WO2023035903A1 - Catalyseur de cuivrage autocatalytique et procédé de formation d'une grille métallique l'utilisant - Google Patents

Catalyseur de cuivrage autocatalytique et procédé de formation d'une grille métallique l'utilisant Download PDF

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WO2023035903A1
WO2023035903A1 PCT/CN2022/113510 CN2022113510W WO2023035903A1 WO 2023035903 A1 WO2023035903 A1 WO 2023035903A1 CN 2022113510 W CN2022113510 W CN 2022113510W WO 2023035903 A1 WO2023035903 A1 WO 2023035903A1
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copper plating
electroless copper
plating catalyst
hyperdispersant
present
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PCT/CN2022/113510
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English (en)
Chinese (zh)
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王钧
李阳
江建国
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浙江鑫柔科技有限公司
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    • 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

Definitions

  • the invention belongs to the field of electroless copper plating, and in particular relates to an electroless copper plating catalyst and a method for forming a metal grid by using the same.
  • Coated roll structures on flexible substrates are currently typically made from a UV-curable base layer, a middle layer containing colloidal palladium nanoparticles, and a protective layer on top.
  • Mask UV exposure was performed on the coated roll, followed by wet development to obtain a composite structure formed by a UV-cured base layer and palladium nanoparticles on the top, and then the palladium nanoparticles deposited on the UV-cured base layer were used as a catalyst for chemical copper plated.
  • Palladium-based catalysts have high catalytic activity, strong selectivity, convenient catalyst preparation, less usage, can be optimized through changes and improvements in manufacturing methods, compounded with other metals or co-catalyst active components, and can be regenerated and activated repeatedly. , long life, and the palladium metal of the spent catalyst can be recycled and reused.
  • the metal palladium nanoparticle catalyst is widely used in the field of electroless copper plating. Common methods for preparing metal nanoparticles include gas-phase chemical reaction method, precipitation method, liquid-phase reduction method, spray pyrolysis method, sol-gel method, etc. According to the different solvents, the liquid phase reduction method can be simply divided into organic solvent synthesis method and aqueous solution synthesis method. Nanoparticles prepared by organic solvent synthesis have the advantages of good crystallinity, good monodispersity, and easy control of morphology.
  • the method for preparing palladium nanoparticles 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 traditional dispersants in non-aqueous dispersion systems. Compared with other dispersants, it has the following characteristics: (1) Multi-point anchoring is formed on the particle surface, which improves the adsorption fastness and is not easy to desorb; (2) The solvation chain is longer than the lipophilic group of traditional dispersants, which can play a role Effective steric stabilization; (3) form extremely weak capsules, which are easy to move and can quickly move to the surface of the particles to play a role in wetting protection; (4) will not introduce lipophilic film on the surface of the particles, so as not to affect the quality of the final product application performance.
  • the object of the present invention is to improve the catalytic activity and stability of the existing palladium nanoparticle catalyst, and provide a palladium nanoparticle catalyst with more excellent catalytic activity and stability.
  • the inventors have unexpectedly found that the palladium nanoparticle catalyst with palladium nanoparticles of the present invention and a specific dispersant combination has more excellent catalytic activity and stability when used as an electroless copper plating catalyst, and based on this, completed the invention.
  • the present invention provides an electroless copper plating catalyst comprising palladium nanoparticles and a dispersant, wherein the dispersant is selected from polyester hyperdispersants, polyacrylate hyperdispersants and polyolefins One or more of hyperdispersants.
  • the dispersant includes at least a polyolefin hyperdispersant.
  • the polyester hyperdispersant is selected from one or more of Solsperse-3000, Solsperse-9000, Solsperse-24000, Solsperse-46000 and Solsperse-20000.
  • the polyacrylate hyperdispersant is selected from EL-vacit AB 1010, EL-vacit AB 1015, EL-vacit AB 1020, EL-vacit AB 1030, Disperse-AYD15, BYK- One or more of 358, BYK-163 and BYK-154.
