CN114428093A - Measuring point positioning device based on energy spectrometer, energy spectrum testing system and testing method - Google Patents

Measuring point positioning device based on energy spectrometer, energy spectrum testing system and testing method Download PDF

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Publication number
CN114428093A
CN114428093A CN202011049299.1A CN202011049299A CN114428093A CN 114428093 A CN114428093 A CN 114428093A CN 202011049299 A CN202011049299 A CN 202011049299A CN 114428093 A CN114428093 A CN 114428093A
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China
Prior art keywords
energy spectrum
adjusting
energy
beam spot
positioning device
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CN202011049299.1A
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Chinese (zh)
Inventor
张隽
王杰
俞凌杰
鲍芳
芮小庆
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China Petroleum and Chemical Corp
Sinopec Exploration and Production Research Institute
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China Petroleum and Chemical Corp
Sinopec Exploration and Production Research Institute
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Priority to CN202011049299.1A priority Critical patent/CN114428093A/en
Publication of CN114428093A publication Critical patent/CN114428093A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating 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
    • G01N23/22Investigating 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
    • G01N23/2204Specimen supports therefor; Sample conveying means therefore
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating 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
    • G01N23/22Investigating 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
    • G01N23/2206Combination of two or more measurements, at least one measurement being that of secondary emission, e.g. combination of secondary electron [SE] measurement and back-scattered electron [BSE] measurement
    • G01N23/2208Combination of two or more measurements, at least one measurement being that of secondary emission, e.g. combination of secondary electron [SE] measurement and back-scattered electron [BSE] measurement all measurements being of a secondary emission, e.g. combination of SE measurement and characteristic X-ray measurement
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating 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
    • G01N23/22Investigating 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
    • G01N23/227Measuring photoelectric effect, e.g. photoelectron emission microscopy [PEEM]
    • G01N23/2273Measuring photoelectron spectrum, e.g. electron spectroscopy for chemical analysis [ESCA] or X-ray photoelectron spectroscopy [XPS]
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/07Investigating materials by wave or particle radiation secondary emission
    • G01N2223/08Investigating materials by wave or particle radiation secondary emission incident electron beam and measuring cathode luminescence (U.V.)
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/07Investigating materials by wave or particle radiation secondary emission
    • G01N2223/085Investigating materials by wave or particle radiation secondary emission photo-electron spectrum [ESCA, XPS]
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/10Different kinds of radiation or particles
    • G01N2223/101Different kinds of radiation or particles electromagnetic radiation
    • G01N2223/1016X-ray
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/10Different kinds of radiation or particles
    • G01N2223/102Different kinds of radiation or particles beta or electrons

Abstract

The application relates to the field of petroleum geological exploration testing devices, in particular to a measuring point positioning device based on an energy spectrometer, an energy spectrum testing system and a testing method. The measuring point positioning device based on the energy spectrometer comprises an energy spectrum probe adjusting device and a measuring point positioning device. The angle of the connecting piece can be selectively adjusted through a first adjusting piece of the energy spectrum probe adjusting device, so that the energy spectrum probe captures an interesting energy spectrum beam spot on the objective table, and the plane reflecting mirror can be selectively adjusted through a second adjusting piece of the measuring point positioning device to adjust the incident light spot to be coincident with the interesting energy spectrum beam spot. The measuring point positioning device based on the energy spectrometer can achieve accurate and efficient alignment of a target measuring point to an energy spectrum beam spot irradiation range, and guarantees the in-situ performance of an analysis sample to the maximum extent. Meanwhile, the beam spot position can be correspondingly regulated and controlled according to the influence of different mineral thicknesses on the beam spot offset.

Description

Measuring point positioning device based on energy spectrometer, energy spectrum testing system and testing method
Technical Field
The application relates to the field of petroleum geological exploration testing devices, in particular to a measuring point positioning device based on an energy spectrometer, an energy spectrum testing system and a testing method.
Background
Cathodoluminescence is the visible light produced when a sample is bombarded by an electron beam, different minerals produce different cathodoluminescence due to the different activator elements, the device used to excite and produce cathodoluminescence is called cathodoluminescence apparatus, and the device used in combination with an energy spectrometer capable of detecting mineral elements is called cathodoluminescence (energy spectrum) apparatus. The sample chamber of cathode luminescence (energy spectrum) instrument is a vacuum chamber mounted on the microscope stage, the X-ray energy spectrum probe is covered on the sample vacuum chamber, the cold cathode electron gun is used as the upper cover plate of the vacuum chamber, the produced electrons can be passed through the focusing coil and fed into the sample chamber so as to attain the goal of bombarding sample and collecting cathode luminescence and X-ray energy spectrum of rock mineral.
