CN101812181A - Nano silver dispersion and jet printing ink - Google Patents
Nano silver dispersion and jet printing ink Download PDFInfo
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- CN101812181A CN101812181A CN 200910007847 CN200910007847A CN101812181A CN 101812181 A CN101812181 A CN 101812181A CN 200910007847 CN200910007847 CN 200910007847 CN 200910007847 A CN200910007847 A CN 200910007847A CN 101812181 A CN101812181 A CN 101812181A
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- nano silver
- sulphonate
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Abstract
The invention provides a nano silver dispersion comprising sulfonate base water dispersible polyester which is a random copolymer with the molecular formula as follows: R1 or R2 independently comprises OCH2CH2, OCH2CH2CH2CH2 or nano silver solution. The invention also provides a jet printing ink comprising the nano silver dispersion.
Description
Technical field
The present invention relate to a kind of can be with the homodisperse nano silver dispersion of nanometer silver, and be particularly related to a kind of ink-jet ink that comprises this nano silver dispersion, its electroconductibility is good and to the strong adhesion of base material.
Background technology
Because spraying print preparing process possesses energy-conservation and advantage material-saving, therefore at present just active development it, intend replacing the yellow optical micro-image preparation technology of the electronics/opto-electronics now of the spray printing photoresistance used with transparency electrode, PCB with brightening diffusion sheet, photoelectric subassembly with spectral filter, LCD such as LCD, led chip encapsulation etc.And if silver-colored lead can form and will bigger benefit be arranged to industry with spraying print preparing process, and the most important critical material of this preparation technology is the high conduction of tool, stable dispersion and the conductive ink that can adhere to base material.
The existing problem of conductive ink comprises ink dispersion stabilization deficiency now, and for conductive ink can firmly be attached on the base material, metropolitan is in wherein adding resin (binding agent, binder) so that nano silver particles in the conductive ink and base material close attachment, but since resin (binding agent) so can reduce the conductance of conductive ink for isolator.Therefore in order to overcome problems such as above-mentioned, many relevant researchs are arranged in recent years.
The nano particle that U.S. Patent Publication No. US 2006/0044382 describes with Ag-Pd alloy (Pd content 10-40%) is mixed with conductive ink, and it can overcome the breaking phenomena that environment caused of general conductive silver ink at hot and humid degree.In addition, be in this invention with dodecane sulfonic acid sodium (sodium dodecyl sulfate) as dispersion agent, but be that small molecules type dispersion agent is poor to the base material tack because of it.
The U.S. Patent Publication No. US 2007/0283848 open different content of nanometer silver that add 20-85wt% of utilizing mix the different inks (2-100cps) of viscosity, and the dispersion agent of its adding is the glycerols solvent, so but be that small molecules type dispersion agent is not good to the base material tack yet because of it.
U.S. Patent Publication No. US 2007/0244220 discloses a conductive ink and contains the macromolecule dispersing agent of aminocompound derivative and nitrogenous oxygen by interpolation with stably dispersing silver.And its open utilization is improved silver content with the lifting conductance, but because of it is nitrogenous oxygen type dispersion agent, can cause unstable to the acidic system nano silver dispersion that has prepared.
Summary of the invention
The object of the present invention is to provide a kind of nano silver dispersion of high stability.
Another object of the present invention is to provide a kind of electroconductibility good and to ink-jet ink strong adhesion, that comprise this nano silver dispersion of base material.
The invention provides a kind of nano silver dispersion, comprising in order to dispersing nanometer silver: monosulfonic acid alkali water dispersible polyester, this sulphonate-base water-dispersion polyester is a random copolymers, its molecular formula is:
The present invention also provides a kind of ink-jet ink, comprising: monosulfonic acid alkali water dispersible polyester, and this sulphonate-base water-dispersion polyester is a random copolymers, its molecular formula is:
Therefore the invention has the advantages that: the dispersion agent in the nano silver dispersion of the present invention not only has the sulphur atom strong to silver-colored adsorptivity, and can be scattered in the water, and nano silver dispersion of the present invention can allow nano silver particles stable and be dispersed in the water; And ink-jet ink of the present invention, on the one hand owing to the sulphonate-base water-dispersion polyester as dispersion agent can adhere to base material, therefore make ink-jet ink to fit tightly with base material, on the other hand because sulphonate-base water-dispersion polyester is not that nano silver particles is coated, and only be to be adsorbed in nano silver particles, therefore the space that can see through between dispersion agent between nano silver particles contacts with each other, and keeps good electrical conductivity
For above and other objects of the present invention, feature and advantage can be become apparent, preferred embodiment cited below particularly, and cooperate appended accompanying drawing, be described in detail below:
Description of drawings
Fig. 1 shows that ink-jet ink of the present invention is attached on the base material and keeps the synoptic diagram of satisfactory electrical conductivity;
Wherein, primary clustering nomenclature:
101～base material, 103～ink-jet ink
105～sulphonate-base water-dispersion polyester (dispersion agent)
The signal route of 107～nano silver particles 109～conduction.
