NL2032037A - Method and equipment for delivering dynamic deformation beam spots by la-icp-ms - Google Patents
Method and equipment for delivering dynamic deformation beam spots by la-icp-ms Download PDFInfo
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- NL2032037A NL2032037A NL2032037A NL2032037A NL2032037A NL 2032037 A NL2032037 A NL 2032037A NL 2032037 A NL2032037 A NL 2032037A NL 2032037 A NL2032037 A NL 2032037A NL 2032037 A NL2032037 A NL 2032037A
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- 238000000034 method Methods 0.000 title claims abstract description 38
- 238000000095 laser ablation inductively coupled plasma mass spectrometry Methods 0.000 title claims description 31
- 238000009826 distribution Methods 0.000 claims abstract description 34
- 238000002679 ablation Methods 0.000 claims description 26
- 239000012159 carrier gas Substances 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 14
- 230000005284 excitation Effects 0.000 claims description 12
- 239000002775 capsule Substances 0.000 claims description 5
- 239000004973 liquid crystal related substance Substances 0.000 claims description 5
- 230000008033 biological extinction Effects 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims 1
- 238000000576 coating method Methods 0.000 claims 1
- 239000000523 sample Substances 0.000 description 86
- 239000012071 phase Substances 0.000 description 37
- 229910052500 inorganic mineral Inorganic materials 0.000 description 29
- 239000011707 mineral Substances 0.000 description 29
- 235000010755 mineral Nutrition 0.000 description 23
- 230000000875 corresponding effect Effects 0.000 description 22
- 238000010586 diagram Methods 0.000 description 16
- 238000005070 sampling Methods 0.000 description 11
- 238000004458 analytical method Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 238000002156 mixing Methods 0.000 description 5
- 239000012535 impurity Substances 0.000 description 4
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 4
- 230000001788 irregular Effects 0.000 description 4
- 238000002834 transmittance Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000004364 calculation method Methods 0.000 description 3
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- 238000005516 engineering process Methods 0.000 description 3
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- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
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- 241000894007 species Species 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 235000013619 trace mineral Nutrition 0.000 description 2
- 239000011573 trace mineral Substances 0.000 description 2
- 229910052845 zircon Inorganic materials 0.000 description 2
- 206010001497 Agitation Diseases 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
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- 229910052729 chemical element Inorganic materials 0.000 description 1
- ZPUCINDJVBIVPJ-LJISPDSOSA-N cocaine Chemical compound O([C@H]1C[C@@H]2CC[C@@H](N2C)[C@H]1C(=O)OC)C(=O)C1=CC=CC=C1 ZPUCINDJVBIVPJ-LJISPDSOSA-N 0.000 description 1
- 238000002591 computed tomography Methods 0.000 description 1
- 238000011840 criminal investigation Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000010433 feldspar Substances 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 239000002223 garnet Substances 0.000 description 1
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- 239000011521 glass Substances 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical compound O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- 230000007775 late Effects 0.000 description 1
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- 229910052683 pyrite Inorganic materials 0.000 description 1
- 239000011028 pyrite Substances 0.000 description 1
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 1
- 229910052611 pyroxene Inorganic materials 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
- H01J49/0459—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components for solid samples
- H01J49/0463—Desorption by laser or particle beam, followed by ionisation as a separate step
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/626—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using heat to ionise a gas
-
- G—PHYSICS
- 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
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B27/00—Optical systems or apparatus not provided for by any of the groups G02B1/00 - G02B26/00, G02B30/00
- G02B27/09—Beam shaping, e.g. changing the cross-sectional area, not otherwise provided for
- G02B27/0927—Systems for changing the beam intensity distribution, e.g. Gaussian to top-hat
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- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Optics & Photonics (AREA)
- Electrochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Sampling And Sample Adjustment (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
A method and equipment for delivering a dynamic deformation beam spot by LArICP—MS are provided; the method includes: obtaining a surface phase boundary shape of a sample and a three—dimensional phase distribution inside the sample; determining a target grain and, a standard, sample according to the three—dimensional phase distribution, and performing laser spot control on the standard sample to obtain a beam spot of the target grain; obtaining each ablated layer according to the three—dimensional phase distribution; determining a change sequence on cross—section shapes of the target grain of a corresponding sample of a beam deformable piece according to the cross—section shape of the ablated, layer of the target grain corresponding to the three— dimensional phase distribution; performing frame—by—frame operation on the beam deformable piece according to the order of the change sequence on cross—section shapes of the target grain such that the sample is ablated by the light beam.
