CN115867008A - Film system with selective electromagnetic shielding and high transmittance and preparation method thereof - Google Patents
Film system with selective electromagnetic shielding and high transmittance and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a film system with selective electromagnetic shielding and high transmittance, which comprises a curved optical window, an electromagnetic shielding functional film, an electrode film and an infrared anti-reflection film, wherein the curved optical window is provided with a plurality of transparent electrodes; the film system materials, structures and thicknesses of the electromagnetic shielding functional film and the electrode film are the same; the optical window adopts a curved surface, the functional coating is prepared on the concave surface of the optical window and is sealed in the system, the same effect as the prior art is realized, the external exposure of any functional coating is avoided, the damage of wind sand, rain erosion and radiation to the film layer caused by the external environment is thoroughly solved, and the capability of resisting severe environments such as high and low temperature, damp and hot and the like is greatly improved.
Description
Technical Field
The invention relates to the technical field of functional coatings, in particular to an optical window film layer system with frequency-selective electromagnetic shielding and high-transmittance functions and a preparation method thereof.
Background
In the military fields of aerospace, naval vessels and the like, electromagnetic interference of space environments of various aircrafts and weaponry is increasingly complex, and an optical window on the space environment needs to have high light transmittance and excellent imaging effect, so that the requirements of precise detection and observation are met. Meanwhile, the electromagnetic shielding performance is required to be excellent, and electromagnetic interference of enemy radars, interference systems and the like is effectively avoided. Generally, a composite functional coating is plated on a window for transmitting information between a photoelectric system and the outside, so that the problems of high-efficiency transmission of target information of the window and interference of information electromagnetic shielding are solved.
Patent CN 110519976A "a sapphire optical window with electromagnetic shielding function and preparation method" plates an aluminum oxide film layer on a sapphire substrate by an ion beam sputtering method, encapsulates a metal grid in the aluminum oxide film layer for protection, plates an electrode, an anti-reflection film and a hydrophobic film on the aluminum oxide film layer by an evaporation method, and plates a metal film by chemical plating, which has a good protection effect, but the preparation process is relatively complex and the cost is relatively high.
CN 109743872A, "a method for preparing an electromagnetic shielding film", prepares a grid structure layer by imprinting, and fills conductive silver paste in the groove to form a conductive grid. In patent CN 109652774A, "method for manufacturing electromagnetic shielding optical window of embedded metal grid", a Y2O3 film plated on a window by heat treatment is used to make the film generate random net cracks, and a metal grid with a thickness smaller than that of the Y2O3 film is deposited on the surface of the cracked film, so as to embed the metal grid. The surfaces of the metal grids of the two patents are not plated with a protective film, and the metal grids are exposed in the environment, are easy to oxidize, fall off and break, influence the electromagnetic shielding performance, and cannot be used in the environments of high and low temperature, damp and hot and the like for a long time.
Patent CN 101121575A "method for realizing selective metallization of glass surface by femtosecond laser" selectively irradiates silver nitrate film coated on glass surface by femtosecond laser to form silver particles, and realizes metallization of irradiated area by chemical copper plating. In patent CN 103442544A, "method for manufacturing embedded metal grid", a grid groove is formed by femtosecond laser scanning and etching, and copper is plated by chemical plating after heat treatment. The metal mesh grid prepared by the two methods has the advantages of high bonding strength, good wear resistance and the like, but the femtosecond laser processing efficiency is low, the cost is too high, and the metal mesh grid is not suitable for preparing a large-aperture optical window.
Patent CN 104837325A "preparation method of embedded metal net bars electromagnetic shielding optical window" coats titanium dioxide solution on the substrate through the method of spin-coating, form the crackle template after the natural drying, blade coating conductive silver thick liquid forms embedded random crackle metal net bars on the crackle template, can effectively avoid nanometer silver thick liquid to damage and cause optical window electromagnetic shielding performance to be destroyed, but titanium dioxide solution is as the chap liquid, volume shrink is serious in the drying process, make the crack warpage, increase crack width, influence optical window light permeability. In patent CN 104837326A, "method for manufacturing an electromagnetic shielding curved optical window with a metal grid structure", crack paint is coated on the surface of a substrate, a conductive metal layer is deposited on the surface of a crack template after drying, and a random crack metal grid is obtained after removing the crack template. The method avoids using titanium dioxide as a cracking liquid, but the metal grid is prepared on the convex surface of an optical window exposed to the external environment and is easily influenced by strong sunlight, rain erosion, sand erosion, complex electromagnetic counterenvironments and the like, so that the chemical denaturation, breakage or falling of a surface film layer of the metal grid and the metal grid are realized.
Patent CN 109407252A "high electromagnetic shielding optical window and manufacturing method thereof" protects the metal grid by placing it in the sandwich structure of two pieces of optical glass, avoids the metal grid from being affected by external environment, and can solve the problems of firmness and wear resistance. However, the transmittance of the two pieces of optical glass is affected, and the adhesive of the optical glass is aged after being irradiated by light for a long time, which affects the service life of the optical window.
In patent CN 110730608A, "a transparent infrared electromagnetic shielding optical window", the internal and external sides of gallate infrared glass are respectively plated with an antireflection film and a metal grid, and the metal grid is plated with a slip enhancing film and a protective film, which improve the mechanical strength, wear resistance and humidity and heat resistance of the grid, but the optical window has low transmittance and has a problem of long-term stability when exposed to external protective films.
In addition, the fixtures used for coating the optical window are expensive, each fixture has a budget of more than 10 ten thousand yuan, and generally cannot be purchased in large quantities, so that in the process of coating a batch of parts once, spare positions are often left on a tool disc of a vacuum coating machine, and the parts cannot be fully placed, so that the problems of coating material waste and low processing efficiency are caused.
Disclosure of Invention
The present invention aims to overcome the disadvantages of the prior art and to provide a film system with selective electromagnetic shielding and high transmittance and a method for preparing the same.
