CN110895252A - Optical sample rod system for in-situ liquid-gas environment transmission electron microscope - Google Patents
Optical sample rod system for in-situ liquid-gas environment transmission electron microscope Download PDFInfo
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- CN110895252A CN110895252A CN201910912795.6A CN201910912795A CN110895252A CN 110895252 A CN110895252 A CN 110895252A CN 201910912795 A CN201910912795 A CN 201910912795A CN 110895252 A CN110895252 A CN 110895252A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—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
- G01N23/02—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
- 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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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—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
- G01N23/20—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 using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—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
- G01N23/20—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 using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
- G01N23/20025—Sample holders or supports therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/26—Electron or ion microscopes; Electron or ion diffraction tubes
- H01J37/261—Details
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/26—Electron or ion microscopes; Electron or ion diffraction tubes
- H01J37/28—Electron or ion microscopes; Electron or ion diffraction tubes with scanning beams
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Abstract
The invention discloses an optical sample rod system for an in-situ liquid and gas atmosphere transmission electron microscope, which comprises: the sample holder comprises a sealed small sample holder frame, a hollow sample rod frame, gas and liquid conduits, an energy transmission optical fiber, a sealing rubber ring and the like, wherein the sealed small sample holder frame is used for manufacturing liquid and gas environments with different pressures in an ultrahigh vacuum environment. The gas (liquid) environment exists inside the sample rod head frame and is connected with an external gas (liquid) inlet device through a gas (liquid) conduit. One end of the energy transmission optical fiber with the controllable wave band is fixed on the miniature sample stage, and the main body of the energy transmission optical fiber extends out of the clamping groove in the miniature sample stage, penetrates through the sample rod frame and is connected with the external light path unit, and is used for adjusting the illumination environment inside the miniature sample stage. The invention is suitable for exploring physicochemical life reaction processes such as various gas phase reactions, liquid phase reactions, solid-phase gas-phase interfaces, solid-phase liquid-phase interfaces, photochemical reactions and the like.
Description
Technical Field
The invention relates to the field of in-situ experimental research of transmission electron microscope components and nano materials, in particular to an optical sample rod system for a transmission electron microscope in an in-situ liquid-gas environment.
Background
The external environment where the material is located and the interaction between various external fields and the material are sources of structural changes of the material performance and the micro-nano or even atomic scale, and whether the microstructure evolution process of the material under the effects of the external environment and the various external fields where the material is located can be detected in situ on the micro-nano or even the atomic scale becomes a key point for exploring the physical and chemical life characteristics of the material. The in-situ and synchronous high-resolution monitoring technology of the atomic scale structure and the characteristics of the substances under the action of the external field environment directly determines the research capability of the materials, is a common key technology for realizing guidance of material structure design and relevant macroscopic performance adjustment and control in a plurality of fields such as energy, environment, life and the like, and also directly determines whether the international competition of microstructure research in China can continuously maintain advantages. Therefore, the development of atomic scale in-situ, synchronous and dynamic monitoring methods and the improvement of the limit resolution of the observation technology under the environmental action become one of the important research contents in the current microstructure characterization technology project in China.
