CN106398397A - Method for preparing monodisperse graphene based nano silver composite - Google Patents
Method for preparing monodisperse graphene based nano silver composite Download PDFInfo
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- CN106398397A CN106398397A CN201610705162.4A CN201610705162A CN106398397A CN 106398397 A CN106398397 A CN 106398397A CN 201610705162 A CN201610705162 A CN 201610705162A CN 106398397 A CN106398397 A CN 106398397A
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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
Abstract
The invention discloses a method for preparing a monodisperse graphene based nano silver composite, and the method comprises the following steps: first, ultrasonic dispersion of graphene oxide in water, drop-wise addition of a silver ammonia solution and a sodium citrate solution, and after even mixing, repeated ultrasonic treating and ice water cooling until complete reaction; and after the reaction is completed, filtration by suction, washing and drying to obtain the monodisperse graphene based nano silver composite. The method does not need to add any stabilizer, and uses nontoxic sodium citrate as a reducing agent, and the process is simple. Nano silver in the monodisperse graphene based nano silver composite prepared by the method has a particle size of single dispersion, and the monodisperse graphene based nano silver composite is expected to be better applied in Raman enhanced substrates and catalysts. The monodisperse graphene based nano silver composite prepared by the method is hydrophilic, can stably exist for a month in the water without addition of any surfactant, and can replace general conductive ink for realization of with high conductivity and high flexibility.
Description
Technical field
The present invention relates to field of nanocomposite materials, more particularly to a kind of preparation side of graphene-based nano-ag composite
Method, is directed to the technology of preparing of conductive ink.
Background technology
Graphene has high electron mobility, excellent thermal conductivity and high resiliency mould due to its special electronic structure
Amount.Nano Silver, because its huge specific surface area is while keeping block silver high conductivity, high-termal conductivity, has higher work
Property and lower fusing point, additionally have good bactericidal properties and photocatalytic.Grapheme material and the combination of nano silver material
The performance that can be made them gets a promotion in some aspects, and as more preferable in electric conductivity, pliability is more excellent.The combination of the two makes this new
Composite receive much attention, and obtained in the fields such as conducting resinl, transparency electrode, conductive ink and sensor important should
With.
In recent years, the preparation of graphene-based nano silver composite material has become a new study hotspot, and such as Zhou etc. uses
One-step method grown different nano-Ag particles in single-layer graphene oxide and redox graphene, and its particle diameter is from several
Ten nanometers are all distributed (Zhou X, Huang X, Qi X, et al. In situ synthesis of in micrometer range
metal nanoparticles on single-layer graphene oxide and reduced graphene oxide
surfaces[J]. Journal of Physical Chemistry C, 2009, 113(25):10842)；Tien etc. utilizes
Nano Silver particle diameter in the compound that sodium borohydride and ethylene glycol two-step method reduced graphene and silver nitrate obtain is 13 ± 3 nm,
But its agents useful for same concentration is low, and experimental period is long, and the sodium borohydride used has strong reducing property, belongs to hazardous chemical
(Tien H W, Huang Y L, Yang S Y, et al. The production of graphene nanosheets
decorated with silver nanoparticles for use in transparent, conductive films
[J]. Carbon, 2011, 49(5):1550).Xu etc. is combined using glucose reduced graphene and silver nitrate under room temperature
Thing is although experiment is more simple and convenient, but the particle diameter of Nano Silver is not concentrated, and reunite more serious (Xu C, Wang X.
Fabrication of flexible metal-nanoparticle films using graphene oxide sheets
as substrates[J]. Small, 2009, 5(19):2212).The particle size of these methods or preparation is larger, point
Cloth is uneven；Or the reactant using low concentration, reaction rate is slow, efficiency is low；Or need using poisonous strong reductant.
It is therefore desirable to a kind of safety of exploitation, quick, the again higher method of the performance of Nano Silver is preparing graphene-based Nano Silver simultaneously
Compound.
