Rapid washing-out denudation pool

Abstract

A rapid washing-out denudation pool capable of overcoming the spatial position effect comprises a sample pool, a denudation pool, a sample pool air inlet pipe, a sample outlet pipe, a sample outlet air inlet pipe, denudation laser and a driving platform, the sample pool is placed above the driving platform, a sample table used for containing a sample is arranged in the sample pool, the denudation pool is installed on the sample pool, and the driving platform is arranged on the driving platform. The denudation laser is arranged above the denudation pool and is used for denudating the sample. The gas inlet and the sample outlet are formed in the bottom of the denudation pool, and the gas inlet is formed in the outer side of the sample outlet, so that the gas flow transmission distance between the gas inlet and the sample outlet is reduced, and gas entering the sample pool through the gas inlet carries a denudation sample to be directly discharged from the sample outlet; and a spatial position effect caused by an overlong transmission distance of the carrier gas in the sample pool is avoided.

Description

Technical Field

[0001] The invention belongs to the technical field of laser ablation pools, and in particular relates to a fast wash-out ablation pool. Background Art

[0002] Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is the preferred tool for direct analysis of solid materials and has a wide range of applications in various fields. The key indicators for evaluating the quality of the ablation cell are the sample washout time and spatial repeatability. The sample washout time refers to the time span for the mass spectrometer to detect the signal peak under single pulse ablation, and is generally measured by the time span of 10% peak signal (FW0.1). Low-diffusion sample cells can improve sample test sensitivity, reduce detection limits, and increase sample test throughput. Spatial repeatability refers to the consistency of each position of the ablation cell, which directly affects the accuracy and precision of the sample test. The spatial position effect is caused by the difference in airflow distribution inside the sample cell. The low-diffusion denudation cell generally adopts a double-volume denudation cell, which can be divided into two types according to the placement of the displacement stage. The displacement stage moves the small-volume denudation cell outside the denudation cell through a motor to achieve relative motion and positioning. Due to airflow reasons, the spatial position effect of this type of denudation cell is poor, and the sample washing time is long; the displacement stage is placed in the denudation cell, resulting in a larger volume of the entire denudation cell, greater gas waste and a higher possibility of sample contamination. Summary of the invention

[0003] In view of the above shortcomings, the technical problem to be solved by the present invention is to provide a fast wash-out denudation pool, reduce the transmission distance of the sample output gas flow, and avoid the spatial position effect caused by the long transmission distance of the gas sample pool.

[0004] In order to solve the above technical problems, the technical solution adopted by the present invention is: A rapid wash-out denudation tank comprising: A sample pool, which is provided with a sample table for placing samples; The erosion cell is installed on the sample cell, and includes a coaxially arranged sample outlet tube and a blow tube. A sample outlet is provided at the bottom of the sample outlet tube, and an air inlet channel is formed between the sample outlet tube and the blow tube. A first carrier gas is introduced outside the sample outlet through the air inlet channel, so that the erosion sample in the sample cell is driven by the first carrier gas to be discharged from the sample outlet. The sample cell air inlet pipe is connected to the air blowing cylinder and is used to introduce the first carrier gas into the sample cell; The sample outlet pipe and the sample outlet air inlet pipe are respectively connected to the sample outlet tube, and the second carrier gas is introduced through the sample outlet air inlet pipe to drive the ablation sample to be discharged from the sample outlet pipe; The ablation laser component is used to ablate the sample, and the ablation laser component is arranged opposite to the sample outlet.

[0005] As a preferred solution of the present invention, the bottom end surface of the blowing cylinder is arranged higher than the bottom end surface of the sample outlet cylinder.

[0006] As a preferred solution of the present invention, the sample outlet tube is arranged in a conical shape, and the diameter of the sample outlet tube decreases from the top of the sample outlet tube to the sample outlet.

[0007] As a preferred embodiment of the present invention, the ablation laser assembly includes a laser generator and an objective lens, and the objective lens is arranged between the laser generator and the sample pool. The relationship between the taper of the sample outlet tube and the objective lens is as follows: θ=arcsin(NA)*f / d, wherein θ is the taper of the sample outlet tube, NA is the aperture value of the objective lens, f is the focal length of the objective lens, and d is the distance between the objective lens and the ablation pool.

[0008] As a preferred solution of the present invention, the ablation cell further comprises a window piece, and a sample outlet tube and an air blow tube are connected to the bottom of the window piece.

