CN206223570U - A kind of Electronic Speculum power coupling test device in situ for macroscopical sample - Google Patents
A kind of Electronic Speculum power coupling test device in situ for macroscopical sample Download PDFInfo
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- CN206223570U CN206223570U CN201621190157.6U CN201621190157U CN206223570U CN 206223570 U CN206223570 U CN 206223570U CN 201621190157 U CN201621190157 U CN 201621190157U CN 206223570 U CN206223570 U CN 206223570U
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Abstract
The utility model discloses a kind of Electronic Speculum power coupling test device in situ for macroscopical sample, quantitative mechanical test module, the mechanics controller for controlling quantitative mechanical test module including heating sample base, temperature controller, specimen holder, pressure head, the power for measuring pressure head and displacement, wherein quantify mechanical test module to be integrated on specimen holder, heating sample base is detachable；If heating sample base includes matrix, wire, heat insulation, warm table, heating test resistance and dry-eye disease fixing tooth pin, the device at high temperature to carrying out the mechanical tests such as in situ quantitation compression, stretching by the micro/nano-scale sample of macroscopical sample preparation, and can accurately measure the temperature and mechanical property of sample.
Description
Technical field
The utility model belongs to electron microscope accessory and nano material in-situ measuring study field, is related to a kind of for grand
See the Electronic Speculum power coupling test device in situ of sample.
Background technology
Electron microscope (in-situ TEM) technology in situ refers to change by electron microscope and its specimen holder
Make, other external drives, such as power, heat, electricity, and real-time monitored sample in the presence of these external drives are applied to institute's sample
Pattern, the technology of the dynamic changing process of structure.In numerous existing electron microscopies in situ, in-situ mechanical is especially in situ fixed
Measure one's own ability is to obtain the most field of breakthrough achievement.In situ quantitation Experiments of Machanics can dynamically observe the dynamic of material in real time
Change procedure, and the one-to-one relationship of mechanical property and microstructure is obtained, for research material microdeformation mechanism is provided
Valuable help.
The existing device that in situ quantitation Mechanics Performance Testing is carried out in Electronic Speculum can be divided into active and passive type two
Major class.Active type device is integrated with mechanical test module in itself, and sample is integrated on a single die with mechanical test module, every time
Whole chip is changed during experiment.This device is relatively costly due to mechanical test module making, is easily damaged in sample transfer process
It is bad, and every time using being preceding required for individually being calibrated, and calibration needs to be carried out in the state of no sample, thus application compared with
It is few.Passive type device mechanical test module is integrated on specimen holder, and experiment every time only need to change sample part.This device mechanics
Test module can be reused, and test data confidence level is higher, and experimental cost is relatively low, and once experiment can be to multiple samples
Product are tested, therefore are widely used, and passive type mechanics test device common at present is the PI of Hysitron companies of the U.S.
95 series of samples bars, the pressure head of the specimen holder is connected on three class control device (Mechanical course coarse adjustment, piezoelectric ceramics fine tuning, power/position
Displacement sensor accurate adjustment and measurement), can carry out accurate adjustment to the position of pressure head, and the power that can be subject to pressure head and displacement are entered
Row is accurately controlled and measures.The series of samples bar has turned into the main flow instrument of international in situ quantitation mechanics study at present.
Tested by calculating simulation and macroscopic material it has been proved that at high temperature, the mechanical behavior and its texturing machine of material
System can change, but wherein still have many key scientific problems to have to be explained.For example, the metal of cold deformation is heat treated
Usually occur dynamic recrystallization phenomenon also usually occur in recrystallization phenomenon, then metal hot-working in journey, these phenomenons are tight
The development of metal working process is govern again, but lacks the understanding of system always to its microcosmic mechanism.Therefore, in the urgent need to one kind
The device of in situ quantitation power coupling test can be entered to carry out at high temperature to block sample under Electronic Speculum.
