CN109187595A - The device of local equivalents pressure caused by micro- gas beam in a kind of measurement transmission electron microscope - Google Patents
The device of local equivalents pressure caused by micro- gas beam in a kind of measurement transmission electron microscope Download PDFInfo
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- CN109187595A CN109187595A CN201811127484.0A CN201811127484A CN109187595A CN 109187595 A CN109187595 A CN 109187595A CN 201811127484 A CN201811127484 A CN 201811127484A CN 109187595 A CN109187595 A CN 109187595A
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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
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/03—Investigating materials by wave or particle radiation by transmission
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Abstract
The device of local equivalents pressure caused by micro- gas beam is specifically related to the field environment transmission electron microscope (ETEM) in a kind of measurement transmission electron microscope, the present invention near sample the micro- gas beam of local space spray caused by equivalent pressure in situ measurement the technical issues of the device that proposes.Described device is to utilize the environment transmission electron microscope sample table while integrated installation the gas microbeam spray head in situ and the nano-hardness tester system, and the original position gas microbeam spray head and the nano-hardness tester system contain nano-scale original position dynamometry probe.The nano-hardness tester dynamometry probe can be in micro- gas beam jeting area.The nano-hardness tester dynamometry probe is in sample near zone three-dimensional accurate movement, while the small reaction force that can be generated with precise measurement gas injection.The gas microbeam spray when Electronic Speculum inside and outside average pressure, gaseous species (molecular weight), nano-hardness tester dynamometry pop one's head in sectional area, by measuring obtained reaction force, the equivalent pressure for obtaining the locating nano-scale local space of the nano-hardness tester probe can be calculated, the present invention has the simple and efficient and high feature of accuracy.
Description
Technical field
The present invention relates to what is installed in a kind of environment transmission electron microscope (ETEM), in situ measurement in electron microscopic sample
The device of equivalent pressure caused by neighbouring nano-scale local space is sprayed due to micro- gas beam, and in particular to saturating to a kind of measurement
The device of local equivalents pressure caused by micro- gas beam in radio mirror.
Background technique
Environment transmission electron microscopy Electronic Speculum (ETEM, also referred to as atmosphere in situ TEM) technology, referring to will be a kind of or more
Kind atmosphere enters electron microscopic sample room by external micro-channel, and the high vacuum environment in the form of gas microbeam in sample room carries out
Injection, thus the electron microscopy in situ of observational study gas-solid interface.Gas into sample room will be by being mounted on the other side
Difference vacuum system is extracted, to guarantee that Electronic Speculum high vacuum environment is unaffected.
It is had not been reported in ETEM at present to micro- gas beam caused by local nano-scale space near electron microscopic sample
Equivalent pressure carries out the device of in situ measurement.Current ETEM is by fixed position internally provided with vacuum degree probes multiple in Electronic Speculum
(macro-size, far from sample), measures the average vacuum value of multiple positions in Electronic Speculum, reflects that micro- gas beam injection is drawn indirectly
The pressure (its caused vacuum situation of change) risen.In the present invention, we are in situ by transmission electron microscope nano-hardness tester and atmosphere
Sample stage is integrated, using can the nano-hardness tester dynamometry of three-dimensional accurate movement pop one's head in, the part near sample is empty
Between, small reaction force caused by the micro- gas beam of precise measurement in situ sprays further provides micro- gas beam injection by calculating
The equivalent pressure caused by the local space of nano-scale.Equivalent pressure concept is based on the local space unit time by single
Position sectional area gas molecule quantity: in Electronic Speculum gas be nonequilibrium state, if gas microbeam part caused by the physical quantity with
Another equilibrium state gas phase is worked as, then it is assumed that the two equivalent pressure having the same.
However, development is up to the present, existing environment transmission electron microscope, which is utilized in Electronic Speculum, fixes position installation vacuum
Probe carries out detection pressure, so that some average pressure for fixing position (farther out from sample) can only be tested, this is for venting one's spleen
The specific situation of sample surfaces (gas-solid interface) in the experiment of atmosphere original position is inadequate.Seldom existing can accurate in situ measurement
The device of equivalent pressure caused by local space minimum gas beam sprays near sample.
