CN114713840A - Manufacturing method for manufacturing broadband electromagnetic shielding curved surface optical window based on composite micro-nano additive manufacturing - Google Patents
Manufacturing method for manufacturing broadband electromagnetic shielding curved surface optical window based on composite micro-nano additive manufacturing Download PDFInfo
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- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/10—Formation of a green body
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
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- B22F10/60—Treatment of workpieces or articles after build-up
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D1/00—Electroforming
- C25D1/003—3D structures, e.g. superposed patterned layers
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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- General Chemical & Material Sciences (AREA)
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- Thermal Sciences (AREA)
- Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
Abstract
The invention discloses a manufacturing method of a broadband electromagnetic shielding curved surface optical window based on composite micro-nano additive manufacturing, which comprises the steps of preprocessing a base material; the method comprises the following steps of driving a spray deposition curved surface conformal micro-nano 3D printer to conformally print a metal mesh grid microstructure by using a five-axis linkage electric field based on an extraction electrode; conducting treatment on the metal mesh microstructure; forming a magnetic conduction layer structure by electrochemical deposition additive forming, and depositing a layer of magnetic conduction material on the surface of the conductive grid structure and wrapping the magnetic conduction material to form a conductive/magnetic conduction composite material; and (5) sample post-processing. According to the invention, the large-size broadband electromagnetic shielding curved surface or the 3D conformal optical window is manufactured efficiently and at low cost by the composite micro-nano additive manufacturing technology.
Description
Technical Field
The invention belongs to the field of electromagnetic shielding of optical transparent parts, and particularly relates to a method for efficiently manufacturing a large-size broadband electromagnetic shielding curved surface or a 3D conformal optical window with low cost by adopting a composite micro-nano additive manufacturing technology.
Background
In recent years, the electromagnetic shielding technology has a wide application foundation in civil and military fields, such as satellite/mobile communication navigation, broadcasting/television/radar, medical diagnosis, and ship/automobile/optical instrument windows, especially in the application of national defense military equipment, and has become one of the national defense high-tech technologies which are mainly developed in various countries in the world, such as the application in fifth generation fighters, missiles, aircrafts, ships, tanks and rocket bullets: infrared/visible light transmitting optical windows, optical fairings, radar antennas and radomes, cruise missile guidance hoods, electromagnetic warfare and the like.
However, the curved surface and 3D conformal optical window of military equipment is different from the traditional spherical surface or plane window, and the window has to meet the requirement of specific outline, is more beneficial to the stealth and maneuvering performance of military equipment, can also avoid the problems of electromagnetic leakage and the like caused by a flat plate splicing window, and has extremely important function in the fields of optical transparencies of cockpits of fifth generation of aircraft, intercontinental missiles, optical windows of spacecrafts and the like. Particularly, with military stealth technology and current electromagnetic warfare, the importance of a new generation of light broadband wave-absorbing material is gradually shown, for example, the current infrared precise guided weapon not only needs to have high-efficiency infrared transmittance, but also needs to have better electromagnetic shielding efficiency, is compatible with electromagnetic shielding infrared window films, has good transmittance in a specific infrared band, and can shield electromagnetic wave signals in a certain frequency band; in addition, for example, the stealth problem of radar antennas, antenna covers and cruise missile guide head covers cannot simply use the appearance technology or wave-absorbing material technology, the working requirements of the antennas and the antenna covers must be ensured, and the cruise missile guide head covers must meet the efficient transmission of infrared rays for imaging guidance. More importantly, with the use of a large amount of electromagnetic equipment, the electromagnetic environment is increasingly complex, and the current electromagnetic shielding equipment is mainly focused on the electric field shielding direction, and only has higher shielding performance for the middle and high frequency electric fields, but has very low shielding efficiency for the low frequency magnetic field, and is difficult to meet the requirement of higher shielding efficiency, and when the low frequency magnetic field shielding and the high frequency electric field shielding are considered, the shielding material is urgently expected to realize the electromagnetic shielding capability of wider frequency band and high broadband shielding efficiency, so that higher and higher requirements are provided for the curved conformal optical window in various fields such as military, aerospace and the like: strong electromagnetic shielding efficiency, high light transmission characteristic and broadband strong electromagnetic shielding effectiveness.
