Processing device, system, method and program

Abstract

According to the present invention, there are provided a processing device, system, method and program capable of calculating the structure factor of a thin film formed on a substrate. [Solution] Processing device 100 mainly comprises measurement data acquisition unit 110, total scattering data calculation unit 120, and structure factor calculation unit 130. Processing device 100 is configured to be able to calculate the structure factor of a film formed on a substrate. Total scattering data calculation unit 120 acquires first total scattering data and second total scattering data from measurement data acquisition unit 110, and calculates total scattering data I for only the film portion based on these. TF Calculate the total scattering data for the film only. TF is the second total scattering data I sub and the absorption factor A of the substrate sub The product of this and the first total scattering data I sp It can be calculated by subtracting from

Description

[Technical Field]

[0001] The present invention relates to a processing device, a system, a method and a program capable of calculating a structure factor. [Background technology]

[0002] To properly understand the functions of materials, information about their three-dimensional structure is essential. Since many conventional materials are crystalline materials with regularity, their crystal structure was determined using X-ray analysis, which is capable of analyzing regular materials, and information about their three-dimensional structure was obtained from this. However, in recent years, in fields such as batteries and electronics, amorphous materials with actively reduced regularity have come to be used in order to maximize the desired functions and physical properties.

[0003] In recent years, Pair Distribution Function (PDF) analysis has been studied as a method for analyzing amorphous materials using X-rays. In PDF analysis, the structure factor of a sample is calculated from data obtained by total scattering measurement. However, to prevent this calculation method from becoming complicated, the shape of the sample that can be measured has been limited. For example, in the case of a thin film sample formed on a substrate, one possible method is to peel the film from the substrate and turn it into a measurable powder. However, this method raises concerns that the structure of the sample may change due to physical effects during the peeling and powdering process. Therefore, a method that can analyze thin film samples in their original state as they are formed on the substrate is needed.

[0004] A method for measuring thin film samples has been proposed in the past. By irradiating X-rays obliquely onto the thin film sample, the penetration depth of the X-rays into the thin film sample is reduced, and total scattering data of the X-rays from the thin film sample is obtained, thereby obtaining the scattering intensity of the thin film sample (Non-Patent Document 1). [Prior art documents] [Non-patent literature]

[0005] [Non-Patent Document 1] A.-C. Dippel, M. Roelsgaard, U. Boettger, T. Schneller, O. Gutowski, U. Ruett, IUCrJ. 6 (2019) 290-298. Summary of the Invention [Problem to be solved by the invention]

[0006] However, the total scattering data obtained by irradiating a thin film sample on a substrate with X-rays includes total scattering data from both the substrate and the thin film sample. Therefore, in order to obtain total scattering data for only the thin film sample formed on a substrate, it is necessary to eliminate the influence of the substrate from the obtained total scattering data by some method. However, the aforementioned Non-Patent Document 1 does not disclose such a method.

[0007] The present invention has been made in view of the above problems, and has an object to provide a processing device, system, method, and program that are capable of calculating the structure factor of a thin film formed on a substrate. [Means for solving the problem]

[0008] (1) In order to achieve the above object, a processing apparatus according to the present invention is a processing apparatus for calculating a structure factor of a film portion formed on a substrate, the processing apparatus comprising: a measurement data acquisition unit that acquires first total scattering data obtained by measuring a first sample including the substrate and the film under measurement conditions where X-rays are obliquely incident, and second total scattering data obtained by measuring a second sample including the first sample other than the film under the same measurement conditions; a total scattering data calculation unit that calculates total scattering data of the film portion based on the first total scattering data and the second total scattering data; a structure factor calculation unit that calculates a structure factor of the film portion based on the total scattering data of the film portion; Equipped with.

[0009] (2) It is preferable that the total scattering data calculation unit calculates the total scattering data of the film portion by subtracting the product of the second total scattering data and an absorption factor of the substrate from the first total scattering data.

[0010] (3) It is preferable that the total scattering data calculation unit calculates the absorption factor of the substrate based on the X-ray incident angle, diffraction angle, film thickness of the film portion, absorption coefficient of the film portion, and / or refractive index of the film portion.

[0011] (4) The measurement conditions include information about the angle of incidence of X-rays, and the angle of incidence of X-rays is preferably equal to or less than twice the critical angle of total reflection.

[0012] (5) The system according to the present invention comprises: an X-ray diffraction apparatus comprising: an X-ray generator that generates X-rays; an X-ray detector that detects the X-rays; a sample stage on which a sample is placed; and a goniometer that controls the angle between the X-rays generated by the X-ray generator and the surface of the sample, and the angle between the X-rays received by the X-ray detector and the surface of the sample; the processing device, The X-ray diffraction instrument generates the first total scattering data and the second total scattering data using the X-ray generator, the X-ray detector, and the goniometer.

