CN109827820A - A kind of in situ TEM sample preparation methods based on heating chip - Google Patents
A kind of in situ TEM sample preparation methods based on heating chip Download PDFInfo
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- 238000010438 heat treatment Methods 0.000 title claims abstract description 135
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 73
- 238000005464 sample preparation method Methods 0.000 title claims abstract description 29
- 239000011241 protective layer Substances 0.000 claims abstract description 119
- 238000010884 ion-beam technique Methods 0.000 claims abstract description 103
- 238000002360 preparation method Methods 0.000 claims abstract description 46
- 238000005530 etching Methods 0.000 claims description 51
- 238000005520 cutting process Methods 0.000 claims description 33
- 238000000151 deposition Methods 0.000 claims description 22
- 238000010894 electron beam technology Methods 0.000 claims description 22
- 230000008021 deposition Effects 0.000 claims description 20
- 238000012512 characterization method Methods 0.000 claims description 10
- 239000010410 layer Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 abstract description 37
- 238000005070 sampling Methods 0.000 abstract description 6
- 230000001737 promoting effect Effects 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 374
- 238000010586 diagram Methods 0.000 description 10
- 239000010949 copper Substances 0.000 description 9
- 230000005540 biological transmission Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004452 microanalysis Methods 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 238000012552 review Methods 0.000 description 2
- 238000000137 annealing Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000002164 ion-beam lithography Methods 0.000 description 1
- 239000006101 laboratory sample Substances 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000000386 microscopy Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
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Abstract
The invention discloses the in situ TEM sample preparation methods based on heating chip, comprising the following steps: initial sample and heating chip are separately fixed in plane and inclined-plane adjacent on prefabricated sample stage, transfers in FIB-SEM double-beam system and vacuumizes；Pt protective layer is deposited on initial sample surface using ion beam, obtains the initial sample for being deposited with Pt protective layer；The initial sample for being deposited with Pt protective layer is cut using ion beam, obtains the strip sample that cross section is triangle；Strip sample is shifted using manipulator and is fixed on the sample hole slot of heating chip；It adjusts the position of prefabricated sample stage and substep is carried out to strip sample using ion beam and be thinned, obtain the in situ TEM sample based on heating chip.The present invention carries out the preparation of TEM sample in situ using FIB-SEM double-beam system, it is only necessary to which single injected sampling enormously simplifies process flow, and simple and direct-viewing operation is conducive to the yield rate for promoting sample preparation.
Description
Technical field
The invention belongs to materialogy electronic micro-analysis field, it is related to a kind of In Situ Heating transmission electron microscope (TEM) sample
Preparation method, in particular to focused ion beam (FIB) processing method of a kind of in situ TEM sample based on heating chip.
Background technique
In situ TEM (TEM) characterization method can be used for analysis of material internal organizational structure variation with temperature rule,
Obtain the physics law that material microstructure changes with external environment.The TEM laboratory sample in situ of high quality is to carry out original position
The premise of TEM characterization.In Situ Heating TEM experiment is generally basede on In Situ Heating chip, needs sample to be fixed on chip, then subtract
Thin to hundred nanometers or less thickness.After the completion of sample preparation, chip is placed on the TEM sample bar with heating function, then carry out original
Position heating TEM characterization experiment.
Traditional TEM sample preparation method can be transferred to sample on copper mesh and carry out thinned, then carry out tem analysis table
Sign.The sample as made from the technique be placed on copper mesh edge carry out it is thinned, can not be by sample preparation to being laid in add in-place
On hot chip.Such as documents " review (the A review of of focused-ion-beam lithography method progress TEM sample preparation
Focused ion beam milling techniques for TEM specimen preparation) ", it is loaded in
" Micron " disclosed in 1999, Vol.30, No.3:197-204, and " utilizes focused ion beam to carry out transmission electron microscope sample preparation
New method (Novel scheme for the preparation of transmission electron microscopy
Specimens with a focused ion beam) ", it is loaded in " Journal of Vacuum Science&Technology
B ", disclosed in 1993, Vol.11, No.6:2021-2024.
Although at present there are also based on heating chip TEM sample preparation method in situ, multiple sample stages, repeatedly
Disengaging sample could be completed, and process is more complicated, sample directly cannot be transferred to heating chip, and then complete being thinned for sample.
Such as documents " quick preparation (the Convenient preparation of of high quality original position TEM Heating Experiment sample
high-quality specimens for annealing experiments in the transmission electron
Microscope) ", it is loaded in " Microscopy and Microanalysis ", 2014, Vol.20, No.6:1638-1645 institute
It is open.
In addition, also having document to disclose completes the transmission in situ based on heating chip using a sample stage and single injected sampling
The preparation method of electron microscopic sample, but there is also some problems.Such as sample needed for not using Pt to protect when ingressing and sampling,
It is easy to cause damage of the Ga ion implanting to sample, material especially sensitive to Ga ion implanting.The sample of these documents preparation
Product thickness is about 100nm, high/low atomic number material is needed for thinner TEM sample, such as 50nm, there is also difficulties.
From the point of view of intuitive, 100nm and 50nm difference is little, practical difficult in realization, below with semiconductor chip ruler
Very little development and change briefly explain its difficulty.Semiconductor chip industry, the 1 μm of technique of appearance in 1989 use 0.6 μm in 1993
Technique uses 0.18 μm of technique for 2000, uses within 2003 90nm technique, and realization 65nm technique in 2005 is realized for 2007
45nm technique, realization 32nm technique in 2009, the semiconductor technology of more microsize is also in lasting research and development.Lift semiconductor chip
The development example of size is primarily to explanation, size is smaller, and difficulty is bigger.What the present invention described prepares small TEM sample
Method is different with semiconductor microactuator small-size chips technique.
Therefore it needs to improve the TEM sample preparation method in situ based on heating chip, optimizes preparation flow, realize thinner
It is prepared by the integrated molding of high quality In Situ Heating TEM sample.
