CN107966337A - The baddeleyite preparation method in situ for surveying year sample in basic-ultrabasic rock - Google Patents
The baddeleyite preparation method in situ for surveying year sample in basic-ultrabasic rock Download PDFInfo
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- CN107966337A CN107966337A CN201711122625.5A CN201711122625A CN107966337A CN 107966337 A CN107966337 A CN 107966337A CN 201711122625 A CN201711122625 A CN 201711122625A CN 107966337 A CN107966337 A CN 107966337A
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
The invention discloses a kind of preparation method in situ for surveying year sample of baddeleyite in gold-bearing property, including：Gold-bearing property sample on the chip sample is divided into more sub-regions；To the chip sample spraying plating conductive material；Zr element in gold-bearing property sample is found by scanning electron microscope energy disperse spectroscopy, obtains zr element mapping；The position for zr element peak occur in the gold-bearing property sample of Electronic Speculum is navigate in the visible visual field；Determine the position of the baddeleyite mineral in the gold-bearing property sample in the visual field；The position of the baddeleyite mineral is marked on gold-bearing property sample；Drill through the mineral baddeleyite marked.The present invention can solve the problems, such as to be difficult to sub-elect baddeleyite from gold-bearing property.
Description
Technical field
The present invention relates to a kind of survey year sample in situ of baddeleyite in dating technology field, more particularly to basic-ultrabasic rock
Preparation method.
Background technology
Baddeleyite (ZrO2) be a kind of common accessory mineral, be silicon is unsaturated or critical saturation conditions under formed, its
There are output, such as kimberlite, carbonatite, syenite, basic-ultrabasic rock and spherolite igneous rock in various rock types
Deng.
Baddeleyite is preferable and reliable geology timer.Accurate li of the crystallization epoch of basic-ultrabasic rock intrusive body
Fixed is exactly to rely on baddeleyite U-Pb isotope methods.Main cause is：Baddeleyite is tied late period mafic magma crystallization differentiation
It is brilliant；Include the high U of various concentrations and insignificant initial p b contents；It is substantially absent from basic-ultrabasic rock to catch
Carry off inheritance baddeleyite existing for crystalline form；With zircon (ZrSiO4) compare, it is not susceptible to the phenomenon of Pb loss.It is oblique as can be seen here
Zircon is significant to the Chronologic Study of basic-ultrabasic rock.
Zircon, monazite for intermediate-felsic rock etc. survey year accessory mineral, and conventional sample preparation methods are：Rock Powder
It is broken to 200 mesh, pick out mineral grain using the methods of table concentration.This method is applied to be sorted in basic-ultrabasic rock
Effect is very poor during baddeleyite, and Major Difficulties are：1. baddeleyite amount commonly is seldom and crystal grain is very tiny, general width
Less than 30 μm；2. baddeleyite brittleness is big, during rock sample smashes, it is easy to be broken into the particle of smaller, cause
Easily it is missed during sieving；3. the diversity of baddeleyite physical aspect so that be difficult to recognize in election process, cause
The baddeleyite mineral purity chosen is inadequate；4. during sorting mineral, the unmanageable increasing of shaking table condition when sorting baddeleyite
Technical difficulty is added.
Therefore, by traditional method sub-elected from basic-ultrabasic rock baddeleyite need to expend substantial amounts of sample it is (several
Ten even up to a hundred kilograms of rocks), when sample size Datong District, brings the puzzlement of distinguishing period length, it is important to substantial amounts of sample sorting effect
Fruit is not necessarily good, is difficult often to choose up to a hundred baddeleyites, there may come a time when to pick out several, or even do not find out.In recent years, oblique zirconium
Stone Secondary Ion Mass Spectrometry (SIMS) original position U-Pb dating technologies are gradually ripe, yet with above-mentioned influence sample preparation it is many because
Element, baddeleyite sample selects and has been prepared into the bottleneck for restricting dating technology in mafic-Ultrabasic.
