CN108956669A - A kind of metal fuel particle surface oxide layer detection method - Google Patents
A kind of metal fuel particle surface oxide layer detection method Download PDFInfo
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- CN108956669A CN108956669A CN201810586395.6A CN201810586395A CN108956669A CN 108956669 A CN108956669 A CN 108956669A CN 201810586395 A CN201810586395 A CN 201810586395A CN 108956669 A CN108956669 A CN 108956669A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
- G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
Abstract
The present invention relates to Solid Rocket Propulsion Technologies, it is desirable to provide a kind of metal fuel particle surface oxide layer detection method.This kind of metal fuel particle surface oxide layer detection method, comprising steps of the dispersion and load of metal fuel particle；The micro-nano of metal fuel particle etches slice；The detection of metal fuel particle slice surface oxide layer.The present invention provides intuitive, comprehensive, accurate observation, analysis and measurement method to study preservation, generation and the Evolution Characteristics of metal fuel surface oxide layer, it can be used for detecting the metal fuel particle surface oxide layer of variety classes, partial size, pretreatment and degree of oxidation, have a wide range of application, technology versatility is good.
Description
Technical field
The present invention relates to Solid Rocket Propulsion Technology field, in particular to a kind of metal fuel particle surface oxide layer detection side
Method.
Background technique
Metal fuel is added in solid propellant can not only increase calorific value and the specific impulse of propellant, additionally aid alleviation and push away
Into the high-frequency combustion wild effect of agent.Common metal fuel both includes that (although boron is the elemental metals such as boron, aluminium, magnesium particle
It is nonmetallic, but be generally also referred in metal fuel in industry according to its application range), it also include boron magnesium compound, aluminium
The metal composites composition granules such as magnesium alloy, aluminium boron compound.
The combustion process of metal fuel particle shows as the process that there is the metallic atom of reproducibility to be oxidized in chemistry.
Therefore, the surface of metal fuel particle can generate oxide layer in its combustion process.Generation, differentiation and the elimination of the oxide layer are advised
Rule often influences the key factor of metal fuel particle energies release characteristics.Further, since containing certain density in air
Oxygen, metal fuel particle can occur slowly to aoxidize with being also difficult to avoid that in storage process, form initial surface oxidation
Layer, to influence the firing characteristic of metal fuel particle.Therefore, to the initial surface oxide layer of metal fuel particle and burned
Morphology, Elemental redistribution and the thickness of the oxide layer generated in journey are detected to analysis metal fuel particle surface object
Material reaction and diffusion mechanism are significant.Existing detection method is difficult to carry out metal fuel particle surface oxide layer straight
It sees, is comprehensive, accurate observation, analyzing and measure.
Summary of the invention
It is a primary object of the present invention to overcome deficiency in the prior art, provide a kind of micro- based on two-beam focused ion beam
The metal fuel particle surface oxide layer detection method that etching of receiving is sliced.In order to solve the above technical problems, solution party of the invention
Case is:
A kind of metal fuel particle surface oxide layer detection method is provided, specifically include the following steps:
(1) dispersion and load of metal fuel particle:
It takes solvent A and metal fuel particle to be mixed and made into suspension, and suspension is surpassed using ultrasonic wave separating apparatus
Sound dispersion；Then, the suspension after acquisition (1mL) dispersion that (uses the devices such as rubber head dropper or syringe) is transferred to carrier table
Face, and solvent evaporating completely is waited under room temperature (25 DEG C)；
Wherein, the mixing ratio of solvent A and metal fuel particle are as follows: 50mL:1.0mg；
The solvent A refers to the solvent not chemically reacted with metal fuel particle and its surface oxide layer, using going
Ionized water or dehydrated alcohol；But when metal fuel particle is boron particles, solvent A cannot be using deionized water (boron oxide tool
There is water imbibition)；
The metal fuel particle refers to the metal fuel particle of pure metals or the metal fuel particle of composite material；
The carrier uses monocrystalline silicon piece (P doped monocrystalline silicon sheet)；
(2) micro-nano of metal fuel particle etches slice:
In vacuum environment, using two-beam focused ion beam micro-nano technology instrument, to the metal fuel for being supported on carrier surface
Particle carries out micro-nano etching slice；Specifically include following sub-steps:
1) it (is acted on using ion beam sputter depositing) and plates one layer of platinum in metal fuel particle upper surface, to prevent from being sliced
Surface is destroyed by ion beam；
2) (under 47nA high current) ion beam is used successively to perform etching to platinum coating two sides, it is preliminary to obtain the thick of sample
Slice；
3) thick slice is taken out using tungsten needle, and thick slice is fixed on the tooth needle of molybdenum net；
4) use (under 2.5nA low current) ion beam thick slice online to molybdenum carries out thinned, until thick slice is subtracted
The thin ultra-thin section at a thickness of 220~330nm；
(3) metal fuel particle slice surface oxide layer detects:
It is super to metal fuel particle using scanning transmission electron microscope and its subsidiary X-ray energy spectrum elemental analyser
Morphology, different location elemental constituent and the surface oxide layer thickness of slice are detected.
