CN207993796U - A kind of transmission electron microscope specimen holder in situ - Google Patents
A kind of transmission electron microscope specimen holder in situ Download PDFInfo
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- CN207993796U CN207993796U CN201820104077.7U CN201820104077U CN207993796U CN 207993796 U CN207993796 U CN 207993796U CN 201820104077 U CN201820104077 U CN 201820104077U CN 207993796 U CN207993796 U CN 207993796U
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- test chamber
- sealing test
- specimen holder
- situ
- electron microscope
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Abstract
The utility model is related to material analysis technical field of measurement and test more particularly to transmission electron microscope accessory and low-dimensional materials in situ measurement research fields.The utility model solves the technical issues of transmission electron microscope can not achieve low-temperature space accurate temperature controlling with specimen holder in situ, a kind of transmission electron microscope specimen holder in situ is provided, the specimen holder includes sample club body, sealing test chamber, passive type refrigerator, active refrigeration device, thermal detector and thermostat, sealing test chamber is set in front of sample club body, passive type refrigerator carries out passive type refrigeration to sealing test chamber, active refrigeration device carries out active refrigeration to sealing test chamber, thermal detector detects sealing test chamber indoor temperature, thermostat controls active refrigeration device according to the measured value of thermal detector and carries out active refrigeration.Freezed using passive type refrigerator as level-one, active refrigeration device freezes as two level, and specimen holder is made to may be implemented in low-temperature space accurate temperature controlling.
Description
Technical field
The utility model is related to material analysis technical field of measurement and test more particularly to transmission electron microscope accessories and low-dimensional material
Expect in situ measurement research field.
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
The differentiation of structure or chemical constituent also just becomes the key of cognition material property.Nano-scale structures under environment and outer field action
Our cognitive abilities for material are directly determined with the original position of characteristic, Real-time High Resolution characterization technique, are to realize guidance letter
Design on material structure and the Key Common Technologies of association physicochemical property regulation and control in the various fields such as breath, the energy, environment, biology,
Can directly determine continue to keep advantage of the China in nanosecond science and technology international competition.Thus, development nanoscale is in situ, real
When, dynamic characterization method and detection technique and the limiting resolution that improves under outer field action also just become current nanometer section of China
One of important research content in skill special project.
In situ TEM analytical technology can gaseous state, liquid, solid-state, plasma state environment and irradiation, power,
It is in situ, simultaneously and dynamically related between the composed structure to physicochemical properties of 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.In recent years, in situ TEM characterization technique is disclosing
Lithium ion battery anode material discharge and recharge reaction principle, low-dimension nano material mechanical property, electrochemical corrosion mechanism, electroluminescent resistive
Numerous scientific research fields such as effect mechanism, nanocatalyst activity, biological cell structure all achieve with initiative research at
Fruit.While researcher can be used transmission electron microscopy observation nano material that complicated physics, chemical reaction occurs, supervise in real time
Ingredient, crystal structure, the differentiation of tissue defects, surface/interface chemical reaction etc. are surveyed, to realize in nanoscale in situ study
Military service behavior of the material in complex environment, discloses the essential mechanism of material failure, promotes the micro- knot of better designing material
Structure and performance.
Current main problem be R＆D institution of China for a long time used in advanced analysis characterization instrument seriously according to
The American-European-Japanese equal developed countries of Lai Yu, this kind of high-end analytical equipment almost all of transmission electron microscope system are originated from import.As
Most potential micro- characterization technique, simulated environment tem study characterization technique in situ are sent out in developed country
It opens up extremely rapid.In recent years, tem study characterization equipment aspect is developed in situ in China, but is obviously fallen
It makes the country prosperous afterwards in world technology, there are still larger gaps for the relevant technologies equipment.As China is to research work supporting dynamics
Increasing step by step, the R＆D institution and enterprise of domestic nearly all equipment transmission electron microscope have using transmitted electron in situ
The demand of microscope example lever system.However, designing and producing the skill of simulated environment in situ and multi- scenarios method function sample lever system
Art difficulty is big, and key technology and core patent all rest in offshore company's hand so that the emulation in situ of domestic goods at present
Environmental sample bar is all by offshore company's import, and price is very expensive, has almost accounted for the half of transmission electron microscope price,
Seriously hinder in situ TEM characterization technique promoting the use of in China.
More distinct issues are that the use function of the specimen holder in situ of China's import is restricted, and no response type is customized,
It is difficult to be changed according to the demand of scientific research mission.And can only import to emulation vacuum environment and with simple heat, electric outfield work(
The air-liquid state specimen holder in situ of energy does not have heating and accurate temperature controlling function, this far can not meet research work complicated and changeable
It is required, the development in China transmission electron microscope characterization technique field in situ is greatlyed restrict, not only in research work
Hold limit, it is often more important that lose the ability for carrying out original Journal of Sex Research and technological accumulation.Possessing original research equipment is
Obtain the antecedent basis of original scientific achievement and the most powerful guarantee.
In addition, cryogenic freezing technology is widely used in the scientific domains such as physics, chemistry, biology, material, external import it is saturating
The electron microscope specimen holder used under all vacuum environments of cryogenic freezing specimen holder is penetrated, and does not have accurate temperature controlling work(
Energy.Also, stabilization is deposited under the conditions of the transmission electron microscope cryogenic freezing specimen holder of external import can only observe cryogenic vacuum
Solid sample, application range is extremely limited.Due to technology restriction, there is no at present commercial in-situ low-temperature freezing research liquid,
The sample lever system of gaseous sample, and this is only the more universal existence form of research object.
