TWI753490B - X-ray reflectometry and method thereof for measuring three dimensional nanostructures on flat substrate - Google Patents

Abstract

This invention relates to an apparatus and methods for applying X-ray reflectometry (XRR) in characterizing three dimensional nanostructures supported on a flat substrate with a miniscule sampling area and a thickness in nanometers. In particular, this invention is targeted for addressing the difficulties encountered when XRR is applied to samples with intricate nanostructures along all three directions, e.g. arrays of nanostructured poles or shafts. Convergent X-ray with long wavelength, greater than that from a copper anode or 0.154 nm and less than twice of the characteristic dimensions along the film thickness direction, is preferably used with appropriate collimations on both incident and detection arms to enable the XRR measurements of samples with limited sample area and scattering volumes.

Description

X-ray reflection for inspection of 3D nanostructures on flat substrates Radiometer and its method

The present invention relates to a detection device, and more particularly, to an X-ray reflectometry (XRR) for detecting three-dimensional nanostructures on a planar substrate and a method thereof.

X-ray reflectometry is a method for in-depth analysis of monolayer and multilayer nanosamples by electron density, as well as the study of surfaces and interfaces, including their roughness, interfacial diffusion, and monolayer and multilayer film thickness. In addition, the literature states that X-ray reflectometers are capable of detecting cross-sectional profiles of surface patterns, eg, periodic grating cross-sections fabricated by nanoimprint. The cross-sectional profile of the above X-ray reflectometer applied to the surface pattern is based on the effective medium approximation (EMA) method. The equivalent concept of EMA has been used for elliptically polarized or scattering porous materials to estimate the effective refractive index. The effectiveness of EMA for nanostructures depends on the coherence length of the incident X-rays; EMA only becomes applicable when the coherence length is greater than the lateral characteristic length of the nanostructure along the detection direction. In this case, the structure-to-space ratio at any given sample depth can be inferred from the X-ray reflectometry results. When the incident X-ray is along the detection direction With sufficient effective interference length, X-ray reflectometers can be used to measure film thickness and cross-sectional shape of grating arrays. In the specular geometry of an X-ray reflectometer, the effective interference length along the y-axis is in micrometer units, and the effective interference length along the x-axis is in nanometer units. For the grating, the structural change along the x-axis is very small, almost no change, but it is not suitable for 3D nanostructure; the 3D nanostructure sample in this case does not have the best azimuth direction. Therefore, in addition to the challenges in the lateral interference length measured by X-ray reflectometers of nanostructures on flat substrates, there is also the design of condensed X-rays using wider slit widths to reduce scattered light as well as off-specular ) reflected light is concentrated on the target sample. The non-specular intensities can reach comparable intensities in the high qz region and can be used to measure samples with pronounced lateral structures such as the 3D nanostructures described herein.

NOVA's invention patent in 2018 (US 2018/10119925 B2) uses a conical light source with a scattering angle of 20 to 40 degrees, which is different from the light source used in this application. The focused beam in this invention patent is limited by a slit in the z direction, so that the scattering angle is less than or equal to 1 degree; in the x direction, the angle is 15 to 25 degrees, so a multi-angle scattering pattern can be obtained in this direction. A line cut is performed at each angle on the scatter plot to obtain specular intensity values. Then, the light intensity within the opening angle range is all integrated to obtain the reflected signal at the incident angle θ. The method developed by NOVA can only obtain a 2D scattering pattern on the entire 2D detector screen, and many non-specular reflection signals will overlap on the screen, which is difficult to analyze and distinguish. One solution NOVA attempted to propose was to use different azimuths to separate the promiscuous multi-angle scattering patterns. However, results and practical methods to obtain light intensity signals in each xyz direction are still lacking, which makes it impossible to analyze complex 3D structures. In the NOVA invention patent, it is impossible to analyze the depth value of the sample in the z direction according to different incident angles.