The in-situ transmission electron microscope technology can be used for in-situ and dynamically observing the relevance between the components and the structure of the material and the macroscopic physical and chemical properties under the gas phase, liquid phase, solid phase and plasma state environment and external parts such as radiation, illumination, external force, heat release, electrification and the like, the observation technology has high resolution characteristics in time and space, the intrinsic performance of the material can be researched from ultrahigh space-time and sub-angstrom microstructure resolution levels, the synthesis and macroscopic performance optimization of the material are promoted, and favorable guidance is provided for the research and development of new materials. The technology is the most advanced and most space-exploring research field in microstructure characterization at present. However, some problems of the in-situ transmission electron microscope technology still restrict the development of China in the field of high-end in-situ transmission electron microscope technology design and research. The method is mainly characterized in that most scientific research units in China only use large-scale analytical instruments for microscopic research, and the products of the instruments, such as a transmission electron microscope, a scanning electron microscope, an atomic force microscope and the like, are seriously dependent on developed countries such as the west, and the high-end characterization equipment almost comes from imports. As a microscopic characterization and analysis technique with the highest development potential and value, the in-situ environmental electron microscopy analysis technique has started to advance greatly in Western countries. In recent years, China has made progress in the field of in-situ transmission electron microscopy, but obviously lags behind the scientific and technological strong countries such as the United states, Japan and the like, and the level of related technical instruments still has a large gap. With the increasing support of scientific research in China, almost all domestic units with transmission electron microscopes have the requirement of in-situ transmission electron microscope sample rod systems. However, the technical difficulty in producing and designing the sample rod system with the in-situ liquid-gas environment and the multi-field synergistic function is great, and the core technology is mastered in the first great hands of foreign industries, so that the in-situ sample rod system commercialized in China is imported by related companies at present. The price of some in-situ transmission electron microscope sample rod systems even exceeds that of the transmission electron microscope, and the development and the application of the in-situ observation technology in China are seriously hindered. The more serious problem is that the use functions of related products imported in China are greatly limited, flexible requirements are customized, and the requirements of scientific research industries in China are difficult to be better met. Therefore, the in-situ sample rod system imported from foreign countries and having a single external environment can not meet the research work requirements in most cases, and the development of China in the in-situ observation technical field is greatly limited. The bought-type technology development mode more importantly enables scientific research in China to lose the capability of original exploration and experience accumulation, and is a great challenge for research and development of a new-generation original scientific research instrument and acquisition of the original technology exploration. Aiming at the technical field of electron microscopes, at present, no commercial sample rod system for a transmission electron microscope capable of realizing an in-situ illumination liquid environment and an in-situ illumination gas environment exists at home and abroad, and based on the appeal and the working basis of the applicant in the field for years, the invention maximally realizes the introduction of a gas environment, a liquid environment and an optical signal in an ultrahigh vacuum environment of the transmission electron microscope to measure and research the evolution process of the macroscopic property and the atomic scale microstructure of a material. The technology is widely applied to the fields of exploring various liquid phase reactions, gas phase reactions, solid-liquid phase interface reactions, solid-gas phase interface reactions, photochemical reactions, life sciences and the like.
Disclosure of Invention
Aiming at the technical problems of the current transmission electron microscope, the invention aims to provide an optical sample rod system for an in-situ liquid-gas environment transmission electron microscope, which can introduce a liquid environment, a gas environment and an optical signal into an ultrahigh vacuum environment in the transmission electron microscope to perform atomic scale characterization measurement and research on the macroscopic property and microstructure of a material.
The technical scheme of the invention is as follows:
an optical sample rod system for an in-situ liquid-gas environment transmission electron microscope comprises a sample rod frame, a high-vacuum circular sealing connector, a liquid-gas dual-purpose guide pipe, a small sample table, an energy transmission optical fiber, a sealed liquid-gas environment chamber, a sealing rubber ring, a cover plate, an external light path unit and the like, wherein the high-vacuum circular sealing connector is used for transmitting liquid and gas and fixing the optical fiber, and the energy transmission optical fiber can transmit light with wavelength ranging from infrared light to ultraviolet light; the concrete structure is as follows:
the sample rod frame is of a hollow structure, and the tail end of the sample rod frame is connected with a high-vacuum circular sealing connector. The high-vacuum round sealing connector is connected with the front end of the sample rod frame through a liquid-gas dual-purpose conduit, and the high-vacuum round sealing connector also comprises a sealing liquid, a gas environment chamber and an external liquid flowing and gas flowing controller which are arranged in the small sample platform; one end of the energy transmission optical fiber is fixed at the back of the small sample stage and forms a certain angle with the small sample stage, and illumination is introduced into a sealed liquid gas environment chamber in the small sample stage through a hole in the middle of the small sample stage. The main body of the energy transmission optical fiber extends out of the small sample platform, penetrates through the sample rod frame and the high-vacuum circular sealing connector and is connected with the external light path unit, and the external light path unit is used for adjusting the illumination environment of the internal liquid or gas environment of the small sample platform.
The cover plate, the sealing rubber ring and the groove in the small sample table form a sealed liquid-gas environment chamber in the small sample table. And the liquid-gas dual-purpose conduit is connected with an external liquid inlet and gas inlet device and is used for monitoring the types and flow rates of liquid and gas in the liquid and gas environment in the small sample stage.
