CN115060755A - Depth analysis method for unknown sample layer structure - Google Patents
Depth analysis method for unknown sample layer structure Download PDFInfo
- Publication number
- CN115060755A CN115060755A CN202210990257.0A CN202210990257A CN115060755A CN 115060755 A CN115060755 A CN 115060755A CN 202210990257 A CN202210990257 A CN 202210990257A CN 115060755 A CN115060755 A CN 115060755A
- Authority
- CN
- China
- Prior art keywords
- layer
- data group
- initial
- unknown sample
- etching
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/227—Measuring photoelectric effect, e.g. photoelectron emission microscopy [PEEM]
- G01N23/2273—Measuring photoelectron spectrum, e.g. electron spectroscopy for chemical analysis [ESCA] or X-ray photoelectron spectroscopy [XPS]
Landscapes
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention belongs to the technical field of detection, and particularly relates to a depth profiling method for a layer structure of an unknown sample. By respectively obtaining the first data group and the second data group, judging whether the data in the second data group is the same as the preset value or not and judging whether the second data group is the same as the preset value or not, the invention can accurately judge the analyzing effect of the unknown sample and solves the defect that the analyzing effect of the unknown sample cannot be accurately judged in the related technology.
Description
Technical Field
The invention belongs to the technical field of detection, and particularly relates to a depth profiling method for an unknown sample layer structure.
Background
The semiconductor integrated circuit is a symbol of manufacturing precision of modern human society industry; following the pace of moore's law, researchers are continually challenging and refreshing device dimensions and performance limits. Since modern devices are typically multi-layered structures on the nanometer scale, materials are gradually transformed from general bulk material properties to quantum properties: quantum size effects and quantum confinement effects have not been ignored. Compared with general bulk materials, the layer structure and the interface structure in the nano system have rapidly increased research proportion compared with the surface, which makes the layer structure and the interface structure characterization in the semiconductor heterostructure more important.
When XPS depth analysis is performed on a semiconductor product, the specificity of corresponding elements and chemical state compositions of the current etching layer self-layer structure, the interface structure and the key attention area is easily ignored, so that the analysis effect on the unknown sample cannot be accurately judged.
Disclosure of Invention
The invention mainly aims to provide a depth analysis method for an unknown sample layer structure, and aims to solve the technical problem that the analysis effect of an unknown sample cannot be accurately judged in the related technology.
In order to achieve the above object, in a first aspect, the present invention provides a method for depth profiling of an unknown sample layer structure, including the following steps:
obtaining a first data set of the unknown sample; the first data set comprises the number of structural layers of the unknown sample, a first thickness corresponding to each structural layer, a first element group corresponding to each structural layer and the content of each element in each first element group;
setting initial preset parameters according to the first data group;
acquiring a second data group of the unknown sample by using the initial preset parameters; the unknown sample comprises a current etching layer, and the current etching layer comprises a current acquisition layer and at least one layer to be acquired, which is adjacent to the current acquisition layer;
judging whether the second data group is the same as a preset value or not;
and if the second data group is different from the preset value, optimizing the initial preset parameter so as to enable the second data group to be the same as the preset value.
The initial preset parameters comprise initial etching parameters;
if the second data group is different from the preset value, the step of optimizing the preset parameter to make the second data group identical to the preset value comprises:
if the second data group is different from the preset value, optimizing the initial etching parameters according to at least one of the layer thickness of the current etching layer or the attention degree of the current etching layer so as to enable the second data group to be the same as the preset value; and the initial etching parameters comprise initial etching speed and initial etching time corresponding to the current acquisition layer.
Optionally, the initial preset parameters further include initial acquisition parameters;
if the second data group is different from the preset value, the step of optimizing the preset parameter to make the second data group identical to the preset value further comprises:
if the second data group is different from the preset value, optimizing the initial preset parameter according to at least one of the content of each element of the current acquisition layer or the strength of a spectral peak signal corresponding to each element, so that the second data group is the same as the preset value; wherein the initial acquisition parameters comprise initial acquisition times.
Optionally, in the step of optimizing the initial preset parameter according to at least one of a content of each element of the current acquisition layer or a strength of a spectral peak signal corresponding to each element if the second data group is different from the preset value, so that the second data group is the same as the preset value;
judging whether the content of each element of the current acquisition layer or the variation value of any one of the intensity of a spectrum peak signal corresponding to each element is less than or equal to 10%;
and if the variation value is less than or equal to 10%, increasing the initial acquisition times by at least 3 times.
Optionally, if the second data group is different from the preset value, the step of optimizing the initial preset parameter so that the second data group is the same as the preset value includes:
if the second data set is different from the preset value, optimizing the initial preset parameter to obtain an optimized parameter;
and taking the optimized parameters as the initial preset parameters, and returning to execute the step of acquiring a second data group of the unknown sample by using the initial preset parameters until the second data group is the same as the preset value.
Optionally, the step of obtaining a first data set of the unknown sample comprises:
etching the unknown sample layer by layer and synchronously acquiring a first full-scanning spectrogram and a first narrow-scanning spectrogram group corresponding to each structural layer; wherein the first narrow-scan spectrum group comprises a C1s spectrum and narrow-scan spectra of each element;
analyzing the first full-scanning spectrum and the first narrow-scanning spectrum group to obtain a first thickness corresponding to each structural layer, a first element group corresponding to each structural layer and the content of each element in each first element group, and forming the first data group.
Optionally, the step of obtaining a first data set of the unknown sample comprises:
etching the current etching layer and synchronously acquiring the first full-scanning spectrogram corresponding to the current etching layer; the first full-scanning spectrogram comprises elements contained in each structural layer and content variation trends corresponding to the elements;
judging whether the current etching layer is etched completely according to the corresponding variation trend of the content of each element;
and if the corresponding variation trend of each content is not changed, the current etching layer is not etched completely.