In the present invention, the metal fuel particle refers to boron particles, alumina particles, magnesium granules, boron magnesium composite particles, aluminium
Magnesium alloy particles or aluminium boron compound particle.
In the present invention, the metal fuel particle is primary particles without any processing, by pretreated modification
Particle or residues of combustion particle with different degree of oxidation.
In the present invention, the monocrystalline silicon piece as carrier, thickness is no more than 1mm, having a size of 5mm × 5mm；And monocrystalline
Silicon wafer carried out polishing treatment as what carrier substrates used on one side.
In the present invention, in the step (1), when carrying out ultrasonic disperse to suspension using ultrasonic wave separating apparatus, ultrasound
The frequency of dispersion is 40KHz, power 720W, and the time of ultrasonic disperse is 20min.
In the present invention, in the step (2), the ion beam window and electron beam of two-beam focused ion beam micro-nano technology instrument
Window bias angle is 52 °, can observe metal fuel particle slice from different perspectives.
In the present invention, in the step (2), molybdenum net is the dedicated support grid of two-beam focused ion beam, and material is metal molybdenum, and
At least there is a rooted tooth needle.
In the present invention, in the step (2), the morphology of the ultra-thin section and different location elemental constituent
Detection carries out in scanning transmission electron microscope dark field environment, and surface oxide layer thickness is detected in scanning transmission electron microscope
It is carried out in light field environment.
Compared with prior art, the beneficial effects of the present invention are:
1, the present invention for research metal fuel surface oxide layer preservation, generation and Evolution Characteristics provide it is intuitive, comprehensive,
Accurate observation, analysis and measurement method.
2, the present invention can be used for the metal fuel particle surface oxidation to variety classes, partial size, pretreatment and degree of oxidation
Layer is detected, and is had a wide range of application, technology versatility is good.
3, the present invention carries out micro-nano etching slice to metal fuel particle using two-beam focused ion beam, forms to micron
Or the precise machining process of the micro/nano-scale of the metal fuel particle of submicron order.
4, the ultra-thin section of metal fuel particle is fixed on the tooth needle of molybdenum net by the present invention, is the daily guarantor of ultra-thin section
It is convenient to deposit offer, prevents naked eyes to be difficult to the metal fuel particle ultra-thin section differentiated loss, while convenient for during late detection
Metal fuel particle ultra-thin section is positioned under scanning transmission electron microscope form.
5, the present invention gives full play to the instrument characteristic of scanning transmission electron microscope, in conjunction with its subsidiary X-ray energy spectrum elemental analysis
Instrument assists linear measure longimetry and element point, line, surface scanning function to realize metal fuel particle and cut by bright, dark field switching, software
Piece surface oxide layer morphology, different location elemental constituent and surface oxide layer thickness complete detection.
6, the metal fuel particle and its quantity of solvent that the present invention uses are few, facilitate operation, save testing cost.
Detailed description of the invention
Fig. 1 is to observe the boron particles schematic diagram loaded on silicon wafer using two-beam focused ion beam micro-nano technology instrument.
