CN107727677A - The cathodoluminescence imaging method of monazite - Google Patents
The cathodoluminescence imaging method of monazite Download PDFInfo
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- CN107727677A CN107727677A CN201710866383.4A CN201710866383A CN107727677A CN 107727677 A CN107727677 A CN 107727677A CN 201710866383 A CN201710866383 A CN 201710866383A CN 107727677 A CN107727677 A CN 107727677A
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- 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]
- G01N23/2254—Measuring cathodoluminescence
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Abstract
The invention discloses a kind of cathodoluminescence imaging method of monazite, including：Target processed is carried out to monazite minerals particle, obtains resin target；The resin target is polished, monazite is exposed to the resin target；Plated film is carried out in the monazite for being exposed to the resin target, plated film is face-up, and the resin target after plated film is fixed on the sample stage of field emission scanning electron microscope with conducting resinl, the sample bin of field emission scanning electron microscope is vacuumized, the resin target is under vacuum condition；Select the operating distance of cathodoluminescence probe；Select the accelerating potential of electron beam；Select the beam spot size of electron beam；Select primary gain value；Obtain the image of monazite individual particle.The present invention carries out high-resolution cathodoluminescence luminescence imaging to monazite, and solving the problems, such as monazite, cathodoluminescence is integrally black all the time, reaches the inner structural features for clearly reflecting monazite, serves the purpose that year accurate reconnaissance is determined in monazite in-situ micro area.
Description
Technical field
The present invention relates to technical field of image acquisition, particularly relates to a kind of cathodoluminescence imaging side of individual particle monazite
Method.
Background technology
Monazite (Ce, La, Nd, Th) (PO4) be widely present in respectively as the phosphate mineral containing light rare earth (LREE)
In rocks, its composition composition can react host's rock characteristic.Simultaneously as monazite has higher U, Th content, compared with
Low initial common Pb compositions, high Pb closure temperatures (about 750 DEG C), in the absence of the influence for sloughing off crystallization, become excellent
Geological epoch counts..With the secondary ion probe (SIMS) and laser ablation plasma mass spectrograph (LA-ICP-MS) of microcell,
And the rapid development of electron probe (EPMA) dating technique, monazite have become most important in-situ micro area chronology analysis
One of accessory mineral.
However, from the monazite of different lithology, its mineral internal structure and geochemical information can show various
Property feature.Therefore, according to mineral internal structure, precisely choose and survey year analysis position, help to disclose the chronology of geologic event
Meaning, this is also that most basic, most important primary work in year is surveyed in individual particle mineral in-situ micro area.
At present, scholars taken mostly before chronology analysis is carried out ESEM and electron probe backscatter images or
X-ray mapping mode observes the internal structure of monazite.X-ray Mapping can reflect solitary to a certain extent
The composition information of stone internal structure, but its analysis time long (in hours calculate), spatial resolution are relatively low；BSE (back scatterings
Electronic imaging) graphical analysis can fast imaging, but its reflection be element contained by monazite synthesis contrast information, image is special
Direct correlation is not present with inner structural features in sign.If it is unclear to determine year monazite inner structural features, cannot be effective
Instruct the selection of survey year analysis position, in some instances it may even be possible to the chronology result of mistake can be caused to understand.
The content of the invention
In view of this, it is an object of the invention to propose a kind of cathodoluminescence imaging method of monazite, with simple and efficient
Ground obtains the information of monazite inner structural features.
Based on above-mentioned purpose, the cathodoluminescence imaging method of monazite provided in an embodiment of the present invention comprises the following steps：
Target processed is carried out to monazite minerals particle, obtains resin target；
The resin target is polished, monazite is exposed to the resin target；
Plated film is carried out in the monazite for being exposed to the resin target, plated film is face-up, and with conducting resinl by after plated film
Resin target is fixed on the sample stage of field emission scanning electron microscope, and the sample bin of field emission scanning electron microscope is vacuumized, and makes the tree
Fat target is under vacuum condition；
Select the operating distance on monazite resin target surface；
Select the accelerating potential of electron beam；
Select the beam spot size of electron beam；
Select the high-voltage value of photomultiplier；
Obtain the image of monazite individual particle.
In some embodiments of the invention, the operating distance on the selection monazite resin target surface, including：
Monazite resin target is placed in the focal position of cathodoluminescence probe parabolic lens；
The multiple of monazite particle is amplified to whole field range；
Contrast monazite resin target be placed in cathodoluminescence probe parabolic lens focal position and its it is neighbouring when monazite figure
As feature, the operating distance that operating distance is imaged as monazite cathodoluminescence when selecting monazite image most clear.
