CN105990078B - The double specimen holders that incline of transmission electron microscope original position low-and high-frequency fatigue - Google Patents
The double specimen holders that incline of transmission electron microscope original position low-and high-frequency fatigue Download PDFInfo
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Abstract
The double specimen holders that incline of transmission electron microscope original position low-and high-frequency fatigue, it is main to include holding handle, specimen holder, sample rod head end and sample loading stage；Sample loading stage is mainly made of two loading units and connecting portion, and loading unit is symmetrically fixed on connecting portion both ends, and having between two loading units allows its close to each other or be located remotely from each other deformation gap；Loading unit includesAxis, fatigue loading part and sample clamping part；Sample rod head end set actuator, actuator withAxis is in close contact, when actuator moves to the second position from first position,One angular travel of axis stepping；When actuator resets to first position from the second position,Axis is fixed；Actuator moves to the second position and reset to first position from the second position from first position forms a period of motion,Rotational angle=N* of axis, wherein N is the number of the period of motion.The present invention have can realize that sample existsThe maximum angle that verts of axis is more than ± 30oThe advantages of.
Description
Technical field
The present invention relates to the component of transmission electron microscope, the double shaft tilting sample of particularly a kind of transmission electron microscope
Product bar.
Technical background
Transmission electron microscope（Transmission Electron Microscope, hereinafter referred to as TEM）It is a kind of use
In material microstructure characterization large-scale experimental device, can simultaneously analysis of material microcell tissue morphology, crystal structure, composition
Element etc..Its image-forming principle is that high-power electron beam penetrates sample, and transmission electron beam is collected through over-focusing and amplification using detector
Signal is simultaneously imaged.Modern high resolution transmission electron microscopy can usually accomplish atomic resolution, and especially nearly 5 years rapid
The spherical aberration correcting technology of development makes the limiting resolution of TEM reach 50 pm.However it is often difficult to reach instrument in actual test
Limiting resolution.Main reason is that experimental result is not only limited by TEM performances itself, it is often more important that depending on sample feelings
Condition.One of essential condition is crystal orientation of the sample relative to incident beam.For TEM high-resolution imagings, only
Have and work as the projection that electron beam can just show corresponding atom periodic arrangement along a certain crystallographic direction incidence of sample, so as to obtain
Atomic lattice arranges image namely atomic resolution.It is real for how enabling incident beam parallel with Sample crystals direction
The basic premise of existing TEM high-resolution imagings.Usually there are two types of approach：First, fixed sample is motionless, and fascinate electron beam incident angle
Degree, makes electron beam parallel with a certain crystallographic direction of sample；Second, stationary electron beams, fascinate sample so that a certain crystal of sample
Direction parallel electron beam.The first approach is due to being related to the system reform to TEM electron-optical circuits and electron beam fascinates range
Limited and less application.For common technology route mainly using second of approach, this requires load the device of sample to have at present
It fascinates function.
The device for loading sample generally includes two parts, and a part is the sample chamber of TEM, also referred to as angle measurement platform；Another portion
It is divided into specimen holder.TEM sample is fixed on sample club head, and specimen holder is inserted into angle measurement platform.The angle measurement platform of TEM is generally configured with around sample
The function of bar axial-rotation namely so-calledAxis verts.Can sample be realized by verting for angle measurement platform in this wayAxis verts.
However for spatial orientation, verting for direction can not often realize that a certain crystallographic direction of sample is parallel with electron beam.
Also need to have sample surround perpendicular toAxisAxis verts function.The partial function can only be realized by specimen holder.
I.e. specimen holder must be provided with some tumblers and realize that sample existsAxis verts.Fig. 1 illustrates the original of verting of TEM sample bar
Reason.The eccentric crankshaft or connecting rod on head are driven by the vertical shaft for wearing entire sample club shaft A, it will be around the rotation in specimen holder axle center
Be changed into specimen cup B flexion-extension movement, so as to fulfill sample aroundAxis C's verts.
Simultaneously with the development of scientific research, requirement of experiment can not be met by TEM carrying out simple High Resolution Observations.
