CN105949884A - Preparation method of liquid phase stripping high-concentration graphene ink - Google Patents
Preparation method of liquid phase stripping high-concentration graphene ink Download PDFInfo
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- CN105949884A CN105949884A CN201610397015.5A CN201610397015A CN105949884A CN 105949884 A CN105949884 A CN 105949884A CN 201610397015 A CN201610397015 A CN 201610397015A CN 105949884 A CN105949884 A CN 105949884A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/52—Electrically conductive inks
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/38—Inkjet printing inks characterised by non-macromolecular additives other than solvents, pigments or dyes
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention discloses a preparation method of liquid phase stripping high-concentration graphene ink, and belongs to the field of chemical materials. In the process of preparing the graphene ink through liquid phase stripping under the high-energy shearing action of an ultrasonic wave, addition of ordinary organic dispersant can reduce electrical conductivity of print lines, the water solubility of graphene oxide is good, graphene oxide has the excellent electrical conductivity, after graphene oxide is used for graphene, graphene oxide can be distributed between graphene sheets in an intercalated mode, good dispersity is achieved, and porosity among graphene can be reduced through a connection function. The graphene ink can be used for printing key electronic devices in the fields of a print full electronic technology, radio-frequency identification systems, thin film switches, wearable textiles and the like.
Description
Technical field
The present invention relates to a kind of liquid phase and peel off the preparation method of high concentration graphene ink, belong to chemical materials neck
Territory.
Background technology
Along with the fast development of China's electronic technology, conductive ink has become as full printed electronics technology, wireless penetrates
The critical material in the fields such as identification system frequently, thin film open the light, wearable textile.Conductive ink is typically by conducting electricity
The component such as material, adhesive, additive and solvent is constituted, conductive material be generally gold, silver, copper, white carbon black,
The inorganic electronic conductors such as graphite.Compared with the ink of metal packing, carbon slurry, graphite, white carbon black, graphite oxide are made
The conductive ink low cost of conductive filler, light weight, good processability, adhesive force are good.Graphene is by monolayer carbon
Emerging two materials of atomic building, have the thin softness of matter, and intensity is big, the feature of heat-conductivity conducting superior performance,
For fields such as intelligent electronic label, RFID antenna, mobile phone faceplate, computor-keyboard and solar panels
Research and develop significant.
In the many application approaches of Graphene, prepare Graphene ink by liquid phase stripping method, then by stone
Ink alkene ink is applied to various base material with inkjet printing methods and remains Graphene large-scale production, high effect
One of important channel.During exploitation Graphene ink, the interpolation of various auxiliary agents can improve graphite
The concentration of alkene ink and stability, but the electric conductivity for Graphene ink creates negative effect, therefore develops
High concentration, the Graphene ink of high conductivity are highly important.
Summary of the invention
For the deficiencies in the prior art, a kind of liquid phase of offer is provided and peels off high concentration graphite
The preparation method of alkene ink.
For realizing aforementioned invention purpose, the technical scheme that the present invention takes is as follows:
(1) by the graphite flake of the 5-10g/L pre-dispersed 2-4h of ultrasound wave under the conditions of the dispersant of 5-15g/L；
(2) under Ultrasonic Conditions, in graphite flake pre-dispersed liquid, the graphene oxide of 1-3g/L is added by several times
Powder, continues ultrasonic 6-8h；
(3) by the centrifugal 1h under 11000rpm rotating speed of the dispersion liquid after ultrasonic Treatment, the supernatant is collected；
(4) supernatant is continued under 60 DEG C of environment ultrasound wave dispersion 2-3h, is reducing graphene layer further
While number, water is evaporated, make Graphene concentration reach 3-5g/L, obtain high concentration graphene ink.
Described dispersant is isopropanol, N, at least one in N '-dimethyl Methanamide, N-Methyl pyrrolidone.
Described graphene oxide is the dispersant of Graphene, does not interferes with the conduction printing Graphene lines after application
Property.
During preparing Graphene ink by the high energy shear effect liquid phase stripping of ultrasound wave, common organic dispersion
The electric conductivity adding membership reduction printing lines of agent, and graphene oxide good water solubility, itself just has excellence
Electric conductivity, after Graphene can be distributed in the way of intercalation between graphene film, play good dispersion
Property, but also can by interconnection function reduce between Graphene porosity, and then increase the conduction printing lines
Property.
Detailed description of the invention
In view of deficiency of the prior art, inventor, through studying for a long period of time and putting into practice in a large number, is proposed this
Bright technical scheme.Below in conjunction with some case study on implementation, the present invention is further detailed explanation.
Embodiment 1:
By the graphite flake of 6g/L ultrasonic pre-dispersed 4h under the conditions of the isopropanol of 15g/L, under ultrasound condition,
In graphite flake pre-dispersed liquid, add the graphene oxide powder of 3g/L by several times, continue ultrasonic 7h；After ultrasonic
Dispersion liquid centrifugal 1h under 11000rpm rotating speed, collect the supernatant, supernatant continued under 60 DEG C of environment
Continuous ultrasonic disperse, improves the dispersibility of Graphene while solvent evaporates further, continual ultrasonic 2h and get final product
High concentration graphene ink.
Embodiment 2:
By the graphite flake of 10g/L at N, the ultrasonic pre-dispersed 3h under N '-dimethyl stringency conditions of 10g/L,
Under ultrasound condition, in graphite flake pre-dispersed liquid, add the graphene oxide powder of 2g/L by several times, continue ultrasonic
7h；By the centrifugal 1h under 11000rpm rotating speed of the dispersion liquid after ultrasonic, collect the supernatant, by supernatant in
Continue ultrasonic disperse under 60 DEG C of environment, while solvent evaporates, improve the dispersibility of Graphene further, continue
Ultrasonic 3h i.e. obtains high concentration graphene ink.
