CN111781148B - Method, device, terminal and system for detecting longitudinal non-uniformity of film - Google Patents

Method, device, terminal and system for detecting longitudinal non-uniformity of film Download PDF

Info

Publication number
CN111781148B
CN111781148B CN201910273286.3A CN201910273286A CN111781148B CN 111781148 B CN111781148 B CN 111781148B CN 201910273286 A CN201910273286 A CN 201910273286A CN 111781148 B CN111781148 B CN 111781148B
Authority
CN
China
Prior art keywords
film
model
sample
uniformity
curve
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.)
Active
Application number
CN201910273286.3A
Other languages
Chinese (zh)
Other versions
CN111781148A (en
Inventor
孙瑶
钟大龙
王新宇
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shenhua Beijing Photovoltaic Technology Research And Development Co ltd
Original Assignee
Shenhua Beijing Photovoltaic Technology Research And Development Co ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Shenhua Beijing Photovoltaic Technology Research And Development Co ltd filed Critical Shenhua Beijing Photovoltaic Technology Research And Development Co ltd
Priority to CN201910273286.3A priority Critical patent/CN111781148B/en
Publication of CN111781148A publication Critical patent/CN111781148A/en
Application granted granted Critical
Publication of CN111781148B publication Critical patent/CN111781148B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/21Polarisation-affecting properties
    • G01N21/211Ellipsometry
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/27Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands using photo-electric detection ; circuits for computing concentration
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/21Polarisation-affecting properties
    • G01N21/211Ellipsometry
    • G01N2021/213Spectrometric ellipsometry

Abstract

The invention discloses a method, a device, a system and a terminal for detecting longitudinal non-uniformity of a film, which relate to the technical field of film detection and aim to improve the application range of a method for nondestructive detection of the longitudinal non-uniformity of the film. The method for detecting the longitudinal non-uniformity of the film comprises the following steps: receiving ellipsometry curve information of a sample to be detected, wherein the sample to be detected at least comprises a film to be detected; establishing an isotropic physical model according to the characteristics of the measured sample, wherein the physical model at least comprises a film model; converting at least one variable parameter contained in the film model into a graded variable parameter; taking ellipsometry curve information of a measured sample as a curve fitting target, and performing curve fitting on the graded variable parameters by using a film model to obtain variation curve information of the photoelectric parameters of the measured sample in the longitudinal direction of the measured sample; and determining the longitudinal non-uniformity of the tested sample according to the change curve information. The invention is used for detecting the longitudinal non-uniformity of the film.