In some embodiments of the invention, the accelerating potential of the selection electron beam, including：
The monazite image under different beam voltages is contrasted, acceleration when selecting monazite image most clear
Accelerating potential of the voltage as electron beam.
In some embodiments of the invention, the scope of the accelerating potential of the different electron beam is：500V-30kV.
In some embodiments of the invention, the accelerating potential of the different electron beam is respectively：5kV、10kV、15kV
And 20kV.
In some embodiments of the invention, the beam spot size of the selection electron beam, including：
The monazite image under different electron beam spot sizes is contrasted, beam spot when selecting monazite image most clear
Beam spot size as electron beam.
In some embodiments of the invention, the beam spot size of the different electron beam is：It is maximum from electron beam spot
Value starts, and gradually successively decreases.
In some embodiments of the invention, the high-voltage value of the selection photomultiplier, including：
The gradually high-voltage value of increase photomultiplier, and picture contrast and brightness are adjusted, until image light and shade details is clear
It is clear visible.
In some embodiments of the invention, the image for obtaining monazite individual particle, including：
It is 50-90 μ s to set every residence time of sweep speed.
In some embodiments of the invention, carbon film or golden film, thickness 2-5nm are plated；And/or
Target processed is carried out using epoxy resin.
The cathodoluminescence imaging method of monazite provided in an embodiment of the present invention is sent out using field emission scanning electron microscope and negative electrode
Photothermal spectroscopic analyzer is combined, and high-resolution cathodoluminescence luminescence imaging is carried out to monazite, and solving monazite, negative electrode is sent out all the time
The problem of finishing body is black, reach the inner structural features for clearly reflecting monazite, serve monazite in-situ micro area and determine year essence
The purpose of quasi- reconnaissance.The cathodoluminescence imaging method of monazite provided in an embodiment of the present invention causes monazite minerals internal structure
Combination with the age can be easier and accurate.
Brief description of the drawings
Fig. 1 is the comparison diagram before and after the monazite resin target surface clean of the embodiment of the present invention；
Fig. 2 is the contrast that the multiple by monazite individual particle of the embodiment of the present invention is amplified to before and after whole field range
Figure；
Fig. 3 is imaging contrast's figure that the monazite sample surfaces of the embodiment of the present invention are placed at different operating distance；
Fig. 4 is imaging contrast's figure under the different accelerating potentials of the embodiment of the present invention；
Fig. 5 is imaging contrast's figure under the different beam spot sizes of the embodiment of the present invention.
Embodiment
For the object, technical solutions and advantages of the present invention are more clearly understood, below in conjunction with specific embodiment, and reference
Accompanying drawing, the present invention is described in more detail.
Unless otherwise defined, the technical term or scientific terminology that the present invention uses, which are should be in art of the present invention, to be had
The ordinary meaning that the personage for having general technical ability is understood." first ", " second " and the similar word used in the present invention is simultaneously
Any order, quantity or importance are not indicated that, and is used only to distinguish different parts.Equally, "one", " one " or
The similar word such as person's "the" does not indicate that quantity limits yet, but represents to exist at least one." comprising " or "comprising" etc. are similar
Word mean to occur element before the word either object cover the element for appearing in the word presented hereinafter or object and its
It is equivalent, and it is not excluded for other elements or object.The similar word such as " connection " or " connected " be not limited to physics or
The connection of person's machinery, but electrical connection can be included, it is either directly or indirect.
The reason for cathodoluminescence, is mainly relevant with the addition of lattice defect, impurity or trace element, and utilizes cathodoluminescence
Technology obtains monazite inner structural features image, has no relevant report at present, its reason is mainly in monazite minerals
U, the micronutrient levels such as Th is high and cause the characteristic of weak light, with the equipment and technological means of routine, can not get at all
The signal of its cathodoluminescence.
ESEM-cathodoluminescence imaging technical principle：It is the high-power electron beam using field emission scanning electron microscope by sample
" valence-band electrons " be energized into " conduction band ", while conduction band energy is unstable, and during valence band is returned, energy is in the form of light
Release.
As one embodiment of the present of invention, the cathodoluminescence imaging method of the monazite comprises the following steps：
1) target processed is carried out to monazite minerals particle, obtains resin target；
2) the resin target is polished, monazite maximum crystal axial plane is exposed to the resin target；
3) plated film is carried out in the monazite for being exposed to the resin target, plated film is face-up, and with conducting resinl by after plated film
Resin target be fixed on the sample stage of field emission scanning electron microscope, the sample bin of field emission scanning electron microscope is vacuumized, made described
Resin target is under vacuum condition；
4) operating distance on monazite resin target surface is selected；
5) accelerating potential of electron beam is selected；
6) electron beam spot size is selected；
7) high-voltage value of photomultiplier is selected；
8) image of monazite individual particle is obtained.