Optionally, after the step of determining whether the etching of the current etching layer is completed according to the corresponding variation trend of the content of each element, the method further includes:
if the corresponding variation trend of each content is changed, the current etching layer is etched;
taking the next layer to be etched adjacent to the current etching layer as the current etching layer, returning to the step of etching the current etching layer and synchronously acquiring a first full-scanning spectrum corresponding to the current etching layer until all structural layers of the unknown sample are etched;
and taking the thickness corresponding to the difference between the two first full-scan spectrograms adjacent to the current etching layer as the thickness of the current etching layer.
Optionally, the preset value is the first data group;
the step of judging whether the second data group is the same as a preset value comprises the following steps:
judging whether each data in the first data group is the same as each corresponding data in the second data group acquired for the first time or not;
and/or the presence of a gas in the gas,
the preset value is the second data group obtained in any two adjacent times;
the step of judging whether the second data group is the same as a preset value comprises the following steps:
and judging whether the corresponding data in the second data group obtained at any two adjacent times are the same.
Optionally, the step of obtaining a second data set of the unknown sample using the initial preset parameters includes:
etching layer by layer on the unknown sample by utilizing the initial preset parameters and synchronously acquiring a second full-scanning spectrogram and a second narrow-scanning spectrogram group corresponding to each structural layer; wherein the second narrow-scan spectrogram group comprises high-resolution narrow-scan spectrograms corresponding to the elements;
and analyzing the second full-scanning spectrogram and the second narrow-scanning spectrogram group to obtain a second thickness corresponding to each structural layer, a second element composition corresponding to each structural layer and the content of each element in each second element composition, so as to obtain the second data group.
The technical scheme includes that the number of structural layers of an unknown sample, the first thickness of each structural layer, a first element group and the content of each element in the first element group are obtained, the obtained data information is used as a first data group, then a preset initial parameter is set according to the first data group, next the content of a neutralization element in the second thickness, the second element group and the second element group of the unknown sample is obtained according to the preset initial parameter and is used as a second data group, then whether the second data group is the same as a preset value or not is judged, and when the second data group is different from the preset value, the initial preset parameter is optimized, so that the preset value is the same as the second data group. By respectively obtaining the first data group and the second data group, judging whether the data in the second data group is the same as the preset value or not and judging whether the second data group is the same as the preset value or not, the invention can accurately judge the analyzing effect of the unknown sample, and solves the defect that the analyzing effect of the unknown sample cannot be accurately judged due to neglecting the layer structure, the interface structure and the elements corresponding to the key concerned area and the chemical state of the current etching layer of the unknown sample in the related technology.
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 the structures shown in the drawings without creative efforts.
FIG. 1 is a flow chart of an example method of depth profiling of an unknown sample layer structure according to the present invention;
FIG. 2 is a detailed flowchart of step S300 illustrated in FIG. 1;
FIG. 3 is a schematic structural view of the unknown sample illustrated in FIG. 1 in accordance with the present invention;
FIG. 4(a) is a full scan spectrum of an unknown sample exemplified in the present invention, and FIG. 4(b) is a spectrum of C1s of the unknown sample exemplified in FIG. 1 of the present invention;
fig. 5(a) is a Pd3p, O1s high-resolution narrow-scan spectrum of an unknown sample exemplified by the present invention, and fig. 5(b) is an Au4f spectrum of an unknown sample exemplified by the present invention;
FIG. 6(a) is a full scan spectrum corresponding to an unknown sample of the present invention with a total etching time of 10000 s; the full-scan spectrum corresponding to the total etching time 14000s for the unknown sample illustrated in fig. 6 (b); FIG. 6(c) is a full scan corresponding to a total etching time of 25000s for an unknown sample according to an exemplary embodiment of the present invention;
FIG. 7 is a schematic illustration of the elements of an unknown sample of the present invention as a function of etch time;
fig. 8(a) is a full scan spectrum of Al2p for the bottom layer of an unknown sample of an example of the present invention, and fig. 8(b) is a spectrum of O1s for the bottom layer of an unknown sample of an example of the present invention.
Description of reference numerals:
| reference numerals | Name (R) | Reference numerals | Name(s) |
| 100 | |
200 | |
| 300 | Second layer |
The objects, features and advantages of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that all directional indicators (such as upper, lower, left, right, front and rear … …) in the embodiment of the present invention are only used to explain the relative position relationship between the components, the movement situation, etc. in a specific posture (as shown in the drawing), and if the specific posture is changed, the directional indicator is changed accordingly.
In the present invention, unless otherwise expressly stated or limited, the terms "connected," "secured," and the like are to be construed broadly, and for example, "secured" may be a fixed connection, a removable connection, or an integral part; can be mechanically or electrically connected; they may be directly connected or indirectly connected through intervening media, or they may be connected internally or in any other suitable relationship, unless expressly stated otherwise. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In addition, if there is a description of "first", "second", etc. in an embodiment 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 relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In addition, the meaning of "and/or" appearing throughout includes three juxtapositions, exemplified by "A and/or B" including either A or B or both A and B. In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention.
The inventive concept of the present invention will be further elucidated below in connection with some specific embodiments.
The invention provides a depth profiling method for an unknown sample layer structure.
As shown in fig. 1 to fig. 8(b), an embodiment of the depth profiling method for unknown sample layer structure according to the present invention is provided.
