CN112526663A - Atomic layer deposition-based absorption film and manufacturing method thereof - Google Patents

Atomic layer deposition-based absorption film and manufacturing method thereof Download PDF

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CN112526663A
CN112526663A CN202011214378.3A CN202011214378A CN112526663A CN 112526663 A CN112526663 A CN 112526663A CN 202011214378 A CN202011214378 A CN 202011214378A CN 112526663 A CN112526663 A CN 112526663A
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film
layer
absorption
atomic layer
absorption film
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沈伟东
郑婷婷
章岳光
杨陈楹
王海兰
陈潇
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Zhejiang University ZJU
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    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/20—Filters
    • G02B5/28—Interference filters
    • G02B5/281—Interference filters designed for the infrared light
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/32—Carbides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/40—Oxides
    • C23C16/401—Oxides containing silicon
    • C23C16/402—Silicon dioxide
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45523—Pulsed gas flow or change of composition over time
    • C23C16/45525—Atomic layer deposition [ALD]
    • C23C16/45527—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations
    • C23C16/45529—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations specially adapted for making a layer stack of alternating different compositions or gradient compositions
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/20—Filters
    • G02B5/28—Interference filters
    • G02B5/285—Interference filters comprising deposited thin solid films

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Abstract

The invention discloses an absorption film based on atomic layer deposition, which consists of a substrate and a multi-layer absorption film system on the substrate, wherein the multi-layer absorption film system consists of absorption film layers and medium film layers alternately, and the absorption film layers are the innermost layers and are arranged close to the substrate; the dielectric film layer is the outermost layer; the multilayer absorption film is obtained by an atomic layer deposition method. The invention skillfully combines the advantages of the design and preparation of the absorption film and the atomic layer deposition technology, and overcomes the difficulty that the traditional physical vapor deposition method can not meet the basic requirements of the uniformity and the coverage rate of the deposited film of the large-curvature element. The absorption film prepared by the atomic layer deposition technology has the absorption rate of over 99 percent in a design waveband, can be applied to special fields such as complex optical surfaces with high depth-to-width ratios and optical elements with large curvature, is expected to be widely applied in the aspects of virtual reality, anti-counterfeiting and the like, and makes contributions to the fields of national economy, social development, scientific technology, national defense construction and the like.

Description

Atomic layer deposition-based absorption film and manufacturing method thereof
Technical Field
The invention provides a novel atomic layer deposition-based absorption film and a manufacturing method thereof, and particularly relates to the fields of stray light elimination, detection, imaging and the like.
Background
Large-curvature optical elements such as hemispherical lenses, aspherical mirrors, quartz tubes, etc., are important elements in optical systems such as laser systems, optical microscope systems, and projection systems. In order to meet the requirements of different optical systems on transmittance, reflectivity and polarization, it is usually necessary to deposit a thin film on the surface of a large-curvature optical element, and the uniformity and coverage of the thin film have an important influence on the performance (such as imaging quality, testing accuracy and the like) of the optical system. The existing physical vapor deposition method has the defects that the distribution and the motion trail of deposited particles in the deposition process have directionality, and the spatial distribution is sensitive to the film thickness, so that the uniformity of preparing the film on a large-curvature optical element and a complex surface is greatly limited. The uniformity of the film on the surface of the regular optical element with large curvature can be improved by changing the methods of air flow distribution, element track, target position and the like, but the full coverage of the surface with high depth-width ratio and complex surface is still difficult to realize.
The Atomic Layer Deposition (ALD) technique is a method of forming thin films by alternately pulsing a vapor phase precursor into a reactor and chemisorbing and reacting on a deposition substrate. It was proposed by Finnish scientists in the 70's of the 20 th century, and with the development of microelectronic and deep submicron chip technologies in the mid 90's, ALD has become more widely used in the semiconductor field. In addition, compared with the conventional optical thin film deposition method, the thin film grown by ALD has incomparable advantages in deposition temperature, concentration density and conformality, so that the preparation of the optical thin film by ALD is gradually a hot spot of research.
In order to meet the requirements of different optical systems on transmittance, reflectivity and polarization, a thin film is generally required to be deposited on the surface of a large-curvature optical element, and especially, an absorption film in a visible light-near infrared band plays a key role in suppressing stray light of various complex optical systems. In addition, the uniformity and coverage of the thin film have an important influence on the performance of the optical system (such as imaging quality and testing accuracy). Therefore, the invention is expected to be widely applied in the aspects of detection, imaging and the like, and makes contributions to the fields of national economy, social development, scientific technology, national defense construction and the like in China.