At present, an electron gun of a cathode luminescence (energy spectrum) instrument mainly adopts an oblique incidence mode, and although the signal to noise ratio of cathode luminescence is improved, the position of a light spot of an energy spectrum instrument is also deviated. In the field of petroleum geological exploration, a rock slice with the thickness of 0.04mm is placed on a sample disc in a sample chamber, full-field cathodoluminescence collection is carried out on rock minerals under an ocular observation point through an electron gun of a cathodoluminescence (energy spectrum) instrument, and meanwhile, X-ray energy spectrum collection is carried out on part of interest measuring points, such as target measuring points of dolostone girdle, microcracks, trace minerals and the like. Because the diameter of a beam spot of an energy spectrometer of the lens is generally 50-100 micrometers, the energy spectrometer cannot cover a single view field with different magnification factors under a microscope, when oblique incidence light emitted by an electron gun is irradiated on the surface of a sample, the beam spot deviates from the center of an objective lens, in-situ energy spectrum collection cannot be directly carried out on a target measuring point, and the sample can only be manually shifted through subjective observation, so that a large error exists in alignment between the target measuring point and the energy spectrum beam spot.
The prior patent (application No. CN103730311B) proposes a cathode light-emitting device, which comprises an electron gun, a sample chamber, a vacuum pump and a controller, wherein the electron gun and the sample holder have an included angle of 20-30 °, and a light-transmitting window is arranged at the center of the lower part of a vacuum chamber housing. The invention has the advantages that the electron gun and the sample frame have a certain included angle, the electron beam can directly bombard the sample without using an external magnetic field to act on the electron beam, a light spot with definite and regular edge and uniform electron beam current intensity can be generated on the surface of the sample, and the observation is easy. The defect of the patent is that the energy spectrum light spot with a small beam spot cannot be aligned with a target measuring point at the center of an objective lens, so that the acquisition position of an X-ray energy spectrum under cathodoluminescence is seriously deviated from the target measuring point, and the error of cathodoluminescence energy spectrum test and the uncertainty of data are enlarged. At present, no in-situ analysis sample stage device and target measuring point positioning method for combined use of cathodoluminescence and an energy spectrometer exist.
Disclosure of Invention
In view of the above, an object of the embodiments of the present application is to provide a measuring point positioning device, an energy spectrum testing system and a testing method based on an energy spectrometer, which can effectively solve the above technical problems.
In a first aspect, an embodiment of the present application provides a measuring point positioning device based on an energy spectrometer, including an energy spectrum probe adjusting device and a measuring point positioning device. The energy spectrum probe adjusting device comprises a connecting piece for mounting the energy spectrum probe and a first adjusting piece for adjusting an included angle of the connecting piece relative to a horizontal plane; the measuring point positioning device comprises a plane reflector and a second adjusting piece used for adjusting the reflection angle of the plane reflector. The angle of the connecting piece is selectively adjusted through the first adjusting piece, so that the energy spectrum probe captures an interesting energy spectrum beam spot on the objective table, and the plane reflecting mirror is selectively adjusted through the second adjusting piece to adjust the incident light spot to be coincident with the interesting energy spectrum beam spot.
In an alternative embodiment according to the first aspect, the first adjusting member includes a fixing member and an adjusting lever slidably coupled to the fixing member, and one end of the adjusting lever is coupled to the connecting member and the other end is slidably coupled to the fixing member to move the connecting member closer to or farther from the fixing member. Will first regulating part set up to include the mounting and with but mounting sliding connection's regulation pole, in the use, through adjusting the pole with mounting sliding connection, and then realize that the connecting piece is kept away from or is close to the mounting, also realize installing in the angle modulation between the energy spectrum probe on the connecting piece and the objective table, and then be convenient for catch the position of interest energy spectrum.
In an alternative embodiment according to the first aspect, the fixing member includes a base and a threaded sleeve protruding from the base, and the adjusting rod is provided as a threaded rod cooperating with the threaded sleeve. Will the mounting includes the base and protruding locating the threaded sleeve of base sets up the holistic stability of base can be convenient for stabilize the connecting piece, through threaded rod and threaded sleeve's connected mode, both can realize adjusting the pole and drive the connecting piece and go up and down, can realize adjusting the pole simultaneously and drive the connecting piece and realize controlling the rotation, and then can enlarge the capture range.