The types of electromagnetic shielding materials are currently roughly classified into two types: one is a thin film type material; one is a mesh grid type material. Wherein the film type mainly comprises an oxide film (TCO), a metal film, a conductive high polymer film and a composite film; the grid type material is mainly a continuous regular or irregular metal grid pattern made of metals such as gold, silver, copper, nickel, iron and the like. Indium Tin Oxide (ITO) film, which is also an oxide film, is most widely used among many electromagnetic shielding materials, however, it is only used in the place where visible light is transmitted, and the low-frequency electromagnetic shielding effect is very weak; the metal thin film materials (gold, silver, copper and the like) have lower sheet resistance and higher magnetic conductivity, and can perform electromagnetic shielding on high magnetic fields, but the metal thin film (within 20 nm) made of the materials is difficult to meet the requirement of high light transmission, so the application capability of the metal thin film materials is further limited; the conductive polymer film generally has good conductivity, but has poor thermal stability, and is not well applied in practical application. Compared with other existing processes, the shielding effect of the superstructure stealth material with ultralow resistance and high transmittance represented by a metal mesh grid and the like on radar waves is adopted, the infrared rays with accurate guidance are not influenced to efficiently penetrate, the electromagnetic anti-interference capability of new-generation weapon equipment is greatly improved, and the stealth capability of the weapon equipment is better realized.
However, at present, there is no single material capable of achieving the broadband electromagnetic shielding performance of the electromagnetic shielding device, and the broadband electromagnetic shielding effect is mainly achieved by compounding multiple materials, for example, patent 201811196275.1, "a preparation method of a broadband electromagnetic shielding composite material" provides a preparation method of a composite material for broadband electromagnetic shielding, although the shielding effectiveness of the composite material is equal to or more than 35dB within 30MHz-1.5GHz, the composite material cannot meet the use requirement of an optical window with light transmission performance. The electromagnetic shielding technology for the curved optical window mainly focuses on the following four aspects: the filter is a frequency selective surface technology, an electric control sensitive material technology, a transparent conductive film technology and a filtering technology based on a metal mesh grid. As the frequency selective surface technology relates to part of national defense technology in aerospace, reports related to the technology at home and abroad on a curved optical shielding window are relatively few, and as for the electric control sensitive material technology, although an optical window on any surface type can be manufactured, the process method has the defects of low transmission energy and narrow wave band, and in the actual use process in severe environment, the electromagnetic sensitive material cannot simultaneously meet the targets of electromagnetic shielding and optical transmission. The electromagnetic shielding materials commonly used in various transparent conductive film technologies at present mainly comprise steel oxide, oxidation, tin oxide and tin-infiltrated steel oxide, and the related processing technological processes mainly comprise chemical vapor deposition, blade coating, spin coating, spray coating, electroplating, magnetron sputtering and the like, for example, patent 202110061140.X "an electromagnetic shielding curved optical window based on an ultrathin doped metal/medium composite structure", the patent adopts deposition modes such as electron beam evaporation coating, thermal evaporation coating or direct current, magnetron sputtering coating and the like to sequentially deposit a medium film and an ultrathin metal film on the surface of a curved substrate according to a design sequence, and the whole coating process is complex in operation and complicated in process. Since the transparent conductive film easily absorbs infrared light, it is not suitable for use in infrared target recognition. The electromagnetic shielding preparation based on the metal mesh mainly adopts the photoetching technology, wherein the photoetching technology is divided into the mask photoetching technology (contact photoetching technology, proximity photoetching technology and projection photoetching technology) and the maskless photoetching technology (electron beam direct writing technology, laser direct writing technology and near field direct writing technology), and the data show that the research institution of the firstly disclosed curved surface laser direct writing system is the research institute of the German Fragile optical technology, and then the national Changchun optical engine institute of the Chinese academy and the university of Zhejiang develop the photoetching direct writing system which also has the function of processing the graph on the curved surface, although the photoetching technology is a better scheme for processing the graph on the curved surface with small curvature, the technology has rigorous requirements on the processing technology environment, the material cost is high, the equipment cost is expensive and the like, only a few micro-electronics industry macros can use the electromagnetic shielding conformal optical window with the longitude and latitude mesh structure, for example, the patent 201010239355.8 provides a conformal optical window suitable for the conformal optical window The method for manufacturing the electromagnetic shielding structure of the longitude and latitude-shaped metal mesh grid is difficult in processing process because the method depends on special processing equipment when manufacturing the electromagnetic shielding structure of the longitude and latitude-shaped metal mesh grid. In addition, screen printing, ink jet printing and other mixed printing modes, including micro-contact printing, indirect transfer printing methods and some novel mixed printing modes, are gradually new choices for processing large-size metal grids, however, most of the processing of curved surface microstructure patterns still depends on special processing equipment and has the defects and defects of high processing cost, complex process, small processing size, unsuitability for non-developed curved surfaces, low precision, low efficiency and the like. Therefore, the prior arts are difficult to realize low-frequency electromagnetic shielding, especially, the high-efficiency and low-cost system of the wide-band electromagnetic shielding curved conformal optical window (the prior arts are difficult to solve the following problems, such as high precision manufacture of curved surfaces and 3D conformal micro-nano patterns, low-frequency magnetic conductive material, large processing size, low manufacturing cost, high efficiency, etc.)