Summary of the invention
The present invention in view of the above technical problems, propose it is a kind of install in environment transmission electron microscope, Ke Yiyuan
The device of equivalent pressure caused by the micro- gas beam of position measurement local space near sample sprays.
In sample caused by the measurement micro- gas beam injection of the present invention installed in environment transmission electron microscope
The device of the equivalent pressure of neighbouring nano-scale local space, the function that can be realized are to measure in environment transmission electron microscope in situ
The equivalent pressure of multiple nanoscale local spaces near sample, the equivalent pressure are the most important of environment transmission electron microscope experiment
One of parameter.
Further, described device is mainly by the gas microbeam spray head in situ for being integrated in environment transmission electron microscope sample table
With the nano-hardness tester system composition for being equally integrated in environment transmission electron microscope sample table.
Further, the dynamometry probe of the nano-hardness tester system can be in the area three-dimensional of micro- gas beam injection
Accurate movement, the accuracy are 100 micromicron order of magnitude precision, the small reaction generated by the precise measurement gas injection
Power, the accuracy are 100 skin ox order of magnitude precision, are obtained described in being generated as micro- gas beam of the nano-scale local space
Equivalent pressure.
Further, the equivalent pressure concept is to pass through the gas of unit cross-sectional area based on the local space unit time
Molecular amounts.
It further, is nonequilibrium state in the Electronic Speculum, if gas microbeam is put down in the physical quantity locally generated with another
Weighing apparatus state gas phase is worked as, then it is assumed that the two equivalent pressure having the same.In experiment, it is known that in the Electronic Speculum of the injection of body microbeam described in gas
Outer average pressure, gaseous species (molecular weight), nano-hardness tester dynamometry probe sectional area, obtain reaction force by measurement, i.e.,
The gas molecule quantity of unit time arrival unit cross-sectional area in local space where obtaining nano-hardness tester probe can be calculated.
Further, the nano-hardness tester probe can move out the gas beam jet space after completing test,
Subsequent atmosphere original position electron microscope experiment is not influenced.
Detailed description of the invention
The equivalent pressure of local space caused by the micro- gas beam of measurement installed in Fig. 1 environment transmission electron microscope sprays
Apparatus structure schematic diagram.
Wherein, appended drawing reference: 1, micro- gas beam spray head；2, nano-hardness tester dynamometry is popped one's head in；3, there is gas zone；4, electronics
Number；5, vacuum area；
Specific embodiment
Present invention will be further explained below with reference to the attached drawings and examples.
Term as used in the present invention generally has those of ordinary skill in the art usual unless otherwise specified
The meaning of understanding.
Below in an example, the various processes and method being not described in detail are conventional methods as known in the art.
Case study on implementation utilizes environment transmission electron microscope (the model Titan of FEI Co.'s productionTMETEM) stage+module measures micro- gas
The device of the equivalent pressure of local space caused by body beam sprays.Using Hysitron nano-hardness tester (2) the integrated installation gas
Atmosphere pipeline and micro- gas beam spray head (1): the gas path pipe is titanium alloy material, 400 microns of internal diameter, 900 microns of outer diameter, described micro-
Meter Jing Du motor control pipeline is mobile, and micro- gas beam spray head (1) is mounted in the gas path pipe end, the gas beam
100 microns of internal diameter of spray head (1), 50 microns of preceding internal diameter, 200 microns of outer diameter, 1 millimeter of length.The nano-hardness tester dynamometry probe
(2) line focus ion beam processing is 200nm × 200nm in gas injection direction (3) sectional area, according to known ETEM's
Gas tank O2Average pressure 2atm, vacuum degree 10 in Electronic Speculum-5Pa surveys to obtain O in situ2The injection of gas microbeam generates reaction force
2.5nN has shown that the equivalent pressure of the environment transmission electron microscope part (200nm × 200nm) is 0.07atm.
