CN113219570B - Visible light-near infrared wide spectrum enhanced grating type optical element and preparation method and application thereof - Google Patents
Visible light-near infrared wide spectrum enhanced grating type optical element and preparation method and application thereof Download PDFInfo
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- CN113219570B CN113219570B CN202110484128.XA CN202110484128A CN113219570B CN 113219570 B CN113219570 B CN 113219570B CN 202110484128 A CN202110484128 A CN 202110484128A CN 113219570 B CN113219570 B CN 113219570B
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- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/18—Diffraction gratings
- G02B5/1866—Transmission gratings characterised by their structure, e.g. step profile, contours of substrate or grooves, pitch variations, materials
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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
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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
- G02B5/1847—Manufacturing methods
- G02B5/1857—Manufacturing methods using exposure or etching means, e.g. holography, photolithography, exposure to electron or ion beams
Abstract
The invention relates to a visible light-near infrared wide spectrum transmission type grating optical element and a preparation method and application thereof, wherein the visible light-near infrared wide spectrum transmission type grating optical element comprises a substrate, the substrate is provided with a front surface and an opposite back surface, the front surface of the substrate is provided with a submicron-order microstructure periodic array; the microstructure periodic array comprises two micro-nano structure units with different bottom surface diameters. According to the visible light-near infrared wide spectrum anti-reflection grating type optical element provided by the invention, the purposes of reducing reflection and enhancing transmission of a wide spectrum are realized by constructing a composite micro-nano structure array combination on the surface of the optical element. The optical element can be used as an optical lens or an optical window independently, and can also be used in a coupling way with a conventional optical lens or an optical window, so that the comprehensive performance of related instruments and equipment is improved.
Description
Technical Field
The invention belongs to the technical field of optical elements and design and manufacture of the optical elements, and particularly relates to a visible light-near infrared wide spectrum transmission type grating optical element and a preparation method and application thereof.
Background
The visible light-near infrared wide spectrum transmission type optical element is used as an optical lens or an optical window with high transmission in a visible light-near infrared band, and is mainly applied to aspects of low-light-level night vision detection, satellite remote sensing detection, visible light-near infrared spectrum analysis and the like. With the development of society and the progress of technology, optical elements are developing towards the direction of excellent comprehensive performance of broad spectrum, high transmittance, anti-reflection and stray light elimination, and especially in the key fields of military affairs, aerospace, security protection, detection and the like, more attention is paid to the broad spectrum anti-reflection optical elements.
In order to prepare an optical element with wide spectrum, high transmittance, anti-reflection and stray light elimination, the traditional solution is realized by plating a single-layer or multi-layer anti-reflection dielectric film on the surface of the existing optical element, but the film has the problems of limited material types, mismatched expansion coefficients between adjacent materials, difficult guarantee of corrosion resistance and thermal stability in a severe environment and the like. Meanwhile, this method can only add a thin film layer to an existing optical element, and cannot reduce the volume and weight of the optical element. Obviously, the conventional method for plating a thin film has great limitations and cannot well meet the performance requirements of high-end optical elements.
Disclosure of Invention
In view of this, the main objective of the present invention is to provide a visible light-near infrared wide spectrum transmission-enhanced grating optical element with anti-reflection, high transmission and stray light elimination, and a preparation method and an application thereof. The grating optical element manufactured based on the method and the composite microstructure array combination has the functions of anti-reflection and stray light elimination in a visible light-near infrared wide spectrum range, is suitable for a light, thin and flat optical element, and can be independently used as an optical lens or an optical window to improve the comprehensive performance of related instruments and equipment.
The purpose of the invention and the technical problem to be solved are realized by adopting the following technical scheme. The invention provides a visible light-near infrared wide spectrum anti-reflection grating optical element, which comprises a substrate, wherein the substrate is provided with a front surface and an opposite back surface, the front surface is used for receiving and transmitting incident light, and the front surface of the substrate is provided with a submicron-order microstructure periodic array; the microstructure periodic array comprises two micro-nano structure units with different bottom surface diameters.
Preferably, in the visible light-near infrared wide spectrum transmission-enhanced grating optical element, two of the micro-nano structure units have a convex morphology.
Preferably, in the foregoing visible-near-infrared wide-spectrum transmittance-increasing grating optical element, the shape of the protrusion is a cone, a truncated cone, a paraboloid, or a gaussian surface, and the projection of the protrusion on the plane is circular.
Preferably, in the visible light-near infrared wide spectrum transmission-enhanced grating optical element, the two micro-nano structure units have the same morphology.
Preferably, in the visible light-near infrared broad spectrum transmission-enhanced grating optical element, the center distance between two types of micro-nano structure units in the longitudinal direction is 430-470 nm, the center distance between two types of micro-nano structure units in the transverse direction is 580-620 nm, the diameters of the bottom surfaces of the two types of micro-nano structure units are 480-520 nm and 340-380 nm respectively, and the height of the convex morphology is 260-400 nm.
Preferably, in the visible-near infrared wide-spectrum transmittance grating optical element, the substrate is made of quartz optical glass, flint optical glass or crown optical glass.
Preferably, in the aforementioned visible light-near infrared wide spectrum transmittance grating optical element, a silica thin film layer or an alumina thin film layer is evaporated or deposited on the surface of the substrate; and the two micro-nano structure units are respectively arranged on the silicon dioxide film layer or the alumina film layer.
Preferably, in the foregoing visible light-near infrared wide spectrum transmittance grating optical element, the thickness of the substrate is 0.5mm to 5 mm; the shape of the substrate is a circular sheet, a square sheet or a special-shaped sheet.
The object of the present invention and the technical problems solved thereby can be further achieved by the following technical measures. The invention provides a preparation method of a visible light-near infrared wide spectrum anti-reflection grating type optical element, which comprises the following steps:
etching a pre-designed microstructure array with a raised appearance on the surface of the substrate by adopting an etching process; and cleaning and drying the optical grating to obtain the visible light-near infrared wide spectrum anti-reflection type optical grating element.
Preferably, in the optical device, a step of a chemical etching process is further included after the etching process, so as to assist in further improving the etched profile.