In an alternative embodiment according to the first aspect, the adjustment bar is arranged vertically on the stage, and the connection is configured to arrange the energy spectrum probe at an angle to the stage. Will adjust the pole and set up perpendicularly on the objective table, the connecting piece is constructed to make the energy spectrum probe be the contained angle setting with the objective table, is convenient for realize that the incline direction of energy spectrum probe and oblique insertion formula energy spectrum appearance keeps roughly unanimous, and then is convenient for catch and predetermines the energy spectrum.
In an alternative embodiment according to the first aspect, the connecting member is arranged obliquely to the adjustment lever. The purpose of setting the energy spectrum probe and the objective table at an included angle is realized by obliquely arranging the connecting piece on the adjusting rod.
In an alternative embodiment according to the first aspect, the second adjusting member comprises a worm wheel and a worm screw which are matched, the plane mirror is connected to a central shaft of the worm wheel, and the worm screw is rotated to drive the worm wheel to rotate so as to rotate the plane mirror. The ground adjusting part is arranged to comprise a worm wheel and a worm which are matched, the plane reflecting mirror is connected to the central shaft of the worm wheel, and the worm is rotated to drive the worm wheel to rotate so as to enable the plane reflecting mirror to rotate. In practice, the worm gear can be rotated by a user by turning the worm to rotate the plane mirror.
In an alternative embodiment according to the first aspect, the second adjusting member further comprises a mirror support, the mirror support comprises a support rod and a support base, one end of the support rod is rotatably connected with the central shaft of the turbine, and the other end of the support rod is connected with the support base. The reflector bracket is arranged to support the reflector conveniently, so that the stability of the reflector is ensured. The support of the reflecting mirror is arranged to comprise a supporting rod and a supporting seat, and the installation stability of the plane reflecting mirror is further ensured.
In a second aspect, the embodiment of the present application further provides an energy spectrum testing system, where the energy spectrum testing system includes an energy spectrometer, a cathodoluminescent instrument, an object stage, a microscope, a polarizer, and the measuring point positioning device based on the energy spectrometer; the energy spectrum probe of the energy spectrometer is arranged on the connecting piece, and the cathodoluminescent instrument is selectively connected with the connecting piece; the objective table is horizontally arranged; the lens of the microscope is arranged opposite to the objective table, and the polarizer is arranged corresponding to the plane reflector.
In an alternative embodiment according to the second aspect, the spectroscopic test system further comprises a light-transmissive vacuum chamber, the stage being disposed within the light-transmissive vacuum chamber.
In a third aspect, an embodiment of the present application further provides a testing method using the energy spectrum testing system, where the testing method includes:
sample bombardment: bombarding a rock slice sample to be detected on the objective table by the cathode luminoscope;
determining the position of the energy spectrum beam spot: adjusting the first adjusting piece to enable an energy spectrum probe of the energy spectrometer to capture an interesting energy spectrum beam spot on the objective table;
positioning target measuring points: opening the polarizer, enabling the polarizer to emit incident light to irradiate the plane reflector, and adjusting the second adjusting piece to enable an incident light spot reflected by the plane reflector to coincide with the interesting energy spectrum beam spot;
energy spectrum beam spot calibration: calibrating by further adjusting the first adjusting part to ensure that the incident light spot coincides with the energy spectrum beam spot of interest;
and acquiring a preset energy spectrum, adjusting the incident light spot to coincide with the interested energy spectrum beam spot, and acquiring the preset energy spectrum of the rock slice sample to be detected on the objective table through an energy spectrum probe of the energy spectrum.
The application provides a measurement station positioner based on energy spectrometer compares with prior art, possesses following beneficial effect at least:
the measuring point positioning device based on the energy spectrometer comprises an energy spectrum probe adjusting device and a measuring point positioning device. The angle of the connecting piece can be selectively adjusted through a first adjusting piece of the energy spectrum probe adjusting device, so that the energy spectrum probe captures an interesting energy spectrum beam spot on the objective table, and the plane reflecting mirror can be selectively adjusted through a second adjusting piece of the measuring point positioning device to adjust the incident light spot to be coincident with the interesting energy spectrum beam spot. The measuring point positioning device based on the energy spectrometer can achieve accurate and efficient alignment of a target measuring point to an energy spectrum beam spot irradiation range, and guarantees the in-situ performance of an analysis sample to the maximum extent. Meanwhile, the beam spot position can be correspondingly regulated and controlled according to the influence of different mineral thicknesses on the beam spot offset.