  • the polyolefin hyperdispersant is selected from one or more of PVP K15, PVP K30, PVP K60 and PVP K90.
  • the weight ratio of the palladium nanoparticles to the dispersant is 0.1-10:1, preferably 0.2-5:1, more preferably 0.5-2:1.
  • the present invention also provides a method for forming a metal grid on a flexible substrate, wherein the method includes the following steps:
  • the coating is wet coating.
  • the UV curable material is a positive photoresist or a negative photoresist.
  • the present invention also provides a metal grid touch sensor, wherein the metal grid of the metal grid touch sensor is formed by the above-mentioned method.
  • the technical solution of the present invention at least includes the following advantages:
  • the electroless copper plating catalyst provided by the present invention has excellent catalytic activity, and when using the electroless copper plating catalyst of the present invention (especially when comprising polyolefin hyperdispersant in the catalyzer) to form metal copper grid lines, there is a reduction in chemical Advantages such as the starting time of plating of metal grid in the copper plating process, reducing the line width of metal copper grid lines have higher practicability; Precipitation did not occur.
  • FIG. 1 shows a flowchart of an exemplary method of forming a metal mesh according to an embodiment of the present invention.
  • Fig. 2 shows the copper metal grid sample prepared according to embodiment 1 and embodiment 3 of the present invention, the sample shown in the figure is 20 times magnification, and the copper metal grid sample prepared by embodiment 3 can be plated with copper for 5 seconds Start plating, and the copper metal grid sample that embodiment 1 prepares is plated copper 30s and just can start plating.
  • Fig. 3 shows the line width of the sample prepared according to Example 1-1 of the present invention after copper plating and development.
  • FIG. 4 shows the line widths of samples prepared according to Examples 1-2 of the present invention after copper plating and development.
  • FIG. 5 shows the line widths of samples prepared according to Examples 1-3 of the present invention after copper plating and development.
  • Fig. 6 shows the line width of the sample prepared according to Example 2-1 of the present invention after copper plating and development.
  • FIG. 7 shows the line widths of the samples prepared according to Example 2-2 of the present invention after copper plating and development.
  • FIG. 8 shows the line widths of samples prepared according to Examples 2-3 of the present invention after copper plating and development.
  • Fig. 9 shows the line width of the sample prepared according to Example 3-1 of the present invention after copper plating and development.
  • Fig. 10 shows the line width of the sample prepared according to Example 3-2 of the present invention after copper plating and development.
  • Fig. 11 shows the line widths of samples prepared according to Example 3-3 of the present invention after copper plating and development.
  • Example 12 shows the copper plating effect that can be achieved after exposure and development using the electroless copper plating catalyst of Example 3 and a photomask with a line width of 1.25 ⁇ m according to an embodiment of the present invention.
  • FIG. 13 shows test results of adhesion after copper plating using the electroless copper plating catalyst of Example 3 according to an embodiment of the present invention.
  • the present invention provides an electroless copper plating catalyst comprising palladium nanoparticles and a dispersant, wherein the dispersant is selected from polyester hyperdispersants, polyacrylate hyperdispersants and polyolefins One or more of hyperdispersants.
  • the electroless copper plating catalyst of the present invention selects one or more of polyester type hyperdispersants, polyacrylate type hyperdispersants and polyolefin hyperdispersants as dispersants, palladium can be made The nanoparticles are better wrapped and dispersed, and the obtained colloidal palladium nanoparticles have smaller particle size and stronger catalytic activity.
  • Using palladium nanoparticles with smaller particle size and stronger catalytic activity as the coating material of the second layer can reduce the plating start time of the metal grid during the electroless copper plating process.
  • the palladium nanoparticles in the electroless copper plating catalyst prepared by the present invention are more stable, and can be placed at room temperature for a longer period of time without precipitation.
  • the dispersant may at least contain a polyolefin hyperdispersant.
  • the dispersant may only comprise, or consist of, a polyolefin-based hyperdispersant.
  • the dispersant may comprise or consist of both a polyolefin hyperdispersant and a polyester hyperdispersant.
