CN111856637A - X-ray-based multilayer film zone plate correction method and system - Google Patents
X-ray-based multilayer film zone plate correction method and system Download PDFInfo
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- CN111856637A CN111856637A CN202010810946.XA CN202010810946A CN111856637A CN 111856637 A CN111856637 A CN 111856637A CN 202010810946 A CN202010810946 A CN 202010810946A CN 111856637 A CN111856637 A CN 111856637A
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/18—Diffraction gratings
- G02B5/1838—Diffraction gratings for use with ultraviolet radiation or X-rays
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
- G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/18—Diffraction gratings
- G02B5/1876—Diffractive Fresnel lenses; Zone plates; Kinoforms
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- G—PHYSICS
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- G21K—TECHNIQUES FOR HANDLING PARTICLES OR IONISING RADIATION NOT OTHERWISE PROVIDED FOR; IRRADIATION DEVICES; GAMMA RAY OR X-RAY MICROSCOPES
- G21K1/00—Arrangements for handling particles or ionising radiation, e.g. focusing or moderating
- G21K1/06—Arrangements for handling particles or ionising radiation, e.g. focusing or moderating using diffraction, refraction or reflection, e.g. monochromators
Abstract
The invention relates to a correction method and a system based on an X-ray multilayer film zone plate, wherein the method comprises the following steps: plating N layers of periodic films on the upper end and the lower end of the multilayer film zone plate respectively; grazing incidence X-ray reflection test is carried out on the N layers of plated periodic films, and the periodic thickness of the N layers of plated periodic films at two ends is determined; shooting the multilayer film zone plate and the N layers of periodic films plated at two ends by using an electron microscope to obtain a shot image; reading the thickness of each layer of the zone plate in the shot image and the thickness of the N layers of the periodic films plated at two ends; and correcting the thickness of each layer of the zone plate in the shot image according to the period thickness and the period film thickness in the shot image. According to the invention, the periodic films are added at the upper end and the lower end of the multi-layer film zone plate, so that errors introduced during image shooting of an electron microscope are corrected, and the accuracy of positioning and thickness characterization of the electron microscope is improved.
Description
Technical Field
The invention relates to the technical field of multilayer film zone plates, in particular to a correction method and system based on an X-ray multilayer film zone plate.
Background
The X-ray wave band covers the resonance lines of most elements, the wavelength is short, the penetrability is strong, and nondestructive measurement can be realized. Therefore, X-ray microscopy is an important research tool in the research fields of biology, medicine, materials, physics, chemistry and the like. The resolution of the X-ray microscopic imaging system is determined by the size of the focal spot available from the focusing element, and therefore, the development of high-quality nano focusing optical elements is a prerequisite for realizing high-resolution X-ray microscopy. The X-ray multilayer film zone plate is an ideal novel optical element for converging X-rays at present. This method was proposed in 2004 and is based on the physical idea of an X-ray laue lens. Depositing thousands of nano film layers by adopting a sputtering technology, and then slicing and thinning the cross section of the film layers to prepare the wave zone plate with the depth of microns. The preparation process of the X-ray multilayer film zone plate is extremely precise, and is the ultimate challenge of the current micro-nano processing technology.
For the research of the multilayer film zone plate, the current international main face is the stress problem, the accurate positioning problem of the nanometer film layer and the bottleneck problem of the resolution improvement. To solve the problem of the multilayer film zone plate, a high-resolution electron microscope (SEM) is required to observe and mark the nano film layer. At present, the main research groups of all countries in the world adopt electron microscope assistance to obtain very good research results. However, when SEM imaging is used, errors may be caused by the angle change between the incident electrons and the sample surface and mechanical vibration, and for a multi-layer zone plate with thousands of layers, the accumulation of errors may cause distortion of the layer positioning and thickness characterization.
Disclosure of Invention
The invention aims to provide a correction method and a correction system based on an X-ray multilayer film zone plate, which are used for correcting errors introduced during image shooting of an electron microscope and improving the accuracy of positioning and thickness characterization of the electron microscope.