The energy spectrum testing system provided by the application also has the beneficial effects due to the fact that the measuring point positioning device based on the energy spectrum instrument is included.
The test method provided by the application is a test method using the energy spectrum test system, so that the test method has the beneficial effects.
Drawings
The present application will be described in more detail below on the basis of embodiments and with reference to the accompanying drawings.
FIG. 1 is a schematic diagram of the overall structure of a measuring point positioning device based on an energy spectrometer, provided by an embodiment of the first aspect of the present application;
fig. 2 is a schematic structural diagram of an overall energy spectrum testing system provided in an embodiment of the second aspect of the present application.
In the drawings, like parts are provided with like reference numerals. The figures are not drawn to scale.
Reference numerals:
10-measuring point positioning device based on energy spectrometer; 11-a spectrum probe adjusting device; 111-a connector; 113-a first adjustment member; 1131-fixing piece; 1131 a-base; 1131b — threaded sleeve; 1133, adjusting a rod; 12-measuring point positioning means; 121-a plane mirror; 123-a second adjustment member; 124-adjusting valve; 125-mirror support; 125 a-support bar; 125 b-a support seat; 20-energy spectrum testing system; 21-an object stage; 23-a microscope; 25-polarizer; 26-an incident light spot; 27-energy spectral beam spot.
Detailed Description
The present application is further described below in conjunction with the detailed description. It should be understood that these specific embodiments are merely illustrative of the present application and are not intended to limit the scope of the present application.
The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention.
All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present application, it is to be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, which are for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; either directly or indirectly through an intermediary, or the communication of the support members within the two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Only some numerical ranges are specifically disclosed herein. However, any lower limit may be combined with any upper limit to form ranges not explicitly recited; and any lower limit may be combined with any other lower limit to form a range not explicitly recited, and similarly any upper limit may be combined with any other upper limit to form a range not explicitly recited. Furthermore, each separately disclosed point or individual value may itself, as a lower or upper limit, be combined with any other point or individual value or with other lower or upper limits to form ranges not explicitly recited.
In the description herein, it is to be noted that, unless otherwise specified, "above" and "below" are inclusive and "one or more" mean "several" two or more.
Unless otherwise indicated, terms used in the present application have well-known meanings that are commonly understood by those skilled in the art. Unless otherwise indicated, the numerical values of the parameters mentioned in the present application can be measured by various measurement methods commonly used in the art (for example, the test can be performed according to the methods given in the examples of the present application).
Example 1:
referring to fig. 1, the spectrometer-based station positioning device 10 provided by the present application includes a spectrum probe adjusting device 11 and a station positioning device 12. The energy spectrum probe adjusting device 11 comprises a connecting piece 111 for installing an energy spectrum probe and a first adjusting piece 113 for adjusting an included angle of the connecting piece 111 relative to a horizontal plane; the measuring point positioning device 12 comprises a plane mirror 121 and a second adjusting piece 123 for adjusting the reflection angle of the plane mirror 121. Wherein, the angle of the connecting part 111 can be selectively adjusted by the first adjusting part 113 to enable the energy spectrum probe to capture the energy spectrum beam spot 27 of interest on the object stage 21, and the plane mirror 121 can be selectively adjusted by the second adjusting part 123 to adjust the incident light spot 26 to coincide with the energy spectrum beam spot 27 of interest.
The measuring point positioning device 10 based on the energy spectrometer comprises an energy spectrum probe adjusting device 11 and a measuring point positioning device 12. The angle of the connecting piece 111 can be selectively adjusted through the first adjusting piece 113 of the energy spectrum probe adjusting device 11 so that the energy spectrum probe captures the energy spectrum beam spot 27 of interest on the object stage 21, and the plane mirror 121 can be selectively adjusted through the second adjusting piece 123 of the measuring point positioning device 12 so as to adjust the incident light spot 26 to coincide with the energy spectrum beam spot 27 of interest. The measuring point positioning device 10 based on the energy spectrometer can achieve accurate and efficient alignment of a target measuring point to the irradiation range of the energy spectrum beam spot 27, and guarantees the in-situ performance of an analysis sample to the maximum extent. Meanwhile, the beam spot position can be correspondingly regulated and controlled according to the influence of different mineral thicknesses on the beam spot offset.