Embodiment
Nano silver dispersion in order to dispersing nanometer silver of the present invention, it is filled a prescription in detail and is formulated as follows described.
At first monosulfonic acid alkali water dispersible polyester is added in the suitable quantity of water, heat afterwards and stir, make its dissolving and form the monosulfonic acid alkali water dispersible polyester aqueous solution.And above-mentioned sulphonate-base water-dispersion polyester is a random copolymers, and its molecular formula is:
The sulphonate-base water-dispersion polyester aqueous solution of being prepared, its sulphonate-base water-dispersion amount of polyester can be about 5-50wt%, is about 30wt% in one embodiment.And the sulfonate content of this sulphonate-base water-dispersion polyester for this reason sulphonate-base water disperse about 13.5-70mol% of polyester, in one embodiment, the sulfonate content of sulphonate-base water-dispersion polyester is about 13.5mol%.The weight-average molecular weight of sulphonate-base water-dispersion polyester is about 4000-8000.Again in one embodiment, the sulphonate-base water-dispersion polyester of the above-mentioned molecular formula of employed tool, its R
1With R
2All be OCH
2CH
2
And because sulphonate-base water-dispersion polyester not only has the sulphur atom strong to silver-colored adsorptivity, and can be scattered in the water, therefore come preparation of nano silver dispersion liquid can allow nano silver particles stable and be dispersed in the water as a dispersion agent it.
Then the sulphonate-base water-dispersion polyester aqueous solution is added in the Nano silver solution to form the nano silver dispersion in order to dispersing nanometer silver of the present invention.And in nano silver dispersion of the present invention, the content of sulphonate-base water-dispersion polyester is about 0.1-6wt%, and the content of Nano silver solution is about 94-99.9wt%.Wherein the composition of above-mentioned Nano silver solution comprises silver, water and stablizer.Stablizer can be polyvinyl alcohol (polyvinylalcohol, PVA), glycol ether (diethylene glycol, DEG) or glycerine.In Nano silver solution, silver accounts for about 5-50%, water accounts for about 47-94.9%, and the about 0.1-3% of stabilizer comprises.In one embodiment, employed Nano silver solution comprises 20% silver, 78.5% water and 1.5% stablizer.
Again, sulphonate-base water-dispersion polyester as dispersion agent has good tack for base material, therefore the above-mentioned nano silver dispersion spray printing in order to dispersing nanometer silver is fixed on the base material, then it is carried out hundred lattice adhesive tape tests (ASTM D3359-93), its tack to base material can reach more than 3 grades, be preferably more than 4 grades, be more preferred from 5 grades.And base material can comprise plastic basis material, general paper wood or photograph paper wood.
It is to utilize the above-mentioned ink-jet ink that nano silver dispersion was mixed with in order to dispersing nanometer silver that of the present invention another implemented the sample attitude.
And being formulated as of ink-jet ink adds a wetting Agent for Printing Inks after the above-mentioned nano silver dispersion in order to dispersing nanometer silver mixes, and promptly forms ink-jet ink of the present invention.Wetting Agent for Printing Inks can be 2-Pyrrolidone (2-pyrolidone), glycol ether or glycerine.In one embodiment, the content of ink-jet ink sulphonate-base water-dispersion polyester of the present invention is about 0.1-1.5wt%, and the content of Nano silver solution is about 5-15wt% for the content of about 83.5-94.9wt% and this wetting Agent for Printing Inks.
In another embodiment, the composition of ink-jet ink also can add an additive except that above-mentioned composition, fit property in order to adjust ink-jet, and additive can comprise the multipolymer of tool pigment affinity group, for example DISPERBYK
-192 (BYK Chemie), or tool ether modified dimethyl polysiloxane, for example BYK333 (BYK Chemie).And in this embodiment, the content of ink-jet ink sulphonate-base water-dispersion polyester is about 0.1-2.0wt%, and the content of Nano silver solution is that the content of about 76-94.89wt%, wetting Agent for Printing Inks is that about 5-20wt% and content of additive are about 0.01-2wt%.
