CN113466141B - Method for nondestructive testing of metal substrate oxidation denaturation by using elliptical polarization spectrometer - Google Patents

Method for nondestructive testing of metal substrate oxidation denaturation by using elliptical polarization spectrometer Download PDF

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CN113466141B
CN113466141B CN202110552737.4A CN202110552737A CN113466141B CN 113466141 B CN113466141 B CN 113466141B CN 202110552737 A CN202110552737 A CN 202110552737A CN 113466141 B CN113466141 B CN 113466141B
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CN113466141A (en
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瞿敏妮
程秀兰
乌李瑛
权雪玲
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Shanghai Jiaotong University
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Abstract

The invention relates to a method for nondestructively detecting the oxidation denaturation of a metal substrate by using an elliptical polarization spectrometer, which uses a spectrum of 'metal substrate-target oxide' as a target spectrum and a spectrum of 'metal substrate-metal oxidation interface-target oxide' as a reference spectrum, can quickly judge the existence of the metal oxidation interface by fitting and comparing, and further analyze the information of the components, the thickness and the like of the metal oxidation interface, and simultaneously obtain the thickness and the optical constant of the target oxide. The method has high measurement precision, no damage to the sample and universality on thin film materials.

Description

Method for nondestructive testing of metal substrate oxidation denaturation by using elliptical polarization spectrometer
Technical Field
The invention relates to the technical field of thin film detection, in particular to a method for nondestructively detecting oxidation denaturation of a metal substrate by using an elliptical polarization spectrometer.
Background
The deposition of dielectric films on metal substrates is an important building block for optical devices. The structure unit can realize selective spectral absorption through a metal-medium single-layer or multi-layer film design, and meanwhile, when the device works in the atmospheric atmosphere and at a temperature higher than room temperature, the medium layer can protect the metal surface from being corroded and oxidized by moisture and oxygen. However, in the deposition of dielectric films, especially in the growth process of oxide dielectric films (such as silicon oxide, aluminum oxide, etc.), an oxidizing atmosphere of water, oxygen, ozone, etc. is usually required, and different processes involve high temperature around 300 ℃ or an environment in which plasma, etc. is liable to aggravate the oxidation process. Thus, eventually, in addition to the generation of the target grown oxide layer, a metal-backed oxide interface layer may also be present. The interface layer formed by oxidizing the metal substrate is very thin and is 10nm thick, and the interface layer formed by oxidizing the metal substrate and the oxide layer grown on the target are difficult to distinguish in morphology, so that high testing sensitivity is required.
The prior art can adopt a secondary ion mass spectrometry method for measurement, but the method has the defects of low measurement speed, material damage and the like.
The ellipsometry spectrum technique measures the change of the polarization state of the incident polarized light after the polarization state is reflected by the surface of a sample and the interface of each film layer. The change in polarization state is directly related to the thickness, optical constants (index of refraction n and extinction coefficient k), structure of the material. The data measured by the elliptical polarization spectrum is a comprehensive result of the interaction of the reflected light of the upper surface and the lower surface of each film layer, so that the thickness and the optical constant of each film layer are deduced. Because the polarization state variation contains intensity and phase information, the measurement sensitivity of the elliptical polarization spectrum technology is extremely high and can reach the sub-nanometer level. Based on the characteristics, the elliptical polarization spectrum technology can be used for researching the analysis of interfaces of different materials. In the application of oxide thin film testing and characterization, the target oxide layer is usually measured by using the ellipsometry technology, and how to construct a suitable model to measure the interfacial layer formed by the oxidation of the metal substrate by using the ellipsometry technology is rarely reported.
Patent No. CN 112361972A discloses a method for detecting the thickness and optical properties of a multilayer film, which adopts an elliptical polarization technique to measure the thickness and optical constants of the film, but uses fitting of different wave bands to distinguish a diamond film from a diamond-like film, and cannot detect an interface layer formed by oxidation of a metal substrate.
The invention provides a method for detecting whether a metal substrate is oxidized and denatured in the process of depositing an oxide medium by utilizing an elliptical polarization spectrum technology. The method can rapidly judge the existence of the metal oxidation interface by constructing a metal substrate-target oxide spectrum as a target spectrum and a metal substrate-metal oxidation interface-target oxide spectrum as a reference spectrum through fitting and comparison by utilizing different models, further analyze the information such as the component, the thickness and the like of the metal oxidation interface, and simultaneously obtain the thickness and the optical constant of the target oxide. The method has high measurement precision, no damage to the sample and universality on thin-film materials.