A KLA patent issued in 2019 (US 2019/0017946 A1) proposes that different focusing optics can be used to generate focused beams with different wavelengths, for example, using a multi-layer coating on the focusing optics lens to focus different wavelengths on the sample. However, the focused beam will still encounter multiple scattering in the xyz directions at the same time, making accurate analysis and distinction impossible. There is also no description in the KLA patent how to precisely illuminate the different wavelengths onto the sample. In contrast, the long-wavelength light source described in the previous patent invention (US 2016/0341674 A1) can be efficiently focused on the sample through a monochomator and a slit in the z-direction.

Additionally, the KLA patent mentions that response function models can be used to calculate and fit 3D structures. However, it was difficult to build a 3D model before this due to the extremely complex scattering pattern of the 3D pattern.

According to an embodiment of the present invention, an X-ray reflectometer for detecting three-dimensional nanostructures on a flat substrate is provided, including an X-ray light source, an X-ray reflector, an incident slit and an X-ray detector. The X-ray light source is used to emit X-rays with a wavelength greater than 0.154 nm. X-ray reflectors are used to focus a fan-shaped X-ray onto a surface of a sample. The entrance slit is located between the X-ray reflector and the sample, and the width of the entrance slit is 10 times or more larger than its opening, and its width is perpendicular to the plane of reflection of the X-rays. The X-ray detector has good pixel resolution and is used to collect fan-shaped X-rays reflected from the surface of the sample. Among them, the fan-shaped X-ray has an incident angle that can be adjusted within a predetermined range, the incident angle of the fan-shaped X-ray is controlled by the opening size of the group of slits, and the divergence angle of the fan-shaped X-ray is controlled by the width of the group of slits. , where the fan-shaped X-rays collected on the X-ray detector For each azimuth of the ray, the non-specular value is calculated and removed from the reflected X-ray intensity.

According to an embodiment of the present invention, a method for X-ray reflectometry (XRR) is provided for detecting three-dimensional nanostructures on a planar substrate, including the following steps. A fan-shaped X-ray spot is focused on a surface of a sample, wherein the incident angle of the fan-shaped X-ray is adjustable within a preset angle range, and the light wavelength of the fan-shaped X-ray is greater than 0.154 nm. When the incident angle is changed, the incident opening angle of the fan-shaped X-ray is adjusted according to the incident angle, wherein the incident opening angle of the fan-shaped X-ray is controlled by the opening size of an incident slit. A divergence angle of the fan-shaped X-rays is adjusted by the width of the incident slit. The fan-reflected X-rays are collected using an X-ray detector. In each azimuth angle of the fan-shaped X-rays collected on the X-ray detector, the non-specular reflection value is calculated and removed from the reflected X-ray intensity. The specular component of the reflected X-ray intensity remaining in each azimuth is integrated to obtain the specular intensity for each angle of incidence. Within a predetermined incident angle range, the ratio of the specular reflection intensity to the total intensity of the incident beam is collected to analyze the surface structure information of the sample.

According to an embodiment of the present invention, a method for X-ray reflectometry (XRR) is provided for detecting three-dimensional nanostructures on a planar substrate, including the following steps. Specular and non-specular reflections are collected in a fan of X-rays using an X-ray detector. In each azimuth angle of the fan-shaped X-rays collected on the X-ray detector, the non-specular reflection value is calculated and removed from the reflected X-ray intensity.

In order to have a better understanding of the above-mentioned and other aspects of the present invention, the following specific examples are given and described in detail in conjunction with the accompanying drawings as follows:

10: X-ray reflectometer

100: X-ray light source

102: X-ray reflector

200: entrance slit

201: Detector slit

202: Opening

300: X-ray detector

301: Analyzer

400: Sample

401: Surface

410: Flat substrate

500: Sample stage

ω: azimuth angle

δθ: Incident opening angle

:發散張角

: divergent opening angle

θ: Incident angle

m': specular reflection point

ij: incident light wavefront

i'j': reflected light wavefront

W: slit width

Fig. 1 is a schematic diagram of an X-ray reflectometer according to an embodiment of the present invention; Fig. 2A is a fan-shaped incident beam reflected on a sample; Fig. 2B is a top view of Fig. 2A; Fig. 3 is an incident wavefront ij is specularly reflected on the sample surface; Figure 4A shows the scatter plot from a 2D detector of a 3D nanoporous film on a silicon substrate; Figure 4B shows when the fan-shaped incident beam shown in Figure 2A hits a Figure 4A shows the scattering plot of the 2D detector for the 3D nanoporous thin film sample; Figure 4C shows the scattering intensity distribution along the line m'n' shown in Figure 4B; and Figure 5 shows the A flowchart of a method for an X-ray reflectometer according to an embodiment of the present invention.

