CN109581564B - Multilayer metal ceramic film with structural color and preparation method thereof - Google Patents
Multilayer metal ceramic film with structural color and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a multilayer metal ceramic film with structural colors, which sequentially comprises a metal layer, a dielectric layer and a metal nanowire array-ceramic composite layer from a substrate to the outside; in the metal nanowire array-ceramic composite layer, metal nanowires are vertically distributed in a ceramic phase, the diameter of each metal nanowire is not less than 2nm, the height of each metal nanowire is the same as the thickness of the metal nanowire array-ceramic composite layer, and the distance between every two metal nanowires is 1.5-20 nm. The absorption characteristic of the multilayer metal ceramic film in the visible light wave band range is easy to regulate, and the obtained color has a large color gamut range and good brightness and saturation. Also discloses a preparation method of the multilayer metal ceramic film with structural colors, which is simple, low in cost and suitable for large-area preparation.
Description
Technical Field
The invention belongs to the field of nano materials, and particularly relates to a multilayer metal ceramic film with structural colors and a preparation method thereof.
Background
Traditional chemical dyes and pigments produce different colors through selective absorption of visible light, but they tend to be toxic and harmful, are not environment-friendly, are susceptible to fading under illumination and high temperature, and are difficult to recycle. Compared with chemical dyes, the structural color material based on the artificial microstructure has the characteristics of being recyclable, convenient to use, good in chemical stability and the like, and meanwhile, the diffraction limit can be broken through, and the imaging resolution is improved. The characteristics enable the structural color to have important potential application in the fields of ultrahigh resolution imaging, flat panel display, optical sensing detection, high-end optical anti-counterfeiting and the like.
The light irradiates on the surface of the metal to induce the collective oscillation of the free charges of the metal, namely the surface plasmon. Coupling between photons and free electron gas in the metal micro-nano structure forms plasmon resonance to absorb (or radiate) visible light in a specific frequency band, so that a plasmon structure color is generated. The purpose of regulating and controlling the light characteristics is achieved by changing the appearance and the size of the plasmon metal nano structure, so that different colors can be produced by the same material, and the manufacturing process of units with different colors is greatly simplified. Compared with periodic medium structures such as photonic crystals and semiconductor nanowires, the size of the device can be more miniaturized due to the plasmon effect of the strong confinement on the surface of the nano metal structure. The anisotropy of the noble metal nanowire structure causes the surface plasmon resonance of the noble metal nanowire structure to have multiple resonance modes such as axial resonance mode and radial resonance mode, and the array formed by a large number of nanowires with adjacent spacing smaller than 5nm enables the resonance modes to show strong coupling, so that the multiband selective absorption characteristic of the noble metal nanowire structure to light can be realized. In a nanowire array, the electric field is strongly localized between adjacent nanowires, and standing wave resonances also occur. In addition, the dipoles generated by the metal nanowires in the alternating electromagnetic field induce image charges in the metal layer, and more complex coupling action among plasmon resonance modes can be realized. As a plurality of mechanisms simultaneously act, the color development regulation and control of related micro-nano structures can be more flexible and diversified. Meanwhile, the metal structure can be used as an electrode of a device while exciting a plasmon, so that the driving of an external power supply is realized, and the metal structure has a huge application prospect in the field of photoelectric integration.
Chinese patent publication No. CN104914494A discloses a method for obtaining full-color spectrum structural color by using nano-imprint to prepare metal holes with a chassis, wherein the nano-structure is a series of four-direction arranged hole array patterns with different diameters/periods, and has an abnormal transmission peak with adjustable peak position (360 nm-810 nm) in a visible light band.
The chinese patent publication No. CN108059829A discloses a strength-enhanced low-angle dependent structural color material and a preparation method thereof, the material is composed of an anti-protein photonic crystal and an elastomer filled in pores of the anti-protein photonic crystal anti-protein structure, and the color of the material is not changed under different observation angles and different tensile strengths.