Disclosure of Invention
The invention provides a novel absorption film based on an atomic layer deposition technology and a preparation method thereof, the absorption film has a simple structure, the preparation method is convenient, the full coverage of the surface of a large-curvature optical element and a complex optical surface can be realized, the uniformity is good, the absorptivity of a visible-near infrared band is high and can reach more than 99%, and the absorption film has good incident angle insensitivity.
An absorption film based on atomic layer deposition is composed of a substrate and a multi-layer absorption film system on the substrate, wherein the multi-layer absorption film system is composed of absorption film layers and medium film layers in an alternating mode, the absorption film layers are the innermost layers and are arranged close to the substrate; the dielectric film layer is the outermost layer, and incident light is incident from the air side or from the substrate side; the multilayer absorption film is obtained by an atomic layer deposition method.
The substrate material is not limited, the substrate can be selected from glass materials such as K9, fused quartz, float glass and the like, can also be selected from semiconductor materials such as silicon wafers, germanium sheets and the like, can also be selected from metal materials or alloy materials such as aluminum, tin, stainless steel and the like, and can also be selected from organic polymer materials such as organic glass (acrylic, PMMA, polymethyl methacrylate and the like), CR-39 (polypropylene-based diglycol carbonate), PC (polyethylene carbonate), PS (styrene) and the like. Further preferably K9 glass.
Preferably, the multilayer absorption film system consists of absorption film layers and medium film layers in an alternating mode, the alternating times are 2-30, and 2-5 alternating layers are preferred; even more preferably 3 or 5 alternating layers.
Preferably, the absorbing film layer is made of TiAlC, which is a titanium aluminum compound, and is made of trimethyl aluminum (TMA) and titanium tetrachloride (TiCl)4) Prepared by an atomic layer deposition technology, the ratio of main elements of titanium (Ti) and aluminum (Al) is over 95 percent, and the titanium-aluminum-titanium alloy has remarkable absorption metallicity in a visible-near infrared band.
Preferably, the thickness of the absorbing film layer is between 10nm and 1000 nm; further preferably 20 to 500 nm; the thickness of the absorption film layer which plays a main absorption role is larger than 100nm, preferably 200-300 nm, and the thickness of the rest absorption film layers is 10-150 nm.
Preferably, the dielectric film layer is a film layer formed by one or more mixed materials of oxide, nitride, fluoride, sulfide and selenide. More preferably, the dielectric film layer is made of an oxide such as titanium dioxide, silicon dioxide, aluminum oxide, hafnium oxide, or tantalum oxide, a nitride such as silicon nitride or titanium nitride, a fluoride such as magnesium fluoride or yttrium fluoride, a sulfide such as zinc sulfide or molybdenum sulfide, a selenide such as zinc selenide, or the like, preferably silicon dioxide, and is prepared by atomic layer deposition from precursors such as tri-t-butoxysilanol (TBS) and Trimethylaluminum (TMA). The thickness of the dielectric layer is 10 nm-300 nm, and the further preferable thickness is 20 nm-100 nm; the dielectric film layer at the outermost layer is preferably low refractive index material silicon dioxide, aluminum oxide and the like, the thickness is 10 nm-300 nm, and the further preferable thickness is 10 nm-80 nm.
Preferably, the multilayer absorption film system is (titanium aluminum compound/silicon dioxide)SAnd S is an integer and represents an alternating number. Preferably, S is 3 to 5.
As a specific embodiment, the absorbent film consists of: substrate | TiAlC (10-20nm) | SiO2(30-50nm)|TiAlC(200-300nm)|SiO2(10-20nm)|TiAlC(15-30nm)|SiO2(50-80 nm). More preferably, the substrate | TiAlC (15nm) | SiO2(41nm)|TiAlC(240nm)|SiO2(17nm)|TiAlC(23nm)|SiO2(63 nm). When the absorption film is incident from the air side or the substrate side, the average reflectivity of the absorption film to the visible light wave band (400-700nm) is below 1 percent, and the average absorptivity is above 99 percent, so that the high absorption of the visible light wave band 400-700nm can be realized.
