CN105086632A - Silver conductive ink in uniform size - Google Patents
Silver conductive ink in uniform size Download PDFInfo
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- CN105086632A CN105086632A CN201510646158.0A CN201510646158A CN105086632A CN 105086632 A CN105086632 A CN 105086632A CN 201510646158 A CN201510646158 A CN 201510646158A CN 105086632 A CN105086632 A CN 105086632A
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Abstract
The invention discloses silver conductive ink in the uniform size. A preparation method of the ink comprises steps as follows: preparation of silver nanowires and particles as well as separation of an organic high-polymer material; preparation of mixed ink; size separation of the ink for obtaining conductive ink in the uniform size; blending of ink concentration. Silver nanomaterials in the prepared ink have the uniform size, and ink in different sizes can be selected according to different requirements. Meanwhile, with the adoption of the preparation method, the problem that a lot of silver materials in improper sizes are abandoned during preparation of most of silver ink is solved, the produced silver nanomaterials are classified and play respective roles, the cost is greatly reduced, and the ink can be widely applied to the field of electronic information products.
Description
Technical field
The invention belongs to conductive ink field, be specifically related to a kind of silver-colored conductive ink of size uniform.
Background technology
In all metals, the conduction of silver and heat conductivility the best, therefore it is widely used in fields such as electronic information.In such applications, silver occurs with forms such as silver powder, silver nano-grain, nano silver wires.Wherein, the neutral gear between nano silver wire makes its consumption much smaller than other ag materials, and then can significantly reduce costs.Meanwhile, the neutral gear between nano silver wire also gives a lot of peculiar property of its film, as good light transmission.Therefore, it is considered to the ideal material that conducting wire builds, and is extensively studied.Such as, in patent CN103008679A, CN104650653A, CN103627255A and CN104464880A, people's nano silver wire and various auxiliary agent have been mixed with the silver-colored conductive ink of difference in functionality, and then prepared silver-colored conductive film with these inks, in a lot of, achieve application.
But different occasion needs the nano silver wire mating different size just can reach the requirement of low cost and high conduction performance.Such as, the nano silver wire for spraying touch-screen conductive film is distinguished, mostly at 10-20 μm to some extent according to the difference of shower nozzle; Nano silver wire for some fine-line (< 6 μm) then requires at 1-5 μm; Nano silver wire for blade coating then can reach 40 μm.But above-mentioned patent nano silver wire used then can not ensure size uniformity.Patent at present about silver nanoparticle ink size uniformity does not then have substantially.Meanwhile, in conventional silver-colored ink preparation process, the silver nano material that a lot of size departs from requirement is rejected, and this greatly adds silver-colored ink cost, is unfavorable for that it is applied.
Therefore, exploitation can be close to the homogeneous silver-colored conductive ink of the silver nano material that 100% utilizes reaction to produce is the problem that solution is needed in conductive ink field badly.