The following examples are provided for detailed description, and the examples are only used as examples to illustrate, and are not intended to limit the scope of protection of the present invention. In the following, the same/similar symbols are used to represent the same/similar elements for description. The directional terms mentioned in the following embodiments, such as: up, down, left, right, front or rear, etc., only refer to the directions of the accompanying drawings. Accordingly, the directional terms used are illustrative and not limiting of the present invention.

The present invention relates to how to detect 3D nanostructure features on planar substrates. More specifically, the X-ray reflectometer of the present invention is suitable for having a complex 3D structure and having a limited thickness or height (nanoscale) and at the same time having a limited sample detection area. In the previous patent for invention (US 2016/0341674 A1), for samples with small sample volume, thickness and area, a concentrated light source and optical path are used to increase the incident light flux, thereby increasing the intensity of the reflected signal, and at the same time, the scattering vector Qz In other words, the ideal resolution is maintained, and its Qz is defined as (4π/λ) sinθ; λ represents the wavelength of the X-ray, and θ represents the incident angle between the sample surface and the incident X-ray. Since the previous patent only deals with specular reflection, the incident angle θ is also the detection angle relative to the sample surface. In the previous invention patent, long-wavelength X-rays are focused on the target sample with a strictly controlled opening angle δθ, while maintaining the maximum opening angle in the azimuthal direction to allow sufficient X-ray flux to hit the sample. The aim of the present invention is to extend the above-described X-ray reflectometer to measure 3D nanostructures on planar substrates.

In this case, a 2D detector is used to collect the specular and non-specular reflection or scattered X-rays of the X-ray reflectometer. The non-specular reflection or scattering comes from the limited coherence length and the limited lateral direction caused by the complex 3D nanostructure. Scattering quantities Qx and Qy, the specular reflection intensity can be obtained by removing the above integrals.

When X-ray reflectometry is used for nanostructure surface analysis, the most important information available is along the sample thickness direction (with respect to the given z-axis of the sample surface). The X-ray reflectometer-derived structural result is the result of the transverse average over the interference length at a particular depth. In order to obtain the 3D length of the precise nanostructure from the X-ray reflectometer, additional external feature lengths are required, and the relevant features can be obtained from transmission small-angle X-ray scattering (tSAXS) at normal incidence. value. Therefore, the analysis procedures in this paper can use the tSAXS data together with the X-ray reflectometry data above.

In the condensed beam shown herein, the scattering vectors Qx and Qy are projected onto the sample surface or xy surface from the opening and closing angles of the entrance slit and detector slit. For simplicity, the size of the openings of the incident slit and the detector slit are set to be the same and denoted as Φ. Starting from simple geometric considerations, the following formulas can be listed; Qx=(π/λ)cos θ[-2Φ,2Φ]Qy=(π/λ)cos θ[-Φ ² ,Φ ² ]

Φ is in radians and its value is usually less than 1, when Φ=0.26 radians (rad) or 15°, Qx is in the range of ±0.52(π/λ)cos θ, and Qy is in the range of ±0.068(π/λ) ) cos θ. In a concentrator X-ray reflectometer setup, the aperture angle of the slit in the optical design is typically 15° to 20°, which results in the Qx>Qy situation in most concentrator X-ray reflectometry measurements. For thin-film samples, the limited scattering vectors Qx, Qy and the transverse interference length make the application of concentrating X-ray reflectometers unrestricted because there are no lateral structural changes. For measuring grating samples, it is desirable to align the grating with the x-axis to mitigate the effects of Qx in X-ray reflectometry measurements. Alignment along the x-axis is also critical for lateral interference lengths, which are fairly small. Using a highly collimated ribbon incident beam, grating misalignment can also be seen with conventional X-ray reflectometry measurements.