As another specific embodiment, the absorbent film consists of: substrate | TiAlC (8-15nm) | SiO2(50-80nm)|TiAlC(25-40nm)|SiO2(30-50nm)|TiAlC(200-300nm)|SiO2(20-40nm)|TiAlC(20-40nm)|SiO2(30-50nm)|TiAlC(15-30nm)|SiO2(50-100 nm). More preferably, the substrate | TiAlC (10nm) | SiO2(60nm)|TiAlC(30nm)|SiO2(42nm)|TiAlC(230nm)|SiO2(28nm)|TiAlC(34nm)|SiO2(43nm)|TiAlC(21nm)|SiO2(80 nm). The average reflectivity of the absorption film to the visible light-near infrared band 400-1100nm is lower than 0.8 percent when the absorption film is incident from the air side or the substrate side; the average absorption rate is more than 99 percent, thereby realizing high absorption of visible light-near infrared band 400-1100 nm.
In the visible light-near infrared band absorption film system based on atomic layer deposition, a layer of absorption film (i.e. an absorption film layer playing a main absorption role) is arranged to be thick enough, so that no light can penetrate through the whole structure, and the transmittance of the film is 0. When the incident light is incident from the air side, the admittance of the absorption film layer which plays the main absorption role is directly adopted as the initial admittance, and in order to ensure that the reflectivity is minimized, the final admittance of the film system is matched with the admittance of the incident medium air, so that the antireflection film layer is deposited on the absorption film layer, the reflectivity of the absorption film layer is reduced, and the same is true when the light is incident from the substrate layer. For a broadband and low-reflectivity absorption film system, the antireflection layer is formed by alternately stacking the dielectric film layers and the absorption film layers, and the integral combined admittance is close to the admittance (1.0) of air by continuously stacking the dielectric film layers and the absorption film layers, so that the characteristics of low reflection and high absorption are realized. In the present invention, the absorbent film layer or the thickest absorbent film layer, which plays a main absorbent role, is generally disposed at or near the middle of the multilayer absorbent film system.
The invention also provides a preparation method of the atomic layer deposition-based absorption film, which adopts the atomic layer deposition method to deposit the multilayer absorption film system on the substrate layer by layer.
Preferably, the absorption film layer is a titanium aluminum compound film layer and is obtained by depositing precursors of trimethylaluminum and titanium tetrachloride through an atomic layer; the dielectric film layer is a silicon dioxide film layer and is obtained by atomic layer deposition of a precursor tri-tert-butoxy silanol and trimethylaluminum.
Preferably, the preparation method of the novel visible light-near infrared band absorption film based on the atomic layer deposition technology comprises the following steps:
(1) according to the material of the absorbing film layer, the material of the dielectric film layer and the base material, as well as the requirements on the bandwidth and the absorptivity of the absorber, the visible-near infrared band absorbing film system capable of realizing corresponding absorption characteristics is designed by using optical design software and optimizing the thickness of each layer of film.
(2) Cleaning a substrate: when the substrate is cleaned, the substrate can be wiped by using an ethanol/diethyl ether mixed solution, and the substrate can also be cleaned by using a solution ultrasonic method; for example, the substrate may be first treated with ultrasound in acetone solution and then washed with ethanol; then putting the substrate into an ethanol solution for ultrasonic treatment, and then cleaning the substrate by using deionized water; finally, the substrate is placed into deionized water for ultrasonic treatment, and then the substrate is washed again by the deionized water.
(3) Preparing an absorption film by utilizing an atomic layer deposition system: according to the film thickness designed in the step (1) and the selected film material, carrying out layer-by-layer precipitation by using an atomic layer deposition system to obtain a target absorption film;
preferably, the vacuum cavity and the reaction cavity system are in a vacuum environment below 10mbar in the film preparation process, the substrate in the reaction cavity is heated and preheated and keeps heating in reaction, and N is introduced into the vacuum cavity and the reaction cavity2The flow rates of the flow rate control agent are respectively 150-250 sccm and 500-1000 sccm.
(4) Respectively depositing an absorption film layer and a medium film layer: while the preparation of the absorbing film using titanium aluminum compound and silicon dioxide as the material of the absorbing film and the dielectric film is exemplified herein, preferably, Trimethylaluminum (TMA) and titanium tetrachloride (TiCl) can be selected4) Preparation of TiAlC as a titanium aluminide precursor, alternatively, SiO can be prepared using tri-tert-butoxysilanol (TBS) and Trimethylaluminum (TMA) as precursors2，TMA、TiCl4Can be volatilized into the reaction chamber at room temperature by means of the saturated vapor pressure of the TBS, and the TBS is heated to the saturated vapor pressure and then is heated by nitrogen (N)2) Carried into the cavity for reaction.