[0013] (6) The system according to the present invention preferably further comprises a measurement condition determination unit that determines the measurement conditions, the measurement conditions having information regarding the angle of incidence of X-rays, and the measurement condition determination unit determines the angle of incidence of X-rays with respect to the first sample and the second sample based on the film thickness of the film portion, the absorption coefficient of the film portion, and / or the critical angle of total reflection between the first sample and the X-rays.

[0014] (7) The system of the present invention may further include a sample information acquisition unit that determines the film thickness and density of the film portion or the total reflection critical angle of the film portion by X-ray reflectivity measurement based on data obtained using the X-ray diffraction device.

[0015] (8) The system according to the present invention may further include a correlation calculation unit that determines the correlation of atoms included in the film portion based on the structural factor of the film portion.

[0016] (9) A program according to the present invention is capable of calculating a structural factor of a film portion formed on a substrate, and is executed by a computer, the program comprising: acquiring first total scattering data obtained by measuring a first sample including the substrate and the film portion under measurement conditions in which X-rays are obliquely incident; acquiring second total scattering data obtained by measuring the second sample including the portion of the first sample other than the film portion under the measurement conditions; calculating total scattering data of the film portion based on the first total scattering data and the second total scattering data; calculating a structure factor of the film portion based on the total scattering data of the film portion; Equipped with.

[0017] (10) A method according to the present invention is a method capable of calculating a structure factor of a film portion formed on a substrate, the method comprising: acquiring first total scattering data obtained by measuring a first sample including the substrate and the film portion under measurement conditions in which X-rays are obliquely incident; acquiring second total scattering data obtained by measuring the second sample including the portion of the first sample other than the film portion under the measurement conditions; calculating total scattering data of the film portion based on the first total scattering data and the second total scattering data; calculating a structure factor of the film portion based on the total scattering data of the film portion; Equipped with. [Effects of the Invention]

[0018] According to the present invention, it is possible to provide a processing device, system, method and program capable of calculating the structure factor of a thin film formed on a substrate. [Brief explanation of the drawings]

[0019] [Figure 1] 1 is a block diagram that schematically illustrates a processing device 100 according to an embodiment of the present invention. [Figure 2] FIG. 1 is a diagram schematically illustrating the relationship between X-rays and a sample. [Figure 3] 10 is a diagram showing the relationship between the incident angle θin of an X-ray onto a sample and the incident angle θR onto a film portion. FIG. [Figure 4] 1 is a block diagram that schematically illustrates a system 10 according to one embodiment of the present invention. [Figure 5] 4 is a flowchart illustrating a measurement process according to an embodiment of the present invention. [Figure 6] 1 is a flowchart illustrating a sample positioning process according to an embodiment of the present invention. [Figure 7] 1 is a flowchart illustrating a total scatter data acquisition process according to one embodiment of the present invention. [Figure 8] FIG. 1 shows the results of measuring X-ray reflectivity by X-ray reflectometry using MoKα wavelength. [Figure 9] FIG. 1 is a diagram showing the relationship between the diffraction angle 2θ and the absorption factor A(θ) of the substrate. [Figure 10] FIG. 10 shows total scattering data of a sample in which an ITO film is formed on a glass substrate, total scattering data of the glass substrate, and data obtained by extracting total scattering data of only the film portion from these total scattering data. [Figure 11] FIG. 1 shows the scattering intensity of a sample normalized to the atomic scattering factor. [Figure 12] FIG. 10 is a diagram showing structural factors of a membrane portion. DETAILED DESCRIPTION OF THE INVENTION

[0020] Next, an embodiment of the present invention will be described with reference to the drawings. To facilitate understanding of the description, the same reference numerals are used to designate the same components in the drawings, and duplicated descriptions will be omitted.

[0021] [Embodiment] Referring to Fig. 1, a processing device 100 according to one embodiment of the present invention will be described. The processing device 100 is a computer having components such as a CPU (Central Processing Unit), ROM (Read Only Memory), RAM (Random Access Memory), an interface, and memory connected to a bus L, and is mainly equipped with a measurement data acquisition unit 110, a total scattering data calculation unit 120, and a structure factor calculation unit 130. The measurement data acquisition unit 110, the total scattering data calculation unit 120, and the structure factor calculation unit 130 are realized by the aforementioned components of the computer. The processing device 100 is configured to be able to calculate the structure factor of a film formed on a substrate.

[0022] The measurement data acquisition unit 110, the total scattering data calculation unit 120, and the structure factor calculation unit 130 are configured to be able to send and receive information via a control bus L.

[0023] The processing device 100 can be connected to a measurement device such as an X-ray diffraction device 300 via a control device 200, which will be described later.

[0024] An input device 510 and a display device 520 are connected to the CPU of the processing device 100 via an interface. The input device 510 is, for example, a keyboard or a mouse, and performs input to the processing device 100. The display device 520 is, for example, a display, and displays total scattering data, measurement conditions, structure factors, PDFs, etc.

[0025] The measurement data acquisition unit 110 acquires total scattering data of the sample from outside the processing device 100. The total scattering data of the sample is measured by the X-ray diffraction device 300.