Disclosure of Invention
The invention aims to provide a method for nondestructively detecting the oxidation denaturation of a metal substrate by using an elliptical polarization spectrometer, aiming at the defects in the prior art, and the aim of the invention is realized by the following technologies:
the invention relates to a method for nondestructive testing of metal substrate oxidation denaturation by an elliptical polarization spectrometer, which comprises the following steps:
s1: depositing a target oxide dielectric film onto a metal substrate;
s2: measuring the elliptical polarization spectrum of the film in the interval from ultraviolet to near infrared spectrum to form an actual measurement spectrum;
s3: establishing a 'metal substrate-target oxide' structure model;
s4: adjusting the model parameters in the structural model in S3 to obtain the goodness of fit between the spectrum of the structural model and the actually measured spectrum, namely R 2
S5: s4 measurement of the resulting R 2 : if R is 2 Not less than 0.9, the metal substrate oxidative denaturation can be described by the structural model established by S3, i.e. the metal substrate does not undergo oxidative denaturation, and R can be obtained based on the condition 2 The thickness and optical constant values of each layer of the film are measured, and subsequent steps are not carried out; if R is 2 <0.9, the metal substrate oxidation denaturation condition can not be described by the structural model established by S3, namely, if an intermediate layer possibly exists between the target oxide dielectric film and the metal substrate, model fitting continues;
s6: establishing a structural model of metal substrate-metal oxidation interface-target oxide;
s7: adjusting model parameters in the structure model in S6 to obtain the coincidence degree between the spectrum and the actually measured spectrum of the structure model, namely R' 2
S8: r 'obtained from S7' 2 : if R' 2 Not less than 0.9, the oxidative denaturation of the metal substrate can be described by a structural model established by S6, namely the oxidative denaturation of the surface of the metal substrate is generated, and the condition based on R 'can be obtained' 2 The thickness and optical constant values of each layer of the film are measured, and subsequent steps are not carried out; if R' 2 <0.9, the oxidation denaturation condition of the metal substrate can not be described by the structural model established by S6, and model fitting is continued;
s9: adjusting the class of the metal oxide interface in the S6 structural model, and repeating S7-S9; and if the circulation times of S7-S9 exceed 10 times, exiting the circulation.
As an embodiment of the invention, the thickness of the target oxide dielectric thin film in the step S1 is 20-30nm.
In one embodiment of the present invention, the target oxide dielectric thin film material in step S1 is selected from one of silicon oxide, aluminum oxide, hafnium oxide and titanium oxide.
As an embodiment of the present invention, the metal substrate in step S1 is one selected from copper, silver, titanium, chromium, gold, and platinum.
As an embodiment of the present invention, the thin film deposition process in step S1 is one selected from atomic layer deposition, plasma enhanced chemical vapor deposition, inductively coupled plasma chemical vapor deposition, and magnetron sputtering.
As an embodiment of the present invention, the elliptical polarization spectra in step S2 are psi and delta at different wavelengths, both of which are equal to the Fresnel reflection coefficient R p And R s The method specifically comprises the following steps:
R p /R s =tan(Ψ)e
wherein R is p Is the reflection coefficient of p light, R s In terms of the reflection coefficient of s-light, tan (Ψ) is the ratio of the amplitude of the reflected p-light to that of the reflected s-light, and Δ is the change in the phase difference between the p-light and the s-light.
As an embodiment of the present invention, the target oxide in step S3 is described by one or more dispersion models of Cauchy, sellmeier, lorentz, tauc-Lorentz, gauss.
In step S4, the spectrum of the structural model is psi and Δ at different wavelengths, which are the fresnel reflection coefficient R p And R s The specific steps are as follows:
R p /R s =tan(Ψ)e
wherein R is p Is the reflection coefficient of p light, R s In terms of the reflectance of s-light, tan (Ψ) is the ratio of the amplitude of the reflected p-light to the amplitude of the reflected s-light, and Δ is the change in the phase difference between the p-light and the s-light.
As an embodiment of the present invention, the model parameters in step S4 include model parameters describing a dispersion model corresponding to the target oxide in S3, such as variable parameters in the Cauchy model, and the model library has an initial value and a fitting range, i.e., a maximum and a minimum value, for each model; s3, providing a predicted value for the thickness d of the target oxide film from an initial value according to a growth process, growth speed and time or other measurement means by a user; as well as the angle of incidence bias and the model constant term.