The depth analysis method for the unknown sample layer structure comprises the following steps:
s100, acquiring a first data set of an unknown sample; the first data set comprises the number of structural layers of an unknown sample, a first thickness corresponding to each structural layer, a first element group corresponding to each structural layer and the content of each element in each first element group;
in this embodiment, when the first data set is obtained, an etching region with an area of 1m square meter is selected on the surface of an unknown sample, and then a light spot with a size of 200 μm is used to etch in the etching region at an initial etching speed of 0.02nm/s to 0.2nm/s, and meanwhile, the single-layer etching time can be set to 10 to 500 s. That is, when the exemplary light spot is used to etch the current acquisition layer, in order to more accurately acquire the element composition of the current acquisition layer and the corresponding content of each element, the acquisition time for acquiring the current acquisition layer needs to be set longer.
It is specifically and explicitly stated that in this example, the unknown sample of the example consists of at least two current etch layers in a stacked arrangement, which in turn consist of at least two current acquisition layers in a stacked arrangement. That is, the exemplary current etch layer may be the bottom layer 100, the first layer 200, or the second layer 300 illustrated in fig. 3.
By way of example, the method and the device enable a first data set of an unknown sample to be acquired in the implementation process, and the number of layers of the unknown sample, the corresponding approximate thickness of each layer, the elemental composition of each layer and the corresponding approximate content of each element can be acquired.
It should be noted that, in the specific implementation process, the number of layers of the unknown sample may be preliminarily determined according to the variation trend of the element content in the full-scan spectrogram of the unknown sample acquired during the first etching, and the criterion of the determination is that when the element content is changed, the mutation region may be regarded as the layering position of two adjacent structural layers of the unknown sample. That is, there are several change points in the full-scan spectrum corresponding to the whole unknown sample, and there are several layers in the unknown sample. The corresponding approximate thickness of each layer can be obtained by measuring the spacing between two points of variation. The element composition and the approximate content of each element can be obtained by observing a full-sweep spectrogram. The method for obtaining the element composition and the approximate content of each element according to the full-scan spectrogram is the prior art, and the method is not improved, so that the method is not repeated.
In this embodiment, it is specifically and explicitly stated that the exemplary first data set is a data set formed after the material to be tested is completely etched and the test is completed in a top-down order, that is, if the material to be tested has 3 layers in total, the first data set includes data of three layers.
S200, setting initial preset parameters according to the first data group;
in this embodiment, the initial preset parameters are set up by determining, after the first data set is obtained, the etching time and etching rate of the current acquisition layer at the time of obtaining the second data set for the first time, for the number of layers of the unknown sample, the approximate layer thickness of each layer, the elemental composition of each layer, and the approximate content of each element, which are described in the first data set. The initial preset parameters are determined in this way, so that the initial preset parameters required by the second data group can be adjusted and preset in the implementation process of the method, and the acquired second data group is more accurate.
S300, acquiring a second data group of the unknown sample by using the initial preset parameters; the unknown sample comprises a current etching layer, and the current etching layer comprises a current acquisition layer and at least one layer of to-be-acquired layer adjacent to the current acquisition layer;
in this embodiment, a 1mm area may be selected on the surface of the unknown sample when the second data set is acquired 2 And then etching the etched area by adopting a light spot with the light spot set size of 200 mu m at the initial etching speed of 0.02-0.2 nm/s, and simultaneously setting the single-layer etching time to be 10-500 s. The method and the device can determine the initial etching parameters according to the layer thickness of each layer of the unknown sample, the element composition in each layer and the content corresponding to each element in the implementation process, further accurately obtain the second data group, and finally achieve the purpose of accurately obtaining the etching effect of the unknown sample.
It should be clear that the present etch layer and the present acquisition layer of the present embodiment and the following examples are all the cases illustrated and described in step S100.
S400, judging whether the second data group is the same as a preset value or not;
in this embodiment, after the second data group is obtained, it is determined whether the second data group is the same as the preset value. It should be clear that, the preset value exemplified in this embodiment may be the first data set, or may be another second data set adjacent to the second data set in the collection times. It can be understood that, in this embodiment, taking a case that etching is performed on an unknown sample three times in total from the top of the unknown sample to the bottom thereof as an example, data obtained after the first etching is completed is a first data group, data obtained after the second etching is completed is a second data group a, and data obtained after the third etching is completed is a second data group b, and when judging whether the second data group a is the same as a preset value, it is only necessary to judge whether each data in the second data group a is the same as corresponding data in the first data group or the second data group b.
S500, if the second data group is different from the preset value, optimizing the initial preset parameter so that the second data group is the same as the preset value.
In this embodiment, when the second data set is different from the preset value, the initial etching parameters are optimized, and during the optimization, the initial etching parameters are mainly optimized, such as decreasing the etching speed, increasing the etching time or increasing the acquisition time.
When the initial preset parameters are optimized, the initial etching parameters can be optimized according to at least one of the layer thickness of the current etching layer or the attention degree of the current etching layer, so that the collected second data group can be the same as the preset parameters. The initial preset parameters can also be optimized according to at least one of the content of each element of the current acquisition layer or the intensity of the spectral peak signal corresponding to each element, so that the second data group acquired can be the same as the preset parameters.
It can be further explained that, no matter whether the initial etching parameters or the initial acquisition parameters are optimized, attention needs to be paid and whether the parameters corresponding to the optimization can enable the full-scan spectrogram of the current etching layer and the high-resolution narrow-scan spectrogram of each element of the current acquisition layer acquired in the second data set to be clear, and a person skilled in the art can obtain corresponding data information according to the full-scan spectrogram and the narrow-scan spectrogram.
It is to be particularly clear and described that the data information illustrated in the present embodiment is information known by those skilled in the art, and this embodiment only refers to this embodiment to illustrate the present embodiment, and does not relate to improvement, increase, decrease, or design of the example information, so that the example information is not described in detail.
