CN109261646A - A method of utilizing the nearly local electrode of focused ion beam cleaning three-dimensional atom probe - Google Patents
A method of utilizing the nearly local electrode of focused ion beam cleaning three-dimensional atom probe Download PDFInfo
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- CN109261646A CN109261646A CN201810917874.1A CN201810917874A CN109261646A CN 109261646 A CN109261646 A CN 109261646A CN 201810917874 A CN201810917874 A CN 201810917874A CN 109261646 A CN109261646 A CN 109261646A
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- local electrode
- dimensional atom
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B7/00—Cleaning by methods not provided for in a single other subclass or a single group in this subclass
- B08B7/0035—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by radiant energy, e.g. UV, laser, light beam or the like
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Abstract
The invention discloses a kind of methods using the nearly local electrode of focused ion beam cleaning three-dimensional atom probe, method includes: that the sample stage with the nearly local electrode of three-dimensional atom probe is placed on three-dimensional atom probe nearly local electrode in focused ion beam to loaded on focused ion beam sample stage；In focused ion beam, vert sample stage, and adjustment imaging offset angle adjusts operating distance；The nearly local electrode of the three-dimensional atom probe that will be cut snaps to bosom under FIB image model；The root of protrusion defect on the outer ring of the ring cutting ring of FIB local electrode centers ring close with three-dimensional atom probe is aligned, inner ring is aligned with the tip edge of center ring upper process defect, ring cutting to the nearly local electrode ring surfaces free from admixture of three-dimensional atom probe.Method for cleaning provided by the invention clears up local electrode by focused ion beam, realizes the thorough cleaning of the nearly local electrode of three-dimensional atom probe, especially internal thorough cleaning, has saved cost.
Description
Technical field
The present invention relates to Material Fields, and in particular to a kind of to utilize the nearly local electricity of focused ion beam cleaning three-dimensional atom probe
The method of pole.
Background technique
Three-dimensional atom probe is a kind of measurement and analysis method with atom level spatial resolution.Based on " field evaporation " original
Reason, three-dimensional atom probe are become its surface atom by applying a strong voltage pulse or laser pulse on sample one by one
Pass through nearly local electrode at ion and collects.This requires the cleannes of electrode surface itself high, just can guarantee it is collected from
Son is the ion on sample, rather than is present in the foreign ion of electrode surface.When sample is broken in collection process, break
Splitting part can be adhered on electrode centers ring week shape inner surface, lead to nearly local electrode fouling, the data acquisition after influencing.
There are two types of the processing methods of traditional contaminated electrode, one is the electrode after use is done scrap processing and again
Buy new electrode or return genuine and reprocess, have a disadvantage in that: the period for causing electrode to waste, purchase electrode is long, influences equipment
Normal use.Another kind has cleaning halfway using the method for the nearly local electrode of hyperfrequency voltage cleaning three-dimensional atom probe
The shape defect of disadvantage, electrode internal ring portion can not solve, and cannot reach good cleaning effect.
Summary of the invention
It is an object of the invention to overcome, contaminated three-dimensional atom probe local electrode, genuine are reprocessed clearly in the prior art
The problems such as bottom is not cut at high cost, hyperfrequency voltage cleaning is managed, to provide a kind of utilization focused ion beam cleaning Three-dimensional atom spy
The method of the nearly local electrode of needle clears up the nearly local electrode of three-dimensional atom probe by focused ion beam, can obtain good clear
Reason is as a result, can save plenty of time and expense again.
To realize above-mentioned technical purpose and the technique effect, the invention is realized by the following technical scheme:
A method of utilizing the nearly local electrode of focused ion beam cleaning three-dimensional atom probe, which is characterized in that use ring
The ring week shape inner surface of the nearly local electrode centers of focused ion beam cleaning three-dimensional atom probe of shape.
