CN108314932A - One kind being based on photocuring Graphene conductive ink printing process - Google Patents
One kind being based on photocuring Graphene conductive ink printing process Download PDFInfo
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- CN108314932A CN108314932A CN201810040618.9A CN201810040618A CN108314932A CN 108314932 A CN108314932 A CN 108314932A CN 201810040618 A CN201810040618 A CN 201810040618A CN 108314932 A CN108314932 A CN 108314932A
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M5/00—Duplicating or marking methods; Sheet materials for use therein
- B41M5/0011—Pre-treatment or treatment during printing of the recording material, e.g. heating, irradiating
- B41M5/0017—Application of ink-fixing material, e.g. mordant, precipitating agent, on the substrate prior to printing, e.g. by ink-jet printing, coating or spraying
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M5/00—Duplicating or marking methods; Sheet materials for use therein
- B41M5/0023—Digital printing methods characterised by the inks used
-
- 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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- Chemical & Material Sciences (AREA)
- 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 present invention relates to electrically conductive ink technical fields, disclose one kind and being based on photocuring Graphene conductive ink printing process, include the following steps：S1. Graphene conductive ink is prepared：10~30 parts of graphenes, 10~20 parts of chlorinated polypropylenes, 20~60 parts of solvents, 8~20 parts of graphene quantum dots, 20~70 parts of monomers, 1~5 part of crosslinking agent and 1~10 part of auxiliary agent are mixed, carry out ultrasonic disperse, then dispersion is transferred in grinder and is ground, until ink fineness be less than 10 μm, obtain Graphene conductive ink；S2. ink-jet：Light curing agent is added in the Graphene conductive ink obtained to step S1, addition is 0.1~1wt% of monomer, and on the surface of the substrate by design configuration spraying, whole process is carried out under the atmosphere of ultraviolet light or laser beam, and wavelength is 365~405nm.
Description
Technical field
The present invention relates to electrically conductive ink technical fields, and photocuring Graphene conductive ink is based on more particularly, to one kind
Printing process.
Background technology
With the high speed development of science and technology, the large-scale use of integrated circuit, microelectronic component increasingly minimizes, printing electricity
The electronic circuit of road, intelligent label, flexible display device, sensor etc. is also to small, fining, various sexual development, to leading
The demand of electric ink is increasing.
Graphene (Graphene) is a kind of honey comb like two-dimensional structure flat thin of the hexagonal lattice being made of sp2 carbon atoms
Film and two-dimensional material are the another great discoveries after carbon nanotube, fullerene.It is special that graphene shows novel physics
Property, single-layer graphene has the good transparency, only absorbs 2.3% light；Its electron mobility is more than 15000cm under room temperature2/V·s.Graphene has excellent electric conductivity and physical mechanical property, and laterally (in face) conductivity is up to 106S/m, the limit are strong
Degree is up to 130GPa, stretch modulus 1.01TPa, and good heat conductivity, thermal conductivity are 5000W/ (mK), and density is only 1.3
~2g/cm3.It is chemically and thermally had excellent performance since graphene has, the spy that conductivity is big, large specific surface area, mechanical strength are big
Property so that the material based on graphene has extensive industrial applicability, and adsorbent, catalyst carrier, heat can be used to pass
The fields such as defeated media, composite material, electronic component, battery/capacitor.
Occurs graphene ink currently on the market.There are lamellar interfaces when however, preparing conductive material using graphene
Resistance, prepared electrically conductive ink are easily reunited, bad dispersibility, and practical electric conductivity has a long way to go with graphene theory electric conductivity.Mesh
Preceding to ensure that it leads performance by the way of adding nano silver in graphene, the additive amount of this method nano silver is generally higher than
50wt%；The preparation of nano silver also very complicated, this undoubtedly increases production cost；In addition, in the electrically conductive ink of this state
Graphene and nano silver are solid-state, and the dispersion of particle and certain mode of printings (such as ink-jet, direct write) are applied in being prepared to ink
Bring difficulty.
