CN108081781B - The method for improving inkjet printing film forming thickness - Google Patents

The method for improving inkjet printing film forming thickness Download PDF

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Publication number
CN108081781B
CN108081781B CN201711336819.5A CN201711336819A CN108081781B CN 108081781 B CN108081781 B CN 108081781B CN 201711336819 A CN201711336819 A CN 201711336819A CN 108081781 B CN108081781 B CN 108081781B
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nano
ink
metal
inkjet printing
metal particle
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CN108081781A (en
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张蓉
周剑飞
李宏建
夏辉
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Hunan Xingwei New Material Co Ltd
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Hunan Xingwei New Material Co Ltd
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    • 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
    • B41M5/0047Digital printing on surfaces other than ordinary paper by ink-jet printing
    • 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

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Inks, Pencil-Leads, Or Crayons (AREA)
  • Ink Jet Recording Methods And Recording Media Thereof (AREA)
  • Conductive Materials (AREA)

Abstract

The invention discloses a kind of methods for improving inkjet printing film forming thickness, it is the following steps are included: weigh the surface-treated nano-metal particle that mass percent is 2-30%, it is dispersed in metal salt solution, the uniform and stable solution containing nano-metal particle is formed, and the complexing agent that mass percent is 0.1% is added;Then dispersing agent is added in the resulting mixed solution of step 1 in the requirement to viscosity of surface tension and printing device of substrate according to ink or required marking ink is made in stabilizer;The resulting marking ink of step 2 is fitted into the print cartridge of ink-jet printer, ink-jet printer carries out inkjet printing to substrate by product requirement;Gradient baking sintering is carried out to the substrate after inkjet printing, until solvent volatilizees completely, reduction reaction occurs in situ and generates fine and close metal solid for metal ion;The partial size of the nano-metal particle is 5-500nm;The thickness of printing-filming can be improved without repeatedly printing for Method of printing provided by the present invention.