The object of the present invention and the technical problems solved thereby can be further achieved by the following technical measures. The invention provides an optical device which comprises the visible light-near infrared wide spectrum anti-reflection type grating optical element.
Preferably, in the aforementioned optical device, the optical device is a low-light night vision detector, a near-satellite remote sensing detector or a visible-near infrared spectrum analyzer.
By the technical scheme, the visible light-near infrared wide spectrum enhanced grating optical element and the preparation method and application thereof provided by the invention at least have the following advantages:
the visible light-near infrared wide spectrum anti-reflection grating optical element provided by the invention can effectively improve the transmittance of 400 nm-1500 nm visible light-near infrared bands made of the same material and having the same thickness.
The visible light-near infrared wide spectrum anti-reflection grating optical element provided by the invention can be used as an optical lens or an optical window to replace the traditional common optical element for single use.
The visible light-near infrared broad spectrum anti-reflection grating optical element provided by the invention can also be combined with the original traditional optical device in a coupling mode, namely, the visible light-near infrared broad spectrum anti-reflection grating optical element is coupled at an incident end, and the front surfaces of the microstructure and the substrate face incident light.
In summary, the visible light-near infrared wide spectrum transmittance grating optical element of the present invention can significantly improve the spectrum transmittance of the visible light-near infrared band, and can be used alone or coupled with a conventional optical device, thereby greatly being compatible with conventional optical devices and greatly improving the optical performance of corresponding devices.
The foregoing is a summary of the present invention, and in order to provide a clear understanding of the technical means of the present invention and to be implemented in accordance with the present specification, the following is a detailed description of the preferred embodiments of the present invention.
Drawings
FIG. 1 is a schematic diagram of a microstructure array period of a visible light-near infrared wide spectrum anti-reflection grating optical element according to the present invention;
fig. 2 is a structural diagram of a visible light-near infrared wide spectrum anti-reflection grating optical element according to embodiment 1 of the present invention;
FIG. 3 is a comparison graph of the transmission spectra of the visible-near infrared wide-spectrum anti-reflection grating optical device and the conventional optical device in example 1 of the present invention;
fig. 4 is a structural diagram of a visible light-near infrared wide spectrum anti-reflection grating optical element according to embodiment 2 of the present invention;
fig. 5 is a comparison graph of the transmission spectra of the visible-near-infrared wide-spectrum anti-reflection grating optical element and the conventional optical element in example 2 of the present invention;
fig. 6 is a structural diagram of a visible light-near infrared wide spectrum antireflection type grating optical element according to embodiment 3 of the present invention;
FIG. 7 is a comparison graph of the transmission spectra of the visible-near infrared wide-spectrum anti-reflection grating optical device and the conventional optical device in example 3 of the present invention;
fig. 8 is a structural diagram of a visible light-near infrared wide spectrum antireflection type grating optical element according to embodiment 4 of the present invention;
fig. 9 is a comparison graph of the transmission spectra of the visible-near-infrared wide-spectrum anti-reflection grating optical element and the conventional optical element in example 4 of the present invention;
fig. 10 is a structural diagram of a visible light-near infrared wide spectrum antireflection type grating optical element according to embodiment 5 of the present invention;
fig. 11 is a comparison graph of the transmission spectra of the visible-near-infrared wide-spectrum anti-reflection grating optical element and the conventional optical element in example 5 of the present invention;
fig. 12 is a structural diagram of a visible light-near infrared wide spectrum antireflection type grating optical element according to embodiment 6 of the present invention;
fig. 13 is a comparison graph of the transmission spectra of the visible-near-infrared wide-spectrum anti-reflection grating optical element and the conventional optical element in example 6 of the present invention;
fig. 14 is a diagram showing the effect of observing the lamp source in the night by using the visible light-near infrared wide spectrum anti-reflection grating optical element of the present invention and the common optical element of the same material and thickness in the prior art, (a) the common optical element, and (B) the visible light-near infrared wide spectrum anti-reflection grating optical element of the present invention;
wherein, the substrate-1; microstructure unit-2; film layer-3.
Detailed Description
To further illustrate the technical means and effects of the present invention adopted to achieve the predetermined objects, the following detailed description will be given to a visible-near-infrared broadband spectral transmittance grating optical element, a method for manufacturing the same, and specific embodiments, structures, characteristics and effects thereof applied to the same according to the present invention, in conjunction with the preferred embodiments. In the following description, different "one embodiment" or "an embodiment" refers to not necessarily the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
The following materials or reagents, unless otherwise specified, are all commercially available.
As shown in fig. 1-2, 4, 6, 8, 10 and 12, the present invention provides a visible light-near infrared wide spectrum transmittance-enhanced grating optical element, which includes a substrate 1, where the substrate 1 has a front surface for receiving incident light and an opposite back surface, and the front surface of the substrate is provided with a periodic array of micro structures in submicron order; the microstructure periodic array comprises two micro-nano structure units 2 with different bottom surface diameters. The two micro-nano structure units 2 are in a convex shape; the shape of the bulge is conical, truncated cone-shaped, paraboloid-shaped or Gaussian surface-shaped, preferably conical and truncated cone-shaped, and compared with the shape of the paraboloid-shaped or Gaussian surface-shaped, the transmittance of the conical and truncated cone-shaped microstructure optical element in the near-infrared band range of 400-1500 nm is better in improvement effect; the projections of the convex shapes on the plane of the substrate are all circular, and the projections on the plane are all circular; the two micro-nano structure units have the same appearance, the central distance of the two micro-nano structure units in the longitudinal direction is 430-470 nm, the central distance of the two micro-nano structure units in the transverse direction is 580-620 nm, the diameters of the bottom surfaces of the two micro-nano structure units are 480-520 nm and 340-380 nm respectively, and the height of the protruding appearance is 260-400 nm; the anti-reflection effect of the broad spectrum is realized by the combination of the two periodic sizes, and the anti-reflection degree is controlled by the diameter and the shape height of the bottom surface.