The purpose of the invention is realized by the following technical scheme: a film system with selective electromagnetic shielding and high transmittance comprises a curved optical window, an electromagnetic shielding functional film, an electrode film and an infrared antireflection film; the film system materials, structures and thicknesses of the electromagnetic shielding functional film and the electrode film are the same;
furthermore, a mesh grid groove is formed on the concave surface of the curved optical window; the electromagnetic shielding functional film is plated in the grid groove; the electrode film is plated on the electromagnetic shielding function film; the infrared antireflection film is coated in the whole effective caliber of the curved optical window;
furthermore, the period of the grid groove is 320 +/-10 microns to 500 +/-10 microns; the line width is 12 +/-2 mu m;
furthermore, the curved optical window adopts a K9 glass substrate, a ZnS substrate, a Si substrate or a Ge substrate;
furthermore, the film system materials of the electromagnetic shielding functional film and the electrode film comprise one or more of gold, silver, chromium, copper, aluminum, nickel, titanium and silver alloy;
furthermore, the film layer structure of the electromagnetic shielding functional film and the motor film comprises a connecting layer, a functional layer and a protective layer;
according to a further technical scheme, the infrared antireflection film comprises a single-layer or double-layer film prepared from one or two of magnesium fluoride, silicon dioxide and OS-50;
further, the present invention provides a method for preparing an optical window film system having frequency selective electromagnetic shielding and high-efficiency transmission functions, comprising the steps of: etching the photoresist of the curved optical window by laser direct writing and developing a grid groove by a developing process; depositing metal in the grid groove to obtain a metal grid;
further, the specific steps of depositing the metal include: evaporating an electromagnetic shielding functional film by adopting a physical vapor deposition mode; after removing the photoresist, evaporating an electrode film by adopting a physical vapor deposition mode; plating an infrared anti-reflection film on the effective aperture of the curved optical window in a physical vapor deposition mode;
the further technical scheme is that the evaporation temperature of an electromagnetic shielding functional film and an electrode film is evaporated by adopting a physical vapor deposition process is 60 to 120 ℃, the evaporation rate is 0.2 to 1.0nm/s, the vacuum degree is 3.0 multiplied by 10 < -3 > to 9.0 multiplied by 10 < -4 > Pa, the vacuum oxygen introduction amount is 8 to 12 sccm, the ion energy is 425 to 445eV, and the electron beam current is 63 to 83mA; the evaporation temperature of the infrared antireflection film evaporated by adopting a physical vapor deposition process is 160 to 240 ℃: the evaporation rate is 0.2 to 0.9nm/s, the vacuum degree is 3.0 multiplied by 10 < -3 > to 9.0 multiplied by 10 < -4 > Pa, the vacuum oxygen introduction amount of the OS-50 is 8 to 15 sccm, the vacuum oxygen introduction amount of the silicon dioxide is 0 sccm, the electron beam current of the OS-50 is 280 to 340mA, and the electron beam current of the silicon dioxide is 80 to 120mA.
The invention has the following advantages:
1. the optical window adopts a curved surface, the functional coating is prepared on the concave surface of the optical window and is sealed in the system, the same effect as the prior art is realized, meanwhile, the external exposure of any functional coating is avoided, the damage of wind, sand, rain erosion and radiation to the film layer brought by the external environment is thoroughly solved, and the capabilities of resisting high and low temperatures, damp and hot and other severe environments are greatly improved;
2. the electromagnetic shielding function film and the electrode film are made of the same film system material, structure and thickness, so that the respective functions of the electromagnetic shielding function film and the electrode film can not be influenced, and the electromagnetic shielding film and the electrode film can be respectively plated in different areas of two batches of products, for example, an optical part without the electromagnetic shielding function film is plated in the first batch, an electromagnetic shielding function film is plated in the second batch, the optical part with the electrode film is prepared, the two batches of parts are placed in a vacuum film plating machine at the same time, and the two films are simultaneously plated, so that the preparation efficiency can be improved, the utilization rate of film materials can be improved, waste is avoided, and the two batches of products are not required to be separately subjected to an evaporation process;
3. the invention is provided with the grid groove on the concave surface of the curved optical window of the optical system, after the film system is plated on the grid groove, a metal grid with a certain pattern is formed, the period of the metal grid is far more than visible light or infrared light, and is far less than the electromagnetic wavelength, because the period of the metal grid is far less than the electromagnetic wavelength, the metal grid has the electromagnetic shielding function, namely, the electromagnetic wave with longer wavelength can not pass through, and because the period of the metal grid is far more than the visible light or infrared light wavelength, the metal grid has little influence on the visible light or infrared light transmittance, and the metal grid has the frequency filtering function of transmitting high-frequency light waves and cutting off low-frequency microwaves due to the selection of the structural size;
4. the film system prepared by the invention has higher optical transmittance of a target waveband, higher penetration effect of the target waveband and good interference electromagnetic wave shielding effect, and the whole film system has better environmental adaptability such as high and low temperature resistance, damp and hot resistance and the like;
5. in the invention, the electromagnetic shielding function film and the electrode film are preferably made of the same film system material, structure and thickness, and can be provided with multiple layers in principle, the more the layers are, the higher the transmittance is, but each layer has absorption, the more the layers are, the higher the absorption is, and the transmittance is reduced; the more the number of layers is, the adhesive force and the stress of each layer are not matched, and the firmness is also deteriorated; in addition, the more the number of layers is, each layer has a certain error in the actual plating process, the more the number of layers is, the more the accumulated errors are, and the performance of the film layer may also be deteriorated, so that the structural arrangement is that the connecting layer, the functional layer and the protective layer can meet the use requirements of resistivity and film layer firmness;
6. the functional layer positioned in the middle of the film system structure is metal or metal alloy and plays a main function role, the connecting layer in the film system structure is used for enhancing the firmness of the combination between the substrate material and the functional layer, and the protective layer is used for separating the functional layer from air and protecting the metal or metal alloy of the functional layer from being scratched and from chemically reacting with the atmosphere;
7. the metal or the thickness of different layer positions in the film system structure is different, and the film system structure mainly aims to realize the respective functions, such as a connecting layer and a protective layer, and needs to realize the functions of connection and protection, and finally the film layer is firm and can bear the firmness of the film layer, so that the film system structure disclosed by the invention can be seen to have good firmness and no demolding phenomenon through an adhesion force test, the temperature cycle test result is better, the film system structure can be kept for 2 hours at minus 45 ℃ and plus 55 ℃ respectively and can be cycled for 3 times, the surface of a product is tested after the test, and a metal mesh grid is not cracked and does not fall off; the function of the functional layer is embodied on electromagnetic shielding, and the functional layer is plated with different metals and thicknesses, so that different surface resistances can be achieved, and the electromagnetic shielding efficiency is influenced finally;
8. according to the invention, the grid groove is etched on the concave surface of the curved optical window in a preferred laser direct writing mode, and the grid groove is developed by a developing technology, so that the laser direct writing mode has weak etching strength and low price, and can not generate fragments which are difficult to remove; although the strength of laser etching is weak, the structure of the etched grid groove is controlled, the period and the line width of the grid groove are controlled, and the generated metal grid has the frequency filtering function of transmitting high-frequency light waves and cutting off low-frequency microwaves by combining with the special film system; if femtosecond laser and other etching modes are adopted, the intensity is high, the price is more expensive, but more chips are generated, and the cleaning of the curved optical window is inconvenient.