There is an urgent need to carry out fatigue experiment in situ in TEM to disclose the machine of fatigue of materials failure for fatigue failure phenomenon in a large amount of engineering
System.This just puts forward higher requirements the specimen holder of TEM, can not only realize double shaft tilting, and can be provided simultaneously with fatigue loading work(
Energy.
The specimen holder that can have TEM loading functions in situ at present mainly has three classes：The first kind, the production of Gatan companies of the U.S.
654 original position stretching uniclinal specimen holders of Gatan；Second class, the STM/TEM nanometers of Nanofactory companies of Sweden production are single
Body uniclinal specimen holder；Third class, the PI95 nano impress uniclinal specimen holders that Hysitron companies of the U.S. produce.
Principle design drawing such as attached drawing 2 and Fig. 3 of the Gatan654 original position stretching uniclinal specimen holders of Gatan companies of U.S. production
Shown, operation principle is material can be fixed on drawing stand head.Drawing stand head one end is movable and connects with steel cable inside bar
It connects, steel cable other end connection step micro motor.Micro machine is driven to can control the movement of drawing stand one end so as to pull sample, to examination
Sample realizes the deformation of different displacements.The specimen holder can realize the original position stretching in TEM, by the tension and relaxation that control motor
It is expected to realize the drawing pulling fatigue experimental of low frequency.But since motor tenses the lag intrinsic with relaxation, it can not realize high frequency
Draw pulling fatigue experimental.And the specimen holder does not have double shaft tilting function, TEM angle measurements platform can only be relied on to realize verting for a axis.Cause
This certain crystallographic direction parallel electron beam for being difficult to be adjusted to sample of interest region and realize atom level full resolution pricture shoot
Condition.
Nanofactory companies of Sweden production STM/TEM nano single uniclinal specimen holders operation principle be by
Piezoelectric ceramic tube drives a probe motion, if nanotube sample can be fixed on to the fixing end of probe and opposite side, is expected to realize
The repeated tension and compression test of high and low frequency.But due to its flexible loading characteristic, size is only applicable in the pole of 100 below nm
Thin nano wire.More crucially the specimen holder does not have double shaft tilting function yet, TEM angle measurements platform can only be relied on to realize inclining for a axis
Turn.Atom level full resolution pricture is realized therefore, it is difficult to be adjusted to a certain crystallographic direction parallel electron beam in sample of interest region
Shooting condition.
The PI95 nano impress uniclinal specimen holders that Hysitron companies of the U.S. produce and Nanofactory companies of Sweden
STM/TEM nano single uniclinal specimen holders are similar and are driven by piezoelectric ceramics, and probe only is changed into Buddha's warrior attendant
Stone pressure head is simultaneously attached to force snesor, can realize the repeated tension and compression test of high and low frequency.The similary specimen holder does not have double yet
Axis verts function, TEM angle measurements platform can only be relied on to realizeAxis verts.Therefore, it is difficult to be adjusted to a certain of sample of interest region
Crystallographic direction parallel electron beam and realize atom level full resolution pricture shooting condition.
It is comprehensive that Chinese patent 201110145305.8 discloses a kind of power in situ of used in transmission electron microscope double shaft tilting, electrical property
Close test sample bar（As shown in Figure 4）, main to include holding handle, specimen holder, sample head front end 3 ', sensor microscope carrier 4 ' passes through position
Two support shafts 5 ' in 3 ' two inside of sample head front end are fixed on sample head front end 3 ', around support shaft 5 ' perpendicular to sample
It verts in the plane of head（I.e. around Y-axis rotation ± 30o）, on the wall of 3 both sides of sample head front end, it is symmetrically distributed with from Electronic Speculum
The conducting wire I6 ' that outside is introduced by specimen holder, and be connected with the queue electrode I7 ' being distributed on 3 ' two side of sample head front end,
The other end of conducting wire I6 ' is connected on the electrode interface held on handle, is connected by electrode interface with Electronic Speculum external equipment.Queue
The position of electrode I7 ' is that line is symmetrically distributed on the two side of sample head front end 3 ' centered on support shaft 5 '.Sensor microscope carrier
4 ' rotation be by be located at the Y-axis of its tail portion vert driver 9 ' drive.In being with support shaft 5 ' on sensor microscope carrier 4 '
Heart line makes a groove 10 ', and groove 10 ' is a through-hole, and there is support in lower part along sensor is supported, and the thickness of sensor sets
It counts into and it to be put into groove 10 ' in plane where upper surface and TEM e-book focusing center are generally aligned in the same plane afterwards, make TEM
Electron beam is by the gap on sensor and groove 10 ' and focuses on the sample of sensor upper surface.