In summary, the current electromagnetic shielding curved optical window related to the broadband mainly faces the following problems: aiming at special application occasions (shielding performance of more than 40 dB), the electromagnetic radiation power is enhanced, and the high-performance electromagnetic shielding performance of a broadband can not be realized by a single metal layer structure or a conductive metal film; secondly, the processing of the curved surface microstructure is difficult to realize, and the curved surface microstructure mostly depends on special processing equipment, so that the problems of high processing cost, complex and complicated process, strict environmental requirements, low efficiency and the like exist; thirdly, the application requirements of high light transmittance and high shielding efficiency cannot be simultaneously met. Therefore, the processing of the curved optical window with the broadband electromagnetic shielding function needs to break through a series of bottlenecks of a traditional processing mode, complex equipment, high environmental requirement, low processing efficiency and the like, and the wide-band electromagnetic shielding curved optical window is simple, efficient, good in adaptability, large in size, complex curved surface and non-flat surface and low in cost. The various existing processing techniques cannot meet these requirements.
Disclosure of Invention
In order to solve the problems and the defects, the electromagnetic shielding structure and the material in the prior art are particularly limited in broadband and high-performance (high light transmittance, strong electromagnetic shielding effectiveness, good weather-resistant performance and the like) electromagnetic shielding of a curved optical window. The invention discloses a micro-nano composite additive manufacturing method for a broadband electromagnetic shielding curved optical window based on a composite metal mesh, which combines the five-axis linkage electric field based on an extraction electrode to drive the jet deposition micro-nano 3D printing high-precision curved conformal printing and the precision micro-electroforming high-efficiency body forming, completely utilizes a micro-nano additive manufacturing technology to prepare a composite metal mesh (silver-nickel) structure with a curved surface and a 3D conformal structure, and realizes the efficient and low-cost manufacturing of a large-size broadband high-performance (high light transmittance and strong electromagnetic shielding efficiency) electromagnetic shielding curved optical window.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a manufacturing method for manufacturing a broadband electromagnetic shielding curved surface optical window based on composite micro-nano additive manufacturing mainly comprises the following steps:
step 1: pretreating a base material: carrying out surface hydrophobic treatment on the curved surface base material;
step 2: conformal printing of metal mesh microstructure: the method comprises the steps that a five-axis linkage electric field based on an extraction electrode is used for driving a spray deposition curved surface conformal micro-nano 3D printer, metal mesh grid microstructures are printed on a curved surface substrate according to designed and optimized mesh grid types (squares, diamonds, triangles, hexagons and the like), sizes (line widths, periods and the like) and geometric arrangement and other parameters in combination with optimized 3D printing process parameters, and manufacturing of the metal mesh grid microstructures with different printing line widths, periods and height-width ratios is achieved by adjusting the printing process parameters; the printing material of the conductive metal mesh structure comprises but is not limited to conductive silver paste, conductive copper paste and conductive polymer, the line width of the conductive metal mesh structure is 0.5-50 mu m, the period is 20-500 mu m, and the height is 2-20 mu m;
and step 3: conducting treatment of metal mesh microstructure: placing the metal mesh grid microstructure printed in the step 2 in a vacuum box for sintering to carry out conductive treatment, and then cleaning and drying with nitrogen to completely remove dirt on the metal mesh grid and the substrate;
and 4, step 4: electrochemical deposition additive forming of a magnetic conduction layer structure: depositing a layer of magnetic conductive material on the surface of the metal mesh grid structure subjected to the electric conduction treatment obtained in the step 3 through an electroforming or chemical plating process to form a composite metal mesh grid structure of a high electric conduction layer and a high magnetic conduction layer; the thickness of the electrochemical deposition magnetic conduction layer is 3-30 microns.
And 5: sample post-treatment: and carrying out ultrasonic treatment on the optical window sample piece obtained after electroforming or chemical plating to remove surface residues, and carrying out drying or nitrogen blow-drying treatment to finish the manufacture of the large-size broadband curved optical window.
