CN116299813A - Reflective polarization grating with high depth-to-width ratio and narrow period and preparation method thereof - Google Patents
Reflective polarization grating with high depth-to-width ratio and narrow period and preparation method thereof Download PDFInfo
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- CN116299813A CN116299813A CN202310115946.1A CN202310115946A CN116299813A CN 116299813 A CN116299813 A CN 116299813A CN 202310115946 A CN202310115946 A CN 202310115946A CN 116299813 A CN116299813 A CN 116299813A
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- C—CHEMISTRY; METALLURGY
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- G02B5/3058—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state comprising electrically conductive elements, e.g. wire grids, conductive particles
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- G—PHYSICS
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- Engineering & Computer Science (AREA)
- General Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Mechanical Engineering (AREA)
- Metallurgy (AREA)
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- Polarising Elements (AREA)
Abstract
The invention discloses a reflective polarization grating with high aspect ratio and narrow period and a preparation method thereof, wherein the method comprises the following steps: s1, uniformly coating photoresist on the surface of a flexible substrate; s2, transferring the pattern of the wide-period grating template to the photoresist through nano imprinting; s3, curing by using UV light; s4, plating a metal film by a physical or chemical vapor deposition method; s5, plasma etching is used for thinning; s6, removing the residual photoresist grating structure. The invention provides a method for manufacturing a narrow period polarization grating by using a wide period grating nano imprinting template, and the preparation process and the difficulty of the wide period grating template are far smaller than those of the narrow period grating template, so that the process can obviously improve the efficiency and save the cost in mass production; the invention can lay a foundation for the preparation process and practical application of the reflective polarization grating which can be prepared in a large area, has better repeatability, controllable size and excellent polarization characteristic.
Description
Technical Field
The invention relates to the technical field of optics, in particular to a reflective polarization grating with high aspect ratio and narrow period and a preparation method thereof.
Background
With the continuous development of micro-nano processing technology, the optical component with the dimensions of submillimeter, micrometer and even nanometer can provide higher integration level and stability for an optical system, and further meet the requirements of miniaturization, batch and low cost of photoelectric display devices and imaging devices. The form and kind of consumer electronics products represented by VR (Virtual Reality), AR (Augmented Reality ), MR (Mixed Reality), XR (Extended Reality) are endless. The reflective polarization brightness enhancement film is used as a core component of the light path system, and plays important roles of enhancing brightness, widening a viewing angle, improving image contrast and the like. Theory proves that the sub-wavelength grating has reflection polarization characteristics, can realize the transmission/reflection function of light in a specific polarization direction, and compared with the traditional absorption type polaroid, the reflection type polarization grating has the advantages of no incidence angle limitation, excellent heat resistance and moisture resistance, capability of realizing cutting of complex shapes, bonding with other materials, curved surface forming and the like.
The reflective brightness enhancement film, also known as a reflective polarizer, can recycle S polarized light, thereby improving the utilization of the incident light energy. As a core component of polarization imaging (LCD, OLED, VR, etc.), the reflective brightness enhancement film on the market is mainly monopolized by the us 3M company.
The sub-wavelength metal polarization grating also has the characteristic of P polarized light transmission and S polarized light reflection, and is very expected to become another breakthrough direction of the new generation of wide-angle highlighting display technology. Therefore, how to realize high transmission of P polarized light and high reflection of S polarized light of the sub-wavelength metal grating, thereby breaking the technical monopoly of the U.S. 3M company, has become one of the key points of development of display technology under the eyes and in the future.
In general, the preparation of the sub-wavelength metal polarization grating is not separated from a high-precision mask plate, in order to improve the polarization degree and imaging quality of the grating, the period size of the grating needs to be controlled to be in the order of hundred nanometers, and in order to improve the imaging color saturation, the depth-to-width ratio of the grating needs to be as large as possible. The preparation process of the high-precision mask plate mainly depends on holographic lithography, electron beam etching and other modes. Holographic lithography exposes the photoresist through interference fringes between light and dark formed by two beams of coherent light, and forms periodic spatial distribution with refractive index difference on a molecular level. The grating prepared by holographic lithography has extremely high diffraction efficiency, but is limited by Bragg diffraction conditions, so that the problem of color uniformity is difficult to solve, and the market demand cannot be met. The electron beam etching is to accurately draw a pattern on the photoresist by using a high-energy electron beam, so that the etching precision is very high, but the efficiency is very low, the plate making period is long, and the electron beam etching equipment is high in price and has no advantage in the aspect of mass production. In addition, the thickness of the metal grating deposited/evaporated by sputtering is usually 50-150 nm, resulting in the aspect ratio of the grating being 0.5-1.5, and the lower aspect ratio is also an important factor in the difficult application of the polarization grating in the display field.
