CN106645252A - XPS imaging analysis method for representation of material surface element distribution - Google Patents
XPS imaging analysis method for representation of material surface element distribution Download PDFInfo
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- CN106645252A CN106645252A CN201611212864.5A CN201611212864A CN106645252A CN 106645252 A CN106645252 A CN 106645252A CN 201611212864 A CN201611212864 A CN 201611212864A CN 106645252 A CN106645252 A CN 106645252A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- 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]
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Abstract
The invention discloses an XPS imaging analysis method for representation of material surface element distribution and belongs to the technical field of material surface analysis. The method comprises steps as follows: a to-be-detected sample requiring XPS imaging is prepared as needed, and then loaded; a monochromic X ray gun is triggered, and the spot diameter ranges from 200 mu m to 500 mu m; the imaging area ranges from 200 mu m *200 mu m to 2,000 mu m*2,000 mu m; XPS narrow spectra of elements are collected, and pass energy is required to be identical when X ray photoelectron energy spectra of each element are collected; a data processing and imaging conversion process is implemented and comprises background removal, atlas fitting, calculation of relative content of elements and imaging conversion. The method has the advantages that data analysis is direct and accurate.
Description
Technical field
The invention belongs to material surface analysis technical field, more particularly to a kind of sign material surface Elemental redistribution
XPS i mage analysis methods.More particularly to a kind of XPS imaging analysis sides for characterizing material surface element and different valence state Elemental redistribution
Method.Suitable for domain analysis such as System of Detecting Surface Defects For Material, corrosion, oxidation, colour fadings.
Technical background
X-ray photoelectron spectroscopy (X-ray Photoelectron Spectroscopy, abridge XPS), is mainly used in
The information such as the element on research material pole surface and element different valence state composition.It is using excitation of X-rays sample surfaces element
Internal layer energy level electronic signal, then photoelectronic kinetic energy and intensity are detected with electron spectrometer, and then determine the species and valency of element
The information such as state.And background, collection of illustrative plates fitting are further removed to photoelectron spectroscopy, sensitivity factor method is carried out to peak area are repaiied
Just waiting data processing then can calculate the relative amount of element.
In the conventional technology, XPS is mainly used to carry out point analysis sign to material surface, this is because the hot spot of X-ray
Diameter generally larger (more than tens μm), therefore the application for carrying out surface-element imaging by XPS is considerably less, parallel imaging method is
One of method of XPS imaging applications.1) as document [Liu Fen, Qiu Limei, Zhao Liangzhong. analytical chemistry research notes .vol.31
(2003), No.9, pp.1082-1084.] it is described, by parallel imaging technology to AgCl and Na2S2O3XPS imagings are carried out, its use
Can locate spectral peak area with being combined less than 7～8eV of spectral peak for photoelectron spectrum peak area in the peak area of calculating elements relative amount
Difference.2) as document [Martin F, Lopez MC, Carrera, et al.Surface and interface analysis,
Vol.36 (2004), pp.8-16.] described, the ZrO by XPS parallel imaging technical research2/ 304SS (873K) material is in Jing
The EDS maps situation of Zn after Ar ion etchings, O, Fe, Cr spectral strength.
As described above, method 1,2 is similar, distribution situation of the element in material surface is characterized by parallel imaging method,
The advantage of parallel imaging is that acquisition time is short, have the disadvantage cannot accurate definition background position, as described in method 1, its will be less than spectrum
7～8eV of peak to be combined and be defined as background position at energy, it is impossible to avoid other x-ray photoelectron peaks, electron scattering spectral peak, auger spectrum
The impact to background such as peak, as described in method 2, the distribution situation of element is characterized by XPS spectrum peak intensity, not to spectral peak
Carry out eliminating background process, inevitably error is brought due to the presence of inelastic scattering background.This patent provides one
The XPS i mage analysis methods for characterizing material surface element and different valence state Elemental redistribution are planted, by pointwise to material surface element
Collection photoelectron spectroscopy is obtained, and by the narrow spectrum of element collected to each point careful data processing is carried out, and can be obtained
The different valence state distribution situation of material surface element and element.