As an embodiment of the present invention, R in step S4 2 In the range of 0 to 1,R 2 =1 represents that the fitting result completely agrees with the test result; r 'in step S7' 2 Has a numerical value range of 0 to 1,R' 2 And =1 represents that the fitting result completely coincided with the test result.
As an embodiment of the present invention, the metal oxide interface and the target oxide in the structural model in step S6 may be described by one or more dispersion models of Cauchy, lorentz, cody-Lorentz, tauc-Lorentz, gauss, and Sellmeier, or by fixed n and k at different wavelengths; n is a refractive index, and k is an extinction coefficient; in step S7, the spectrum of the structural model is psi and Δ at different wavelengths, and the two are the fresnel reflection coefficient R p And R s The specific steps are as follows:
R p /R s =tan(Ψ)e
wherein R is p Is the reflection coefficient of p light, R s In terms of the reflection coefficient of s-light, tan (Ψ) is the ratio of the amplitude of the reflected p-light to that of the reflected s-light, and Δ is the change in the phase difference between the p-light and the s-light.
In step S6 of the present invention, the metal oxide interface and the target oxide in the structural model may be described by one or more dispersion models of Cauchy, lorentz, cody-Lorentz, tauc-Lorentz, gauss, and Sellmeier, or by fixed n and k at different wavelengths, where the fixed n and k at different wavelengths may be obtained from data rates in test software of an elliptical polarization spectrometer.
As an embodiment of the present invention, the metal oxide interface in the structure model in step S6 is a single metal oxide layer or a mixed layer of multiple metal oxides corresponding to the metal substrate.
Compared with the prior art, the invention has the following beneficial effects:
(1) By selecting the elliptical polarization spectrum measurement technology, the effects of non-contact and nondestructive measurement, high measurement speed and the like can be realized;
(2) The method can distinguish the metal oxide interface layer from the target oxide dielectric layer by establishing a metal substrate-target oxide structural model and a metal substrate-metal oxide interface-target oxide structural model; the material range of the measured metal substrate and the target oxide dielectric layer is wide; and can detect the ultrathin interface layer with the magnitude of 10 nm.
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Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is an interface diagram of model parameter adjustment in the fitting of example 1;
FIG. 2 is a schematic diagram of the structure obtained by fitting example 1 under a "metal substrate-target oxide" structure model;
FIG. 3 is a graph of measured and fitted Ψ and Δ R, R, for the "metal substrate-target oxide" structure model of example 1 2 =0.95242;
FIG. 4 is a graph of measured and fitted Ψ and Δ values, R, under a "metal substrate-target oxide" structure model in example 2 2 =0.24113;
FIG. 5 is a schematic diagram of the structure obtained by fitting example 2 under the structural model "metal substrate-metal oxide interface-target oxide";
FIG. 6 is a measured and fitted graph, R ', of Ψ and Δ and of the structure of example 2 under the "Metal substrate-Metal oxide interface-target oxide" structural model' 2 =0.91707;
FIG. 7 is a surface Scanning Electron Microscope (SEM) image of the samples of example 1 (left) and example 2 (right);
FIG. 8 is a cross-sectional view of a sample Focused Ion Beam (FIB) according to the present invention: example 1 (left) and example 3 (right);
FIG. 9 is a scanning image of an X-ray energy spectrometer (EDX) line on a cross section of example 3.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
The following examples were conducted in accordance with the respective specific parameters and the following procedures.
Step 1): depositing a target oxide dielectric film with a preset thickness on a metal substrate;
step 2): measuring an elliptical polarization spectrum of the sample in an interval from ultraviolet to near infrared spectrum;
step 3): establishing a model by using a metal substrate-target oxide structure;
step 4): in the whole measurement spectrum range, each film layer is described by respective thickness and model parameters, and an estimated value is used for unknown parameters;
and step 5): adjusting unknown parameters to improve the goodness of fit, R, between the spectrum produced by the model and the measured spectrum 2
Step 6): such as R 2 The material composition, the thickness and the optical parameters of each layer of film which are close to 0.9 or more are properly selected, and the fitting result can accurately describe the actual structure. It is here meant that no additional oxide interface layer is created between the metal substrate and the target oxide or that the interface layer is almost negligible;
step 7): to obtain a compound based on the above R 2 The thickness and optical constant values of each layer;
step 8): such as R 2 Much less than 0.9 represents that the model built cannot accurately describe the actual structure. It is here represented that there is a high probability of an oxide interface layer between the metal substrate and the target oxide;
step 9): establishing a model by using a structure of metal substrate-metal oxidation interface-target oxide to describe each layer of film;
step 10): repeating the step 4) 5);
step 11): such as R 2 Approximately 0.9 or more represents the material composition, thickness, optical parameter of each layer filmThe number is properly selected, and the fitting result can accurately describe the actual structure. Here it is represented that an oxide interfacial layer is present between the metal substrate and the target oxide and as described by the model;
step 12): to obtain a radical based on the above R 2 The film thickness and optical constant values of each layer;
step 13): such as R 2 Much less than 0.9 represents that the model built cannot accurately describe the actual structure. The material composition, thickness, optical parameters, etc. representing the metal oxide interface here need to be adjusted;
step 14): re-enter step 9).
