CN207743192U - A kind of transmission electron microscope electricity sample lever system in situ - Google Patents
A kind of transmission electron microscope electricity sample lever system in situ Download PDFInfo
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- CN207743192U CN207743192U CN201820024768.6U CN201820024768U CN207743192U CN 207743192 U CN207743192 U CN 207743192U CN 201820024768 U CN201820024768 U CN 201820024768U CN 207743192 U CN207743192 U CN 207743192U
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Abstract
The utility model is related to transmission electron microscope accessory and low-dimensional materials in situ measurement research field, specially a kind of transmission electron microscope electricity sample lever system in situ.The system includes：For conducting the high vacuum circle hermetic connector of electric signal, the hollow specimen holder frame of surface insulation, the conducting wire being placed in specimen holder frame, ceramic heating flake, thermistor, control temperature unit, heating chip etc..Thermistor and ceramic heat are integrated on minute sample platform, are connect with external circuit unit by conducting wire and round hermetic connector, heating temperature, the rate of heat addition and temperature stability for monitoring minute sample platform；Heating chip is placed on minute sample platform, can further be regulated and controled into trip temperature to sample microcell.The atomic scale of material macro property is measured and studied under the utility model is realized to the maximum extent in vacuum environment and heating, power-up condition of external field, is widely used in probing into various high-temperature phase-changes, electric property, thermoelectricity capability, chemical reaction etc..
Description
Technical field
The utility model is related to transmission electron microscope accessory and low-dimensional materials in situ measurement research fields, specially a kind of
Transmission electron microscope electricity sample lever system in situ.
Background technology
Ambient enviroment and more physics outfields couple structure change of the caused material in sub-nanometer or atomic scale
The root of its macroscopic properties, and can observe that material is micro- under environment and outer field action in sub-nanometer or atomic scale
Structure or chemical constituent develop the key for also just becoming cognition material property.Nano-scale structures under environment and outer field action and
The original position of characteristic, Real-time High Resolution characterization technique directly determine our cognitive abilities for material, are to realize tutorial message, energy
Design on material structure and the Key Common Technologies of association physicochemical property regulation and control in the various fields such as source, environment, biology, also directly certainly
It is surely no to continue to keep advantage of the China in nanosecond science and technology international competition.Thus, development nanoscale original position, real-time, dynamic
Characterizing method also just becomes the current nanosecond science and technology special project in China with the limiting resolution of detection technique and raising under outer field action
In one of important research content.
In situ TEM analytical technology can gaseous state, liquid, solid-state, plasma state environment and irradiation, power,
It is in situ, related in real time, between the composed structure and physicochemical properties of dynamic research material under the condition of external field such as heat, electricity
Property, this analysis and characterization technology are provided simultaneously with time scale and the high-resolution characteristic of space scale, can be from deep layer understanding material
Intrinsic attribute, promote the design and performance of material to optimize, greatly improve the efficiency of research and development of new material, be current nanostructure table
Most novel and most development space research field during sign is learned.Its main problem is that R＆D institution of China is made for a long time
Advanced analysis characterization instrument depends critically upon American-European-Japanese Deng developed countries, this kind of high-end analysis of transmission electron microscope system
Equipment almost all is originated from import.As most potential micro- characterization technique, simulated environment transmission electron microscope analysis in situ
Characterization technique develops extremely rapid in developed country.In recent years, transmission electron microscope analysis characterization equipment aspect has in situ in China
Developed, but lag significantly behind world technology power, there are still larger gaps for the relevant technologies equipment.As China is to section
The increasing step by step of work supporting dynamics is ground, the R＆D institution and enterprise of domestic nearly all equipment transmission electron microscope have using in situ
The demand of transmission electron microscope sample lever system.However, designing and producing simulated environment in situ and multi- scenarios method function sample lever system
Technical difficulty is big, and key technology and core patent all rest in offshore company's hand so that the original position of domestic goods is imitative at present
True environmental sample lever system is all by offshore company's import, and price is very expensive, almost accounts for transmission electron microscope price
Half is serious to hinder in situ TEM characterization technique promoting the use of in China.More distinct issues are China's imports
The use function of sample lever system in situ is restricted, and no response type is customized, it is difficult to be changed according to the demand of scientific research mission.And
And can only import to emulation vacuum environment and the sample lever system in situ with simple heat, electric outfield function, this far can not expire
Foot research work requirement complicated and changeable greatly restricts the development in China transmission electron microscope characterization technique field in situ, not only
Research work content is limited, it is often more important that loses the ability for carrying out original Journal of Sex Research and technological accumulation, possesses original section
It is the antecedent basis for obtaining original scientific achievement and the most powerful guarantee to grind equipment.Due to technology restriction, at present both at home and abroad
The ripe commercial used in transmission electron microscope sample lever system that can realize In Situ Heating and power-up function simultaneously is there is no, and has sample in situ
The heating function of product bar exists accurate to high temp samples constituent analysis (Energy Dispersive Spectroscopy, EDS)
The disadvantages such as property is poor, and anti-interference ability is low, based on this demand and applicant working foundation sturdy in this field for many years, this reality
It is realized to the maximum extent in vacuum environment and under heating, power-up condition of external field to the atomic scale of material macro property with novel
It measures and studies, be widely used in probing into various high-temperature phase-changes, electric property, thermoelectricity capability, chemical reaction etc..