By the protrusion on the outer ring of the ring cutting ring of focused ion beam local electrode centers ring close with three-dimensional atom probe
The root of defect is aligned, and the inner ring of ring cutting ring is aligned with the tip edge of center ring upper process defect, so that protrusion defect is clear
Reason is fallen.
Described method includes following steps:
Step S1: the nearly local electrode of three-dimensional atom probe is attached on focused ion beam sample stage, and vert sample stage, adjustment
Imaging compensating angle adjusts operating distance；
Step S2: the center of ring cutting ring local electrode centers close with three-dimensional atom probe are aligned under FIB imaging pattern；
Step S3: by the protrusion defect on the outer ring of the ring cutting ring of FIB local electrode centers ring close with three-dimensional atom probe
Root alignment, the inner ring of ring cutting ring is aligned with the tip edge of center ring upper process defect；
Step S4: ring cutting is not until having impurity between the inner ring and outer ring in ring cutting ring.
The step S1 specifically comprises the following steps:
S11: the nearly local electrode of three-dimensional atom probe is fixed on sample stage；
S12: the nitrogen in surge bunker is bled off, and opens surge bunker door；
S13: sample stage is loaded on the surge bunker sample sewing platform base in surge bunker；
S14: surge bunker door is closed；
S15: sample stage is pushed on working bin sample sewing platform base by transfer sample stage from surge bunker sample sewing platform base；
S16: working bin door is closed；
S17: opening electron gun, and sample stage is adjusted to immediately below electron gun after opening electron gun；
S18: vert sample stage, and the tilt angle that sample stage verts is 54 °, so that the nearly local electrode institute of three-dimensional atom probe
In plane and ion gun at plumbness；
S19: adjustment operating distance, the specific operating distance that adjusts is to 5.1mm, so that its working distance for being in ion gun
From.
The step S2 specifically comprises the following steps:
S21: ion gun is opened；
S22: the visual field under SEM image mode is adjusted to consistent with the visual field under FIB image model；
S23: adjustment focused ion beam, to recall ring cutting ring.
The step S3 specifically comprises the following steps:
S31: by the root of the protrusion defect on the outer ring of the ring cutting ring of FIB local electrode centers ring close with three-dimensional atom probe
Portion's alignment；
S32: the inner ring of the ring cutting ring of FIB is aligned with the tip edge of center ring upper process defect.
The step S4 specifically comprises the following steps:
S41: start ring cutting；
S42: adjusting ring cutting ring position, and the adjusting ring cutting ring position is carried out after a ring cutting suspends, it is ensured that under
Secondary ring cutting position is correct；
S43: do not have to terminate ring cutting when impurity between the inner ring and outer ring of ring cutting ring.
The S22 step of the step S2 specifically comprises the following steps:
S221: image is switched to before FIB mode, ion gun electric current is first adjusted to 2nA；
S222: image is switched to FIB mode after selection image reference point；
S223: it is clear by Image Adjusting after FIB mode that image is switched to, it is described by Image Adjusting be clearly by adjusting
Amplification, focusing, astigmatism, brightness, contrast are realized；
S224: be switched to FIB mode by Image Adjusting it is clear after FIB image and SEM image be adjusted to same position.
The beneficial effects of the present invention are: the method for cleaning of the nearly local electrode of three-dimensional atom probe provided by the invention, passes through
Focused ion beam clears up local electrode, realizes the thorough cleaning of the nearly local electrode of three-dimensional atom probe, and especially internal is thorough
Bottom cleaning, has saved cost.The present invention clears up the nearly local electrode of three-dimensional atom probe by focused ion beam, can obtain good
Cleaning as a result, plenty of time and expense can be saved again.
Detailed description of the invention
Fig. 1 present invention clears up the flow diagram of the method for the nearly local electrode of three-dimensional atom probe using focused ion beam.
Fig. 2 present invention is visited using ring cutting ring when focused ion beam cleaning three-dimensional atom probe nearly local electrode and Three-dimensional atom
The nearly local electrode alignment figure of needle.
