CN114481063A - Multilayer film polarizer and preparation method thereof - Google Patents
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- 238000004544 sputter deposition Methods 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 7
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- 238000000576 coating method Methods 0.000 description 3
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- G02B5/30—Polarising elements
- G02B5/3025—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state
- G02B5/3033—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid
- G02B5/3041—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid comprising multiple thin layers, e.g. multilayer stacks
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Abstract
The invention relates to a multilayer film polarizer and a preparation method thereof. According to the multilayer film polarizer provided by the invention, the periodic multilayer films are plated at different positions in the transverse direction (namely the first material layer and the second material layer are alternately arranged, and the thicknesses of the first material layer and the second material layer and the gradient along the transverse direction are increased), so that the working bandwidth of the polarizer can be expanded by only translating the polarizer in use aiming at different working energy points, further the polarized optical element with continuously adjustable working energy of 400 + 1000eV can be realized, and the polarization detection effect and accuracy are improved.
Description
Technical Field
The invention relates to the technical field of optical elements and preparation thereof, in particular to a multilayer film polarizer and a preparation method thereof.
Background
In order to achieve high polarization performance of soft X-ray beams, determine the polarization state of incident light, and inspect the polarization state of outgoing light, polarization measurement devices are constructed using polarization elements. Different polarizing optical elements are required according to different working energies. However, in the soft X-ray energy region, all materials are strongly absorbing and thus effective polarization cannot be obtained with transmission methods. The refractive index of any material is close to 1, and the reflectivity of a single interface is very low according to the Fresnel formula, so that the reflective polarizing element cannot be manufactured by a multi-reflection method of a single-layer interface. In addition, there is no natural crystal in nature whose lattice constant matches the wavelength of this band. Therefore, the polarization element of this energy region needs to be developed by a special method.
The soft X-ray multilayer film can effectively increase the reflectivity under the non-grazing incidence condition, and is an important optical element in a soft X-ray energy area. The multilayer film polarizing element with wide energy spectrum bandwidth not only has high reflectivity, but also can cover a large energy spectrum range. There are two types of broadband multilayer films. One approach is to provide a non-periodic multilayer film, each of which has a different thickness and is distributed in a substantially gradient manner in the longitudinal direction, so that different layers reflect incident light of different wavelengths, thereby achieving bandwidth expansion. However, for soft X-rays with higher energy (shorter wavelength), such as energy band of 400-.
Disclosure of Invention
In order to solve the above problems in the prior art, the present invention provides a multilayer film polarizer and a method for manufacturing the same.
In order to achieve the purpose, the invention provides the following scheme:
a multilayer film polarizer, comprising: a first material layer and a second material layer;
the first material layers and the second material layers are alternately arranged; the thickness and the transverse gradient of the first material layer and the second material layer are increased.
Preferably, the first material layer is WSi2Film or W film.
Preferably, when the first material layer is WSi2When the film is formed, the second material layer is a Si film layer;
when the first material layer is a W film layer, the second material layer is B4And C, a film layer.
Preferably, the WSi2The thickness of the film layer and the Si film layer is in the range of 1.5nm-2.03 nm.
Preferably, the W film layer and the B4The thickness of the C film layer is 1.13nm-2.18 nm.
Preferably, the WSi2The thickness and the gradient along the transverse direction of the film layer and the Si film layer are increased gradually and are 0.018 nm/mm.
Preferably, the W film layer and the B4The thickness and the gradient of the C film layer increasing along the transverse direction are 0.021 nm/mm.
Preferably, the thickness ratio of the first material layer to the second material layer ranges from 0.2 to 0.8.
The invention also provides a preparation method of the multilayer film polarizer, which comprises the following steps:
alternately preparing a first material layer and a second material layer on the substrate by adopting a direct-current magnetron sputtering method and a time control method until the periodicity of the first material layer and the second material layer meets the preset requirement to obtain the multilayer film polarizer;
the thickness of the first material layer and the second material layer increases along the transverse gradient in the preparation process.