Content of the invention
The invention aims to overcome that process complexity in prior art is loaded down with trivial details, the poisonous harm of chemical reagent, Nano Silver
Particle dispersity is poor, the defect of complex stabilities difference, provide a kind of simple, quickly prepare high performance graphene-based Nano Silver
The preparation method of compound.
To achieve these goals, the present invention provides a kind of side preparing monodispersed graphene-based nano-ag composite
Method, step is：
S1 adds graphene oxide in water, ultrasonic disperse 10-60 min, and the graphene oxide obtaining 0.5-3 mg/mL divides
Dispersion liquid, dropping concentrated ammonia liquor adjusts pH to 7-9 stand-by；
S2 is by AgNO3It is dissolved in the silver nitrate solution obtaining in deionized water that concentration is 0.05-0.35 M, then drip 2- thereto
10 % ammoniacal liquor just dissolve until the initial precipitation producing, and make silver ammino solution stand-by；
S3 stirs 5-40 min after mixing graphene oxide dispersion with silver ammino solution at 0-25 DEG C；Slow thereto again
The aqueous solution of the dropping sodium citrate of g containing 0.3-1.0, stirs 3-10 min；
Mixed solution in ultrasonic 5-40 min, is then cooled down 1-5 min in 0-25 DEG C of water-bath by S4；
The ultrasonically treated and water cooling of S5 repeat step S4 is until reaction is complete；
Mixture after S6 terminates to reaction carries out suction filtration, washing and drying, obtains monodispersed graphene-based Nano Silver and is combined
Thing powder.
Water-bath in described step S4 is ice-water bath.
In described step S1, ultrasonically treated power is 200 W.
In described step S4, ultrasonically treated power is 200 W to 400W.
The reaction of described step S5 is entirely repeat step S4 five to seven times.
The uniform particle sizes of Nano Silver in the graphene-based nano-ag composite of present invention preparation, its particle size can be by adjusting
Section AgNO3Concentration is realizing：AgNO3Concentration is bigger, and particle diameter is bigger.The density that Nano Silver is distributed on Graphene can be by adjusting
AgNO3To realize with the mass ratio of graphene oxide：Mass ratio is bigger, and density is bigger.The graphene-based nanometer of present invention preparation
Nano Silver particle diameter in silver composite has monodispersity, is hopeful to obtain preferably should in Raman enhancing substrate, catalyst
With.The graphene-based nano-ag composite of present invention preparation has hydrophily and stability, is not required to add any surfactant
Just can substitute, in stable existence in water one month as long as, the ink-jet that general conductive ink realizes high conductivity, high flexibility
Print.
Brief description
Accompanying drawing 1 is that the graphene-based nano-ag composite of embodiment 1 preparation reacts UV-Visible absorption light when carrying out
Spectrogram.
Fig. 2 is the atomic force microscopy of the graphene-based nano-ag composite of embodiment 1 preparation.
Fig. 3 is the Raman scattering spectrogram of the graphene-based nano-ag composite of embodiment 2 preparation.
Fig. 4 is the atomic force microscopy of the graphene-based nano-ag composite of embodiment 2 preparation.
Fig. 5 is the atomic force microscopy of the graphene-based nano-ag composite of embodiment 3 preparation.
Specific embodiment
Hereinafter the specific embodiment of the present invention is described in detail.It should be appreciated that it is described herein concrete
Embodiment is merely to illustrate and explains the present invention, is not limited to the present invention.
