CN218646716U - Laser ablation device - Google Patents

Laser ablation device Download PDF

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Publication number
CN218646716U
CN218646716U CN202222911745.6U CN202222911745U CN218646716U CN 218646716 U CN218646716 U CN 218646716U CN 202222911745 U CN202222911745 U CN 202222911745U CN 218646716 U CN218646716 U CN 218646716U
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sample
axis
laser
galvanometer
laser ablation
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梁燕
蒋建兵
胡勇刚
王辉
王忠强
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Shanghai Kailai Instrument Co ltd
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Shanghai Kailai Instrument Co ltd
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Abstract

The utility model discloses a laser ablation device, laser ablation device includes: the system comprises a femtosecond laser module, a galvanometer system and a field lens, wherein the galvanometer system comprises an X-axis galvanometer and a Y-axis galvanometer; the X-axis galvanometer adjusts the position of laser focusing on the surface of the sample along the X-axis direction, and the Y-axis galvanometer adjusts the position of laser focusing on the surface of the sample along the Y-axis direction; the X-axis direction and the Y-axis direction are perpendicular to each other; the X-axis galvanometer and the Y-axis galvanometer can perform high-frequency reciprocating rotation around the axis at a preset frequency so as to switch the laser focus among a plurality of positions; the field lens is used to focus the laser pulses onto the sample. The utility model discloses a laser ablation device can be in nanosecond time quantum laser ablation different regional samples, and to the homogeneity sample, the particle number that produces is more, and sensitivity during elemental analysis is higher; for different samples, the generated particles are mixed uniformly, and the sample information obtained during element analysis is richer.