Preferably, a formula is adopted
Determining a sputter thickness of the first material layer or a sputter thickness of the second material layer;
using a formula
Determining the film thickness of one point on the first material layer or one point on the second material layer;
wherein t is the sputtering thickness, mxThe molar mass of the sputtered material, h is the target base distance, r is the equivalent etching ring radius, a is the position from the calculated point to the center of the substrate, and a is (x)2+y2)1/2(x, y) is the position coordinate of the center of the substrate, x1Is the initial position of a point on the first material layer or the second material layer passing through the sputtering zone, x2The end position of a point on the first material layer or the second material layer which passes through the sputtering area is defined as rho, the target density is defined as t/t0Is the sputtering thickness at a-0, vt0Deposition rate of sputtered particles at zero point, vsub(x) The rate at which a point on the material layer passes over the target, T (y) the thickness of a point on the first material layer or a point on the second material layer, [1+ f (a)]t/t0For the film relative thickness distribution, f (a) is an additional polynomial term introduced.
According to the specific embodiment provided by the invention, the invention discloses the following technical effects:
according to the multilayer film polarizer provided by the invention, the periodic multilayer films are plated at different positions in the transverse direction (namely the first material layer and the second material layer are alternately arranged, and the thicknesses of the first material layer and the second material layer and the gradient along the transverse direction are increased progressively), so that the working bandwidth of the polarizer can be expanded by only translating the polarizer in use aiming at different working energy points, and further the polarized optical element with continuously adjustable working energy of 400-1000eV can be realized, and the effect and the accuracy of polarization detection are 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 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 creative efforts.
FIG. 1 is a schematic structural diagram of a multilayer film polarizer provided by the present invention;
FIG. 2 is a graph of the results of testing a multilayer film polarizer for P-polarized light and S-polarized light at a grazing incidence angle of 45 (quasi-Brewster' S angle) provided by an embodiment of the present invention; wherein, fig. 2(a) is a test result graph of the multilayer film polarizer on P polarized light when the grazing incidence angle is 45 °, and fig. 2(b) is a test result graph of the multilayer film polarizer on S polarized light when the grazing incidence angle is 45 °;
fig. 3 is a schematic diagram of the polarization rate distribution with energy of a multilayer film polarizer at a grazing incidence angle of 45 ° 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 multilayer film polarizer and a preparation method thereof, which can effectively expand the bandwidth of the polarizer, realize the polarization detection of soft X-rays with higher energy and further improve the effect and the accuracy of the polarization detection.
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.
As shown in fig. 1, the present invention provides a multilayer film polarizer comprising: a first material layer H and a second material layer L.
The first material layers H and the second material layers L are alternately disposed. The thicknesses and the gradients of the first material layer H and the second material layer L increase along the transverse direction.
The material selection of the soft X-ray transverse broadband gradient multilayer film polarizer mainly comprises the following principles: starting from the optical principle, the absorption rate of the materials in the designed energy band is required to be as small as possible, and the refractive index difference of the two materials is larger, so that the absorption rate is the same as that of the materialsThe two materials are required to have no mutual reaction and diffusion, stable physical and chemical properties and no toxicity. Therefore, in response to the energy band requirement of 400-1000eV (covering the L absorption edge and the 'water window' energy band of Fe, Co and Ni), the invention selects W/B4C and WSi2Film pair of/Si. In particular, the method comprises the following steps of,
when the first material layer is WSi2When the film is formed, the second material layer is a Si film. When the first material layer is W film layer, the second material layer is B4And C, a film layer.
When the design is in practical application, the W/B is periodically arranged for different material layers4C, the bottom layer of the multilayer film is W, and the top layer is B4And C, alternately plating a double-layer structure multilayer film on the two materials to obtain the polarizer. WSi2The bottom layer of the/Si multilayer film is WSi2The top layer is Si, and the two materials are alternately plated with a double-layer structure multilayer film to obtain the polarizer.