Drawings
FIG. 1 is a schematic view of the structure of an optical window film system according to the present invention.
FIG. 2 is a flow chart of the process for preparing the optical window film system of the present invention.
FIG. 3 is a graph of the transmittance in the 800-1000nm range for the K9-320 samples prepared in example 4.
FIG. 4 is a graph showing the transmittance in the range of 8 to 12 μm of Zn-S-500 samples prepared in example 5.
FIG. 5 is a graph of the transmittance in the 800-1000nm range for the K9-400 samples prepared in example 3.
FIG. 6 is a graph showing the electromagnetic shielding efficiency in the range of 240MHz to 2.5GHz for the samples K9-400 prepared in example 3.
FIG. 7 shows the electromagnetic shielding efficiency of the K9-320 sample prepared in example 4 in the range of 240MHz-2.5 GHz.
FIG. 8 is a graph showing the electromagnetic shielding efficiency in the range of 240MHz to 2.5GHz of the ZnS-500 sample prepared in example 5.
FIG. 9 shows the electromagnetic shielding effectiveness in the range of 240MHz to 2.5GHz for the Ge-400 sample prepared in example 6.
FIG. 10 is a graph showing the electromagnetic shielding efficiency in the range of 240MHz to 2.5GHz of the Si-400 sample prepared in example 7.
In the figure, 1-K9 glass substrate, 2-electromagnetic shielding function film connecting layer, 3-electromagnetic shielding function film metal mesh grid layer, 4-electromagnetic shielding function film protective layer, 5-electrode connecting layer, 6-electrode metal mesh grid layer, 7-electrode protective layer and 8-infrared antireflection film.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings of the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
In addition, the embodiments of the present invention and the features of the embodiments may be combined with each other without conflict.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, or orientations or positional relationships that the present invention is used to usually place, or orientations or positional relationships that are usually understood by those skilled in the art, which are merely for convenience of description and simplification of the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and the like are used merely to distinguish one description from another, and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should also be noted that, unless otherwise explicitly stated or limited, the terms "disposed," "mounted," "connected," and "connected" are to be construed broadly and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in a specific case to those of ordinary skill in the art.
Example 1: the film system with selective electromagnetic shielding and high transmittance comprises a curved optical window, an electromagnetic shielding functional film, an electrode film and an infrared anti-reflection film; the film system materials, structures and thicknesses of the electromagnetic shielding functional film and the electrode film are the same; the optical window adopts a curved surface, the functional coating is prepared on the concave surface of the optical window and is sealed in the system, the same effect as the prior art is realized, meanwhile, the external exposure of any functional coating is avoided, the damage of wind, sand, rain erosion and radiation to the film layer brought by the external environment is thoroughly solved, and the capabilities of resisting high and low temperatures, damp and hot and other severe environments are greatly improved; the electromagnetic shielding function film and the electrode film are made of the same film system material, the same structure and the same thickness, so that the respective functions of the electromagnetic shielding function film and the electrode film cannot be influenced, the electromagnetic shielding film and the electrode film can be respectively plated in different areas of two batches of products, for example, the first batch is an optical part without the electromagnetic shielding function film, the second batch is an optical part with the electromagnetic shielding function film, the optical part with the electrode film is prepared, the two batches of parts are placed in a vacuum film plating machine at the same time, the two films are simultaneously plated, on one hand, the preparation efficiency can be improved, on the other hand, the utilization rate of the film material can be improved, the waste of the film material and the residual space in the vacuum film plating machine is avoided, and the two batches of products are not required to be separately subjected to the evaporation process.
A grid groove is formed in the concave surface of the curved optical window; the electromagnetic shielding functional film is plated in the grid groove; the electrode film is plated on the electromagnetic shielding function film; the infrared antireflection film is coated in the whole effective caliber of the curved optical window; the invention arranges the grid groove on the concave surface of the curved optical window of the optical system, and forms a metal grid with a certain pattern after plating the film layer system on the grid groove, and the invention preferentially plates the electrode film layer on the position required by the electromagnetic shielding function film layer, thereby not affecting the function of the electrode film layer; the infrared anti-reflection film is coated in the whole effective aperture of the curved surface optical window, which is beneficial to playing the role of protection and whole anti-reflection. The film system prepared by the invention has higher optical transmittance of a target waveband, higher penetration effect of the target waveband and good interference electromagnetic wave shielding effect, and the whole film system has better environmental adaptability such as high and low temperature resistance, damp and hot resistance and the like.