Preferably, in the visible light-near infrared broad spectrum transmittance grating optical element, the microstructure periodic array is a periodic array formed by two convex units with diameters of bottoms a and B, the center-to-center distance (period T1) between longitudinal AB or BA is 430 to 470nm, and the center-to-center distance (period T2) between transverse AA or BB is 580 to 620 nm; the diameter A of the bottom is 480-520 nm, the diameter B of the bottom is 340-380 nm, and the height of the protruding appearance is 260-400 nm. The purpose of the arrangement is to effectively distinguish the microstructure from the target light wave of 400 nm-1500 nm, so that the surface of the microstructure is equivalent to a transition material with gradually changed refractive index, the Fresnel reflection effect of an incident light interface is effectively reduced, the back-and-forth reflection stray light of the upper inner surface and the lower inner surface is also reduced, the incident transmittance of the target light wave is improved, the signal to noise ratio of the target light wave is also improved, and the accuracy and the definition of the signal are improved.
In specific implementation, the substrate 1 may be made of quartz optical glass, flint optical glass or crown optical glass, which are transparent in visible light and near infrared, and can make the visible light and near infrared band have high spectral transmittance.
In specific implementation, a silicon dioxide film layer 3 or an aluminum oxide film layer 3 is evaporated or deposited on the surface of the substrate 1, and both the silicon dioxide film layer and the aluminum oxide film layer are visible light-near infrared transmitting film layers, and the silicon dioxide film layer and the aluminum oxide film layer have the characteristics of near infrared transmission, lower refractive index, good thermal stability, good acid and alkali stability, high mechanical strength and the like; and the silicon dioxide film layer 3 or the alumina film layer 3 is arranged on the front surface of the substrate 1, and the two micro-nano structure units are respectively arranged on the silicon dioxide film layer 3 or the alumina film layer 3, so that the film layer can protect the interface of the passivated substrate surface, and the stability and the special environment applicability of the substrate, particularly the glass substrate, are enhanced.
In specific implementation, the thickness of the substrate 1 is 0.5 mm-5 mm; the shape of the substrate can be round, square, special-shaped and the like, and is related to the instrument design of specific application, and the number of the round and square is large.
The invention also provides a preparation method of the visible light-near infrared wide spectrum anti-reflection grating type optical element, which comprises the following steps:
etching a pre-designed microstructure array with a convex appearance on the surface of the substrate by adopting an etching process; and cleaning and drying the optical grating type near-infrared transmission-type optical element to obtain the optical grating type near-infrared transmission-type optical element.
In the specific implementation, a step of chemical etching process is also included after the etching process to assist in further improving the etching morphology.
In specific implementation, the preparation method comprises the following steps:
s1, ultrasonically cleaning the substrate by acetone, absolute ethyl alcohol and deionized water respectively, repeatedly cleaning for many times, and blow-drying the substrate by high-purity nitrogen in a purification workshop to obtain a clean substrate for later use;
s2, etching a pre-designed A and B composite microstructure array with a convex shape (conical shape, truncated cone shape, paraboloid shape or Gaussian shape) on the surface of a substrate by adopting a conventional etching technology in the semiconductor industry, wherein the longitudinal AB or BA center spacing (period T1) of the convex array is 430-470 nm, and the transverse AA or BB center spacing (period T2) is 580-620 nm; the diameter A of the bottom is 480-520 nm, the diameter B of the bottom is 340-380 nm, and the height of the protruding appearance is 260-400 nm, as shown in figure 1;
after S3 etching is finished, dilute sulfuric acid, hydrogen peroxide and deionized water (photoresist can be removed) are added according to the requirement; dilute hydrofluoric acid and sodium hydroxide solution (which can remove the substrate material by corrosion and improve the surface appearance of the substrate); and ultrasonic cleaning with acetone, absolute ethyl alcohol and deionized water (removing pollutants such as organic grease and dust which are contacted and polluted in the substrate flowing process). And blowing the glass fiber in a purification workshop by using high-purity nitrogen to obtain the clean visible light-near infrared transmission type optical element with the microstructure array.
The present invention also provides an optical device comprising the above visible light-near infrared transmission-enhanced optical element; the optical device can be a low-light night vision detector, a satellite remote sensing detector or a visible light-near infrared spectrum analysis instrument.
The present invention is further illustrated by the following specific examples.
Example 1
A K9 optical glass sheet (one of crown optical glass) with the diameter of 20 x 0.5mm is used as a transparent substrate, the transparent substrate is cleaned for 5 minutes by acetone, absolute ethyl alcohol and deionized water through ultrasonic waves (the power is 80kHz), the cleaning is repeated for 3 times, and high-purity nitrogen is used for drying in a cleaning room to obtain a clean substrate for later use.
And etching a raised conical microstructure periodic array on the surface of the K9 optical glass sheet by adopting an electron beam direct writing technology. The operating parameters of the electron beam direct writing technology are as follows: working vacuum degree of 5 x 10-4Pa, maximum accelerating voltage of 100kV, scanning main frequency of 12MHz, scanning step distance of 2nm, and minimum beam spot of 5 nm. The conical microstructure periodic array comprises a plurality of conical microstructure units, wherein the diameter A of the bottom of the conical bulge is 480nm, the diameter B of the bottom of the conical bulge is 360nm, the height of the cone (bulge) is 380nm, and the plurality of conical micro-structures are arranged in a mode that the conical micro-structures are arranged in parallelThe structural units are arranged in a periodic manner, the longitudinal period T1 of the conical microstructure array is 450nm, and the transverse period T2 of the conical microstructure array is 580nm, as shown in figures 1 and 2.
After the etching is finished, ultrasonic cleaning is carried out for 5 minutes by acetone, absolute ethyl alcohol and deionized water (the power is 80kHz), and the cleaning is repeated for 3 times (the cleaning is caused by organic pollution, grease and dust pollution in the flowing process and the operation process of the sample); then, carrying out ultrasonic cleaning for 10 minutes by using dilute hydrofluoric acid with the concentration of 0.2 vol%, sodium hydroxide solution with the concentration of 1 wt% and absolute ethyl alcohol (the power is 45kHz), and carrying out ultrasonic cleaning for 3 times (an acid-base alternative corrosion chemical corrosion method assists in further improving the etching morphology to finally obtain a conical morphology); and blowing the glass body in a purification room by using high-purity nitrogen to obtain a clean K9 optical glass-based visible light-near infrared transmission type optical element with a microstructure array, wherein the transmittance of the optical element in a visible-near infrared band of 400-1500 nm can be enhanced by 1.6-5.2 percent (see figure 3) compared with the transmittance of a K9 optical glass sheet (0.5mm thick) with the same thickness and the same material.
