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CN110328972B - Surface treatment method of printing nozzle - Google Patents

Surface treatment method of printing nozzle Download PDF

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Publication number
CN110328972B
CN110328972B CN201910715361.7A CN201910715361A CN110328972B CN 110328972 B CN110328972 B CN 110328972B CN 201910715361 A CN201910715361 A CN 201910715361A CN 110328972 B CN110328972 B CN 110328972B
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China
Prior art keywords
printing nozzle
treatment
solution
printing
metal layer
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CN201910715361.7A
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Chinese (zh)
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CN110328972A (en
Inventor
眭俊
李哲
黄航
苏亮
田亚蒙
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Guangdong Juhua Printing Display Technology Co Ltd
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Guangdong Juhua Printing Display Technology Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B41PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41JTYPEWRITERS; SELECTIVE PRINTING MECHANISMS, i.e. MECHANISMS PRINTING OTHERWISE THAN FROM A FORME; CORRECTION OF TYPOGRAPHICAL ERRORS
    • B41J2/00Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed
    • B41J2/005Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed characterised by bringing liquid or particles selectively into contact with a printing material
    • B41J2/01Ink jet
    • B41J2/135Nozzles
    • B41J2/16Production of nozzles
    • B41J2/1621Manufacturing processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B41PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41JTYPEWRITERS; SELECTIVE PRINTING MECHANISMS, i.e. MECHANISMS PRINTING OTHERWISE THAN FROM A FORME; CORRECTION OF TYPOGRAPHICAL ERRORS
    • B41J2/00Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed
    • B41J2/005Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed characterised by bringing liquid or particles selectively into contact with a printing material
    • B41J2/01Ink jet
    • B41J2/135Nozzles
    • B41J2/16Production of nozzles
    • B41J2/1621Manufacturing processes
    • B41J2/164Manufacturing processes thin film formation
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C18/00Chemical 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
    • C23C18/16Chemical 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
    • C23C18/1601Process or apparatus
    • C23C18/1633Process of electroless plating
    • C23C18/1655Process features
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C18/00Chemical 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
    • C23C18/16Chemical 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
    • C23C18/18Pretreatment of the material to be coated
    • C23C18/1803Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
    • C23C18/1824Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
    • C23C18/1837Multistep pretreatment
    • C23C18/1844Multistep pretreatment with use of organic or inorganic compounds other than metals, first
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C18/00Chemical 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
    • C23C18/16Chemical 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
    • C23C18/31Coating with metals
    • C23C18/32Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C18/00Chemical 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
    • C23C18/16Chemical 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
    • C23C18/31Coating with metals
    • C23C18/42Coating with noble metals
    • C23C18/44Coating with noble metals using reducing agents

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Particle Formation And Scattering Control In Inkjet Printers (AREA)
  • Chemically Coating (AREA)

Abstract

The invention discloses a surface treatment method of a printing nozzle, which comprises the following steps: plating a base metal layer on the surface of the printing nozzle; and plating a hydrophobic metal layer on the surface of the base metal layer. According to the invention, the base metal layer is plated on the printing nozzle firstly, and then the hydrophobic metal layer is plated on the base metal layer, so that the problem that ink is easily hung on the nozzle or the nozzle is easily blocked in the printing process of the existing printing nozzle is effectively solved.

Description

Surface treatment method of printing nozzle
Technical Field
The invention relates to the technical field of printing equipment, in particular to the technical field of surface treatment of printing nozzles, and specifically relates to a surface treatment method of a printing nozzle.
Background
The display technology has completed a qualitative leap from the early Cathode Ray Tube (CRT) to the Liquid Crystal Display (LCD) and Plasma Display Panel (PDP) in the middle of the 80 th year of the 20 th century to the current mainstream OLED/QLED display. With the development of nanomaterial technology and device technology, in OLED/QLED display technology, low-cost, large-area printing preparation on a rigid/flexible substrate by inkjet printing is the most favored technology.
In the existing ink-jet printing equipment, printing nozzles are uniformly customized, but there are many printing inks, such as polymer ink, quantum dot ink, metal oxide semiconductor ink, and the like, and the viscosity, surface tension, fluidity, and volatility of each ink are different, so that some ink is sometimes caught on the surface of a printing nozzle during printing, and the nozzle is blocked due to incomplete wiping, thereby affecting the printing effect.
The current solution mainly has two directions, one is to adjust the property of ink to improve the printing characteristic, but this often results in low performance of the manufactured device, and the other is to find the printing equipment manufacturer to customize the nozzle for the ink, but this is too high cost.
Disclosure of Invention
The invention mainly aims to provide a surface treatment method of a printing nozzle, aiming at solving the problem that ink is easy to block the nozzle to influence the printing process.
In order to achieve the above object, the present invention provides a surface treatment method for a printing nozzle, comprising the following steps:
plating a base metal layer on the surface of the printing nozzle;
and plating a hydrophobic metal layer on the surface of the base metal layer.
Optionally, the metal of the base metal layer is nickel; and/or the metal of the hydrophobic metal layer is gold.
Optionally, the step of plating a base metal layer on the surface of the print head includes:
and soaking the printing spray head in nickel plating solution to carry out chemical nickel plating so as to form the base metal layer on the surface of the printing spray head.
Optionally, the nickel plating solution comprises nickel sulfate, sodium acetate, sodium hypophosphite, citric acid, ammonia water and deionized water, the concentration of the nickel sulfate, the concentration of the sodium acetate, the concentration of the sodium hypophosphite and the concentration of the citric acid in the nickel plating solution are respectively 15-40 g/L, 5-30 g/L, 3-35 g/L and 2-26 g/L, and the pH value of the nickel plating solution is 8.5-10.5; and/or the printing nozzle is soaked in the nickel plating solution for chemical nickel plating at the nickel plating temperature of 40-100 ℃ for 3-40 min.
Optionally, the step of plating a hydrophobic metal layer on the surface of the base metal layer includes: soaking the printing nozzle in a gold plating solution to carry out chemical gold plating;
the gold plating solution comprises gold sodium sulfite, monopotassium phosphate, anhydrous sodium sulfate and deionized water, the concentrations of the gold sodium sulfite, monopotassium phosphate and anhydrous sodium sulfate in the gold plating solution are respectively 2-12 g/L, 5-35 g/L, 4-28 g/L and 2-26 g/L, and the pH value of the gold plating solution is 6.5-7.5; and/or the printing nozzle is soaked in the gold plating solution for chemical gold plating at the gold plating temperature of 40-60 ℃ for 1-30 min.
Optionally, the gold plating solution further comprises polyethylene glycol, and the concentration of the polyethylene glycol in the gold plating solution is 0.1-2.0 g/L; and/or the presence of a gas in the gas,
the gold plating solution also comprises polyacrylamide, and the concentration of the polyacrylamide in the gold plating solution is 0.1-2.0 g/L.
Optionally, before the step of plating the base metal layer on the surface of the print head, the method further includes:
and preprocessing the printing nozzle, wherein the preprocessing comprises coarsening processing, sensitizing processing and activating processing.
Optionally, the printing head is pretreated, and the pretreatment includes a roughening treatment, a sensitizing treatment and an activating treatment, where the roughening treatment includes: soaking the printing nozzle in a roughening solution to carry out roughening treatment;
wherein, the coarsening liquid comprises mixed liquid of hydrofluoric acid and deionized water and nitric acid.