But, existing passive type in-situ mechanical test device can only be tested at room temperature mostly, and lack high temperature
The ability of test.A kind of only device for carrying out the quantitative mechanical test of high temperature is that Hysitron companies add on the market at present
Hot sample base, this sample base is made by quartz glass, and heater strip micro fabrication is integrated in into heating bottom
Seat front end.But there is problems with this heated base：From processing technology, due to quartz glass processing difficulties, machining accuracy
It is low, be difficult to be miniaturized, it is this heating sample base cost of manufacture it is high, manufacturer's price is up to 700 dollars of a piece of, use cost poles
It is high.From design, this heated base heating region is the thick heat blocks of 2500um 500um long 500um wide, heats volume mistake
Greatly, cause sample thermal drift huge, generally require to wait the time of dozens of minutes just to make sample after sample temperature is changed in experiment
Product thermal drift reaches stabilization, has a strong impact on experimentation；Simultaneously as heating volume is excessive, to avoid other positions of specimen holder
It is heated and causes more serious thermal drift, the temperature of heating region is strictly limited within 400 DEG C, and this temperature range is simultaneously
The demand of actual experiment can not be met.Upper from using, this heated base can only be by silicon tapered beam (Silicon wedge) sample
The end face of heated base is bonded at special bonding agent, due to the requirement of the homocentric height of transmission electron microscope, sample part on tapered beam
Position is it is essential to ensure that in the error range of 100um, this process needs the pure manual operations under light microscopic, due to hand tremor etc.
Problem, glues sample difficulty greatly, simultaneously as quartz material is more crisp in itself, is damaged easily in viscous sample and sample transfer process and added
Hot base, in actual use, sample once successfully could can be sent into Electronic Speculum, Success in Experiment by average every five experiments
Rate is extremely low, further improves experimental cost；Meanwhile, the sample that can be fixed on tapered beam only has various nano particles and thin
Film, and cannot be fixed using most laminar samples from macroscopical block sample preparation for actual Experiments of Machanics, this pole
The big application for limiting heated base.
In sum, due to existing heated base sample type limitation, thermal drift is big, temperature range is small, process and use
The shortcoming of high cost, can not try carrying out the thermal coupling of in situ quantitation power by the micro/nano-scale sample of macroscopical sample preparation under high temperature
The demand tested.
Utility model content
The purpose of this utility model is the shortcoming for overcoming above-mentioned prior art, there is provided a kind of original for macroscopical sample
Position Electronic Speculum power coupling test device, the device can carry out various to the micro/nano-scale sample of macroscopical sample preparation at high temperature
In situ quantitation mechanical test.
To reach above-mentioned purpose, the Electronic Speculum power coupling test device in situ for macroscopical sample described in the utility model
Quantitative mechanical test including heating sample base, temperature controller, specimen holder, pressure head, the power for measuring pressure head and displacement
Module, the mechanics controller for controlling quantitative mechanical test module, wherein quantitatively mechanical test module is integrated on specimen holder,
And the output shaft of quantitative mechanical test module is connected with pressure head；
If heating sample base includes matrix, wire, heat insulation, warm table, heating test resistance and dry-eye disease fixing tooth
Pin, offers the groove of up/down perforation on the end face of matrix, warm table is located in the groove, and warm table end face is hanging, plus
The other three end face of thermal station is connected by heat insulation with matrix, and the hanging one end of warm table is provided with some for fixing sample
The tooth pin of product, heating test resistance is located on warm table, and the exit for heating test resistance is drawn by wire through heat insulation surface
Go out to after the upper surface of matrix and be connected with temperature controller through external circuitry；Pressure head carries out quantitative mechanical test just to sample
When with sample directly contact.
Heat insulation is less than rigidity of the heat insulation along other directions along the rigidity in sample direction.
Two end face both sides of groove are equipped with safe bar.
Safe bar free end is much larger than distance of the tooth pin free end apart from the matrix plane of reference apart from the distance of the matrix plane of reference.
The upper surface of the upper surface of matrix, the upper surface of warm table and heat insulation is in the same plane, under heat insulation
The lower surface of surface and warm table is in the same plane.
Lower surface of the lower surface of warm table higher than matrix.
