CN112017942A - Method for improving mass spectrum imaging spatial resolution of secondary ion probe mass spectrometer - Google Patents
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Abstract
The invention relates to the field of mass spectrometry imaging, and discloses a method for improving the mass spectrometry imaging spatial resolution of a secondary ion probe mass spectrometer, which comprises the steps of utilizing the secondary ion mass spectrometer to sequentially scan a sample to form a mass spectrometry image with 2m multiplied by 2n pixel points, and recording a secondary ion spectrum peak sequence of each ion beam scanning area; establishing a secondary ion signal intensity recurrence equation and a secondary ion signal intensity initial condition according to a secondary ion spectrum peak sequence of each ion beam scanning area; and obtaining a secondary ion spectrum peak sequence corresponding to the 1/4 region at the upper left corner of each ion beam scanning region according to a secondary ion signal intensity recurrence equation and a secondary ion signal intensity initial condition. The invention adopts the ion beam interleaving technology and combines with the recurrence calculation of the spectrum peak value in the scanning area, improves the spatial resolution of the existing instrument, further improves the image resolution of the mass spectrum imaging of the instrument, can be used for redesigned new mass spectrum instruments or shaped or installed commercial mass spectrum instruments, and has universality.
Description
Technical Field
The invention relates to the field of secondary ion mass spectrometry imaging, in particular to a method for improving the mass spectrometry imaging spatial resolution of a secondary ion probe mass spectrometer.
Background
The working principle of the Mass Spectrometry Imaging (MSI) technology is as follows: firstly, obtaining and preparing a sample to be detected in a proper mode, scanning and bombarding the sample by a mass spectrometer by utilizing a high-energy ion beam according to a preset acquisition program to enable molecules or ions on the surface of the sample to be desorbed and ionized to generate secondary ions, obtaining the mass-to-charge ratio and the ion intensity of the ions at each position on the surface of the sample by the secondary ions through a mass analyzer, searching the mass spectrum peak of the ions with any specified mass-to-charge ratio in mass spectrum data of each pixel point by means of matched mass spectrum imaging software, and drawing a two-dimensional distribution graph of the corresponding molecules or ions on the surface of the sample by combining the signal intensity of the corresponding ions and the positions of the corresponding ions on the; and then the software is adopted to further process the data of the two-dimensional distribution map of the sample continuous slice to obtain the three-dimensional spatial distribution of the object to be measured in the sample.
Mass spectrometry has two "resolution" concepts when imaging, one being "mass resolution" and the other being "spatial resolution". The mass resolution determines the minimum difference in mass between two ions of similar mass that the mass spectrometer distinguishes. And the latter is the diameter size of the smallest pixel in mass spectrometry imaging. In mass spectrometry imaging, spatial resolution is a critical instrument performance, as is the magnification of a microscope, which determines the minimum space that we can see, and thus breaking through the spatial resolution limit of mass spectrometry imaging is particularly important.
Secondary ion mass spectrometry imaging requires higher spatial resolution for revealing the chemical and structural features of unknown organisms in ancient bodies; the information of elements and isotopes obtained from MSI can help to judge the causes of microsomites and biomarkers; and to clarify the source of poor preservation of organic residuals in the earth's old rocks. The existing method for improving MSI resolution is to improve spatial resolution by changing the design of an ion optical system and compressing the diameter of an ion beam. For example, the Cameca Nano SIMS adopts an ion optical coaxial design, the distance between a focusing lens and a sample is shortened, the diameter of a beam spot of a primary ion beam reaching the surface of the sample is greatly reduced, and the transmission rate of secondary ions is remarkably improved. However, the diameter of the ion beam spot and the sensitivity of the instrument are contradictory parameters, the SIMS spatial resolution can reach 5 μm or even smaller at present, and theoretically, the diameter of a micro beam can be focused to be smaller through an ion optical lens, but when the ion beam spot becomes smaller, the generated secondary ion signal is weak, so that the detector cannot accurately measure, and the spatial distribution of the corresponding molecules or ions on the surface of the sample cannot be accurately obtained, which becomes a technical bottleneck limiting the improvement of the mass spectrum imaging spatial resolution. Meanwhile, according to the traditional scheme for improving the MSI spatial resolution, an SIMS ion optical system needs to be redesigned, the technical difficulty is high, the method is usually only suitable for being adopted in the research and development stage of instruments, and the method has no effect on the SIMS instruments which are delivered from factories or are shaped.
Disclosure of Invention
The invention provides a method for improving the mass spectrum imaging spatial resolution of a secondary ion probe mass spectrometer, thereby solving the problems in the prior art.