Example 2
The method comprises the steps of adopting K9 optical glass sheets with the diameter of 100 x 5mm as transparent substrates, ultrasonically cleaning the transparent substrates for 5 minutes by acetone, absolute ethyl alcohol and deionized water (the power is 80kHz), repeatedly cleaning the transparent substrates for 3 times, and drying the transparent substrates by using high-purity nitrogen in a purification room to obtain clean substrates for later use.
Etching a raised circular truncated cone-shaped microstructure periodic array on the surface of a K9 optical glass sheet by adopting a plasma etching technology; the method specifically comprises the following steps: coating 500nm photoresist on the surface of a K9 optical glass sheet through spin coating, and exposing and developing to obtain a periodic array rubber mold pattern with the diameter A of 490nm, the diameter B of 380nm, the longitudinal period T1 of 430nm and the transverse period T2 of 600 nm; the parameters of the plasma etching are set as follows: the pre-pumping time is 120s, the air supply time is 200s, the process pressure is 12Pa, the glow power is 600W, the glow time is 650s, the substrate bias power is 10W, the oxygen flow is 50sccm, the CF4 flow is 300sccm, and a pit array with the depth of 400nm is etched on the surface of a bare K9 optical glass sheet; then, dilute sulfuric acid with the concentration of 10 vol%, hydrogen peroxide with the concentration of 20 vol% and deionized water are used for ultrasonic cleaning for 5 minutes respectively (the power is 80kHz), and the ultrasonic cleaning is repeated for 3 times to remove the rubber mold.
After the etching is finished, ultrasonic cleaning is carried out for 8 minutes by using a dilute hydrofluoric acid solution with the concentration of 0.1 vol%, a sodium hydroxide solution with the concentration of 1 wt% and absolute ethyl alcohol respectively (the power is 80kHz), and the ultrasonic cleaning is repeated for 3 times (an acid-base alternative corrosion chemical corrosion method is used for assisting in further improving the etching morphology, so that the circular truncated cone-shaped morphology is finally obtained). The circular truncated cone-shaped microstructure periodic array comprises a plurality of circular truncated cone-shaped microstructure units, wherein the diameter A of the bottom of a circular truncated cone-shaped bulge is 490nm, the diameter of the top of the circular truncated cone-shaped bulge is 80nm, the diameter B of the bottom of the circular truncated cone-shaped bulge is 380nm, the diameter of the top of the circular truncated cone-shaped bulge is 60nm, the height of the circular truncated cone (bulge) is 400nm, the circular truncated cone-shaped microstructure units are arranged periodically, the longitudinal period T1 of the circular truncated cone-shaped microstructure array is 430nm, and the transverse period T2 of the circular truncated cone-shaped microstructure array is 600nm, and the circular truncated cone-shaped microstructure periodic array is shown in fig. 1 and fig. 4.
Ultrasonic cleaning is carried out for 5 minutes respectively by acetone, absolute ethyl alcohol and deionized water, and cleaning is repeated for 3 times (cleaning is carried out because the sample is polluted by organic grease and dust in the flowing and rotating process and the operating process); and blowing the glass body in a purification room by using high-purity nitrogen to obtain a clean K9 optical glass-based near visible light-infrared anti-reflection optical element with a composite microstructure array, wherein the transmittance of the optical element in a 400-1500 nm visible-near infrared band can be enhanced by 1.5-5 percent (see figure 4) compared with the same thickness and material of a K9 optical glass sheet (5mm in thickness) without a microstructure.
Example 3
A quartz optical glass sheet with the thickness of 100 x 3mm is used as a transparent substrate, ultrasonic cleaning is carried out on the transparent substrate for 5 minutes by acetone, absolute ethyl alcohol and deionized water (the power is 80kHz), cleaning is repeated for 3 times, and high-purity nitrogen is used for blow-drying in a purification room, so that a clean substrate is obtained for later use.
Forming a raised parabolic microstructure periodic array on the surface of the quartz optical glass by adopting a plasma etching technology; the method specifically comprises the following steps: and coating 300nm of photoresist on the surface of the quartz optical glass sheet through spin coating, exposing, developing and removing the photoresist to obtain a solid array pattern, wherein the diameter of the unit A is 500nm, the diameter of the unit B is 380nm, the center distance of AB or BA is 430nm, and the center distance of AA or BB is 600 nm. The parameters of the plasma etching are set as follows: the pre-pumping time is 120s, the gas supply time is 200s, the process pressure is 10Pa, the glow power is 650W, the glow time is 600s, the substrate bias power is 8W, the oxygen flow is 55sccm, and the CF4 flow is 320 sccm; etching a pit with the depth of 300nm on the surface of the bare quartz optical glass, then ultrasonically cleaning the pit for 5 minutes by using dilute sulfuric acid with the concentration of 10 vol% and hydrogen peroxide with the concentration of 20 vol% and deionized water (with the power of 80kHz), and repeatedly ultrasonically cleaning the pit for 3 times; and then, respectively ultrasonically cleaning for 10 minutes (the power is 80kHz) by using a dilute hydrofluoric acid solution with the concentration of 5 vol%, a sodium hydroxide solution with the concentration of 10 wt% and absolute ethyl alcohol (the etching morphology is further improved by the aid of a chemical corrosion method of acid-base alternating corrosion, and finally the paraboloid-shaped morphology is obtained), and repeatedly ultrasonically treating for 3 times. The parabolic microstructure periodic array comprises a plurality of parabolic microstructure units, wherein the diameter A of the bottom of the parabolic protrusion is 500nm, the diameter B of the bottom of the parabolic protrusion is 380nm, the height of the parabolic protrusion is 330nm, the parabolic microstructure units are arranged periodically, the longitudinal period T1 of the parabolic microstructure array is 430nm, and the transverse period T2 of the parabolic microstructure array is 600nm, as shown in fig. 1 and 6.
