CN109187595B - Device for measuring local equivalent pressure caused by micro gas beams in transmission electron microscope - Google Patents
Device for measuring local equivalent pressure caused by micro gas beams in transmission electron microscope Download PDFInfo
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- CN109187595B CN109187595B CN201811127484.0A CN201811127484A CN109187595B CN 109187595 B CN109187595 B CN 109187595B CN 201811127484 A CN201811127484 A CN 201811127484A CN 109187595 B CN109187595 B CN 109187595B
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- G—PHYSICS
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- 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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
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Abstract
The invention discloses a device for measuring local equivalent pressure caused by micro gas beams in a transmission electron microscope, particularly relates to the field of an Environmental Transmission Electron Microscope (ETEM), and aims to provide a device for the in-situ measurement of the equivalent pressure caused by the injection of the micro gas beams in a local space near a sample. The device is characterized in that the in-situ gas micro-beam spray head and the nanoindenter system are simultaneously and integrally installed on the environmental transmission electron microscope sample stage, and the in-situ gas micro-beam spray head and the nanoindenter system contain the nanometer-size in-situ force measuring probe. The nanoindenter force probe may be in the micro-gas beam injection region. The nanoindenter force measurement probe moves three-dimensionally and accurately in the area near the sample, and can accurately measure the tiny reaction force generated by gas injection. The invention has the characteristics of simplicity, convenience, rapidness and high accuracy.
Description
Technical Field
The invention relates to a device which is arranged in an Environmental Transmission Electron Microscope (ETEM) and is used for in-situ measurement of equivalent pressure caused by micro gas beam injection in a nano-size local space near an electron microscope sample, in particular to a device for measuring the local equivalent pressure caused by micro gas beams in a transmission electron microscope.
Background
The environmental transmission electron microscopy (ETEM, also called an atmospheric in-situ transmission electron microscope) technology refers to an in-situ electron microscope technology for observing and researching a gas-solid interface by introducing one or more atmospheres into an electron microscope sample chamber through an external micro pipeline and jetting the atmospheres in a high-vacuum environment of the sample chamber in a gas microbeam form. The gas entering the sample chamber is pumped out through a differential vacuum system arranged on the other side, so that the high vacuum environment of the electron microscope is not affected.
At present, no device for carrying out in-situ measurement on equivalent pressure caused by a micro gas beam in a local nano-size space near an electron microscope sample is reported in ETEM. In the present invention, a transmission electron microscope nano-indenter and an atmosphere in-situ sample stage are integrated, a nano-indenter force measuring probe capable of moving three-dimensionally and accurately is used for measuring a micro reaction force caused by micro-gas beam injection in a local space near a sample in an in-situ manner, and an equivalent pressure caused by the micro-gas beam injection in the nano-sized local space is further obtained through calculation. The equivalent pressure concept is based on the number of gas molecules per unit time through unit cross-sectional area of the local space: the gas in the electron mirror is in a non-equilibrium state, and if the physical quantity caused by the gas micro-beam locally is equivalent to another equilibrium state gas, the two gases are considered to have the same equivalent pressure.
However, the existing environmental transmission electron microscope has been developed so far, and the vacuum probe is installed at a fixed position in the electron microscope to detect the pressure, so that only the average pressure at a certain fixed position (far from the sample) can be tested, which is not enough to know the specific condition of the sample surface (air-solid interface) in the atmosphere in-situ experiment. There are few devices that can accurately measure in situ the equivalent pressure caused by the ejection of a micro-gas beam in a local space near a sample.
Disclosure of Invention
The invention provides a device which is arranged in an environmental transmission electron microscope and can measure the equivalent pressure caused by the ejection of a micro gas beam in a local space near a sample in situ.
