CN110596076B - Automatic sample loading device of glow discharge spectrometer and loading method thereof - Google Patents
Automatic sample loading device of glow discharge spectrometer and loading method thereof Download PDFInfo
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/11—Filling or emptying of cuvettes
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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- G01N21/13—Moving of cuvettes or solid samples to or from the investigating station
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/66—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence
- G01N21/67—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence using electric arcs or discharges
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N2021/0106—General arrangement of respective parts
- G01N2021/0112—Apparatus in one mechanical, optical or electronic block
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/03—Cuvette constructions
- G01N2021/0367—Supports of cells, e.g. pivotable
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/11—Filling or emptying of cuvettes
- G01N2021/115—Washing; Purging
Abstract
The invention relates to an automatic sample loading device of a glow discharge spectrometer and a loading method thereof, wherein a sample is placed at the bottom of an objective table of the automatic sample loading device and is connected with a power supplier of the glow discharge spectrometer; the stage moves to another position as set for excitation and cleaning. The method can realize the full-automatic acquisition of the three-dimensional distribution information of the element content of the sample.
Description
Technical Field
The invention discloses an automatic sample loading device and method for a glow discharge spectrometer, and belongs to the technical field of spectral analysis.
Background
The glow discharge emission spectroscopy (GDS for short) can sputter the atomic layers on the surface of the material layer by layer in an ion sputtering manner, so that the quantitative analysis result of the surface chemical components of the material is obtained layer by layer (the depth resolution can reach 1-10 nm), and the thickness of the coating or the interface can be visually seen (as shown in fig. 4). The GDS technology can be used for directly performing surface layer analysis and layer-by-layer analysis on solid samples such as conductors, non-metals, thin films, semiconductors, insulators, organic materials and the like, and has wide application. At present, the GDS technology has been successfully applied to the application fields of semiconductor industry, automobile industry, steel industry, glass, ceramic industry, building material industry, etc., and the analysis and application in various material industries have important roles in controlling the quality of materials and improving the performance of materials.
However, the existing glow discharge spectrometer can only obtain multi-element component information in the depth direction of the material once, and cannot automatically move to another analysis sputtering point for deep analysis after the deep distribution analysis of one sputtering point is carried out, so that the three-dimensional distribution data of the chemical elements of the sample can be obtained.
Disclosure of Invention
The invention designs an automatic sample loading device of a glow discharge spectrometer and a loading method thereof aiming at the prior art, and aims to detect the three-dimensional distribution information of chemical components of a sample by using the glow discharge spectrometer.
In order to achieve the purpose, the invention adopts the following technical scheme:
the automatic sample loading device of the glow discharge spectrometer comprises a moving mechanism with a Z-axis portal frame 1 and an X-axis portal frame 2, an objective table 3 is arranged on the Z-axis portal frame 1 and the X-axis portal frame 2 which are arranged in a crossed manner and moves along the Z-axis portal frame 1 and the X-axis portal frame 2 along with the control of a control system 6, and the bearing surface of the objective table 3 is an elastomer and is connected with a power supply 5 of a glow discharge spectrometer 8;
a glow discharge spectrometer 8 controlled by a control system 6 is arranged on the back of the bearing surface of the objective table 3, and an excitation hole 7 of the glow discharge spectrometer 8 is opposite to the moving mechanism;
the front side of the bearing surface of the objective table 3 is provided with a rotating table 10, the rotating axial direction of the rotating table 10 is parallel to the horizontal Y axis in the portal frame coordinate system, the front end surface of the rotating table 10 is provided with a rod-shaped clamping head 11 and a first cleaning head 12, the rotating table 10, the clamping head 11 and the first cleaning head 12 are controlled by a control system 6, and the clamping head 11 and the first cleaning head 12 have structures of an inward-retracting rotary table 10.
In one embodiment, the resilient body of the load-bearing surface of the object table 3 is formed by a spring 4.
In one embodiment, the position of the object table 3 on the Z-axis gantry 1 and the X-axis gantry 2 is locked by a locking device 9 located around the object table 3.