Description

The method for improving inkjet printing film forming thickness
Technical field
The present invention relates to inkjet printing technology fields, and in particular to a method of improve inkjet printing film forming thickness.
Background technique
Inkjet printing refers to the printing that ink is ejected into in substrate dropwise under the control of the computer and is constituted dot matrix film layer Technique.Wherein, electronics inkjet printing has the characteristics that inexpensive, efficient, quick, contactless digital fabrication, is both applicable in Rigid substrate also adapts to flexible substrates, therefore is widely used to printed circuit board, Organic Light Emitting Diode, conducting wire, soft Property display device, RF tag etc..
In metal salt conductive ink, metal exists in the form of water-soluble or oil-soluble salt, dissolves shape in a solvent At the solution of stable homogeneous;In use, printing device, which is injected into substrate, spreads out composition film layer, make metal through Overheating Treatment Reduction reaction occurs in situ and generates fine and close metal solid for ion.Wherein, the metal ion content in conductive ink is to film layer Thickness plays a decisive role, and because of the volatilization of the limited and most of solvent of its concentration, finally formed conductive film layer thickness is small, nothing Method meets the printing requirement of thick-layer ink, can only realize the printing of thin layer ink.
In the prior art, the method for mostly using multilayer repeatedly to print can increase the thickness of conductive film layer, but it can be dropped The accuracy of low filming width and the resolution ratio of printing.
Therefore, now need to provide a kind of raising inkjet printing that not only can guarantee precision and resolution ratio but also can increase film forming thickness at The method of film thickness.
Summary of the invention
For this purpose, the present invention provides a kind of methods for improving inkjet printing film forming thickness comprising following steps:
Step 1: weighing the surface-treated nano-metal particle that mass percent is 2-30%, it is dispersed in metal salt In solution, the uniform and stable solution containing nano-metal particle is formed, and the complexing agent that mass percent is 0.1% is added;
Step 2: then according to ink substrate the requirement to viscosity of surface tension and printing device in step 1 obtained by Mixed solution in dispersing agent or stabilizer is added required marking ink is made;
Step 3: the resulting marking ink of step 2 is fitted into the print cartridge of ink-jet printer, ink-jet printer presses product It is required that carrying out inkjet printing to substrate;
Step 4: carrying out gradient baking sintering to the substrate after inkjet printing, until solvent volatilizees completely, metal ion is in situ Reduction reaction occurs and generates fine and close metal solid;
Wherein, the partial size of the nano-metal particle is 5-500nm.
In step 1, surface treatment, which refers to, carries out oil removing, processing of rust removing and nano metal to nano-metal particle Grain removes oxide process, and nano-metal particle is then placed in alcohol after processing and carries out ultrasonic cleaning 0.5h, is then dried And 1h is impregnated using enveloping agent solution or coupling agent solution, to guarantee that nano-metal particle is not reunited in metal salt solution And stable dispersion.
Wherein, the complexing agent in preferred steps one is organic amine complex.
Specifically, in step 4, the substrate after inkjet printing is put into the air dry oven for being preset as 80 DEG C first Baking sintering is carried out, temperature is then promoted with 50 DEG C/15-20min, until temperature is increased to 230 DEG C.
The nano-metal particle is set as silver, copper, gold, any one nanoscale metal particles in aluminium.
The nano-metal particle is set as nano-titanium dioxide, nano zine oxide, nano tin dioxide, nano indium oxide, receives Any one nanosize metal oxide particle in rice zirconium oxide.
Metal ion in the metal salt solution is silver ion or copper ion or nickel ion.
The metal salt solution is set as water-soluble conductive ink, and the dispersing agent or stabilizer that add in step 2 are Polyvinylpyrrolidone, polyvinyl alcohol, any one aqueous polymer in polyoxyethylene analog derivative.If the gold Belonging to the dispersing agent or stabilizer that salting liquid is set as the conductive ink of solvent borne, and adds in step 2 is polar group containing end group Alkyl compound.
The present invention compared with the existing technology, has the following advantages that place:
In the present invention, nano metal particles are added in metal salt solution, the appropriate addition of nano-metal particle can change The surface hardness and fastness of kind conductive film layer, the content for increasing nano-metal particle in a certain range can improve the cause of ink trace Close property and conductivity, obtaining under the premise of reducing different ink-jet printing times has certain thickness requirement and the good conduction of electric property Film layer;At the same time, because nano-metal particle content is higher, a possibility that ink jam nozzle, is bigger, therefore by nanogold The size controlling of metal particles is within the scope of 5-500nm, that is to say, that is processed into extremely tiny and not easy to reunite receive The phenomenon that rice metallic particles is to effectively avoid plug nozzle generation;Therefore, Method of printing provided by the present invention is without multiple The thickness of printing-filming can be improved in printing.
Specific embodiment
Technical solution of the present invention will be clearly and completely described below, it is clear that described embodiment is this hair Bright a part of the embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not having Every other embodiment obtained under the premise of creative work is made, shall fall within the protection scope of the present invention.