Description
P1357 /NL
METHOD AND EQUIPMENT FOR DELIVERING DYNAMIC DEFORMATION BEAM SPOTS
BY LA-ICP-MS
The present invention relates to the field of testing tech- nology for geological samples ablated by dynamic deformation laser beam spots; and in particular to a method and equipment for deliv- ering dynamic deformation beam spots by LA-ICP-MS.
The existing laser ablation-inductively coupled plasma-mass spectrometry (collectively referred to LA-ICP-MS) methods and equipment can be applied to solid phase composition analysis, in- cluding the fields such as, geology, materials science, criminal investigation, archaeology and environmental science. Geological samples are featured by complicated and changeable micro- topography; based on the features of the LA-ICP-MS method and equipment known to the public, the cross-section shape of a beam spot can only be determined through aperture with a fixed shape, but the cross-section shape of a beam spot is nondeformable during laser ablation, which will ablate all the composition within the beam spot region, leading to difficulties in real-time change and selection of beam spot shape, thereby causing the problem of blending impurities into ablation points.
Even though a method for continuous adjustment of spatial form of focusing optical fiber laser beams has been disclosed in the prior art, the defocusing distance corresponding to the beam spatial form required by actual processing needs to be obtained by calculation. The distance from top to bottom of the adjustable cladding head is adjusted continuously vertically to achieve the purpose of changing the defocusing distance on the finished sur- face continuously, such that the continuous adjustment on the spa- tial form of laser beams can be achieved. It is commonly known that LA-ICP-MS pulse laser will change the surface topography and defocusing distance of a sample every ablation. Moreover, when the sample is a geological sample, the distance from top to bottom of the adjustable cladding head is adjusted only to change the defo- cusing distance, which will still make non-target grains within beam spots ablated; these calculation and adjustment steps to the laser beams adjustment are time-consuming.
The prior art further discloses a spatial shaping device for laser beams; the filter holes are located at the focal point (en- ergy density is up to the maximum) of a confocal system; the beam shaping can be achieved only when the beam within the energy range that the filter holes are not ablated, which cannot achieve the deformation of the laser beam spot within the LA-ICP-MS ablation energy range and thus, does not conform to the technical require- ments of LA-ICP-MS.
To overcome the shortcomings of the prior art, the objective of the present invention is to provide a method and equipment for delivering dynamic deformation beam spots by LA-ICP-MS.
To achieve the objective above, the present invention pro- vides the following solutions: a method for delivering dynamic deformation beam spots by LA-
ICP-MS, including the following steps: obtaining a surface phase boundary shape of a sample and a three-dimensional phase distribution inside the sample; determining a target grain and a standard sample according to the three-dimensional phase distribution of the sample, and per- forming laser spot control on the standard sample to obtain a beam spot of the target grain; obtaining each ablated layer according to the three- dimensional phase distribution, and determining a change sequence on cross-section shapes of the target grain of a corresponding sample of a beam deformable piece according to the cross-section shape of the ablated layer of the target grain corresponding to the three-dimensional phase distribution, where a bright area of the beam deformable piece has a shape corresponding to a geometri- cally similar graph of the cross-section shape of the beam spot to be ablated;
performing frame-by-frame operation on the beam deformable piece according to the order of the change sequence on cross- section shapes of the target grain, such that the sample is ablat- ed by a light beam; when the sample is ablated by the light beam for once, the beam deformable piece is changed for a next one in a deeper position of the corresponding sample, thus changing the shape of the beam spot successively to implement LA-ICP-MS.
Preferably, when the beam deformable piece is operated frame by frame, the light beam transmits through the beam deformable piece via parallel light beyond a double focal length of a lens.
Preferably, when the target grain has a position with a con- stant vertical cross-section shape in the three-dimensional phase distribution, the shape of the beam spot ablated at least for two times is not changed after the light beam transmits through the beam deformable piece.