At present, for obtaining a metal micro-nano structure manufactured artificially, common micro-nano processing technologies comprise electron beam lithography technology, nano imprinting technology, focused ion beam etching technology, laser direct writing technology and the like. The methods have complex process, high cost and high requirements on equipment, and are difficult to realize large-area preparation. In addition, typical structural colors include metal grating nanostructures, metal film nanohole structures, metal-dielectric-metal resonant structures, and the like, and these structures often have poor stability and mechanical properties in atmospheric environment, further limiting their practical applications.
Disclosure of Invention
The invention provides a multilayer metal ceramic film with structural colors and a preparation method thereof, the absorption characteristic of the film in a visible light wave band range is easy to regulate, and the obtained color has a large color gamut range and good brightness and saturation.
The technical scheme of the invention is as follows:
a multilayer metal ceramic film with structural color sequentially comprises a metal layer, a dielectric layer and a metal nanowire array-ceramic composite layer from a substrate to the outside;
in the metal nanowire array-ceramic composite layer, metal nanowires are vertically distributed in a ceramic phase, the diameter of each metal nanowire is not less than 2nm, the height of each metal nanowire array-ceramic composite layer is the same as the thickness of the metal nanowire array-ceramic composite layer, and the distance between every two metal nanowires is 1.5-20 nm.
In the multilayer metal ceramic film, the metal nanowire arrays are distributed in the ceramic phase orderly and densely, different nanowire microstructures can be obtained by controlling the distribution state of the metal nanowire arrays, the different nanowire microstructures have different colors corresponding to samples, the metal layer mainly plays a role in transmitting and reflecting incident light, the dielectric layer is positioned between the metal layer and the metal nanowire array-ceramic composite layer and mainly regulates and controls the charge coupling effect between the metal nanowires and the metal layer, so that the absorption peak position of the composite film can be controlled accurately, and the color of a device can be regulated and controlled.
When the diameter of the metal nanowires in the metal nanowire array-ceramic composite layer is not less than 2nm, the distance between the metal nanowires is 1.5-20nm, and the volume percentage of the metal nanowires in the metal nanowire array-ceramic composite layer is 5% -60%.
The response characteristic of the multilayer metal ceramic film to incident light is closely related to the microstructure characteristics of the metal nanowires, namely the size and arrangement condition of the metal nanowires and the dielectric constant of the medium around the nanowires. Moderate changes of the diameters and adjacent distances of the nanowires can remarkably regulate and control the resonance frequency of surface plasmons, and cause the movement of absorption peak positions and obvious changes of absorption strength. Therefore, in order to obtain the multilayer metal ceramic film with large color gamut range and good brightness and saturation, the diameter of the metal nanowires is 3-7 nm, and the distance between the metal nanowires is 2.5-10 nm. Thus, the volume percentage of the metal nanowires in the metal nanowire array-ceramic composite layer reaches 10-40%.
Preferably, the thickness of the metal nanowire array-ceramic composite layer is 50-300 nm.
The dielectric layer and the metal layer have small regulation amplitude on the absorption characteristic, and the obtained color can be finely adjusted. In order to accurately regulate and control the strength of charge coupling between the metal nanowire and the metal layer and accurately control the absorption peak position of the composite film, so that the color of the device is regulated and controlled, and the thickness of the dielectric layer is 0.5-30 nm. In order to meet the dual requirements of color development in a reflection mode or a transmission mode, the thickness of the metal layer is 3-200 nm.
The metal layer material is the same as the metal nanowire material, and the dielectric layer material is the same as the ceramic phase material. Therefore, the preparation method is simplified while the absorption characteristic of the multilayer metal ceramic film in the visible light wave band range is easy to regulate and control.
Preferably, the metal material is one of gold, platinum, silver, copper and aluminum, or an alloy of any two of them, that is, the metal nanowire may be a gold, platinum, silver, copper or aluminum nanowire, the metal layer may be a gold, silver, aluminum or platinum layer, and may also be a gold-silver, gold-platinum or silver-aluminum alloy layer; the dielectric layer material is oxide, nitride, carbide, boride or silicon dioxide; the ceramic phase is an oxide, nitride, carbide, boride or silica.
