CN105067400B - A kind of in situ quantitation heater for ultramicroscope - Google Patents
A kind of in situ quantitation heater for ultramicroscope Download PDFInfo
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- CN105067400B CN105067400B CN201510437346.2A CN201510437346A CN105067400B CN 105067400 B CN105067400 B CN 105067400B CN 201510437346 A CN201510437346 A CN 201510437346A CN 105067400 B CN105067400 B CN 105067400B
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Abstract
The invention discloses a kind of in situ quantitation heater for ultramicroscope, including matrix, warm table, tooth pin, heating test resistance, some wires and some flexible connecting members；Matrix surface is provided with groove, warm table is positioned at described groove, one end of flexible connecting member is connected with the side of warm table, the other end of flexible connecting member is connected with the inwall of described groove, the unsettled one end of warm table is provided with some tooth pins for placing sample, heating test resistance is positioned on warm table, and the exit of heating test resistance is connected with external circuits be drawn out to the upper surface of matrix by wire after, and wire is positioned on flexible connecting member and matrix.The present invention can utilize focused ion bundle to prepare sample for use in transmitted electron microscope from macroscopic material easily, and sample carries out in situ quantitation heating, and thermal drift is little.
Description
Technical field
Ultramicroscope accessory of the present invention and micro Nano material in site measurement research field, relate to one
In situ quantitation heater for ultramicroscope.
Background technology
Ultramicroscope refer to be come by electronics the microscope of imaging, such as transmission electron microscope and
Scanning electron microscope.Ultramicroscope (in-situ TEM) technology refers to by electronics in situ
Microscope and specimen holder thereof are transformed, and sample applies other external drives, such as power, heat, electricity
Deng, and real-time monitored dynamic change of the pattern of sample, structure under the effect of these external drives
The technology of process.
Sample for ultramicroscope especially transmission electron microscope can be divided into two types,
A kind of nano material being Bottom-up approach and growing, such as nano-particle, nano wire etc., this sample
The sign of product is relatively easy to, it is only necessary to observing in sample dispersion to contained network.Another kind is certainly
Pushing up downward method to be prepared by macroscopic view sample, typically have two kinds of methods, a kind of is traditional passing through
Block sample is thinned to tens microns by the mode of grinding and polishing, then subtracts by the method for double spray/ion millings
It is as thin as tens to hundreds of nanometer thickness.For needing the occasion observing ad-hoc location (such as interface, deformation
District etc.), this method success rate is the lowest, it is difficult to fixed point observation.Another kind is to utilize focused ion bundle
(FIB) extraction method in technology (liftout), cuts into 1-2um by block sample fixed point thick,
The thin slice of 10-20um length/width, then with nano-machine hands, thin slice is proposed from block sample, then
Flakelet is soldered in the special contained network of FIB, finally with FIB, flakelet is thinned to tens to several
Hundred nanometer thickness.This method can pinpoint making sample for use in transmitted electron microscope, is therefore becoming increasingly popular.
In recent years, ultramicroscope situ heating technique achieves a series of progress, at catalyst
A series of progress is achieved in the working mechanism of nano-particle, inefficacy mechanism etc. field.But it is existing former
The many nano materials (such as nano-particle, nano wire) for Bottom-up approach growth of position warm table
Design, the heating of the sample for use in transmitted electron microscope prepared for top-down approach still lacks effective means.
Investigation shows, the most can not fully meet research worker under high spatial resolution
The sample prepared from macroscopic view sample is carried out the Electronic Speculum heating testboard of in situ quantitative study demand.
Can be used for the ultramicroscope add in-place thermal station from block materials heating in the market can divide
It is two classes, the most traditional stove formula heating and MEMS heating.
Stove formula heating (such as Gatan 628 uniclinal heating pole) is by by little for traditional macro warm table
Type, is processed into Φ 3mm by macroscopic view sample by modes such as grinding and polishing, double spray, ion millings
Flake, by fixed resistance silk, whole Φ 3mm sample is heated below sample.Phase
For effective area of observation coverage of sample, this mode of heating heating volume is excessive, thus in high power
Presenting huge thermal drift in ultramicroscope after amplification, this makes moving in heating and cooling process
The observation of state high power is extremely difficult to be carried out.Another shortcoming of such warm table is area of observation coverage sample temperature
Being difficult to accurately control, and heat-stable time is long, heat/cool rates is the slowest, limits and can see
The experimental phenomena observed.It addition, for needing to carry out the experiment of fixed point observation, prepared by this sample
The success rate of mode is the lowest.