Summary of the invention
It is an object of the invention to overcome problems of the prior art, a kind of original position based on heating chip is provided
TEM sample preparation method simplifies preparation flow and realizes the integrated molding preparation of In Situ Heating TEM sample.
The present invention provides a kind of in situ TEM sample preparation methods based on heating chip, the preparation method packets
Include following steps:
A, initial sample and heating chip are separately fixed in plane and inclined-plane adjacent on prefabricated sample stage, then will be pre-
Sample preparation sample platform is transferred in FIB-SEM double-beam system and vacuumizes, wherein the planar inclination of the prefabricated sample stage is for 0 ° and oblique
Face inclination alpha is 23 °~65 °, and the angle β between the ion beam and electron beam of the FIB-SEM double-beam system is 45 °~55 °；
B, Pt protective layer is deposited on initial sample surface using ion beam, obtains the initial sample for being deposited with Pt protective layer；
C, the initial sample for being deposited with Pt protective layer is cut using ion beam, obtaining cross section is triangle
Strip sample；
D, the strip sample is shifted using manipulator and is fixed on the sample hole slot of the heating chip；
E, it adjusts the position of prefabricated sample stage and substep is carried out to the strip sample using ion beam and be thinned, be based on
Heat chip in situ TEM sample, wherein it is described based on heating chip in situ TEM thickness of sample d be 50~
55nm。
One embodiment of in situ TEM sample preparation methods according to the present invention based on heating chip, it is described prefabricated
The inclination angle of inclined plane α of sample stage is 45 °~50 °, angle β between the ion beam and electron beam of FIB-SEM double-beam system is 48 °~
52°。
One embodiment of in situ TEM sample preparation methods according to the present invention based on heating chip, in step A
In, the sample hole slot of the heating chip is set as orthogonal in the longitudinal direction with heating chip.
One embodiment of in situ TEM sample preparation methods according to the present invention based on heating chip, in step B
In, tilting prefabricated sample stage β keeps initial sample surface vertical with ion beam direction and carries out Pt protective layer on initial sample surface
Deposition obtain the initial sample for being deposited with Pt protective layer, the Pt protective layer with a thickness of 1~3 μm and length and width is
3~20 μm, wherein the length of the Pt protective layer is greater than the sample well groove width of the heating chip and is less than the sample well
Heat the distance between electrode in slot both sides.
One embodiment of in situ TEM sample preparation methods according to the present invention based on heating chip, the step
C includes following sub-step:
C-1: after deposition is complete, using ion beam the initial sample for being deposited with Pt protective layer Pt protective layer
Side end edge etch a deep trouth, the etching depth of the deep trouth is 8~12 μm, length is 8~12 μm, width 8
~12 μm；
C-2: by prefabricated sample stage reversed dip make the included angle X 23 between initial sample surface and ion beam direction~
43 °, the one side edge using ion beam in the Pt protective layer of the initial sample for being deposited with Pt protective layer carries out strip sample
The etching of a line is cut, and the etching depth of cut of the strip sample a line is 8~12 μm, length is 13~17 μm, wide
Degree is 3~5 μm；
C-3: same reversed dip makes between initial sample surface and ion beam direction after prefabricated sample stage is rotated 180 °
Included angle X be 23~43 °, using ion beam in the other side of the Pt protective layer of the initial sample for being deposited with Pt protective layer
Edge carries out the etching cutting of the another a line of strip sample, and the etching depth of cut of the another a line of strip sample is 8~12 μ
M, length is 13~17 μm, width is 3~5 μm, obtains the strip sample that cross section is triangle.
One embodiment of in situ TEM sample preparation methods according to the present invention based on heating chip, the step
D includes following sub-step:
D-1: it controls prefabricated sample stage and does not tilt and rotate clockwise pre- sample preparation in the case where overlooking along beam direction
90 ° of sample platform, one jiao that manipulator is protruded into and contacted the strip sample is deposited by Assisted by Ion Beam Pt by manipulator and length
Bar sample is soldered to together；
D-2: using ion beam along the end side of the Pt protective layer of the initial sample for being deposited with Pt protective layer
By the connection cutting between strip sample and initial sample, strip sample is proposed by the retraction of manipulator；
D-3: 90 ° of prefabricated sample stage is rotated clockwise in the case where overlooking along beam direction again, and is tilted prefabricated
Sample stage keeps heating chip surface vertical with beam direction, and strip sample is transferred to the sample of heating core on piece by mobile manipulator
Above sample wells slot and contact heating chip；
D-4: the connection realized between heating chip and strip sample is deposited by Assisted by Ion Beam Pt, recycles ion beam
Strip sample is simultaneously finally fixed on the sample hole slot of the heating chip by the connection of etching cutting machine hand and strip sample.
One embodiment of in situ TEM sample preparation methods according to the present invention based on heating chip, the step
E includes following sub-step:
E-1: the tilt angle of prefabricated sample stage is adjusted to θ and to heat between chip surface and ion beam direction be in
5 °~25 ° of angle γ, wherein θ=90- β-γ；
E-2: strip is carried out by the plus-minus of the tilt angle of the prefabricated sample stage and the adjustment of ion beam etching parameter
The removal of sample being thinned with final amorphous layer finally obtains the transmission in situ based on heating chip that thickness d is 50~55nm
Electron microscopic sample.
One embodiment of in situ TEM sample preparation methods according to the present invention based on heating chip, it is described to be based on
The in situ TEM sample of chip is heated when actually carrying out TEM characterization, the thickness d that sample is passed through by the electron beam of TEMTEM
=d/cos γ=1d~1.1d.
Compared with prior art, the present invention is only needed using the preparation process that FIB-SEM double-beam system carries out TEM sample in situ
Single injected sampling is wanted, process flow is enormously simplified, increases sample preparation efficiency；Sample preparation overall process simple and direct-viewing operation, is conducive to
Promote the yield rate of sample preparation；Electron beam penetration thickness when the thickness of final sample is observed close to TEM, sample quality are available
Effective guarantee.