In order to achieve the purpose, the invention provides the following scheme:
a correction method based on an X-ray multilayer film zone plate comprises the following steps:
plating N layers of periodic films on the upper end and the lower end of the multilayer film zone plate respectively; n is a positive integer greater than 2;
grazing incidence X-ray reflection test is carried out on the N layers of plated periodic films, and the periodic thickness of the N layers of plated periodic films at two ends is determined to be the first upper end thickness and the first lower end thickness;
shooting the multilayer film zone plate and the N layers of periodic films plated at two ends by using an electron microscope to obtain a shot image;
reading the thickness of each layer of the zone plate in the shot image and the thickness of the N layers of the periodic films plated at two ends; the read thickness of the N layers of periodic films plated at the two ends comprises a second upper end thickness and a second lower end thickness;
and correcting the thickness of each layer of the zone plate in the shot image according to the first upper end thickness, the first lower end thickness, the second upper end thickness and the second lower end thickness.
Preferably, the X-ray source in the X-ray reflection test is a Cu-Ka line, the wavelength is 0.154nm, and the test mode is a theta-2 theta linkage scanning mode.
Preferably, the determining the periodic thickness of the N-layer periodic film plated at the two ends specifically comprises: and determining the periodic thickness of the N layers of periodic films plated at two ends according to a Bragg formula.
Preferably, the bragg formula is as follows:
wherein D is the period thickness of N layers of periodic films at the end to be measured, thetarThe grazing incidence angle corresponding to the r-th Bragg peak, q is the diffraction order, and lambda is the wavelength of X-ray and is the average refraction small quantity of the multilayer film.
Preferably, the correcting the thickness of each layer of the zone plate in the captured image according to the first upper end thickness, the first lower end thickness, the second upper end thickness, and the second lower end thickness includes:
determining a proportional function according to the first upper end thickness, the first lower end thickness, the second upper end thickness and the second lower end thickness;
and correcting the thickness of each layer of the film zone plate in the shot image according to the proportional function.
Preferably, the specific formula for correcting the thickness of each layer of the film zone plate in the shot image according to the proportional function is as follows:
wherein y is the thickness of each layer of the film zone plate after correction, and delta D1＝D1-D′1，ΔD2＝D2-D′2，D1Is a first upper end thickness, D2Is a first lower end thickness, D'1Is a second upper end thickness, D'2And the thickness of the second lower end is n, the total number of film layers of the multilayer film zone plate is n, and the thickness of each film zone plate in the shot image is x.
An X-ray multilayer film zone plate-based correction system, comprising:
the plating module is used for plating N layers of periodic films on the upper end and the lower end of the multilayer film zone plate respectively; n is a positive integer greater than 2;
the X-ray reflection testing module is used for carrying out grazing incidence X-ray reflection testing on the plated N layers of periodic films and determining the periodic thicknesses of the N layers of periodic films plated at two ends, namely the thickness of the first upper end and the thickness of the first lower end;
the shooting module is used for shooting the multilayer film zone plate and the N layers of periodic films plated at two ends by using an electron microscope to obtain a shot image;
the thickness reading module is used for reading the thickness of each layer of the zone plate in the shot image and the thickness of the N layers of the periodic films plated at two ends; the read thickness of the N layers of periodic films plated at the two ends comprises a second upper end thickness and a second lower end thickness;
and the correcting module is used for correcting the thickness of each layer of the zone plate in the shot image according to the first upper end thickness, the first lower end thickness, the second upper end thickness and the second lower end thickness.