The content of the invention
In view of this, the embodiment of the present invention provides baddeleyite in a kind of basic-ultrabasic rock the preparation in situ for surveying year sample
Method, can solve the problems, such as to be difficult to sub-elect baddeleyite from basic-ultrabasic rock.
To achieve the above object, an embodiment of the present invention provides a kind of survey year sample in situ of baddeleyite in basic-ultrabasic rock
The preparation method of product, including：
Basic-ultrabasic rock sample is placed on glass slide, obtains chip sample；
Basic-ultrabasic rock sample on the chip sample is divided into more sub-regions；
To the chip sample spraying plating conductive material；
Zr element in basic-ultrabasic rock sample is found by scanning electron microscope energy disperse spectroscopy, obtains zr element mapping；
The position for zr element peak occur in the basic-ultrabasic rock sample of Electronic Speculum is navigate in the visible visual field；
Determine the position of the baddeleyite mineral in the basic-ultrabasic rock sample in the visual field；
The position of the baddeleyite mineral is marked on basic-ultrabasic rock sample；
Drill through the mineral baddeleyite marked.
In some embodiments of the invention, the zirconium member in basic-ultrabasic rock sample is found by scanning electron microscope power spectrum
Element, obtains zr element mapping, including：
The chip sample for being sprayed with conductive material is placed in scanning electron microscope example storehouse, and is fixed on sample stage, then
Zr element in basic-ultrabasic rock sample is found by energy dispersion X-ray detector, obtains zr element mapping.
In some embodiments of the invention, the zirconium in basic-ultrabasic rock sample is found by scanning electron microscope energy disperse spectroscopy
Element, obtains zr element mapping, including：
It is multiple units by each sub-zone dividing；
Find the zr element in each unit one by one by scanning electron microscope energy disperse spectroscopy, obtain the corresponding single width zirconium of each unit
Element area profile；
All single width zr element mappings are spliced into the corresponding zr element mapping of the subregion.
In some embodiments of the invention, the method further includes：
Epoxy resin standard target is made in the baddeleyite for drilling through out and standard specimen together under the microscope, is mafic-super
Baddeleyite is in situ in basic rock surveys year sample.
In some embodiments of the invention, the basic-ultrabasic rock sample on the chip sample is divided into multiple
Subregion, including：
Basic-ultrabasic rock sample average on the chip sample is divided into more sub-regions.
In some embodiments of the invention, on basic-ultrabasic rock sample to the positions of the baddeleyite mineral into
Line flag, including：
Cut using Ga ions and cut on basic-ultrabasic rock sample, to mark the baddeleyite mineral
Position.
In some embodiments of the invention, the conductive material is carbon.
In some embodiments of the invention, the thickness of the conductive material is 1-10 nanometers.
Advantages of the present invention：
Compared to traditional smashing sieving, the method for separation by shaking table, preparation method provided by the invention substantially increases oblique zirconium
Stone selects efficiency, and amount of samples greatly reduces, and pollution-free.
Further effect adds hereinafter in conjunction with embodiment possessed by above-mentioned non-usual optional mode
With explanation.
Brief description of the drawings
Attached drawing is used to more fully understand the present invention, does not form inappropriate limitation of the present invention.Wherein：
Fig. 1 is the region division schematic diagram of chip sample according to embodiments of the present invention.
Embodiment
Explain below in conjunction with attached drawing to the one exemplary embodiment of the present invention, including the various of the embodiment of the present invention
Details should think them only exemplary to help understanding.Therefore, those of ordinary skill in the art should recognize
Arrive, various changes and modifications can be made to the embodiments described herein, without departing from scope and spirit of the present invention.Together
Sample, for clarity and conciseness, eliminates the description to known function and structure in following description.
Step 1：Basic-ultrabasic rock sample is cut, is roughly ground, is placed on glass slide, obtains chip sample.
Specifically, the fresh basic-ultrabasic rock sample gathered cut, roughly ground, after cutting, corase grinding
Sample is sticked on glass slide, sample of laminating together with glass slide.For example, 5 centimetres long, 2 centimetres wide, thickness can be made
50 microns of chip sample, the size of the basic-ultrabasic rock sample is less than the size of glass slide, but is not limited to the ruler
It is very little.