Detailed description of the invention
Fig. 1 shows the in situ TEM sample preparation side according to an exemplary embodiment of the present invention based on heating chip
The flow chart of method.
Fig. 2 a shows the in situ TEM sample preparation according to an exemplary embodiment of the present invention based on heating chip
The structural schematic diagram of prefabricated sample stage in method, Fig. 2 b shows initial sample and heating chip is fixed on prefabricated sample stage
Position view, Fig. 2 c show the arragement construction schematic diagram of sample hole slot in heating chip.
Fig. 3 shows the in situ TEM sample preparation side according to an exemplary embodiment of the present invention based on heating chip
The structural schematic diagram of the initial sample of Pt protective layer is deposited in method.
Fig. 4 a shows the in situ TEM sample preparation according to an exemplary embodiment of the present invention based on heating chip
The structural schematic diagram of strip sample in method, Fig. 4 b show the main view of Fig. 4 a, and Fig. 4 c shows the top view of Fig. 4 a, Fig. 4 d
Show the schematic view of the front view of strip sample.
Fig. 5 a is the relative position schematic diagram of line and prefabricated sample stage when strip sample to be fixed to heating chip, Fig. 5 b
The overlooking structure diagram on strip sample to the sample hole slot of heating chip is welded for manipulator, Fig. 5 c is that strip sample is fixed
Schematic view of the front view on the sample hole slot of heating chip.
Fig. 6 shows the cross section structure signal of the in situ TEM sample based on heating chip obtained after distribution is thinned
Figure.
Fig. 7 a shows the microscopic appearance figure for depositing Pt protective layer in embodiment 1 in initial sample, and Fig. 7 b shows reality
It applies in example 1 and etches the microcosmic shape of a deep trouth in the side end edge for the Pt protective layer for being deposited with the initial sample of Pt protective layer
Looks figure, Fig. 7 c is shown in embodiment 1 to be grown in the one side edge for the Pt protective layer for being deposited with the initial sample of Pt protective layer
The microscopic appearance figure of sample a line etching cutting, Fig. 7 d are shown in embodiment 1 in the initial sample for being deposited with Pt protective layer
Another side edge of the Pt protective layer of product carries out the microscopic appearance figure of the another a line etching cutting of strip sample, and Fig. 7 e shows reality
It applies and adjusts the strip sample surfaces microscopic appearance figure vertical with ion beam direction in example 1, Fig. 7 f shows in embodiment 1 and deposits Pt
The microscopic appearance figure that manipulator and strip sample are welded together, Fig. 7 g show cutting in embodiment 1 and connect and take out length
The microscopic appearance figure of bar sample, Fig. 7 h, which is shown, to be transferred to strip sample in embodiment 1 above the sample hole slot of heating chip
Microscopic appearance figure, Fig. 7 i show in embodiment 1 realize strip sample be fixed to heating chip sample hole slot microcosmic shape
Looks figure.
Fig. 8 a to Fig. 8 c shows strip sample in embodiment 1 and carries out the thinned microscopic appearance figure of substep, and Fig. 8 d is shown
The microscopic appearance figure of TEM sample obtained in embodiment 1.
Fig. 9 a to Fig. 9 f respectively illustrates clapping under scanning transmission electron microscope for TEM sample obtained in embodiment 1
The angle of elevation annular dark field image of the different zones arrived.
Figure 10 a is shown in embodiment 2 in the side end edge for the Pt protective layer for being deposited with the initial sample of Pt protective layer
Edge etches the microscopic appearance figure of a deep trouth, and Figure 10 b shows in embodiment 2 and is being deposited with the initial sample of Pt protective layer
The one side edge of Pt protective layer carries out the microscopic appearance figure of strip sample a line etching cutting, and Figure 10 c is shown in embodiment 2
The another a line etching cutting of strip sample is carried out in another side edge for the Pt protective layer for being deposited with the initial sample of Pt protective layer
Microscopic appearance figure, Figure 10 d, which is shown, adjusts the strip sample surfaces microscopic appearance vertical with ion beam direction in embodiment 2
Figure.
Figure 11 a is shown in embodiment 3 in the side end edge for the Pt protective layer for being deposited with the initial sample of Pt protective layer
Edge etches the microscopic appearance figure of a deep trouth, and Figure 11 b shows in embodiment 3 and is being deposited with the initial sample of Pt protective layer
The one side edge of Pt protective layer carries out the microscopic appearance figure of strip sample a line etching cutting, and Figure 11 c is shown in embodiment 3
The microscopic appearance figure that manipulator and strip sample are welded together deposition Pt, Figure 11 d show cutting in embodiment 3 and connect simultaneously
The microscopic appearance figure of strip sample is taken out, Figure 11 e shows the sample well that strip sample is transferred to heating chip in embodiment 3
Microscopic appearance figure above slot, Figure 11 f show the sample hole slot for realizing that strip sample is fixed to heating chip in embodiment 3
Microscopic appearance figure.
Description of symbols:
1- plane, 2- initial sample, the inclined-plane 3-, 4- heating chip, 5- sample hole slot, 6-Pt protective layer, 7- electron beam,
8- ion beam, 9- strip sample, 10- manipulator, the prefabricated sample stage of 11-, 12-Pt solder joint, 13- heating chip part, 14- subtract
In situ TEM sample after thin.
Specific embodiment
All features disclosed in this specification or disclosed all methods or in the process the step of, in addition to mutually exclusive
Feature and/or step other than, can combine in any way.
Any feature disclosed in this specification unless specifically stated can be equivalent or with similar purpose by other
Alternative features are replaced.That is, unless specifically stated, each feature is an example in a series of equivalent or similar characteristics
?.
With reference to the accompanying drawing to the present invention is based on the in situ TEM sample preparation methods of heating chip to carry out specifically
It is bright.The present invention is that the FIB-SEM double-beam system for being 45~55 ° based on existing ion beam and electron beam angle β carries out, and the present invention is logical
Cross improved In Situ Heating TEM sample preparation method, it is only necessary to which single injected sampling can complete sample preparation, simplify sample system
Standby process, sample preparation quality are also higher.Be conducive to be promoted the sample preparation efficiency and characterization precision of In Situ Heating TEM experiment.