The core technology of ink-jet method making pcb board is the development of electrically conductive ink, and conductive path is made using ink-jet technology,
It can be used for extremely fine wiring diagram, and minimum line width and minimum line spacing can be reduced to obtain high-density circuit figure
Case, although the power of conductive coating can be improved by being suitably added heat reactive resin under conditions of ensureing that resistivity can reach requirement
Performance is learned, but heat reactive resin curing rate is slow, is unfavorable for improving the resolution ratio of pcb board.Simultaneously because heat reactive resin
Solidification temperature is higher, and the requirement to substrate material high temperature resistance is harsh.
Invention content
The technical problems to be solved of the present invention are that in view of the deficiencies of the prior art introducing graphene quantum dot, which is used as, to be added
Add agent to be added to Graphene conductive ink, and light is drawn into method and ink-jet method combination, provides a kind of based on photocuring graphene
Electrically conductive ink printing process.
The purpose of the present invention is achieved by the following technical programs：
One kind is provided and is based on photocuring Graphene conductive ink printing process, is included the following steps：
S1. Graphene conductive ink is prepared：
By 10~30 parts of graphenes, 10~20 parts of chlorinated polypropylenes, 20~60 parts of solvents, 8~20 parts of graphene amounts
Sub- point, 20~70 parts of monomers, 1~5 part of crosslinking agent and 1~10 part of auxiliary agent mixing, carry out ultrasonic disperse, then shift dispersion
It is ground in grinder, using Hegman grind gage testing conductive ink fineness, until ink fineness is less than 10 μm, obtains stone
Black alkene electrically conductive ink；
S2. ink-jet：
Light curing agent (photoinitiator) is added in the Graphene conductive ink obtained to step S1, addition is monomer
0.1~1wt%, on the surface of the substrate by design configuration spraying, whole process is carried out under the atmosphere of ultraviolet light or laser beam,
Wavelength is 365~405nm.
Graphene quantum dot is introduced in step S1 of the present invention and is added to Graphene conductive ink as additive, further
The dispersibility for increasing graphene, prevents from reuniting, and compares high molecular surfactant and dispersant, and will not introduce new impurity reduces
Electric conductivity；In step S2 by light curing agent ultraviolet light or laser beam effect so that organic monomer be chemically crosslinked or object
Reason is cross-linked into three-dimensional network-like structure, and graphene is got up by polymer molecule or polymer monomer package isolation immediately, effective gram
Graphene has been taken from the generation reunited, has improved electric conductivity.
The present invention improves the resolution ratio of PCB, ink jet process is always in certain ultraviolet light or laser to reduce hardening time
It being carried out under the atmosphere of beam, so as to accelerate the polymerization of organic monomer so that the electrically conductive ink for being sprayed on substrate surface cures rapidly, when
The conductive film being fully cured is can be obtained after the completion of ink-jet, and due to being no longer needed under the atmosphere of ultraviolet light or laser beam
Sintering.
Further, graphene described in step S1 is the graphene less than five layers, ensures electric conductivity.
Further, solvent described in step S1 is one or both of water, dimethylbenzene, butanone or three kinds.
Further, graphene quantum dot described in step S1 is various carbon sources through strong acid oxidizing process, Two-step anodization, water
What hot method or solvent-thermal method were prepared.
Further, monomer described in step S1 is N, N- methylene bisacrylamide acyls.
Further, crosslinking agent described in step S1 is methylene-bisacrylamide.
Further, auxiliary agent described in step S1 is at least one of antifoaming agent, levelling agent.
Further, ultrasonic power described in step S1 is 1000~1200W, and the time is 40~60min.
Further, light curing agent described in step S2 is light curing agent 819.
Further, substrate described in step S2 is appointing for glass, polyester film, polyamide film or polycarbonate film
Meaning is a kind of.
Compared with prior art, the beneficial effects of the invention are as follows：
Present invention introduces graphene quantum dots to be added to as additive in Graphene conductive ink, utilizes graphene quantum
Point good dispersibility, and its stronger noncovalent interaction between graphene sheet layer in a solvent, promotes graphene in solvent
Stable dispersion, compare conventional polymer surfactant and dispersant, will not introduce new impurity reduces electric conductivity.
