CN105304157A - Transparent conductive thin film with conductive copper network and preparation method thereof - Google Patents
Transparent conductive thin film with conductive copper network and preparation method thereof Download PDFInfo
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- CN105304157A CN105304157A CN201410292996.8A CN201410292996A CN105304157A CN 105304157 A CN105304157 A CN 105304157A CN 201410292996 A CN201410292996 A CN 201410292996A CN 105304157 A CN105304157 A CN 105304157A
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Abstract
The invention relates to a transparent conductive thin film with a conductive copper network. The transparent conductive thin film comprises a transparent flexible substrate and a transparent adhesive layer arranged on the transparent flexible substrate, the surface of the transparent adhesive layer is provided with a trench network which is filled with copper mesoporous material. The invention further discloses a preparation method of the transparent conductive thin film. The preparation method comprises the following steps: firstly forming the trench network on the transparent flexible substrate and then filling the trench network with conductive ink and sintering, wherein the conductive ink is nanometer copper oxide conductive ink, the specific sintering method is that a broad-spectrum light source with wave length of 200-1500nm is used for radiating the trench network filled with the nanometer copper oxide conductive ink so that nanometer copper oxide particulates in the nanometer copper oxide conductive ink is reduced into nanometer copper particulates which are sintered and solidified. The method has the advantages that ultraviolet ray is used for reducing the nanometer copper oxide conductive ink and infrared ray is used for sintering and solidifying the reduced nanometer copper, the application limitation of conductive copper in the storage, printing and sintering process can be overcome and the cost of the whole process flow can be lowered.
Description
Technical field
The present invention relates to transparent conductive film technical field, particularly relate to and a kind of there is transparent conductive film of conductive copper network and preparation method thereof.
Background technology
Transparent conductive film has satisfactory electrical conductivity, and have a kind of film of high transmission rate at visible light wave range, current nesa coating has been widely used in the fields such as flat panel display, photovoltaic device, contact panel and electromagnetic shielding, has the wide market space.Flexible printed circuit board and FPC are a kind of special printed circuit boards, its feature be lightweight, thickness is thin, soft, flexible, is mainly applicable to a lot of product such as mobile phone, notebook computer, PDA, digital camera, LCDs.
The traditional manufacturing technique of transparent conductive film and flexible printed circuit board is etching method, and often need the multiple working procedures such as exposure, development, etching and cleaning, metal materials a large amount of in etching process is scrapd, and to the corrosion of sheet material, its selection is restricted.And the print process of rising in recent years eliminates follow-up complexity and the etching technics of easy contaminated environment, as long as in general print and solidification twice master operation, there is higher production efficiency.
Print process is that particle diameter is prepared into conductive ink at the metal material of nanometer scale, uses typography that conductive ink is printed on flexible material film surface, after sintering, forms required conductive network.But the conductive network that printing technology is made is the exposed bulge-structure on flexible material substrate surface, and anti-skidding scratch resistant characteristic is poor; Made conductive network graphics resolution is subject to the restriction of typography, cannot meet in recent years to the demand of high-resolution conductive network; Equally due to the restriction of technique, before sintering, under fixed line width, the amount of conductive ink is difficult to improve further, and namely under the prerequisite of selected live width and conductive ink, the amount of electric conducting material is difficult to improve, and the conductance of film is also difficult to improve; Finally, sintering process also can have an impact to transparent flexible base material in the process be cured conductive ink, and the selection of fexible film needs consideration heat-resisting indeformable, selects limited.
Silver chemical stable in properties, activity is low, price, heat conduction, conduct electricity very well, be not subject to chemicals corrosion, matter is soft, rich ductility, the conductive ink being main component with argent particulate makes in conductive network most widely used in the print process of present stage, but ag material price is at 600 ~ 800 dollars every kilogram, and cost of manufacture is high.Novel conductive ink-the nano-copper conductive ink in recent years market occurred, price due to metallic copper material has huge advantage (price is at 80 ~ 120 dollars every kilogram), and resistivity level is suitable with silver-colored line, have received increasing concern, but nano-copper conductive ink under normal temperature needs to mix up complicated antioxidant or coating to prevent copper particulate oxide, not easily preserve, and printing and sintering process in equipment and requirement for environmental conditions high, need special agglomerating plant toward contact, virtually add manufacturing cost.