Fig. 2 is the thick slice schematic diagram that using ion beam boron particles two sides are successively carried out with micro-nano etching and is obtained.
Fig. 3 is the schematic diagram for being slightly sliced and being fixed on molybdenum net tooth needle using tungsten needle intake boron.
Fig. 4 is slightly to be sliced the ultra-thin section schematic diagram for carrying out that acquisition is thinned to boron using the ion beam under low current.
Fig. 5 be using scanning transmission electron microscope (dark field) observation boron ultra-thin section go forward side by side row element analysis signal
Figure.
Fig. 6 is the signal using scanning transmission electron microscope (light field) measurement boron ultra-thin section surface oxide layer thickness
Figure.
Fig. 7 is that the boron residues of combustion particle loaded on silicon wafer is observed using two-beam focused ion beam micro-nano technology instrument
Schematic diagram.
Fig. 8 is successively to carry out the thick slice that micro-nano etching obtains to boron residues of combustion particle two sides using ion beam to illustrate
Figure.
Fig. 9 is the schematic diagram for being slightly sliced and being fixed on molybdenum net tooth needle using tungsten needle intake boron residues of combustion.
Figure 10 is slightly to be sliced the ultra-thin section for be thinned acquisition to boron residues of combustion using the ion beam under low current to show
It is intended to.
Figure 11 is row element point of being gone forward side by side using scanning transmission electron microscope (dark field) observation boron residues of combustion ultra-thin section
The schematic diagram of analysis.
Figure 12 is to measure boron residues of combustion ultra-thin section surface oxidation thickness using scanning transmission electron microscope (light field)
The schematic diagram of degree.
Figure 13 is to observe the alumina particles schematic diagram loaded on silicon wafer using two-beam focused ion beam micro-nano technology instrument.
Figure 14 is that using ion beam alumina particles two sides are successively carried out with micro-nano etching to obtain thick slice schematic diagram.
Figure 15 is the schematic diagram for being slightly sliced and being fixed on molybdenum net tooth needle using tungsten needle intake aluminium.
Figure 16 is slightly to be sliced the ultra-thin section schematic diagram for carrying out that acquisition is thinned to aluminium using the ion beam under low current.
Figure 17 be using scanning transmission electron microscope (dark field) observation aluminium ultra-thin section go forward side by side row element analysis signal
Figure.
Figure 18 is the signal using scanning transmission electron microscope (light field) measurement aluminium ultra-thin section surface oxide layer thickness
Figure.
Specific embodiment
Present invention is further described in detail with specific embodiment with reference to the accompanying drawing:
A kind of metal fuel particle surface oxide layer detection method is right based on two-beam focused ion beam micro-nano etching slice
Metal fuel particle surface oxide layer is detected, and three steps are specifically included: the 1. dispersion and load of metal fuel particle；②
The micro-nano of metal fuel particle etches slice；3. metal fuel particle slice surface oxide layer detects.
Step is 1.: the dispersion and load of metal fuel particle, refers to that (boron oxide has water suction using 50mL deionized water
Property, thus be not useable for boron particles detection) or dehydrated alcohol as solvent, be mixed and made into suspension with 1.0mg metal fuel particle,
And after using ultrasonic wave separating apparatus to carry out ultrasonic disperse (frequency 40KHz, power 720W, time 20min) to suspension, glue is used
Suspension after the head devices such as the dropper or syringe acquisition above-mentioned dispersion of 1mL is transferred to monocrystalline silicon piece or other similar carrier table
Face, and the operating process of solvent evaporating completely is waited at low temperature.
As the monocrystalline silicon piece of carrier, it is on sale that crystal silicon material Co., Ltd is found in Zhejiang.Monocrystalline silicon piece thickness is usually no more than
1mm, having a size of 5mm × 5mm, the one side used as carrier substrates should carry out polishing treatment.