In an alternative exemplary embodiment, the first adjusting member 113 includes a fixing member 1131 and an adjusting rod 1133 slidably connected to the fixing member 1131, wherein one end of the adjusting rod 1133 is connected to the connecting member 111, and the other end is slidably connected to the fixing member 1131 to enable the connecting member 111 to approach or separate from the fixing member 1131. It should be noted that, the first adjusting member 113 is configured to include a fixing member 1131 and an adjusting rod 1133 slidably connected to the fixing member 1131, and in the use process, the adjusting rod 1133 is slidably connected to the fixing member 1131, so as to further implement that the connecting member 111 is far away from or close to the fixing member 1131, that is, to implement the angle adjustment between the spectrum probe mounted on the connecting member 111 and the object stage 21, thereby facilitating capturing the position of the energy spectrum of interest. It is understood that the specific structure of the first connecting member 111 is not limited herein, and in other specific embodiments, the first connecting member 111 may be arranged to be connected by a pin according to the actual requirement of the user, so as to rotate the connecting member 111 by rotating the rotating shaft, thereby enabling the connecting member to perform a pitching operation, and further capturing an interest energy spectrum on the object stage 21.
In an alternative exemplary embodiment, the fixing member 1131 includes a base 1131a and a threaded sleeve 1131b protruding from the base 1131a, and the adjusting rod 1133 is configured as a threaded rod cooperating with the threaded sleeve 1131 b. It should be noted that, the fixing member 1131 includes a base 1131a and a threaded sleeve 1131b protruding from the base 1131a, the base 1131a is configured to stabilize the overall stability of the connecting member 111, and by using the connection manner of the threaded rod and the threaded sleeve 1131b, the adjusting rod 1133 can be used to drive the connecting member 111 to lift, and meanwhile, the adjusting rod 1133 can be used to drive the connecting member 111 to rotate left and right, so as to expand the capturing range. It should be noted that, the specific manner of implementing the lifting and rotating of the adjusting rod 1133 is not limited herein, and it can be understood that, in other specific embodiments, the adjusting rod 1133 can be configured as a telescopic rod and a rotating platform according to the requirement of the user, so as to implement the lifting and rotating.
It is also to be noted that a shifted resetting of the energy spectrum beam spot 27 caused by a change in the thickness of the rock mineral is achieved. The connecting piece 111 lifts the energy spectrum probe by rotating the threaded rod according to a first preset direction, so that the included angle between the energy spectrum probe and the objective table 21 in the horizontal direction is increased, and the energy spectrum beam spot 27 moves towards the first direction of the X axis of the objective table 21; by rotating the threaded rod in the second preset direction, the connecting rod descends the spectrum probe, so that the included angle between the spectrum probe and the objective table 21 in the horizontal direction is reduced, and the spectrum beam spot 27 moves towards the first direction of the X axis of the objective table 21. The first direction and the second direction are opposite directions along the X axis.
In an alternative exemplary embodiment, the adjustment rod 1133 is vertically disposed on the object stage 21, and the connecting member 111 is configured to enable the energy spectrum probe to be disposed at an angle with respect to the object stage 21. It should be noted that, the adjusting rod 1133 is vertically disposed on the object stage 21, and the connecting member 111 is configured to enable the energy spectrum probe to form an included angle with the object stage 21, so as to facilitate the keeping of the inclination directions of the energy spectrum probe and the obliquely inserted energy spectrum instrument approximately consistent, and further facilitate the capturing of the preset energy spectrum.
It should be further noted that the connecting member 111 is used for fixing the position of the energy spectrum probe, so that the energy spectrum probe is perpendicular to the X-axis direction of the object stage 21, and meanwhile, the first adjusting member 113 manually adjusts the included angle between the energy spectrum probe and the object stage 21 in the horizontal direction, so as to realize the offset resetting of the energy spectrum beam spot 27 caused by the thickness change of the rock mineral.
In an alternative exemplary embodiment, the connecting member 111 is obliquely disposed to the adjusting lever 1133. Specifically, in the present embodiment, the purpose of setting the energy spectrum probe at an angle with respect to the stage 21 is achieved by obliquely setting the connecting member 111 on the adjusting rod 1133. In particular, the top surface of the adjustment bar 1133 is provided with a groove for placing the top corner of the obliquely arranged connecting piece 111.