Summary of the invention
The object of the embodiment of the present invention is for the structural shortcoming/blank of prior art, a kind of method for preparing transparent conductive film with conductive copper network is proposed, by ultraviolet reduced nano cupric oxide conductive ink, sinter Metal copper nanoparticles with infrared ray simultaneously, this overcome the application limitation of conductive copper paste in preservation, printing, sintering process, reduce the cost of whole technological process.
In order to reach foregoing invention object, a kind of method for preparing transparent conductive film with conductive copper network that the embodiment of the present invention proposes is achieved through the following technical solutions:
Have a method for preparing transparent conductive film for conductive copper network, first the method forms trench network on transparent flexible base material, afterwards filled conductive ink sintering in trench network; It is characterized in that: described conductive ink is nano oxidized copper conductive ink, the concrete grammar of described sintering adopts light-pulse generator to irradiate the trench network of filling nano oxidized copper conductive ink, make the nano cupric oxide particulate in nano oxidized copper conductive ink be reduced into Metal copper nanoparticles and be sintered solidification, described light-pulse generator at least emission wavelength is greater than the pulsed infrared of 800nm in the pulsed ultraviolet of 200-400nm and wavelength.
In technique scheme, nano oxidized copper conductive ink comprises the copper oxide nanometer particle of 5-30% and the solvent of 70-95%.
In a preferred embodiment, described solution is water, and the content of described copper oxide nanometer particle is 12%, and the granular size of copper oxide nanometer particle is between 85-130nm.
Described light-pulse generator is the wide spectrum light source of 200-1500nm wavelength, and its burst length is 25-10000 μ s, and maximum pulse rate is higher than KHz, and minimum pulse spacing is 20 μ s, and described light-pulse generator total energy output area is 4-21J/cm
2.
In a kind of preferred scheme, the concrete steps forming described trench network are: at the thin transparent impression glue of transparent flexible substrate surface coating; Then to be fitted in one on transparent impression glue with the outer impression block of transparent violet of trench network reverse mould and to apply pressure; Adopt the outer impression block of transparent violet described in ultraviolet source irradiation afterwards; After impression adhesive curing, namely outer for the transparent violet impression block demoulding is formed described trench network on described transparent flexible substrate surface.
In this technical scheme, the outer impression block of described transparent violet is quartzy masterplate.
In another kind of preferred scheme, the concrete steps forming described trench network are: to fit transparent impression glue-line at impression substrate surface; Then heating transparent impression glue makes it be rubbery state; Then to be fitted in one on transparent impression glue-line with the hot padding template of trench network reverse mould and to apply pressure; After impression glue-line cooling again solidification, by the demoulding of hot padding template, described impression film surface forms described trench network; Finally remove impression substrate, glue-line bottom surface will be impressed and transparent flexible base material is fitted.
In this technical scheme, described hot padding template adopts silicon or silicon dioxide to make.
In addition, the concrete steps of filled conductive ink are: a side surface justifying first on transparent flexible base material with trench network applies the nano oxidized copper conductive ink of one deck, are then removed by the nano oxidized copper conductive ink beyond groove with scraper.
In addition, filled conductive ink can also adopt the mode of a glue, and concrete steps are as follows: scraper is moved along side surface transparent flexible base material with trench network, puts glue inside scraper simultaneously.
Finally, the present invention also provides a kind of transparent conductive film with conductive copper network, this transparent conductive film, comprise transparent flexible base material and be located at the substratum transparent on transparent flexible base material, described substratum transparent surface has trench network, described trench network is filled with electric conducting material, and described electric conducting material is copper mesoporous material.
The aperture of described copper mesoporous material is 2-50nm.