[0026] In this embodiment, the samples include a first sample having a thin film (hereinafter referred to as a film portion) formed on the surface of a substrate, and a second sample having only the substrate. That is, the first sample includes a substrate made of, for example, glass, and a film portion formed on the surface of the substrate.

[0027] Examples of samples include samples consisting of one substrate and samples consisting of two substrates. In a sample consisting of one substrate, a film portion is formed on one portion of the substrate, and only the substrate appears on the other portion of the substrate. A sample consisting of two substrates includes a first substrate on which a film portion is formed and a second substrate consisting of only the substrate. When the sample consists of one substrate, the portion on which the film portion is formed (first sample) and the portion consisting of only the substrate (second sample) are measured to obtain two types of total scattering data. When the sample consists of two substrates, the first substrate on which the film portion is formed (first sample) and the second substrate consisting of only the substrate (second sample) are measured to obtain two types of total scattering data. In this specification, the total scattering data of the first sample is referred to as first total scattering data, and the total scattering data of the second sample is referred to as second total scattering data, and these are collectively referred to as the total scattering data of the sample.

[0028] The total scattering data of a sample is obtained by a measurement technique in which X-rays are incident on the sample obliquely. In this measurement technique, the incident angle θ of the X-rays on the sample is in The angle is fixed at or below a predetermined angle, and X-rays are obliquely incident on the sample. Then, the receiving optical system is operated on an arc centered on the sample, and the scattering intensity of the X-rays emitted from the sample is measured. The collection of multiple scattering intensities obtained in this way is called total scattering data. The scattering intensity includes the position of the measurement point (the diffraction angle 2θ formed by the receiving optical system and the sample surface) and the intensity of the X-rays measured at that position, and the total scattering data is a collection of scattering intensity values ​​at multiple measurement points. The predetermined angle is preferably slightly larger than the critical angle of total reflection of the film part, and is determined depending on the characteristics of the film part and the X-rays. Specific values ​​of the predetermined angle are, for example, preferably 1° or less, more preferably 0.1° to 0.5°, and even more preferably 0.1° to 0.3°. The incident angle θ of the X-rays in By fixing the angle at this angle, the X-rays are incident on the first sample and then refracted at the angle θ R and the light is refracted at an exit angle θ (≒ 2θ-θ R ) and the X-rays are incident on the surface of the first sample, that is, the penetration depth of the X-rays (penetration depth l p) can be shortened (see Figure 2). This makes it possible to reduce the influence of the substrate in the first total scattering data obtained by measurement. More specifically, when measuring the first sample, the scattering intensity caused by the substrate can be reduced and the scattering intensity caused by the film portion can be relatively increased in the first total scattering data, thereby obtaining highly accurate measurement data with less scattering intensity caused by the substrate.

[0029] The second total scattering data and the first total scattering data are preferably measured under the same measurement conditions. The same measurement conditions here refer to the same system, i.e., the same processing device and X-ray diffraction device, and the same incident angle θ in The wavelength of the X-rays generated and the sensitivity of the X-rays to light are subject to slight changes due to deterioration of the processing device and the X-ray diffraction device. Therefore, even if the same model number of the device is used, the measurement results may differ slightly. Therefore, the second total scattering data and the first total scattering data are measured at the same incident angle θ using the same processing device and X-ray diffraction device. in By performing measurements using this method, it is possible to eliminate the effects of equipment degradation and to perform measurements while suppressing the effects of errors using the same X-ray penetration depth. Furthermore, when measuring multiple film portions formed on the same substrate, it is possible to use one piece of second total scattering data measured at one location for each of multiple pieces of first total scattering data obtained by measuring multiple film portions.

[0030] The total scattering data calculation unit 120 acquires the first total scattering data and the second total scattering data from the measurement data acquisition unit 110, and calculates the total scattering data I of only the film portion based on these. TF Calculate the total scattering data for the film only. TF is, for example, expressed as the second total scattering data I sub and the absorption factor A of the substrate sub The product of this and the first total scattering data I sp The absorption factor of the substrate, A, is calculated by subtracting sub This will be discussed later.

[0031]

number

[0032] Another example of a method for calculating the total scattering data of the film portion is shown in equation (2).