The present invention draws method, in graphene solution on the basis of obtaining the graphene solution of good dispersion in conjunction with light
Monomer and crosslinking agent is added, by light curing agent so that monomer chemistries crosslinking or physical crosslinking are at three-dimensional network-like structure, graphite
Alkene is got up by polymer molecule or polymer monomer package isolation immediately, can not only effectively overcome graphene from the hair reunited
It is raw, improve electric conductivity.
The present invention draws method using light, by light curing agent (photoinitiator) under the action of ultraviolet light or laser beam, makes
Coating rapid curing is obtained, can be obtained the conductive film being fully cured after the completion of ink-jet, heat cure or sintering is compared, reduces
Hardening time improves the discrimination efficiency of PCB, the high temperature resistance no requirement (NR) to substrate.
Present invention thermoplastic resin chlorinated polypropylene has stronger bonding force to polypropylene, polyethylene, to paper,
The materials such as PET have good bonding.
Specific implementation mode
It is further illustrated the present invention with reference to specific embodiment.Following embodiment is only illustrative examples, not structure
At inappropriate limitation of the present invention, the multitude of different ways that the present invention can be limited and be covered by invention content is implemented.Unless special
Do not mentionlet alone bright, reagent, compound and the equipment that the present invention uses is the art conventional reagent, compound and equipment.
Embodiment 1
The present embodiment provides one kind being based on photocuring Graphene conductive ink printing process, includes the following steps：
S1. Graphene conductive ink is prepared：
10 parts of graphenes, 10 parts of chlorinated polypropylenes, 20 parts of water, 8 parts of graphene quantum dots, 20 parts of monomers N, N- are sub-
The double acryloyls of methyl, 1~5 part of crosslinking agent methylene-bisacrylamide, 0.5 part of antifoaming agent, 0.5 part of levelling agent mixing, are surpassed
Sound disperses, and ultrasonic power is 1000~1200W, and the time is 40~60min, and then dispersion is transferred in grinder and is ground
Mill until ink fineness is less than 10 μm, obtains Graphene conductive ink using Hegman grind gage testing conductive ink fineness；
S2. ink-jet：
Light curing agent 819 is added in the Graphene conductive ink obtained to step S1, addition is the 0.1wt% of monomer,
By design configuration spraying on the surface of the substrate, whole process is carried out under the atmosphere of ultraviolet light or laser beam, wavelength be 365~
405nm。
Wherein, graphene described in step S1 is the graphene less than five layers, and the graphene quantum dot is various carbon sources
It is prepared through strong acid oxidizing process, Two-step anodization, hydro-thermal method or solvent-thermal method.
Substrate described in step S2 is any one of glass, polyester film, polyamide film or polycarbonate film.
Embodiment 2
The present embodiment provides one kind being based on photocuring Graphene conductive ink printing process, includes the following steps：
S1. Graphene conductive ink is prepared：
By 20 parts of graphenes, 15 parts of chlorinated polypropylenes, 30 parts of dimethylbenzene, 12 parts of graphene quantum dots, 40 parts of monomers
N, N- methylene bisacrylamide acyl, 2 parts of crosslinking agent methylene-bisacrylamides, 2 parts of antifoaming agent, 8 parts of levelling agent mixing, carry out ultrasound
Dispersion, ultrasonic power are 1000~1200W, and the time is 40~60min, and then dispersion is transferred in grinder and is ground
Mill until ink fineness is less than 10 μm, obtains Graphene conductive ink using Hegman grind gage testing conductive ink fineness；
S2. ink-jet：
Light curing agent 819 is added in the Graphene conductive ink obtained to step S1, addition is the 0.5wt% of monomer,
By design configuration spraying on the surface of the substrate, whole process is carried out under the atmosphere of ultraviolet light or laser beam, wavelength be 365~
405nm。
Wherein, graphene described in step S1 is the graphene less than five layers, and the graphene quantum dot is various carbon sources
It is prepared through strong acid oxidizing process, Two-step anodization, hydro-thermal method or solvent-thermal method.
Substrate described in step S2 is any one of glass, polyester film, polyamide film or polycarbonate film.