Step 15): step 8) -step 14) are cycled for more than 10 times, and the loop is exited. The actual structure represented by the method is very complex, the established model cannot be accurately described, and the model needs to be analyzed by combining other measurement means.
When the spectrum of the structural model is fitted with the actually measured spectrum (obtaining goodness of fit R) 2 Time), the fitting principle inside the test software is actually fitting the Ψ ' and Δ ' obtained from the elliptically polarized spectrum of the structural model in S3/S6 to the Ψ ' and Δ values obtained from the elliptically polarized spectrum in S2. After the final fitting is finished, software can automatically calculate and output n and k of the target oxide and/or metal oxidation interface spectrum in the structure model in S3/S6, and then the corresponding S1 sample to be detected metal substrate oxidation denaturation condition and the corresponding n and k of the film spectrum can be obtained.
The adjustable structure model parameters in the invention comprise three parts: 1. dispersion model parameters for describing optical characteristics of each layer of film, such as variable parameters in the Cauchy model, wherein each model has an initial value and a fitting range, namely a maximum value and a minimum value in the model library; 2. a thickness parameter for describing the thickness of each thin film, the initial value of which is provided by a user according to the growth process, growth speed and time, or other measurement means; 3. other adjustable parameters, such as: angle of incidence deviation, model constant term. And why "tunable" is emphasized because if the optical properties of each film are described in 1 by a fixed list of n, k values at each wavelength, instead of a dispersion model, then these parameters cannot be tuned, only 2 thickness and 3 others.
Example 1
Depositing Al on a Cu substrate using an atomic layer deposition process 2 O 3 The film has a growth cycle number of 200 cycles, an estimated thickness of 20-30nm, and a process mode of a water method corresponding to a temperature of 300 ℃. The ellipsometer adopted in this embodiment is SE-2000, the testing software is SEA software on the ellipsometer, and the Cauchy model is used to describe the target oxide (i.e. Al) in the structural model of "metal substrate-target oxide 2 O 3 Film), adjusting parameters and incident angle deviation of the Cauchy model, a model constant term, and setting the initial thickness of the film to be a certain Value within the range of 20-30nm, and fig. 1 is an interface diagram for model parameter adjustment in fitting of embodiment 1, wherein several types of parameters are in a box, a field of Fit is hooked to represent participation in fitting, value is an initial Value, min and Max represent minimum and maximum values of the fitting range, and the adjusting method is to click start Fit after setting. Then, fitting can be performed, and fig. 2 is a structural overview diagram obtained by fitting in a "metal substrate-target oxide" structural model in example 1; FIG. 3 is a graph of measured and fitted Ψ and Δ values, R, under a "metal substrate-target oxide" structure model according to example 1 2 =0.95242, it was basically determined that there was no interfacial layer in the middle of the structure, and the Cu substrate had not undergone surface oxidative denaturation in the process.
Example 2
The test apparatus and software were the same as in example 1.