Utility model content
(1) technical problems to be solved
First purpose of the utility model be：It solves transmission electron microscope and can not achieve low-temperature space with specimen holder in situ
The technical issues of accurate temperature controlling；
Second purpose of the utility model be：It solves transmission electron microscope and can not achieve full warm area with specimen holder in situ
The technical issues of accurate temperature controlling；
The third purpose of the utility model is：Transmission electron microscope is solved at least to be surveyed in low-temperature space with specimen holder in situ
The technical issues of solid sample being only used for when examination and not being suitable for gas, fluid sample.
(2) technical solution
In order to achieve the above object, the main technical schemes of the utility model use include：
The utility model provides a kind of transmission electron microscope specimen holder in situ, including：Sample club body；Set on sample
Sealing test chamber in front of club body；The passive type refrigerator of passive type refrigeration is carried out to sealing test chamber；Sealing is surveyed
Try the active refrigeration device that chamber carries out active refrigeration；Detect the thermal detector of sealing test chamber indoor temperature；And with actively
The thermostat that formula refrigerator is connected with thermal detector.
According to the utility model, passive type refrigerator includes low-temperature receiver and heat-conducting piece, heat-conducting piece and low-temperature receiver and sealing test chamber
Room connects, to form passive heat transfer between；Active refrigeration device includes thermoelectric cooling part, thermoelectric cooling part with lead
Warmware is connected with sealing test chamber, to take out heat from sealing test chamber to heat-conducting piece.
According to the utility model, further include：Load-bearing part for carrying sample, load-bearing part are set in sealing test chamber；
The primary heater of heat transfer is formed with the cavity wall of sealing test chamber；And microcell is carried out to the working region in load-bearing part and is added
The secondary heater of heat；Primary heater and secondary heater are connect with thermostat.
According to the utility model, primary heater includes the ceramic heating flake being fixed in the cavity wall of sealing test chamber；
Secondary heater includes fixed heating electrode on the load bearing member；Thermal detector include fixed thermometric electrode on the load bearing member and
The thermistor being fixed in the cavity wall of sealing test chamber, thermometric electrode are connect with thermostat with thermistor.
According to the utility model, the inside of sample club body has rod cavity, the airtight company in rear end of low-temperature receiver and sample club body
It connects, heat-conducting piece is arranged in rod cavity；Transmission electron microscope original position specimen holder further includes hermetic connector, hermetic connector with
The rear side of sample club body connects；Wherein, hermetic connector can carry out electrical conduction, thermoelectric cooling part, primary heater,
Secondary heater, thermometric electrode and thermistor are electrically connected by hermetic connector and the conducting wire and controller that are arranged in rod cavity
It connects；And/or in rod cavity and hermetic connector be equipped with fluid channel, fluid source by the fluid channel of rod cavity and hermetic connector with
Sealing test chamber in fluid communication.
According to the utility model, the external of low-temperature receiver coats low temperature resistant heat-insulating material；And/or low-temperature receiver passes through with sample club body
Conduction At Low Temperature airtight connecting piece connects, and the external of Conduction At Low Temperature airtight connecting piece coats low temperature resistant heat-insulating material.
According to the utility model, low-temperature receiver include for accommodate one in liquid nitrogen, liquid helium, solid acetonide and solid alcohol or
Multiple containers.
According to the utility model, further include：Load-bearing part for carrying sample, load-bearing part are set in sealing test chamber；
Load-bearing part includes two window substrates and multiple supporting members, and multiple supporting members supports are between two window substrates；Sealing test
Chamber is equipped with the through-hole that passes through of power supply beamlet, is equipped with window corresponding with through-hole on two window substrates, two windows it
Between folded region form working region.
According to the utility model, sealing test chamber includes the pedestal and cover board being removably joined together, pedestal and
It is respectively equipped with the through-hole that power supply beamlet passes through in cover board, is sealed by the first sealing ring between pedestal and cover board；Load-bearing part is located at
In the region that pedestal, cover board and the first sealing ring enclose, the second sealing ring, load-bearing part and bottom are folded between load-bearing part and cover board
It is folded with third sealing ring between seat；The first groove for placing the first sealing ring is formed on pedestal and/or cover board；Shape on cover board
At the second groove for having the second sealing ring of placement；The third groove for placing third sealing ring is formed on pedestal；Pedestal and/or lid
The 4th groove for placing load-bearing part is formed on plate.
According to the utility model, pedestal and cover board are made of Cu-W alloys；And/or the material of window substrate be aluminium oxide,
Silica, silicon nitride or silicon carbide；And/or transmission electron microscope specimen holder in situ further includes the chamber with sealing test chamber
Wall forms the primary heater of heat transfer and carries out the secondary heater of microcell heating, level-one to the working region in load-bearing part
Heater and secondary heater are connect with thermostat, and secondary heater is fixed multiple heating electrodes on the load bearing member, heating
Electrode deposition is Cr/Au/Al on window, heating the material of electrode2O3、Ti/Au/Al2O3、Cr/Pt/Al2O3、Ti/Pt/
Al2O3、Cr/Cu/Al2O3、Ti/Cu/Al2O3、Cr/Ag/Al2O3、Ti/Ag/Al2O3、Cr/SiC/Al2O3Or Ti/SiC/Al2O3。
(3) advantageous effect
The utility model has the beneficial effects that：
The transmission electron microscope of the utility model specimen holder in situ, passive type refrigerator freezes as level-one, to close
It seals test chamber and carries out passive type refrigeration, the temperature of sealing test chamber is substantially reduced to desired value, later, thermostat can
Active refrigeration device is controlled according to the measured value of thermal detector and carries out active refrigeration, actively adjusts the refrigerating capacity of active refrigeration device,
The temperature of sealing test chamber is accurately reduced to desired value.Freezed as a result, using active refrigeration device as two level, makes sample
Product bar may be implemented in low-temperature space accurate temperature controlling.