Optionally, the volume ratio of the hydrofluoric acid to the deionized water is 1: 1-1: 9, and the volume of the nitric acid is 0.1-1% of the volume of the mixed solution; and/or the coarsening temperature of the printing spray head is 20-30 ℃ when the printing spray head is soaked in the coarsening liquid for coarsening treatment, and the coarsening time is 10-30 min.
Optionally, the printing head is pretreated, and the pretreatment includes a roughening treatment, a sensitizing treatment and an activating treatment, and the sensitizing treatment includes: soaking the printing nozzle in a sensitizing solution for sensitizing treatment;
wherein the sensitizing solution comprises stannous chloride, hydrochloric acid and deionized water.
Optionally, the concentration of the stannous chloride and the concentration of the hydrochloric acid in the sensitizing solution are respectively 5-20 g/L and 6-22 mL/L; and/or the printing nozzle is soaked in the sensitizing solution for sensitizing treatment at the sensitizing temperature of 20-60 ℃ for 2-20 min.
Optionally, the printing head is pretreated, and the pretreatment includes a roughening treatment, a sensitizing treatment, and an activation treatment, where the activation treatment includes: soaking the printing nozzle in an activating solution for activating treatment;
wherein the activating solution comprises an aqueous solution of silver nitrate.
Optionally, the concentration of silver nitrate in the silver nitrate aqueous solution is 0.5-8.5 g/L; and/or the printing spray head is soaked in the activating solution for activation treatment, the activation temperature is 20-60 ℃, and the activation time is 5-25 min.
Optionally, after the step of plating the hydrophobic metal layer on the surface of the base metal layer, the method further includes: and carrying out hydrophobic surface treatment on the hydrophobic metal layer.
Optionally, the step of performing hydrophobic surface treatment on the hydrophobic metal layer includes:
cleaning the printing nozzle plated with the hydrophobic metal layer, and then placing the printing nozzle into hydroxylation treatment liquid for hydroxylation treatment;
cleaning and drying the hydroxylated printing nozzle, putting the printing nozzle into a silane coupling agent, and performing hydrophobic treatment under an ultrasonic condition to finish the hydrophobic surface treatment of the printing nozzle;
the hydroxylation treatment liquid comprises concentrated sulfuric acid and hydrogen peroxide, and the volume ratio of the concentrated sulfuric acid to the hydrogen peroxide is 7: (2-4), wherein the treatment temperature of the hydroxylation treatment is 75-85 ℃, and the treatment time is 3-4 h; and/or the presence of a gas in the gas,
the silane coupling agent comprises tetrahydrofuran and octadecyltrichlorosilane, and the volume ratio of the tetrahydrofuran to the octadecyltrichlorosilane is 30 mL: (1-15) mu L, wherein the treatment temperature of the hydrophobic treatment is 20-30 ℃, and the treatment time is 20-60 min.
According to the technical scheme provided by the invention, a base metal layer is plated on the printing spray head, then a hydrophobic metal layer is plated on the base metal layer, and then the hydrophobic metal layer is subjected to further hydrophobic surface treatment; meanwhile, the hydrophobic metal layer has certain hydrophobicity, so that ink can be prevented from hanging on the printing nozzle, and the nozzle can be prevented from being blocked.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other related drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a schematic flow chart illustrating a surface treatment method of a print head according to an embodiment of the present invention;
FIG. 2 is a schematic flow chart of step S10 in FIG. 1;
fig. 3 is a schematic flowchart of step S40 in fig. 1.
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
It should be noted that if the description of "first", "second", etc. is provided in the embodiment of the present invention, the description of "first", "second", etc. is only for descriptive purposes and is not to be construed as indicating or implying relative importance or implicitly indicating the number of indicated technical features. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In addition, the meaning of "and/or" appearing throughout includes three juxtapositions, exemplified by "A and/or B" including either A or B or both A and B. In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention.
In the existing ink-jet printing equipment, printing nozzles are uniformly customized, but there are many printing inks, such as polymer ink, quantum dot ink, metal oxide semiconductor ink, and the like, and the viscosity, surface tension, fluidity, and volatility of each ink are different, so that some ink is sometimes caught on the surface of a printing nozzle during printing, and the nozzle is blocked due to incomplete wiping, thereby affecting the printing effect. The current solution mainly has two directions, one is to adjust the property of ink to improve the printing characteristic, but this often results in low performance of the manufactured device, and the other is to find the printing equipment manufacturer to customize the nozzle for the ink, but this is too high cost.
In view of this, the present invention provides a surface treatment method for a print head, which is used to perform a sufficient surface treatment on a print spray so that ink is not easy to remain on the surface of the print head or block the print head, and fig. 1 shows an embodiment of the surface treatment method for a print head according to the present invention. Referring to fig. 1, in the present embodiment, the method for processing the surface of the print head includes the following steps:
step S20, plating a base metal layer on the surface of the printing nozzle;
the purpose of plating the substrate metal layer on the surface of the printing nozzle is mainly to prepare for the subsequent plating of the hydrophobic metal layer, so that the obtained hydrophobic metal layer is more uniform, and the bonding force between the hydrophobic metal layer and the printing nozzle is better. Specifically, the base metal layer may be a tin plating layer, a nickel plating layer, and the like, and in this embodiment, the nickel plating layer is preferred, so that the adhesion force on the surface of the printing nozzle (usually, a silicon-based material) is better, and the bonding force is stronger, while the nickel plating layer disposed on the surface of the printing nozzle may be formed by vacuum plating or chemical plating, and in this embodiment, the chemical nickel plating is used, so that the process is simple and the equipment cost is low.
Chemical nickel plating is generally performed by using a solution containing a main salt such as nickel sulfate or nickel acetate as a plating solution, and using a reducing agent such as hypophosphite, sodium borohydride, borane, or hydrazine to reduce nickel atoms by an oxidation-reduction reaction and deposit the nickel atoms on the surface of a plating object to form a plating layer. Preferably, in this embodiment, the electroless nickel plating includes: and soaking the printing spray head in a nickel plating solution to carry out chemical nickel plating, wherein the nickel plating solution comprises nickel sulfate, sodium acetate, sodium hypophosphite, citric acid, ammonia water and deionized water, the concentration of the nickel sulfate, the sodium acetate, the sodium hypophosphite and the citric acid in the nickel plating solution is preferably 15-40 g/L, 5-30 g/L, 3-35 g/L and 2-26 g/L, and the pH value of the nickel plating solution is 8.5-10.5. When the nickel plating solution is prepared, a small amount of alkaline substances, such as sodium bicarbonate, ammonia water and the like, can be added to adjust the pH value of the nickel plating solution to 8.5-10.5, and in the embodiment, the ammonia water is selected for adjustment.
Further, the nickel plating temperature of the printing spray head is 40-100 ℃ when the printing spray head is soaked in the nickel plating solution for chemical nickel plating, and the nickel plating time is 3-40 min. Under the conditions of the nickel plating solution, the nickel plating temperature and the nickel plating time, a bright, uniform and good-binding-force nickel plating layer can be stably and efficiently plated on the surface of the printing spray head.
Preferably, in order to improve the coverage and the bonding force of the base metal layer on the surface of the print head, before plating the base metal layer, a process of performing a pretreatment on the surface of the print head is further included, and referring to fig. 1 in detail, before step S20, the method further includes:
and step S10, preprocessing the printing nozzle, wherein the preprocessing comprises coarsening processing, sensitizing processing and activating processing.
