CN104708930A - Nanometer metal particle-containing conductive ink-based printing method - Google Patents
Nanometer metal particle-containing conductive ink-based printing method Download PDFInfo
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Abstract
The invention discloses a nanometer metal particle-containing conductive ink-based printing method. The method comprises the following steps of 1, providing nanometer metal particle-containing conductive ink with solid content less than 45wt%, 2, spraying the conductive ink to a base by a gas flow jet printing method to obtain a first metal pattern layer with a loose porous structure, and 3, printing the conductive ink on the first metal pattern layer by an ink-jet printing method so that an uniform metal layer with thickness more than 1 micrometer is formed, wherein the uniform metal layer has square resistance less than 1 omega/square. Preferably, the step 2 comprises sintering the first metal pattern layer. The method has simple processes and a low cost, can realize high conductive metal pattern printing preparation by the existing metal ink, and is free of increasing of metal ink viscosity and metal solid content. The metal conductive patterns produced by the method do not contain a resin component and has conductivity higher than that of the patterns formed from the traditional silver slurry.
Description
Technical field
The present invention relates to a kind of Method of printing of conductive ink, particularly relating to a kind of Method of printing containing nano-metal particle conductive ink containing utilizing air-flow spray printing and inkjet technology to realize.
Background technology
Printed electronic (printed electronics) technology refers to and adopts the method for the directly electronic work ergosphere such as printed conductor, semiconductor, dielectric material, insulating materials on substrate to manufacture the production technology of electronic product.In the past few decades, reducing costs, improving cost performance is the motive force that electronic industry development grows all the time.And be compared to the subtractive process (subtractive manufacturing) that conditional electronic industry etching forms circuit, with printing be representative addition process (additive manufacturing) by electronic material film forming with realize the large process of patterning two and unite two into one, have economize in raw materials, the advantage such as technique is simple, environmental protection (industrial wastes produced is few), and be easy to coordinate new material to realize large area flexible device, advantageously in the requirement meeting electronic industry and reduce costs, expand market.The correlative study of current printed electronic device has expanded to field quite widely, the organic assembly that the material relating to the kinds such as conductor, semiconductor, dielectric material, electrolyte is made.Utilizing printing process to produce electronic product and effectively can reduce production cost, is the academic institution of current countries in the world and the emphasis of business research.In view of traditional printing industry is very ripe, once the bottleneck of printed electronic industry is resolved, be expected within the quite short time, electronics manufacturing and press to be combined, thus bring declining to a great extent and the very big expansion of application of electronic product cost, and solve the environment and resources problem of puzzlement electron trade at present, and sustainable development.
In the research field of printed electronic, printing metal conductive patterns is problem the most ripe, but the metal conductive patterns how utilizing the method for inkjet printing acquisition square resistance to be less than 1 Europe remains a challenge.In theory, the electric conductivity improving print pattern only needs to increase print thickness, and according to the Conductivity Calculation after existing printing ink solidification sintering, the thickness of metal pattern needs to be greater than 1 μm and just likely obtains desirable square resistance.But inkjet printing ink used has the feature of low viscosity, low-solid content; the printed pattern of dissolved destruction is often understood in multilayer print procedure ink inside; make repeatedly printing effect be similar in fact single and print more ink, thus make ink be easy to occur before the drying the phenomenon of neous flow in substrate such as similar " coffee ring ".In this case, be difficult to effectively obtain uniform abundant metal level only by repeatedly printing, the phenomenon that easily aggravation large area became uneven is even further on the contrary, affects the raising of electric conductivity.Often print one deck namely to carry out sintering theory significantly can improve the even problem of became uneven in wide area, but all strictly must control ink amount owing to printing at every turn, the operation repeatedly repeatedly " printing-sintering " is wasted time and energy, and cost is higher.
Summary of the invention
For the deficiencies in the prior art, the object of the present invention is to provide a kind of Method of printing of the conductive ink containing nano-metal particle, to obtain high-quality metal conducting layer.
For achieving the above object, present invention employs following technical scheme:
A Method of printing for conductive ink containing nano-metal particle, comprising:
(1) conductive ink containing nano-metal particle is provided, and in described conductive ink the content of solid lower than 45wt%;
(2) with air-flow spray printing method, described conductive ink is ejected on base material, forms first metal pattern layer with loose and porous structure;
(3) with ink-jet printing process by described printing of conductive inks in described first metal pattern layer, to forming the homogenous metal layer of thickness more than 1 μm, described homogenous metal layer after sintering square resistance is less than 1 Ω/, is particularly less than 50m Ω/.