A preparation method of a multilayer metal ceramic film with structural colors comprises the following steps:
(1) pretreating a substrate;
(2) selecting metal and ceramic as target materials, controlling the metal target to work, and carrying out magnetron sputtering deposition on the surface of the substrate treated in the step (1) to obtain a metal layer; then, controlling the ceramic target to work, and carrying out magnetron sputtering deposition on the metal layer to deposit a dielectric layer; finally, controlling the metal target and the ceramic target to work simultaneously, and depositing a metal nanowire array-ceramic composite layer on the dielectric layer through magnetron sputtering to obtain a multilayer metal ceramic film;
during magnetron sputtering, the metal target is driven by a pulse, radio frequency or direct current power supply, and the ceramic target is driven by a radio frequency power supply.
Compared with common micro-nano processing means, the preparation process of magnetron sputtering is simple, the parameter adjustment is convenient, and the selection range of compound ceramics and metal is wider. In the sputtering process, the arrangement and the size of the metal nanowires in the composite film are adjusted in a large range by regulating and controlling the power of the compound ceramic target and the metal target and combining with the regulation of low-energy ion bombardment with the selective etching effect.
Wherein the substrate can be a metal material (copper, aluminum, stainless steel, etc.), or an inorganic non-metal material (glass, ceramic, oxide, nitride, etc.), or a flexible material (PET, PI, PVA, etc.). In order to facilitate optical testing, the substrate is made of quartz, sapphire, glass slide, PET, organic glass and other transparent materials.
In the step (1), the pretreatment process of the substrate comprises: carrying out ultrasonic cleaning on the transparent substrate by using acetone, ethanol and deionized water in sequence, and then carrying out heating desorption and plasma sputtering cleaning to optimize the surface cleanliness of the substrate; for organic or flexible substrates, ultrasonic cleaning is performed only with a cleaning agent and deionized water, and surface activation treatment is performed. After the substrate is pretreated, the high-quality growth of the metal ceramic film is facilitated.
In the step (2), magnetron sputtering is performed in an argon atmosphere. The change of the microstructure characteristics such as the size, the spacing and the like of the metal nanowires can be realized to a greater extent by adjusting the power of the magnetron sputtering metal target and the compound ceramic target, combining the selective etching of substrate bias plasmas with different powers and the change of the deposition time. The composite films with different microstructures and the dielectric layers with different thicknesses act together, so that the absorption peak position in a visible wave band can be adjusted and controlled according to expectation, and the structural color covered by full color can be obtained.
Preferably, when the metal nanowire array-ceramic composite layer is sputtered and deposited, the power density range of the sputtering metal target is 0.3-1.5W/cm2(ii) a The power density range of the sputtering ceramic target is 2.5-15W/cm2The sputtering pressure range is 0.1-1 Pa, and the target base distance is higher than 70 mm.
When the substrate is an insulating transparent substrate, the type of the substrate bias voltage is a radio frequency bias voltage; when the substrate is an insulating conductive transparent substrate, the type of the substrate bias voltage is a radio frequency bias voltage or a pulse bias voltage; the substrate bias power density is in the range of 0.5-3W/cm2The self-bias voltage is higher than-50V. When the substrate bias power density is lower than 0.5W/cm2In the process, the metal is difficult to realize selective growth, and the self-organization growth of the nanowire array structure cannot be realized, so that the selective absorption performance and the color of the multilayer film are not ideal.
Further, when the metal nanowire array-ceramic composite layer is sputtered and deposited, the power density range of the sputtering metal target is 0.5-1.2W/cm2(ii) a The power density range of the sputtering ceramic target is 5-12W/cm2The sputtering pressure is 0.15-0.6 Pa, the target base distance is higher than 90mm, and the substrate bias power density is 1-2.5W/cm2The self-bias voltage is higher than-70V.
The multilayer metal ceramic film can also comprise a metal nanowire array-ceramic composite layer, a dielectric layer and a metal layer from the substrate to the outside in sequence, and the specific structural parameter limitation is the same as that described above.
The multilayer metal ceramic film has a plurality of absorption peaks, is insensitive to incident angle, and has the variation range of the absorption peaks in visible light and near infrared bands of 350-1000 nm.