The device for measuring the equivalent pressure in the nano-scale local space near the sample caused by the micro-gas beam injection, which is arranged in the environmental transmission electron microscope, can realize the function of in-situ measuring the equivalent pressure in a plurality of nano-scale local spaces near the sample in the environmental transmission electron microscope, wherein the equivalent pressure is one of the most important parameters of the environmental transmission electron microscope experiment; the device mainly comprises the in-situ micro gas beam spray head integrated on the environmental transmission electron microscope sample stage and the nano indenter system also integrated on the environmental transmission electron microscope sample stage; the force measuring probe of the nanoindenter system can move accurately in three dimensions in the area where the micro gas beams are sprayed, the accuracy is 100 picometers-level accuracy, and the equivalent pressure generated by the micro gas beams in the nano-size local space is obtained by accurately measuring the micro reaction force generated by the gas spraying, wherein the accuracy is 100 picometers-level accuracy.
Further, the equivalent pressure concept is based on the number of gas molecules per unit time through unit cross-sectional area of the local space.
Further, the inside of the electron mirror is in a non-equilibrium state, and if the physical quantity locally generated by the gas micro-beam is equivalent to another equilibrium state gas, the two are considered to have the same equivalent pressure. In the experiment, the average pressure inside and outside the electron microscope of the gas microbeam jet, the gas type (molecular weight) and the sectional area of the nano-indenter force measuring probe are known, and the reaction force is obtained through measurement, so that the number of gas molecules reaching the unit sectional area in unit time in the local space where the nano-indenter force measuring probe is located can be calculated.
Furthermore, the nanoindenter force measurement probe can move out of the gas beam injection space after the test is finished, and subsequent atmosphere in-situ electron microscope experiments are not affected.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for measuring a local spatial equivalent pressure caused by micro-gas beam injection installed in an environmental transmission electron microscope.
Wherein, the reference numbers: 1. an in-situ micro gas beam showerhead; 2. a nanoindenter force measurement probe; 3. a gas area is formed; 4. the number of electrons; 5. a vacuum zone.
The invention is further illustrated with reference to the following figures and examples.
Terms used in the present invention have generally meanings as commonly understood by one of ordinary skill in the art, unless otherwise specified.
In the following examples, various procedures and methods not described in detail are conventional methods well known in the art.
Example an environmental transmission electron microscope (model Titan) manufactured by FEI corporation was usedTMThe ETEM platform is equipped with means to measure the local spatial equivalent pressure caused by the micro-gas beam injection. Using the Hysitron nano-scaleThe indentation instrument (2) is integrated with an atmosphere pipeline and an in-situ micro gas beam nozzle (1); the gas circuit pipeline is made of titanium alloy materials, the inner diameter of the gas circuit pipeline is 400 micrometers, the outer diameter of the gas circuit pipeline is 900 micrometers, the micrometer precision motor controls the pipeline to move, the in-situ micro gas beam spray head (1) is installed in the end head of the gas circuit pipeline, the inner diameter of the in-situ micro gas beam spray head (1) is 100 micrometers, the front inner diameter of the in-situ micro gas beam spray head is 50 micrometers, the outer diameter of the in-situ micro gas beam spray. The cross section of the force measuring probe (2) of the nano-indenter in the gas injection direction (3) is 200nm multiplied by 200nm after being processed by focused ion beams, the reaction force generated by in-situ O2 gas micro-beam injection is measured to be 2.5nN according to the average pressure of 2atm of O2 of a gas tank of the known ETEM and the vacuum degree of 10-5Pa in an electron microscope, and the equivalent pressure of the local (200nm multiplied by 200nm) of the environmental transmission electron microscope is obtained to be 0.07 atm.
It will be understood that the above embodiments are merely exemplary embodiments for illustrating the principles of the present invention, and the present invention is not limited thereto. It will be apparent to those skilled in the art that various modifications and improvements can be made without departing from the spirit and substance of the invention, and these modifications and improvements are also considered to be within the scope of the invention.
Claims (3)
1. A device for measuring local equivalent pressure caused by micro gas beams in a transmission electron microscope is characterized in that an in-situ micro gas beam spray head and a nano indenter system are simultaneously and integrally installed on an environmental transmission electron microscope sample stage, and the in-situ micro gas beam spray head and the nano indenter system comprise a nano indenter force measuring probe; the nanoindenter force measurement probe is positioned in the micro gas beam injection area; the nanoindenter force measurement probe moves in three dimensions in the area near the sample, and can measure the reaction force generated by gas injection;
when the gas micro-beam is sprayed, the internal and external average pressure intensity of an electron microscope, the gas type and the sectional area of the force measuring probe of the nanoindenter can be calculated and obtained through the measured reaction force;
the equivalent pressure concept is based on the number of gas molecules per unit time through unit cross-sectional area in local space.
