CN110423183A - A kind of characterizing method of aluminum composition micron order aluminium ball surface oxide layer - Google Patents
A kind of characterizing method of aluminum composition micron order aluminium ball surface oxide layer Download PDFInfo
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- CN110423183A CN110423183A CN201910690167.8A CN201910690167A CN110423183A CN 110423183 A CN110423183 A CN 110423183A CN 201910690167 A CN201910690167 A CN 201910690167A CN 110423183 A CN110423183 A CN 110423183A
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- C06B33/00—Compositions containing particulate metal, alloy, boron, silicon, selenium or tellurium with at least one oxygen supplying material which is either a metal oxide or a salt, organic or inorganic, capable of yielding a metal oxide
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- G—PHYSICS
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Abstract
The invention discloses a kind of characterizing methods of aluminum composition micron order aluminium ball surface oxide layer, comprising the following steps: (1) disperses conducting resinl surface for aluminium powder, be sent into focused ion beam vacuum chamber and vacuumize；(2) gas injection system for using focused ion beam deposits one layer of Pt on its surface；(3) by Ga ion beam current, region two sides to be processed are cut into U-typed is hanging, region to be processed is cut to the thin slice with a thickness of 1 μm or so；(4) thin slice is removed into aluminium ball surface by the way that mechanical arm is mobile；(5) thin slice is separated with the cutting of mechanical arm probe coupling part；(6) thin slice is thinned to obtain sample；(7) characterization is carried out to sample and judges alumina layer thickness.The technology is based on focused ion beam micro-nano technology technique, passes through the deposition of high vacuum and aluminium ball surface Pt metal layer in process, realizes protection of the ion beam bombardment in the process to oxide layer.
Description
Technical field
The present invention relates to material micro-nano processing and characterization technique fields, and in particular to a kind of aluminum composition micron order aluminium ball
The characterizing method of micro-nano technology and surface oxide layer.
Background technique
Quick-fried heat be measure one of the basic parameter of explosive detonation characteristic, and determine explosive charge injure characteristic source it is dynamic
Power.It is the activity of aluminium powder used to the principal element that Detonation Heat of Al-containing Explosives is affected, since aluminium powder is that a kind of chemical property is non-
Often active amphoteric metal material, easily leads to aluminium ball surface oxidation and active reduction, in turn under certain temperature and humidity conditions
Influence the key energy characterisitic parameter of energetic material.Therefore, the activity of accurate evaluation aluminium ball uses the longevity to prediction explosive loading
Life and quick-fried thermal energy are of great significance.The active evaluation method of aluminium powder mainly includes two classes at present: pure aluminum Content Method and heat
Analyze parametric method.Wherein pure aluminum Content Method mainly passes through chemical reagent and after pure aluminum reacts, and passes through reaction product
Weight extrapolates the simple substance aluminium content in aluminium powder and calculates the activity of aluminium powder.But this method requires simple substance aluminium content to be greater than 80%,
And easily occur situations such as reaction is incomplete in experimentation, cause the deviation of result.Heat analysis parametric method is mainly by aluminium powder
The parameters such as the oxidation behavior in combustion process, i.e. oxidation onset temperature, maximum oxidation rate calculate the activity of aluminium powder, but the party
Method is larger by the microscopic appearance and Size Distribution of aluminium powder, can not be used as the active unique criterion of aluminium powder.
The activity of aluminium powder depends primarily on the thickness of aluminium ball surface oxide layer, if the oxide layer on energy quantitatively characterizing aluminium ball surface
Thickness will provide key reference to the accurate activity for calculating aluminium powder.The aluminium powder in aluminum composition is generally by diameter in micro-nano at present
The aluminium ball of meter level forms, and high resolution transmission electron microscopy can be realized the directly perceived characterization to micro/nano level material microstructure.