The transmission electron microscope of the utility model specimen holder in situ, is arranged primary heater and secondary heater, can
To carry out high-temperature region test, is tested in conjunction with above-mentioned low-temperature space, assemble a kind of specimen holder for full warm area.Also, by level-one
Heater first integrally heats the internal environment of sealing test chamber, then carries out microcell to working region by secondary heater
Heated for controlling temperature realizes the accurate temperature controlling in high-temperature region.Further combined with the accurate temperature controlling of above-mentioned low-temperature space, the utility model it is saturating
Penetrate the accurate temperature controlling that full warm area may be implemented with specimen holder in situ for electron microscope.
The transmission electron microscope of the utility model specimen holder in situ, fluid source can be gentle close by sample club body
Fluid channel in connector and sealing test chamber in fluid communication.The transmission electron microscope of the utility model is former as a result,
Position specimen holder can be used for the test of liquid, gas, solid sample, applied widely.
Description of the drawings
Fig. 1 is the stereochemical structure signal for the transmission electron microscope specimen holder in situ that following specific implementation mode provides
Figure；
Fig. 2 is the side structure schematic view of the front end of the transmission electron microscope specimen holder in situ in Fig. 1；
Fig. 3 is the configuration schematic diagram of the front end of the transmission electron microscope specimen holder in situ in Fig. 1；
Fig. 4 is the structural schematic diagram of the load-bearing part of the transmission electron microscope specimen holder in situ in Fig. 1.
【Reference numeral】
1：Sample club body；2：Sealing test chamber；3：Passive type refrigerator；4：Active refrigeration device；5：Low-temperature receiver；6：It leads
Warmware；7：Conduction At Low Temperature airtight connecting piece；8：High-thermal conductive metal connection sheet；9：Positioning pin；10：Primary heater；11：Two level adds
Hot device；12：Thermometric electrode；13：Thermistor；14：Hermetic connector；15：Window substrate；16：Supporting member；17：Window；18：
Metal lead wire；19：Pedestal；20：Cover board；21：Through-hole；22：First sealing ring；23：Second sealing ring；24：Third sealing ring；
25：First groove；26：Second groove；27：Third groove；28：4th groove；29：Bolt.
Specific implementation mode
It is below in conjunction with the accompanying drawings, right by specific implementation mode in order to understand in order to preferably explain the utility model
The utility model is described in detail.
Referring to Fig.1, the present embodiment provides a kind of transmission electron microscope original position specimen holders (following abbreviation specimen holder).It should
Specimen holder includes sample club body 1, sealing test chamber 2, passive type refrigerator 3, active refrigeration device 4, thermal detector and temperature control
Device.
Wherein, sample club body 1 is revolving body, and cross section is circle, its own is composed in series by multiple rod segments.In sample
The peripheral surface of club body 1 is equipped with positioning pin 9, so that specimen holder can pass through positioning pin after being inserted into transmission electron microscope
9 positioning rotate ± 30 ° in that can surround the central axes of its own.In multiple rod segments at least partly between rod segment can relative rotation company
It connects, it is preferable that the central axes that sample club body 1 can be surrounded between two rod segments rotate ± 30 °.
Wherein, sealing test chamber 2 is set to the front of sample club body, as the head of specimen holder, for placing test
Sample.
Wherein, passive type refrigerator 3 carries out passive type refrigeration to sealing test chamber 2.Passive type refrigeration refers to using not
The consumption energy or the mode for consuming few energy cause the local temperature difference to realize cooling mode.
Wherein, active refrigeration device 4 carries out active refrigeration to sealing test chamber 2.Active refrigeration refers to consume
Electric energy (or other energy) is the refrigeration of cost.
Wherein, temperature in thermal detector detection sealing test chamber 2, thermostat are connect with active refrigeration device 4 and thermal detector,
Thermostat can control active refrigeration device 4 according to the measured value of thermal detector and work.
As a result, in the present embodiment, passive type refrigerator 3 freezes as level-one, and passive type is carried out to sealing test chamber 2
Refrigeration, desired value is substantially reduced to by the temperature of sealing test chamber 2, and later, thermostat is controlled according to the measured value of thermal detector
Active refrigeration device 4 carries out active refrigeration, the refrigerating capacity of active refrigeration device 4 is actively adjusted, by the temperature of sealing test chamber 2
Accurately it is reduced to desired value.The two level of active refrigeration device 4 is utilized to freeze as a result, the specimen holder of the present embodiment may be implemented
In low-temperature space accurate temperature controlling, this is for studying and controlling cryochemistry synthetic reaction, material solid-gas-liquid phase height, low-temperature biological
Chemistry, lithium ion battery electrode material low temperature discharge and recharge reaction, antifreeze protein deactivation temperature point etc. have very important significance.
In the present embodiment, the lower 200 DEG C of temperature ranges to room temperature of low-temperature space nulling.Certainly, not limited to this, the lower limiting value of low-temperature space
It can be lower.
Further, in the present embodiment, passive type refrigerator 3 includes low-temperature receiver 5 and heat-conducting piece 6, heat-conducting piece 6 and low-temperature receiver 5 and
Sealing test chamber 2 connects, to form passive heat transfer between low-temperature receiver 5 and sealing test chamber 2, and then to sealing test
Chamber 2 freezes.Wherein, between heat-conducting piece 6 and low-temperature receiver 5 and sealing test chamber 2 can direct or indirect connection, and can be used can
The connection of dismounting.