After the etching is finished, ultrasonically cleaning the sample for 5 minutes by adopting acetone, absolute ethyl alcohol and deionized water (the power is 80kHz), and repeatedly cleaning the sample for 3 times (the cleaning is caused by organic grease pollution and dust pollution in the flowing and rotating process and the operating process of the sample); and blowing the quartz optical glass-based visible light-near infrared transmission type optical element with the microstructure array in a purification room by using high-purity nitrogen for drying to obtain the clean quartz optical glass-based visible light-near infrared transmission type optical element with the microstructure array, wherein the transmittance of the optical element in a 400-1500 nm visible-near infrared band is enhanced by 1.5-2.5 percent (see figure 6) compared with a quartz optical glass sheet (3mm in thickness) with the same thickness and the same material.
Example 4
Quartz optical glass with the diameter of 200 x 4mm is used as a transparent substrate, the substrate is cleaned for 5 minutes by acetone, alcohol and deionized water through ultrasonic waves (the power is 80kHz), the cleaning is repeated for 3 times, and high-purity nitrogen is used for blow-drying in a purification room to obtain a clean substrate for later use.
Etching a raised Gaussian surface-shaped microstructure periodic array on the surface of the quartz optical glass sheet by adopting a laser direct writing etching technology; the parameters of the laser direct writing etching technology are set as follows: the working vacuum degree is 5E-4pa, the maximum etching depth is 300nm, the maximum light intensity is 3mW, the automatic focusing is realized, the minimum resolution distance is 3nm, the writing speed is 100-2000 square millimeters/minute, the maximum stroke and step are 115mm, the repeatability is less than 20nm RMS, the maximum scanning speed is 200mm/s, and the straightness axis is less than 0.5 mu m. The Gaussian-surface-shaped microstructure periodic array comprises a plurality of Gaussian-surface-shaped microstructure units, wherein the diameter A of the bottom of each Gaussian-surface-shaped protrusion is 520nm, the diameter B of the bottom of each Gaussian-surface-shaped protrusion is 340nm, the height of each Gaussian-surface-shaped protrusion is 300nm, the Gaussian-surface-shaped microstructure units are arranged periodically, the longitudinal period T1 of the Gaussian-surface-shaped microstructure array is 430nm, and the transverse period T2 of the Gaussian-surface-shaped microstructure array is 620nm, as shown in the figures 1 and 8.
After the etching is finished, ultrasonic cleaning is carried out for 5 minutes by acetone, absolute ethyl alcohol and deionized water (the power is 80kHz), and the cleaning is repeated for 3 times (the cleaning is caused by organic grease pollution and dust pollution in the flowing and rotating process and the operation process of the sample); and blowing the quartz optical glass-based visible light-near infrared transmission type optical element with the microstructure array in a purification room by using high-purity nitrogen for drying to obtain the clean quartz optical glass-based visible light-near infrared transmission type optical element with the microstructure array, wherein the transmittance of the optical element in a 400-1500 nm visible-near infrared band is enhanced by 1.5-2.5 percent (see figure 7) compared with the same thickness of quartz optical glass sheets (4mm in thickness) made of the same material and without microstructures.
Example 5
An F6 optical glass sheet (one of flint optical glass) with the diameter of 30 x 0.5mm is used as a transparent substrate (containing a silicon dioxide film layer with the thickness of 260 nm-300 nm on the surface), the substrate is cleaned for 5 minutes by acetone, absolute ethyl alcohol and deionized water through ultrasonic waves (the power is 80kHz), the cleaning is repeated for 3 times, and the substrate is dried by high-purity nitrogen in a purification room to obtain a clean substrate for later use.
And etching the raised conical microstructure periodic array on the surface of the F6 optical glass sheet by adopting a dry electron beam etching technology. The parameters of the electron beam etching technology are set as follows: the working vacuum degree is 5E-4Pa, the maximum accelerating voltage is 100kV, the scanning main frequency is 12MHz, the scanning step distance is 2nm, and the minimum beam spot is 5 nm. The conical microstructure periodic array comprises a plurality of conical microstructure units, wherein the diameter A of the bottom of a conical bulge is 520nm, the diameter B of the bottom of the conical bulge is 340nm, the height of a cone is 260nm, the conical microstructure units are arranged periodically, the longitudinal period T1 of the conical microstructure array is 470nm, and the transverse period T2 of the conical microstructure array is 620nm, as shown in fig. 1 and 10.
After the etching is finished, ultrasonic cleaning is carried out for 5 minutes by acetone, absolute ethyl alcohol and deionized water (the power is 80kHz), and cleaning is repeated for 3 times (the cleaning is caused by organic grease pollution and dust pollution in the flowing and rotating process and the operating process of the sample); then, ultrasonic cleaning is carried out for 10 minutes by hydrofluoric acid solution with the concentration of 0.1 vol%, sodium hydroxide solution with the concentration of 1 wt% and absolute ethyl alcohol (the power is 80kHz), and ultrasonic treatment is repeated for 3 times (as the dry-etched microstructure may have some burrs and relatively sharp substrate appearance, the substrate is moderately corroded by an acid-base dilution liquid chemical corrosion method, and the microstructure with few defects can be obtained); and blowing the glass plate in a purification room by using high-purity nitrogen to obtain a clean F6 optical glass-based visible light-near infrared transmission type optical element with a microstructure array, wherein the optical element can achieve 2% of enhancement at a 400-1500 nm visible-near infrared waveband compared with an F6 optical glass sheet (0.5mm) with the same thickness and the same material (see figure 8).
Example 6
An F6 optical glass sheet with the diameter of 50 x 2mm is used as a transparent substrate (an alumina thin film layer with the thickness of 350-400 nm is deposited on the surface of the substrate), the substrate is ultrasonically cleaned for 5 minutes by acetone, absolute ethyl alcohol and deionized water (the power is 80kHz), the cleaning is repeatedly carried out for 3 times, and high-purity nitrogen is used for blow-drying in a purification room, so that a clean substrate is obtained for later use.