Embodiment 3
The present embodiment provides one kind being based on photocuring Graphene conductive ink printing process, includes the following steps：
S1. Graphene conductive ink is prepared：
By 25 parts of graphenes, 10 parts of chlorinated polypropylenes, 50 parts of butanone, 16 parts of graphene quantum dots, 60 parts of monomer N,
N- methylene bisacrylamides acyl, 4 parts of crosslinking agent methylene-bisacrylamides and 5 parts of antifoaming agent mixing, carry out ultrasonic disperse, ultrasonic work(
Rate is 1000~1200W, and the time is 40~60min, and then dispersion is transferred in grinder and is ground, thin using scraper plate
Degree measurement examination electrically conductive ink fineness, until ink fineness be less than 10 μm, obtain Graphene conductive ink；
S2. ink-jet：
Light curing agent 819 is added in the Graphene conductive ink obtained to step S1, addition is the 0.8wt% of monomer,
By design configuration spraying on the surface of the substrate, whole process is carried out under the atmosphere of ultraviolet light or laser beam, wavelength be 365~
405nm。
Wherein, graphene described in step S1 is the graphene less than five layers, and the graphene quantum dot is various carbon sources
It is prepared through strong acid oxidizing process, Two-step anodization, hydro-thermal method or solvent-thermal method.
Substrate described in step S2 is any one of glass, polyester film, polyamide film or polycarbonate film.
Embodiment 4
The present embodiment provides one kind being based on photocuring Graphene conductive ink printing process, includes the following steps：
S1. Graphene conductive ink is prepared：
By 30 parts of graphenes, 20 parts of chlorinated polypropylenes, 60 parts of butanone, 20 parts of graphene quantum dots, 70 parts of monomer N,
N- methylene bisacrylamides acyl, 5 parts of crosslinking agent methylene-bisacrylamides and 5 parts of antifoaming agent mixing, carry out ultrasonic disperse, ultrasonic work(
Rate is 1000~1200W, and the time is 40~60min, and then dispersion is transferred in grinder and is ground, thin using scraper plate
Degree measurement examination electrically conductive ink fineness, until ink fineness be less than 10 μm, obtain Graphene conductive ink；
S2. ink-jet：
Light curing agent 819 is added in the Graphene conductive ink obtained to step S1, addition is the 1wt% of monomer, is pressed
Design configuration spray on the surface of the substrate, whole process is carried out under the atmosphere of ultraviolet light or laser beam, wavelength be 365~
405nm。
Wherein, graphene described in step S1 is the graphene less than five layers, and the graphene quantum dot is various carbon sources
It is prepared through strong acid oxidizing process, Two-step anodization, hydro-thermal method or solvent-thermal method.
Substrate described in step S2 is any one of glass, polyester film, polyamide film or polycarbonate film.
Comparative example 1
This comparative example is substantially the same manner as Example 1, the difference is that, do not add graphene quantum dot in step S1.
Comparative example 2
This comparative example is substantially the same manner as Example 1, the difference is that, monomer and crosslinking agent, phase are not added in step S1
It answers in ground step S2 and does not add light curing agent 819, specifically include following steps：
S1. Graphene conductive ink is prepared：
By 10 parts of graphenes, 10 parts of chlorinated polypropylenes, 20 parts of water, 8 parts of graphene quantum dots, 0.5 part of antifoaming agent,
0.5 part of levelling agent mixing carries out ultrasonic disperse, and ultrasonic power is 1000~1200W, and the time is 40~60min, then will dispersion
Object is transferred in grinder and is ground, using Hegman grind gage testing conductive ink fineness, until ink fineness is less than 10 μm,
Obtain Graphene conductive ink；
S2. ink-jet：
The Graphene conductive ink that step S1 is obtained is sprayed by design configuration on the surface of the substrate, after ambient temperature curing
It is sintered, sintering temperature is 150~250 DEG C, and sintering time is 60~300min.
Wherein, graphene described in step S1 is the graphene less than five layers, and the graphene quantum dot is various carbon sources
It is prepared through strong acid oxidizing process, Two-step anodization, hydro-thermal method or solvent-thermal method.
Substrate described in step S2 is any one of glass, polyester film, polyamide film or polycarbonate film.