The utility model has the advantages that：
The design of sample placement tooth pin allows to directly by the nano-machine in focused ion beam in the utility model
Be transferred to macroscopical sample on heating specimen holder by hand, sample further can be processed into required pattern afterwards, is such as used to press
Contract nano-pillar, the I-shaped sample for extension test, the cantilever beam for crooked test of test etc., realizes stretching, compression
Nanometer mechanics etc. various functions are tested.The process of sample transfer and the focused ion beam extraction method (liftout of standard
Process it is) identical, pure placement sample by hand is needed relative to existing glass heated base, the precision that sample is placed is higher, sample
Be prepared into that power is higher, while can be processed in multiple mechanics samples and each heating sample base on each sample for extracting
Multiple tooth pins are provided with, multiple extraction samples can be placed, so as to greatly improve the efficiency of experiment, reduce experimental cost.In addition, plus
Heat insulation is provided between thermal station and matrix, heating region small volume in warm table, so as to the thermal drift of sample is greatly reduced, side
Just under high temperature sample mechanical property test, while realizing heat-insulated between specimen holder and sample, the heating in the utility model
Platform can be warmed up to more than 1000 DEG C of high temperature without causing the temperature change of specimen holder other parts, thus sample heating temperature
Degree scope is larger.In experiment, the motion of pressure head is controlled by mechanics controller, measuring pressure head by mechanical test module is subject to
Power, so as to realize that the micro/nano-scale sample at high temperature to macroscopical sample preparation carries out in situ quantitation mechanical test.
Further, the both ends of the surface of groove are provided with safe bar, prevent external impact and make specimen breakdown.
Further, the lower surface of warm table prevents from colliding sample and damaging sample from below higher than the lower surface of matrix
Wound.
Brief description of the drawings
Fig. 1 is structural representation of the present utility model；
Fig. 2 is the enlarged drawing of the part of warm table 4 in Fig. 1；
Fig. 3 is the structural representation that the utility model is arranged on specimen holder 201；
Fig. 4 is schematic cross-section of the present utility model；
Fig. 5 is power thermal coupling test philosophy schematic diagram of the present utility model.
Wherein, 1 for heating sample base, 2 be wire, 3 be heat insulation, 4 be warm table, 5 be heating test resistance, 6 be
Tooth pin, 7 be sample, 8 be safe bar, 9 for heating sample base fixing hole, 101 are matrix, 201 are specimen holder, 202 to fix
Screw, 211 be pressure head, 212 be mechanical test module, 210 be mechanics controller, 200 be temperature controller.
Specific embodiment
The utility model is described in further detail below in conjunction with the accompanying drawings：
With reference to Fig. 1, Fig. 3, the Electronic Speculum power coupling test device in situ for macroscopical sample described in the utility model, bag
Include determining for heating sample base 1, temperature controller 200, specimen holder 201, pressure head 211, the power for measuring pressure head 211 and displacement
Measure one's own ability and learn test module 212, the mechanics controller 210 for controlling quantitative mechanical test module 212, wherein quantitatively mechanical test
Module 212 is integrated on specimen holder 201, and the output shaft of quantitative mechanical test module 212 is connected with pressure head 211；Heating sample
Product base 1 is detachable；
With reference to Fig. 1, Fig. 2, heating sample base 1 includes matrix 101, wire 2, heat insulation 3, warm table 4, heating test electricity
If resistance 5 and dry-eye disease fixing tooth pin 6, the groove of up/down perforation is offered on the end face of matrix 101, warm table 4 is located at described recessed
In groove, the end face of warm table 4 is hanging, and the other three end face of warm table 4 is connected by heat insulation 3 with matrix 101, warm table
4 hanging one end are provided with some tooth pins 6 for fixing sample 7, and heating test resistance 5 is located on warm table 4, heating test
The exit of resistance 5 is after wire 2 is drawn out to the upper surface of matrix 101 through the surface of heat insulation 3 through external circuitry and temperature control
Device processed 200 is connected；Pressure head 211 just to sample 7, with the directly contact of sample 7 when carrying out quantitative mechanical test.Two ends of groove
Face both sides are equipped with safe bar 8.The free end of safe bar 8 is much larger than the free end distance of tooth pin 6 apart from the distance of the matrix plane of reference 100
The distance of the matrix plane of reference 100.