Preferably, the step of obtaining each ablated layer accord- ing to the three-dimensicnal phase distribution includes the fol- lowing steps: obtaining a volume and a depth of internal phase distribution according to the three-dimensional phase distribution; obtaining the ablated layer according to an ablation rate of each phase, the volume and the depth; where the ablation rate is obtained when the standard sample is subjected to laser spot con- trol.
Preferably, the position of the beam spot is restrained by the surface phase boundary shape.
Preferably, the light beam transmits through the beam deform- able piece via a parallel or confocal way; the light beam is al- lowed to transmit when the beam deformable piece pauses; the pause period of the beam deformable piece is not less than a single pulse period of the light beam.
Equipment for delivering dynamic deformation beam spots by
LA-ICP-MS, used for the above method for delivering dynamic defor- mation beam spots by LA-ICP-MS; where the equipment includes a mass spectrometer module, a beam deformable piece, a lens module, a sample storehouse, a laser module, a carrier gas module and a vacuum module.
The beam deformable piece is generated by a three-dimensional phase layered structure of a sample; pipeline of the sample store- house is respectively connected with the mass spectrometer module, the carrier gas module and the vacuum module; the sample store- house is used for placing the sample; the laser module is used for emitting a light beam; when the sample storehouse is vacuumized by the vacuum module and the sample is fixed detachably, the light beam forms a beam spot through the lens module and the beam de- formable piece to ablate the sample; and the ablated product is fed into the mass spectrometer module via a carrier gas of the carrier gas module for analyzing the sample composition; the beam deformable piece is a photographic film, a flake- like excitation source arranged in bands, a liquid crystal polar- izing film having a direction of extinction greater than one shape or a digital-control deformable excitation source.
Preferably, when the beam deformable piece is the photograph- ic film or the flake-like excitation source arranged in bands, the equipment further includes a first stepper motor, a second stepper motor, a first turning wheel connected with the first stepper mo- tor and a second turning wheel connected with the second stepper motor; the first stepper motor is used for driving the first running wheel such that the first turning wheel entwines to fix the beam deformable piece where no light beam transmits; the second stepper motor is used for driving the second run- ning wheel such that the second turning wheel entwines to fix the beam deformable piece where a light beam has transmitted.
Preferably, when the beam deformable piece is the liquid crystal polarizing film or the digital-control deformable excita- tion source, the beam deformable piece attaches to fix on a posi- tion where the laser module emits the light beam.
Preferably, the mass spectrometer module, the sample capsule, the laser module, the light beam, the beam spot, the sample, the carrier gas module and the vacuum module at least include a hori- zontal coplane; the beam spot has a surface coating-free polishing surface on the surface of the sample, thus implementing ablation.
According to the detailed examples provided herein, the pre-
sent invention discloses the following technical effects:
The present invention provides a method and equipment for de- livering dynamic deformation beam spots by LA-ICP-MS; the method includes: obtaining a surface phase boundary shape of a sample and 5 a three-dimensional phase distribution inside the sample; deter- mining a target grain and a standard sample according to the three-dimensional phase distribution of the sample, and performing laser spot control on the standard sample to obtain a beam spot of the target grain; obtaining each ablated layer according to the three-dimensional phase distribution, and determining a change se- quence on cross-section shapes of the target grain of a corre- sponding sample of a beam deformable piece according to the cross- section shape of the ablated layer of the target grain correspond- ing to the three-dimensional phase distribution, where a bright area of the beam deformable piece has a shape corresponding to a geometrically similar graph of the cross-section shape of the beam spot to be ablated; performing frame-by-frame operation on the beam deformable piece according to the order of the change se- quence on cross-section shapes of the target grain, such that the sample is ablated by a light beam; when the sample is ablated by the light beam for once, the beam deformable piece is changed for a next one in a deeper position of the corresponding sample, thus changing the shape of the beam spot successively to implement LA-
ICP-MS. In this present invention, sampling is performed on the dynamic deformation ablation within the ablation region; a paral- lel light or laser beam spot with a real-timely deformable cross- section shape is used to replace the laser beam spot which is free of deformation or only changes defocusing distance during the ab- lation process. The present invention not only achieves the dynam- ic sampling for an irregular ablation region, but also purposeful- ly selects specific composition, such that sampling is performed at a single point to reduce the impurity blending and improve the accuracy of the sample composition data and to save the sample.