Summary of the invention
The object of the present invention is to provide a kind of silver-colored conductive ink of size uniform, solve the silver nano material waste problem in silver nano material yardstick heterogeneity in current ink and ink production process.In the ink of the present invention's exploitation, silver nano material yardstick is homogeneous.Meanwhile, the silver nano material that reaction produces is close to 100% utilization, greatly reduces the cost of ink.These make these inks can in electronic information field large-scale application.The feature of this ink is, its preparation process is:
(1) preparation of nano silver wire and particle, the separation of organic polymer material;
(2) preparation of mixed ink;
(3) ink apart thus obtain the conductive ink of size uniform;
(4) allotment of body;
(1) in, the preparation process of nano silver wire and particle is: Silver Nitrate and polyvinylpyrrolidone (PVP) are mixed with solution by glycerol, then join in polyvinylpyrrolidonesolution solution by silver nitrate solution, be uniformly mixed.Then mixing solutions is transferred in reactor, reactor is put into the baking oven that temperature has risen to design temperature.After held for some time, take out and put into cold water to be cooled to room temperature pending;
(1) in, the sepn process of organic polymer material is: diluted by silver nano material mother liquor dehydrated alcohol in reactor, centrifuge washing; Then the throw out dehydrated alcohol redilution will obtained, centrifuge washing; By the two times centrifugal washing nearly all glycerol of removing and PVP, obtain the silver nano-grain of different size and the mixing material of nano silver wire.This process notes rotating speed (being greater than 12000 turns), ensure that particle also can deposit;
(2) the consisting of of ink inside: silver nano material content is about 1%.Except silver nano material, ink is also containing dispersion agent, tensio-active agent, flow agent, wetting Agent for Printing Inks and binding agent etc.Solvent comprises water, methyl alcohol, ethanol, Virahol etc.;
(2) preparation steps of ink inside is: determine formula composition, calculate the amount needed for often kind of material.Then weigh all components and add to stir in defoamer and stir 30 minutes, obtain mixed ink;
(3) separation of ink inside relates to our homemade many sized nanostructures material separation returnable bottle.This bottle has large, medium and small three kinds of specifications, and total size of the appendage of its tank body and outside corresponds to the centrifugal bottle size of conventional large, medium and small whizzer.In often kind of returnable bottle, at the bottom of from bottleneck to bottle, have 7 metafiltration films.Filter sizes size is respectively 50 μm, 40 μm, 30 μm, 20 μm, 10 μm, 5 μm and 1 μm from top to bottom.Meanwhile, there is an osculum that can open and shut every metafiltration film position on the upper side a little, and is used for releasing ink;
(3) sepn process of ink inside is: joined by the ink that (2) obtain in Separation and Recovery bottle, centrifugal twice.Then Separation and Recovery bottle is carefully taken out, do not vibrate.From top to bottom, the ink of different layers is released respectively, obtain the conductive ink of size uniform;
(4) in, existing body deterministic process is: choose a small-sized centrifuge tube, weigh m
1.Then from certain ink, take out 2ml ink, weigh m
2.Then add alcohol dilution centrifugal, outwell upper solution, continue repetition twice.Then vacuum drying oven is put into dry 10 minutes.Take out and weigh m
3.Calculate existing silver nano material content (m
3-m
1)/(m
2-m
1);
(4) ink inside concentration allocation process is: according to measuring the content data obtained, and calculates dilution or the concentrated amount needing the solvent adding or remove.If dilution, directly add the solvent of aequum, then stir 30 minutes.If concentrated, then, after solvent being removed a part with Rotary Evaporators, add solvent makeup to required amount.By above means, can obtain size uniform, silver nano material content about 1% silver-colored conductive ink;
The present invention has the following advantages: in (1) ink, the yardstick of silver nano material is homogeneous, can select most suitable silver-colored conductive ink according to different occasion; (2) be close to the silver nano material that 100% make use of reaction generation in ink preparation process, thus ink cost is low; (3) preparation process is simple, and production unit requires low, is applicable to scale operation.
Accompanying drawing explanation
Fig. 1: many sized nanostructures material separation returnable bottle structural representation;
Specific embodiment
Embodiment:
By Silver Nitrate and polyvinylpyrrolidone (PVP, M
w> > 1300000) be mixed with solution by glycerol, then silver nitrate solution is joined in polyvinylpyrrolidonesolution solution, be uniformly mixed.Then mixing solutions is transferred in reactor, reactor is put into the baking oven that temperature has risen to design temperature (170 ~ 200 DEG C).After held for some time, take out and put into cold water to be cooled to room temperature pending;
Diluted by silver nano material mother liquor dehydrated alcohol in reactor, centrifugal (rotating speed is greater than 12000) washs; Then the throw out dehydrated alcohol obtained is diluted redilution, centrifuge washing; By the two times centrifugal washing nearly all glycerol of removing and PVP, obtain the silver nano-grain of different size and the mixing material of nano silver wire;
Select that ZonylFSO-100 is tensio-active agent, 2-amino-2-methyl-1-propanol is dispersion anti-settling agent, propylene glycol monomethyl ether is flow agent, hexalin is wetting Agent for Printing Inks, 2-hexyl ethanol is defoamer, Virahol is that solvent is to prepare slurry.Determine ink composition (1% silver nano material content), the amount needed for calculating.Then these materials and the silver nano material mix and blend in stirring defoamer that take aequum obtain silver-colored mixed ink;
Mixed ink is joined in many sized nanostructures material separation returnable bottle.After centrifugal twice, Separation and Recovery bottle is carefully taken out, does not vibrate.From top to bottom, the ink of different layers is released respectively, obtain the conductive ink of size uniform;
The content of silver nano material in certain ink of survey calculation.According to its gap from 1% silver nano material content, dilution or concentrated solvent, obtain the silver-colored conductive ink of the size uniformity of 1% silver nano material content.