But when test-material yardstick is reduced to micro-nano magnitude, due to the limitation of machining accuracy, the means such as traditional ion milling, double sprays are
It is unable to satisfy transmission electron microscope sample preparation and the requirement of characterization.Therefore, with advanced micro-nano processing technology, exploitation is for low
The structural characterization new method for tieing up sized materials, it is significant to the structure evolution process of research micro Nano material.Focused ion
Beam technology is ion beam spot to be focused on sub-micron even nano-grade size, and the new skill of fine Shu Jiagong is realized by deflection system
Art can realize the functions such as pattern etching, insulation and the production of metal material nano-precision sample and scanning ion imaging, energy respectively
It is enough that micro Process and observation are carried out with micron, nanometer dimension, it can be quick, high-precision for analysis means systems such as transmission electron microscopes
Sample.The technology has been widely used and micrometer/nanometer manufacture field at present.For the micron order aluminium ball in aluminum composition, pass through conjunction
The Technical Design of reason overcomes chondritic to the fixation of sample and turns under the premise of not destroying sample surfaces oxide layer
Moving bring operation difficulty is that characterization is successfully crucial.
Summary of the invention
In order to solve the above-mentioned technical problems, the present invention provides a kind of tables of aluminum composition micron order aluminium ball surface oxide layer
Sign method, this method provides the micron order aluminium ball processing schemes that one kind does not destroy surface oxide layer, it is made to meet transmission electron microscope
Characterization requirement to thickness of sample less than 200nm.The technology is based on focused ion beam micro-nano technology technique, leads in process
The deposition of high vacuum and aluminium ball surface Pt metal layer is crossed, realizes protection of the ion beam bombardment in the process to oxide layer.By aluminium ball plus
After work is suitably sized, then pass through the thickness of its surface oxide layer of high resolution electron microscopy quantitatively characterizing.This is technically simple effectively, can
Strong operability is, it can be achieved that accurate Characterization to aluminium ball surface oxide layer thickness.
In order to reach above-mentioned technical effect, the present invention provides a kind of tables of aluminum composition micron order aluminium ball surface oxide layer
Sign method, comprising the following steps:
(1) conducting resinl surface is dispersed by aluminium powder, then conducting resinl is sent into focused ion beam vacuum chamber and is taken out true
It is empty；
(2) by electron beam imaging systems, the single aluminium ball in area-of-interest is selected, using the gas of focused ion beam
Injected system deposits one layer of Pt on its surface, to protect the thickness of aluminium ball surface oxide layer not influenced by process；
(3) by the Ga ion beam current in focused ion beam system, it is hanging that region two sides to be processed are cut into U-typed,
Region to be processed is cut to the thin slice with a thickness of 1 μm；
(4) nano-machine arm probe is contacted with region to be processed, is deposited by Pt and probe is connected with thin slice, then uses Ga
The two sides that thin slice to be processed is connect by ion beam with aluminium ball are cut off, and thin slice can be removed aluminium ball surface by the way that mechanical arm is mobile；
(5) thin slice is moved into the dedicated half point support grid marked locations of focused ion beam sample, and is deposited by Pt by sample
Product are connected with support grid, are then separated thin slice with the cutting of mechanical arm probe coupling part by Ga ion beam；
(6) 90~110nm is thinned to thin slice upper and lower surface by Ga ion beam current, sample processing is completed；
(7) the half point support grid for completing the process sample will be loaded with and be transferred to transmission electron microscope Special sample bar, and sample is carried out
High-resolution-ration transmission electric-lens characterization, finds the interface cohesion region of Pt sedimentary and sample and amplifies, to the region from Pt layers to aluminium
Direction of bowl does energy spectral line scanning, and by Al, the distribution of O and Pt element can determine whether alumina layer thickness.
Further technical solution is that the quality of aluminium powder is 2~5g in the step (1), and the size of conducting resinl is 10mm
× 10mm, vacuum chamber air pressure are evacuated to 10-4Pa。
Further technical solution is that Pt source metal purity is 99.99% in the step (2), deposition process intermediate ion
Beam current density is 2~6pA/ μm2, sedimentation time is 2~3min, and Pt layers with a thickness of 0.8~1.2 μm.