Description

Method, device, terminal and system for detecting longitudinal non-uniformity of film
Technical Field
The present invention relates to the field of film detection technologies, and in particular, to a method and apparatus for detecting longitudinal non-uniformity of a film, a terminal, and a detection system.
Background
The transparent conductive oxide (Transparent Conductive Oxide, abbreviated as TCO) film is an important optical material, so that the photoelectric characteristics of bandwidth inhibition, low resistivity, high light transmittance in the visible light range, high light reflectance in the infrared spectrum range and the like are dominant in the transparent conductive film, and the transparent conductive oxide film is widely applied to the photoelectric fields of solar cells, liquid crystal displays, gas sensors, heat conducting glass (anti-fog and anti-icing) for airplanes and automobiles and the like.
The oxygen content in the TCO film has an important influence on the photoelectric performance, and if the oxygen content is low, the TCO film presents a metal-like color and loses transparency; if the oxygen content is high, the number of oxygen vacancies is reduced, so that the effect of doping the external donor impurities is lost, resulting in the chemical composition of the TCO film approaching the insulator until becoming an insulator; when the oxygen content is proper, the quantity of oxygen vacancies in the TCO film is proper, and the substitutional impurity plays a role of a donor, so that the TCO film has excellent photoelectric performance. During the coating process, there is inevitably an uneven distribution of oxygen content along the longitudinal direction of the surface of the TCO film due to the surface relaxation and surface energy effects of the TCO film, so that the components contained in the surface and the inside thereof are transited to achieve the balance between energy and substances. The longitudinal non-uniformity of the TCO film surface has an important effect on the photovoltaic properties of the film and therefore it is necessary to detect the longitudinal non-uniformity of the film material.
In the prior art, a depth analysis method is adopted to test the change of element components in the TCO film along with the depth, and the longitudinal non-uniformity of the film is determined according to the change of the element components in the TCO film along with the depth. The test instruments used for depth profiling are typically X-ray photoelectron spectroscopy (XPS), auger Electron Spectroscopy (AES), secondary Ion Mass Spectrometry (SIMS) or glow discharge spectroscopy (GDOES), but these test instruments inevitably damage the sample under test during the detection process. At present, some techniques for non-destructive testing of the longitudinal non-uniformity of a film have been developed, but the application range is relatively narrow.
Disclosure of Invention
The embodiment of the invention provides a method, a device, a terminal and a system for detecting longitudinal non-uniformity of a film, which are used for improving the application range of the nondestructive detection method for the longitudinal non-uniformity of the film.
In order to achieve the above purpose, the embodiment of the present invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for detecting longitudinal non-uniformity of a film, including:
acquiring ellipsometry curve information of a sample to be tested, wherein the sample to be tested at least comprises a film to be tested;
establishing an isotropic physical model according to the characteristics of the tested sample, wherein the physical model at least comprises a film model;
Converting at least one variable parameter contained in the film model into at least one group of graded variable parameters;
taking ellipsometry curve information of the measured sample as a curve fitting target, and performing curve fitting on at least one group of gradient variable parameters by using the film model to obtain change curve information of photoelectric parameters of the measured sample in the longitudinal direction of the measured sample;
and determining the longitudinal non-uniformity of the measured sample according to the change curve information of the photoelectric parameter of the measured sample in the longitudinal direction of the measured sample.
In some embodiments, the convergence condition for performing the curve fitting is a mean square error value of less than 80.
In some embodiments, the convergence condition for performing the curve fitting is a mean square error value of less than 20.
In some embodiments, the optoelectronic parameters of the sample under test include an optical constant that satisfies the cremer-kroney relationship and/or a dielectric constant that satisfies the cremer-kroney relationship.
In some embodiments, the physical model further comprises a matrix model and a surface model, the film model is located between the matrix model and the surface model, the matrix model is a cauchy model, the film model is a lorentz model or a gaussian model, and the surface model is an effective medium model.
In some embodiments, the converting the at least one variable parameter contained by the film model to at least one set of graded variable parameters comprises:
according to the order of influencing the weight from high to low on the fitting result, one or two variable parameters in the film model are selected for gradient conversion;
and/or the number of the groups of groups,
the graded variable parameter comprises a variable parameter of linear gradient change or a variable parameter of nonlinear gradient change.
In a second aspect, the present invention also provides a device for detecting longitudinal non-uniformity of a film, comprising:
the receiving unit is used for acquiring ellipsometric spectrum curve information of a sample to be detected, wherein the sample to be detected at least comprises a film to be detected;
a modeling unit, configured to establish an isotropic physical model according to the characteristics of the sample to be measured, where the physical model includes at least a thin film model; converting at least one variable parameter contained in the film model into at least one group of graded variable parameters;
the curve fitting unit is used for performing curve fitting on at least one group of gradient variable parameters by using the film model by taking ellipsometry curve information of the tested sample as a curve fitting target to obtain change curve information of photoelectric parameters of the tested sample in the longitudinal direction of the tested sample;
And the analysis unit is used for evaluating the longitudinal non-uniformity of the tested sample according to the change curve information of the photoelectric parameter of the tested sample in the longitudinal direction of the tested sample.
In some embodiments, the convergence condition for performing the curve fitting is a root mean square error value of less than 80;
and/or the number of the groups of groups,
the photoelectric parameters of the tested sample comprise optical constants meeting the Kramer-Croney relation and/or dielectric constants meeting the Kramer-Croney relation;
and/or the number of the groups of groups,
the physical model further comprises a matrix model and a surface model, the film model is positioned between the matrix model and the surface model, the matrix model is a cauchy model, the film model is a lorentz model or a gaussian model, and the surface model is an effective medium model;
and/or the number of the groups of groups,
the converting the at least one variable parameter contained in the film model into at least one set of graded variable parameters comprises:
according to the order of influencing the weight from high to low on the fitting result, one or two variable parameters in the film model are selected for gradient conversion;
and/or the number of the groups of groups,
the graded variable parameter comprises a variable parameter of linear gradient change or a variable parameter of nonlinear gradient change.
In some embodiments, the convergence condition for performing the curve fitting is a root mean square error value of less than 20.
In a third aspect, the present invention also provides a method for detecting longitudinal non-uniformity of a film, including:
measuring an ellipsometric spectrum curve of a measured sample;
transmitting ellipsometry curve information of the detected sample to a thin film longitudinal non-uniformity detection device according to the scheme; the ellipsometry curve information of the sample to be tested represents an ellipsometry curve of the sample to be tested;
and determining the longitudinal non-uniformity of the tested sample by using the film longitudinal non-uniformity detection device.
In some embodiments, the measuring an ellipsometry profile of a sample under test comprises:
and (3) incident linearly polarized light to the surface of the sample to be detected, and detecting an amplitude ratio spectrum curve and a phase difference spectrum curve of elliptical polarized p light and s light of the sample to be detected.
In some embodiments, the measuring an ellipsometry profile of a sample under test comprises:
setting the incidence angle of the linearly polarized light, wherein the incidence angle of the linearly polarized light comprises at least one first incidence angle and at least one second incidence angle, each first incidence angle is larger than the brewster angle of the tested sample material, and each second incidence angle is smaller than the brewster angle of the tested sample material;
At least one first incidence angle and at least one second incidence angle, respectively, linearly polarized light is incident to the measured sample, and the amplitude ratio of the elliptical polarized p light to the s light of the measured sample and the phase difference of the elliptical polarized p light and the s light of the measured sample are detected;
obtaining an ellipsometric amplitude ratio spectrum curve of the measured sample according to the amplitude ratio of the ellipsometric p light to the s light of the measured sample and the wavelength range of the linearly polarized light;
and obtaining an ellipsometric phase difference spectrum curve of the measured sample according to the phase difference between the ellipsometric p-light and the s-light of the measured sample and the wavelength range of the linearly polarized light.
In some embodiments, the linearly polarized light has a wavelength in the range of 300nm to 2400nm.
In a fourth aspect, embodiments of the present invention also provide a detection system, including:
ellipsometry apparatus;
the device for detecting the longitudinal non-uniformity of the film according to the scheme, wherein a receiver included in the device for detecting the longitudinal non-uniformity of the film is connected with the ellipsometer.
In a fifth aspect, the present invention provides a terminal, including:
a memory for storing one or more computer software instructions comprising a program for performing the method for detecting longitudinal non-uniformities of a film described in the above schemes;
And the processor is used for executing one or more computer software instructions to realize the program related to the method for detecting the longitudinal non-uniformity of the film in the scheme.
According to the method for detecting the longitudinal non-uniformity of the film, provided by the invention, an isotropic physical model is established according to the characteristics of a sample to be detected, so that the physical model at least comprises a film model; converting at least one variable parameter contained in the film model into at least one group of graded variable parameters, then taking ellipsometry curve information of the measured sample as a curve fitting target, and performing curve fitting on the at least one group of graded variable parameters by using the film model to obtain change curve information of photoelectric parameters of the measured sample in the longitudinal direction of the measured sample; at this time, the change curve information of the photoelectric parameter of the measured sample in the longitudinal direction of the measured film is adapted to the ellipsometric spectrum curve information of the measured sample, which indicates that the established physical model is matched with the actual measured sample, and the change curve information of the photoelectric parameter of the measured film in the longitudinal direction of the measured film can reflect the longitudinal non-uniformity of the measured film, so that when the established physical model is matched with the actual measured sample, the longitudinal non-uniformity of the measured sample can be determined according to the change curve information of the photoelectric parameter of the measured sample in the longitudinal direction of the measured sample; therefore, the method for detecting the longitudinal non-uniformity of the film can carry out nondestructive detection on any film sample so as to determine the longitudinal non-uniformity of the film, and is not limited by the composition of the film; meanwhile, when the longitudinal non-uniformity of the measured sample is determined, the influence of the process parameters and/or the film composition on the gradient variable parameters used in the fitting process can be judged by adjusting the process parameters and/or the film composition, and if the process parameters and/or the film composition are found to have influence on the gradient variable parameters used in the fitting process, the process parameters and/or the film composition are indicated to cause the longitudinal non-uniformity of the film. That is, the method for detecting the longitudinal non-uniformity of the film provided by the invention can also be used for analyzing the reasons for generating the longitudinal non-uniformity of the film by utilizing the gradient variable parameters used for fitting so as to guide the film forming process or the selection of the film composition.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a block diagram of a detection system according to an embodiment of the present invention;
FIG. 2 is a flowchart of a method for detecting longitudinal non-uniformity of a thin film according to a first embodiment of the present invention;