Individual particle of the cathodoluminescence imaging method based on field emission scanning electron microscope of monazite provided in an embodiment of the present invention
Monazite cathodoluminescence imaging method, there can be high-resolution image with effective acquisition, to disclose its inner structural features, reach
The purpose of the year accurate reconnaissance of work is determined to in-situ micro area.
Specifically, described another embodiment of the invention, the cathodoluminescence imaging method of the monazite is including following
Step：
1) target processed is carried out to monazite minerals particle, obtains resin target.
In this step, epoxy resin target is carried out to the monazite minerals particle picked out.
2) the resin target is finely polished, monazite maximum crystal axial plane is exposed to the resin target.
In this step, monazite resin target can be polished using 100nm diamond dust cream polishing agents, makes monazite
It is exposed to the smooth no marking of surfacing of the resin target.
Further, suitable alcohols solution can also be dipped using Shu Jie board paper extraction paper handkerchiefs to enter monazite resin target surface
Row cleaning, micro- Microscopic observation, ensure that monazite resin target surface is totally pollution-free.If there is pollution on surface, can be sent out in negative electrode
In light (CL) imaging process, the various architectural features for being difficult to judge are produced, as shown in Figure 1.
3) plated film is carried out on the monazite surface for being exposed to the resin target, plated film is face-up, and will be plated with conducting resinl
Resin target after film is fixed on the sample stage of field emission scanning electron microscope, and the sample bin of field emission scanning electron microscope is vacuumized, made
The resin target is under vacuum condition.
In this step, plated film, the i.e. table in monazite particle can be carried out in the monazite for being exposed to the resin target
Face carries out plated film, and the thickness of film can be 2-5nm, ensures that monazite sample under with satisfactory electrical conductivity, reduces plating as far as possible
The thickness of film.It is alternatively possible to carry out plating carbon film or golden film, to improve electric conductivity.
Then, the monazite resin target after plated film is fixed on sample platform of scanning electronic microscope using conducting resinl, coated surface court
On.Then, vacuumize, sample bin is under high vacuum condition.
4) operating distance on monazite resin target surface is selected.
Alternatively, the step includes：
Monazite resin target is placed in the focal position of cathodoluminescence probe parabolic lens；
The multiple of monazite particle is amplified to whole field range；
Contrast monazite sample be placed in cathodoluminescence probe parabolic lens focal position and its it is neighbouring when characteristics of image, selection
The operating distance that operating distance when image is most clear is imaged as monazite cathodoluminescence, i.e., as best effort distance.
Specifically, with model FEI NovananoSEM450 ESEM and Gantan MonolCL4 cathodoluminescence light
Exemplified by spectrometer, cathodoluminescence Spectroscopy instrument selection Pan patterns, the focal position of parabolic lens is 13.5mm.I.e. by monazite resin target
Coated surface be placed at 13.5mm and be imaged, the 13.5mm of focal position at, there is maximum luminous flux, but focused spot diameter
There are~150 μm, therefore, the multiple of monazite individual particle is amplified to whole field range, just it is observed that clearly internal junction
The characteristics of image of structure, as shown in Figure 2.
Then, it is imaged respectively at focus upper-lower position, such as 13.4mm, 13.7mm and 13.9mm, carries out image comparison,
As shown in Figure 3.Being can be seen that by Fig. 3 contrast at 13.4mm, 13.7mm and 13.9mm, light source, which scatters, to be distributed in visual field,
Luminous flux is reduced, and causes imaging signal to weaken therewith, image is not clear enough.Proved by a large amount of many experiments, monazite sample
In cathodoluminescence probe focus position 13.5mm, image is most clear, in non-focus position, presents and obscures or occur without negative electrode
Luminescent image.Therefore, then the best effort distance being imaged using 13.5mm as monazite cathodoluminescence.
5) accelerating potential of electron beam is selected.
In this step, the monazite image under different beam voltages is contrasted, selects monazite image most
What accelerating potential when clear was imaged as monazite cathodoluminescence, accelerating potential, i.e., optimal accelerating potential.Alternatively, it is described
The scope of the accelerating potential of different electron beams is：500V-30kV.