(5) And depositing film layers with different periods alternately to obtain the absorbing film system with the thickness corresponding to the design.
Preferably, when the titanium-aluminum compound film layer is precipitated by an atomic layer precipitation method, titanium tetrachloride is used as a first precursor; with N2Introducing excessive first precursor into the reaction cavity for carrier gas; the pulse time is 2-5 s; TiCl (titanium dioxide)4Chemisorbing on the surface of the substrate until saturation; subsequently introducing inert gas N2Adding excessive TiCl4And blowing the excessive byproducts generated in the previous step out of the reaction cavity, wherein the blowing time is 5-20 s, and finishing the first half reaction; then use N2Introducing excessive TMA (TMA) as a second precursor, wherein the pulse time is 0.2-0.5 s, and carrying out chemical reaction with a surface group generated in the first half reaction until saturation; finally introducing inert gas N2Removing excessive reactants and byproducts, wherein the purging time is 5-20 s, only the TiAlC chemical is left on the substrate, and the second half reaction is completed. According to the steps, one period of precipitation operation is completed.
Preferably, when the silicon dioxide film layer is precipitated by utilizing an atomic layer precipitation method; similar to the deposition of titanium-aluminum compound film, TBS is used as the first precursor, and N is added after heating to saturated vapor pressure2Introducing carrier gas, wherein the pulse time is 0.3-1 s until adsorption saturation; subsequently introducing inert gas N2Purging the redundant TBS and the redundant byproducts generated in the previous step from the reaction cavity for 5-20 s, and finishing the first half reaction; then with N2Introducing excessive TMA (TMA) serving as a second precursor into the carrier, wherein the pulse time is 0.2-0.5 s, and carrying out chemical reaction on the TMA and a surface group generated in the first half reaction until the TMA is saturated; finally introducing inert gas N2Removing excessive reactants and byproducts, wherein the purging time is 5-10 s, only silicon dioxide is left on the substrate, and the second half reaction is completed.
The invention can obtain the absorption film layer and the medium film layer with target thickness by controlling the precipitation speed and the precipitation period number.
The Atomic Layer Deposition (ALD) technique is a method of forming thin films by alternately passing pulses of vapor phase precursors into a reactor to chemisorb and react on a substrate. Due to the self-limiting nature of ALD surface reactions, the accuracy of ALD deposition can theoretically reach atomic levels. The technology overcomes the difficulty that the traditional physical vapor deposition method can not meet the basic requirements of uniformity and coverage rate of the deposited film of the large-curvature element, and the grown film has incomparable advantages in deposition temperature, aggregation density and conformality. Therefore, the absorption film prepared by the atomic layer deposition technology can be applied to the special fields of complex optical surfaces with high aspect ratios, large-curvature optical elements and the like.
The invention skillfully combines the advantages of the design and preparation of the absorption film and the atomic layer deposition technology, and overcomes the difficulty that the traditional physical vapor deposition method can not meet the basic requirements of the uniformity and the coverage rate of the deposited film of the large-curvature element.
The invention is based on the atomic layer deposition technology, and achieves the effect of adjusting the optical thickness of the film system by simply and conveniently regulating and controlling the layer number and the thickness of the atomic layer deposition high-low refractive index material, thereby causing the destructive interference effect, and realizing that the average absorption rate is higher than 99% in the visible light-near infrared 400-doped 1100nm wave band. The method can be applied to the special fields of complex optical surfaces with high depth-to-width ratios, large-curvature optical elements and the like, can realize stray light suppression of complex optical systems with high absorptivity, is expected to be widely applied to the aspects of virtual reality, anti-counterfeiting, detection, imaging and the like, and makes contributions to the fields of national economy, social development, scientific technology, national defense construction and the like.