[0009] As a preferred solution of the present invention, the sample outlet tube includes a sample outlet section for outputting the denudation sample and a tapered section for connecting the sample outlet section and the denudation pool, and the diameter of the tapered section decreases from the denudation pool side to the sample outlet side.

[0010] As a preferred solution of the present invention, a connector for increasing the air flow velocity is provided on the sample outlet and air inlet pipe, and the sample outlet and air inlet pipe is connected to the erosion tank via the connector.

[0011] As a preferred solution of the present invention, a driving platform is provided at the bottom of the sample pool, and a magnetic component movable relative to the sample pool is provided in the driving platform. The magnetic component is connected to the sample stage, and the sample stage is driven to move in the sample pool by driving the magnetic component to move.

[0012] As a preferred solution of the present invention, a ball bearing is provided at the bottom of the sample stage, and the sample stage is movably placed in the sample pool through the ball bearing.

[0013] As a preferred solution of the present invention, the sample pool includes a pool body, an upper cover plate installed on the pool body and a window fixing plate arranged in the middle of the upper cover plate, a mounting block is provided at the bottom of the window fixing plate, and the erosion pool is fixed to the window fixing plate through the mounting block.

[0014] Compared with the prior art, the present invention has the following advantages: (1) by arranging the air inlet channel outside the sample outlet, the transmission distance of the carrier gas in the sample pool is reduced, thereby reducing the spatial position repeatability of the sample pool and improving the accuracy and precision of the test.

[0015] (2) By setting up the sample inlet pipe and the sample outlet pipe, the erosion sample in the erosion pool can be quickly discharged out of the device, thereby further improving the accuracy and precision of the test.

[0016] (3) By placing the driving platform outside the sample pool, it is convenient to reduce the volume of the sample pool, reduce the helium consumption required to empty the sample pool, and reduce the risk of sample contamination in the sample pool.

[0017] (4) By associating the taper of the sample outlet tube with the objective lens parameters of the ablation laser assembly, the internal volume of the sample outlet tube is minimized on the one hand, and swirl of the airflow in the sample outlet tube is avoided on the other hand. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 It is a structural diagram of the device.

[0019] Figure 2 It is a schematic diagram of the structure of the denudation pool.

[0020] Figure markings: sample pool 1, sample table 1-1, ball 1-2, pool body 1-3, upper cover plate 1-4, window fixing plate 1-5, mounting block 1-6, erosion pool 2, air inlet channel 2-1, sample outlet 2-2, sample outlet tube 2-3, air blow tube 2-4, window piece 2-5, sample pool air inlet pipe 3, sample outlet tube 4, sample outlet section 4-1, conical section 4-2, sample outlet air inlet pipe 5, connector 5-1, erosion laser assembly 6, laser generator 6-1, objective lens 6-2, driving platform 7, magnetic suction part 7-1, base 7-2. DETAILED DESCRIPTION

[0021] The present invention will be further described below in conjunction with the accompanying drawings.

[0022] A fast washing out ablation cell comprises: a sample cell 1, an ablation cell 2, a sample cell air inlet pipe 3, a sample outlet pipe 4, a sample outlet air inlet pipe 5, an ablation laser assembly 6 and a driving platform 7. The sample cell 1 is placed above the driving platform 7, a sample table 1-1 for placing a sample is provided inside the sample cell 1, the ablation cell 2 is installed on the sample cell 1, and the ablation laser assembly 6 is arranged above the ablation cell 2 for ablation of the sample. An air inlet channel 2-1 and a sample outlet 2-2 are provided at the bottom of the erosion pool 2. The air inlet channel 2-1 is used to ventilate the sample pool 1 so that the air pressure in the sample pool 1 increases. When the air pressure in the sample pool 1 increases to a certain value, the erosion sample generated by erosion and the gas in the sample pool 1 form an aerosol and are discharged from the sample pool 1 through the sample outlet 2-2; the air inlet channel 2-1 is arranged on the outside of the sample outlet 2-2, thereby reducing the airflow transmission distance of the air inlet channel 2-1 and the sample outlet 2-2, so that the gas entering the sample pool 1 through the air inlet channel 2-1 can carry the erosion sample and be discharged directly from the sample outlet 2-2, thereby avoiding the spatial position effect caused by the excessively long transmission distance of the carrier gas in the sample pool. The sample pool air inlet pipe 3 is connected to the air inlet channel 2-1, and is used to introduce a first carrier gas, which is helium. The helium enters the sample pool 1 through the sample pool air inlet pipe 3 and the air inlet channel 2-1 in turn, and inflates the sample pool 1, thereby increasing the air pressure of the sample pool 1. The sample outlet air inlet pipe 5 and the sample outlet tube 4 are respectively connected to the sample outlet port 2-2. Preferably, the sample outlet air inlet pipe 5 is arranged opposite to the sample outlet tube 4, and the sample outlet tube 4 is blown through the sample outlet air inlet pipe 5. The second carrier gas is introduced into the sample outlet air inlet pipe 5, and the second carrier gas is argon. The erosion sample entering the sample outlet tube 4 is discharged through the argon gas, thereby improving the discharge efficiency of the erosion sample.