Utility model content
In view of the problems of the existing technology, it is in situ to be to provide a kind of transmission electron microscope for the purpose of this utility model
Electricity sample lever system, can be realized in transmission electron microscope in vacuum environment and heating, bias condition of external field under to material
The Macroscopic physical of material, the atomic scale of chemical property measure and research.
The technical solution of the utility model is：
A kind of transmission electron microscope electricity sample lever system in situ, the system include successively hollow specimen holder frame,
It conducts the high vacuum circle hermetic connector of electric signal, ceramic heating flake, thermistor, external circuit unit, be placed in hollow sample
Plain conductor, minute sample platform, heating chip in product bar frame, concrete structure are as follows：
Specimen holder frame is hollow structure, and surface deposits insulating coating, avoids plain conductor therein and specimen holder frame
Frame short circuit generates security risk, and the end of specimen holder frame is connected with the high vacuum circle hermetic connector of conduction electric signal, leads to
The high vacuum circle hermetic connector of conduction electric signal is crossed, specimen holder lower portion high vacuum and atmosphere outside are completely cut off, is passed
The high vacuum circle hermetic connector of electrically conductive signal connects the ceramic heating flake of specimen holder system front end, temperature-sensitive by plain conductor
Resistance, heating chip and external circuit unit；
Ceramic heating flake and thermistor are integrated on minute sample platform, pass through the Gao Zhen of plain conductor and conduction electric signal
Empty circle hermetic connector is connected with external circuit unit, for monitoring heating temperature and the rate of heat addition to minute sample platform.
Transmission electron microscope electricity sample lever system in situ, minute sample platform is metal material, surface
Deposition has 80~120 μ m-thick Al2O3Insulating layer avoids heating chip and sample from generating security risk with minute sample platform short circuit.
Transmission electron microscope electricity sample lever system in situ, heating chip are placed in minute sample platform,
Regulate and control for micro-area temperature, while carrying various solid samples, heating chip is by the transparent aluminium oxide of transmission electron beam, oxidation
Silicon, silicon nitride or silicon carbide window composition, with good chemically and physically stability.
Transmission electron microscope electricity sample lever system in situ, the heating electrode deposition of heating core on piece is in window
On mouth, heating electrode uses Cr/Au/Al2O3、Ti/Au/Al2O3、Cr/Pt/Al2O3、Ti/Pt/Al2O3、Cr/Cu/Al2O3 Ti/
Cu/Al2O3、Cr/Ag/Al2O3Or Ti/Ag/Al2O3, heat the Al of electrode top layer2O3For high heat conductive insulating inert material, sample is avoided
Product are reacted with window material.
Transmission electron microscope electricity sample lever system in situ, heating electrode use four electrode structures, two-way
Electrode is used for thermometric, and two path electrodes are for heating, and heating wires are surrounded on window surrounding, it is ensured that sample homogeneous heating.
Transmission electron microscope electricity sample lever system in situ, heating core on piece deposits simultaneously bias plasma
Pole, bias electrode use four electrode structures, two path electrodes to be used for turn-on current, and two path electrodes are dropped for monitoring voltage.
The transmission electron microscope is deposited on electricity sample lever system in situ, bias electrode on window, bias plasma
Pole uses refractory metal material：Cr/Au, Ti/Au, Cr/Pt, Ti/Pt, Cr/Cu Ti/Cu, Cr/Ag or Ti/Ag.