  • the dispersant may comprise or consist of both polyolefin-based hyperdispersants and polyacrylate-based hyperdispersants.
  • the dispersant may comprise or consist of polyester hyperdispersant, polyacrylate hyperdispersant and polyolefin hyperdispersant.
  • the present invention is not particularly limited to the specific types of polyester type hyperdispersant, polyacrylate type hyperdispersant and polyolefin type hyperdispersant, any polyester type hyperdispersant, polyacrylate known to the skilled person can be used type hyperdispersant and polyolefin hyperdispersant.
  • the polyester type hyperdispersant can be selected from one or more of Solsperse-3000, Solsperse-9000, Solsperse-24000, Solsperse-46000 and Solsperse-20000;
  • Polyacrylate hyperdispersant can be selected from 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 hyperdispersant can be selected from one or more of PVP K15, PVP K30, PVP K60 and PVP K90, but not limited thereto.
  • the present invention has no special limitation on the palladium nanoparticles and dispersant in the electroless copper plating catalyst, and can be adjusted according to the experience and actual needs of those skilled in the art.
  • the weight ratio of the palladium nanoparticles to the dispersant can be 0.1-10:1 (for example, 0.1:1, 0.2:1, 0.3:1, 0.5:1, 0.8:1 1, 1:1, 1.2:1, 1.5:1, 2:1, 3:1, 5:1 or 8:1, etc.), preferably 0.2-5:1, more preferably 0.5-2:1.
  • the present invention also provides a method for forming a metal grid on a flexible substrate, wherein the method includes the following steps:
  • FIG. 1 shows a flow chart of an exemplary method of forming a metal mesh according to an embodiment of the present invention, wherein by sequentially coating a UV curable material on one surface of a substrate, chemical A copper catalyst, and a protective layer material are plated to sequentially form a UV curable layer, a Pd nanoparticle layer, and a water-soluble protective layer on the surface of the substrate.
  • the UV curable material can be a positive photoresist or a negative photoresist.
  • the positive photoresist may preferably include a resin material that is soluble in a developer after exposure
  • the negative photoresist may preferably include a resin material that is insoluble in a developer after exposure.
  • Described developing solution is usually the aqueous solution that contains alkaline compound and surfactant, and alkaline compound can be inorganic or organic alkaline compound, and these inorganic and organic alkaline compounds can be used alone or in combination of two or more; And as surface active As an agent, at least one selected from the group consisting of nonionic surfactants, anionic surfactants and cationic surfactants can be used, and these surfactants can be used alone or in combination of two or more.
  • the UV curable material also includes a photoinitiator, for example, in one embodiment of the present invention, the photoinitiator can be selected from acetophenone compounds, benzophenone compounds, triazines At least one of the group consisting of compound, thioxanthone compound and oxime ester compound.
  • acetophenone compounds may include 2-hydroxy-2-methyl-1-phenylpropan-1-one, diethoxyacetophenone, and 2-(4-methylbenzyl)-2- (Dimethylamino)-1-(4-morpholinophenyl)butan-1-one, etc.
  • benzophenone compounds may include benzophenone, methyl o-benzoylbenzoate, 4-benzoyl-4'-methyldiphenyl sulfide, and 2,4,6-trimethyl benzophenone etc.
  • triazine compounds may include 2,4-bis(trichloromethyl)-6-(4-methoxyphenyl)-1,3,5-triazine, 2,4-bis(trichloromethyl) Methyl)-6-(4-methoxynaphthyl)-1,3,5-triazine, 2,4-bis(trichloromethyl)-6-[2-(3,4-dimethoxy phenyl)vinyl]-1,3,5-triazine and 2,4-bis(trichloromethyl)-6-2-(4-diethylamino-2-methylphenyl)ethenyl ]-1,3,5-triazine etc.
  • thioxanthone compounds may include 2-isopropylthioxanthone, 2,4-diethylthioxanthone, 2,4-dichlorothioxanthone, and 1-chloro-4-propoxythioxanthone xanthone etc.