Fig. 3 present invention utilizes the effect before ring cutting when focused ion beam cleaning three-dimensional atom probe nearly local electrode and after ring cutting
Fruit comparison diagram；Before wherein figure a is ring cutting, figure b is after ring cutting.
Fig. 4 present invention utilizes SEM before ring cutting when focused ion beam cleaning three-dimensional atom probe nearly local electrode and after ring cutting
Figure；Before wherein figure a is ring cutting, figure b is after ring cutting.
The nearly local electrode of Fig. 5 three-dimensional atom probe of the present invention, sample stage, pedestal three cooperate schematic diagram.
Fig. 6 FIB/SEM double-beam system partial schematic diagram of the present invention.
Mark representative meaning as follows in figure:
1- protrusion defect, 2- electrode body, 3- inner ring, 4- outer ring, 5- pedestal, 6- sample stage, 7- three-dimensional atom probe are close
Local electrode, 8- sample stage transfer levers contact position, 9- working bin, 10- working bin door, 11- surge bunker door, 12- buffering
Storehouse, 13- surge bunker sample sewing platform base, 14- working bin sample sewing platform base.
Specific embodiment
It is below with reference to the accompanying drawings and in conjunction with the embodiments, next that the present invention will be described in detail.
A method of it is one used by this method using the nearly local electrode of focused ion beam cleaning three-dimensional atom probe
Kind FIB/SEM double-beam system, wherein FIB is Focused Ion Beam, i.e. focused ion beam, SEM Scanning
Electron Microscope, i.e. scanning electron microscope；The method mainly includes the following steps:
S1: the nearly local electrode 7 of three-dimensional atom probe is attached on focused ion beam sample stage 6, and vert sample stage 6, adjustment
Imaging compensating angle adjusts operating distance；
S2: the center of ring cutting ring 7 center of local electrode close with three-dimensional atom probe is aligned under FIB imaging pattern；
S3: by the protrusion defect 1 on the outer ring of the ring cutting ring of FIB 7 center ring of local electrode close with three-dimensional atom probe
Root alignment, inner ring are aligned with the tip edge of center ring upper process defect 1；
S4: ring cutting is not until having impurity between the inner ring and outer ring in ring cutting ring.
The step S1 is specifically included:
S11: the nearly local electrode 7 of three-dimensional atom probe is fixed on sample stage 6；
More preferably, the described nearly local electrode 7 of three-dimensional atom probe is fixed on sample stage 6 will be fixed to slightly
Until cannot firmly continuing to tighten, to prevent sample from falling in instrument.
S12: the nitrogen in surge bunker 12 is bled off, and opens surge bunker door 11；
S13: sample stage 6 is loaded on the sample sewing platform base in surge bunker 12；
S131: sample stage transfer levers are twisted after sample stage 6 is loaded well.
More preferably, sample stage transfer levers be screwed to it is motionless until, prevent sample stage 6 from falling off.
S14: surge bunker door 11 is closed；
S15: transfer sample stage 6；
S151: sample stage 6 is shifted on working bin sample sewing platform base from surge bunker sample sewing platform base 13.
More preferably, described to shift sample stage 6 onto working bin sample sewing platform base from surge bunker sample sewing platform base 13
Upper is specially to shift bottom onto, is fallen off to avoid sample stage 6.
S152: described shift sample stage 6 on working bin sample sewing platform base onto later unscrews transfer levers.
More preferably, it is described transfer levers are unscrewed specially be screwed to both transfer levers and sample stage 6 be not bound with for
Only, it prevents from dragging sample stage 6 so that falling off from working bin sample sewing platform base when withdrawing transfer levers.
S16: working bin door 10 is closed；
S17: electron gun is opened；
S171: sample stage 6 is adjusted to immediately below electron gun after opening electron gun；
More preferably, described to open the auxiliary for determining central region when sample stage 6 is adjusted to immediately below electron gun
Tool CROSS is assisted, accurately to determine central region position
It is described to be adjusted to sample stage 6 to adjust sample stage 6 particular by adjustment operating stick X/Y immediately below electron gun
Horizontal position.