In an alternative exemplary embodiment, the second adjusting member 123 includes a worm gear and a worm screw (not shown), the plane mirror 121 is connected to a central shaft of the worm gear, and the worm screw is rotated to rotate the worm gear to rotate the plane mirror 121. The ground adjusting part is arranged to comprise a worm wheel and a worm, wherein the worm wheel and the worm are matched, the plane mirror 121 is connected to the central shaft of the worm wheel, and the worm is rotated to drive the worm wheel to rotate so as to enable the plane mirror 121 to rotate. In practice, the worm gear can be rotated by a user to rotate the plane mirror 121; further, in this embodiment, the second adjusting part 123 further includes an adjusting valve 124, the adjusting valve 124 is connected to the worm, and in the using process, the adjusting valve 124 is used to realize rotation of the worm, further realize rotation of the worm wheel, and the central shaft of the worm wheel rotates therewith, further realize rotation of the plane mirror 121, further realize change of the angle of the plane mirror 121, so that the plane mirror 121 can adjust the angle of incident light, and better realize coincidence of the incident light spot 26 and the energy spectrum beam spot 27.
It should be further noted that, specifically, in the use process, the angle of the plane mirror 121 is regulated and controlled by the regulating valve 124, so that the included angle between the reflected light of the incident light on the plane mirror 121 and the horizontal direction of the object stage 21 is equal to the included angle between the energy spectrum probe and the horizontal direction of the object stage 21; further, in this embodiment, the included angle between the energy spectrum probe and the horizontal direction of the object stage 21 is in the range of 20 ° to 30 °. It is understood that the range of the angle between the energy spectrum probe and the horizontal direction of the object stage 21 is not limited herein, and it is understood that in other embodiments, the range of the angle between the energy spectrum probe and the horizontal direction of the object stage 21 can be adaptively changed according to the actual needs of the user.
In an alternative exemplary embodiment, the second adjusting member 123 further includes a mirror bracket 125, and the mirror bracket 125 includes a support rod 125a and a support base 125b, wherein one end of the support rod 125a is rotatably connected to the central shaft of the worm gear, and the other end is connected to the support base 125 b. It should be noted that the mirror support 125 is provided to support the mirror, so as to ensure the stability of the mirror. The support of the reflector is configured to include a support rod 125a and a support seat 125b, so as to further ensure the stability of the installation of the plane reflector 121.
Example 2:
referring to fig. 2, in a second aspect, the present embodiment further provides an energy spectrum testing system 20, where the energy spectrum testing system 20 includes an energy spectrometer (not shown), a cathodometer (not shown), an object stage 21, a microscope 23, a polarizer 25, and the above-mentioned measuring point positioning device 10 based on an energy spectrometer; the energy spectrum probe of the energy spectrometer is arranged on the connecting piece 111, and the cathodometer is selectively connected to the connecting piece 111; the object stage 21 is horizontally arranged; the lens of the microscope 23 is disposed opposite to the stage 21, and the polarizer 25 is disposed corresponding to the plane mirror 121. It should be noted that the energy spectrum testing system 20 provided in the present application also has the above-mentioned advantages because it includes the above-mentioned station locating device 10 based on an energy spectrometer.
In an alternative embodiment according to the second aspect, the spectroscopic test system 20 further comprises a light-transmissive vacuum chamber, the stage 21 being placed within the light-transmissive vacuum chamber. It should be noted that the transparent vacuum chamber is provided to facilitate observation and collection of the predetermined energy spectrum, and to avoid unnecessary interference during bombardment, thereby further ensuring stable development of the experiment.
In an alternative embodiment according to the second aspect, the spectrometer comprises a spectroscopic probe for finding a target measurement point. The cathodometer, in this embodiment, is primarily operated in oblique incidence, although the signal-to-noise ratio of cathodoluminescence is improved. The object stage 21 is used for placing a rock sample to be tested. The microscope 23 is used to observe the condition of the sample during the test. The polarizer 25 is used for emitting incident light, so that observation of the interested measuring point is facilitated.
Example 3:
in a third aspect, an embodiment of the present application further provides a testing method using the energy spectrum testing system 20, where the testing method includes:
sample bombardment: bombarding a rock slice sample to be detected on the object stage 21 by the cathode luminometer;
determining the position of the energy spectrum beam spot 27: adjusting the first adjusting part 113 to make the energy spectrum probe of the energy spectrometer capture the energy spectrum beam spot 27 of interest on the object stage 21;
positioning target measuring points: the polarizer 25 is opened, the polarizer 25 emits incident light to irradiate the plane mirror 121, and the second adjusting part 123 is adjusted to enable the incident light spot 26 reflected by the plane mirror 121 to coincide with the energy spectrum beam spot 27 of interest;
energy spectrum beam spot 27 calibration: calibration is performed by further adjusting the first adjusting member 113 to ensure that the incident light spot 26 coincides with the energy spectrum beam spot 27 of interest;
and acquiring a preset energy spectrum, adjusting the incident light spot 26 to coincide with the interested energy spectrum beam spot 27, and acquiring the preset energy spectrum of the rock slice sample to be detected on the objective table 21 through an energy spectrum probe of the energy spectrum.
