CN116908234B - XPS data analysis method, system and medium for multilayer sample structure - Google Patents
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Abstract
The invention relates to the technical field of material detection and analysis, in particular to an XPS data analysis method, system and medium of a multi-layer sample structure, which are characterized in that spectral peak data of elements corresponding to each layer of material layers to be detected are obtained, then for any layer of material to be detected, according to the variation trend of each element in the spectral peak data, the real-time content of each element at each time point is obtained, then fitting treatment is carried out on all bimodal spectrograms meeting the symmetry requirement to form a spectral peak time variation curve graph, the real-time content of curve sections except for a target curve section in each current fitting spectral peak curve is set to be 0, the corresponding current curve section is obtained, and the obtained spectral peak data is processed in a mode of outputting structural layer information of the multi-layer sample structure according to the current curve section, so that only the corresponding current curve section exists in the spectral peak time variation curve of each layer of the material layers to be detected of the multi-layer sample structure, and the mutual influence among the spectral peak time variation curve graphs of each layer to be detected is avoided.
Description
Technical Field
The invention relates to the technical field of material detection and analysis, in particular to an XPS data analysis method, system and medium of a multilayer sample structure.
Background
XPS, which is known as X-ray Photoelectron Spectroscopy (X-ray photoelectron spectroscopy), and was also known as ESCA (Electron Spectroscopy for Chemical Analysis) in the early days, is a method for measuring the energy distribution of photoelectrons and Auger electrons emitted from the surface of a sample when X-ray photons are irradiated using an electron spectrometer.
In the related art, when multi-layer complex data of a sample containing a metal element, which is unevenly distributed in-plane or depth components, is subjected to peak-splitting fitting processing, the following problems occur:
1) Qualitative confirmation and quantitative treatment of the corresponding spectrum peaks of the appearing or/and disappearing elements;
2) Multiple element spectrum peaks appear in the same area, and the spectrum peaks of the multi-layer data are identified and quantitatively confirmed;
3) Most of metal element spectrum peaks show asymmetric peak shapes and are accompanied by satellite peaks, and a good fitting effect cannot be obtained by adopting a single group of double peaks;
4) The data requires manual layer-by-layer analysis.
The XPS data processing corresponding to the metal element is complex: symmetry spectrum peaks such as Au and the like can be fitted by adopting conventional double peaks; when the sample contains asymmetric spectrum peaks such as Ni, fe, ti, co, ce, the fitting effect obtained by adopting a single group of double peaks is poor, and when the sample has non-uniformity (even appearance or disappearance of elements) in an in-plane or depth range and the element spectrum peaks are overlapped, an analyst is required to perform layer-by-layer peak-by-peak fitting on each data, so that great data processing difficulty and inconvenience are caused, and the reliability of data analysis results is not high.
Disclosure of Invention
The invention aims to provide an XPS data analysis method, system and medium of a multilayer sample structure, and aims to solve the technical problems that when a sample contains asymmetric spectrum peaks such as Ni, fe, ti, co, ce and the like, the fitting effect obtained by adopting a single group of double peaks is poor, when the sample has in-plane or depth range non-uniformity (even appearance or disappearance of elements) and overlapping element spectrum peaks, an analyst is required to perform layer-by-layer peak fitting on each data, so that great data processing difficulty and inconvenience are caused, and the reliability of data analysis results is low.
In order to achieve the above object, in a first aspect, the present invention provides an XPS data analysis method for a multi-layer sample structure, where the multi-layer sample structure includes a plurality of material layers to be tested stacked sequentially from top to bottom, each material layer to be tested includes at least one element;
the XPS data analysis method of the multilayer sample structure comprises the following steps:
acquiring spectral peak data of elements corresponding to each layer of the material to be tested; wherein, the spectrum peak data is recorded with a double-peak spectrogram of the element corresponding to each layer of the material layer to be detected;
Aiming at any material layer to be detected, according to the change trend of each element in the spectrum peak data, obtaining the real-time content corresponding to each element at each time point;
fitting all the bimodal spectrograms meeting the symmetry requirement to form a spectral peak time variation graph; the spectral peak time change curve graph comprises a current fitting spectral peak curve corresponding to each element, each point in the current fitting spectral peak curve is obtained by the real-time content corresponding to each moment of the element, and the current fitting spectral peak curve comprises a target curve segment corresponding to the actual etching time segment of the element;
setting the real-time content of the curve segments except the target curve segment in each current fitting spectrum peak curve to 0, and obtaining a corresponding current curve segment;
and outputting structural layer information of the multi-layer sample structure according to the current curve segment.
Optionally, the step of setting the real-time content of the curve segments except the target curve segment in each of the currently fitted spectral peak curves to 0 to obtain a corresponding current curve segment includes:
screening one layer of the material layer to be tested from the multi-layer sample structure to serve as a designated layer;
Setting the real-time content of the curve sections except the target curve section in the current fitting spectrum peak curve corresponding to the designated layer to be 0, and obtaining a corresponding current curve section;
and sequentially taking the remaining material layers to be tested in the multi-layer sample structure as the appointed layers, and repeatedly executing the step of setting the real-time content of the curve sections except the target curve section in the current fitting spectral peak curve corresponding to the appointed layers to be 0 until all the material layers to be tested are taken as the appointed layers, so as to obtain a plurality of current curve sections.
Optionally, in the step of obtaining the corresponding current curve segment, the real-time content of the curve segments except the target curve segment in the current fitting spectral peak curve corresponding to the specified layer is set to 0,
when the specified layer comprises at least two elements, the real-time content of curve segments except the target curve segment in all the currently-fitted spectral peak curves in the specified layer is set to 0 in sequence to form the current curve segments corresponding to all the currently-fitted spectral peak curves.