Embodiment 1：
20 mg graphene oxides are dissolved in the ultra-pure water of 15 mL, ultrasonic disperse 30 min, pH to 8 adjusted by dropping concentrated ammonia liquor,
In ultrasonic cell disruptor, ultrasonic 30 min of 200 W obtain brown color liquid.By 0.2 g AgNO3It is dissolved in 10 ml ultra-pure waters
In, then drip 2% ammoniacal liquor thereto and just dissolve until the initial precipitation producing, make water white transparency silver ammino solution stand-by.0 ℃
Lower graphene oxide dispersion is mixed with silver ammino solution after stir 30 min.It is slowly added dropwise 20 mL more thereto and contain 0.42 g
The aqueous solution of sodium citrate, stirs 5 min.Mixed solution is cooled down 3 min after ultrasonic 30 min of 250 W in frozen water, continues
Continue and repeat ultrasonic and frozen water cooling down operation 7 times until reaction is complete.Mixture after reaction is terminated carries out suction filtration, washing, does
Graphene-based nano-ag composite powder is obtained after dry.Compound ink will be can get after composite powder ultrasonic disperse in water
Water, room temperature deposit 30 days after the no significant change of uv-visible absorption spectroscopy figure.
Fig. 1 is ultraviolet-visible when being carried out according to the graphene-based nano-ag composite reaction of the embodiment of the present invention 1 preparation
Optical absorption spectra figure.It will be seen from figure 1 that with the carrying out of reaction, compound slowly generates, react completely after about 240 min.
Spectrogram in 400 nm about strong absworption peak occurs, and peak shape is sharp, and symmetry preferably, shows that the particle diameter of Nano Silver is little and be distributed collection
In.After ultrasonic 240 min, absworption peak red shift, to 410 nm, shows that Nano Silver particle diameter has increased.
Fig. 2 is the atomic force microscopy of the graphene-based nano-ag composite according to the embodiment of the present invention 1 preparation.From
Fig. 2 can be seen that Nano Silver and is evenly distributed, and particle diameter has monodispersity.971 particle statistics particle diameters in the visual field are obtained averagely
Particle diameterD=18.1 nm.
Embodiment 2：
20 mg graphene oxides are dissolved in the ultra-pure water of 15 mL, ultrasonic disperse 30 min, pH to 8 adjusted by dropping concentrated ammonia liquor,
In ultrasonic cell disruptor, ultrasonic 30 min of 200 W obtain brown color liquid.By 0.3 g AgNO3It is dissolved in 10 ml ultra-pure waters
In, then drip 5% ammoniacal liquor thereto and just dissolve until the initial precipitation producing, make water white transparency silver ammino solution stand-by.20
30 min are stirred with silver ammino solution after graphene oxide dispersion being mixed at DEG C.It is slowly added dropwise 20 mL more thereto and contain 0.51
The aqueous solution of g sodium citrate, stirs 5 min.Mixed solution is cooled down 3 min after ultrasonic 30 min of 200 W in frozen water, continues
Continue and repeat ultrasonic and frozen water cooling down operation 6 times until reaction is complete.Mixture after reaction is terminated carries out suction filtration, washing, does
Graphene-based nano-ag composite powder is obtained after dry.Composite powder be can get compound conductive after ultrasonic disperse in water
Ink, room temperature deposit 30 days after the no significant change of uv-visible absorption spectroscopy figure.
Fig. 3 is the Raman scattering spectrogram of the graphene-based nano-ag composite according to the embodiment of the present invention 2 preparation.From Fig. 3
As can be seen that the Raman signal intensity having loaded the graphene oxide of silver is approximately 9 times of former graphene oxide, show that silver absorption exists
On graphene oxide fragment, enhance the intensity of Graphene.
Fig. 4 is the atomic force microscopy of the graphene-based nano-ag composite according to the embodiment of the present invention 2 preparation.From
Fig. 4 can be seen that Nano Silver and is evenly distributed, and particle diameter has monodispersity.1033 particle statistics particle diameters in the visual field must be put down
All particle diametersD=22.5 nm.