The test method provided by the present application is a test method using the energy spectrum test system 20, and therefore, has the above-described advantageous effects.
It should be noted that, in the implementation process, the application takes the acquisition of an X-ray energy spectrum as an example:
sample bombardment: and bombarding the rock slice sample to be detected on the object stage 21 by the cathodoluminometer, namely finding out the point of interest by cathodoluminescence identification. In the actual operation process, according to the SY/T5916-2013 rock mineral cathodoluminescence identification method, cathodoluminescence rock slices with the thickness of about 0.04mm are placed in the 3 object stage 21 (vacuum cavity), a cathodoluminescence electron gun and a cover plate bound on an energy spectrum probe are placed on the object stage 21 (vacuum cavity), certain electron beam current and voltage intensity are set to bombard a cathodoluminescence rock slice sample, and the cathodoluminescence identification of the rock mineral is carried out through a certain magnification and a full visual field of the microscope 23;
determining the position of the energy spectrum beam spot 27: adjusting the first adjusting part 113 to make the energy spectrum probe of the energy spectrometer capture the energy spectrum beam spot 27 of interest on the object stage 21; and adjusting and installing the energy spectrum probe, and determining the position of the energy spectrum beam spot 27. The probe direction of the energy spectrum probe is adjusted to ensure that the adjusting rod 1133 is perpendicular to the X-axis direction of the object stage 21 (vacuum cavity), and is fixed on the base 1131 a. And adjusting the threaded rod to rotate relative to the threaded sleeve 1131b, so that the included angle between the energy spectrum probe and the energy spectrum beam spot 27 in the horizontal direction of the object stage 21 is between 20 and 30 degrees, and determining the position of the energy spectrum beam spot 27.
Positioning target measuring points: the polarizer 25 is opened, the polarizer 25 emits incident light to irradiate the plane mirror 121, and the second adjusting part 123 is adjusted to enable the incident light spot 26 reflected by the plane mirror 121 to coincide with the energy spectrum beam spot 27 of interest; namely, the polarizer 25 is opened to emit incident light, the reflection of the plane reflector 121 is adjusted by the second adjusting piece 123, the included angle between the plane reflector 121 and the objective table 21 is adjusted and controlled by the adjusting valve 124, so that the included angle between the reflected light on the plane reflector 121 and the horizontal direction of the objective table 21 is between 20 and 30 degrees, the included angle between the energy spectrum probe and the horizontal direction of the objective table 21 is met, the included angle is equal to the included angle between the reflected light on the plane reflector 121 and the horizontal direction of the objective table 21, the target measuring point is accurately positioned to the energy spectrum beam spot 27, and the light spot is overlapped with the beam spot;
energy spectrum beam spot 27 calibration: calibration is performed by further adjusting the first adjusting member 113 to ensure that the incident light spot 26 coincides with the energy spectrum beam spot 27 of interest; due to the shift of the energy spectrum beam spot 27 caused by the change of the thickness of the rock mineral, the calibration and resetting of the energy spectrum beam spot 27 is manually performed by the first adjusting member 113 so that the energy spectrum beam spot 27 does not deviate. The connecting piece 111 lifts the energy spectrum probe by rotating the threaded rod according to a first preset direction, so that the included angle between the energy spectrum probe and the objective table 21 in the horizontal direction is increased, and the energy spectrum beam spot 27 moves towards the first direction of the X axis of the objective table 21; by rotating the threaded rod in the second preset direction, the connecting rod descends the spectrum probe, so that the included angle between the spectrum probe and the objective table 21 in the horizontal direction is reduced, and the spectrum beam spot 27 moves towards the first direction of the X axis of the objective table 21. The first direction and the second direction are opposite directions along the X axis. Rotation along a first predetermined direction or a second predetermined direction may be selected as required to calibrate the incident light spot 26 to coincide with the energy spectrum beam spot 27 of interest
And (3) presetting energy spectrum acquisition: after the incident light spot 26 is adjusted to coincide with the energy spectrum beam spot 27 of interest, a preset energy spectrum of the rock slice sample to be measured placed on the objective table 21 is acquired through an energy spectrum probe of the energy spectrum spectrometer, that is, an X-ray energy spectrum is acquired. When the calibrated energy spectrum beam spot 27 is superposed with the light spot of the target measuring point positioned by the measuring point positioning device 12, the X-ray energy spectrum of the rock mineral arranged in the objective table 21 (vacuum cavity) can be collected by the energy spectrum probe.