Fig. 1 shows the in situ TEM sample preparation side according to an exemplary embodiment of the present invention based on heating chip
The flow chart of method, as shown in Figure 1, an exemplary embodiment of the present invention, the in situ TEM based on heating chip
Sample preparation methods mainly include following multiple steps.
Step A:
Initial sample 2 and heating chip 4 are separately fixed in plane 1 and inclined-plane 2 adjacent on prefabricated sample stage 11, then
Prefabricated sample stage 11 is transferred in FIB-SEM double-beam system and is vacuumized.
Fig. 2 a shows the in situ TEM sample preparation according to an exemplary embodiment of the present invention based on heating chip
The structural schematic diagram of prefabricated sample stage in method, Fig. 2 b shows initial sample and heating chip is fixed on prefabricated sample stage
Position view, Fig. 2 c show the arragement construction schematic diagram of sample hole slot in heating chip.
As shown in Figure 2 a and 2 b, the prefabricated sample stage 11 in the present invention has plane 1 and inclined-plane 3 simultaneously, respectively at this
Initial sample 2 and heating chip 4 are placed on two faces and is fixed, i.e., initial sample 2 are fixed in plane 1 and on inclined-plane 3
Upper fixed heating chip 4.Wherein, the inclination angle of plane 1 is 0 °, and the inclination alpha on inclined-plane 3 is 23 °~65 °, preferably 45 °~50 °.?
That is, the tilt angle on inclined-plane 3 can be adjusted on the basis of 45 °~50 °, but maximum value needs to be less than θ, and θ is equipment behaviour
The inclined maximum angle of institute's energy during work, generally 65 °；Minimum value should be greater than particular value δ, δ be equal to ion beam direction with
The angle when angle of horizontal plane subtracts thinned between ion beam direction and heating chip, generally 23 °.
As shown in Figure 2 c, it sets the sample hole slot 5 for heating chip 4 to rectangular heating chip 4 in length direction
It is upper orthogonal.
Step B:
Pt protective layer is deposited on 2 surface of initial sample using ion beam, obtains the initial sample for being deposited with Pt protective layer.
Fig. 3 shows the in situ TEM sample preparation side according to an exemplary embodiment of the present invention based on heating chip
The structural schematic diagram of the initial sample of Pt protective layer is deposited in method.
Keep 2 surface of initial sample vertical with 8 direction of ion beam and in initial sample as shown in figure 3, tilting prefabricated sample stage β
2 surfaces carry out Pt protective layer 6 deposition obtain the initial sample for being deposited with Pt protective layer 6, wherein Pt protective layer with a thickness of 1
~3 μm and length and width are 3~20 μm.
Before the deposition, the sample preparation region that length is 3~20 μm and width is 3~20 μm, last TEM can first be chosen
Sample size is substantially equal to the size of the protective layer.Also, the length of Pt protective layer should be set greater than the sample of heating chip 4
5 width of hole slot and it is less than 5 both sides of sample hole slot heating the distance between electrode (not shown), width dimensions are preferably at 6~12 μm
Interior appropriateness adjustment.
Sample needed for being protected when ingressing and sampling using Pt due to the present invention, can be to avoid Ga ion implanting to the damage of sample
Wound, advantageously ensures that sample quality.
Step C:
The initial sample 2 for being deposited with Pt protective layer 6 is cut using ion beam 8, obtaining cross section is triangle
Strip sample 9.
Fig. 4 a shows the in situ TEM sample preparation according to an exemplary embodiment of the present invention based on heating chip
The structural schematic diagram of strip sample in method, Fig. 4 b show the main view of Fig. 4 a, and Fig. 4 c shows the top view of Fig. 4 a, Fig. 4 d
Show the schematic view of the front view of strip sample.
As shown in Fig. 4 a to Fig. 4 d, this step has specifically included following multiple sub-steps.
1) after deposition is complete, using ion beam 8 the initial sample 2 for being deposited with Pt protective layer 6 Pt protective layer one
One deep trouth of side end etching edge, the etching depth of the deep trouth is 8~12 μm, length is 8~12 μm, width is 8~12 μ
m。
2) prefabricated sample stage 11 is reversely inclined make 23 ° of included angle X between initial sample surface and ion beam direction~
53 °, the one side edge using ion beam in the Pt protective layer 6 for the initial sample 2 for being deposited with Pt protective layer carries out strip sample one
The etching cutting on side, the etching depth of cut of the strip sample a line is 8~12 μm, length is 13~17 μm, width is
3~5 μm.
3) same reversed dip makes 2 surface of initial sample and 8 direction of ion beam after prefabricated sample stage 11 being rotated 180 ° again
Between included angle X be 23 °~53 °, using ion beam 8 the initial sample 2 for being deposited with Pt protective layer Pt protective layer it is another
Side edge carry out the another a line of strip sample etching cutting, size with it is previous identical.
Above-mentioned included angle X is that the base angle angle of strip sample of triangle is equal such as excellent with the cross section etched
It is selected as 33 degree.
Wherein, the length in ion beam etching region can be adjusted according to the width of Pt protective layer, but wider than this
Big 4 μm of angle value or more.
Step D:
Strip sample 9 is shifted using manipulator 10 and is fixed on the sample hole slot 5 of heating chip 4.
Fig. 5 a is the relative position schematic diagram of line and prefabricated sample stage when strip sample to be fixed to heating chip, Fig. 5 b
The overlooking structure diagram on strip sample to the sample hole slot of heating chip is welded for manipulator, Fig. 5 c is that strip sample is fixed
Schematic view of the front view on the sample hole slot of heating chip.
Shown in as shown in Figure 5 a to 5 c, this step has specifically included following multiple sub-steps.
