CN211350574U - Laser ablation platform sample loading device - Google Patents

Laser ablation platform sample loading device Download PDF

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CN211350574U
CN211350574U CN202020335361.2U CN202020335361U CN211350574U CN 211350574 U CN211350574 U CN 211350574U CN 202020335361 U CN202020335361 U CN 202020335361U CN 211350574 U CN211350574 U CN 211350574U
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carrier gas
sample
fixed
cell
cover
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戴智慧
王敬富
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Institute of Geochemistry of CAS
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Institute of Geochemistry of CAS
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Abstract

The utility model discloses a laser ablation platform carries a kind device aims at providing an analytical accuracy is good, efficient ablation platform carries a kind device. Comprises a sample cell consisting of a cell body (7) and a cell cover (1), and a target holder arranged in the sample cell through a moving mechanism; the tank cover is provided with an ablation window (16), the side wall of the ablation window is provided with a gas outlet (15), and the ablation window (16) is sealed by a calcium fluoride glass sheet (14); the moving mechanism consists of two wheel shafts (8) arranged in the tank body (7), belt pulleys (2) fixed on the wheel shafts (8), a belt (12) wound on the two belt pulleys (2) and a pair of bevel gears for driving the belt to move; the target holder is composed of a sample chamber (6) fixed on a belt (12), a spring (5) positioned in the sample chamber, and a chamber cover (4) fixed on the sample chamber (6). The utility model discloses can hold a plurality of standard samples, and can instantaneous output smooth signal.