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 technician in the art, all should by the determined protection domain of claims under this invention's idea on the basis of existing technology by the available experiment of logical analysis, reasoning, or a limited experiment and technical scheme.
Claims (9)
1. a silver-colored conductive ink for size uniform, is characterized in that, its preparation process is:
(1) preparation of nano silver wire and particle, the separation of organic polymer material;
(2) preparation of mixed ink;
(3) ink apart thus obtain the conductive ink of size uniform;
(4) allotment of body.
2. silver-colored conductive ink according to claim 1, it is characterized in that: in (1), the preparation process of nano silver wire and particle is: Silver Nitrate and polyvinylpyrrolidone (PVP) are mixed with solution by glycerol, then silver nitrate solution is joined in polyvinylpyrrolidonesolution solution, be uniformly mixed; Then mixing solutions is transferred in reactor, reactor is put into the baking oven that temperature has risen to design temperature; After held for some time, take out and put into cold water to be cooled to room temperature pending.
3. silver-colored conductive ink according to claim 1, is characterized in that: in (1), the sepn process of organic polymer material is: diluted by silver nano material mother liquor dehydrated alcohol in reactor, centrifuge washing; Then the throw out dehydrated alcohol redilution will obtained, centrifuge washing; By the two times centrifugal washing nearly all glycerol of removing and PVP, obtain the silver nano-grain of different size and the mixing material of nano silver wire; This process notes rotating speed, ensure that particle also can deposit.
4. silver-colored conductive ink according to claim 1, is characterized in that: consisting of of (2) ink inside: silver nano material content is about 1%; Except silver nano material, ink is also containing dispersion agent, tensio-active agent, flow agent, wetting Agent for Printing Inks and binding agent etc.; Solvent comprises water, methyl alcohol, ethanol, Virahol etc.
5. silver-colored conductive ink according to claim 1, is characterized in that: the preparation steps of (2) ink inside is: determine formula composition, calculate the amount needed for often kind of material; Then weighing all components joins to stir in defoamer and stirs 30 minutes, obtains mixed ink.
6. silver-colored conductive ink according to claim 1, is characterized in that: the separation of (3) ink inside relates to uses our homemade many sized nanostructures material separation returnable bottle; This bottle has large, medium and small three kinds of specifications, and total size of the appendage of its tank body and outside corresponds to the centrifugal bottle size of conventional large, medium and small whizzer; In often kind of returnable bottle, at the bottom of from bottleneck to bottle, have 7 metafiltration films; Filter sizes size is respectively 50 μm, 40 μm, 30 μm, 20 μm, 10 μm, 5 μm and 1 μm from top to bottom; Meanwhile, there is an osculum that can open and shut every metafiltration film position on the upper side a little, and is used for releasing ink.
7. silver-colored conductive ink according to claim 1, is characterized in that: the sepn process of (3) ink inside is: joined by the ink that (2) obtain in Separation and Recovery bottle, centrifugal twice; Then Separation and Recovery bottle is carefully taken out, do not vibrate; From top to bottom, the ink of different layers is released respectively, obtain the conductive ink of size uniform.