Again, referring to Fig. 1.Fig. 1 shows that ink-jet ink of the present invention is attached on the base material and keeps the synoptic diagram of satisfactory electrical conductivity.In ink-jet ink 103 of the present invention,, therefore can fit tightly with base material 101 owing to can adhere to base material 101 as the sulphonate-base water-dispersion polyester 105 of dispersion agent.Sulphonate-base water-dispersion polyester 105 is not that nano silver particles 107 is coated again, and only is to be adsorbed in nano silver particles 107, so the spaces that 107 of nano silver particles can see through 105 of dispersion agents contact with each other, and keeps good electrical conductivity.The signal route of conduction is shown in curve 109.
Therefore, will be fixed on the base material according to above-mentioned formed ink-jet ink, and then it be carried out hundred lattice adhesive tape tests (ASTM D3359-93), its tack to base material can reach more than 3 grades, is preferably more than 4 grades, is more preferred from 5 grades.And base material can comprise plastic basis material, general paper wood or photograph paper wood.And in one embodiment, the electroconductibility of ink-jet ink of the present invention represents with sheet resistance, and when the spray printing thickness of ink-jet ink of the present invention is 1 μ m when thick, its sheet resistance can be less than about 42.0 (Ω/mouth), preferable can be less than about 14.6 (Ω/).
[embodiment] nano silver dispersion
1. prepare the sulphonate-base water-dispersion polyester aqueous solution
(1) takes by weighing the sulphonate-base water-dispersion polyester of 60g
(2) be heated to 80-90 ℃, and stirring and dissolving.
(3) be mixed with the sulphonate-base water-dispersion polyester aqueous solution that content is 30wt%.
2. preparation of nano silver dispersion liquid embodiment 1-9
As shown in table 1, take by weighing the required 30wt% sulphonate-base water-dispersion polyester aqueous solution addition (dispersion soln addition) of embodiment 1-9 respectively, add Nano silver solution AG-100-20 (composition: silver 20% respectively again; Water 78.5%; Stablizer 1.5%) in, being formulated as total amount all is the nano silver dispersion embodiment 1-9 of 10g.
3. preparation of nano silver dispersion liquid comparative example 1-3
(1) the nano silver dispersion comparative example 1
Directly use Nano silver solution AG-100-20 (composition: silver 20%; Water 78.5%; Stablizer 1.5%), do not import dispersion agent
(2) nano silver dispersion comparative example 2-3
As shown in table 1, take by weighing the required dispersion agent addition of comparative example 2-3 (dispersion soln addition) respectively, add Nano silver solution AG-100-20 (composition: silver 20% respectively again; Water 78.5%; Stablizer 1.5%) in, being formulated as total amount all is the nano silver dispersion comparative example 2-3 of 10g.
4. the embodiment of nano silver dispersion and comparative example are tested the base material tack
Embodiment 1-9 and comparative example 1-3 with nano silver dispersion is individually fixed in paper and polyethylene terephthalate base material respectively, test its tack to paper and polyethylene terephthalate base material with adhesive tape hundred lattice tests (ASTM D3359-93) then, test result is as shown in table 1.
The embodiment of table 1, nano silver dispersion and comparative example
Ink-jet ink
1. prepare ink-jet ink embodiment A-F
As shown in table 2, weigh the amount of the required wetting Agent for Printing Inks of embodiment A-F (DEG) and water respectively and mix, again with its as shown in table 2 adding respectively among the above embodiments 2-7, be about to ink-jet ink embodiment A-E preparation and finish.
2. prepare ink-jet ink Comparative examples A-C
(1) ink-jet ink Comparative examples A
After 1.5g wetting Agent for Printing Inks (DEG) and 1g water mixed, directly import Nano silver solution AG-100-20 (composition: silver 20%; Water 78.5%; Stablizer 1.5%) in.
(2) ink-jet ink comparative example B-C
As shown in table 2, take by weighing the amount of the required wetting Agent for Printing Inks of comparative example B-C (DEG) and water respectively and mix, again with its as shown in table 2 adding respectively among the above-mentioned comparative example 2-3, be about to ink-jet ink comparative example B-C preparation and finish.
3. the embodiment of ink-jet ink and comparative example are tested the base material tack
Embodiment A-F and Comparative examples A-C with ink-jet ink is fixed in paper and polyethylene terephthalate base material respectively, test it to the tack of photo paper (Mitsubishi) with polyethylene terephthalate base material (PET film) with adhesive tape hundred lattice tests (ASTM D3359-93) then, test result is as shown in table 2.