Optionally, the steps of sequentially taking the remaining material layers to be measured in the multi-layer sample structure as the designated layers and repeatedly executing the steps of setting the real-time content of the curve segments except the target curve segment in the currently fitted spectral peak curve corresponding to the designated layers to be 0 until all the material layers to be measured are taken as the designated layers, and obtaining a plurality of current curve segments include:
setting the real-time content of the curve sections except the target curve section in the current fitting spectrum peak curve corresponding to the appointed layer to be 0 by taking one layer of the material layer to be measured adjacent to the appointed layer as the appointed layer and repeatedly executing the steps;
and repeating the steps of setting the real-time content of the curve sections except the target curve section in the current fitting spectrum peak curve corresponding to the designated layer to be 0 until all the material layers to be measured are used as the designated layer, and obtaining a plurality of current curve sections.
Optionally, before the step of fitting all the bimodal spectrograms meeting the symmetry requirement to form a spectral peak time variation graph, the method further includes:
Sequentially judging whether all the bimodal spectrograms meet the symmetry requirement;
the step of fitting all the bimodal spectrograms meeting the symmetry requirement to form a spectrogram peak time variation graph comprises the following steps:
and when all the bimodal spectrograms meet the symmetry requirement, executing the fitting processing on all the bimodal spectrograms meeting the symmetry requirement to form a spectrogram peak time variation graph.
Optionally, before the step of performing the fitting processing on all the bimodal spectrograms that meet the symmetry requirement to form a spectral peak time variation graph when all the bimodal spectrograms meet the symmetry requirement, the method further includes:
when at least one of the two-peak spectrograms does not meet the symmetry requirement, sequentially adding a reference spectrum peak into the two-peak spectrograms which do not meet the symmetry requirement, and performing fitting treatment on the two-peak spectrograms which do not meet the symmetry requirement until all the two-peak spectrograms meet the symmetry requirement.
Optionally, after the step of setting the real-time content of the curve segments except the target curve segment in each of the currently fitted spectral peak curves to 0, obtaining a corresponding current curve segment, the method further includes:
Judging whether the real-time content of the curve sections except the target curve section in each current fitting spectral peak curve is set to be 0 or not, and obtaining the corresponding current curve section meets the preset requirement or not;
when at least one of all the target curve segments does not meet the preset requirement, determining all the current curve segments which do not meet the preset requirement, and taking the current curve segments as curve segments to be processed;
outputting all the curve segments to be processed, and enabling service personnel to restore the curve segments to be processed until all the current curve segments meet the preset requirement.
Optionally, the step of outputting all the curve segments to be processed and enabling service personnel to restore the curve segments to be processed until all the current curve segments meet the preset requirement includes:
outputting all the curve segments to be processed;
taking one of the curve segments to be processed as a current curve segment to be restored; the current curve section to be restored comprises the target curve section, two first curve sections to be restored and two second curve sections to be restored, wherein the two first curve sections to be restored are respectively arranged at two ends of the target curve section, and one end, far away from the target curve section, of each first curve section to be restored is connected with one second curve section to be restored;
Reducing the two sections of the first curve section to be reduced by the service personnel to obtain a first curve section to be reduced;
judging whether the first reduction curve segment meets the preset requirement or not;
when the first reduction curve segment does not meet the preset requirement, enabling the service personnel to restore the two second curve segments to be restored in the first reduction curve segment until all the current curve segments meet the preset requirement.
Based on the same technical idea, in a second aspect, the present invention provides a data analysis system of a multi-layer sample structure, including:
etching equipment for etching the multilayer sample structure;
the data acquisition equipment is used for acquiring the spectral peak data of the multilayer sample structure; the method comprises the steps of,
the etching device and the data acquisition device are both in communication connection with the data analysis device, and the data analysis device is used for executing the XPS data analysis method of the multilayer sample structure in the first aspect.
Based on the same technical idea, in a third aspect, the present invention proposes a computer storage medium having stored thereon a data analysis program of a multi-layer sample structure, which when executed by a processor, implements the steps of the XPS data analysis method of the multi-layer sample structure according to the first aspect.