To describe the examples of the present invention more clear- ly, accompanying drawings used in the examples will be introduced briefly. Apparently, the accompanying drawings described hereafter are merely some examples of the present invention. Moreover, a person skilled in the art can further obtain other drawings ac- cording to these accompanying drawings on the premise of no in- ventive efforts.
FIG. 1 is a flow diagram showing a method in Example 1 pro- vided by the present invention;
FIG. 2 is a schematic diagram showing a structure in Example 2 provided by the present invention;
FIG. 3 is a schematic diagram showing a structure in Example 3 provided by the present invention;
FIG. 4 is a schematic diagram showing a structure in Example 4 provided by the present invention;
FIG. 5 is a schematic diagram showing a beam deformable piece for analyzing a geological sample in Example 5 provided by the present invention;
FIG. 6 is a schematic diagram showing a beam deformable piece for analyzing a geological sample in Example 6 provided by the present invention;
FIG. 7 is a schematic diagram showing a beam deformable piece for analyzing a geological sample in Example 7 provided by the present invention; and
FIG. 8 is a schematic diagram showing a beam deformable piece for analyzing a geological sample in Example 8 provided by the present invention.
Explanation of numerals: 1-Mass spectrometer module, 1l-first stepper motor, 101-first turning wheel, 12-second stepper motor, 102-second turning wheel, 2-beam deformable piece, 21-single-mineral deformable piece, 22- annular deformable piece, 23-scattered mineral deformable piece, 24-non-euhedral grain deformable piece, 3-lens module, 31-prism module, 4-sample capsule, 5-laser module, 6-light beam, 61-beam spot, 7-sample, 8-carrier gas module, and 9-vacuum module.
The technical solution in the examples of the present inven- tion will be described clearly and completely with reference to the accompanying drawings in the examples of the present inven- tion. Apparently, the examples described herein are merely a por- tion of examples of the present invention instead of all the exam- ples. Based on the examples of the present invention, all the oth- er examples obtained by a person skilled in the art without any inventive effort shall fall within the protection scope of the present invention.
The “examples” mentioned herein mean that specific features, structures or properties described in combination with the exam- ples may be contained in at least one example of the present ap- plication. The phrase in each position of the description neither always refers to the same example, nor an independent or alterna- tive example mutually exclusive to other examples. It is under- stood explicitly and implicitly by a person skilled in the art that the examples described herein may be in combination with oth- er examples.
Terms “first”, “second”, “third”, “fourth, and the like in the description, claims and the accompanying drawings of the pre- sent application are used to differ from different objects instead of describing a specific order. Moreover, terms “comprise” and “have” as well as any variant thereof are intended to cover non- exclusive inclusion. For example, the expression of containing a series of steps, processes, methods and the like is not limited to the steps listed, but optionally further includes the steps not listed, or optionally further includes other inherent step ele- ments directed to these processes, methods, products or equipment.
The objective of the present invention is to provide a method and equipment for delivering dynamic deformation beam spots by LA-
ICP-MS, thus achieving the sampling on the dynamic deformation ab- lation within the ablation region. A parallel light or laser beam spot with a real-timely deformable cross-section shape is used to replace the laser beam spot which is free of deformation or only changes defocusing distance during the ablation process. The pre- sent invention not only achieves the dynamic sampling for an ir- regular ablation region, but also purposefully selects specific composition, such that sampling is performed at a single point to reduce the impurity blending, improve the accuracy of the sample composition data and to save the sample.
To make the above objective, features and advantages of the present invention more apparent and understandable, the present invention will be further specifically described with reference to the accompanying drawings and detailed embodiments.
Example 1:
FIG. 1 is a flow diagram showing a method in Example 1 pro- vided by the present invention. As shown in FIG. 1, the present invention provides a method for delivering dynamic deformation beam spots by LA-ICP-MS, including the following steps: step 100: obtaining a surface phase boundary shape of a sam- ple and a three-dimensional phase distribution inside the sample; step 200: determining a target grain and a standard sample according to the three-dimensional phase distribution of the sam- ple, and performing laser spot control on the standard sample to obtain a beam spot of the target grain; step 300: obtaining each ablated layer according to the three-dimensional phase distribution, and determining a change se- quence on cross-section shapes of the target grain of a corre- sponding sample of a beam deformable piece according to the cross- section shape of the ablated layer of the target grain correspond- ing to the three-dimensional phase distribution, where a bright area of the beam deformable piece has a shape corresponding to a geometrically similar graph of the cross-section shape of the beam spot to be ablated; step 400: performing frame-by-frame operation on the beam de- formable piece according to the order of the change sequence on cross-section shapes of the target grain, such that the sample is ablated by a light beam; when the sample is ablated by the light beam for once, the beam deformable piece is changed for a next one in a deeper position of the corresponding sample, thus changing the shape of the beam spot successively to implement LA-ICP-MS.