FIG. 3 is a flowchart of another method for detecting longitudinal non-uniformity of a thin film according to a first embodiment of the present invention;
FIG. 4 is a schematic diagram of a structure of a sample to be tested according to a first embodiment of the present invention;
FIG. 5 is a frame diagram of a film longitudinal non-uniformity detection terminal provided by an embodiment of the present invention;
FIG. 6 is a flowchart showing an ellipsometry curve of a sample to be measured according to an embodiment of the present invention;
FIG. 7 is an ellipsometric delta spectrum of an ITO film of the second embodiment;
FIG. 8 is an ellipsometric ψ spectrum of ITO thin film of the second embodiment;
FIG. 9 is a graph showing the distribution of center peak positions of linear gradient changes in the second embodiment;
FIG. 10 is a graph showing the variation of refractive index and extinction coefficient of an ITO thin film in the longitudinal direction of a sample to be tested in accordance with the second embodiment;
FIG. 11 is a graph showing the dielectric constant of the top and bottom of the ITO film according to the photon energy in the second embodiment;
FIG. 12 is an ellipsometric delta spectrum of an AZO film in example three;
FIG. 13 is a graph of ellipsometric ψ spectra of AZO films in example three;
FIG. 14 is a graph showing the distribution of central peak positions of nonlinear gradient changes in the third embodiment;
FIG. 15 is a graph showing the variation of refractive index and extinction coefficient of AZO thin film in the longitudinal direction of a sample to be tested in example III;
fig. 16 is a graph showing the dielectric constant of the top and bottom of AZO films as a function of photon energy in the third embodiment.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The transparent conductive film is an important photoelectric material, has high conductivity, high light transmittance in a visible light range and high reflectivity in a far infrared range, and is widely applied to photoelectric fields such as solar cells, liquid crystal displays, gas sensors, heat conducting glass (anti-fog and anti-icing) for aircrafts and automobiles, and the like.
The oxygen content in the transparent conductive film has an important influence on the photoelectric performance, and if the oxygen content is low, oxygen vacancies cause the transparent conductive film to take on the color of metalloid and lose transparency; if the oxygen content is high, the number of oxygen vacancies in the transparent conductive film is reduced, or external donor impurities (donor impurities refer to atoms which can be artificially doped with a certain chemical element to control the property of a semiconductor, and extra valence electrons generated by doping impurity elements and the valence electrons of a semiconductor material can break loose and become conductive free electrons, and positive centers are formed after the impurities are ionized) lose doping effect, so that the chemical composition of the transparent conductive film is close to 100%, and even the transparent conductive film loses conductivity to become an insulator; when the oxygen content is proper, the amount of oxygen vacancies in the transparent conductive film is proper, and substitutional impurities (taking semiconductor material silicon as an example, after the impurity atoms enter the semiconductor silicon, the impurity atoms can only exist in two modes, namely, one mode is that the impurity atoms are positioned at the gap positions among lattice atoms and are commonly called as gap impurities, and the other mode is that the impurity atoms are removed from the lattice atoms and are positioned at lattice sites and are commonly called as substitutional impurities), so that the photoelectric performance of the transparent conductive film is excellent.
The transition between the components or structures exists between the surface and the inside of the film due to the action of surface relaxation and surface energy so as to realize the balance between energy and substances, so that the unavoidable distribution of oxygen content in the transparent conductive film formed by adopting a film coating process is uneven along the longitudinal direction of the transparent conductive film (the thickness direction of the transparent conductive film), and therefore the detection of the longitudinal non-uniformity of the film material is required. In view of this, in the prior art, it is generally required to obtain the longitudinal non-uniformity of the sample to be tested by applying energy to the sample to be tested and detecting the fluorescent spectrum of the emitted particles or emissions, such as by using X-ray irradiation or bombardment etching, but the sample to be tested is damaged, which is a destructive detection. Although there is also provided a method for nondestructively detecting longitudinal non-uniformities of a film, the detected film belongs to a two-component system, and an effective medium model is required to be used for establishing a film model, which has no universality.
The embodiment of the invention provides a detection system, as shown in fig. 1, which comprises an ellipsometer 100 and a thin film longitudinal non-uniformity detection device 200, wherein the ellipsometer 100 is connected with the thin film longitudinal non-uniformity detection device 200. The following description of the detection method of the detection system according to the embodiment of the present invention is given by way of explanation, not limitation, with reference to fig. 1 and 2.
The first step: the ellipsometer 100 measures an ellipsometric spectrum curve of a sample to be measured; the ellipsometer is also called an ellipsometer, can detect an ellipsometric spectrum curve of a sample to be detected, and the ellipsometric spectrum curve can be an ellipsometric phase difference spectrum curve (also called an ellipsometric delta spectrum curve) and/or an ellipsometric amplitude ratio ψ spectrum curve (also called an ellipsometric ψ spectrum curve).
And a second step of: the ellipsometry curve information of the sample to be measured is transmitted to the thin film longitudinal non-uniformity detecting device 200.
And a third step of: the longitudinal non-uniformity of the sample to be measured is determined by the thin film longitudinal non-uniformity detection device 200.
In a first implementation, referring to fig. 3, an embodiment of the present invention provides a method for detecting longitudinal non-uniformity of a thin film, where the longitudinal non-uniformity refers to non-uniformity of optical constants or dielectric constants caused by non-uniformity of components or structures in the longitudinal direction of the thin film. The method for detecting the longitudinal non-uniformity of the film comprises the following steps:
step S110: and acquiring ellipsometry curve information of the sample to be detected, wherein an ellipsometry curve (ellipsometry spectrum) characterized by the ellipsometry curve information is the ellipsometry curve. The sample to be tested at least comprises a film to be tested 402, and the number of layers of the film to be tested can be one layer or multiple layers; for example, the film to be tested is a transparent conductive oxide film, and the material used can be In 2 O 3 、SnO 2 、ZnO、In 2 O 3 :Sn(ITO)、In 2 O 3 :Mo(IMO)、SnO 2 :Sb(ATO)、SnO 2 F (FTO), znO, al (AZO), etc., although not limited thereto.
As shown in fig. 4, on the basis of meeting the practical situation, considering that the tested sample/air interface is not an ideal smooth plane, the tested sample further comprises a rough layer 401 and a substrate layer 403, the tested film 402 is positioned between the substrate layer 403 and the rough layer 401, and the tested film 402 is manufactured on the surface of the substrate by adopting film forming equipment. The film forming process is selected from any one of electron beam evaporation, magnetron sputtering and chemical vapor deposition, but is certainly not limited thereto.
The substrate layer 403 is transparent glass, transparent plastic, etc. of various kinds, the rough layer 401 is the surface of the measured film contacting the atmosphere, which is not dense and loose, and is designed by adopting an effective medium theory, which is a model theory of a composite nano metal ceramic film microstructure formed by dispersing nano metal particles in a ceramic (dielectric) substrate, the designed rough layer comprises a surface loose layer with 50% porosity, namely the surface loose layer comprises 50% of pores by volume and 50% of measured film material by volume, and the optical constant of the measured film is half of that of the measured film.
Step S120: and establishing an isotropic physical model according to the characteristics of the tested sample, wherein the physical model at least comprises a film model. When the sample to be tested further comprises a matrix layer and a rough layer, the physical model is set to further comprise a matrix model and a surface model.
Specifically, a matrix model is built according to the characteristics of the matrix layer, a film model is built according to the characteristics of the film to be tested, and a surface model is built according to the characteristics of the rough layer.
The film model, the matrix model, and the surface model included in the isotropic physical model are all considered to be isotropic models, and the substance included in the corresponding solid film layer is isotropic. Isotropy (also called homogeneity) refers to a characteristic that the physical, chemical, etc. properties of an object do not change due to differences in direction.
The characteristics of the sample may include the composition of the sample, or the photoelectric parameter of the sample. Since the physical Model is established to be characterized by the composition of the material of the sample to be measured, and the ellipsometer measures the ellipsometric spectrum curve of the sample to be measured, the physical Model selection of the sample to be measured is very important for post-fitting, and the physical Model here includes, but is not limited to, cauchy Model, lorentz Model, gaussian Model, and Du Lude Model, drude Model. The physical model of each film layer included in the tested sample is selected according to the characteristics of the tested sample; of these, the cauchy model is applicable to transparent or weakly absorbing materials, the lorentz model and the gaussian model are both applicable to semiconductor materials, and the Du Lude model is applicable to metallic materials. For example: when the substrate layer 203 is transparent glass, a cauchy model is selected as a physical model of the substrate layer; when the measured thin film 402 is a transparent conductive thin film, a lorentz model and a gaussian model are selected as physical models of the transparent conductive thin film. When the film layer corresponding to the surface model has a certain roughness, an effective medium method is adopted to construct the surface model, and the type of the surface model is an effective medium model.
Step S130: at least one variable parameter contained in the film model is converted into at least one set of graded variable parameters. I.e. one variable parameter may be converted into a set of graded variable parameters.
For example: the measured film is prone to longitudinal non-uniformity, so that at least one variable parameter in the film model is selected, and the variable parameter is graded into the variable parameter. Considering that a plurality of variable parameters exist in the film model, at least one variable parameter is selected and converted into a gradient variable parameter in order to reduce fitting difficulty. Preferably, the variable parameter is converted to a graded variable parameter by expressing a gradient function of the variable parameter along the depth of the membrane layer.
It can be understood that the variation of the variable parameter included in the film model in the numerical value along the depth direction (longitudinal direction) gradient is mostly caused by the longitudinal non-uniformity caused by the film production process, such as the supply of oxygen, the variation of longitudinal free energy, the variation of electronegativity and other driving forces. Based on this, the converting the at least one variable parameter contained in the film model into at least one set of graded variable parameters includes:
And selecting one or two variable parameters in the film model to perform gradient conversion according to the order of influencing the weight from high to low on the fitting result.
For example: and selecting one variable parameter in the film model for gradient conversion, and selecting one variable parameter with the greatest influence weight on the fitting result from the film model for gradient conversion.
Also for example: and selecting two variable parameters in the film model for gradient conversion, and selecting the variable parameters ranked in the first two bits from the film model for gradient conversion according to the order of influencing the weight from high to low on the fitting result.
The variable parameters of the gradient include variable parameters of linear gradient change or variable parameters of nonlinear gradient change. If two variable parameters are selected for gradient transformation, one variable parameter can be selected for linear gradient transformation as required, and the other variable parameter can be selected for nonlinear gradient transformation. The variable parameter is converted into the variable parameter of linear gradient change or the variable parameter of nonlinear gradient change is determined by trial and error. The trial-and-error priority is fitted according to the variable parameter fitting curve of the linear gradient change, a better result cannot be obtained through fitting, and then the variable parameter fitting curve of the nonlinear gradient change is converted; if the fitting is not finished, another variable parameter is selected to carry out trial and error again. If the fit is still not successful, consideration needs to be given to whether the established physical model is appropriate. For example: the original metal model is established as a cauchy model suitable for transparent materials; or whether the input initial value deviates too much from the actual situation, for example: the initial value of the film thickness of the film with the film thickness of 350nm is input to 1000nm, and the fitting result is greatly deviated from the actual situation.