In one implementation, the diameter of the excitation holes is 1mm, 2mm, 4mm, 7mm, or 8 mm.
In one implementation, the movement mechanism, stage 3 and rotation stage 10, and the excitation well 7 of the glow discharge spectrometer 8 are in a sample chamber 14.
In one implementation, the center of the carrying surface of the stage 3 is 8-20cm from the center of the excitation well 7 of the glow discharge spectrometer 8. This distance keeps the stage 3 away from the excitation hole 7, leaving a place for the excitation hole 7 to be cleaned, but too far away, which can result in too long a movement time and an excessively large device volume;
in one implementation, a rod-shaped second cleaning head 13 is further arranged on the front end surface of the rotary table 10, the second cleaning head 13 is controlled by the control system 6, and the rotary table 10 is retracted;
in one implementation, the first cleaning head 12 is made of a steel brush and is used for cleaning the excitation hole 7, and the diameter of the first cleaning head is 0.05mm-0.20mm smaller than that of the excitation hole 7; the second cleaning head 13 is a copper pipe, and the diameter of the second cleaning head is 0.05mm-0.20mm smaller than that of the exciting hole 7. The steel brush can brush away the positive pole surface attachment, and the copper pipe can also play the friction effect except that falling positive pole bottom and surface attachment on every side, avoids the positive pole inner circle to have the scratch owing to brush the washing just for a long time. The cleaning can also be carried out by only using a first cleaning head;
the technical scheme of the invention also provides a loading method for the automatic sample loading device of the glow discharge spectrometer, which is characterized in that: the method comprises the following steps:
the method comprises the following steps: placing a sample on a bearing surface of an objective table 3, locking the objective table 3 by using a locking device 9, and connecting a power supply 5 of a glow discharge spectrometer 8 with circulating cooling water;
step two: the control system 6 controls the rotation of the rotating platform 10 to enable the clamping head 11 to be positioned on a working station, the working station enables the clamping head 11, the first cleaning head 12 or the second cleaning head 13 to be aligned with the excitation hole 7 of the glow discharge spectrometer 8, and the outer contour of the sample is positioned outside the outer diameter of the excitation hole 7;
the control system 6 controls the moving mechanism to move so that the sample is positioned between the clamping head 11 and the excitation hole 7;
step three, the control system 6 controls the rotating platform 10 to move forwards, the sample is pushed to the excitation hole 7 through the elastic deformation of the bearing surface of the objective table 3, the sample excitation position corresponding to the excitation hole 7 is the initial excitation position at the moment, and the bin door of the sample bin 14 is closed;
step four: under the control of the control system 6, the glow discharge spectrometer 8 sequentially performs vacuumizing, argon filling, excitation and detection to obtain element content distribution detection data of the sample in the depth direction at the initial excitation position, and transmits the data and the initial excitation position information to the control system 6, and the control system 6 calculates to obtain an element depth distribution curve of the element content of the sample at the position according to the received signal intensity and the depth information;
step five: after the excitation at the initial excitation position is finished, stopping argon filling and vacuumizing in sequence to enable the excitation hole 7 to be communicated with the atmosphere, and driving the clamping head 11 to move backwards by the rotary table 10;
step six: the moving mechanism drives the objective table 3 to move upwards so as to leave the position for cleaning operation;
step seven: the rotary table 10 rotates to the first cleaning head 12 and is positioned on a working station, the clamping head 11 and the second cleaning head 13 are retracted into the rotary table 10, and the rotary table 10 moves forwards until the steel brush of the first cleaning head 12 extends into the excitation hole 7 for cleaning;
the cleaning steps of the cleaning head are as follows: rotating 3-7 circles in one direction, then rotating 3-7 circles in the other direction, and then advancing and retreating 3-5 times; the rotation, the forward movement and the backward movement are all used for brushing off residues attached to the anode copper ring at the position of the excitation hole, time is wasted when the times are too many, and the anode copper ring cannot be cleaned when the times are too few;
step eight: the rotary table 10 drives the first cleaning head 12 to move backwards, meanwhile, the rotary table 10 rotates to the second cleaning head 13 to be located on a working station, the clamping head 11 and the first cleaning head 12 are retracted and rotated into the rotary table 10, and gas in the exciting holes 7 is blown outwards for cleaning; the rotating platform 10 moves forwards again until the steel pipe of the second cleaning head 13 goes deep into the excitation hole 7 for cleaning;
step nine: the rotating platform 10 drives the second cleaning head 13 to move backwards, and the gas in the exciting hole 7 is blown outwards for cleaning;
step ten: the moving mechanism drives the object stage 3 to slightly move to another set position, and the steps from two to nine are repeated to excite, clean and detect the other position on the surface of the sample.