The adjustment operating stick X/Y is come to adjust 6 position of sample stage be specifically by nearly 7 center of local electrode of three-dimensional atom probe
The center of ring is adjusted to consistent with the center CROSS.
S18: vert sample stage 6；
The direction of verting that sample stage 6 is verted is vertical clockwise direction.
More preferably, the tilt angle that sample stage 6 is verted is 54 °, so that the nearly local of three-dimensional atom probe
7 place plane of electrode and ion gun are at plumbness.
S19: adjustment operating distance；
More preferably, the adjustment operating distance is adjustment operating distance to 5.1mm, so that it is in ion gun
Operating distance.
More preferably, mould first should be imaged in SEM (scanning electron microscope) before the adjustment operating distance to 5.1mm
It is under formula that Image Adjusting is clear, it is accurate with the operating distance for guaranteeing adjusted.
S191: described under SEM imaging pattern that Image Adjusting is clear preceding first by CAMERA (camera) opening SEM mode.
Described is clearly by adjusting Magnification (amplification), Focus by Image Adjusting under SEM imaging pattern
(focusing), Stigmator (astigmatism), Brightness (brightness), Contrast (contrast) are come what is realized.
The step S2 is specifically included:
S21: ion gun is opened；
S22: the visual field under SEM image mode is adjusted to consistent with the visual field under FIB image model；
Visual field under the mode by SEM image is first in SEM image before being adjusted to consistent with the visual field under FIB image model
Image reference point is selected under mode, it is ensured that adjustment is consistent.
More preferably, CROSS is opened when the selection image reference point to assist determining reference point.
The opening CROSS assists determining that reference point is adjusted in the center ring of CROSS by reference point.
It is realized in the center ring that reference point is adjusted to CROSS by adjusting operating stick X/Y.
S221: image is switched to before FIB mode, ion gun electric current is first adjusted to 2nA.
S2212: image is switched to FIB mode after selection image reference point.
S2213: it is first clear by Image Adjusting after FIB mode that image is switched to.
More preferably, it is described by Image Adjusting be clearly by adjusting Magnification, Focus,
Stigmator, Brightness, Contrast are realized.
S2214: be switched to FIB mode by Image Adjusting it is clear after FIB image and SEM image be adjusted to same position.
It is more preferably, described to open CROSS auxiliary adjustment when FIB image and SEM image are adjusted to same position,
It is accurate to ensure to adjust.
More preferably, the reference point chosen under SEM image mode is adjusted to by the opening CROSS auxiliary adjustment
In CROSS center ring.
It is described that the reference point chosen under SEM image mode is adjusted in CROSS center ring particular by adjustment X/Z
(horizontal X-direction/vertical direction) is realized.
More preferably, it is described the reference point chosen under SEM image mode is adjusted in CROSS center ring after
It is whether consistent with the picture position in FIB that image is switched to SEM mode confirmation SEM again.
More preferably, whether described image is switched to after SEM mode confirms image reference point in CROSS center ring
In.
More preferably, the confirmation image reference point whether in CROSS center ring particularly, if at this
Step is completed.
More preferably, the confirmation image reference point whether in CROSS center ring particularly, if not existing,
Reference point is adjusted in CROSS center ring again.
More preferably, described again reference point to be adjusted in CROSS center ring to be by adjusting Beam Shift
X/Y (the horizontal position X/Y of electron beam) is come what is realized.
S23: adjustment focused ion beam, to recall ring cutting ring；
The first opening control software before recalling ring cutting ring.
More preferably, it is described recall it is first that the image adjustment in control software display interface is clear before ring cutting ring
It is clear, to ensure that ring cutting position is accurate.
More preferably, it is described by control software display interface in image adjustment be clearly by adjusting
Magnification, Focus, Stigmator, Brightness, Contrast are realized.
