CN105067400A - In-situ quantitative heating apparatus for electron microscope - Google Patents
In-situ quantitative heating apparatus for electron microscope Download PDFInfo
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- CN105067400A CN105067400A CN201510437346.2A CN201510437346A CN105067400A CN 105067400 A CN105067400 A CN 105067400A CN 201510437346 A CN201510437346 A CN 201510437346A CN 105067400 A CN105067400 A CN 105067400A
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Abstract
The present invention discloses an in-situ quantitative heating apparatus for an electron microscope. The in-situ quantitative heating apparatus comprises a base body, a heating table, tooth needles, a heating test resistor, a plurality of conducting wires, and a plurality of flexible connection members, wherein the base body surface is provided with a concave groove, the heating table is positioned inside the concave groove, one ends of the flexible connection members are connected with the side surface of the heating table, the other ends of the flexible connection members are connected with the inner wall of the concave groove, the suspension end of the heating table is provided with a plurality of the tooth needles for placing a sample, the heating test resistor is positioned on the heating table, the lead-out end of the heating test resistor is led out onto the upper surface of the base body through the conducting wire and then the lead-out end is connected with an external circuit, and the conducting wires are positioned on the flexible connection members and the base body. According to the present invention, the transmission electron microscope sample can be prepared from the macroscopic material by conveniently using the focusing ion beam, the sample is subjected to in-situ quantitative heating, and the thermal drift is small.
Description
Technical field
Electron microscope accessory of the present invention and micro Nano material in site measurement research field, relate to a kind of in situ quantitation heating arrangement for electron microscope.
Background technology
Electron microscope refers to the microscope being carried out imaging by electronics, such as transmission electron microscope and scanning electron microscope.Original position electron microscope (in-situTEM) technology refers to by transforming electron microscope and specimen holder thereof, other external drives are applied to sample, as power, heat, electricity etc., and the technology of the real-time monitored pattern of sample, dynamic changing process of structure under the effect of these external drives.
Sample for electron microscope especially transmission electron microscope can be divided into two types, a kind of nano material being Bottom-up approach and growing, as nano particle, nano wire etc., the sign of this sample is comparatively easy, only needs sample dispersion to observe to carrying on the net.Another kind be top-down approach by macroscopical sample preparation, generally have two kinds of methods, a kind of is traditional by the mode of grinding and polishing, block sample is thinned to tens microns, then is thinned to tens to hundreds of nanometer thickness by the method for two spray/ion milling.For needing the occasion (as interface, distorted area etc.) of observing ad-hoc location, this method success ratio is very low, is difficult to fixed point observation.Another kind is the extraction method (liftout) utilized in focused ion beam (FIB) technology, block sample fixed point is cut into 1-2um thick, the thin slice of 10-20um length/width, with nano-machine hand, thin slice is proposed from block sample again, again flakelet is soldered to special year of FIB online, finally with FIB, flakelet is thinned to tens to hundreds of nanometer thickness.This method can fix a point to make sample for use in transmitted electron microscope, therefore more and more welcome.
In recent years, electron microscope situ heating technique achieves a series of progress, achieves a series of progress in the field such as working mechanism, inefficacy mechanism of the nano particles such as catalyzer.But the nano material (as nano particle, nano wire) that existing add in-place thermal station spininess grows Bottom-up approach designs, the heating of the sample for use in transmitted electron microscope prepared for top-down approach still lacks effective means.Investigation shows, can not meet researchist carries out in situ quantitative study demand under high spatial resolution Electronic Speculum heating test board to the sample from macroscopical sample preparation in the market completely.
Can be used in the market can being divided into two classes from the electron microscope add in-place thermal station of block materials heating, namely traditional stove formula heating and MEMS heating.
Stove formula heating (as Gatan628 uniclinal heating pole) is by by the miniaturization of traditional macro warm table, macroscopical sample is processed into the flake of Φ 3mm by modes such as grinding and polishing, two spray, ion millings, by fixed resistance silk, whole Φ 3mm sample is heated below sample.For effective area of observation coverage of sample, this type of heating heating volume is excessive, thus presents huge thermal drift in electron microscope after magnification at high multiple, and this makes, and the dynamic high power observation in heating and cooling process is extremely difficult to be carried out.Another shortcoming of such warm table is that area of observation coverage sample temperature is difficult to accurate control, and heat-stable time is long, and heat/cool rates is excessively slow, limits the experimental phenomena that can observe.In addition, for needing the experiment carrying out fixed point observation, the success ratio of this sample preparation mode is very low.