Even if the condensed incident beam is not used in this paper, it is still very important to discuss the interference length and the scattering vectors Qx, Qy, because the only difference between using a condensed or a ribbon beam is the value of Φ, and the value of Φ of the condensed incident beam used in this case is between the From 15° to 25°, and for ribbon beams, the value of Φ is about 1° or less.

For 3D nanostructured samples, there is usually no apparent lateral alignment relative to the axes of conventional X-ray reflectometers (such as the x- or y-axis shown in Figure 2A), using To reduce the loss due to finite interference length and lateral scattering vectors Qx and Qy. The purpose of the present invention is to address the lack of the method using concentrated X-ray reflectometry to measure 3D nanostructures on planar substrates.

The present invention can solve the problems of the conventional concentrating X-ray reflector. First, the method in this paper adopts different incident angles θ, which can analyze the depth value of the sample in the z direction. The focused light combines the xy and reflected signals of the 3D sample. By analyzing the electron density along the z-direction corresponding to the structural composition of different depths, combined with the known external line width or line spacing value, the composition and size of the 3D material can be successfully resolved.

The problem to be solved in this case is that in the past, the common methods for detecting critical dimensions were atomic force microscope (AFM) and scanning electron microscope (SEM), but both encountered bottlenecks in measuring critical dimensions. The present invention proposes a method for detecting the critical dimensions of 3D nanostructures on a planar substrate by using long-wavelength condensing light of an X-ray reflectometer. The fan-shaped condensing can effectively increase the light intensity, reduce the detection area, and simultaneously receive different plane orientations. The signal of azimuthal angle, thickness and density information can be obtained by integration and EMA approximation method, and the depth map can be analyzed with the density, which can be used for high-precision detection of the pattern thickness of the component process, as well as the line width of the detection component and Variation in line spacing and high resolution (less than 0.1 nm).

Please refer to FIG. 1 , which shows a schematic diagram of an X-ray reflector 10 according to an embodiment of the present invention. The X-ray reflector 10 may include an X-ray light source 100 , an X-ray reflector 102 , an entrance slit 200 , a detector slit 201 , an X-ray detector 300 and at least one analyzer 301 . The X-ray light source 100 is used for emitting X-rays with a wavelength greater than 0.154 nm. The X-ray reflector 102 is used to focus a fan-shaped X-ray on a surface 401 of a sample 400, the fan The shaped X-ray has an incident angle θ that can be adjusted within a predetermined range. In one embodiment, the sample 400 is located on a planar substrate 410 and can be rotated 360 degrees by the sample stage 500 . The flat substrate 410 is, for example, a semiconductor substrate.

通過入射狹縫200的寬度來控制。另外，偵測器狹縫201位在X射線偵測器300和樣品400之間，用以調整反射X射線的張角。 Furthermore, the entrance slit 200 is located between the X-ray reflector 102 and the sample 400, and its width is perpendicular to the plane of reflection of the X-rays. The width of the incident slit 200 is, for example, 10 times or more larger than the opening 202 thereof, but the invention is not limited thereto. In one embodiment, the incident opening angle δ θ of the fan-shaped X-ray is controlled by the size of the opening 202 of the incident slit 200 , and a divergent opening angle of the fan-shaped X-ray is

Controlled by the width of the incident slit 200 . In addition, the detector slit 201 is located between the X-ray detector 300 and the sample 400 to adjust the opening angle of the reflected X-rays.

In addition, the X-ray detector 300 has a good pixel resolution for collecting fan-shaped X-rays reflected from the surface of the sample 400 . In one embodiment, in each azimuth angle ω of the fan-shaped X-rays collected on the X-ray detector 300, the non-specular reflection value is calculated and removed from the reflected X-ray intensity.

Please refer to FIG. 2A, which shows a fan-shaped incident beam reflected on sample 400. The angle between the incident beam and the xy plane, θ, is the same as the angle between the reflected beam and the xy plane.