Drawings
FIG. 1 is a schematic structural diagram of an atomic layer deposition-based absorber film according to the present invention;
FIG. 2 is a flow chart of the preparation of an atomic layer deposition based absorber film according to the present invention;
FIG. 3 is a table of specific parameters of TiAlC, a titanium aluminum compound, for an absorption film layer of an atomic layer deposition-based absorption film according to the present invention;
FIG. 4 is a table of specific parameters of a dielectric film layer silicon dioxide of an atomic layer deposition based absorber film according to the present invention;
FIG. 5 shows a schematic diagram of a system according to the present inventionThe structure of the atomic layer deposited absorption film in the visible light band (400-700nm) is schematically shown, in which fused silica is used as the substrate, TiAlC is used as the absorption film layer, and silicon dioxide (SiO)2) Is a medium film layer, the alternation frequency of the absorption film layer and the medium film layer is 3, and the specific film system is a substrate of | TiAlC (15nm) | SiO2(41nm)|TiAlC(240nm)|SiO2(17nm)|TiAlC(23nm)|SiO2(63 nm). FIG. 6 is a graph of a reflection spectrum of a visible light band (400-700nm) of an atomic layer deposition-based absorption film of the present invention, in which curve (a) represents a reflection spectrum incident from an air side and curve (b) represents a reflection spectrum incident from a substrate side;
FIG. 7 is a graph of the absorption spectrum of the visible light band (400-700nm) of an atomic layer deposition-based absorption film of the present invention, in which curve (a) represents the absorption spectrum incident from the air side and curve (b) represents the absorption spectrum incident from the substrate side;
FIG. 8 is a schematic structural diagram of a visible-near infrared band (400-1100nm) of an absorption film based on atomic layer deposition, in which K9 glass is used as a substrate, TiAlC is used as an absorption film, and SiO (SiO)2) The absorption film layer and the medium film layer are alternated for 5 times, and the specific film system is a substrate of | TiAlC (10nm) | SiO2(60nm)|TiAlC(30nm)|SiO2(42nm)|TiAlC(230nm)|SiO2(28nm)|TiAlC(34nm)|SiO2(43nm)|TiAlC(21nm)|SiO2(80nm)；
FIG. 9 is a graph of a reflection spectrum of a visible-near infrared band (400-1100nm) of an atomic layer deposition-based absorption film of the present invention, in which curve (a) represents a reflection spectrum incident from an air side and curve (b) represents a reflection spectrum incident from a substrate side;
FIG. 10 is a graph showing the absorption spectrum in the visible-near infrared band (400-1100nm) of an atomic layer deposition-based absorption film of the present invention, in which curve (a) shows the absorption spectrum incident from the air side and curve (b) shows the absorption spectrum incident from the substrate side.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings.
As shown in FIG. 1, an atomic layer basedThe deposited absorption film is composed of a substrate 1 and an absorption film system 2. The substrate material 1 mainly plays a supporting role, the material itself is not strictly limited, the substrate can be made of glass materials such as K9, fused quartz, float glass and the like, can also be made of semiconductor materials such as silicon wafers, germanium sheets and the like, can also be made of metal materials or alloy materials such as aluminum, tin, stainless steel and the like, and can also be made of organic polymer materials such as organic glass (acrylic, PMMA, polymethyl methacrylate and the like), CR-39 (polypropylene-based diglycol carbonate), PC (polyethylene carbonate), PS (styrene) and the like. The absorption film system 2 is formed by alternately depositing an absorption film layer 201 and a dielectric film layer 202, wherein the absorption film layer is preferably TiAlC, which is a titanium aluminum chemical, the dielectric film layer is selected from oxides such as titanium dioxide, silicon dioxide, aluminum oxide, hafnium oxide and tantalum oxide, nitrides such as silicon nitride and titanium nitride, fluorides such as magnesium fluoride and yttrium fluoride, sulfides such as zinc sulfide and molybdenum sulfide, selenides such as zinc selenide, and the like, the absorption film system is preferably silicon dioxide, and the film system structure is preferably (titanium aluminum compound/silicon dioxide)SWherein S is an integer. The film system structure can effectively realize the high-efficiency absorption of visible light-near infrared wave bands.
The preparation of the atomic layer deposition-based absorption film is realized by adjusting the number and thickness of the atomic layer deposition absorption layer and the dielectric layer. As shown in fig. 2, the atomic layer deposition-based absorption film is prepared as follows:
(1) according to the material of the absorbing film layer, the material of the dielectric film layer and the base material, as well as the requirements on the bandwidth and the absorptivity of the absorber, the visible-near infrared band absorbing film system capable of realizing corresponding absorption characteristics is designed by using optical design software and optimizing the thickness of each layer of film.