Specifically, low-temperature receiver 5 includes container, container is for accommodating in liquid nitrogen, liquid helium, solid acetonide and solid alcohol
One or more containers.When using the container, liquid nitrogen, liquid helium, liquid acetone or liquid alcohol are added thereto.
Wherein, when the cooling medium of addition is liquid acetone or liquid alcohol, the directly cooling liquid acetone of liquid nitrogen, liquid helium is used
Or liquid alcohol obtains solid acetonide or solid alcohol, using solid acetonide or solid alcohol as the cooling medium finally used,
It so can effectively inhibit the boiling and small vibrations that liquid nitrogen, liquid helium generate in cooling procedure.The vibrations can pass through each heat conduction
Connector is transmitted in transmission electron microscope, the space high-resolution imaging of severe jamming sample to be analysed.The external cladding of low-temperature receiver 5 is resistance to low
Warm heat-insulating material plays the role of heat preservation and completely cuts off the water in air, prevents the 5 surface frosting of heat loss and low-temperature receiver.Wherein, this is resistance to
Cryo Heat Insulation material can at least bear subzero 200 DEG C, and low temperature resistant heat-insulating material is preferably glass fibre, alumina silicate foamed material
Deng.
Wherein, it should be appreciated that although the specimen holder of the present embodiment includes low-temperature receiver 5, be not limited to refrigeration source (such as liquid
Nitrogen, liquid helium, solid acetonide, solid alcohol) it is stored in specimen holder always, as long as system can be played using process in specimen holder
The device of cold-working is each fallen in the range of the low-temperature receiver 5 of the utility model.
Specifically, heat-conducting piece 6 is high heat conductivity metal bar, to accelerate the cooling rate of sealing test chamber, wherein high
The thermal conductivity of thermal conductivity metal bar is more than or equal to 400Wm-1K-1.In the present embodiment, heat-conducting piece 6 is copper bar.The one of heat-conducting piece 6
End is removably connect with the container of low-temperature receiver 5, and the two contacts to form heat transfer.Due to conduction copper bar and sealing test chamber phase
Even, for ease of " zero " position centering of through-hole and transmission electron microscope electron beam on sealing test chamber, and convenient for control with
Sample drifts about caused by tracking is expanded with heat and contract with cold due to conduction copper bar, sealing test chamber etc., axis and the specimen holder bar of the copper bar
The axis of body 1 is at least parallel, can also overlap.
Specifically, the inside of sample club body 1 has the rod cavity for being through to its rear end by its front end, the receiving of low-temperature receiver 5
Device and the rear end of sample club body 1 removably are connect by cylindrical Conduction At Low Temperature airtight connecting piece 7, as a result, low-temperature receiver 5 and
It is tightly connected between sample club body 1.Copper bar as heat-conducting piece 6 is arranged in Conduction At Low Temperature airtight connecting piece 7 and specimen holder bar
In the rod cavity of body 1.Conduction At Low Temperature airtight connecting piece 7 is used to completely cut off the internal environment and atmosphere outside of sample club body 1.It is low
The external of temperature conduction airtight connecting piece 7 coats low temperature resistant heat-insulating material, plays the role of heat preservation and completely cuts off the water in air, prevents
The 7 surface frosting of heat loss and Conduction At Low Temperature airtight connecting piece.Wherein, the low temperature that Conduction At Low Temperature airtight connecting piece 7 can carry out passes
Lead the refrigeration degree corresponding to low-temperature receiver；The low temperature resistant heat-insulating material of package Conduction At Low Temperature airtight connecting piece 7 can at least bear zero
Lower 200 DEG C, low temperature resistant heat-insulating material is preferably glass fibre, alumina silicate foamed material etc..
Specifically, active refrigeration device 4 includes thermoelectric cooling part, the separate container of thermoelectric cooling part and heat-conducting piece 6
One end connection and simultaneously connect with sealing test chamber 2, to take out heat from sealing test chamber 2 to heat-conducting piece 6.In the present embodiment
In, active refrigeration device 4 only includes thermoelectric cooling part (it is thermoelectric cooling part that can also be expressed as active refrigeration device 4), thermoelectricity system
Cold part is fixed in the cavity wall of sealing test chamber 2, and is connect with controller.Thermoelectric cooling part is thermoelectricity system in the present embodiment
Cold, thermoelectric module is the active refrigeration (" taking out heat ") using semiconductor electronic refrigerating principle, as long as thermostat control pair
Thermoelectric cooling part passes to direct current, will make a heating in heat-conducting piece 6 and sealing test chamber 2 connected to it, one
Turn cold, freeze flux >=6W/cm2, cooling rate can be accelerated and accurately controlled, so realize the accurate temperature controlling of low-temperature space.Certainly,
The utility model is not limited to this, and in the other embodiment of the present embodiment, active refrigeration device can be selected other and realize master
The device of dynamic refrigeration, as long as two level refrigeration can be used as to carry out accurate temperature controlling to low-temperature space.
Further, in the present embodiment, thermoelectric cooling part (i.e. active refrigeration device 4) passes through a high-thermal conductive metal connection sheet
8 connect with heat-conducting piece 6, and wherein the thermal conductivity of high-thermal conductive metal connection sheet 8 is more than or equal to 400W m-1K-1, preferably copper sheet,
The heat transfer that active refrigeration device 4 can be extracted out rapidly is to heat-conducting piece 6.And, it is preferable that high-thermal conductive metal connection sheet 8 is logical
It crosses bolt 29 removably to connect with thermoelectric cooling part and heat-conducting piece 6 respectively, in turn, makes sealing test chamber 2 and be fixed on
Device thereon is removably connect with the front end of sample club body 1.
To sum up, in the present embodiment, test temperature can reach subzero 200 DEG C.
Further, in the present embodiment, specimen holder further includes load-bearing part, primary heater 10 and secondary heater 11.