As long as in addition, the non-structure each other of technical characteristic involved in invention described below different embodiments It can be combined with each other at conflict.
Embodiment 1
Present embodiments provide a kind of method for improving inkjet printing film forming thickness comprising following steps:
Step 1: weighing the surface-treated nano-metal particle that mass percent is 2-30%, it is dispersed in metal salt In solution, the uniform and stable solution containing nano-metal particle is formed, and the complexing agent that mass percent is 0.1% is added;
Step 2: then according to ink substrate the requirement to viscosity of surface tension and printing device in step 1 obtained by Mixed solution in dispersing agent or stabilizer is added required marking ink is made;
Step 3: the resulting marking ink of step 2 is fitted into the print cartridge of ink-jet printer, ink-jet printer presses product It is required that carrying out inkjet printing to substrate;
Step 4: carrying out gradient baking sintering to the substrate after inkjet printing, until solvent volatilizees completely, metal ion is in situ Reduction reaction occurs and generates fine and close metal solid.Meanwhile the complexing agent in the present embodiment preferred steps one is organic amine complexing Object.
In the present embodiment, nano metal particles, the appropriate addition energy of nano-metal particle are added in metal salt solution Improve the surface hardness and fastness of conductive film layer, the content for increasing nano-metal particle in a certain range can improve ink trace Compactness and conductivity, obtaining under the premise of reducing different ink-jet printing times has certain thickness requirement and electric property is good leads Electrolemma layer;At the same time, because nano-metal particle content is higher, a possibility that ink jam nozzle, is bigger, therefore by nanometer The size controlling of metallic particles is within the scope of 5-500nm, that is to say, that is processed into ultrafine nano metal Grain, while adding dispersing agent or stabilizer and forming tiny nano-metal particle not easy to reunite to effectively avoid plug nozzle Phenomenon occurs;Method of printing described in the present embodiment is in the thickness that printing-filming also can be improved without repeatedly printing.
Specifically, in step 1, surface treatment, which refers to, carries out oil removing, processing of rust removing and nanometer to nano-metal particle Metallic particles removes oxide process, and nano-metal particle is then placed in alcohol after processing and carries out ultrasonic cleaning 0.5h, and It dries afterwards and impregnates 1h using enveloping agent solution or coupling agent solution, to guarantee that nano-metal particle is not sent out in metal salt solution Raw reunion and stable dispersion.
In step 4, the substrate after inkjet printing is put into the air dry oven for be preset as 80 DEG C toasts first Then sintering promotes temperature with 50 DEG C/15-20min, until temperature is increased to 230 DEG C.
Wherein, the preferably described nano-metal particle is set as silver, copper, gold, any one nanoscale metal particles in aluminium;Institute State nano-metal particle be set as nano-titanium dioxide, nano zine oxide, nano tin dioxide, nano indium oxide, in nano zircite Any one nanosize metal oxide particle;Metal ion in the metal salt solution is silver ion or copper ion or nickel Ion.
In the present embodiment, when the metal salt solution is set as water-soluble conductive ink, then addition divides in step 2 Powder or stabilizer are aqueous polymer;Specifically, the aqueous polymer be set as polyvinylpyrrolidone, One of polyvinyl alcohol, polyoxyethylene analog derivative;As disposable embodiment, when the metal salt solution is set as molten When the conductive ink of agent, then dispersing agent is added in step 2 or stabilizer is the alkyl compound of the polar group containing end group. The effect of above-mentioned dispersing agent used or stabilizer contributes to nano-metal particle and uniformly and stably divides in metal salt solution It dissipates, so that the phenomenon for avoiding the nozzle of ink-jet printer blocked occurs.
Embodiment 2
On the basis of embodiment 1, the present embodiment further provides for a kind of specific embodiment:
Step 1: weighing the surface-treated nano-Ag particles that mass percent is 2%, it is dispersed in citric acid In silver-colored solution, and the uniform and stable solution containing nano-Ag particles is formed, and it is 0.1% that mass percent, which is added, in the solution Organic amine complex, organic amine complex be complexing agent;
Step 2: being handled in the requirement to viscosity of surface tension and printing device of substrate through step 1 according to ink In solution afterwards, suitable alcohols is added as regulator, thus the marking ink needed for obtaining;
Step 3: step 2 marking ink obtained is fitted into the print cartridge of ink-jet printer, the ink-jet printer Inkjet printing is carried out by product requirement;
Baking sintering is carried out Step 4: the printed substrate for having ink trace is put into the air dry oven for be preset as 80 DEG C, With the rate heating of 50 DEG C/15-20min until temperature reaches 230 DEG C;Such gradient-heated, so that it is guaranteed that solvent volatilizees completely, Reduction reaction occurs in situ and generates fine and close metal solid for metal ion;
Step 5: taking out the product after step 4 is processed, its thickness is tested, measures it with a thickness of 0.77 μ M, the film forming thickness (about 0.40 μm) which less adds the ink-jet printing ink of nano-metal particle are significantly improved.
Embodiment 3
On the basis of embodiment 1, the present embodiment further provides for a kind of specific embodiment:
Step 1: weighing the surface-treated nano copper particle that mass percent is 5%, it is dispersed in neodecanoic acid In silver-colored solution, and the uniform and stable solution containing nano copper particle is formed, and it is 0.1 % that mass percent, which is added, in the solution Organic amine complex, organic amine complex be complexing agent;
Step 2: being handled in the requirement to viscosity of surface tension and printing device of substrate through step 1 according to ink In solution afterwards, suitable alcohols is added as regulator, thus the marking ink needed for obtaining;
Step 3: step 2 marking ink obtained is fitted into the print cartridge of ink-jet printer, the ink-jet printer Inkjet printing is carried out by product requirement;
Baking sintering is carried out Step 4: the printed substrate for having ink trace is put into the air dry oven for be preset as 80 DEG C, It is often heated up with the rate of 50 DEG C/15-20min, until temperature reaches 230 DEG C;Such gradient-heated, so that it is guaranteed that solvent is waved completely Reduction reaction occurs in situ and generates fine and close metal solid for hair, metal ion;
Step 5: taking out the product after step 4 is processed, its thickness is tested, it is after tested with a thickness of 1.04 μm, the film forming thickness that the thickness of the product less adds the ink-jet printing ink of nano-metal particle is significantly improved.
Embodiment 4
On the basis of embodiment 1, the present embodiment further provides for a kind of specific embodiment:
Step 1: weighing the surface-treated titanium dioxide nanoparticle that mass percent is 10%, it is dispersed in In oxalic acid nickel solution, and the uniform and stable solution containing titanium dioxide nanoparticle is formed, and quality hundred is added in the solution Score is organic amine complex of 0.1 %, which is complexing agent;
Step 2: being handled in the requirement to viscosity of surface tension and printing device of substrate through step 1 according to ink In solution afterwards, suitable alcohols is added as regulator, thus the marking ink needed for obtaining;
Step 3: step 2 marking ink obtained is fitted into the print cartridge of ink-jet printer, the ink-jet printer Inkjet printing is carried out by product requirement;
Baking sintering is carried out Step 4: the printed substrate for having ink trace is put into the air dry oven for be preset as 80 DEG C, It is heated up with the rate of 50 DEG C/15-20min, until temperature reaches 230 DEG C;Such gradient-heated, so that it is guaranteed that solvent is waved completely Reduction reaction occurs in situ and generates fine and close metal solid for hair, metal ion;
Step 5: taking out the product after step 4 is processed, its thickness is tested, it is after tested with a thickness of 1.58 μm, it is known that the film forming thickness that the thickness of the product less adds the ink-jet printing ink of nano-metal particle is significantly improved.
Embodiment 5
On the basis of embodiment 1, the present embodiment further provides for a kind of specific embodiment:
Step 1: weighing the surface-treated nano zircite particle that mass percent is 20%, it is dispersed in vinegar In sour copper solution, and the uniform and stable solution containing nano zircite particle is formed, and mass percent is added in the solution For organic amine complex of 0.1 %, which is complexing agent;
Step 2: being handled in the requirement to viscosity of surface tension and printing device of substrate through step 1 according to ink In solution afterwards, suitable alcohols is added as regulator, thus the marking ink needed for obtaining;
Step 3: step 2 marking ink obtained is fitted into the print cartridge of ink-jet printer, the ink-jet printer Inkjet printing is carried out by product requirement;
Baking sintering is carried out Step 4: the printed substrate for having ink trace is put into the air dry oven for be preset as 80 DEG C, It is heated up with the rate of 50 DEG C/15-20min, until temperature reaches 230 DEG C;Such gradient-heated, so that it is guaranteed that solvent is waved completely Reduction reaction occurs in situ and generates fine and close metal solid for hair, metal ion;
Step 5: taking out the product after step 4 is processed, its thickness is tested, it is after tested with a thickness of 2.13 μm, it is known that the film forming thickness that the thickness of the product less adds the ink-jet printing ink of nano-metal particle is significantly improved.
Embodiment 6
On the basis of embodiment 1, the present embodiment further provides for a kind of specific embodiment:
Step 1: weighing the surface-treated nano-Ag particles that mass percent is 30%, it is dispersed in succinic acid In copper solution, and the uniform and stable solution containing nano-Ag particles is formed, and it is 0.1 % that mass percent, which is added, in the solution Organic amine complex, organic amine complex be complexing agent;
Step 2: being handled in the requirement to viscosity of surface tension and printing device of substrate through step 1 according to ink In solution afterwards, suitable alcohols is added as regulator, thus the marking ink needed for obtaining;
Step 3: step 2 marking ink obtained is fitted into the print cartridge of ink-jet printer, the ink-jet printer Inkjet printing is carried out by product requirement;
Baking sintering is carried out Step 4: the printed substrate for having ink trace is put into the air dry oven for be preset as 80 DEG C, It is heated up with the rate of 50 DEG C/15-20min, until temperature reaches 230 DEG C;Such gradient-heated, so that it is guaranteed that solvent is waved completely Reduction reaction occurs in situ and generates fine and close metal solid for hair, metal ion;
Step 5: taking out the product after step 4 is processed, its thickness is tested, it is after tested with a thickness of 0.77 μm, it is known that the film forming thickness that the thickness of the product less adds the ink-jet printing ink of nano-metal particle is significantly improved.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or It changes still within the protection scope of the invention.