Further, the substrate pretreatment in the step 1 refers to surface hydrophobic treatment of the curved substrate, so that the surface energy of the curved substrate is reduced, and the printing precision and stability are improved.
Further, the material used for printing the metal mesh microstructure in the step 2 is low-temperature cured nano silver paste with high solid content (65-80 wt%), high-temperature cured nano silver paste, nano copper paste, conductive polymer, or other conductive paste.
Furthermore, the printing nozzle used in the step 2 is other conductive nozzles such as a gold-sprayed glass nozzle with an inner diameter of 1-100 μm, a coaxial glass-stainless steel nozzle, a ceramic nozzle and the like.
Furthermore, the printing of the metal mesh grid microstructure in the step 2 adopts an electric field driven spray deposition curved surface conformal micro-nano 3D printing technology based on an extraction electrode, a corresponding processing code printing path can be generated according to actual requirements, different printing process parameters are preferably selected, and the curved surface conformal or 3D conformal high-precision printing of metal mesh grids with different line widths (1-15 μm), different periods (50-1000 μm) and different aspect ratios is completed.
Further, the printing process parameter range in the step 2 is as follows: the applied voltage is 300-2000V, the air pressure is 30-200kPa, and the printing speed is 1-100 mm/s.
Further, in the step 3, the conductive treatment process of the metal mesh grid microstructure is to place the metal mesh grid microstructure in a vacuum drying oven at 100-600 ℃ for curing and sintering for 10-40min according to the optimal curing process condition of the used conductive silver paste, so as to ensure that the metal mesh grid structure has excellent conductive performance and adhesion performance.
Further, in the step 4, in the electroforming process of the magnetic conduction layer, reagent materials required by the electroforming solution are firstly weighed according to a certain proportion, then are fully dissolved in sequence to finally obtain the required electroforming solution, and the pH value of the solution is adjusted to be within a range of 3-4.5.
Further, in the chemical plating process of the magnetic conduction layer in the step 4, firstly, reagent materials required by the chemical plating solution are weighed according to a certain proportion, then, the reagent materials are fully dissolved in sequence, the required chemical plating solution is finally obtained, and the pH value of the solution is adjusted to be within the range of 3-4.5.
Further, in the step 4, the magnetic conductive layer structure is manufactured by attaching a conductive copper tape to one side of the conductive metal mesh grid structure to be connected to a cathode of the precision micro-electroforming equipment, connecting a metal plate to an anode, placing the metal plate in electroforming solution, and starting the electroforming equipment to manufacture the magnetic conductive layer structure.
Further, in the step 4, the conductive layer structure is manufactured by placing the conductive metal mesh grid structure in a chemical plating solution for chemical plating.
Furthermore, in the electroforming process in the step 4, the surface roughness can be reduced by adopting a smaller current density, and the current density is 0.5-3A/m2。
Further, in the electroforming process in the step 4, a constant temperature monitoring system and a solution circulating system are adopted to control the temperature of the electroforming solution in real time, so that the temperature of the electroforming solution is always within 45-55 ℃, and the solution circulating speed in the solution circulating system is 1-2 m/s.
Furthermore, in the electroforming process in the step 4, an ultrasonic vibrator is additionally arranged in the electroforming solution, so that bubbles on the surface of the electrode are quickly discharged, and the effects of reducing concentration polarization and improving the flow field characteristics are achieved.
Further, the drying temperature range in the sample post-treatment in the step 5 is 50-100 ℃.
Further, the curved optical window is not limited to a curved surface, a spherical surface, a hemispherical surface, a cylindrical surface, a 3D conformal surface, etc.
Further, the magnetic conduction layer structure material is not limited to one or a mixture of two or more of iron, nickel, chromium and copper.