number

[0033] Absorption factor A of the substrate sub is a value indicating the magnitude of the scattering intensity from the substrate taking into account attenuation at the film portion. Here, in the case of a substrate provided with a film portion, the scattering intensity from the substrate includes the following components: 1. Components that are incident on the membrane and transmitted through the membrane 2. Components from 1 above that reach the substrate and are absorbed by the substrate 3. The scattered X-rays generated in the process of step 2 above that are absorbed by the substrate 4. The scattered X-rays generated in the process 2 above that penetrate the membrane The components 2 and 3 above can be obtained by measuring the scattering intensity of the substrate only (second sample). Therefore, the absorption factor A of the substrate used in equation (2) can be calculated as follows: sub When calculating the absorption factor A of the substrate, the components 1 and 4 above are taken into account. sub is the ratio of the scattering intensity from the substrate with the film portion to the scattering intensity from the substrate alone. In this case, the absorption factor A of the substrate sub The value of is 1 if there is no film and 0 if the film is infinitely thick. subThe calculation method is shown in equation (3). Referring to equation (3), the absorption factor A of the substrate sub is the optical path length of the X-rays that pass through the film, reach the substrate, and then pass through the film and exit the sample, multiplied by the absorption coefficient μ TF The absorption coefficient of the film part μ TF is calculated based on the transmittance of the film obtained using the Beer-Lambert law. Referring to Figure 2, the optical path length of the X-rays that pass through the film to reach the substrate and then pass through the film to exit the sample is calculated as follows: TF , the incident angle θ to the film portion R , calculated using the diffraction angle 2θ.

[0034]

number

[0035] Here, the incident angle θ R << When the diffraction angle is 2θ, for example, when the X-rays are incident on the sample very shallowly, the optical path from when the X-rays are scattered to when they are emitted from the sample is extremely short. Therefore, the second term of equation (3), (1 / sin(2θ-θ)), which corresponds to the length of this optical path, R )) is negligibly small. Therefore, an equation with the second term deleted may be used. Here, as will be described later with reference to FIG. 9, the absorption factor A sub is an approximately constant value. Therefore, even if we use an equation that ignores the second term, there is almost no effect on the conclusion.

[0036] Incident angle θ to the film R is the incident angle θ of the X-rays on the sample in and the complex refractive index of the material for X-rays, n * The complex refractive index of a material for X-rays, n * is shown in equation (4), and the incident angle θ R is shown in equation (5).

[0037]

number

[0038]

number

[0039] The refractive index of a material for X-rays is the complex refractive index n * is expressed as the real part of the angle θ, which is slightly smaller than 1. R When X-rays are incident on a sample at the following angle, the complex refractive index n * is an imaginary number, and the real part is the incident angle θ R The incident angle of the X-rays on the sample at this time is called the critical angle of total reflection θ c The critical angle of total reflection is θ c is expressed by equation (6). As shown in equation (6), the critical angle of total reflection θ c and the complex refractive index n * The real parts of are commutative.

[0040]

number

[0041] Figure 3 shows the incident angle θ of the X-rays on the sample when the critical angle of total reflection is 0.098°. in and the incident angle θ R The relationship between the critical angle of total reflection and the c When X-rays are incident on the sample at an angle slightly larger than the incident angle θ R is almost 0. By using this phenomenon, the critical angle of total reflection θ c By irradiating the sample with X-rays at an angle slightly larger than the critical angle θ, the optical path length of the X-rays in the film can be lengthened, resulting in a greater scattering intensity from the film. c If the incident angle of the X-rays to the sample is more than twice the angle of in and the incident angle θ R This shows that the incident angle of the X-rays on the sample, θ in is the critical angle of total reflection θ c It is preferable that the temperature is not more than twice the temperature.

[0042] Incident angle θ of X-rays on the sample in can be set to a value that allows X-rays to be sufficiently absorbed by the film portion. This value can be calculated, for example, by the penetration depth l of X-rays into the film portion shown in Equation (7). p The penetration depth l calculated by Equation (7) is determined based on p indicates the thickness of the film at which the intensity of the X-rays that enter and exit the film is attenuated to 1 / e. in For example, the thickness of the membrane t TF and penetration depth l p For example, the thickness of the membrane t TF is the penetration depth l p The incident angle θ of the X-rays on the sample is set to a positive real number multiple (for example, 1, 2, or 3) or more. in is determined. This positive real number multiplication factor is preferably a value of 1 or more so that the X-rays are sufficiently absorbed by the film portion. By using a constant multiplication factor such as a positive real number multiplication factor, the incident angle θ in Here, the penetration depth of the X-ray into the film, l p is the absorption coefficient of the film μ TF (Equation (8)) and the critical angle of total reflection θ c Therefore, the incident angle θ of the X-rays on the sample in is the thickness of the membrane t TF , the absorption coefficient μ of the membrane TF , and the critical angle of total reflection θ c As shown in equation (8), the complex refractive index n * and the absorption coefficient μ TF is a commutative relation.

[0043]

number

[0044]

number

[0045] The structure factor calculation unit 130 calculates the structure factor of the film using the total scattering data of the film calculated by the above method. A known method can be used to convert the total scattering data into a scattering vector. For example, the structure factor calculation unit 130 calculates the structure factor of the film by performing background correction, absorption correction, polarization correction, atomic scattering factor, and normalization by Compton scattering on the total scattering data of the film. The calculated structure factor of the film may be displayed in the form of a structure factor, or may be displayed in the form of a PDF after performing an inverse Fourier transform.