According to the specific embodiment provided by the invention, the invention discloses the following technical effects:
the invention discloses a correction method and a system based on an X-ray multilayer film zone plate, wherein the method comprises the following steps: plating N layers of periodic films on the upper end and the lower end of the multilayer film zone plate respectively; grazing incidence X-ray reflection test is carried out on the N layers of plated periodic films, and the periodic thickness of the N layers of plated periodic films at two ends is determined to be the first upper end thickness and the first lower end thickness; shooting the multilayer film zone plate and the N layers of periodic films plated at two ends by using an electron microscope to obtain a shot image; reading the thickness of each layer of the zone plate in the shot image and the thickness of the N layers of the periodic films plated at two ends; the read thickness of the N layers of periodic films plated at the two ends comprises a second upper end thickness and a second lower end thickness; and correcting the thickness of each layer of the zone plate in the shot image according to the first upper end thickness, the first lower end thickness, the second upper end thickness and the second lower end thickness. According to the invention, the periodic films are added at the upper end and the lower end of the multi-layer film zone plate, so that errors introduced during image shooting of an electron microscope are corrected, and the accuracy of positioning and thickness characterization of the electron microscope is improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
Fig. 1 is a flowchart of a correction method based on an X-ray multilayer film zone plate according to an embodiment of the present invention;
fig. 2 is a block diagram of a multilayer film zone plate provided by an embodiment of the present invention;
fig. 3 is a structural diagram of a correction system based on an X-ray multilayer film zone plate according to an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention aims to provide a correction method and a correction system based on an X-ray multilayer film zone plate, which are used for correcting errors introduced during image shooting of an electron microscope and improving the accuracy of positioning and thickness characterization of the electron microscope.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Example 1
Fig. 1 is a flowchart of a correction method based on an X-ray multilayer film zone plate according to an embodiment of the present invention, as shown in fig. 1, the method includes:
step 101: plating N layers of periodic films on the upper end and the lower end of the multilayer film zone plate respectively; n is a positive integer greater than 2.
Step 102: and performing grazing incidence X-ray reflection test on the plated N layers of periodic films, and determining the periodic thicknesses of the N layers of periodic films plated at two ends as the first upper end thickness and the first lower end thickness.
In this embodiment, the X-ray source in the X-ray reflection test is Cu-K α line, the wavelength is 0.154nm, and the test mode is θ -2 θ linkage scan mode. The detector receives the reflected signal at an angle 2 theta when the incident light is incident on the sample at a grazing incidence angle theta. And obtaining a reflectivity curve according to the test result, fitting the reflectivity curve, and determining the periodic thickness of the N layers of periodic films plated at two ends according to a Bragg formula.
The Bragg formula for determining the periodic thickness of the N-layer periodic film plated at two ends is as follows:
d is the period thickness of the N layers of periodic films at the end to be detected, theta r is the grazing incidence angle corresponding to the r-th Bragg peak, q is the diffraction order, and lambda is the wavelength of X rays and is the average refraction small quantity of the multilayer film.
Step 103: and shooting the multilayer film zone plate and the N layers of periodic films plated at two ends by using an electron microscope to obtain a shot image.
Step 104: reading the thickness of each layer of the zone plate in the shot image and the thickness of the N layers of the periodic films plated at two ends; the read thicknesses of the N layers of periodic films plated at two ends comprise a second upper end thickness and a second lower end thickness.
Step 105: and correcting the thickness of each layer of the zone plate in the shot image according to the first upper end thickness, the first lower end thickness, the second upper end thickness and the second lower end thickness.
In this embodiment, step 105 specifically includes:
determining a proportional function according to the first upper end thickness, the first lower end thickness, the second upper end thickness and the second lower end thickness.
Correcting the thickness of each layer of the film zone plate in the shot image according to a proportional function, wherein the specific formula is as follows:
wherein y is the thickness of each layer of the film zone plate after correction, and delta D1＝D1-D′1，ΔD2＝D2-D′2，D1Is a first upper end thickness, D2Is a first lower end thickness, D'1Is a second upper end thickness, D'2And the thickness of the second lower end is n, the total number of film layers of the multilayer film zone plate is n, and the thickness of each film zone plate in the shot image is x.
Example 2
This example is for designing WSi with total thickness R17242.61821 nm and 1435 layers in total2the/Si multilayer film zone plate is used for SEM (high-resolution electron microscope) positioning and film thickness characterization. The process is as follows:
(1) according to the structure of the multilayer film zone plate, 10 layers of WSi are respectively plated at the upper end and the lower end of the multilayer film zone plate2The thickness of the periodic film is 20 nm. Fig. 2 is a structural diagram of a multilayer film zone plate provided in an embodiment of the present invention, in which the upper and lower ends are periodic films, and the middle structure is a multilayer film zone plate.