The technical scheme includes that the number of structural layers of an unknown sample, the first thickness of each structural layer, a first element group and the content of each element in the first element group are obtained, the obtained data information is used as a first data group, then a preset initial parameter is set according to the first data group, next the content of a neutralization element in the second thickness, the second element group and the second element group of the unknown sample is obtained according to the preset initial parameter and is used as a second data group, then whether the second data group is the same as a preset value or not is judged, and when the second data group is different from the preset value, the initial preset parameter is optimized, so that the preset value is the same as the second data group. By respectively obtaining the first data group and the second data group, judging whether the data in the second data group is the same as the preset value or not and judging whether the second data group is the same as the preset value or not, the invention can accurately judge the analyzing effect of the unknown sample, and solves the defect that the analyzing effect of the unknown sample cannot be accurately judged due to neglecting the layer structure, the interface structure and the elements corresponding to the key concerned area and the chemical state of the current etching layer of the unknown sample in the related technology.
In some embodiments, referring to fig. 2, the initial predetermined parameters include initial etching parameters;
if the second data set is different from the preset value, optimizing the preset parameter to make the second data set the same as the preset value, comprising the following steps:
a510, if the second data group is different from a preset value, optimizing initial etching parameters according to at least one of the layer thickness of the current etching layer or the attention degree of the current etching layer so as to enable the second data group to be the same as the preset value; the initial etching parameters comprise initial etching speed and initial etching time corresponding to the current acquisition layer.
In this embodiment, when the etching rate, the single-layer etching time, or the total etching time of the current layer cannot meet the etching requirement of the current layer, the etching parameters need to be optimized according to the actual sample data.
In some improved embodiments, the initial preset parameters further include initial acquisition parameters;
if the second data set is different from the preset value, optimizing the preset parameter to make the second data set the same as the preset value, further comprising:
b510, if the second data group is different from the preset value, optimizing initial preset parameters according to at least one of the content of each element of the current acquisition layer or the strength of a spectral peak signal corresponding to each element so as to enable the second data group to be the same as the preset value; wherein the initial acquisition parameters include initial acquisition times.
In this embodiment, in the data acquisition process, when the current acquired element data signal is relatively good or the relative content of the element is less than 10%, the acquisition parameters need to be optimized when the data signal optimization by the acquisition pass can play a large role (the data acquisition pass can be increased according to the actual sample data condition).
In some embodiments, referring to fig. 3, if the second data group is different from the preset value, the step of optimizing the initial preset parameter according to at least one of the content of each element of the current acquisition layer or the intensity of the peak signal corresponding to each element, so that the second data group is the same as the preset value;
b511, judging whether the content of each element of the current acquisition layer or the variation value of any one of the intensity of the spectrum peak signal corresponding to each element is less than or equal to 10%;
in this embodiment, it may be explicitly stated that, in the specific implementation, the determining method is to compare the content of each element in the second data group or the intensity of the peak signal corresponding to each element, which is acquired at any time, with the content of each element in the current acquisition layer corresponding to any one of the two adjacent second data groups of the second data group or the intensity of the peak signal corresponding to each element, or compare the content of each element in the current acquisition layer corresponding to the second data group or the intensity of the peak signal corresponding to each element, which is acquired at any time, so that, in the implementation, the present invention may determine and obtain whether the change value of any one of the content of each element in the current acquisition layer in the second data group or the intensity of the peak signal corresponding to each element is less than or equal to 10%.
And B512, if the change value is less than or equal to 10%, increasing the initial acquisition times by at least 3 times.
In this embodiment, the determination method for the variation value may be: the change value is obtained by observing the wave peaks of the corresponding spectrum peak signals in the two mutually corresponding current acquisition layers and measuring and calculating according to the corresponding numerical values of the two wave peaks.
In some embodiments, referring to fig. 2, if the second data set is different from the predetermined value, the step of optimizing the initial predetermined parameter to make the second data set identical to the predetermined value includes:
s510, if the second data group is different from the preset value, optimizing the initial preset parameter to obtain an optimized parameter;
in this embodiment, when the second data set is different from the preset value, the initial preset parameter can be optimized in the manner as described in the foregoing example. It can be explicitly stated that, during the specific optimization, the initial etching parameters may be optimized, or only the initial acquisition parameters may be optimized, or both may be optimized.
S520, the optimized parameters are used as initial preset parameters, and the step of obtaining a second data group of the unknown sample by using the initial preset parameters is returned to be executed until the second data group is the same as the preset value.
In this embodiment, after the optimized parameter is used as the initial preset parameter, the step of obtaining the second data group by using the initial preset parameter is returned to be executed, in this loop process, as long as the loop needs to be repeated, the last initial preset parameter needs to be optimized, and the optimized parameter after being optimized again is used as the initial preset parameter.
In some embodiments, the step of obtaining a first data set of the unknown sample comprises:
s110, etching layer by layer on an unknown sample and synchronously acquiring a first full-scanning spectrogram and a first narrow-scanning spectrogram group corresponding to each structural layer; wherein the first narrow-scan spectrogram group comprises a C1s spectrogram and narrow-scan spectrograms of each element;
in this embodiment, after the C1s spectrum is acquired, the C1s spectrum needs to be subjected to charge calibration.
And S120, analyzing the first full-scanning spectrogram and the first narrow-scanning spectrogram group to obtain the first thickness corresponding to each structural layer, the first element group corresponding to each structural layer and the content of each element in each first element group, so as to form a first data group.
In some embodiments, the step of obtaining a first data set of the unknown sample includes etching the current etching layer and synchronously acquiring a first full-scan spectrum corresponding to the current etching layer; the first full-scanning spectrogram comprises elements contained in each structural layer and content variation trends corresponding to the elements; judging whether the current etching layer is etched completely according to the corresponding variation trend of the content of each element; if the corresponding variation trend of each content is not changed, the current etching layer is not etched.