The shortcomings that this specimen holder, is：1st, driver is verted by being set to the Y-axis of sensor microscope carrier tail portion to drive
Sensor microscope carrier around Y-axis rotation, Y-axis vert driver include shaft, moving block and connection sensor microscope carrier connecting rod, shaft
When being rotated with moving block, connecting rod raising or reduction so as to which sensor microscope carrier one end be driven to be raised and lowered, realize that sensor carries
Platform verts around Y-axis, and there are the shortcomings that the volume of driving mechanism is big, and transmission parts quantity is more for this type of drive.
2nd, the loading of sample is：Line makes a groove centered on support shaft on sensor microscope carrier, which is one
There are support in a through-hole, lower part along supporting sensor；Sensor is put into groove, sensor is fixed on sensor with tabletting
On microscope carrier, it is a pair of that the queue electrode III in tabletting is located at the queue electrode II mono- made on the electrode and sensor below tabletting
It should be connected, the depth of sensor thickness and groove and TEM Electron Beam Focusings center are in the same plane；Sensor microscope carrier
A through-hole I is made close to the vert position of driver of Y-axis far from support shaft, through-hole I ensures that sensor microscope carrier is revolved around Y-axis
It will not be contacted when turning and when specimen holder is integrally rotated around X-axis with the pole shoe of Electronic Speculum.As it can be seen that in addition to loading sample on sensor
Other than the space of product, it is also necessary to there is the space of setting electrode, and tabletting will push down sensor, the area of tabletting is obviously greater than biography
Sensor area, and sensor microscope carrier not only needs the space in the space, also through-hole I that accommodate tabletting, it follows that sensor
The area of microscope carrier will be much larger than the area of sample.The Y-axis driver that verts is the entire sensor microscope carrier of driving to reach the sample that verts
Purpose, and the height space in specimen holder is limited, usually only 2 mm, therefore cause sample in the maximum angle that verts of Y-axis
Be difficult to be more than30 oThe shortcomings that.
Invention content
In order to overcome existing specimen holder that can not realize in Y-axis（I.e.Axis）It verts or sensor microscope carrier is excessive causes to incline
Turn maximum angle and be difficult to be more than ± 30oThe shortcomings that, it can realize that sample exists the present invention provides one kindThe maximum angular of verting of axis
Degree is more than ± 30oThe double specimen holders that incline of transmission electron microscope original position low-and high-frequency fatigue.
The double specimen holders that incline of transmission electron microscope original position low-and high-frequency fatigue, it is main to include holding handle, sample club body, sample
Rod head end and the sample loading stage for loading sample, sample loading stage withAxis is fixed,Axis is rotatably installed on sample
Rod head end；
It is characterized in that：Sample loading stage is mainly made of two loading units and connecting portion, and loading unit is symmetrically fixed on
Connecting portion both ends, having between two loading units allows its close to each other or is located remotely from each other deformation gap；Each loading unit includes
Respective b axis, fatigue loading part and sample clamping part,Axis and fatigue loading part are fixed respectively with sample clamping part；Sample fills
When being sandwiched in sample loading stage, the both ends in sample across the deformation gap and sample are separately fixed on a sample clamping part；
The setting driving of sample rod head endThe actuator of axis rotated stepwise, actuator and b axis are in close contact, actuator from
When first position moves to the second position,One angular travel of axis stepping；Actuator resets to first from the second position
When putting,Axis is fixed；Actuator moves to the second position from first position and resets to first position composition one from the second position
A period of motion,Rotational angle=N* of axis, wherein N is the number of the period of motion.