The period of the grid groove is 320 +/-10 mu m-500 +/-10 mu m; the line width is 12 +/-2 mu m; in this embodiment, the period of the metal mesh is much longer than the visible light or infrared light, and much shorter than the electromagnetic wavelength. The metal mesh grid has the electromagnetic shielding function because the period of the metal mesh grid is far shorter than the electromagnetic wavelength, namely, electromagnetic waves with longer wavelength can not pass through the metal mesh grid, and the period of the metal mesh grid is far longer than the wavelength of visible light or infrared light, so that the metal mesh grid has little influence on the transmittance of the visible light or the infrared light. The structure size is selected to enable the metal mesh grid to have the frequency filtering function of transmitting high-frequency light waves and cutting off low-frequency microwaves.
The curved optical window adopts a K9 glass substrate, a ZnS substrate Si substrate or a Ge substrate;
the film system material of the electromagnetic shielding function film and the electrode film comprises one or more of gold, silver, chromium, copper, aluminum, nickel, titanium and silver alloy;
the film layer structure of the electromagnetic shielding functional film and the motor film comprises a connecting layer, a functional layer and a protective layer; the electromagnetic shielding function film and the electrode film are made of the same film system material, structure and thickness, and can be provided with multiple layers in principle, the more the layers, the higher the transmittance, but each layer has absorption, the more the layers, the higher the absorption, and the transmittance may be reduced on the contrary; the more the number of layers, the mismatching of the adhesive force and the stress of each layer and the deterioration of the firmness are caused; in addition, the more the number of layers, the more each layer has a certain error in the actual plating process, the more the number of layers, the more the accumulated errors are, and the performance of the film layer may also become poor, so that the structural arrangement of the connecting layer, the functional layer and the protective layer can meet the use requirements of resistivity and film firmness; the functional layer positioned in the middle of the film system structure is metal or metal alloy and plays a main function role, the connecting layer in the film system structure is used for enhancing the firmness of the combination between the substrate material and the functional layer, and the protective layer is used for separating the functional layer from air and protecting the metal or metal alloy of the functional layer from being scratched and from chemically reacting with the atmosphere; the metal or the thickness at different layer positions in the film system structure is different, and the respective functions are mainly realized, for example, a connecting layer and a protective layer, the functions of connection and protection need to be realized, and finally, the film is firm and can bear the firmness of the film; the function of the functional layer is embodied on the electromagnetic shielding, and the functional layer is plated with different metals and thicknesses, so that different surface resistances can be achieved, and the electromagnetic shielding efficiency is finally influenced.
The infrared antireflection film includes a single-layer or double-layer film having a layer made of one or two of magnesium fluoride, silicon dioxide, and OS-50.
Example 2: a method for preparing an optical window film system with frequency selective electromagnetic shielding and high-efficiency transmission functions comprises the following steps: etching the photoresist of the curved optical window by laser direct writing and developing a grid groove by a developing process; depositing metal in the grid groove to obtain a metal grid;
according to the invention, the grid groove is etched on the concave surface of the curved optical window in a preferred laser direct writing mode, and the grid groove is developed by a developing technology, so that the laser direct writing mode has weak etching strength and low price, and can not generate fragments which are difficult to remove; although the intensity of laser etching is weak, the structure of an etched grid groove is controlled, the period and the line width of the grid groove are controlled, and then the special metal film layer system is deposited in the grid groove, so that the generated metal grid has the frequency filtering function of transmitting high-frequency light waves and cutting off low-frequency microwaves; if femtosecond laser etching is adopted, the intensity is high, the price is more expensive, but the generated debris is more, and the cleaning of the curved optical window is inconvenient. The grid groove can be prepared by adopting a mask method, but due to the slit diffraction effect, the mask method is difficult to uniformly prepare grid lines with the line width of micrometer magnitude on a large-area base surface; in addition, as the metal mesh is prepared on the inner surface of the curved optical window, other etching and developing modes such as a mask plate and the like are difficult to ensure to be consistent with the surface shape of the inner surface of the optical window, the manufactured mesh has a phenomenon of local unevenness. Laser direct writing photoetching focuses laser beams on the inner surface of an optical window, a direct writing path is controlled by a computer, and uniform grid lines can be obtained after development without using a mask plate.
The specific steps of depositing the metal include: evaporating an electromagnetic shielding functional film by adopting a physical vapor deposition mode; after removing the photoresist, evaporating an electrode film by adopting a physical vapor deposition mode; plating an infrared anti-reflection film on the effective aperture of the curved optical window in a physical vapor deposition mode; deposition techniques include physical vapor deposition, chemical vapor deposition, and the like. The physical vapor deposition uses a vacuum coating machine, the thickness of the film can be accurately controlled, the strength of the film is good, and the physical vapor deposition is widely adopted at present. The method for removing the photoresist attached to the optical window outside the grid comprises the step of placing the curved optical window with the grid groove developed into the acetone or N-methyl pyrrolidone solution.
The evaporation temperature of the electromagnetic shielding functional film and the electrode film is evaporated by adopting a physical vapor deposition process is 60 to 120 ℃, the evaporation rate is 0.2 to 1.0nm/s, and the vacuum degree is 3.0 multiplied by 10 -3 ~9.0×10 -4 Pa, vacuum oxygen introduction amount of 8-12 sccm, ion energy of 425-445 eV, and electron beam current of 63-83mA; the evaporation temperature of the infrared antireflection film evaporated by adopting a physical vapor deposition process is 160 to 240 ℃: the evaporation rate is 0.2 to 0.9nm/s, and the vacuum degree is 3.0 multiplied by 10 -3 ~9.0×10 -4 Pa, OS-50 vacuum oxygen introduction amount is 8-15 sccm, silicon dioxide vacuum oxygen introduction amount is 0 sccmThe electron beam current of-50 is 280 to 340mA, and the electron beam current of silicon dioxide is 80 to 120mA.
Example 3: the K9-400 sample is prepared by the following steps: on a clean K9 glass substrate engraved with grid grooves with the period of 400 +/-10 mu m and the line width of 12 +/-2 mu m, an electromagnetic shielding functional film is evaporated by adopting a physical vapor deposition method, materials of a connecting layer, a metal layer and a protective layer of the electromagnetic shielding functional film are respectively chromium, copper and chromium, the thicknesses of the connecting layer, the metal layer and the protective layer are respectively 10nm, 400nm and 20nm, and the evaporation parameters are as follows: the evaporation temperature is 120 ℃, the chromium evaporation rate is 0.3nm/s, the copper evaporation rate is 0.8nm/s, the vacuum degree is 3.0 multiplied by 10 -3 ~9.0×10 -4 Pa, electron beam current 72mA, vacuum oxygen introduction 8sccm.