Therefore, the development of a manufacturing process with higher cost performance, which can effectively shorten the grating period and improve the grating depth-to-width ratio, has important theoretical significance and engineering application value for realizing the high-stability roll-to-roll reflective polarization grating mass production technology. Patent CN 114296168A proposes a narrow grating pattern transfer scheme with variable period, wherein the width of the grating pattern is controlled by controlling the thickness of silicon oxide deposited on the side surface of the imprint resist layer pattern, so as to obtain a narrow grating pattern with high aspect ratio, but the pattern transfer process requires three plasma etching techniques, and the substrate material, imprint resist and silicon oxide require special types to realize selective etching, so that the whole process flow is complex.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a reflective polarization grating with high aspect ratio and narrow period and a preparation method thereof aiming at the defects in the prior art.
In order to solve the technical problems, the invention adopts the following technical scheme: a preparation method of a reflective polarization grating with high aspect ratio and narrow period comprises the following steps:
s1, uniformly coating photoresist on the surface of a flexible substrate;
s2, transferring the pattern of the wide-period grating template to the photoresist through nano imprinting;
s3, curing the photoresist by utilizing UV light, and removing the wide-period grating template to obtain a photoresist grating structure with a wide-period grating pattern;
s4, plating a metal film on the surface of the photoresist grating structure by a physical or chemical vapor deposition method, and covering the photoresist grating structure to form a metal grating structure;
s5, etching and thinning the top of the metal grating structure and the grooves by utilizing plasma etching, wherein the etching depth is consistent with the thickness of the film layer of the metal grating structure;
and S6, removing the residual photoresist grating structure to obtain a metal grating structure formed on the surface of the flexible substrate, and obtaining the reflective polarization grating with high aspect ratio and narrow period.
Preferably, in the step S4, a metal film is plated on the surface of the photoresist grating structure by using an electron beam evaporation, magnetron sputtering or atomic layer deposition process.
Preferably, in the step S4, a metal film is plated on the surface of the photoresist grating structure by using a roll-to-roll ALD process.
Preferably, the metal film is a metal simple substance film or a metal alloy film.
Preferably, the metal film is an aluminum film or an aluminum alloy film.
Preferably, the roll-to-roll ALD method adopted in the step S4 specifically includes:
trimethyl aluminum is used as a precursor A, hydrogen is used as a precursor B, and space atomic layer deposition equipment is adopted to realize roll-to-roll deposition of an aluminum film layer on the surface of a photoresist grating structure under the assistance of plasma;
in the roll-to-roll deposition process, the vacuum degree of the coating chamber is 1 multiplied by 10 -3 Pa, the temperature of the film coating roller is 0 degree, the flow rates of trimethylaluminum and hydrogen are respectively set to be 60sccm and 100sccm, and the running speed of the film coating roller is set to be 0.1m/min to 1m/min.
Preferably, in the step S5: etching and thinning the top and the groove of the metal grating structure by adopting inductively coupled plasma, and etching gas Cl 2 Ar, gas flow rate of 8sccm to ultraThe etching power is between 400 and 800W, the etching bias voltage can be between-65 and-150V, and the etching rate is between 50 and 150nm/min correspondingly.
Preferably, the etching and thinning process using the inductively coupled plasma in the step S5 is as follows: etching gas Cl 2 Ar, the gas flow rate is 8sccm, 18sccm in sequence, the etching power is 400W, the etching bias voltage is-65V, the corresponding etching rate is 50nm/min, the etching direction is vertical to the upper surface of the metal grating structure, and the etching time is 1min.
Preferably, the flexible substrate is a cellulose triacetate film having a thickness of 40 μm to 80 μm.
The invention also provides a reflective polarization grating with high aspect ratio and narrow period, which is prepared by the method.