Description

Laser ablation platform sample loading device
Technical Field
The utility model relates to a laser instrument sampling system's improvement especially relates to an improvement that is used for Coherent laser system's degradation platform to carry appearance device, belongs to normal position micro-area analysis field.
Background
In the early development stage of the laser technology, the energy coupling efficiency is low, the fractionation is serious, and the analysis precision is poor. YAG lasers with four frequency multiplication (266nm) and five frequency multiplication (213nm) are sequentially generated, particularly, the development of the micro-area technology is greatly promoted when a 193nmARF quasi-molecular gas laser is generated, the aerosol particle size generated by the laser is uniform in distribution, higher in ionization efficiency, good in bombardment pit shape and weak in fractionation effect, the requirement on matrix matching calibration is greatly reduced, and the analysis precision and accuracy are improved. Since Gray in 1985 firstly combines the laser ablation technology with ICP-MS (inductively coupled plasma-mass spectrometer), the technology has made great progress in the research fields of instrument structural performance and analysis application due to the characteristics of low cost, high efficiency and high spatial resolution, and even becomes the first choice method for solid sample micro-area analysis.
Generally, the laser ablation system consists of a laser generator and an ablation platform, wherein the laser generator is divided into a solid state and a gas state, and commonly used nanosecond lasers comprise a solid Nd-YAG laser generator and an excimer ArF laser generator. The ablation platform comprises a light beam transmission system (prism system), a sample cell and a microscopic observation system. The denudation pool is a completely closed box body, and the upper part of the denudation pool is provided with a cover plate with calcium fluoride glass. The good denudation pool has the characteristics of easy sample replacement, tight air tightness, convenient quick flushing and the like. The horizontal laser beam is reflected by a 45-degree prism and then focused on the surface of a sample through a focusing system. The sample is vaporized as a result of the large laser energy striking the sample surface, and the aerosol sample is then transported out of the sample cell by the carrier gas. Since the laser produces a blank of about 0.08 seconds between each sample ablation, while the ICP-MS detector is continuously operated, the signal collected when LA is used in conjunction with ICP-MS is jagged. A good ablation cell should be able to output aerosol samples quickly and stably, so that aerosol losses can be minimized. Therefore, the design of the denudation pool and the design of the subsequent pipeline have a great influence on the smoothness of the signal.
In order to improve the fluctuation of the timing value of the LA and ICP-MS, a sample mixing vessel is usually added between a laser and a plasma mass spectrometer at present, so that an aerosol sample degraded by the laser has a pause before entering the mass spectrometer and is fully mixed, and finally, a signal received by the mass spectrometer is continuously and smoothly. Although the technology can obtain a continuous and smooth signal, the aerosol sample stops in the sample mixing vessel, and the mixing process delays the transient signal received by the mass spectrometer. Signal delay for samples that require detection of transient signals (e.g., bag in mineral samples), the bag and substrate composition cannot be distinguished because the aerosol mixes with the substrate during transport.
The Coherent laser was equipped with an ablation cell having a cylindrical sample chamber with a diameter of 5.5 cm. While the domestic geological samples are generally two types, one is an epoxy resin target with the diameter of 1 inch, and the other is
Figure DEST_PATH_GDA0002568099030000021
The sheet of (1). The use of LA-ICP-MS techniques for testing geological samples is often calibrated using multiple external standards, which requires that sufficient space be available to hold multiple standards while the sample is placed in the sample chamber. The existing denudation pool can only contain 1-2 samples to be tested, and the samples need to be frequently replaced, so that the operation is troublesome, the efficiency is low, and the stability of the instrument is also unfavorable. In addition, the aerosol sample is easy to form a high-speed rotating airflow in the circular hole-shaped ablation window and is not easy to be quickly discharged out of the ablation pool. Therefore, it is necessary to develop a denudation cell that can accommodate a plurality of samples and instantaneously output a smooth signal for testing geological samples using LA-ICP-MS analysis.
Disclosure of Invention
To the above-mentioned defect that exists among the prior art, the utility model aims at providing a laser ablation platform that test analysis precision is good, work efficiency is high carries appearance device.
In order to achieve the above purpose, the utility model adopts the following technical scheme: the device comprises a closed sample cell with a carrier gas inlet and a carrier gas outlet, a target holder arranged in the sample cell through a moving mechanism, and a calcium fluoride glass sheet fixed on the surface of the sample cell; the sample tank consists of a tank body and a tank cover, wherein the tank body is provided with two carrier gas inlets on the tank wall, the tank cover is used for sealing the tank body, the surface of the tank cover is provided with an ablation window, the side wall of the ablation window is provided with a carrier gas outlet, and a calcium fluoride glass sheet fixed on the surface of the tank cover seals the ablation window; the moving mechanism consists of at least two wheel shafts vertically arranged in the tank body, belt pulleys fixed on the wheel shafts, belts laterally surrounding the two belt pulleys, a driven bevel gear fixed on one of the wheel shafts, and a driving bevel gear arranged on the tank body and meshed with the driven bevel gear; the target seats are multiple, and each target seat is composed of a sample cabin fixed on the surface of the belt, a spring positioned in the sample cabin and a cabin cover fixed on the sample cabin.