With reference to Fig. 4, the upper surface of the upper surface, the upper surface of warm table 4 and heat insulation 3 of matrix 101 is generally aligned in the same plane
On, the lower surface of heat insulation 3 and the lower surface of warm table 4 are in the same plane.The lower surface of warm table 4 is higher than matrix 101
Lower surface.The heating test resistance 5 is made by platinum, tungsten or molybdenum.The material of the heat insulation 3 is silica.
With reference to Fig. 5, the sample 7 in the utility model is fixed on tooth pin 6, in the making of sample 7, can be by macroscopical sample
Product are first fixed on tooth pin, and then macroscopical sample is processed into the sample of various shapes again, for example, for the nanometer of compression verification
Post, the I-shaped sample 7 etc. for extension test are straight with pressure head 211 by sample 7 by mechanics controller 210 during mechanical test
Contact, realizes the nanometer mechanics test of various functions such as stretching, compression.To ensure the reliability of Mechanical Data, the edge of heat insulation 3
The rigidity in the direction of sample 7 is less than rigidity of the heat insulation 3 along other directions.
With reference to Fig. 3 and Fig. 5, test philosophy of the present utility model is：
Sample 7 is heated using the Joule heat for heating test resistance 5, at the same using heat the resistance of test resistance 5-
Temperature relation measures the temperature of heating test resistance 5 in real time, due to the excellent thermal insulation of heat insulation 3 and warm table 4 is excellent leads
Hot, the temperature including the whole warm table 4 including tooth pin 6 can be regarded as and be uniformly distributed, thus can be according to heating test resistance 5
Temperature estimation sample 7 temperature, accurate closed loop control can be carried out to the temperature of sample 7 using external temperature controller 200
System.During mechanical test, pressure head 211 is directly contacted with sample 7, can be read by mechanical test module 212 and mechanics controller 210
Go out the displacement of the power and pressure head 211 that are subject on pressure head 211, so as to obtain the power and the displacement that are subject on sample 7.Carry out power thermal coupling
During test, sample 7 is heated to given temperature T first with temperature controller 200, recycles pressure head 211 to quantify sample 7
Mechanical test, so as to obtain the Mechanical Data at high temperature of sample 7.
Claims (6)
1. a kind of Electronic Speculum power coupling test device in situ for macroscopical sample, it is characterised in that including heating sample base
(1), the quantitative power of temperature controller (200), specimen holder (201), pressure head (211), the power for measuring pressure head (211) and displacement
Learn test module (212), the mechanics controller (210) for controlling quantitative mechanical test module (212), quantitative mechanical test mould
Block (212) is integrated on specimen holder (201), and the output shaft of quantitative mechanical test module (212) is connected with pressure head (211)；
Heating sample base (1) includes matrix (101), wire (2), heat insulation (3), warm table (4), heating test resistance (5)
And if dry-eye disease fixing tooth pin (6), the groove of up/down perforation is offered on the end face of matrix (101), warm table (4) is positioned at described
In groove, warm table (4) end face is hanging, and the other three end face of warm table (4) passes through heat insulation (3) and matrix (101) phase
Connection, hanging one end of warm table (4) is provided with some tooth pins (6) for fixing sample (7), heats test resistance (5) position
In on warm table (4), the exit of heating test resistance (5) is drawn out to matrix by wire (2) through heat insulation (3) surface
(101) it is connected with temperature controller (200) through external circuitry behind upper surface, pressure head (211) is just to sample (7).
2. the Electronic Speculum power coupling test device in situ for macroscopical sample according to claim 1, it is characterised in that every
Hot block (3) is less than rigidity of the heat insulation (3) along other directions along the rigidity in sample (7) direction.
3. the Electronic Speculum power coupling test device in situ for macroscopical sample according to claim 1, it is characterised in that recessed
Two end face both sides of groove are equipped with safe bar (8).