Specifically, the step 100 of obtaining a surface phase boundary shape of a sample and a three-dimensional phase distribu- tion inside the sample may be achieved by the ways such as, CT scanning, or X-ray transmission imaging, or three-dimensional con- focal Raman spectra, or acquisition of mineral zones by Cathodo
Luminescence (CL) images.
Further, the step 200 is as follows: firstly determining spe- cies of the phase according to the phase distribution in the step 100, and determining at least one target grain to be ablated ac- cording to the species of the phase; selecting a mineral which has uniform composition and whose at least one element composition is the same with the target grain, or a mineral which has a mineral phase the same as the target grain as a standard sample; then pre- ablating the standard sample by a laser beam spot with a certain power, wavelength and radius to measure the ablation rate of each phase; and adjusting to obtain a beam spot with the power, wave- length and radius suitable for a specific sample. The objective of the step 200 is to select the mineral to be analyzed and the standard sample.
Optionally, the step 300 is as follows: obtaining each ablated layer via dividing the ablation rate of each phase by the volume and depth of the phase distribution inside the sample respectively, and generating changes on cross- section shapes of the target grain of a corresponding sample of the beam deformable piece according to the cross-section shapes of the ablated layer of the target grain corresponding to the three- dimensional phase distribution inside the sample and performing arrangement from light to dark; where a bright area of the beam deformable piece has a shape corresponding to a geometrically sim- ilar graph of the cross-section shape of the beam spot to be ab- lated; and the position of the beam spot is restrained by the sur- face phase boundary shape.
Specifically, the beam deformable piece is operated frame by frame according to the order of arrangement in the step 300; dur- ing the operation, the light beam transmits through the beam de- formable piece via a parallel or confocal way beyond a double fo- cal length of one side where the lens module is backward facing to the sample capsule; the light beam is allowed to be transmitted when the beam deformable piece pauses, and the pause period is 2 a single pulse period of the light beam; when the sample is ablated by the light beam for once, the beam deformable piece is changed for a next one in a deeper position of the corresponding sample,
thus changing the shape of the beam spot successively to implement
LA-ICP-MS.
Preferably, when the target grain has a position with more than one constant vertical cross-section shapes in the three- dimensional phase distribution, the shape of the beam spot ablated at least for two times is not changed after the light beam trans- mits through the beam deformable piece.
Example 2:
FIG. 2 is a schematic diagram showing a structure in Example 2 provided by the present invention. As shown in FIG. 2, the LA-
ICP-MS equipment for a dynamic deformation beam spot includes: a mass spectrometer module 1, a beam deformable piece 2, a lens mod- ule 3, a sample capsule 4, a laser module 5, a carrier gas module 8, and a vacuum module 9. The beam anamorphic piece 2 is more than one photographic films generated based on a three-dimensional phase layered structure of the sample 7. Pipeline of the sample storehouse 4 is connected with the mass spectrometer module 1, the carrier gas module 8 and the vacuum module 9; the laser module 5 emits a light beam 6; when the sample storehouse 4 is vacuumized by the vacuum module 9 and the sample 7 is fixing detachably, the light beam 6 forms a beam spot 61 through the lens module 3 and the beam deformable piece 2 to ablate the sample 7; a prism module 31 may be further added when the light beam 6 is a parallel beam or a light beam within the non-ablation energy range; the prism module 31 deviates the light beam 6 transmitting into the beam de- formable piece 2 or the lens module 3; the ablated product is fed into the mass spectrometer module 1 via a carrier gas of the car- rier gas module 8 for analyzing composition of the sample 7; when the beam deformable piece 2 is a photographic film or flake-like excitation source arranged in bands, the first stepper motor 11 drives the first turning wheel 101 such that the first turning wheel 101 entwines to fix the beam deformable piece 2 where the light beam 6 does not transmit; the second stepper motor 12 drives the second turning wheel 102 such that the second turning wheel 102 entwines to fix the beam deformable piece 2 where the light beam 6 has transmitted.