The beneficial effects of the invention are as follows:
(1) The preparation of the high-aspect-ratio and narrow-period reflective polarization grating can be realized through single etching and single developing processes, and compared with a traditional reflective brightness enhancement film, the polarization separation generated by the sub-wavelength nano grating has excellent polarization separation function in the longer wavelength fields of visible light, infrared rays and the like;
(2) The invention provides a method for manufacturing a narrow period polarization grating by using a wide period grating nano imprinting template, and the preparation process and the difficulty of the wide period grating template are far smaller than those of the narrow period grating template, so that the process can obviously improve the efficiency and save the cost in mass production; the invention can lay a foundation for the preparation process and practical application of the reflective polarization grating which can be prepared in a large area, has better repeatability, controllable size and excellent polarization characteristic.
(3) The high aspect ratio and narrow period reflection type polarization grating prepared by the invention has TM transmittance higher than that of the traditional wide period polarization grating, TE reflectivity lower than that of the traditional wide period polarization grating, and extinction ratio is greatly improved, and meanwhile, the high-aspect ratio and narrow period reflection type polarization grating has excellent heat resistance and moisture resistance; the flexible substrate is used, so that the flexible substrate can realize cutting of complex shapes, and has the advantages of being beneficial to bonding with other materials, forming curved surfaces and the like.
Drawings
FIG. 1 is a process flow diagram of a method of fabricating a high aspect ratio, narrow period reflective polarization grating of the present invention;
fig. 2: (a) Comparing uniformity of different coating processes, (b) performing a schematic diagram of a roll-to-roll atomic layer deposition process;
FIG. 3 is a graph showing specific parameters of a wide period grating template and a high aspect ratio, narrow period reflective polarization grating prepared in example 1;
fig. 4: (a) A conventional broad period grating polarizer spectral diagram, (b) a narrow period grating polarizer spectral diagram prepared in example 1;
FIG. 5 shows the results of high aspect ratio, narrow period polarization grating 60 ℃, 90% RH, 1000hr reliability testing prepared in example 1.
Reference numerals illustrate:
1-a flexible substrate; 2-photoresist; 3-a wide period grating template; 4-metal grating structure.
Detailed Description
The present invention is described in further detail below with reference to examples to enable those skilled in the art to practice the same by referring to the description.
It will be understood that terms, such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
The test methods used in the following examples are conventional methods unless otherwise specified. The material reagents and the like used in the following examples are commercially available unless otherwise specified. The following examples were conducted under conventional conditions or conditions recommended by the manufacturer, without specifying the specific conditions. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The invention provides a preparation method of a reflective polarization grating with high aspect ratio and narrow period, referring to FIG. 1, comprising the following steps:
s1, uniformly coating photoresist 2 on the surface of a flexible substrate 1;
in a preferred embodiment, the flexible substrate 1 is a cellulose triacetate film having a thickness of 40 μm to 80 μm;
s2, transferring the pattern of the wide-period grating template 3 to the photoresist 2 through nano imprinting;
s3, curing the photoresist 2 by utilizing UV light, and removing the wide-period grating template 3 through a demolding procedure to obtain a photoresist grating structure with a wide-period grating pattern;
s4, plating a metal film on the surface of the photoresist grating structure by a physical or chemical vapor deposition method, and covering the photoresist grating structure to form a metal grating structure 4;
in the invention, the surface of the photoresist grating structure can be plated with a metal film by adopting an electron beam evaporation, magnetron sputtering or atomic layer deposition process, and in a preferred embodiment, the surface of the photoresist grating structure can be plated with a metal film by adopting an atomic layer deposition process, more preferably, a roll-to-roll ALD (space atomic layer deposition) process, which comprises the following steps:
trimethyl aluminum is used as a precursor A, hydrogen is used as a precursor B (reducing agent), and space type atomic layer deposition equipment is adopted to realize roll-to-roll deposition of an aluminum film layer on the surface of a photoresist grating structure under the assistance of plasma;
in the roll-to-roll deposition process, the vacuum degree of the coating chamber is 1 multiplied by 10 -3 Pa, the temperature of the film coating roller is 0 degree, the flow rates of trimethylaluminum and hydrogen are respectively set to be 60sccm and 100sccm, and the running speed of the film coating roller is set to be 0.1m/min to 1m/min.