Specifically, load-bearing part is detachably arranged in sealing test chamber 2, for carrying sample.Have in load-bearing part
Working region, observation is positioned at sample segment in working region under transmission electron microscope.Primary heater 10 and sealing test
The cavity wall of chamber 2 forms heat transfer, is integrally heated with the internal environment to sealing test chamber 2.Secondary heater 11 is right
Working region in load-bearing part carries out microcell heating.Primary heater 10 and secondary heater 11 are connect with thermostat, thermostat
The work of primary heater 10 and secondary heater 11 can be controlled according to the measured value of thermal detector.
The specimen holder of the present embodiment can also carry out high-temperature region test as a result, tested in conjunction with above-mentioned low-temperature space, assemble one
The specimen holder of the full warm area of kind.Also, first the internal environment of sealing test chamber 2 is integrally heated by primary heater 10,
Microcell heated for controlling temperature is carried out to working region by secondary heater 11 again, realizes the accurate temperature controlling in high-temperature region.Further combined with
The accurate temperature controlling of full warm area may be implemented in the accurate temperature controlling of above-mentioned low-temperature space, the specimen holder of the present embodiment.This is for studying and controlling
Chemosynthesis reaction processed, material solid-gas-liquid phase height, biochemical reaction temperature, electrode material low-temperature oxidation reduction reaction,
Antifreeze protein deactivation temperature point etc. has very important significance.
Further, primary heater 10 includes the ceramic heating flake being fixed in the cavity wall of sealing test chamber 2, in this reality
It applies in example, primary heater 10 only includes above-mentioned ceramic heating flake (it is ceramic heating flake that can also be expressed as primary heater 10).
Secondary heater 11 includes fixed multiple heating electrodes on the load bearing member, and in the present embodiment, secondary heater 11 only includes
Above-mentioned multiple heating electrodes (it is multiple heating electrodes that can also be expressed as secondary heater 11).Thermal detector includes being fixed on load-bearing part
On thermometric electrode 12 and the thermistor 13 that is fixed in the cavity wall of sealing test chamber 2, thermometric electrode 12 is for measuring
The temperature of the working region of load-bearing part, thermistor 13 are used to measure the environment temperature inside sealing test chamber 2, thermometric electrode
12 and thermistor 13 connect with thermostat.In the present embodiment, test temperature can reach 200 DEG C above freezing.
To sum up, primary heater 10, thermistor 13 and active refrigeration device 4 are integrated in the cavity wall of sealing test chamber 2
On, secondary heater 11 and thermometric electrode 12 integrate and form chip on the load bearing member, and in sealing test chamber 2, by
This, it is appreciated that in addition to passive type refrigerator 3, primary heater 10, secondary heater 11, thermal detector (including thermistor 13
With thermometric electrode 12), active refrigeration device 4 and load-bearing part be integrated on sealing test chamber 2, sealing test chamber 2 as a result,
And above-mentioned integrated device thereon can form a sealing test chamber combination, whole and sample club body 1 and/or heat conduction
Part 6 is detachably connected, and in the present embodiment, sealing test chamber combination passes through 4 (i.e. thermoelectricity system of active refrigeration device therein
Cold part) it is removably connect with heat-conducting piece 6, to realize that sealing test chamber is detachably arranged at the front of sample club body 1.When
So, the utility model is not limited to this, in other embodiments, sealing test chamber also can directly with before sample club body 1
End part is fixed or is removably connected.
Also, primary heater 10, secondary heater 11, thermal detector (including thermistor 13 and thermometric electrode 12), master
Dynamic formula refrigerator 4 is connect with thermostat, cryogenic temperature, cooling rate, heating temperature and system for monitoring and adjusting specimen holder
Hot rate, also, temperature is accurately controlled using two-stage refrigeration, two-stage heating and the realization of two-stage thermometric.
Further, in the present embodiment, specimen holder further includes cylindrical hermetic connector 14, hermetic connector 14 and sample
The rear side of product club body 1 connects, and is hermetic connector 14 in the present embodiment perpendicular to sample club body 1, the air-tight connection
Device 14 can be used as operator and hold the handle of specimen holder, and completely cut off the internal environment and atmosphere outside of sample club body 1.
Wherein, there is conductive structure so that hermetic connector 14 can carry out electrical conduction in hermetic connector 14.It is arranged in
One end of conducting wire in the rod cavity of sample club body 1 is electrically connected with hermetic connector 14, the other end and active refrigeration device 4, one
Grade heater 10, secondary heater 11, thermal detector (including thermometric electrode 12 and thermistor 13) electrical connection, and be tightly connected
Device 14 is electrically connected with the controller.As a result, active refrigeration device 4, primary heater 10, secondary heater 11, thermal detector (including survey
Warm electrode 12 and thermistor 13) it is electrically connected with the controller by hermetic connector 14 and conducting wire, conduct electric signal.Wherein, exist
When sealing test chamber is detachably arranged at sample 1 front of club body, conducting wire can be made of multistage conducting wire and electric connection, to fit
It answers the dismounting of sealing test chamber, replace.
In addition, being additionally provided with fluid channel, the outlet of fluid source and gas in the rod cavity and hermetic connector 14 of sample club body 1
The entrance of the fluid channel of close connector 14 is connected to, in the outlet of the fluid channel of hermetic connector 14 and sample club body 1
The entrance of fluid channel is connected to, and the outlet of the fluid channel in sample club body 1 is connected to the inside of sealing test chamber, is carried
The working region of part is connected to the inside of sealing test chamber, in summary that is, the inside of fluid source and sealing test chamber is logical
The fluid channel crossed in fluid channel and rod cavity in hermetic connector 14 is in fluid communication with sealing test chamber 2.This reality as a result,
The specimen holder for applying example can be used for the test of liquid, gas, solid sample, applied widely.