A method for improving the mass spectrum imaging spatial resolution of a secondary ion probe mass spectrometer comprises the following steps:
s1) carrying out 2 Xm × 2 Xn times of ion beam staggered scanning on a sample with the size of m × n × d × d area by using a secondary ion mass spectrometer from left to right and from top to bottom, wherein the diameter of an ion beam is d, the scanning step length is d/2, mass spectrum images of 2m × 2n pixel points are obtained, and a secondary ion spectrum peak sequence of each ion beam scanning area is recorded;
s2) establishing a secondary ion signal intensity recurrence equation and a secondary ion signal intensity initial condition according to the secondary ion spectrum peak sequence of each ion beam scanning area;
s3) obtaining a secondary ion spectrum peak sequence corresponding to the 1/4 region at the upper left corner of each ion beam scanning region according to a secondary ion signal intensity recurrence equation and the initial condition of the secondary ion signal intensity.
Further, the secondary ion signal intensity recursion a (i, j) ═ P (i, j) -a (i +1, j) -a (i, j +1) -a (i +1, j +1), where a (i, j) represents the sequence of secondary ion spectrum peaks corresponding to the 1/4 regions at the upper left corner of the ith row and jth column ion beam scanning region; a (i +1, j) represents a secondary ion spectrum peak sequence corresponding to the 1/4 region at the upper left corner of the j column ion beam scanning region of the i +1 th row; a (i, j +1) represents a secondary ion spectrum peak sequence corresponding to 1/4 area at the upper left corner of the j +1 th ion beam scanning area of the ith row; a (i +1, j +1) represents a secondary ion spectrum peak sequence corresponding to the 1/4 region at the upper left corner of the j +1 th column ion beam scanning region of the i +1 th row; p (i, j) represents a secondary ion spectrum peak sequence of an ith row and jth column ion beam scanning area; the initial conditions of the secondary ion signal intensity are that a (2n-1,2m-1) ═ P (2n-1,2m-1), a (2n-1,2m-1) denotes the sequence of secondary ion spectrum peaks corresponding to the region 1/4 at the upper left corner of the ion beam scanning region of column 2m-1 of row 2n-1, and P (2n-1,2m-1) denotes the sequence of secondary ion spectrum peaks of the ion beam scanning region of column 2m-1 of row 2 n-1.
The invention has the beneficial effects that: the invention provides a method for improving the spatial resolution of secondary ion mass spectrometry imaging, which utilizes an ion beam interleaving analysis technology and combines a high-precision three-dimensional sample stage, can break through the original spatial resolution limit of an instrument on the premise of keeping the physical parameters of the instrument unchanged, improves the spatial resolution of mass spectrometry imaging, and avoids the disadvantages brought by improving the spatial resolution of mass spectrometry imaging by relying on a traditional ion optical system. The invention can be used for redesigned new mass spectrometer and also can be used for commercial mass spectrometer which is already shaped or installed, and has universality.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the embodiments are briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
Fig. 1 is a schematic view of an ion scanning process of conventional mass spectrometry imaging.
Fig. 2 is a schematic view of an ion scanning process of mass spectrometry provided in this embodiment.
FIG. 3 is a schematic view of a 2n-1 row and 2m-1 column ion scanning area provided in this embodiment.
Fig. 4 is a schematic view of the 2n-1 row, 2m-2 column ion scanning area provided in the first embodiment.
Fig. 5 is a schematic view of the 2n-1 th row, 2m-3 th column ion scanning area provided in the first embodiment.
Fig. 6 is a schematic view of the 2n-1 th row and 0 th column ion scanning area provided in the first embodiment.
Fig. 7 is a schematic view of a 2n-2 nd row and 2m-1 th column ion scanning area provided in the first embodiment.
Fig. 8 is a schematic view of the 2n-2 nd row and 2m-2 nd column ion scanning area provided in the first embodiment.
Fig. 9 is a schematic view of an ith row and a jth column ion scanning area provided in the first embodiment.
Fig. 10 is a flowchart of a method for improving the mass spectrum imaging spatial resolution of a secondary ion probe mass spectrometer according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to the accompanying drawings. It should be understood that the detailed description and specific examples, while indicating the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
The ion scanning process of the conventional mass spectrometry imaging is shown in fig. 1, the beam spot diameter of an ion beam is d, the conventional mass spectrometry imaging scanning starts with the upper left corner (coordinates are (0, 0)) as an origin, the first line scanning is completed from left to right, then the ion beam or the sample stage is adjusted to make the scanned ion beam return to the leftmost side, the ion beam moves downwards by a step length d, the second line scanning is performed from left to right, and so on, a sample with the scanning area size of mxnxdxdxdxdxdxdxdxdxdxdxd is scanned line by line, the m × n times of scanning is needed, the ion detector records secondary ion signals at the same time of each scanning, the secondary ion spectrum peak sequence of each ion beam scanning area is obtained, and a mass spectrometry image with m × n pixel points.