In some embodiments, after the step of determining whether the etching of the current etching layer is completed according to the corresponding trend of the content of each element, the method further includes that if the corresponding trend of each content changes, the etching of the current etching layer is completed; taking the next layer to be etched adjacent to the current etching layer as the current etching layer, returning to the step of etching the current etching layer and synchronously acquiring a first full-scanning spectrogram corresponding to the current etching layer until all structural layers of unknown samples are etched; and taking the thickness corresponding to the difference between the two first full-scan spectrograms adjacent to the current etching layer as the thickness of the current etching layer.
In some embodiments, the predetermined value is a first data set;
judging whether the second data group is the same as a preset value or not, wherein the step comprises the following steps of:
judging whether each data in the first data group is the same as each corresponding data in the first acquired second data group; in specific implementation, the preset value can also be a second data group obtained at any two adjacent times;
judging whether the second data group is the same as a preset value or not, wherein the step comprises the following steps of:
and judging whether the corresponding data in the second data group obtained at any two adjacent times are the same.
In some embodiments, the step of obtaining a second data set of the unknown sample using the initial preset parameters comprises:
s310, etching layer by layer on the unknown sample by using initial preset parameters and synchronously acquiring a second full-scanning spectrogram and a second narrow-scanning spectrogram group corresponding to each structural layer; the second narrow-scan spectrogram group comprises high-resolution narrow-scan spectrograms corresponding to all elements;
and S320, analyzing the second full-scanning spectrum and the second narrow-scanning spectrum group to obtain a second thickness corresponding to each structural layer, a second element composition corresponding to each structural layer and the content of each element in each second element composition, so as to obtain a second data group.
In some embodiments, referring to fig. 3 to fig. 8(b), the present embodiment is directed to a nano-scale multi-layer structure device as an example. In the invention, the XPS depth analysis function is utilized to carry out real-time test parameter optimization by a method for carrying out qualitative and quantitative analysis on elements layer by etching layer by layer and combining the actual condition of the sample, the layer structure of the sample is further known, the problem of quickly searching the key attention area of the multilayer sample is effectively solved, and the accurate acquisition of the element composition and the chemical state information of the key attention area is realized.
First, collecting known information about an unknown sample, such as the approximate thickness of interest (e.g., within 50nm, within 100nm, within 200nm, within 500 nm), the number of layers of the sample, the material composition, the thickness of each layer; and if the actual situation allows, collecting important attention information of the unknown sample. It should be noted that the important information in the present embodiment includes, but is not limited to, the layer structure of the unknown sample, the position of the layer to be measured, and the elemental composition and chemical state of the layer to be measured.
According to the known information and the important attention information, in order to reduce the damaged area of the sample, the first etching can be carried out on the corner position of the unknown sample for the first time so as to obtain a first data set.
When etching, the etching area can be selected to be 1mm 2 The size of the light spot is set to be 200 mu m, deep etching parameters such as etching speed and single-layer etching time are set, when the thickness difference of each layer of the sample is large, the setting parameters of the single-layer etching time can be customized, namely, the etching time of each layer can be optimized according to the actual sample to be detected. In this embodiment, the initial etching speed may be set to 0.02nm/s to 0.2nm/s for single layer etchingThe time interval can be set to 10s to 500 s.
And acquiring a full-scanning spectrogram of the surface and each layer and a C1s spectrogram in the etching process, carrying out charge calibration by using the C1s spectrogram, and observing element information contained in each layer and the content change trend information of each element as far as possible in real time. In this example, the peak position of the C1s spectrum in the chemical state corresponding to the contaminated carbon C-C was usually 284.8eV for the charge calibration.
In this embodiment, when the element content of the sample is found to be stable for a long time, which indicates that the thickness of the layer is large, the single-layer etching time and the number of etching layers can be increased, or a larger etching rate is set for continuing etching; when the content change of the sample element is found to be particularly obvious, the sample element is positioned at the interface position or the next layer structure position, so that the single-layer etching time can be reduced, and more fine layer structure information can be obtained; when the initial test program is found to be set to be finished, the test requirement of layer structure observation is not met, which indicates that the total etching time is too short and the etching time needs to be increased or the etching rate needs to be increased; when the etching is found not to be finished but the test requirement is met, the experiment can be finished after the current layer is collected.
Obtaining preliminary sample layer structure information according to element information contained in each layer of the whole material and the content change trend information of each element; and feeds back to a data receiver to further obtain more accurate test requirements (such as layer structure or specific layer element composition and chemical state information);
and optimizing the test parameters, selecting a new position for testing, carrying out etching layer-by-layer data acquisition (the data acquisition comprises a full-scanning spectrogram and a high-resolution narrow-scanning spectrogram of key attention elements) according to the latest test requirement in the process, and observing element information contained in each layer and content change trend information of each element as much as possible in real time.
In this embodiment, when the content of the key attention elements is found to be low, the customization of the single-layer data acquisition pass setting parameters can be performed (that is, each layer of key attention elements can be optimized according to the content of the elements and the intensity of the spectrum peak signal, so as to achieve a better signal-to-noise ratio); optimizing and modifying test parameters (such as acquisition range and acquisition times) at any time according to the test data; and after the requirement of etching test is met, obtaining final sample layer structure information through the element content variation trend of each element high-resolution narrow-scanning spectrogram.
When the requirements for accurate characterization of the element composition and the chemical state of the key concern region exist, the position of the key concern region can be obtained according to the sample layer structure information obtained by testing, the single ion mode in depth profiling is utilized to carry out rapid etching, when the key concern region is reached, the single ion mode or the cluster mode with smaller energy is adopted to carry out etching, and the method of layer-by-layer etching layer-by-layer element qualitative and quantitative analysis is also adopted to carry out accurate characterization of the element composition and the chemical state of the key concern region.
In specific implementation, firstly, the layer structure of an unknown sample is unknown, and a tester needs to know the rough layer structure information of the material through XPS.