Transmission electron microscope electricity sample lever system in situ, which can be in the high vacuum of transmission electron microscope
Realize that the atomic scale in the case where heating and powering up condition of external field to material macro property measures and research, minute sample Tai Jiarewen
Spend range：For room temperature to 200 DEG C, chip maximum heating rate >=500 DEG C/sec are heated in maximum heating rate >=10 DEG C/sec, maximum
Cooling rate >=500 DEG C/sec, heating temperature range：Room temperature is to 1000 DEG C, temperature stability≤± 0.1 DEG C, be biased≤±
30V, electric current≤1A.
The advantages of the utility model and advantageous effect are：
1, the utility model includes mainly：For conducting the high vacuum circle hermetic connector of electric signal, surface insulation
Hollow specimen holder frame, the conducting wire being placed in specimen holder frame, ceramic heating flake, thermistor, control temperature unit, heating chip
Deng thermistor and ceramic heat are integrated on minute sample platform, pass through conducting wire and round hermetic connector and external circuit list
Member connection, heating temperature, the rate of heat addition and temperature stability for monitoring minute sample platform, heating chip are placed in minute sample
On platform, further sample microcell can be regulated and controled into trip temperature.
2, it is based on above-mentioned sample rod structure in situ, which can realize in the high vacuum of transmission electron microscope is heating and powering up
The atomic scale of material macro property is measured and is studied, minute sample platform heating temperature range under condition of external field：Room temperature is to 200
DEG C, maximum heating rate >=10 DEG C/sec, heating chip maximum heating rate >=500 DEG C/sec, maximum cooling rate >=500 DEG C/
Second, heating temperature range：For room temperature to 1000 DEG C, temperature stability≤± 0.1 DEG C is biased≤± 30V, electric current≤1A.
3, the utility model ceramic heating flake and thermistor, which are used in conjunction, is integrated on minute sample platform, can be precisely controlled macroscopic view
The temperature of sample under scale.
4, the heating chip on the utility model minute sample platform can accurately monitor sample micro-area temperature, maximum limit in real time
Realize the temp regulating function to sample in degree ground.
5, the utility model bias function uses four electrode structures, can accurately measure the electricity letter of sample under different temperatures
Number, it is not influenced by contact resistance, strong antijamming capability.
6, the effective microcell heating surface (area) (HS of the utility model is small and concentrates, and caused infra-red radiation is for transmission electron microscope EDS
The back end noise jamming of analysis influences small, it can be achieved that 650 DEG C or more the accurate ingredients for analyzing sample.
Description of the drawings
Fig. 1 used in transmission electron microscope original position electricity specimen holder system effect figure.
Fig. 2 specimen holders front end minute sample platform assembling stereogram.
The minute sample platform stereoscopic schematic diagram that Fig. 3 assembly is completed.
Fig. 4 has the heating chip structure schematic diagram of bias function.
The reference numerals are as follows：
1 --- specimen holder frame；2 --- the high vacuum circle hermetic connector of conduction electric signal；3 --- ceramic heat
Piece；4 --- thermistor；5 --- plain conductor；6 --- minute sample platform；7 --- heating chip；8 --- window；9——
Heat electrode；10 --- bias electrode.
Specific implementation mode
The specific implementation mode of utility model is described in further detail with reference to the accompanying drawings and examples.For this
The detailed description of a little embodiments, it is understood that those skilled in the art can be put into practice by the utility model, and can be with
By using other embodiments, in the case where not departing from the spirit and the utility model scope of the appended claims, to institute
Show that example is modified and/or changes.Although in addition, in embodiment announce the utility model special characteristic, it is this
Special characteristic can be suitably modified, and realize the function of the utility model.
As shown in Figures 1 to 4, the utility model transmission electron microscope electricity sample lever system in situ includes mainly：
Hollow specimen holder frame 1, the high vacuum circle hermetic connector 2 for conducting electric signal, ceramic heating flake 3, thermistor 4, outside
The parts such as circuit unit, the plain conductor 5 being placed in hollow specimen holder frame, minute sample platform 6, heating chip 7, concrete structure
It is as follows：
Specimen holder frame 1 is hollow structure, and surface deposits insulating coating, avoids plain conductor 5 and specimen holder therein
1 short circuit of frame generates security risk, 2 phase of high vacuum circle hermetic connector of the end and conduction electric signal of specimen holder frame 1
Even, the high vacuum circle hermetic connector 2 for conducting electric signal completely cuts off 1 inside high vacuum of specimen holder frame and atmosphere outside,
The high vacuum circle hermetic connector 2 for conducting electric signal connects specimen holder system front end ceramic heating flake by plain conductor 5 again
3, thermistor 4, heating chip 7 and external circuit unit, the effect of external circuit unit be：Monitor ceramic heating flake, heating
Chip temperature and bias electrode and size of current.
