CN113049753A - Preparation and characterization integrated method of high-purity low-dimensional electronic material - Google Patents
Preparation and characterization integrated method of high-purity low-dimensional electronic material Download PDFInfo
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- G01N23/04—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and forming images of the material
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- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
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- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
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Abstract
The high-purity low-dimensional electronic material preparation and characterization system comprises a main interconnection device, a material growth platform, a device processing platform, a test analysis platform and a function adjusting device, and is characterized in that the main interconnection device is composed of 2-10 split devices, different split devices are connected through a T-shaped large transition bin, and a plurality of split devices can be used independently or combined and connected in pairs to form an integrated cavity. The operation method of the high-purity low-dimensional electronic material preparation and characterization system comprises the following steps: (1) putting the experimental raw materials and the device into a T-shaped transition bin; (2) a function adjusting device and an anti-vibration system for adjusting the split device; (3) transferring the feedstock and apparatus to a synthesis zone; (4) carrying out material synthesis; (5) transferring the target material to a characterization area through a T-shaped transition bin; (6) the material morphology and structure characterization (7) transfers the material to a device processing and measuring area (8) through a T-shaped transition bin, and the device processing and measuring (9) closes the equipment. The invention has the beneficial effects that: firstly, the material has high purity and little pollution; secondly, the vibration is small; and the use is convenient, and the maintenance is convenient.
Description
Technical Field
The invention relates to an integrated method for preparing and characterizing electronic materials, in particular to an integrated method for preparing and characterizing high-purity low-dimensional electronic materials.
Background
From the current academic development trends at home and abroad, the research objects of the novel electronic materials show that the dimensions of the novel electronic materials are developed from high dimensions to low dimensions. Micro-nano scale systems in low dimension, such as two-dimensional electronic materials and one-dimensional materials represented by carbon nanotubes, which are led by graphene, transition metal sulfur compounds (TMDCs), two-dimensional transition metal carbon/nitride (MXene), and the like, are becoming the mainstream of research on related electronic materials. Just as the electronic grade high-purity silicon for chips requires 99.999999999% (11, 9), the purity is also a main reason for restricting the further development of these low-dimensional materials. The existing low-dimensional electronic material has low purity due to two main reasons, namely, the material has a complex structure, for example, TMDCs have different phases of 2H and 1T, and carbon nanotubes are divided into a metal type and a semi-conductor type; on the other hand, the huge specific surface area of the low-dimensional material inevitably adsorbs oxygen and water in the existing preparation and processing processes, so that surface doping and structural change are caused. Therefore, how to obtain high-purity low-dimensional electronic materials is a key to seize the manufacturing high point of next-generation electronic information materials and devices.
Chinese patent publication No. CN108061808A provides a vacuum interconnection system and method for nanomaterial experiments. The system comprises a material growth platform, a device process platform, a test analysis platform and an interconnection platform, wherein the growth, the test, the processing and other operations of the material can be carried out in a vacuum environment through vacuum interconnection among the platforms, and a scientific research platform of material, structure and performance relations under various extreme conditions is provided.
Chinese patent publication No. CN209144257U provides a separable vacuum interconnection system, which can realize that a plurality of separate devices can be used independently or combined and connected in pairs to form an integrated cavity for use through the combined connection and separation between main-interconnection fixing devices. The system is flexible and convenient to use, small in occupied area and small in requirements on indoor space and bearing, and the cost of the vacuum interconnection device is greatly reduced.
Chinese patent publication No. CN212375257U provides a superclean bench combination unit, wherein a double-door sterilizer is arranged on one side of the superclean bench, and a carbon dioxide cell incubator is arranged on the other side; during the use, the experiment operation is all carried out in superclean bench, can avoid external world to influence the growth environment of cell completely, does benefit to the growth of cell.
However, the existing nano processing and analysis testing platform cannot provide the anhydrous and oxygen-free environment required by the preparation and characterization of high-purity low-dimensional electronic materials, the common vacuum interconnection technology is only applied in the ultra-high vacuum environment, and cannot be used for the preparation and characterization of wet materials, the requirements on the smoothness and cleanliness of the material surface are strict, and the processing and device preparation processes of many low-dimensional electronic materials are greatly limited. In addition, the existing large-scale processing and characterization platform is expensive in equipment, high in maintenance cost and poor in fault tolerance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides a high-purity low-dimensional electronic material preparation and characterization system, and solves the problems that an ultra-clean operation system in the existing low-dimensional electronic material processing and device preparation process is limited to an ultra-high vacuum environment and cannot be used for preparation and characterization of wet materials, and traditional ultra-clean room equipment is expensive, high in maintenance cost and poor in fault tolerance.