  • oxime ester compounds may include o-ethoxycarbonyl- ⁇ -oxyimino-1-phenylpropan-1-one, 1,2-octanedione, 1-(4-phenylthio)benzene base and 2-(o-benzoyl oxime), etc.
  • the Pd nano particle layer as the second layer is the electroless copper plating catalyst of the present invention, and is the key to the technology of forming the metal grid on the flexible substrate of the present invention. Since the components and contents of the electroless copper plating catalyst of the present invention have been described in detail in the previous section, the characteristics of the electroless copper plating catalyst will not be described in detail in this section to avoid unnecessary redundancy.
  • the protective layer material of the third layer mainly plays a protective role in the exposure stage, and then it will be washed away by the developer in the development stage.
  • the protective layer material can be made using conventional protective layer materials in the art.
  • the protective layer material may be a water-soluble material, so that it can be dissolved in an aqueous developer solution during the development stage.
  • the coating methods of the above three coating materials can preferably be carried out by wet coating, that is, the UV curable material in liquid or solution form, the electroless copper plating catalyst, and the protective layer material can be sequentially coated on one surface of the substrate.
  • step (2) the substrate coated with UV curable material, electroless copper plating catalyst, and protective layer material in sequence is exposed to ultraviolet rays and a mask with a desired pattern is set therebetween, thereby forming a desired pattern on the substrate. pattern. Subsequently, during development, the UV curable material and the protective layer material that are not cured may be removed during development, as described above.
  • step (3) since the protective layer material has been removed, the palladium nanoparticle layer is at the top layer and can be used as a catalyst for copper plating, so this step only needs to carry out copper plating on the pattern, such as using electroless copper plating
  • the way can be, so as to form the required metal grid.
  • 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 for forming the metal grid as described above.
  • the electroless copper plating catalyst provided by the present invention has excellent catalytic activity, and when using the electroless copper plating catalyst of the present invention (especially when comprising polyolefin hyperdispersant in the catalyst) to form metallic copper grid lines , it has the advantages of reducing the plating time of the metal grid in the electroless copper plating process, reducing the line width of the metal copper grid line, and has higher practicability; and the electroless copper plating catalyst of the present invention has excellent stability and can be used at room temperature It can be left for a longer period of time without precipitation.
  • a negative photoresist coating containing Irgacure 907 was coated on one surface of a flexible substrate using a coating wire bar, and then dried in an oven at a temperature of 70° C. for 120 seconds to obtain a coating with a thickness of 800 nm;
  • the top of the photoresist film is coated with a palladium-containing nanoparticle catalyst coating prepared as above, and then coated with a layer of water-soluble material for protecting the above two coatings, and then exposed with ultraviolet light having a peak wave of 314nm;
  • the substrate is rinsed with an alkaline developer to remove the water-soluble protective coating and the uncured negative photoresist coating, and the resulting sample is immersed in an electroless copper plating solution to grow a copper grid, which contains palladium
  • the nanoparticle catalyst plays the role of catalyzing the copper plating reaction.
  • Copper plating is carried out in a method similar to Example 1, except that the copper plating catalyst is prepared as follows: get 90% solvent, 4% palladium acetate, and 6% dispersant B by mass components and mix and heat to 105 ° C, stir After 2h, the resulting mixed solution was mixed with pure water and a surfactant to obtain a palladium-containing nanoparticle catalyst coating, wherein the solvent was ethyl lactate, B was a hyperdispersant PVP K30, and the surfactant was a fluorosurfactant.
  • the solvent was ethyl lactate
  • B was a hyperdispersant PVP K30
  • the surfactant was a fluorosurfactant.
  • Copper plating is carried out in a method similar to Example 1, except that the copper plating catalyst is prepared as follows: get 90% solvent, 4% palladium acetate, 1% dispersant A, 5% dispersant B by mass components and mix Heating to 105°C, stirring for 2 hours, taking the resulting mixed solution, mixing it with pure water and a surfactant to prepare a catalyst coating, wherein the solvent is ethyl lactate, A is the hyperdispersant Solsperse46000, and B is the hyperdispersant PVP K30.