Compared with prior art, the invention has the beneficial effects as follows: the extensive use that the present invention makes copper material prepare in conductive network technique in print process becomes possibility.Utilize ultraviolet reduced nano cupric oxide conductive ink, sinter Metal copper nanoparticles with infrared ray simultaneously, this overcome the application limitation of conductive copper paste in preservation, printing, sintering process, reduce the cost of whole technological process; Finally prepd copper material has splendid resistivity, suitable with argent; Metallic copper, relative to low price the silver as rare metal, in reducing the cost of multiple application (touch-screen, wiring board etc.), serves huge progradation.
Accompanying drawing explanation
By the description carried out its exemplary embodiment below in conjunction with accompanying drawing, the above-mentioned feature and advantage of the present invention will become apparent and easy understand.
Fig. 1 is the principle schematic that the embodiment of the present invention 1 forms trench network;
Fig. 2 is the principle schematic of the embodiment of the present invention 1 filled conductive ink;
Fig. 3 is the principle schematic of the embodiment of the present invention 1 sintering step;
The structural representation of the transparent conductive film that Fig. 4 is formed for the embodiment of the present invention 1;
Fig. 5 is the principle schematic that the embodiment of the present invention 2 forms trench network;
Fig. 6 is the principle schematic of the embodiment of the present invention 2 filled conductive ink.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in further detail, so that the understanding of technical staff of the same trade:
As shown in figures 1 to 6, label represents respectively:
The outer impression block 3 of transparent flexible base material 1, transparent impression glue 2, transparent violet, trench network 4, nano oxidized copper conductive ink 5, scraper 6, Nanometer Copper electric conductor 7, impression substrate 8, transparent impression glue-line 9, hot padding template 10.
Embodiment 1:
Shown in Fig. 1-4, provide a kind of method for preparing transparent conductive film with conductive copper network in the present embodiment 1, the method comprises the steps:
The first step, ultraviolet stamping
See Fig. 1, under transparent flexible base material 1 surface-coated one deck normal temperature, first have the thin transparent impression glue 2 of mobility, in ultraviolet stamping, transparent impression glue adopts UV glue.Then fit one with transparent impression glue 2 with the outer impression block 3 of transparent violet of required trench network reverse mould, and apply certain pressure and make the two laminating very close to each other; On the outer impression block 3 of transparent violet, arrange a ultraviolet source afterwards, the ultraviolet light of downward radiation makes transparent impression glue 2 (UV glue) solidify; Finally by after outer for transparent violet impression block 3 demoulding, fixing trench network 4 can be formed on transparent flexible base material 1 surface.
The outer impression block 4 of transparent violet can adopt quartzy masterplate.
Second step, filled conductive ink
See that the employing of Fig. 2, this step scrapes technique and is fed in trench network 4 to make nano oxidized copper conductive ink 5.First, at the nano oxidized copper conductive ink 5 that transparent impression glue 2 surface-coated one deck of solidification is very thin, then with scraper 6, the nano oxidized copper conductive ink 5 beyond the groove of trench network 4 is struck off.
3rd step, sintering
See Fig. 3, this step adopts high energy pulse formula wide spectrum light source to irradiate trench network 4 part of filling nano oxidized copper conductive ink 5.High energy pulse formula wide spectrum light source at least emission wavelength is greater than the pulsed infrared of 800nm in the pulsed ultraviolet of 200-400nm and wavelength., in specific embodiment, wide spectrum light source launches the light wave of 200-1500nm wavelength, and its total energy exports relevant to the coating thickness of nano oxidized copper conductive ink 5, and approximate range is 4-21J/cm2.
Nano cupric oxide particulate in nano oxidized like this copper conductive ink 5 is reduced into Metal copper nanoparticles under ultra-violet radiation, become nano-copper conductive ink, simultaneously due to ultrared heat effect, the nano-copper conductive ink after reduction is almost sintered instantaneously and solidify to form Nanometer Copper electric conductor 7.
In sintering step, adopt the object of pulsed light to be: the thermal effect of continuous light is obvious, and pulsed light energy is concentrated but the time is short, in contrast can not accumulate heat.Therefore, in sintering step of the present invention, strobe pulse light carries out photocuring, can avoid producing high temperature, and then serves the object avoiding destroying material around region to be solidified and structure.