Embodiment 3:
By the graphite flake of 5g/L ultrasonic pre-dispersed 2h under the conditions of the N-Methyl pyrrolidone of 6g/L, ultrasonic
Under the conditions of, in graphite flake pre-dispersed liquid, add the graphene oxide powder of 1g/L by several times, continue ultrasonic 7h；
Dispersion liquid after ultrasonic is centrifuged 1h under 11000rpm rotating speed, collects the supernatant, by supernatant in 60 DEG C
Continue ultrasonic disperse under environment, while solvent evaporates, improve the dispersibility of Graphene, continual ultrasonic further
2h i.e. obtains high concentration graphene ink.
High concentration graphene ink prepared by Example 1-3, tests its electric conductivity, each Specimen Determination 3
Secondary average.
| Sample | Electric conductivity |
| Embodiment 1 | 75.6KΩcm2 |
| Embodiment 2 | 78.4KΩcm2 |
| Embodiment 3 | 69.2KΩcm2 |
Should be appreciated that above-described embodiment is only technology design and the feature of the explanation present invention, its object is to allow ripe
The personage knowing technique will appreciate that present disclosure and implements according to this, can not limit the present invention's with this
Protection domain.All equivalence changes made according to spirit of the invention or modification, all should contain the present invention's
Within protection domain.
Claims (3)
1. the preparation method of a liquid phase stripping high concentration graphene ink, it is characterised in that include following step
Rapid:
(1) by the graphite flake of the 5-10g/L pre-dispersed 2-4h of ultrasound wave under the conditions of the dispersant of 5-15g/L；
(2) under Ultrasonic Conditions, in graphite flake pre-dispersed liquid, the graphene oxide of 1-3g/L is added by several times
Powder, continues ultrasonic 6-8h；
(3) by the centrifugal 1h under 11000rpm rotating speed of the dispersion liquid after ultrasonic Treatment, the supernatant is collected；
(4) supernatant is continued under 60 DEG C of environment ultrasound wave dispersion 2-3h, is reducing graphene layer further
While number, water is evaporated, make Graphene concentration reach 3-5g/L, obtain high concentration graphene ink.
A kind of liquid phase the most as claimed in claim 1 peels off the preparation method of high concentration graphene ink, and it is special
Levy and be that described dispersant is isopropanol, N, at least in N '-dimethyl Methanamide, N-Methyl pyrrolidone
Kind.
A kind of liquid phase the most as claimed in claim 1 peels off the preparation method of high concentration graphene ink, and it is special
Levy the dispersant being that described graphene oxide is Graphene, do not interfere with after application and print leading of Graphene lines
Electrically.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610397015.5A CN105949884A (en) | 2016-06-07 | 2016-06-07 | Preparation method of liquid phase stripping high-concentration graphene ink |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610397015.5A CN105949884A (en) | 2016-06-07 | 2016-06-07 | Preparation method of liquid phase stripping high-concentration graphene ink |
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| CN105949884A true CN105949884A (en) | 2016-09-21 |
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| CN201610397015.5A Pending CN105949884A (en) | 2016-06-07 | 2016-06-07 | Preparation method of liquid phase stripping high-concentration graphene ink |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106519804A (en) * | 2016-10-31 | 2017-03-22 | 湖南航天新材料技术研究院有限公司 | Graphene conductive ink as well as preparing method and application thereof |
| CN109036868A (en) * | 2018-09-07 | 2018-12-18 | 南京师范大学 | Graphene oxide assists liquid phase removing preparing graphite alkene/graphene oxide composite material method and its composite material and application |
| WO2020181713A1 (en) * | 2019-03-12 | 2020-09-17 | 上海集成电路研发中心有限公司 | Method for preparing aqueous graphene oxide ink |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101974266A (en) * | 2010-09-30 | 2011-02-16 | 彩虹集团公司 | Low-temperature conductive carbon slurry and preparation method thereof |
| CN104973591A (en) * | 2014-04-11 | 2015-10-14 | 中国科学院上海硅酸盐研究所 | High-quality graphene and preparation method thereof |
-
2016
- 2016-06-07 CN CN201610397015.5A patent/CN105949884A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101974266A (en) * | 2010-09-30 | 2011-02-16 | 彩虹集团公司 | Low-temperature conductive carbon slurry and preparation method thereof |
| CN104973591A (en) * | 2014-04-11 | 2015-10-14 | 中国科学院上海硅酸盐研究所 | High-quality graphene and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106519804A (en) * | 2016-10-31 | 2017-03-22 | 湖南航天新材料技术研究院有限公司 | Graphene conductive ink as well as preparing method and application thereof |
| CN106519804B (en) * | 2016-10-31 | 2019-12-13 | 长沙新材料产业研究院有限公司 | Graphene conductive ink and preparation method and application thereof |
| CN109036868A (en) * | 2018-09-07 | 2018-12-18 | 南京师范大学 | Graphene oxide assists liquid phase removing preparing graphite alkene/graphene oxide composite material method and its composite material and application |
| WO2020181713A1 (en) * | 2019-03-12 | 2020-09-17 | 上海集成电路研发中心有限公司 | Method for preparing aqueous graphene oxide ink |
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Application publication date: 20160921 |
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