As one of comparatively preferred embodiment, step (2) comprising: described conductive ink atomization is produced the ink droplet that diameter is less than 10 μm, described ink droplet is delivered to jet hole by recycling feeding air-flow, the liquid stream then utilizing focused gas flow ink droplet to be converged to diameter to be less than 300 μm, and be ejected in substrate.
Further, step (2) comprising:
By changing the solvent of ink droplet described in atomization power adjusting, thus control the concentration of injected conductive ink, wherein, atomization power is less, and the concentration of the conductive ink be ejected is higher;
And/or, regulated the solvent of injected liquid stream ink inside droplet by the flow proportional changing feeding air-flow and focused gas flow, thus control the concentration of injected conductive ink, wherein, the flow proportional of feeding air-flow and focused gas flow is lower, and the concentration of the conductive ink be ejected is higher;
And/or regulated the solvent of injected liquid stream ink inside droplet by the temperature changing jet hole, thus control the concentration of injected conductive ink, wherein, the temperature of jet hole is higher, and the concentration of the conductive ink be ejected is higher.
Further, described first metal pattern layer rough surface waviness is more than 0.5 μm." waviness " herein refers on this first metal pattern layer surface, the difference of the height of peak and the height of minimum point.
As one of comparatively preferred embodiment, step (2) also comprises: carry out heat-agglomerating process to described first metal pattern layer, heat-agglomerating temperature is at 80-300 DEG C.
Further, the mode of aforementioned heat-agglomerating process comprises any one or two or more combinations in warm table, baking oven, hot blast, light wave or heating using microwave sintering processing, but is not limited thereto.
Further, in described conductive ink, contained metallic element can comprise any one or the two or more combinations in gold, silver, copper, nickel, aluminium, platinum, but is not limited thereto.
As one of comparatively preferred embodiment, in aforementioned air-flow spray printing and/or ink jet printing process, also heat substrate, heating-up temperature is 35-150 DEG C.
Further, described substrate comprises dielectric base.
Further, step (3) comprising: printed more than one time in the first metal pattern layer with inkjet printing methods by described conductive ink.
Compared to prior art, beneficial effect of the present invention at least comprises:
(1) utilize method of the present invention, the printing preparation that existing metallic ink realizes high-conductive metal pattern can be based oneself upon, do not need the viscosity and the metal solid content that additionally increase metallic ink;
(2) utilize the not resinous composition of metal conductive patterns that method of the present invention obtains, compared with starching with conventional silver the pattern that prints, there is higher electric conductivity.
Accompanying drawing explanation
Fig. 1 is the principle schematic that in the present invention, air-flow spray printing device prints loose porous metal pattern, and wherein, 11 is nozzle, and 12 for being deposited on suprabasil metal level, and 13 is substrate;
Fig. 2 is the microphotograph of the loose porous silver-colored pattern formed by air-flow spray printing in the embodiment of the present invention 1.
Detailed description of the invention
As previously mentioned, because of the restriction of the aspects such as ink-jet printing ink inherent characteristic, such that industry is more difficult obtains comparatively uniform abundant metal level by inkjet printing methods, such as, square resistance is less than 1 Europe, is particularly less than the metal conductive patterns layer of 50 milliohms.
In view of the deficiencies in the prior art, inventor, through studying for a long period of time and putting into practice in a large number, proposes technical scheme of the present invention, and it mainly realizes based on air-flow Printing techniques and InkJet printing processes.
Generally, technical scheme of the present invention comprises:
(1) conductive ink containing nano-metal particle is provided, and in described conductive ink the content of solid lower than 45wt%;
(2) be ejected on base material with air-flow spray printing method by described conductive ink, form first metal pattern layer with loose and porous structure, rough surface waviness can more than 0.5 μm;
(3) with ink-jet printing process by described printing of conductive inks in described first metal pattern layer, until form the homogenous metal layer of thickness more than 1 μm, described homogenous metal layer after sintering square resistance is less than 1 Ω/, is particularly less than 50m Ω/.
In the present invention, because have employed air-flow Printing techniques, when using low viscosity, low-solid content metallic conduction ink equally, not similar with the inkjet printing single ink droplet ejected, but ejection is containing taking a liter air-flow for (fL) rank drop in a large number.Owing to having larger specific area, these ultra-fine droplets by suitable state modulator (as changed ratio or the nozzle temperature of atomization power, feeding air-flow and focused gas flow) can reduce spray the solvent of ink, thus obtain thicker but loose porous metal pattern layer, and when carrying out inkjet printing on these metal patterns, conductive ink can infilter in metal pattern, and its neous flow is because surface tension effects can be subject to strict restriction.In the case, the even phenomenon of large area became uneven will significantly be contained, thus is conducive to obtaining the homogenous metal layer of thickness more than 1 μm, and then significantly improves the electric conductivity printing metal level.
