CN108441843B - Laser direct-writing preformed photocatalytic plating preparation method for metal patterns on surface of material - Google Patents
Laser direct-writing preformed photocatalytic plating preparation method for metal patterns on surface of material Download PDFInfo
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- CN108441843B CN108441843B CN201810205131.1A CN201810205131A CN108441843B CN 108441843 B CN108441843 B CN 108441843B CN 201810205131 A CN201810205131 A CN 201810205131A CN 108441843 B CN108441843 B CN 108441843B
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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
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1813—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by radiant energy
- C23C18/182—Radiation, e.g. UV, laser
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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
- C23C18/1601—Process or apparatus
- C23C18/1603—Process or apparatus coating on selected surface areas
- C23C18/1607—Process or apparatus coating on selected surface areas by direct patterning
- C23C18/1612—Process or apparatus coating on selected surface areas by direct patterning through irradiation means
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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
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
- C23C18/1862—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by radiant energy
- C23C18/1868—Radiation, e.g. UV, laser
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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
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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
- C23C18/38—Coating with copper
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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
- C23C18/42—Coating with noble metals
Abstract
A laser direct-writing pre-forming photocatalytic plating preparation method of metal patterns on the surface of a material belongs to the technical field of material surface treatment. The invention combines the laser direct writing technology and the photocatalysis plating technology, and prepares the high-quality metal pattern by photocatalysis plating on the basis of preforming the high-precision nano semiconductor film pattern by laser direct writing etching. The laser direct-writing pre-forming photocatalytic plating preparation method for the metal pattern on the surface of the material is green and environment-friendly, short in process, metal-saving, efficient, low in cost, universal and high in stability, and the prepared metal pattern is high in size precision, good in coating surface quality, high in bonding strength with a substrate and excellent in performance.
Description
Technical Field
The invention relates to the technical field of material surface treatment, and particularly provides a laser direct-writing preformed photocatalytic plating preparation method of metal patterns on the surface of a material.
Background
Surface metallization materials (such as printed circuit boards, surface metallization semiconductor chips, end surface metallization vacuum tubes, solar cells, metallized film capacitors, and the like) have excellent comprehensive properties of electrical conductivity, weldability, insulation, heat conduction, and the like, and are widely applied to the fields of electronic information, intelligent transportation, medical care, aerospace, energy and power, daily life, and the like. In the actual production of surface metallization materials, not only a metallization layer needs to be coated on the surface of a base material, but also the metallization layer is usually processed to prepare a metal pattern (such as a metal circuit, a gate electrode, etc.). The traditional method for preparing the metal pattern on the surface of the material mainly comprises two methods, namely a short-process preparation method for directly preparing the metal pattern on the surface of the material, and a long-process preparation method for obtaining the metal pattern by performing subsequent treatment after a metallization layer is integrally coated on the surface of the material.
The traditional short-flow preparation method of the metal pattern on the surface of the material is mainly a screen printing method. The short-flow direct preparation of the thick-film metal pattern on the surface of the material can be realized by the selective printing and high-temperature sintering of the slurry in a specific area on the surface of the material by adopting a screen printing method, the operation is simple and convenient, and the cost is low, so that the method is widely applied to the manufacture of products such as metalized ceramic substrates and the like; however, the method has high energy consumption in the production process, and the prepared metal pattern coating is easy to have defects of cracks, pores and the like and has poor surface flatness.
The traditional long-flow preparation method of the metal pattern on the surface of the material is mainly a method for integrally preparing a thin film metallization layer on the surface of the material by a magnetron sputtering method, a vacuum evaporation method, a chemical plating method or a direct metal plating method and then preparing the metal pattern by means of a photoetching technology and the like. The thin film metal pattern with excellent performances such as flatness, density and conductivity can be prepared on the surface of the material by adopting the conventional long-flow preparation process; however, in the production process of these methods, the metal plating layer outside the pattern region needs to be removed by etching, the process flow is complicated, and the waste of plating metal is serious.
The invention discloses a method for preparing a high-quality metal pattern on the surface of a ceramic circuit substrate, which is a main development direction in the future, wherein the method for preparing a high-quality metal pattern through a short-flow die-free preparation method on the surface of a new material is developed based on an autonomously developed green, environment-friendly, simple, quick and low-cost photocatalysis plating technology [ see: Liuxue peak, Xiaoqing of bear, Xianshuang, a photocatalytic chemical plating preparation method for a surface metallization composite material, Chinese patent invention patent, grant number ZL200910081920.X, grant number 2010-08-18], a photocatalytic oxidation reduction reaction is carried out on a nano semiconductor film on the surface of the material through irradiation of certain energy light, a metallization layer is prepared by reducing metal ions in the plating solution, and further, a preparation method for a refined metal pattern on the surface of the ceramic circuit substrate through controlling the shape of a light irradiation area, combining a laser direct writing technology and a photocatalysis technology [ see: Liu, a short-flow die-prepared metal pattern through a laser irradiation process, a high-energy absorption and a high-energy absorption rate of a high-intensity of a laser-light source, a high-intensity of a high-energy-luminous intensity of a rare metal pattern, a high-luminous intensity of a luminous energy-luminous material, a luminous intensity of a luminous material, a luminous intensity of a luminous.
In summary, in order to solve the above problems in the preparation of the metal pattern on the surface of the material at present, it is of great importance to develop a new method for preparing a high-precision and high-performance metal pattern on the surface of the material in a short-flow mold-free manner, which has high light energy utilization rate, good adaptability, high processing efficiency, short production flow, environmental friendliness and low cost.
Disclosure of Invention
The invention is based on the characteristics of high energy density, high processing speed, good forming flexibility, high forming precision and capability of realizing high-precision pattern forming on the surface of a material by etching, introduces the characteristics into the field of preparation of metal patterns on the surface of the material, combines the photocatalytic plating technology which is green, environment-friendly, simple, convenient and quick and is easy to realize large-scale production, realizes short-flow die-free preparation of the metal patterns by performing laser direct writing etching on nano semiconductor films on the surface of the material to form high-precision patterns and performing subsequent photocatalytic plating, and develops a novel method for stably, accurately, short-flow, efficiently, low-cost, green and flexibly preparing high-quality metal patterns on the surface of the material. The invention aims to provide a laser direct-writing pre-forming photocatalytic plating preparation method for metal patterns on the surface of a material, which can improve the precision and the performance of the metal patterns on the surface of the prepared material, shorten the process flow, improve the production efficiency, reduce the environmental pollution, reduce the metal loss of a coating, reduce the production cost and the equipment requirement, further improve the general applicability and the practicability of the process and easily realize large-scale popularization and application.
The technical scheme of the invention is as follows: inputting shape and size data of a design pattern in a control computer of a laser direct writing system, and setting corresponding parameters to determine a laser direct writing etching area and etching depth; placing the substrate material with the surface deposited with the nano semiconductor film on a working platform of a laser direct writing system, and positioning and focusing the etching area on the surface of the nano semiconductor film; removing the nano semiconductor film outside the designed pattern area on the surface of the base material by using laser etching to prepare a nano semiconductor film pattern with the shape and the size consistent with those of the designed pattern; immersing the substrate material subjected to laser direct writing etching into a cleaning agent, ultrasonically cleaning for a certain time to remove powder remaining on the surface, then transferring the substrate material into a chemical plating solution, then irradiating a catalytic light source for a certain time against the nano semiconductor film pattern, and carrying out photocatalytic oxidation reduction reaction on the surface of the nano semiconductor film pattern to reduce metal ions in the plating solution into elemental metal or alloy to be deposited on the surface of the nano semiconductor film pattern so as to generate a primary metal plating layer with the shape and the size consistent with those of the designed pattern; after the illumination is finished, the base material is continuously placed in the chemical plating solution for autocatalytic chemical plating, so that the primary metal pattern is thickened, and finally, a high-quality metal pattern with the required thickness and the shape and the size of the designed pattern is formed on the surface of the base material in a short process and high efficiency.
A laser direct-writing pre-forming photocatalytic plating preparation method of metal patterns on the surface of a material comprises the following specific processes:
1. inputting shape and size data of a design pattern into a control computer of a laser direct writing system, setting the frequency and power of a laser, a laser scanning path, scanning speed and scanning times, and determining a laser direct writing etching area and etching depth on the surface of a base material;
2. placing the substrate material with the nano semiconductor film deposited on the surface on a working platform of a laser direct writing system, enabling the surface of the nano semiconductor film to face a laser light source, and positioning and focusing an etching area;
3. starting a laser direct-writing program, performing direct-writing etching on the nano semiconductor film in the etching area, and preparing a nano semiconductor film pattern with the same shape and size as the designed pattern on the surface of the base material;
4. immersing the substrate material subjected to laser direct writing etching into a cleaning agent, and ultrasonically cleaning for 1-40 min to remove residual powder on the surface of the substrate material;
5. immersing the cleaned substrate material into a chemical plating solution to enable the nano semiconductor film pattern to face a catalytic light source with the wavelength of 200-580 nm;
6. opening a catalytic light source, illuminating for 1-15 min by using a positive photocatalysis or backlight catalysis mode, and carrying out photocatalytic oxidation reduction reaction on the surface of the nano semiconductor film pattern to reduce metal ions in the plating solution into elemental metal or alloy to be deposited on the surface of the nano semiconductor film pattern so as to generate a primary metal plating layer with the shape and the size consistent with those of the designed pattern;
7. continuously carrying out autocatalytic chemical plating in the plating solution by taking the primary metal plating layer as an activation center, wherein the reaction time is 0-120 min, so that the continuous growth of the primary metal plating layer in the plating solution is realized, and finally, a high-quality metal pattern with the required thickness, shape and size is prepared on the surface of the substrate material;
8. and taking out the base material with the surface plated with the metal pattern, and drying in the sun or blow drying after washing to finish the preparation of the metal pattern on the surface of the base material.
The laser direct writing system is a continuous laser direct writing system or a pulse laser direct writing system; the laser wavelength lambda is more than or equal to 150nm and less than or equal to 1650 nm; the scanning speed v is more than 0<8000 mm/s; the etching depth h1H is not less than 0.01 mu m1Less than or equal to 200 mu m and more than or equal to the thickness h of the nano semiconductor film2。
The base material is at least one of a metal material, an inorganic non-metal material, a high polymer material or a composite material.
The nano semiconductor film is at least one of an oxide nano semiconductor film, a non-oxide nano semiconductor film and a composite nano semiconductor film with a photocatalytic effect; thickness h of the nano semiconductor film2Is 0 < h2≤900nm。
The working platform is at least one of a rectangular coordinate type working platform, a polar coordinate type working platform and a combined type working platform.
The cleaning agent is a solvent type cleaning agent or a water-based cleaning agent; the water-based cleaning agent is an acidic cleaning agent, an alkaline cleaning agent or a neutral cleaning agent.
The chemical plating solution is chemical gold plating, silver plating, copper plating, nickel plating, tin plating, palladium plating, aluminum plating, iron plating, cobalt plating, zinc plating, chromium plating, molybdenum plating, platinum plating, tungsten plating, rare earth metal plating and alloy plating.
The catalytic light source is a linear light source or a nonlinear light source.
The metal is at least one of gold, silver, copper, nickel, tin, palladium, aluminum, iron, cobalt, zinc, chromium, molybdenum, platinum, tungsten, rare earth metals, and alloys thereof.
The main advantages of the invention are:
1. the method combines the advanced laser direct writing technology and the photocatalytic plating technology, realizes the short-process non-mold photocatalytic plating preparation of the metal pattern on the surface of the material through the accurate pre-forming of the nano semiconductor film pattern, has the advantages of high processing speed, good flexibility and high pattern precision, is green and environment-friendly, has short process flow and low production cost, and can realize the stable production of the high-quality metal pattern on the surface of the material.
2. The method reduces the strict requirements on the stability of production conditions such as laser wavelength, plating solution depth, uniformity and the like in the original laser catalysis direct-writing metal plating pattern process, reduces the production cost such as equipment cost and the like, and improves the general applicability and the practicability of the method.
3. The method solves the problems of ablation, difficult pattern precision control, poorer plating uniformity, reduced bonding strength and energy loss caused by the fact that the laser directly impacts the plating layer in the original laser catalysis direct-writing metal plating pattern process, and the plating solution or the base material needs to be penetrated, can fully play the advantages of high laser energy density and high processing precision on the surface of the material, and improves the forming precision and the energy utilization rate.
4. The method can simply, conveniently and quickly realize the direct preparation of the complex metal patterns on the surface of the plane, curved surface or three-dimensional material, does not need the early-stage template prefabrication and the later-stage photoetching, shortens the process flow, saves the plating metal, reduces the production cost and the energy consumption, can improve the product quality and the labor productivity, and is easy to realize the large-scale automatic production.
Detailed Description
The present invention is described in detail below with reference to the following examples, which are necessary to point out here only for further illustration of the present invention and should not be construed as limiting the scope of the present invention, and those skilled in the art can make some insubstantial modifications and adaptations to the present invention based on the above-mentioned disclosure.
Example 1:
inputting shape and size data of a designed circuit pattern into a control computer of a pulse laser direct writing system with the wavelength of 355nm, setting the frequency of a laser to be 75KHz and the power to be 4.375W, scanning a laser scanning path point by point from left to right at the scanning speed of 220mm/s for 1 time, wherein a laser direct writing etching area is a part outside the designed circuit pattern on the surface of the alumina substrate, and the etching depth is 20 microns; placing an alumina substrate with a 150 nm-thick nano titanium dioxide film deposited on the surface on a rectangular coordinate type working platform of a laser direct writing system, so that the surface of the nano titanium dioxide film faces a laser light source, and positioning and focusing an etching area; starting a laser direct-writing program, performing direct-writing etching on the nano titanium dioxide film in the etching area, and preparing a nano titanium dioxide film pattern with the same shape and size as the designed circuit pattern on the surface of the alumina substrate; immersing the aluminum oxide substrate subjected to laser direct writing etching into deionized water, and ultrasonically cleaning for 20min to remove residual powder on the surface of the substrate; immersing the cleaned alumina substrate into chemical copper plating solution to enable the nano titanium dioxide film pattern to face a high-pressure mercury lamp catalytic light source with the wavelength of 365 nm; opening a catalytic light source, illuminating for 6min by using a positive photocatalysis mode, and carrying out photocatalytic oxidation reduction reaction on the surface of the nano titanium dioxide film pattern to reduce copper ions in the plating solution into copper simple substances to be deposited on the surface of the nano titanium dioxide film pattern so as to generate a primary copper plating layer with the shape and the size consistent with those of the designed circuit pattern; continuously carrying out autocatalytic chemical plating in the plating solution by taking the primary copper plating layer as an activation center, wherein the reaction time is 5min, so that the continuous growth of the primary copper plating layer in the plating solution is realized, and finally, a high-quality copper circuit pattern with the required thickness and shape and size is prepared on the surface of the alumina substrate; and taking out the alumina substrate plated with the copper circuit pattern on the surface, and airing or blow-drying the alumina substrate after washing to finish the preparation of the copper circuit pattern on the surface of the alumina substrate.
Example 2:
inputting shape and size data of a designed nine-fold concentric circular ring pattern into a control computer of a pulse laser direct writing system with the wavelength of 1030nm, setting the frequency of a laser to be 50KHz and the power to be 5.7W, scanning a laser scanning path from right to left point by point, scanning speed to be 180mm/s, scanning times to be 1 time, etching areas by laser direct writing and etching to be the parts outside the designed nine-fold concentric circular ring pattern on the surface of a polyimide flexible substrate, and etching depth to be 10 mu m; placing a polyimide flexible substrate with a nitrogen-doped nano titanium dioxide film with the thickness of 100nm deposited on the surface on a polar coordinate type working platform of a laser direct writing system, enabling the surface of the nitrogen-doped nano titanium dioxide film to face a laser light source, and positioning and focusing an etching area; starting a laser direct writing program, performing direct writing etching on the nitrogen-doped nano titanium dioxide film in the etching area, and preparing a nitrogen-doped nano titanium dioxide film pattern with the same shape and size as the designed nine-layer concentric circular ring pattern on the surface of the polyimide flexible substrate; immersing the polyimide flexible substrate subjected to laser direct writing etching into deionized water, and ultrasonically cleaning for 10min to remove residual powder on the surface of the substrate; immersing the cleaned polyimide flexible substrate into a chemical nickel plating solution, and enabling the nitrogen-doped nano titanium dioxide film pattern to face a catalytic light source of a high-pressure mercury lamp with the wavelength of 355 nm; opening a catalytic light source, illuminating for 8min by using a positive photocatalysis mode, and carrying out photocatalytic oxidation reduction reaction on the surface of the nitrogen-doped nano titanium dioxide film pattern to ensure that nickel ions in the plating solution are reduced into a nickel simple substance to be deposited on the surface of the nitrogen-doped nano titanium dioxide film pattern so as to generate a primary nickel plating layer with the shape and the size consistent with those of the nine-fold concentric circular ring pattern; continuously carrying out autocatalytic chemical plating in a plating solution by taking the primary nickel plating layer as an activation center, wherein the reaction time is 3min, so that the continuous growth of the primary nickel plating layer in the plating solution is realized, and finally, preparing a high-quality nine-weight concentric ring pattern nickel plating layer with the required thickness, shape and size on the surface of the polyimide flexible substrate; and taking out the polyimide flexible substrate with the surface plated with the nine-fold concentric circular ring pattern nickel plating layer, and airing or blow-drying the polyimide flexible substrate after washing to finish the preparation of the nine-fold concentric circular ring pattern nickel plating layer on the surface of the polyimide flexible substrate.
Example 3:
inputting shape and size data of a designed dragon-shaped pattern into a control computer of a 905nm wavelength three-dimensional pulse laser direct writing system, setting the frequency of a laser to be 100KHz and the power to be 7.3W, scanning a laser scanning path from left to right and from bottom to top point by point and layer by layer, wherein the scanning speed is 1000mm/s, the scanning frequency is 1 time, a laser direct writing etching area is a part outside the designed dragon-shaped pattern on the surface of an arched aluminum substrate, and the etching depth is 200 nm; placing an arched aluminum substrate with a nano zinc oxide film with the thickness of 200nm deposited on the surface on a right-angle standard type working platform of a laser direct writing system, enabling the surface of the nano zinc oxide film to face a laser light source, and positioning and focusing an etching area; starting a laser direct writing program, performing direct writing etching on the nano zinc oxide film in the etching area, and preparing a nano zinc oxide film pattern with the same shape and size as the designed dragon-shaped pattern on the surface of the arched aluminum substrate; immersing the arched aluminum substrate subjected to laser direct writing etching into deionized water, and ultrasonically cleaning for 12min to remove residual powder on the surface of the substrate; immersing the cleaned arched aluminum substrate into a chemical nickel-phosphorus plating solution, and enabling the nano zinc oxide film pattern to face a high-pressure mercury lamp catalytic light source with the wavelength of 315 nm; opening a catalytic light source, illuminating for 5min by using a positive photocatalysis mode, and carrying out photocatalytic oxidation reduction reaction on the surface of the nano zinc oxide film pattern to reduce nickel ions in the plating solution into a nickel simple substance, and depositing the nickel simple substance and phosphorus atoms on the surface of the nano zinc oxide film pattern together to generate a primary nickel-phosphorus plating layer with the shape and the size consistent with those of the designed dragon-shaped pattern; continuously carrying out autocatalytic chemical plating in the plating solution by taking the primary nickel-phosphorus plating layer as an activation center, wherein the reaction time is 20min, so that the continuous growth of the primary nickel-phosphorus plating layer in the plating solution is realized, and finally, preparing the high-quality dragon-shaped pattern nickel-phosphorus plating layer with the required thickness and shape and size on the surface of the arched aluminum substrate; and taking out the arched aluminum substrate coated with the dragon-shaped pattern nickel-phosphorus coating on the surface, washing, and airing or blow-drying to finish the preparation of the dragon-shaped pattern nickel-phosphorus coating on the surface of the arched aluminum substrate.
Example 4:
inputting shape and size data of a designed parallel stripe pattern into a control computer of a three-dimensional pulse laser direct writing system with the wavelength of 532nm, setting the frequency of a laser to be 200KHz and the power to be 4.3W, scanning a laser scanning path from left to right and from bottom to top point by point and layer by layer, wherein the scanning speed is 500mm/s, the scanning frequency is 1 time, a laser direct writing etching area is a part outside the designed parallel stripe pattern on the surface of the cylindrical hollow quartz glass tube, and the etching depth is 50 mu m; placing a cylindrical hollow quartz glass tube with the outer surface deposited with a nano bismuth vanadate film with the thickness of 300nm on a polar coordinate type working platform of a laser direct writing system, so that the surface of the nano bismuth vanadate film faces a laser light source, and positioning and focusing an etching area; starting a laser direct-writing program, performing direct-writing etching on the nano bismuth vanadate film in the etching area, and preparing a nano bismuth vanadate film pattern with the same shape and size as the designed parallel stripe pattern on the surface of the cylindrical hollow quartz glass tube; immersing the cylindrical hollow quartz glass tube subjected to laser direct writing etching into deionized water, and ultrasonically cleaning for 4min to remove residual powder on the surface of the glass tube; immersing the cleaned cylindrical hollow quartz glass tube into chemical silver plating solution to enable the nano bismuth vanadate film pattern to be in contact with the plating solution, and then putting a xenon lamp catalytic light source with the dominant wavelength of 560nm into the cylindrical hollow quartz glass tube; opening a catalytic light source, illuminating for 6min by using a backlight catalytic mode, and carrying out photocatalytic oxidation reduction reaction on the surface of the nano bismuth vanadate film pattern to reduce silver ions in the plating solution into silver simple substances to be deposited on the surface of the nano bismuth vanadate film pattern so as to generate a primary silver plating layer with the shape and the size consistent with those of the designed parallel stripe pattern; continuously carrying out autocatalytic chemical plating in the plating solution by taking the primary silver plating layer as an activation center, wherein the reaction time is 6min, so that the continuous growth of the primary silver plating layer in the plating solution is realized, and finally, preparing a high-quality parallel stripe pattern silver plating layer with the required thickness and shape and size on the surface of the cylindrical hollow quartz glass tube; and taking out the cylindrical hollow quartz glass tube coated with the parallel stripe pattern silver coating on the surface, and drying in the sun or blow drying after washing to finish the preparation of the parallel stripe pattern silver coating on the surface of the cylindrical hollow quartz glass tube.
Claims (8)
1. A laser direct-writing pre-forming photocatalytic plating preparation method of metal patterns on the surface of a material is characterized by comprising the following preparation processes:
(1) inputting shape and size data of a design pattern into a control computer of a laser direct writing system, setting the frequency and power of a laser, a laser scanning path, scanning speed and scanning times, and determining a laser direct writing etching area and etching depth on the surface of a base material;
(2) placing the substrate material with the nano semiconductor film deposited on the surface on a working platform of a laser direct writing system, enabling the surface of the nano semiconductor film to face a laser light source, and positioning and focusing an etching area;
(3) starting a laser direct-writing program, performing direct-writing etching on the nano semiconductor film in the etching area, and preparing a nano semiconductor film pattern with the same shape and size as the designed pattern on the surface of the base material;
(4) immersing the substrate material subjected to laser direct writing etching into a cleaning agent, and ultrasonically cleaning for 1-40 min to remove residual powder on the surface of the substrate material;
(5) immersing the cleaned substrate material into a chemical plating solution to enable the nano semiconductor film pattern to face a catalytic light source with the wavelength of 200-580 nm;
(6) opening a catalytic light source, illuminating for 1-15 min by using a positive photocatalysis or backlight catalysis mode, and carrying out photocatalytic oxidation reduction reaction on the surface of the nano semiconductor film pattern to reduce metal ions in the plating solution into elemental metal or alloy to be deposited on the surface of the nano semiconductor film pattern so as to generate a primary metal plating layer with the shape and the size consistent with those of the designed pattern;
(7) continuously carrying out autocatalytic chemical plating in the plating solution by taking the primary metal plating layer as an activation center, wherein the reaction time is 0-120 min, so that the continuous growth of the primary metal plating layer in the plating solution is realized, and finally, a high-quality metal pattern with the required thickness, shape and size is prepared on the surface of the substrate material;
(8) taking out the base material with the surface plated with the metal pattern, and drying in the sun or blow drying after washing to finish the preparation of the metal pattern on the surface of the base material;
the laser direct writing system is a continuous laser direct writing system or a pulse laser direct writing system, the laser wavelength lambda is not less than 150nm and not more than 1650nm, and the scanning speed v is more than 0 and not more than v<8000mm/s, said etching depth h1H is not less than 0.01 mu m1Less than or equal to 200 mu m and more than or equal to the thickness h of the nano semiconductor film2。
2. The method for preparing the laser direct-writing preformed photocatalytic coating of the metal pattern on the surface of the material according to claim 1, wherein the base material is at least one of a metal material, an inorganic non-metal material, a polymer material or a composite material.
3. The method for preparing the laser direct-writing preformed photocatalytic coating of the metal pattern on the surface of the material according to claim 1, wherein the nano semiconductor film is at least one of an oxide nano semiconductor film, a non-oxide nano semiconductor film and a composite nano semiconductor film with a photocatalytic effect, and the thickness h of the nano semiconductor film2Is 0 < h2≤900nm。
4. The method for preparing the laser direct-writing preformed photocatalytic coating of the metal pattern on the surface of the material according to claim 1, wherein the working platform is at least one of a rectangular coordinate type working platform, a polar coordinate type working platform and a combined type working platform.
5. The preparation method of the laser direct writing preformed photocatalytic coating of the metal pattern on the surface of the material as claimed in claim 1, wherein the cleaning agent is a solvent type cleaning agent or a water-based cleaning agent, and the water-based cleaning agent is an acid cleaning agent, an alkaline cleaning agent or a neutral cleaning agent.
6. The method for preparing the laser direct writing preformed photocatalytic plating of the metal pattern on the surface of the material according to claim 1, wherein the electroless plating solution is electroless gold, silver, copper, nickel, tin, palladium, aluminum, iron, cobalt, zinc, chromium, molybdenum, platinum, tungsten, rare earth metal and alloy solution thereof.
7. The method for preparing the laser direct-writing preformed photocatalytic coating of the metal pattern on the surface of the material according to claim 1, wherein the catalytic light source is a linear light source or a nonlinear light source.
8. The method of claim 1, wherein the metal is at least one of gold, silver, copper, nickel, tin, palladium, aluminum, iron, cobalt, zinc, chromium, molybdenum, platinum, tungsten, rare earth metals, and alloys thereof.
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| CN112924510B (en) * | 2021-01-27 | 2022-03-15 | 中国科学院上海微系统与信息技术研究所 | Graphene-based high-entropy alloy nanoparticle and preparation method and application thereof |
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