Further technical solution is that Ga source metal purity is 99.99% in the step (3), cutting process intermediate ion
Beam current is 3nA, and total elapsed time is 5~6min, and cutting profile is rectangle, having a size of 2 μm of 10 μ m, working depth is 10~
15 μm, machining accuracy 5nm.
Further technical solution is that focused ion line is in the Pt deposition process in the step (4) and step (5)
30pA, cutting line are 3nA.
Further technical solution is that it is 0.1~1nA, machining accuracy that beam current, which is thinned, in Ga ion beam in the step (6)
For 5nm.
Compared with prior art, the invention has the following beneficial effects: the technologies to pass through focused ion beam micro-nano technology hand
Section, preparation can be used for the aluminium ball chip sample of high-resolution-ration transmission electric-lens characterization, and compared with prior art, which can be microcosmic
Scale is directly realized by the quantitatively characterizing of aluminium ball surface oxide layer, can assess for the activity of aluminum composition and provide key parameter.Pass through
Pt protective layer is deposited on aluminium ball surface, it is ensured that aluminium ball surface oxide layer is not damaged in processing and transfer process, it is ensured that table
Levy data it is true and reliable, the technological invention clear thinking, directly it is effective, easily operated, be suitable for diameter in some tens of pm aluminium ball
Processing and oxide layer characterization.
Detailed description of the invention
Fig. 1 is the microscopic appearance SEM picture of aluminium ball to be processed；
Fig. 2 is that aluminium ball surface deposits Pt protective layer SEM picture；
Fig. 3 is aluminium ball surface U-typed machining area SEM side view；
Fig. 4 is aluminium ball surface U-typed machining area SEM top view；
Fig. 5 is that processing thin slice and aluminium ball matrix cut separation process SEM picture；
Fig. 6 is that processing thin slice is transferred to half point support grid SEM picture；
Fig. 7 is the thin slice pattern SEM picture after being thinned；
Fig. 8 is 1 high-resolution-ration transmission electric-lens of embodiment to energy spectral line scanning result picture at Pt and example interface；
Fig. 9 is 2 high-resolution-ration transmission electric-lens of embodiment to energy spectral line scanning result picture at Pt and example interface；
Figure 10 is 3 high-resolution-ration transmission electric-lens of embodiment to energy spectral line scanning result picture at Pt and example interface.
Specific embodiment
The invention will be described in further detail in the following with reference to the drawings and specific embodiments, and the invention discloses a kind of microns
Grade aluminium ball surface oxide layer characterizing method, this method specifically includes the following steps:
Step 1, sample pre-treatments；
Conducting resinl surface is dispersed by a certain amount of aluminium powder and is sent into the vacuum chamber of focused ion beam system, and air pressure is taken out
To 10-4Pa；
Step 2, Pt protective layer in aluminium ball surface deposits；
Under the electronic imaging system of focused ion beam, single aluminium ball of the diameter at 30-80 μm or so is selected.Pass through gas
Injected system deposits Pt protective layer to aluminium ball surface to be processed, and deposition process beam current density is 2~6pA/ μm2, sink
Product time 2min, obtains the Pt protective layer of 1 μm of 1 μ m of about 10 μ m of aluminium ball surface size shown in Fig. 2；
Step 3, focused ion beam processed sample；
Cutting processing is carried out to target area using Ga ion beam, ion beam current 3nA is in along Pt protective layer two sides
U-typed cutting, working depth are 10~15 μm, obtain the chip sample of 10 μ m, 1 μ m (10~15 μm)；
Step 4, sample is shifted and is thinned；
By nano-machine arm probe and flap contact in focused ion beam system, by Pt ion beam depositing by probe with it is thin
Piece is weldingly connected, then is cut off with the two sides that thin slice to be processed is connect by Ga ion beam with aluminium ball, and can be moved by mechanical arm will
Thin slice removes aluminium ball surface；Then thin slice is moved in the dedicated half point support grid of transmission electron microscope sample.Pass through Pt ion beam depositing
Thin slice is fixed on support grid designated position, deposition line is 30pA, sedimentation time about 1min.It by thin slice and is visited by Ga ion beam
The cutting separation of needle coupling part, i.e. removable probe, Ga ion beam current are 3nA.Again using Ga ion beam to thin slice intermediate region
It is further thinned to thickness about 100nm or so, Ga ion beam current is 0.1~1nA in thinning process；
Step 5, high resolution electron microscopy characterizes sample oxidation thickness degree；
High-resolution-ration transmission electric-lens characterization is carried out to chip sample.It finds the interface cohesion region of Pt sedimentary and sample and puts
Greatly, it does energy spectral line to aluminium ball direction from Pt layers to the region to scan, according to Al, the distribution of O and Pt element can determine whether oxygen
Change aluminum layer thickness.