It is alternatively possible to two surfaces of basic-ultrabasic rock sample are all cut successively, are roughly ground, fine grinding, throwing
Light, in order to sample that it laminates together with glass slide, is also convenient for follow-up positioning, target processed etc..
Step 2：Basic-ultrabasic rock sample on the chip sample is divided into more sub-regions.
Specifically, the basic-ultrabasic rock sample on the chip sample ground is divided into 3-8 sub-regions.It is optional
Ground, along the length direction of the chip sample, is divided into 3-8, i.e., per height by the basic-ultrabasic rock sample average
The area in region is identical.The division of suitable average area is carried out to the basic-ultrabasic rock sample on chip sample, can be kept away
Exempting from sample area causes greatly the baddeleyite of fine particle to be submerged very much, and cannot be found, while if dividing too many region,
Again efficiency can be made to become low.
As shown in Figure 1, basic-ultrabasic rock sample is divided into 5 sub-regions, and every sub-regions length and width, thick phase
Together, it is respectively 1 centimetre, 2 centimetres and 50 microns., can also be by basic-ultrabasic rock sample as another embodiment of the present invention
Product are divided into 4 sub-regions, 6 sub-regions etc., and every sub-regions length and width, thickness are identical.
Step 3：To the chip sample spraying plating conductive material.
Alternatively, basic-ultrabasic rock sample (is sprayed with using surface spraying plating conductive material of the spraying plating instrument in chip sample
A side surface), to ensure that the surface of basic-ultrabasic rock sample is coated with continuous conductive material, and in scanning electron microscope electricity
It is conductive under the bombardment of beamlet.
As one embodiment of the present of invention, the conductive material can be carbon, to chip sample spraying plating carbon, with sample
Surface plates continuous carbon film.As another embodiment of the present invention, the thickness of the conductive material can be 1-10 nanometers.
Under the thickness range, sample conduction can be not only ensured, but also do not interfere with observation sample.For example, it can be 5 nanometers,
It can be 3.5 nanometers, 6.6 nanometers etc..
Step 4：Zr element in basic-ultrabasic rock sample is found by scanning electron microscope energy disperse spectroscopy, obtains zr element face
Distribution map.
In this step, the chip sample for being sprayed with conductive material is placed in scanning electron microscope example storehouse, and is fixed on sample
In sample platform, zirconium (Zr) element in basic-ultrabasic rock sample is then found by energy dispersion X-ray detector.Specifically,
By the one side for being sprayed with conductive material upward, it is fixed on sample stage, vacuumized using conducting resinl (such as carbonaceous conductive glue),
Plus high pressure, it is 5 to select accelerating potential 15kV, Spot size, and operating distance WD is 6mm.
Then, the zr element in finding one by one per sub-regions, obtains the corresponding zr element mapping of every sub-regions.
Specifically, it is multiple units by each sub-zone dividing, finds the zr element in each unit one by one, obtains each unit and correspond to
Single width zr element mapping；All single width zr element mappings are spliced into the corresponding zr element of the subregion again
Mapping.
Alternatively, as an alternative embodiment of the invention, as shown in Figure 1, exemplified by being averagely divided into 5 sub-regions,
The subregion 1 of basic-ultrabasic rock chip sample is selected, sets the coordinate position of two points of diagonal (A and B), single width figure
Amplification factor (generally 120 times) and pixel (generally 1024), through system-computed, 1 (length and width of region：1 centimetre * 2 lis
Rice) it there are about 300 width pictures (i.e. 300 units) altogether；Meanwhile target Zr elements are added in distribution map details, i.e., with Zr
For element as object element, the Element area profile of operation area 1, finds the zr element in each unit one by one, obtains each
The corresponding single width zr element mapping of unit；After end of run, this 300 single width zr element mappings are spliced into one
Big figure, the Zr Element area profiles of last output area 1.
After region 1 is completed, the zr element EDS maps of the corresponding subregion of the step are carried out to region 2,3,4,5 one by one
Figure.