Referring to fig. 4(a), fig. 4(b), fig. 5(a), and fig. 5(b), a full-scan spectrum and a C1s high-resolution data spectrum of the current etching layer of the unknown sample are collected, and a charge calibration is performed by using a peak position 284.8eV of a C1s spectrum in a chemical state corresponding to the contaminated carbon C-C; as can be seen from fig. 4(a) and 5(a), the current etching layer of the unknown sample contains elements of O, Pd, and Au in addition to the element C, and high-resolution narrow-scan spectrograms corresponding to the elements of the current etching layer are collected to perform chemical state analysis. After charge calibration according to fig. 4(b), the spectrum of C-C, C-O, C = O after calibration of the layer can be obtained. The elemental content of Au was obtained in step 5 (b).
Because the layer structure is thicker, the depth analysis test is carried out by adopting a single-particle mode (the ion energy is 2000eV, the ion beam current is 1uA, the area of an etching area is 1mm to 1mm, and the etching parameter corresponds to Ta 2 O 5 The etch rate of the reference material is about 0.15 nm/s); and (3) acquiring a full-scanning spectrogram and a C1s high-resolution data spectrogram simultaneously in the depth analysis process according to a layer-by-layer etching layer-by-layer element qualitative and quantitative analysis principle, and performing charge calibration by using 284.8eV of the peak position of the C1s spectrum in the chemical state corresponding to the carbon-carbon contamination.
Referring to fig. 6(a), fig. 6(b) and fig. 6(c), during the acquisition process, the full-scan spectrum is observed to understand the approximate layer structure and the approximate corresponding elements.
Referring to fig. 6(a), 6(b), 6(c) and 7, a new sample position is reselected for depth analysis according to the general layer structure and the corresponding element condition, and a full-scan spectrogram and high-resolution narrow-scan spectrograms of all key elements of the material thereof are collected, so as to further clarify the layer structure and chemical state information of each layer of key elements.
By observing the change of the content of each important element of interest of the sample with the etching time, the layer structure can be further presumed to be approximately as shown in fig. 3:
referring to fig. 8(a) and 8(b), content information of elements and chemical state-corresponding elements contained in the base layer structure sample is obtained: the layer sample can be inferred to be Al through peak position observation 2 O 3 And the atomic percentage of Al and O elements is 41: 59, further proving that the layer material composition infers correct.
It should be specifically and clearly noted that the depth analysis method according to the exemplary embodiment of the present invention may be applied to analysis of an unknown sample in which the number of layers, the thickness of layers, the elemental composition of each layer, and the corresponding content of each element are unknown, or may be applied to analysis of an unknown sample in which the number of layers, the thickness of layers, the elemental composition of each layer, and the corresponding content of each element are partially unknown, or may be applied to analysis of an unknown sample in which the number of layers, the thickness of layers, the elemental composition of each layer, and the corresponding content of each element are preliminarily known. In practice, the method of the present invention may be carried out.
The technical scheme includes that the number of structural layers of an unknown sample, the first thickness of each structural layer, a first element group and the content of each element in the first element group are obtained, the obtained data information is used as a first data group, then a preset initial parameter is set according to the first data group, next the content of a neutralization element in the second thickness, the second element group and the second element group of the unknown sample is obtained according to the preset initial parameter and is used as a second data group, then whether the second data group is the same as a preset value or not is judged, and when the second data group is different from the preset value, the initial preset parameter is optimized, so that the preset value is the same as the second data group. By respectively obtaining the first data group and the second data group, judging whether the data in the second data group is the same as the preset value or not and judging whether the second data group is the same as the preset value or not, the invention can accurately judge the analyzing effect of the unknown sample, and solves the defect that the analyzing effect of the unknown sample cannot be accurately judged due to neglecting the layer structure, the interface structure and the elements corresponding to the key concerned area and the chemical state of the current etching layer of the unknown sample in the related technology.
The above description is only an alternative embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which are made by the contents of the present specification and the accompanying drawings, or directly/indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (10)
1. A depth profiling method for an unknown sample layer structure is characterized by comprising the following steps:
obtaining a first data set of the unknown sample; the first data set comprises the number of structural layers of the unknown sample, a first thickness corresponding to each structural layer, a first element group corresponding to each structural layer and the content of each element in each first element group;
setting initial preset parameters according to the first data group;
acquiring a second data set of the unknown sample by using the initial preset parameters; the unknown sample comprises a current etching layer, and the current etching layer comprises a current acquisition layer and at least one layer to be acquired, which is adjacent to the current acquisition layer;
judging whether the second data set is the same as a preset value or not;
and if the second data group is different from the preset value, optimizing the initial preset parameter so as to enable the second data group to be the same as the preset value.
2. The method of claim 1, wherein the initial predetermined parameters comprise initial etching parameters;
if the second data group is different from the preset value, the step of optimizing the preset parameter to make the second data group identical to the preset value comprises:
if the second data group is different from the preset value, optimizing the initial etching parameters according to at least one of the layer thickness of the current etching layer or the attention degree of the current etching layer so as to enable the second data group to be the same as the preset value; and the initial etching parameters comprise the initial etching speed and the initial etching time corresponding to the current acquisition layer.
3. The method of depth profiling of unknown sample layer structure according to claim 2,
the initial preset parameters also comprise initial acquisition parameters;
if the second data group is different from the preset value, the step of optimizing the preset parameter to make the second data group identical to the preset value further comprises:
if the second data group is different from the preset value, optimizing the initial preset parameter according to at least one of the content of each element of the current acquisition layer or the strength of a spectral peak signal corresponding to each element, so that the second data group is the same as the preset value; wherein the initial acquisition parameters include an initial acquisition number.