1) prefabricated sample stage 11 is controlled not tilt and rotate clockwise pre- sample preparation in the case where overlooking along 7 direction of electron beam
90 ° of sample platform, one jiao that manipulator 10 is protruded into and contacted strip sample 9, by ion beam 8 assist Pt deposition by manipulator with
10 strip samples 9 are soldered to together, as shown in Figure 5 a.
2) it will be grown using ion beam 8 along the end side of the Pt protective layer for the initial sample 2 for being deposited with Pt protective layer
Connection cutting between sample 9 and initial sample 2, is proposed strip sample 9 by the retraction of manipulator 10.
3) 90 ° of prefabricated sample stage is rotated clockwise in the case where overlooking along 7 direction of electron beam again, and tilts pre- sample preparation
Sample platform 11 keeps heating 4 surface of chip vertical with 7 direction of electron beam, and strip sample 9 is transferred to heating chip 4 by mobile manipulator 10
On the top of sample hole slot 5 and contact heating chip 4, as shown in Fig. 5 b.
4) it assists Pt deposition to realize the connection between heating chip 4 and strip sample 9 by ion beam 8, recycles ion
Beam 8 etches the connection of cutting machine hand 10 and strip sample 9 and strip sample 9 is finally fixed on to the sample well of heating chip 4
On slot 5, as shown in Figure 5 c.
Step E:
After fixing strip sample, adjust the position of prefabricated sample stage 11 and using ion beam 8 to strip sample 9 into
Row substep is thinned, and obtains the in situ TEM sample 14 based on heating chip.Wherein, the method for the present invention is obtained based on heating
The in situ TEM thickness of sample d of chip is 50~55nm.
Fig. 6 shows the cross section structure signal of the in situ TEM sample based on heating chip obtained after distribution is thinned
Figure.
As shown in fig. 6, this step includes following multiple sub-steps:
1) tilt angle of prefabricated sample stage 11 is adjusted to θ and to heat between 4 surface of chip and 8 direction of ion beam
In 5 °~25 ° of angle γ, wherein θ=90- β-γ；
2) strip sample 9 is carried out by the adjustment of the plus-minus of the tilt angle of prefabricated sample stage 11 and ion beam etching parameter
Be thinned and final amorphous layer removal, finally obtain thickness d be 50~55nm based on heating chip in situ TEM
Sample 14.
According to the present invention, TEM characterization is carried out using the above-mentioned in situ TEM sample 14 based on heating chip is practical
When, thickness d that sample is passed through by the electron beam of TEMTEM=d/cos γ=1d~1.1d.
The experimental results showed that this novel TEM sample preparation method in situ of the present invention can obtain sample with one-pass molding,
It does not need to carry out repeating sample introduction process, reduces sample preparation process；The strong operability of sample making course, prepared TEM sample are thick
Degree tens nanometers and the thin area's area of sample it is big, can sufficiently meet TEM In Situ Heating experiment the needs of, obtain it is clearly high
Differentiate the original position TEM experimental image.
The present invention is further detailed combined with specific embodiments below, but the scope of the present invention is without being bound by this
The embodiment of invention.
Embodiment 1:
Fig. 7 a shows the microscopic appearance figure for depositing Pt protective layer in embodiment 1 in initial sample, and Fig. 7 b shows reality
It applies in example 1 and etches the microcosmic shape of a deep trouth in the side end edge for the Pt protective layer for being deposited with the initial sample of Pt protective layer
Looks figure, Fig. 7 c is shown in embodiment 1 to be grown in the one side edge for the Pt protective layer for being deposited with the initial sample of Pt protective layer
The microscopic appearance figure of sample a line etching cutting, Fig. 7 d are shown in embodiment 1 in the initial sample for being deposited with Pt protective layer
Another side edge of the Pt protective layer of product carries out the microscopic appearance figure of the another a line etching cutting of strip sample, and Fig. 7 e shows reality
It applies and adjusts the strip sample surfaces microscopic appearance figure vertical with ion beam direction in example 1, Fig. 7 f shows in embodiment 1 and deposits Pt
The microscopic appearance figure that manipulator and strip sample are welded together, Fig. 7 g show cutting in embodiment 1 and connect and take out length
The microscopic appearance figure of bar sample, Fig. 7 h, which is shown, to be transferred to strip sample in embodiment 1 above the sample hole slot of heating chip
Microscopic appearance figure, Fig. 7 i show in embodiment 1 realize strip sample be fixed to heating chip sample hole slot microcosmic shape
Looks figure.
The present embodiment chooses aluminium (Al) film as the material for preparing sample, based on In Situ Heating chip and utilizes the present invention
Method carry out In Situ Heating TEM sample preparation.
Firstly, choosing while having the prefabricated sample stage of 0 ° of plane and 45 ° of inclined-planes, Al film sample is fixed on 0 ° of plane
On, the In Situ Heating chip with strip sample hole slot is fixed on 45 ° of inclined-planes, the sample hole slot of strip with it is rectangular
It is orthogonal in the longitudinal direction to heat chip.The prefabricated sample stage for placing initial sample and heating chip is transferred to ion
In the FIB-SEM double-beam system that beam is 52 ° with electron beam angle and vacuumize.
Keep initial sample surface vertical with ion beam direction secondly, tilting 52 ° of prefabricated sample stage, carries out Pt protective layer
Deposition.Pt protective layer with a thickness of 2 μm, length and width are 6 μm of 8 μ m, it is specific as shown in Figure 7a, the rectangle on initial sample surface is
For the Pt protective layer of deposition.
After the completion of Pt protective layer deposition, a deep trouth is etched in the side end edge of Pt protective layer, etching depth is 10 μ
M, length are 10 μm, and width is 10 μm, as shown in Figure 7b.
5 ° of prefabricated sample stage reversed dip, make 33 ° of angle between ion beam direction and initial sample surface, benefit
The quarter of strip sample a line is carried out in the one side edge for the Pt protective layer for being deposited with the initial sample of Pt protective layer with ion beam
Erosion cutting, the etching depth along ion beam direction are 10 μm, and length is 15 μm, and width is 3 μm, as shown in Figure 7 c.
