CN107955459A - A kind of ink-jet printing ink and the method for metal-oxide film is prepared by it - Google Patents

A kind of ink-jet printing ink and the method for metal-oxide film is prepared by it Download PDF

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Publication number
CN107955459A
CN107955459A CN201711175602.0A CN201711175602A CN107955459A CN 107955459 A CN107955459 A CN 107955459A CN 201711175602 A CN201711175602 A CN 201711175602A CN 107955459 A CN107955459 A CN 107955459A
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China
Prior art keywords
ink
substrate
jet printing
temperature
polyacrylamide
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Granted
Application number
CN201711175602.0A
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Chinese (zh)
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CN107955459B (en
Inventor
宁洪龙
朱镇南
姚日晖
蔡炜
魏靖林
陶瑞强
陈建秋
周尚雄
邓培淼
彭俊彪
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South China University of Technology SCUT
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South China University of Technology SCUT
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00Inks
    • C09D11/30Inkjet printing inks
    • C09D11/36Inkjet printing inks based on non-aqueous solvents
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B41PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41MPRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
    • B41M5/00Duplicating or marking methods; Sheet materials for use therein
    • B41M5/0011Pre-treatment or treatment during printing of the recording material, e.g. heating, irradiating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B41PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41MPRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
    • B41M5/00Duplicating or marking methods; Sheet materials for use therein
    • B41M5/0023Digital printing methods characterised by the inks used
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B41PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41MPRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
    • B41M5/00Duplicating or marking methods; Sheet materials for use therein
    • B41M5/0041Digital printing on surfaces other than ordinary paper
    • B41M5/007Digital printing on surfaces other than ordinary paper on glass, ceramic, tiles, concrete, stones, etc.
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B41PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41MPRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
    • B41M7/00After-treatment of prints, e.g. heating, irradiating, setting of the ink, protection of the printed stock
    • B41M7/0054After-treatment of prints, e.g. heating, irradiating, setting of the ink, protection of the printed stock using protective coatings or film forming compositions cured by thermal means, e.g. infrared radiation, heat
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00Inks
    • C09D11/30Inkjet printing inks
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00Inks
    • C09D11/30Inkjet printing inks
    • C09D11/38Inkjet printing inks characterised by non-macromolecular additives other than solvents, pigments or dyes

Abstract

The invention belongs to printed electronic field, discloses a kind of ink-jet printing ink and prepares the method for metal-oxide film by it.The ink-jet printing ink is made of the chlorine hydrate zirconium oxide of solvent ethylene glycol, the polyacrylamide of 0.3~5wt.% and 0.1~0.6M.By substrate after pretreatment, ink-jet printer substrate temperature is set as 25~30 DEG C, 55~65 DEG C of 30~40V of nozzle voltage, temperature, ink droplet spacing carries out inkjet printing on substrate for 30~45 μm, after the completion of printing, substrate is warming up to 40~60 DEG C, stands 10~15min, after the complete gel of liquid film, heat at a temperature of 250~500 DEG C and obtain zirconia film.The present invention has chelation, and make system quick-gelatinizing after heating by adding the water-soluble polymer polyacrylamide containing polar group to metal ion, limitation solvents migration, suppression coffee toroidal effect.