Compared with the prior art, the invention has the following advantages:
(1) compared with common micro-nano processing means such as photoetching and the like, the magnetron sputtering method adopted by the invention does not need a template, has simple process and lower cost, is suitable for large-area preparation and is convenient for parameter adjustment. Different from the existing mode of generating structural color, the action mechanism between the closely arranged superfine metal nanowire array and the metal layer structure and the incident light is more diversified, so that the regulation and control means is more flexible, and the obtained color is richer.
(2) The invention has wider selection range of metal materials and ceramic matrixes, and different metals or ceramic materials can be selected in each layer to construct the composite film according to the requirements so as to meet the requirements of different practical applications.
(3) The invention has no special requirement on the used substrate material, and rigid or flexible, insulating or conductive, organic or inorganic materials can be used as the substrate, thereby greatly expanding the application range of related devices.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a low-magnification TEM morphology of a cross-section of a cermet multilayer composite film prepared in example 1;
FIG. 2 is a high power TEM topography of a cermet multilayer composite film cross-section prepared in example 1;
FIG. 3 is an optical photograph of the cermet multilayer composite film prepared in example 1 and the corresponding absorption spectrum;
FIG. 4 is a high power TEM topography of a cermet multilayer composite film cross-section prepared in example 2;
FIG. 5 is an optical photograph of the cermet multilayer composite film prepared in example 2 and the corresponding absorption spectrum;
fig. 6 is an optical photograph of a large-area cermet multilayer composite film deposited on the flexible PET substrate prepared in example 3.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be further described in detail with reference to the accompanying drawings and examples. It should be understood that the detailed description and specific examples, while indicating the scope of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
In the following examples, silicon wafers, quartz wafers and PET were used as substrates, gold and silver were selected as metal materials, silica and alumina were selected as ceramic materials, silica and alumina were selected as dielectric materials, and gold thin films were selected as metal layer materials. By adjusting the relevant sputtering parameters, the size and distribution of the metal nanowires in the metal ceramic film layer are changed, the thickness of the dielectric layer is adjusted, and the composite films with different colors are prepared. And testing the reflection performance of the light source by using a spectrum type ellipsometer, and characterizing the response characteristic of the light source to incident light.
Example 1
Sequentially and respectively ultrasonically cleaning a silicon wafer and a quartz wafer for 15min by using acetone, ethanol and deionized water to remove surface pollutants; drying the cleaned silicon wafer by using nitrogen, and fixing the silicon wafer on a substrate tray; the tray is loaded into the deposition chamber of the magnetron sputtering device and is pre-vacuumized to 10 DEG at the same time-4Pa below; introducing argon gas flow to keep the pressure of the deposition chamber at 0.4Pa, cleaning the gold target material and the silicon dioxide target material for 10min by using radio frequency sputtering, and applying bias voltage to clean the substrate for 5 min; after etching and cleaning, adjusting the air pressure of the deposition chamber to 0.3Pa, closing a silicon dioxide target power supply, opening a baffle plate in front of the gold target, starting sputtering, and adjusting the sputtering power density of the gold target to 3.5W/cm2And depositing a metal layer for 25 min. The gold target driving power supply is closed, the silicon dioxide target driving power supply is started at the same time, and the power density is set to be 5W/cm2While applying a substrate biasThe power density is 1W/cm2And depositing a silicon dioxide dielectric layer for 5 min. Starting the gold target driving power supply again, co-sputtering the two targets, wherein the sputtering power densities of the gold target and the silicon dioxide target are respectively 0.8W/cm2And 5W/cm2The substrate bias power density is 2.5W/cm2And after 1h of deposition, closing the gold target, the silicon dioxide target and the bias driving power supply to finally obtain the multilayer metal ceramic film with structural color.
The cross-sectional morphology of the thin film sample is observed and analyzed by a Transmission Electron Microscope (TEM). Fig. 1 shows the low-power cross-sectional TEM morphology of the color thin film of the multilayer structure in example 1, and the layering situation and different thicknesses of the metal ceramic composite layer, the dielectric layer and the metal layer of the nanowire array can be clearly seen from the figure. The thickness of the metal nanowire array-ceramic composite layer is 110-120 nm, wherein the gold nanowires are embedded in the silicon dioxide matrix and are in a typical periodic arrangement structure, and the thickness of the metal layer serving as a reflecting layer is larger than 150 nm. FIG. 2 is a high-power cross-sectional TEM morphology of the multilayer structure color thin film in example 1, and it can be observed that the average diameter of the gold nanowires is about 6nm, the edge distance is 2.5-3 nm, and the thickness of the silicon dioxide dielectric layer is within the range of 5-7 nm.