[0046] The structure factor is calculated by equation (9).

number

[0047] As described above, the processing apparatus 100 according to this embodiment can extract the total scattering intensity of only the film portion formed on the substrate from the total scattering data, and can accurately calculate only the structure factor of the film portion.

[0048] [Overall system] The processing device 100 of the present invention can be included in, for example, a computing system 10. Fig. 4 is a conceptual diagram showing an example of the configuration of the computing system 10. The computing system 10 will be described with reference to Fig. 4. The computing system 10 mainly includes the processing device 100, a control device 200, and an X-ray diffraction device 300.

[0049] [Control device] The control device 200 is, for example, a computer having a CPU, ROM, RAM, interface, display, and memory connected to a bus L, and includes a control unit 210, an apparatus information storage unit 220, a measurement condition determination unit 230, a measurement data storage unit 240, a sample information acquisition unit 250, and a display unit 260. The control unit 210, the apparatus information storage unit 220, the measurement condition determination unit 230, the measurement data storage unit 240, the sample information acquisition unit 250, and the display unit 260 are realized by the aforementioned components of the computer. The control device 200 is connected to the X-ray diffraction instrument 300 and controls the X-ray diffraction instrument 300 and processes and stores acquired data. The control device 200 is also connected to an input device 610 and a display device 620 via an appropriate interface. These input device 610 and display device 620 are different from those connected to the processing device 100.

[0050] The control unit 210 controls the operation of the X-ray diffraction instrument 300 , that is, the operation of the device information storage unit 220 , the measurement condition determination unit 230 , the measurement data storage unit 240 , the sample information acquisition unit 250 , and the display unit 260 .

[0051] The device information storage unit 220 stores device information acquired from the X-ray diffraction device 300. The device information includes information about the X-ray diffraction device 300, such as the model number of the X-ray diffraction device 300, the type of X-ray source, the wavelength of the X-rays, and background caused by the X-ray diffraction device 300, as well as information specific to the X-ray diffraction device 300 itself. In addition, the device information may include all of the measurement conditions determined by the measurement condition determination unit 230 (described below), the shape, refractive index, density, type of constituent elements, composition, film thickness, total reflection critical angle, and absorption coefficient of the sample, or any of these information necessary for obtaining measurement data using the X-ray diffraction device 300.

[0052] The measurement condition determination unit 230 determines the measurement conditions to be applied to the X-ray diffraction device 300 during measurement. These measurement conditions include conditions related to the irradiation-side optical system, such as the angle of incidence of the X-rays on the sample and the width of the entrance-side slit, and conditions related to the reception-side optical system, such as the scan axis, scan range, step, speed, and reception-side slit conditions of the reception-side optical system. As described above, the measurement condition determination unit 230 determines the thickness t of the film portion. TF , the absorption coefficient μ of the membrane TF , total internal reflection critical angle θ c The angle of incidence of the X-rays can be determined based on the above.

[0053] The measurement data storage unit 240 stores the measurement data acquired from the X-ray diffraction device 300. The measurement data may include, for example, total scattering data and data obtained by measurement using X-ray reflectivity measurement. Furthermore, the measurement data may also include information similar to that stored in the device information storage unit 220.

[0054] The sample information acquisition unit 250 uses the X-ray diffraction device 300 to perform X-ray reflectivity measurement and determine the thickness, density, and total reflection critical angle of the film portion. Conventional methods can be used to determine the thickness, density, and total reflection critical angle of the film portion using X-ray reflectivity measurement. The X-ray diffraction device 300 used to perform X-ray reflectivity measurement may be the same as or different from the device used to acquire total scattering data. Table 1 shows the configuration of the device used to determine the total reflection critical angle in the X-ray reflectivity measurement used in this embodiment, and Table 2 shows the measurement conditions. [Table 1] [Table 2]

[0055] The display unit 260 displays the measurement data on the display device 520. This allows the user to check the measurement data. The user can also give instructions and designations to the control device 200 based on the measurement data. Furthermore, the display unit 260 can be connected to the processing device 100 and display structure factors and PDFs.

[0056] [X-ray diffractometer] The X-ray diffraction apparatus 300 mainly comprises an X-ray generation unit 310 that generates X-rays from an X-ray focus, i.e., an X-ray source, an incident-side optical unit 320, a goniometer 330, a sample stage 340 on which a sample is placed, an exit-side optical unit 350, and an X-ray detector 360 that detects X-rays.

[0057] When measuring total scattering data, the X-ray generation unit 310 preferably uses a high-energy radiation source using silver, molybdenum, or the like as a target metal. On the other hand, when performing measurements using X-ray reflectivity, it is preferable to use a low-energy radiation source using copper. However, when measuring total scattering data and performing measurements using X-ray reflectivity using the same device, it is preferable to use molybdenum as the target metal. Note that the entrance side optical unit 320, goniometer 330, sample stage 340, exit side optical unit 350, and X-ray detector 360 can be conventional components, so their description will be omitted.