Claims (4)

1. improve inkjet printing film forming thickness method, it is characterised in that: itself the following steps are included:
Step 1: weighing the surface-treated nano-metal particle that mass percent is 2-30%, it is molten to be dispersed in metal salt In liquid, the uniform and stable solution containing nano-metal particle is formed, and the complexing agent that mass percent is 0.1% is added;
Step 2: then resulting mixed in step 1 in the requirement to viscosity of surface tension and printing device of substrate according to ink It closes addition dispersing agent or stabilizer in solution and required marking ink is made;
Wherein, the metal salt solution is waterborne conductive ink or solvent borne conductive ink, the metal ion in solution be silver from Son, copper ion or nickel ion;When the metal salt solution is set as water-soluble conductive ink, the dispersing agent that is added in step 2 Or stabilizer is polyvinylpyrrolidone, any one aqueous high molecular polymerization in polyvinyl alcohol, polyoxyethylene analog derivative Object;When the metal salt solution is set as the conductive ink of solvent borne, the dispersing agent or stabilizer added in step 2 is containing end The alkyl compound of based polar group;
Step 3: the resulting marking ink of step 2 is fitted into the print cartridge of ink-jet printer, ink-jet printer presses product requirement Inkjet printing is carried out to substrate;
Step 4: carrying out gradient baking sintering to the substrate after inkjet printing, until solvent volatilizees completely, metal ion occurs in situ Reduction reaction generates fine and close metal solid;Wherein, gradient baking sintering specifically: be first put into the substrate after inkjet printing It is preset as carrying out baking sintering in 80 DEG C of air dry oven, temperature is then promoted with 50 DEG C/15-20min, until temperature increases To 230 DEG C;
Wherein, the partial size of the nano-metal particle is 5-500nm.
2. the method according to claim 1 for improving inkjet printing film forming thickness, it is characterised in that: in step 1, table Surface treatment, which refers to, carries out oil removing, processing of rust removing and nano-metal particle except oxide process, processing to nano-metal particle Nano-metal particle is then placed in alcohol afterwards and carries out ultrasonic cleaning 0.5h, then dry and uses enveloping agent solution or coupling Agent solution impregnates 1h, and reunion and stable dispersion do not occur to guarantee nano-metal particle in metal salt solution.
3. the method according to claim 1 or 2 for improving inkjet printing film forming thickness, it is characterised in that: in step 1 Complexing agent is organic amine complex.
4. the method according to claim 1 for improving inkjet printing film forming thickness, it is characterised in that: the nano metal Particle is silver, copper, gold, any one or more nanoscale metal particles in aluminium, can also be nano-titanium dioxide, nano oxidized Zinc, nano tin dioxide, nano indium oxide, any one or more nanosize metal oxide particle in nano zircite.
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JP7157597B2 (en) * 2018-08-31 2022-10-20 花王株式会社 Water-based fine metal particle dispersion
CN111086330B (en) * 2018-10-23 2021-08-31 广东聚华印刷显示技术有限公司 Drying device and drying process
CN109261970B (en) * 2018-10-23 2020-10-16 武汉三迪创为科技有限公司 3D printing equipment and method for preparing medical porous tantalum metal implant material by using same
CN114324480B (en) * 2020-07-21 2023-08-29 艾感科技(广东)有限公司 Gas sensor array and printing solution preparation method thereof
CN115197609B (en) * 2022-08-22 2023-06-16 上海应用技术大学 Preparation and printing method of conductive ink for commercial inkjet printer

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CN103619129A (en) * 2013-11-25 2014-03-05 深圳大学 Method for printing copper conducting circuits in ink-jet mode
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