Embodiment 3：
30 mg graphene oxides are dissolved in the ultra-pure water of 15 mL, ultrasonic disperse 30 min, pH to 8 adjusted by dropping concentrated ammonia liquor,
In ultrasonic cell disruptor, ultrasonic 30 min of 200 W obtain brown color liquid.By 0.5 g AgNO3It is dissolved in 10 ml ultra-pure waters
In, then drip 10% ammoniacal liquor thereto and just dissolve until the initial precipitation producing, make water white transparency silver ammino solution stand-by.10
30 min are stirred with silver ammino solution after graphene oxide dispersion being mixed at DEG C.It is slowly added dropwise 20 mL more thereto and contain 1.0 g
The aqueous solution of sodium citrate, stirs 5 min.Mixed solution is cooled down 3 min after ultrasonic 30 min of 300 W in frozen water, continues
Continue and repeat ultrasonic and frozen water cooling down operation 7 times until reaction is complete.Mixture after reaction is terminated carries out suction filtration, washing, does
Graphene-based nano-ag composite powder is obtained after dry.Compound ink will be can get after composite powder ultrasonic disperse in water
Water, room temperature deposit 30 days after the no significant change of uv-visible absorption spectroscopy figure.
Fig. 5 is the atomic force microscopy of the graphene-based nano-ag composite according to the embodiment of the present invention 3 preparation.From
Fig. 5 can be seen that Nano Silver and is evenly distributed, and particle diameter has monodispersity.443 particle statistics particle diameters in the visual field are obtained averagely
Particle diameterD=46.4 nm.
Embodiment 4：
40 mg graphene oxides are dissolved in the ultra-pure water of 15 mL, ultrasonic disperse 30 min, pH to 8 adjusted by dropping concentrated ammonia liquor,
In ultrasonic cell disruptor, ultrasonic 30 min of 200 W obtain brown color liquid.By 0.2 g AgNO3It is dissolved in 10 ml ultra-pure waters
In, then drip 2% ammoniacal liquor thereto and just dissolve until the initial precipitation producing, make water white transparency silver ammino solution stand-by.0 ℃
Lower graphene oxide dispersion is mixed with silver ammino solution after stir 30 min.It is slowly added dropwise 20 mL more thereto and contain 0.35 g
The aqueous solution of sodium citrate, stirs 5 min.Mixed solution is cooled down 3 min after ultrasonic 30 min of 300 W in frozen water, continues
Continue and repeat ultrasonic and frozen water cooling down operation 7 times until reaction is complete.Mixture after reaction is terminated carries out suction filtration, washing, does
Graphene-based nano-ag composite powder is obtained after dry.Compound ink will be can get after composite powder ultrasonic disperse in water
Water, room temperature deposit 30 days after the no significant change of uv-visible absorption spectroscopy figure.
The preferred embodiment of the present invention described in detail above, but, the present invention is not limited in above-mentioned embodiment
Detail, in the range of the technology design of the present invention, multiple simple variant can be carried out to technical scheme, this
A little simple variant belong to protection scope of the present invention.
Claims (5)
1. a kind of method preparing monodispersed graphene-based nano-ag composite, step is：
S1 adds graphene oxide in water, ultrasonic disperse 10-60 min, and the graphene oxide obtaining 0.5-3 mg/mL divides
Dispersion liquid, dropping concentrated ammonia liquor adjusts pH to 7-9 stand-by；
S2 is by AgNO3It is dissolved in the silver nitrate solution obtaining in deionized water that concentration is 0.05-0.35 M, then drip 2-10 thereto
% ammoniacal liquor just dissolves until the initial precipitation producing, and makes silver ammino solution stand-by；
S3 stirs 5-40 min after mixing graphene oxide dispersion with silver ammino solution at 0-25 DEG C；Slow thereto again
The aqueous solution of the dropping sodium citrate of g containing 0.3-1.0, stirs 3-10 min；
Mixed solution in ultrasonic 5-40 min, is then cooled down 1-5 min in 0-25 DEG C of water-bath by S4；
The ultrasonically treated and water cooling of S5 repeat step S4 is until reaction is complete；
Mixture after S6 terminates to reaction carries out suction filtration, washing and drying, obtains monodispersed graphene-based Nano Silver and is combined
Thing powder.