The content of the invention
Present invention aim at there is provided a kind of XPS i mage analysis methods of sign material surface Elemental redistribution, solving
The problem of background position can not be defined using technology at present.Realize and intended by careful collection of illustrative plates while background position is defined
Close, obtain the surface information of material, there is provided accurately reference data directly perceived.
It is a kind of characterize material surface Elemental redistribution XPS i mage analysis methods, concrete steps and parameter it is as follows：
1st, the requirement according to photoelectron spectrograph to sample, preparation needs to carry out the testing sample of XPS imagings, according to photoelectricity
The dress sample of sub- energy disperse spectroscopy is required into luggage sample.
2nd, the monochromatic X ray rifle is opened, the region to needing imaging carries out XPS point analysis, it is determined that needing what is be imaged
Element；Imaging region and scan node are set；Pointwise is to each narrow spectrum of element XPS needed for node collection；Finally, with XPS point
Analysis software (commercially available) carries out data processing and imaging conversion to the narrow spectrum of photoelectron spectroscopy of each element.
The monochromatic X ray rifle spot diameter arranges scope：200 μm～500 μm.
Imaging region arranges scope：2000 μm of 200 μ m, 200 μm～2000 μ m, imaging region is preferably set to 1000 μ
m×1000μm。
It is 3 × 3～64 × 64 that the quantity of scan node arranges scope, preferred scope value：10 × 10～32 × 32.
3rd, the narrow spectrums of element XPS are gathered, the x-ray photoelectron power spectrum highest peak of element is chosen, when the x-ray photoelectron of element
Power spectrum highest peak overlaps with other elements spectral peak, then choose time strong peak or the highest peak misaligned with other elements spectral peak.Collection
Each element x-ray photoelectron energy time spectrum, it is desirable to which logical energy is identical.
It is logical that scope can be set for 10～50eV.
4th, data processing and imaging conversion process：
(1) background is removed：XPS analysis software has three kinds of background types (name) to select：Linear、
Shirley, Tougaard, preferably select Shirley type backgrounds, and background range of choice is can determine photoelectron spectroscopy peak area
Justice is out defined.
The purpose for removing background is the inelastic scattering background for removing photoelectron spectroscopy, by the photoelectron spectroscopy spectral peak of element
Area is defined and, and then peak area is modified with sensitivity factor method, and the relative amount of each element is calculated.
(2) collection of illustrative plates fitting：It is fitted using collection of illustrative plates when there is photoelectron spectrum overlap of peaks situation, selects the presence of the photoelectricity for overlapping
Sub- spectral peak, clicks on collection of illustrative plates fitting function Peak fit (English button on screen), adds the corresponding spectral peak of each peak position and is fitted,
The corresponding spectral peak of each peak position is named respectively simultaneously, is determined the ownership of the photoelectron spectral peak.
(3) calculating of element relative amount：XPS analysis software be furnished with Scofield (name) sensitivity factor databases or
Wagner (name) sensitivity factor database.It is preferred that Scofield sensitivity factor databases are selected, in sensitivity factor one
Hurdle is input into the sensitivity factor of each element, that is, obtain the revised peak area of each element spectral peak；By the revised peak of all elements
Area sum normalizing is 100%, and the relative amount of each element is the revised peak area of each element after all elements amendment
Peak area sum in shared ratio.
When removing background, collection of illustrative plates fit procedure by photoelectron spectroscopy, element spectral peak-to-peak area has been defined and, but by
The parameters such as section, inelastic scattering mean free path are produced in the photoelectron of each element to differ, to each element relative amount meter
Need to carry out sensitivity factor method correcting process to peak area during calculation.
(4) imaging conversion：The height of all node each element relative amounts is presented in the form of pseudo- color image,
To show the distribution situation of each element.Imaging conversion Creat Profile (English button on screen) are clicked on, that is, presents each list
The relative amount distribution map of individual element, adjusting image interpolation Grade I nterpolationlevel can change over the resolution of picture
Rate, it is 256～512 that interpolation level arranges scope.Click on and overlap button Overlay Map (on screen English button), can be by
Being imaged on an image for all elements is presented, and each element is represented with a kind of color, can more intuitively be found out
The distribution situation of each element, adjusting color rank Colour Level can change over the resolution ratio of picture, and color rank arranges model
Enclose for 4～32.