Such as, as preferably one of embodiment, in the process of aforementioned air-flow spray printing, first conductive ink atomization can be produced the ink droplet that diameter is less than 10 μm, ink droplet is delivered to jet hole by recycling feeding air-flow, the liquid stream then utilizing focused gas flow ink droplet to be converged to diameter to be less than 300 μm, and be ejected in substrate.
Further, comparatively preferably, also can carry out heat-agglomerating process to described first metal pattern layer, heat-agglomerating temperature, at 80-300 DEG C, then carries out inkjet printer operation.The various kinds of equipment that the mode of heat-agglomerating process involved herein can be commonly used by industry or method are implemented, and such as, can select warm table, baking oven, hot blast, light wave or heating using microwave sintering processing etc., and be not limited thereto.
Postscript, the pass of aforementioned inkjet printing can be one time, also can be multipass, its according to practical application demand and determine.
Postscript, and according to the needs of practical application, in aforesaid conductive ink, contained metallic element can be selected from but be not limited to any one or the two or more combinations in gold, silver, copper, nickel, aluminium, platinum.
Again and, comparatively preferably, in aforementioned air-flow spray printing and/or ink jet printing process, can also heat substrate, heating-up temperature is 35-150 DEG C simultaneously.
Aforementioned substrates can select all kinds of substrates, particularly dielectric base that meet application demand, such as Kapton, there is the silicon chip etc. of insulating barrier, but to be not limited thereto.
Obviously, method of the present invention is simple to operate, with low cost, and the printing preparation of high-conductive metal pattern can be realized based on existing metallic ink, without the need to additionally increasing viscosity and the metal solid content of metallic ink, the institute's metal conductive patterns that obtains not resinous composition, and compared with starching with conventional silver the pattern that prints, there is more high conductivity.
In order to be illustrated more clearly in technical scheme of the present invention, below in conjunction with accompanying drawing and preferred embodiment, the present invention is described in further detail, apparently, description is below only section Example of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other invention can also be obtained according to these embodiments.
embodiment 1
Be that the transparent polyimide film of 0.12 millimeter is successively immersed in each ultrasonic cleaning 10-30 minute in ethanol, isopropyl alcohol and water by cut growth 100 millimeters, wide 40 millimeters, thickness, dry up with high pure nitrogen after taking-up.Then air-flow spray printing device is utilized to print with ethylene glycol and the water commercialization silver ink that is solvent on film, atomizer actual power 18-25 watt in print procedure, nozzle temperature scope 40-90 DEG C, substrate heating temperature range 50-120 DEG C, flow proportional scope 1:5 to the 1:15 of feeding air-flow and focused gas flow.Then the pattern obtained is sintered 30 minutes on the warm table of 150-160 DEG C.The metal pattern thickness obtained is 2-3 micron, and average roughness waviness is more than 0.8 micron.
The silver-colored pattern completing sintering prints again with ink jet printing device, print point spacing (dot spacing) is set to 10 microns, amount to inkjet printing 3-6 time, the silver-colored ink printed is subject to the restriction of ground floor textured metal pattern, still keeps the thickness in wide area smooth after the drying.After again carrying out 30 minutes sintering with the warm table of 150-160 DEG C, square resistance is lower than 0.05 Ω/.
embodiment 2
Be that the band silicon dioxide insulating layer silicon chip of 0.12 millimeter is successively immersed in each ultrasonic cleaning 10-30 minute in ethanol, isopropyl alcohol and water by square for cut growth 20 millimeters, thickness, dry up with high pure nitrogen after taking-up.Then utilize air-flow spray printing device to print on film with ethers to be the commercialization gold ink of solvent main component, atomizer actual power 15-20 watt in print procedure, nozzle temperature scope 40-60 DEG C, substrate heating temperature range 50-75 DEG C, flow proportional scope 1:3 to the 1:12 of feeding air-flow and focused gas flow.Then the pattern of acquisition is sintered 15-30 minute on the warm table of 150-160 DEG C.The metal pattern thickness obtained is 1-2 micron, and average roughness waviness is more than 0.5 micron.