Because electric conductor is formed by Nanometer Copper, so the mesoporous material that Nanometer Copper electric conductor 7 is formed for Metal copper nanoparticles.The aperture of this mesoporous material is 2-50nm.
Visible Fig. 4 of structure of the transparent conductive film of final formation.
The innovative point of the present embodiment is:
The present embodiment adopts nano oxidized copper conductive ink, the stable chemical nature of copper oxide nano material own, and it can carry out printing and sintering under normal air environment, does not need to mix inert gas or reducibility gas to suppress chemical change.Meanwhile, cupric oxide is relatively cheap relative to price argent.
After ultraviolet reduction and ultrared sintering, nano oxidized copper conductive ink is converted into the copper of solidification, and the steel structure made conducts electricity very well, and is a kind of mesoporous material, is the aperture of 2-50nm containing a large amount of aperture.
The wide spectrum light source of the present embodiment application has reductive copper oxide and sintered copper two kinds of functions, and in the course of the work, owing to adopting light-pulse generator, thermal effect is little, affects minimum on cell wall and transparent flexible base material, ensure that integrally-built stable.
Embodiment 2:
See Fig. 5, the present embodiment adopts hot press printing technology, and its concrete step is:
First be solid-state thin transparent impression glue-line 9 under impression substrate 8 surface laminating one deck normal temperature, hot padding impression glue material used is extensive, and conventional material has PC, PMMA etc.
One heat source impression glue is set afterwards, the temperature of transparent impression glue-line 9 is reached on its glass transition temperature, becomes rubbery state.Usually, impression substrate 8 adopts high heat conductive material, and thermal source directly adds hot padding substrate 8, makes it temperature and raises, and the transparent impression glue-line 9 on impression substrate 8 melts.
Then apply pressure on being fitted in rubbery state transparent impression glue-line 9 by one with the hot padding template 10 of required trench network reverse mould, make both laminating gaplesss, hot padding template 10 adopts silicon or silicon dioxide to make.
Remove thermal source afterwards, keep transparent impression glue-line 9 after a period of time to lower the temperature and again solidify.
After hot padding template 10 demoulding, the groove structure on transparent impression glue-line 9 can be formed.
Finally, impression base material 8 is removed, and transparent impression glue-line 9 is directly fitted, for subsequent handling is prepared with a transparent flexible base material 1.
See Fig. 6, the present embodiment fill ink adopts puts a glue mode, and its concrete step is: inside scraper 6, adopt nano oxidized copper conductive ink 5 in the method putting glue, afterwards along with the motion of scraper 6, run into the groove of trench network 4, nano oxidized copper conductive ink 5 will fall into and filling groove.Treat that justifying has been scraped, trench network 4 is just filled naturally.
Follow-up sintering step is identical with embodiment 1.
Compare embodiment 1, the advantage of the present embodiment 2 is:
Conductive network graphics resolution is determined by the groove of impression gained, and the hot press printing technology of employing can form micron to nano level trench network on transparent flexible substrate surface, greatly improves the resolution of conductive network.
The mode of some glue is adopted relatively to save in material.
By multiple embodiment, invention intention of the present invention and execution mode are described in detail above; but one of ordinary skill in the art of the present invention are appreciated that; the above embodiment of the present invention is only one of the preferred embodiments of the present invention; for length restriction; here can not all execution modes of particularize; any enforcement that can embody the claims in the present invention technical scheme, all in protection scope of the present invention.
It should be noted that; above content is in conjunction with concrete execution mode further description made for the present invention; can not assert that the specific embodiment of the present invention is only limitted to this; under the guidance of above-described embodiment; those skilled in the art can carry out various improvement and distortion on the basis of above-described embodiment, and these improve or distortion drops in protection scope of the present invention.