The multilayer film polarizer provided based on the above and the main preparation method thereof comprise:
and alternately preparing the first material layer and the second material layer on the substrate by adopting a direct-current magnetron sputtering method and a time control method until the periodicity of the first material layer and the second material layer meets the preset requirement to obtain the multilayer film polarizer. Wherein, the thickness of the first material layer and the thickness of the second material layer are increased along the transverse gradient in the preparation process.
The design principle and implementation process of the multilayer film polarizer and the preparation method thereof provided above will be described in detail by referring to an embodiment, but in practical application, the design principle and implementation process are not limited to the example of the embodiment.
In this embodiment, the preparation and implementation process of the multilayer film polarizer is written by using a multilayer film recurrence formula of the thin film optical theory. Carrying out optimization design by utilizing a simplex optimization algorithm, wherein the parameters of the designed multilayer film polarizing element comprise: the material selected for the corresponding segment, the period thickness d of the multilayer film, the period number N of the film layer, the thickness ratio gamma and the grazing incidence angle theta.
The quasi-brewster angle of the film layer is typically around a 45 ° angle of incidence (the refractive index of soft X-ray band materials is very close to 1). Light is incident at a 45 angle and the reflectivity of the multilayer film for the s and p light components can be several orders of magnitude different, thus obtaining the desired polarization. And selecting initial conditions during optimization design, optimizing the period thickness d and the film thickness ratio gamma, and determining to meet the requirements of high polarization rate and reflectivity.
In order to take account of both the reflectivity and the polarization performance, the present embodiment designs and measures two incident angles of 45 ° and 30 °, respectively. WSi is respectively designed aiming at the 400-fold 1000eV energy section of the soft X-ray2[ W/B ] and/or Si4And C, two multi-layer film systems. In this embodiment, WSi2The period thickness range of the/Si gradient multilayer film is 1.15nm-2.03 nm. W/B4The period thickness range of the C gradient multilayer film is 1.13nm-2.18 nm.
For example, with the WSi2/Si gradient multilayer film sample prepared, p-polarized light and s-polarized light were measured at every 2.5mm in the long-side direction of the sample, respectively, and the grazing incidence angle was 45 ° (quasi-Brewster's angle), Rs(reflectance of S-polarized component of light) and RpThe curve of the change in (reflectance of the P-polarized component of light) with wavelength is shown in fig. 2.
In this embodiment, the preparation of the nano-periodic multilayer film is realized by a magnetron sputtering coating technology. The magnetron sputtering coating technology has stable process and good repeatability, and the thickness of the film layer can be controlled by using a time control method. When preparing X-ray multilayer film, the control error of film thickness can reach 0.01nm, and under the condition that the film number is more than 100, the whole thickness error of film system is less than 0.05 nm. In the embodiment, the deposition rates of different positions of the substrate are corrected by the programmed film thickness correction template and the grazing target speed regulation method, so that the transverse gradient periodic multilayer film plating is realized. WSi2The thickness gradient of the/Si gradient multilayer film is 0.018nm/mm, and the W/B4The thickness gradient of the C gradient multilayer film is 0.021 nm/mm.