More preferably, it is described by control software display interface in image adjustment it is clear when first to adjust FIB at
Image current size.
More preferably, electric current is specifically adjusted to 2nA by the adjusting FIB imaging size of current.
Step S3 is specifically included:
S31: by the protrusion defect 1 on the outer ring of the ring cutting ring of FIB 7 center ring of local electrode close with three-dimensional atom probe
Root alignment；
Protrusion defect 1 on the outer ring of the ring cutting ring by FIB 7 center ring of local electrode close with three-dimensional atom probe
It realizes at the alignment specific inner ring size control point in the inner ring of mobile ring cutting ring in root.
Protrusion defect 1 on the outer ring of the ring cutting ring by FIB 7 center ring of local electrode close with three-dimensional atom probe
Root can not be perfectly aligned if not being complete circle if nearly 7 center ring of local electrode of three-dimensional atom probe when being aligned, at this time to the greatest extent
The two may be aligned.
More preferably, described that the two is aligned nearly 7 center of local electrode of three-dimensional atom probe that should can not allow as far as possible
The outer ring of ring and ring cutting ring has intersection, prevents nearly 7 ontology 2 of local electrode of damage three-dimensional atom probe.
S32: the inner ring of the ring cutting ring of FIB is aligned with the tip edge of center ring upper process defect 1；
More preferably, the inner ring of the ring cutting ring by FIB is aligned with the tip edge of center ring upper process defect 1
What the specific outer ring size control point on the outer ring of mobile ring cutting ring was realized.
More preferably, the inner ring of the ring cutting ring by FIB is aligned with the tip edge of center ring upper process defect 1
Any impurity on ring cutting ring inner ring 3 and center ring, which should be adjusted, does not have intersection point.
Step S4 is specifically included:
S41: start ring cutting；
More preferably, start (beginning) realization for starting ring cutting by clicking control software.
More preferably, ring cutting electric current should first be adjusted before the start for clicking control software.
More preferably, the adjusting ring cutting electric current is by ring cutting current regulation to 2nA.
S42: ring cutting ring position is adjusted；
More preferably, the adjusting ring cutting ring position be the pause of ring cutting or after carry out, it is ensured that
The ring cutting position of next time is correct.
The concrete operation step for adjusting ring cutting ring position is identical as step S3's.
S43: terminate ring cutting；
More preferably, the end ring cutting is operated when not having impurity between the inner ring and outer ring of ring cutting ring.
Three-dimensional atom spy may be implemented using the nearly local electrode method of focused ion beam cleaning three-dimensional atom probe in the present invention
The thorough cleaning of the nearly local electrode of needle, from the SEM figure before and after local electrode ring cutting shown in Fig. 4, it can be seen that near electrode
Pollutant is effectively removed；Method of the invention has reached unexpected beneficial effect.
Claims (8)
1. a kind of method using the nearly local electrode of focused ion beam cleaning three-dimensional atom probe, which is characterized in that using cyclic annular
Nearly local electrode (7) center of focused ion beam cleaning three-dimensional atom probe ring week shape inner surface.
2. the method according to claim 1, wherein by the outer ring (4) of the ring cutting ring of the focused ion beam with
The root of protrusion defect (1) on nearly local electrode (7) center ring of three-dimensional atom probe is aligned, and the inner ring (3) of ring cutting ring is in
The tip edge of thimble upper process defect (1) is aligned, so that protrusion defect (1) be cleaned up.
3. according to the method described in claim 2, it is characterized in that, described method includes following steps:
Step S1: the nearly local electrode (7) of three-dimensional atom probe is attached on focused ion beam sample stage (6), vert sample stage
(6), adjustment imaging offset angle, adjusts operating distance；
Step S2: the center of ring cutting ring local electrode (7) center close with three-dimensional atom probe is aligned under FIB imaging pattern；
Step S3: the protrusion on the outer ring (4) of the ring cutting ring of FIB local electrode (7) center ring close with three-dimensional atom probe is lacked
The root alignment of (1) is fallen into, the inner ring (3) of ring cutting ring is aligned with the tip edge of center ring upper process defect (1)；
Step S4: ring cutting is not until having impurity between the inner ring of ring cutting ring (3) and outer ring (4).