(2) The substrate is cleaned, either by wiping it with a mixed ethanol/ether solution or by cleaning it by solution sonication: firstly, performing ultrasonic treatment on a substrate in an acetone solution, and then cleaning the substrate by using ethanol; then putting the substrate into an ethanol solution for ultrasonic treatment, and then cleaning the substrate by using deionized water; finally, the substrate is placed into deionized water for ultrasonic treatment, and then the substrate is washed again by the deionized water.
(3) Utilizing an atomic layer deposition systemPreparing an absorption film, wherein the vacuum cavity and the reaction cavity system are both in a vacuum environment below 10mbar in the film preparation process, the substrate in the reaction cavity is heated and preheated and keeps heating in reaction, and N is introduced into the vacuum cavity and the reaction cavity2The flow rates of (1) are 200sccm and 600sccm, respectively. The control of the thickness of the film layer can be realized by controlling the deposition speed and the deposition period.
As shown in fig. 3, the single cycle atomic layer deposition process includes four steps, which are summarized as two half-reactions, where a reaction precursor is introduced at the beginning of each half-reaction, and then a purge gas is introduced to purge excess reactants and byproducts. The method for alternately depositing the titanium aluminum compound TiAlC of the absorption film layer by utilizing the atomic layer deposition system comprises the following specific steps:
the substrate in the reaction chamber is preheated by heating and is maintained at 350 ℃ for reaction.
(1) Pulse 1: with N2Introducing excessive first precursor TiCl into the reaction chamber as carrier gas4Pulse time of 3s, TiCl4Chemically adsorbing on the surface of the substrate until the substrate is saturated;
(2) puge 1: inert gas N is introduced2Adding excessive TiCl4And excessive byproducts generated in the step of Pulse1 are purged from the reaction chamber, the purging time is 10s, and the first half reaction is finished;
(3) pulse 2: with N2Introducing excessive TMA (trimethyl aluminum) as a second precursor into the carrier gas, wherein the Pulse time is 0.3s, and the excessive TMA and the surface groups generated in the half reaction of Pulse1 are subjected to chemical reaction until the second precursor is saturated;
(4) puge 2: inert gas N is introduced2To remove excess reactants and byproducts, with a purge time of 10s, leaving only the titanium aluminide TiAlC on the substrate and the second half-reaction completed.
As shown in FIG. 4, the present invention utilizes an atomic layer deposition system to alternately deposit a dielectric film layer of silicon dioxide SiO2The method comprises the following specific steps:
the substrate in the reaction chamber is preheated by heating and is maintained at 350 ℃ for reaction.
(1) Pulse 1: TBS (Tri-tert-butoxysilanol) was heated to 100 deg.CTo the saturated vapor pressure, in N2Introducing excessive first precursor TBS into a reaction cavity for carrier gas, wherein the pulse time is 0.5s, and the TBS is chemically adsorbed on the surface of a substrate until the TBS is in a saturated state;
(2) puge 1: inert gas N is introduced2Purging excess TBS and excess by-products generated in the Pulse1 step from the reaction chamber for 6s, and completing the first half reaction;
(3) pulse 2: with N2Introducing excessive TMA as a second precursor into the carrier gas, wherein the Pulse time is 0.3s, and the excessive TMA and surface groups generated in the half reaction of Pulse1 are subjected to chemical reaction until the second precursor is saturated;
(4) puge 2: inert gas N is introduced2To remove excess reactants and by-products, with a purge time of 8s, leaving only silica on the substrate, and the second half-reaction is complete.
Example 1: the specific film structure in the visible light band is preferably substrate | TiAlC (15nm) | SiO2(41nm)|TiAlC(240nm)|SiO2(17nm)|TiAlC(23nm)|SiO2(63nm), as shown in FIG. 5. The final equivalent admittance of the film system is matched with the admittance of the incident medium air, and the incident light beam generates destructive interference effect when being reflected on the surface of the film layer, thereby reducing the reflection loss of the surface of the film system. When incident from the air side, the average reflectance in the visible light band of 400-700nm is as low as 0.39%, as shown in (a) of FIG. 6; when incident from the substrate side, the average reflectance in the visible light band of 400-700nm was 0.91%, as shown in (b) of FIG. 6.