FIG. 3 is an optical photograph of the color film of the multi-layered structure of example 1 and the corresponding absorption spectrum. The sample appeared bright yellow with a higher reflectivity in the yellow band. From fig. 3, it can be found that the main surface plasmon absorption peak of the sample is located around 495 nm.
Example 2
Sequentially and respectively ultrasonically cleaning a silicon wafer and a quartz wafer for 15min by using acetone, ethanol and deionized water to remove surface pollutants; drying the cleaned silicon wafer by using nitrogen, and fixing the silicon wafer on a substrate tray; the tray is loaded into the deposition chamber of the magnetron sputtering device and is pre-vacuumized to 10 DEG at the same time-4Pa below; introducing argon gas flow to keep the pressure of the deposition chamber at 0.4Pa, cleaning the gold target material and the silicon dioxide target material for 10min by using radio frequency sputtering, and applying bias voltage to clean the substrate for 5 min; after the etching cleaning is finished, adjusting the air pressure of the deposition chamber to 0.3Pa, closing a silicon dioxide target power supply, opening a baffle plate in front of the gold target, starting sputtering, and adjusting the power density of the gold targetThe degree is 3.5W/cm2And depositing a metal reflecting layer for 25 min. The gold target driving power supply is closed, the silicon dioxide target driving power supply is started at the same time, and the power density is set to be 5W/cm2While applying a substrate bias power density of 1W/cm2And depositing a silicon oxide dielectric layer for 10 min. Starting the gold target driving power supply again, co-sputtering the two targets, wherein the sputtering power densities of the gold target and the silicon dioxide target are respectively 0.8W/cm2And 5W/cm2The substrate bias power density is 2.5W/cm2And after 1.1h of deposition, closing the gold target, the silicon dioxide target and the bias driving power supply, and finally obtaining the multilayer metal ceramic film with structural color.
And observing and analyzing the cross-sectional morphology of the film sample by a TEM. FIG. 4 shows the high-power cross-sectional TEM morphology of the multilayer structure color thin film in example 2, and it can be observed that the average diameter of the gold nanowires is about 8nm, and the edge distance is 2-2.5 nm. Compared with the embodiment 1, the method proves that the diameter, the spacing and other structural parameters of the gold nanowires in the metal ceramic composite layer can be regulated and controlled by changing the sputtering power and other deposition parameters of the target. Fig. 5 is an optical photograph of the sample of example 2 and the corresponding reflectance spectrum. The sample showed a purple red color, and compared with example 1, the intensity of the surface plasmon absorption peak was increased, and the peak position was red-shifted by about 40nm, confirming that the color appearance of the multilayer composite film can be significantly affected by the change of the gold nanowire structure.
Example 3
Sequentially and respectively ultrasonically cleaning the PET sheet for 15min by using acetone, ethanol and deionized water to remove surface pollutants; drying the cleaned silicon wafer by using nitrogen, and fixing the silicon wafer on a substrate tray; the tray is loaded into the deposition chamber of the magnetron sputtering device and is pre-vacuumized to 10 DEG at the same time-4Pa below; introducing argon gas flow to keep the pressure of the deposition chamber at 0.4Pa, cleaning the silver target material by direct current sputtering, cleaning the aluminum oxide target material by radio frequency sputtering for 20min, and cleaning the substrate by applying bias voltage for 5 min; after the etching cleaning is finished, the air pressure of the deposition chamber is adjusted to 0.25Pa, a baffle plate in front of the silver target and the silicon dioxide target is opened, the co-sputtering is started, and meanwhile, the substrate bias voltage is applied. Wherein the sputtering power density of the silver target and the alumina target is 1.5W/cm respectively2And 4.5W/cm2The substrate bias power density is 2.4W/cm2. And after depositing for 1.5h, closing the silver target driving power supply, and continuously depositing a silicon oxide dielectric layer for 15 min. The alumina target driving power supply and the bias power supply are closed, the silver target driving power supply is started, and the sputtering power density of the silver target is adjusted to be 2.8W/cm2And depositing a metal reflecting layer for 30 min. And (5) closing the silver target driving power supply to finally obtain the structural color film on the flexible substrate.