MEMS heating refers to the warm table with the miniature heating region processed by MEMS technology.The resistance of MEMS warm table general special metal, semiconductor heats sample.This warm table is little owing to heating volume, and can obtain very little thermal drift, and can compare accurate control to the temperature of sample area, development in recent years is rapid.But this kind of sample stage is mainly for the heating design of the material such as nano particle, nano wire, be film-form heating region centered by sample stage, surrounding is the structure in thick district, is difficult to the sample prepared from macroscopic material to be transferred to above it.Can only process the thin district for transmission electron microscope observing at present in advance in macroscopic material, Zai Jiangbao district transfers to both sides, heating plate Shang Bingbao district deposition Pt and fixes.But this method exists following two problems: first, transfer to after on heating plate cannot carry out thinning in Zai Duibao district due to sample, the Pt deposited during fixed sample therefore cannot be avoided the pollution in the thin district of sample; Secondly, for the consideration of extraction method success ratio, be difficult in advance thin for sample district is worked into very thin.Therefore the sample that this method makes is difficult to meet the demand of carrying out carrying out testing under higher spatial resolution.
Above-mentioned all In Situ Heating devices for electron microscope, due to the defect of design, all cannot meet researchist carries out quantitative heating research under high spatial resolution condition demand to the sample prepared by macroscopic material.
Summary of the invention
The object of the invention is to the shortcoming overcoming above-mentioned prior art, provide a kind of in situ quantitation heating arrangement for electron microscope, this device can utilize focused ion beam to prepare sample for use in transmitted electron microscope from macroscopic material easily, and carries out in situ quantitation heating to sample, and thermal drift is little.
For achieving the above object, the in situ quantitation heating arrangement for electron microscope of the present invention comprises matrix, warm table, tooth pin, heating test resistance, some wires and some flexible connecting members;
The side of matrix is provided with the groove run through up and down, 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 be positioned at the upper of warm table, heating test resistance exit be drawn out to the upper surface of matrix by wire after be connected with external circuits, wire is positioned on flexible connecting member and matrix.
The rigidity that flexible connecting member edge and warm table surface of contact normal orientation are out of shape is greater than the rigidity that edge is out of shape with any direction in warm table surface of contact.
The upper surface of the upper surface of matrix, the upper surface of warm table and flexible connecting member is in the same plane.
Described heating test resistance is snakelike being 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.
Described matrix comprises the first protective seam, the first insulation course, the first top silicon layer, silicon dioxide intermediate layer and the layer-of-substrate silicon that distribute successively from top to bottom, and wherein, wire is between the first protective seam and the first insulation course.
Described warm table comprises the second protective seam, the second insulation course and the second top silicon layer that distribute successively from top to bottom, and wherein, heating test resistance is between the second protective seam and the second insulation course.
Each wire is symmetrical.
The present invention has following beneficial effect:
Of the present invention unsettled for microheating stage one end in the in situ quantitation heating arrangement of electron microscope, free end is with the tooth pin for fixed sample, extraction method (lift-outprocess) is used to be extracted from macroscopic material by sample and be fixed on after on tooth pin, further sample can be thinned to tens nanometer by focused ion beam, the Pt deposited when solving fixed sample, to the pollution problem in the thin district of sample, realizes the observation of sample under high spatial resolution.In addition, because in situ quantitation heating devices heat volume of the present invention is very little, therefore thermal expansion is minimum, and be connected by flexible connecting member between warm table with matrix, the power that the thermal expansion of warm table produces is discharged by the distortion of flexible connecting member, thus avoid warm table in heating process to heave, sample is avoided to change in short transverse, thus reduce the thermal drift of sample in heating process, realize carrying out quantitative heating research to the sample prepared by macroscopic material under high spatial resolution condition.In addition, flexible connecting member can effectively reduce the heat transfer of warm table to matrix, makes each regional temperature of warm table even, thus accurately can record the temperature in territory, sample deposition, be convenient to control the temperature in territory, sample deposition.
Further, each wire is symmetrical, can the resistance of Accurate Measurement heating test resistance, and by the temperature of resistance-temperature relationship Accurate Measurement warm table of heating test resistance; When the exit of described heating test resistance is more than or equal to 3, the FEEDBACK CONTROL to temperature can be realized, solve sample actual temperature and design temperature under atmospheric condition and there is the problem of relatively large deviation.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention;
Fig. 2 is the enlarged drawing at A place in Fig. 1;
Fig. 3 is the sectional view of Fig. 2;
Fig. 4 is circuit diagram of the present invention.