Wherein, hermetic connector 14 is in addition to the effect for realizing above-mentioned electrical conduction and fluid transmission, be with external environment every
Exhausted.
Wherein, the fluid channel in sample club body 1 can be the circular passage of the inner wall and heat-conducting piece formation of its rod cavity,
It can also be the fluid circuit being individually threaded through in rod cavity, be in the present embodiment the latter.The stream of which kind of either above-mentioned form
Body channel, it is preferably to so that fluid channel is as much as possible is contacted with heat-conducting piece, to cool down in advance to fluid, anti-fluid stopping
Excessive influence is caused to temperature therein after body injection sealing test chamber 2.It may also be appreciated that entering sealing test chamber in fluid
Behind room 2, temperature therein will certainly be influenced, thus be arranged can actively, the thermoelectric cooler of fast cooling is to sealing test chamber
The temperature control of room 2 has great benefit.
And fluid circuit can be also equipped in hermetic connector 14 as fluid channel, and the fluid in hermetic connector 14
Pipeline connect to form a fluid circuit with the fluid circuit in sample club body 1, and one end and the fluid source of the fluid circuit connect
It connects, the other end is connect with sealing test chamber 2.
Further, in the present embodiment, load-bearing part includes two window substrates 15 and multiple supporting members 16, multiple supporting members
16 are supported between two window substrates 15 so that form space between two window substrates 15.Also, two window substrates 15
On be respectively equipped with a window 17, the window 17 on two window substrates 15 on sealing test chamber 2 power beamlet pass through
Through-hole 21 correspond to.Folded region forms above-mentioned working region between two windows 17 on two window substrates 15.Load-bearing part
It is placed in sealing test chamber 2, thus the working region folded by load-bearing part is connected to 2 internal environment of sealing test chamber, close
The temperature of envelope 2 internal environment of test chamber can influence the temperature of working region, and sealing test chamber is entered from sample club body 1
Fluid in 2 can also enter in working region.It is understood that if detection solid sample, solid sample support is in two windows
Between mouth substrate 15, if detection fluid sample or gaseous sample, can flow between two window substrates 15, as above belong to
In carrying sample.
In the present embodiment, the material of window substrate 15 is aluminium oxide, silica, silicon nitride or silicon carbide, window substrate
15 have good chemically and physically stability.Window 17 is self-supporting film, and is transparent.
In the present embodiment, window substrate 15 is square plate, and window 17 is rectangular film.Two supporting members 16 are set,
Two supporting members 16 are arranged diagonal about window 17.Electrode deposition is heated on window substrate 15 and around 17 uniform cloth of window
It sets, around four sides of window 17, the material for heating electrode is Cr/Au/Al2O3、Ti/Au/Al2O3、Cr/Pt/Al2O3、Ti/Pt/
Al2O3、Cr/Cu/Al2O3、Ti/Cu/Al2O3、Cr/Ag/Al2O3、Ti/Ag/Al2O3、Cr/SiC/Al2O3Or Ti/SiC/Al2O3。
Al2O3For high heat conductive insulating inert material, it on the one hand may insure that window temperature raises and reduces rapidly, and be evenly distributed, it is another
Aspect can avoid sample and be reacted with window material.
Four electrode structures, two path electrodes are used to be used for thermometric in the present embodiment, as above-mentioned thermometric electrode 12, two-way electricity
Electrode is heated in pole for heating, as above-mentioned two, that is, is used as above-mentioned secondary heater 11.Four electrodes are by being deposited on window base
Metal lead wire 18 on plate is connected (i.e. one as above-mentioned conducting wire of metal lead wire 18 with the circuit outside sealing test chamber 2
Point), observable influence is not generated on the sealing performance of sealing test chamber 2.Further, sealing test chamber 2 includes passing through
The pedestal 19 and cover board 20 that bolt 29 is removably joined together, pedestal 19 and cover board 20 replaceable load-bearing part when dismantling, or
Solid sample is placed in load-bearing part.The through-hole 21 that power supply beamlet passes through, 19 He of pedestal are respectively equipped in pedestal 19 and cover board 20
Cover board 20 is sealed by the first sealing ring 22.
The region that pedestal 19, cover board 20 and the first sealing ring 22 enclose constitutes the inner cavity of sealing test chamber 2, load-bearing part position
In in the region that pedestal 19, cover board 20 and the first sealing ring 22 enclose, the second sealing ring is folded between load-bearing part and cover board 20
23, it is folded with third sealing ring 24 between load-bearing part and pedestal 19, is formed on pedestal 19 and places the first of the first sealing ring 22
Groove 25, is certainly not limited to this, and in other embodiments, the first groove 25 may be formed on cover board 20, also can be in cover board 20
With corresponding two the first grooves 25 are formed on pedestal 19.The second groove for placing the second sealing ring 23 is formed on cover board 20
26, it is formed with the third groove 27 for placing third sealing ring 24 on pedestal 19, is formed on pedestal 19 and places the 4th of load-bearing part
Groove 28, is certainly not limited to this, and in other embodiments, the 4th groove 28 may be formed on cover board 20, also can be in cover board 20
With corresponding two the 4th grooves 28 are formed on pedestal 19.In the present embodiment, in pedestal 19 be equipped with for fluid by
The one end in duct, duct is connected to the fluid channel in sample club body 1, in the present embodiment with the fluid positioned at base exterior
The other end of pipeline connection, duct is opened on the cell wall of the 4th groove 28, and fluid is sent between two window substrates 15
Region, and then fluid enters working region.