It is 60~180min that this comparative example cures average time in room temperature, and sintering temperature is up to 150~250 DEG C, unfavorable
It is and very high to substrate heat resistant requirements in the resolution ratio for improving pcb board, while graphene is in the cured process of electrically conductive ink
In, it may occur that from reuniting, to reduce electric conductivity.
Performance test and characterization
Examples 1 to 4 and comparative example 1~2 are tested for the property, the results are shown in Table 1.
Table 1
The present invention illustrates the detailed process equipment and processing step of the present invention, people in the art by above-described embodiment
Member is not it should be appreciated that the present invention is limited by above-described embodiment, and the above embodiments and description only describe the present invention
Principle, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, this is to this field
It is it will be apparent that these changes and improvements all fall within the protetion scope of the claimed invention for technical staff.
Claims (10)
1. one kind being based on photocuring Graphene conductive ink printing process, which is characterized in that include the following steps：
S1. Graphene conductive ink is prepared：
By 10~30 parts of graphenes, 10~20 parts of chlorinated polypropylenes, 20~60 parts of solvents, 8~20 parts of graphene quantum dots,
20~70 parts of monomers, 1~5 part of crosslinking agent and 1~10 part of auxiliary agent mixing, carry out ultrasonic disperse, are then transferred to dispersion and grind
Be ground in grinding machine, until ink fineness be less than 10 μm, obtain Graphene conductive ink；
S2. ink-jet：
Light curing agent is added in the Graphene conductive ink obtained to step S1, addition is 0.1~1wt% of monomer, by design
Figure sprays on the surface of the substrate, and whole process is carried out under the atmosphere of ultraviolet light or laser beam, and wavelength is 365~405nm.
2. being based on photocuring Graphene conductive ink printing process according to claim 1, which is characterized in that institute in step S1
It is the graphene less than five layers to state graphene.
3. being based on photocuring Graphene conductive ink printing process according to claim 1, which is characterized in that institute in step S1
It is any one in water, dimethylbenzene, butanone to state solvent.
4. being based on photocuring Graphene conductive ink printing process according to claim 1, which is characterized in that institute in step S1
The various carbon sources of graphene quantum dot are stated to be prepared through strong acid oxidizing process, Two-step anodization, hydro-thermal method or solvent-thermal method.
5. being based on photocuring Graphene conductive ink printing process according to claim 1, which is characterized in that institute in step S1
It is N, N- methylene bisacrylamide acyls to state monomer.
6. being based on photocuring Graphene conductive ink printing process according to claim 1, which is characterized in that institute in step S1
It is methylene-bisacrylamide to state crosslinking agent.
7. being based on photocuring Graphene conductive ink printing process according to claim 1, which is characterized in that institute in step S1
State at least one that auxiliary agent is antifoaming agent, levelling agent.
8. being based on photocuring Graphene conductive ink printing process according to claim 1, which is characterized in that institute in step S1
It is 1000~1200W to state ultrasonic power, and the time is 40~60min.
9. being based on photocuring Graphene conductive ink printing process according to claim 1, which is characterized in that institute in step S2
It is light curing agent 819 to state light curing agent.
10. being based on photocuring Graphene conductive ink printing process according to claim 1, which is characterized in that in step S2
The substrate is any one of glass, polyester film, polyamide film or polycarbonate film.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110337191A (en) * | 2019-07-03 | 2019-10-15 | 常州轻工职业技术学院 | A method of the 3D printing great power LED printed circuit board based on Graphene conductive ink |
| CN112876907A (en) * | 2021-03-03 | 2021-06-01 | 郝宝民 | Preparation method of photo-cured graphene conductive ink |
| CN113201246A (en) * | 2021-04-24 | 2021-08-03 | 深圳市撒比斯科技有限公司 | High-conductivity photosensitive electronic ink |
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| CN110337191A (en) * | 2019-07-03 | 2019-10-15 | 常州轻工职业技术学院 | A method of the 3D printing great power LED printed circuit board based on Graphene conductive ink |
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| CN113201246A (en) * | 2021-04-24 | 2021-08-03 | 深圳市撒比斯科技有限公司 | High-conductivity photosensitive electronic ink |
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Application publication date: 20180724 |