And etching the raised circular truncated cone-shaped microstructure periodic array on the alumina film layer by adopting a dry ion beam etching technology. The parameters of the dry ion beam etching technology are set as follows: adopting argon ion source, pre-vacuum degree is 5X 10-4Pa, ion beam energy of 1000eV, scanning frequency of 10MHz, scanning step pitch of 2nm, and minimum beam spot of 2 nm. The circular truncated cone-shaped microstructure periodic array comprises a plurality of circular truncated cone-shaped microstructure units 2, as shown in FIG. 3, wherein the diameter A of the bottom of the circular truncated cone-shaped bulge is 510nm, the diameter of the top of the circular truncated cone-shaped bulge is 90nm, the diameter B of the bottom of the circular truncated cone-shaped bulge is 350nm, and the diameter of the top of the circular truncated cone-shaped bulge is 60nm, the height of the truncated cone is 280nm, the plurality of truncated cone-shaped microstructure units are arranged periodically, the longitudinal period T1 of the truncated cone-shaped microstructure array is 460nm, and the transverse period T2 of the truncated cone-shaped microstructure array is 580nm, as shown in the figures 1 and 12.
After the etching is finished, ultrasonic cleaning is carried out for 5 minutes by acetone, absolute ethyl alcohol and deionized water (the power is 80kHz), and cleaning is repeated for 3 times (the cleaning is caused by organic grease pollution and dust pollution in the flowing and rotating process and the operating process of the sample); and then ultrasonically cleaning the glass substrate for 10 minutes by hydrofluoric acid solution with the concentration of 0.1 vol%, sodium hydroxide solution with the concentration of 1 wt% and absolute ethyl alcohol at 80kHz (the power is 80kHz), repeatedly ultrasonically drying the glass substrate for 3 times (because the dry-etched microstructure may have some burrs and relatively sharp substrate appearance, and the substrate is moderately corroded by an acid-base dilution liquid chemical corrosion method to obtain a microstructure with less defects) in a cleaning room by high-purity nitrogen gas to obtain a clean F6 optical glass-based visible light-near infrared transmission-type optical element with a microstructure array, wherein the transmittance of the optical element in a visible-near infrared band of 400nm to 1500nm is enhanced by 1-2% compared with an F6 optical glass sheet (the thickness is 2mm) which is made of the same thickness and has no microstructure and is made of the same material (see figure 9).
Example 7
A K9 optical glass sheet (one of crown optical glass) with the diameter of 20 x 0.5mm is used as a transparent substrate, the transparent substrate is cleaned for 5 minutes by acetone, absolute ethyl alcohol and deionized water through ultrasonic waves (the power is 80kHz), the cleaning is repeated for 3 times, and high-purity nitrogen is used for drying in a cleaning room to obtain a clean substrate for later use.
Etching a raised circular truncated cone-shaped microstructure periodic array on the surface of a K9 optical glass sheet by adopting a plasma etching technology; the method specifically comprises the following steps: coating 500nm photoresist on the surface of a K9 optical glass sheet through spin coating, and exposing and developing to obtain a periodic array rubber mold pattern with the diameter A of 480nm, the diameter B of 360nm, the longitudinal period T1 of 450nm and the transverse period T2 of 580 nm; the parameters of the plasma etching are set as follows: the pre-pumping time is 120s, the air supply time is 200s, the process pressure is 12Pa, the glow power is 600W, the glow time is 650s, the substrate bias power is 10W, the oxygen flow is 50sccm, the CF4 flow is 300sccm, and a pit array with the depth of 380nm is etched on the surface of a bare K9 optical glass sheet; then, dilute sulfuric acid with the concentration of 10 vol%, hydrogen peroxide with the concentration of 20 vol% and deionized water are used for ultrasonic cleaning for 5 minutes respectively (the power is 80kHz), and the ultrasonic cleaning is repeated for 3 times to remove the rubber mold.
After the etching is finished, cleaning for 8 minutes by ultrasonic treatment (power is 80kHz) through 2 vol% hydrofluoric acid solution, 10 wt% sodium hydroxide solution and absolute ethyl alcohol, and performing ultrasonic treatment for 3 times (chemical corrosion method of acid-base alternating corrosion is used for assisting in further improving the etching morphology to finally obtain the paraboloid-shaped morphology); the circular truncated cone-shaped microstructure periodic array comprises a plurality of circular truncated cone-shaped microstructure units, wherein the diameter A of the bottom of a circular truncated cone-shaped bulge is 480nm, the diameter of the top of the circular truncated cone-shaped bulge is 80nm, the diameter B of the bottom of the circular truncated cone-shaped bulge is 360nm, the diameter of the top of the circular truncated cone-shaped bulge is 60nm, the height of the circular truncated cone (bulge) is 380nm, the circular truncated cone-shaped microstructure units are arranged periodically, the longitudinal period T1 of the circular truncated cone-shaped microstructure array is 450nm, and the transverse period T2 of the circular truncated cone-shaped microstructure array is 580 nm.
Ultrasonic cleaning is carried out for 5 minutes respectively by acetone, absolute ethyl alcohol and deionized water, and cleaning is repeated for 3 times (cleaning is carried out because the sample is polluted by organic grease and dust in the flowing and rotating process and the operating process); and blowing the glass body in a purification room by using high-purity nitrogen to obtain a clean K9 optical glass-based near visible light-infrared anti-reflection optical element with a composite microstructure array, wherein the transmittance of the optical element in a 400-1500 nm visible-near infrared band can be enhanced by 1.5-5.5% compared with the transmittance of a K9 optical glass sheet (0.5mm thick) which has the same thickness and is made of the same material and is not provided with a microstructure.
Example 8
A K9 optical glass sheet (one of crown optical glass) with the diameter of 20 x 0.5mm is used as a transparent substrate, the transparent substrate is cleaned for 5 minutes by acetone, absolute ethyl alcohol and deionized water through ultrasonic waves (the power is 80kHz), the cleaning is repeated for 3 times, and high-purity nitrogen is used for drying in a cleaning room to obtain a clean substrate for later use.