Further, fatigue loading part loads for piezoelectric ceramic piece or made of magnetostriction materials piece.
Further, the fixed block that connecting portion has U-type groove for one, loading unit are symmetrical arranged along U-type groove centerline axis, fatigue
Loaded member and the outer end wall of fixed block are fixed.
Further, when actuator moves to the second position from first position, actuator withSliding friction is generated between axis
Power makesAxis follows actuator to rotate；When actuator resets to the speed of first position from the second position and resets actuatorAxis
Momentum close to constant.
Further, actuator is pressed in by hold-down mechanismAxis, hold-down mechanism include tabletting, fixed screw and spring,
Fixed screw is fixed across tabletting with sample rod head end, and fixed screw has multiple, one spring of socket, bullet on each fixed screw
Between sample rod head end and tabletting, actuator is fixed in tabletting spring, and tabletting makes actuator be pressed in b axis.
Further, actuator mainly includes driving signal generator and piezoelectric ceramic piece or magnetostriction materials.
The advantage of the invention is that：
1st, b axis and fatigue loading part are fixed, and are pushed by actuatorAxis stepwise motion, then can be by fatigue loading part
Width makes the equivalent width with sample, and the size of sample loading stage is small, so as to obtain the angle of inclination space of bigger.
2nd, using piezoelectric ceramic piece or by magnetostriction materials as fatigue loading part, the electricity of the voltage signal of loading is controlled
Pressure and frequency are the loading force of controllable fatigue loading part, are quick on the draw and accuracy is high.
3rd, make every timeShaft rotation moves a fixed low-angle stroke, such as unit angle, using step-by-step movement accumulative effect come
Reaching makesAxis achievees the purpose that big rotational travel, and the angle rotated needed for each b axis is small, so that actuator each period
Driving trip it is short, have in the short space for being placed into transmission electron microscope so as to enable actuator volume sufficiently small
Possibility.
4th, by the use of piezoelectric ceramic piece or magnetostriction materials as actuator, by control actuator power-on time and
I.e. controllable actuator moved to the time of the second position from first position and reset to first from the second position dead electricity time
The time put, and actuator response is rapid；Only actuator and external driving signal generator need to be connected with conducting wire, driven
Moving part it is small, it is simple in structure, can be placed into the short space of transmission electron microscope.
Description of the drawings
Fig. 1 is the schematic diagram that TEM sample bar verts in the prior art.
Fig. 2 is the decomposition diagram of the Gatan654 original position stretching uniclinal specimen holders of Gatan companies of U.S. production.
Fig. 3 is the principle design drawing of the Gatan654 original position stretching uniclinal specimen holders of Gatan companies of U.S. production.
Fig. 4 is the schematic diagram of the sample head front end of Chinese patent 201110145305.8.
Fig. 5 is the schematic diagram of the present invention.
Fig. 6 is the schematic diagram of sample loading stage.
Fig. 7 is the position side view that verts of sample rod head end.
Specific embodiment
As shown in figure 5, the double specimen holders that incline of transmission electron microscope original position low-and high-frequency fatigue, main to include holding handle 5, sample
Club body 4, sample rod head end 1 and the sample loading stage 2 for loading sample, sample loading stage 2 and b axis 9 are fixed,Axis with can
It is rotatably mounted to 4 head end of specimen holder.The signaling interface of specimen holder 4, which is set to, to be held on handle 5.
As shown in fig. 6, sample loading stage 2 is mainly made of two loading units A1, A2 and connecting portion 15, loading unit A1, A2
15 both ends of connecting portion are symmetrically fixed on, having between two loading units A1, A2 allows its close to each other or be located remotely from each other deformation
Clearance C；Each loading unit includes respectiveAxis 9, fatigue loading part 14 and sample clamping part 13,Axis 9 and fatigue loading part
14 fix respectively with sample clamping part 13；When sample is clamped in sample loading stage 2, sample is across the two of the deformation gap and sample
End is separately fixed on a sample clamping part 13.When two fatigue loading parts 14 move toward one another, deformation gap becomes smaller, sample
It is compressed.When two 14 counter motions of fatigue loading part, be located remotely from each other when, deformation gap becomes larger, and sample is stretched.Pass through change
The direction of motion of two fatigue loading parts realizes the loading of compressing force or drawing force to sample.