4. according to the method described in claim 3, it is characterized in that, the step S1 specifically comprises the following steps:
S11: the nearly local electrode (7) of three-dimensional atom probe is fixed on sample stage (6)；
S12: the nitrogen in surge bunker (12) is bled off, and opens surge bunker door (11)；
S13: sample stage (6) is loaded on the surge bunker sample sewing platform base (13) in surge bunker (12)；
S14: it closes surge bunker door (11)；
S15: sample stage (6) is pushed into working bin sample sewing platform base by transfer sample stage (6) from surge bunker sample sewing platform base (13)
(14) on；
S16: it closes working bin door (10)；
S17: opening electron gun, and sample stage (6) is adjusted to immediately below electron gun after opening electron gun；
S18: the sample stage that verts (6), the tilt angle that sample stage (6) verts is 54 °, so that the nearly local electrode of three-dimensional atom probe
(7) plane and ion gun are at plumbness where；
S19: adjustment operating distance, the specific operating distance that adjusts is to 5.1mm, so that its operating distance for being in ion gun.
5. according to the method described in claim 3, it is characterized in that, the step S2 specifically comprises the following steps:
S21: ion gun is opened；
S22: the visual field under SEM image mode is adjusted to consistent with the visual field under FIB image model；
S23: adjustment focused ion beam, to recall ring cutting ring.
6. according to the method described in claim 3, it is characterized in that, the step S3 specifically comprises the following steps:
S31: by the protrusion defect on the outer ring (4) of the ring cutting ring of FIB local electrode (7) center ring close with three-dimensional atom probe
(1) root alignment；
S32: the inner ring (3) of the ring cutting ring of FIB is aligned with the tip edge of center ring upper process defect (1).
7. according to the method described in claim 3, it is characterized in that, the step S4 specifically comprises the following steps:
S41: start ring cutting；
S42: adjusting ring cutting ring position, and the adjusting ring cutting ring position is carried out after a ring cutting suspends, it is ensured that next
Ring cutting position is correct；
S43: do not have to terminate ring cutting when impurity between the inner ring (3) and outer ring (4) of ring cutting ring.
8. according to the method described in claim 5, it is characterized in that, the S22 step of the step S2 specifically comprises the following steps:
S221: image is switched to before FIB mode, ion gun electric current is first adjusted to 2nA；
S222: image is switched to FIB mode after selection image reference point；
S223: it is clear by Image Adjusting after FIB mode that image is switched to, and described by Image Adjusting is clearly by adjusting putting
Greatly, focusing, astigmatism, brightness, contrast are realized；
S224: be switched to FIB mode by Image Adjusting it is clear after FIB image and SEM image be adjusted to same position.
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| CN201810917874.1A CN109261646B (en) | 2018-08-13 | 2018-08-13 | Method for cleaning three-dimensional atom probe near-local-area electrode by using focused ion beam |
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| CN201810917874.1A CN109261646B (en) | 2018-08-13 | 2018-08-13 | Method for cleaning three-dimensional atom probe near-local-area electrode by using focused ion beam |
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| CN109261646B CN109261646B (en) | 2022-04-01 |
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| CN114392985A (en) * | 2022-01-19 | 2022-04-26 | 南京理工大学 | Method for cleaning three-dimensional atom probe near-local electrode by using Tesla coil |
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| CN114392985B (en) * | 2022-01-19 | 2023-10-10 | 南京理工大学 | Method for cleaning near-local electrode of three-dimensional atomic probe by using Tesla coil |
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| Publication number | Publication date |
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| CN109261646B (en) | 2022-04-01 |
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