The technical scheme adopted for realizing the purpose of the invention is as follows: a high-purity low-dimensional electronic material preparation and characterization system comprises a main interconnection device, a material growth platform, a device processing platform, a test analysis platform and a function adjusting device, and is characterized in that the main interconnection device consists of 2-10 split devices, different split devices are connected through a T-shaped large transition bin, and a plurality of split devices can be used independently or combined and connected in pairs to form an integrated cavity; the split devices are all provided with independent vacuum systems, purification systems, anti-vibration systems and 2-10 independent glove ports; the function adjusting device consists of an oxygen content detecting and adjusting system and a water vapor content detecting and adjusting system.
The split device is internally provided with more than 10-grade cleaning modules, and the split device is internally provided with an inert gas environment.
The material growth platform comprises but is not limited to a chemical vapor deposition instrument, an electrochemical operation platform, a magnetron sputtering deposition system, a conventional chemical synthesis operation device and the like.
The device processing platform comprises but is not limited to electronic material processing equipment such as a film coating machine, a packaging machine, a micro photoetching machine and the like.
The test analysis platform comprises nano material test equipment such as a scanning electron microscope, a transmission electron microscope, an atomic force microscope, a fiber tensile testing machine and the like.
The integrated method for preparing and characterizing the high-purity low-dimensional electronic material is characterized by comprising the following operation steps:
(1) starting a system power supply, putting the experimental raw materials and the device into a T-shaped large transition bin, then closing the T-shaped large transition bin, adjusting a vacuum system and a purification system, and adjusting the gas atmosphere in the T-shaped large transition bin;
(2) adjusting the function adjusting device and the anti-vibration system in a single split device or all split devices to ensure that parameters adjusted by the internal oxygen content detecting and adjusting system, the water vapor content detecting and adjusting system and the anti-vibration system of the system all meet the requirement of practical operation;
(3) communicating the T-shaped large transition bin with a split device where the material growth platform is located, transferring the raw materials and the device for the experiment to the material growth platform through a glove port, and operating material growth platform equipment to synthesize a target material;
(4) transferring the synthesized target material to a test analysis platform through a glove port for performance test, or transferring the target material to a device processing platform for device assembly, and then transferring the target material to the test analysis platform for performance test;
(5) adjusting and communicating the oxygen content, the water vapor content and the vacuum degree in the T-shaped large transition bin to enable the oxygen content, the water vapor content and the vacuum degree to be consistent with the internal environment of the split device, and transferring the target material, the raw material and the device to the T-shaped large transition bin through a glove port;
(6) and closing a communication switch between the T-shaped large transition bin and the corresponding split device to enable the T-shaped large transition bin and the split device to be in an isolated state, and transferring a target material, an experimental principle and a device.
The invention has the beneficial effects that: the shock absorption degree is high, room temperature atomic imaging can be realized in a split device, and the Z-direction noise is less than 15 pm; high cleanliness reaching the level 10 ultra-clean degree; the glove box regeneration system has the advantages that the use is convenient, the maintenance is convenient, the water solution and the organic solvent can be used in the glove box through the glove box regeneration system, the experiment operation range is widened, and the glove box regeneration system is convenient to use and maintain compared with the traditional ultra-clean room.
Drawings
Fig. 1 is a structural schematic diagram of 3 split devices in a straight-line-shaped arrangement.
Wherein the reference numeral 11-a splitting device I12-a splitting device II 13-a splitting device III
20-T type large transition bin
31-material growth platform 32-device processing platform 33-test analysis platform
41-vacuum system 42-purification system 43-anti-vibration system
51-oxygen content detection and Regulation System 52-Water vapor content detection and Regulation System
53-glove port
Detailed Description
The present invention is further illustrated by the following examples, which are intended to be purely exemplary and are not intended to limit the scope of the invention, as various equivalent modifications of the invention will occur to those skilled in the art upon reading the present specification and which fall within the limits of the appended claims.
Example 1
A high-purity low-dimensional electronic material preparation and characterization system comprises a main interconnection device, a material growth platform, a device processing platform, a test analysis platform and a function adjusting device, and is characterized in that the main interconnection device consists of 2 split devices, different split devices are connected through a T-shaped large transition bin, and the split devices can be used independently; the split devices are all provided with independent vacuum systems, purification systems, anti-vibration systems and 2 independent glove ports; the function adjusting device consists of an oxygen content detecting and adjusting system and a water vapor content detecting and adjusting system.
The inside of the split device is provided with more than 10-grade cleaning modules, and the inside of the split device is in a nitrogen protection environment.
The material growth platform comprises a chemical vapor deposition instrument.
The device processing platform comprises a film coating machine.
The test analysis platform comprises a scanning electron microscope.