The small sample table is made of materials such as corrosion-resistant titanium alloy, aluminum alloy and copper alloy which are subjected to special surface treatment, so that the corrosion of liquid and gas environments to the small sample table is avoided, and potential safety hazards are prevented. The back of the small sample table is provided with a conical groove structure, so that the signal acquisition of other transmission electron microscopes is facilitated.
The upper surface of the liquid gas environment is sealed by using a cover plate, the liquid environment and the gas environment are isolated from the high vacuum environment in the transmission electron microscope by using the groove of the small sample table and three sealing rubber rings, and the cover plate consists of an aluminum oxide, silicon nitride, a carbon material or a silicon carbide window which is transparent to transmission electron beams and has good stability.
The liquid and gas conduits in the sample rod frame are made of corrosion-resistant materials such as polytetrafluoroethylene plastic materials, so that the internal liquid is prevented from leaking and corroding.
The energy transmission optical fiber capable of transmitting light in the range from infrared light to ultraviolet light is arranged in the groove at the back of the small sample stage, is used for transmitting light signals in a liquid gas environment, and has good chemical and physical stability.
The system can realize atomic scale measurement and research of photochemical performance of the material in a high vacuum of a transmission electron microscope in an illumination environment or a liquid and gas environment, the wavelength range of illumination applied by a small sample stage is 10nm-2000nm, the liquid flow rate is less than or equal to 150 ml/min, the gas flow rate is less than or equal to 150 ml/min, and the gas pressure is controlled to be less than or equal to 3 atmospheric pressures.
The invention has the advantages and beneficial effects that:
1. the invention mainly comprises the following steps: the sample rod comprises a sample rod frame, a high-vacuum circular sealing connector for transmitting liquid (gas) and fixing optical fibers, liquid, a gas dual-purpose guide pipe, a small sample platform, an energy transmission optical fiber capable of transmitting light from infrared light to ultraviolet light range wavelength, sealing liquid, a gas environment chamber, a sealing rubber ring, a cover plate, an external light path unit and the like, wherein the liquid (gas) environment exists inside the sample rod head frame and is connected with external liquid inlet (gas inlet) equipment through the liquid (gas) guide pipe, and the liquid rod is used for monitoring the liquid flow rate inside the small sample platform, the liquid type and liquid flow rate stability and gas pressure, and the gas type and gas flow rate stability. One section of the energy transmission optical fiber with the controllable wave band is fixed on the small sample table, and the main body of the energy transmission optical fiber extends out of the clamping groove in the small sample table, penetrates through the sample rod frame and is connected with the external light path unit, and is used for adjusting the illumination environment of the liquid or gas environment in the small sample table.
2. Based on the in-situ sample rod structure, the system can realize atomic scale measurement and research on macroscopic properties and microstructures of materials in a liquid environment, a gas environment and introduction of optical signals in high vacuum in a transmission electron microscope. The wavelength range of the light applied by the small sample stage is 10nm-2000nm, the liquid flow rate is less than or equal to 150 ml/min, the gas flow rate is less than or equal to 150 ml/min, and the gas pressure is controlled to be less than or equal to 3 atmospheric pressures.
3. The invention utilizes the small sample stage, the cover plate and the sealing rubber ring to jointly form a liquid environment and a gas environment which are isolated from a high vacuum environment.
4. The in-situ illumination function of the invention provides the transmission of light signals in the liquid gas environment by the energy transmission optical fiber which can stably transmit light with the wavelength from infrared light to ultraviolet light.
Drawings
FIG. 1 is an effect diagram of an optical sample rod system for an in-situ liquid-gas environment transmission electron microscope.
Fig. 2 is an assembled perspective view of a small sample stage at the front end of a sample rod.
Fig. 3 is a perspective view of the assembled small sample stage.
Fig. 4 is a schematic front view of the assembled compact sample stage.
The reference numerals are explained below:
1-sample rod frame; 2-high vacuum circular sealing connector; 3-liquid and gas dual-purpose conduit; 4-small sample stage; 5-energy transmission fiber; 6-sealing the liquid gas environment chamber; 7-sealing rubber ring; and 8, covering plates.