Specifically, as one embodiment of the present of invention, different accelerating potential 5kV, 10kV, 15kV and 20kV are carried out
Monazite imaging contrast.Select to be imaged under 5kV first, then carry out 10kV, 15kV and 20kV imaging successively.It is because low
Accelerating potential is favorably improved the spatial resolution of cathodoluminescence (CL) image, showed fine relative to high accelerating potential
The image of structure, this determines the monazite that the not same period time be present year work and accurately instructed；But by image comparison, find
Brownout such as 5kV, can cause CL signals to weaken therewith, cause image not clear enough, can not accomplish accurately to select to surveying year position
Take；15kV and 20kV image resolution ratio is deteriorated, as shown in Figure 4.Proved by a large amount of many experiments, 10kV is best effort electricity
Pressure, ensure that the spatial resolution of CL images and enough signal collections.
6) the beam spot size of electron beam is selected.
In this step, the monazite image under different electron beam spot sizes is contrasted, selects monazite image most
The optimal beam spot value of beam spot size of the beam spot size as electron beam, i.e. cathodoluminescence imaging when clear.Alternatively, from electronics
The maximum of beam beam spot starts, and gradually successively decreases.
Specifically, as yet another embodiment of the present invention, using model FEI NovananoSEM450 ESEM as
Example, monazite imaging contrast is carried out to the numerical value 4,5,6 and 7 of different beam spot sizes.First since maximum 7, then successively
6,5 and 4 imaging is carried out, as shown in Figure 5.Because improving electron beam spot numerical value, corresponding electric current also increases, had therewith
Help produce more CL signals.But electron beam spot numerical value is excessive, the circumgranular resin of monazite can be caused soft and only
Occupy stone particle itself to be burnt, this can have a certain impact to the degree of accuracy for surveying annual bearing.Electron beam spot numerical value is too small, right
The electric current answered also decreases, then CL signals will be weak, and image noise is big, causes monazite internal structure unintelligible, to surveying
Year position can not accomplish accurately to choose.Proved by a large amount of many experiments, can when electron beam spot size elects 6 as
Ensure enough signal collection amounts, it also avoid being damaged for sample.
7) high-voltage value of photomultiplier is selected；
Optical signal is changed into electric signal and forms cathodoluminescence image by imaging detector photomultiplier (PMT), passes through tune
PMT high-voltage value is saved, strengthens the output of electric signal, it is appropriate to adjust contrast and brightness to reduce noise, improve useful signal
Intensity.Specifically, can be with the high-voltage value of cumulative big photomultiplier, and picture contrast and brightness are adjusted, until image light and shade
Details is high-visible.
According to the luminescence feature of monazite, PMT high-voltage value typically changes between -600V~-900V.
8) image of monazite individual particle is obtained.
It is 50-90 μ s to set every residence time of sweep speed.Alternatively, it is 90 to set every residence time of sweep speed
μ s, ensure that each image obtains the time at 2 minutes or so.
It should be noted that step 4) to step 8), is all first fixed other specification value, then the ginseng of the step is contrasted
Numerical value.
Therefore, the cathodoluminescence imaging method of monazite provided in an embodiment of the present invention is based on field emission scanning electron microscope, can
There is high-resolution image with effective acquisition, to disclose its inner structural features, determine year work essence so as to reach in-situ micro area
The purpose of true reconnaissance.
Case study on implementation one
Granite sample：Monazite particle is picked out, is imaged according to imaging method provided by the invention, will be handled well
Monazite resin target be fixed on two-sided carbonaceous conductive glue on the sample stage of FEI NovananoSEM450 ESEMs, energy
High-resolution cathodoluminescence image is accessed, clearly the feature of the visible rhythm oscillatory zones magma monazite of internal structure；Enter
Row SIMS monazites U-Pb determines year, and it is consistent to determine annual bearing with original zircons.Therefore, imaging method provided in an embodiment of the present invention has
Direct to effect magma monazite determines year work.
Case study on implementation two
Granulite sample：Monazite particle is picked out, is imaged according to imaging method provided by the invention, will be located
The monazite resin target managed is fixed on the sample stage of FEI NovananoSEM450 ESEMs with two-sided carbonaceous conductive glue
On, high-resolution cathodoluminescence image, the rotten monazite feature of high-visible core-side structure more phases time can be obtained；Respectively
SIMS monazites U-Pb is carried out to core portion and edge and determines year, obtains the close age, this shows that the earth's crust have passed through a quick lift
The process risen.Therefore, imaging method provided in an embodiment of the present invention is determined to do geologic event in year work in monazite
Go out rationally appropriate explanation.