In the present embodiment, the first sealing ring 22, the second sealing ring 23 and third sealing ring 24 are O-shaped fluorine silicone rubber circle,
Utilize above three sealing ring and four groove fitted seals so that sealing test chamber can be subjected to subzero 200 DEG C to above freezing
Temperature change within the scope of 200 DEG C ensures sealing performance, leak rate≤3.0 × 10-8PaL/s, it is ensured that sealing is one of the various
Gas, liquid, solid sample will not be to the high vacuum of transmission electron microscope mirror within the scope of subzero 200 DEG C to 200 DEG C above freezing
Environment generates any adverse effect.It is 1.5 × 10 that 2 maximum of sealing test chamber, which can bear pressure,5Pa。
Further, pedestal 19 and cover board 20 are made of metal material, which is Cu-W alloys.The material has good
Good heat conductivility and extremely low coefficient of thermal expansion effectively inhibit sealing test chamber 2 during heating and cooling due to heat
Drift caused by swollen shrinkage effect, influences the stability of transmission electron microscope imaging.
To sum up, the specimen holder of the present embodiment can be realized former to gas, liquid, solid sample in transmission electron microscope
Position cryogenic freezing is to subzero 200 DEG C, from the real-time dynamic studies material of atomic scale at 200 DEG C above freezing to subzero 200 DEG C of temperature models
Various physics, chemical change in enclosing.The specimen holder of the present embodiment realizes the material in gaseous state and liquid environment to the maximum extent
The macro property of material is measured with the atomic scale of gas liquid solid interfacial reaction mechanism and research, is widely used in probing into various low temperature
Chemosynthesis reaction, low temperature electrochemical reaction, material phase transformation, cryobiochemistry reaction etc..
It is different from common passive heat transfer using thermoelectric module as two level refrigerator based on above-mentioned sample rod structure,
Active adjusting refrigeration flux can be achieved, be used in conjunction with ceramic heating flake and thermistor, be precisely controlled refrigerating capacity and rate.And
And the load-bearing part for being integrated with secondary heater 11 and thermometric electrode 12 can accurately monitor sample micro-area temperature in real time, to greatest extent
Realize the temp regulating function to gaseous state, liquid, solid sample in ground.
Based on above-mentioned sample rod structure, the operating temperature range that can be realized is subzero 200 DEG C to 200 DEG C above freezing, maximum
Cooling rate >=10 DEG C/sec, maximum heating rate >=10 DEG C/sec, maximum heating rate >=500 DEG C/sec of secondary heater, two
Maximum cooling rate >=500 DEG C/sec that the temperature of microcell declines after grade heater is stopped, temperature stability≤± 0.1 DEG C.
The above content is only the preferred embodiment of the utility model, for those of ordinary skill in the art, according to this reality
With novel thought, there will be changes in the specific implementation manner and application range, and the content of the present specification should not be construed as
Limitations of the present invention.
Claims (10)
1. a kind of transmission electron microscope specimen holder in situ, which is characterized in that including：
Sample club body (1)；
Sealing test chamber (2) in front of the sample club body (1)；
The passive type refrigerator (3) of passive type refrigeration is carried out to the sealing test chamber (2)；
The active refrigeration device (4) of active refrigeration is carried out to the sealing test chamber (2)；
Detect the thermal detector of the interior temperature of the sealing test chamber (2)；And
The thermostat being connect with the active refrigeration device (4) and the thermal detector.
2. transmission electron microscope according to claim 1 specimen holder in situ, which is characterized in that
The passive type refrigerator (3) includes low-temperature receiver (5) and heat-conducting piece (6), the heat-conducting piece (6) and the low-temperature receiver (5) and institute
Sealing test chamber (2) connection is stated, to form passive heat transfer between；
The active refrigeration device (4) includes thermoelectric cooling part, the thermoelectric cooling part and the heat-conducting piece (6) and the sealing
Test chamber (2) connects, to take out heat from the sealing test chamber (2) to the heat-conducting piece (6).
3. transmission electron microscope according to claim 2 specimen holder in situ, which is characterized in that further include：
Load-bearing part for carrying sample, the load-bearing part are set in the sealing test chamber (2)；
The primary heater (10) of heat transfer is formed with the cavity wall of the sealing test chamber (2)；And
The secondary heater (11) of microcell heating is carried out to the working region in the load-bearing part；
The primary heater (10) and the secondary heater (11) are connect with the thermostat.
4. transmission electron microscope according to claim 3 specimen holder in situ, which is characterized in that
The primary heater (10) includes the ceramic heating flake being fixed in the cavity wall of the sealing test chamber (2)；
The secondary heater (11) includes the heating electrode being fixed on the load-bearing part；
The thermal detector includes the thermometric electrode (12) being fixed on the load-bearing part and is fixed on the sealing test chamber
(2) thermistor (13) in cavity wall, the thermometric electrode (12) connect with the thermostat with the thermistor (13)
It connects.
5. transmission electron microscope according to claim 4 specimen holder in situ, which is characterized in that
The inside of the sample club body (1) has rod cavity, the rear end of the low-temperature receiver (5) and the sample club body (1) airtight
Connection, the heat-conducting piece (6) are arranged in the rod cavity；
Transmission electron microscope specimen holder in situ further includes hermetic connector (14), the hermetic connector (14) and institute
State the rear side connection of sample club body (1)；
Wherein,
The hermetic connector (14) can carry out electrical conduction, the thermoelectric cooling part, the primary heater (10), described two
Grade heater (11), the thermometric electrode (12) and the thermistor (13) by the hermetic connector (14) and are arranged in
Conducting wire in the rod cavity is electrically connected with the controller；And/or
Fluid channel is equipped in the rod cavity and the hermetic connector (14), fluid source passes through the rod cavity and the airtight company
The fluid channel and the sealing test chamber (2) for connecing device (14) are in fluid communication.