In specific implementation, the order of the roughening treatment, the sensitizing treatment, and the activating treatment may not be limited, and in this embodiment, the roughening treatment, the sensitizing treatment, and the activating treatment are preferably performed on the print head in sequence. The coarsening treatment has the effects of enabling the surface of the printing spray head to be coarsened, enabling the adhesion force of the plated substance to be enhanced and not to fall off easily, and being beneficial to depositing certain chemical substances on the surface of the plated part after coarsening and improving the adhesion force of the plating layer. In the technical solution of the present invention, any process that can perform a roughening effect on the surface of the print head may be selected, for example, mechanical abrasion or chemical corrosion, and in this embodiment, a method of chemical corrosion is taken as an example, and the roughening treatment includes: and soaking the printing nozzle in roughening liquid for roughening treatment, wherein the roughening liquid comprises mixed liquid of hydrofluoric acid and deionized water and nitric acid, more preferably, the volume ratio of the hydrofluoric acid to the deionized water is 1: 1-1: 9, and the volume of the nitric acid is 0.1-1% of the volume of the mixed liquid. When the roughening solution is prepared, the hydrofluoric acid and the deionized water are mixed in proportion to prepare a mixed solution, and then the nitric acid is added into the mixed solution to be mixed, so that the roughening solution is obtained correspondingly.
The concentration of the hydrofluoric acid and the nitric acid added to the roughening solution is not limited, and a product with a common concentration specification is selected, and preferably, in this embodiment, the mass concentration of the hydrofluoric acid is 35 to 45%, and the mass concentration of the nitric acid is 65 to 68%. Furthermore, the coarsening temperature of the printing nozzle when the printing nozzle is soaked in the coarsening liquid for coarsening is 20-30 ℃, and the coarsening time is 10-30 min, so that the coarsening treatment of the printing nozzle can be completed, and a coarse structure is formed on the surface of the printing nozzle.
The sensitization treatment has the effect of forming tiny condensation nuclei on the surface of the printing spray head, so that plated substances are favorably precipitated on the surface of the printing spray head, and the chemical plating reaction is more sensitive. In the technical scheme of the invention, any process can be selected as long as the process can sensitize the surface of the printing spray head, a certain reagent is usually adopted for soaking, and the selected reagent is generally a reagent which is easy to react with a subsequently used reagent. In this embodiment, the sensitization process includes: and soaking the printing nozzle in a sensitizing solution for sensitizing, wherein the sensitizing solution comprises stannous chloride, hydrochloric acid and deionized water, and more preferably, the concentration of the stannous chloride and the concentration of the hydrochloric acid in the sensitizing solution correspond to 5-20 g/L and 6-22 mL/L. When the sensitizing solution is prepared, the stannous chloride can be dissolved in the hydrochloric acid and then mixed with deionized water, or the stannous chloride can be dissolved in the deionized water and then mixed with the hydrochloric acid, or the stannous chloride and the hydrochloric acid are added into the deionized water together for dissolving and mixing, so long as the concentration of the stannous chloride and the concentration of the hydrochloric acid in the sensitizing solution meet the concentration range provided by the above.
Further, when the printing nozzle is soaked in the sensitizing solution for sensitizing treatment, the sensitizing temperature is 20-60 ℃, and the sensitizing time is 2-20 min, so that the sensitizing treatment on the printing nozzle can be completed, and the surface of the printing nozzle forms condensation nuclei.
The activation treatment has the function of converting the material from an inactive state to an active state, thereby being beneficial to improving the plating efficiency in the later period and improving the effect of subsequent chemical nickel plating. In the technical scheme of the present invention, any process that can sensitize the surface of the print head may be used, and in this embodiment, the print head is immersed in an activation solution to perform an activation treatment, where the activation solution includes an aqueous solution of silver nitrate. In the process of performing the activation treatment by using the silver nitrate aqueous solution, the concentration of the silver nitrate, the activation temperature, and the activation time all affect the deposition rate, the coverage rate of the nickel plating layer, the bonding force between the nickel plating layer and the surface of the printing head, and the like in the subsequent electroless nickel plating, and preferably, in this embodiment, the concentration of the silver nitrate in the silver nitrate aqueous solution is preferably 0.5 to 8.5g/L, and more preferably 5 g/L. Further, the activation temperature of the printing nozzle when being soaked in the activation solution for activation treatment is 20-60 ℃, the activation time is 5-25 min, and more preferably the activation temperature is 40 ℃ and the activation time is 15 min. In a preferred embodiment of the surface treatment method of the printing nozzle provided by the invention, the concentration of the silver nitrate is limited to 5g/L, the activation temperature is 40 ℃, the activation time is 15min, and the performance of the obtained nickel plating layer is optimal.
The pretreatment of coarsening, sensitization and activation is carried out on the printing nozzle in sequence, so that the subsequent nickel plating layer is easy to form, and the coverage rate of the nickel plating layer and the binding force between the nickel plating layer and the printing nozzle are improved. Preferably, during the pretreatment operation of the print head, between the roughening, sensitizing and activating steps, the treated print head generally needs to be cleaned to avoid pollution to the next treatment process, and the like, referring to fig. 2 specifically, in this embodiment, the step of pretreating the print head in step S10 specifically includes:
step S11, carrying out coarsening treatment on the printing nozzle after carrying out absolute ethyl alcohol ultrasonic cleaning, deionized water cleaning and deionized water ultrasonic cleaning in sequence;
step S12, carrying out deionized water washing and deionized water ultrasonic wave washing on the coarsened printing nozzle in sequence, and then carrying out sensitization treatment;
and step S13, carrying out deionized water cleaning on the sensitized printing nozzle, and then carrying out activation treatment to finish the pretreatment of the printing nozzle.
Before the coarsening treatment is carried out on the printing nozzle, firstly carrying out absolute ethyl alcohol ultrasonic cleaning, deionized water washing and deionized water ultrasonic cleaning on the printing nozzle to fully remove impurities such as oil stains on the surface of the printing nozzle, and then carrying out the coarsening treatment; after the coarsening treatment is finished, carrying out deionized water flushing and deionized water ultrasonic cleaning to completely remove the coarsening liquid remained on the surface of the printing nozzle, and then carrying out sensitization treatment; and after the sensitization treatment is finished, removing the sensitization liquid remained on the surface of the printing spray head by deionized water cleaning, and then carrying out the activation treatment, wherein the pretreatment of the printing spray head is finished after the activation treatment is finished. It should be noted that, when the printing nozzle after the sensitization treatment is cleaned by deionized water, the printing nozzle cannot be cleaned by ultrasonic wave or washed, and preferably is soaked in deionized water for a period of time, so that not only can the sensitizing solution remained on the printing nozzle be removed, but also stannous ions adsorbed on the surface of the printing nozzle cannot be separated.
Step S30, plating a hydrophobic metal layer on the surface of the base metal layer;
the purpose of plating the hydrophobic metal layer on the surface of the printing nozzle is to make the surface of the printing nozzle smooth, improve the hydrophobicity, and can be realized by adopting a gold plating layer or a silver plating layer, but considering that the hydrophobic gold plating layer is also required to have the characteristics of high stability, acid and alkali corrosion resistance, organic solvent corrosion resistance and difficult oxidation when being used as the outermost surface metal, the hydrophobic gold plating layer is preferably arranged on the surface of the substrate metal layer, and the gold itself has the hydrophobicity, so that the contact angle between the ink and the printing nozzle can be improved, the ink is difficult to hang on the surface of the printing nozzle, and the blockage of the printing nozzle is difficult to cause. Similarly, the gold plating layer disposed on the surface of the base metal layer may be vacuum plated or chemically plated, and the like, and in this embodiment, the gold plating method is adopted, so that the process is simple and the equipment cost is low.