Claims (10)
1. have a method for preparing transparent conductive film for conductive copper network, first the method forms trench network on transparent flexible base material, afterwards filled conductive ink sintering in trench network; It is characterized in that: described conductive ink is nano oxidized copper conductive ink, the concrete grammar of described sintering adopts light-pulse generator to irradiate the trench network of filling nano oxidized copper conductive ink, make the nano cupric oxide particulate in nano oxidized copper conductive ink be reduced into Metal copper nanoparticles and be sintered solidification, described light-pulse generator at least emission wavelength is greater than the pulsed infrared of 800nm in the pulsed ultraviolet of 200-400nm and wavelength.
2. a kind of method for preparing transparent conductive film with conductive copper network according to claim 1, is characterized in that: described nano oxidized copper conductive ink comprises the copper oxide nanometer particle of 5-30% and the solvent of 70-95%.
3. a kind of method for preparing transparent conductive film with conductive copper network according to claim 2, is characterized in that: described solvent is water, the content of described copper oxide nanometer particle is 12%, and the granular size of copper oxide nanometer particle is between 85-130nm.
4. a kind of method for preparing transparent conductive film with conductive copper network according to claim 1, it is characterized in that: described light-pulse generator is the wide spectrum light source of 200-1500nm wavelength, its burst length is 25-10000 μ s, maximum pulse rate is higher than KHz, minimum pulse spacing is 20 μ s, and described light-pulse generator total energy output area is 4-21J/cm
2.
5. a kind of method for preparing transparent conductive film with conductive copper network according to claim 1-4 any one, is characterized in that, the concrete steps forming described trench network are: at the thin transparent impression glue of transparent flexible substrate surface coating; Then to be fitted in one on transparent impression glue with the outer impression block of transparent violet of trench network reverse mould and to apply pressure; Adopt the outer impression block of transparent violet described in ultraviolet source irradiation afterwards; After impression adhesive curing, namely outer for the transparent violet impression block demoulding is formed described trench network on described transparent flexible substrate surface.
6. a kind of method for preparing transparent conductive film with conductive copper network according to claim 1-4 any one, is characterized in that, the concrete steps forming described trench network are: to fit transparent impression glue-line at impression substrate surface; Then heating transparent impression glue makes it be rubbery state; Then to be fitted in one on transparent impression glue-line with the hot padding template of trench network reverse mould and to apply pressure; After impression glue-line cooling again solidification, by the demoulding of hot padding template, described impression film surface forms described trench network; Finally remove impression substrate, glue-line bottom surface will be impressed and transparent flexible base material is fitted.
7. a kind of method for preparing transparent conductive film with conductive copper network according to claim 1-4 any one, it is characterized in that, the concrete steps of described filled conductive ink are: a side surface justifying first on transparent flexible base material with trench network applies the nano oxidized copper conductive ink of one deck, are then removed by the nano oxidized copper conductive ink beyond groove with scraper.
8. a kind of method for preparing transparent conductive film with conductive copper network according to claim 1-4 any one, it is characterized in that, the concrete steps of described filled conductive ink are: scraper is moved along side surface transparent flexible base material with trench network, put glue inside scraper simultaneously.
9. one kind has the transparent conductive film of conductive copper network, comprise transparent flexible base material and be located at the substratum transparent on transparent flexible base material, described substratum transparent surface has trench network, and described trench network is filled with electric conducting material, it is characterized in that: described electric conducting material is copper mesoporous material.
10. a kind of transparent conductive film with conductive copper network according to claim 9, is characterized in that: the aperture of described copper mesoporous material is 2-50nm.
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| CN110246607B (en) * | 2019-04-30 | 2020-04-07 | 山东大学 | Flexible transparent conductive film with high light transmittance and high bonding strength as well as preparation method and application thereof |
| CN110972403A (en) * | 2019-12-04 | 2020-04-07 | 广东工业大学 | Forming method of fine embedded circuit based on nano copper |
| CN112566365A (en) * | 2020-12-09 | 2021-03-26 | 浙江日久新材料科技有限公司 | Metal grid film and preparation method thereof |
| CN113327721A (en) * | 2021-08-04 | 2021-08-31 | 西安宏星电子浆料科技股份有限公司 | Preparation method of low-temperature cured conductive copper paste |
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