According to the technical scheme, the spectral peak data of the elements corresponding to each layer of material to be tested is obtained, then the real-time content of each element corresponding to each time point is obtained according to the change trend of each element in the spectral peak data for any layer of material to be tested, then fitting processing is carried out on all the bimodal spectrograms meeting the symmetry requirement to form a spectral peak time change graph, the real-time content of curve sections except for a target curve section in each current fitted spectral peak curve is set to be 0, the corresponding current curve section is obtained, finally the obtained spectral peak data is processed in a mode of outputting structural layer information of a multi-layer sample structure according to the current curve section, only the corresponding current curve section exists in the spectral peak time change graph of each layer of the multi-layer sample structure, the mutual influence between the spectral peak time change graphs of each material to be tested is avoided, and further the problem that in the prior art, when a sample contains asymmetric spectral peaks such as Ni, fe, ti, co, ce, the fitting effect obtained by adopting a single group of bimodals is poor, and when the sample has uneven (even element or even peak appears or disappears) in the range, the number of the sample is not uniform, the problem that the data can be analyzed by a person is not analyzing the quality of the data, and the problem of analyzing the data is not being difficult is solved, and the quality of the fitting is not easy is caused by the quality of the data.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to the structures shown in these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flowchart of an XPS data analysis method for a multi-layered sample structure according to one embodiment of the invention;
fig. 2 is a flowchart of step S400 illustrated in fig. 1;
fig. 3 is a flowchart of step S430 illustrated in fig. 2;
fig. 4 is a flowchart of step S300 illustrated in fig. 1;
fig. 5 is a flowchart of step S320 illustrated in fig. 4;
fig. 6 is a flowchart of step S323 illustrated in fig. 5;
FIG. 7 is a flow chart of some embodiments of examples of the invention;
FIG. 8 is a data diagram of elements of the multi-layer sample structure of the present invention at an etching time of 0 s;
FIG. 9 is a data diagram of elements of the multi-layer sample structure of the present invention at an etching time of 310 s;
FIG. 10 is a schematic diagram of data of elements at 970s etching time in the multi-layer sample structure of the present invention;
FIG. 11 is a data diagram of elements of the multi-layer sample structure of the invention at an etching time of 1390 s;
FIG. 12 is a graph showing the relative content of the original state of each element in a multilayer sample structure according to an example of the present invention as a function of etching time;
FIG. 13 is a narrow spectrum of elements at different etch times for an example of the present invention;
fig. 14 (a) is a narrow sweep of Au element at etching time 0s for an example of the present invention; fig. 14 (b) is a narrow sweep of Au element at etching time 1390s, which is an example of the present invention;
fig. 15 is a narrow spectrum of Au element at different etching moments collected in the depth direction according to an example of the present invention;
FIG. 16 is a narrow spectrum of Ni element corresponding to an etching time of 310s according to an example of the present invention;
fig. 17 is a narrow sweep of Au element corresponding to the surface of the multilayer sample structure of the present invention;
fig. 18 is a narrow sweep of Au element at different etching times that does not meet the symmetry requirement for the example of the present invention;
fig. 19 is a graph of the current curve segment of an exemplary multilayer sample structure of the present invention.
The achievement of the objects, functional features and advantages of the present invention will be further described with reference to the accompanying drawings, in conjunction with the embodiments.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be noted that all directional indicators (such as up, down, left, right, front, and rear … …) in the embodiments of the present invention are merely used to explain the relative positional relationship, movement, etc. between the mechanisms in a specific posture (as shown in the drawings), and if the specific posture is changed, the directional indicator is correspondingly changed.
In the present invention, unless specifically stated and limited otherwise, the terms "connected," "affixed," and the like are to be construed broadly, and for example, "affixed" may be a fixed connection, a removable connection, or an integral body; can be mechanically or electrically connected; either directly or indirectly, through intermediaries, or both, may be in communication with each other or in interaction with each other, unless expressly defined otherwise. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
In addition, if there is a description of "first", "second", etc. in the embodiments of the present invention, the description of "first", "second", etc. is for descriptive purposes only and is not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. In addition, the meaning of "and/or" as it appears throughout includes three parallel schemes, for example "A and/or B", including the A scheme, or the B scheme, or the scheme where A and B are satisfied simultaneously. In addition, the technical solutions of the embodiments may be combined with each other, but it is necessary to base that the technical solutions can be realized by those skilled in the art, and when the technical solutions are contradictory or cannot be realized, the combination of the technical solutions should be considered to be absent and not within the scope of protection claimed in the present invention.
The inventive concept of the present invention is further elucidated below in connection with some embodiments.
The invention provides an XPS data analysis method of a multilayer sample structure.
As shown in fig. 1 to 19, an embodiment of an XPS data analysis method of the multi-layer sample structure of the present invention is provided.
In this embodiment, referring to fig. 1 to 19, in the XPS data analysis method of the multi-layer sample structure, the multi-layer sample structure includes a plurality of material layers to be tested stacked sequentially from top to bottom, each material layer to be tested includes at least one element;
the XPS data analysis method of the multilayer sample structure comprises the following steps:
s100, acquiring spectral peak data of elements corresponding to each layer of material to be tested; wherein, the spectral peak data is recorded with a double-peak spectrogram of the element corresponding to each layer of the material to be detected;
in this embodiment, when obtaining the spectral peak data of the element corresponding to the material layer to be tested, the multi-layer sample structure should be etched layer by layer, and in the etching process, the XPS instrument is synchronously used to collect the bimodal spectrograms corresponding to the element of each layer of the multi-layer sample structure layer by layer.
In the acquisition process, when XPS is used for data acquisition, continuous acquisition is also performed when an asymmetric bimodal spectrogram exists in acquired spectrum peak data.
It should be specifically and explicitly stated that, in this embodiment, a curve spectrogram is performed in which a bimodal spectrogram is in a two-dimensional state, and the unit of the abscissa of the bimodal spectrogram is the etching time, that is, the unit of the abscissa is s, and the unit of the ordinate is the real-time content of the corresponding element.
S200, aiming at any material layer to be detected, according to the change trend of each element in the spectral peak data, obtaining the real-time content corresponding to each element at each time point;
in this embodiment, after etching the multi-layer sample structure and acquiring XPS data and obtaining corresponding spectral peak data, the spectral peak data is observed, and then for any material layer to be tested, according to the variation trend of each element in the spectral peak data, the real-time content corresponding to each element at each time point is obtained, and according to the obtained real-time content, the approximate start-stop position of each material layer to be tested can be obtained, so as to facilitate subsequent processing.