It should be noted that in the mapping of basic-ultrabasic rock sample, there is the only zircon at Zr elements peak
(ZrSiO4) and baddeleyite (ZrO2) two kinds of mineral, Zr elements may also be contained in other mineral, but since its is micro, scanning electricity
The energy dispersion X-ray detector of mirror can not detect Zr elements, thus exclude non-targeted mineral.The present invention is using power spectrum face point
Pattern splicing method in Butut, the EDS maps for carrying out all elements in region scan, the foundation Zr elemental map locations drawing, so as to
Zircon (ZrSiO is accurately positioned out4) and baddeleyite (ZrO2) both mineral.
Step 5：The position for zr element peak occur in the basic-ultrabasic rock sample of Electronic Speculum is navigate into the visible visual field
In.
Specifically, observe in Zr Element area profiles and the region of Zr elements occur, utilize the coordinate between Electronic Speculum and power spectrum
Association, the position for occurring Zr elements peak in the chip sample of Electronic Speculum is navigate in the visible visual field.
Step 6：Determine the position of the baddeleyite mineral in the basic-ultrabasic rock sample in the visual field.
Specifically, the chip sample in the visual field is amplified to suitable multiple, selects energy dispersion X-ray detector
(EDX) Point ID carry out point analysis in, observe element spectral peak feature to be confirmed whether it is baddeleyite mineral (ZrO2), exclude
Other possible interference signals and caused by vacation Zr peaks.
Sxemiquantitative constituent analysis is carried out to mineral using power spectrum point analysis, and then mineral are differentiated, wherein zircon
(ZrSiO4) compared to baddeleyite (ZrO2) more Si and two O in power spectrum point analysis, so as to identify the oblique zirconium of target mineral
Stone.
Step 7：The position of the baddeleyite mineral is marked on basic-ultrabasic rock sample.
In this step, the baddeleyite obtained using gallium (Ga) ion on basic-ultrabasic rock sample to mapping
Surrounding carries out ion cutting, to mark the position of the baddeleyite mineral.
Specifically, another embodiment as the present invention, focused ion beam scanning electron microscopy is moved into by chip sample
In mirror (FIB-SEM), all cut near the baddeleyite that is found in 5 regions of thin slice using Ga ions, and make position
Mark.It ensure that after taking out chip sample from Electronic Speculum, moreover it is possible to the position of the target mineral baddeleyite of accurate definite micron level.
The present invention is made marks using the Ga ion guns of FIB-SEM at target mineral baddeleyite, to position in micro-scale, precisely to divide
Separate out baddeleyite.
Step 8：Drill through the mineral baddeleyite marked.
Specifically, chip sample is taken out from scanning electron microscope energy disperse spectroscopy, utilizes micro- all targets for drilling through and having marked
Mineral baddeleyite.
Because baddeleyite SIMS U-Pb, which survey year, at least needs 15, in order to guarantee to search out enough baddeleyites
Grain, can circulate the process that previous step one arrives step 8, until finding sufficient amount of baddeleyite particle.
Step 9：Epoxy resin standard target is made in the baddeleyite for drilling through out and standard specimen together under the microscope, light mill
And polish, being that baddeleyite is in situ in basic-ultrabasic rock surveys year sample, you can for Secondary Ion Mass Spectrometry (SIMS) survey in situ
Year analysis.
Baddeleyite mineral growth is fewer in basic-ultrabasic rock sample, and surveying year sample at least needs 15 baddeleyites,
This needs grinds as big as possible or multi-block thin slice sample to increase the discovery probability of baddeleyite.But by scanning electron microscope visual field model
Limitation is enclosed, the size about 1mm*1mm of its single breadth distribution map under minimum multiple, can not cover whole chip sample.It is right
In a chip sample general in geology, when large area EDS maps picture mosaic, (it is less than because the particle diameter of baddeleyite is too small more
30 μm), cause it to be resolved out in mapping.Therefore, method provided by the invention is first to large-sized thin slice
Suitable area size is divided into, EDS maps picture mosaic scanning then is carried out to every sub-regions one by one, so as to ensure baddeleyite
It was found that probability.