Step S140: and (3) taking ellipsometry curve information of the measured sample as a curve fitting target, performing curve fitting on at least one group of gradient variable parameters by using a film model, and if fitting is successful, obtaining the change curve information of the photoelectric parameters of the measured sample in the longitudinal direction of the measured sample. The photoelectric parameters comprise one or more of refractive index n, extinction coefficient k and dielectric constant, and different types of photoelectric parameters are specifically selected according to actual needs.
For example: and selecting one to two variable parameters, converting the variable parameters into gradient variable parameters to obtain one to two groups of gradient variable parameters, and substituting the one to two groups of gradient variable parameters into a film model to perform fitting through inversion calculation. If the fitting fails, the other variable parameters are selected again for gradient processing, and then the fitting is carried out. If the fitting still fails, it is indicated that the isotropic physical model may not be suitable, and the procedure returns to step S120 to change the type of the isotropic physical model, and then steps S130 and S140 are performed until the fitting is successful.
S150: and determining the longitudinal non-uniformity of the measured sample according to the change curve information of the photoelectric parameter of the measured sample in the longitudinal direction of the measured sample. Because the photoelectric parameters reflect the uniformity of the film layer to a certain extent, the longitudinal non-uniformity of the measured sample can be determined through the change curve of the photoelectric parameters of the measured sample in the longitudinal direction of the measured sample, so that the property of the measured sample can be further confirmed, and the measured sample can be applied to the proper field.
From the above, it can be seen that: establishing an isotropic physical model according to the characteristics of the measured sample, so that the physical model at least comprises a film model; converting at least one variable parameter contained in the film model into at least one group of graded variable parameters, then taking ellipsometry curve information of the measured sample as a curve fitting target, and performing curve fitting on the at least one group of graded variable parameters by using the film model to obtain change curve information of photoelectric parameters of the measured sample in the longitudinal direction of the measured sample; at this time, the change curve information of the photoelectric parameter of the measured sample in the longitudinal direction of the measured film is adapted to the ellipsometric spectrum curve information of the measured sample, which indicates that the established physical model is matched with the actual measured sample, and the change curve information of the photoelectric parameter of the measured film in the longitudinal direction of the measured film can reflect the longitudinal non-uniformity of the measured film, so that when the established physical model is matched with the actual measured sample, the longitudinal non-uniformity of the measured sample can be determined according to the change curve information of the photoelectric parameter of the measured sample in the longitudinal direction of the measured sample; therefore, the method for detecting the longitudinal non-uniformity of the film provided by the embodiment of the invention can carry out nondestructive detection on any film sample so as to determine the longitudinal non-uniformity of the film, and is not limited by the composition of the film; meanwhile, when the longitudinal non-uniformity of the measured sample is determined, the influence of the process parameters and/or the film composition on the gradient variable parameters used in the fitting process can be judged by adjusting the process parameters and/or the film composition, and if the process parameters and/or the film composition are found to have influence on the gradient variable parameters used in the fitting process, the process parameters and/or the film composition are indicated to cause the longitudinal non-uniformity of the film. That is, the method for detecting the longitudinal non-uniformity of the film provided by the invention can also be used for analyzing the reasons for generating the longitudinal non-uniformity of the film by utilizing the gradient variable parameters used for fitting so as to guide the film forming process or the selection of the film composition. Therefore, compared with the prior art, the method for detecting the longitudinal non-uniformity of the film provided by the embodiment of the invention does not need to detect emergent particles or glow-emitting fluorescence generated by collision of incident particles or ray beams and a detected sample, is non-contact nondestructive detection, does not damage the material composition of the detected sample, does not influence the service performance of the detected sample, and is very suitable for nondestructive detection of products or laboratory samples on a production line.
In some embodiments, the curve fitting is based primarily on a mean square error value (Mean Squared Error, abbreviated MSE) to determine whether the curve fitting was successful; wherein, the smaller the mean square error value is, the more the fitted change curve information is matched with the ellipsometry curve information of the measured sample. The curve fitting is a process of searching a minimum mean square error value, and the convergence condition for curve fitting is set to be that the mean square error value is smaller than 80; further, the convergence condition for curve fitting is set to be smaller than 20, so that the change curve information of the photoelectric parameters of the tested sample in the longitudinal direction of the tested sample meeting the requirements can be fitted quickly.
It can be understood that due to film forming processes such as a film coating method or a chemical deposition method, a certain error exists in the finished product specification of the manufactured film inevitably, that is, a certain gap exists between the finished product specification and the required specification, which results in that when the known value of the film is input into the basic model, the fitted result and the set specification come in and go out. For example: when the initial film thickness of the transparent conductive thin film is 350nm, the initial value of 350nm as the basic model is inputted into the basic model, and the fitting result obtained is about 350nm without keeping the same as the initial film thickness, which error is allowable. In order to improve the accuracy of fitting, the known initial value may be input into the basic model for fitting before curve fitting, and then the initial value of the film thickness may be reset to 100nm-700nm according to the fitting result, and the result may be fitted at this time, but the MSE value result may be different, but if the deviation of the initial value of the film thickness is too much, for example, the initial value of the film thickness is set to 1000nm, the fitting result is far different. Therefore, in the fitting process, the parameters to be fitted are set as a group of gradient variable parameters, so that the fitting time can be effectively shortened, and the fitting accuracy is improved.
In order to make the obtained change curve information of the photoelectric parameter of the measured sample in the longitudinal direction of the measured sample more accurate, the photoelectric parameter of the measured sample may be required to satisfy the Kramer-Kronig relationship (K-K relationship for short), and the photoelectric parameter may be one or two of optical constant and dielectric constant.
For example: the optical constant includes a refractive index n and an extinction coefficient K, and when the optical constant satisfies the K-K relationship, the refractive index n and the extinction coefficient K satisfy the K-K relationship. In addition, since the light is electromagnetic in nature, the relationship between the optical constant and the dielectric constant can be derived from maxwell's equations: n is n 2 -k 2 =ε r ,2nk=σ/(ωe 0 )(ε r The relative dielectric constant is complex; sigma is the conductivity, omega is the angular frequency of the plane wave, e 0 Vacuum dielectric constant). The mathematical relationship between the optical constant and the dielectric constant can be determined according to the relational expression between the optical constant and the dielectric constant, so that when curve fitting is performed, whether the fitting result is the optical constant or the dielectric constant or both the optical constant and the dielectric constant can be selected according to actual needs.
It will be appreciated that the method for detecting the longitudinal non-uniformity of a film described above may be performed by means of a processor, which may be a single processor or a collective term of a plurality of processing elements. For example, the processor may be a central processing unit (Central Processing Unit, CPU for short), an application specific integrated circuit (Application Specific Integrated Circuit, ASIC for short), or one or more integrated circuits configured to implement embodiments of the present invention, such as: one or more microprocessors (digital signal processor, abbreviated as DSPs), or one or more field programmable gate arrays (Field Programmable Gate Array, abbreviated as FPGAs).
In practical application, the processor can be arranged in the ellipsometer so that the processor is used as a part of the ellipsometer, thereby realizing upgrading and reconstruction of the ellipsometer; meanwhile, the processor can be integrated with a processor in an ellipsometer in the form of a chip. Of course, the processor may be provided in another terminal device, and the terminal device may be kept in communication with the ellipsometer.
The embodiment of the invention also provides a terminal 300 for detecting longitudinal non-uniformity of a film, as shown in fig. 5, including: a memory 301 and a processor 302; wherein the memory 301 is configured to store one or more computer software instructions, which include a program for executing the method for detecting longitudinal non-uniformity of a thin film according to the first implementation manner; the processor 302 is configured to execute one or more computer software instructions to implement the method for detecting longitudinal film non-uniformities in the above-described embodiments.
The film longitudinal non-uniformity detection terminal further comprises a transceiver 303 and a bus 304, wherein the memory 301, the processor 302 and the transceiver 303 are communicated with each other through the bus 304; the transceiver 303 may support the processor in communication with the ellipsometer 100 and the display module 500.
The memory 301 may be a storage device or a combination of a plurality of storage elements, and is configured to store program codes for executing the aspects of the present invention, and the processor 302 controls the execution. The Memory 301 may be, but is not limited to, a read-Only Memory (ROM) or other type of static storage device that can store static information and instructions, a random access Memory (random access Memory, RAM) or other type of dynamic storage device that can store information and instructions, an electrically erasable programmable read-Only Memory (Electrically Erasable Programmable Read-Only Memory, EEPROM), a compact disc (Compact Disc Read-Only Memory) or other optical disk storage, optical disk storage (including compact disc, laser disc, optical disc, digital versatile disc, blu-ray disc, etc.), magnetic disk storage media or other magnetic storage devices, or any other medium that can be used to carry or store desired program code in the form of instructions or data structures and that can be accessed by a computer.
The processor 302 may be one processor or may be a combination of multiple processing elements. For example, the processor 302 may be a central processing unit (Central Processing Unit, CPU for short), an application specific integrated circuit (Application Specific Integrated Circuit, ASIC for short), or one or more integrated circuits configured to implement embodiments of the present invention, such as: one or more microprocessors (digital signal processor, abbreviated as DSPs), or one or more field programmable gate arrays (Field Programmable Gate Array, abbreviated as FPGAs).
The transceiver 303 is used to communicate with other devices or communication networks, such as ethernet, radio Access Network (RAN), wireless local area network (Wireless Local Area Networks, WLAN), etc.
The bus 304 may be an industry standard architecture (Industry Standard Architecture, ISA) bus, an external device interconnect (Peripheral Component, PCI) bus, or an extended industry standard architecture (Extended Industry Standard Architecture, EISA) bus, among others. The bus 304 may be classified as an address bus, a data bus, a control bus, or the like. For ease of illustration, only one thick line is shown in fig. 5, but not only one bus or one type of bus.
Referring to fig. 1 and 3, an embodiment of the present invention provides a thin film longitudinal non-uniformity detection apparatus, which may perform the thin film longitudinal non-uniformity detection method in the first implementation manner, where the thin film longitudinal non-uniformity detection apparatus includes:
the receiving unit 201 is configured to obtain ellipsometric spectrum information of a sample to be measured, as shown in fig. 4, where the sample to be measured includes at least a film 402 to be measured.
A modeling unit 202 for creating an isotropic physical model according to the composition of matter of the sample to be measured, the physical model including at least a thin film model; at least one variable parameter contained in the film model is converted into at least one set of graded variable parameters.