It is an advantage of the current invention that：Pointwise gathers photoelectron spectroscopy, then the number that Jing is careful to imaging region inner surface element
After according to process, the distribution map of each element relative amount is accurately obtained.Having abandoned existing parallel imaging method can not define background position
The shortcoming put, while being fitted by careful collection of illustrative plates, can obtain more valuable material surface information, such as different valence state unit
Distribution of element etc., so as to provide accurately reference data more directly perceived for research work.
Description of the drawings
Fig. 1 is the full spectrograms of XPS of T-5CA tin plate sample spot corrosion areas.
Fig. 2 is the setting schematic diagram of imaging region and scan node.
Fig. 3 is X=0 μm, the narrow spectrograms of Sn3d that Y=0 μm of node is collected.
Fig. 4 is X=0 μm, and the narrow spectrograms of Sn3d remove the spectral peak area obtained after Shirley backgrounds and illustrate at Y=0 μm of node
Figure.
Fig. 5 is X=0 μm, the swarming fitted figure of the narrow spectrograms of Sn3d at Y=0 μm of node.
Fig. 6 is imaged picture for the Sn elements XPS of T-5CA tin plate sample spot corrosion areas.
Fig. 7 is imaged picture for the Cr elements XPS of T-5CA tin plate sample spot corrosion areas.
Fig. 8 is imaged picture for the Fe elements XPS of T-5CA tin plate sample spot corrosion areas.
Fig. 9 is imaged picture for the O elements XPS of T-5CA tin plate sample spot corrosion areas.
Figure 10 is the Sn of T-5CA tin plate sample spot corrosion areas4+Element XPS is imaged picture.
Figure 11 is imaged picture for the simple substance Sn elements XPS of T-5CA tin plate sample spot corrosion areas.
Figure 12 is imaged picture for the XPS of T-5CA tin plate sample spot corrosion area tetra- kinds of Elemental redistributions of Sn, Cr, Fe, O.
Specific embodiment
Embodiment 1
The specific embodiment of the present invention is illustrated below in conjunction with the accompanying drawings：
In order to characterize the distribution situation of T-5CA spot corrosion tin plate sheet surface elements, to determine region and the corrosion of spot corrosion
Degree, to T-5CA spot corrosion tin plate XPS imaging analysis are carried out, and concrete steps and parameter are as follows：
1st, the requirement according to photoelectron spectrograph to sample, prepares spot corrosion T-5CA tin plate samples, according to photoelectron energy
The dress sample of spectrometer is required into luggage sample；
2nd, the monochromatic X ray rifle is opened, XPS point analysis is carried out to tin plate spot corrosion region, Fig. 1 is to collect X to penetrate
The full spectrogram of photoelectron spectra, it can be seen that tin plate spot corrosion region mainly contains the elements such as Sn, Cr, Fe, O, connects
Get off and carry out XPS imagings to Sn, Cr, Fe, O.
The monochromatic X ray rifle spot diameter is set to：200 microns.
Imaging region is set to：1000μm×1000μm.
The quantity of scan node is set to：32×32.
Fig. 2 is the setting schematic diagram of imaging region and scan node.
3rd, the narrow spectrums of element XPS are gathered, the x-ray photoelectron power spectrum highest peak Sn3d of Sn, Cr, O is chosen, Cr2p, O1s is carried out
The collection of the narrow spectrums of XPS, because the XPS highest peaks Fe2p and Sn3p of Fe have overlapping cases, then from the XPS strong peak of Fe
Fe3p carries out the collection of the narrow spectrums of XPS.
It is logical to be set to 20eV.
Fig. 3 is the narrow spectrograms of Sn3d that Y=0 μm of node is collected at X=0 μm.
4th, data processing and imaging conversion process：
(1) background is removed：Open Thermo Avantage (Ver.5.952) software, be test obtain Sn3d, Cr2p,
Fe3p and O1s spectral peaks remove background, and background form is set to Shirley, obtains each element spectral peak peak area.Fig. 4 is shown X=
0 μm, the narrow spectrograms of Sn3d remove the spectral peak area schematic diagram obtained after Shirley backgrounds at Y=0 μm of node.Then software is automatic
The Scofield sensitivity factors of each element in database are called in, the relative amount shared by each element, Sn, Cr, Fe and O is calculated
Each shared relative mass percentage is respectively 54%, 22%, 7% and 17%.