Depositing Al on a Cu substrate using an atomic layer deposition process 2 O 3 Film, growth cycle number 200cycle, predicted thickness 20-30nm, process by oxygen plasma method corresponding to temperature 150 deg.C, carrier gas N 2 . Establishing target oxide (Al) in metal substrate-target oxide structural model by Cauchy model 2 O 3 Film), finally, fig. 4 is a graph of measured and fitted Ψ and Δ R, for example 2 under a "metal substrate-target oxide" structural model 2 =0.24113, cu + Al for which it was basically judged that the structure was not simple 2 O 3 Middle poleAn interfacial layer may be present. Continuing the test, establishing a structure model of 'metal substrate-metal oxidation interface-target oxide' (the target oxide is described by the Cauchy model; the metal oxidation interface is described by n and k values under different wavelengths), wherein the metal oxidation interface is Cu 2 O, setting an initial value for the layer thickness. The final fitting results are shown in fig. 5 and fig. 6, wherein fig. 5 is a structural outline diagram obtained by fitting the structural outline diagram of example 2 under a structural model of "metal substrate-metal oxide interface-target oxide"; FIG. 6 is a measured and fitted graph, R ', of Ψ and Δ and of the structure of example 2 under the "Metal substrate-Metal oxide interface-target oxide" structural model' 2 =0.91707. According to step 11), it was confirmed that the surface oxidation denaturation of the Cu substrate occurred in the process to generate 10.1nm of Cu 2 O。
FIG. 7 is a Scanning Electron Microscope (SEM) image of the surface of the sample of example 1 (left) and example 2 (right),
the sample described in example 2 is a flat and uniform film observed under an optical microscope and a scanning electron microscope, and has no obvious difference compared with example 1, and whether the problem of interfacial oxidative denaturation exists cannot be judged, but the sample shows obvious difference under the measurement of an ellipsometry technology. The test results show that Al 2 O 3 The thickness of (a) is 21.2nm, which accords with the predicted thickness; and in the presence of 10.1nm Cu 2 And O is a surface oxidation layer formed on the surface of the Cu substrate under the oxygen plasma process.
Example 3
The test apparatus and software were the same as in example 1.
Depositing Al on Cu substrate by atomic layer deposition process 2 O 3 The growth cycle number of the film is 200 cycles, the predicted thickness is 20-30nm, the process mode is a thermal method, ozone is used as an oxidant, and the corresponding temperature is 300 ℃. Cauchy model is adopted to describe target oxide (namely Al) in structural model of metal substrate-target oxide 2 O 3 Film) the final result is R obtained in step 8) 2 =0.32272, and basically judges that the structure is not Cu + Al simple 2 O 3 In the middle, there is a high probability of an interfacial layer. Then, build up "metalSubstrate-metal oxide interface-target oxide "structure model (target oxide is established by Cauchy model; metal oxide interface is described by n, k values at different wavelengths), wherein" metal oxide interface "is Cu 2 O, setting an initial value for the thickness of the layer, continuously fitting, and judging a coefficient R 'according to a fitting result' 2 =0.34361; readjust "metal oxide interface" to Cu, cu 2 O mixture, fitting result determination coefficient R' 2 =0.28341; after multiple adjustments, a good fitting result cannot be obtained. As can be seen from step S9, the actual structure may be very complex, and the model cannot be accurately described.
Subsequently, the cross section of the sample obtained in this example was cut by a Focused Ion Beam (FIB) system for observation, fig. 8 is a Focused Ion Beam (FIB) cross section observation of the sample of the present invention: example 1 (left) and example 3 (right), from which it was found that the 200nm Cu film in example 3 was cracked and the surface became very rough. An X-ray energy spectrometer (EDX) is used to perform line scanning on the cross section from top to bottom to obtain atomic number fraction distribution curves of O, cu, al and Si elements, and fig. 9 is a line scanning diagram of the X-ray energy spectrometer (EDX) on the cross section of example 3. Carefully observing the distribution curves of O and Al, finding that the trends of the O and the Al are not completely consistent, and the distribution of O is also improved at the position with higher Cu distribution, thus proving the existence of Cu oxide. Although a better fitting result is more difficult to obtain in embodiment 3, the technical scheme has nondestructively provided evidence that the interface is oxidized and denatured, and the measurement speed is high, so that a foundation can be laid for subsequent analysis.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.