4. The method of claim 3, wherein in the step of optimizing the initial predetermined parameter according to at least one of the content of each element of the current acquisition layer or the intensity of the spectral peak signal corresponding to each element if the second data set is different from the predetermined value, so that the second data set is the same as the predetermined value;
judging whether the content of each element of the current acquisition layer or the variation value of any one of the intensity of a spectrum peak signal corresponding to each element is less than or equal to 10%;
and if the variation value is less than or equal to 10%, increasing the initial acquisition times by at least 3 times.
5. The method of depth profiling of unknown sample layer structure according to claim 4,
if the second data group is different from the preset value, the step of optimizing the initial preset parameter to make the second data group identical to the preset value comprises:
if the second data group is different from the preset value, optimizing the initial preset parameter to obtain an optimized parameter;
and taking the optimized parameters as the initial preset parameters, and returning to execute the step of acquiring a second data group of the unknown sample by using the initial preset parameters until the second data group is the same as the preset value.
6. The method of claim 1, wherein the step of obtaining the first data set of the unknown sample comprises:
etching the unknown sample layer by layer and synchronously acquiring a first full-scanning spectrogram and a first narrow-scanning spectrogram group corresponding to each structural layer; wherein the first narrow-scan spectrum group comprises a C1s spectrum and narrow-scan spectra of each element;
analyzing the first full-scanning spectrum and the first narrow-scanning spectrum group to obtain a first thickness corresponding to each structural layer, a first element group corresponding to each structural layer and the content of each element in each first element group, and forming the first data group.
7. The method of depth profiling of unknown sample layer structure according to claim 6,
the step of obtaining a first data set of the unknown sample comprises:
etching the current etching layer and synchronously acquiring the first full-scanning spectrogram corresponding to the current etching layer; the first full-scan spectrogram comprises elements contained in each structural layer and content variation trends corresponding to the elements;
judging whether the current etching layer is etched completely according to the corresponding variation trend of the content of each element;
and if the corresponding variation trend of each content is not changed, the current etching layer is not etched.
8. The method of depth profiling of unknown sample layer structure according to claim 7,
after the step of judging whether the current etching layer is etched according to the corresponding variation trend of the content of each element, the method further comprises the following steps:
if the corresponding variation trend of each content is changed, the current etching layer is etched;
taking the next layer to be etched adjacent to the current etching layer as the current etching layer, returning to the step of etching the current etching layer and synchronously acquiring a first full-scanning spectrum corresponding to the current etching layer until all structural layers of the unknown sample are etched;
and taking the thickness corresponding to the difference between the two first full-scan spectrograms adjacent to the current etching layer as the thickness of the current etching layer.
9. The method of depth profiling of unknown sample layer structure according to any of the claims 1 to 8, characterized in that the preset value is the first data set;
the step of judging whether the second data group is the same as a preset value comprises the following steps:
judging whether each data in the first data group is the same as each corresponding data in the second data group acquired for the first time or not;
and/or the presence of a gas in the gas,
the preset value is the second data group obtained in any two adjacent times;
the step of judging whether the second data group is the same as a preset value comprises the following steps:
and judging whether the corresponding data in the second data group obtained at any two adjacent times are the same.
10. The method of any one of claims 1 to 8, wherein the step of obtaining the second data set of the unknown sample by using the initial preset parameters comprises:
etching layer by layer on the unknown sample by utilizing the initial preset parameters and synchronously acquiring a second full-scanning spectrogram and a second narrow-scanning spectrogram group corresponding to each structural layer; wherein the second narrow-scan spectrogram group comprises high-resolution narrow-scan spectrograms corresponding to the elements;
and analyzing the second full-scanning spectrum and the second narrow-scanning spectrum group to obtain a second thickness corresponding to each structural layer, a second element composition corresponding to each structural layer and the content of each element in each second element composition, so as to obtain the second data group.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210990257.0A CN115060755B (en) | 2022-08-18 | 2022-08-18 | Depth analysis method for unknown sample layer structure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210990257.0A CN115060755B (en) | 2022-08-18 | 2022-08-18 | Depth analysis method for unknown sample layer structure |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115060755A true CN115060755A (en) | 2022-09-16 |
| CN115060755B CN115060755B (en) | 2022-11-01 |
Family
ID=83207318
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210990257.0A Active CN115060755B (en) | 2022-08-18 | 2022-08-18 | Depth analysis method for unknown sample layer structure |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115060755B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116735643A (en) * | 2023-08-14 | 2023-09-12 | 季华实验室 | Method for measuring interface point of sample structure |
| CN116908234A (en) * | 2023-09-13 | 2023-10-20 | 季华实验室 | Data analysis method, system and medium for multilayer sample structure |
Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0849789A2 (en) * | 1996-12-20 | 1998-06-24 | Texas Instruments Incorporated | Method of etching a multilayer IC dielectric structure |
| US20040238735A1 (en) * | 2001-10-26 | 2004-12-02 | Larson Paul E. | System and method for depth profiling and characterization of thin films |