Description

Laser ablation device
Technical Field
The utility model belongs to the technical field of laser ablation, especially, relate to a laser ablation device.
Background
With the gradual maturity of the laser ablation system, the application of the laser ablation system is more and more extensive, and the laser ablation system is more and more common as a solid sample feeding mode. The prior art typically uses an objective lens to focus the laser on a specific area of the sample, which is then ablated into particles and then transported into the elemental analysis system by a carrier gas. However, the conventional laser ablation system has no solution to the problem of requiring ultra-rapid ablation of different areas.
At present, for the technology of quantitatively testing the element content of a sample by laser ablation, a standard sample matched with a sample matrix is difficult to find, and the difference between the concentration of a standard sample and the concentration of the sample is large, so the technical progress of quantitatively testing the element content in the sample by laser ablation is slow. The existing method for quantifying sample elements by laser ablation is a sample and standard sample alternative measurement method, namely, after a sample is tested, an ablation signal of a standard sample is tested, and the difficulty is that the standard sample is difficult to match with a sample substrate, and the difference between the sample concentration and the standard sample is large. The accuracy of the element concentration of the sample quantified in this way is low, and the precision is low.
Therefore, how to guarantee high accuracy of analysis and test and simultaneously degrade a sample at an ultra-fast speed is a problem to be solved urgently.
SUMMERY OF THE UTILITY MODEL
In view of this, an object of the present invention is to provide a laser ablation apparatus for ablating a sample by exciting a multi-pulse laser in different regions and in an ultra-fast time period (nanosecond) using a femtosecond laser ablation instrument.
In order to achieve the above object, the present invention provides a laser ablation apparatus, comprising a femtosecond laser module, a galvanometer system and a field lens, wherein the galvanometer system comprises an X-axis galvanometer and a Y-axis galvanometer;
the X-axis galvanometer adjusts the focusing position of the laser on the surface of the sample along the X-axis direction, and the Y-axis galvanometer adjusts the focusing position of the laser on the surface of the sample along the Y-axis direction;
the X-axis direction and the Y-axis direction are mutually vertical;
the X-axis galvanometer and the Y-axis galvanometer can perform high-frequency reciprocating rotation around the axis at a preset frequency so as to switch the laser focus among a plurality of positions;
the field lens is used to focus the laser pulses onto the sample.
The laser ablation device of the utility model can ablate samples in different areas in nanosecond time period, and for homogeneous samples, the number of generated particles is more, and the sensitivity during element analysis is higher; for different samples, the information of the samples obtained by element analysis after the generated particles are uniformly mixed is richer.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
Fig. 1 is a schematic flow diagram of a laser ablation apparatus disclosed in the present invention;
fig. 2 is a schematic diagram of the high-frequency reciprocating rotation of the X-axis galvanometer around the axis in the laser ablation method disclosed by the present invention;
fig. 3 is a schematic diagram of the high-frequency reciprocating rotation of the Y-axis galvanometer of the laser ablation method disclosed by the present invention.
Wherein: 1 femtosecond laser module; 2X-axis galvanometers; 3Y-axis galvanometers; 4 field lens; 5-1 sample; 5-2 high content standard sample; 5-3 low content standard sample; 6 laser pulses.
Detailed Description
One of the cores of the utility model is to provide a laser ablation method, which combines the galvanometer technique and the field lens technique to realize the method of setting different pulse numbers on the sample, the high-content standard sample and the low-content standard sample, and to complete the target of the standard addition method.
Another core of the present invention is to provide a sample detection method for the above laser ablation method, which combines the field lens to focus on different areas of the sample, and then the femtosecond laser multi-pulse ablation sample with ultra-short pulse width generates mixed particles to enter the analysis and test of the elemental analysis system.
The utility model discloses a still another core lies in providing a laser ablation device to utilize femto second laser ablation appearance to set up and arouse many pulse laser mode in different regions and ultrafast time quantum (nanosecond) and erode the sample.
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative efforts all belong to the protection scope of the present invention.
Referring to fig. 1, the laser ablation method disclosed in this embodiment is applied to a laser ablation apparatus, and a person skilled in the art can understand that the laser ablation apparatus includes a femtosecond laser module 1, a galvanometer system and a field lens 4, the galvanometer system includes an X-axis galvanometer 2 and a Y-axis galvanometer 3, the X-axis galvanometer 2 adjusts the position of the laser focused on the surface of a sample 5-1 along the X-axis direction, and the Y-axis galvanometer 3 adjusts the position of the laser focused on the surface of the sample 5-1 along the Y-axis direction; the X-axis direction and the Y-axis direction are mutually vertical; the X-axis galvanometer 2 and the Y-axis galvanometer 3 can perform high-frequency reciprocating rotation around the axis at a preset frequency so as to switch the laser focus among a plurality of positions; the field lens 4 is used to focus the laser pulse 6 onto the sample 5-1.
In the actual use process, a sample 5-1 to be tested is placed on a sample table, then the height is adjusted to enable the upper surface of the sample 5-1 to be located on a focal plane focused by a laser pulse field lens, then the high-frequency vibration frequency of an X-axis vibrating mirror 2 and a Y-axis vibrating mirror 3 and the high-frequency reciprocating rotation amplitude of the X-axis vibrating mirror 2 and the Y-axis vibrating mirror 3 around a shaft are set, finally, a femtosecond laser module 1 is controlled to emit laser pulses 6 to erode the sample, and generated particles enter an analysis test.
The embodiment of the utility model provides an utilize femto second laser to degrade the appearance and set up and arouse many pulse laser mode in different regions and ultrafast time quantum (nanosecond) and degrade sample 5-1, collect the particle that the degradation produced and carry out the analysis and test. The advantages of this are that on one hand, the homogeneous sample can be scanned by multiple pulses, the number of generated particles is more, and the sensitivity of the element analysis is improved after the particles enter the element analysis system; the second aspect can carry out multi-pulse scanning to different samples, and the generated particles enter an element analysis system after being uniformly mixed, so that the obtained sample information is richer.
The embodiment of the utility model provides an in the disclosed laser ablation method include following step:
s1: a femtosecond laser module 1, an X-axis galvanometer 2, a Y-axis galvanometer 3 and a field lens 4 are arranged, the X-axis galvanometer 2 and the Y-axis galvanometer 3 can respectively perform high-frequency reciprocating rotation around an axis, and laser pulses 6 emitted by the femtosecond laser module 1 are focused on a focal plane of an object space after being reflected by the X-axis galvanometer 2 and the Y-axis galvanometer 3 and refracted by the field lens;
s2: arranging at least one sample 5-1 on a sample table, and adjusting the position of a focal plane to coincide with the upper surface of the sample 5-1;
s3: setting the ratio of the period of transmitting laser pulse 6 by the femtosecond laser module 1, the period of high-frequency reciprocating rotation of the X-axis galvanometer 2 around the shaft and the period of high-frequency reciprocating rotation of the Y-axis galvanometer 3 around the shaft as an integer ratio, and setting the amplitude of high-frequency reciprocating rotation of the X-axis galvanometer 2 around the shaft and the amplitude of high-frequency reciprocating rotation of the Y-axis galvanometer 3 around the shaft, so that the focuses of the laser pulse are switched in a reciprocating mode at different positions when the laser pulse is focused on a plane corresponding to the surface of the sample 5-1, and the positions of at least two focuses are on the upper surface of the sample 5-1;
s4: controlling the femtosecond laser module to emit laser pulse 6 to denude the surface of the sample 5-1, and collecting mixed particles generated by denude of the laser pulse 6 for analysis and test.
Wherein, fig. 2 and fig. 3 show the directional diagrams of the laser pulse 6 after the X-axis galvanometer 2 and the Y-axis galvanometer 3 rotate around the axis in a reciprocating way at high frequency, respectively. The embodiment of the utility model provides an utilize femto second laser module 1 to combine the device of galvanometer system and field lens 4 to sample 5-1, high content trade sample 5-2, low content trade sample 5-3 degrade out the particle and mix and reentry elemental analysis system test in the nanosecond time quantum.
In some other preferred embodiments, step S2 specifically includes: arranging at least two samples 5-1 on a sample table, wherein the upper surfaces of the samples are flush, and the position of an adjusting focal plane is coincided with the upper surfaces of the samples; the step S3 of "the positions of at least two of the focal points are on the upper surface of the sample" specifically includes: the positions of at least two of the focal points are on the upper surfaces of different samples, respectively.
The utility model discloses femtosecond laser module 1's pulse width is very narrow (femto second), combines the method that shakes the mirror technique and field lens technique and just can realize setting up different pulse numbers on sample 5-1, high content standard sample 5-2 and the low content standard sample 5-3, and the benefit of doing so is that the base member of sample 5-1, high content standard sample 5-2 and low content standard sample 5-3 matches basic unanimously, and the concentration difference is little, so quantitative sample element concentration degree of accuracy and precision are higher.
In addition, the embodiment of the utility model provides an in still disclose the sample testing method of laser denudation method, include following step:
s1: preparing a high-content standard sample 5-2 containing the element to be detected and having a concentration of C1, and a low-content standard sample 5-3 containing the element to be detected and having a concentration of C2, wherein C1 and C2 are preset known concentrations, and C 1 >C 2 >0;
S2: setting the emission pulse frequency of a femtosecond laser module 1, the reciprocating rotation frequency of an X-axis vibrating mirror 2 and the reciprocating rotation frequency of a Y-axis vibrating mirror 3, periodically switching the laser focus on the upper surfaces of a high-content standard sample 5-2, a low-content standard sample 5-3 and a sample 5-1, wherein the pulse numbers focused on the upper surfaces of the high-content standard sample 5-2, the low-content standard sample 5-3 and the sample 5-1 in one period are respectively X, Y and Z, wherein X, Y and Z are positive integers, collecting mixed particles generated by laser pulse 6 ablation for analysis and test to obtain a total signal value U, and calculating the standard addition concentration according to a formula (1);
C(p)=(C 1 X+C 2 Y)/Z (1);
wherein, C (p) is the standard addition concentration.
S3: and repeating the step S2 for a plurality of times, keeping the Z value unchanged and the (X + Y) value unchanged in each test, and carrying out linear fitting by taking the C (p) of each test as an X coordinate and the total signal value U as a Y coordinate to obtain the absolute value of the X-axis intercept as the content of the element to be detected in the sample, wherein the X values of at least two tests are different.
The embodiment of the utility model provides a through the pulse number that sets up sample 5-1, high content standard sample 5-2 and low content standard sample 5-3 surface denudation, guarantee simultaneously that total pulse number is unanimous, control sample 5-1, high content standard sample 5-2 and low content standard sample 5-3 add the method of different concentration standard sample particle numbers and realize adding concentration gradient. Thus, the element concentration in the unknown sample 5-1 can be calculated by measuring the number of particles after mixing and from the element concentrations and the number of pulses of the known high content standard 5-2 and low content standard 5-3. And (3) calculating according to a formula (1), and performing linear fitting by taking C (p) as an x axis and taking the total signal value U as a y axis to obtain the absolute value of the x-axis intercept, namely the content of the element to be detected in the sample 5-1. The result obtained by the method solves the problem that the result is inaccurate due to different ionization efficiencies of elements in the plasma caused by different matrixes and the problem that the difference between the standard sample concentration and the sample concentration is large by setting the pulse number.
In the present specification, the embodiments are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (1)

1. A laser ablation device is characterized by comprising a femtosecond laser module, a galvanometer system and a field lens, wherein the galvanometer system comprises an X-axis galvanometer and a Y-axis galvanometer;
the X-axis galvanometer adjusts the focusing position of the laser on the surface of the sample along the X-axis direction, and the Y-axis galvanometer adjusts the focusing position of the laser on the surface of the sample along the Y-axis direction;
the X-axis direction and the Y-axis direction are mutually vertical;
the X-axis galvanometer and the Y-axis galvanometer can carry out high-frequency vibration at a preset frequency so as to switch the laser focus among a plurality of positions;
the field lens is used to focus the laser pulses onto the sample.
CN202222911745.6U 2022-11-02 2022-11-02 Laser ablation device Active CN218646716U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116329769A (en) * 2023-05-29 2023-06-27 上海凯来仪器有限公司 Laser ablation laser ionization device, method and mass spectrometer

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116329769A (en) * 2023-05-29 2023-06-27 上海凯来仪器有限公司 Laser ablation laser ionization device, method and mass spectrometer
CN116329769B (en) * 2023-05-29 2023-08-04 上海凯来仪器有限公司 Laser ablation laser ionization device, method and mass spectrometer

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