The integrated method for preparing and characterizing the high-purity low-dimensional electronic material is characterized by comprising the following operation steps:
(1) starting a system power supply, putting the experimental raw materials and the device into a T-shaped large transition bin, then closing the T-shaped large transition bin, adjusting a vacuum system and a purification system, and adjusting the gas atmosphere in the T-shaped large transition bin;
(2) adjusting the function adjusting device and the anti-vibration system in a single split device or all split devices to ensure that parameters adjusted by the internal oxygen content detecting and adjusting system, the water vapor content detecting and adjusting system and the anti-vibration system of the system all meet the requirement of practical operation;
(3) communicating the T-shaped large transition bin with a split device where the material growth platform is located, transferring the raw materials and the device for the experiment to the material growth platform through a glove port, and operating material growth platform equipment to synthesize a target material;
(4) transferring the synthesized target material to a test analysis platform through a glove port for coating, and then transferring to the test analysis platform for scanning electron microscope testing;
(5) adjusting and communicating the oxygen content, the water vapor content and the vacuum degree in the T-shaped large transition bin to enable the oxygen content, the water vapor content and the vacuum degree to be consistent with the internal environment of the split device, and transferring the target material, the raw material and the device to the T-shaped large transition bin through a glove port;
(6) and closing a communication switch between the T-shaped large transition bin and the corresponding split device to enable the T-shaped large transition bin and the split device to be in an isolated state, and transferring a target material, an experimental principle and a device.
Example 2
A high-purity low-dimensional electronic material preparation and characterization system comprises a main interconnection device, a material growth platform, a device processing platform, a test analysis platform and a function adjusting device, and is characterized in that the main interconnection device consists of 6 split devices, different split devices are connected through a T-shaped large transition bin, and the split devices are combined and connected in pairs to form an integrated cavity for use; the split devices are all provided with independent vacuum systems, purification systems, anti-vibration systems and 6 independent glove ports; the function adjusting device consists of an oxygen content detecting and adjusting system and a water vapor content detecting and adjusting system.
The split device is internally provided with more than 10-grade cleaning modules, and the split device is internally protected by argon.
The material growth platform comprises an electrochemical operation platform, a magnetron sputtering deposition system, conventional chemical synthesis operation equipment and the like.
The device processing platform comprises electronic material processing equipment such as a packaging machine, a micro photoetching machine and the like.
The test analysis platform comprises a transmission electron microscope and an atomic force microscope.
The integrated method for preparing and characterizing the high-purity low-dimensional electronic material is characterized by comprising the following operation steps:
(1) starting a system power supply, putting the experimental raw materials and the device into a T-shaped large transition bin, then closing the T-shaped large transition bin, adjusting a vacuum system and a purification system, and adjusting the gas atmosphere in the T-shaped large transition bin;
(2) adjusting the function adjusting device and the anti-vibration system in a single split device or all split devices to ensure that parameters adjusted by the internal oxygen content detecting and adjusting system, the water vapor content detecting and adjusting system and the anti-vibration system of the system all meet the requirement of practical operation;
(3) communicating the T-shaped large transition bin with a split device where the material growth platform is located, transferring the raw materials and the device for the experiment to the material growth platform through a glove port, and operating material growth platform equipment to synthesize a target material;
(4) transferring the synthesized target material to a test analysis platform through a glove port for performance test, or transferring the target material to a device processing platform for photoetching operation and packaging, and then transferring the target material to the test analysis platform for testing a projection electron microscope and an atomic force microscope;
(5) adjusting and communicating the oxygen content, the water vapor content and the vacuum degree in the T-shaped large transition bin to enable the oxygen content, the water vapor content and the vacuum degree to be consistent with the internal environment of the split device, and transferring the target material, the raw material and the device to the T-shaped large transition bin through a glove port;
(6) and closing a communication switch between the T-shaped large transition bin and the corresponding split device to enable the T-shaped large transition bin and the split device to be in an isolated state, and transferring a target material, an experimental principle and a device.
Example 3
A high-purity low-dimensional electronic material preparation and characterization system comprises a main interconnection device, a material growth platform, a device processing platform, a test analysis platform and a function adjusting device, and is characterized in that the main interconnection device consists of 10 split devices, different split devices are connected through a T-shaped large transition bin, and a plurality of split devices are distributed in a linear shape and connected to form an integrated cavity for use; the split devices are all provided with independent vacuum systems, purification systems, anti-vibration systems and 10 independent glove ports; the function adjusting device consists of an oxygen content detecting and adjusting system and a water vapor content detecting and adjusting system.
The inside of the split device is provided with more than 10-grade cleaning modules, and the inside of the split device is protected by helium gas.
The material growth platform comprises a chemical vapor deposition instrument, an electrochemical operation platform, a magnetron sputtering deposition system and a hydrothermal reaction device.
The device processing platform comprises a film coating machine, a packaging machine and a micro photoetching machine.