The setting driving of 4 head end of specimen holderThe actuator of 9 rotated stepwise of axis, actuator withAxis 9 is in close contact, driving
When part moves to the second position from first position,Axis 9 stepping, one angular travel；Actuator is reset to from the second position
During first position,Axis 9 is fixed；Actuator moves to the second position from first position and resets to first position from the second position
A period of motion is formed,Rotational angle=N* of axis 9, wherein N is the number of the period of motion.
Fatigue loading part 14 is made by piezoelectric ceramic piece or by magnetostriction materials.Fatigue loading part 14 passes through conducting wire and hand
Signaling interface connection on lever 5, signaling interface are connect with the source driving signal that driving fatigue loading part 14 moves.Drive signal
Source changes the direction of motion of the i.e. controllable fatigue loading part 14 in direction of voltage signal using voltage signal as drive signal, from
And it realizes and compressing force or drawing force is loaded to sample.
The fixed block that connecting portion 15 has U-type groove for one, loading unit are symmetrical arranged along U-type groove centerline axis 9, fatigue loading
Part 14 and the outer end wall of fixed block are fixed.
When actuator moves to the second position from first position, actuator withForce of sliding friction is generated between axis 9 to be made
Axis 9 follows actuator to rotate；When actuator resets to the speed of first position from the second position and resets actuatorAxis 9 moves
It measures close to constant.
Actuator 10 is pressed in by hold-down mechanismAxis 9, hold-down mechanism include tabletting 11, fixed screw 8 and spring 7,
Fixed screw 8 is fixed across tabletting with 4 head end of specimen holder, and fixed screw 8 has multiple, one bullet of socket on each fixed screw 8
Spring 7, spring 7 are located between 4 head end of specimen holder and tabletting 11, and actuator 10 is fixed in tabletting 11, and tabletting 11 makes actuator 10
It is pressed inAxis 9.Actuator 10 and hold-down mechanism, which are formed, to be drivenAxis rotated stepwiseAxis rotation system 3.
Actuator mainly includes driving signal generator and piezoelectric ceramic piece or magnetostriction materials.
The advantage of the invention is that：
1、Axis is fixed with fatigue loading part, and b axis stepwise motions are pushed by actuator, then can be by fatigue loading part
Width makes the equivalent width with sample, and the size of sample loading stage is small, so as to obtain the angle of inclination space of bigger.
2nd, using piezoelectric ceramic piece or by magnetostriction materials as fatigue loading part, the electricity of the voltage signal of loading is controlled
Pressure and frequency are the loading force of controllable fatigue loading part, are quick on the draw and accuracy is high.
3rd, make every timeShaft rotation moves a fixed low-angle stroke, such as unit angle, using step-by-step movement accumulative effect come
Reaching makesAxis achievees the purpose that big rotational travel, every timeThe angle rotated needed for axis is small, so that actuator is each all
The driving trip of phase is short, has in the short space for being placed into transmission electron microscope so as to enable actuator volume sufficiently small
Possibility.
4th, by the use of piezoelectric ceramic piece or magnetostriction materials as actuator, by control actuator power-on time and
I.e. controllable actuator moved to the time of the second position from first position and reset to first from the second position dead electricity time
The time put, and actuator response is rapid；Only actuator and external driving signal generator need to be connected with conducting wire, driven
Moving part it is small, it is simple in structure, can be placed into the short space of transmission electron microscope.
Content described in this specification embodiment is only enumerating to the way of realization of inventive concept, protection of the invention
Range is not construed as being only limitted to the concrete form that embodiment is stated, protection scope of the present invention is also and in art technology
Personnel according to present inventive concept it is conceivable that equivalent technologies mean.