Fig. 6 is an optical photograph of the structural color film on the large-area PET substrate in the bending state in example 3, which proves that the preparation method of the present invention is suitable for various substrates such as flexible substrates, rigid substrates, etc., and can be used for large-area preparation, and the obtained structural color film has good mechanical properties.
The above-mentioned embodiments are intended to illustrate the technical solutions and advantages of the present invention, and it should be understood that the above-mentioned embodiments are only the most preferred embodiments of the present invention, and are not intended to limit the present invention, and any modifications, additions, equivalents, etc. made within the scope of the principles of the present invention should be included in the scope of the present invention.
Claims (8)
1. The multilayer metal ceramic film with structural colors is characterized by comprising a metal layer, a dielectric layer and a metal nanowire array-ceramic composite layer from a substrate to the outside in sequence, wherein the metal layer is prepared by magnetron sputtering deposition;
in the metal nanowire array-ceramic composite layer, metal nanowires are vertically distributed in a ceramic phase, the diameter of each metal nanowire is not less than 2nm, the height of each metal nanowire is the same as the thickness of the metal nanowire array-ceramic composite layer, and the distance between every two metal nanowires is 1.5-20 nm;
the thickness of the metal nanowire array-ceramic composite layer is 50-300 nm, the thickness of the dielectric layer is 0.5-30 nm, and the thickness of the metal layer is 3-200 nm.
2. The multilayer cermet film with structural color of claim 1, wherein the metal nanowires have a diameter of 3 to 7nm and a spacing of 2.5 to 10 nm.
3. The structured color multilayer cermet film of claim 1, wherein the metal layer material and the metal nanowires material are the same, and the dielectric layer material and the ceramic phase material are the same.
4. The structural color multi-layer cermet film of claims 1 or 3, wherein the metallic material is one of gold, platinum, silver, copper, aluminum, or an alloy of any two; the dielectric layer is made of oxide, nitride, carbide or boride; the ceramic phase is an oxide, nitride, carbide or boride.
5. A method for preparing the multilayer metal ceramic film with structural color according to any one of claims 1 to 4, comprising the following steps:
(1) pretreating a substrate;
(2) selecting metal and ceramic as target materials, controlling the metal target to work, and carrying out magnetron sputtering deposition on the surface of the substrate treated in the step (1) to obtain a metal layer; then, controlling the ceramic target to work, and carrying out magnetron sputtering deposition on the metal layer to deposit a dielectric layer; finally, controlling the metal target and the ceramic target to work simultaneously, and depositing a metal nanowire array-ceramic composite layer on the dielectric layer through magnetron sputtering to obtain a multilayer metal ceramic film;
during magnetron sputtering, the metal target is driven by a pulse, radio frequency or direct current power supply, and the ceramic target is driven by a radio frequency power supply.
6. The method according to claim 5, wherein the sputtering power density of the sputtering target is 0.3-1.5W/cm2(ii) a The power density range of the sputtering ceramic target is 2.5-15W/cm2The sputtering pressure range is 0.1-1 Pa, and the target base distance is higher than 70 mm.
7. The method for preparing a multilayer cermet film having a structural color as set forth in claim 5, wherein when the substrate is an insulating transparent substrate, the type of the substrate bias voltage is a radio frequency bias voltage; when the substrate is an insulating conductive transparent substrate, the type of the substrate bias voltage is a radio frequency bias voltage or a pulse bias voltage; the substrate bias power density is in the range of 0.5-3W/cm2The self-bias voltage is higher than-50V.
8. The method according to claim 5, wherein the sputtering power density of the sputtering target is 0.5-1.2W/cm when the metal nanowire array-ceramic composite layer is sputtered and deposited2(ii) a The power density range of the sputtering ceramic target is 5-12W/cm2The sputtering pressure is 0.15-0.6 Pa, the target base distance is higher than 90mm, and the substrate bias power density is 1-2.5W/cm2The self-bias voltage is higher than-70V.
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