MEMS heating refers to the heating with the miniature heating region processed by MEMS technology
Platform.MEMS warm table typically utilizes special metal, sample is heated by the resistance of quasiconductor.This
Plant warm table little owing to heating volume, it is possible to obtain the least thermal drift, and can be to sample area
The temperature in territory compares and is accurately controlled, and development in recent years is rapid.But the main pin of this kind of sample stage
Heating design to the material such as nano-particle, nano wire, is the film like thermal treatment zone centered by sample stage
Territory, surrounding is the structure in thick district, it is difficult to transferred to above it by the sample prepared from macroscopic material.
The thin district for transmission electron microscope observing, Zai Jiangbao district can only be processed at present in advance in macroscopic material
Transfer to both sides, heating plate Shang Bingbao district deposition Pt fix.But this method exists following two asks
Topic: firstly, since sample cannot carry out thinning in Zai Duibao district after transferring on heating plate, therefore without
Method avoids the pollution in the Pt district thin to sample deposited during fixing sample；Secondly, for extraction method success
The consideration of rate, is difficult to be worked into the thinnest by thin for sample district in advance.The sample that the most this method makes
It is difficult to meet the demand carrying out carrying out testing under higher spatial resolution.
The above-mentioned all of In Situ Heating device for ultramicroscope, due to the defect of design, all
Research worker cannot be met under the conditions of high spatial resolution, the sample prepared by macroscopic material is carried out
The demand of quantitative heating research.
Summary of the invention
It is an object of the invention to the shortcoming overcoming above-mentioned prior art, it is provided that a kind of for electronics
Microscopical in situ quantitation heater, this device can utilize focused ion bundle from macroscopic view easily
Sample for use in transmitted electron microscope prepared by material, and sample carries out in situ quantitation heating, and thermal drift is little.
For reaching above-mentioned purpose, the in situ quantitation for ultramicroscope of the present invention adds hot charging
Put and include matrix, warm table, tooth pin, heating test resistance, some wires and some flexibilities
Connector；
The side of matrix is provided with the groove run through up and down, and warm table is positioned at described groove, and flexibility is even
One end of fitting is connected with the side of warm table, the other end of flexible connecting member and described groove
Inwall is connected, and the unsettled one end of warm table is provided with some tooth pins for placing sample, and heating is surveyed
Examination resistance is positioned at the upper of warm table, and the exit of heating test resistance is drawn out to matrix by wire
Being connected with external circuits after upper surface, wire is positioned on flexible connecting member and matrix.
Flexible connecting member is more than edge and warm table along the rigidity with the deformation of warm table contact surface normal orientation
The rigidity of any direction deformation in contact surface.
The upper surface of the upper surface of matrix, the upper surface of warm table and flexible connecting member is positioned at same flat
On face.
Described heating test resistance is serpentine-like to be coiled on warm table.
The quantity of the exit of heating test resistance is more than or equal to 3.
Described heating test resistance is made by platinum or tungsten.
The first protective layer that described matrix includes being sequentially distributed from top to bottom, the first insulating barrier, first
Top silicon layer, silicon dioxide intermediate layer and layer-of-substrate silicon, wherein, wire is positioned at the first protective layer and the
Between one insulating barrier.
Described warm table includes the second protective layer, the second insulating barrier and being sequentially distributed from top to bottom
Two top silicon layers, wherein, heating test resistance is between the second protective layer and the second insulating barrier.
Each wire is symmetrical.
The method have the advantages that
Microheating stage one end in the in situ quantitation heater of ultramicroscope of the present invention
Unsettled, free end, with the tooth pin for fixing sample, uses extraction method (lift-out process)
After sample being extracted from macroscopic material and being fixed on tooth pin, can be entered by focused ion bundle
Sample is thinned to tens nanometer by one step, solves the dirt in the Pt district thin to sample of deposition during fixing sample
Dye problem, it is achieved to sample observation under high spatial resolution.Additionally, due to it is of the present invention
In situ quantitation heating devices heat volume is the least, and therefore thermal expansion is minimum, and warm table and matrix
Between be connected by flexible connecting member, the power that the thermal expansion of warm table produces passes through flexible connecting member
Deformation release, thus avoid warm table in heating process to heave, it is to avoid sample is sent out in short transverse
Changing, thus reduce sample thermal drift in heating process, it is achieved at high spatial resolution bar
Under part, the sample prepared by macroscopic material is carried out quantitative heating research.It addition, flexible connecting member energy
Enough effectively reduce the warm table heat transfer to matrix, make each regional temperature of warm table uniform, thus can
Accurately to record the temperature in territory, sample deposition, it is simple to the temperature in territory, sample deposition is controlled.