The surface shape of the thin film on the substrate is mainly determined by the initial surface shape of the substrate and the spatial distribution of the sputtered particles. In the preparation process of the film layer, the particle density right above the target gun is the largest, the particle density far away from the target gun is small, the thickness of the deposited film is in the distribution of thick middle and thin edge. In magnetron sputtering, the thickness distribution of particles from a ring-shaped sputtering source deposited on a stationary substrate can be given by the following formula:
wherein t is the film thickness, mxThe mass (molar mass) of the sputtering material, h is the target base distance, r is the equivalent etching ring radius, a is the position from the calculation point to the center of the substrate, and rho is the density of the target material. The relative thickness distribution t/t can be utilized0To describe the film thickness distribution, t/t0Is the thickness at a-0. In the formula of the relative thickness distribution, mxAnd p will be eliminated and other parameters can be obtained by experimental measurements. During the actual experiment, in order to better describe the actual film thickness distribution, an additional polynomial term f (a) was introduced to fit the difference between the experiment and the theoretical calculation. Thus, the final film relative thickness distribution is [1+ f (a)]t/t0。
A linear type coating machine is adopted to prepare the multilayer film, the moving direction of a substrate is set to be an X-axis direction, the direction which is perpendicular to the moving direction and is parallel to a target surface is set to be a Y-axis direction, and the position corresponding to the center of the target is set to be a zero point. When the substrate is at a velocity vsub(x) The film thickness at a certain point p on the substrate when sweeping the target source is:
vt0deposition rate of sputtered particles at zero point, vsub(x) The rate at which point p sweeps across the target, a ═ x2+y2)1/2，x1And x2Corresponding to the initial and end positions of the p-point sweep of the sputtering zone. Let T (Y) in the above equation be equal to the designed gradient film thickness profile, i.e., linearly smaller in the Y direction. The size of the opening above the shielding cylinder of the target source is 80mm x 72 mm. Let x1X can be calculated by a computer at-40 mm2And (4) obtaining a value, namely a profile curve corresponding to the mask plate. The samples of this example were tested for optical and polarization properties in a Diamond illuminant of the uk.
Designing and preparing a broadband gradient multilayer film according to the requirements of I21 inelastic scattering experiments newly built by a Diamond light source in UK, and designing WSi corresponding to the energy band of 400-1000eV in the example2a/Si periodic multilayer film. WSi (Wireless sensor network interface)2The period thickness range of the/Si gradient multilayer film is 1.15nm-2.03nm, and the thickness gradient is 0.018 nm/mm. In order to take both the reflectivity and the polarization performance into consideration, two incidence angles of 45 degrees and 30 degrees are respectively designed and measured.
The average polarization degree at the quasi-Brewster angle of 45 degrees is 99.38 percent, and the highest polarization rate reaches 99.77 percent. WSi2The maximum reflectance of the/Si gradient multilayer film is 4.05% at 30 DEG incidence with the energy of 638 eV. The continuously adjustable broadband polarization element with the working energy covering the absorption edges of Fe, Co and Ni materials L and the energy section of a water window is realized. As shown in FIG. 3, the test is at a 45 ° angle, WSi2The polarization rate of the/Si gradient multilayer film is along with the energy distribution curve, the difference is not limited, the polarization rate is close to 99 percent, and the measurement requirement of polarization application can be met. Comparison of measurements at a reflectivity bandwidth (resolution) of 500eV, obtained by data fitting, WSi2The bandwidth of/Si is 4.02.
By adopting the method of the invention, the W/B is designed and prepared in the example according to the requirements of I21 inelastic scattering experiment newly built by a Diamond light source in England and the energy band of 400- & lt 1000eV4The C gradient multilayer film respectively designs and measures two incident angles of 45 degrees and 30 degrees in order to give consideration to reflectivity and polarization performance.
The average polarization degree at the quasi-Brewster angle of 45 degrees is 99.55 percent, and the highest polarization rate reaches 99.71 percent. Under the condition of 30-degree incidence, the highest reflectivity reaches 2.67%. The continuously adjustable broadband polarization element with the working energy covering the absorption edges of Fe, Co and Ni materials L and the energy section of a water window is realized. As shown in FIG. 3, the test was conducted at an angle of 45 DEG, W/B4The polarization rate of the C gradient multilayer film is along with the energy distribution curve, no difference is limited, the polarization degree is close to 99 percent, and the measurement requirement of polarization application can be met. Comparison of measurements at a reflectivity bandwidth (resolution) of 500eV, obtained by data fitting, W/B4The bandwidth of C is 8.45 eV.
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.