[0023] The erosion pool 2 comprises a window piece 2-5, a sample outlet tube 2-3 and a blow tube 2-4 arranged coaxially, the sample outlet tube 2-3 and the blow tube 2-4 abut against the bottom of the window piece 2-5, and the sample outlet tube 2-3, the blow tube 2-4 and the window piece 2-5 are sealed and connected by an O-ring, a mounting block 1-6 is fixed at the bottom of the window fixing plate 1-5, and the blow tube 2-4 is abutted against the bottom of the window piece 2-5 by the mounting block 1-6, and at the same time, since the sample outlet tube 4 and the sample outlet air inlet tube 5 pass through the blow tube 2-4 and are connected to the sample outlet tube 2-3, the relative position between the blow tube 2-4 and the sample outlet tube 2-3 is fixed, and when the blow tube 2-4 abuts against the bottom of the window piece 2-5, the sample outlet tube 2-3 also abuts against the bottom of the window piece 2-5. During operation, a microscope can be arranged above the window piece 2-5 so as to observe the erosion progress in the sample pool 1 through the microscope. The sample outlet tube 2-3 is arranged on the inner side of the air cylinder 2-4, an air inlet channel 2-1 is formed between the sample outlet tube 2-3 and the air cylinder 2-4, and a sample outlet port 2-2 is formed at the bottom of the sample outlet tube 2-3; the sample pool air inlet pipe 3 is connected with the air cylinder 2-4, and the sample outlet pipe 4 and the sample outlet air inlet pipe 5 pass through the air cylinder 2-4 and are connected with the sample outlet tube 2-3. As a preferred embodiment, the ablation laser assembly 6 is coaxially arranged with the sample outlet tube 2-3 and the air cylinder 2-4, and the ablation laser assembly 6 includes a laser generator 6-1 and an objective lens 6-2. The laser generated by the laser generator 6-1 is focused by the objective lens 6-2 and enters the sample pool 1 facing the sample outlet port 2-2, so that the laser can ablate the sample after passing through the window piece 2-5.

[0024] The sample outlet tube 2-3 is set in a conical shape, and the diameter of the sample outlet tube 2-3 decreases from the top of the sample outlet tube 2-3 (close to the side of the window piece 2-5) to the sample outlet 2-2, so as to facilitate the erosion sample to enter the sample outlet tube 2-3 from the sample pool 1. In order to ensure sample extraction and observation of the microscopic field of view, the overall height of the erosion pool 2 does not exceed 5mm, the diameter of the sample outlet 2-2 is 1-2mm, and the relationship between the taper of the sample outlet tube 2-3 and the objective lens of the erosion laser assembly is as follows: θ=arcsin(NA)*f / d, wherein θ is the taper of the sample outlet tube 2-3, NA is the aperture value of the objective lens 6-2, f is the focal length of the objective lens 6-2, and d is the distance between the objective lens 6-2 and the erosion pool 2; by setting the taper of the sample outlet tube 2-3, on the one hand, the internal volume of the sample outlet tube 2-3 is reduced to the maximum extent, and on the other hand, the airflow in the sample outlet tube 2-3 is prevented from swirling. The air blowing tube 2-4 can be conical or cylindrical.

[0025] A connector 5-1 is provided on the sample outlet air inlet pipe 5, and the diameter of the connector 5-1 is smaller than that of the sample outlet air inlet pipe 5, so that the flow rate of other gases passing through the connector 5-1 is increased, and the sample outlet air inlet pipe 5 is connected to the sample outlet cylinder 2-3 through the connector 5-1. Preferably, the connector 5-1 is a pipe of equal diameter.