Embodiment 1
As shown in Figure 1, dispersing conducting resinl surface for 2g aluminium powder, it is put into the vacuum chamber of focused ion beam system, gas
Pressure is evacuated to 10-4Pa；Under the electronic imaging system of focused ion beam, single aluminium ball of the diameter at 80 μm or so is selected.Pass through gas
Body injected system deposits Pt protective layer to aluminium ball surface to be processed, and deposition process beam current density is 2pA/ μm2, deposition
Time 2min obtains the Pt protective layer of 1 μm of 1 μ m of about 10 μ m of aluminium ball surface size shown in Fig. 2；Such as Fig. 3, shown in 4,5, use
Ga ion beam carries out cutting processing to target area, and ion beam current 3nA is cut along Pt protective layer two sides in U-typed, processing
Depth is 15 μm, obtains the chip sample of 15 μm of 10 μ m, 1 μ m；As shown in fig. 6, passing through 2pA/ μm2Pt ion beam depositing
Nano-machine arm probe is weldingly connected with thin slice, then the two sides for being connect thin slice to be processed with aluminium ball with the Ga ion beam of 3nA
Thin slice is removed aluminium ball surface by the way that mechanical arm is mobile by excision；Thin slice is moved in the dedicated half point support grid of transmission electron microscope sample.
Thin slice is fixed on support grid designated position by Pt ion beam depositing, deposition line is 30pA, sedimentation time about 1min.Pass through
The Ga ion beam of 3nA separates thin slice with the cutting of probe coupling part, then removes probe.Again using Ga ion beam in thin slice
Between region be further thinned to thickness about 100nm or so, be thinned initial procedure in Ga ion beam current be 1nA, with thin slice thickness
The reduction of degree, is gradually adjusted to 0.1nA, and sample is as shown in Figure 7 after the completion of being thinned；Under high-resolution-ration transmission electric-lens, thin slice is found
The interface of middle Pt protective layer and sample is simultaneously amplified to 100,000 times (such as Fig. 8 (a)), pass through can spectral line scanning technique, characterize Pt, Al
With tri- kinds of elements of O by passing through the peak of O Elemental redistribution as shown in Fig. 8 (b-d) to the changes in distribution of Pt protective layer inside aluminum slice
It is worth region, the deducibility aluminium ball surface oxide layer thickness about 65nm.