The denudation window is a cam-shaped structure consisting of an arc surface and two planes which are distributed in a splayed shape, and the carrier gas outlet is positioned between the two planes; the carrier gas outlet is positioned on the back of the tank cover, the two carrier gas inlets are positioned on the front of the tank body and close to the bottom of the tank, and the two carrier gas inlets are symmetrically distributed on the two sides of the carrier gas outlet; the carrier gas outlet is connected with an air outlet nozzle fixed on the tank cover, and each carrier gas inlet is connected with the three-way pipe through an air inlet nozzle respectively fixed on the tank body; the driving bevel gear is connected with a stepping motor fixed on the box body.
Compared with the prior art, the utility model discloses owing to adopted above-mentioned technical scheme, improved on the basis of traditional structure, consequently had following advantage:
1) the round hole-shaped ablation window is changed into a cam or peach-shaped structure, so that the carrier gas can be guided to carry the sample aerosol to be rapidly and completely output through the carrier gas outlet, and the defect that the aerosol is difficult to rapidly and completely output due to the fact that the vortex is easily formed in the traditional structure is overcome.
2) The original carrier gas inlet is changed into two symmetrically distributed carrier gas inlets, and a three-way pipe is adopted to connect the two carrier gas inlets, so that the pressure balance of the gas at the two sides of the inner cavity can be kept, and the carrier gas is prevented from being retained in the tank body.
3) The moving mechanism driven by the stepping motor can quickly and accurately realize the movement of the target holder, thereby reducing the labor intensity and improving the operation efficiency.
4) A plurality of sample cabins are fixed on the belt, so that a plurality of standard samples can be installed at one time, the trouble that the tank cover needs to be frequently disassembled to replace the samples in the prior art is avoided, and the working efficiency is improved.
5) The spring is additionally arranged in the sample cabin, so that a thin sample or an epoxy resin target can be tightly pushed and positioned, the surfaces of all samples can be ensured to be in the same plane, and the rapid focusing is convenient.
Drawings
Fig. 1 is a schematic structural diagram of the present invention;
FIG. 2 is a top view of FIG. 1;
FIG. 3 is a cross-sectional view A-A of FIG. 1;
fig. 4 is a view from direction B in fig. 1.
In the figure: the device comprises a pool cover 1, a belt pulley 2, a sample 3, a cabin cover 4, a spring 5, a sample cabin 6, a pool body 7, a wheel shaft 8, a driven bevel gear 9, a driving bevel gear 10, a stepping motor 11, a belt 12, a gland 13, a calcium fluoride glass sheet 14, a carrier gas outlet 15, an ablation window 16, an air outlet nozzle 17, an air inlet nozzle 18, an arc surface 19 and a plane 20.
Detailed Description
The invention will be further described with reference to the accompanying drawings and specific embodiments.
As shown in FIGS. 1-4: the sample cell is composed of a cell body 7 with two carrier gas inlets (not shown) on the cell wall, and a cell cover 1 fixed on the cell body by screws (not shown) and sealing the cell body. The surface of the tank cover is provided with an ablation window 16, and the side wall of the ablation window is provided with a carrier gas outlet 15 communicated with the sample tank; a calcium fluoride glass plate 14 fixed to the surface of the cell cover 1 by a press cover 13 seals the ablation window 16. The tank body 7 is internally provided with a moving mechanism which is composed of at least two wheel shafts 8 vertically arranged at the bottom of the tank through bearings (not shown in the figure), belt pulleys 2 fixed on the wheel shafts 8, a belt 12 laterally surrounding the two belt pulleys 2, a driven bevel gear 9 fixed on one wheel shaft 8, and a driving bevel gear 10 arranged on the wall of the tank through a bearing and meshed with the driven bevel gear. In order to avoid the belt 12 slipping off, both ends of the belt pulley 2 are provided with flanges; to avoid slack in the belt 12, a plurality of belt tensioners (labeled for this purpose in the figures) may also be provided between the drive pulley and the driven pulley. A plurality of target seats are uniformly distributed on the belt 12, and each target seat is composed of a sample cabin 6 fixed on the surface of the belt 12, a spring 5 positioned in the sample cabin 6 and a cabin cover 4 fixed on the sample cabin 6. In order to facilitate the flow of the carrier gas, the sample chamber 6 is of a cylindrical structure with a hatch (not shown in the figure) at the bottom; similarly, the hatch is opened on the top of the hatch 4. The sample chamber 6 and the belt 12 are fixed in various ways, such as magnetic adsorption, adhesive fixation, elastic rubber ring binding, screw connection, and slot fixation.
In order to facilitate rapid removal of the aerosol and avoid the formation of a vortex in the air flow in the erosion window 16, the erosion window 16 adopts a cam-shaped structure formed by an arc surface 19 and two splayed planes 20, and the carrier gas outlet 15 is arranged between the two planes 20.
In order to ensure the pressure balance of all parts in the sample cell and avoid dead angles, the carrier gas outlet 15 is arranged on the back of the cell cover 1, the two carrier gas inlets are arranged on the front of the cell body 7 and close to the bottom of the cell, and the two carrier gas inlets are symmetrically distributed on two sides of the carrier gas outlet 15. In order to facilitate the connection of the air pipes, an air outlet nozzle 17 communicated with the carrier gas outlet 15 is fixed on the tank cover 1, an air inlet nozzle 18 communicated with the corresponding carrier gas inlet is fixed on the tank body 7, and the two air inlet nozzles 18 are connected with the three-way pipe through air pipes (not marked in the figure).
In order to improve the efficiency and reduce the labor intensity, a stepping motor 11 connected with a driving bevel gear 10 is fixed on the tank body 7.
In order to improve the sealing performance of the sample cell, sealing rings (not shown in the figure) are arranged between the cell body 7 and the cell cover 1 and between the driving bevel gear shaft and the cell body 7.
When in use, the belt 12 is driven to move by a manual or stepping motor 11 until the required target holder moves to the position of the ablation window 16; inputting carrier gas, starting a vacuum pump, and irradiating the sample 3 in the target holder by laser.

