CN104332215A - Preparation method for low specific resistance transparent conducting film - Google Patents
Preparation method for low specific resistance transparent conducting film Download PDFInfo
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- CN104332215A CN104332215A CN201410604067.6A CN201410604067A CN104332215A CN 104332215 A CN104332215 A CN 104332215A CN 201410604067 A CN201410604067 A CN 201410604067A CN 104332215 A CN104332215 A CN 104332215A
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Abstract
A preparation method for a low specific resistance transparent conducting film comprises the following steps of (a) combining a high length-diameter ratio silver nanowire through silver wire raw materials; (b) deploying conducting silver paste with silver wires obtained from the step (a) being served as padding; (c) coating the conducting silver paste obtained from the step (b) on a substrate to form into a film layer; (d) performing postprocessing on the film layer. The preparation method for the low specific resistance transparent conducting film develops the novel technology that the high length-diameter ratio silver nanowire replaces a spherical nano-silver particle to be served as main padding materials of the conducting silver paste, a conducting purpose is achieved through mutual contact between silver wires in the paste, and compared with the particle contact, the wire-shaped nano-silver can improve the reliability and meanwhile obviously improves the conductivity.
Description
Technical field
The present invention relates to this electronic information display field, its prepare conducting film, be the very important thin-film materials such as liquid crystal display in electronic information field (LCD), plasma display (PDP), electroluminescent display (EL/OLED), touch-screen (Touch Panel).
Background technology
The products such as following mobile terminal, wearable device, intelligent appliance, solid demand is had to touch panel, simultaneously along with contact panel is in large size, low priceization, and conventional I TO film can not be used for flexible application, the factors such as the essential problem such as conductivity and light transmittance not easily overcomes, many panel vendors begin one's study the substitute of ITO one after another, comprise the materials such as nano-silver thread, metal grill, CNT (carbon nano-tube) and Graphene.New material technology application can extend to the equipment of more than 20 inches from conventional panel size one tunnel of smart mobile phone, and its resistance, and extensibility, bendability is all better than ito thin film.
Nano-silver thread technology will be the new technology being hopeful alternative ito thin film in recent emerging touch technology most.Nano-silver thread (SNW, silvernanowire) technology, is spread upon on flexibility or glass substrate by nano-silver thread ink material, then utilizes technology for coating, makes the transparent conductive film with Nano grade silver line conductive network pattern.Make physical mechanism because it is special, the diameter of the live width of nano-silver thread is very little, is about 50nm, much smaller than 1um, thus there is not the problem of unauspicious interference, can be applied on the display screen of various sizes.In addition, because live width is less, the film that the conductive film that silver-colored line technology is made is made compared to metal grill technology can reach higher light transmittance.Secondly, nano-silver thread film has less bending radius compared to metal grill film, and resistance change rate is less when bending, is applied in the equipment with curved-surface display, such as intelligent watch, time on bracelet etc., has more advantage.
Summary of the invention
The present invention aims to provide novel low resistivity, transparent conducting film (TCF) preparation method.
In order to reach above-mentioned purpose, the preparation method providing a kind of low resistivity, transparent conducting film of the present invention, comprises the steps: that (a) utilizes silver-colored line Material synthesis nano silver wires with high length-diameter ratio; B () is filler allotment conductive silver paste with described silver-colored line obtained in step (a); C the conductive silver paste obtained in step (b) is coated on substrate and forms rete by (); And (d) is to described rete reprocessing.
In some embodiments, described silver-colored line raw material comprises silver nitrate, ethylene glycol, and polyvinylpyrrolidone, react 30 ~ 120 minutes at 100 ~ 200 DEG C of temperature, the mol ratio of obtained described nano silver wires with high length-diameter ratio wherein above-mentioned substance is as follows: silver nitrate: ethylene glycol: polyvinylpyrrolidone=1:1 ~ 20:0.05 ~ 5.
In some embodiments, step (b) comprising: (b1) prepares matrix resin; (b2) described matrix resin and described nano-silver thread is mixed according to mass ratio 1:1 ~ 20:1; And the curing accelerator that (b3) adds described matrix resin consumption 1% ~ 3% mixes.
In some embodiments, described matrix resin comprises the bisphenol A type epoxy resin that mass ratio is the ratio of 1:0.05 ~ 0.5:0.2 ~ 2, epoxy active diluent, and the mixture of curing agent 4-methylhexahydrophthaacid acid.
In some embodiments, described curing accelerator comprises (1-cyano group 2-ethyl 4-methylimidazole 2ZE4MZ-CN).