Step eleven: and the control system 6 calculates a three-dimensional distribution diagram of the content of the sample elements according to the received excitation position and the element depth distribution curve data of the corresponding position.
In one implementation, argon is used for blowing cleaning, and the gas flow is 2-5L/min during blowing cleaning, and the flushing is carried out for 1-3 times, 1-3s each time. The flow is too small, the flushing effect is not achieved, the flow is too large, the safety is not good, and the human body and parts in the sample bin are damaged; the gas is flushed for 1 to 3 times, 1 to 3 seconds each time, the flushing effect may not be achieved if the flushing frequency is too short, and the argon and the time are wasted if the flushing frequency is too high.
Further, the sample was a nickel-base superalloy.
The technical scheme of the invention can ensure that the equipment automatically moves to another analysis sputtering point for depth analysis after the depth distribution analysis of one sputtering point is carried out on the sample plane until the required two-dimensional analysis sputtering point is obtained on the sample plane, and the depth distribution curve carried out on each sputtering point is added, thereby obtaining the millimeter-scale and depth-direction nanoscale chemical element three-dimensional distribution data on the surface of the sample, and obtaining the mesoscopic scale micron-scale analysis data when a plurality of nanometer layer data are subjected to superposition statistical calculation.
In the method, after the first excitation hole is excited, the position of an excitation point and the depth distribution information of element components at the position are obtained, then the position is automatically adjusted to obtain the excitation holes with two-dimensional distribution on the surface of the sample, and each excitation hole has the depth distribution information of the element components, so that the three-dimensional distribution information of the element components of the sample is formed. The diameter of each excitation hole is in millimeter level, such as 1mm, 2mm, 4mm, 7mm and 8mm, and the depth distribution information of nm level can be obtained during the depth distribution analysis of elements. The technology is applied to the nickel-based superalloy, and the cross-scale macroscopic, mesoscopic and microscopic three-dimensional distribution data of the chemical elements of the nickel-based superalloy can be obtained. Therefore, by developing an automatic sample loading device and a glow discharge emission spectrum three-dimensional component determination method, high-throughput characterization of multi-scale three-dimensional component distribution can be realized.
Drawings
FIG. 1 is a schematic view of a moving mechanism with a stage
FIG. 2 is a schematic view of a turntable
FIG. 3 is a schematic structural diagram of an automatic sample loading device of a glow discharge spectrometer
FIG. 4 is a diagram showing the result of quantitative analysis of chemical components on the surface of a galvanized steel sheet by glow discharge spectroscopy
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and embodiments, it being understood that the following embodiments are illustrative of the invention only and are not limiting.