It should be further clear that, in the present embodiment, the curve relationship between the etching time and the percentage content of the corresponding element is obtained according to the curve relationship between the bonding energy and the signal intensity, which is not improved or designed, so that the description is not repeated here, but in the present embodiment, it may be stated that the specific process of obtaining the curve relationship between the etching time and the percentage content of the corresponding element according to the curve relationship between the bonding energy and the signal intensity may be implemented in the manner described in "XPS combined fluoride ion analysis chemical state of Si/C multilayer film" of journal of materials science and engineering, volume 40, article No. 1, 1673-2812 (2022) 01-0046-06.
It should be specifically and explicitly stated that, in this embodiment, the purpose of setting the real-time content of the curve sections except the target curve section in each current fitting spectral peak curve to 0 is to avoid the influence of the corresponding current fitting spectral peak curve and other current fitting spectral peak curves of the curve sections except the target curve in each current fitting spectral peak curve by this setting mode, so as to further solve the influence of the real-time content recorded by the curve sections except the target curve section in the prior art on the target curve.
S300, fitting all the bimodal spectrograms meeting the symmetry requirement to form a spectral peak time variation graph; the spectral peak time change curve graph comprises a current fitting spectral peak curve corresponding to each element, each point in the current fitting spectral peak curve is obtained by the real-time content of the element corresponding to each moment, and the current fitting spectral peak curve comprises a target curve segment corresponding to the actual etching time segment of the element;
in this embodiment, when a bimodal spectrogram meeting symmetry requirements is subjected to fitting processing, a gaussian/lorentz ratio is mainly adopted to cancel the limitation to perform free fitting, a corresponding spectral peak time variation graph can be obtained after the free fitting is completed, and then a relationship between signal intensity of each element in a corresponding material layer to be measured and an energy axis of the corresponding element is obtained according to the spectral peak time variation graph.
It should be specifically and explicitly noted that, in this embodiment, when each layer of the material to be tested in the multi-layer sample structure is etched layer by layer, the element corresponding to each layer of the material to be tested will show different real-time contents along with the increase of the etching time, and the element exists in a plurality of real-time contents and shows an increasing change from a specific content value, and after a period of increasing etching time, the content of the element reaches the highest content value and tends to be stable after a period of etching time, the content value of the element starts to decrease from the highest content and reaches the minimum content value after a period of etching time. In the specific implementation, a real-time content curve between the starting etching time when the content of the element in the material layer to be detected starts to decrease from the highest content and the ending etching time when the content reaches the minimum content is taken as the current curve section.
It may be further exemplified that in the present embodiment, taking the structure of the multilayer sample structure as Au, al, ni, ti in the order from top to bottom as an example, it is assumed that the actual etching time period of Au is 0s-110s, then the target curve segment corresponding to Au element is the curve segment of 0s-110s, the appearance position of the erected Al element is from 100s to 250s, then the target curve segment corresponding to Al element is the curve segment of 100s-250s, if the appearance position of Ni element is from 220s to 390s, then the target curve segment corresponding to Ni element is the curve segment of 220s-390s, and assuming that the appearance position of Ti element is from 350s to 800s, then the target curve segment corresponding to Ti element is the curve segment of 350s-800 s.
S400, setting the real-time content of curve segments except for the target curve segment in each current fitting spectrum peak curve to be 0, and obtaining a corresponding current curve segment;
in this embodiment, in implementation, first, according to the process of step S200, the content of the corresponding element in each material layer to be measured is determined, which time period the curve segment of the element is located in is determined, then the curve segment in the time period is taken as the target curve segment, and the curve segment adjacent to the time period is taken as the first curve segment.
It should be specifically and explicitly noted that, in this embodiment, after the process of obtaining the current fitted spectral peak curve is to perform a corresponding operation on the curve relationship between the binding energy of the corresponding element and the signal intensity, a corresponding current fitted spectral peak curve is obtained, which is an example of the current fitted spectral peak curve.
S500, outputting structural layer information of the multi-layer sample structure according to the current curve segment.
In this embodiment, by obtaining the spectral peak data of the elements corresponding to each layer of the material layer to be tested, then obtaining the real-time content corresponding to each element at each time point according to the variation trend of each element in the spectral peak data for any layer of the material layer to be tested, then performing fitting processing on all the bimodal spectrograms meeting the symmetry requirement to form a spectral peak time variation graph, setting the real-time content of the curve sections except for the target curve section in each current fitted spectral peak curve to be 0, obtaining the corresponding current curve section, and finally processing the obtained spectral peak data according to the current curve section in a mode of outputting the structural layer information of the multi-layer sample structure, so that only the corresponding current curve section exists in the spectral peak time variation graph of each layer to be tested of the multi-layer sample structure, and the mutual influence between the spectral peak time variation graphs of each layer to be tested is avoided, thereby the invention can solve the problem that in the prior art that when the sample contains asymmetric spectral peaks such as Ni, fe, ti, co, ce, the fitting effect obtained by adopting a single group of bimodality is poor, and when the sample has the in-plane or depth range (even element or even peak) or the appearance of the element or the peak has the appearance of the peak, the peak and the problem that the analysis of the element or the element is extremely poor in the depth is difficult to analyze the quality, and the analysis of each layer is difficult.
In some specific embodiments, the step of setting the real-time content of the curve segments except the target curve segment in each current fitted spectral peak curve to 0 to obtain the corresponding current curve segment includes:
s410, screening a layer of material to be tested from the multi-layer sample structure to serve as a designated layer;
in this embodiment, when one layer of the material to be tested is selected from the multi-layer sample structure as the specified layer, the first layer of the material to be tested in the multi-layer sample structure may be used as the specified layer, or other layers may be used as the specified layers.