In some embodiments, with blade coating, lift, described conductive silver paste is coated on described substrate by spin coating mode.
In some embodiments, described substrate comprises glass, PET, or PVA.
In some embodiments, the described substrate base of having plated film to be placed under 100 ~ 350 DEG C of temperature conditions heat treatment 20 ~ 200 minutes, to obtain low resistivity, transparent conducting film.
Compared with prior art, the invention has the advantages that: develop and replace the new technology of spherical nano-Ag particles as the main packing material of conductive silver paste using nano silver wires with high length-diameter ratio, realize reaching conduction object with contacting with each other between line silver-colored in slurry, compared to particle type contact, linear nano silver obviously improves its electric conductivity while raising reliability.In addition, because wire arrangement can realize with less Nano Silver to realize Thin film conductive, therefore production cost have also been obtained and significantly reduces, and this is to Realization of Product large-scale production tool significance.In addition, the conductive silver paste prepared has good impressionability, conductivity and superpower adhesive force, and the film manufactured on this basis integrates transparent, frivolous, bent, slip-off preventing, and this is not available for like product.
Accompanying drawing explanation
By reference to the accompanying drawings, by detailed description hereafter, above-mentioned and other feature and advantage of the present invention more clearly can be understood, wherein:
The flow chart of the preparation method of Fig. 1 embodiment of the present invention; And
Fig. 2 is the schematic diagram utilizing the conducting film prepared according to the preparation method of the embodiment of the present invention.
Embodiment
See the accompanying drawing of the specific embodiment of the invention, hereafter in more detail the present invention will be described.But the present invention can realize in many different forms, and should not be construed as by the restriction in the embodiment of this proposition.On the contrary, it is abundant and complete open in order to reach for proposing these embodiments, and makes those skilled in the art understand scope of the present invention completely.
Description, describes the preparation method of the low resistivity, transparent conducting film according to the embodiment of the present invention in detail.
As shown in Figure 1, in step S101, utilize silver-colored line Material synthesis nano silver wires with high length-diameter ratio.Described silver-colored line raw material comprises silver nitrate, ethylene glycol, and polyvinylpyrrolidone, react 30 ~ 120 minutes at 100 ~ 200 DEG C of temperature, the mol ratio of obtained described nano silver wires with high length-diameter ratio wherein above-mentioned substance is as follows: silver nitrate: ethylene glycol: polyvinylpyrrolidone=1:1 ~ 20:0.05 ~ 5.Raw material used comprises silver nitrate, ethylene glycol, polyvinylpyrrolidone etc. at 100 ~ 200 DEG C, preferably react 30 ~ 120 minutes at 130 ~ 180 DEG C of temperature, can obtain nano silver wires with high length-diameter ratio, wherein the mol ratio of above-mentioned substance is as follows: silver nitrate: ethylene glycol: polyvinylpyrrolidone=1:1 ~ 20:0.05 ~ 5.
In step S102, with described silver-colored line obtained in step S101 for conductive silver paste allocated by filler.Particularly, first matrix resin is prepared.In order to reduce the viscosity of formula, promote the dispersion in the epoxy of nanometer silver granuel/line, epoxide resin reactive diluent is with the addition of in formula, after adding this diluent, need the consumption increasing original curing agent, the concrete formula of conducting resinl and preparation technology are adjusted to: be that bisphenol A type epoxy resin, epoxy active diluent and curing agent 4-methylhexahydrophthaacid acid are joined and mixed by the ratio of 1:0.05 ~ 0.5:0.2 ~ 2 according to mass ratio, make the matrix resin of conducting resinl.
After this, the curing accelerator (1-cyano group 2-ethyl 4-methylimidazole 2ZE4MZ-CN) finally adding basis material consumption 1% ~ 3% according to nano-silver thread obtained in mass ratio 1:1 ~ 20:1 mixed matrix material and step S101 again mixes, thus forms conductive silver paste.
In step S103, the conductive silver paste obtained is coated on substrate forms rete in step S102.Can adopt blade coating, lift, described conductive silver paste is coated on described substrate by spin coating mode.Described substrate comprises glass, PET, or PVA.
In step S104, to described rete reprocessing.In the present embodiment, the described substrate base of having plated film to be placed under 100 ~ 350 DEG C of temperature conditions heat treatment 20 ~ 200 minutes, to obtain low resistivity, transparent conducting film.Preferably heat treatment 20 ~ 200 minutes under 200 ~ 300 DEG C of temperature conditions, obtains novel low resistivity, transparent conducting film, and the object of heating the nano-silver thread in film is better contacted because of sintering merge to form continuous print conductive network, reduces resistivity.