Further, each wire is symmetrical, can accurately measure the resistance of heating test resistance, and
The temperature of warm table is accurately measured by the resistance-temperature relationship of heating test resistance；Described heating is surveyed
When the exit of examination resistance is more than or equal to 3, it is possible to realize the feedback control to temperature, solve gas
The problem that under the conditions of atmosphere, sample actual temperature and design temperature exist relatively large deviation.
Accompanying drawing explanation
Fig. 1 is the structural representation of the present invention；
Fig. 2 is the enlarged drawing in Fig. 1 at A；
Fig. 3 is the sectional view of Fig. 2；
Fig. 4 is the circuit diagram of the present invention.
Wherein, 1 be matrix, 2 be wire, 3 be flexible connecting member, 4 be warm table, 5 for adding
Thermal test resistance, 6 be tooth pin, 7 be sample, 8 be groove, 9 be layer-of-substrate silicon, 10 for dioxy
SiClx intermediate layer, 111 be the first top silicon layer, 121 be the first insulating barrier, 131 be the first protective layer,
112 it is the second top silicon layer, 122 is the second insulating barrier, 132 is the second protective layer.
Detailed description of the invention
Below in conjunction with the accompanying drawings the present invention is described in further detail:
With reference to Fig. 1, Fig. 2, the in situ quantitation heater for ultramicroscope of the present invention
Including matrix 1, warm table 4, tooth pin 6, heating test resistance 5, some wires 2, Yi Jiruo
Dry flexible connecting member 3；The side of matrix 1 is provided with the groove 8 run through up and down, and warm table 4 is positioned at institute
Stating in groove 8, one end of flexible connecting member 3 is connected with the side of warm table 4, flexibly connects
The other end of part 3 is connected with the inwall of described groove 8, if the unsettled one end of warm table 4 is provided with
Doing the tooth pin 6 for placing sample 7, heating test resistance 5 is positioned at the upper of warm table 4, heating
The exit of test resistance 5 by wire 2 be drawn out to after the upper surface of matrix 1 with external circuits phase
Connecting, wire 2 is positioned on flexible connecting member 3 and matrix 1.
It should be noted that flexible connecting member 3 deforms along with warm table 4 contact surface normal orientation
Rigidity more than along and the rigidity of any direction deformation in warm table 4 contact surface, the upper surface of matrix 1,
The upper surface of warm table 4 and the upper surface of flexible connecting member 3 are in the same plane；Add Thermal test
Resistance 5 is serpentine-like to be coiled on warm table 4；The quantity of the exit of heating test resistance 5 is more than
Equal to 3；Heating test resistance 5 is made by platinum or tungsten, and each wire 2 is symmetrical.
With reference to Fig. 3, the first protective layer 131 that described matrix 1 includes being sequentially distributed from top to bottom, the
One insulating barrier 121, first pushes up silicon layer 111, silicon dioxide intermediate layer 10 and layer-of-substrate silicon 9, its
In, wire 2 is between the first protective layer 131 and the first insulating barrier 121；Warm table 4 includes
The second protective layer the 132, second insulating barrier 122 and the second top silicon layer 112 being sequentially distributed from top to bottom,
Wherein, heating test resistance 5 is between the second protective layer 132 and the second insulating barrier 122.
With reference to Fig. 2, Fig. 4, heating test resistance 5 is snakelike coils in microheating stage 4 upper surface, profit
Can heat microheating stage 4 with its Joule heat, microheating stage 4 and matrix 1 are only by soft
Property connector 3 connects, and flexible connecting member 3 decreases the microheating stage 4 heat transfer to matrix 1, makes
The each regional temperature of microheating stage 4 is uniform, such that it is able to by the temperature of microheating stage 4 is surveyed
The temperature of sample 7 is measured and is controlled in amount and control；Heating test resistance 5 is divided by four symmetries
The wire 2 of cloth is drawn, and utilizes the circuit shown in Fig. 4, can accurately measure heating test resistance
The resistance of 5, and then utilize the resistance-temperature relationship of heating test resistance 5 accurately to measure the temperature of sample
Degree, and temperature can be carried out feedback control, thus solve sample actual temperature under atmospheric condition
The problem that there is relatively large deviation with design temperature.