6. transmission electron microscope according to claim 5 specimen holder in situ, which is characterized in that
The external of the low-temperature receiver (5) coats low temperature resistant heat-insulating material；And/or
The low-temperature receiver (5) is connect with the sample club body (1) by Conduction At Low Temperature airtight connecting piece (7), the Conduction At Low Temperature
The external of airtight connecting piece (7) coats low temperature resistant heat-insulating material.
7. transmission electron microscope according to claim 2 specimen holder in situ, which is characterized in that
The low-temperature receiver (5) includes the receiving for accommodating one or more of liquid nitrogen, liquid helium, solid acetonide and solid alcohol
Device.
8. transmission electron microscope according to claim 1 specimen holder in situ, which is characterized in that further include：
Load-bearing part for carrying sample, the load-bearing part are set in the sealing test chamber (2)；
The load-bearing part includes two window substrates (15) and multiple supporting members (16), and multiple supporting members (16) are supported on two
Between a window substrate (15)；
The sealing test chamber (2) is equipped with the through-hole (21) that passes through of power supply beamlet, on two window substrates (15)
Equipped with window (17) corresponding with the through-hole (21), folded region forms working region between two windows (17).
9. transmission electron microscope according to claim 8 specimen holder in situ, which is characterized in that
The sealing test chamber (2) includes the pedestal (19) being removably joined together and cover board (20), the pedestal
(19) and in the cover board (20) it is respectively equipped with the through-hole (21), passes through between the pedestal (19) and the cover board (20)
One sealing ring (22) seals；
The load-bearing part is located in the region that the pedestal (19), the cover board (20) and first sealing ring (22) enclose,
The second sealing ring (23) is folded between the load-bearing part and the cover board (20), between the load-bearing part and the pedestal (19)
It is folded with third sealing ring (24)；
The first groove for placing first sealing ring (22) is formed on the pedestal (19) and/or the cover board (20)
(25)；
The second groove (26) for placing second sealing ring (23) is formed on the cover board (20)；
The third groove (27) for placing the third sealing ring (24) is formed on the pedestal (19)；
The 4th groove (28) for placing the load-bearing part is formed on the pedestal (19) and/or the cover board (20).
10. transmission electron microscope according to claim 9 specimen holder in situ, which is characterized in that
The pedestal (19) and the cover board (20) are made of Cu-W alloys；And/or
The material of the window substrate (15) is aluminium oxide, silica, silicon nitride or silicon carbide；And/or
Transmission electron microscope specimen holder in situ further includes forming heat transfer with the cavity wall of the sealing test chamber (2)
Primary heater (10) and in the load-bearing part working region carry out microcell heating secondary heater (11), it is described
Primary heater (10) and the secondary heater (11) are connect with the thermostat, and the secondary heater (11) is to be fixed on
Multiple heating electrodes on the load-bearing part, the heating electrode deposition is on the window (17), the material of the heating electrode
Material is Cr/Au/Al2O3、Ti/Au/Al2O3、Cr/Pt/Al2O3、Ti/Pt/Al2O3、Cr/Cu/Al2O3、Ti/Cu/Al2O3、Cr/
Ag/Al2O3、Ti/Ag/Al2O3、Cr/SiC/Al2O3Or Ti/SiC/Al2O3。
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| CN201820104077.7U CN207993796U (en) | 2018-01-22 | 2018-01-22 | A kind of transmission electron microscope specimen holder in situ |
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|---|---|---|---|
| CN201820104077.7U CN207993796U (en) | 2018-01-22 | 2018-01-22 | A kind of transmission electron microscope specimen holder in situ |
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| CN207993796U true CN207993796U (en) | 2018-10-19 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109781499A (en) * | 2019-01-29 | 2019-05-21 | 中国科学院微电子研究所 | Thermotonus device and preparation method thereof |
| CN110006740A (en) * | 2019-03-21 | 2019-07-12 | 北京工业大学 | In Situ Heating mechanics specimen holder |
| 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 |
| 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 |
| CN111312573A (en) * | 2020-03-12 | 2020-06-19 | 厦门超新芯科技有限公司 | Transmission electron microscope high-resolution in-situ liquid phase heating chip and preparation method thereof |
| CN113345784A (en) * | 2020-02-18 | 2021-09-03 | 中国科学院物理研究所 | Low-temperature in-situ sample rod |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109781499A (en) * | 2019-01-29 | 2019-05-21 | 中国科学院微电子研究所 | Thermotonus device and preparation method thereof |
| CN109781499B (en) * | 2019-01-29 | 2021-07-23 | 中国科学院微电子研究所 | Temperature reactor and manufacturing method thereof |
| CN110006740A (en) * | 2019-03-21 | 2019-07-12 | 北京工业大学 | In Situ Heating mechanics specimen holder |
| 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 |
| CN110021512B (en) * | 2019-04-04 | 2022-02-08 | 北京工业大学 | Electrothermal sample rod system for in-situ liquid environment transmission electron microscope |
| 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 |
| CN113345784A (en) * | 2020-02-18 | 2021-09-03 | 中国科学院物理研究所 | Low-temperature in-situ sample rod |
| CN113345784B (en) * | 2020-02-18 | 2023-06-02 | 中国科学院物理研究所 | Low-temperature in-situ sample rod |
| CN111312573A (en) * | 2020-03-12 | 2020-06-19 | 厦门超新芯科技有限公司 | Transmission electron microscope high-resolution in-situ liquid phase heating chip and preparation method thereof |
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