In the deposition process, trimethylaluminum and hydrogen are sequentially and alternately formed into a single-layer saturated adsorption (self-limiting) on the surface of the substrate, meanwhile, precursors are kept physically separated through an intermediate inert gas (Ar) purging step (refer to fig. 3 b), and the accurate growth of the thickness of the aluminum film is realized by exposing the substrate to positions containing different precursors. ALD is more applicable to three-dimensional micro-nano structure samples than traditional PVD and CVD coating modes (refer to FIG. 3 a); the thickness of the deposited metal film layer is controlled by changing the cycle size according to the requirement.
Wherein the metal film is a metal simple substance film or a metal alloy film, and in a preferred embodiment, the metal film is an aluminum film or an aluminum alloy film.
S5, etching and thinning the top and the groove of the metal grating structure 4 by utilizing Inductively Coupled Plasma (ICP), wherein the etching depth is consistent with the thickness of the film layer of the metal grating structure 4;
specifically, the top and the groove of the metal grating structure 4 are etched and thinned by using inductively coupled plasma, and etching gas Cl 2 Ar, the gas flow rate is 8 sccm-20 sccm, the etching power is 400-800W, the etching bias voltage can be selected to be-65-150V, and the corresponding etching rate is 50-150 nm/min.
And S6, removing the residual photoresist grating structure by adopting a developing process to obtain a metal grating structure 4 formed on the surface of the flexible substrate 1, and thus obtaining the reflective polarization grating with high aspect ratio and narrow period.
Example 1
A reflection type polarization grating with high aspect ratio and narrow period is prepared by the following steps:
s1, uniformly coating photoresist on the surface of a flexible substrate;
the flexible substrate (C) is a cellulose triacetate film with the thickness of 40-80 mu m;
s2, transferring the pattern of the wide-period grating template (A) to photoresist through nano imprinting;
in this embodiment, the wide-period grating template (a) is a nickel plate, and specific parameters of the wide-period grating are: period of grating mask plate (P) 1 ) 200nm, line width (W 1 ) 150nm, height (H 1 ) 150nm, and a corresponding aspect ratio (height/line width) of 1;
s3, curing the photoresist by utilizing UV light, and removing the wide-period grating template through a demolding procedure to obtain a photoresist grating structure with a wide-period grating pattern;
s4, plating a 50nm metal film on the surface of the photoresist grating structure by adopting a roll-to-roll ALD (space atomic layer deposition) process, so as to cover and form a metal grating structure (B) on the photoresist grating structure;
the specific process comprises the following steps: trimethyl aluminum is used as a precursor A, hydrogen is used as a precursor B, and space atomic layer deposition equipment is adopted to realize roll-to-roll deposition of an aluminum film layer on the surface of a photoresist grating structure under the assistance of plasma;
in the roll-to-roll deposition process, the vacuum degree of the coating chamber is 1 multiplied by 10 -3 Pa, the temperature of the film coating roller is 0 degree, the flow rates of trimethylaluminum and hydrogen are respectively set to be 60sccm and 100sccm, and the running speed of the film coating roller is set to be 0.1m/min to 1m/min.
S5, etching and thinning the top of the metal grating structure and the grooves by utilizing Inductively Coupled Plasma (ICP), wherein the etching depth is consistent with the thickness of the film layer of the metal grating structure;
the specific etching process comprises the following steps: etching gas Cl 2 Ar, the gas flow rate is 8sccm, 18sccm in sequence, the etching power is 400W, the etching bias voltage is-65V, the corresponding etching rate is 50nm/min, the etching direction is vertical to the upper surface of the metal grating structure, and the etching time is 1min.
S6, removing the residual photoresist grating structure by adopting a developing process to obtain a metal grating structure formed on the surface of the flexible substrate, namely the reflective polarization grating with high aspect ratio and narrow period, wherein the specific parameters are as follows: period (P) 2 ) 100nm of line width (W 2 ) 50nm, height (H 2 ) 150nm, a corresponding aspect ratio (height/linewidth) of 3; i.e. the grating aspect ratio is improved by a factor of 3. Specific parameters of the wide-period grating template (A) and the high-aspect-ratio and narrow-period reflective polarization grating prepared by the embodiment are shown in fig. 3, wherein the metal mask plate is the wide-period grating template (A).
Referring to fig. 4 (a) and fig. 4 (b) for comparing the optical performance of the wide-period grating prepared by the conventional scheme and the narrow-period grating prepared by the embodiment 1 of the present invention, it can be seen that the present invention can obtain a high aspect ratio, narrow-period reflective polarization grating product which is difficult to obtain by the conventional scheme, the TM transmittance of the present invention is higher than that of the conventional wide-period polarization grating, the TE reflectance is lower than that of the conventional wide-period polarization grating, and the extinction ratio (ext. Ratio) is greatly improved.