2. The apparatus according to claim 1, wherein the electron microscope is in a non-equilibrium state, and the number of gas molecules passing through a unit cross-sectional area of the micro gas beam in a local space per unit time is equal to that of another gas in an equilibrium state, so that the micro gas beam and the gas in the other equilibrium state are considered to have the same equivalent pressure.
3. The device for measuring local equivalent pressure caused by micro gas beams in a transmission electron microscope according to claim 1, wherein the nanoindenter force measurement probe can move out of the gas beam injection space after completing force measurement without affecting subsequent atmosphere in-situ electron microscope experiments.
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| CN201811127484.0A CN109187595B (en) | 2018-09-27 | 2018-09-27 | Device for measuring local equivalent pressure caused by micro gas beams in transmission electron microscope |
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| CN201811127484.0A CN109187595B (en) | 2018-09-27 | 2018-09-27 | Device for measuring local equivalent pressure caused by micro gas beams in transmission electron microscope |
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| CN109187595A CN109187595A (en) | 2019-01-11 |
| CN109187595B true CN109187595B (en) | 2021-05-11 |
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| EP1304717A1 (en) * | 2000-07-27 | 2003-04-23 | Ebara Corporation | Sheet beam test apparatus |
| CN1511332A (en) * | 2000-12-01 | 2004-07-07 | Ү���о�����չ����˾ | Device and method ofr examination of samples in non-vacuum environment using scanning electron microscope |
| CN101067992A (en) * | 2006-04-26 | 2007-11-07 | 李炳寰 | Apparatus for operating gas and providing for observing under vacuum or low-voltage environment |
| CN103868776A (en) * | 2014-03-27 | 2014-06-18 | 西安交通大学 | Vacuum sample pre-reaction chamber of vacuum electron microscope |
| CN105223215A (en) * | 2015-11-16 | 2016-01-06 | 南京大学 | A kind of gas electronic diffraction instrument installed in environment transmission electron microscope |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4823006A (en) * | 1987-05-21 | 1989-04-18 | Electroscan Corporation | Integrated electron optical/differential pumping/imaging signal detection system for an environmental scanning electron microscope |
| US7903704B2 (en) * | 2006-06-23 | 2011-03-08 | Pranalytica, Inc. | Tunable quantum cascade lasers and photoacoustic detection of trace gases, TNT, TATP and precursors acetone and hydrogen peroxide |
| JP2013114854A (en) * | 2011-11-28 | 2013-06-10 | Hitachi High-Technologies Corp | Sample observation device and marking method |
| CN106680305B (en) * | 2016-11-23 | 2023-08-04 | 聚束科技（北京）有限公司 | Vacuum atmosphere treatment device, sample observation system and method |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1998034092A2 (en) * | 1997-01-21 | 1998-08-06 | Rave, L.L.C. | Object inspection and/or modification system and method |
| EP1304717A1 (en) * | 2000-07-27 | 2003-04-23 | Ebara Corporation | Sheet beam test apparatus |
| CN1511332A (en) * | 2000-12-01 | 2004-07-07 | Ү���о�����չ����˾ | Device and method ofr examination of samples in non-vacuum environment using scanning electron microscope |
| CN101067992A (en) * | 2006-04-26 | 2007-11-07 | 李炳寰 | Apparatus for operating gas and providing for observing under vacuum or low-voltage environment |
| CN103868776A (en) * | 2014-03-27 | 2014-06-18 | 西安交通大学 | Vacuum sample pre-reaction chamber of vacuum electron microscope |
| CN105223215A (en) * | 2015-11-16 | 2016-01-06 | 南京大学 | A kind of gas electronic diffraction instrument installed in environment transmission electron microscope |
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