(2) collection of illustrative plates fitting：In order to analyze the distribution situation of Sn element different valence states, swarming process of fitting treatment is carried out to Sn3d,
Collection of illustrative plates fitting function Peak fit is clicked on, is added the corresponding spectral peak of each peak position and is fitted.Fig. 5 is X=0 μm, Y=0 μm of node
The swarming fitted figure of the narrow spectrograms of place Sn3d, according to Sn3d5/2A、Sn3d5/2Peak position 484.9eV, 486.4eV of B, judges
Sn3d5/2A、Sn3d5/2The ownership at B peaks is respectively simple substance Sn and Sn4+, then software call in the Scofield of Sn in database automatically
Sensitivity factor, calculates the relative amount shared by each valence states of Sn, simple substance Sn and Sn4+Each shared relative mass percentage difference
For 12%, 42%.
(3) imaging conversion：Each element is selected, imaging conversion Creat Profile are clicked on, each individual element is presented
Relative amount distribution map, adjust image interpolation Grade I nterpolation level for 512, Fig. 6～Figure 11 be respectively Sn, Cr,
Fe、O、Sn4+Picture is imaged with the XPS of simple substance Sn.Tetra- elements of Sn, Cr, Fe and O are selected, is clicked on and is overlapped button Overlay
Map, being imaged on an image for these four elements is presented, and it is 8, Tu12Shi to adjust color rank Colour Level
The XPS imaging pictures of tetra- kinds of Elemental redistributions of Sn, Cr, Fe, O.
Summarize, can be seen that center spot corrosion region Cr, Sn are less from Fig. 6～Fig. 9, Fe, O are more, illustrate tin plate spot corrosion
Region passivating film is substantially thinning with tin layers, and spot corrosion is obvious, but spot corrosion region Sn contents are still higher, and spot corrosion is also not apparent from expanding to
At substrate, from Figure 10, Figure 11 tin plate sheet surface Sn is can be seen that4+It is many compared with simple substance Sn, because surface mainly contains Sn, Cr, Fe, O
Four kinds of elements, Sn4+Very likely with SnO2Form is present, and illustrates that the oxidation of material surface Sn is serious.Contrast Figure 10 and Figure 11,
Sn4+Imaging dark portion region it is less, Sn4+Relative amount it is minimum to 20.6%, and the imaging of center spot corrosion region simple substance Sn is dark
Portion region is larger, and the relative amount of simple substance Sn is minimum to 4.56%；And in remaining normal region of tin plate, Sn4+Relative amount
The relative amount up to 10.7% of up to 30.6%, simple substance Sn, spot corrosion region Sn4+It is remote with the relative amount ratio of simple substance Sn
Higher than normal region, illustrate that, in center spot corrosion region, higher proportion of Sn elements are used for the oxidation of.It can be recognized from fig. 12 that point
Corrosion centers Fe constituent content highests, and spot corrosion edge is mainly dispersed with O elements, non-corrosion area Sn, Cr content is higher, also
Containing some O elements, and Fe elements then almost do not have.
Above example matches the XPS analysis software Thermo Avantage that Mo Feishier companies produce using the U.S.