As a example by the sample 7 prepared from nanocrystalline copper block sample is carried out In Situ Heating test, its
Detailed description of the invention is as described below:
1. nanocrystalline copper block Sample Preparation Procedure under focused ion bundle (FIB):
1) nanocrystalline copper block sample and heater 1 of the present invention are put into focused ion simultaneously
In bundle (FIB)；
2) extraction method is utilized to be cut into about by region FIB interested for nanocrystalline copper block
The thin slice of 20*10*3um, then the end thereof contacts with nano-machine hands Yu thin slice, and weld, by thin
The other end of sheet cuts off, mobile nano-machine hands, is proposed by thin slice from nanocrystalline copper block sample
Come；
4) with nano-machine hands by the tooth pin 6 in the flap contact present invention, and thin slice is welded in tooth pin
On 6；
5) one end that thin slice and nano-machine hands weld is cut off, withdraw nano-machine hands；
6) the thin slice FIB being fixed on tooth pin 6 is thinned to be suitable for the thickness of transmission electron microscope observing
(about 100nm), becomes sample 7；
2. In Situ Heating experimentation under transmission electron microscope:
1) heater 1 being welded with sample 7 is placed on specimen holder, by four wires 2 and sample
On bar, four conductive pins are connected；
2) specimen holder is connected with power-supply controller of electric；
3) in transmission electron microscope, find the suitable viewing area of sample 7；
4) sample 7 is heated, and utilize the resistance-temperature of the heating test resistance 5 calibrated in advance
Degree relation carries out real time temperature measurement and control to sample 7.
Claims (6)
1. the in situ quantitation heater for ultramicroscope, it is characterised in that include base
Body (1), warm table (4), tooth pin (6), heating test resistance (5), some wires (2), with
And some flexible connecting members (3)；
Matrix (1) side is provided with the groove (8) run through up and down, and warm table (4) is positioned at described groove
(8) in, one end of flexible connecting member (3) is connected with the side of warm table (4), and flexibility is even
The other end of fitting (3) is connected with the inwall of described groove (8), and warm table (4) is unsettled
One end is provided with some tooth pins (6) for placing sample (7), and heating test resistance (5) is positioned at and adds
In thermal station (4), the exit of heating test resistance (5) is drawn out to matrix (1) by wire (2)
Upper surface after be connected with external circuits, wire (2) is positioned at flexible connecting member (3) and matrix (1)
On；
Flexible connecting member (3) is more than edge along the rigidity with the deformation of warm table (4) contact surface normal orientation
With the rigidity of any direction deformation in warm table (4) contact surface；
The upper surface of matrix (1), the upper surface of warm table (4) and flexible connecting member (3) upper
Surface is in the same plane；
Described heating test resistance (5) is serpentine-like to be coiled on warm table (4).
In situ quantitation heater for ultramicroscope the most according to claim 1, its
Being characterised by, the quantity of the exit of heating test resistance (5) is more than or equal to 3.
In situ quantitation heater for ultramicroscope the most according to claim 1, its
Being characterised by, described heating test resistance (5) is made by platinum or tungsten.
In situ quantitation heater for ultramicroscope the most according to claim 1, its
It is characterised by, the first protective layer (131) that described matrix (1) includes being sequentially distributed from top to bottom,
First insulating barrier (121), the first top silicon layer (111), silicon dioxide intermediate layer (10) and silicon substrate
Layer (9), wherein, wire (2) is positioned at the first protective layer (131) and the first insulating barrier (121)
Between.
In situ quantitation heater for ultramicroscope the most according to claim 4, its
It is characterised by, the second protective layer (132) that described warm table (4) includes being sequentially distributed from top to bottom,
Second insulating barrier (122) and the second top silicon layer (112), wherein, heating test resistance (5) is positioned at
Between second protective layer (132) and the second insulating barrier (122).
In situ quantitation heater for ultramicroscope the most according to claim 1, its
Being characterised by, each wire (2) is symmetrical.
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| CN105301027B (en) * | 2015-11-22 | 2017-11-14 | 北京工业大学 | A kind of transmission/ESEM power, the experiment porch in situ of thermal coupling field loading |
| 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 |
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| CN102401758A (en) * | 2010-09-17 | 2012-04-04 | 中芯国际集成电路制造(上海)有限公司 | Method for manufacturing TEM sample |
| US8258473B2 (en) * | 2010-11-12 | 2012-09-04 | Nanotem, Inc. | Method and apparatus for rapid preparation of multiple specimens for transmission electron microscopy |
| CN102539213B (en) * | 2012-02-15 | 2013-06-19 | 西北工业大学 | Preparation method for transmission electron microscope (TEM) specimen of cadmium zinc tellurium (CdZnTe) and metal interface |
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| CN104319220B (en) * | 2014-10-14 | 2016-08-24 | 西安交通大学 | A kind of quantitative nano warm table for electron microscope |
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