Now describe the example of the preparation method according to the embodiment of the present invention in detail.
Embodiment
By 0.10mol silver nitrate, 1.1mol ethylene glycol and 0.08mol polyvinylpyrrolidone, at 160 DEG C of temperature, mix and blend reacts the 60min diameter obtained as shown in Figure 1 is 66nm, and length is the nano-silver thread of 7.4um; Be that bisphenol A type epoxy resin, epoxy active diluent and curing agent 4-methylhexahydrophthaacid acid are joined and mixed by the ratio of 1:0.15:0.9 according to mass ratio, make the matrix resin of conducting resinl; Again according to ratio mixed matrix material and the nano-silver thread prepared above of mass ratio 5:1; The curing accelerator (l cyano group 2-ethyl 4-methylimidazole 2ZE4MZ-CN) finally adding basis material consumption 1.5% mixes.Stand-by.
Utilize automatic coating doctor knife coater to carry out film in the flexible pet sheet face cleaned up, after drying, obtain nano-silver thread wet film.Finally the wet film after drying to be placed under 280 DEG C of temperature conditions heat treatment 35 minutes, to obtain nesa coating.
After tested, the resistivity of this nano-silver thread nesa coating is 1.6 × 10-4 Ω cm, visible light transmissivity 85%, through 200 times 180 ° repeatedly to bend after film without fracture or silver-colored obscission, meet the instructions for uses such as liquid crystal display in electronic information field (LCD), plasma display (PDP), electroluminescent display (EL/OLED), touch-screen (Touch Panel) completely.
The conducting film formed thus as shown in Figure 2.
Compared with prior art, the invention has the advantages that: develop and replace the new technology of spherical nano-Ag particles as the main packing material of conductive silver paste using nano silver wires with high length-diameter ratio, realize reaching conduction object with contacting with each other between line silver-colored in slurry, compared to particle type contact, linear nano silver obviously improves its electric conductivity while raising reliability.In addition, because wire arrangement can realize with less Nano Silver to realize Thin film conductive, therefore production cost have also been obtained and significantly reduces, and this is to Realization of Product large-scale production tool significance.In addition, the conductive silver paste prepared has good impressionability, conductivity and superpower adhesive force, and the film manufactured on this basis integrates transparent, frivolous, bent, slip-off preventing, and this is not available for like product.
More than describe preferred embodiment of the present invention in detail.Should be appreciated that those of ordinary skill in the art just design according to the present invention can make many modifications and variations without the need to creative work.All technical staff in the art, all should by the determined protection range of claims under this invention's idea on the basis of existing technology by the available technical scheme of logical analysis, reasoning, or a limited experiment.
Claims (8)
1. a preparation method for low resistivity, transparent conducting film, is characterized in that, comprises the steps:
A () utilizes silver-colored line Material synthesis nano silver wires with high length-diameter ratio;
B () is filler allotment conductive silver paste with described silver-colored line obtained in step (a);
C the conductive silver paste obtained in step (b) is coated on substrate and forms rete by (); And
D () is to described rete reprocessing.
2. preparation method according to claim 1, it is characterized in that, described silver-colored line raw material comprises silver nitrate, ethylene glycol, and polyvinylpyrrolidone, react 30 ~ 120 minutes at 100 ~ 200 DEG C of temperature, the mol ratio of obtained described nano silver wires with high length-diameter ratio wherein above-mentioned substance is as follows: silver nitrate: ethylene glycol: polyvinylpyrrolidone=1:1 ~ 20:0.05 ~ 5.
3. preparation method according to claim 2, is characterized in that, step (b) comprising:
(b1) matrix resin is prepared;
(b2) described matrix resin and described nano-silver thread is mixed according to mass ratio 1:1 ~ 20:1; And
(b3) curing accelerator adding described matrix resin consumption 1% ~ 3% mixes.
4. preparation method according to claim 3, it is characterized in that, described matrix resin comprises the bisphenol A type epoxy resin that mass ratio is the ratio of 1:0.05 ~ 0.5:0.2 ~ 2, epoxy active diluent, and the mixture of curing agent 4-methylhexahydrophthaacid acid.
5. preparation method according to claim 4, is characterized in that, described curing accelerator comprises (1-cyano group 2-ethyl 4-methylimidazole 2ZE4MZ-CN).
6. preparation method according to claim 1, is characterized in that, with blade coating, lift, described conductive silver paste is coated on described substrate by spin coating mode.
7. preparation method according to claim 1, is characterized in that, described substrate comprises glass, PET, or PVA.