[0058] [Measurement method and program] A sample is placed in the X-ray diffraction instrument 300, and the goniometer is driven under predetermined conditions under the control of the control device 200. X-rays are then incident on the sample, and diffracted X-rays generated from the sample are detected. This acquires diffraction data. The X-ray diffraction instrument 300 transmits the acquired diffraction data and apparatus information to the control device 200 as measurement data. The structure factor of the film portion formed on the substrate can be calculated from such measurement data using the processing device 100, calculation system 10, method, and / or program of the present invention. This will be explained in detail below.

[0059] First, the sample position adjustment process will be described with reference to Fig. 5. The sample position adjustment process is carried out by adjusting the density ρ of the film portion and the incident angle θ in This is a process for obtaining the above, and is mainly executed by the control unit 210, the sample information acquisition unit 250, and the X-ray diffraction device 300.

[0060] When the process starts, first, in step S51, the X-ray diffraction apparatus 300 controlled by the control unit 210 adjusts the position of the sample placed on the sample stage 340.

[0061] In the next step S52, the sample information acquisition unit 250 uses the X-ray diffraction device 300 to perform X-ray reflectivity measurement and measure the X-ray reflectivity of the sample.

[0062] In the next step S53, the sample information acquisition unit 250 calculates the total reflection critical angle θ using the X-ray reflectivity obtained in step S52. c Calculate.

[0063] In the next step S54, the sample information acquisition unit 250 reads out the constituent elements and composition ratio of the film portion from the sample information acquisition unit 250, calculates the density ρ of the film portion based on these, and further calculates the refraction angle θ of the film portion based on these. R Calculate.

[0064] In the next step S55, the sample information acquisition unit 250 calculates the total reflection critical angle θ obtained in step S53. c and the density ρ of the film portion obtained in step S54, the oblique incidence angle θ in Determine.

[0065] Then, in step S56, the control unit 210 and the X-ray diffraction device 300 adjust the oblique incidence angle θ obtained in step S53. in The total scattering data is measured using the formula: and the process is then terminated.

[0066] The sample position adjustment process may be implemented as a computer program, or may be stored as a computer program in a storage medium.

[0067] Next, the measurement process will be described with reference to Fig. 6. The measurement process is carried out by adjusting the density ρ of the film portion obtained by the sample position adjustment process and the incident angle θ in This is a process for obtaining total scattering data of a sample including a film portion and a substrate, and total scattering data of the substrate only, using the above, and is mainly executed by the control unit 210, the sample information acquisition unit 250, and the X-ray diffraction device 300.

[0068] When the process starts, first, in step S61, the X-ray diffraction instrument 300 drives the goniometer 330 under predetermined conditions based on control by the control unit 210 with respect to the sample placed on the sample stage 340. Then, the X-ray diffraction instrument 300 causes X-rays from the exit optical unit 350 to be incident on the sample, and detects diffracted X-rays generated from the sample using the X-ray detector 350. The data obtained in this manner is diffraction data. The X-ray diffraction instrument 300 changes the position of the X-ray detector 350 with respect to the sample and detects diffracted X-rays at multiple positions. This obtains total scattering data for the sample. The total scattering data for the sample is transmitted to the measurement data storage unit 240 and stored therein.

[0069] In the next step S62, the X-ray diffraction instrument 300 drives the goniometer 330 under predetermined conditions based on control by the control unit 210, with respect to only the substrate placed on the sample stage 340. Then, the X-ray diffraction instrument 300 causes X-rays from the exit optical unit 350 to be incident on the substrate, and detects diffracted X-rays generated from the substrate using the X-ray detector 350. The data obtained in this manner is diffraction data. The X-ray diffraction instrument 300 changes the position of the X-ray detector 350 with respect to the substrate, and detects diffracted X-rays at multiple positions. This obtains total scattering data for only the substrate. The total scattering data for only the substrate is transmitted to and stored in the measurement data storage unit 240. Then, the process ends.

[0070] It should be noted that steps S61 and S62 do not have to be executed in the order described above, and step S61 may be executed after step S62, or may be executed simultaneously.

[0071] The measurement process may be implemented as a computer program, and may be stored in a storage medium as a computer program.

[0072] Next, the total scattering data acquisition process will be described with reference to Fig. 7. The total scattering data acquisition process is a process for obtaining total scattering data for only the film portion from the total scattering data for the sample including the film portion and the substrate obtained by the measurement process and the total scattering data for only the substrate, and for determining the structure factor of the film portion, and is mainly executed by the processing device 100.

[0073] When the process starts, first, in step S71, the measurement data acquisition unit 110 acquires total scattering data I of the sample including the film portion and the substrate. sp is acquired from the measurement data storage unit 240.

[0074] Next, in step S72, the measurement data acquisition unit 110 acquires the total scattering data I sub is acquired from the measurement data storage unit 240.

[0075] In the next step S73, the total scattering data calculation unit 120 first obtains the absorption coefficient μ of the film portion from the device information storage unit 230 and the sample information acquisition unit 250. TF , thickness of the membrane t TF , the incident angle θ of the X-rays on the film R , and the diffraction angle 2θ is read out, and the absorption factor A of the substrate sub Calculate.