S420, setting the real-time content of curve segments except for a target curve segment in the current fitting spectrum peak curve corresponding to the designated layer to be 0, and obtaining a corresponding current curve segment;
in this embodiment, when the real-time content of the curve sections except the target curve section in the currently fitted spectral peak curve corresponding to the designated layer is set to 0, and the corresponding currently fitted curve section is obtained, the position of the target curve in the currently fitted spectral peak curve corresponding to the designated layer may be determined first, that is, the element composition in the designated layer is determined, and the element composition of the designated layer may be determined by observing the fitted spectral peak curve to obtain the change region of the real-time content in the currently fitted spectral peak curve, which may further be exemplified, where the data information recorded in one currently fitted spectral peak curve corresponds to an Au element, and the Au element is located at the top layer of the multi-layer sample structure, and when the Au element is collected, it should be noted that the Au element is located only at the top layer of the multi-layer sample structure, and if the data information of Au appears in the etching period, it is indicated that the data of the corresponding etching period is not the Au element.
S430, sequentially taking the remaining material layers to be tested in the multi-layer sample structure as designated layers, and repeatedly executing the step of setting the real-time content of the curve sections except the target curve section in the current fitting spectrum peak curve corresponding to the designated layers to be 0 until all the material layers to be tested are taken as designated layers, and obtaining a plurality of current curve sections.
In this embodiment, a layer-by-layer processing manner is adopted, so that each layer of the material to be tested in the multi-layer sample structure can be processed when the method is used.
In some embodiments, in the step of setting the real-time content of the curve segments except the target curve segment in the currently fitted spectral peak curve corresponding to the specified layer to 0, to obtain the corresponding current curve segment,
when the designated layer comprises at least two elements, the real-time content of curve segments except the target curve segment in all the currently-fitted spectral peak curves in the designated layer is set to 0 in sequence to form current curve segments corresponding to all the currently-fitted spectral peak curves.
In some embodiments, the remaining layers of the material to be measured in the multi-layer sample structure are sequentially used as designated layers, and the steps of setting the real-time content of the curve segments except the target curve segment in the currently fitted spectral peak curve corresponding to the designated layers to be 0 are repeatedly executed until all the layers of the material to be measured are used as designated layers, and a plurality of current curve segments are obtained, including:
S431, taking a layer of to-be-measured material adjacent to the designated layer as the designated layer, and repeatedly executing the step of setting the real-time content of the curve sections except the target curve section in the current fitting spectrum peak curve corresponding to the designated layer to be 0;
and S432, continuously and repeatedly executing a layer of material to be measured adjacent to the designated layer to serve as the designated layer, and repeatedly executing the step of setting the real-time content of the curve sections except the target curve section in the current fitting spectral peak curve corresponding to the designated layer to be 0 until all the material layers to be measured serve as the designated layer, and obtaining a plurality of current curve sections.
In some specific embodiments, before the step of fitting all the bimodal spectrograms meeting the symmetry requirement to form the spectral peak time variation graph, the method further comprises:
s600, judging whether all the dual-peak spectrograms meet the symmetry requirement in sequence;
fitting all the bimodal spectrograms meeting the symmetry requirement to form a spectral peak time variation curve chart, wherein the fitting process comprises the following steps:
and S310, when all the dual-peak spectrograms meet the symmetry requirement, executing fitting processing on all the dual-peak spectrograms meeting the symmetry requirement to form a spectrum peak time change curve graph.
In some specific embodiments, when all the bimodal spectrograms meet the symmetry requirement, the step of performing fitting processing on all the bimodal spectrograms meeting the symmetry requirement to form a spectrogram peak time variation graph further comprises:
and S320, when at least one of the two-peak spectrograms in all the two-peak spectrograms does not meet the symmetry requirement, sequentially adding a reference spectrum peak into the two-peak spectrograms which do not meet the symmetry requirement, and performing fitting treatment on the two-peak spectrograms which do not meet the symmetry requirement until all the two-peak spectrograms meet the symmetry requirement.
In some specific embodiments, after the step of setting the real-time content of the curve segments except the target curve segment in each current fitted spectral peak curve to 0, the method further includes:
s321, judging whether the real-time content of the curve sections except the target curve section in each current fitting spectral peak curve is set to be 0, and obtaining the corresponding current curve section meets the preset requirement or not;
s322, when at least one of all target curve segments does not meet the preset requirement, determining all current curve segments which do not meet the preset requirement, and taking the current curve segments as curve segments to be processed;
S323, outputting all curve segments to be processed, and enabling service personnel to restore the curve segments to be processed until all current curve segments meet preset requirements.
In this embodiment, when the service personnel restores the curve segment to be processed, the main operation is to cancel the previously set step of setting the real-time content of the curve segment except the target curve segment in each currently fitted spectral peak curve to 0, that is, the real-time content of the curve segment of the portion where the real-time content is originally set to 0 is no longer set to 0.
In some embodiments, outputting all curve segments to be processed, and enabling the service personnel to restore the curve segments to be processed until all current curve segments meet preset requirements, including:
s323a, outputting all curve segments to be processed;
s323b, taking one of the curve segments to be processed as a current curve segment to be restored; the current curve section to be restored comprises a target curve section, two first curve sections to be restored and two second curve sections to be restored, wherein the two first curve sections to be restored are respectively arranged at two ends of the target curve section, and one end of each first curve section to be restored, which is far away from the target curve section, is connected with one second curve section to be restored;
S323c, enabling service personnel to restore the two first curve segments to be restored to obtain a first restoring curve segment;
s323d, judging whether the first reduction curve segment meets the preset requirement;
s323e, when the first restoring curve segment does not meet the preset requirement, enabling service personnel to restore the two second curve segments to be restored in the first restoring curve segment until all the current curve segments meet the preset requirement.