Example 3:
FIG. 3 is a schematic diagram showing a structure in Example 3 provided by the present invention. As shown in FIG. 3, compared with the mentioned above, the beam deformable piece 2 in Example 3 is a flake-like excitation source arranged in bands to directly change the shape of the excitation source, thus changing the shape of the light source. It is publicly known that the shape of the beam spot 61 may be restrained by changing the shape of the light source which is beyond double focal length of the convex lens of the lens module. At this time, the beam deformable piece 2 trans- mits through the laser module 5 unidirecticnally; and the beam de- formable piece 2 will be attached on but not fix the position where the laser module 5 emits the light beam 6, thus changing the shape of the light beam 6. The first stepper motor 11 drives the first turning wheel 101 such that the first turning wheel 101 en- twines to fix the beam deformable piece 2 which does not transmit through the laser module 5; the second stepper motor 12 drives the second turning wheel 102 such that the second turning wheel 102 entwines to fix the beam deformable piece 2 which has transmitted through the laser module 5.
Example 4:
FIG. 4 is a schematic diagram showing a structure in Example 4 provided by the present invention. As shown in FIG. 4, compared with Examples 2 and 3, the beam deformable piece 2 is one of the liquid crystal polarizing film or the digital-control deformable excitation source, the beam deformable piece 2 attaches to fix on a position where the laser module 5 emits the light beam 6. At this time, the shape of the layered beam spot 61 of the beam de- formable piece 2 is controlled and saved by a computer.
Example 5:
FIG. 5 is a schematic diagram showing a beam deformable piece for analyzing a geological sample in Example 5 provided by the present invention. As shown in FIG. 5, a single-mineral grain with changes on the vertical cross-section shapes in the sample 7 is analyzed based on the above equipment, for example, zonal-free garnet or pyrite with decreased cross-section radius from the sur- face to the deep portion of the sample 7. It needs to avoid blend- ing with the ablation of other minerals during the ablation pro-
cess of the beam spot 61 towards the deep portion. At this time, the beam deformable piece 2 is subdivided into a single-mineral deformable piece 21; the single-mineral deformable piece 21 has a continuous shape of its bright area and uniform transmittance.
Example 6:
FIG. 6 is a schematic diagram showing a beam deformable piece for analyzing a geological sample in Example 6 provided by the present invention. As shown in FIG. 6, based on Examples 2, 3 and 4, mineral zones with changes on the vertical cross-section shapes in the sample 7 are analyzed, for example, zonal zircons, apa- tites, monazites, garnets, pyroxenes and feldspars. The beam spot 61 needs to ablate the corresponding period of minerals during the ablation process towards the deep portion. At this time, the beam deformable piece 2 is subdivided into a zonal deformable piece 22; the shape of the bright area of the zonal deformable piece 22 and the corresponding mineral zone form a similar graph; moreover, the transmittance of the wide zone is higher than that of the narrow one. During ablation focusing, the beam spot 61 is overlapped and focused on the zone of the target grain. When there are a plurali- ty of zones, the mineral zones are analyzed from inside to outside of the cross section thereof. Methods for judging inner and outer zones are publicly known technology. If a single zone is through- out the whole crystal and the mean width is narrower than 1 um, sampling for the single zone may be abandoned. According to common general knowledge, zone is the cause of crystals of different min- erals in different periods. Mineral zones in the corresponding pe- riod should be selected as much as possible in chronology studies.
Therefore, the zone is precisely selected in this example, which is beneficial to improving the accuracy of chronological data.