是入射光和反射光的發散張角。i代表被樣品400鏡面反射到i'的光束；j表示被樣品400鏡面反射到j'的光束。圖中的另一個標示為光束m，光束m相對於y軸的角度為ω，經由樣品400鏡面反射到m’，ij線和i’j’線分別代表入射光波前和反射光波前。 Please refer to FIG. 2B, which shows a top view of FIG. 2A. In Figure 2A,

is the divergence angle of the incident and reflected light. i represents the beam specularly reflected by the sample 400 to i'; j represents the beam specularly reflected by the sample 400 to j'. The other in the figure is labeled as beam m, the angle of beam m relative to the y-axis is ω, and it is specularly reflected to m' by the sample 400, and the lines ij and i'j' represent the incident light wavefront and the reflected light wavefront, respectively.

Figure 3 shows that the incident light wavefront ij is specularly reflected on the surface of the sample 400 and the reflected wavefront is recorded on the 2D detector as line i'j'. Each point m' on line i'j' represents a specular reflection from point m on the incident wave surface, as shown in Figure 2B. A specular line can be interpreted as a collection of many specular points m'.

Figure 4A shows the scatter plot of a 2D detector from a 3D nanoporous film on a silicon substrate, where the light source is a well-collimated pencil beam. Figure 4B shows the scatter plot of the 2D detector when the fan-shaped incident beam shown in Figure 2A impinges on the 3D nanoporous thin film sample 400 as described in Figure 4A.

Fig. 4C shows the scattering intensity distribution along the line m'n' shown in Fig. 4B. The shaded area represents the distribution of non-specular reflections, which should be integrated and subtracted to obtain the specular reflection values at the incident angle θ shown in Figure 2A. The XRR signal can be obtained by measuring the specular reflection intensity within the predetermined incident angle θ range.

。在步驟S240中，使用一X射線偵測器300收集扇形反射之X射線。在步驟S250中，在X射線 偵測器300上收集的扇形X射線的每個方位角ω中，計算非鏡面反射值，並將非鏡面反射值從反射X射線強度中去除，如第4C圖所示。在步驟S260中，在每個方位角ω中剩餘的反射X射線強度的鏡面反射分量，將其積分以獲得每個入射角θ之鏡面反射強度。在步驟S270中，在預定的入射角θ範圍內，收集鏡面反射強度與入射光束的總強度之比，用以分析樣品400之表面結構訊息。 Please refer to FIGS. 1 and 5, wherein FIG. 5 illustrates a flowchart of a method for an X-ray reflector 10 according to an embodiment of the present invention. The method includes the following steps. First, in step S210, a fan-shaped X-ray spot is focused on a surface 401 of a sample 400, wherein the incident angle θ of the fan-shaped X-ray is adjustable within a preset angle range, and Fan X-rays have optical wavelengths greater than 0.154 nm. In step S220, when the incident angle θ is changed, the incident angle δ θ of the fan-shaped X-ray is adjusted according to the incident angle θ , wherein the incident angle δ θ of the fan-shaped X-ray is controlled by the size of the opening 202 of an incident slit 200, and the incident angle δ θ is, for example, a tangent function of the incident angle θ . In step S230 , the divergence angle of the fan-shaped X-rays is adjusted by the width W of the incident slit 200 (see FIG. 2B )

. In step S240, an X-ray detector 300 is used to collect fan-reflected X-rays. In step S250, in each azimuth angle ω of the fan-shaped X-rays collected on the X-ray detector 300, the non-specular reflection value is calculated, and the non-specular reflection value is removed from the reflected X-ray intensity, as shown in Fig. 4C shown. In step S260, the specular reflection component of the reflected X-ray intensity remaining in each azimuth angle ω is integrated to obtain the specular reflection intensity for each incident angle θ . In step S270 , the ratio of the specular reflection intensity to the total intensity of the incident light beam is collected within a predetermined incident angle θ range to analyze the surface structure information of the sample 400 .

In one embodiment, the wavelength of the light does not exceed twice the characteristic length along the normal to the surface of the structure of the sample 400 .