Claims (6)
1. the double specimen holders that incline of transmission electron microscope original position low-and high-frequency fatigue, main to include holding handle, sample club body, specimen holder
Head end and the sample loading stage for loading sample, sample loading stage withAxis is fixed,Axis is rotatably installed on specimen holder
Head end；
It is characterized in that：Sample loading stage is mainly made of two loading units and connecting portion, and loading unit is symmetrically fixed on connection
Portion both ends, having between two loading units allows its close to each other or is located remotely from each other deformation gap；Each loading unit includes respective
'sAxis, fatigue loading part and sample clamping part,Axis and fatigue loading part are fixed respectively with sample clamping part；Sample is clamped in
During sample loading stage, the both ends in sample across the deformation gap and sample are separately fixed on a sample clamping part；
The setting driving of sample rod head endThe actuator of axis rotated stepwise, actuator withAxis is in close contact, and actuator is from the
When one position moves to the second position,One angular travel of axis stepping；Actuator resets to first position from the second position
When,Axis is fixed；Actuator moves to the second position and reset to first position from the second position from first position forms one
The period of motion,Rotational angle=N* of axis, wherein N is the number of the period of motion.
2. the double specimen holders that incline of transmission electron microscope original position as described in claim 1 low-and high-frequency fatigue, it is characterised in that：Fatigue
Loaded member is piezoelectric ceramic piece or piece is loaded made of magnetostriction materials.
3. the double specimen holders that incline of transmission electron microscope original position as claimed in claim 2 low-and high-frequency fatigue, it is characterised in that：Connection
The fixed block that portion has U-type groove for one, loading unit is symmetrical arranged along U-type groove centerline axis, fatigue loading part and fixed block it is outer
End wall is fixed.
4. the double specimen holders that incline of transmission electron microscope original position low-and high-frequency fatigue as described in one of claim 1-3, feature exist
In：When actuator moves to the second position from first position, actuator withForce of sliding friction is generated between axis to be madeAxis follows
Actuator rotates；When actuator resets to the speed of first position from the second position and resets actuatorThe momentum of axis is not close to
Become.
5. the double specimen holders that incline of transmission electron microscope original position as claimed in claim 4 low-and high-frequency fatigue, it is characterised in that：Driving
Part is pressed in by hold-down mechanismAxis, hold-down mechanism include tabletting, fixed screw and spring, and fixed screw passes through tabletting and sample
Product rod head end is fixed, fixed screw have it is multiple, on each fixed screw be socketed a spring, spring be located at sample rod head end with press
Between piece, actuator is fixed in tabletting, and tabletting is pressed in actuatorAxis.
6. the double specimen holders that incline of transmission electron microscope original position as claimed in claim 5 low-and high-frequency fatigue, it is characterised in that：Driving
Part mainly includes driving signal generator and piezoelectric ceramic piece or magnetostriction materials.
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| CN107576823A (en) * | 2017-09-05 | 2018-01-12 | 浙江大学 | Nanopositioner for transmission electron microscope sample bar |
| CN109725005B (en) * | 2017-10-27 | 2021-07-27 | 北京纳米能源与系统研究所 | Transmission electron microscope sample rod head and transmission electron microscope sample rod applying same |
| CN111257354B (en) * | 2018-11-30 | 2021-03-05 | 浙江大学 | Multi-degree-of-freedom sample rod |
| CN111257355B (en) * | 2018-11-30 | 2021-04-27 | 浙江大学 | Multi-degree-of-freedom sample rod with rotating shaft driving assembly |
| CN111638476B (en) * | 2020-04-28 | 2022-11-04 | 香港中文大学（深圳） | Electric transmission sample carrying structure and electric transmission sample carrying operation method |
| CN114199902B (en) * | 2021-10-26 | 2024-04-12 | 清华大学 | Sample carrying device for electron microscope |
| CN114203504B (en) * | 2021-11-23 | 2023-10-24 | 百实创(北京)科技有限公司 | Tilting structure of transmission electron microscope sample stage |
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| JP5798749B2 (en) * | 2011-01-24 | 2015-10-21 | 株式会社メルビル | Sample holder and sample holder driving device |
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| CN102262996A (en) * | 2011-05-31 | 2011-11-30 | 北京工业大学 | Comprehensive test sample rod for double-shaft tilting in-situ force and electric property of transmission electron microscope |
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