It is understood that the principle that embodiment of above is intended to be merely illustrative of the present and illustrative embodiments,
However the present invention is not limited thereto.For those skilled in the art, do not depart from spirit of the invention and
In the case where essence, various changes and modifications can be made therein, these variations and modifications are also considered as protection scope of the present invention.
Claims (7)
1. the device of local equivalents pressure caused by micro- gas beam in a kind of measurement transmission electron microscope, which is characterized in that described device
It is to utilize the environment transmission electron microscope sample table while the integrated installation micro- gas beam spray head in the original position and the nano impress
Instrument system, the original position gas microbeam spray head and the nano-hardness tester system contain nano-scale original position dynamometry probe.
2. the device of local equivalents pressure caused by micro- gas beam in a kind of measurement transmission electron microscope according to claim 1,
It is characterized in that, the nano-hardness tester dynamometry probe can be in micro- gas beam jeting area.
3. the device of local equivalents pressure caused by micro- gas beam in a kind of measurement transmission electron microscope according to claim 2,
It is characterized in that, the nano-hardness tester dynamometry is popped one's head in sample near zone three-dimensional accurate movement, while can be with precise measurement
The small reaction force that gas injection generates.
4. the device of local equivalents pressure caused by micro- gas beam in a kind of measurement transmission electron microscope according to claim 1,
It is characterized in that, the gas microbeam spray when Electronic Speculum inside and outside average pressure, gaseous species (molecular weight), nano-hardness tester dynamometry
Sectional area of popping one's head in can calculate by measuring obtained reaction force and obtain the locating nano-scale of the nano-hardness tester probe
The equivalent pressure of local space.
5. the device of local equivalents pressure caused by micro- gas beam in a kind of measurement transmission electron microscope according to claim 1,
It is characterized in that, the equivalent pressure concept is to pass through the gas molecule of unit cross-sectional area based on the local space unit time
Quantity.
6. the device of local equivalents pressure caused by micro- gas beam in a kind of measurement transmission electron microscope according to claim 5,
It is characterized in that, being nonequilibrium state in the Electronic Speculum, if gas microbeam physical quantity caused by part and another equilibrium state gas
Body is suitable, then it is assumed that the two equivalent pressure having the same.
7. the device of local equivalents pressure caused by micro- gas beam in a kind of measurement transmission electron microscope according to claim 6,
It is characterized in that, the nano-hardness tester probe can move out the gas beam jet space after completing dynamometry, after not influencing
Continuous atmosphere original position electron microscope experiment.
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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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Citations (10)
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|---|---|---|---|---|
| CN1039324A (en) * | 1988-02-19 | 1990-01-31 | 电子扫描公司 | Electron optics/the differential pressure that is used for the whole series of environment (Environmental) scanning electron microscopy is bled/signal detection system |
| 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 |
| US20080159341A1 (en) * | 2006-06-23 | 2008-07-03 | Patel C Kumar N | Tunable quantum cascade lasers and photoacoustic detection of trace gases, TNT, TATP and precursors acetone and hydrogen peroxide |
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2018
- 2018-09-27 CN CN201811127484.0A patent/CN109187595B/en active Active
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| CN1039324A (en) * | 1988-02-19 | 1990-01-31 | 电子扫描公司 | Electron optics/the differential pressure that is used for the whole series of environment (Environmental) scanning electron microscopy is bled/signal detection system |
| 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 |
| US20080159341A1 (en) * | 2006-06-23 | 2008-07-03 | Patel C Kumar N | Tunable quantum cascade lasers and photoacoustic detection of trace gases, TNT, TATP and precursors acetone and hydrogen peroxide |
| US20130134308A1 (en) * | 2011-11-28 | 2013-05-30 | Hitachi High-Technologies Corporation | Sample observation apparatus and method of marking |
| 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 |
| CN106680305A (en) * | 2016-11-23 | 2017-05-17 | 聚束科技（北京）有限公司 | Vacuum atmosphere processing device as well as sample observing system and sample observing method |
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