While the application has been described with reference to a preferred embodiment, various modifications may be made and equivalents may be substituted for elements thereof without departing from the scope of the application. In particular, the technical features mentioned in the embodiments can be combined in any way as long as there is no structural conflict. The present application is not intended to be limited to the particular embodiments disclosed herein but is to cover all embodiments that may fall within the scope of the appended claims.

Claims (10)

1. A measuring point positioning device based on an energy spectrometer is characterized by comprising:
the device comprises an energy spectrum probe adjusting device and a control device, wherein the energy spectrum probe adjusting device comprises a connecting piece for mounting an energy spectrum probe and a first adjusting piece for adjusting an included angle of the connecting piece relative to a horizontal plane; and
the measuring point positioning device comprises a plane reflector and a second adjusting piece for adjusting the reflection angle of the plane reflector;
the angle of the connecting piece is selectively adjusted through the first adjusting piece, so that the energy spectrum probe captures an interesting energy spectrum beam spot on the objective table, and the plane reflecting mirror is selectively adjusted through the second adjusting piece to adjust the incident light spot to be coincident with the interesting energy spectrum beam spot.
2. The spectrometer-based station positioning device according to claim 1, wherein the first adjusting member comprises a fixed member and an adjusting rod slidably connected with the fixed member, one end of the adjusting rod is connected with the connecting member, and the other end of the adjusting rod is slidably connected with the fixed member so as to enable the connecting member to approach or depart from the fixed member.
3. The spectrometer-based station positioning device according to claim 2, wherein the fixing member comprises a base and a threaded sleeve protruding from the base, and the adjusting rod is a threaded rod matched with the threaded sleeve.
4. The spectrometer-based station positioning device of claim 2, wherein the adjustment rod is vertically disposed on the stage, and the connection is configured to angle the energy spectrum probe from the stage.
5. The spectrometer-based station positioning device according to claim 4, wherein the connecting piece is obliquely arranged on the adjusting rod.
6. The spectrometer-based station positioning device according to any one of claims 1 to 5, wherein the second adjusting part comprises a turbine and a worm, wherein the turbine and the worm are matched, the plane mirror is connected to the central shaft of the turbine, and the worm is rotated to drive the turbine to rotate so as to rotate the plane mirror.
7. The spectrometer-based station positioning device according to claim 6, wherein the second adjusting part further comprises a mirror support, the mirror support comprises a support rod and a support seat, one end of the support rod is rotatably connected with the central shaft of the turbine, and the other end of the support rod is connected with the support seat.
8. An energy spectrum testing system, which is characterized by comprising an energy spectrometer, a cathodoluminometer, a stage, a microscope, a polarizer and the measuring point positioning device based on the energy spectrometer, which is disclosed by any one of claims 1 to 7; the energy spectrum probe of the energy spectrometer is arranged on the connecting piece, and the cathodoluminescent instrument is selectively connected with the connecting piece; the objective table is horizontally arranged; the lens of the microscope is arranged opposite to the objective table, and the polarizer is arranged corresponding to the plane reflector.
9. The system according to claim 8, further comprising a light-transmissive vacuum chamber, wherein the stage is disposed within the light-transmissive vacuum chamber.
10. A testing method using the spectrum testing system of claim 8 or 9, the testing method comprising:
sample bombardment: bombarding a rock slice sample to be detected on the objective table by the cathode luminoscope;
determining the position of the energy spectrum beam spot: adjusting the first adjusting piece to enable an energy spectrum probe of the energy spectrometer to capture an interesting energy spectrum beam spot on the objective table;
positioning target measuring points: opening the polarizer, enabling the polarizer to emit incident light to irradiate the plane reflector, and adjusting the second adjusting piece to enable an incident light spot reflected by the plane reflector to coincide with the interesting energy spectrum beam spot;
energy spectrum beam spot calibration: calibrating by further adjusting the first adjusting part to ensure that the incident light spot coincides with the energy spectrum beam spot of interest;
and acquiring a preset energy spectrum, adjusting the incident light spot to coincide with the interested energy spectrum beam spot, and acquiring the preset energy spectrum of the rock slice sample to be detected on the objective table through an energy spectrum probe of the energy spectrum.
CN202011049299.1A 2020-09-29 2020-09-29 Measuring point positioning device based on energy spectrometer, energy spectrum testing system and testing method Pending CN114428093A (en)

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