(2) Periodic thicknesses of the upper and lower periodic films were characterized by GIXRR (grazing incidence X-ray reflection), and fitting gave a film thickness D1-20.799 nm at the upper end and D2-20.827 nm at the lower end, which was calculated to give a drift rate of 0.15%.
(3) And reading the thickness of the periodic film at the upper end and the lower end and the parameters of the film layer of the multilayer film zone plate by using SEM images to obtain the total thickness R1 of the multilayer film zone plate which is 17320.74158nm and has a deviation of 4.5 percent from the theoretical value.
(4) And comparing the periodic film thickness of the upper and lower periodic films obtained by the SEM with the GIXR fitting result, correcting the multi-layer film zone plate image shot by the SEM, wherein the corrected total thickness R2 is 17239.71492nm, and the error from the theoretical value is 0.2%.
(5) According to the correction result, the SEM image error of the multilayer film zone plate is reduced by 4.3%, the SEM image error is basically consistent with the drift rate of the coating film, and the accuracy of the correction method is verified.
Example 3
Fig. 3 is a structural diagram of a correction system based on an X-ray multilayer film zone plate according to an embodiment of the present invention, as shown in fig. 3, the system includes
A plating module 201 for plating N layers of periodic films on the upper and lower ends of the multilayer film zone plate; n is a positive integer greater than 2.
And the X-ray reflection testing module 202 is used for performing grazing incidence X-ray reflection testing on the plated N layers of periodic films and determining the periodic thicknesses of the N layers of periodic films plated at two ends, namely the first upper end thickness and the first lower end thickness.
And the shooting module 203 is used for shooting the multilayer film zone plate and the N layers of periodic films plated at the two ends by using an electron microscope to obtain a shot image.
The thickness reading module 204 is used for reading the thickness of each layer of the zone plate in the shot image and the thickness of the N layers of the periodic films plated at the two ends; the read thicknesses of the N layers of periodic films plated at two ends comprise a second upper end thickness and a second lower end thickness.
A correcting module 205, configured to correct the thickness of each layer of zone plate in the captured image according to the first upper end thickness, the first lower end thickness, the second upper end thickness, and the second lower end thickness.
According to the specific embodiment disclosed by the invention, the invention discloses the following technical effects:
on the basis of the original SEM characterization technology, the method is combined with a GIXRR method, periodic films are added on the upper surface and the lower surface of a multi-layer film zone plate, SEM images are corrected, SEM errors are corrected, and accurate high-resolution SEM image positioning and characterization are achieved.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. For the system disclosed by the embodiment, the description is relatively simple because the system corresponds to the method disclosed by the embodiment, and the relevant points can be referred to the method part for description.
The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (7)
1. A correction method based on an X-ray multilayer film zone plate is characterized by comprising the following steps:
plating N layers of periodic films on the upper end and the lower end of the multilayer film zone plate respectively; n is a positive integer greater than 2;
grazing incidence X-ray reflection test is carried out on the N layers of plated periodic films, and the periodic thickness of the N layers of plated periodic films at two ends is determined to be the first upper end thickness and the first lower end thickness;
shooting the multilayer film zone plate and the N layers of periodic films plated at two ends by using an electron microscope to obtain a shot image;
reading the thickness of each layer of the zone plate in the shot image and the thickness of the N layers of the periodic films plated at two ends; the read thickness of the N layers of periodic films plated at the two ends comprises a second upper end thickness and a second lower end thickness;
and correcting the thickness of each layer of the zone plate in the shot image according to the first upper end thickness, the first lower end thickness, the second upper end thickness and the second lower end thickness.
2. The correction method according to claim 1, wherein the X-ray source in the X-ray reflection test is a Cu-ka line, the wavelength is 0.154nm, and the test mode is a θ -2 θ linked scan mode.
