CN103613986A - Preparation method of nano graphite conductive ink - Google Patents

Preparation method of nano graphite conductive ink Download PDF

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Publication number
CN103613986A
CN103613986A CN201310625014.8A CN201310625014A CN103613986A CN 103613986 A CN103613986 A CN 103613986A CN 201310625014 A CN201310625014 A CN 201310625014A CN 103613986 A CN103613986 A CN 103613986A
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CN
China
Prior art keywords
nano
preparation
conductive ink
electrically conductive
byk
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Pending
Application number
CN201310625014.8A
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Chinese (zh)
Inventor
何勇
储婷婷
叶斌
钱建平
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WEIDISEN INK CO Ltd ZHANGJIAGANG CITY
Original Assignee
WEIDISEN INK CO Ltd ZHANGJIAGANG CITY
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Priority to CN201310625014.8A priority Critical patent/CN103613986A/en
Publication of CN103613986A publication Critical patent/CN103613986A/en
Pending legal-status Critical Current

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Abstract

The invention discloses a preparation method of a nano graphite conductive ink. The preparation method comprises the steps of adding nano silver particles, sodium carboxymethylcellulose, hydroxyethyl cellulose, BYK-024, BYK-028, Surfynol 465 and a pigment into a solution including glycerol and glycol, mixing and stirring; then performing ultrasonic dispersion and filtration to obtain the nano graphite conductive ink. According to the preparation method disclosed by the invention, all the components are balanced in matching, and the ink is excellent in conductivity. The sodium carboxymethylcellulose and hydroxyethyl cellulose are added to serve as a binding agent, so that the stability of the ink is increased.