Putting the sample piece plated with the electromagnetic shielding functional film into acetone or N-methylpyrrolidone solution for cleaning, removing residual photoresist, plating an electrode on the edge of a part in a physical vapor deposition mode, wherein the connecting layer, the metal layer and the protective layer of the electrode are respectively made of chromium, copper and chromium, the thicknesses of the connecting layer, the metal layer and the protective layer are respectively 10nm, 400nm and 20nm, and the parameters of evaporation are as follows: the evaporation temperature is 120 ℃, the chromium evaporation rate is 0.3nm/s, the copper evaporation rate is 0.8nm/s, and the vacuum degree is 3.0 multiplied by 10 -3 ~9.0×10 -4 Pa, electron beam current 72mA, vacuum oxygen introduction 8sccm.
An infrared antireflection film is plated on the electromagnetic shielding layer in a physical vapor deposition mode, wherein the infrared antireflection film materials are OS-50 and silicon dioxide, the thicknesses of the infrared antireflection film materials are 23nm and 163nm respectively, the evaporation temperature is 200 ℃, the evaporation rate of the OS-50 is 0.3nm/s, the evaporation rate of the silicon dioxide is 0.8nm/s, the vacuum degree is 3.0 multiplied by 10 < -3 > -9.0 multiplied by 10 < -4 > Pa, the vacuum oxygen flux of the OS-50 is 8sccm, the vacuum oxygen flux of the silicon dioxide is 0 sccm, the electron beam current of the OS-50 is 300mA, and the electron beam current of the silicon dioxide is 100mA.
Example 4: the K9-320 sample is prepared by the following steps: on a clean K9 glass substrate engraved with grid lines with the period of 320 +/-10 mu m and the line width of 12 +/-2 mu m, an electromagnetic shielding functional film is evaporated by adopting a physical vapor deposition method, materials of a connecting layer, a metal layer and a protective layer of the electromagnetic shielding functional film are respectively chromium, copper and chromium, the thicknesses of the connecting layer, the metal layer and the protective layer are respectively 10nm, 400nm and 20nm, and the parameters of evaporation are as follows: the evaporation temperature is 120 ℃, the chromium evaporation rate is 0.3nm/s, the copper evaporation rate is 0.8nm/s, the vacuum degree is 3.0 multiplied by 10 -3 ~9.0×10 -4 Pa, electron beam current 72mA, vacuum oxygen introduction 8sccm.
Putting the sample piece plated with the electromagnetic shielding functional film into acetone or N-methylpyrrolidone solution for cleaning, removing photoresist, plating an electrode on the edge of the part in a physical vapor deposition mode, wherein the connecting layer, the metal layer and the protective layer of the electrode are respectively made of chromium, copper and chromium, the thicknesses of the connecting layer, the metal layer and the protective layer are respectively 10nm, 400nm and 20nm, and the parameters of evaporation are as follows: the evaporation temperature is 120 ℃, the chromium evaporation rate is 0.3nm/s, the copper evaporation rate is 0.8nm/s, the vacuum degree is 3.0 multiplied by 10 -3 ~9.0×10 -4 Pa, electron beam current 72mA, ion aeration 8sccm.
An infrared antireflection film is plated on the electromagnetic shielding functional film by adopting a physical vapor deposition mode, wherein the first layer material and the second layer material of the infrared antireflection film are respectively OS-50 and silicon dioxide, the thicknesses of the first layer material and the second layer material are 23nm and 163nm respectively, the evaporation temperature is 200 ℃, the evaporation rate of the OS-50 is 0.3nm/s, the evaporation rate of the silicon dioxide is 0.8nm/s, the vacuum degree is 3.0 multiplied by 10 -3 ~9.0×10 -4 Pa, OS-50 vacuum oxygen introduction of 8sccm, silica vacuum oxygen introduction of 0 sccm, OS-50 electron beam current of 300mA, and silica electron beam current of 100mA.
Example 5: the ZnS-500 sample is prepared by the following steps: on a clean ZnS substrate engraved with grid lines with the period of 500 +/-10 mu m and the line width of 12 +/-2 mu m, an electromagnetic shielding functional film is evaporated by adopting a physical vapor deposition method, wherein materials of a connecting layer, a metal layer and a protective layer of the electromagnetic shielding functional film are respectively chromium, copper and chromium, the thicknesses of the connecting layer, the metal layer and the protective layer are respectively 10nm, 500nm and 20nm, and the evaporation parameters are as follows: the evaporation temperature is 120 ℃, the chromium evaporation rate is 0.3nm/s, the copper evaporation rate is 0.8nm/s, the vacuum degree is 3.0 multiplied by 10 -3 ~9.0×10 -4 Pa, electron beam current 72mA, vacuum oxygen introduction 8sccm.
Putting a sample piece plated with the electromagnetic shielding functional film into acetone or N-methyl pyrrolidone solution for cleaning, removing residual photoresist, plating an electrode layer on the edge of a part in a physical vapor deposition mode, wherein the connecting layer, the metal layer and the protective layer of the electrode are respectively made of chromium, copper and chromium, the thicknesses of the connecting layer, the metal layer and the protective layer are respectively 10nm, 500nm and 20nm, and evaporation parameters are as follows: the evaporation temperature is 120 ℃, the chromium evaporation rate is 0.3nm/s, and the copper evaporation rateAt 0.8nm/s and a vacuum of 3.0X 10 -3 ~9.0×10 -4 Pa, electron beam current 72mA, vacuum oxygen introduction 8sccm.