In a first embodiment, a method for improving the spatial resolution of mass spectrometry imaging of a secondary ion probe mass spectrometer, as shown in fig. 10, includes the following steps:
s1) carrying out 2 Xm × 2 Xn times of ion beam staggered scanning on the sample with the size of m × n × d × d area from left to right and from top to bottom by using a secondary ion mass spectrometer, wherein the diameter of the ion beam is d, the scanning step length is d/2, mass spectrum images of 2m × 2n pixel points are obtained, and a secondary ion spectrum peak sequence of each ion beam scanning area is recorded.
As shown in fig. 2, in this embodiment, the step length of each ion beam horizontal scanning or longitudinal scanning is set to d/2, a sample with the size of m × n × d × d region is scanned, the scanning step length is d/2, 2 × m × 2 × n scans need to be performed, a mass spectrum image with 2 × 2n pixel points is formed, the imaging spatial resolution is d/2, and compared with the spatial resolution of the conventional mass spectrum imaging method, the spatial resolution of the present application is increased by 1 time, and the image resolution is increased by 4 times.
S2), since the true distribution information of the pixel points covered by each 1/4 area may be different due to the non-uniformity of the sample within the beam spot diameter d, 1/4 of the received secondary ion spectrum peak sequence of each ion beam scanning area cannot be directly used as the signal intensity of the ion beam scanning area, which may obscure the true information of the sample surface due to signal aliasing. In the ion beam scanning process, each ion beam scanning area is overlapped with three adjacent ion beam scanning areas, a secondary ion signal intensity recurrence equation and a secondary ion signal intensity initial condition are established according to a secondary ion spectrum peak sequence of each ion beam scanning area, the secondary ion signal intensity recurrence equation A (i, j) ═ P (i, j) -A (i +1, j) -A (i, j +1) -A (i +1, j +1) represents a secondary ion spectrum peak sequence corresponding to the 1/4 area at the upper left corner of the ith row and jth column ion beam scanning areas; a (i +1, j) represents a secondary ion spectrum peak sequence corresponding to the 1/4 region at the upper left corner of the j column ion beam scanning region of the i +1 th row; a (i, j +1) represents a secondary ion spectrum peak sequence corresponding to 1/4 area at the upper left corner of the j +1 th ion beam scanning area of the ith row; a (i +1, j +1) represents a secondary ion spectrum peak sequence corresponding to the 1/4 region at the upper left corner of the j +1 th column ion beam scanning region of the i +1 th row; p (i, j) represents a secondary ion spectrum peak sequence of an ith row and jth column ion beam scanning area; the initial conditions of the secondary ion signal intensity are that a (2n-1,2m-1) ═ P (2n-1,2m-1), a (2n-1,2m-1) denotes the sequence of secondary ion spectrum peaks corresponding to the region 1/4 at the upper left corner of the ion beam scanning region of column 2m-1 of row 2n-1, and P (2n-1,2m-1) denotes the sequence of secondary ion spectrum peaks of the ion beam scanning region of column 2m-1 of row 2 n-1.
S3) obtaining a secondary ion spectrum peak sequence corresponding to the 1/4 region at the upper left corner of each ion beam scanning region according to a secondary ion signal intensity recurrence equation and the initial condition of the secondary ion signal intensity.