Referring to attached drawings 1-3, an automatic sample loading device of a glow discharge spectrometer is connected with the glow discharge spectrometer for use, the automatic sample loading device of the glow discharge spectrometer comprises a moving mechanism with a Z-axis portal frame 1 and an X-axis portal frame 2, an object stage 3 is arranged between the crossed Z-axis portal frame 1 and the crossed X-axis portal frame 2 and can move along the X-axis direction and the Z-axis direction along with the setting of a control system 6, the vertical distance from the center of the object stage 3 to the center of an excitation hole 7 of the glow discharge spectrometer 8 is 18cm after the object stage 3 moves due to the sizes of the Z-axis portal frame 1 and the X-axis portal frame 2, a spring 4 is arranged at the bottom of the object stage 3, and locking devices 9 are arranged on the periphery of the object stage 3;
the rotating platform 10 is provided with a clamping head 11, a first cleaning head 12 and a second cleaning head 13 which can rotate under the control of the control system 6 and can move towards the excitation hole 7 of the glow discharge spectrometer 8, the first cleaning head 12 is made of a steel brush, the diameter of the first cleaning head is 0.05mm-0.20mm smaller than that of the excitation hole 7, and the first cleaning head can be just inserted into the excitation hole 7; the second cleaning head 13 is a copper pipe, the diameter of the second cleaning head is 0.05mm-0.20mm smaller than that of the exciting hole 7, and the second cleaning head can be just inserted into the exciting hole 7;
a power supply device 5 of the glow discharge spectrometer 8 is connected with a bottom spring 4 of the objective table 3, circulating cooling water is introduced into the power supply device 5, the glow discharge spectrometer 8 is connected with a sample bin door 14 which can be opened and closed, and the closed sample bin door 14 can cover the automatic sample loading device;
when the automatic loading and detection of the sample are carried out, the following steps are carried out:
the method comprises the following steps: placing a sample on a bearing surface of an objective table 3, locking the objective table 3 by using a locking device 9, and connecting a power supply 5 of a glow discharge spectrometer 8 with circulating cooling water;
step two: the control system 6 controls the rotation of the rotating platform 10 to enable the clamping head 11 to be positioned on a working station, the working station enables the clamping head 11, the first cleaning head 12 or the second cleaning head 13 to be aligned with the excitation hole 7 of the glow discharge spectrometer 8, and the outer contour of the sample is positioned outside the outer diameter of the excitation hole 7;
the control system 6 controls the moving mechanism to move so that the sample is positioned between the clamping head 11 and the excitation hole 7;
step three, the control system 6 controls the rotating platform 10 to move forwards, the sample is pushed to the excitation hole 7 through the elastic deformation of the bearing surface of the objective table 3, the sample excitation position corresponding to the excitation hole 7 is the initial excitation position at the moment, and the bin door of the sample bin 14 is closed;
step four: under the control of the control system 6, the glow discharge spectrometer 8 sequentially performs vacuumizing, argon filling, excitation and detection to obtain element content distribution detection data of the sample in the depth direction at the initial excitation position, and transmits the data and the initial excitation position information to the control system 6, and the control system 6 calculates to obtain an element depth distribution curve of the element content of the sample at the position according to the received signal intensity and the depth information;
step five: after the excitation at the initial excitation position is finished, stopping argon filling and vacuumizing in sequence to enable the excitation hole 7 to be communicated with the atmosphere, and driving the clamping head 11 to move backwards by the rotary table 10;
step six: the moving mechanism drives the objective table 3 to move upwards so as to leave the position for cleaning operation;
step seven: the rotary table 10 rotates to the first cleaning head 12 and is positioned on a working station, the clamping head 11 and the second cleaning head 13 are retracted into the rotary table 10, and the rotary table 10 moves forwards until the steel brush of the first cleaning head 12 extends into the excitation hole 7 for cleaning;
the cleaning steps of the cleaning head are as follows: rotating 3-7 circles in one direction, then rotating 3-7 circles in the other direction, and then advancing and retreating 3-5 times; the rotation, the forward movement and the backward movement are all used for brushing off residues attached to the anode copper ring at the position of the excitation hole, time is wasted when the times are too many, and the anode copper ring cannot be cleaned when the times are too few;
step eight: the rotary table 10 drives the first cleaning head 12 to move backwards, meanwhile, the rotary table 10 rotates to the second cleaning head 13 to be located on a working station, the clamping head 11 and the first cleaning head 12 are retracted and rotated into the rotary table 10, and gas in the exciting holes 7 is blown outwards for cleaning; the rotating table 10 is moved forward again until the steel pipe of the second cleaning head 13 enters the excitation hole 7, and cleaning is performed.