Referring to FIG. 5, the results of the 60℃90% RH 1000hr reliability test for the high aspect ratio, narrow period reflective polarization grating prepared in example 1 show that the reflective polarization grating has excellent heat and moisture resistance.
Although embodiments of the present invention have been disclosed above, it is not limited to the use of the description and embodiments, it is well suited to various fields of use for the invention, and further modifications may be readily apparent to those skilled in the art, and accordingly, the invention is not limited to the particular details without departing from the general concepts defined in the claims and the equivalents thereof.
Claims (10)
1. The preparation method of the reflective polarization grating with high aspect ratio and narrow period is characterized by comprising the following steps:
s1, uniformly coating photoresist on the surface of a flexible substrate;
s2, transferring the pattern of the wide-period grating template to the photoresist through nano imprinting;
s3, curing the photoresist by utilizing UV light, and removing the wide-period grating template to obtain a photoresist grating structure with a wide-period grating pattern;
s4, plating a metal film on the surface of the photoresist grating structure by a physical or chemical vapor deposition method, and covering the photoresist grating structure to form a metal grating structure;
s5, etching and thinning the top of the metal grating structure and the grooves by utilizing plasma etching, wherein the etching depth is consistent with the thickness of the film layer of the metal grating structure;
and S6, removing the residual photoresist grating structure to obtain a metal grating structure formed on the surface of the flexible substrate, and obtaining the reflective polarization grating with high aspect ratio and narrow period.
2. The method for preparing a high aspect ratio, narrow period reflective polarization grating according to claim 1, wherein in step S4, a metal film is coated on the surface of the photoresist grating structure by using electron beam evaporation, magnetron sputtering or atomic layer deposition process.
3. The method of claim 1, wherein in step S4, a metal film is coated on the surface of the photoresist grating structure by using a roll-to-roll ALD process.
4. The method for manufacturing a high aspect ratio, narrow period reflective polarization grating according to claim 1, wherein the metal film is a metal simple substance film or a metal alloy film.
5. The method for manufacturing a high aspect ratio, narrow period reflective polarization grating according to claim 1, wherein the metal film is an aluminum film or an aluminum alloy film.
6. The method for preparing a reflective polarization grating with high aspect ratio and narrow period according to claim 1, wherein the roll-to-roll ALD method adopted in the step S4 specifically comprises:
trimethyl aluminum is used as a precursor A, hydrogen is used as a precursor B, and space atomic layer deposition equipment is adopted to realize roll-to-roll deposition of an aluminum film layer on the surface of a photoresist grating structure under the assistance of plasma;
in the roll-to-roll deposition process, the vacuum degree of the coating chamber is 1 multiplied by 10 -3 Pa, the temperature of the film coating roller is 0 degree, the flow rates of trimethylaluminum and hydrogen are respectively set to be 60sccm and 100sccm, and the running speed of the film coating roller is set to be 0.1m/min to 1m/min.
7. The method for manufacturing a high aspect ratio, narrow period reflective polarization grating according to claim 1, wherein in the step S5: etching and thinning the top and the groove of the metal grating structure by adopting inductively coupled plasma, and etching gas Cl 2 Ar, the gas flow rate is 8 sccm-20 sccm, the etching power is 400-800W, the etching bias voltage can be selected to be-65-150V, and the corresponding etching rate is 50-150 nm/min.
8. The method for manufacturing a high aspect ratio and narrow period reflective polarization grating according to claim 1, wherein the etching and thinning process using inductively coupled plasma in step S5 is that: etching gas Cl 2 Ar, the gas flow rate is 8sccm, 18sccm in sequence, the etching power is 400W, the etching bias voltage is-65V, the corresponding etching rate is 50nm/min, the etching direction is vertical to the upper surface of the metal grating structure, and the etching time is 1min.
9. The method for manufacturing a high aspect ratio, narrow period reflective polarization grating according to claim 1, wherein the flexible substrate is a cellulose triacetate film with a thickness of 40 μm to 80 μm.
10. A high aspect ratio, narrow period reflective polarization grating produced by the method of any one of claims 1 to 9.
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