Then 180 ° of prefabricated sample stage is rotated, 5 ° of same reversed dip is simultaneously being deposited with Pt protective layer using ion beam
The one side edge of the Pt protective layer of initial sample carries out the etching cutting of strip sample a line, size and previous identical, such as figure
Shown in 7d.
After the completion of the etching cutting on strip sample both sides, tilting 52 ° of prefabricated sample stage makes prefabricated sample surfaces and ion beam
Direction is vertical, as shown in figure 7e.Then, 90 ° of (edges of prefabricated sample stage are rotated clockwise in the not inclined situation of prefabricated sample stage
Beam direction is overlooked), one jiao that manipulator is protruded into and contacted sample P t protective layer is deposited by Assisted by Ion Beam Pt by machine
Tool hand is soldered to together with sample, as depicted in fig. 7f.
The connection between strip sample and substrate is cut off along 8 μm of sides of Pt protective layer using ion beam, passes through manipulator
Retraction strip sample is put forward, as shown in figure 7g.
90 ° of prefabricated sample stage is rotated clockwise again and tilts 45 ° of prefabricated sample stage, makes to heat chip surface and electron beam
Direction is vertical.Strip sample is transferred to above the sample hole slot of heating core on piece simultaneously contact chip by mobile manipulator, such as
Shown in Fig. 7 h.
The connection realized between heating chip and strip sample is deposited by Assisted by Ion Beam Pt, is cut using ion beam etching
The connection of disconnected manipulator and strip sample, it is final to realize that Al film sample is transferred on heating chip, as shown in figure 7i.
Fig. 8 a to Fig. 8 c shows strip sample in embodiment 1 and carries out the thinned microscopic appearance figure of substep, and Fig. 8 d is shown
The microscopic appearance figure of TEM sample obtained in embodiment 1, Fig. 8 d show the microcosmic shape of TEM sample obtained in embodiment 1
Looks figure.
The tilt angle of prefabricated sample stage is adjusted to 23 °, so that the angle between heating chip surface and ion beam is
15°.On the basis of this inclination angle, passes through the plus-minus of tilt angle and adjust ion beam etching parameter, carry out being thinned for TEM sample
And final amorphous layer removal, as shown in Fig. 8 a to 8c, finally obtain thickness d ≈ 50nm (along it is thinned when ion beam direction)
The In Situ Heating TEM sample of Al film, as shown in Fig. 8 d.
Practical sample when carrying out TEM characterization by electron beam pass through with a thickness of dTEM=d/cos15 ° of ≈ 52nm, effect is very
It is good.Fig. 9 a to Fig. 9 f respectively illustrates photographing not under scanning transmission electron microscope for TEM sample obtained in embodiment 1
With the angle of elevation annular dark field image in region, from Fig. 9 a to Fig. 9 f it can be seen that the sample contrast is uniform, lattice is clear, explanation
TEM sample is high-quality.
Embodiment 2:
Figure 10 a is shown in embodiment 2 in the side end edge for the Pt protective layer for being deposited with the initial sample of Pt protective layer
Edge etches the microscopic appearance figure of a deep trouth, and Figure 10 b shows in embodiment 2 and is being deposited with the initial sample of Pt protective layer
The one side edge of Pt protective layer carries out the microscopic appearance figure of strip sample a line etching cutting, and Figure 10 c is shown in embodiment 2
The another a line etching cutting of strip sample is carried out in another side edge for the Pt protective layer for being deposited with the initial sample of Pt protective layer
Microscopic appearance figure, Figure 10 d, which is shown, adjusts the strip sample surfaces microscopic appearance vertical with ion beam direction in embodiment 2
Figure.
The present embodiment chooses aluminium (Al) film as the material for preparing sample, based on In Situ Heating chip and utilizes the present invention
Method carry out In Situ Heating TEM sample preparation.
Firstly, choosing while having the prefabricated sample stage of 0 ° of plane and 45 ° of inclined-planes, Al film sample is fixed on 0 ° of plane
On, the In Situ Heating chip with strip sample hole slot is fixed on 45 ° of inclined-planes, the sample hole slot of strip with it is rectangular
It is orthogonal in the longitudinal direction to heat chip.The prefabricated sample stage for placing initial sample and heating chip is transferred to ion
In the FIB-SEM double-beam system that beam is 52 ° with electron beam angle and vacuumize.
Keep initial sample surface vertical with ion beam direction secondly, tilting 52 ° of prefabricated sample stage, carries out Pt protective layer
Deposition.Pt protective layer with a thickness of 2 μm, length and width are 6 μm of 8 μ m, it is specific as shown in Figure 7a, the rectangle on initial sample surface is
For the Pt protective layer of deposition.
After the completion of Pt protective layer deposition, a deep trouth is etched in the side end edge of Pt protective layer, etching depth is 10 μ
M, length are 12 μm, and width is 10 μm, as shown in Figure 10 a.
5 ° of prefabricated sample stage reversed dip, make 33 ° of angle between ion beam direction and initial sample surface, utilizes
Ion beam carries out the etching of strip sample a line in the one side edge for the Pt protective layer for being deposited with the initial sample of Pt protective layer
Cutting, the etching depth along ion beam direction are 10 μm, and length is 15 μm, and width is 3 μm, as shown in fig. lob.
Then 180 ° of prefabricated sample stage is rotated, 5 ° of same reversed dip is simultaneously being deposited with Pt protective layer using ion beam
The one side edge of the Pt protective layer of initial sample carries out the etching cutting of strip sample a line, size and previous identical, such as figure
Shown in 10c.
After the completion of the etching cutting on strip sample both sides, 52 ° of sample stage of inclination keeps sample surfaces vertical with ion beam direction,
As shown in fig. 10d, about 3 μm of triangle height.Then, make to rotate clockwise prefabricated sample in the not inclined situation of prefabricated sample stage
90 ° of platform (is overlooked) along beam direction.Manipulator is protruded into one jiao of contact sample P t protective layer, is sunk by Assisted by Ion Beam Pt
Product is soldered to manipulator and sample together.