[0076] In the next step S74, the total scattering data calculation unit 120 acquires the first total scattering data and the second total scattering data from the measurement data acquisition unit 110, and calculates the total scattering data I of only the film portion based on these. TF Calculate.

[0077] In the next step S75, the structure factor calculation unit 130 calculates the structure factor of the film portion using the total scattering data of only the film portion. The calculated structure factor is stored in the measurement data storage unit 240. Then, the process ends.

[0078] The structural factors of the film portion are transmitted to the display device 520 and displayed as a state of the structural factors or in a PDF format.

[0079] Here, the total scattering data acquisition process may be implemented as a computer program, or may be stored in a storage medium as a computer program.

[0080] [Example] Total scattering data of an ITO film formed on a glass substrate was measured using the system 10. Table 3 shows the configuration of the apparatus used in this example, and Table 4 shows the measurement conditions. [Table 3] [Table 4]

[0081] Figure 8 shows the results of X-ray reflectivity measurements using the MoKα wavelength (0.7107 Å). The analysis results showed that the ITO film thickness was 77.6 nm and the density was 6.62 g / cm. 3 From these results, the critical angle of total reflection θ c is 0.1602°, δ=3.91×10 -6 , β=8.60×10 -8 It was calculated that:

[0082] Considering the above results, the measurement conditions for total scattering data are as follows: the incident angle θ in The critical angle of total reflection θ c The angle of incidence θ on the film was set to 0.17°, which is slightly larger than the value of 0.1602°. When this value was substituted into equations (5) and (7), the angle of incidence θ R The value of 0.0567° and the penetration depth l p The value obtained was 65.64 nm.

[0083] Figure 9 shows the relationship between the diffraction angle 2θ and the absorption factor A(θ) of the substrate, which was determined based on total scattering data measured for the substrate only. Since the absorption factor A(θ) of the substrate is approximately 0.3 over almost the entire range of diffraction angles, it was found that the influence of the glass substrate is approximately 30% in the actual measured value.

[0084] Figure 10 shows the total scattering data for a sample with an ITO film formed on a glass substrate (blue line) and a sample with a glass substrate (black line), and also shows the results of extracting the total scattering data for the film portion from these total scattering data (red line). Figure 11 shows the scattering intensity of the sample normalized to the atomic scattering factor, and Figure 12 shows the structure factor of the film portion. In general, the quality of the correction for conversion to the structure factor is judged by whether the total scattering data overlaps with the sum of the atomic scattering factor and Compton scattering in the high wavenumber region. In the high wavenumber region (12Å ―1 In the above cases, the total scattering data of the ITO film is <f 2 > and Compton Scattering I inc The sum of <f 2 >+I inc It was found that the correction was good because the image overlapped with the original image (see Figure 11).

[0085] From the above results, the processing apparatus, method, and program of the present invention can accurately calculate the structural factor of a film portion formed on a substrate while the film portion remains attached to the substrate.

[0086] In the method of the present invention, since X-rays do not need to pass through the substrate, a high-energy X-ray source is not required and there are no restrictions on the type of substrate.

[0087] Furthermore, when the conventional method described in Non-Patent Document 1, for example, is applied to a thin-film sample with a small thickness, data containing scattering intensities originating not only from the thin-film sample but also from the substrate may be detected, which may result in failure to obtain the scattering intensity of only the thin film formed on the substrate. If the scattering intensity of only the thin film cannot be obtained, an appropriate three-dimensional structure cannot be obtained. However, according to the present invention, even if the measurement data contains total scattering data originating from the substrate in addition to the total scattering data of the film portion, the total scattering data originating from the substrate can be accurately subtracted. Therefore, the present invention can be applied even to thin-film samples, which always contain total scattering data originating from the substrate.

[0088] Furthermore, to obtain information about the three-dimensional structure of a thin film sample on a substrate, it is necessary to obtain the scattering intensity of only the thin film formed on the substrate. In order to eliminate the influence of the scattering intensity from the substrate, the incident angle θ of the X-rays on the thin film sample is in However, according to the present invention, the incident angle θ of the X-rays on the sample is in is the critical angle of total reflection θ c It was found that it is preferable that the incident angle of the X-rays is less than twice the angle θ in can be determined easily and accurately.

[0089] In the method described in Non-Patent Document 1, as described above, the incident angle θ is set to prevent the detection of the scattering intensity from the substrate. in In this regard, when synchrotron radiation with low parallelism is used, the incident angle θ in However, according to the present invention, the scattering intensity originating from the substrate can be accurately subtracted, so there is no need to use the output of a synchrotron radiation facility with a high degree of collimation.

[0090] The processing device 100 may be, for example, a PC terminal or a server on the cloud, and the entire processing device 100 may be provided on the cloud, or part of the processing device 100 or part of the functions of the processing device 100 may be provided on the cloud.