In one embodiment, the above-mentioned characteristic length is selected from the film thickness on the surface of the sample 400 and the nanostructure height on the surface of the sample 400 .

In one embodiment, the X-ray reflector 102 is selected from a combination of a single crystal monochromator and a multilayer mirror, and the wavelength dispersion of the multilayer mirror of the X-ray reflector 102 is less than 0.01.

In one embodiment, the above-mentioned incident opening angle δθ is a function of the incident angle θ. That is, the incident opening angle δθ can be changed with different incident angles θ.

In one embodiment, the above-mentioned incident opening angle δθ is equal to the tangent function of the incident angle θ multiplied by a constant K (ie, δθ=K*tanθ).

In one embodiment, the above-mentioned X-ray light source 100 includes a well-focused aluminum target.

In one embodiment, the above-mentioned analyzer 301 is used during the period when the X-rays are collected by the X-ray detector 300. The analyzer 301 includes an X-ray photoelectron spectrometer (XPS) and/or an X-ray fluorescence spectrometer. X-ray fluorescence spectrometer.

In the above step S230, the sample stage 500 may also be rotated along the surface normal of the sample 400, so that the X-rays are carried out at different azimuth angles ω. The angle between the planes of reflection of the rays.

In the above step S240, during the collection of reflected X-rays, X-ray photoelectron spectroscopy (XPS) signals may be collected; during the collection of reflected X-rays, X-ray fluorescence (X-ray fluorescence) signals may be collected , XRF) spectral signal, and analyze the surface structure information of the sample 400 from the XPS signal, the XRF signal and the XRR signal.

According to the X-ray reflectometer and the method thereof according to the above-mentioned embodiments of the present invention, the critical dimension of the sample in the z direction can be analyzed by using different incident angles θ. Since the present invention gathers the Qx, Qy signals of the sample and the reflection signal Qz, only the light intensity in the Qz direction is taken, and the electron density versus depth map along the z direction is analyzed, and the known external line distance value can be successfully analyzed. Critical dimensions for different depths. In addition, the X-ray reflectometer of the present invention uses long-wavelength concentrated X-rays, the wavelength of which is greater than 0.154nm of general commercial copper targets, and less than twice the feature size along the film thickness direction. The collimator can measure samples of micro-area and limited scattering volume, such as three-dimensional nanostructure samples on a flat substrate (semiconductor substrate), to solve the problem when X-ray reflectometers have complex nanostructures in three coordinate directions. Difficulties encountered, complex structures such as nanoscale arrays of rods or axes.

To sum up, although the present invention has been disclosed by the above embodiments, it is not intended to limit the present invention. Those skilled in the art to which the present invention pertains can make various changes and modifications without departing from the spirit and scope of the present invention. Therefore, the present invention The scope of protection shall be determined by the scope of the appended patent application.

10: X-ray reflectometer

100: X-ray light source

102: X-ray reflector

200: entrance slit

201: Detector slit

202: Opening

300: X-ray detector

301: Analyzer

400: Sample

401: Surface

410: Flat substrate

500: Sample stage

δθ: Incident opening angle

θ: Incident angle

Claims (19)