4. the Electronic Speculum power coupling test device in situ for macroscopical sample according to claim 1, it is characterised in that peace
Full bar (8) free end is much larger than tooth pin (6) free end apart from the matrix plane of reference (100) apart from the distance of the matrix plane of reference (100)
Distance.
5. the Electronic Speculum power coupling test device in situ for macroscopical sample according to claim 1, it is characterised in that base
The upper surface of the upper surface, the upper surface of warm table (4) and heat insulation (3) of body (101) is in the same plane, heat insulation (3)
Lower surface and warm table (4) lower surface it is in the same plane.
6. the Electronic Speculum power coupling test device in situ for macroscopical sample according to claim 1, it is characterised in that plus
Lower surface of the lower surface of thermal station (4) higher than matrix (101).
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| Application Number | Priority Date | Filing Date | Title |
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| CN201621190157.6U CN206223570U (en) | 2016-11-04 | 2016-11-04 | A kind of Electronic Speculum power coupling test device in situ for macroscopical sample |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201621190157.6U CN206223570U (en) | 2016-11-04 | 2016-11-04 | A kind of Electronic Speculum power coupling test device in situ for macroscopical sample |
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| CN206223570U true CN206223570U (en) | 2017-06-06 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110044700A (en) * | 2019-04-26 | 2019-07-23 | 北京工业大学 | Transmission electron microscope in-situ liquid environmental mechanics test platform |
| CN110926974A (en) * | 2019-11-27 | 2020-03-27 | 北京大学 | Method for testing mechanical property of small sample |
| CN111272549A (en) * | 2020-01-31 | 2020-06-12 | 浙江大学 | Sample loading method and sample clamp for transmission electron microscope in-situ pressure test |
| CN111272548A (en) * | 2020-01-31 | 2020-06-12 | 浙江大学 | In-situ pressure experiment system for transmission electron microscope and sample preparation method |
| CN113237733A (en) * | 2021-05-14 | 2021-08-10 | 东南大学 | In-situ force thermoelectric multi-field coupling test chip and preparation method thereof |
| CN113237734A (en) * | 2021-05-14 | 2021-08-10 | 东南大学 | High-precision in-situ mechanical test chip and preparation method thereof |
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2016
- 2016-11-04 CN CN201621190157.6U patent/CN206223570U/en active Active
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110044700A (en) * | 2019-04-26 | 2019-07-23 | 北京工业大学 | Transmission electron microscope in-situ liquid environmental mechanics test platform |
| CN110044700B (en) * | 2019-04-26 | 2024-04-12 | 北京工业大学 | Transmission electron microscope in-situ liquid environment mechanical test platform |
| CN110926974A (en) * | 2019-11-27 | 2020-03-27 | 北京大学 | Method for testing mechanical property of small sample |
| CN111272549A (en) * | 2020-01-31 | 2020-06-12 | 浙江大学 | Sample loading method and sample clamp for transmission electron microscope in-situ pressure test |
| CN111272548A (en) * | 2020-01-31 | 2020-06-12 | 浙江大学 | In-situ pressure experiment system for transmission electron microscope and sample preparation method |
| CN111272548B (en) * | 2020-01-31 | 2022-03-11 | 浙江大学 | In-situ pressure experiment system for transmission electron microscope and sample preparation method |
| CN111272549B (en) * | 2020-01-31 | 2022-04-22 | 浙江大学 | Sample loading method and sample clamp for transmission electron microscope in-situ pressure test |
| CN113237733A (en) * | 2021-05-14 | 2021-08-10 | 东南大学 | In-situ force thermoelectric multi-field coupling test chip and preparation method thereof |
| CN113237734A (en) * | 2021-05-14 | 2021-08-10 | 东南大学 | High-precision in-situ mechanical test chip and preparation method thereof |
| CN113237734B (en) * | 2021-05-14 | 2022-03-01 | 东南大学 | High-precision in-situ mechanical test chip and preparation method thereof |
| CN113237733B (en) * | 2021-05-14 | 2022-03-01 | 东南大学 | In-situ force thermoelectric multi-field coupling test chip and preparation method thereof |
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