The curve fitting unit 203 is configured to perform curve fitting on the graded variable parameters by using at least one set of film models with ellipsometry curve information of the sample to be measured as a curve fitting target, so as to obtain change curve information of the photoelectric parameters of the sample to be measured in the longitudinal direction of the sample to be measured.
And an analysis unit 204 for evaluating the longitudinal non-uniformity of the sample according to the change curve information of the photoelectric parameter of the sample in the longitudinal direction of the sample.
In practice, the receiving unit 201 receives ellipsometry curve information of a sample to be measured; as shown in fig. 4, the sample to be measured includes a roughened layer 401, a thin film to be measured 402, and a base layer 403, considering that the sample to be measured/air interface is not an ideal smooth plane; the roughened layer 401 is composed of 50% by volume of the film under test and 50% by volume of voids, and the film under test 402 may be more than one layer.
The modeling unit 202 establishes an isotropic physical model for the sample to be measured to simulate a physical model conforming to the characteristics of the sample to be measured, and the established physical model includes at least a thin film model in consideration of a thin film layer that is decisive for the photoelectric constant of the sample to be measured; the film model comprises a plurality of variable parameters, and at the same time, at least one variable parameter is converted into at least one group of gradient variable parameters due to the fact that the measured film is prone to longitudinal non-uniformity.
The curve fitting unit 203 uses the ellipsometry curve information as a fitting target, and performs curve fitting on at least one group of gradient variable parameters by using a film model to obtain the change curve information of the photoelectric parameters of the measured sample in the longitudinal direction of the measured sample.
The analysis unit 204 determines the longitudinal non-uniformity of the sample to be measured from the information of the variation curve of the photoelectric parameter of the sample to be measured in the longitudinal direction of the sample to be measured.
It is understood that the physical model includes a transparent material physical model and/or a refractive dispersion vibrator model; the graded variable parameter includes a variable parameter of linear gradient change or a variable parameter of nonlinear gradient change, and the detailed effect analysis is referred to above, and will not be repeated here.
The process of curve fitting is essentially a process of searching a minimum mean square error value, and in order to obtain the change curve information of the photoelectric parameter of the measured sample in the longitudinal direction of the measured sample faster, the convergence condition for curve fitting is set to be that the mean square error value is smaller than 80; further, a convergence condition for performing curve fitting is set to be less than 20 in mean square error value.
In order to make the obtained change curve information of the photoelectric parameter of the measured sample in the longitudinal direction of the measured sample more accurate, the optical constant and/or the dielectric constant of the measured sample may be required to satisfy the K-K relationship.
In a second implementation manner, as shown in fig. 2, a method for detecting longitudinal non-uniformity of a film is provided, including:
step S210: the ellipsometry spectrum curve of the measured sample can be measured by adopting an ellipsometry method, and the ellipsometry method has high sensitivity and high precision, is a nondestructive and non-contact detection mode and can not damage the measured sample.
Step S220: and transmitting the ellipsometry curve information of the tested sample to the film longitudinal non-uniformity detection device. The ellipsometry curve information of the measured sample characterizes the ellipsometry curve of the measured sample.
Step S230: and determining the longitudinal non-uniformity of the tested sample by using a film longitudinal non-uniformity detection device.
Compared with the prior art, the method for detecting the longitudinal non-uniformity of the film provided by the embodiment of the invention can be described in the foregoing, and is not described in detail herein.
In some embodiments, as shown in fig. 6, the ellipsometry curve for measuring the sample to be measured specifically includes:
step S211: the incidence angle of the linearly polarized light is set so that the incidence angle of the linearly polarized light comprises at least one first incidence angle and at least one second incidence angle, wherein the first incidence angle is larger than the Brewster angle of the measured sample material, and the second incidence angle is smaller than the Brewster angle of the measured sample material.
Step S212: and (3) incidence of linear polarized light to the measured sample, and detection of the amplitude ratio of the elliptical polarized p light to the s light of the measured sample and the phase difference of the elliptical polarized p light and the s light of the measured sample. Since the gradient change of the optical constant of the transparent conductive film or other films exists in the visible and near infrared bands, the wavelength range of the linearly polarized light is set to 300nm to 2400nm.
Step S213: according to the amplitude ratio of the elliptical polarized p light to the s light of the measured sample and the wavelength range of the linear polarized light, an elliptical polarized psi spectrum curve of the measured sample is obtained; and obtaining an ellipsometric delta spectrum curve of the measured sample according to the phase difference between the ellipsometric p light and the s light of the measured sample and the wavelength range of the linearly polarized light.
When the first incident angle is larger than the Brewster angle of the measured sample material and the second incident angle is smaller than the Brewster angle of the measured sample material, the measured phase difference between the ellipsometric p-light and the s-light of the measured sample is provided with a mutation, and whether a later curve fitting result is accurate or not can be determined by utilizing the mutation, so that when the first incident angle is larger than the Brewster angle of the measured sample material and the second incident angle is smaller than the Brewster angle of the measured sample material, the measured ellipsometric curve of the measured sample is favorable for later curve fitting; if the first incident angle and the second incident angle are both larger than the brewster angle of the measured sample material, or the first incident angle and the second incident angle are both smaller than the brewster angle of the measured sample material, the measured ellipsometry spectrum curves of the measured sample are not greatly different, so that the later curve fitting is not facilitated, and the problem of inaccurate curve fitting is easily caused. For example: if the brewster angle of the glass is 56.7 deg., then the test angle requires at least two angles of incidence less than 56.7 deg. and greater than 56.7 deg., respectively.
The number of the first incident angles and the number of the second incident angles can be determined according to practical situations; when the number of the first incidence angles is at least two, the first incidence angles are different, and when the number of the second incidence angles is at least two, the second incidence angles are different.
Example two
The embodiment of the invention provides a method for detecting longitudinal non-uniformity of a film, which comprises the following steps:
first, an elliptical polarization spectrometer is used to test In with a film thickness of 350nm 2 O 3 Sn (also called ITO) film, and the elliptical polarization spectrometer is a V-type automatic angle-changing spectroscopic elliptical polarization spectrometer manufactured by J.A. Woollam company of America. In with film thickness of 350nm was measured by ellipsometry 2 O 3 The Sn (also called ITO) film comprises: setting linear polarization when the V-type automatic angle-changing spectral elliptical polarization spectrometer is in a high-precision modeThe incidence angle of the light is 52.5-75 degrees, and the wavelength range of the linearly polarized light is 300-900 nm; and under the condition that the incidence angle of the linearly polarized light is 52.5-75 degrees, the linearly polarized light is used for irradiating the ITO film, so that an ellipsometric delta spectrum actual measurement curve of the ITO film shown by a thick dotted line in fig. 7 and an ellipsometric psi spectrum actual measurement curve of the ITO film shown by the thick dotted line in fig. 8 are obtained.
The second step, the ITO film is formed on the substrate layer, and the second step also comprises a rough layer formed on the ITO film far away from the substrate layer; the substrate layer is common float glass with the thickness of 6mm, the rough layer is an ITO film with the volume percentage of 50 percent and a surface loose layer with the pore with the volume percentage of 50 percent which are set by adopting an effective medium theory, and the optical constant of the rough layer is half of that of the ITO film. Based on the above, an isotropic physical model is built according to the characteristics of the substrate layer, the ITO film and the rough layer, the physical model comprises a surface model, an ITO model and a substrate model, and the surface model, the ITO model and the substrate model are built in sequence according to the modeling space sequence in the modeling process, so that the surface model, the ITO model and the substrate model are in the sequence from top to bottom in the modeling space.
The surface model is an effective medium model established according to the characteristics of the rough layer, the ITO model is established according to the characteristics of the ITO film, the matrix model is a transparent material which is established according to the characteristics of float glass and is used for the float glass, and the established matrix model is a Cauchy model. For the ITO film, the material used for the ITO film is a semiconductor material, and the established film model is a Lorentz model or a Gaussian model. Based on this, according to the transparent conductive property of the ITO film, a gaussian model is established as an ITO model, which is a model formed by precisely quantizing objects with a gaussian probability density function (the corresponding curve is a normal distribution curve), and decomposing one object into several based on the gaussian probability density function.
Third, the variable parameters in the Gaussian model include center peak position En, amplitude (i.e. peak height Amp), half-width Br, etc. The central peak position En is selected from the Gaussian model as a variable parameter, the central peak position En is converted into a variable parameter with linear gradient change, namely the central peak position En is divided into a plurality of steps between a maximum value and a minimum value in the longitudinal direction, and the more the number of steps is, the longer the fitting time is, but the better the fitting effect is; the smaller the number of steps, the shorter the fitting time but the poor fitting effect.
For example: fig. 9 shows a schematic diagram of a central peak position distribution of a linear gradient change, wherein the ordinate is the central peak position En, and the abscissa is the depth (or the longitudinal length) of a solid membrane layer corresponding to a gaussian model. As shown in fig. 9, the center peak position En is set to 10 steps of equal height that vary in the longitudinal direction (the longitudinal direction or the thickness direction of the solid film layer corresponding to the gaussian model) using a linear gradient model, and the center peak position of the linear gradient variation is obtained.
Fourthly, performing curve fitting on linear gradient center peak positions by using a Gaussian model in an inversion calculation mode, wherein the fitted MSE value is 9; in the process of curve fitting, the fitted curve is an ellipsometric delta spectrum fitting curve of the ITO film shown by a thin solid line in fig. 7 and an ellipsometric ψ spectrum fitting curve of the ITO film shown by a thin solid line in fig. 8. When fitting is successful, the obtained ellipsometry delta spectrum fitting curve of the ITO film and the obtained ellipsometry delta spectrum fitting curve of the ITO film are transformed to obtain the related information of the change curve of the refractive index and the extinction coefficient of the ITO film in the longitudinal direction of the tested sample shown in fig. 10, and the related information of the change curve of the dielectric constants of the top and the bottom of the ITO film along with photon energy shown in fig. 11 can be obtained.
In fig. 7 and 8, a to j represent incidence angles of linearly polarized light, a=52.5 °, b=57.5 °, c=62.5 °, d=55 °, e=65 °, f=60 °, g=70 °, h=67.5 °, i=72.5 °, j=75°; comparing the measured ellipsometry delta spectrum curve of the ITO film shown by the thick dotted line in fig. 7 with the fitted ellipsometry delta spectrum curve of the ITO film shown by the thin solid line, it can be found that: according to the established Gaussian model and the set variable parameters of the linear gradient change, an ellipsometry delta spectrum fitting curve of the ITO film is matched with an ellipsometry delta spectrum actual measurement curve of the ITO film, the ellipsometry delta spectrum actual measurement curve of the ITO film meets the K-K relation, and a good fitting result of fitting the central peak position of the linear gradient change by adopting the Gaussian model is shown. Comparing the measured ellipsometric ψ spectrum curve of the ITO film shown by the thick dotted line in fig. 8 with the fitted ellipsometric ψ spectrum curve of the ITO film shown by the thin solid line, it can be found that: according to the established Gaussian model and the set variable parameters of the linear gradient change, an ellipsoi spectrum fitting curve of the ITO film is matched with an ellipsoi spectrum actual measurement curve of the ITO film, the ellipsoi spectrum actual measurement curve of the ITO film meets the K-K relation, and a fitting result of fitting the central peak position of the linear gradient change by adopting the Gaussian model is good. At this time, the information of the variation curve of the refractive index and extinction coefficient of the ITO film shown in fig. 10 in the longitudinal direction of the sample to be measured can be output, or the variation curve of the dielectric constants of the top and bottom of the ITO film shown in fig. 11 along with the photon energy can be selected to be output, and the output fig. 10 and 11 can be displayed by the display module to facilitate data analysis.