Embodiment 2
Conducting resinl surface is dispersed by 3g aluminium powder, is put into the vacuum chamber of focused ion beam system, air pressure is evacuated to 10- 4Pa；Under the electronic imaging system of focused ion beam, single aluminium ball of the diameter at 50 μm or so is selected.It is injected by gas and is
It unites and deposits Pt protective layer to aluminium ball surface to be processed, deposition process beam current density is 2pA/ μm2, sedimentation time
2min obtains the Pt protective layer of 1 μm of 1 μ m of about 10 μ m of aluminium ball surface size；Target area is cut using Ga ion beam
Processing is cut, ion beam current 3nA is cut along Pt protective layer two sides in U-typed, and working depth is 10 μm, obtains 1 μm of 10 μ m
× 10 μm of chip sample；Pass through 2pA/ μm2Pt ion beam depositing nano-machine arm probe is weldingly connected with thin slice, then use
The two sides that thin slice to be processed is connect by the Ga ion beam of 3nA with aluminium ball are cut off, and thin slice is removed aluminium ball table by the way that mechanical arm is mobile
Face；Thin slice is moved in the dedicated half point support grid of transmission electron microscope sample.Thin slice support grid is fixed on by Pt ion beam depositing to refer to
Positioning is set, and deposition line is 30pA, sedimentation time about 1min.Thin slice and probe interconnecting piece are cut by the Ga ion beam of 3nA
Separation is cut, probe is then removed.Thickness about 100nm or so is further thinned to thin slice intermediate region using Ga ion beam again,
Ga ion beam current is gradually adjusted to 0.1nA with the reduction of sheet thickness for 1nA in thinned initial procedure；It is thinned and completes
Afterwards, it under high-resolution-ration transmission electric-lens, finds the interface of Pt protective layer and sample in thin slice and is amplified to 100,000 times of (such as Fig. 9
(a)), by can spectral line scanning technique, characterization tri- kinds of elements of Pt, Al and O by inside aluminum slice to the changes in distribution of Pt protective layer,
As shown in Fig. 9 (b-d), pass through the peak region of O Elemental redistribution, the deducibility aluminium ball surface oxide layer thickness about 55nm.
Embodiment 3
Conducting resinl surface is dispersed by 5g aluminium powder, is put into the vacuum chamber of focused ion beam system, air pressure is evacuated to 10- 4Pa；Under the electronic imaging system of focused ion beam, single aluminium ball of the diameter at 40 μm or so is selected.It is injected by gas and is
It unites and deposits Pt protective layer to aluminium ball surface to be processed, deposition process beam current density is 4pA/ μm2, sedimentation time
1min obtains the Pt protective layer of 1 μm of 1 μ m of about 10 μ m of aluminium ball surface size；Target area is cut using Ga ion beam
Processing is cut, ion beam current 3nA is cut along Pt protective layer two sides in U-typed, and working depth is 10 μm, obtains 1 μm of 10 μ m
× 10 μm of chip sample；Pass through 2pA/ μm2Pt ion beam depositing nano-machine arm probe is weldingly connected with thin slice, then use
The two sides that thin slice to be processed is connect by the Ga ion beam of 3nA with aluminium ball are cut off, and thin slice is removed aluminium ball table by the way that mechanical arm is mobile
Face；Thin slice is moved in the dedicated half point support grid of transmission electron microscope sample.Thin slice support grid is fixed on by Pt ion beam depositing to refer to
Positioning is set, and deposition line is 30pA, sedimentation time about 1min.Thin slice and probe interconnecting piece are cut by the Ga ion beam of 3nA
Separation is cut, probe is then removed.Thickness about 100nm or so is further thinned to thin slice intermediate region using Ga ion beam again,
Ga ion beam current is gradually adjusted to 0.1nA with the reduction of sheet thickness for 1nA in thinned initial procedure；It is thinned and completes
Afterwards, it under high-resolution-ration transmission electric-lens, finds the interface of Pt protective layer and sample in thin slice and is amplified to 100,000 times of (such as Figure 10
(a)), by can spectral line scanning technique, characterization tri- kinds of elements of Pt, Al and O by inside aluminum slice to the changes in distribution of Pt protective layer,
As shown in Figure 10 (b-d), pass through the peak region of O Elemental redistribution, the deducibility aluminium ball surface oxide layer thickness about 35nm.
Although reference be made herein to invention has been described for explanatory embodiment of the invention, and above-described embodiment is only this hair
Bright preferable embodiment, embodiment of the present invention are not limited by the above embodiments, it should be appreciated that those skilled in the art
Member can be designed that a lot of other modification and implementations, these modifications and implementations will fall in principle disclosed in the present application
Within scope and spirit.