8. preparation method according to claim 1, is characterized in that, the described substrate base of having plated film to be placed under 100 ~ 350 DEG C of temperature conditions heat treatment 20 ~ 200 minutes, to obtain low resistivity, transparent conducting film.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104952551A (en) * | 2015-06-16 | 2015-09-30 | 北京石油化工学院 | Method and equipment for preparing flexible substrate silver nanowire transparent conducting thin film |
| CN106833353A (en) * | 2016-12-21 | 2017-06-13 | 华南理工大学 | A kind of touch-screen UV curing nano silver wire slurries and preparation method thereof |
| CN106910551A (en) * | 2017-02-14 | 2017-06-30 | 哈尔滨工业大学深圳研究生院 | One kind plating metal enhancing nesa coating and preparation method thereof |
| CN111063747A (en) * | 2019-12-25 | 2020-04-24 | 中国科学院苏州纳米技术与纳米仿生研究所 | Low-cost ohmic contact electrode preparation method and solar cell |
| CN111148586A (en) * | 2017-09-27 | 2020-05-12 | 同和电子科技有限公司 | Silver powder mixture, method for producing same, and conductive paste |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101555393A (en) * | 2009-04-03 | 2009-10-14 | 江苏工业学院 | High-temperature resistant one-component isotropic conductive adhesive and preparation method thereof |
| CN102118918A (en) * | 2011-04-12 | 2011-07-06 | 中国计量学院 | Flexible transparent electronic circuit and preparation method thereof |
| CN103440907A (en) * | 2013-09-05 | 2013-12-11 | 中国科学院青岛生物能源与过程研究所 | Cellulose nanofibers and silver nanowires composite conductive film and preparation method of composite conductive film |
| WO2014114828A1 (en) * | 2013-01-28 | 2014-07-31 | Fundacion Itma | Method for obtaining silver nanostructures and nanostructures produced by means of said method |
| CN104099050A (en) * | 2014-07-17 | 2014-10-15 | 深圳市华星光电技术有限公司 | Conductive adhesive preparation method and conductive adhesive |
-
2014
- 2014-10-30 CN CN201410604067.6A patent/CN104332215A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101555393A (en) * | 2009-04-03 | 2009-10-14 | 江苏工业学院 | High-temperature resistant one-component isotropic conductive adhesive and preparation method thereof |
| CN102118918A (en) * | 2011-04-12 | 2011-07-06 | 中国计量学院 | Flexible transparent electronic circuit and preparation method thereof |
| WO2014114828A1 (en) * | 2013-01-28 | 2014-07-31 | Fundacion Itma | Method for obtaining silver nanostructures and nanostructures produced by means of said method |
| CN103440907A (en) * | 2013-09-05 | 2013-12-11 | 中国科学院青岛生物能源与过程研究所 | Cellulose nanofibers and silver nanowires composite conductive film and preparation method of composite conductive film |
| CN104099050A (en) * | 2014-07-17 | 2014-10-15 | 深圳市华星光电技术有限公司 | Conductive adhesive preparation method and conductive adhesive |
Non-Patent Citations (1)
| Title |
|---|
| 宋琼等: ""改性环氧树脂的固化与稀释增韧研究"", 《上海涂料》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104952551A (en) * | 2015-06-16 | 2015-09-30 | 北京石油化工学院 | Method and equipment for preparing flexible substrate silver nanowire transparent conducting thin film |
| CN106833353A (en) * | 2016-12-21 | 2017-06-13 | 华南理工大学 | A kind of touch-screen UV curing nano silver wire slurries and preparation method thereof |
| CN106833353B (en) * | 2016-12-21 | 2019-10-18 | 华南理工大学 | A kind of touch screen UV curing nano silver wire slurry and preparation method thereof |
| CN106910551A (en) * | 2017-02-14 | 2017-06-30 | 哈尔滨工业大学深圳研究生院 | One kind plating metal enhancing nesa coating and preparation method thereof |
| CN106910551B (en) * | 2017-02-14 | 2019-01-08 | 哈尔滨工业大学深圳研究生院 | A kind of plating metal enhancing transparent conductive film and preparation method thereof |
| CN111148586A (en) * | 2017-09-27 | 2020-05-12 | 同和电子科技有限公司 | Silver powder mixture, method for producing same, and conductive paste |
| CN111063747A (en) * | 2019-12-25 | 2020-04-24 | 中国科学院苏州纳米技术与纳米仿生研究所 | Low-cost ohmic contact electrode preparation method and solar cell |
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Application publication date: 20150204 |