[0091] Although the total scattering data of the sample has been described as being measured by the X-ray diffraction device 200, it may be acquired by another device capable of acquiring total scattering data of the sample, instead of the X-ray diffraction device 200.

[0092] In addition, in equations (1) and (2), scattering intensity may be used instead of total scattering data. The above-mentioned effects can be obtained even when scattering intensity is used.

[0093] The processing device 100 and the control device 200 may be provided in one computer. In this case, the processing device 100 and the control device 200 share an input device and a display device.

[0094] The size, shape, and quantity of each member shown in the present specification and drawings are examples and are not limited to these. Furthermore, the materials of each member are examples and are not limited to these.

[0095] Although embodiments of the present invention have been described herein with reference to the accompanying drawings, it will be apparent to those skilled in the art that modifications may be made in the structure and relationship of the parts without departing from the scope and spirit of the invention as described. [Explanation of symbols]

[0096] 10. Computing Systems 100 Processing equipment 110 Measurement data acquisition unit 120 Total scattering data calculation unit 130 Structure factor calculation part 200 control device 210 Control Unit 220 Device information storage unit 230 Measurement condition determination unit 240 Measurement data storage unit 250 Sample Information Acquisition Unit 260 Display 300 X-ray Diffractometer 310 X-ray generator 320 Incident optical unit 330 Goniometer 340 Sample Stage 350 Output optical unit 360 X-ray detector 510 Input Device 520 Display device 610 Input Device 620 Display device

Claims

1. A processing device capable of calculating a structural factor of a film portion formed on a substrate, a measurement data acquisition unit that acquires first total scattering data obtained by measuring a first sample including the substrate and the film portion under measurement conditions in which X-rays are obliquely incident, and second total scattering data obtained by measuring a second sample including the first sample other than the film portion under the measurement conditions; a total scattering data calculation unit that calculates total scattering data of the film portion based on the first total scattering data and the second total scattering data; a structure factor calculation unit that calculates a structure factor of the film portion based on the total scattering data of the film portion; A processing device comprising:

2. The processing apparatus according to claim 1 , wherein the total scattering data calculation unit calculates the total scattering data of the film portion by subtracting the product of the second total scattering data and an absorption factor of the substrate from the first total scattering data.

3. The processing apparatus according to claim 2 , wherein the total scattering data calculation unit calculates the absorption factor of the substrate based on the angle of incidence of X-rays, the angle of diffraction, the film thickness of the film portion, the absorption coefficient of the film portion, and / or the refractive index of the film portion.

4. 4. The processing apparatus according to claim 1, wherein the measurement conditions include information about an incident angle of X-rays, and the incident angle of X-rays is equal to or smaller than twice the critical angle of total reflection.

5. an X-ray diffraction apparatus including an X-ray generator that generates X-rays, an X-ray detector that detects the X-rays, a sample stage on which a sample is placed, and a goniometer that controls the angle between the X-rays generated by the X-ray generator and the surface of the sample, and the angle between the X-rays received by the X-ray detector and the surface of the sample; The processing device according to any one of claims 1 to 4, The X-ray diffraction instrument generates the first total scattering data and the second total scattering data using the X-ray generator, the X-ray detector, and the goniometer.

6. 6. The system according to claim 5, further comprising a measurement condition determination unit that determines the measurement conditions, the measurement conditions having information about angles of incidence of X-rays, and the measurement condition determination unit determines angles of incidence of X-rays with respect to the first sample and the second sample based on a film thickness of a film portion, an absorption coefficient of the film portion, and / or a critical angle of total reflection between the first sample and the X-rays.

7. The system described in claim 6, further comprising a sample information acquisition unit that determines the film thickness and density of the film portion or the total reflection critical angle of the film portion by X-ray reflectivity measurement based on data obtained using the X-ray diffraction device.

8. The system according to claim 5 , further comprising a correlation calculation unit that determines a correlation of atoms included in the film portion based on a structural factor of the film portion.

9. A program capable of calculating a structural factor of a film portion formed on a substrate, acquiring first total scattering data obtained by measuring a first sample including the substrate and the film portion under measurement conditions in which X-rays are obliquely incident; acquiring second total scattering data obtained by measuring the second sample including the portion of the first sample other than the film portion under the measurement conditions; calculating total scattering data of the film portion based on the first total scattering data and the second total scattering data; calculating a structure factor of the film portion based on the total scattering data of the film portion; A program executed by a computer, comprising:

10. A method capable of calculating a structure factor of a film portion formed on a substrate, comprising: acquiring first total scattering data obtained by measuring a first sample including the substrate and the film portion under measurement conditions in which X-rays are obliquely incident; acquiring second total scattering data obtained by measuring the second sample including the portion of the first sample other than the film portion under the measurement conditions; calculating total scattering data of the film portion based on the first total scattering data and the second total scattering data; calculating a structure factor of the film portion based on the total scattering data of the film portion; A method comprising:

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