Forming a raised parabolic microstructure periodic array on the surface of a K9 optical glass sheet by adopting a plasma etching technology; the method specifically comprises the following steps: coating 400nm photoresist on the surface of a K9 optical glass sheet through spin coating, exposing, developing and removing the photoresist to obtain a solid array pattern, wherein the diameter of a unit A is 480nm, the diameter of a unit B is 360nm, the center-to-center distance of AB or BA is 450nm, and the center-to-center distance of AA or BB is 580 nm. The parameters of the plasma etching are set as follows: the pre-pumping time is 120s, the gas supply time is 200s, the process pressure is 10Pa, the glow power is 600W, the glow time is 600s, the substrate bias power is 10W, the oxygen flow is 55sccm, and the CF4 flow is 310 sccm; etching a pit with the depth of 380nm on the surface of a bare K9 optical glass sheet, then ultrasonically cleaning the pit for 5 minutes by using dilute sulfuric acid with the concentration of 10 vol% and hydrogen peroxide with the concentration of 20 vol% and deionized water (with the power of 80kHz), and repeatedly ultrasonically cleaning the pit for 3 times; then, the wafer is cleaned by hydrofluoric acid solution with the concentration of 4 vol%, sodium hydroxide solution with the concentration of 10 wt% and absolute ethyl alcohol respectively in an ultrasonic mode (the power is 45kHz) for 10 minutes, and the ultrasonic mode is repeated for 3 times (a chemical corrosion method of acid-base alternating corrosion assists in further improving the etching morphology, and finally the paraboloid-shaped morphology is obtained). The parabolic microstructure periodic array comprises a plurality of parabolic microstructure units, wherein the diameter A of the bottom of the parabolic protrusion is 480nm, the diameter B of the bottom of the parabolic protrusion is 360nm, the height of the parabolic protrusion is 380nm, the parabolic microstructure units are arranged periodically, the longitudinal period T1 of the parabolic microstructure array is 450nm, and the transverse period T2 of the parabolic microstructure array is 580 nm.
After the etching is finished, ultrasonically cleaning the sample for 5 minutes by adopting acetone, absolute ethyl alcohol and deionized water (the power is 80kHz), and repeatedly cleaning the sample for 3 times (the cleaning is caused by organic grease pollution, dust pollution and the like in the flowing and rotating process and the operation process of the sample); and blowing the glass body in a purification room by using high-purity nitrogen to obtain a clean K9 optical glass-based visible light-near infrared transmission type optical element with a microstructure array, wherein the transmittance of the optical element in a visible-near infrared band of 400-1500 nm is enhanced by 1.2-2.8 percent compared with that of a K9 optical glass sheet (0.5mm in thickness) with the same thickness and the same material.
Example 9
A K9 optical glass sheet (one of crown optical glass) with the diameter of 20 x 0.5mm is used as a transparent substrate, the transparent substrate is cleaned for 5 minutes by acetone, absolute ethyl alcohol and deionized water through ultrasonic waves (the power is 80kHz), the cleaning is repeated for 3 times, and high-purity nitrogen is used for drying in a cleaning room to obtain a clean substrate for later use.
Etching a raised Gaussian surface-shaped microstructure periodic array on the surface of a K9 optical glass sheet by adopting a laser direct writing etching technology; the parameters of the laser direct writing etching technology are set as follows: the working vacuum degree is 5E-4pa, the maximum etching depth is 380nm, the maximum light intensity is 3mW, the automatic focusing is realized, the minimum resolution distance is 2nm, the writing speed is 100-2000 square millimeters/minute, the maximum stroke and step are 100mm, the repeatability is less than 20nm RMS, the maximum scanning speed is 200mm/s, and the straightness axis is less than 0.5 mu m. The Gaussian surface-shaped microstructure periodic array comprises a plurality of Gaussian surface-shaped microstructure units, wherein the diameter A of the bottom of the Gaussian surface-shaped bulge is 480nm, the diameter B of the bottom of the Gaussian surface-shaped bulge is 360nm, the height of the Gaussian surface-shaped bulge is 380nm, the Gaussian surface-shaped microstructure units are arranged periodically, the longitudinal period T1 of the Gaussian surface-shaped microstructure array is 450nm, and the transverse period T2 of the Gaussian surface-shaped microstructure array is 580 nm.
After the etching is finished, the substrate is cleaned for 5 minutes by ultrasonic waves (the power is 80kHz) of acetone, absolute ethyl alcohol and deionized water, and the cleaning is repeated for 3 times (the cleaning is caused by organic grease pollution, dust pollution and the like in the flowing and rotating process and the operation process of the sample). Then, ultrasonic cleaning is carried out for 5 minutes by hydrofluoric acid solution with the concentration of 0.1 vol%, sodium hydroxide solution with the concentration of 1 wt% and absolute ethyl alcohol respectively (the power is 45kHz), and ultrasonic cleaning is carried out for 3 times repeatedly (an acid-base alternative corrosion chemical corrosion method is used for assisting in further improving the etching morphology, and finally the paraboloid-shaped morphology is obtained). And blowing the glass body in a purification room by using high-purity nitrogen to obtain a clean K9 optical glass-based visible light-near infrared transmission type optical element with a microstructure array, wherein the transmittance of the optical element in a 400-1500 nm visible-near infrared band is enhanced by 1.5-2.8 percent compared with the transmittance of a K9 optical glass sheet (0.5mm thick) which has the same thickness and is made of the same material and is not provided with a microstructure.
The specific applications of the visible light-near infrared transmittance enhancement type microstructure optical elements of the above examples 1 to 9 are as follows:
1. the microstructure optical element can be used as an independent optical lens and an independent optical window and applied to optical signal detection or optical instruments in a visible light-near infrared wide spectral range, the transmittance of incident light signals of the microstructure optical element can be improved by 5.5%, and the reflectivity can be reduced by 30%.
2. The microstructure optical element can be coupled with a traditional optical lens and an optical window used in optical instrument equipment, and is compatible with the traditional optical element, and the utilization rate of incident light of the microstructure optical element can be improved by 5.5%, so that the service performance of the instrument equipment is improved.