The calculation process of the secondary ion signal intensity recurrence equation is opposite to the scanning process of mass spectrum imaging, and the calculation is carried out in a recurrence manner from right to left and from bottom to top in sequence. The initial condition of the secondary ion signal intensity is a (2n-1,2m-1) ═ P (2n-1,2m-1), as shown in fig. 3, only the upper left corner 1/4 area of the last ion scanning pixel point covers the sample surface, and the other 3/4 area of the ion scanning pixel point is outside the sample (i.e. on other substrates, such as resin), so that it does not contribute to the secondary ion signal intensity excited by the ion beam. As shown in fig. 4, a (2n-1,2m-2) ═ P (2n-1,2m-2) -a (2n-1,2m-1) -a (2n,2m-1) ═ P (2n-1,2m-2) -0-a (2n-1,2m-1) -0 ═ P (2n-1,2m-2) -a (2n-1,2 m-1); as shown in fig. 5, a (2n-1,2m-3) ═ P (2n-1,2m-3) -a (2n-1,2 m-2); as shown in fig. 6, a (2n-1,0) ═ P (2n-1,0) -a (2n-1, 1); as shown in fig. 7, a (2n-2,2m-1) ═ P (2n-2,2m-1) -a (2n-1,2 m-1); as shown in fig. 8, a (2n-2,2m-2) ═ P (2n-2,2m-2) -a (2n-2,2m-1) -a (2n-1,2m-2) -a (2n-1,2 m-1); as shown in fig. 9, a secondary ion signal intensity recurrence equation a (i, j) ═ P (i, j) -a (i +1, j) -a (i, j +1) -a (i +1, j +1) is obtained. The invention utilizes the ion beam interleaving analysis technology, calculates the 1/4 spectrum peak intensity at the upper left corner of each ion beam scanning area (namely the secondary ion spectrum peak sequence corresponding to the 1/4 area at the upper left corner of each ion beam scanning area) by recursion, and is equivalent to reduce the diameter of an ion beam to half of the original diameter (namely d/2) under the condition of not changing an ion optical system and hardware, and the ion beam coverage area is 1/4 of the original diameter. Compared with the traditional mass spectrum imaging, the imaging spatial resolution is improved by 1 time, and the imaging pixel value is improved by 4 times. Because the shape of the ion beam is limited by an ion optical system and a limiting micropore, the ion beam is generally elliptical, the recursive calculation of the invention adopts approximate calculation to approximate the ellipse to the circle, and meanwhile, when the recursive formula is calculated, approximate calculation needs to be carried out on 1/4 areas adjacent to the coverage area of two times of scanning.
By adopting the technical scheme disclosed by the invention, the following beneficial effects are obtained:
the invention provides a method for improving the spatial resolution of secondary ion mass spectrometry imaging, which utilizes an ion beam interleaving analysis technology and combines a high-precision three-dimensional sample stage, can break through the original spatial resolution limit of an instrument on the premise of keeping the physical parameters of the instrument unchanged, improves the spatial resolution of mass spectrometry imaging, and avoids the disadvantages brought by improving the spatial resolution of mass spectrometry imaging by relying on a traditional ion optical system. The invention can be used for redesigned new mass spectrometer and also can be used for commercial mass spectrometer which is already shaped or installed, and has universality.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that it will be apparent to those skilled in the art that various modifications and improvements can be made without departing from the principle of the present invention, and such modifications and improvements should also be considered within the scope of the present invention.
Claims (2)
1. A method for improving the mass spectrum imaging spatial resolution of a secondary ion probe mass spectrometer is characterized by comprising the following steps:
s1) carrying out 2 Xm × 2 Xn times of ion beam staggered scanning on a sample with the size of m × n × d × d area by using a secondary ion mass spectrometer from left to right and from top to bottom, wherein the diameter of an ion beam is d, the scanning step length is d/2, mass spectrum images of 2m × 2n pixel points are obtained, and a secondary ion spectrum peak sequence of each ion beam scanning area is recorded;
s2) establishing a secondary ion signal intensity recurrence equation and a secondary ion signal intensity initial condition according to the secondary ion spectrum peak sequence of each ion beam scanning area;
s3), according to the secondary ion signal intensity recurrence equation and the initial condition of the secondary ion signal intensity, obtaining a secondary ion spectrum peak sequence corresponding to the 1/4 region at the upper left corner of each ion beam scanning region.
2. The method of claim 1, wherein the secondary ion signal intensity recursion a (i, j) ═ P (i, j) -a (i +1, j) -a (i, j +1) -a (i +1, j +1), a (i, j) represents the sequence of secondary ion spectrum peaks corresponding to the 1/4 regions at the top left corner of the ith row and jth column ion beam scan region; a (i +1, j) represents a secondary ion spectrum peak sequence corresponding to the 1/4 region at the upper left corner of the j column ion beam scanning region of the i +1 th row; a (i, j +1) represents a secondary ion spectrum peak sequence corresponding to 1/4 area at the upper left corner of the j +1 th ion beam scanning area of the ith row; a (i +1, j +1) represents a secondary ion spectrum peak sequence corresponding to the 1/4 region at the upper left corner of the j +1 th column ion beam scanning region of the i +1 th row; p (i, j) represents a secondary ion spectrum peak sequence of an ith row and jth column ion beam scanning area; the initial conditions of the secondary ion signal intensity are that a (2n-1,2m-1) ═ P (2n-1,2m-1), a (2n-1,2m-1) denotes the sequence of secondary ion spectrum peaks corresponding to the region 1/4 at the upper left corner of the ion beam scanning region of column 2m-1 of row 2n-1, and P (2n-1,2m-1) denotes the sequence of secondary ion spectrum peaks of the ion beam scanning region of column 2m-1 of row 2 n-1.
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