The electroless gold plating method is a method of placing a plating object in a plating solution, reducing gold by an oxidation-reduction reaction, and depositing the gold on the surface of the plating object to form a plating layer, and any process capable of chemically plating nickel on the surface of the printing nozzle can be used in the technical scheme of the present invention. Preferably, in this embodiment, the electroless gold plating includes: and soaking the printing spray head in a gold plating solution for chemical gold plating, wherein the gold plating solution comprises gold sodium sulfite, monopotassium phosphate, anhydrous sodium sulfate and deionized water, more preferably, the concentrations of the gold sodium sulfite, monopotassium phosphate and anhydrous sodium sulfate in the gold plating solution are respectively 2-12 g/L, 5-35 g/L, 4-28 g/L and 2-26 g/L, and the pH value of the gold plating solution is 6.5-7.5. The gold plating solution is preferably a neutral solution, and more preferably the pH of the gold plating solution is 7.0.
Furthermore, polyethylene glycol can be added into the gold plating solution, and the concentration of the polyethylene glycol in the gold plating solution is 0.1-2.0 g/L. Or polyacrylamide is also added into the gold plating solution, and the concentration of the polyacrylamide in the gold plating solution is 0.1-2.0 g/L and 0.1-2.0 g/L. The gold plating solution can comprise the polyethylene glycol or the polyacrylamide or both the polyethylene glycol and the polyacrylamide besides the gold sulfite, the monopotassium phosphate and the anhydrous sodium sulfate, and can achieve the purpose of successfully forming a gold plating layer on the printing nozzle by an electroless gold plating process.
Furthermore, the printing nozzle is immersed in the gold plating solution for chemical gold plating at a gold plating temperature of 40-60 ℃ for 1-30 min. Under the conditions of the gold plating solution, the gold plating temperature and the gold plating time, a bright, uniform and good-binding-force gold plating layer can be stably and efficiently plated on the surface of the printing nozzle.
It should be noted that, in this embodiment, it is preferable that the base metal layer is a nickel plating layer, and the hydrophobic metal layer is a gold plating layer, so that the bonding force between the gold plating layer and the printing head can be significantly enhanced, and the hydrophobicity of the surface of the printing head can be improved, so that ink is not easily left or blocks the printing head. In other embodiments of the present invention, other metal materials capable of forming a smooth hydrophobic surface on the surface of the print head may be selected as the hydrophobic metal layer, and a metal material having a good adhesion on the surface of the silicon-based material and capable of improving the adhesion between the outer metal layer and the print head may be selected as the base metal layer, which will not be described in detail herein.
Preferably, in order to further improve the hydrophobicity of the nozzle, after the plating of the hydrophobic metal layer on the surface of the base metal layer, a process of performing a hydrophobic surface treatment on the hydrophobic metal layer is further included, and referring to fig. 1 in detail, the step S30 is further followed by:
and step S40, carrying out hydrophobic surface treatment on the hydrophobic metal layer.
Plating at the printing shower nozzle and establishing behind the hydrophobic metal layer, carry out again hydrophobic nature surface treatment's purpose is the hydrophobicity that further strengthens printing the shower nozzle, makes the ink more be difficult to remain on the surface of printing the shower nozzle, has avoided the hanging liquid condition, further reduces to cause the probability that prints the shower nozzle and block up, even make the ink remain in the shower nozzle always because shutting down for a long time, then the ink volatilizees and causes the nozzle to block up, also makes the nozzle resume normal unobstructed state very easily after doing the soaking treatment. In the technical scheme of the invention, a process which can play a role of hydrophobicity on the gold-plating layer can be used as the hydrophobic surface treatment process, for example, a contact angle between a printing spray head and ink is increased by a surface treatment reagent, or a hydrophobic layer is formed on the surface of the gold-plating layer, and the like. Preferably, in the present embodiment, referring to fig. 3, the hydrophobic surface treatment includes:
step S41, after cleaning the printing nozzle plated with the hydrophobic metal layer, placing the printing nozzle into hydroxylation treatment liquid for hydroxylation treatment;
and step S42, cleaning and drying the hydroxylated printing nozzle, putting the printing nozzle into a silane coupling agent, and performing hydrophobic treatment under an ultrasonic condition to finish the hydrophobic surface treatment of the printing nozzle.
After the hydrophobic metal layer is plated, cleaning the printing nozzle to remove residual dirt on the surface of the printing nozzle, for example, performing ultrasonic treatment on the printing nozzle by using ethanol as a cleaning solvent; and then carrying out hydroxylation treatment on the cleaned printing nozzle to enable hydroxyl to be attached to the surface of the printing nozzle, then carrying out deionized water washing, ethanol cleaning and ethanol ultrasonic treatment (the ultrasonic treatment time is not specifically limited, and is preferably 5-15 min in the embodiment), then drying (the drying temperature is not specifically limited, so as to quickly dry the residual solvent on the surface of the printing nozzle on the basis of not influencing the performance of the gold plating layer, in the embodiment, drying can be carried out at 75-85 ℃, finally carrying out hydrophobic surface treatment through a silane coupling agent, and carrying out hydroxylation and silane coupling agent treatment to enable the gold plating layer to have excellent hydrophobicity, so that the phenomenon that the gold plating layer is hung on the printing nozzle or blocks the printing nozzle is basically avoided.
Further, in this embodiment, the hydroxylation treatment liquid includes concentrated sulfuric acid and hydrogen peroxide, and a volume ratio of the concentrated sulfuric acid to the hydrogen peroxide is 7: (2-4), wherein the treatment temperature of the hydroxylation treatment is 75-85 ℃, and the treatment time is 3-4 h. Still further, the silane coupling agent includes tetrahydrofuran and octadecyltrichlorosilane, and the volume ratio of the tetrahydrofuran to the octadecyltrichlorosilane is 30 mL: (1-15) mu L, wherein the treatment temperature of the hydrophobic treatment is 20-30 ℃, and the treatment time is 20-60 min.
In the embodiment provided by the invention, the printing nozzle is fully pretreated, including coarsening, sensitizing and activating treatment, then the printing nozzle is chemically plated with nickel, the nickel plating layer is chemically plated with gold, and finally the gold plating layer is subjected to hydrophobic treatment, wherein the pretreatment of coarsening, sensitizing and activating is carried out on the printing nozzle, so that the nickel plating layer is easier to form, and the coverage rate of the nickel plating layer and the binding force between the printing nozzle and the printing nozzle are improved; the formation of the nickel plating layer can form an activation center in advance for the next step of chemical gold plating, so that the binding force between gold and a printing nozzle is improved, and the gold plating layer is not easy to fall off; furthermore, because gold itself has certain hydrophobicity, can prevent that the ink from hanging liquid on printing the shower nozzle, prevent that the nozzle from blockking up, and can further improve its hydrophobicity after doing the hydrophobicity processing on gold-plated layer, can prevent the ink hanging liquid condition on printing the shower nozzle better, can not influence the printing process, also can not block up the shower nozzle easily, even make the ink remain in the shower nozzle always because of shutting down for a long time, then the ink volatilizees and causes the nozzle to block up, also makes the nozzle reply normal unobstructed state after doing the soaking processing very easily.
The technical solutions of the present invention are further described in detail below with reference to specific examples and drawings, it should be understood that the following examples are merely illustrative of the present invention and are not intended to limit the present invention.