Description

A kind of ink-jet printing ink and the method for metal-oxide film is prepared by it
Technical field
The invention belongs to printed electronic field, and in particular to a kind of ink-jet printing ink and to prepare metal oxide by it thin The method of film.
Background technology
It is existing to prepare the technique of metal-oxide film more using spin coating, dip-coating method using collosol and gel principle Etc. technique, there is high chemically active precursor by the way that metal alkoxide or inorganic salts are dissolved in water and alcohol to be formed, then will Solution coating generates metal-oxide film into liquid film, then through Overheating Treatment.In recent years, above-mentioned solution system is in ink-jet Applied in printing.By selecting suitable solvent, the solution that physical property meets inkjet printing demand can be obtained.
Coffee toroidal effect is universal phenomenon present in inkjet printing, when the solution of above-mentioned system is applied in inkjet printing It is no exception.Since edge solvent evaporation rate is more than center solvent, the solute concentration difference at edge and center is caused, is triggered outer To capillary flow, finally so that edge soluterich, the pattern after film drying is the concave ring-type pattern in the high center in edge. In electronic device preparation, performance influence of the film surface flatness for device is very huge, therefore above-mentioned system is in ink-jet Application in printing has very big limitation.
The content of the invention
For more than in place of shortcoming and defect existing in the prior art, primary and foremost purpose of the invention is to provide a kind of ink-jet Marking ink.
Another object of the present invention is to provide a kind of to prepare metal-oxide film using above-mentioned ink-jet printing ink Method.
The object of the invention is achieved through the following technical solutions:
A kind of ink-jet printing ink, is made of solvent ethylene glycol, polyacrylamide and chlorine hydrate zirconium oxide, and described poly- third The addition of acrylamide is the 0.3~5% of quality of glycol, and the concentration of the chlorine hydrate zirconium oxide is 0.1~0.6M.
Above-mentioned ink-jet printing ink can be prepared via a method which to obtain:Polyacrylamide is added into ethylene glycol solvent, More than 3h is stirred at 45 DEG C makes it fully dissolve, and then adds chlorine hydrate zirconium oxide, and magnetic agitation makes its dissolving, is aged It is spare after 24h.
Preferably, the weight average molecular weight of the polyacrylamide is 40000~130000.
A kind of method that metal-oxide film is prepared using above-mentioned ink-jet printing ink, is included the following steps:
By substrate after pretreatment, use ink-jet printer to set substrate temperature as 25~30 DEG C, nozzle voltage for 30~ 40V, 55~65 DEG C of nozzle temperature, ink droplet spacing carries out inkjet printing on substrate for 30~45 μm, after the completion of printing, by substrate 40~60 DEG C are warming up to, 10~15min is stood, after the complete gel of liquid film, is placed in thermal station, is added at a temperature of 250~500 DEG C It is thermally treated resulting in zirconia film.
Further, the substrate is preprocessed refers to using 50~80s of UV irradiation pretreatments.
The principle of the present invention is:The present invention starts with from the essence of coffee toroidal effect, has polar group by being introduced in system The water-soluble polymer polyacrylamide of group, the polymer are crosslinked with temperature rise, form gel, and have to metal ion Chelation, can effectively limit the migration of solvent solute.
The invention has the advantages that and beneficial effect:
(1) present invention has metal ion by adding the water-soluble polymer polyacrylamide containing polar group Chelation, and make system quick-gelatinizing after heating, limitation solvents migration, suppresses coffee toroidal effect.
(2) present invention selects the ethylene glycol with higher and viscosity to make it export-oriented under normal temperature state as solvent Capillary flow it is weaker;And since ethylene glycol viscosity is higher, it is therefore desirable to raise nozzle temperature to reduce its viscosity, improve spray Penetrate performance.
(3) present invention further pre-processes substrate using UV irradiations, improves its hydrophily.
Brief description of the drawings
Fig. 1 is the gelation process figure of liquid film when substrate heats up in the embodiment of the present invention.
Fig. 2 is the step instrument scanning figure on final gained zirconia film surface in the embodiment of the present invention.
Embodiment
With reference to embodiment and attached drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited In this.
Embodiment
(1) toward the polyacrylamide (weight average molecular weight 40000) that quality of glycol 0.5% is added in ethylene glycol solvent, More than 3h is stirred at 45 DEG C makes it fully dissolve, and then adds the chlorine hydrate zirconium oxide that molar concentration is 0.3M, and magnetic force stirs Mixing makes its dissolving, and it is spare to obtain the ink-jet printing ink after ageing 24h.
(2) prepared ink is filling into ink-jet printer (Dimatix2800) clip, substrate used is glass, lining Bottom uses UV irradiation pretreatments 50s.Printer substrate is set to 25 DEG C during printing, and nozzle voltage is 30V, and 55 DEG C of nozzle temperature is black It is 30 μm to drip spacing.After the completion of printing, substrate is warming up to 40 DEG C, 10min is stood, after the complete gel of liquid film, is placed in thermal station On, 1h is heated at 400 DEG C, obtains zirconia film.(embodiment expression is once representative specific experiment, its Parameter is the value once set)
The gelation process of liquid film is as shown in Figure 1 when the present embodiment substrate heats up.As seen from Figure 1, substrate temperature is worked as During rise, gelation, central liquid phase region rapid drop, final whole liquid film gelation occur at first for liquid film edge.This implementation The step instrument scanning figure on the final gained zirconia film surface of example is as shown in Figure 2.As seen from Figure 2, film morphology has no bright Aobvious coffee toroidal effect, it is overall more smooth.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention and from above-described embodiment Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification, Equivalent substitute mode is should be, is included within protection scope of the present invention.