Wherein, 1 be matrix, 2 be wire, 3 be flexible connecting member, 4 be warm table, 5 be tooth pin, 7 be sample, 8 be groove, 9 be layer-of-substrate silicon, 10 be the second protective seam for silicon dioxide intermediate layer, 111 be the first top silicon layer, 121 be the first insulation course, 131 be the first protective seam, 112 be the second top silicon layer, 122 is the second insulation course, 132 for heating test resistance, 6.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in further detail:
With reference to figure 1, Fig. 2, the in situ quantitation heating arrangement for electron microscope of the present invention comprises matrix 1, warm table 4, tooth pin 6, heating test resistance 5, some wires 2 and some flexible connecting members 3; The side of matrix 1 is provided with the groove 8 run through up and down, warm table 4 is positioned at described groove 8, one end of flexible connecting member 3 is connected with the side of warm table 4, the other end of flexible connecting member 3 is connected with the inwall of described groove 8, the unsettled one end of warm table 4 is provided with some tooth pins 6 for placing sample 7, heating test resistance 5 is positioned at the upper of warm table 4, be connected with external circuits the exit of heating test resistance 5 is drawn out to the upper surface of matrix 1 by wire 2 after, wire 2 is positioned at flexible connecting member 3 with on matrix 1.
It should be noted that, flexible connecting member 3 is greater than the rigidity along being out of shape with any direction in warm table 4 surface of contact along the rigidity of being out of shape with warm table 4 surface of contact normal orientation, and the upper surface of the upper surface of matrix 1, the upper surface of warm table 4 and flexible connecting member 3 is in the same plane; Heating test resistance 5 is coiled on warm table 4 in snakelike; The quantity of the exit of heating test resistance 5 is more than or equal to 3; Heating test resistance 5 is made by platinum or tungsten, and each wire 2 is symmetrical.
With reference to figure 3, described matrix 1 comprises the first protective seam 131, first insulation course 121, first top silicon layer 111, silicon dioxide intermediate layer 10 and the layer-of-substrate silicon 9 distributed successively from top to bottom, wherein, wire 2 is between the first protective seam 131 and the first insulation course 121; Warm table 4 comprises the second protective seam 132, second insulation course 122 and the second top silicon layer 112 distributed successively from top to bottom, and wherein, heating test resistance 5 is between the second protective seam 132 and the second insulation course 122.
With reference to figure 2, Fig. 4, test resistance 5 is snakelike coils in microheating stage 4 upper surface in heating, utilize its Joule heat can heat microheating stage 4, microheating stage 4 is connected by means of only flexible connecting member 3 with matrix 1, flexible connecting member 3 decreases the heat transfer of microheating stage 4 to matrix 1, make each regional temperature of microheating stage 4 even, thus can by measuring the temperature of microheating stage 4 and control to measure and the temperature of Quality control 7; Heating test resistance 5 is drawn by four symmetrical wires 2, utilize the circuit shown in Fig. 4, accurately can measure the resistance of heating test resistance 5, and then utilize the temperature of the resistance-temperature relationship Accurate Measurement sample heating test resistance 5, and FEEDBACK CONTROL can be carried out to temperature, thus under solving atmospheric condition there is the problem of relatively large deviation in sample actual temperature and design temperature.
To carry out In Situ Heating test to the sample 7 from the sample preparation of nanocrystalline copper block, its embodiment is as described below:
1. nanocrystalline copper block Sample Preparation Procedure under focused ion beam (FIB):
1) nanocrystalline copper block sample and heating arrangement of the present invention 1 are put into focused ion beam (FIB) simultaneously;
2) utilize extraction method that interested for nanocrystalline copper block region FIB is cut into the thin slice of about 20*10*3um, use the end thereof contacts of nano-machine hand and thin slice again, and weld, the other end of thin slice is cut off, mobile nano-machine hand, puts forward thin slice from nanocrystalline copper block sample;
4) use nano-machine hand by the tooth pin 6 in flap contact the present invention, and thin slice is welded on tooth pin 6;
5) one end that thin slice and nano-machine hand weld is cut off, withdraw nano-machine hand;
6) the thin slice FIB be fixed on tooth pin 6 is thinned to the thickness (about 100nm) of applicable transmission electron microscope observing, becomes sample 7;
2. In Situ Heating experimentation under transmission electron microscope:
1) heating arrangement 1 being welded with sample 7 is placed on specimen holder, four wires 2 are connected with four conductive pins on specimen holder;
2) specimen holder is connected with power-supply controller of electric;
3) in transmission electron microscope, the viewing area that sample 7 is suitable is found;
4) sample 7 is heated, and utilize the resistance-temperature relationship of the heating test resistance 5 of having calibrated in advance to carry out real time temperature measurement and control to sample 7.
Claims (9)
1. the in situ quantitation heating arrangement for electron microscope, it is characterized in that, comprise matrix (1), warm table (4), tooth pin (6), heating test resistance (5), some wires (2) and some flexible connecting members (3);
Matrix (1) side is provided with the groove (8) run through up and down, warm table (4) is positioned at described groove (8), one end of flexible connecting member (3) is connected with the side of warm table (4), the other end of flexible connecting member (3) is connected with the inwall of described groove (8), the unsettled one end of warm table (4) is provided with some tooth pins (6) for placing sample (7), heating test resistance (5) is positioned on warm table (4), the exit of heating test resistance (5) passes through to be connected with external circuits after wire (2) is drawn out to the upper surface of matrix (1), wire (2) is positioned at flexible connecting member (3) with on matrix (1).
2. the in situ quantitation heating arrangement for electron microscope according to claim 1, it is characterized in that, the rigidity that flexible connecting member (3) edge and warm table (4) surface of contact normal orientation are out of shape is greater than the rigidity that edge is out of shape with any direction in warm table (4) surface of contact.
3. the in situ quantitation heating arrangement for electron microscope according to claim 1, it is characterized in that, the upper surface of the upper surface of matrix (1), the upper surface of warm table (4) and flexible connecting member (3) is in the same plane.
4. the in situ quantitation heating arrangement for electron microscope according to claim 1, is characterized in that, described heating test resistance (5) is coiled on warm table (4) in snakelike.
5. the in situ quantitation heating arrangement for electron microscope according to claim 1, is characterized in that, the quantity of the exit of heating test resistance (5) is more than or equal to 3.
6. the in situ quantitation heating arrangement for electron microscope according to claim 1, is characterized in that, described heating test resistance (5) is made by platinum or tungsten.
7. the in situ quantitation heating arrangement for electron microscope according to claim 1; it is characterized in that; described matrix (1) comprise distribute successively from top to bottom the first protective seam (131), the first insulation course (121), the first top silicon layer (111), silicon dioxide intermediate layer (10) and layer-of-substrate silicon (9); wherein, wire (2) is positioned between the first protective seam (131) and the first insulation course (121).
8. the in situ quantitation heating arrangement for electron microscope according to claim 7; it is characterized in that; described warm table (4) comprise distribute successively from top to bottom the second protective seam (132), the second insulation course (122) and second top silicon layer (112); wherein, heat test resistance (5) to be positioned between the second protective seam (132) and the second insulation course (122).
9. the in situ quantitation heating arrangement for electron microscope according to claim 1, is characterized in that, each wire (2) is symmetrical.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510437346.2A CN105067400B (en) | 2015-07-22 | 2015-07-22 | A kind of in situ quantitation heater for ultramicroscope |
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| CN201510437346.2A CN105067400B (en) | 2015-07-22 | 2015-07-22 | A kind of in situ quantitation heater for ultramicroscope |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105301027A (en) * | 2015-11-22 | 2016-02-03 | 北京工业大学 | Transmission/scanning electron microscope mechanical-thermal coupling field loaded in-situ experimental platform |
| 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 |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101017123A (en) * | 2007-03-02 | 2007-08-15 | 北京工业大学 | Method for eliminating electric charging effect of insulating ceramic sample by heating |
| 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 |
| CN102539213A (en) * | 2012-02-15 | 2012-07-04 | 西北工业大学 | Preparation method for transmission electron microscope (TEM) specimen of cadmium zinc tellurium (CdZnTe) and metal interface |
| US8258473B2 (en) * | 2010-11-12 | 2012-09-04 | Nanotem, Inc. | Method and apparatus for rapid preparation of multiple specimens for transmission electron microscopy |
| CN104319220A (en) * | 2014-10-14 | 2015-01-28 | 西安交通大学 | Quantitative nanometer heating table for electron microscope |
| US20150137003A1 (en) * | 2013-11-21 | 2015-05-21 | United Microelectronics Corp. | Specimen preparation method |
-
2015
- 2015-07-22 CN CN201510437346.2A patent/CN105067400B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101017123A (en) * | 2007-03-02 | 2007-08-15 | 北京工业大学 | Method for eliminating electric charging effect of insulating ceramic sample by heating |
| 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 |
| CN102539213A (en) * | 2012-02-15 | 2012-07-04 | 西北工业大学 | Preparation method for transmission electron microscope (TEM) specimen of cadmium zinc tellurium (CdZnTe) and metal interface |
| US20150137003A1 (en) * | 2013-11-21 | 2015-05-21 | United Microelectronics Corp. | Specimen preparation method |
| CN104319220A (en) * | 2014-10-14 | 2015-01-28 | 西安交通大学 | Quantitative nanometer heating table for electron microscope |
Non-Patent Citations (1)
| Title |
|---|
| 田琳等: "聚焦离子束在微纳尺寸材料力学性能研究中的应用", 《中国材料进展》, vol. 32, no. 12, 31 December 2013 (2013-12-31), pages 706 - 715 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105301027A (en) * | 2015-11-22 | 2016-02-03 | 北京工业大学 | Transmission/scanning electron microscope mechanical-thermal coupling field loaded in-situ experimental platform |
| 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 |
| 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 |
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