Step is 2.: the micro-nano of metal fuel particle etches slice, refers to using two-beam focused ion beam micro-nano technology instrument pair
A certain metal fuel particle for being supported on monocrystalline silicon piece or other similar carrier surface carries out the operation that micro-nano etching is sliced
Journey.Above-mentioned micro-nano etching slicing processes specifically include: 1) being acted on above-mentioned metal fuel particle using ion beam sputter depositing
One layer of platinum is plated on surface, to prevent slice surface from being destroyed by ion beam；2) successively right using the ion beam under 47nA high current
Platinum coating two sides perform etching, the preliminary thick slice for obtaining sample；3) above-mentioned thick slice is taken out using tungsten needle, and slice is fixed
On the tooth needle of molybdenum net；4) carried out using the thick slice online to above-mentioned molybdenum of the ion beam under 2.5nA low current it is thinned, until general
The ultra-thin section of 220~330nm of thickness is thinned into thick slice.Aforesaid operations are in two-beam focused ion beam micro-nano technology instrument vacuum
It is carried out in environment.
The ion beam window and electron beam window misalignment angle of two-beam focused ion beam micro-nano technology instrument are 52 °, Ke Yicong
Different angle observes metal fuel particle slice.
Molybdenum net is the dedicated support grid of two-beam focused ion beam (Beijing Zhongjing Tech Technology Co., Ltd. is on sale) of market sale,
Material is metal molybdenum, and should at least have a rooted tooth needle.
Step is 3.: the detection of metal fuel particle slice surface oxide layer, refer to using scanning transmission electron microscope and its
Subsidiary X-ray energy spectrum elemental analyser is first to morphology, the different location of above-mentioned metal fuel particle ultra-thin section
The operating process that plain component and surface oxide layer thickness are detected.
The morphology of ultra-thin section and different location elemental constituent detection are generally in scanning transmission electron microscope
It is carried out in dark field environment, surface oxide layer thickness detection generally carries out in scanning transmission electron microscope light field environment.
The following examples can make the professional technician of this profession that the present invention be more fully understood, but not with any side
The formula limitation present invention.
Embodiment 1
Embodiment 1 selects Puri in Baoding to open up the amorphous boron particulate samples of Science and Technology Ltd.'s production, while selecting nothing
Water-ethanol is as solvent A, and P doped monocrystalline silicon sheet is as carrier.
1. boron particles sample is dispersed and loaded by above-mentioned steps, is existed using two-beam focused ion beam micro-nano technology instrument
A boron particles to be processed are found on silicon wafer, as shown in Figure 1.
One layer of platinum is plated in above-mentioned boron particles upper surface, to prevent slice surface from being destroyed by ion beam.Then, it uses
Ion beam under 47nA high current successively performs etching boron particles two sides, the preliminary thick slice for obtaining boron particles sample, such as Fig. 2
It is shown.Take out thick slice using tungsten needle, and will thick slice to be fixed on molybdenum online, as shown in Figure 3.It is thicker due to being slightly sliced, it is difficult to
Example interface is observed, it is thinned therefore, it is necessary to be carried out to slice.Using the ion beam under 2.5nA low current to sample thickness be sliced into
Row is thinned, and obtains the ultra-thin section of boron particles sample, with a thickness of 328nm, as shown in Figure 4.
Boron particles sample ultra-thin section is observed using scanning circumstance transmission electron microscope (dark field), discovery slice
From top to bottom be respectively platinum coating, boron simple substance layer, surface oxide layer and silicon substrate, as shown in Figure 5.The each not phase of each level contrast
Together, interface is high-visible.Using X-ray energy spectrum elemental analyser to elemental analysis is carried out in Fig. 50,1,2 three, as a result such as table 1
It is shown.It is boron simple substance at 1 it follows that being platinum coating at indicated in Fig. 50, is surface oxide layer at 2.
1 boron particles ultra-thin section elemental analysis result (based on mass fraction) of table
Using scanning circumstance transmission electron microscope (light field) to boron particles sample ultra-thin section surface oxide layer thickness into
Row measurement, as shown in Figure 6.
Embodiment 2
Embodiment 2 selects Puri in Baoding to open up the amorphous boron particle that Science and Technology Ltd. produces, through thermobalance in air
After being heated to 700 DEG C under atmosphere with the rate of heat addition of 10 DEG C/min, the combustion that argon atmosphere and natural cooling obtain is switched to rapidly
Remaining sample is burnt, while selecting dehydrated alcohol as solvent A, P doped monocrystalline silicon sheet is as carrier.