Compared with the prior art, the invention has the beneficial effects that:
(1) the five-axis linkage electric field based on the extraction electrode is used for driving the jet deposition curved surface conformal micro-nano 3D printer to print the curved surface metal mesh grid in a high-precision conformal manner, so that large-size, high-precision, high-efficiency and low-cost manufacturing is realized, especially the extraction electrode breaks through the limitation of the traditional electro-jet printing height, the influence of jet flow dispersion on the printing precision is reduced, and the printing stability and precision are improved;
(2) according to the invention, the five-axis linkage electric field driven jet deposition curved surface conformal micro-nano 3D printing and the micro-electroforming (chemical plating) process are combined, so that the high-efficiency and low-cost manufacturing of the composite multilayer electromagnetic shielding structure of the high conducting layer and the high magnetic conducting layer is realized, the problems of difficult curved surface multilayer printing, long production period and poor consistency are solved, the high-efficiency manufacturing of the composite metal mesh grid is realized, and the special advantage of wide-band strong electromagnetic shielding effectiveness is achieved;
(3) compared with the traditional single shielding structure, the multilayer composite shielding structure of the high conducting layer and the high magnetic conducting layer breaks through the limit of the electromagnetic shielding capability of a single-layer structure, so that the shielding structure has better shielding efficiency in full frequency bands (low frequency, high frequency and ultrahigh frequency), provides guarantee for the manufacture of a high-performance electromagnetic shielding optical window (device), and has the advantages of strong expansibility and wide adaptability;
(4) the processing scheme for manufacturing the superconducting large-size curved optical window based on the micro-nano additive has the advantages of simple process, short production flow, high efficiency, low cost, environmental friendliness and good flexibility;
(5) the technology completely adopts a micro-nano additive manufacturing process, and has the advantages of high material utilization rate almost reaching 100 percent, (the material waste rate of the existing material reduction processes such as photoetching, laser and the like is high, 90 percent of materials are wasted), no pollution and environmental protection;
(6) the curved surface metal mesh grid printed by the five-axis linkage electric field driven jet deposition curved surface conformal micro-nano 3D printing technology based on the extraction electrode is simple and flexible in structure, does not relate to pattern generation and transfer of a traditional micro-processing method, and has the remarkable advantages of simplicity, low cost and high efficiency.
(7) The defect self-repairing capacity, high stability and consistency are realized; the defects of breakage, unevenness and the like exist in the directly printed conductive grid, so that the conductivity and the stability and consistency of the product are seriously influenced; according to the invention, through a precise micro-electroforming technology, the surface fracture and defect of the printing grid can be repaired, a continuous and compact conductive network is formed, and the stability and consistency of the product performance can be ensured by controlling electroplating parameters; the problem of the biggest super large-size electromagnetic shielding glass is solved.
(8) The composite structure metal grid has the advantages of good weather resistance, corrosion resistance and high stability, has good bonding property with a glass substrate, has good service life, has excellent weather resistance and corrosion resistance, and can be used in harsh natural environment.
(9) The invention provides a novel composite micro-nano additive manufacturing process, which is low in cost and flexible in manufacturing, and the manufacturing of the ultra-large-size high-performance metal mesh transparent electromagnetic shielding glass is completely realized through an additive manufacturing technology; the additive manufacturing technology has the remarkable advantages of metal saving, strong adaptability and customization; the ordered grid structure with various shapes (squares, diamonds and the like), periods and line widths can be flexibly printed according to the requirement with high precision, and various application requirements are met.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description, serve to explain the invention and not to limit the invention.
FIG. 1 is a schematic view of a broadband strong electromagnetic shielding curved optical window according to some embodiments of the present invention.
FIG. 2 is a process flow chart of the manufacturing method of the broadband strong electromagnetic shielding curved optical window according to the embodiment of the present invention.
FIG. 3 is a schematic diagram of a principle of conformal micro-nano 3D printing of a spray deposition curved surface based on five-axis linkage electric field driving of an extraction electrode.
Fig. 4 is a schematic view of a "high conductive-magnetic conductive" layer composite electromagnetic shielding structure finally obtained by using an electroplating or electroless plating principle.
In the figure, 301 is an air inlet duct, 302 is an air inlet duct adapter, 303 is a storage tank, 304 is an extraction electrode structure, and 305 is a printing and printing nozzle.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms "a", "an", and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
The present invention will be further described with reference to the following examples.
Example 1
In the embodiment, nanometer conductive silver paste is used as a printing material, and a metal mesh grid microstructure is printed on a curved surface substrate by utilizing a five-axis linkage electric field driving spray deposition curved surface conformal micro-nano 3D printing technology based on an extraction electrode; then carrying out low-temperature sintering conductive treatment on the printed metal mesh microstructure; and then, carrying out micro-electroforming processing on the metal grid microstructure electrode subjected to electric conduction treatment, depositing a layer of metal nickel magnetic conduction material on the surface of the metal grid structure (single-step body forming), forming a high-conducting layer and high-magnetic-conduction layer composite electromagnetic shielding structure (nickel/silver composite metal grid structure), and finally carrying out post-treatment on the sample to obtain the curved optical window with the broadband strong electromagnetic shielding function.
The method for manufacturing the broadband electromagnetic shielding curved optical window based on the composite micro-nano additive manufacturing comprises the following specific steps:
step 1: pretreating substrates
And the surface hydrophobic treatment is carried out on the selected cylindrical surface curved surface base material, so that the surface energy of the base material is reduced, and the printing precision and consistency are improved.
Step 2: conformal printing metal mesh microstructure
Placing the pretreated cylindrical surface curved surface substrate on a printing platform, and printing a metal mesh microstructure on the cylindrical surface substrate by utilizing a five-axis linkage electric field driven spray deposition curved surface conformal micro-nano 3D printing technology based on an extraction electrode, wherein the printing line width is 10 micrometers, the period is 200 micrometers, and the height-to-width ratio is 0.5: 1. Printing process parameters: the applied voltage is 1000V, the printing speed is 10mm/s, the applied air pressure is 180kPa, the printing height is 100 μm, and the printing nozzle is a glass-stainless steel coaxial nozzle with the inner diameter of 20 μm.
And step 3: low-temperature sintering conductive treatment for printing metal mesh
And (3) placing the metal mesh structure printed in the step (2) in a vacuum drying oven for conducting sintering, wherein the specific curing process comprises the following steps: and (4) solidifying and sintering for 45min at 145 ℃. The purpose is to improve the conductive capability of the metal mesh grid structure and enhance the adhesive force of the metal mesh grid structure and the curved surface base material.
And 4, step 4: electroforming magnetic conduction layer structure (metallic nickel)
And (3) carrying out nickel electroforming on the metal mesh grid structure with high conductivity obtained in the step (3), and firstly weighing the components of an electroplating solution in sequence according to the proportion: 100g/L of nickel sulfamate, 10g/L of nickel chloride, 30g/L of boric acid and 0.1g/L of sodium dodecyl sulfate, adjusting the pH value of the electroforming solution to be 4, setting the temperature of the solution to be 50 ℃, and setting the current density to be 1A/dm2And electroforming for 3min, wherein the circulating flow rate of the solution is 1.5m/s, then attaching a conductive copper adhesive tape on one side of the conductive metal grid structure to be connected to a cathode of precise micro-electroforming equipment, connecting a metal nickel plate with an anode, placing the metal nickel plate in electroforming solution, starting the electroforming equipment to manufacture a magnetic conduction layer structure, and finally obtaining a final composite structure (a metal nickel/silver composite metal grid microstructure) of the high conductive layer and the high magnetic conduction layer.
And 5: post-treatment of the shaped sample
And (3) placing the electroformed sample piece into ultrasonic equipment for cleaning and ultrasonic treatment, setting the ultrasonic power to be 400W, removing surface residues, and drying at the drying temperature of 85 ℃ to finally obtain the curved optical window with the broadband electromagnetic shielding function.
Example 2
In the embodiment, nanometer conductive silver paste (NT-ST20E) is used as a printing material, and a metal mesh grid structure electrode structure is printed on a spherical substrate by utilizing a five-axis linkage electric field driven jet deposition curved surface conformal micro-nano 3D printing technology based on an extraction electrode; then conducting treatment is carried out on the printed metal mesh grid structure electrode; and finally, cleaning and post-processing the electroformed sample piece to obtain the curved surface optical device with the broadband electromagnetic shielding function.
The manufacturing method of the broadband electromagnetic shielding spherical optical window based on the composite micro-nano additive manufacturing comprises the following specific process steps:
step 1: pretreating substrates
The selected spherical curved surface substrate is cleaned and subjected to surface hydrophobic treatment, so that the surface energy of the substrate is reduced, and the printing precision and consistency are improved.
Step 2: conformal printing metal mesh microstructure
And (3) placing the processed spherical substrate on a printing platform, and printing a metal mesh grid electrode structure on the spherical substrate by utilizing a curved surface conformal micro-nano 3D printing technology, wherein the line width is 8 micrometers, the period is 300 micrometers, and the height-to-width ratio is 0.3: 1. Printing process parameters: the applied driving voltage is 1000V, the printing speed is 5mm/s, the applied air pressure is 200kPa, the printing height is 100 μm, and the printing nozzle is a stainless steel dispensing nozzle with an inner diameter of 15 μm.
And step 3: low-temperature sintering conductive treatment for printing metal mesh
And (3) placing the metal mesh structure printed in the step (2) in a vacuum drying oven for conducting sintering, wherein the specific curing process comprises the following steps: and (3) curing and sintering for 30min at 150 ℃.
And 4, step 4: electroforming magnetic conduction layer structure (metallic nickel)
Electroforming the metal mesh grid structure with high conductivity obtained in the step 3, firstly weighing the components of the electroplating solution in sequence according to the proportion: 180g/L of nickel sulfate, 60g/L of ferrous sulfate, 15g/L of sodium chloride, 30g/L of boric acid, 2g/L of saccharin, 1g/L of antioxidant and 0.15g/L of sodium dodecyl sulfate, adjusting the pH value of the electroforming solution to be 3.5, and setting the solutionThe temperature of the solution was 50 ℃ and the current density used was 0.8A/dm2And electroforming for 3min, wherein the solution circulation flow rate is 1.5m/s, then attaching a conductive copper adhesive tape on one side of the conductive metal mesh grid structure to be connected to a cathode of precise micro-electroforming equipment, connecting a metal nickel plate with an anode, placing the metal nickel plate in electroforming solution, starting the electroforming equipment to manufacture a magnetic conduction layer structure, and finally obtaining a final composite structure of the high conductive layer and the high magnetic conduction layer.
And 5: post-treatment of the shaped sample
And (3) placing the electroformed sample piece into ultrasonic equipment for cleaning and ultrasonic treatment, setting the ultrasonic power to be 400W, removing surface residues, and drying at the drying temperature of 90 ℃ to finally obtain the curved optical window with the broadband electromagnetic shielding function.
Example 3
In the embodiment, nanometer conductive silver paste (NT-ST20E) is used as a printing material, and a metal mesh grid electrode structure is printed on a spherical substrate by utilizing a five-axis linkage electric field driving spray deposition curved surface conformal micro-nano 3D printing technology based on an extraction electrode; then conducting treatment is carried out on the printed metal mesh grid structure electrode; and finally, cleaning and post-processing a sample piece after chemical plating to obtain the curved surface optical device with the broadband electromagnetic shielding function.
The manufacturing method of the broadband electromagnetic shielding spherical optical window based on the composite micro-nano additive manufacturing comprises the following specific process steps:
step 1: pretreating substrates
The selected spherical curved surface substrate is cleaned and subjected to surface hydrophobic treatment, so that the surface energy of the substrate is reduced, and the printing precision and consistency are improved.
Step 2: conformal printing metal mesh microstructure
And (3) placing the processed spherical substrate on a printing platform, and printing a metal mesh grid electrode structure on the spherical substrate by utilizing a curved surface conformal micro-nano 3D printing technology, wherein the line width is 10 micrometers, the period is 350 micrometers, and the height-to-width ratio is 0.2: 1. Printing process parameters: the applied driving voltage is 1000V, the printing speed is 5mm/s, the applied air pressure is 200kPa, the printing height is 100 μm, and the printing nozzle is a stainless steel dispensing nozzle with an inner diameter of 15 μm.
And step 3: low-temperature sintering conductive treatment for printing metal mesh
And (3) placing the metal mesh structure printed in the step (2) in a vacuum drying oven for conducting, curing and sintering, wherein the specific curing process is as follows: and (3) curing and sintering for 30min at 150 ℃.
And 4, step 4: electroforming magnetic conduction layer structure (metallic nickel)
And (4) carrying out chemical plating treatment on the metal mesh structure with high conductivity obtained in the step (3), firstly weighing the components of a chemical plating solution in sequence according to the proportion: nickel sulfate: 40g/L, sodium hypophosphite: 35g/L, ammonium hydroxide: 25ml/L, brightener ND-1: 25ml/L, complexing agent-ND-2: 25 ml/L. Adjusting the pH value of the plating solution to 8.5, setting the solution temperature to 40 ℃, placing the conductive metal mesh grid structure in the chemical plating solution, starting stirring equipment to manufacture the magnetic conduction layer structure, and finally obtaining the final composite structure of the high conductive layer and the high magnetic conduction layer.
And 5: post-treatment of the shaped sample
And cleaning the sample piece subjected to chemical plating to remove surface residues, and drying at 90 ℃ to finally obtain the curved optical window with the broadband electromagnetic shielding function.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A manufacturing method for manufacturing a broadband electromagnetic shielding curved surface optical window based on composite micro-nano additive manufacturing comprises the following steps:
step 1: pretreating a base material: carrying out surface hydrophobic treatment on the curved surface base material;
step 2: conformal printing of metal mesh microstructures: the method comprises the steps that a five-axis linkage electric field based on an extraction electrode is used for driving a spray deposition curved surface conformal micro-nano 3D printer, a metal mesh grid microstructure is printed on a curved surface substrate, and manufacturing of the metal mesh grid microstructure with different printing line widths, periods and height-to-width ratios is achieved by adjusting printing process parameters; the conductive metal grid structure is made of materials including but not limited to conductive silver paste, conductive copper paste and conductive polymer, the type of the metal grid includes but not limited to square, diamond, triangle and hexagon, the line width of the metal grid structure is 0.5-50 μm, the period is 20-500 μm, and the height is 2-20 μm;
and step 3: and (3) conducting treatment of the metal mesh microstructure: placing the metal mesh microstructure printed in the step 2 in a vacuum box for sintering to carry out conductive treatment, and then cleaning and drying with nitrogen to completely remove dirt on the metal mesh microstructure;
and 4, step 4: electrochemical deposition additive forming of the magnetic conduction layer structure: depositing a layer of magnetic conductive material on the surface of the metal mesh grid microstructure subjected to the electric conduction treatment obtained in the step 3 through an electroforming or chemical plating process to form a composite metal mesh grid structure of a conducting layer and a magnetic conductive layer; the thickness of the magnetic conduction layer is 3-30 μm.
And 5: sample post-treatment: and carrying out ultrasonic treatment on the composite metal mesh grid structure obtained after electroforming or chemical plating to remove surface residues, and carrying out drying or nitrogen blow-drying treatment to finish the manufacture of the broadband electromagnetic shielding curved surface optical window.
2. The method of claim 1, wherein: the printing nozzle used in the step 2 is a gold-sprayed glass nozzle with the inner diameter of 1-100 mu m, a coaxial glass-stainless steel nozzle or a ceramic nozzle.
3. The method of claim 1, wherein: the printing of the metal mesh grid microstructure in the step 2 adopts an electric field driven spray deposition curved surface conformal micro-nano 3D printing technology based on an extraction electrode, generates a corresponding processing code printing path according to actual requirements, and completes the curved surface conformal or 3D conformal high-precision printing of the metal mesh grid according to different printing process parameters; further preferably, the printing process parameter range in step 2 is: the applied voltage is 300-2000V, the air pressure is 30-200kPa, and the printing speed is 1-100 mm/s.
4. The method of claim 1, wherein: the conductive treatment process of the metal mesh grid microstructure in the step 3 is to place the metal mesh grid microstructure in a vacuum drying box for curing and sintering for 10-40min at the temperature of 100 ℃ and 600 ℃ according to the optimal curing process condition of the used conductive silver paste, so that the metal mesh grid structure is ensured to have excellent conductive performance and adhesion performance.
5. The method of claim 1, wherein: in the step 4, reagent materials required by the electroforming solution are weighed according to a certain proportion, and are fully dissolved in sequence to finally obtain the required electroforming solution, and the pH value of the solution is adjusted to be within the range of 3-4.5.
6. The method of claim 1, wherein: in the step 4, the chemical plating process of the magnetic conduction layer comprises the steps of firstly weighing reagent materials required by the chemical plating solution according to a certain proportion, then fully dissolving the reagent materials in sequence to finally obtain the required chemical plating solution, and adjusting the pH value of the solution to be within the range of 3-4.5.
7. The method of claim 5, wherein: and 4, manufacturing the magnetic conduction layer structure in the step 4, attaching a conductive copper adhesive tape on one side of the conductive metal mesh grid microstructure to be connected to the cathode of the precise micro-electroforming equipment, connecting the metal plate with the anode, placing the metal plate in electroforming liquid, and starting the electroforming equipment to manufacture the magnetic conduction layer structure.
8. The method of claim 6, wherein: and 4, manufacturing the magnetic conduction layer structure in the step 4, and placing the conductive metal mesh grid structure in a chemical plating solution for chemical plating treatment.
9. The method of claim 7, wherein: in the electroforming process in the step 4, the surface roughness is favorably reduced by adopting smaller current density, and the current density is 0.5-3A/m2(ii) a Preferably, in the electroforming process in the step 4, the temperature of the electroforming solution is controlled in real time by adopting a constant temperature monitoring system and a solution circulating system, so that the temperature of the electroforming solution is always within 45-55 ℃, and the solution circulating speed in the solution circulating system is 1-2 m/s; more preferably, in the step 4, in the electroforming process, an ultrasonic vibrator is added in the electroforming solution, so that bubbles on the surface of the electrode are quickly discharged, and the effects of reducing concentration polarization and improving flow field characteristics are achieved.
10. The method of claim 1, wherein: the drying temperature range in the sample post-treatment in the step 5 is 50-100 ℃; preferably, the curved optical window comprises a curved surface, a spherical surface, a hemispherical surface, a cylindrical surface, and a 3D conformal surface; further, the magnetic conduction layer structure material comprises at least one of iron, nickel, chromium and copper.
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