Substrate of absorbing film structure | TiAlC (15nm) | SiO2(41nm)|TiAlC(240nm)|SiO2(17nm)|TiAlC(23nm)|SiO2(63nm), a TiAlC chemical substance close to the substrate side is used as an absorption layer, a TMA precursor is fully decomposed at the reaction temperature of 350 ℃, the Ti and Al content in the film is high, the film is less oxidized after being exposed in the air, the oxygen content of the film is very low, the thickness of the film is 240nm, the film layer is thick enough, light is hardly transmitted through a device, the antireflection layer is combined, so that the final equivalent admittance of the film system is matched with the admittance of the air of an incident medium, and the high absorption of a visible light waveband of 400-ion 700nm is realized, wherein when the film is incident from the air side, the average absorption rate is as high as99.5%, as shown in fig. 7 (a); when incident from the substrate side, the average absorptance was 99%, as shown in fig. 7 (b).
Example 2: the absorption film in the visible-near infrared band takes the full absorption in the 400-1100nm band as the design target, and the specific absorption film system structure is preferably the substrate | TiAlC (10nm) | SiO2(60nm)|TiAlC(30nm)|SiO2(42nm)|TiAlC(230nm)|SiO2(28nm)|TiAlC(34nm)|SiO2(43nm)|TiAlC(21nm)|SiO2(80nm), as shown in FIG. 8, the average reflectance in the visible-near infrared band 400-1100nm at the time of incidence from the air side is as low as 0.77%, as shown in (a) of FIG. 9; the visible-near infrared band 400-1100nm average reflectance upon incidence from the substrate side was 0.50%, as shown in (b) of FIG. 9.
The absorption of the visible-near infrared band is obviously increased, the middle absorption layer is thick enough, so that no light is transmitted through the device, the reflection loss of the band is further reduced by the antireflection combination of the upper layer and the lower layer, and the absorption efficiency is improved, so that the high absorption of the visible-near infrared band of 400-1100nm is realized. Wherein the average absorption rate when incident from the air side was 99.06%, as shown in (a) of fig. 10; when incident from the substrate side, the average absorption was 99.34%, as shown in fig. 10 (b).

Claims (10)

1. An absorption film based on atomic layer deposition is composed of a substrate and a multi-layer absorption film system on the substrate, and is characterized in that the multi-layer absorption film system is composed of absorption film layers and medium film layers in an alternating mode, the absorption film layers are the innermost layers and are arranged close to the substrate; the dielectric film layer is the outermost layer; the multilayer absorption film is obtained by an atomic layer deposition method.
2. The atomic layer deposition based absorber film according to claim 1, wherein the absorber film layer is a titanium aluminide film layer.
3. The atomic layer deposition-based absorption film according to claim 1, wherein the dielectric film layer is a film layer composed of one or more mixed materials of oxide, nitride, fluoride, sulfide and selenide.
4. The atomic layer deposition-based absorption film according to claim 3, wherein the dielectric film layer is a film layer composed of one or more mixed materials of titanium dioxide, silicon dioxide, aluminum oxide, hafnium oxide, tantalum oxide, silicon nitride, titanium nitride, magnesium fluoride, yttrium fluoride, zinc sulfide, molybdenum sulfide, and zinc selenide.
5. The atomic layer deposition based absorber film according to claim 1, wherein the multilayer absorber film system is (titanium aluminide/silicon dioxide)SAnd S is an integer and represents an alternating number.
6. The atomic layer deposition based absorber film according to claim 1, wherein the thickness of the dominating absorber film layer is greater than 100 nm.
7. The atomic layer deposition-based absorber film of claim 1, wherein the thickness of the absorber film layer is each independently selected from 10nm to 1000 nm; the thickness of the dielectric film layer is 10 nm-300 nm.
8. The atomic layer deposition based absorber film according to claim 5, wherein S is 2-30; the thickness of the thickest absorbing film layer is 200 nm-300 nm; the thickness of the rest absorption film layers is 10 nm-100 nm; the thickness of the dielectric film layer is 10 nm-80 nm.
9. The method for preparing the atomic layer deposition-based absorption film according to any one of claims 1 to 7, wherein the multi-layer absorption film system is deposited on the substrate layer by using an atomic layer deposition method.
10. The method for preparing the atomic layer deposition-based absorption film according to claim 9, wherein the absorption film layer is a titanium aluminum compound film layer obtained by atomic layer deposition from precursors of trimethylaluminum and titanium tetrachloride; the dielectric film layer is a silicon dioxide film layer and is obtained by atomic layer deposition of a precursor tri-tert-butoxy silanol and trimethylaluminum.
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