Claims (4)

  1. A kind of 1. ink-jet printing ink, it is characterised in that:The ink-jet printing ink is by solvent ethylene glycol, polyacrylamide and eight Basic zirconium chloride composition is hydrated, the addition of the polyacrylamide is the 0.3~5% of quality of glycol, the chlorine hydrate oxygen The concentration for changing zirconium is 0.1~0.6M.
  2. A kind of 2. ink-jet printing ink according to claim 1, it is characterised in that:The Weight-average molecular of the polyacrylamide Measure as 40000~130000.
  3. 3. a kind of method that ink-jet printing ink using described in claim 1 or 2 prepares metal-oxide film, its feature exists In including the following steps:
    By substrate after pretreatment, ink-jet printer is used to set substrate temperature as 25~30 DEG C, nozzle voltage is 30~40V, 55~65 DEG C of nozzle temperature, ink droplet spacing carry out inkjet printing for 30~45 μm, after the completion of printing, substrate are heated up on substrate To 40~60 DEG C, 10~15min is stood, after the complete gel of liquid film, is placed in thermal station, at a temperature of 400~500 DEG C at heating Reason obtains zirconia film.
  4. A kind of 4. method for preparing metal-oxide film according to claim 3, it is characterised in that:The substrate is through pre- Processing refers to using 50~80s of UV irradiation pretreatments.
CN201711175602.0A 2017-11-22 2017-11-22 Ink for ink-jet printing and method for preparing metal oxide film by using ink Active CN107955459B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109251587A (en) * 2018-08-17 2019-01-22 华南理工大学 A kind of method that gel template method prepares inkjet printing sull
CN109266099A (en) * 2018-08-22 2019-01-25 华南理工大学 A kind of zirconium oxide ink-jet printing ink and the method for preparing zirconium oxide nano crystal film
CN111239203A (en) * 2018-11-29 2020-06-05 中国科学院大连化学物理研究所 Preparation method of copper oxide film
CN111269614A (en) * 2020-03-23 2020-06-12 华南理工大学 Method for reducing cracking of gel film in ink-jet printing
CN111293230A (en) * 2018-12-10 2020-06-16 广东聚华印刷显示技术有限公司 Thin film packaging layer and preparation method thereof, and preparation method of display panel

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CN1124184A (en) * 1994-12-29 1996-06-12 武汉工业大学 Zirconium oxide plasma spraying powder and codeposition coagulation/sintering method
CN1948163A (en) * 2006-11-09 2007-04-18 中国科学院宁波材料技术与工程研究所 Preparation method of zirconium oxide colloidal sol
CN107151483A (en) * 2017-05-31 2017-09-12 华南理工大学 A kind of ink jet ink for printing and preparation method and the zirconia film by its printing

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CN1124184A (en) * 1994-12-29 1996-06-12 武汉工业大学 Zirconium oxide plasma spraying powder and codeposition coagulation/sintering method
CN1948163A (en) * 2006-11-09 2007-04-18 中国科学院宁波材料技术与工程研究所 Preparation method of zirconium oxide colloidal sol
CN107151483A (en) * 2017-05-31 2017-09-12 华南理工大学 A kind of ink jet ink for printing and preparation method and the zirconia film by its printing

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109251587A (en) * 2018-08-17 2019-01-22 华南理工大学 A kind of method that gel template method prepares inkjet printing sull
CN109266099A (en) * 2018-08-22 2019-01-25 华南理工大学 A kind of zirconium oxide ink-jet printing ink and the method for preparing zirconium oxide nano crystal film
CN111239203A (en) * 2018-11-29 2020-06-05 中国科学院大连化学物理研究所 Preparation method of copper oxide film
CN111293230A (en) * 2018-12-10 2020-06-16 广东聚华印刷显示技术有限公司 Thin film packaging layer and preparation method thereof, and preparation method of display panel
CN111269614A (en) * 2020-03-23 2020-06-12 华南理工大学 Method for reducing cracking of gel film in ink-jet printing

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