3. The photoelectric sensor can be coupled with the microstructure optical element, the acquisition capacity of the photoelectric sensor on incident light signals of visible light-near infrared wide spectral bands can be improved, the incident light signals are subjected to anti-reflection and anti-reflection effects of the microstructure optical element, the intensity of the light signals received by the photoelectric sensor can be obviously improved to 5.5%, and meanwhile, the influence of stray light background noise on the signals can be reduced by 35%.
4. The photoelectric cathode can be integrated with the microstructure optical element, the sensitivity of the photoelectric cathode to incident light signals of visible light-near infrared wide spectral band can be improved by 30%, the utilization capacity can reach 30%, and the use performance of the photoelectric cathode in the range of visible light-near infrared wide spectral band can be expanded.
Since light rays are refracted and reflected when incident on the interface of two media, such reflected light is sometimes useless and even unnecessarily harmful to optical components. For example, stray light is caused by reflection in an optical imaging system of a low-light level night vision device, so that a glare phenomenon is caused, and the observation target information is blurred and has serious potential safety hazard. For example, in an imaging system of a near-infrared optical analysis instrument, the light is reflected back and forth on the upper and lower inner surfaces of an optical glass substrate, so that the transmitted signal is weakened, the target signal is disordered, the background noise is increased, and the accuracy and the reliability of the analysis instrument are seriously reduced.
As can be seen from fig. 3, 5, 7, 9, 11 and 13, the grating-type near-infrared transmittance increasing optical element according to embodiments 1 to 6 of the present invention can effectively increase the transmittance of the same material with the same thickness in the near-infrared band of 400 to 1500nm, for example, by 1% to 6%.
In the embodiments 1-7 of the present invention, the microstructure is prepared on the surface of the substrate, when the period size of the microstructure is smaller than the wavelength of the incident light, the incident light cannot identify the microstructure, and the microstructure can be equivalently regarded as that the refractive index of the surface of the substrate changes along the thickness direction of the substrate, and the fresnel reflection effect caused by the sharp change of the refractive index is reduced by controlling the size and the dimension of the convex shape; when the period size of the microstructure is smaller than the wavelength of incident light and larger than the ratio of the wavelength of the incident light to the refractive index of the substrate, only reflection zero-order diffraction exists, and transmission multi-order diffraction exists, in this case, 0-order diffraction waves and +/-1-order diffraction waves in the grating layer are coupled, and when the equivalent refractive index is proper, a good anti-reflection and anti-reflection effect can be achieved in a wider waveband.
In addition, the visible light-near infrared wide spectrum anti-reflection grating optical element in embodiment 1 of the present invention and the common optical element in the prior art were tested for observing the light source at night. As can be seen from a and B in fig. 14, the visible light-near infrared wide spectrum anti-reflection grating optical element in embodiment 1 of the present invention is transparent in the visible light-near infrared band, and can reduce stray light, reduce a dazzling phenomenon, and facilitate accurate observation of a target signal.
In the foregoing embodiments, the descriptions of the respective embodiments have respective emphasis, and for parts that are not described in detail in a certain embodiment, reference may be made to related descriptions of other embodiments.
The microstructure disclosed by the invention is used for modifying, protecting or passivating the surface of the microstructure by simply depositing a film layer on the surface of the microstructure, and is within the protection scope of the invention.
The recitation of numerical ranges herein includes all numbers subsumed within that range and includes any two numbers subsumed within that range. Different values of the same index appearing in all embodiments of the invention can be combined arbitrarily to form a range value.
The features of the invention claimed and/or described in the specification may be combined, and are not limited to the combinations set forth in the claims by the recitations therein. The technical solutions obtained by combining the technical features in the claims and/or the specification also belong to the scope of the present invention.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiment according to the technical spirit of the present invention are still within the scope of the technical solution of the present invention.
Claims (9)
1. A visible light-near infrared wide spectrum anti-reflection grating optical element is characterized in that the visible light-near infrared wide spectrum anti-reflection grating optical element comprises a substrate, wherein the substrate is provided with a front surface and an opposite back surface, the front surface of the substrate is provided with a submicron-order microstructure periodic array, and the front surface of the substrate is provided with a micro-structure periodic array; the microstructure periodic array comprises two micro-nano structure units with different bottom surface diameters; the two micro-nano structure units have the same appearance, the central distance between the two micro-nano structure units in the longitudinal direction is 430-470 nm, the central distance between the two micro-nano structure units in the transverse direction is 580-620 nm, the diameters of the bottom surfaces of the two micro-nano structure units are 480-520 nm and 340-380 nm respectively, and the height of the protruding appearance is 260-400 nm.
2. The visible-near-infrared wide-spectrum antireflection grating type optical element according to claim 1, wherein two types of the micro-nano structure units have a convex morphology.
3. The visible-near-infrared wide-spectrum antireflection grating optical element of claim 2, wherein the convex features are conical, truncated conical, parabolic or gaussian, and the projections of the convex features on the substrate plane are circular.
4. The visible-near infrared wide spectrum antireflection grating optical element of claim 1, wherein the substrate is made of quartz optical glass, flint optical glass or crown optical glass.
5. The visible-near-infrared wide-spectrum antireflection grating optical element of claim 4, wherein a silica thin film layer or an alumina thin film layer is evaporated or deposited on the surface of the substrate; and the two micro-nano structure units are respectively arranged on the silicon dioxide film layer or the alumina film layer.
6. The visible-near-infrared wide-spectrum antireflection grating optical element of claim 1, wherein the thickness of the substrate is 0.5mm to 5 mm; the shape of the substrate is a circular sheet, a square sheet or a special-shaped sheet.
7. A method for preparing a visible light-near infrared wide spectrum anti-reflection grating optical element according to any one of claims 1 to 6, comprising the following steps:
preparing a pre-designed microstructure array with a raised appearance on the surface of the substrate by adopting an etching process; and cleaning and drying the optical grating to obtain the visible light-near infrared wide spectrum anti-reflection type optical grating element.
8. An optical device comprising the visible-near infrared wide-spectrum antireflection type grating optical element according to any one of claims 1 to 7.
9. The optical device of claim 8, wherein the optical device is a low-light night vision detector, a near-satellite remote sensing detector, or a visible-near infrared spectroscopy device.
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