An X-ray reflectometer for detecting three-dimensional nanostructures on a flat substrate, comprising: an X-ray light source for emitting X-rays with a light wavelength greater than 0.154 nanometers; an X-ray reflector for focusing a fan-shaped X-ray on a surface of a sample; an entrance slit, located between the X-ray reflector and the sample, the entrance slit having a width 10 times or more larger than its opening and perpendicular to the width of the X-ray a reflecting plane; and an X-ray detector with good pixel resolution for collecting the fan-shaped X-rays reflected from the surface of the sample, wherein the fan-shaped X-rays have an incident angle adjustable within a predetermined range, the The incident opening angle of the fan-shaped X-ray is controlled by the opening size of the incident slit, and a divergent opening angle of the fan-shaped X-ray is controlled by the width of the incident slit, wherein the fan-shaped X-ray collected on the X-ray detector is For each azimuth of the ray, the non-specular value is calculated and removed from the reflected X-ray intensity. The X-ray reflectometer of claim 1, wherein the light wavelength does not exceed twice the characteristic length along the normal to the structured surface of the sample. The X-ray reflectometer of claim 2, wherein the characteristic length is selected from the film thickness of the surface and the nanostructure height of the surface. The X-ray reflector according to claim 1, wherein the X-ray reflector is selected from the combination of a single crystal monochromator and a multilayer mirror, and the wavelength dispersion of the multilayer mirror of the X-ray reflector is less than 0.01. The X-ray reflectometer of claim 1, wherein the incident opening angle is a function of the incident angle. The X-ray reflectometer of claim 5, wherein the incident opening angle is equal to the tangent function of the incident angle multiplied by a constant. The X-ray reflectometer of claim 1, wherein the X-ray light source comprises a well-focused aluminum target. The X-ray reflectometer as claimed in claim 1, further comprising at least one analyzer for use in the period during which the X-rays are collected by the X-ray detector, the at least one analyzer including an X-ray photoelectron spectrometer and/or an X-ray photoelectron spectrometer Ray fluorescence spectrometer. A method for X-ray reflectometry (XRR) for detecting three-dimensional nanostructures on a planar substrate, comprising: focusing a fan-shaped X-ray spot onto a surface of a sample, wherein the incidence of the fan-shaped X-ray The angle can be adjusted within a preset angle range, and the light wavelength of the fan-shaped X-ray is greater than 0.154 nm; when the incident angle changes, the incident angle of the fan-shaped X-ray is adjusted according to the incident angle, wherein the fan-shaped X-ray is The incident opening angle is controlled by the opening size of an incident slit; a divergent opening angle of the fan-shaped X-ray is adjusted by the width of the incident slit; an X-ray detector is used to collect the X-ray reflected by the fan-shaped; In each azimuth angle of the fan-shaped X-rays collected on the X-ray detector, a non-specular reflection value is calculated and removed from the reflected X-ray intensity; in each of the azimuth angles remaining The specular reflection component of the reflected X-ray intensity is integrated to obtain the specular reflection intensity for each incident angle; and within the predetermined range of the incident angle, the ratio of the specular reflection intensity to the total intensity of the incident beam is collected, using to analyze the surface structure information of the sample. The method of claim 9, comprising rotating along the surface normal of the sample at different azimuths, the azimuth being the angle between a given axis of the sample surface and a reflection plane. The method of claim 9, wherein the wavelength of the light does not exceed twice the characteristic length along the surface normal to the structure of the sample. The method of claim 11, wherein the characteristic length is selected from the film thickness of the surface and the nanostructure height of the surface. The method of claim 9, wherein the angle of incidence is a function of the angle of incidence. The method of claim 13, wherein the incident angle is equal to the tangent function of the incident angle multiplied by a constant. The method of claim 9, collecting X-ray photoelectron spectroscopy (XPS) signals during the collection of the reflected X-rays; collecting X-ray fluorescence (XRF) spectral signals during the collection of the reflected X-rays, and The surface structure information of the sample was analyzed from XPS signal, XRF signal and XRR signal. A method for X-ray reflectometry (XRR) for detecting three-dimensional nanostructures on a planar substrate, comprising: collecting a fan of specular and non-specular X-rays using an X-ray detector; and For each azimuth angle of the fan-shaped X-rays collected on the X-ray detector, a non-specular reflection value is calculated and removed from the reflected X-ray intensity. The method of claim 16, further comprising integrating the remaining specular component of the reflected X-ray intensity in each azimuth angle to obtain the specular intensity for each incident angle. The method of claim 17, further comprising collecting the ratio of the specular reflection intensity to the total intensity of the incident beam of the fan-shaped X-ray within the predetermined incident angle range for analyzing the surface structure information of a sample. The method of claim 16, collecting X-ray photoelectron spectroscopy (XPS) signals during the collection of the reflected X-rays; collecting X-ray fluorescence (XRF) spectral signals during the collection of the reflected X-rays, and The surface structure information of a sample is analyzed from XPS signal, XRF signal and XRR signal.

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