An infrared antireflection film is plated on the electromagnetic shielding functional film by adopting a physical vapor deposition mode, wherein the infrared antireflection film materials are OS-50 and silicon dioxide, the thicknesses of the OS-50 and the silicon dioxide are 23nm and 163nm respectively, the evaporation temperature is 200 ℃, the evaporation rate of the OS-50 is 0.3nm/s, the evaporation rate of the silicon dioxide is 0.8nm/s, and the vacuum degree is 3.0 multiplied by 10 -3 ~9.0×10 -4 Pa, OS-50 vacuum oxygen introduction of 8sccm, silica vacuum oxygen introduction of 0 sccm, OS-50 electron beam current of 300mA, and silica electron beam current of 100mA.
Example 6: the Ge-400 sample is prepared by the following steps: on a clean Ge substrate engraved with grid grooves with the period of 400 +/-10 mu m and the line width of 12 +/-2 mu m, an electromagnetic shielding functional film is evaporated by adopting a physical vapor deposition method, materials of a connecting layer, a metal layer and a protective layer of the electromagnetic shielding functional film are respectively chromium, copper and chromium, the thicknesses of the connecting layer, the metal layer and the protective layer are respectively 10nm, 400nm and 20nm, and the parameters of evaporation are as follows: the evaporation temperature is 120 ℃, the chromium evaporation rate is 0.3nm/s, the copper evaporation rate is 0.8nm/s, and the vacuum degree is 3.0 multiplied by 10 -3 ~9.0×10 - 4 Pa, electron beam current 72mA, vacuum oxygen introduction 8sccm.
Putting a sample piece plated with the electromagnetic shielding functional film into acetone or N-methyl pyrrolidone solution for cleaning, removing residual photoresist, plating an electrode on the edge of a part in a physical vapor deposition mode, wherein the connecting layer, the metal layer and the protective layer of the electrode are respectively made of chromium, copper and chromium, the thicknesses of the connecting layer, the metal layer and the protective layer are respectively 10nm, 400nm and 20nm, and the parameters of evaporation are as follows: the evaporation temperature is 120 ℃, the chromium evaporation rate is 0.3nm/s, the copper evaporation rate is 0.8nm/s, the vacuum degree is 3.0 multiplied by 10 -3 ~9.0×10 -4 Pa, electron beam current 72mA, vacuum oxygen introduction 8sccm.
Plating an infrared antireflection film on the electromagnetic shielding layer by physical vapor deposition, wherein the infrared antireflection film comprises OS-50 and silicon dioxide with thicknesses of 23nm and 163nm, evaporation temperature of 200 deg.C, evaporation rate of OS-50 of 0.3nm/s, evaporation rate of silicon dioxide of 0.8nm/s, and vacuum degree of 3.0 × 10 -3 ~9.0×10 -4 Pa, OS-50, the vacuum oxygen flux of 8sccm, the vacuum oxygen flux of 0 sccm,the OS-50 electron beam current is 300mA, and the silicon dioxide electron beam current is 100mA.
Example 7: the Si-400 sample is prepared by the following steps: on a clean Si substrate engraved with grid grooves with the period of 400 +/-10 mu m and the line width of 12 +/-2 mu m, an electromagnetic shielding functional film is evaporated by adopting a physical vapor deposition method, materials of a connecting layer, a metal layer and a protective layer of the electromagnetic shielding functional film are respectively chromium, copper and chromium, the thicknesses of the connecting layer, the metal layer and the protective layer are respectively 10nm, 400nm and 20nm, and the evaporation parameters are as follows: the evaporation temperature is 120 ℃, the chromium evaporation rate is 0.3nm/s, the copper evaporation rate is 0.8nm/s, the vacuum degree is 3.0 multiplied by 10 -3 ~9.0×10 - 4 Pa, electron beam current 72mA, vacuum oxygen introduction 8sccm.
Putting a sample piece plated with the electromagnetic shielding functional film into acetone or N-methyl pyrrolidone solution for cleaning, removing residual photoresist, plating an electrode on the edge of a part in a physical vapor deposition mode, wherein the connecting layer, the metal layer and the protective layer of the electrode are respectively made of chromium, copper and chromium, the thicknesses of the connecting layer, the metal layer and the protective layer are respectively 10nm, 400nm and 20nm, and the parameters of evaporation are as follows: the evaporation temperature is 120 ℃, the chromium evaporation rate is 0.3nm/s, the copper evaporation rate is 0.8nm/s, and the vacuum degree is 3.0 multiplied by 10 -3 ~9.0×10 -4 Pa, electron beam current 72mA, vacuum oxygen introduction 8sccm.
Plating an infrared antireflection film on the electromagnetic shielding layer by physical vapor deposition, wherein the infrared antireflection film comprises OS-50 and silicon dioxide with thicknesses of 23nm and 163nm, evaporation temperature of 200 deg.C, evaporation rate of OS-50 of 0.3nm/s, evaporation rate of silicon dioxide of 0.8nm/s, and vacuum degree of 3.0 × 10 -3 ~9.0×10 -4 Pa, OS-50 vacuum oxygen introduction of 8sccm, silica vacuum oxygen introduction of 0 sccm, OS-50 electron beam current of 300mA, and silica electron beam current of 100mA.
Example 8: firm experiment of film
The film layer firmness test is performed according to GJB2485-1995, and the film layer is firmly stuck on the surface of the film layer by using adhesive tape paper with the width of 2cm and the peel strength of not less than 2.74N/cm, and after the adhesive tape paper is vertically and quickly pulled up, the film layer does not fall off.