2. a kind of method preparing monodispersed graphene-based nano-ag composite according to claim 1, its feature exists
In the water-bath in described step S4 is ice-water bath.
3. a kind of method preparing monodispersed graphene-based nano-ag composite according to claim 1, its feature exists
In in described step S1, ultrasonically treated power is 200 W.
4. a kind of method preparing monodispersed graphene-based nano-ag composite according to claim 1, its feature exists
In in described step S4, ultrasonically treated power is 200 W to 400W.
5. a kind of method preparing monodispersed graphene-based nano-ag composite according to claim 1, its feature exists
It is entirely S4 five to seven times in, described step S5 reaction.
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Cited By (7)
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| CN107445145A (en) * | 2017-08-09 | 2017-12-08 | 张家港市汇鼎新材料科技有限公司 | A kind of preparation method based on graphene composite material |
| CN107915221A (en) * | 2017-12-13 | 2018-04-17 | 天津宝兴威科技股份有限公司 | A kind of preparation method of the strong stannic oxide/graphene nano ag material of antibiotic property |
| CN108645837A (en) * | 2018-05-11 | 2018-10-12 | 哈尔滨工业大学深圳研究生院 | A kind of preparation method and applications of Ag@NGO composite nano materials |
| CN109535847A (en) * | 2018-11-26 | 2019-03-29 | 国宏中晶集团有限公司 | The electrically conductive ink and preparation method and flexible-paper-base conducting wire of a kind of containing graphene |
| CN111423834A (en) * | 2020-04-01 | 2020-07-17 | 徐文忠 | Preparation method of sintered graphene/nano-silver composite conductive adhesive |
| CN111972435A (en) * | 2019-05-24 | 2020-11-24 | 浙江海纳新材料科技有限公司 | Preparation method of nano-silver-graphene oxide composite material |
| WO2021133161A1 (en) * | 2019-12-24 | 2021-07-01 | Mimos Berhad | A method for preparing a graphene-based inkjet ink |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107445145A (en) * | 2017-08-09 | 2017-12-08 | 张家港市汇鼎新材料科技有限公司 | A kind of preparation method based on graphene composite material |
| CN107915221A (en) * | 2017-12-13 | 2018-04-17 | 天津宝兴威科技股份有限公司 | A kind of preparation method of the strong stannic oxide/graphene nano ag material of antibiotic property |
| CN108645837A (en) * | 2018-05-11 | 2018-10-12 | 哈尔滨工业大学深圳研究生院 | A kind of preparation method and applications of Ag@NGO composite nano materials |
| CN108645837B (en) * | 2018-05-11 | 2021-07-20 | 哈尔滨工业大学深圳研究生院 | Preparation method and application of Ag @ NGO composite nano material |
| CN109535847A (en) * | 2018-11-26 | 2019-03-29 | 国宏中晶集团有限公司 | The electrically conductive ink and preparation method and flexible-paper-base conducting wire of a kind of containing graphene |
| CN109535847B (en) * | 2018-11-26 | 2021-12-28 | 国宏中晶集团有限公司 | Graphene-containing conductive ink, preparation method thereof and flexible paper-based conductive circuit |
| CN111972435A (en) * | 2019-05-24 | 2020-11-24 | 浙江海纳新材料科技有限公司 | Preparation method of nano-silver-graphene oxide composite material |
| WO2021133161A1 (en) * | 2019-12-24 | 2021-07-01 | Mimos Berhad | A method for preparing a graphene-based inkjet ink |
| CN111423834A (en) * | 2020-04-01 | 2020-07-17 | 徐文忠 | Preparation method of sintered graphene/nano-silver composite conductive adhesive |
| CN111423834B (en) * | 2020-04-01 | 2021-08-17 | 徐文忠 | Preparation method of sintered graphene/nano-silver composite conductive adhesive |
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Application publication date: 20170215 |