Moreover, scanning electron microscope can carry out microcosmic imaging, scanning electron microscope power spectrum (SEM- to the material performance of sample surfaces material
EDX) mapping can carry out image elemental map, the distribution characteristics of the mainly mineral Main elements of reflection.
Limited by scanning electron microscope field range, although under minimum multiple single breadth distribution map size about 1mm*1mm,
Whole chip sample far can not be covered, however, the picture mosaic in power spectrum mapping can be automatically performed all of whole region
The EDS maps of element.Meanwhile power spectrum point analysis can carry out sxemiquantitative constituent analysis to mineral, and then mineral are differentiated,
Such as zircon (ZrSiO4) compared to baddeleyite (ZrO2) should be more Si and two O in power spectrum point analysis；Focused ion
Beam-scanning electron microscope (FIB-SEM) double-beam system can carry out position mark using Ga ion etchings sample.
Embodiment 1
Step 1：The basalt sample 2kg that Changbai Mountain is fresh is taken, it is automatic using SPQJ-300 types slicer, MG-301 types
Wafer lapping machine and ML-180 type automatic polishing machines are cut, ground and are polished respectively, are then sticked on glass slide, with glass slide one
Rise and 10 chip samples are made (first with a sample, remaining 9 in this, as spare).For example, can be made 5 lis long
Rice, 2 centimetres wide, 50 microns thick chip sample, the size of the basic-ultrabasic rock sample are less than the size of glass slide, but
It is not limited to the size.
It is alternatively possible to two surfaces of basic-ultrabasic rock sample are all cut successively, are roughly ground, fine grinding, throwing
Light, in order to sample that it laminates together with glass slide, is also convenient for follow-up positioning, target processed etc..
Step 2：The division of 5 sub-regions average parallels is carried out to the basic-ultrabasic rock sample on chip sample, with note
Number pen has marked the position of ABCDEF.
Step 3：It is thick to chip sample plating carbon 5nm using card EM ACE200 spraying platings instrument is come.
Step 4：By the sample one side for having plated carbon upward, it is fixed in carbonaceous conductive glue on sample stage, is placed in FEI
In Nova NanoSEM450 scanning electron microscope examples storehouse, vacuumize, plus high pressure, selection accelerating potential 15kV, Spot size is
5, operating distance WD are 6mm；In the Oxford Aztec X-ray energy spectrometers (EDX) of model X-MAXN80, setting area 1 is right
The coordinate position of two points of linea angulata (A and B), single width figure amplify 120 times and pixel 1024, target Zr elements in addition, progress
The automatic picture mosaic of large area in the region；After region 1 is completed, the corresponding EDS maps of the step progressively are carried out to region 2,3,4,5
Figure；5 regions export its Zr Element area profile to more than one by one, observed multiple Zr elements peaks.
Step 5：Using Electronic Speculum airmanship, Zr elements peak position is returned to one by one and amplifies the region in the visual field.
Step 6：Whether Point ID carry out Zr elements peak that point analysis confirms that each occurs for oblique zirconium in selection EDX
Stone ore thing (ZrO2), exclude other possible interference signals and caused by vacation Zr peaks, confirm 3 baddeleyites altogether.
Step 7：The chip sample is moved into focused ion beam-scanning of model Zeiss Auriga Compact
In electron microscope (FIB-SEM) double-beam system, cut near the baddeleyite found using Ga ion beams, make position
Mark.
Step 8：Chip sample is taken out from FIB-SEM, target mineral baddeleyite is drilled through using micro-；More than repeating
Step, has searched out altogether 19 baddeleyites in 4 plate sheets.
Step 9：Epoxy resin mark is made in all baddeleyites for drilling through out and Phalaborwa baddeleyites standard specimen together
Quasi- target, gently grinds and polishes, that is, completes the SIMS U-Pb preparations in situ for surveying year baddeleyite sample.
Advantages of the present invention：
Compared to traditional smashing sieving, the method for separation by shaking table, preparation method provided by the invention substantially increases oblique zirconium
Stone selects efficiency, and amount of samples greatly reduces, and pollution-free.