Samples prepared in examples 3 to 7 were set as experimental groups 1 to 5;
comparative group 1: the electrode is prepared by the same method as the embodiment 3, and the difference is that the materials of the connecting layer, the metal layer and the protective layer of the electrode are respectively chromium, copper and chromium, and the thicknesses of the connecting layer, the metal layer and the protective layer are respectively 10nm, 400nm and 20nm;
comparative group 2: the electrode is prepared by the same method as the embodiment 4, and the difference is that the materials of the connecting layer, the metal layer and the protective layer of the electrode are respectively iron, copper and iron, and the thicknesses of the connecting layer, the metal layer and the protective layer are respectively 8nm, 400nm and 15nm;
comparative group 3: the electrode is prepared by the same method as the embodiment 5, and the difference is that the connecting layer, the metal layer and the protective layer of the electrode are respectively made of gold, copper and aluminum, and the thicknesses of the connecting layer, the metal layer and the protective layer are respectively 8nm, 400nm and 10nm;
comparative group 4: the electrode is prepared by the same method as the embodiment 6, and the difference is that the materials of the connecting layer, the metal layer and the protective layer of the electrode are respectively silver, copper and nickel, and the thicknesses of the connecting layer, the metal layer and the protective layer are respectively 9nm, 400nm and 12nm;
comparative group 5: the electrode is prepared by the same method as the embodiment 7, and the difference is that the materials of the connecting layer, the metal layer and the protective layer of the electrode are respectively aluminum, copper and titanium, and the thicknesses are respectively 10nm, 400nm and 18nm;
the results of the experiment are shown in table 1.
Example 9: temperature cycling experiment
The temperature cycle experiment is carried out according to GJB2485-1995, the temperature is respectively kept for 2h at-45 ℃ and +55 ℃, the cycle is 3 times, and the surface of the product is inspected after the experiment, so that the metal mesh grid is not broken and does not fall off.
Samples prepared in examples 3 to 7 were set as experimental groups 1 to 5;
comparative group 1: the electrode is prepared by the same method as the embodiment 3, and the difference is that the materials of the connecting layer, the metal layer and the protective layer of the electrode are respectively chromium, copper and chromium, and the thicknesses of the connecting layer, the metal layer and the protective layer are respectively 10nm, 400nm and 20nm;
comparative group 2: the electrode is prepared by the same method as the embodiment 4, and the difference is that the materials of the connecting layer, the metal layer and the protective layer of the electrode are respectively iron, copper and iron, and the thicknesses of the connecting layer, the metal layer and the protective layer are respectively 8nm, 400nm and 15nm;
comparative group 3: the electrode is prepared by the same method as the embodiment 5, and the difference is that the connecting layer, the metal layer and the protective layer of the electrode are respectively made of gold, copper and aluminum, and the thicknesses of the connecting layer, the metal layer and the protective layer are respectively 8nm, 400nm and 10nm;
comparative group 4: the electrode is prepared by the same method as the embodiment 6, and the difference is that the materials of the connecting layer, the metal layer and the protective layer of the electrode are respectively silver, copper and nickel, and the thicknesses of the connecting layer, the metal layer and the protective layer are respectively 9nm, 400nm and 12nm;
comparative group 5: the electrode is prepared by the same method as the embodiment 7, and the difference is that the materials of the connecting layer, the metal layer and the protective layer of the electrode are respectively aluminum, copper and titanium, and the thicknesses are respectively 10nm, 400nm and 18nm;
table 1 firmness, resistance to harsh environments, high and low temperature, humidity and heat, etc. of film systems prepared with different film structures.
From the results in table 1, it can be seen that the high and low temperature resistance and the moist heat resistance are mainly related to the film system, and the film system and the metal thickness in the technical scheme of the present invention are different, which has an influence on the high and low temperature resistance and the moist heat resistance, and the film system structure of the experimental groups 1 to 5 includes a connection layer and a protection layer of appropriate metal material and thickness, so that the influence on the high and low temperature resistance and the moist heat resistance is small and almost negligible; and once the metal materials and the thicknesses of the connecting layer and the protective layer are changed, the high and low temperature resistance and the damp and heat resistance are obviously changed. The firmness of the film system is the same.
Example 10: transmittance test
Experimental group 1: transmittance experiments were performed in the 800-1000nm range using the K9-400 samples prepared in example 3, and the results are shown in fig. 5. From the results of FIG. 5, it can be seen that the transmittance is close to 90% in the range of 800 to 1000 nm.
Experimental group 2: transmittance experiments were performed in the 800-1000nm range using the K9-320 samples prepared in example 4, and the structure is shown in fig. 3. From the results in FIG. 3, it can be seen that the transmittance in the 800-1000nm range will be 82.16%.
Experimental group 3: transmittance experiments were performed in the range of 8-12um using ZnS-500 samples prepared in example 5, and the results are shown in fig. 4. From the results of FIG. 4, it can be seen that the average transmittance was 83.42% and the peak transmittance was 88.88% in the range of 8 to 12 um.
It can be seen from the comparison of experimental groups 1 and 2 that the same substrate material, different film layer structures, in particular the thickness of the functional layer, have an influence on the transmittance; it can be seen from the comparison between the experimental group 1 and the experimental group 3 that different base materials and different metal grid structures have different results on the transmittance of different wave bands. This demonstrates the effect of the substrate material, the film structure, in particular the functional layer, and the metal grid on the transmission.
Example 11: electromagnetic shielding experiment
Experimental group 1: the K9-400 sample prepared in example 3 was measured to have a frequency of 240MHZ to 2.5GHZ using a vector network analyzer N5225A, and the electromagnetic shielding effect is shown in FIG. 6.
Experimental group 2: the K9-320 sample prepared in example 4 was used, and the vector network analyzer N5225A was used to detect the frequency of 240MHZ-2.5GHZ, and the electromagnetic shielding effect is shown in FIG. 7.
Experimental group 3: using the ZnS-500 sample prepared in example 5, the frequency was measured at 240MHz to 2.5GHz by a vector network analyzer N5225A, and the electromagnetic shielding effect is shown in FIG. 8.
Experimental group 4: the Ge-400 sample prepared in example 6 was used, and the vector network analyzer N5225A was used to detect the frequency of 240MHZ-2.5GHz, and the electromagnetic shielding effect is shown in FIG. 9.
Experimental group 5: the Si-400 sample prepared in example 7 was used, and the vector network analyzer N5225A was used to detect the frequency of 240MHZ to 2.5GHZ, and the electromagnetic shielding effect is shown in FIG. 10.