3. The correction method according to claim 1, wherein the periodic thickness of the N layers of periodic films plated at both ends is determined by: and determining the periodic thickness of the N layers of periodic films plated at two ends according to a Bragg formula.
4. The correction method according to claim 3, wherein the Bragg formula is as follows:
wherein D is the period thickness of N layers of periodic films at the end to be measured, thetarThe grazing incidence angle corresponding to the r-th Bragg peak, q is the diffraction order, and lambda is the wavelength of X-ray and is the average refraction small quantity of the multilayer film.
5. The correction method according to claim 1, wherein the correcting the thickness of each layer of the zone plate in the captured image according to the first upper end thickness, the first lower end thickness, the second upper end thickness, and the second lower end thickness includes:
determining a proportional function according to the first upper end thickness, the first lower end thickness, the second upper end thickness and the second lower end thickness;
and correcting the thickness of each layer of the film zone plate in the shot image according to the proportional function.
6. The correction method according to claim 5, wherein the specific formula for correcting the thickness of each layer of the film zone plate in the captured image according to the proportional function is as follows:
wherein y is the thickness of each layer of the film zone plate after correction, and delta D1＝D1-D′1，ΔD2＝D2-D′2，D1Is a first upper end thickness, D2Is a first lower end thickness, D'1Is a second upper end thickness, D'2And the thickness of the second lower end is n, the total number of film layers of the multilayer film zone plate is n, and the thickness of each film zone plate in the shot image is x.
7. An X-ray multilayer film zone plate-based correction system is characterized by comprising:
the plating module is used for plating N layers of periodic films on the upper end and the lower end of the multilayer film zone plate respectively; n is a positive integer greater than 2;
the X-ray reflection testing module is used for carrying out grazing incidence X-ray reflection testing on the plated N layers of periodic films and determining the periodic thicknesses of the N layers of periodic films plated at two ends, namely the thickness of the first upper end and the thickness of the first lower end;
the shooting module is used for shooting the multilayer film zone plate and the N layers of periodic films plated at two ends by using an electron microscope to obtain a shot image;
the thickness reading module is used for reading the thickness of each layer of the zone plate in the shot image and the thickness of the N layers of the periodic films plated at two ends; the read thickness of the N layers of periodic films plated at the two ends comprises a second upper end thickness and a second lower end thickness;
and the correcting module is used for correcting the thickness of each layer of the zone plate in the shot image according to the first upper end thickness, the first lower end thickness, the second upper end thickness and the second lower end thickness.
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| CN113903488A (en) * | 2021-09-30 | 2022-01-07 | 中国科学院高能物理研究所 | Single-order diffraction Laue lens and manufacturing method thereof |
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| CN106756864A (en) * | 2016-12-10 | 2017-05-31 | 中国科学院长春光学精密机械与物理研究所 | One kind prepares non-sensitive layer error control method and device in multilayer film element process |
| CN107893216A (en) * | 2017-09-30 | 2018-04-10 | 同济大学 | A kind of method corrected quartzy monitoring method and prepare broadband anti-reflection film deposition errors |
| CN209098790U (en) * | 2019-01-23 | 2019-07-12 | 天宫真空科技(广州)有限公司 | Adjustable film coating correction plate mechanism |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106756864A (en) * | 2016-12-10 | 2017-05-31 | 中国科学院长春光学精密机械与物理研究所 | One kind prepares non-sensitive layer error control method and device in multilayer film element process |
| CN107893216A (en) * | 2017-09-30 | 2018-04-10 | 同济大学 | A kind of method corrected quartzy monitoring method and prepare broadband anti-reflection film deposition errors |
| CN209098790U (en) * | 2019-01-23 | 2019-07-12 | 天宫真空科技(广州)有限公司 | Adjustable film coating correction plate mechanism |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113903488A (en) * | 2021-09-30 | 2022-01-07 | 中国科学院高能物理研究所 | Single-order diffraction Laue lens and manufacturing method thereof |
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