[0026] The sample outlet tube 4 includes a sample outlet section 4-1 and a tapered section 4-2. The two ends of the tapered section 4-2 are respectively connected to the sample outlet section 4-1 and the erosion pool 2. The sample outlet section 4-1 is connected to the sample outlet tube 2-3. The diameter of the tapered section 4-2 decreases from the side of the sample outlet tube 2-3 to the side of the sample outlet section 4-1, so as to facilitate the erosion sample to enter the tapered section 4-2.

[0027] The inner diameter of the sample outlet section 4-1 is 1.5 times the inner diameter of the sample outlet air inlet pipe 5, thereby ensuring the pressure difference between the sample outlet section 4-1 and the sample outlet air inlet pipe 5, improving the transmission rate of the particles, and realizing the rapid washing out of the eroded sample.

[0028] In order to further improve the washing efficiency of the sample, the bottom end face of the blow tube 2-4 is higher than the bottom end face of the sample outlet tube 2-3, and the spacing between the sample outlet tube 2-3 and the blow tube 2-4 is 1mm, which is convenient for increasing the helium flow rate entering the sample pool 1 and reducing the helium consumption. When the airflow inside the sample pool 1 reaches a steady state, the internal pressure of the sample pool 1 is higher than the pressure of the extraction pool 2. The helium flow introduced into the sample pool 1 will directly carry the eroded sample into the sample outlet tube 2-3, and then be transmitted to the sample outlet tube 4, which is conducive to the rapid washing of the sample; at the same time, when different positions of the sample pool 1 are eroded, the erosion environment and the airflow delivery environment pressure are consistent when the inlet flow rate remains unchanged, avoiding the problem of inconsistent airflow in the sample pool due to the inlet channel 2-1 and the sample outlet 2-2 being far away, thereby greatly reducing the spatial position repeatability of the sample pool and improving the accuracy and precision of the test.

[0029] The sample pool 1 includes a pool body 1-3, an upper cover plate 1-4 installed on the pool body 1-3 and a window fixing plate 1-5 arranged in the middle of the upper cover plate 1-4. A mounting groove is provided in the middle of the window fixing plate 1-5, and the window piece 2-5 is fixed in the mounting groove. The mounting block 1-6 is arranged at the connection between the window piece 2-5 and the window fixing plate 1-5. On the one hand, it is used to fix the window piece 2-5 on the window fixing plate 1-5, and on the other hand, it is used to increase the connection sealing of the window piece 2-5 and the window fixing plate 1-5. At the same time, the sample pool air inlet pipe 3, the sample outlet pipe 4, and the sample outlet air inlet pipe 5 are arranged through the mounting block 1-6, so that the sample pool air inlet pipe 3, the sample outlet pipe 4, and the sample outlet air inlet pipe 5 can be fixed through the mounting block.

[0030] A ball 1 - 2 is provided in the cell body 1 - 3 , and the sample stage 1 - 1 is movably placed in the sample cell 1 through the ball 1 - 2 , so that the sample stage 1 - 1 can be translated in the sample cell 1 .

[0031] The driving platform 7 includes a base 7-2, a driving member and a magnetic member 7-1. The sample pool 1 is also mounted on the base 7-2 through a ball bearing. The driving member adopts a screw slider structure and is mounted on the base 7-2. The magnetic member 7-1 is mounted on the screw slider. The magnetic member 7-1 is driven by the screw slider to translate. Preferably, a magnetic member is also provided in the sample platform 1-1. The driving member drives the magnetic member 7-1 in the driving platform 7 to move. Under the action of magnetic force, the sample platform 1-1 moves in the sample pool 1 as the magnetic member 7-1 moves. By arranging the driving platform 7 outside the sample pool 1, on the one hand, the volume of the sample pool 1 can be reduced, and on the other hand, the driving structure can be prevented from causing contamination to the sample.

[0032] The above description of the disclosed embodiments enables one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be apparent to one skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention; therefore, the present invention will not be limited to the embodiments shown herein, but rather to the widest scope consistent with the principles and novel features disclosed herein.

[0033] Although this article uses more terms corresponding to the figure marks in the figures, it does not exclude the possibility of using other terms; these terms are used only to more conveniently describe and explain the essence of the present invention; interpreting them as any additional limitations is contrary to the spirit of the present invention.