Example 7:
FIG. 7 is a schematic diagram showing a beam deformable piece for analyzing a geological sample in Example 7 provided by the present invention. As shown in FIG. 7, based on Examples 2, 3 and 4, a plurality of same fine-grained minerals in the sample 7 are analyzed; and Example 7 is mainly used for the grade analysis of lean ores, scattered minerals, and precious metal ore minerals; for example, PGE analysis on the sulfide of sparsely disseminated
Cu-Ni-Pt ores, analysis on the fine-grained rare-earth minerals in alkaline rocks, and trace element analysis on separation struc- tures of sulfide solid solution, needle-clustered rutile and il- menite. At this time, the beam deformable piece 2 is subdivided into a scattered mineral deformable piece 23; the shape of the bright area of the scattered mineral deformable piece 23 is dis- continuously point-like; and the transmittance of the bright area decreases progressively according to the size of the corresponding target grain. Methods for changing the transmittance of the beam deformable piece 2 are publicly known technology.
Example 8:
FIG. 8 is a schematic diagram showing a beam deformable piece for analyzing a geological sample in Example 8 provided by the present invention. As shown in FIG. 8, based on Examples 2, 3 and 4, the glass, allogenic minerals and other non-euhedral crystal phases in the sample 7 are analyzed, and the beam deformable piece 2 is subdivided into a non-euhedral grain deformable piece 24 at this time. It is quite possible for the target grain to have a po- sition with a constant vertical cross-section shape in the three- dimensional phase distribution (for example, volcanic glass beads}; if existence, the shape of the beam spot 61 ablated at least for two times is not changed after the light beam 6 trans- mits through the beam deformable piece 2.
Furthermore, Examples 5, 6, 7 and 8 are subject to the prin- ciple of progressively decreased diameter during the ablation pro- cess of the beam spot 61 from the surface to the deep portion of the sample 7. If there is a non-target grain covered on the sur- face of the target grain, or the target grain forms a tapered zone, the non-target grain may be ablated in advance. The ablation of the non-target grain from the target grain is beneficial to im- proving the accuracy of the LA-ICP-MS data.
Features not specified in detail in this present are common general knowledge, for example, the mass spectrometer module 1 re- lates to a mass spectrometer, laser type of the laser module 5, gas path system of the carrier gas module 8, vacuum equipment of the vacuum module 9, computer control system and its method for generating the beam deformable piece 2, specific types and materi-
als of the stepper motors, running wheels, lens module 3 and prism module 31, and the composition calculation method of the sample 7.
Beneficial effects of the present invention are as follows: (1) The real-time morphologic change of the beam spot is achieved by the three-dimensional topography of the geclogical sample obtained in advance, thereby decreasing the time consuming on the measurement and adjustment of the prior art. (2) The present invention may achieve the dynamic sampling on the ablation region of irregular shapes (for example, microscopic mineral inclusions, solid solution separation structures and fined zones of a geological sample), and may analyze micro, discontinu- ous or irregular grains which are hardly run ideal analysis by conventional LA-ICP-MS (for example, needle-like ilmenite in moon rocks, rutile and irregular vitric fragments), thus expanding the universality of the detectable scope of geological samples. (3) Furthermore, specific mineral composition may be selected purposefully such that sampling is performed at a single point to reduce the impurity blending and improve the accuracy of the sam- ple composition data (for example, single-mineral isotope ratio, single-mineral trace element contents, and dating of zircons, apa- tites and monazites). (4) The simultaneous sampling of a plurality of same mineral grains may be further achieved when ablation is scanned in a wide range to calculate the ore grade, thus saving the sampling time.
Each example in the description is described in a progressive way; what is focused in each example lies in the difference from other examples; the same or similar portions in each example may be referenced with each other. Because the equipment disclosed in the example is corresponding to the method disclosed in the exam- ple and thus, is described comparatively simply; the related por- tions are referring to the description of the method.
A specific example is applied herein to explain the principle and embodiments of the present invention. Description of the above examples is merely used to help understanding the method of the present invention and the core idea thereof. Meanwhile, a person skilled in the art may make changes in the embodiments and range of application based on the idea of the present invention. To sum up, the disclosure of the description shall be not construed as limiting the present invention.
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| CHEW DAVID ET AL: "LA-ICP-MS imaging in the geosciences and its applications to geochronology", CHEMICAL GEOLOGY, ELSEVIER SCIENCE PUBLISHER B.V., AMSTERDAM, NL, vol. 559, 12 October 2020 (2020-10-12), XP086406832, ISSN: 0009-2541, [retrieved on 20201012], DOI: 10.1016/J.CHEMGEO.2020.119917 * |
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