Example 1
(1) Putting the printing nozzle into a nickel plating solution for 2mm, chemically plating nickel for 3min at 90 ℃, cleaning with deionized water and drying after the nickel plating is finished, wherein the nickel plating solution is prepared by the following steps: dissolving nickel sulfate, sodium acetate, sodium hypophosphite and citric acid in deionized water to prepare 500mL of nickel plating solution with the nickel sulfate concentration of 25g/L, the sodium acetate concentration of 10g/L, the sodium hypophosphite concentration of 20g/L and the citric acid concentration of 10g/L, and then adding ammonia water to adjust the pH value to 10.0;
(2) putting the printing nozzle after nickel plating into a gold plating solution for 2mm, chemically plating gold for 10min at 50 ℃, cleaning with deionized water and drying after the gold plating is finished, wherein the preparation step of the gold plating solution is as follows: preparing 500mL of gold plating solution with the concentration of gold sodium sulfite being 2g/L, the concentration of monopotassium phosphate being 15g/L, the concentration of anhydrous sodium sulfate being 13g/L, the concentration of polyethylene glycol being 1.2g/L and the concentration of polyacrylamide being 0.8g/L by using gold sodium sulfite, monopotassium phosphate, anhydrous sodium sulfate, polyethylene glycol and polyacrylamide, wherein the pH value is 7.0;
(3) ultrasonically cleaning the gold-plated printing nozzle by using absolute ethyl alcohol, and removing residual dirt on the surface of the gold-plated printing nozzle; then putting the cleaned printing nozzle into a mixed solution of concentrated sulfuric acid and hydrogen peroxide (the volume ratio of the concentrated sulfuric acid to the hydrogen peroxide is 7:3), and carrying out hydroxylation treatment for 3.5h under the condition of 80 ℃ water bath; taking out the printing nozzle, washing with deionized water and ethanol, ultrasonic treating with anhydrous ethanol for 10min, and oven drying at 80 deg.C; and finally, placing the mixture into a prepared silane coupling agent (150mL of tetrahydrofuran and 20 mu L of octadecyl trichlorosilane), and ultrasonically shaking for 30min at 25 ℃ to finish the surface treatment of the printing nozzle.
The printing nozzle treated by the surface treatment method has no phenomenon that ink is hung on the surface of the nozzle, and the nozzle is not wiped cleanly or blocked in the printing process.
Example 2
(1) Firstly, carrying out absolute ethyl alcohol ultrasonic cleaning, deionized water washing and deionized water ultrasonic cleaning on a printing nozzle in sequence, then putting the printing nozzle into roughening liquid for 2mm, and treating the printing nozzle for 10min at 25 ℃, wherein the roughening liquid is prepared by the following steps: mixing hydrofluoric acid (the mass concentration of the hydrofluoric acid is 40%) and deionized water according to the volume ratio of 1:2 to form a mixed solution, and then adding nitric acid (the mass concentration of the nitric acid is 65%) accounting for 0.5% of the mass of the mixed solution to prepare 500mL of coarsening solution;
(2) and (3) sequentially carrying out deionized water washing and deionized water ultrasonic cleaning on the coarsened printing nozzle, then putting the printing nozzle into sensitizing solution for 2mm, and treating for 4min at 40 ℃, wherein the preparation step of the sensitizing solution is as follows: mixing stannous chloride, hydrochloric acid and deionized water to prepare 500mL of sensitizing solution with stannous chloride concentration of 15g/L and hydrochloric acid concentration of 10 mL/L;
(3) and (3) putting the sensitized printing nozzle into deionized water for washing and soaking for 2min, then putting the printing nozzle into an activating solution for 2mm, and treating for 15min at 40 ℃, wherein the activating solution is prepared by the following steps: dissolving silver nitrate in deionized water to prepare 500mL of activation solution with silver nitrate concentration of 5 g/L;
(4) placing the sensitized printing nozzle into a nickel plating solution for 2mm, chemically plating nickel for 3min at 90 ℃, cleaning with deionized water and drying after the nickel plating is finished, wherein the nickel plating solution is prepared by the following steps: dissolving nickel sulfate, sodium acetate, sodium hypophosphite and citric acid in deionized water to prepare 500mL of nickel plating solution with the nickel sulfate concentration of 25g/L, the sodium acetate concentration of 10g/L, the sodium hypophosphite concentration of 20g/L and the citric acid concentration of 10g/L, and then adding ammonia water to adjust the pH value to 10.0;
(5) putting the printing nozzle after nickel plating into a gold plating solution for 2mm, chemically plating gold for 10min at 50 ℃, cleaning with deionized water and drying after the gold plating is finished, wherein the preparation step of the gold plating solution is as follows: preparing 500mL of gold plating solution with the concentration of gold sodium sulfite being 2g/L, the concentration of monopotassium phosphate being 15g/L, the concentration of anhydrous sodium sulfate being 13g/L, the concentration of polyethylene glycol being 1.2g/L and the concentration of polyacrylamide being 0.8g/L by using gold sodium sulfite, monopotassium phosphate, anhydrous sodium sulfate, polyethylene glycol and polyacrylamide, wherein the pH value is 7.0;
(6) ultrasonically cleaning the gold-plated printing nozzle by using absolute ethyl alcohol, and removing residual dirt on the surface of the gold-plated printing nozzle; then putting the cleaned printing nozzle into a mixed solution of concentrated sulfuric acid and hydrogen peroxide (the volume ratio of the concentrated sulfuric acid to the hydrogen peroxide is 7:3), and carrying out hydroxylation treatment for 3.5h under the condition of 80 ℃ water bath; taking out the printing nozzle, washing with deionized water and ethanol, ultrasonic treating with anhydrous ethanol for 10min, and oven drying at 80 deg.C; and finally, placing the mixture into a prepared silane coupling agent (150mL of tetrahydrofuran and 20 mu L of octadecyl trichlorosilane), and ultrasonically shaking for 30min at 25 ℃ to finish the surface treatment of the printing nozzle.
The printing nozzle treated by the surface treatment method has no phenomenon that ink is hung on the surface of the nozzle, and the nozzle is not wiped cleanly or blocked in the printing process.
Example 3
(1) Firstly, carrying out absolute ethyl alcohol ultrasonic cleaning, deionized water washing and deionized water ultrasonic cleaning on a printing nozzle in sequence, then putting the printing nozzle into roughening liquid for 2mm, and treating the printing nozzle for 30min at 25 ℃, wherein the roughening liquid is prepared by the following steps: mixing hydrofluoric acid (the mass concentration of the hydrofluoric acid is 35%) and deionized water according to the volume ratio of 1:1 to form a mixed solution, and then adding nitric acid (the mass concentration of the nitric acid is 66%) accounting for 1% of the mixed solution to prepare 500mL of coarsening solution;
(2) and (3) sequentially carrying out deionized water washing and deionized water ultrasonic cleaning on the coarsened printing nozzle, then putting the printing nozzle into sensitizing solution for 2mm, and treating for 10min at 50 ℃, wherein the preparation steps of the sensitizing solution are as follows: mixing stannous chloride, hydrochloric acid and deionized water to prepare 500mL of sensitizing solution with the concentration of the stannous chloride being 10g/L and the concentration of the hydrochloric acid being 14 mL/L;
(3) and (3) putting the sensitized printing nozzle into deionized water for washing and soaking for 2min, then putting the printing nozzle into an activating solution for 2mm, and treating for 5min at 60 ℃, wherein the activating solution is prepared by the following steps: dissolving silver nitrate in deionized water to prepare 500mL of activation solution with the silver nitrate concentration of 7 g/L;
(4) placing the sensitized printing nozzle into a nickel plating solution for 2mm, chemically plating nickel for 5min at 100 ℃, cleaning with deionized water and drying after the nickel plating is finished, wherein the nickel plating solution is prepared by the following steps: dissolving nickel sulfate, sodium acetate, sodium hypophosphite and citric acid in deionized water to prepare 500mL of nickel plating solution with the nickel sulfate concentration of 30g/L, the sodium acetate concentration of 15g/L, the sodium hypophosphite concentration of 30g/L and the citric acid concentration of 5g/L, and then adding ammonia water to adjust the pH value to 10.5;
(5) putting the printing nozzle after nickel plating into a gold plating solution for 2mm, chemically plating gold for 15min at 45 ℃, cleaning with deionized water and drying after the gold plating is finished, wherein the preparation step of the gold plating solution is as follows: preparing 500mL of gold plating solution with the concentration of 5g/L gold sulfite sodium, 10g/L monopotassium phosphate, 8g/L anhydrous sodium sulfate, 1.5g/L polyethylene glycol and 1.2g/L polyacrylamide by using gold sulfite sodium, monopotassium phosphate, anhydrous sodium sulfate, polyethylene glycol and polyacrylamide, wherein the pH value is 6.5;
(6) ultrasonically cleaning the gold-plated printing nozzle by using absolute ethyl alcohol, and removing residual dirt on the surface of the gold-plated printing nozzle; then putting the cleaned printing nozzle into a mixed solution of concentrated sulfuric acid and hydrogen peroxide (the volume ratio of the concentrated sulfuric acid to the hydrogen peroxide is 7:2), and carrying out hydroxylation treatment for 4 hours under the condition of a water bath at 75 ℃; taking out the printing nozzle, washing with deionized water and ethanol, ultrasonic treating with anhydrous ethanol for 10min, and oven drying at 80 deg.C; and finally, placing the mixture into a prepared silane coupling agent (150mL of tetrahydrofuran and 5 mu L of octadecyl trichlorosilane), and carrying out ultrasonic oscillation for 40min at the temperature of 20 ℃, thus finishing the surface treatment of the printing nozzle.
The printing nozzle treated by the surface treatment method has no phenomenon that ink is hung on the surface of the nozzle, and the nozzle is not wiped cleanly or blocked in the printing process.
Example 4
(1) Firstly, carrying out absolute ethyl alcohol ultrasonic cleaning, deionized water washing and deionized water ultrasonic cleaning on a printing nozzle in sequence, then putting the printing nozzle into roughening liquid for 2mm, and treating the printing nozzle for 15min at 20 ℃, wherein the roughening liquid is prepared by the following steps: mixing hydrofluoric acid (the mass concentration of the hydrofluoric acid is 45%) and deionized water according to the volume ratio of 1:4 to form a mixed solution, and then adding nitric acid (the mass concentration of the nitric acid is 67%) accounting for 0.8% of the mass of the mixed solution to prepare 500mL of coarsening solution;
(2) and (3) sequentially carrying out deionized water washing and deionized water ultrasonic cleaning on the coarsened printing nozzle, then putting the printing nozzle into sensitizing solution for 2mm, and treating for 2min at 30 ℃, wherein the preparation step of the sensitizing solution is as follows: mixing stannous chloride, hydrochloric acid and deionized water to prepare 500mL of sensitizing solution with the concentration of the stannous chloride being 20g/L and the concentration of the hydrochloric acid being 18 mL/L;
(3) and (3) putting the sensitized printing nozzle into deionized water for washing and soaking for 2min, then putting the printing nozzle into an activating solution for 2mm, and treating for 10min at 50 ℃, wherein the activating solution is prepared by the following steps: dissolving silver nitrate in deionized water to prepare 500mL of activation solution with the silver nitrate concentration of 8.5 g/L;
(4) placing the sensitized printing nozzle into a nickel plating solution for 2mm, chemically plating nickel for 25min at 60 ℃, cleaning with deionized water and drying after the nickel plating is finished, wherein the nickel plating solution is prepared by the following steps: dissolving nickel sulfate, sodium acetate, sodium hypophosphite and citric acid in deionized water to prepare 500mL of nickel plating solution with the nickel sulfate concentration of 40g/L, the sodium acetate concentration of 20g/L, the sodium hypophosphite concentration of 12g/L and the citric acid concentration of 2g/L, and then adding ammonia water to adjust the pH value to 9.0;
(5) putting the printing nozzle after nickel plating into a gold plating solution for 2mm, chemically plating gold for 22min at 40 ℃, cleaning with deionized water and drying after the gold plating is finished, wherein the preparation step of the gold plating solution is as follows: preparing 500mL of gold plating solution with gold sodium sulfite concentration of 8g/L, monopotassium phosphate concentration of 5g/L, anhydrous sodium sulfate concentration of 4g/L, polyethylene glycol concentration of 1.8g/L and polyacrylamide concentration of 2.0g/L by using gold sodium sulfite, monopotassium phosphate, anhydrous sodium sulfate, polyethylene glycol and polyacrylamide, wherein the pH value is 7.5;
(6) ultrasonically cleaning the gold-plated printing nozzle by using absolute ethyl alcohol, and removing residual dirt on the surface of the gold-plated printing nozzle; then putting the cleaned printing nozzle into a mixed solution of concentrated sulfuric acid and hydrogen peroxide (the volume ratio of the concentrated sulfuric acid to the hydrogen peroxide is 7:4), and carrying out hydroxylation treatment for 3h under the condition of a water bath at 85 ℃; taking out the printing nozzle, washing with deionized water and ethanol, ultrasonic treating with anhydrous ethanol for 10min, and oven drying at 80 deg.C; and finally, placing the mixture into a prepared silane coupling agent (150mL of tetrahydrofuran and 40 mu L of octadecyl trichlorosilane), and ultrasonically shaking for 20min at the temperature of 30 ℃ to finish the surface treatment of the printing spray head.
The printing nozzle treated by the surface treatment method has no phenomenon that ink is hung on the surface of the nozzle, and the nozzle is not wiped cleanly or blocked in the printing process.