It can be seen from the comparison of experimental groups 1 and 2 that the same substrate material and different film structures have an influence on the electromagnetic shielding, because the metal is mainly used for achieving the electromagnetic shielding effect, and the plating with different metals and thicknesses is mainly used for achieving different sheet resistances, and finally the electromagnetic shielding efficiency is reflected. The film systems are different, the metal thicknesses are different, the surface resistances of the parts are different, the surface resistances are different, and the electromagnetic shielding efficiencies are different; in addition, the grid period of the book-passing grid of the experimental group 2 is 320 mu m, the shielding efficiency in the frequency band range of 240MHz to 2.5GHz exceeds 35dB and is slightly higher than the structure corresponding to the experimental group 1, but the average transmittance of the experimental group 2 in the range of 800-1000nm is reduced to 82.16 percent compared with that of the experimental group 1.
It can be seen from the comparison between the experimental group 4 and the experimental group 5 that the experimental group 4 and the experimental group 5 are identical in metal grid structure (period is 400 ± 10 μm, line width is 12 ± 2 μm) and metal film structure (the materials of the electromagnetic shielding function film connecting layer, the metal layer and the protective layer are respectively chromium, copper and chromium, and the thicknesses are respectively 10nm, 400nm and 20 nm), and the difference is only that the base materials are respectively germanium (Ge) and silicon (Si); according to the electromagnetic shielding efficiency detection report in the frequency range of 240MHz to 2.5GHz, as can be seen from fig. 9 and fig. 10, the electromagnetic shielding efficiency of the Ge substrate in the frequency range of 240MHz to 2.5GHz exceeds 41dB, and the electromagnetic shielding efficiency of the Si substrate exceeds 31 dB. The metal mesh grid with better electromagnetic shielding effect can be prepared on the Ge and Si substrate, and different window materials can be selected according to the working requirements to prepare the metal mesh grid under different application conditions correspondingly in the background technology.
From the comparison between the experimental group 1 and the experimental group 3, it can be seen that the shielding efficiency of different wave bands is greatly affected by different substrate materials, different metal grids and different film layer structures, and the transmittance of the experimental group 3 in the range of 8-12 μm has an average transmittance of 83.42% and a peak transmittance of 88.88%.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes in the embodiments and/or modifications of the invention can be made, and equivalents and modifications of some features of the invention can be made without departing from the spirit and scope of the invention.
Claims (10)
1. A film system having selective electromagnetic shielding and high transmittance, comprising: comprises a curved optical window, an electromagnetic shielding functional film, an electrode film and an infrared anti-reflection film; the electromagnetic shielding functional film and the electrode film are made of the same film material, structure and thickness.
2. The film-layer system with selective electromagnetic shielding and high transmittance of claim 1, wherein: a grid groove is formed on the concave surface of the curved optical window; the electromagnetic shielding functional film is plated in the grid groove; the electrode film is plated on the electromagnetic shielding function film; the infrared antireflection film is coated in the whole effective caliber of the curved optical window.
3. The film layer system with selective electromagnetic shielding and high transmittance of claim 2, wherein: the period of the grid groove is 320 +/-10 mu m-500 +/-10 mu m; the line width was 12. + -.2. Mu.m.
4. The film-layer system with selective electromagnetic shielding and high transmittance of claim 2, wherein: the curved optical window adopts a K9 glass substrate, a ZnS substrate, a Si substrate or a Ge substrate.
5. The film layer system with selective electromagnetic shielding and high transmittance of claim 1, wherein: the film system material of the electromagnetic shielding function film and the electrode film comprises one or more of gold, silver, chromium, copper, aluminum, nickel, titanium and silver alloy.
6. The film layer system with selective electromagnetic shielding and high transmittance of claim 5, wherein: the film layer structure of the electromagnetic shielding functional film and the motor film comprises a connecting layer, a functional layer and a protective layer.
7. The film-layer system with selective electromagnetic shielding and high transmittance of claim 1, wherein: the infrared antireflection film includes a single-layer or double-layer film having a layer made of one or two of magnesium fluoride, silicon dioxide, and OS-50.
8. A method of making an optical window film system having frequency selective electromagnetic shielding and high efficiency transmission, comprising: the method comprises the following steps: etching the photoresist of the curved optical window by laser direct writing and developing a grid groove by a developing process; and depositing metal in the grid groove to obtain the metal grid.
9. The method for preparing an optical window film system with frequency selective electromagnetic shielding and high-efficiency transmission functions as claimed in claim 8, wherein the step of depositing metal comprises: evaporating an electromagnetic shielding functional film by adopting a physical vapor deposition mode; after removing the photoresist, evaporating an electrode film by adopting a physical vapor deposition mode; and plating an infrared antireflection film on the effective aperture of the curved optical window by adopting a physical vapor deposition mode.
10. The method for producing an optical window film system having frequency selective electromagnetic shielding and high-efficiency transmission functions according to claim 9, wherein: the evaporation temperature of the electromagnetic shielding functional film and the electrode film is evaporated by adopting a physical vapor deposition process is 60 to 120 ℃, the evaporation rate is 0.2 to 1.0nm/s, and the vacuum degree is 3.0 multiplied by 10 -3 ~9.0×10 -4 Pa, vacuum oxygen introduction amount of 8 to 12 sccm, ion energy of 425 to 445eV and electron beam current of 63 to 83mA; the evaporation temperature of the evaporation infrared antireflection film by adopting a physical vapor deposition process is 160 to 240 ℃: the evaporation rate is 0.2 to 0.9nm/s, and the vacuum degree is 3.0 multiplied by 10 -3 ~9.0×10 -4 Pa, the vacuum oxygen introduction amount of the OS-50 is 8 to 15 sccm, the vacuum oxygen introduction amount of the silicon dioxide is 0 sccm, the electron beam current of the OS-50 is 280 to 340mA, and the electron beam current of the silicon dioxide is 80 to 120mA.
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| CN116241808B (en) * | 2023-05-12 | 2023-08-15 | 有研国晶辉新材料有限公司 | Preparation method of electromagnetic shielding curved surface optical window, curved surface light source and equipment |
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