1. boron residues of combustion particulate samples are dispersed and loaded by above-mentioned steps, use two-beam focused ion beam micro-nano
Processing instrument finds a boron residues of combustion particle to be processed on silicon wafer, as shown in Figure 7.
One layer of platinum is plated in above-mentioned boron residues of combustion particle upper surface, to prevent slice surface from being destroyed by ion beam.With
Afterwards, successively boron residues of combustion particle two sides are performed etching using the ion beam under 47nA high current, tentatively obtains above-mentioned boron combustion
The thick slice of residual particles sample is burnt, as shown in Figure 8.Take out thick slice using tungsten needle, and will thick slice to be fixed on molybdenum online, such as
Shown in Fig. 9.Sample thickness slice is carried out using the ion beam under 2.5nA low current thinned, obtains the super of boron residues of combustion particle
Slice, with a thickness of 256nm, as shown in Figure 10.
Boron residues of combustion particle ultra-thin section is observed using scanning circumstance transmission electron microscope (dark field), is such as schemed
Shown in 11.Each level contrast is different, and interface is high-visible.Using X-ray energy spectrum elemental analyser in Figure 11 3,4 liang at
Elemental analysis is carried out, the results are shown in Table 2.It follows that being the lower boron oxide of oxygen content at indicated in Figure 11 3, it is at 4
The higher boron oxide of oxygen content.
2 boron residues of combustion particle ultra-thin section elemental analysis result (based on mass fraction) of table
Using scanning circumstance transmission electron microscope (light field) to boron residues of combustion particle ultra-thin section surface oxidation thickness
Degree measures, as shown in figure 12.
Embodiment 3
Embodiment 3 selects the spherical aluminum particles sample of Shanghai paddy field Science and Technology Ltd. production, while selecting deionized water
As solvent A, P doped monocrystalline silicon sheet is as carrier.
1. alumina particles sample is dispersed and loaded by above-mentioned steps, is existed using two-beam focused ion beam micro-nano technology instrument
An alumina particles to be processed are found on silicon wafer, as shown in figure 13.
One layer of platinum is plated in above-mentioned alumina particles upper surface, to prevent slice surface from being destroyed by ion beam.Then, it uses
Ion beam under 47nA high current successively performs etching alumina particles two sides, tentatively obtains the thick slice of above-mentioned alumina particles sample,
As shown in figure 14.Take out thick slice using tungsten needle, and will thick slice to be fixed on molybdenum online, as shown in figure 15.Use the low electricity of 2.5nA
The ion beam flowed down carries out thinned to sample thickness slice, obtains the ultra-thin section of alumina particles, with a thickness of 221nm, as shown in figure 16.
Alumina particles ultra-thin section is observed using scanning circumstance transmission electron microscope (dark field), as shown in figure 17.
Each level contrast is different, and interface is high-visible.It is first to being carried out in Figure 17 5,6 liang using X-ray energy spectrum elemental analyser
Element analysis, the results are shown in Table 3.It is surface oxide layer at 6 it follows that being pure aluminum at indicated in Figure 17 5.
3 alumina particles ultra-thin section elemental analysis result (based on mass fraction) of table
Alumina particles ultra-thin section surface oxide layer thickness is surveyed using scanning circumstance transmission electron microscope (light field)
Amount, as shown in figure 18.
Finally it should be noted that the above enumerated are only specific embodiments of the present invention.It is clear that the invention is not restricted to
Above embodiments can also have many variations.Those skilled in the art can directly lead from present disclosure
Out or all deformations for associating, it is considered as protection scope of the present invention.