Description

A kind of preparation method of nano-graphite electrically conductive ink
Technical field
The invention belongs to technical field of ink, be specifically related to a kind of preparation method of nano-graphite electrically conductive ink.
Background technology
Granule type conductive ink mainly comprises graphite based conducting ink and metal matrix base conductive ink.The conductive compositions of graphite based conducting ink is mainly carbon nanotube and Graphene, due to existing manufacturing processing technic, cause carbon nanotube and graphene-structured defect, had a strong impact on the electroconductibility of carbon nanotube and Graphene, make graphite based conducting ink electroconductibility poor, be generally not used in and make low-resistance electro-conductive material.Therefore in conductive ink, applying more is metal matrix conductive ink, comprises gold and silver, copper, platinum etc.Wherein, due to gold and platinum expensive, its application is subject to many limitations; And although copper has high electroconductibility and relative cheap cost, its chemical property ripple comparatively alive, easily oxidation, its application is subject to certain limitation equally; Silver has the electroconductibility of superelevation, stronger unreactiveness, good resistance of oxidation, and it receives much concern in the research of conductive ink.
Summary of the invention
Technical problem to be solved by this invention is: the nano-graphite electrically conductive ink that a kind of conductivity is good is provided.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method of nano-graphite electrically conductive ink: its step: by nano-Ag particles, Xylo-Mucine, Natvosol, BYK-024(Guangzhou Yi Tong macromolecular material company limited), BYK-028(Guangzhou Yi Tong macromolecular material company limited), Surfynol 465(Guangzhou Lian Gu fine chemistry company limited), pigment joins mix and blend in glycerol and ethylene glycol solution, carry out again ultrasonic dispersion, filter, obtain nano-graphite electrically conductive ink.
Mass ratio between described nano-Ag particles, Xylo-Mucine, Natvosol, BYK-024, BYK-028, Surfynol 465, pigment, glycerol, ethylene glycol is: 1:0.2~0.4:0.1~0.3:0.6~0.8:0.4~0.8:0.4~0.6:0.08~0.12:4.0~6.0:3.0~5.0.
The preparation method of described nano-Ag particles, the steps include: Silver Nitrate and polyvinylpyrrolidone to be added to the water dissolving; By concentration, be that 50~60mg/mL sodium borohydride solution is added dropwise in silver nitrate solution, rate of addition is 3~6mL/min; After dropwising, filter, get filtrate centrifugation, acetone soln cleaning, centrifugation, cleaning repeatable operation at least 3 times, centrifugal speed 800~1000rpm, each centrifugation time 7~8min; Centrifugal product is placed in loft drier and is dried, and drying temperature is 40~45 ℃, and time of drying, 7~8h, obtained nano-Ag particles.
The molar ratio of described Silver Nitrate, polyvinylpyrrolidone, sodium borohydride is: 1:0.3~0.5:2.4~2.8.
The particle diameter of described nano-Ag particles is less than 2nm.
Described pigment is a kind of in following substances: C.I. is directly black 166, and C.I. is directly black 19, and C.I. is directly black 168, C.I. acid yellow 23, C.I. Xylene Red 52, C.I. acid blue 9.
Beneficial effect of the present invention: complex equilibrium between each component in the present invention, ink conductivity is good.In the present invention, added Xylo-Mucine and Natvosol as tackiness agent, the stability of ink is increased.
Embodiment
Embodiment 1
5mol Silver Nitrate and 1.5mol polyvinylpyrrolidone are added in 800mL water and dissolved, be stirred to solution and be water white transparency; By concentration, be that 50~60mg/mL sodium borohydride (12mol) solution is added dropwise in silver nitrate solution, rate of addition is 3~6mL/min; After dropwising, filter, get filtrate centrifugal, acetone soln (200mL * 3 time) cleans, eccentric cleaning repeatable operation 3 times, centrifugal speed 900rpm, each centrifugation time 7min; Centrifugal product is placed in loft drier and is dried, and drying temperature is 40~45 ℃, and time of drying, 7h, obtained nano-Ag particles.
Nano-Ag particles 100g, Xylo-Mucine 30g, Natvosol 13g, BYK-02470g, BYK-02850g, Surfynol 46550g, pigment 10g are joined to mix and blend in glycerol 500g and ethylene glycol 450g, carry out again ultrasonic dispersion, filter, obtain nano silver conductive ink.
Embodiment 2
3mol Silver Nitrate and 1mol polyvinylpyrrolidone are added in 400mL water and dissolved, be stirred to solution and be water white transparency; By concentration, be that 50~60mg/mL sodium borohydride (8mol) solution is added dropwise in silver nitrate solution, rate of addition is 3~6mL/min; After dropwising, filter, get filtrate centrifugal, acetone soln (200mL * 3 time) cleans, eccentric cleaning repeatable operation 3 times, centrifugal speed 800rpm, each centrifugation time 7min; Centrifugal product is placed in loft drier and is dried, and drying temperature is 40~45 ℃, and time of drying, 7h, obtained nano-Ag particles.
Nano-Ag particles 80g, Xylo-Mucine 24g, Natvosol 16g, BYK-02445g, BYK-02840g, Surfynol 46540g, pigment 8g are joined to mix and blend in glycerol 450g and ethylene glycol 400g, carry out again ultrasonic dispersion, filter, obtain nano silver conductive ink.

Claims (6)