It should be specifically and explicitly noted that, in the present embodiment, when the first reduction curve meets the preset requirement, step S310 is performed.
Based on the same technical idea, in a second aspect, the present invention provides a data analysis system of a multi-layer sample structure, including:
etching equipment, which is used for etching the multi-layer sample structure;
the data acquisition equipment is used for acquiring spectral peak data of the multilayer sample structure; the method comprises the steps of,
the data analysis device, the etching device and the data acquisition device are all in communication connection with the data analysis device, and the data analysis device is used for executing the XPS data analysis method of the multilayer sample structure of the first aspect.
Based on the same technical idea, in a third aspect, the present invention proposes a computer storage medium, on which a data analysis program of a multi-layer sample structure is stored, which when executed by a processor implements the steps of the XPS data analysis method of the multi-layer sample structure of the first aspect.
Specifically, a computer storage medium refers to a terminal device or a network device capable of realizing network connection, which may be a terminal device such as a mobile phone, a computer, a tablet computer, a portable computer, or a network device such as a server and a cloud platform.
It will be appreciated that a computer storage medium may also include a communication bus, a user interface, and a network interface. Wherein the communication bus is used for realizing connection communication among the components; the user interface is used for connecting the client and communicating data with the client, and can comprise an output unit such as a display screen and an input unit such as a keyboard; the network interface is used to connect to and communicate data with the background server, and may include an input/output interface, such as a standard wired interface, a wireless interface.
The memory is used to store various types of data, which may include, for example, instructions of any application or method in the one computer storage medium, as well as application-related data. The Memory may be implemented by any type of volatile or non-volatile Memory device or combination thereof, such as static random access Memory (Static Random Access Memory, SRAM for short), random access Memory (Random Access Memory, RAM for short), electrically erasable programmable Read-Only Memory (Electrically Erasable Programmable Read-Only Memory, EPROM for short), programmable Read-Only Memory (Programmable Read-Only Memory, PROM for short), read-Only Memory (ROM for short), magnetic Memory, flash Memory, magnetic or optical disk, optionally, the Memory may also be a processor-independent Memory device.
The processor is used to call up the data analysis program of the multi-layer sample structure stored in the memory and execute the XPS data analysis method of the multi-layer sample structure as described above, and the processor may be an application specific integrated circuit (Application Specific Integrated Circuit, abbreviated as ASIC), a digital signal processor (Digital Signal Processor, abbreviated as DSP), a digital signal processing device (Digital Signal Processing Device, abbreviated as DSPD), a programmable logic device (Programmable Logic Device, abbreviated as PLD), a field programmable gate array (Field Programmable Gate Array, abbreviated as FPGA), a controller, a microcontroller, a microprocessor or other electronic components for executing all or part of the steps of the various embodiments of the XPS data analysis method of the multi-layer sample structure as described above.
Based on the same inventive concept, this embodiment provides a computer readable storage medium, such as a flash memory, a hard disk, a multimedia card, a card memory (e.g., SD or DX memory, etc.), a Random Access Memory (RAM), a Static Random Access Memory (SRAM), a read-only memory (ROM), a programmable read-only memory (PROM), an erasable programmable read-only memory (EPROM), an electrically erasable programmable read-only memory (EEPROM), a magnetic memory, a magnetic disk, an optical disk, a server, etc., on which a computer program is stored, which computer program is executable by one or more processors, and which computer program, when executed by the processors, can implement all or part of the steps of the various embodiments of the XPS data analysis method of the multi-layered sample structure of the present invention.
In some exemplary embodiments, the material is predominantly Au, ni, ti, al metal film with a depth profile as shown in the figure, as can be seen:
1) The sample has a relatively obvious 4-layer structure;
2) Apart from the fact that Ti element slightly diffuses between Al layers, the rest layers of the sample basically have no diffusion phenomenon;
3) The data of each layer of sample is complex, the Au element spectrum peak is relatively symmetrical, and the error of the conventional fitting method is small; the asymmetric phenomenon of the spectrum peak is caused by the partial oxidation of Ti and Al elements; the metallic Ni element itself spectrum peak presents an asymmetric peak shape and is accompanied with a satellite peak, so that a good fitting effect cannot be obtained by adopting a single group of double peaks;
4) Multiple layers of data analysts aiming at single complex spectrum peaks need to carry out multiple groups of double-peak fitting processing on single chemical states layer by layer, which greatly increases the complexity and difficulty of data processing.
The variation of each element with etching time (sample thickness) is typically obtained by simple back-off for multi-layer data without elemental spectral peak overlap. The data result of the nano-scale multilayer metal film material plated on the silicon wafer is shown in the following graph, and the data analysis result can not well show the intrinsic condition of the sample (the actual sample Al element is not diffused between the Ni layers), so that the final data analysis result is not credible, and therefore, the data peak-splitting fitting treatment is needed.