Fifth, the upper refractive index shown in fig. 10 means the refractive index of the surface of the ITO thin film with respect to the rough layer (hereinafter abbreviated as the top of the ITO thin film), the lower refractive index means the refractive index of the surface of the ITO thin film with respect to the base layer (hereinafter abbreviated as the bottom of the ITO thin film), and the lower refractive index may be used to represent the internal refractive index of the ITO thin film; the upper extinction coefficient refers to the extinction coefficient at the top of the ITO film, the lower extinction coefficient refers to the extinction coefficient at the bottom of the ITO film, and the lower extinction coefficient can be used for representing the internal extinction coefficient of the ITO film. As can be seen from fig. 10: for the refractive index, the top refractive index of the ITO film is larger than the bottom (inner) refractive index of the ITO film, and the difference is unchanged with wavelength. For extinction coefficients, in the short wavelength range, the top extinction coefficient of the ITO film is the same as the bottom (internal) extinction coefficient of the ITO film; in the range of long wavelength, the top extinction coefficient of the ITO film is greater than the bottom (inner) extinction coefficient of the ITO film, so that it is possible to determine the variation of the refractive index and extinction coefficient of the ITO film along the longitudinal direction of the ITO film at the same time according to fig. 10, and to determine the variation of the oxygen content of the ITO film along the longitudinal direction of the ITO film when the refractive index and extinction coefficient of the ITO film at the same time vary along the longitudinal direction.
Upper epsilon shown in figure 11 1 The real part of the surface of the ITO film (hereinafter referred to as the top of the ITO film) with respect to the rough layer, lower ε 1 Is the real part of the surface of the ITO film opposite to the substrate layer (hereinafter referred to as the bottom surface of the ITO film); upper epsilon 2 The real part of the surface of the ITO film (hereinafter referred to as the top of the ITO film) with respect to the rough layer, lower ε 2 Is the real part of the surface of the ITO film opposite to the base layer (hereinafter referred to as the bottom part of the ITO film). As can be seen from FIG. 11, the real part ε of the top dielectric constant of ITO film 1 And imaginary part epsilon 2 Are all larger than the real part epsilon of the bottom dielectric constant of the ITO film 1 And imaginary part epsilon 2 Therefore, it can be determined from fig. 11 that the dielectric constant of the ITO film varies along the longitudinal direction of the ITO film; and when the dielectric constant of the ITO film varies along the longitudinal direction of the ITO film, it is determined that the oxygen content of the ITO film is not uniform along with the longitudinal direction of the ITO film.
Example III
In the first step, an elliptical polarization spectrometer is adopted to test a ZnO: al (also called AZO) film with the film thickness of 250nm, wherein the elliptical polarization spectrometer is a V-shaped automatic angle-changing spectroscopic elliptical polarization spectrometer manufactured by J.A. Woollam company of America. In with film thickness of 350nm was measured by ellipsometry 2 O 3 The Sn (also called ITO) film comprises: when the V-type automatic angle-changing spectral elliptical polarization spectrometer is in a high-precision mode, setting the incidence angle of linearly polarized light to be 55 degrees and 65 degrees, wherein the wavelength range of the linearly polarized light is 300-2500nm; and respectively irradiating the ITO film with linearly polarized light at incidence angles of 55 degrees and 65 degrees to obtain an ellipsometric delta spectrum actual measurement curve of the AZO film shown by a thick dotted line in fig. 12 and an ellipsometric psi spectrum actual measurement curve of the AZO film shown by a thick dotted line in fig. 13.
And secondly, forming the AZO film on the surface of the substrate layer, and simultaneously forming a rough layer on the surface of the substrate layer based on the AZO film principle, wherein the substrate layer is of 6mm thick ordinary float glass, and the rough layer is a surface loose layer of 50% by volume of AZO film and 50% by volume of pores set by adopting an effective medium theory, and the optical constant of the rough layer is half of that of the AZO film. Based on the above, an isotropic physical model is built according to the characteristics of the matrix layer, the AZO film and the rough layer, the physical model comprises a surface model, an AZO model and a matrix model, and the surface model, the ITO model and the matrix model are built in sequence according to a modeling space sequence in the modeling process, so that the surface model, the ITO model and the matrix model are in a sequence from top to bottom in the modeling space.
The surface model is an effective medium model established according to the characteristics of the rough layer, the AZO model is established according to the characteristics of the AZO film, and the matrix model is established according to the characteristics of float glass. For float glass, the transparent material is used for float glass, and the type of the established matrix model is a cauchy model. For the AZO film, the material used for the AZO film is a semiconductor material, and the established film model is a Lorentz model or a Gaussian model. Based on the above, according to the transparent conductive property of the AZO film, a gaussian model is established as an AZO model, wherein the gaussian model precisely quantifies things by using a gaussian probability density function (the corresponding curve is a normal distribution curve), and one thing is decomposed into a plurality of models formed based on the gaussian probability density function.
Third, the variable parameters in the Gaussian model include center peak position En, amplitude (i.e. peak height Amp), half-width Br, etc. The central peak position En is selected from the Gaussian model as a variable parameter, the central peak position En is converted into a variable parameter of nonlinear gradient change, namely the central peak position En is divided into a plurality of steps between a maximum value and a minimum value in the longitudinal direction, and the more the number of steps is, the longer the fitting time is, but the better the fitting effect is; the smaller the number of steps, the shorter the fitting time but the poor fitting effect.
For example: fig. 14 shows a schematic diagram of a distribution of central peak positions of nonlinear gradient changes, wherein the ordinate is central peak position En, and the abscissa is depth (longitudinal length) of a solid membrane layer corresponding to a gaussian model. As shown in fig. 14, a nonlinear gradient model is adopted to set the central peak position En as 20 gradient steps which are unevenly changed along the longitudinal direction (the longitudinal direction or the thickness direction of the solid film layer corresponding to the gaussian model), and the step trend is descending and ascending, so as to obtain the central peak position of the nonlinear gradient change.
Fourthly, performing curve fitting on the central peak position of the nonlinear gradient change by using a Gaussian model in an inversion calculation mode, wherein the fitted MSE value is 6; in the process of curve fitting, the fitted curves are an ellipsometric delta spectrum fitting curve of the AZO film shown by a thin solid line in fig. 12 and an ellipsometric ψ spectrum fitting curve of the AZO film shown by a thin solid line in fig. 13. When fitting is successful, the obtained ellipsometry delta spectrum fitting curve of the AZO film and the obtained ellipsometry delta spectrum fitting curve of the AZO film are transformed to obtain the related information of the variation curve of the refractive index and the extinction coefficient of the AZO film in the longitudinal direction of the measured sample shown in fig. 14, and the related information of the variation curve of the dielectric constants of the top and the bottom of the AZO film along with photon energy shown in fig. 15 can be obtained.
A and b in fig. 12 and 13 represent incidence angles of linearly polarized light, a=55°, and b=65°; comparing the measured ellipsometry delta spectrum curve of the AZO film shown by the thick dotted line in fig. 12 with the fitted ellipsometry delta spectrum curve of the AZO film shown by the thin solid line, it can be found that: according to the established Gaussian model and the set variable parameters of the nonlinear gradient change, an ellipsometry delta spectrum fitting curve of the AZO film is identical with an ellipsometry delta spectrum actual measurement curve of the AZO film, the ellipsometry delta spectrum actual measurement curve of the AZO film meets the K-K relation, and a good fitting result of fitting the central peak position of the nonlinear gradient change by adopting the Gaussian model is shown. Comparing the measured ellipsometric ψ spectrum curve of the AZO film shown by the thick dotted line in fig. 13 with the fitted ellipsometric ψ spectrum curve of the AZO film shown by the thin solid line can be found: according to the established Gaussian model and the set variable parameters of the nonlinear gradient change, an ellipsoi spectrum fitting curve of the AZO film is matched with an ellipsoi spectrum actual measurement curve of the AZO film, the ellipsoi spectrum actual measurement curve of the AZO film meets the K-K relation, and a fitting result of fitting the central peak position of the nonlinear gradient change by adopting the Gaussian model is good. At this time, the information of the variation curve of the refractive index and extinction coefficient of the AZO film in the longitudinal direction of the sample to be measured as shown in fig. 15 may be output, or the variation curve of the dielectric constants of the top and bottom of the AZO film with photon energy as shown in fig. 16 may be selected to output, and the output fig. 15 and 16 may be displayed by a display module to facilitate data analysis.
Fifth, the upper refractive index shown in fig. 15 means the refractive index of the surface of the AZO film with respect to the rough layer (hereinafter referred to as the top of the AZO film), the lower refractive index means the refractive index of the AZO film with respect to the surface of the base layer (hereinafter referred to as the bottom of the AZO film), and the lower refractive index may be used to represent the internal refractive index of the AZO film; the upper extinction coefficient refers to the extinction coefficient at the top of the AZO film, the lower extinction coefficient refers to the extinction coefficient at the bottom of the AZO film, and the lower extinction coefficient can be used to represent the internal extinction coefficient of the AZO film. As can be seen from fig. 15: for refractive index, the top refractive index of AZO film is larger than the bottom (inner) refractive index of AZO film, and the difference is unchanged with wavelength. As for the extinction coefficient, in the short wavelength range, the top extinction coefficient of the AZO film is the same as the bottom (internal) extinction coefficient of the AZO film; in the long wavelength range, the extinction coefficient at the top of the AZO film is greater than that at the bottom (inside) of the AZO film, and thus, it is possible to determine that the refractive index and extinction coefficient of the AZO film vary simultaneously in the longitudinal direction of the AZO film according to fig. 15, and that the oxygen content of the ITO film is not uniform in the longitudinal direction of the AZO film when the refractive index and extinction coefficient of the AZO film vary simultaneously in the longitudinal direction.
Upper epsilon shown in figure 16 1 Is the real part of the surface of the AZO film (hereinafter simply referred to as the top of the AZO film), the lower ε 1 Is the real part of the AZO film relative to the surface of the substrate layer (hereinafter abbreviated as the real part of the bottom of the AZO film; upper ε 2 The real part of the ITO film relative to the surface of the substrate layer (hereinafter simply referred to as the top of the AZO film), lower ε 2 Is the real part of the surface of the AZO film against the base layer (hereinafter simply referred to as the bottom of the AZO film). As can be seen from FIG. 16, the real part ε of the top dielectric constant of AZO film 1 And imaginary part epsilon 2 Are all larger than the real part epsilon of the bottom dielectric constant of the AZO film 1 And imaginary part epsilon 2 Therefore, it can be determined from fig. 16 that the dielectric constant of the AZO film varies along the longitudinal direction of the AZO film; and determining the AZO film when the dielectric constant of the AZO film varies along the longitudinal direction of the AZO filmThe oxygen content of (a) is not uniform along the longitudinal direction of the AZO film.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and any person skilled in the art will readily recognize that variations or substitutions are within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.

