental data processing module, the front end webpage is provided with experiment reservation page, experimental conditions and looks over the page, experimental data looks over the page, the page is looked over to the reaction process, stops the experiment page.
2. The intelligent system for hydrothermal synthesis of new materials, according to claim 1, wherein the front-end webpage further includes a login page for identification.
3. The intelligent system for synthesis of new material hydrothermal method according to claim 2, wherein the real-time monitoring module is provided with an alarm module for warning and reminding.
4. The intelligent system for hydrothermally synthesizing new material according to claim 3, wherein the hydrothermal reaction system comprises: retort, the supporter that is provided with perception sensor, the arm and the manipulator that can realize X, Y, Z, A axle direction and remove to and be provided with the oven of gate electro-magnet.
5. The intelligent system for hydrothermally synthesizing new material according to claim 4, wherein the hydrothermal reaction system further comprises: the system comprises an MCU controller for system control and an Ethernet interface for realizing communication between the MCU controller and the mechanical arm, wherein the MCU controller is in real-time communication connection with a cloud database and a front end webpage.
6. A control method of an intelligent system for synthesizing a new material by a hydrothermal method is characterized by comprising the following steps:
s1, the laboratory technician opens the front end webpage to enter the reservation page to perform the experiment reservation and waits for the auditor to check;
s2, checking that the hydrothermal reaction system is started to start reaction when the checking is passed, and returning to the step S1 when the checking is not passed;
s3, the data detection recording module records and uploads various detection parameters in the reaction process to a cloud database;
s4, the monitoring module monitors abnormal parameters of the reaction process and uploads real-time data to a cloud database;
s5, executing the step S4 when the reaction process is monitored to be abnormal, and executing the step S6 when the reaction process is monitored to be abnormal;
s6, the real-time monitoring module sends out an early warning to remind experimenters, and the early warning is reminded to eliminate within the set time of the system and the step S5 is returned;
s7, if the early warning reminding is not eliminated within the set time of the system, automatically stopping the experiment;
and S8, when the whole reaction time reaches the preset time, ending the experiment, and if not, returning to the step S2.
7. The method according to claim 6, wherein the step S1 is as follows:
s101, the experimenter identifies the identity, sets the experiment name, the reaction temperature, the reaction duration and the position number of the to-be-reacted tank, and enters an appointment page through front-end webpage setting to submit and audit information.
8. The method of claim 7, further comprising the steps of:
the following steps can be carried out by entering an experiment condition viewing page, an experiment data viewing page, a reaction process viewing page and an experiment stopping page through a front-end webpage:
s301, checking a webpage through experimental conditions, checking real-time reaction temperature and residual reaction duration data, and selecting a placement number for a reaction tank after the reaction is finished;
s302, searching a current reaction process or a historical reaction process according to the experiment name and the experiment date through a reaction process viewing page;
and S303, searching current reaction data or historical reaction data according to the experiment name and the experiment date through the experiment data viewing webpage.
9. The method of claim 8, further comprising the steps of:
s401, the cloud database stores the reaction process and the experimental data, and performs big data analysis processing on the experimental data to provide experimental optimization data support.
10. The method of claim 9, further comprising the steps of:
s501, receiving an instruction of front-end webpage control software by an MCU (microprogrammed control Unit) controller, sensing the working state of equipment, ignoring the control instruction when the equipment is in a busy state, detecting the states of a designated shelf position number and a designated oven position number when the equipment is in an idle state, and executing the instruction if both the equipment and the equipment are idle;
s502, resetting the reaction equipment, wherein the MCU controller controls the mechanical arm to move towards the directions of an A axis, an X axis, a Y axis and a Z axis so that the mechanical arm corresponds to a target shelf position number, the mechanical arm is used for grabbing the reaction tank for synthesizing materials, the reaction tank runs to a target oven position number, and the reaction tank is placed;
s503, the fixed reaction tank exits from the oven, and the door of the oven is closed through a door-controlled electromagnet, so that the equipment can automatically synthesize materials;
s504, after the synthesis is completed, resetting the A shaft of the mechanical arm and moving the A shaft to the target position of the oven, opening the door of the oven, coordinating the X shaft, the Y shaft and the Z shaft of the mechanical arm to the target position of the oven, clamping the synthesized reaction tank by matching with the mechanical arm, moving the X shaft, the Y shaft and the Z shaft of the mechanical arm to the corresponding position of the storage rack, and placing the reaction tank by using the mechanical arm;
and the data in the reaction process is uploaded to a cloud database in real time for storage and big data analysis, so that data support is provided for material synthesis optimization.
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Application publication date: 20201106 |