Confirming the source of the spectral peak: if the 65-70eV area is an Al element main peak area, but a section of the multilayer data has Ni spectrum peaks, although two elements do not appear at the same time, the interference of Ni signals is eliminated when the content of the Al element spectrum peaks in the multilayer data is processed;
if the Au4f peak-out area in the 80-98eV area has other element interference, the two elements do not appear at the same time, but the signal interference is needed to be eliminated when the spectrum peak content of the Au element is processed;
observing the multi-layer data to determine element change trend (cut-off layer of element appearance or disappearance);
taking an Au element as an example, observing the multi-layer data of the Au element, determining that the peak intensity of the Au element is gradually reduced, and basically eliminating the content of the Au element after 250s, wherein the spectral peak height of the data after 250s is set to be 0 artificially;
data analysis: a. searching a proper reference spectrum peak (generally selecting a layer of data with highest intensity in the data as a reference spectrum) aiming at the spectrum peak corresponding to the asymmetric peak shape; introducing a reference spectrogram into data analysis, and performing multi-layer data fitting;
taking Ni element analysis as an example, observing that only difference of spectral peak intensity exists in the Ni element spectral peaks in the sample, and basically no difference of spectral peak shapes exists, so that the strongest spectral peak of the Ni element in the etching process can be selected as a reference spectral peak for spectral peak fitting;
b. Conventional bimodal fitting is carried out on single chemical state spectrum peaks symmetrical to spectrum peaks (taking Au element as an example, conventional bimodal fitting is carried out on Au, and free fitting is carried out by canceling the Gaussian/Lorentz ratio of peak shape for better fitting effect);
setting the height of the corresponding spectral peak (namely the spectral peak content) of the layer of the element vanishing layer to be 0 according to the vanishing and appearance phenomena of the element content, and copying and pasting a specified layer (or a specified multiple layer) under the limiting condition (taking Au element data as an example);
a. copying and pasting the limiting condition of 'free fitting is carried out on the Gaussian/Lorentz ratio cancellation limitation of peak shape' into all layer data;
b. setting the spectral peak height of all etching layers after 250s to 0, copying and pasting the limiting condition that the height is set to 0 into all data after 250s, and manually confirming the disappearance of the Au element);
c. and selecting all layers to fit.
Confirming the data processing results of each layer one by one, and carrying out proper modification aiming at unsuitable data processing;
obtaining the variation trend of the sample content along with the in-plane/depth, and obtaining the real sample information;
for a series of multiple sets of data, the overall processing constraints of a particular set of data are directly copied and pasted to the other sets of data for fitting.
Aiming at the asymmetric peak shape fitting, the invention adopts a certain layer of data in the data as a reference spectrogram, has the advantages of simple operation and high matching degree, and simultaneously avoids the defects of difficult acquisition of the reference spectrogram, poor reliability of data analysis results and the like; meanwhile, aiming at the phenomenon that the element content is uneven (the disappearance and appearance of the element content), the height of the corresponding spectral peak (namely the spectral peak content) can be set to 0, and the phenomenon that no spectral peak has content is effectively avoided by limiting the data analysis conditions through human interference, so that the data is ensured to be reliable; in addition, various different data analysis limiting conditions can be carried out on the data, and the specified multi-layer data is copied and pasted by the data analysis limiting conditions of the specific layer, so that the intensity and difficulty of data analysis are greatly reduced; finally, when a series of multi-group data exists, the special group data processing limiting conditions can be directly copied and pasted into other groups of data, and the accurate result of the series of multi-group data can be directly and efficiently obtained through simple and proper modification.
According to the method, the system and the device, the spectral peak data of the elements corresponding to each layer of the material to be tested are obtained, the real-time content of each element corresponding to each time point is obtained according to the change trend of each element in the spectral peak data for any layer of the material to be tested, then fitting processing is carried out on all the bimodal spectrograms meeting the symmetry requirement to form a spectral peak time change graph, the real-time content of curve sections except for a target curve section in each current fitting spectral peak curve is set to be 0, the corresponding current curve section is obtained, finally, the obtained spectral peak data is processed in a mode of outputting structural layer information of a multi-layer sample structure according to the current curve section, only the corresponding current curve section exists in the spectral peak time change graph of each material to be tested of the multi-layer sample structure, the mutual influence between the spectral peak time change graphs of each material to be tested is avoided, and further, the problem that in the prior art, when the sample contains asymmetric spectral peaks such as Ni, fe, ti, co, ce, the effect obtained by adopting a single group of bimodals is poor, when the sample has uneven (even appearance or even overlapping of the elements) in the range of the surface or depth of the sample, the fitting data is required to be analyzed, and the data is difficult to analyze each layer by layer, and the analysis is difficult.
The foregoing description is only of the optional embodiments of the present invention, and is not intended to limit the scope of the invention, and all the equivalent structural changes made by the description of the present invention and the accompanying drawings or the direct/indirect application in other related technical fields are included in the scope of the invention.