Claims (6)
1. a kind of characterizing method of aluminum composition micron order aluminium ball surface oxide layer, which comprises the following steps:
(1) conducting resinl surface is dispersed by aluminium powder, then conducting resinl is sent into focused ion beam vacuum chamber and is vacuumized；
(2) by electron beam imaging systems, the single aluminium ball in area-of-interest is selected, is injected using the gas of focused ion beam
System deposits one layer of Pt on its surface, to protect the thickness of aluminium ball surface oxide layer not influenced by process；
(3) by the Ga ion beam current in focused ion beam system, it is hanging that region two sides to be processed are cut into U-typed, it is to be added
Work area domain is cut to the thin slice with a thickness of 1 μm；
(4) nano-machine arm probe is contacted with region to be processed, is deposited by Pt and probe is connected with thin slice, then with Ga ion
The two sides that thin slice to be processed is connect by beam with aluminium ball are cut off, and thin slice can be removed aluminium ball surface by the way that mechanical arm is mobile；
(5) thin slice is moved into the dedicated half point support grid marked locations of focused ion beam sample, and by Pt deposition by sample with
Support grid is connected, and is then separated thin slice with the cutting of mechanical arm probe coupling part by Ga ion beam；
(6) 90~110nm is thinned to thin slice upper and lower surface by Ga ion beam current, sample processing is completed；
(7) the half point support grid for completing the process sample will be loaded with and be transferred to transmission electron microscope Special sample bar, and high score is carried out to sample
It distinguishes that transmission electron microscope characterizes, finds the interface cohesion region of Pt sedimentary and sample and amplify, to the region from Pt layers to aluminium ball side
To energy spectral line scanning is done, by Al, the distribution of O and Pt element can determine whether alumina layer thickness.
2. the characterizing method of aluminum composition micron order aluminium ball surface oxide layer according to claim 1, which is characterized in that institute
The quality for stating aluminium powder in step (1) is 2~5g, and the size of conducting resinl is 10mm × 10mm, and vacuum chamber air pressure is evacuated to 10-4Pa。
3. the characterizing method of aluminum composition micron order aluminium ball surface oxide layer according to claim 1, which is characterized in that institute
Stating Pt source metal purity in step (2) is 99.99%, and deposition process beam current density is 2~6pA/ μm2, when deposition
Between be 2~3min, Pt layers with a thickness of 0.8~1.2 μm.
4. the characterizing method of aluminum composition micron order aluminium ball surface oxide layer according to claim 1, which is characterized in that institute
Stating in step (3) Ga source metal purity is 99.99%, and cutting process beam current is 3nA, total elapsed time is 5~
6min, cutting profile are rectangle, and having a size of 2 μm of 10 μ m, working depth is 10~15 μm, machining accuracy 5nm.
5. the characterizing method of aluminum composition micron order aluminium ball surface oxide layer according to claim 1, which is characterized in that institute
Stating focused ion line in the Pt deposition process in step (4) and step (5) is 30pA, and cutting line is 3nA.
6. the characterizing method of aluminum composition micron order aluminium ball surface oxide layer according to claim 1, which is characterized in that institute
Stating Ga ion beam in step (6) and beam current is thinned is 0.1~1nA, machining accuracy 5nm.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111238894A (en) * | 2020-02-03 | 2020-06-05 | 天津理工大学 | Preparation method of in-situ electric TEM sample |
| CN111238894B (en) * | 2020-02-03 | 2023-02-28 | 天津理工大学 | Preparation method of in-situ electric TEM sample |
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| CN112858362B (en) * | 2021-01-08 | 2022-05-27 | 重庆大学 | Preparation method of micron-sized spherical particle section for electron microscope observation |
| CN113189123A (en) * | 2021-04-30 | 2021-07-30 | 东南大学 | Observation micro-area positioning method based on internal standard substance microarray |
| CN113189123B (en) * | 2021-04-30 | 2023-01-31 | 东南大学 | Observation micro-area positioning method based on internal standard substance microarray |
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