As shown in Fig. 2-Fig. 3, ceramic heating flake 3 and thermistor 4 are installed on minute sample platform 6, pass through plain conductor 5
It is connected with external circuit unit with the high vacuum circle hermetic connector 2 of conduction electric signal, for monitoring to minute sample platform
Heating temperature and the rate of heat addition.Minute sample platform 6 be metal (such as：Copper-tungsten alloy etc.) material, surface, which deposits, 100 μ m-thicks
Al2O3Insulating layer avoids heating chip and sample from generating security risk with 6 short circuit of minute sample platform.
As shown in figure 4, heating chip 7 is placed in minute sample platform 6, regulate and control for micro-area temperature, while carrying various
Solid sample, it is had good by being formed to the transparent aluminium oxide of electron beam, silica, silicon nitride or silicon carbide window 8
Chemically and physically stability.Heating electrode 9 on heating chip 7 is deposited on window 8, and heating electrode 9 uses Cr/Au/
Al2O3、Ti/Au/Al2O3、Cr/Pt/Al2O3、Ti/Pt/Al2O3、Cr/Cu/Al2O3、Ti/Cu/Al2O3、Cr/Ag/Al2O3Or Ti/
Ag/Al2O3, it is located at the Al of top layer2O3For high heat conductive insulating inert material, it can avoid sample and reacted with window material.Heat electrode
9 use four electrode structures, two path electrodes to be used for thermometric, and two path electrodes are for heating, and heating wires are surrounded on 8 surrounding of window, really
Protect sample homogeneous heating.Deposition has bias electrode 10 simultaneously on heating chip 7, equally uses four electrode structures, two path electrodes
For turn-on current, two path electrodes are dropped for monitoring voltage.Bias electrode 10 is deposited on window 8, using refractory metal material
Material, such as：Cr/Au, Ti/Au, Cr/Pt, Ti/Pt, Cr/Cu Ti/Cu, Cr/Ag or Ti/Ag etc..
Embodiment the result shows that, the utility model is realized to the maximum extent in vacuum environment and heating, power-up outfield item
The atomic scale of material macro property is measured and studied under part, is widely used in probing into various high-temperature phase-changes, electric property, heat
Electrical property, chemical reaction etc..
The embodiments of the present invention are described above in conjunction with attached drawing, but the utility model be not limited to it is above-mentioned
Specific implementation mode, above-mentioned specific embodiment is only illustrative, rather than restrictive, the ordinary skill people of this field
Member is not departing from the utility model aims and scope of the claimed protection under the enlightenment of the utility model, also
Many forms can be made, these belong within the protection of the utility model.
Claims (7)
1. a kind of transmission electron microscope electricity sample lever system in situ, it is characterised in that：The system includes hollow sample successively
Product bar frame (1) conducts the high vacuum circle hermetic connector (2) of electric signal, is ceramic heating flake (3), thermistor (4), outer
Portion's circuit unit, the plain conductor (5) being placed in hollow specimen holder frame, minute sample platform (6), heating chip (7), it is specific to tie
Structure is as follows：
Specimen holder frame (1) is hollow structure, and surface deposits insulating coating, avoids plain conductor therein (5) and specimen holder
Frame (1) short circuit generates security risk, the high vacuum circle hermetic connector of the end and conduction electric signal of specimen holder frame (1)
(2) be connected, by conducting the high vacuum circle hermetic connector (2) of electric signal, the internal high vacuum of isolation specimen holder frame (1) with
Atmosphere outside, the high vacuum circle hermetic connector (2) for conducting electric signal connect sample lever system by plain conductor (5)
Ceramic heating flake (3), thermistor (4), heating chip (7) and the external circuit unit of front end；
Ceramic heating flake (3) and thermistor (4) are integrated on minute sample platform (6), pass through plain conductor (5) and conduction telecommunications
Number high vacuum circle hermetic connector (2) be connected with external circuit unit, for monitoring heating temperature to minute sample platform
And the rate of heat addition.