Claims (14)

1. A method for detecting longitudinal non-uniformity of a film, comprising:
acquiring ellipsometry curve information of a sample to be tested, wherein the sample to be tested at least comprises a film to be tested;
establishing an isotropic physical model according to the characteristics of the tested sample, wherein the physical model at least comprises a film model;
converting at least one variable parameter contained in the film model into at least one group of graded variable parameters;
taking ellipsometry curve information of the measured sample as a curve fitting target, and performing curve fitting on at least one group of gradient variable parameters by using the film model to obtain change curve information of photoelectric parameters of the measured sample in the longitudinal direction of the measured sample;
determining the longitudinal non-uniformity of the measured sample according to the change curve information of the photoelectric parameter of the measured sample in the longitudinal direction of the measured sample;
wherein the at least one variable parameter is converted into at least one set of graded variable parameters by expressing a gradient function of the at least one variable parameter along the depth of the membrane layer.
2. The method for detecting longitudinal non-uniformity of a film according to claim 1, wherein said convergence condition for performing curve fitting is a mean square error value of less than 80.
3. The method for detecting longitudinal non-uniformity of a film according to claim 1, wherein said convergence condition for performing curve fitting is a mean square error value of less than 20.
4. The method for detecting longitudinal non-uniformity of a thin film according to claim 1, wherein the photoelectric parameters of the sample to be detected include an optical constant satisfying the cremer-kroney relationship and/or a dielectric constant satisfying the cremer-kroney relationship.
5. The method of claim 1, wherein the physical model further comprises a matrix model and a surface model, the film model being located between the matrix model and the surface model, the matrix model being a cauchy model, the film model being a lorentz model or a gaussian model, the surface model being an effective medium model.
6. The method of any one of claims 1 to 5, wherein converting at least one variable parameter contained in the film model into at least one set of graded variable parameters comprises:
according to the order of influencing the weight from high to low on the fitting result, one or two variable parameters in the film model are selected for gradient conversion;
And/or the number of the groups of groups,
the graded variable parameter comprises a variable parameter of linear gradient change or a variable parameter of nonlinear gradient change.
7. A thin film longitudinal non-uniformity detection device, comprising:
the receiving unit is used for acquiring ellipsometric spectrum curve information of a sample to be detected, wherein the sample to be detected at least comprises a film to be detected;
a modeling unit, configured to establish an isotropic physical model according to the characteristics of the sample to be measured, where the physical model includes at least a thin film model; converting at least one variable parameter contained in the film model into at least one group of graded variable parameters; wherein the at least one variable parameter is converted into at least one set of graded variable parameters by expressing a gradient function of the at least one variable parameter along the depth of the membrane layer;
the curve fitting unit is used for performing curve fitting on at least one group of gradient variable parameters by using the film model by taking ellipsometry curve information of the tested sample as a curve fitting target to obtain change curve information of photoelectric parameters of the tested sample in the longitudinal direction of the tested sample;
and the analysis unit is used for evaluating the longitudinal non-uniformity of the tested sample according to the change curve information of the photoelectric parameter of the tested sample in the longitudinal direction of the tested sample.
8. The apparatus for detecting longitudinal non-uniformity of a film according to claim 7, wherein said convergence condition for performing curve fitting is that a root mean square error value is less than 80;
and/or the number of the groups of groups,
the photoelectric parameters of the tested sample comprise optical constants meeting the Kramer-Croney relation and/or dielectric constants meeting the Kramer-Croney relation;
and/or the number of the groups of groups,
the physical model further comprises a matrix model and a surface model, the film model is positioned between the matrix model and the surface model, the matrix model is a cauchy model, the film model is a lorentz model or a gaussian model, and the surface model is an effective medium model;
and/or the number of the groups of groups,
the converting the at least one variable parameter contained in the film model into at least one set of graded variable parameters comprises:
according to the order of influencing the weight from high to low on the fitting result, one or two variable parameters in the film model are selected for gradient conversion;
and/or the number of the groups of groups,
the graded variable parameter comprises a variable parameter of linear gradient change or a variable parameter of nonlinear gradient change.
9. The apparatus for detecting longitudinal non-uniformity of a film according to claim 7, wherein said convergence condition for performing curve fitting is that the root mean square error value is less than 20.
10. A method for detecting longitudinal non-uniformity of a film, comprising:
measuring an ellipsometric spectrum curve of a measured sample;
transmitting ellipsometry curve information of a sample to be measured to the thin film longitudinal non-uniformity detection device according to any one of claims 7 to 9; the ellipsometry curve information of the sample to be tested represents an ellipsometry curve of the sample to be tested;
and determining the longitudinal non-uniformity of the tested sample by using the film longitudinal non-uniformity detection device.
11. The method for detecting longitudinal non-uniformity of a film according to claim 10, wherein said measuring an ellipsometry curve of a sample under test comprises:
setting the incidence angle of the linearly polarized light, wherein the incidence angle of the linearly polarized light comprises at least one first incidence angle and at least one second incidence angle, each first incidence angle is larger than the brewster angle of the tested sample material, and each second incidence angle is smaller than the brewster angle of the tested sample material;
at least one first incidence angle and at least one second incidence angle, respectively, linearly polarized light is incident to the measured sample, and the amplitude ratio of the elliptical polarized p light to the s light of the measured sample and the phase difference of the elliptical polarized p light and the s light of the measured sample are detected;
Obtaining an ellipsometric amplitude ratio spectrum curve of the measured sample according to the amplitude ratio of the ellipsometric p light to the s light of the measured sample and the wavelength range of the linearly polarized light;
and obtaining an ellipsometric phase difference spectrum curve of the measured sample according to the phase difference between the ellipsometric p-light and the s-light of the measured sample and the wavelength range of the linearly polarized light.
12. The method for detecting longitudinal non-uniformity of a film according to claim 11, wherein said linearly polarized light has a wavelength in the range of 300nm to 2400nm.
13. A detection system, comprising:
ellipsometry apparatus;
the thin film longitudinal non-uniformity detection apparatus according to any one of claims 7 to 9, wherein a receiver included in the thin film longitudinal non-uniformity detection apparatus is connected to the ellipsometer.
14. A film longitudinal non-uniformity detection terminal, comprising:
a memory for storing one or more computer software instructions comprising a program for performing the method for detecting longitudinal non-uniformities in a film of any one of claims 1-6;
a processor for executing one or more computer software instructions to implement the method for detecting longitudinal non-uniformities in a film of any one of claims 1-6.
CN201910273286.3A 2019-04-04 2019-04-04 Method, device, terminal and system for detecting longitudinal non-uniformity of film Active CN111781148B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910273286.3A CN111781148B (en) 2019-04-04 2019-04-04 Method, device, terminal and system for detecting longitudinal non-uniformity of film