Step nine: the rotating platform 10 drives the second cleaning head 13 to move backwards, and the gas in the exciting hole 7 is blown outwards for cleaning;
step ten: the moving mechanism drives the objective table 3 to make micro movement, and the steps from two to nine are repeated to excite, clean and detect the other position of the surface of the sample.
Step eleven: and after the control system controls all the sputtering points to excite and detect, transmitting the obtained element content distribution detection data and the corresponding excitation position information to the control system, and calculating by control system software according to the element content distribution detection data and the corresponding excitation point position information to obtain a three-dimensional distribution map of the element content of the sample.
FIG. 4 is a graph showing the depth distribution of Zn and Fe elements obtained by glow discharge spectroscopy at a certain sputtering point on the surface of a galvanized steel sheet, and showing the variation of the element content at different depth positions of the sputtering point. The ordinate is the element content calculated by the excitation signal intensity, the abscissa is the excitation depth, the zero position of the abscissa is the position of the outermost surface of the sample sputtering point, the positive direction of the abscissa is the depth distance from the sputtering point to the outermost surface, as can be seen from fig. 4, the Zn element is mainly located on the surface of the galvanized steel sheet, then along with the depth change, the Zn element content gradually decreases, the Fe element content gradually increases, the galvanized layer is completely sputtered at the deeper position, and the position is sputtered to the steel sheet, so the Fe element is mainly located.
Claims (11)
1. An automatic sample loading device of glow discharge spectrometer is characterized in that: the device comprises a moving mechanism with a Z-axis portal frame (1) and an X-axis portal frame (2), an objective table (3) is arranged on the Z-axis portal frame (1) and the X-axis portal frame (2) which are arranged in a cross way and moves along the Z-axis portal frame (1) and the X-axis portal frame (2) along with the control of a control system (6), and the bearing surface of the objective table (3) is an elastic body and is connected with a power supply (5) of a glow discharge spectrometer (8);
a glow discharge spectrometer (8) controlled by a control system (6) is arranged on the back of the bearing surface of the objective table (3), and an excitation hole (7) of the glow discharge spectrometer (8) is opposite to the moving mechanism;
a rotating platform (10) is arranged on the front surface of the bearing surface of the objective table (3), the rotating axial direction of the rotating platform (10) is parallel to the horizontal Y axis in the portal frame coordinate system,
the front end surface of the rotating platform (10) is provided with a rod-shaped clamping head (11) and a first cleaning head (12), the rotating platform (10), the clamping head (11) and the first cleaning head (12) are controlled by a control system (6), and the clamping head (11) and the first cleaning head (12) are provided with structures of an inward-retracting rotary rotating platform (10).
2. The automatic sample loading device of glow discharge spectrometer of claim 1, wherein: the elastic body of the bearing surface of the objective table (3) is composed of a spring (4).
3. The automatic sample loading device of glow discharge spectrometer of claim 1, wherein: the positions of the objective table (3) on the Z-axis portal frame (1) and the X-axis portal frame (2) are locked by locking devices (9) positioned on the periphery of the objective table (3).
4. The automatic sample loading device of glow discharge spectrometer of claim 1, wherein: the diameter of the excitation holes is 1mm, 2mm, 4mm, 7mm or 8 mm.
5. The automatic sample loading device of glow discharge spectrometer of claim 1, wherein: the moving mechanism, the object stage (3), the rotating stage (10) and the excitation hole (7) of the glow discharge spectrometer (8) are arranged in a sample chamber (14).
6. The automatic sample loading device of glow discharge spectrometer of claim 1, wherein: the shortest distance between the center of the bearing surface of the object stage (3) and the center of the excitation hole (7) of the glow discharge spectrometer (8) is 8-20 cm.
7. The automatic sample loading device of glow discharge spectrometer of claim 1, wherein: the front end surface of the rotating platform (10) is provided with a rod-shaped second cleaning head (13), the second cleaning head (13) is controlled by a control system (6) and has a structure of an inward-shrinkage rotary rotating platform (10).