Detailed Description
The following detailed description of embodiments of the invention is provided in connection with the accompanying drawings and examples. With respect to the detailed description of these embodiments, it is to be understood that one skilled in the art can practice the invention and that other embodiments may be utilized and that changes and/or modifications may be made to the illustrated examples without departing from the spirit and scope of the appended claims. In addition, although specific features of the invention are disclosed in the embodiments, such specific features can be modified as appropriate to achieve the functions of the invention.
As shown in fig. 1 to 4, the optical sample rod system for in-situ liquid-gas ambient transmission electron microscope of the present invention comprises: sample pole frame (1), high vacuum circular sealed connector (2), liquid gas dual-purpose pipe (3), small-size sample platform (4), biography can optic fibre (5), sealed liquid gas environment cavity (6), sealing rubber circle (7), apron (8) and outside light path unit etc. and specific structure is as follows:
the sample rod frame (1) is of a hollow structure, and the tail end of the sample rod frame (1) is connected with the high-vacuum circular sealing connector (2). The high vacuum and the external atmosphere environment in the sample rod frame (1) are isolated through a high vacuum circular sealing connector (2), and the high vacuum circular sealing connector (2) is connected with a sealing liquid-gas environment chamber (6) arranged in a small sample table (4) at the front end of the sample rod frame (1) and an external liquid flow and gas flow controller through a liquid-gas dual-purpose conduit (3);
one end of the energy transmission optical fiber (5) is fixed at the back of the small sample stage (4), and the energy transmission optical fiber (5) and the small sample stage (4) form a certain angle to introduce illumination into a sealed liquid and gas environment chamber (6) arranged in the small sample stage through a hole in the middle of the small sample stage (4). The main body of the energy transmission optical fiber (5) extends out of the small sample platform (4), passes through the sample rod frame (1) and the high-vacuum circular sealing connector (2) to be connected with the external light path unit, and is used for adjusting the illumination environment of the internal liquid or gas environment of the small sample platform.
As shown in figures 2 and 4, the cover plate (8) is matched with a groove in the small sample platform (4) and a sealing rubber ring (7) is arranged in the groove, and a sealed liquid-gas environment chamber (6) arranged in the small sample platform (4) is formed by the space between the cover plate (8) and the small sample platform (4). The liquid and gas dual-purpose conduit (3) is connected with external liquid inlet or gas inlet equipment, and the liquid and gas dual-purpose conduit (3) can be used for monitoring the types and the flow rates of liquid and gas in the liquid and gas environment in the small sample table (4). The back of the small sample table (4) is provided with a conical groove structure, so that the signal acquisition of other transmission electron microscopes is facilitated.
While the present invention has been described with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, which are illustrative and not restrictive, and it will be apparent to those skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (6)
1. An optical sample rod system for an in-situ liquid-gas environment transmission electron microscope comprises a sample rod frame, a high-vacuum circular sealing connector, a liquid-gas dual-purpose guide pipe, a small sample table, an energy transmission optical fiber, a sealed liquid-gas environment chamber, a sealing rubber ring, a cover plate, an external light path unit and the like, wherein the high-vacuum circular sealing connector is used for transmitting liquid and gas and fixing the optical fiber, and the energy transmission optical fiber can transmit light with wavelength ranging from infrared light to ultraviolet light; the concrete structure is as follows:
the sample rod frame is of a hollow structure, and the tail end of the sample rod frame is connected with the high-vacuum circular sealing connector; the high-vacuum round sealing connector is connected with the front end of the sample rod frame through a liquid-gas dual-purpose conduit, and the high-vacuum round sealing connector also comprises a sealing liquid, a gas environment chamber and an external liquid flowing and gas flowing controller which are arranged in the small sample platform; one end of the energy transmission optical fiber is fixed at the back of the small sample stage and forms a certain angle with the small sample stage, and illumination is introduced into a sealed liquid gas environment chamber in the small sample stage through a hole in the middle of the small sample stage; the main body of the energy transmission optical fiber extends out of the small sample platform, penetrates through the sample rod frame and the high-vacuum circular sealing connector and is connected with the external light path unit, and the external light path unit is used for adjusting the illumination environment of the internal liquid or gas environment of the small sample platform;
the cover plate, the sealing rubber ring and the groove in the small sample table form a sealing liquid-gas environment chamber in the small sample table; and the liquid-gas dual-purpose conduit is connected with an external liquid inlet and gas inlet device and is used for monitoring the types and flow rates of liquid and gas in the liquid and gas environment in the small sample stage.