Along 8 μm of sides of Pt protective layer, the connection between strip sample and substrate is cut off using ion beam, passes through manipulator
Retraction strip sample propose.
90 ° of prefabricated sample stage is rotated clockwise again and tilts 45 ° of prefabricated sample stage, makes to heat chip surface and electron beam
Direction is vertical, and strip sample is transferred to above the sample hole slot of heating core on piece simultaneously contact chip by mobile manipulator.
The connection realized between heating chip and strip sample is deposited by Assisted by Ion Beam Pt, is cut using ion beam etching
The connection of disconnected manipulator and strip sample, it is final to realize that Al film sample is transferred on chip.
Finally, the tilt angle of prefabricated sample stage is adjusted to 23 °, so that between heating chip surface and ion beam direction
Angle be 15 °.On the basis of this inclination angle, passes through the plus-minus of tilt angle and adjust ion beam etching parameter, carry out TEM sample
Product be thinned and final amorphous layer removal, finally obtain thickness d ≈ 50nm (along it is thinned when ion beam direction) Al film
In Situ Heating TEM sample.Practical sample when carrying out TEM characterization by electron beam pass through with a thickness of dTEM=d/cos15 ° of ≈
52nm。
Embodiment 3:
Figure 11 a is shown in embodiment 3 in the side end edge for the Pt protective layer for being deposited with the initial sample of Pt protective layer
Edge etches the microscopic appearance figure of a deep trouth, and Figure 11 b shows in embodiment 3 and is being deposited with the initial sample of Pt protective layer
The one side edge of Pt protective layer carries out the microscopic appearance figure of strip sample a line etching cutting, and Figure 11 c is shown in embodiment 3
The microscopic appearance figure that manipulator and strip sample are welded together deposition Pt, Figure 11 d show cutting in embodiment 3 and connect simultaneously
The microscopic appearance figure of strip sample is taken out, Figure 11 e shows the sample well that strip sample is transferred to heating chip in embodiment 3
Microscopic appearance figure above slot, Figure 11 f show the sample hole slot for realizing that strip sample is fixed to heating chip in embodiment 3
Microscopic appearance figure.
Choose fine copper (Cu) block be used as the material for preparing sample, based on In Situ Heating chip and utilization method of the invention into
The preparation of row In Situ Heating TEM sample.
Firstly, choosing while having the prefabricated sample stage of 0 ° of plane and 50 ° of inclined-planes, Cu block sample is fixed on 0 ° of plane
On, the In Situ Heating chip with strip sample hole slot is fixed on 50 ° of inclined-planes, the sample hole slot of strip with it is rectangular
It is orthogonal in the longitudinal direction to heat chip.The prefabricated sample stage for placing initial sample and heating chip is transferred to ion
In the FIB-SEM double-beam system that beam is 48 ° with electron beam angle and vacuumize.
Keep initial sample surface vertical with ion beam direction secondly, tilting 48 ° of prefabricated sample stage, carries out Pt protective layer
Deposition.Pt protective layer with a thickness of 3 μm, length and width are 8 μm of 9 μ m.
After the completion of Pt protective layer deposition, a deep trouth is etched in the side end edge of Pt protective layer, etching depth is 10 μ
M, length are 15 μm, and width is 7 μm, as shown in fig. 11a.
10 ° of prefabricated sample stage reversed dip, the angle between ion beam direction and initial sample surface is 32 °, is utilized
Ion beam carries out the etching of strip sample a line in the one side edge for the Pt protective layer for being deposited with the initial sample of Pt protective layer
Cutting, the etching depth along ion beam direction are 12 μm, and length is 16 μm, and width is 5 μm, as shown in figure 11b.
Then 180 ° of prefabricated sample stage is rotated, 10 ° of same reversed dip is simultaneously being deposited with Pt protective layer using ion beam
The one side edge of the Pt protective layer of initial sample carries out the etching cutting of strip sample a line, size with it is previous identical.
After the completion of the etching cutting on strip sample both sides, tilting 52 ° of prefabricated sample stage makes prefabricated sample surfaces and ion beam
Direction is vertical.90 ° of prefabricated sample stage (overlooking along beam direction) is rotated clockwise in the not inclined situation of prefabricated sample stage,
Manipulator and sample are soldered to one by Assisted by Ion Beam Pt deposition by one jiao that manipulator is protruded into and contacted sample P t protective layer
It rises, as shown in fig. 11c.
The connection between strip sample and substrate is cut off along 9 μm of sides of Pt protective layer using ion beam, such as Figure 11 d institute
Show.Strip sample is proposed by the retraction of manipulator, rotates clockwise 90 ° of prefabricated sample stage again, and tilt prefabricated sample
50 ° of platform, keep heating chip surface vertical with beam direction.Cu sample will be transferred to heating core on piece by mobile manipulator
Sample hole slot above and contact chip, as shown in Figure 11 e.
The connection realized between heating chip and Cu sample is deposited by Assisted by Ion Beam Pt, is cut off using ion beam etching
The connection of manipulator and sample, it is final to realize that Cu sample is transferred on heating chip, as shown in figure 11f.
Finally, prefabricated sample stage tilt angle is adjusted to 22 °, so that the angle between chip surface and ion beam is
20°.On the basis of this inclination angle, passes through the plus-minus of tilt angle and adjust ion beam etching parameter, carry out being thinned for TEM sample
And final amorphous layer removal, finally obtain thickness d ≈ 50nm (along it is thinned when ion beam direction) Cu sample In Situ Heating
TEM sample, practical sample when carrying out TEM characterization by electron beam pass through with a thickness of dTEM=d/cos20 ° of ≈ 53nm.
To sum up, the present invention using the preparation process that FIB-SEM double-beam system carries out TEM sample in situ only need once into
Sample enormously simplifies process flow, increases sample preparation efficiency；Sample preparation overall process simple and direct-viewing operation is conducive to promote sample preparation
Yield rate；Electron beam penetration thickness when the thickness of final sample is observed close to TEM, the available effective guarantor of sample quality
Barrier.