Claims (8)

1. A method for nondestructively detecting the oxidation denaturation of a metal substrate by using an elliptical polarization spectrometer is characterized by comprising the following steps:
s1: depositing a target oxide dielectric film onto a metal substrate;
s2: measuring the elliptical polarization spectrum of the film in the interval from ultraviolet to near infrared spectrum to form an actual measurement spectrum;
s3: establishing a 'metal substrate-target oxide' structure model;
s4: adjusting the model parameters in the structural model in S3 to obtain the coincidence degree between the spectrum of the structural model and the actually measured spectrum, namely R 2
S5: s4 measurement of the resulting R 2 : if R is 2 Not less than 0.9, the metal substrate oxidative denaturation can be described by the structural model established by S3, i.e. the metal substrate does not undergo oxidative denaturation, and R can be obtained based on the condition 2 The thickness and optical constant values of each layer of the film are measured, and subsequent steps are not carried out; if R is 2 <0.9, the metal substrate oxidation denaturation condition can not be described by the structural model established by S3, namely, if an intermediate layer possibly exists between the target oxide dielectric film and the metal substrate, model fitting continues;
s6: establishing a structural model of metal substrate-metal oxidation interface-target oxide;
s7: model parameters in the structure model in S6 are adjusted to obtain the goodness of fit between the spectrum and the actually measured spectrum of the structure model, namely R' 2
S8: r 'from S7' 2 : if R' 2 Not less than 0.9, the oxidative denaturation of the metal substrate can be described by a structural model established by S6, namely the oxidative denaturation of the surface of the metal substrate is generated, and the condition based on R 'can be obtained' 2 The thickness and optical constant values of each layer of the film are measured, and subsequent steps are not carried out; if R' 2 <0.9, the oxidation denaturation condition of the metal substrate can not be described by the structural model established by S6, and model fitting is continued;
s9: adjusting the class of the metal oxide interface in the S6 structural model, and repeating S7-S9; if the cycle times of S7-S9 exceed 10 times, exiting the cycle;
in the step S1, the target oxide dielectric film material is selected from one of silicon oxide, aluminum oxide, hafnium oxide and titanium oxide; in the step S1, the metal substrate is selected from one of copper, silver, titanium, chromium, gold, and platinum.
2. The method of claim 1, wherein the thin film deposition process in step S1 is selected from one of atomic layer deposition, plasma enhanced chemical vapor deposition, inductively coupled plasma chemical vapor deposition, and magnetron sputtering.
3. The method as claimed in claim 1, wherein the ellipsometry spectra in step S2 are psi and delta at different wavelengths, both of which are equal to the Fresnel reflection coefficient R p And R s The specific steps are as follows:
R p /R s =tan(Ψ)e
wherein R is p Is the reflection coefficient of p light, R s In terms of the reflection coefficient of s-light, tan (Ψ) is the ratio of the amplitude of the reflected p-light to that of the reflected s-light, and Δ is the change in the phase difference between the p-light and the s-light.
4. The method of claim 1, wherein the target oxide in step S3 is described by one or more dispersion models selected from the group consisting of Cauchy, sellmeier, lorentz, tauc-Lorentz, gauss.
5. The method of claim 1, wherein in step S4, the spectrum of the structural model is psi and delta at different wavelengths, which are the Fresnel reflection coefficient R p And R s The specific steps are as follows:
R p /R s =tan(Ψ)e
wherein R is p Is the reflection coefficient of p light, R s Tan (Ψ) is the amplitude of the reflected p-light and s-lightThe ratio, Δ, is the change in phase difference between p-light and s-light.
6. The method for nondestructive testing of metal substrate oxidation degradation by using ellipsometry as claimed in claim 1, wherein R in step S4 2 In the range of 0 to 1,R 2 =1 represents that the fitting result completely agrees with the test result; r 'in step S7' 2 Has a numerical value of 0 to 1,R' 2 =1 represents a complete match of the fitting results with the test results.
7. The method for nondestructive testing of oxidation denaturation of metal substrate by using ellipsometry as claimed in claim 1, wherein the metal oxide interface and the target oxide in the structural model in step S6 can be described by one or more dispersion models selected from Cauchy, lorentz, cody-Lorentz, tauc-Lorentz, gauss, and Sellmeier or n, k fixed at different wavelengths; n is a refractive index, and k is an extinction coefficient; in step S7, the spectrum of the structural model is psi and Δ at different wavelengths, and the two are the fresnel reflection coefficient R p And R s The specific steps are as follows:
R p /R s =tan(Ψ)e
wherein R is p Is the reflection coefficient of p light, R s In terms of the reflection coefficient of s-light, tan (Ψ) is the ratio of the amplitude of the reflected p-light to that of the reflected s-light, and Δ is the change in the phase difference between the p-light and the s-light.
8. The method for nondestructive testing of metal substrate oxidation degeneration by using ellipsometry as claimed in claim 1, wherein the metal oxidation interface in the structure model in step S6 is a single metal oxide layer or a mixed layer of multiple metal oxides corresponding to the metal substrate.
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Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103217387B (en) * 2013-03-22 2015-04-15 清华大学 Method for measuring high temperature optical constant of metal oxide layer
CN104458589A (en) * 2014-12-02 2015-03-25 中国航天科工集团第三研究院第八三五八研究所 Method for accurately calibrating optical constant of visible light waveband of optical thin film
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CN110514599B (en) * 2019-08-23 2020-11-03 浙江大学 Optical parameter detection method for fluorine-doped tin oxide coated glass

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