(Ver.5.952)。
Claims (5)
1. it is a kind of characterize material surface Elemental redistribution XPS i mage analysis methods, it is characterised in that concrete steps and parameter are such as
Under：
1) preparing needs to carry out the testing sample of XPS imagings, enters luggage sample；
2) the monochromatic X ray rifle is opened, the region to needing imaging carries out XPS point analysis, it is determined that needing the element being imaged；
Imaging region and scan node are set；Pointwise is to each narrow spectrum of element XPS needed for node collection；Finally, with XPS analysis software
Data processing and imaging conversion are carried out to the narrow spectrum of photoelectron spectroscopy of each element；
The monochromatic X ray rifle spot diameter arranges scope：200 μm～500 μm；
Imaging region arranges scope：2000 μm of 200 μ m, 200 μm～2000 μ m；
It is 3 × 3～64 × 64 that the quantity of scan node arranges scope；
3) the narrow spectrums of element XPS are gathered, the x-ray photoelectron power spectrum highest peak of element is chosen, when the x-ray photoelectron power spectrum of element
Highest peak overlaps with other elements spectral peak, then choose time strong peak or the highest peak misaligned with other elements spectral peak；Gather each
Element x-ray photoelectron energy time spectrum, it is desirable to which logical energy is identical, it is logical that scope can be set for 10～50eV；
4) data processing and imaging conversion process：
1. background is removed：XPS analysis software has three kinds of background types to be：Linear, Shirley, Tougaard, background selects model
Enclose can define photoelectron spectroscopy peak area to be defined；
2. collection of illustrative plates fitting：It is fitted using collection of illustrative plates when there is photoelectron spectrum overlap of peaks situation, selects the presence of the photoelectron spectrum for overlapping
Peak, clicks on collection of illustrative plates fitting function Peak fit, adds the corresponding spectral peak of each peak position and is fitted, while to the corresponding spectrum of each peak position
Peak is named respectively, determines the ownership of the photoelectron spectral peak；
3. the calculating of element relative amount：XPS analysis software is furnished with Scofield sensitivity factors database or Wagner is sensitive
Degree factor data storehouse；The sensitivity factor of each element is input on the hurdle of sensitivity factor one, that is, obtains each element spectral peak revised
Peak area；It is 100% by the revised peak area sum normalizing of all elements, the relative amount of each element is each element amendment
The shared ratio in the revised peak area sum of all elements of peak area afterwards；
4. imaging conversion：The height of all node each element relative amounts is presented in the form of pseudo- color image, with aobvious
Show the distribution situation of each element；Imaging conversion Creat Profile are clicked on, that is, presents the relative amount distribution of each individual element
Figure, adjusts the resolution ratio that image interpolation Grade I nterpolation level changes over picture, clicks on and overlaps button Overlay
Map, being imaged on an image for all elements is presented, and each element is represented with a kind of color, it will be seen that each element
Distribution situation, adjust color rank Colour Level and change over the resolution ratio of picture；It is 4～32 that color rank arranges scope.
2. analysis method according to claim 1, it is characterised in that described step 2) in imaging region scope is set
For：1000μm×1000μm.
3. analysis method according to claim 1, it is characterised in that described step 2) scan node quantitative range value
For：10 × 10～32 × 32.
4. analysis method according to claim 1, it is characterised in that described step 4) in background select Shirley classes
Type background.
5. analysis method according to claim 1, it is characterised in that described step 4) in interpolation level scope be set be
256～512.
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| CN111060545A (en) * | 2019-10-24 | 2020-04-24 | 兰溪致德新能源材料有限公司 | Method for detecting coating integrity of active substance of lithium ion battery |
| CN114460114A (en) * | 2022-04-13 | 2022-05-10 | 季华实验室 | Sample analysis method, device, apparatus and storage medium |
| CN115060755A (en) * | 2022-08-18 | 2022-09-16 | 季华实验室 | Depth analysis method for unknown sample layer structure |
| CN115165945A (en) * | 2022-09-08 | 2022-10-11 | 季华实验室 | Sample analysis method, device, equipment and storage medium based on test optimization |
| CN116908234A (en) * | 2023-09-13 | 2023-10-20 | 季华实验室 | Data analysis method, system and medium for multilayer sample structure |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111060545A (en) * | 2019-10-24 | 2020-04-24 | 兰溪致德新能源材料有限公司 | Method for detecting coating integrity of active substance of lithium ion battery |
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| CN115060755A (en) * | 2022-08-18 | 2022-09-16 | 季华实验室 | Depth analysis method for unknown sample layer structure |
| CN115165945A (en) * | 2022-09-08 | 2022-10-11 | 季华实验室 | Sample analysis method, device, equipment and storage medium based on test optimization |
| 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 |
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Address after: 100041 Shijingshan Road, Shijingshan District, Shijingshan District, Beijing Applicant after: Shougang Group Co. Ltd. Address before: 100041 Shijingshan Road, Shijingshan District, Shijingshan District, Beijing Applicant before: Capital Iron & Steel General Company |
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Application publication date: 20170510 |
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| WD01 | Invention patent application deemed withdrawn after publication |