8. An automatic sample loading device for a glow discharge spectrometer according to claim 1 or 7, wherein: the first cleaning head (12) is made of a steel brush and is used for cleaning the excitation hole (7), and the diameter of the first cleaning head is 0.05mm-0.20mm smaller than that of the excitation hole (7); the second cleaning head (13) is a copper pipe, and the diameter of the second cleaning head is 0.05mm-0.20mm smaller than that of the exciting hole (7).
9. A loading method for the automatic sample loading device of the glow discharge spectrometer as claimed in claim 1 or 7, wherein: the method comprises the following steps:
the method comprises the following steps: placing a sample on a bearing surface of an objective table (3), locking the objective table (3) by using a locking device (9), and connecting a power supply (5) of a glow discharge spectrometer (8) with circulating cooling water;
step two: the control system (6) controls the rotation of the rotating platform (10) to enable the clamping head (11) to be positioned on a working station, and the working station enables the clamping head (11), the first cleaning head (12) or the second cleaning head (13) to be aligned to an excitation hole (7) of the glow discharge spectrometer (8);
the control system (6) controls the moving mechanism to move so that the sample is positioned between the clamping head (11) and the excitation hole (7), and the outer contour of the sample is positioned outside the outer diameter of the excitation hole (7);
step three, the control system (6) controls the rotating platform (10) to move forwards, the sample is pushed to the excitation hole (7) through elastic deformation of the bearing surface of the objective table (3), the sample excitation position corresponding to the excitation hole (7) is the initial excitation position at the moment, and the bin door of the sample bin (14) is closed;
step four: under the control of the control system (6), the glow discharge spectrometer (8) sequentially performs vacuumizing, argon filling, excitation and detection to obtain element content distribution detection data of the sample in the depth direction at the initial excitation position, and transmits the data and the initial excitation position information to the control system (6), and the control system (6) calculates to obtain an element depth distribution curve of the element content of the sample at the position according to the received signal intensity and the depth information;
step five: after the excitation at the initial excitation position is finished, stopping argon filling and vacuumizing in sequence to enable the inside of the excitation hole (7) to be communicated with the atmosphere, and driving the clamping head (11) to move backwards by the rotary table (10);
step six: the moving mechanism drives the objective table (3) to move upwards so as to leave the position for cleaning operation;
step seven: the rotary table (10) rotates to the position that the first cleaning head (12) is located on a working station, the clamping head (11) and the second cleaning head (13) are retracted into the rotary table (10), and the rotary table (10) moves forwards until the steel brush of the first cleaning head (12) penetrates into the excitation hole (7) to be cleaned;
step eight: the rotary table (10) drives the first cleaning head (12) to move backwards, meanwhile, the rotary table (10) rotates to the second cleaning head (13) to be positioned on a working station, the clamping head (11) and the first cleaning head (12) are retracted into the rotary table (10), and gas in the exciting holes (7) is blown outwards for cleaning; the rotating platform (10) moves forwards again until the steel pipe of the second cleaning head (13) goes deep into the excitation hole (7) for cleaning;
step nine: the rotating table (10) drives the second cleaning head (13) to move backwards, and the gas in the exciting hole (7) is blown outwards for cleaning;
step ten: the moving mechanism drives the objective table (3) to make micro movement, the steps from two to nine are repeated, and the other position on the surface of the sample is excited, cleaned and detected;
step eleven: and the control system (6) calculates a three-dimensional distribution diagram of the content of the sample elements according to the received excitation position and the element depth distribution curve data of the corresponding position.
10. The loading method of the automatic sample loading device of the glow discharge spectrometer as claimed in claim 9, wherein: and (4) performing blowing cleaning by adopting argon, wherein the gas flow is 2-5L/min during blowing cleaning, and the flushing is performed for 1-3 times, and each time lasts for 1-3 s.
11. The loading method of the automatic sample loading device of the glow discharge spectrometer as claimed in claim 9, wherein: the sample was a nickel-based superalloy.
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