Example 5
(1) Firstly, carrying out absolute ethyl alcohol ultrasonic cleaning, deionized water washing and deionized water ultrasonic cleaning on a printing nozzle in sequence, then putting the printing nozzle into roughening liquid for 2mm, and treating the printing nozzle for 20min at 30 ℃, wherein the roughening liquid is prepared by the following steps: mixing hydrofluoric acid (the mass concentration of the hydrofluoric acid is 40%) and deionized water according to the volume ratio of 1:6 to form a mixed solution, and then adding nitric acid (the mass concentration of the nitric acid is 68%) accounting for 0.4% of the mass of the mixed solution to prepare 500mL of coarsening solution;
(2) and (3) sequentially carrying out deionized water washing and deionized water ultrasonic cleaning on the coarsened printing nozzle, then putting the printing nozzle into sensitizing solution for 2mm, and treating for 15min at 20 ℃, wherein the preparation step of the sensitizing solution is as follows: mixing stannous chloride, hydrochloric acid and deionized water to prepare 500mL of sensitizing solution with the concentration of the stannous chloride being 5g/L and the concentration of the hydrochloric acid being 22 mL/L;
(3) and (3) putting the sensitized printing nozzle into deionized water for washing and soaking for 2min, then putting the printing nozzle into an activating solution for 2mm, and treating for 20min at 20 ℃, wherein the activating solution is prepared by the following steps: dissolving silver nitrate in deionized water to prepare 500mL of activation solution with silver nitrate concentration of 2 g/L;
(4) placing the sensitized printing nozzle into a nickel plating solution for 2mm, chemically plating nickel for 40min at 40 ℃, cleaning with deionized water and drying after the nickel plating is finished, wherein the nickel plating solution is prepared by the following steps: dissolving nickel sulfate, sodium acetate, sodium hypophosphite and citric acid in deionized water to prepare 500mL of nickel plating solution with the nickel sulfate concentration of 15g/L, the sodium acetate concentration of 30g/L, the sodium hypophosphite concentration of 35g/L and the citric acid concentration of 18g/L, and then adding ammonia water to adjust the pH value to 8.0;
(5) putting the printing nozzle after nickel plating into a gold plating solution for 2mm, chemically plating gold for 30min at 55 ℃, cleaning with deionized water and drying after the gold plating is finished, wherein the preparation step of the gold plating solution is as follows: preparing 500mL of gold plating solution with the concentration of 10g/L gold sulfite sodium, 20g/L monopotassium phosphate, 20g/L anhydrous sodium sulfate, 0.5g/L polyethylene glycol and 0.5g/L polyacrylamide, wherein the pH value is 7.0;
(6) ultrasonically cleaning the gold-plated printing nozzle by using absolute ethyl alcohol, and removing residual dirt on the surface of the gold-plated printing nozzle; then putting the cleaned printing nozzle into a mixed solution of concentrated sulfuric acid and hydrogen peroxide (the volume ratio of the concentrated sulfuric acid to the hydrogen peroxide is 7:3), and carrying out hydroxylation treatment for 3.5h under the condition of 80 ℃ water bath; taking out the printing nozzle, washing with deionized water and ethanol, ultrasonic treating with anhydrous ethanol for 10min, and oven drying at 80 deg.C; and finally, placing the mixture into a prepared silane coupling agent (150mL of tetrahydrofuran and 60 mu L of octadecyl trichlorosilane), and ultrasonically shaking for 50min at 25 ℃ to finish the surface treatment of the printing spray head.
The printing nozzle treated by the surface treatment method has no phenomenon that ink is hung on the surface of the nozzle, and the nozzle is not wiped cleanly or blocked in the printing process.
Example 6
(1) Firstly, carrying out absolute ethyl alcohol ultrasonic cleaning, deionized water washing and deionized water ultrasonic cleaning on a printing nozzle in sequence, then putting the printing nozzle into roughening liquid for 2mm, and treating the printing nozzle for 25min at 25 ℃, wherein the roughening liquid is prepared by the following steps: mixing hydrofluoric acid (the mass concentration of the hydrofluoric acid is 40%) and deionized water according to the volume ratio of 1:9 to form a mixed solution, and then adding nitric acid (the mass concentration of the nitric acid is 65%) accounting for 0.1% of the mass of the mixed solution to prepare 500mL of coarsening solution;
(2) and (3) sequentially carrying out deionized water washing and deionized water ultrasonic cleaning on the coarsened printing nozzle, then putting the printing nozzle into sensitizing solution for 2mm, and treating for 20min at 60 ℃, wherein the preparation step of the sensitizing solution is as follows: mixing stannous chloride, hydrochloric acid and deionized water to prepare 500mL of sensitizing solution with the concentration of the stannous chloride being 18g/L and the concentration of the hydrochloric acid being 6 mL/L;
(3) and (3) putting the sensitized printing nozzle into deionized water for washing and soaking for 2min, then putting the printing nozzle into an activating solution for 2mm, and treating for 25min at 30 ℃, wherein the activating solution is prepared by the following steps: dissolving silver nitrate in deionized water to prepare 500mL of activation solution with silver nitrate concentration of 0.5 g/L;
(4) placing the sensitized printing nozzle into a nickel plating solution for 2mm, chemically plating nickel for 10min at 75 ℃, cleaning with deionized water and drying after the nickel plating is finished, wherein the nickel plating solution is prepared by the following steps: dissolving nickel sulfate, sodium acetate, sodium hypophosphite and citric acid in deionized water to prepare 500mL of nickel plating solution with the nickel sulfate concentration of 35g/L, the sodium acetate concentration of 5g/L, the sodium hypophosphite concentration of 3g/L and the citric acid concentration of 26g/L, and then adding ammonia water to adjust the pH value to 8.5;
(5) putting the printing nozzle after nickel plating into a gold plating solution for 2mm, chemically plating gold for 1min at 60 ℃, cleaning with deionized water and drying after the gold plating is finished, wherein the preparation step of the gold plating solution is as follows: preparing 500mL of gold plating solution with the concentration of gold sodium sulfite being 12g/L, the concentration of monopotassium phosphate being 35g/L, the concentration of anhydrous sodium sulfate being 28g/L, the concentration of polyethylene glycol being 0.1g/L and the concentration of polyacrylamide being 0.1g/L by using gold sodium sulfite, monopotassium phosphate, anhydrous sodium sulfate, polyethylene glycol and polyacrylamide, wherein the pH value is 7.0;
(6) ultrasonically cleaning the gold-plated printing nozzle by using absolute ethyl alcohol, and removing residual dirt on the surface of the gold-plated printing nozzle; then putting the cleaned printing nozzle into a mixed solution of concentrated sulfuric acid and hydrogen peroxide (the volume ratio of the concentrated sulfuric acid to the hydrogen peroxide is 7:3), and carrying out hydroxylation treatment for 3.5h under the condition of 80 ℃ water bath; taking out the printing nozzle, washing with deionized water and ethanol, ultrasonic treating with anhydrous ethanol for 10min, and oven drying at 80 deg.C; and finally, placing the mixture into a prepared silane coupling agent (150mL of tetrahydrofuran and 75 mu L of octadecyl trichlorosilane), and ultrasonically shaking for 60min at 25 ℃ to finish the surface treatment of the printing nozzle.
The printing nozzle treated by the surface treatment method has no phenomenon that ink is hung on the surface of the nozzle, and the nozzle is not wiped cleanly or blocked in the printing process.
Example 7
The procedure was the same as in example 2, except that the gold plating solution of step (5) did not contain polyethylene glycol (other components and corresponding concentrations in the gold plating solution were kept constant).
The printing nozzle treated by the surface treatment method has no phenomenon that ink is hung on the surface of the nozzle, and the nozzle is not wiped cleanly or blocked in the printing process.
Example 8
The procedure was the same as in example 2, except that the gold plating solution of step (5) did not contain polyacrylamide (other components and corresponding concentrations in the gold plating solution remained the same).
The printing nozzle treated by the surface treatment method has no phenomenon that ink is hung on the surface of the nozzle, and the nozzle is not wiped cleanly or blocked in the printing process.
The above is only a preferred embodiment of the present invention, and it is not intended to limit the scope of the invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention shall be included in the scope of the present invention.

Claims (14)

1. A surface treatment method of a printing nozzle is characterized by comprising the following steps:
plating a base metal layer on the surface of the printing nozzle;
plating a hydrophobic metal layer on the surface of the substrate metal layer;
the printing nozzle is made of a silicon-based material;
wherein, after the step of plating the hydrophobic metal layer on the surface of the base metal layer, the method further comprises the following steps: carrying out hydrophobic surface treatment on the hydrophobic metal layer;
the step of subjecting the hydrophobic metal layer to hydrophobic surface treatment includes:
cleaning the printing nozzle plated with the hydrophobic metal layer, and then placing the printing nozzle into hydroxylation treatment liquid for hydroxylation treatment;
cleaning and drying the hydroxylated printing nozzle, putting the printing nozzle into a silane coupling agent, and performing hydrophobic treatment under an ultrasonic condition to finish the hydrophobic surface treatment of the printing nozzle;
the hydroxylation treatment liquid comprises concentrated sulfuric acid and hydrogen peroxide, and the volume ratio of the concentrated sulfuric acid to the hydrogen peroxide is 7: (2-4), wherein the treatment temperature of the hydroxylation treatment is 75-85 ℃, and the treatment time is 3-4 h.