| US20110210246A1 (en) * | 2008-10-22 | 2011-09-01 | Yeda Research And Development Company Ltd. | Method and system for determining depth profiling |
| CN106124549A (en) * | 2016-07-06 | 2016-11-16 | 天津工业大学 | A kind of method characterizing fiber radially different depth chemical constitution |
| CN106645252A (en) * | 2016-12-25 | 2017-05-10 | 首钢总公司 | XPS imaging analysis method for representation of material surface element distribution |
| CN108593695A (en) * | 2018-04-10 | 2018-09-28 | 汕头大学 | The method for directly acquiring film element component distributing from the profile data that fathoms |
| CN110487833A (en) * | 2019-08-28 | 2019-11-22 | 哈尔滨工业大学 | A method of quickly etching analysis of material interface element chemical state using x-ray photoelectron spectroscopy |
| CN110940691A (en) * | 2018-09-21 | 2020-03-31 | 天津大学 | Method for comparing protection effects of different oxide films on metal matrix and application thereof |
| CN112763527A (en) * | 2020-12-11 | 2021-05-07 | 北京科技大学 | Method for directly obtaining material interface oxygen potential and structure |
| CN113218983A (en) * | 2021-04-28 | 2021-08-06 | 大连理工大学 | Method for calibrating XPS depth analysis etching rate of thin film material |
| CN114460114A (en) * | 2022-04-13 | 2022-05-10 | 季华实验室 | Sample analysis method, device, apparatus and storage medium |
| CN114689634A (en) * | 2022-03-05 | 2022-07-01 | 内蒙古科技大学 | Method for measuring polymer sub-layer X photoelectron spectrum by cluster plasma etching |
-
2022
- 2022-08-18 CN CN202210990257.0A patent/CN115060755B/en active Active
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0849789A2 (en) * | 1996-12-20 | 1998-06-24 | Texas Instruments Incorporated | Method of etching a multilayer IC dielectric structure |
| US20040238735A1 (en) * | 2001-10-26 | 2004-12-02 | Larson Paul E. | System and method for depth profiling and characterization of thin films |
| US20110210246A1 (en) * | 2008-10-22 | 2011-09-01 | Yeda Research And Development Company Ltd. | Method and system for determining depth profiling |
| CN106124549A (en) * | 2016-07-06 | 2016-11-16 | 天津工业大学 | A kind of method characterizing fiber radially different depth chemical constitution |
| CN106645252A (en) * | 2016-12-25 | 2017-05-10 | 首钢总公司 | XPS imaging analysis method for representation of material surface element distribution |
| CN108593695A (en) * | 2018-04-10 | 2018-09-28 | 汕头大学 | The method for directly acquiring film element component distributing from the profile data that fathoms |
| CN110940691A (en) * | 2018-09-21 | 2020-03-31 | 天津大学 | Method for comparing protection effects of different oxide films on metal matrix and application thereof |
| CN110487833A (en) * | 2019-08-28 | 2019-11-22 | 哈尔滨工业大学 | A method of quickly etching analysis of material interface element chemical state using x-ray photoelectron spectroscopy |
| CN112763527A (en) * | 2020-12-11 | 2021-05-07 | 北京科技大学 | Method for directly obtaining material interface oxygen potential and structure |
| CN113218983A (en) * | 2021-04-28 | 2021-08-06 | 大连理工大学 | Method for calibrating XPS depth analysis etching rate of thin film material |
| CN114689634A (en) * | 2022-03-05 | 2022-07-01 | 内蒙古科技大学 | Method for measuring polymer sub-layer X photoelectron spectrum by cluster plasma etching |
| CN114460114A (en) * | 2022-04-13 | 2022-05-10 | 季华实验室 | Sample analysis method, device, apparatus and storage medium |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116735643A (en) * | 2023-08-14 | 2023-09-12 | 季华实验室 | Method for measuring interface point of sample structure |
| CN116735643B (en) * | 2023-08-14 | 2023-11-24 | 季华实验室 | Method for measuring interface cut-off point of sample structure |
| CN116908234A (en) * | 2023-09-13 | 2023-10-20 | 季华实验室 | Data analysis method, system and medium for multilayer sample structure |
| CN116908234B (en) * | 2023-09-13 | 2023-11-24 | 季华实验室 | XPS data analysis method, system and medium for multilayer sample structure |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115060755B (en) | 2022-11-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN115060755B (en) | Depth analysis method for unknown sample layer structure | |
| US9335277B2 (en) | Region-of-interest determination apparatus, observation tool or inspection tool, region-of-interest determination method, and observation method or inspection method using region-of-interest determination method | |
| Beretta et al. | Extreme value models for the assessment of steels containing multiple types of inclusion | |
| CN112284999B (en) | Sandstone pore size distribution determination method and application thereof | |
| CN101091101A (en) | Method for measuring nano film thickness through Auger electronic energy spectrum | |
| CN101978241B (en) | Microstructure inspection method, microstructure inspection apparatus | |
| EP1571440A1 (en) | Method and apparatus for void content measurement and method and apparatus for particle content measurement | |
| Farmer et al. | Assessing porosity of proton exchange membrane fuel cell gas diffusion layers by scanning electron microscope image analysis | |
| CN116735643B (en) | Method for measuring interface cut-off point of sample structure | |
| CN101526470B (en) | Method for detecting essence for tobacco | |
| CN111751383A (en) | Defect depth detection method integrating speckle interference and shearing speckle interference | |
| CN115524356A (en) | Method for verifying modification effect of carbon material | |
| US20220244159A1 (en) | Water impurity measurements with dynamic light scattering | |
| CN106442132A (en) | Method for testing mechanical property of thin-wall region of diesel engine block | |
| CN111551579A (en) | Method for determining X-ray background intensity by blank correction | |
| JP6346991B2 (en) | Method for extracting information contained in NMR measurement results as a signal | |
| Bogdanov et al. | A new apparatus for non-destructive evaluation of green-state powder metal compacts using the electrical-resistivity method | |
| CN101526471B (en) | Method for detecting essence for tobacco | |
| US6635869B2 (en) | Step function determination of Auger peak intensity | |
| Sacco et al. | Metrological aspects of tip-enhanced Raman spectroscopy | |
| CN106959313A (en) | A kind of method for quick of objects made from precious metals | |
| CN117392064A (en) | Assessment method for maximum defect of heterogeneous shaft workpiece | |
| JP2012021832A (en) | Image data analysis device | |
| US9052269B1 (en) | Methods for characterizing relative film density using spectroscopic analysis at the device level | |
| Surtchev et al. | Characterization of materials with a combined AFM/Raman microscope |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |