CN113893876A - Electroless copper plating catalyst and method for forming metal grid by using same - Google Patents
Electroless copper plating catalyst and method for forming metal grid by using same Download PDFInfo
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- CN113893876A CN113893876A CN202111061206.1A CN202111061206A CN113893876A CN 113893876 A CN113893876 A CN 113893876A CN 202111061206 A CN202111061206 A CN 202111061206A CN 113893876 A CN113893876 A CN 113893876A
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- Prior art keywords
- copper plating
- electroless copper
- plating catalyst
- hyperdispersant
- metal grid
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- 239000010949 copper Substances 0.000 title claims abstract description 111
- 238000007747 plating Methods 0.000 title claims abstract description 84
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- 238000000034 method Methods 0.000 title claims abstract description 33
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Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
-
- 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
-
- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06F—ELECTRIC DIGITAL DATA PROCESSING
- G06F3/00—Input arrangements for transferring data to be processed into a form capable of being handled by the computer; Output arrangements for transferring data from processing unit to output unit, e.g. interface arrangements
- G06F3/01—Input arrangements or combined input and output arrangements for interaction between user and computer
- G06F3/03—Arrangements for converting the position or the displacement of a member into a coded form
- G06F3/041—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means
-
- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06F—ELECTRIC DIGITAL DATA PROCESSING
- G06F2203/00—Indexing scheme relating to G06F3/00 - G06F3/048
- G06F2203/041—Indexing scheme relating to G06F3/041 - G06F3/045
- G06F2203/04103—Manufacturing, i.e. details related to manufacturing processes specially suited for touch sensitive devices
Abstract
The invention provides an electroless copper plating catalyst and a method for forming a metal grid by using the same, wherein the electroless copper plating catalyst comprises palladium nano-particles and a dispersing agent, wherein the dispersing agent is selected from one or more of polyester type hyperdispersant, polyacrylate type hyperdispersant and polyolefin type hyperdispersant. The electroless copper plating catalyst provided by the invention has excellent catalytic activity, and when the electroless copper plating catalyst provided by the invention is used (particularly when the catalyst contains a polyolefin hyperdispersant), a metal copper grid line is formed, the electroless copper plating catalyst has the advantages of reducing the plating start time of a metal grid in an electroless copper plating process, reducing the line width of the metal copper grid line and the like, and has higher practicability; the electroless copper plating catalyst has excellent stability, and can be placed at normal temperature for a longer time without precipitation.
Description
Technical Field
The invention belongs to the field of electroless copper plating, and particularly relates to an electroless copper plating catalyst and a method for forming a metal grid by using the same.
Background
The preparation process of the metal grid touch sensor mainly comprises coating, exposure, development, copper plating, blackening and the like. The roll-on-roll structure on flexible substrates is currently usually made of a UV-curable base layer, an intermediate layer containing colloidal palladium nanoparticles and a top protective layer. And carrying out mask UV exposure on the coated coil, carrying out wet development to obtain a composite structure formed by an ultraviolet light curing base layer and palladium nano particles on the top, and then carrying out chemical copper plating by using the palladium nano particles deposited on the ultraviolet light curing base layer as a catalyst.
The palladium-based catalyst has the advantages of high catalytic activity, strong selectivity, convenient catalyst preparation, small usage amount, capability of optimizing performance by compounding with other metals or promoter active components through the change and improvement of a preparation method, repeated regeneration and activation use, long service life, capability of recycling and reusing metal palladium of a waste catalyst and the like, and is widely used in the field of chemical copper plating. Common methods for preparing metal nanoparticles include gas phase chemical reaction, precipitation, liquid phase reduction, spray pyrolysis, sol-gel, and the like. The liquid phase reduction method can be simply classified into an organic solvent synthesis method and an aqueous solution synthesis method according to the difference of solvents. The nano-particles prepared by the organic solvent synthesis method have the advantages of good crystallinity, good monodispersity, easy control of morphology and the like. The method for preparing palladium nano particles in the prior art is an organic solvent synthesis method.
Common dispersants can be divided into three categories: inorganic dispersants, organic small molecule dispersants and hyperdispersants. Hyperdispersants overcome the limitations of conventional dispersants in non-aqueous dispersion systems. Compared with other dispersing agents, the dispersing agent has the following characteristics: (1) multi-point anchoring is formed on the particle surface, so that the adsorption fastness is improved, and desorption is not easy to occur; (2) the solvating chain is longer than the lipophilic group of the traditional dispersant, and can play an effective space stabilizing role; (3) forming a very weak capsule, being easy to move, being capable of rapidly moving to the surface of the particles and playing a role in wetting protection; (4) and a lipophilic film cannot be introduced on the surface of the particles, so that the application performance of the final product is not influenced.
However, different dispersants have a significant effect on the activity and solution stability of the palladium nanoparticles, and there is still a need to find a palladium nanoparticle catalyst having excellent catalytic activity and stability, thereby realizing the preparation of copper metal mesh with smaller line width.
Disclosure of Invention
The present invention aims to improve the catalytic activity and stability of the existing palladium nanoparticle catalyst, and to provide a palladium nanoparticle catalyst having more excellent catalytic activity and stability. After the research, the present inventors have unexpectedly found that a palladium nanoparticle catalyst having the combination of the palladium nanoparticle of the present invention and a specific dispersant has more excellent catalytic activity and stability when used as an electroless copper plating catalyst, and have completed the present invention based on this.
In one aspect, the present invention provides an electroless copper plating catalyst comprising palladium nanoparticles and a dispersant, wherein the dispersant is selected from one or more of a polyester-based hyperdispersant, a polyacrylate-based hyperdispersant, and a polyolefin-based hyperdispersant.
In one embodiment of the invention, the dispersant comprises at least a polyolefin-based hyper-dispersant.
In one embodiment of the invention, the polyester-based hyperdispersant is selected from one or more of Solsperse-3000, Solsperse-9000, Solsperse-24000, Solsperse-46000, and Solsperse-20000.
In one embodiment of the invention, the polyacrylate type hyperdispersant is selected from one or more of EL-vacit AB 1010, EL-vacit AB 1015, EL-vacit AB 1020, EL-vacit AB 1030, Disperse-AYD15, BYK-358, BYK-163, and BYK-154.
In one embodiment of the invention, the polyolefin-based hyperdispersant is selected from one or more of PVP K15, PVP K30, PVP K60 and PVP K90.
In one embodiment of the present invention, the weight ratio of the palladium nanoparticle to the dispersant is 0.1 to 10: 1, preferably 0.2 to 5: 1, more preferably 0.5 to 2: 1.
in another aspect, the present invention also provides a method for forming a metal grid on a flexible substrate, wherein the method comprises the steps of:
(1) sequentially coating a UV curable material, an electroless copper plating catalyst as described above, and a protective layer material on one surface of the flexible substrate;
(2) exposing and developing the coated flexible substrate to sequentially form a UV curable layer and a catalytic layer on a surface of the flexible substrate according to a desired pattern; and
(3) plating copper on the pattern to form the metal grid.
In one embodiment of the invention, the coating is a wet coating.
In one embodiment of the present invention, the UV curable material is a positive photoresist or a negative photoresist.
In another aspect, the present invention also provides a metal grid touch sensor, wherein the metal grid of the metal grid touch sensor is formed by the method as described above.
Compared with the prior art, the technical scheme of the invention at least comprises the following advantages:
the electroless copper plating catalyst provided by the invention has excellent catalytic activity, and when the electroless copper plating catalyst provided by the invention is used (particularly when the catalyst contains a polyolefin hyperdispersant), a metal copper grid line is formed, the electroless copper plating catalyst has the advantages of reducing the plating start time of a metal grid in an electroless copper plating process, reducing the line width of the metal copper grid line and the like, and has higher practicability; the electroless copper plating catalyst has excellent stability, and can be placed at normal temperature for a longer time without precipitation.
Drawings
The accompanying drawings, which 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 principles of the invention and not to limit the invention. In the drawings:
fig. 1 shows a flow diagram of an exemplary method of forming a metal grid in accordance with an embodiment of the present invention.
Figure 2 shows the copper metal grid samples prepared according to examples 1 and 3 of the present invention, wherein the samples are shown at 20 x magnification, the copper metal grid sample prepared in example 3 plated copper for 5 seconds only, while the copper metal grid sample prepared in example 1 plated copper for 30 seconds only.
FIG. 3 shows the line widths of the samples produced according to example 1-1 of the present invention after copper plating and after development.
FIG. 4 shows the line widths of the samples produced according to examples 1-2 of the present invention after copper plating and after development.
Fig. 5 shows the line widths of the samples prepared according to examples 1-3 of the present invention after copper plating and after development.
FIG. 6 shows the line widths of the samples produced according to example 2-1 of the present invention after copper plating and after development.
FIG. 7 shows the line widths of the samples produced according to example 2-2 of the present invention after copper plating and after development.
FIG. 8 shows the line widths of the samples produced according to examples 2-3 of the present invention after copper plating and after development.
FIG. 9 shows the line widths of the samples produced according to example 3-1 of the present invention after copper plating and after development.
FIG. 10 shows the line widths of the samples produced according to example 3-2 of the present invention after copper plating and after development.
FIG. 11 shows the line widths after copper plating and after development of the samples prepared according to example 3-3 of the present invention.
Fig. 12 shows the copper plating effect achievable after exposure and development using the electroless copper plating catalyst of example 3 and a reticle with a line width of 1.25 μm according to an embodiment of the present invention.
Fig. 13 shows the results of a test of adhesion after copper plating using the electroless copper plating catalyst of example 3 according to an embodiment of the present invention.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
Unless defined otherwise, all terms (including 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 will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the relevant art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
In one aspect, the present invention provides an electroless copper plating catalyst comprising palladium nanoparticles and a dispersant, wherein the dispersant is selected from one or more of a polyester-based hyperdispersant, a polyacrylate-based hyperdispersant, and a polyolefin-based hyperdispersant.
After research, the chemical copper plating catalyst disclosed by the invention can be used for better wrapping and dispersing palladium nanoparticles when one or more of polyester type hyperdispersant, polyacrylate type hyperdispersant and polyolefin type hyperdispersant is/are selected as the dispersant, so that the obtained colloidal palladium nanoparticles have smaller particle size and stronger catalytic activity. The palladium nanoparticles with smaller particle size and stronger catalytic activity are used as the coating material of the second layer, so that the plating time of the metal grid in the chemical copper plating process can be reduced. Meanwhile, the palladium nanoparticles in the electroless copper plating catalyst prepared by the method have stronger stability, and can be placed at normal temperature for a longer time without precipitation.
In a preferred embodiment of the present invention, the dispersant may include at least a polyolefin-based hyper-dispersant. For example, in one embodiment, the dispersant may comprise or consist of only a polyolefin-based hyper-dispersant. In another embodiment, the dispersant may comprise or consist of both a polyolefin-based hyperdispersant and a polyester-based hyperdispersant. In another embodiment, the dispersant may comprise or consist of both a polyolefin-based hyperdispersant and a polyacrylate-based hyperdispersant. In another embodiment, the dispersant may comprise or consist of three of a polyester-based hyperdispersant, a polyacrylate-based hyperdispersant, and a polyolefin-based hyperdispersant.
The present invention is not particularly limited with respect to the specific types of the polyester type hyperdispersant, the polyacrylate type hyperdispersant and the polyolefin type hyperdispersant, and any of the polyester type hyperdispersant, the polyacrylate type hyperdispersant and the polyolefin type hyperdispersant known to the skilled person can be used. In a preferred embodiment of the present invention, the polyester-based hyperdispersant may be selected from one or more of Solsperse-3000, Solsperse-9000, Solsperse-24000, Solsperse-46000, and Solsperse-20000; the polyacrylate type hyperdispersant can be selected from one or more of EL-vacit AB 1010, EL-vacit AB 1015, EL-vacit AB 1020, EL-vacit AB 1030, Disperse-AYD15, BYK-358, BYK-163 and BYK-154; the polyolefin-based hyperdispersant may be selected from one or more of PVP K15, PVP K30, PVP K60 and PVP K90, but is not limited thereto.
In addition, the palladium nanoparticles and the dispersant in the electroless copper plating catalyst are not particularly limited in the present invention, and can be adjusted according to experience and actual needs of those skilled in the art. In a preferred embodiment of the present invention, the weight ratio of the palladium nanoparticle to the dispersant may be 0.1 to 10: 1 (e.g., 0.1: 1, 0.2: 1, 0.3: 1, 0.5: 1, 0.8: 1, 1: 1, 1.2: 1, 1.5: 1, 2: 1, 3: 1, 5: 1, or 8: 1, etc.), preferably 0.2 to 5: 1, more preferably 0.5 to 2: 1.
in another aspect, the present invention also provides a method for forming a metal grid on a flexible substrate, wherein the method comprises the steps of:
(1) sequentially coating a UV curable material, an electroless copper plating catalyst as described above, and a protective layer material on one surface of the flexible substrate;
(2) exposing and developing the coated flexible substrate to sequentially form a UV curable layer and a catalytic layer on a surface of the flexible substrate according to a desired pattern; and
(3) and plating copper on the pattern to form the metal grid on the flexible substrate.
With respect to step (1), fig. 1 shows a flowchart of an exemplary method of forming a metal mesh according to an embodiment of the present invention, in which a UV curable layer, a Pd nanoparticle layer, and a water-soluble protective layer are sequentially formed on one surface of a substrate by sequentially coating the UV curable material, an electroless copper plating catalyst as described above, and a protective layer material on the surface of the substrate.
For the UV curable material as the first layer (or referred to as the base layer), the UV curable material may be a positive photoresist or a negative photoresist. In one embodiment, the positive photoresist may preferably include a resin material soluble in a developing solution after exposure, and the negative photoresist may preferably include a resin material insoluble in a developing solution after exposure. The developer is usually an aqueous solution containing an alkali compound and a surfactant, the alkali compound may be an inorganic or organic alkali compound, and these inorganic and organic alkali compounds may be used alone or in combination of two or more; as the surfactant, at least one selected from the group consisting of nonionic surfactants, anionic surfactants and cationic surfactants may be used, and these surfactants may be used alone or in combination of two or more.
In addition, a photoinitiator may be further included in the UV curable material, for example, in one embodiment of the present invention, the photoinitiator may be at least one selected from the group consisting of acetophenone-based compounds, benzophenone-based compounds, triazine-based compounds, thioxanthone-based compounds, and oxime-based compounds. Specific examples of the acetophenone-based compound may include 2-hydroxy-2-methyl-1-phenylpropan-1-one, diethoxyacetophenone, 2- (4-methylbenzyl) -2- (dimethylamino) -1- (4-morpholinophenyl) butan-1-one and the like. Specific examples of the benzophenone-based compound may include benzophenone, methyl o-benzoylbenzoate, 4-benzoyl-4' -methyl diphenyl sulfide, 2,4, 6-trimethylbenzophenone, and the like. Specific examples of the triazine-based compound may include 2, 4-bis (trichloromethyl) -6- (4-methoxyphenyl) -1,3, 5-triazine, 2, 4-bis (trichloromethyl) -6- (4-methoxynaphthyl) -1,3, 5-triazine, 2, 4-bis (trichloromethyl) -6- [2- (3, 4-dimethoxyphenyl) vinyl ] -1,3, 5-triazine, and 2, 4-bis (trichloromethyl) -6-2- (4-diethylamino-2-methylphenyl) vinyl ] -1,3, 5-triazine and the like. Specific examples of the thioxanthone-based compound may include 2-isopropylthioxanthone, 2, 4-diethylthioxanthone, 2, 4-dichlorothioxanthone, 1-chloro-4-propoxythioxanthone, and the like. Specific examples of the oxime ester compounds may include o-ethoxycarbonyl- α -oxyimino-1-phenylpropan-1-one, 1, 2-octanedione, 1- (4-phenylthio) phenyl, 2- (o-benzoyloxime), and the like.
The Pd nanoparticle layer as the second layer is the electroless copper plating catalyst of the present invention, and is the key to the technique of forming a metal mesh on a flexible substrate of the present invention. Since the components, contents, etc. of the electroless copper plating catalyst of the present invention have been described in detail in the foregoing section, the features of the electroless copper plating catalyst will not be described in detail in this section to avoid unnecessary redundancy.
The protective layer material as the third layer is mainly used for protection in the exposure stage, and is washed away by the developing solution in the developing stage. According to the present invention, the protective layer material may be performed using a protective layer material that is conventional in the art. In a preferred embodiment, the protective layer material may be a water soluble material to enable it to be dissolved in an aqueous developer solution during the development stage.
According to the present invention, the three coating materials may be preferably applied by wet coating, i.e., a UV curable material, an electroless copper plating catalyst, and a protective layer material in the form of a liquid or solution may be sequentially coated on one surface of the substrate.
With respect to the step (2), the substrate coated with the UV curable material, the electroless copper plating catalyst, and the protective layer material in this order is exposed to ultraviolet rays with a mask having a desired pattern disposed therebetween, thereby forming a desired pattern on the substrate. Subsequently, in the developing process, as described above, the UV curable material and the protective layer material that are not cured may be removed in the developing process.
For step (3), since the protective layer material is removed, and the palladium nanoparticle layer is at the uppermost layer, it can be used as a catalyst for copper plating, so this step only needs to perform copper plating, for example, electroless copper plating, on the pattern, thereby forming the required metal grid.
In another aspect, the present invention also provides a metal grid touch sensor, the metal grid of which is formed by the method of forming a metal grid as described above.
In conclusion, the electroless copper plating catalyst provided by the invention has excellent catalytic activity, and when the electroless copper plating catalyst provided by the invention is used (particularly when the catalyst contains a polyolefin hyper-dispersant), a metal copper grid line is formed, so that the electroless copper plating catalyst has the advantages of reducing the plating start time of a metal grid in an electroless copper plating process, reducing the line width of the metal copper grid line and the like, and has higher practicability; the electroless copper plating catalyst has excellent stability, and can be placed at normal temperature for a longer time without precipitation.
Examples
Example 1
Mixing and heating 90% of solvent, 4% of palladium acetate and 6% of dispersing agent A according to the mass components to 105 ℃, stirring for 2 hours, mixing the obtained mixed solution with pure water and surfactant to obtain the palladium-containing nanoparticle catalyst coating solution, wherein the solvent is ethyl lactate, the A is a hyper-dispersant Solsperse46000, and the surfactant is a fluorine-containing surfactant.
Coating a negative photoresist coating containing Irgacure 907 on one surface of a flexible substrate by using a coating wire rod, and then drying the coating in an oven at the temperature of 70 ℃ for 120 seconds to obtain a coating with the thickness of 800 nm; coating a layer of the palladium-containing nanoparticle catalyst coating prepared as above on the top of the photoresist film, then coating a layer of water-soluble material for protecting the two coatings, and then exposing by using ultraviolet light with a peak wave of 314 nm; after exposure, the substrate is washed by alkaline developing solution to remove the water-soluble protective coating and the uncured negative photoresist coating, the obtained sample is immersed in chemical copper plating solution to grow copper grids, and the palladium-containing nanoparticle catalyst plays a role in catalyzing copper plating reaction in the process.
Example 2
Copper plating was carried out in a similar manner to example 1, except that a copper plating catalyst was prepared as follows: mixing and heating 90% of solvent, 4% of palladium acetate and 6% of dispersing agent B according to the mass components to 105 ℃, stirring for 2 hours, mixing the obtained mixed solution with pure water and surfactant to obtain the palladium-containing nanoparticle catalyst coating, wherein the solvent is ethyl lactate, the B is hyper-dispersant PVP K30, and the surfactant is fluorine-containing surfactant.
Example 3
Copper plating was carried out in a similar manner to example 1, except that a copper plating catalyst was prepared as follows: mixing 90% of solvent, 4% of palladium acetate, 1% of dispersant A and 5% of dispersant B according to the mass components, heating to 105 ℃, stirring for 2 hours, mixing the obtained mixed solution with pure water and surfactant to obtain the catalyst coating, wherein the solvent is ethyl lactate, the A is the hyper-dispersant Solsperse46000, the B is the hyper-dispersant PVP K30, and the surfactant is the fluorine surfactant.
Test example
Three groups of copper metal grid samples prepared according to the procedure of example 1, named as example 1-1, example 1-2 and example 1-3, were measured for the line width of the copper metal grid under a 2.5D two-dimensional manual image measuring instrument.
Three groups of copper metal grid samples prepared according to the procedure of example 2, named as example 2-1, example 2-2 and example 2-3, were measured for the line width of the copper metal grid under a 2.5D two-dimensional manual image measuring instrument.
Three groups of metallic copper grid samples prepared according to the procedure of example 3, named as example 3-1, example 3-2 and example 3-3, were measured for the line width of the metallic copper grid under a 2.5D two-dimensional manual image measuring instrument.
The data of the developed line width average value before copper plating and the metal copper grid line width average value after copper plating of the above 9 groups of samples are shown in the following tables 1 to 2 and fig. 3 to 11.
TABLE 1 mean line widths after development
TABLE 2 average line widths after copper plating
As can be seen from the data in tables 1 and 2, the samples prepared from examples 1-3 each achieved narrower developed line widths and copper metal grid line widths. In particular, the sample prepared in example 3 had the narrowest wire width of the copper metal gridlines, with the developed wire widths being close. This fully confirms that the chemical catalyst provided by the present invention has the advantage of reducing the line width of the copper metal mesh lines when the copper metal mesh lines are prepared by the above method, has high practicability, and is excellent particularly when the hyperdispersant comprises a polyolefin hyperdispersant such as PVP K30.
Meanwhile, the catalyst prepared in example 1 can be placed at normal temperature for 4 days without precipitation, and the catalyst prepared in example 3 can be placed at normal temperature for 10 days without precipitation, and still has good catalytic activity. Thus, it was confirmed that the electroless copper plating catalyst of the present invention has excellent stability and can be left at normal temperature for a longer period of time without precipitation.
In addition, fig. 2 shows the copper metal grid samples prepared in example 1 and example 3, wherein the samples are magnified by 20 times, the copper metal grid sample prepared in example 3 can be plated after being plated with copper for 5 seconds, and the copper metal grid sample prepared in example 1 can be plated with copper for 30 seconds, which confirms that the catalyst prepared in example 3 is more excellent in activity.
As shown in fig. 3 to 5, for the samples prepared in example 1, the difference between the developed line width and the copper-plated line width was about 1.6 μm, i.e., the difference between the copper-plated line width and the developed line width was small.
As shown in fig. 6 to 8, for the samples prepared in example 2, the difference between the developed line width and the copper-plated line width was about 1.9 μm, i.e., the difference between the copper-plated line width and the developed line width was small.
As shown in fig. 9 to 11, for the samples prepared in example 3, the difference between the developed line width and the copper-plated line width was about 0.4 μm, i.e., the difference between the copper-plated line width and the developed line width was very small.
As shown in fig. 12, a coated sample prepared from the catalyst prepared in example 3 was exposed to light using a photomask with a design line width of 1.25 μm and then subjected to development copper plating, and the minimum line width of the copper grid line was 1.5 μm, which shows that the novel electroless copper plating catalyst of the present invention has a more catalytic property and is also useful for reducing the line width after copper plating.
As shown in fig. 13, a coated sample prepared from the catalyst prepared in example 3 was attached to a copper mesh wire using a 3M 610 adhesive tape after copper plating, pressed with a finger until the tape was completely attached, and then the tape was quickly peeled off without the copper wire falling off, which proved that the adhesion after copper plating was good.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (10)
1. An electroless copper plating catalyst comprising palladium nanoparticles and a dispersant, wherein the dispersant is selected from one or more of a polyester-based hyperdispersant, a polyacrylate-based hyperdispersant and a polyolefin-based hyperdispersant.
2. The electroless copper plating catalyst according to claim 1, wherein the dispersant comprises at least a polyolefin-based hyper-dispersant.
3. The electroless copper plating catalyst according to claim 1 or 2, wherein the polyester-based hyperdispersant is selected from one or more of Solsperse-3000, Solsperse-9000, Solsperse-24000, Solsperse-46000 and Solsperse-20000.
4. The electroless copper plating catalyst according to claim 1 or 2 wherein the polyacrylate type hyperdispersant is selected from one or more of EL-vacit AB 1010, EL-vacit AB 1015, EL-vacit AB 1020, EL-vacit AB 1030, Disperse-AYD15, BYK-358, BYK-163 and BYK-154.
5. The electroless copper plating catalyst according to claim 1 or 2, wherein the polyolefin-based hyperdispersant is selected from one or more of PVP K15, PVP K30, PVP K60 and PVP K90.
6. The electroless copper plating catalyst according to claim 1, wherein the weight ratio of the palladium nanoparticles to the dispersant is 0.1-10: 1, preferably 0.2 to 5: 1, more preferably 0.5 to 2: 1.
7. a method for forming a metal grid on a flexible substrate, wherein the method comprises the steps of:
(1) sequentially coating a UV curable material, an electroless copper plating catalyst according to any one of claims 1 to 6, and a protective layer material on one surface of the flexible substrate;
(2) exposing and developing the coated flexible substrate to sequentially form a UV curable layer and a catalytic layer on a surface of the flexible substrate according to a desired pattern; and
(3) plating copper on the pattern to form the metal grid.
8. The method of claim 7, wherein the coating is a wet coating.
9. The method of claim 7, wherein the UV curable material is a negative photoresist.
10. A metal grid touch sensor, characterized in that the metal grid of the metal grid touch sensor is formed by a method according to any of claims 7-9.
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| PCT/CN2022/113510 WO2023035903A1 (en) | 2021-09-10 | 2022-08-19 | Electroless copper plating catalyst and method for forming metal grid by using same |
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| CN115747778A (en) * | 2022-11-16 | 2023-03-07 | 浙江鑫柔科技有限公司 | Preparation method of negative current collector |
| WO2023035903A1 (en) * | 2021-09-10 | 2023-03-16 | 浙江鑫柔科技有限公司 | Electroless copper plating catalyst and method for forming metal grid by using same |
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