8. silver-colored conductive ink according to claim 1, is characterized in that: in (4), existing body deterministic process is: choose a small-sized centrifuge tube, weigh m
1; Then from certain ink, take out 2ml ink, weigh m
2; Then add alcohol dilution centrifugal, outwell upper solution, continue repetition twice; Then vacuum drying oven is put into dry 10 minutes; Take out and weigh m
3; Calculate existing silver nano material content (m
3-m
1)/(m
2-m
1).
9. silver-colored conductive ink according to claim 1, is characterized in that: (4) ink inside concentration allocation process is: according to measuring the content data obtained, and calculates dilution or the concentrated amount needing the solvent adding or remove; If dilution, directly add the solvent of aequum, then stir 30 minutes; If concentrated, then, after solvent being removed a part with Rotary Evaporators, add solvent makeup to required amount; By above means, can obtain size uniform, silver nano material content about 1% silver-colored conductive ink.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106366770A (en) * | 2016-09-22 | 2017-02-01 | 嘉兴学院 | Multi-sized nano-silver conductive ink and rapid preparation method thereof |
CN109370316A (en) * | 2018-10-16 | 2019-02-22 | 嘉兴学院 | Two-step method prepares the method and conductive ink of highly concentrated nano Argent grain conductive ink |
CN109465440A (en) * | 2018-11-08 | 2019-03-15 | 陕西煤业化工技术研究院有限责任公司 | A method of it is separated for silver nanowires length |
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CN101921505A (en) * | 2010-03-25 | 2010-12-22 | 江苏工业学院 | Conductive printing ink composite for printing of wireless radio frequency identification devices (RFID) |
CN102015921A (en) * | 2008-02-26 | 2011-04-13 | 凯博瑞奥斯技术公司 | Method and composition for screen printing of conductive features |
CN102575117A (en) * | 2009-08-24 | 2012-07-11 | 凯博瑞奥斯技术公司 | Purification of metal nanostructures for improved haze in transparent conductors made from the same |
CN103408993A (en) * | 2013-03-30 | 2013-11-27 | 深圳欧菲光科技股份有限公司 | Conductive ink, transparent conductor and preparation method thereof |
CN103443213A (en) * | 2010-10-22 | 2013-12-11 | 凯博瑞奥斯技术公司 | Nanowire ink compositions and printing of same |
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2015
- 2015-10-09 CN CN201510646158.0A patent/CN105086632A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102015921A (en) * | 2008-02-26 | 2011-04-13 | 凯博瑞奥斯技术公司 | Method and composition for screen printing of conductive features |
CN102575117A (en) * | 2009-08-24 | 2012-07-11 | 凯博瑞奥斯技术公司 | Purification of metal nanostructures for improved haze in transparent conductors made from the same |
CN101921505A (en) * | 2010-03-25 | 2010-12-22 | 江苏工业学院 | Conductive printing ink composite for printing of wireless radio frequency identification devices (RFID) |
CN103443213A (en) * | 2010-10-22 | 2013-12-11 | 凯博瑞奥斯技术公司 | Nanowire ink compositions and printing of same |
CN103408993A (en) * | 2013-03-30 | 2013-11-27 | 深圳欧菲光科技股份有限公司 | Conductive ink, transparent conductor and preparation method thereof |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106366770A (en) * | 2016-09-22 | 2017-02-01 | 嘉兴学院 | Multi-sized nano-silver conductive ink and rapid preparation method thereof |
CN106366770B (en) * | 2016-09-22 | 2019-05-28 | 嘉兴学院 | A kind of more sized nanostructures silver conductive inks and its fast preparation method |
CN109370316A (en) * | 2018-10-16 | 2019-02-22 | 嘉兴学院 | Two-step method prepares the method and conductive ink of highly concentrated nano Argent grain conductive ink |
CN109465440A (en) * | 2018-11-08 | 2019-03-15 | 陕西煤业化工技术研究院有限责任公司 | A method of it is separated for silver nanowires length |
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