1. the preparation method of a nano-graphite electrically conductive ink, the steps include: nano-Ag particles, Xylo-Mucine, Natvosol, BYK-024, BYK-028, Surfynol 465, pigment to join mix and blend in glycerol and ethylene glycol solution, carry out again ultrasonic dispersion, filter, obtain nano-graphite electrically conductive ink.
2. the preparation method of a kind of nano-graphite electrically conductive ink according to claim 1, is characterized in that: the mass ratio between described nano-Ag particles, Xylo-Mucine, Natvosol, BYK-024, BYK-028, Surfynol 465, pigment, glycerol, ethylene glycol is: 1:0.2~0.4:0.1~0.3:0.6~0.8:0.4~0.8:0.4~0.6:0.08~0.12:4.0~6.0:3.0~5.0.
3. the preparation method of a kind of nano-graphite electrically conductive ink according to claim 1, is characterized in that: the preparation method of described nano-Ag particles, the steps include: Silver Nitrate and polyvinylpyrrolidone to be added to the water dissolving; By concentration, be that 50~60mg/mL sodium borohydride solution is added dropwise in silver nitrate solution, rate of addition is 3~6mL/min; After dropwising, filter, get filtrate centrifugation, acetone soln cleaning, centrifugation, cleaning repeatable operation at least 3 times, centrifugal speed 800~1000rpm, each centrifugation time 7~8min; Centrifugal product is placed in loft drier and is dried, and drying temperature is 40~45 ℃, and time of drying, 7~8h, obtained nano-Ag particles.
4. the preparation method of a kind of nano-graphite electrically conductive ink according to claim 1, is characterized in that: the molar ratio of described Silver Nitrate, polyvinylpyrrolidone, sodium borohydride is: 1:0.3~0.5:2.4~2.8.
5. the preparation method of a kind of nano-graphite electrically conductive ink according to claim 1, is characterized in that: the particle diameter of described nano-Ag particles is less than 2nm.
6. the preparation method of a kind of nano-graphite electrically conductive ink according to claim 1, is characterized in that: described pigment is a kind of in following substances: C.I. is directly black 166, and C.I. directly black 19, C.I. directly black 168, C.I. acid yellow 23, C.I. Xylene Red 52, C.I. acid blue 9.
CN201310625014.8A 2013-11-28 2013-11-28 Preparation method of nano graphite conductive ink Pending CN103613986A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104610802A (en) * 2015-02-02 2015-05-13 芜湖市宝艺游乐科技设备有限公司 Waterproof polyethylene powder coating containing nanometer silver grafted colloidal graphite and preparation method of waterproof polyethylene powder coating
CN108975309A (en) * 2018-09-03 2018-12-11 南京林业大学 The method and its application of Water-soluble carbon quantum dot and fluorescent ink are prepared using cyanobacteria
CN110402276A (en) * 2017-03-14 2019-11-01 同和电子科技有限公司 The manufacturing method of the good silver nanowires dispersion liquid of line property detached from each other
CN111560188A (en) * 2020-06-01 2020-08-21 南京林业大学 Nano-silver/graphene composite electromagnetic shielding ink and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005350656A (en) * 2004-04-27 2005-12-22 Agfa Gevaert Nv Method for improving quality of dispersed composition
CN101560349A (en) * 2009-04-22 2009-10-21 北京印刷学院 Jet conductive ink
CN102220045A (en) * 2010-04-16 2011-10-19 上海亿金纳米科技有限公司 Low-temperature-sintered solvent-based nano-silver electroconductive ink and preparation process thereof
CN102504647A (en) * 2011-10-31 2012-06-20 天津大学 Conductive ink based on nano metal and application thereof in different jet printing methods and photographic paper

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005350656A (en) * 2004-04-27 2005-12-22 Agfa Gevaert Nv Method for improving quality of dispersed composition
CN101560349A (en) * 2009-04-22 2009-10-21 北京印刷学院 Jet conductive ink
CN102220045A (en) * 2010-04-16 2011-10-19 上海亿金纳米科技有限公司 Low-temperature-sintered solvent-based nano-silver electroconductive ink and preparation process thereof
CN102504647A (en) * 2011-10-31 2012-06-20 天津大学 Conductive ink based on nano metal and application thereof in different jet printing methods and photographic paper

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104610802A (en) * 2015-02-02 2015-05-13 芜湖市宝艺游乐科技设备有限公司 Waterproof polyethylene powder coating containing nanometer silver grafted colloidal graphite and preparation method of waterproof polyethylene powder coating
CN110402276A (en) * 2017-03-14 2019-11-01 同和电子科技有限公司 The manufacturing method of the good silver nanowires dispersion liquid of line property detached from each other
CN108975309A (en) * 2018-09-03 2018-12-11 南京林业大学 The method and its application of Water-soluble carbon quantum dot and fluorescent ink are prepared using cyanobacteria
CN111560188A (en) * 2020-06-01 2020-08-21 南京林业大学 Nano-silver/graphene composite electromagnetic shielding ink and preparation method thereof

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Application publication date: 20140305