2. The surface treatment method of a printing nozzle as defined in claim 1, wherein the metal of the base metal layer is nickel; and/or the metal of the hydrophobic metal layer is gold.
3. The surface treatment method of a print head according to claim 1, wherein the step of plating a base metal layer on the print head surface comprises:
and soaking the printing spray head in nickel plating solution to carry out chemical nickel plating so as to form the base metal layer on the surface of the printing spray head.
4. The surface treatment method of the printing nozzle according to claim 3, wherein the nickel plating solution comprises nickel sulfate, sodium acetate, sodium hypophosphite, citric acid, ammonia water and deionized water, the concentrations of the nickel sulfate, the sodium acetate, the sodium hypophosphite and the citric acid in the nickel plating solution are respectively 15-40 g/L, 5-30 g/L, 3-35 g/L and 2-26 g/L, and the pH value of the nickel plating solution is 8.5-10.5; and/or the printing nozzle is soaked in the nickel plating solution for chemical nickel plating at the nickel plating temperature of 40-100 ℃ for 3-40 min.
5. The surface treatment method of a print head as claimed in claim 1, wherein the step of plating a hydrophobic metal layer on the surface of the base metal layer comprises: soaking the printing nozzle in a gold plating solution to carry out chemical gold plating;
the gold plating solution comprises gold sodium sulfite, monopotassium phosphate, anhydrous sodium sulfate and deionized water, the concentrations of the gold sodium sulfite, monopotassium phosphate and anhydrous sodium sulfate in the gold plating solution are respectively 2-12 g/L, 5-35 g/L and 4-28 g/L, and the pH value of the gold plating solution is 6.5-7.5; and/or the printing nozzle is soaked in the gold plating solution for chemical gold plating at the gold plating temperature of 40-60 ℃ for 1-30 min.
6. The surface treatment method of a printing nozzle according to claim 5, wherein the gold plating solution further comprises polyethylene glycol, and the concentration of the polyethylene glycol in the gold plating solution is 0.1-2.0 g/L; and/or the presence of a gas in the gas,
the gold plating solution also comprises polyacrylamide, and the concentration of the polyacrylamide in the gold plating solution is 0.1-2.0 g/L.
7. The surface treatment method of a print head according to claim 1, wherein before the step of plating the base metal layer on the print head surface, the method further comprises:
and preprocessing the printing nozzle, wherein the preprocessing comprises coarsening processing, sensitizing processing and activating processing.
8. The surface treatment method of a printing head according to claim 7, wherein the roughening treatment comprises: soaking the printing nozzle in a roughening solution to carry out roughening treatment;
wherein, the coarsening liquid comprises mixed liquid of hydrofluoric acid and deionized water and nitric acid.
9. The surface treatment method of the printing nozzle according to claim 8, wherein the volume ratio of the hydrofluoric acid to the deionized water is 1:1 to 1:9, and the volume of the nitric acid is 0.1% to 1% of the volume of the mixed solution; and/or the presence of a gas in the gas,
the coarsening temperature of the printing nozzle when the printing nozzle is soaked in the coarsening liquid for coarsening treatment is 20-30 ℃, and the coarsening time is 10-30 min.
10. The surface treatment method of a print head according to claim 7, wherein the print head is subjected to pretreatment including a roughening treatment, a sensitizing treatment and an activating treatment, and the sensitizing treatment includes: soaking the printing nozzle in a sensitizing solution for sensitizing treatment;
wherein the sensitizing solution comprises stannous chloride, hydrochloric acid and deionized water.
11. The surface treatment method of the printing nozzle as claimed in claim 10, wherein the concentration of the stannous chloride and the concentration of the hydrochloric acid in the sensitizing solution are 5-20 g/L and 6-22 mL/L respectively; and/or the presence of a gas in the gas,
the printing nozzle is soaked in the sensitizing solution for sensitizing treatment at a sensitizing temperature of 20-60 ℃ for 2-20 min.
12. The surface treatment method of a print head according to claim 7, wherein the print head is subjected to a pretreatment including a roughening treatment, a sensitizing treatment, and an activation treatment, and the activation treatment includes: soaking the printing nozzle in an activating solution for activating treatment;
wherein the activating solution comprises an aqueous solution of silver nitrate.
13. The surface treatment method of a print head according to claim 12, wherein the concentration of silver nitrate in the aqueous solution of silver nitrate is 0.5 to 8.5 g/L; and/or the presence of a gas in the gas,
the printing nozzle is soaked in the activating solution for activation treatment, the activation temperature is 20-60 ℃, and the activation time is 5-25 min.
14. The surface treatment method of a printing head according to claim 1, wherein the silane coupling agent comprises tetrahydrofuran and octadecyltrichlorosilane, and the volume ratio of the tetrahydrofuran to the octadecyltrichlorosilane is 30 mL: (1-15) mu L, wherein the treatment temperature of the hydrophobic treatment is 20-30 ℃, and the treatment time is 20-60 min.
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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06177450A (en) * 1992-12-04 1994-06-24 Fuji Electric Co Ltd Piezoelectric element and method of forming electrode thereof
CN1438076A (en) * 2002-02-15 2003-08-27 佳能株式会社 Waterproof member and method of manufacturing ink nozzle
CN1966765A (en) * 2005-11-17 2007-05-23 中国科学院金属研究所 Activation method for chemical plating of non-metallic material and chemical plating therefor
CN101010198A (en) * 2004-07-15 2007-08-01 株式会社理光 Liquid discharging head and method for manufacture thereof, image forming device, nozzzle member of liquid discharging head, method for forming ink-repellent film, liquid discharging head, cartridge,
CN101743210A (en) * 2007-04-18 2010-06-16 恩索恩公司 Metal surface enhanced
CN103242063A (en) * 2013-05-10 2013-08-14 济南大学 Preparation method of piezoelectric ceramic surface electrode
CN103981547A (en) * 2014-05-05 2014-08-13 深圳清华大学研究院 Preparation method for super-hydrophobic metal surface

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06177450A (en) * 1992-12-04 1994-06-24 Fuji Electric Co Ltd Piezoelectric element and method of forming electrode thereof
CN1438076A (en) * 2002-02-15 2003-08-27 佳能株式会社 Waterproof member and method of manufacturing ink nozzle
CN101010198A (en) * 2004-07-15 2007-08-01 株式会社理光 Liquid discharging head and method for manufacture thereof, image forming device, nozzzle member of liquid discharging head, method for forming ink-repellent film, liquid discharging head, cartridge,
CN1966765A (en) * 2005-11-17 2007-05-23 中国科学院金属研究所 Activation method for chemical plating of non-metallic material and chemical plating therefor
CN101743210A (en) * 2007-04-18 2010-06-16 恩索恩公司 Metal surface enhanced
CN103242063A (en) * 2013-05-10 2013-08-14 济南大学 Preparation method of piezoelectric ceramic surface electrode
CN103981547A (en) * 2014-05-05 2014-08-13 深圳清华大学研究院 Preparation method for super-hydrophobic metal surface

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