2. transmission electron microscope described in accordance with the claim 1 electricity sample lever system in situ, it is characterised in that：Miniature sample
Sample platform (6) is metal material, and surface deposition has 80~120 μ m-thick Al2O3Insulating layer, avoid heating chip and sample with it is miniature
Sample stage (6) short circuit generates security risk.
3. transmission electron microscope described in accordance with the claim 1 electricity sample lever system in situ, it is characterised in that：Heating core
Piece (7) is placed in minute sample platform (6), is regulated and controled for micro-area temperature, while carrying various solid samples, heating chip (7)
By being formed to the transparent aluminium oxide window of transmission electron beam, silica window, silicon nitride window or silicon carbide window.
4. according to the electricity sample lever system in situ of the transmission electron microscope described in claim 1 or 3, it is characterised in that：Add
Heating electrode (9) on hot chip (7) is deposited on window (8).
5. transmission electron microscope electricity sample lever system in situ according to claim 4, it is characterised in that：Heating electricity
Pole (9) uses four electrode structures, two path electrodes to be used for thermometric, and for two path electrodes for heating, heating wires are surrounded on window (8) four
Week, it is ensured that sample homogeneous heating.
6. transmission electron microscope electricity sample lever system in situ according to claim 4, it is characterised in that：Heating core
Deposition has bias electrode (10), bias electrode (10) to use four electrode structures simultaneously on piece (7), and two path electrodes are for connecting electricity
Stream, two path electrodes are dropped for monitoring voltage.
7. transmission electron microscope electricity sample lever system in situ according to claim 6, it is characterised in that：Bias plasma
Pole (10) is deposited on window (8).
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| CN201820024768.6U CN207743192U (en) | 2018-01-08 | 2018-01-08 | A kind of transmission electron microscope electricity sample lever system in situ |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201820024768.6U CN207743192U (en) | 2018-01-08 | 2018-01-08 | A kind of transmission electron microscope electricity sample lever system in situ |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108198740A (en) * | 2018-01-08 | 2018-06-22 | 中国科学院金属研究所 | A kind of transmission electron microscope electricity sample lever system in situ |
| CN110161063A (en) * | 2019-05-31 | 2019-08-23 | 南京大学 | A kind of scanning transmission electron beam-induced amperometry system and method |
| CN110895252A (en) * | 2019-09-25 | 2020-03-20 | 北京工业大学 | Optical sample rod system for in-situ liquid-gas environment transmission electron microscope |
| CN111856370A (en) * | 2020-06-12 | 2020-10-30 | 中国计量科学研究院 | Superconducting device test probe rod |
| CN113237755A (en) * | 2021-05-14 | 2021-08-10 | 东南大学 | Two-dimensional material in-situ mechanical parameter testing chip structure and preparation method |
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2018
- 2018-01-08 CN CN201820024768.6U patent/CN207743192U/en active Active
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108198740A (en) * | 2018-01-08 | 2018-06-22 | 中国科学院金属研究所 | A kind of transmission electron microscope electricity sample lever system in situ |
| CN110161063A (en) * | 2019-05-31 | 2019-08-23 | 南京大学 | A kind of scanning transmission electron beam-induced amperometry system and method |
| CN110161063B (en) * | 2019-05-31 | 2020-06-30 | 南京大学 | Scanning transmission electron beam induced current analysis system and method |
| CN110895252A (en) * | 2019-09-25 | 2020-03-20 | 北京工业大学 | Optical sample rod system for in-situ liquid-gas environment transmission electron microscope |
| CN111856370A (en) * | 2020-06-12 | 2020-10-30 | 中国计量科学研究院 | Superconducting device test probe rod |
| CN111856370B (en) * | 2020-06-12 | 2023-10-31 | 中国计量科学研究院 | Superconducting device test probe rod |
| CN113237755A (en) * | 2021-05-14 | 2021-08-10 | 东南大学 | Two-dimensional material in-situ mechanical parameter testing chip structure and preparation method |
| CN113237755B (en) * | 2021-05-14 | 2022-03-25 | 东南大学 | Two-dimensional material in-situ mechanical parameter testing chip structure and preparation method |
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