Claims (4)

1. A laser ablation platform sample loading device comprises a closed sample cell with a carrier gas inlet and a carrier gas outlet, a target holder arranged in the sample cell through a moving mechanism, and a calcium fluoride glass sheet fixed on the surface of the sample cell; the method is characterized in that:
the sample cell is composed of a cell body (7) with two carrier gas inlets on the cell wall and a cell cover (1) for sealing the cell body, wherein the surface of the cell cover is provided with an ablation window (16), the side wall of the ablation window is provided with a carrier gas outlet (15), and a calcium fluoride glass sheet (14) fixed on the surface of the cell cover (1) seals the ablation window (16);
the moving mechanism is composed of at least two wheel shafts (8) vertically arranged in the tank body (7), belt pulleys (2) fixed on the wheel shafts (8), belts (12) laterally surrounding the two belt pulleys (2), a driven bevel gear (9) fixed on one of the wheel shafts (8), and a driving bevel gear (10) arranged on the tank body (7) and meshed with the driven bevel gear;
the target seats are multiple, and each target seat is composed of a sample cabin (6) fixed on the surface of the belt (12), a spring (5) positioned in the sample cabin (6) and a cabin cover (4) fixed on the sample cabin (6).
2. The laser ablation platform sample loading device of claim 1, wherein: the denudation window (16) is a cam-shaped structure consisting of a circular arc surface (19) and two planes (20) which are distributed in a splayed shape, and the carrier gas outlet (15) is positioned between the two planes (20).
3. The laser ablation platform sample loading device of claim 1 or 2, wherein: the carrier gas outlet (15) is positioned on the back of the tank cover (1), the two carrier gas inlets are positioned on the front of the tank body (7) and close to the bottom of the tank, and the two carrier gas inlets are symmetrically distributed on the two sides of the carrier gas outlet (15); the carrier gas outlet (15) is connected with an air outlet nozzle (17) fixed on the tank cover (1), and each carrier gas inlet is connected with the three-way pipe through an air inlet nozzle (18) respectively fixed on the tank body (7).
4. The laser ablation platform sample loading device of claim 1 or 2, wherein: the driving bevel gear (10) is connected with a stepping motor (11) fixed on the tank body (7).
CN202020335361.2U 2020-03-17 2020-03-17 Laser ablation platform sample loading device Expired - Fee Related CN211350574U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114384009A (en) * 2021-05-17 2022-04-22 中国海洋石油集团有限公司 Sealed sample pool for laser high-temperature melting of carbonate sample and use method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114384009A (en) * 2021-05-17 2022-04-22 中国海洋石油集团有限公司 Sealed sample pool for laser high-temperature melting of carbonate sample and use method thereof

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