Claims (7)
1. The XPS data analysis method of the multilayer sample structure is characterized in that the multilayer sample structure comprises a plurality of layers of material to be tested, which are sequentially stacked from top to bottom, and each layer of material to be tested comprises at least one element;
the XPS data analysis method of the multilayer sample structure comprises the following steps:
acquiring spectral peak data of elements corresponding to each layer of the material to be tested; wherein, the spectrum peak data is recorded with a double-peak spectrogram of the element corresponding to each layer of the material layer to be detected;
aiming at any material layer to be detected, according to the change trend of each element in the spectrum peak data, obtaining the real-time content corresponding to each element at each time point;
fitting all the bimodal spectrograms meeting the symmetry requirement to form a spectral peak time variation graph; the spectral peak time change curve graph comprises a current fitting spectral peak curve corresponding to each element, each point in the current fitting spectral peak curve is obtained by the real-time content corresponding to each moment of the element, and the current fitting spectral peak curve comprises a target curve segment corresponding to the actual etching time segment of the element;
Setting the real-time content of the curve segments except the target curve segment in each current fitting spectrum peak curve to 0, and obtaining a corresponding current curve segment;
outputting structural layer information of the multi-layer sample structure according to the current curve segment;
the step of setting the real-time content of the curve segments except the target curve segment in each current fitting spectral peak curve to 0 to obtain a corresponding current curve segment includes:
screening one layer of the material layer to be tested from the multi-layer sample structure to serve as a designated layer;
setting the real-time content of the curve sections except the target curve section in the current fitting spectrum peak curve corresponding to the designated layer to be 0, and obtaining a corresponding current curve section;
sequentially taking the remaining material layers to be tested in the multi-layer sample structure as the appointed layers, and repeatedly executing the step of setting the real-time content of the curve sections except the target curve section in the current fitting spectrum peak curve corresponding to the appointed layers to be 0 until all the material layers to be tested are taken as the appointed layers, so as to obtain a plurality of current curve sections;
Before the step of fitting all the bimodal spectrograms meeting the symmetry requirement to form a spectral peak time variation curve graph, the method further comprises the following steps:
sequentially judging whether all the bimodal spectrograms meet the symmetry requirement;
the step of fitting all the bimodal spectrograms meeting the symmetry requirement to form a spectrogram peak time variation graph comprises the following steps:
when all the bimodal spectrograms meet the symmetry requirement, executing the step of fitting all the bimodal spectrograms meeting the symmetry requirement to form a spectral peak time variation curve graph;
and before the step of performing the fitting processing on all the bimodal spectrograms meeting the symmetry requirement to form a spectral peak time variation graph when all the bimodal spectrograms meet the symmetry requirement, the method further comprises:
when at least one of the two-peak spectrograms does not meet the symmetry requirement, sequentially adding a reference spectrum peak into the two-peak spectrograms which do not meet the symmetry requirement, and performing fitting treatment on the two-peak spectrograms which do not meet the symmetry requirement until all the two-peak spectrograms meet the symmetry requirement.
2. The method for analyzing XPS data of a multi-layered sample structure of claim 1, wherein in said step of obtaining a corresponding current curve segment, said real-time content of curve segments other than said target curve segment in said current fit spectral peak curve corresponding to said specified layer is set to 0,
when the specified layer comprises at least two elements, the real-time content of curve segments except the target curve segment in all the currently-fitted spectral peak curves in the specified layer is set to 0 in sequence to form the current curve segments corresponding to all the currently-fitted spectral peak curves.
3. The XPS data analysis method of the multilayer sample structure according to claim 1, wherein the steps of sequentially taking the remaining material layers to be measured in the multilayer sample structure as the specified layers and repeatedly executing the steps of setting the real-time content of the curve segments except the target curve segment in the currently fitted spectral peak curve corresponding to the specified layers to 0 until all the material layers to be measured are taken as the specified layers, and obtaining a plurality of the current curve segments include:
Setting the real-time content of the curve sections except the target curve section in the current fitting spectrum peak curve corresponding to the appointed layer to be 0 by taking one layer of the material layer to be measured adjacent to the appointed layer as the appointed layer and repeatedly executing the steps;
and repeating the step of setting the real-time content of the curve sections except the target curve section in the current fitting spectral peak curve corresponding to the designated layer to be 0 until all the material layers to be measured are used as the designated layer, and obtaining a plurality of current curve sections.
4. A method of XPS data analysis of a multilayer sample structure as claimed in any one of claims 1 to 3, characterized in that after the step of setting the real-time content of the curve segments of each of the presently fitted spectral peak curves other than the target curve segment to 0, it further comprises:
judging whether the real-time content of the curve sections except the target curve section in each current fitting spectral peak curve is set to be 0 or not, and obtaining the corresponding current curve section meets the preset requirement or not;
When at least one of all the target curve segments does not meet the preset requirement, determining all the current curve segments which do not meet the preset requirement, and taking the current curve segments as curve segments to be processed;
outputting all the curve segments to be processed, and enabling service personnel to restore the curve segments to be processed until all the current curve segments meet the preset requirement.
5. The XPS data analysis method of the multi-layer sample structure of claim 4, wherein the outputting all the curve segments to be processed and the enabling the service personnel to restore the curve segments to be processed until all the current curve segments meet the preset requirement includes:
outputting all the curve segments to be processed;
taking one of the curve segments to be processed as a current curve segment to be restored; the current curve section to be restored comprises the target curve section, two first curve sections to be restored and two second curve sections to be restored, wherein the two first curve sections to be restored are respectively arranged at two ends of the target curve section, and one end, far away from the target curve section, of each first curve section to be restored is connected with one second curve section to be restored;
Reducing the two sections of the first curve section to be reduced by the service personnel to obtain a first curve section to be reduced;
judging whether the first reduction curve segment meets the preset requirement or not;
when the first reduction curve segment does not meet the preset requirement, enabling the service personnel to restore the two second curve segments to be restored in the first reduction curve segment until all the current curve segments meet the preset requirement.
6. A data analysis system for a multi-layered sample structure, comprising:
etching equipment for etching the multilayer sample structure;
the data acquisition equipment is used for acquiring the spectral peak data of the multilayer sample structure; the method comprises the steps of,
a data analysis device, the etching device and the data acquisition device being communicatively connected to the data analysis device, the data analysis device being configured to perform the XPS data analysis method of the multilayer sample structure of any one of claims 1 to 5.
7. A computer storage medium, characterized in that the storage medium has stored thereon a data analysis program of a multi-layered sample structure, which when executed by a processor, implements the steps of the XPS data analysis method of a multi-layered sample structure according to any one of claims 1 to 5.
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