The golden pattern completing sintering prints again with ink jet printing device, print point spacing (dot spacing) is set to 20 microns, amount to inkjet printing 5-8 time, the silver-colored ink printed is subject to the restriction of ground floor textured metal pattern, still keeps the thickness in wide area smooth after the drying.After again carrying out 15-30 minute sintering with the warm table of 150-160 DEG C, square resistance is lower than 0.2 Ω/.
The above is only the specific embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. a Method of printing for the conductive ink containing nano-metal particle, is characterized in that, comprising:
(1) conductive ink containing nano-metal particle is provided, and in described conductive ink the content of solid lower than 45wt%;
(2) with air-flow spray printing method, described conductive ink is ejected on base material, forms first metal pattern layer with loose and porous structure;
(3) with ink-jet printing process by described printing of conductive inks in described first metal pattern layer, to forming the homogenous metal layer of thickness more than 1 μm, described homogenous metal layer after sintering square resistance is less than 1 Ω/.
2. the Method of printing of the conductive ink containing nano-metal particle according to claim 1, it is characterized in that, step (2) comprising: described conductive ink atomization is produced the ink droplet that diameter is less than 10 μm, described ink droplet is delivered to jet hole by recycling feeding air-flow, the liquid stream then utilizing focused gas flow ink droplet to be converged to diameter to be less than 300 μm, and be ejected in substrate.
3. the Method of printing of the conductive ink containing nano-metal particle according to claim 2, it is characterized in that, step (2) comprising:
By changing the solvent of ink droplet described in atomization power adjusting, thus control the concentration of injected conductive ink, wherein, atomization power is less, and the conductive ink concentration be ejected is higher;
And/or, regulated the solvent of injected liquid stream ink inside droplet by the flow proportional changing feeding air-flow and focused gas flow, thus control the concentration of injected conductive ink, wherein, the flow proportional of feeding air-flow and focused gas flow is lower, and the conductive ink concentration be ejected is higher;
And/or regulated the solvent of injected liquid stream ink inside droplet by the temperature changing jet hole, thus control the concentration of injected conductive ink, wherein, the temperature of jet hole is higher, and the conductive ink concentration be ejected is higher.
4. the Method of printing of the conductive ink containing nano-metal particle according to claim 1, it is characterized in that, described first metal pattern layer rough surface waviness is more than 0.5 μm.
5. the Method of printing of the conductive ink containing nano-metal particle according to claim 1, it is characterized in that, step (2) also comprises: carry out heat-agglomerating process to described first metal pattern layer, heat-agglomerating temperature is at 80-300 DEG C.
6. the Method of printing of the conductive ink containing nano-metal particle according to claim 5, it is characterized in that, the mode of heat-agglomerating process comprises any one or two or more combinations in warm table, baking oven, hot blast, light wave or heating using microwave sintering processing.
7. the Method of printing of the conductive ink containing nano-metal particle according to claim 1, is characterized in that, in described conductive ink, contained metallic element comprises any one or the two or more combinations in gold, silver, copper, nickel, aluminium, platinum.
8. the Method of printing of the conductive ink containing nano-metal particle according to claim 1, it is characterized in that, in air-flow spray printing and/or ink jet printing process, also heat substrate, heating-up temperature is 35-150 DEG C.
9. the Method of printing of the conductive ink containing nano-metal particle according to claim 1 or 8, it is characterized in that, described substrate comprises dielectric base.
10. the Method of printing of the conductive ink containing nano-metal particle according to claim 1, it is characterized in that, step (3) comprising: printed more than one time in the first metal pattern layer with inkjet printing methods by described conductive ink.
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| CN112513735A (en) * | 2018-08-22 | 2021-03-16 | 尼瓦洛克斯-法尔股份有限公司 | Method for manufacturing a timepiece component and component obtained by such a method |
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| CN113838799A (en) * | 2020-06-24 | 2021-12-24 | 天津大学 | Method for preparing high-resolution through hole in situ on flexible substrate based on electrofluid ink-jet printer |
| CN116160766A (en) * | 2021-11-25 | 2023-05-26 | 中国科学院大连化学物理研究所 | Method for realizing electrohydrodynamic jet printing on insulating substrate |
| CN116160766B (en) * | 2021-11-25 | 2024-08-20 | 中国科学院大连化学物理研究所 | Method for realizing electrohydrodynamic jet printing on insulating substrate |
| CN114279280A (en) * | 2021-12-27 | 2022-04-05 | 南京理工大学 | Ink-jet printing microstructure transducer element and preparation method thereof |
| CN114279280B (en) * | 2021-12-27 | 2024-04-05 | 南京理工大学 | Ink-jet printing microstructure transduction element and preparation method thereof |
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