The invention is not limited to specific embodiments above-mentioned.The present invention, which expands to, any in the present specification to be disclosed
New feature or any new combination, and disclose any new method or process the step of or any new combination.
Claims (9)
1. a kind of in situ TEM sample preparation methods based on heating chip, which is characterized in that the preparation method includes
Following steps:
A, initial sample and heating chip are separately fixed in plane and inclined-plane adjacent on prefabricated sample stage, then by pre- sample preparation
Sample platform is transferred in FIB-SEM double-beam system and vacuumizes, wherein the planar inclination of the prefabricated sample stage is 0 ° and inclined-plane inclines
Angle α is 23 °~65 °, and the angle β between the ion beam and electron beam of the FIB-SEM double-beam system is 45 °~55 °；
B, Pt protective layer is deposited on initial sample surface using ion beam, obtains the initial sample for being deposited with Pt protective layer；
C, the initial sample for being deposited with Pt protective layer is cut using ion beam, obtains the length that cross section is triangle
Bar sample；
D, the strip sample is shifted using manipulator and is fixed on the sample hole slot of the heating chip；
E, it adjusts the position of prefabricated sample stage and substep is carried out to the strip sample using ion beam and be thinned, obtain based on heating
The in situ TEM sample of chip, wherein it is described based on heating chip in situ TEM thickness of sample d be 50~
55nm。
2. the in situ TEM sample preparation methods according to claim 1 based on heating chip, which is characterized in that described
The inclination angle of inclined plane α of prefabricated sample stage is 45 °~50 °, and the angle β between the ion beam and electron beam of FIB-SEM double-beam system is
48 °~52 °.
3. the in situ TEM sample preparation methods according to claim 1 or claim 2 based on heating chip, which is characterized in that
In step, the sample hole slot of the heating chip is set as orthogonal in the longitudinal direction with heating chip.
4. the in situ TEM sample preparation methods according to claim 1 or claim 2 based on heating chip, which is characterized in that
In stepb, tilting prefabricated sample stage β keeps initial sample surface vertical with ion beam direction and carries out Pt on initial sample surface
The deposition of protective layer obtains the initial sample for being deposited with Pt protective layer, the Pt protective layer with a thickness of 1~3 μm and length and width
Degree is 3~20 μm, wherein the length of the Pt protective layer is greater than the sample well groove width of the heating chip and is less than described
Heat the distance between electrode in sample hole slot both sides.
5. the in situ TEM sample preparation methods according to claim 1 or claim 2 based on heating chip, which is characterized in that
The step C includes following sub-step:
C-1: after deposition is complete, using ion beam in the side of the Pt protective layer of the initial sample for being deposited with Pt protective layer
End edge etches a deep trouth, and the etching depth of the deep trouth is 8~12 μm, length is 8~12 μm, width is 8~12 μm；
C-2: making 23 °~43 ° of the included angle X between initial sample surface and ion beam direction for prefabricated sample stage reversed dip,
One side edge using ion beam in the Pt protective layer of the initial sample for being deposited with Pt protective layer carries out one, strip sample
The etching on side is cut,；
C-3: same reversed dip makes the folder between initial sample surface and ion beam direction after prefabricated sample stage is rotated 180 °
Angle λ be 23 °~43 °, using ion beam the Pt protective layer of the initial sample for being deposited with Pt protective layer another side edge
The etching cutting for carrying out the another a line of strip sample, obtains the strip sample that cross section is triangle.
6. the in situ TEM sample preparation methods according to claim 5 based on heating chip, which is characterized in that described
The etching depth of cut of strip sample a line is 8~12 μm, length is 13~17 μm, width is 3~5 μm, the long galley proof
The etching depth of cut of the another a line of product is also 8~12 μm, length is 13~17 μm, width is 3~5 μm.
7. the in situ TEM sample preparation methods according to claim 1 or claim 2 based on heating chip, which is characterized in that
The step D includes following sub-step:
D-1: it controls prefabricated sample stage and does not tilt and rotate clockwise prefabricated sample stage in the case where overlooking along beam direction
90 °, one jiao that manipulator is protruded into and contacted the strip sample is deposited by Assisted by Ion Beam Pt by manipulator and long galley proof
Product are soldered to together；
D-2: it will be grown using ion beam along the end side of the Pt protective layer of the initial sample for being deposited with Pt protective layer
Connection cutting between sample and initial sample, is proposed strip sample by the retraction of manipulator；
D-3: 90 ° of prefabricated sample stage is rotated clockwise in the case where overlooking along beam direction again, and tilts prefabricated sample
Platform keeps heating chip surface vertical with beam direction, and strip sample is transferred to the sample well of heating core on piece by mobile manipulator
Above slot and contact heating chip；
D-4: the connection realized between heating chip and strip sample is deposited by Assisted by Ion Beam Pt, recycles ion beam etching
Strip sample is simultaneously finally fixed on the sample hole slot of the heating chip by the connection of cutting machine hand and strip sample.
8. the in situ TEM sample preparation methods according to claim 1 or claim 2 based on heating chip, which is characterized in that
The step E includes following sub-step:
E-1: being adjusted to θ for the tilt angle of prefabricated sample stage and to heat between chip surface and ion beam direction in 5 °~
25 ° of angle γ, wherein θ=90- β-γ；
E-2: strip sample is carried out by the plus-minus of the tilt angle of the prefabricated sample stage and the adjustment of ion beam etching parameter
Be thinned and final amorphous layer removal, finally obtain thickness d be 50~55nm based on heating chip in situ TEM
Sample.
9. the in situ TEM sample preparation methods according to claim 8 based on heating chip, which is characterized in that described
In situ TEM sample based on heating chip is when actually carrying out TEM characterization, thickness that sample is passed through by the electron beam of TEM
dTEM=d/cos γ=1d~1.1d.
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Application publication date: 20190531 |