The test analysis platform includes but is not limited to a scanning electron microscope, a transmission electron microscope, an atomic force microscope and a fiber tensile testing machine.
The integrated method for preparing and characterizing the high-purity low-dimensional electronic material is characterized by comprising the following operation steps:
(1) starting a system power supply, putting the experimental raw materials and the device into a T-shaped large transition bin, then closing the T-shaped large transition bin, adjusting a vacuum system and a purification system, and adjusting the gas atmosphere in the T-shaped large transition bin;
(2) adjusting the function adjusting device and the anti-vibration system in a single split device or all split devices to ensure that parameters adjusted by the internal oxygen content detecting and adjusting system, the water vapor content detecting and adjusting system and the anti-vibration system of the system all meet the requirement of practical operation;
(3) communicating the T-shaped large transition bin with a split device where the material growth platform is located, transferring the raw materials and the device for the experiment to the material growth platform through a glove port, and operating material growth platform equipment to synthesize a target material;
(4) transferring the synthesized target material to a test analysis platform through a glove port to perform a fiber tension performance test;
(5) adjusting and communicating the oxygen content, the water vapor content and the vacuum degree in the T-shaped large transition bin to enable the oxygen content, the water vapor content and the vacuum degree to be consistent with the internal environment of the split device, and transferring the target material, the raw material and the device to the T-shaped large transition bin through a glove port;
(6) and closing a communication switch between the T-shaped large transition bin and the corresponding split device to enable the T-shaped large transition bin and the split device to be in an isolated state, and transferring a target material, an experimental principle and a device.
The above description is only three specific embodiments of the present invention, but the design concept of the present invention is not limited thereto, and any insubstantial modifications of the present invention with this idea shall fall within the scope of infringing the protection of the present invention. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (6)
1. A high-purity low-dimensional electronic material preparation and characterization system comprises a main interconnection device, a material growth platform, a device processing platform, a test analysis platform and a function adjusting device, and is characterized in that the main interconnection device consists of 2-10 split devices, different split devices are connected through a T-shaped large transition bin, and a plurality of split devices can be used independently or combined and connected in pairs to form an integrated cavity; the split devices are all provided with independent vacuum systems, purification systems, anti-vibration systems and 2-10 independent glove ports; the function adjusting device consists of an oxygen content detecting and adjusting system and a water vapor content detecting and adjusting system.
2. The system for preparing and characterizing high-purity low-dimensional electronic materials according to claim 1, wherein the split devices are each internally provided with a cleaning module of more than 10 levels, and the split devices are internally provided with an inert gas environment.
3. The system for preparing and characterizing high purity low dimensional electronic materials according to claim 1, wherein the material growth platform comprises a chemical vapor deposition system, an electrochemical operating platform, a magnetron sputtering deposition system, and a conventional chemical synthesis operating device.
4. The system for preparing and characterizing high purity low dimensional electronic materials of claim 1, wherein the device processing platform comprises electronic material processing equipment such as film coating machines, packaging machines, and micro-lithography machines.
5. The system for preparing and characterizing high-purity low-dimensional electronic materials according to claim 1, wherein the testing and analyzing platform comprises nano-material testing equipment such as a scanning electron microscope, a transmission electron microscope, an atomic force microscope and a fiber tensile testing machine.
6. An integrated process for the preparation and characterization of high purity, low dimensional electronic materials, according to the system of claim 1, characterized in that it comprises the following operative steps:
(1) starting a system power supply, putting the experimental raw materials and the device into a T-shaped large transition bin, then closing the T-shaped large transition bin, adjusting a vacuum system and a purification system, and adjusting the gas atmosphere in the T-shaped large transition bin;
(2) adjusting the function adjusting device and the anti-vibration system in a single split device or all split devices to ensure that the parameters adjusted by the internal oxygen content detecting and adjusting system, the water vapor content detecting and adjusting system and the anti-vibration system of the system all meet the experimental operation requirements;
(3) communicating the T-shaped large transition bin with a split device where the material growth platform is located, transferring the experimental raw materials and the device to the material growth platform through a glove port, and operating material growth platform equipment to synthesize a target material;
(4) transferring the synthesized target material to a test analysis platform through a glove port for performance test, or transferring the target material to a device processing platform for device assembly, and then transferring the target material to the test analysis platform for performance test;
(5) adjusting and communicating the oxygen content, the water vapor content and the vacuum degree in the T-shaped large transition bin to enable the oxygen content, the water vapor content and the vacuum degree to be consistent with the internal environment of the split device, and transferring the target material, the raw material and the device to the T-shaped large transition bin through a glove port;
(6) and closing a communication switch between the T-shaped large transition bin and the corresponding split device to enable the T-shaped large transition bin and the split device to be in an isolated state, and transferring a target material, an experimental principle and a device.
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