Claims

1. A rapid wash-out denudation pool, characterized in that: include: A sample pool (1) having a sample table (1-1) inside for placing the sample; The erosion cell (2) is mounted on the sample cell (1), and comprises a coaxially arranged sample outlet tube (2-3) and a blow tube (2-4); a sample outlet (2-2) is provided at the bottom of the sample outlet tube (2-3); an air inlet channel (2-1) is formed between the sample outlet tube (2-3) and the blow tube (2-4); a first carrier gas is introduced outside the sample outlet (2-2) through the air inlet channel (2-1), so that the erosion sample in the sample cell (1) is driven by the first carrier gas to be discharged from the sample outlet (2-2); A sample pool air inlet pipe (3) connected to the air blowing cylinder (2-4) and used for introducing the first carrier gas into the sample pool (1); The sample outlet pipe (4) and the sample outlet air inlet pipe (5) are respectively connected to the sample outlet cylinder (2-3), and the second carrier gas is introduced through the sample outlet air inlet pipe (5) to drive the ablation sample to be discharged from the sample outlet pipe (4); The ablation laser component (6) is used to ablate the sample, and the ablation laser component (6) is arranged directly opposite the sample outlet (2-2).

2. A rapid wash-out erosion pool according to claim 1, characterized in that: The bottom end surface of the blowing cylinder (2-4) is arranged higher than the bottom end surface of the sample outlet cylinder (2-3).

3. A rapid wash-out erosion pool according to claim 1, characterized in that: The sample outlet cylinder (2-3) is arranged in a conical shape, and the diameter of the sample outlet cylinder (2-3) decreases from the top of the sample outlet cylinder (2-3) to the sample outlet (2-2).

4. A rapid wash-out erosion pool according to claim 1, characterized in that: The ablation laser assembly (6) comprises a laser generator (6-1) and an objective lens (6-2), wherein the objective lens (6-2) is arranged between the laser generator (6-1) and the sample pool (1), and the relationship between the taper of the sample outlet tube (2-3) and the objective lens (6-2) is as follows: θ=arcsin(NA)*f / d, wherein θ is the taper of the sample outlet tube (2-3), NA is the aperture value of the objective lens, f is the focal length of the objective lens, and d is the distance between the objective lens and the ablation pool (2).

5. A rapid wash-out erosion pool according to claim 1, characterized in that: The denudation pool (2) further comprises a window piece (2-5), and a sample outlet tube (2-3) and an air blowing tube (2-4) are connected to the bottom of the window piece (2-5).

6. A rapid wash-out erosion pool according to claim 1, characterized in that: The sample outlet tube (4) comprises a sample outlet section (4-1) for outputting the denuded sample and a tapered section (4-2) for connecting the sample outlet section (4-1) and the denudation pool (2), wherein the diameter of the tapered section (4-2) decreases from the side of the denudation pool (2) to the side of the sample outlet section (4-1).

7. A rapid wash-out erosion pool according to claim 1, characterized in that: The sample outlet air inlet pipe (5) is provided with a connector (5-1) for increasing the air flow velocity, and the sample outlet air inlet pipe (5) is connected to the denudation pool (2) via the connector (5-1).

8. A rapid wash-out erosion pool according to claim 1, characterized in that: A driving platform (7) is provided at the bottom of the sample pool (1), a magnetic attraction component (7-1) movable relative to the sample pool (1) is provided in the driving platform (7), the magnetic attraction component (7-1) is connected to the sample platform (1-1), and the sample platform (1-1) is driven to move by driving the magnetic attraction component (7-1) to move.

9. A rapid wash-out erosion pool according to claim 1, characterized in that: A ball bearing (1-2) is provided at the bottom of the sample stage (1-1), and the sample stage (1-1) is movably placed in the sample pool (1) via the ball bearing (1-2).

10. A rapid wash-out erosion pool according to claim 1, characterized in that: The sample pool (1) comprises a pool body (1-3), an upper cover plate (1-4) mounted on the pool body (1-3), and a window fixing plate (1-5) arranged in the middle of the upper cover plate (1-4); a mounting block (1-6) is provided at the bottom of the window fixing plate (1-5); and the denudation pool (2) is fixed on the window fixing plate (1-5) via the mounting block (1-6).

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