4. the electroconductibility of the embodiment of ink-jet ink and comparative example test test
Respectively with the embodiment A-F of ink-jet ink and Comparative examples A-C spray printing in photo paper, carry out the electroconductibility test then, test result is as shown in table 2.
The embodiment of table 2, ink-jet ink and comparative example
Zero: no sedimentation takes place
△: a little sedimentation takes place
X: mostly be sedimentation greatly
Though the present invention with preferred embodiment openly as above; right its is not in order to limit the present invention; any person skilled in the art; without departing from the spirit and scope of the present invention; when can doing a little change and retouching, so protection scope of the present invention is as the criterion when looking the scope that the accompanying Claim book defined.
Claims (20)
1. nano silver dispersion comprises:
Monosulfonic acid alkali water dispersible polyester, described sulphonate-base water-dispersion polyester is a random copolymers, its molecular formula is:
R wherein
1With R
2Be OCH independently
2CH
2, OCH
2CH
2CH
2CH
2Or
And
One Nano silver solution.
2. nano silver dispersion according to claim 1, the content of wherein said sulphonate-base water-dispersion polyester is 0.1-6wt%, the content of described Nano silver solution is 94-99.9wt%.
3. nano silver dispersion according to claim 1, the sulfonate content of wherein said sulphonate-base water-dispersion polyester are the 13.5-70mol% of described sulphonate-base water-dispersion polyester.
4. nano silver dispersion according to claim 1, the weight-average molecular weight of wherein said sulphonate-base water-dispersion polyester is 4000-8000.
5. nano silver dispersion according to claim 1, wherein said Nano silver solution consist of silver, water and stablizer.
6. nano silver dispersion according to claim 5, wherein said stablizer are polyvinyl alcohol, glycol ether or glycerine.
7. nano silver dispersion according to claim 1, wherein said nano silver dispersion is used for the base material attached to plastics, paper wood or photograph.
8. nano silver dispersion according to claim 7, wherein said plastics are polyethylene terephthalate.
9. ink-jet ink comprises:
Monosulfonic acid alkali water dispersible polyester, described sulphonate-base water-dispersion polyester is a random copolymers, its molecular formula is:
R wherein
1With R
2Be OCH independently
2CH
2, OCH
2CH
2CH
2CH
2Or
One Nano silver solution; And
One wetting Agent for Printing Inks.
10. ink-jet ink according to claim 9, the content of wherein said sulphonate-base water-dispersion polyester is 0.1-1.5wt%, the content of described Nano silver solution is that the content of 83.5-94.9wt% and described wetting Agent for Printing Inks is 5-15wt%.
11. ink-jet ink according to claim 9, the sulfonate content of wherein said sulphonate-base water-dispersion polyester are the 13.5-70mol% of described sulphonate-base water-dispersion polyester.
12. ink-jet ink according to claim 9, the weight-average molecular weight of wherein said sulphonate-base water-dispersion polyester is 4000-8000.
13. ink-jet ink according to claim 9, the composition of wherein said Nano silver solution comprises silver, water and stablizer.
14. ink-jet ink according to claim 13, wherein said stablizer are polyvinyl alcohol, glycol ether or glycerine.
15. ink-jet ink according to claim 9, wherein said wetting Agent for Printing Inks are 2-Pyrrolidone, glycol ether or glycerine.
16. ink-jet ink according to claim 9 also comprises an additive, in order to adjust the suitable property of ink-jet.
17. ink-jet ink according to claim 16, the content of wherein said sulphonate-base water-dispersion polyester is 0.1-2.0wt%, and the content of described Nano silver solution is that the content of 76-94.89wt%, described wetting Agent for Printing Inks is that 5-20wt% and described content of additive are 0.01-2wt%.
18. ink-jet ink according to claim 16, wherein said additive are the multipolymer or the tool ether modified dimethyl polysiloxane of tool pigment affinity group.
19. ink-jet ink according to claim 9, wherein said ink-jet ink is used for the base material attached to plastics, paper wood or photograph.