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910273286.3A CN111781148B (en) 2019-04-04 2019-04-04 Method, device, terminal and system for detecting longitudinal non-uniformity of film

Publications (2)

Publication Number Publication Date
CN111781148A CN111781148A (en) 2020-10-16
CN111781148B true CN111781148B (en) 2024-03-12

Family

ID=72755672

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910273286.3A Active CN111781148B (en) 2019-04-04 2019-04-04 Method, device, terminal and system for detecting longitudinal non-uniformity of film

Country Status (1)

Country Link
CN (1) CN111781148B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114324249B (en) * 2021-11-29 2023-08-11 天津津航技术物理研究所 Characterization method of electrical characteristics of transparent conductive film based on full spectrum method

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6057928A (en) * 1999-06-15 2000-05-02 Rensselaer Polytechnic Institute Free-space time-domain method for measuring thin film dielectric properties
JP2006349648A (en) * 2005-06-20 2006-12-28 Toyota Industries Corp Analysis method of organic material used for organic electroluminescence element, analysis method of composite film and analysis method of multilayer film using spectral ellipsometer
DE102007043937A1 (en) * 2006-09-13 2008-03-27 Innovent E.V. Optically transparent dielectric coating thickness and refractive index determining method, involves determining theoretical reflectance minimum through numerical iteration, and finding thickness of coating to be determined
KR20120134493A (en) * 2011-06-02 2012-12-12 단국대학교 산학협력단 Method of measuring band gap and physical defect of target thin film using spectroscpic ellipsometry
CN102980748A (en) * 2012-12-06 2013-03-20 中国科学院长春光学精密机械与物理研究所 Method for measuring optical constants of thin film with non-uniform refractive index
CN103115927A (en) * 2013-02-04 2013-05-22 中国人民解放军国防科学技术大学 Nondestructive testing method for optical glass polishing sub-surface damages
CN103884494A (en) * 2014-03-21 2014-06-25 浙江大学 Optical parameter detecting method for Si-based buffer layer coated glass
CN105136679A (en) * 2015-09-02 2015-12-09 北京航玻新材料技术有限公司 Optical material surface quality evaluation method based on ellipsometer and application of optical material surface quality evaluation method
CN105403581A (en) * 2015-12-08 2016-03-16 四川大学 Ray measurement method for film thickness distribution and uniformity

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10955359B2 (en) * 2013-11-12 2021-03-23 International Business Machines Corporation Method for quantification of process non uniformity using model-based metrology

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6057928A (en) * 1999-06-15 2000-05-02 Rensselaer Polytechnic Institute Free-space time-domain method for measuring thin film dielectric properties
JP2006349648A (en) * 2005-06-20 2006-12-28 Toyota Industries Corp Analysis method of organic material used for organic electroluminescence element, analysis method of composite film and analysis method of multilayer film using spectral ellipsometer
DE102007043937A1 (en) * 2006-09-13 2008-03-27 Innovent E.V. Optically transparent dielectric coating thickness and refractive index determining method, involves determining theoretical reflectance minimum through numerical iteration, and finding thickness of coating to be determined
KR20120134493A (en) * 2011-06-02 2012-12-12 단국대학교 산학협력단 Method of measuring band gap and physical defect of target thin film using spectroscpic ellipsometry
CN102980748A (en) * 2012-12-06 2013-03-20 中国科学院长春光学精密机械与物理研究所 Method for measuring optical constants of thin film with non-uniform refractive index
CN103115927A (en) * 2013-02-04 2013-05-22 中国人民解放军国防科学技术大学 Nondestructive testing method for optical glass polishing sub-surface damages
CN103884494A (en) * 2014-03-21 2014-06-25 浙江大学 Optical parameter detecting method for Si-based buffer layer coated glass
CN105136679A (en) * 2015-09-02 2015-12-09 北京航玻新材料技术有限公司 Optical material surface quality evaluation method based on ellipsometer and application of optical material surface quality evaluation method
CN105403581A (en) * 2015-12-08 2016-03-16 四川大学 Ray measurement method for film thickness distribution and uniformity

Non-Patent Citations (5)

* Cited by examiner, † Cited by third party
Title
A spectroscopic ellipsometry study on the variation of the optical constants of tin-doped indium oxide thin films during crystallization;Yeon Sik Jung;《Solid State Communications》;第129卷(第8期);第491-495页 *
Optical Constants of Electrodeposited Mixed Molybdenum-Tungsten Oxide Films Determined by Variable-Angle Spectroscopic Ellipsometry;R. Alan May等;《The Journal of Physical Chemistry C》;第111卷(第49期);第18251-18257页 *
Yeon Sik Jung.A spectroscopic ellipsometry study on the variation of the optical constants of tin-doped indium oxide thin films during crystallization.《Solid State Communications》.2004,第129卷(第8期),第491-495页. *
光学镀膜宽带膜厚监控系统;刘晓元, 黄云, 周宁平, 龙兴武;国防科技大学学报;20010225(01);全文 *
溅射工艺对 D/M/D 结构中 SiNx介质膜光学常数的影响;孙瑶等;《航空材料学报》;第35卷(第4期);第28-33页 *

Also Published As

Publication number Publication date
CN111781148A (en) 2020-10-16

Similar Documents

Publication Publication Date Title
Coulter et al. Assessing Tauc plot slope quantification: ZnO thin films as a model system
Gao et al. Refractive index determination of SiO2 layer in the UV/Vis/NIR range: spectrophotometric reverse engineering on single and bi-layer designs
CN103323403B (en) Optical parameter detection method of low-radiation coated glass
US20180151368A1 (en) Engineering the optical properties of an integrated computational element by ion implantation
CN110514599B (en) Optical parameter detection method for fluorine-doped tin oxide coated glass
CN111122459B (en) Method and device for correcting depolarization effect caused by uneven thickness in spectroscopic ellipsometry
KR100644390B1 (en) Method of measuring a thickness of a thin film for a semiconductor device and an apparatus for performing the method
CN112881341B (en) Method for determining optical constant and thickness of organic film
JP2006093633A (en) Method for specifying film forming condition, film forming method, and manufacturing method for film body
CN111781148B (en) Method, device, terminal and system for detecting longitudinal non-uniformity of film
CN103884657B (en) A kind of method of measuring online low radiation energy-saving coated glass radiance
CN116879181A (en) Method for measuring optical characteristics and geometric characteristics of film material
CN114324249B (en) Characterization method of electrical characteristics of transparent conductive film based on full spectrum method
CN113281266A (en) Spectral combined analysis method of film substance and application thereof
Nečas et al. The reflectance of non-uniform thin films
WO2009143921A1 (en) A method for determining an optical property of an optical layer
Oiwake et al. Fully automated spectroscopic ellipsometry analyses: Application to MoOx thin films
Zhaoxian et al. Generalized simulated annealing algorithm applied in the ellipsometric inversion problem
KR102504761B1 (en) Method for Measuring Properties of Thin Film
Murata et al. Characterization of μc-Si: H/a-Si: H tandem solar cell structures by spectroscopic ellipsometry
CN113267454A (en) Thin film quality detection method, thin film quality detection device, electronic device, and storage medium
Ohlídal et al. Ellipsometric characterization of inhomogeneous thin films with complicated thickness non-uniformity: application to inhomogeneous polymer-like thin films
CN109001122B (en) Optical constant measuring device and method for gradient or graded index film
Junda et al. A Versatile Optical Model Applied to CdTe and CdSe 1–y Te y Alloys: Sensitivity to Film Composition and Relative Defect Density
JP3959469B2 (en) Method for measuring refractive index and thickness of film, measurement program, and computer-readable recording medium

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