Therefore, the cathodoluminescence imaging method of monazite provided in an embodiment of the present invention uses field emission scanning electron microscope and the moon
Pole luminescence spectrometer is combined, and carries out high-resolution cathodoluminescence luminescence imaging to monazite, it is all the time cloudy to solve monazite
The problem of extremely luminous overall black, reach the inner structural features for clearly reflecting monazite, serve monazite in-situ micro area and determine
The purpose of year accurate reconnaissance.The cathodoluminescence imaging method of monazite provided in an embodiment of the present invention causes inside monazite minerals
The combination at structure and age can be easier and accurate.
Those of ordinary skills in the art should understand that：The discussion of any of the above embodiment is exemplary only, not
It is intended to imply that the scope of the present disclosure (including claim) is limited to these examples；Under the thinking of the present invention, above example
Or can also be combined between the technical characteristic in different embodiments, and the different aspect of the present invention as described above be present
Many other changes, in order to it is concise they do not provided in details.Therefore, within the spirit and principles of the invention,
Any omission for being made, modification, equivalent substitution, improvement etc., should be included in the scope of the protection.
Claims (10)
1. the cathodoluminescence imaging method of a kind of monazite, it is characterised in that comprise the following steps：
Target processed is carried out to monazite minerals particle, obtains resin target；
The resin target is polished, monazite is exposed to the resin target；
Plated film is carried out in the monazite for being exposed to the resin target, plated film is face-up, and with conducting resinl by the resin after plated film
Target is fixed on the sample stage of field emission scanning electron microscope, and the sample bin of field emission scanning electron microscope is vacuumized, and makes the resin target
Under vacuum condition；
Select the operating distance on monazite resin target surface；
Select the accelerating potential of electron beam；
Select the beam spot size of electron beam；
Select the high-voltage value of photomultiplier；
Obtain the image of monazite individual particle.
2. the cathodoluminescence imaging method of monazite according to claim 1, it is characterised in that the selection monazite tree
The operating distance on fat target surface, including：
Monazite resin target is placed in the focal position of cathodoluminescence probe parabolic lens；
The multiple of monazite particle is amplified to whole field range；
Contrast monazite resin target be placed in cathodoluminescence probe parabolic lens focal position and its it is neighbouring when monazite image it is special
Sign, the operating distance that operating distance is imaged as monazite cathodoluminescence when selecting monazite image most clear.
3. the cathodoluminescence imaging method of monazite according to claim 1, it is characterised in that the selection electron beam
Accelerating potential, including：
The monazite image under different beam voltages is contrasted, accelerating potential when selecting monazite image most clear
Accelerating potential as electron beam.
4. the cathodoluminescence imaging method of monazite according to claim 3, it is characterised in that the different electron beam
The scope of accelerating potential be：500V-30kV.
5. the cathodoluminescence imaging method of monazite according to claim 4, it is characterised in that the different electron beam
Accelerating potential be respectively：5kV, 10kV, 15kV and 20kV.
6. the cathodoluminescence imaging method of monazite according to claim 1, it is characterised in that the selection electron beam
Beam spot size, including：
The monazite image under different electron beam spot sizes is contrasted, beam spot conduct when selecting monazite image most clear
The beam spot size of electron beam.
7. the cathodoluminescence imaging method of monazite according to claim 6, it is characterised in that the different electron beam
Beam spot size be：Since electron beam spot maximum, gradually successively decrease.
8. the cathodoluminescence imaging method of monazite according to claim 1, it is characterised in that the selection photomultiplier transit
The high-voltage value of pipe, including：
The gradually high-voltage value of increase photomultiplier, and picture contrast and brightness are adjusted, until image light and shade details clearly may be used
See.
9. the cathodoluminescence imaging method of monazite according to claim 1, it is characterised in that the acquisition monazite list
The image of particle, including：
It is 50-90 μ s to set every residence time of sweep speed.
10. the cathodoluminescence imaging method of monazite according to claim 1, it is characterised in that plating carbon film or golden film,
Thickness is 2-5nm；And/or
Target processed is carried out using epoxy resin.
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| CN114609093A (en) * | 2022-03-24 | 2022-06-10 | 合肥工业大学 | Method for calculating scattering phase function of imaging turbidimeter based on fisheye lens |
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| CN111272797B (en) * | 2020-03-09 | 2021-06-25 | 中南大学 | Mineral exploration method for judging mineralization of granite body by using zircon |
| CN114295664A (en) * | 2021-12-16 | 2022-04-08 | 中国煤炭地质总局勘查研究总院 | Method for detecting rare earth elements in minerals by using cathodoluminescence |
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