2. The in-situ liquid-gas environment transmission electron microscope optical sample rod system according to claim 1, wherein: the small sample table is made of corrosion-resistant titanium alloy, aluminum alloy, copper alloy and other materials subjected to special surface treatment, so that the small sample table is prevented from being corroded by liquid and gas environments, and potential safety hazards are prevented; the back of the small sample table is provided with a conical groove structure.
3. The in-situ liquid-gas environment transmission electron microscope optical sample rod system according to claim 1, wherein: the upper surface of the liquid-gas environment is sealed by a cover plate, the liquid environment and the gas environment are isolated from the high vacuum environment in the transmission electron microscope by using the groove of the small sample table and three sealing rubber rings, and the cover plate is composed of an aluminum oxide window, a silicon nitride window, a carbon material window or a silicon carbide window which are transparent to transmission electron beams.
4. The in-situ liquid-gas environment transmission electron microscope optical sample rod system according to claim 1, wherein: the liquid and gas conduits disposed in the sample rod frame are made of corrosion resistant materials such as polytetrafluoroethylene plastic.
5. The in-situ liquid-gas environment transmission electron microscope optical sample rod system according to claim 1, wherein: the energy transmission optical fiber capable of transmitting light in the range from infrared light to ultraviolet light is arranged in the groove at the back of the small sample stage and used for transmitting light signals in the liquid gas environment.
6. The in-situ liquid-gas environment transmission electron microscope optical sample rod system according to claim 1, wherein: the wavelength range of the light applied by the small sample stage is 10nm-2000nm, the liquid flow rate is less than or equal to 150 ml/min, the gas flow rate is less than or equal to 150 ml/min, and the gas pressure is controlled to be less than or equal to 3 atmospheric pressures.
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| CN201910912795.6A CN110895252A (en) | 2019-09-25 | 2019-09-25 | Optical sample rod system for in-situ liquid-gas environment transmission electron microscope |
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| CN201910912795.6A CN110895252A (en) | 2019-09-25 | 2019-09-25 | Optical sample rod system for in-situ liquid-gas environment transmission electron microscope |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116609362A (en) * | 2023-04-28 | 2023-08-18 | 云南大学 | Transmission electron microscope in-situ sample rod for researching magnetic property of nano material and control method |
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| CN103000480A (en) * | 2012-11-29 | 2013-03-27 | 中国科学院物理研究所 | Transmission electron microscope sample rod capable of being added with optical fibers |
| CN207743192U (en) * | 2018-01-08 | 2018-08-17 | 中国科学院金属研究所 | A kind of transmission electron microscope electricity sample lever system in situ |
| CN207993796U (en) * | 2018-01-22 | 2018-10-19 | 关一 | A kind of transmission electron microscope specimen holder in situ |
| CN109490344A (en) * | 2018-08-21 | 2019-03-19 | 厦门芯极科技有限公司 | A kind of example of transmission electron microscope bar |
| CN110021512A (en) * | 2019-04-04 | 2019-07-16 | 北京工业大学 | A kind of in-situ liquid environment transmission electron microscope electrothermics specimen holder system |
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2019
- 2019-09-25 CN CN201910912795.6A patent/CN110895252A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103000480A (en) * | 2012-11-29 | 2013-03-27 | 中国科学院物理研究所 | Transmission electron microscope sample rod capable of being added with optical fibers |
| CN207743192U (en) * | 2018-01-08 | 2018-08-17 | 中国科学院金属研究所 | A kind of transmission electron microscope electricity sample lever system in situ |
| CN207993796U (en) * | 2018-01-22 | 2018-10-19 | 关一 | A kind of transmission electron microscope specimen holder in situ |
| CN109490344A (en) * | 2018-08-21 | 2019-03-19 | 厦门芯极科技有限公司 | A kind of example of transmission electron microscope bar |
| CN110021512A (en) * | 2019-04-04 | 2019-07-16 | 北京工业大学 | A kind of in-situ liquid environment transmission electron microscope electrothermics specimen holder system |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116609362A (en) * | 2023-04-28 | 2023-08-18 | 云南大学 | Transmission electron microscope in-situ sample rod for researching magnetic property of nano material and control method |
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