Above-mentioned embodiment, does not form limiting the scope of the invention.Those skilled in the art should be bright
It is white, depending on design requirement and other factors, various modifications, combination, sub-portfolio and replacement can occur.It is any
Modifications, equivalent substitutions and improvements made within the spirit and principles in the present invention etc., should be included in the scope of the present invention
Within.
Claims (8)
- A kind of 1. baddeleyite preparation method in situ for surveying year sample in basic-ultrabasic rock, it is characterised in that including：Basic-ultrabasic rock sample is placed on glass slide, obtains chip sample；Basic-ultrabasic rock sample on the chip sample is divided into more sub-regions；To the chip sample spraying plating conductive material；Zr element in basic-ultrabasic rock sample is found by scanning electron microscope energy disperse spectroscopy, obtains zr element mapping；The position for zr element peak occur in the basic-ultrabasic rock sample of Electronic Speculum is navigate in the visible visual field；Determine the position of the baddeleyite mineral in the basic-ultrabasic rock sample in the visual field；The position of the baddeleyite mineral is marked on basic-ultrabasic rock sample；Drill through the mineral baddeleyite marked.
- 2. the baddeleyite preparation method in situ for surveying year sample, its feature exist in basic-ultrabasic rock according to claim 1 In, the zr element in basic-ultrabasic rock sample is found by scanning electron microscope power spectrum, obtains zr element mapping, including：The chip sample for being sprayed with conductive material is placed in scanning electron microscope example storehouse, and is fixed on sample stage, is then passed through Energy dispersion X-ray detector finds the zr element in basic-ultrabasic rock sample, obtains zr element mapping.
- 3. the baddeleyite preparation method in situ for surveying year sample, its feature exist in basic-ultrabasic rock according to claim 1 In, the zr element in basic-ultrabasic rock sample is found by scanning electron microscope energy disperse spectroscopy, obtains zr element mapping, including：It is multiple units by each sub-zone dividing；Find the zr element in each unit one by one by scanning electron microscope energy disperse spectroscopy, obtain the corresponding single width zr element of each unit Mapping；All single width zr element mappings are spliced into the corresponding zr element mapping of the subregion.
- 4. the baddeleyite preparation method in situ for surveying year sample, its feature exist in basic-ultrabasic rock according to claim 1 In further including：Epoxy resin standard target is made in the baddeleyite for drilling through out and standard specimen together under the microscope, is mafic-Ultrabasic Baddeleyite is in situ in rock surveys year sample.
- 5. the baddeleyite preparation method in situ for surveying year sample, its feature exist in basic-ultrabasic rock according to claim 1 In, the basic-ultrabasic rock sample on the chip sample is divided into more sub-regions, including：Basic-ultrabasic rock sample average on the chip sample is divided into more sub-regions.
- 6. the baddeleyite preparation method in situ for surveying year sample, its feature exist in basic-ultrabasic rock according to claim 1 In, the position of the baddeleyite mineral is marked on basic-ultrabasic rock sample, including：Ion cutting is carried out around the baddeleyite obtained using gallium ion on basic-ultrabasic rock sample to mapping, with Mark the position of the baddeleyite mineral.
- 7. the baddeleyite preparation method in situ for surveying year sample, its feature exist in basic-ultrabasic rock according to claim 1 In the conductive material is carbon.
- 8. the baddeleyite preparation method in situ for surveying year sample, its feature exist in basic-ultrabasic rock according to claim 1 In the thickness of the conductive material is 1-10 nanometers.
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| CN109342288A (en) * | 2018-11-02 | 2019-02-15 | 中国石油天然气股份有限公司 | Characterization method of shale reservoir pore space |
| CN111272797A (en) * | 2020-03-09 | 2020-06-12 | 中南大学 | Mineral exploration method for judging mineralization of granite body by using zircon |
| CN111999325A (en) * | 2020-08-20 | 2020-11-27 | 合肥工业大学 | Method for searching in-situ zircon in bedrock |
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