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 (10)
1. A multilayer film polarizer, comprising: a first material layer and a second material layer;
the first material layers and the second material layers are alternately arranged; the thickness and the transverse gradient of the first material layer and the second material layer are increased.
2. The multilayer film polarizer of claim 1, wherein the first material layer is WSi2Film or W film.
3. The multilayer film polarizer of claim 2, wherein when the first material layer is WSi2When the film is formed, the second material layer is a Si film layer;
when the first material layer is a W film layer, the second material layer is B4And C, a film layer.
4. The multilayer film polarizer of claim 3, wherein the WSi2The thickness of the film layer and the Si film layer is in the range of 1.5nm-2.03 nm.
5. The multilayer film polarizer of claim 3, wherein the W film layer and the B film layer4The thickness of the C film layer is 1.13nm-2.18 nm.
6. The multilayer film polarizer of claim 3, wherein WSi is2The thickness and the gradient along the transverse direction of the film layer and the Si film layer are increased gradually and are 0.018 nm/mm.
7. The multilayer film polarizer of claim 3, wherein the W film layer and the B film layer4The thickness and the gradient of the C film layer increasing along the transverse direction are 0.021 nm/mm.
8. The multilayer film polarizer of claim 1, wherein the thickness ratio of the first material layer to the second material layer ranges from 0.2 to 0.8.
9. A method of making a multilayer film polarizer, comprising:
alternately preparing a first material layer and a second material layer on a substrate by adopting a direct current magnetron sputtering method and a time control method until the periodicity of the first material layer and the second material layer meets a preset requirement to obtain the multilayer film polarizer as claimed in any one of claims 1 to 8;
the thickness of the first material layer and the second material layer increases along the transverse gradient in the preparation process.
10. The method of claim 9, wherein the formula is adopted
Determining a sputter thickness of the first material layer or a sputter thickness of the second material layer;
using a formula
Determining the film thickness of one point on the first material layer or one point on the second material layer;
wherein t is the sputtering thickness, mxIs the molar mass of the sputtered material, and h is the target base distanceR is the equivalent etch ring radius, a is the position from the calculated point to the center of the substrate, and a ═ x2+y2)1/2(x, y) is the position coordinate of the center of the substrate, x1Is the initial position of a point on the first material layer or the second material layer passing through the sputtering zone, x2Is the end position of a point on the first material layer or the second material layer which passes through the sputtering area, rho is the target density, t/t0Is the sputtering thickness at a-0, vt0Deposition rate of sputtered particles at zero point, vsub(x) The rate at which a point on the material layer passes over the target, T (y) the thickness of a point on the first material layer or a point on the second material layer, [1+ f (a)]t/t0For the film relative thickness distribution, f (a) is an additional polynomial term introduced.
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| CN1556422A (en) * | 2004-01-06 | 2004-12-22 | 同济大学 | Flexible X-ray reflection type multipayer film broad band poarizer and its preparation method |
| US20140072106A1 (en) * | 2009-12-14 | 2014-03-13 | Brookhaven Science Associates | Zone compensated multilayer laue lens and apparatus and method of fabricating the same |
| CN108165926A (en) * | 2017-12-18 | 2018-06-15 | 苏州宏策光电科技有限公司 | The method of the Mo/Si multilayer films of direct magnetic control technology manufacturing cycle thickness transverse direction two-dimensional gradient distribution |
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| CN1556422A (en) * | 2004-01-06 | 2004-12-22 | 同济大学 | Flexible X-ray reflection type multipayer film broad band poarizer and its preparation method |
| US20140072106A1 (en) * | 2009-12-14 | 2014-03-13 | Brookhaven Science Associates | Zone compensated multilayer laue lens and apparatus and method of fabricating the same |
| CN108165926A (en) * | 2017-12-18 | 2018-06-15 | 苏州宏策光电科技有限公司 | The method of the Mo/Si multilayer films of direct magnetic control technology manufacturing cycle thickness transverse direction two-dimensional gradient distribution |
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