Claims (8)
1. a kind of metal fuel particle surface oxide layer detection method, which is characterized in that specifically include the following steps:
(1) dispersion and load of metal fuel particle:
It takes solvent A and metal fuel particle to be mixed and made into suspension, and ultrasound point is carried out to suspension using ultrasonic wave separating apparatus
It dissipates；Then, the suspension after acquisition dispersion is transferred to carrier surface, and waits solvent evaporating completely at room temperature；
Wherein, the mixing ratio of solvent A and metal fuel particle are as follows: 50mL:1.0mg；
The solvent A refers to the solvent not chemically reacted with metal fuel particle and its surface oxide layer, using deionization
Water or dehydrated alcohol；But when metal fuel particle is boron particles, solvent A cannot use deionized water；
The metal fuel particle refers to the metal fuel particle of pure metals or the metal fuel particle of composite material；
The carrier uses monocrystalline silicon piece；
(2) micro-nano of metal fuel particle etches slice:
In vacuum environment, using two-beam focused ion beam micro-nano technology instrument, to the metal fuel particle for being supported on carrier surface
Carry out micro-nano etching slice；Specifically include following sub-steps:
1) one layer of platinum is plated in metal fuel particle upper surface, to prevent slice surface from being destroyed by ion beam；
2) successively platinum coating two sides are performed etching using ion beam, the preliminary thick slice for obtaining sample；
3) thick slice is taken out using tungsten needle, and thick slice is fixed on the tooth needle of molybdenum net；
4) carried out using the ion beam thick slice online to molybdenum it is thinned, until being thinned into thick slice with a thickness of 220~330nm's
Ultra-thin section；
(3) metal fuel particle slice surface oxide layer detects:
It is ultra-thin to metal fuel particle to cut using scanning transmission electron microscope and its subsidiary X-ray energy spectrum elemental analyser
Morphology, different location elemental constituent and the surface oxide layer thickness of piece are detected.
2. a kind of metal fuel particle surface oxide layer detection method according to claim 1, which is characterized in that the gold
Belong to fuel particle and refers to boron particles, alumina particles, magnesium granules, boron magnesium composite particles, almag particle or aluminium boron compound
Grain.
3. a kind of metal fuel particle surface oxide layer detection method according to claim 1, which is characterized in that the gold
Belonging to fuel particle is primary particles without any processing, by pretreated modified particles or the combustion with different degree of oxidation
Burn residual particles.
4. a kind of metal fuel particle surface oxide layer detection method according to claim 1, which is characterized in that the work
For the monocrystalline silicon piece of carrier, thickness is no more than 1mm, having a size of 5mm × 5mm；And monocrystalline silicon piece used as carrier substrates one
Face carried out polishing treatment.
5. a kind of metal fuel particle surface oxide layer detection method according to claim 1, which is characterized in that the step
Suddenly in (1), when carrying out ultrasonic disperse to suspension using ultrasonic wave separating apparatus, the frequency of ultrasonic disperse is 40KHz, power is
720W, the time of ultrasonic disperse are 20min.
6. a kind of metal fuel particle surface oxide layer detection method according to claim 1, which is characterized in that the step
Suddenly in (2), the ion beam window and electron beam window misalignment angle of two-beam focused ion beam micro-nano technology instrument are 52 °, can be never
With angle observation metal fuel particle slice.
7. a kind of metal fuel particle surface oxide layer detection method according to claim 1, which is characterized in that the step
Suddenly in (2), molybdenum net is the dedicated support grid of two-beam focused ion beam, and material is metal molybdenum, and at least has a rooted tooth needle.
8. a kind of metal fuel particle surface oxide layer detection method according to claim 1, which is characterized in that the step
Suddenly in (2), the morphology of the ultra-thin section and different location elemental constituent detection are in scanning transmission electron microscope
It is carried out in dark field environment, surface oxide layer thickness detection carries out in scanning transmission electron microscope light field environment.
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| CN110308171A (en) * | 2019-06-04 | 2019-10-08 | 甘肃酒钢集团宏兴钢铁股份有限公司 | A kind of method of stainless-steel cold-rolling anneal oxidation skin microcosmic observation |
| CN110423183A (en) * | 2019-07-29 | 2019-11-08 | 中国工程物理研究院化工材料研究所 | A kind of characterizing method of aluminum composition micron order aluminium ball surface oxide layer |
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