  • the active agent is a fluorosurfactant.
  • Example 1-1 Take three groups of metallic copper grid samples prepared according to the steps of Example 1, named as Example 1-1, Example 1-2, and Example 1-3, and measure metallic copper under a 2.5D two-dimensional manual image measuring instrument Grid line width.
  • Example 2-1 Take three groups of metallic copper grid samples prepared according to the steps of Example 2, named as Example 2-1, Example 2-2, and Example 2-3, and measure metallic copper under a 2.5D two-dimensional manual image measuring instrument Grid line width.
  • Example 3-1 Take three groups of metallic copper grid samples prepared according to the steps of Example 3, named as Example 3-1, Example 3-2, and Example 3-3, and measure metallic copper under a 2.5D two-dimensional manual image measuring instrument Grid line width.
  • Table 1-2 and Figure 3-11 show the data of the average development line width before copper plating and the average copper grid line width after copper plating of the above nine groups of samples.
  • the samples prepared in Examples 1-3 all realized narrower development line width and metal copper grid line width.
  • the sample prepared in Example 3 has the narrowest line width of the metal copper grid line when the development line width is close.
  • the chemical catalyst provided by the present invention has the advantage of reducing the width of the metal copper grid line when the metal copper grid line is prepared by the above-mentioned method, and has higher practicability, especially when the hyperdispersant contains polyolefin When using a hyperdispersant such as PVP K30, the above effects are even better.
  • the catalyst prepared in Example 1 can be placed at room temperature for 4 days without precipitation, while the catalyst prepared in Example 3 can be placed at room temperature for 10 days without precipitation, and still has good catalytic activity.
  • the electroless copper plating catalyst of the present invention has excellent stability and can be placed at room temperature for a longer period of time without precipitation.
  • Fig. 2 shows the copper metal grid sample prepared by embodiment 1 and embodiment 3, the sample shown in the figure is 20 times magnification, and the copper metal grid sample prepared by embodiment 3 can be plated in 5 seconds , while the copper metal grid sample prepared in Example 1 could be plated after 30s of copper plating, which confirmed that the catalyst activity prepared in Example 3 was more excellent.
  • the difference between the line width after development and the line width after copper plating is about 1.6 microns, that is, the difference between the line width after copper plating and the line width after development is relatively small.
  • the difference between the line width after development and the line width after copper plating is about 1.9 microns, that is, the difference between the line width after copper plating and the line width after development is relatively small.
  • the difference between the line width after development and the line width after copper plating is about 0.4 microns, that is, the difference between the line width after copper plating and the line width after development is extremely small.

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Abstract

La présente invention concerne un catalyseur de cuivrage autocatalytique et un procédé de formation d'une grille métallique l'utilisant. Le catalyseur de cuivrage autocatalytique contient des nanoparticules de palladium et un dispersant ; et le dispersant est choisi parmi un ou plusieurs parmi un hyperdispersant de type polyester, un hyperdispersant de type polyacrylate, et un hyperdispersant de type polyoléfine. Le catalyseur de cuivrage autocatalytique selon la présente invention a une excellente activité catalytique ; lorsque le catalyseur de cuivrage autocatalytique (en particulier lorsque le catalyseur contient l'hyperdispersant de type polyoléfine) est utilisé pour former une ligne de grille en cuivre métallique, les avantages de la réduction du temps de placage d'une grille métallique dans le procédé de cuivrage autocatalytique, la réduction d'une largeur de ligne de la ligne de grille de cuivre métallique, et similaires sont obtenues, et l'aptitude à la mise en œuvre est élevée ; et le catalyseur de cuivrage autocatalytique selon la présente invention a une excellente stabilité, et peut être placé à température ambiante pendant une durée plus longue sans précipitation.
PCT/CN2022/113510 2021-09-10 2022-08-19 Catalyseur de cuivrage autocatalytique et procédé de formation d'une grille métallique l'utilisant WO2023035903A1 (fr)

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