20. ink-jet ink according to claim 19, wherein said plastics are polyethylene terephthalate.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910007847 CN101812181A (en) | 2009-02-19 | 2009-02-19 | Nano silver dispersion and jet printing ink |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910007847 CN101812181A (en) | 2009-02-19 | 2009-02-19 | Nano silver dispersion and jet printing ink |
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| CN101812181A true CN101812181A (en) | 2010-08-25 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103694778A (en) * | 2013-12-11 | 2014-04-02 | 苏州谊恒印务有限公司 | Silver nano ink |
| JP2016089164A (en) * | 2014-11-03 | 2016-05-23 | ゼロックス コーポレイションＸｅｒｏｘ Ｃｏｒｐｏｒａｔｉｏｎ | Metal nanoparticle-sulfonated polyester composite and environmentally-friendly method of making the same |
| JP2016135918A (en) * | 2015-01-23 | 2016-07-28 | ゼロックス コーポレイションＸｅｒｏｘ Ｃｏｒｐｏｒａｔｉｏｎ | Preparation method of metal nano-dendrimer structure |
| KR20160131890A (en) * | 2015-05-07 | 2016-11-16 | 제록스 코포레이션 | Anti-bacterial aqueous ink compositions comprising self-dispersed sulfonated polyester-silver nanoparticle composites |
| CN107000065A (en) * | 2014-12-26 | 2017-08-01 | 昭和电工株式会社 | The manufacture method of nano silver wire, the nano silver wire obtained by this method and the ink containing the nano silver wire |
| US10007200B2 (en) | 2015-05-07 | 2018-06-26 | Xerox Corporation | Antimicrobial toner |
| CN112275034A (en) * | 2020-09-27 | 2021-01-29 | 华南理工大学 | Electrofluid printing-based silver filter element and preparation method and application thereof |
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2009
- 2009-02-19 CN CN 200910007847 patent/CN101812181A/en active Pending
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103694778A (en) * | 2013-12-11 | 2014-04-02 | 苏州谊恒印务有限公司 | Silver nano ink |
| JP2016089164A (en) * | 2014-11-03 | 2016-05-23 | ゼロックス コーポレイションＸｅｒｏｘ Ｃｏｒｐｏｒａｔｉｏｎ | Metal nanoparticle-sulfonated polyester composite and environmentally-friendly method of making the same |
| US9458305B2 (en) * | 2014-11-03 | 2016-10-04 | Xerox Corporation | Metal nanoparticle-sulfonated polyester composites and green methods of making the same |
| CN107000065B (en) * | 2014-12-26 | 2019-12-27 | 昭和电工株式会社 | Method for producing silver nanowire, silver nanowire obtained by the method, and ink containing the silver nanowire |
| TWI682406B (en) * | 2014-12-26 | 2020-01-11 | 日商昭和電工股份有限公司 | Production method of silver nanowire, silver nanowire produced by production method and ink comprising silver nanowire |
| CN107000065A (en) * | 2014-12-26 | 2017-08-01 | 昭和电工株式会社 | The manufacture method of nano silver wire, the nano silver wire obtained by this method and the ink containing the nano silver wire |
| JP2016135918A (en) * | 2015-01-23 | 2016-07-28 | ゼロックス コーポレイションＸｅｒｏｘ Ｃｏｒｐｏｒａｔｉｏｎ | Preparation method of metal nano-dendrimer structure |
| US9518156B2 (en) * | 2015-01-23 | 2016-12-13 | Xerox Corporation | Methods of preparing metal nanodendrimer structures |
| US9777124B2 (en) | 2015-01-23 | 2017-10-03 | Xerox Corporation | Methods of preparing metal nanodendrimer structures |
| KR20160131890A (en) * | 2015-05-07 | 2016-11-16 | 제록스 코포레이션 | Anti-bacterial aqueous ink compositions comprising self-dispersed sulfonated polyester-silver nanoparticle composites |
| US10007200B2 (en) | 2015-05-07 | 2018-06-26 | Xerox Corporation | Antimicrobial toner |
| JP2016210968A (en) * | 2015-05-07 | 2016-12-15 | ゼロックス コーポレイションＸｅｒｏｘ Ｃｏｒｐｏｒａｔｉｏｎ | Anti-bacterial aqueous ink compositions comprising self-dispersed sulfonated polyester-silver nanoparticle composites |
| KR102338549B1 (en) * | 2015-05-07 | 2021-12-14 | 제록스 코포레이션 | Anti-bacterial aqueous ink compositions comprising self-dispersed sulfonated polyester-silver nanoparticle composites |
| DE102016206831B4 (en) | 2015-05-07 | 2022-08-04 | Xerox Corporation | Aqueous ink composition and process |
| CN112275034A (en) * | 2020-09-27 | 2021-01-29 | 华南理工大学 | Electrofluid printing-based silver filter element and preparation method and application thereof |
| CN112275034B (en) * | 2020-09-27 | 2021-08-10 | 华南理工大学 | Electrofluid printing-based silver filter element and preparation method and application thereof |
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